A Chiral Cyclometalated Iridium Star of David [2]Catenane.
August, David P.; Jaramillo-Garcia, Javier; Leigh, David A.; Valero, Alberto; Vitorica-Yrezabal, Iñigo J; Journal of the American Chemical Society 143 (2021) 1154–1161; doi:10.1021/jacs.0c12038

data_4135572
_publ_section_title
;
 A Chiral Cyclometalated Iridium Star of David [2]Catenane.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1154
_journal_page_last               1161
_journal_paper_doi               10.1021/jacs.0c12038
_journal_volume                  143
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C276 H224 Ir2 N32 O4 Zn4, 10(F6 P)'
_chemical_formula_sum            'C276 H224 F60 Ir2 N32 O4 P10 Zn4'
_chemical_formula_weight         6148.44
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                104.102(4)
_cell_angle_beta                 106.303(6)
_cell_angle_gamma                107.895(5)
_cell_formula_units_Z            2
_cell_length_a                   23.3169(15)
_cell_length_b                   27.5437(10)
_cell_length_c                   27.5621(19)
_cell_measurement_reflns_used    10796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.4800
_cell_measurement_theta_min      1.4690
_cell_volume                     15076.1(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.294
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  2  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 120.00  169
  3  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 240.00  169
  4  \f      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
;
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283522000
_diffrn_orient_matrix_UB_12      -0.0093231000
_diffrn_orient_matrix_UB_13      -0.0224811000
_diffrn_orient_matrix_UB_21      0.0029140000
_diffrn_orient_matrix_UB_22      0.0264965000
_diffrn_orient_matrix_UB_23      0.0042169000
_diffrn_orient_matrix_UB_31      0.0178925000
_diffrn_orient_matrix_UB_32      0.0022977000
_diffrn_orient_matrix_UB_33      -0.0160411000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.1154
_diffrn_reflns_Laue_measured_fraction_full 0.294
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63473
_diffrn_reflns_point_group_measured_fraction_full 0.281
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         15.995
_diffrn_reflns_theta_min         1.471
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             6200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 5674 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.204(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.759
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2429
_refine_ls_number_reflns         30691
_refine_ls_number_restraints     6149
_refine_ls_restrained_S_all      1.911
_refine_ls_R_factor_all          0.2053
_refine_ls_R_factor_gt           0.1400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3240
_refine_ls_wR_factor_ref         0.3499
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.268
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                16897
_reflns_number_total             30691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c12038_si_002.cif
_cod_data_source_block           m_av435a_3_col1_
_cod_original_cell_volume        15076.1(17)
_cod_database_code               4135572
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.887
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     18.25
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C259-C258
 1.45 with sigma of 0.002
 C259-C257
 2.4 with sigma of 0.002
 C253-C259
 2.4 with sigma of 0.002
 C260-C258
 2.4 with sigma of 0.002
 C264-C258
 2.4 with sigma of 0.002
 C96-C100
 2.4 with sigma of 0.002
 C104-C96
 2.4 with sigma of 0.002
 C516-C517
 1.45 with sigma of 0.002
 C735-C736 = C735-C734 = C732-C733 = C731-C732
 1.5 with sigma of 0.01
 C734-C733
 1.35 with sigma of 0.005
 C737-C735
 2.4 with sigma of 0.02
 C734-C736
 2.4 with sigma of 0.02
 C735-C733
 2.4 with sigma of 0.02
 C734-C732
 2.4 with sigma of 0.02
 C733-C731
 2.4 with sigma of 0.02
 C505-C504 = C510-C511
 1.45 with sigma of 0.002
 C509-C508 = C509-C510 = C506-C505 = C506-C507
 1.5 with sigma of 0.01
 C508-C507
 1.35 with sigma of 0.005
 C511-C509
 2.4 with sigma of 0.02
 C510-C508
 2.4 with sigma of 0.02
 C509-C507
 2.4 with sigma of 0.02
 C508-C506
 2.4 with sigma of 0.02
 C507-C505
 2.4 with sigma of 0.02
 C506-C504
 2.4 with sigma of 0.02
 C503-C505 = C505-C499
 2.4 with sigma of 0.02
 C516-C510 = C510-C512
 2.4 with sigma of 0.02
 C105-C104 = C110-C111
 1.45 with sigma of 0.002
 C111-C109
 2.4 with sigma of 0.02
 C110-C108
 2.4 with sigma of 0.02
 C108-C106
 2.4 with sigma of 0.02
 C106-C104
 2.4 with sigma of 0.02
 O213-C214
 1.45 with sigma of 0.002
 C254-C252
 2.4 with sigma of 0.02
 C258-C252
 2.4 with sigma of 0.02
 C248-C247
 1.5 with sigma of 0.01
 C247-C248
 1.5 with sigma of 0.01
 C511-C517
 2.4 with sigma of 0.02
 C556-C548
 2.4 with sigma of 0.02
 C552-C548
 2.4 with sigma of 0.02
 C532-C530
 2.4 with sigma of 0.02
 C71-C68 = C72-C73
 1.45 with sigma of 0.002
 C72-C71
 1.5 with sigma of 0.002
 C123-C120 = C126-C129
 1.45 with sigma of 0.002
 C131-C130
 1.45 with sigma of 0.002
 C414-C410
 2.4 with sigma of 0.02
 O413-C415
 2.4 with sigma of 0.02
 Zn5-C123
 3 with sigma of 0.02
 C128-C120
 2.4 with sigma of 0.02
 N124-C120
 2.4 with sigma of 0.02
 C125-C129
