Coordination Chemistry of a Molecular Pentafoil Knot.
Zhang, Liang; Stephens, Alexander J.; Lemonnier, Jean-François; Pirvu, Lucian; Vitorica-Yrezabal, Iñigo J; Robinson, Christopher J.; Leigh, David A.; Journal of the American Chemical Society 141 (2019) 3952–3958; doi:10.1021/jacs.8b12548

data_4128519
_publ_section_title
;
 Coordination Chemistry of a Molecular Pentafoil Knot.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3952
_journal_page_last               3958
_journal_paper_doi               10.1021/jacs.8b12548
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C260 H220 N30 Ni5, Cl, 9(B F4), C2 N'
_chemical_formula_sum            'C262 H220 B9 Cl F36 N31 Ni5'
_chemical_formula_weight         4912.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 121.371(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.589(5)
_cell_length_b                   28.5973(9)
_cell_length_c                   54.689(4)
_cell_measurement_reflns_used    19665
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.8420
_cell_measurement_theta_min      1.4800
_cell_volume                     60876(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.577
_diffrn_measured_fraction_theta_max 0.997
_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    0.10    --   30.00   0.00   0.00  169
  2  \f      0.00 179.00   1.00    0.10   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      -0.0131432000
_diffrn_orient_matrix_UB_12      0.0095772000
_diffrn_orient_matrix_UB_13      0.0010962000
_diffrn_orient_matrix_UB_21      -0.0111857000
_diffrn_orient_matrix_UB_22      -0.0037643000
_diffrn_orient_matrix_UB_23      -0.0143980000
_diffrn_orient_matrix_UB_31      -0.0037540000
_diffrn_orient_matrix_UB_32      -0.0218219000
_diffrn_orient_matrix_UB_33      0.0030102000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.577
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            139547
_diffrn_reflns_point_group_measured_fraction_full 0.577
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         20.148
_diffrn_reflns_theta_min         1.516
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27665
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             20280
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.682
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2447
_refine_ls_number_reflns         31774
_refine_ls_number_restraints     2175
_refine_ls_restrained_S_all      1.675
_refine_ls_R_factor_all          0.2019
_refine_ls_R_factor_gt           0.1512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4219
_refine_ls_wR_factor_ref         0.4739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16273
_reflns_number_total             31774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12548_si_003.cif
_cod_data_source_block           ni_pentafoil_1_2run
_cod_original_cell_volume        60876(11)