 2.4 with sigma of 0.02
 N319-C323
 2.4 with sigma of 0.02
 Zn2-C318
 3 with sigma of 0.02
 C85-C83
 2.4 with sigma of 0.02
 C85-C82 = C86-C87
 1.45 with sigma of 0.002
 C320-C323
 1.45 with sigma of 0.02
 C28-C29
 1.45 with sigma of 0.02
 C117-C111
 2.4 with sigma of 0.02
 C112-C110
 2.4 with sigma of 0.02
 C99-C95
 2.4 with sigma of 0.02
 C97-C99
 2.4 with sigma of 0.02
 C71-C73
 2.4 with sigma of 0.02
 C137-C134
 1.45 with sigma of 0.002
 C614-C613
 1.5 with sigma of 0.02
 C737-C743
 2.4 with sigma of 0.02
 C743-C741
 2.4 with sigma of 0.02
 C743-C742
 1.45 with sigma of 0.002
 C708-C711 = C712-C713
 1.45 with sigma of 0.002
 C711-C712
 1.5 with sigma of 0.02
 C673-O672 = C668-C671
 1.45 with sigma of 0.002
 C671-O672
 1.5 with sigma of 0.002
 C657-C658
 1.5 with sigma of 0.002
 C658-C659 = C657-C654
 1.45 with sigma of 0.002
 C711-C707
 2.4 with sigma of 0.002
 C709-C711
 2.4 with sigma of 0.002
 C744-C742
 2.4 with sigma of 0.002
 C742-C748
 2.4 with sigma of 0.002
 C736-C738
 2.4 with sigma of 0.002
 C749-C746
 1.45 with sigma of 0.002
 N119-C120
 1.45 with sigma of 0.002
 N22-C18
 2.4 with sigma of 0.002
 C18-C26
 2.4 with sigma of 0.002
 C21-C18
 1.45 with sigma of 0.002
 C229-C228
 1.45 with sigma of 0.002
 C520-C523
 1.45 with sigma of 0.002
 C290-C293
 1.45 with sigma of 0.002
 C711-C713
 2.4 with sigma of 0.02
 C704-C698
 2.4 with sigma of 0.02
 C482-C485
 1.5 with sigma of 0.01
 C465-C463
 2.4 with sigma of 0.02
 C32-C35
 1.45 with sigma of 0.02
 C427-C428
 1.5 with sigma of 0.02
 C486-C485
 1.5 with sigma of 0.02
 C482-C485 = C486-C487
 1.45 with sigma of 0.02
 C115-C117
 2.4 with sigma of 0.02
 C111-C117
 2.4 with sigma of 0.02
 C116-C117
 1.45 with sigma of 0.02
 C534-C537
 1.45 with sigma of 0.02
 C540-C543
 1.45 with sigma of 0.02
 C414-O413
 1.45 with sigma of 0.02
 Ir4-C351 = Ir4-C353
 2.8 with sigma of 0.02
 O344-C350
 2.4 with sigma of 0.02
 C71-C67
 2.4 with sigma of 0.02
 C71-C69
 2.4 with sigma of 0.02
 C109-C110
 1.5 with sigma of 0.02
 C27-C24
 1.45 with sigma of 0.02
 C27-C25
 2.4 with sigma of 0.02
 C76-C84 = N75-C79
 2.4 with sigma of 0.02
 Ir4-C79
 2.8 with sigma of 0.02
 C27-C29 = C34-C28
 2.4 with sigma of 0.02
 C406-C407
 1.45 with sigma of 0.002
 Ir11-C402 = Ir11-C406
 3 with sigma of 0.02
 N61-C65
 2.4 with sigma of 0.02
 C63-C65
 2.4 with sigma of 0.02
 O697-C694
 1.45 with sigma of 0.02
 C614-C615 = C613-C610
 1.45 with sigma of 0.02
 C330-C331
 1.45 with sigma of 0.02
 C126-C130
 2.4 with sigma of 0.02
 C343-O344
 1.45 with sigma of 0.02
 C343-C340 = O344-C345
 1.45 with sigma of 0.02
 C545-O544
 1.45 with sigma of 0.02
 O697-C693
 2.4 with sigma of 0.02
 C695-O697
 2.4 with sigma of 0.02
 C343-C345
 2.4 with sigma of 0.01
 C603-C756
 1.45 with sigma of 0.002
 C472-C471
 1.45 with sigma of 0.002
 C471-C468 = C472-C473
 1.45 with sigma of 0.002
 C343-C340 = C343-O344 = O344-C345
 1.45 with sigma of 0.002
 C756-C755
 1.45 with sigma of 0.002
 C285-C282
 1.45 with sigma of 0.002
 C736-C737
 1.45 with sigma of 0.002
 N745-C749
 2.4 with sigma of 0.02
 C755-C752
 1.45 with sigma of 0.002
 C602-C756
 2.4 with sigma of 0.02
 C496-C499
 1.45 with sigma of 0.002
 C58-C59 = C41-C38
 1.45 with sigma of 0.02
 N701-C705
 2.4 with sigma of 0.02
 N720-C716
 2.4 with sigma of 0.02
 C348-C351
 1.45 with sigma of 0.02
 C60-C58
 2.4 with sigma of 0.02
 C300-C296
 2.4 with sigma of 0.02
 C299-C297
 2.4 with sigma of 0.02
 C299-C296
 1.45 with sigma of 0.02
 C428-C429
 1.45 with sigma of 0.002
 C607-C606
 1.4 with sigma of 0.013
 C606-C607
 1.45 with sigma of 0.02
 C47-C46
 1.5 with sigma of 0.02
 C47-C48
 1.5 with sigma of 0.02
 C49-C48
 1.45 with sigma of 0.02
 C45-C47
 2.4 with sigma of 0.02
 C48-C46
 2.4 with sigma of 0.02
 C49-C47
 2.4 with sigma of 0.02
 C52-C54
 2.4 with sigma of 0.02
 C49-C51
 2.4 with sigma of 0.02
 C52-C51 = C52-C53
 1.5 with sigma of 0.02
 C53-C51
 2.4 with sigma of 0.02
 C50-C49
 1.35 with sigma of 0.01
 C50-C51
 1.45 with sigma of 0.01
 C50-C48
 2.4 with sigma of 0.02
 H48B-H51B
 -2 with sigma of 0.02
 C308-C309
 1.45 with sigma of 0.02
 C308-C307
 1.35 with sigma of 0.02
 C308-C310
 2.4 with sigma of 0.02
 C305-C299
 2.4 with sigma of 0.02
 C305-C307
 2.4 with sigma of 0.02
 C303-C305
 2.4 with sigma of 0.02
 C309-C307
 -2.4 with sigma of 0.02
 C307-C310
 -3 with sigma of 0.02
 C309-C318
 -3 with sigma of 0.02
 C298-H30C
 -2 with sigma of 0.02
 C307-C297
 -3 with sigma of 0.02
 H22C-H230
 -2 with sigma of 0.02
 H30E-H297
 -2 with sigma of 0.02
 H318-H31B
 -2 with sigma of 0.02
 H50-H47B
 -2 with sigma of 0.02
 H342-H335
 -2 with sigma of 0.02
 H653-H65C
 -2 with sigma of 0.02
 H69A-H693
 -2 with sigma of 0.02
 H714-H71E
 -2 with sigma of 0.02
 H733-H73A
 -2 with sigma of 0.02
 C329-C326
 1.45 with sigma of 0.02
 H41A-H409
 -2 with sigma of 0.02
 O544-C543
 1.45 with sigma of 0.01
 C621-C618
 1.45 with sigma of 0.01
 H60-H52B
 -2 with sigma of 0.02
 H270-H263
 -2 with sigma of 0.02
 H298-H291
 -2 with sigma of 0.02
 H495-H50B
 -2 with sigma of 0.02
 C14-O13
 1.45 with sigma of 0.01
 H45-H48B
 -2 with sigma of 0.02
 H748-H73C
 -2 with sigma of 0.02
 H60-H52A
 -2 with sigma of 0.02
 H550_$1-H354
 -2 with sigma of 0.02
 C351-C348
 1.45 with sigma of 0.01
 C698-O697
 1.5 with sigma of 0.01
 H50B-H495
 -2 with sigma of 0.02
 H50A-H50F
 -2 with sigma of 0.02
 H74-H71A
 -2 with sigma of 0.02
 H50F-H50B
 -2 with sigma of 0.02
 Ir1-C7
 3 with sigma of 0.002
 O13-C10
 1.45 with sigma of 0.01
 C316-C317
 1.45 with sigma of 0.02
 C315-C317
 2.4 with sigma of 0.02
 C311-C317
 2.4 with sigma of 0.02
 C311-C310 = C309-C310
 1.5 with sigma of 0.02
 C311-C309
 2.4 with sigma of 0.02
 C312-C310
 2.4 with sigma of 0.02
 C310-C316
 2.4 with sigma of 0.02
 H312-H30D
 -2 with sigma of 0.02
 H154-H54A
 -2 with sigma of 0.02
 C496-H50A
 -2 with sigma of 0.02
 C633-C632 = C638-C639
 1.45 with sigma of 0.002
 C634-C633 = C637-C638 = C634-C635 = C637-C636
 1.5 with sigma of 0.01
 C635-C636
 1.35 with sigma of 0.005
 C632-C634
 2.4 with sigma of 0.02
 C633-C635
 2.4 with sigma of 0.02
 C634-C636
 2.4 with sigma of 0.02
 C635-C637
 2.4 with sigma of 0.02
 C636-C638
 2.4 with sigma of 0.02
 C637-C639
 2.4 with sigma of 0.02
 C645-C644
 1.45 with sigma of 0.01
 C627-C624
 1.45 with sigma of 0.002
 H643-H30F
 -2 with sigma of 0.02
 C633-C627
 -2.35 with sigma of 0.02
 C427-C424
 1.45 with sigma of 0.02
 H42C-H423
 -2 with sigma of 0.02
 C451-C453
 2.4 with sigma of 0.02
 C458-C459
 1.45 with sigma of 0.002
 C109-C108 = C105-C106 = C107-C106
 1.5 with sigma of 0.01
 C107-C108
 1.35 with sigma of 0.005
 C109-C107
 2.4 with sigma of 0.02
 C107-C105
 2.4 with sigma of 0.02
 H11B-H107
 -2 with sigma of 0.02
 C679-C676
 1.45 with sigma of 0.002
 Ir14-C681 = Ir14-C679
 3 with sigma of 0.02
 C151-C148
 1.45 with sigma of 0.01
 C140-C143
 1.45 with sigma of 0.02
 C145-O144
 1.45 with sigma of 0.002
 H146-H14D
 -2 with sigma of 0.02
 H28B-H23
 -2 with sigma of 0.02
 H48A-H51B
 -2 with sigma of 0.02
 H50A-H495
 -2 with sigma of 0.02
 C651-C648
 1.45 with sigma of 0.02
 C306-C307
 1.45 with sigma of 0.02
 C305-C306 = C304-C305
 1.5 with sigma of 0.02
 C304-C306
 2.4 with sigma of 0.02
 C306-C308
 2.4 with sigma of 0.02
 H30B_$2-H24D
 -2 with sigma of 0.02
 N147-C151 = C152-C148
 -2.4 with sigma of 0.02
 C249-C248
 1.5 with sigma of 0.01
 C249-C250
 1.35 with sigma of 0.005
 C250-C251 = C252-C251
 1.5 with sigma of 0.01
 C247-C249
 2.4 with sigma of 0.02
 C248-C250
 2.4 with sigma of 0.02
 C249-C251
 2.4 with sigma of 0.02
 C250-C252
 2.4 with sigma of 0.02
 C251-C253
 2.4 with sigma of 0.02
 C247-C251
 -3 with sigma of 0.02
 C252-H249
 -2.5 with sigma of 0.02
 H264-H25A
 -2 with sigma of 0.02
 C471-C467
 -2.3 with sigma of 0.02
 C488-C486
 2.4 with sigma of 0.02
 C285-C281
 2.4 with sigma of 0.02
 C496-H50B
 -2 with sigma of 0.02
 Ir1-C6
 -3 with sigma of 0.02
 C725-C722
 1.45 with sigma of 0.002
 C732-C730
 2.4 with sigma of 0.02
 C723-C725
 2.4 with sigma of 0.02
 C725-C721
 2.4 with sigma of 0.02
 C726-C727 = C727-C728
 1.45 with sigma of 0.002
 C730-C731
 1.45 with sigma of 0.002
 C748-H73C
 -2 with sigma of 0.02
 H525-H53A
 -2 with sigma of 0.02
 H45C-H302
 -2 with sigma of 0.02
 C93-C90
 1.45 with sigma of 0.02
 C215-C214
 1.45 with sigma of 0.02
 C221-C218
 1.45 with sigma of 0.02
 C705-C702
 1.45 with sigma of 0.02
 H77-H84
 -2 with sigma of 0.02
 Ir4-C206
 2.8 with sigma of 0.02
 C207-C206
 1.45 with sigma of 0.02
 C205-C207
 2.4 with sigma of 0.02
 C201-C207
 2.4 with sigma of 0.02
 C212-C206
 2.4 with sigma of 0.02
 N208-C206
 2.4 with sigma of 0.02
 C207-C201
 -2.4 with sigma of 0.02
 N208-C201
 -2.4 with sigma of 0.02
 Ir4-C202
 -2.4 with sigma of 0.02
 C279-C276
 1.45 with sigma of 0.02
 H44B-H50D_$6
 -2 with sigma of 0.02
 C448-C450
 2.4 with sigma of 0.02
 C450-C452
 2.4 with sigma of 0.02
 H450-H44A
 -2 with sigma of 0.02
 H34A-H346
 -2 with sigma of 0.02
 H726_$5-H34B
 -2 with sigma of 0.02
 H73H_$6-H63F
 -2 with sigma of 0.02
 C435-C433 = C440-C432
 2.4 with sigma of 0.02
 C435-C432
 1.45 with sigma of 0.02
 C438-H44C
 -3 with sigma of 0.02
 C437-H44D
 -2 with sigma of 0.02
 H45D-H449
 -2 with sigma of 0.005
 C449-C450
 1.35 with sigma of 0.02
 C448-C447 = C448-C449 = C450-C451 = C452-C451
 1.5 with sigma of 0.02
 H449-H45D
 -2 with sigma of 0.02
 C446-C448
 2.4 with sigma of 0.02
 C441-C438
 1.45 with sigma of 0.002
 C446-C438 = C437-C441 = C442-C438
 2.4 with sigma of 0.002
 H50D_$5-H445_$4
 -2 with sigma of 0.02
 H445-H503_$6
 -2 with sigma of 0.02
 H503_$6-H445
 -2 with sigma of 0.02
 C443-C203_$3 = C443-C205_$3 = C442-C204_$3 = C443-C204_$3 = C444-C204_$3
 -2.3 with sigma of 0.02
 C443-C204_$3
 -3 with sigma of 0.02
 C443-C203_$3
 -3 with sigma of 0.02
 C447-C446 = C452-C453
 1.45 with sigma of 0.002
 H444-H25A_$7
 -2 with sigma of 0.02
 H442-H204_$3
 -2 with sigma of 0.02
 C252-C253 = C247-C246
 1.45 with sigma of 0.002
 C248-C246
 2.4 with sigma of 0.02
 C238-C241
 1.45 with sigma of 0.02
 H24C_$7-H245_$7
 -2 with sigma of 0.02
 H515-H242
 -2 with sigma of 0.02
 C227-C224
 1.45 with sigma of 0.01
 C235-C232
 1.45 with sigma of 0.01
 O213-C210 \\sim C214-C215
 with sigma of 0.002
 C209-O213 \\sim O213-C211
 with sigma of 0.002
 C504-C496 \\sim C496-C500
 with sigma of 0.02
 C139-N138 \\sim C139-C140
 with sigma of 0.002
 N652-C648 \\sim C648-C656
 with sigma of 0.002
 N647-C651 \\sim C651-C649
 with sigma of 0.002
 C664-C658 \\sim C658-C660
 with sigma of 0.002
 C658-C659 \\sim C657-C654
 with sigma of 0.002
 C653-C657 \\sim C657-C655
 with sigma of 0.002
 C99-C105 \\sim C105-C103
 with sigma of 0.002
 C122-C116 \\sim C116-C118
 with sigma of 0.002
 O413-C410 \\sim C414-C415
 with sigma of 0.002
 C548-Ir11 \\sim Ir11-C546
 with sigma of 0.002
 C546-O544 \\sim O544-C550
 with sigma of 0.002
 C409-O413 \\sim O413-C411
 with sigma of 0.002