_cod_database_code               4128519
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C262H217B9ClF36N31Ni5
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.901
_reflns_odcompleteness_completeness 51.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C281-C282
 1.35 with sigma of 0.002
 C226-C232
 2.4 with sigma of 0.02
 C226-C228
 2.4 with sigma of 0.02
 C281-C283
 2.4 with sigma of 0.02
 C280-C282
 2.4 with sigma of 0.02
 C110-C108
 2.4 with sigma of 0.02
 C224-C226
 2.4 with sigma of 0.02
 C222-C224
 2.4 with sigma of 0.02
 C225-C227
 2.4 with sigma of 0.02
 C223-C221
 2.4 with sigma of 0.02
 C223-C225
 2.4 with sigma of 0.02
 C109-C111
 2.4 with sigma of 0.02
 F2AA-B109 = F4AA-B109 = F44-B109 = F23-B109
 1.35 with sigma of 0.02
 F23-F4AA
 2.2 with sigma of 0.02
 F4AA-F2AA
 2.2 with sigma of 0.02
 F2AA-F23
 2.2 with sigma of 0.02
 F23-F44
 2.2 with sigma of 0.02
 F44-F4AA
 2.2 with sigma of 0.02
 F44-F2AA
 2.2 with sigma of 0.02
 F34-B101 = F14-B101 = F30-B101 = F12-B101
 1.35 with sigma of 0.02
 F12-F34
 2.2 with sigma of 0.02
 F30-F12 = F30-F14
 2.2 with sigma of 0.02
 F12-F14
 2.2 with sigma of 0.02
 F34-F14
 2.2 with sigma of 0.02
 F30-F34
 2.2 with sigma of 0.02
 C110-C116
 2.4 with sigma of 0.02
 C110-C112
 2.4 with sigma of 0.02
 F131-B149 = F212-B149 = F202-B149 = F5AA-B149
 1.35 with sigma of 0.02
 F131-F212
 2.2 with sigma of 0.02
 F131-F5AA
 2.2 with sigma of 0.02
 F131-F202
 2.2 with sigma of 0.02
 F5AA-F202
 2.2 with sigma of 0.02
 F5AA-F212
 2.2 with sigma of 0.02
 F212-F202
 2.2 with sigma of 0.02
 F91-B138 = F3AA-B138 = F116-B138 = F8-B138
 1.35 with sigma of 0.02
 F0AA-B187 = F19-B187 = F28-B187 = F43-B187
 1.35 with sigma of 0.02
 F19-F43
 2.2 with sigma of 0.02
 F28-F19
 2.2 with sigma of 0.02
 F0AA-F19
 2.2 with sigma of 0.02
 F8-F91
 2.2 with sigma of 0.02
 F8-F3AA
 2.2 with sigma of 0.02
 F91-F3AA
 2.2 with sigma of 0.02
 F116-F8
 2.2 with sigma of 0.02
 F116-F3AA
 2.2 with sigma of 0.02
 F116-F91
 2.2 with sigma of 0.02
 F13-B24
 1.35 with sigma of 0.02
 C232-C233
 1.45 with sigma of 0.02
 C227-C233
 2.4 with sigma of 0.02
 C231-C233
 2.4 with sigma of 0.02
 C273-C270
 1.45 with sigma of 0.02
 C278-C270
 2.4 with sigma of 0.02
 F124-B44 = F101-B44 = F207-B44 = F41-B44
 1.35 with sigma of 0.02
 F207-F41
 2.2 with sigma of 0.02
 F207-F101
 2.2 with sigma of 0.02
 F101-F41
 2.2 with sigma of 0.02
 F207-F124
 2.2 with sigma of 0.02
 F124-F101
 2.2 with sigma of 0.02
 F41-F124
 2.2 with sigma of 0.02
 F92-F176
 2.2 with sigma of 0.02
 F219-B21 = F92-B21 = F176-B21 = F47-B21 = F182-B21 = F221-B21
 1.35 with sigma of 0.02
 F47-F219 = F92-F176
 2.2 with sigma of 0.02
 F182-F92
 2.2 with sigma of 0.02
 C107-C105
 2.4 with sigma of 0.02
 C5CB-C4CB
 1.35 with sigma of 0.02
 C162-C6DA
 1.45 with sigma of 0.02
 C53-C70
 1.45 with sigma of 0.02
 C54-C70
 2.4 with sigma of 0.02
 C58-C70
 2.4 with sigma of 0.02
 C52-C54
 2.4 with sigma of 0.02
 C52-C58
 2.4 with sigma of 0.02
 C2EB-C5CB
 2.4 with sigma of 0.02
 C38-C46
 2.4 with sigma of 0.02
 C42-C38
 2.4 with sigma of 0.02
 C47-C45
 2.4 with sigma of 0.02
 C47-C41
 2.4 with sigma of 0.02
 C4HB-C2EB
 1.45 with sigma of 0.02
 C9CB-C60
 2.4 with sigma of 0.02
 C9CB-C64
 2.4 with sigma of 0.02
 C70-C2FB
 2.4 with sigma of 0.02
 C9CB-C70
 2.4 with sigma of 0.02
 C51-C53
 2.4 with sigma of 0.02
 C222-C220
 2.4 with sigma of 0.02
 C3BB-C1CB = C4GB-C6JA
 1.45 with sigma of 0.02
 C1CB-C2BB
 2.4 with sigma of 0.02
 C1B-C1CB
 2.4 with sigma of 0.02
 C106-C104
 2.4 with sigma of 0.02
 C4HB-C4CB
 2.4 with sigma of 0.02
 C3CB-C2CB
 1.35 with sigma of 0.02
 C4GB-C2JB
 2.4 with sigma of 0.02
 C2CB-C2JB
 2.4 with sigma of 0.02
 C2JB-C3CB
 1.45 with sigma of 0.02
 C2CB-C7IB
 1.45 with sigma of 0.02
 C3CB-C6JA
 2.4 with sigma of 0.02
 C51-C49
 2.4 with sigma of 0.02
 C4JB-C1C
 1.35 with sigma of 0.02
 C284-C282
 2.4 with sigma of 0.02
 C283-C285
 2.4 with sigma of 0.02
 C270-C274
 2.4 with sigma of 0.02
 C221-C219
 2.4 with sigma of 0.02
 C9HB-C5AB
 1.35 with sigma of 0.02
 C100-C96
 2.4 with sigma of 0.02
 C96-C104
 2.4 with sigma of 0.02
 C7EB-C9HB
 2.4 with sigma of 0.02
 C9IB-C5AB
 2.4 with sigma of 0.02
 C9IB-C6EB
 1.54 with sigma of 0.02
 C6EB-C5AB
 1.45 with sigma of 0.02
 C1D-C269
 2.4 with sigma of 0.02
 C1D-C271
 2.4 with sigma of 0.02
 C7FB-C5EB = C3HB-C1GB
 1.45 with sigma of 0.02
 C4JB-C9FB
 1.45 with sigma of 0.02
 C3JB-C1C
 1.45 with sigma of 0.02
 F7AA-B199
 1.35 with sigma of 0.02
 F6AA-B199 = F8AA-B199 = F4-B199 = F7AA-B199
 1.35 with sigma of 0.02
 F7AA-F4
 2.2 with sigma of 0.02
 F8AA-F4
 2.2 with sigma of 0.02
 F7AA-F8AA
 2.2 with sigma of 0.02
 C96-C4AB = C96-C99
 1.45 with sigma of 0.02
 C5AB-C1F
 2.4 with sigma of 0.02
 C9IB-C1I = C7EB-C4DB
 1.45 with sigma of 0.02
 C3DB-C117
 1.45 with sigma of 0.02
 C8GB-C117
 2.4 with sigma of 0.02
 C4DB-C117
 2.4 with sigma of 0.02
 C1F-C4DB
 2.4 with sigma of 0.02
 C1E-C7EB
 2.4 with sigma of 0.02
 C108-C106
 2.4 with sigma of 0.02
 C107-C109
 2.4 with sigma of 0.02
 C52-C50
 2.4 with sigma of 0.02
 C48-C46
 2.4 with sigma of 0.02
 C7FB-C1C
 2.4 with sigma of 0.02
 C6EB-C1I
 2.4 with sigma of 0.02
 C7IB-C1CB
 1.45 with sigma of 0.02
 C7FB-C5DB
 2.4 with sigma of 0.02
 C7FB-C83A
 2.4 with sigma of 0.02
 C9IB-C1H
 2.4 with sigma of 0.02
 C4AB-C9IB
 2.4 with sigma of 0.02
 C5EB-C3JB
 2.4 with sigma of 0.02
 C286-C284
 2.4 with sigma of 0.02
 C290-C284
 2.4 with sigma of 0.02
 C1G-C96
 2.4 with sigma of 0.02
 C1I-C96
 2.4 with sigma of 0.02
 C6EB-C9HB
 2.4 with sigma of 0.02
 C9FB-C1C
 2.4 with sigma of 0.02
 C0FB-C233 = C212-C1B
 1.4 with sigma of 0.02
 C212-C1A
 2.4 with sigma of 0.02
 C3BB-C212
 2.4 with sigma of 0.02
 F2-B1 = F5AB-B1 = F3-B1 = F5-B1
 1.35 with sigma of 0.02
 F5AB-F2
 2.2 with sigma of 0.02
 F5AB-F5
 2.2 with sigma of 0.02
 F3-F5
 2.2 with sigma of 0.02
 F5-F2
 2.2 with sigma of 0.02
 F2-F3