 C752-C756 \\sim C603-C755
 with sigma of 0.002
 C667-C671 \\sim C671-C669
 with sigma of 0.002
 C35-Zn3 \\sim Zn3-C37
 with sigma of 0.02
 N31-C35 \\sim C35-C33
 with sigma of 0.02
 C542-C534 \\sim C534-N538
 with sigma of 0.02
 C541-C543 \\sim C543-C539
 with sigma of 0.02
 C351-Ir4 \\sim Ir4-C353
 with sigma of 0.02
 C132-C130 \\sim C130-C136
 with sigma of 0.02
 C262-Zn6 \\sim Zn6-C260
 with sigma of 0.02
 C402-Ir11 \\sim Ir11-C406
 with sigma of 0.002
 N408-C406 \\sim C406-C412
 with sigma of 0.002
 C401-C407 \\sim C407-C405
 with sigma of 0.002
 Zn6-N236 \\sim Zn6-N231 \\sim Zn6-N133 \\sim Zn6-N138 \\sim Zn6-N261 \\sim
Zn6-N266
 with sigma of 0.02
 C336-C330 \\sim C330-C332
 with sigma of 0.02
 C343-O344 \\sim C343-C340 \\sim O344-C345
 with sigma of 0.02
 C339-C343 \\sim C343-C341
 with sigma of 0.02
 C223-C227 \\sim C227-C225
 with sigma of 0.02
 Zn5-N222 \\sim Zn5-N124 \\sim Zn5-N119 \\sim Zn5-N94 \\sim Zn5-N89 \\sim
Zn5-N217
 with sigma of 0.01
 N217-C221 \\sim C221-C219
 with sigma of 0.01
 C674-O672 \\sim O672-C678
 with sigma of 0.02
 C674-Ir14 \\sim Ir14-C676
 with sigma of 0.02
 N338-C334 \\sim C334-C342
 with sigma of 0.02
 Zn3-N333 \\sim Zn3-N338 \\sim Zn3-N36 \\sim Zn3-N31 \\sim Zn3-N61 \\sim Zn3-N66
 with sigma of 0.01
 C738-C736 \\sim C736-C742
 with sigma of 0.02
 N294-C290 \\sim C290-C298
 with sigma of 0.02
 Ir11-C552 \\sim Ir11-N601 \\sim Ir11-N547 \\sim Ir11-N608 \\sim Ir11-C401
\\sim Ir11-N408
 with sigma of 0.1
 C42-C38 \\sim C38-C46
 with sigma of 0.02
 C53-C59 \\sim C59-C57
 with sigma of 0.02
 C60-C58 \\sim C58-C64
 with sigma of 0.02
 C57-C59 \\sim C59-C53
 with sigma of 0.02
 C639-C645 \\sim C645-C643
 with sigma of 0.002
 C650-C644 \\sim C644-C646
 with sigma of 0.002
 C640-C638 \\sim C638-C644
 with sigma of 0.002
 Zn12-N647 \\sim Zn12-N617 \\sim Zn12-N622 \\sim Zn12-N652 \\sim Zn12-N422
\\sim Zn12-N417
 with sigma of 0.002
 C453-C459 \\sim C459-C457
 with sigma of 0.002
 C679-Ir14 \\sim Ir14-C681
 with sigma of 0.002
 Ir14-C680 \\sim Ir14-N675
 with sigma of 0.02
 N675-C679 \\sim C679-C677
 with sigma of 0.02
 C684-C676 \\sim C676-C680
 with sigma of 0.02
 C71-C68 \\sim C129-C130 \\sim C271-C272 \\sim C330-C329 \\sim C143-O144 \\sim
C286-C285 \\sim C27-C28
 \\sim C85-C86 \\sim C227-C228
 with sigma of 0.002
 C150-O144 \\sim O144-C146
 with sigma of 0.002
 N466-C462 \\sim C462-C470
 with sigma of 0.02
 C463-C465 \\sim C465-N461
 with sigma of 0.02
 C729-C731 \\sim C731-C725
 with sigma of 0.002
 C726-C722 \\sim C722-C730
 with sigma of 0.002
 C454-C452 \\sim C452-C458
 with sigma of 0.002
 Ir4-C201 \\sim Ir4-N347 \\sim Ir4-N80 \\sim Ir4-N208 \\sim Ir4-N75
 with sigma of 0.02
 Zn13-N466 \\sim Zn13-N666 \\sim Zn13-N436 \\sim Zn13-N461 \\sim Zn13-N661
\\sim Zn13-N431
 with sigma of 0.02
 C435-Zn13 \\sim Zn13-C437
 with sigma of 0.02
 C446-C438 \\sim C438-C442
 with sigma of 0.002
 C437-C441 \\sim C441-C439
 with sigma of 0.02
 C445-C447 \\sim C447-C441
 with sigma of 0.002
 C242-C238 \\sim C238-C246
 with sigma of 0.002
 C245-C247 \\sim C247-C241
 with sigma of 0.002
3. Restrained planarity
 C262, C263, C264, C259, C260, N261, C258
 with sigma of 0.1
 N261, C260, C259, C264, C263, C262, C258
 with sigma of 0.1
 N36, C35, C40, C39, C38, C37
 with sigma of 0.1
 C255, C254, C253, C258, C256, C252, C257
 with sigma of 0.1
 C260, C259, C264, C263, C262, N261, C258
 with sigma of 0.1
 C505, C499, C504, C503, C502, C501, C500
 with sigma of 0.1
 C510, C511, C516, C515, C514, C513, C512
 with sigma of 0.1
 C259, C264, C263, C262, N261, C260, C258
 with sigma of 0.1
 C548, C554, C555, C556, C551, C552, C553
 with sigma of 0.1
 N231, C232, C233, C234, C229, C230, N236, C237, C235, C238, C239, C240
 with sigma of 0.1
 C100, C99, C104, C103, C102, C101, C96
 with sigma of 0.1
 N319, C320, C321, C322, C317, C318, C325, C326, C327, C328, C323, N324
 with sigma of 0.1
 C708, C707, N706, C705, C710, C709, C711
 with sigma of 0.1
 O413, C410, C411, C412, C407, N408, C409
 with sigma of 0.1
 C749, N750, C752, C753, C754, C751, C746, C747, C748, C743, C744, N745
 with sigma of 0.1
 C741, C742, C737, C738, C739, C740, C736
 with sigma of 0.1
 C499, C504, C503, C502, C501, C500, C496
 with sigma of 0.002
 C255, C254, C253, C258, C257, C256, C259
 with sigma of 0.002
 C746, N745, C744, C743, C748, C747, C742
 with sigma of 0.1
 N289, C290, C291, C293, N294, C295, C296, C297, C298, C288, C287, C292
 with sigma of 0.1
 C298, C293, C295, N294, C297, C296
 with sigma of 0.1
 C24, C23, N22, C21, C26, C25, C18, N17, C16, C15, C20, C19, Zn2
 with sigma of 0.1
 C30, Zn3, N31, C32, C33, C34, C29, C35, N36, C37, C38, C39, C40
 with sigma of 0.1
 N617, C618, C619, C620, C615, C616, N622, C623, C624, C625, C626, C621
 with sigma of 0.1
 C99, C104, C103, C102, C101, C105, C100
 with sigma of 0.1
 C116, C121, C122, C117, C118, N119
 with sigma of 0.1
 C292, C287, C288, N289, C290, C291, C293, N294, C295, C296, C297, C298
 with sigma of 0.1
 N80, C79, C84, C83, C82, C81, C74, C73, C78, C77, C76, N75
 with sigma of 0.1
 N22, C21, C26, C25, C24, C23, C27, C18, N17, C16, C15, C20, C19, C14
 with sigma of 0.1
 N22, C21, C23, C18, N17, C16, C15, C20, C19, C26, C25, C24
 with sigma of 0.1
 C406, C401, C402, C403, C404, C405, C407, C412, C411, C410, C409, N408
 with sigma of 0.1
 C411, C412, C407, C409, C410, N408, C406
 with sigma of 0.1
 C406, C405, C404, C403, C402, C401, C407
 with sigma of 0.1
 C516, C515, C514, C513, C512, C511, C517
 with sigma of 0.1
 C59, C60, N61, C62, C63, C64
 with sigma of 0.01
 C60, C63, C64, C59, C62, N61
 with sigma of 0.1
 C603, C604, C605, C606, N601, C602, C756, C607, C612, C611, C610, C609, N608
 with sigma of 0.1
 C342, C337, N338, C339, C340, C341, C343
 with sigma of 0.1
 C117, C118, N119, C120, C121, C122
 with sigma of 0.1
 C742, C741, C740, C739, C738, C737, C743
 with sigma of 0.1
 N720, C719, C724, C723, C722, C721, Zn16, N715, C716, C717, C718, C713, C714
 with sigma of 0.1
 C735, C734, C733, C732
 with sigma of 0.1
 N119, C118, C117, C122, C121, C120, C123, C128, C127, C126, C125, N124
 with sigma of 0.1
 N61, C60, C59, C64, C63, C62, Zn3
 with sigma of 0.1
 C35, N36, C37, C38, C39, C40
 with sigma of 0.1
 C58, C57, C56, C55, C54, C53, C59
 with sigma of 0.1
 C299, C304, C303, C302, C301, C300, C296
 with sigma of 0.1
 C296, C297, C298, C293, N294, C295, C299
 with sigma of 0.1
 C54, C53, C58, C57, C56, C55, C59
 with sigma of 0.1
 C53, C54, C55, C56, C57, C58
 with sigma of 0.1
 C46, C41, C42, C43, C44, C45
 with sigma of 0.1
 C54, C53, C58, C57, C56, C55, C52
 with sigma of 0.1
 C54, C53, C58, C56, C55, C52, C57
 with sigma of 0.1
 O544, C545, C546, N547, C548, C549, C550
 with sigma of 0.1
 C305, C304, C303, C302, C301, C300, C299
 with sigma of 0.1
 C47, C46, C45, C44, C43, C42, C41
 with sigma of 0.1
 C348, C349, C350, C345, C346, N347, C351, C356, C355, C354, C353, C352
 with sigma of 0.1
 Ir4, C352, C351, C356, C355, C354, C353
 with sigma of 0.1
 C346, N347, C348, C349, C350, C345, Ir4, C352, C353, C354, C355, C356, C351
 with sigma of 0.1
 C509, C508, C507, C506
 with sigma of 0.1
 C48, C49, C50, C51
 with sigma of 0.1
 C228, C229, C234, C233, C232, N231, C230
 with sigma of 0.1
 C315, C314, C313, C312, C311, C316, C317
 with sigma of 0.1
 C322, C317, C318, C321, C320, N319, C315
 with sigma of 0.1
 C315, C314, C313, C312, C311, C316
 with sigma of 0.1
 N319, C320, C321, C322, C317, C318, C316
 with sigma of 0.1
 C310, C311, C312, C313, C314, C315, C316
 with sigma of 0.1
 N519, C520, C521, C517, C518, C523, N524, C525, C526, C528, C527, C516
 with sigma of 0.1
 C638, C640, C639, C644, C643, C642, C641
 with sigma of 0.1
 C633, C632, C627, C628, C629, C630, C631
 with sigma of 0.1
 N422, C423, C424, C425, C426, C421
 with sigma of 0.1
 N422, C421, C423, C424, C425, C418
 with sigma of 0.1
 C418, N417, C416, C415, C420, C419, C421
 with sigma of 0.1
 C424, C423, N422, C421, C426, C425
 with sigma of 0.1
 C454, C453, C458, C457, C456, C455, C459
 with sigma of 0.1
 C681, C682, C683, C684, C679, C680, Ir14, C676, C677, C678, C673, C674, N675
 with sigma of 0.1
 C306, C307, C308, C309
 with sigma of 0.1
 C248, C249, C250, C251
 with sigma of 0.1
 O13, C9, C10, C11, C12, C7, N8, C2, C1, C6, C5, C4, C3
 with sigma of 0.1
 C731, C725, C730, C729, C728, C727, C726
 with sigma of 0.1
 C725, C730, C729, C728, C727, C726, C722
 with sigma of 0.1
 C723, C722, C721, N720, C719, C724, C725
 with sigma of 0.1
 C723, C724, C719, N720, C721, C722, C725
 with sigma of 0.1
 C722, C723, C721, N720, C719, C724, C725
 with sigma of 0.1
 N720, C722, C723, C724, C719, C725
 with sigma of 0.1
 C746, C747, C748, C743, C744, N745, C742
 with sigma of 0.1
 C452, C453, C458, C457, C456, C455, C454
 with sigma of 0.1
 C209, C210, C212, C207, N208, C201, C206, C205, C204, C203, C202
 with sigma of 0.1
 C201, C206, C203, C202, H202, C205, C204, N208, C209, C207, C212, C211, C210,
 O213, Ir4
 with sigma of 0.05
 N436, C437, N431, C430, C438
 with sigma of 0.1
 C448, C449, C450, C451
 with sigma of 0.1
 C441, C446, C445, C444, C443, C442, C438
 with sigma of 0.05
 C435, C440, C439, C438, C437, N436, C441
 with sigma of 0.1
 C447, C446, C445, C444, C443, C442, C441
 with sigma of 0.1
 C235, N236, C237, C238, C239, C240, C241
 with sigma of 0.002
 C247, C246, C241, C242, C243, C244, C245
 with sigma of 0.1
 C246, C245, C244, C243, C242, C241, C238
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F1_1 \\sim F2_1 \\sim F3_1 \\sim F4_1 \\sim F5_1 \\sim F6_1 \\sim F1_2 \\sim
F2_2 \\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2 \\sim F1_3 \\sim F2_3 \\sim
F3_3 \\sim F4_3 \\sim F5_3 \\sim F6_3 \\sim F1_4 \\sim F2_4 \\sim F3_4 \\sim
F4_4 \\sim F5_4 \\sim F6_4 \\sim F1_5 \\sim F2_5 \\sim F3_5 \\sim F4_5 \\sim
F5_5 \\sim F6_5 \\sim F1_6 \\sim F2_6 \\sim F3_6 \\sim F4_6 \\sim F5_6 \\sim
F6_6 \\sim F1_7 \\sim F2_7 \\sim F3_7 \\sim F4_7 \\sim F5_7 \\sim F6_7 \\sim
F1_8 \\sim F2_8 \\sim F3_8 \\sim F4_8 \\sim F5_8 \\sim F6_8 \\sim F1_9 \\sim
F2_9 \\sim F3_9 \\sim F4_9 \\sim F5_9 \\sim F6_9 \\sim F1_10 \\sim F2_10 \\sim
F3_10 \\sim F4_10 \\sim F5_10 \\sim F6_10 \\sim F1_11 \\sim F2_11 \\sim F3_11
\\sim F4_11 \\sim F5_11 \\sim F6_11 \\sim F1_12 \\sim F2_12 \\sim F3_12 \\sim
F4_12 \\sim F5_12 \\sim F6_12 \\sim F1_13 \\sim F2_13 \\sim F3_13 \\sim F4_13
\\sim F5_13 \\sim F6_13 \\sim F1_14 \\sim F2_14 \\sim F3_14 \\sim F4_14 \\sim
F5_14 \\sim F6_14 \\sim F1_15 \\sim F2_15 \\sim F3_15 \\sim F4_15 \\sim F5_15
\\sim F6_15 \\sim F1_16 \\sim F2_16 \\sim F3_16 \\sim F4_16 \\sim F5_16 \\sim
F6_16 \\sim F1_17 \\sim F2_17 \\sim F3_17 \\sim F4_17 \\sim F5_17 \\sim F6_17
\\sim F1_18 \\sim F2_18 \\sim F3_18 \\sim F4_18 \\sim F5_18 \\sim F6_18 \\sim
F1_19 \\sim F2_19 \\sim F3_19 \\sim F4_19 \\sim F5_19 \\sim F6_19 \\sim F1_20