 2.2 with sigma of 0.02
 F43-F0AA
 2.2 with sigma of 0.02
 F43-F28
 2.2 with sigma of 0.02
 C7BB-C2EB
 2.4 with sigma of 0.02
 C4CB-C16A
 2.4 with sigma of 0.02
 C5CB-C16A = C4CB-C2EB
 1.45 with sigma of 0.02
 C16A-C162
 2.4 with sigma of 0.02
 C2IB-C1GB
 2.4 with sigma of 0.02
 C1D-C1GB
 2.4 with sigma of 0.02
 C168-C170
 2.4 with sigma of 0.02
 C168-C174
 2.4 with sigma of 0.02
 C169-C167
 2.4 with sigma of 0.02
 C70-C3FB
 1.54 with sigma of 0.02
 C3FB-C2LA
 2.5 with sigma of 0.02
 C1FB-C3FB
 2.4 with sigma of 0.02
 C9CA-C2LA
 2.4 with sigma of 0.02
 C9CA-C8IA
 1.54 with sigma of 0.02
 C3LA-C70
 2.4 with sigma of 0.02
 C8IA-C3LA
 2.5 with sigma of 0.02
 C2LA-C3LA
 1.35 with sigma of 0.02
 C290-C3
 1.45 with sigma of 0.02
 C285-C3
 2.4 with sigma of 0.02
 C289-C3
 2.4 with sigma of 0.02
 H7FA-H2
 2 with sigma of 0.02
 C165-C164 = C166-C167
 1.45 with sigma of 0.02
 C165-C167
 2.4 with sigma of 0.02
 C32-C35
 1.45 with sigma of 0.02
 C7KA-C176
 2.4 with sigma of 0.02
 C7CA-C175
 2.4 with sigma of 0.02
 C180-C7KA
 2.4 with sigma of 0.02
 C175-C7KA
 1.45 with sigma of 0.02
 C164-C166
 2.4 with sigma of 0.02
 C163-C164
 1.54 with sigma of 0.02
 C130-C129
 1.5 with sigma of 0.02
 C8IA-C2LA
 1.45 with sigma of 0.02
 C3FB-C3LA
 1.45 with sigma of 0.02
 C7BB-C4HB \\sim C162-C6DA
 with sigma of 0.002
 C70-C1FB \\sim C9CA-C1LA
 with sigma of 0.002
 C1LA-C9CA \\sim C53-C70
 with sigma of 0.002
 C9CB-C59 \\sim C58-C59
 with sigma of 0.002
 C38-C8KA \\sim C38-C41
 with sigma of 0.002
 C3BB-C1CB \\sim C4GB-C6JA
 with sigma of 0.002
 C2JB-C6JA \\sim C7IB-C1CB
 with sigma of 0.002
 C3CB-C2JB \\sim C7IB-C2CB
 with sigma of 0.002
 C7FB-C3JB \\sim C9FB-C1GB
 with sigma of 0.002
 C9FB-C4JB \\sim C3JB-C1C
 with sigma of 0.002
 C9IB-C6EB \\sim C7EB-C1F
 with sigma of 0.002
 C6EB-C5AB \\sim C9HB-C1F
 with sigma of 0.002
 C7FB-C5EB \\sim C3HB-C1GB
 with sigma of 0.002
 C7EB-C4DB \\sim C9IB-C1I
 with sigma of 0.002
 C3DB-C117 \\sim C96-C4AB
 with sigma of 0.002
 C212-C215 \\sim C212-C1B
 with sigma of 0.002
 C4HB-C2EB \\sim C16A-C6DA
 with sigma of 0.002
 C4CB-C2EB \\sim C5CB-C16A
 with sigma of 0.002
 C284-C283 \\sim C280-C279 \\sim C110-C109 \\sim C105-C106 \\sim C225-C226
\\sim C222-C221 \\sim C51-
 C52 \\sim C48-C47 \\sim C168-C167 \\sim C163-C164
 with sigma of 0.002
 C163-C162 \\sim C169-C168 \\sim C53-C52 \\sim C47-C46 \\sim C220-C221 \\sim
C227-C226 \\sim C110-C111
 \\sim C105-C104 \\sim C284-C285 \\sim C278-C279
 with sigma of 0.002
 C8IA-C2LA \\sim C3FB-C3LA
 with sigma of 0.002
 C8IA-C9CA \\sim C3FB-C70
 with sigma of 0.002
 C79-C76 \\sim C209-C206 \\sim C239-C236
 with sigma of 0.02
 C83A-C3 \\sim C1D-C270
 with sigma of 0.002
 C281-C282 \\sim C108-C107 \\sim C224-C223 \\sim C49-C50 \\sim C165-C166
 with sigma of 0.002
 C283-C282 \\sim C280-C281 \\sim C106-C107 \\sim C108-C109 \\sim C224-C225
\\sim C222-C223 \\sim C51-
 C50 \\sim C48-C49 \\sim C166-C167 \\sim C165-C164