\\sim F2_20 \\sim F3_20 \\sim F4_20 \\sim F5_20 \\sim F6_20 \\sim P1_1 \\sim
P1_2 \\sim P1_3 \\sim P1_4 \\sim P1_5 \\sim P1_6 \\sim P1_7 \\sim P1_8 \\sim
P1_9 \\sim P1_10 \\sim P1_11 \\sim P1_12 \\sim P1_13 \\sim P1_14 \\sim P1_15
\\sim P1_16 \\sim P1_17 \\sim P1_18 \\sim P1_19 \\sim P1_20: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C255 \\sim C254 \\sim C258 \\sim C257 \\sim C256 \\sim C253: within 2A with
sigma of 0.013 and sigma for terminal atoms of 0.026
C689 \\sim C511 \\sim C516 \\sim C515 \\sim C514 \\sim C513 \\sim C512: within
2A with sigma of 0.013 and sigma for terminal atoms of 0.026
C255 \\sim C254 \\sim C253 \\sim C258 \\sim C257 \\sim C256: within 2A with
sigma of 0.013 and sigma for terminal atoms of 0.026
C554 \\sim C555 \\sim C556 \\sim C551 \\sim C553 \\sim C552: within 2A with
sigma of 0.013 and sigma for terminal atoms of 0.026
C351 \\sim C356 \\sim C355 \\sim C353 \\sim C354 \\sim C352: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C239 \\sim C238 \\sim C240 \\sim Zn6 \\sim N236 \\sim C235 \\sim C237: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C499 \\sim C504 \\sim C503 \\sim C502 \\sim C501 \\sim C500: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C514 \\sim C515 \\sim C516 \\sim C511 \\sim C512 \\sim C513: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N601 \\sim C602 \\sim C603 \\sim C604 \\sim C605 \\sim C606: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C741 \\sim C742 \\sim C738 \\sim C739 \\sim C740 \\sim C737: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C736 \\sim C733 \\sim C734 \\sim C735 \\sim C732 \\sim C731: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C743 \\sim C748 \\sim C747 \\sim C746 \\sim N745 \\sim C744: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C116 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C100 \\sim C99 \\sim C104 \\sim C103 \\sim C102 \\sim C101: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C411 \\sim C410 \\sim C409 \\sim N408 \\sim C407 \\sim C412: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C406 \\sim C405 \\sim C404 \\sim C403 \\sim C402 \\sim C401: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C255 \\sim C254 \\sim C253 \\sim C258 \\sim C256 \\sim C257: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C35: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C626 \\sim C621 \\sim N622 \\sim C623 \\sim C624 \\sim C625 \\sim C618 \\sim
N617 \\sim C616 \\sim C615 \\sim C620 \\sim C619: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C610 \\sim C609 \\sim N608 \\sim C607 \\sim C612 \\sim C611: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C76 \\sim N75 \\sim C74 \\sim C73 \\sim C78 \\sim C77: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C707 \\sim C708 \\sim C709 \\sim C710 \\sim C705 \\sim N706: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C716 \\sim C717 \\sim C718 \\sim C713 \\sim C714 \\sim N715: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C268 \\sim C267 \\sim N266 \\sim C265 \\sim C270 \\sim C269 \\sim C262 \\sim
C263 \\sim C264 \\sim C259 \\sim C260 \\sim N261: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C507 \\sim C508 \\sim C506 \\sim C505 \\sim C509 \\sim C510: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C521 \\sim C520 \\sim N519 \\sim C518 \\sim C517 \\sim C522: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C43 \\sim C46 \\sim C41 \\sim C45 \\sim C42 \\sim C44 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C58 \\sim C57 \\sim C56 \\sim
C55 \\sim C54: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C43 \\sim H71A \\sim H71B \\sim C46 \\sim C45 \\sim C44 \\sim C42 \\sim C41
\\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C7 \\sim N8 \\sim C9 \\sim C10 \\sim C11: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
C214 \\sim O213 \\sim C215 \\sim C220 \\sim C210 \\sim C211: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C60 \\sim N61 \\sim C62 \\sim C63 \\sim C64 \\sim C59: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C316 \\sim C314 \\sim C313 \\sim C312 \\sim C311 \\sim C315 \\sim P1_3 \\sim
C304 \\sim C303 \\sim C302 \\sim C301 \\sim C300 \\sim C299: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C314 \\sim C315 \\sim C312 \\sim C311 \\sim C316 \\sim C313 \\sim C304 \\sim
C303 \\sim C302 \\sim C301 \\sim C300 \\sim H412 \\sim C299: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C640 \\sim C644 \\sim C643 \\sim C642 \\sim C641 \\sim C639: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C638 \\sim C637 \\sim C636 \\sim C635 \\sim C634 \\sim C633 \\sim C631 \\sim
C630 \\sim C632 \\sim C627 \\sim C628: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N422 \\sim C421 \\sim C426 \\sim C425 \\sim C424 \\sim C423: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C107 \\sim C106 \\sim C108 \\sim C109 \\sim C105 \\sim C110: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C539 \\sim N538 \\sim C540 \\sim C541 \\sim C542 \\sim C537: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C683 \\sim C682 \\sim C681 \\sim C680 \\sim C679 \\sim C684: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C143 \\sim O144: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C148 \\sim N147 \\sim C146 \\sim C145 \\sim C150 \\sim C149: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C505 \\sim C506 \\sim C507 \\sim C508 \\sim C509 \\sim C510 \\sim C511 \\sim
C504: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C308 \\sim C306 \\sim C305 \\sim C303 \\sim C299 \\sim C307 \\sim C309 \\sim
C315 \\sim C314 \\sim C313 \\sim C312 \\sim C316 \\sim C311 \\sim C301 \\sim
C300 \\sim C302 \\sim C304: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C650 \\sim C645 \\sim C649 \\sim C648 \\sim N647 \\sim C646: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C156 \\sim C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C297 \\sim C296 \\sim C295 \\sim N294 \\sim C293 \\sim C298: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C531 \\sim C532 \\sim N533 \\sim C534 \\sim C535 \\sim C536: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C139 \\sim N138 \\sim C137 \\sim C142 \\sim C141 \\sim C140: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C251 \\sim C247 \\sim C248 \\sim C249 \\sim C252 \\sim C250: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C725 \\sim C730 \\sim C729 \\sim C727 \\sim C726 \\sim C728: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C453 \\sim C458 \\sim C457 \\sim C456 \\sim C455 \\sim C454 \\sim C452 \\sim
C451: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C614 \\sim C204 \\sim C205 \\sim C206 \\sim C201 \\sim C202 \\sim C203: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C276 \\sim N275 \\sim C274 \\sim C273 \\sim C278 \\sim C277: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C439 \\sim C440 \\sim C435 \\sim N436 \\sim C437 \\sim C438: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C451 \\sim C447 \\sim C448 \\sim C450 \\sim C449 \\sim C452: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
C441 \\sim C442 \\sim C443 \\sim C444 \\sim C445 \\sim C446: within 2A with
sigma of 0.013 and sigma for terminal atoms of 0.026
C246 \\sim C245 \\sim C244 \\sim C243 \\sim C242 \\sim C241: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{P1_2, F1_2, F2_2, F3_2, F4_2, F5_2, F6_2}
{P1_3, F1_3, F2_3, F3_3, F4_3, F5_3, F6_3}
{P1_4, F1_4, F2_4, F3_4, F4_4, F5_4, F6_4}
{P1_5, F1_5, F2_5, F3_5, F4_5, F5_5, F6_5}
{P1_6, F1_6, F2_6, F3_6, F4_6, F5_6, F6_6}
{P1_7, F1_7, F2_7, F3_7, F4_7, F5_7, F6_7}
{P1_8, F1_8, F2_8, F3_8, F4_8, F5_8, F6_8}
{P1_9, F1_9, F2_9, F3_9, F4_9, F5_9, F6_9}
{P1_10, F1_10, F2_10, F3_10, F4_10, F5_10, F6_10}
{P1_11, F1_11, F2_11, F3_11, F4_11, F5_11, F6_11}
{P1_12, F1_12, F2_12, F3_12, F4_12, F5_12, F6_12}
{P1_13, F1_13, F2_13, F3_13, F4_13, F5_13, F6_13}
{P1_14, F1_14, F2_14, F3_14, F4_14, F5_14, F6_14}
{P1_15, F1_15, F2_15, F3_15, F4_15, F5_15, F6_15}
{P1_16, F1_16, F2_16, F3_16, F4_16, F5_16, F6_16}
{P1_17, F1_17, F2_17, F3_17, F4_17, F5_17, F6_17}
{P1_18, F1_18, F2_18, F3_18, F4_18, F5_18, F6_18}
{P1_19, F1_19, F2_19, F3_19, F4_19, F5_19, F6_19}
{P1_20, F1_20, F2_20, F3_20, F4_20, F5_20, F6_20}
as
{P1_1, F1_1, F2_1, F3_1, F4_1, F5_1, F6_1} sigma for 1-2: 0.02 1-3: 0.04
7.a Secondary CH2 refined with riding coordinates:
 C451(H45A,H45B), C698(H69A,H69B), C14(H14A,H14B), C671(H67A,H67B), C272(H27A,
 H27B), C28(H28A,H28B), C228(H22A,H22B), C285(H28C,H28D), C130(H13A,H13B),
 C271(H27C,H27D), C143(H14C,H14D), C712(H71C,H71D), C452(H45C,H45D), C86(H86A,
 H86B), C657(H65A,H65B), C485(H48C,H48D), C110(H11A,H11B), C530(H53A,H53B),
 C711(H71E,H71F), C329(H32A,H32B), C227(H22C,H22D), C129(H12A,H12B), C633(H63A,
 H63B), C638(H63C,H63D), C85(H85A,H85B), C71(H71A,H71B), C251(H25A,H25B),
 C447(H44A,H44B), C613(H61A,H61B), C27(H27E,H27F), C529(H52C,H52D), C286(H28E,
 H28F), C448(H44C,H44D), C543(H54A,H54B), C634(H63E,H63F), C755(H75A,H75B),
 C506(H50A,H50B), C658(H65C,H65D), C505(H50C,H50D), C214(H21A,H21B), C343(H34A,
 H34B), C72(H72A,H72B), C756(H75C,H75D), C614(H61C,H61D), C247(H24A,H24B),
 C414(H41A,H41B), C330(H33A,H33B), C736(H73A,H73B), C735(H73C,H73D), C637(H63G,
 H63H), C732(H73E,H73F), C509(H50E,H50F), C106(H10A,H10B), C731(H73G,H73H),
 C510(H51C,H51D), C109(H10C,H10D), C105(H10E,H10F), C248(H24C,H24D), C252(H25C,
 H25D), C471(H47C,H47D), C472(H47E,H47F), C427(H42A,H42B), C428(H42C,H42D),
 C486(H48E,H48F), C47(H47A,H47B), C48(H48A,H48B), C52(H52A,H52B), C51(H51A,
 H51B), C310(H31A,H31B), C306(H30A,H30B), C309(H30C,H30D), C305(H30E,H30F)
7.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C23(H23), C226(H226), C225(H225), C223(H223), C619(H619),
 C620(H620), C616(H616), C84(H84), C83(H83), C81(H81), C747(H747), C748(H748),
 C744(H744), C667(H667), C670(H670), C669(H669), C325(H325), C327(H327),
 C328(H328), C88(H88), C91(H91), C92(H92), C354(H354), C355(H355), C356(H356),
 C353(H353), C274(H274), C278(H278), C277(H277), C209(H209), C211(H211),
 C212(H212), C439(H439), C440(H440), C437(H437), C491(H491), C492(H492),
 C488(H488), C497(H497), C495(H495), C494(H494), C514(H514), C515(H515),
 C512(H512), C513(H513), C350(H350), C346(H346), C349(H349), C33(H33), C34(H34),
  C30(H30), C95(H95), C97(H97), C98(H98), C255(H255), C254(H254), C257(H257),
 C256(H256), C660(H660), C664(H664), C663(H663), C245(H245), C244(H244),
 C243(H243), C242(H242), C522(H522), C518(H518), C521(H521), C216(H216),
 C220(H220), C219(H219), C67(H67), C69(H69), C70(H70), C525(H525), C527(H527),
 C528(H528), C653(H653), C655(H655), C656(H656), C444(H444), C443(H443),
 C442(H442), C445(H445), C467(H467), C469(H469), C470(H470), C507(H507),
 C741(H741), C738(H738), C739(H739), C740(H740), C332(H332), C336(H336),
 C335(H335), C426(H426), C425(H425), C423(H423), C604(H604), C605(H605),
 C602(H602), C292(H292), C288(H288), C291(H291), C463(H463), C464(H464),
 C460(H460), C100(H100), C103(H103), C102(H102), C101(H101), C546(H546),
 C549(H549), C550(H550), C532(H532), C536(H536), C535(H535), C149(H149),
 C150(H150), C146(H146), C121(H121), C122(H122), C118(H118), C454(H454),
 C457(H457), C456(H456), C455(H455), C623(H623), C625(H625), C626(H626),
 C237(H237), C239(H239), C240(H240), C709(H709), C707(H707), C710(H710),
 C260(H260), C264(H264), C263(H263), C9(H9), C11(H11), C12(H12), C508(H508),
 C270(H270), C269(H269), C267(H267), C295(H295), C297(H297), C298(H298),
 C678(H678), C674(H674), C677(H677), C342(H342), C341(H341), C339(H339),
 C684(H684), C681(H681), C682(H682), C683(H683), C281(H281), C284(H284),
 C283(H283), C74(H74), C78(H78), C77(H77), C411(H411), C412(H412), C409(H409),
 C2(H2), C5(H5), C4(H4), C3(H3), C233(H233), C234(H234), C230(H230), C139(H139),
  C142(H142), C141(H141), C650(H650), C646(H646), C649(H649), C112(H112),
 C113(H113), C114(H114), C115(H115), C751(H751), C753(H753), C754(H754),
 C16(H16), C20(H20), C19(H19), C127(H127), C128(H128), C125(H125), C155(H155),
 C154(H154), C153(H153), C152(H152), C703(H703), C700(H700), C704(H704),
 C321(H321), C322(H322), C318(H318), C717(H717), C718(H718), C714(H714),
 C539(H539), C542(H542), C541(H541), C37(H37), C39(H39), C40(H40), C132(H132),
 C136(H136), C135(H135), C631(H631), C630(H630), C629(H629), C628(H628),
 C612(H612), C611(H611), C609(H609), C554(H554), C555(H555), C556(H556),
 C553(H553), C205(H205), C204(H204), C203(H203), C202(H202), C60(H60), C63(H63),
  C64(H64), C416(H416), C420(H420), C419(H419), C723(H723), C724(H724),
 C721(H721), C450(H450), C449(H449), C405(H405), C404(H404), C403(H403),
 C402(H402), C640(H640), C643(H643), C642(H642), C641(H641), C636(H636),
 C635(H635), C726(H726), C727(H727), C728(H728), C729(H729), C503(H503),
 C502(H502), C501(H501), C500(H500), C733(H733), C734(H734), C107(H107),
 C108(H108), C249(H249), C250(H250), C481(H481), C483(H483), C484(H484),
 C693(H693), C695(H695), C696(H696), C474(H474), C477(H477), C478(H478),
 C433(H433), C434(H434), C430(H430), C689(H689), C688(H688), C687(H687),
 C686(H686), C45(H45), C44(H44), C43(H43), C42(H42), C54(H54), C57(H57),
 C56(H56), C55(H55), C315(H315), C314(H314), C313(H313), C312(H312), C300(H300),
  C301(H301), C302(H302), C303(H303), C49(H49), C50(H50), C308(H308), C307(H307)
7.c Fitted hexagon refined as free rotating group:
 N22(C21,C26,C25,C24,C23), N222(C221,C226,C225,C224,C223), N617(C618,C619,C620,
 C615,C616), N80(C79,C84,C83,C82,C81), C746(C747,C748,C743,C744,N745),
 C668(C667,N666,C665,C670,C669), C325(C326,C327,C328,C323,N324), C88(N89,C90,
 C91,C92,C87), C354(C355,C356,C351,C352,C353), N275(C274,C273,C278,C277,C276),
 N208(C209,C210,C211,C212,C207), C438(C439,C440,C435,N436,C437), N489(C490,C491,
 C492,C487,C488), N498(C497,C496,C495,C494,C493), C514(C515,C516,C511,C512,
 C513), C350(C345,C346,N347,C348,C349), N31(C32,C33,C34,C29,C30), N94(C95,C96,
 C97,C98,C93), C255(C254,C253,C258,C257,C256), N661(C660,C659,C664,C663,C662),
 C246(C245,C244,C243,C242,C241), C522(C517,C518,N519,C520,C521), C218(N217,C216,
 C215,C220,C219), C67(C68,C69,C70,C65,N66), N524(C525,C526,C527,C528,C523),
 C653(C654,C655,C656,C651,N652), C444(C443,C442,C441,C446,C445), N466(C467,C468,
 C469,C470,C465), C741(C742,C737,C738,C739,C740), N333(C332,C331,C336,C335,
 C334), N422(C421,C426,C425,C424,C423), C603(C604,C605,C606,N601,C602),
 C292(C287,C288,N289,C290,C291), C462(C463,C464,C459,C460,N461), C100(C99,C104,
 C103,C102,C101), C546(N547,C548,C549,C550,C545), C534(N533,C532,C531,C536,
 C535), C148(C149,C150,C145,C146,N147), C120(C121,C122,C117,C118,N119),
 C454(C453,C458,C457,C456,C455), N622(C623,C624,C625,C626,C621), N236(C237,C238,
 C239,C240,C235), C709(C708,C707,N706,C705,C710), C260(C259,C264,C263,C262,
 N261), C9(C10,C11,C12,C7,N8), C265(C270,C269,C268,C267,N266), C293(N294,C295,
 C296,C297,C298), C678(C673,C674,N675,C676,C677), C337(C342,C341,C340,C339,
 N338), C684(C679,C680,C681,C682,C683), C281(N280,C279,C284,C283,C282), C74(C73,
 C78,C77,C76,N75), C411(C412,C407,N408,C409,C410), C2(C1,C6,C5,C4,C3),
 N231(C232,C233,C234,C229,C230), C139(N138,C137,C142,C141,C140), C650(C645,C646,
 N647,C648,C649), C116(C111,C112,C113,C114,C115), C749(N750,C751,C752,C753,
 C754), C18(N17,C16,C15,C20,C19), C127(C128,C123,N124,C125,C126), C156(C155,
 C154,C153,C152,C151), C703(C702,N701,C700,C699,C704), N319(C320,C321,C322,C317,
 C318), C716(C717,C718,C713,C714,N715), C540(C539,N538,C537,C542,C541), C37(C38,
 C39,C40,C35,N36), N133(C132,C131,C136,C135,C134), C627(C632,C631,C630,C629,
 C628), C607(C612,C611,C610,C609,N608), C554(C555,C556,C551,C552,C553),
 C201(C206,C205,C204,C203,C202), C60(N61,C62,C63,C64,C59), C418(N417,C416,C415,
 C420,C419), C723(C724,C719,N720,C721,C722), C406(C405,C404,C403,C402,C401),
 C640(C639,C644,C643,C642,C641), C725(C726,C727,C728,C729,C730), C499(C504,C503,
 C502,C501,C500), N480(C481,C482,C483,C484,C479), N692(C693,C694,C695,C696,
 C691), C474(N475,C476,C477,C478,C473), C433(C434,C429,C430,N431,C432),
 C685(C690,C689,C688,C687,C686), C46(C45,C44,C43,C42,C41), C54(C53,C58,C57,C56,
 C55), C315(C314,C313,C312,C311,C316), C304(C299,C300,C301,C302,C303)
;
_shelx_res_checksum              55393
_shelx_hkl_checksum              15378
_shelx_fab_checksum              28148
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.696