 with sigma of 0.002
3. Restrained planarity
 C226, C232, C227, C228, C229, C230, C231
 with sigma of 0.1
 C233, C232, C227, C228, C229, C230, C231
 with sigma of 0.1
 C282, C280, C281, C283
 with sigma of 0.1
 C111, C116, C115, C114, C113, C112, C110
 with sigma of 0.1
 C46, C41, C42, C43, C44, C45, C47
 with sigma of 0.1
 C0FB, C4GB, C6GB, C5GB, C0IA, C3GB, C6JA
 with sigma of 0.1
 C233, C0FB, C4GB, C6GB, C5GB, C0IA, C3GB
 with sigma of 0.1
 C236, C237, C238, C233, C234, N235, C0FB
 with sigma of 0.1
 C271, C270, C269, N268, C267, C272, C273
 with sigma of 0.1
 C270, C2IB, C3HB, C1D, C8DB, C9DB, C8EB
 with sigma of 0.1
 C271, C270, C269, N268, C267, C272, C1D
 with sigma of 0.1
 C1GB, C2IB, C3HB, C1D, C8DB, C9DB, C8EB
 with sigma of 0.1
 C117, C4DB, C3DB, C8GB, C9GB, C5HB, C1E
 with sigma of 0.1
 C117, N119, C120, C121, C122, C3DB
 with sigma of 0.1
 C52, C58, C57, C56, C55, C54, C53
 with sigma of 0.1
 C5AB, C9HB, C1F, C6EB
 with sigma of 0.1
 C50, C51, C48, C49
 with sigma of 0.1
 C1C, C9FB, C4JB, C3JB
 with sigma of 0.1
 C224, C223, C222, C225
 with sigma of 0.1
 C107, C108, C109, C106
 with sigma of 0.1
 C7KA, C7CA, C4BB, C5BB, C6BB, C7BB, C4HB
 with sigma of 0.1
 C1CB, C1B, C3BB, C2BB, C34A, C1BB, C1A
 with sigma of 0.1
 C2EB, C4CB, C5CB, C16A
 with sigma of 0.1
 C279, C277, C278, C273, C274, C275, C276
 with sigma of 0.1
 C3LA, C3FB, C8IA, C2LA
 with sigma of 0.1
 C3, C290, C289, C288, C287, C286, C285
 with sigma of 0.1
 C167, C166, C165, C164
 with sigma of 0.1
 C116, C117, C118, N119, C120, C121, C122
 with sigma of 0.1
4. Rigid bond restraints
 C4CB, C166, C165, C164, C163, C168, C2EB, C167, C6DA
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C226 \\sim C220 \\sim C215 \\sim C216 \\sim C217 \\sim C218 \\sim C219 \\sim
C221 \\sim C224 \\sim C223 \\sim C232 \\sim C227 \\sim C228 \\sim C229 \\sim
C230 \\sim C231 \\sim C222 \\sim C225 \\sim C0FB \\sim C4GB \\sim C6GB \\sim
C5GB \\sim C0IA \\sim C3GB \\sim C6JA \\sim C2JB \\sim C3CB \\sim C2CB \\sim
C7IB \\sim C1CB \\sim C1B \\sim C3BB \\sim C2BB \\sim C34A \\sim C1BB \\sim
C1A: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C282 \\sim C284 \\sim C279 \\sim C280 \\sim C290 \\sim C289 \\sim C288 \\sim
C287 \\sim C286 \\sim C285 \\sim C277 \\sim C278 \\sim C273 \\sim C274 \\sim
C275 \\sim C276 \\sim C281 \\sim C283 \\sim C83A \\sim C3EB \\sim C3IB \\sim
C2HB \\sim C5DB \\sim C5EB \\sim C1C \\sim C7FB \\sim C1GB \\sim C9FB \\sim
C2IB \\sim C3HB \\sim C1D \\sim C8DB \\sim C9DB \\sim C8EB \\sim C4JB \\sim
C3JB: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C107 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim
C111 \\sim C116 \\sim C115 \\sim C114 \\sim C113 \\sim C112 \\sim C105 \\sim
C108 \\sim C109 \\sim C106 \\sim C110 \\sim C4DB \\sim C3DB \\sim C8GB \\sim
C9GB \\sim C5HB \\sim C1E \\sim C5AB \\sim C9IB \\sim C9HB \\sim C1F \\sim C6EB
\\sim C7EB \\sim C4AB \\sim C1G \\sim C7AB \\sim C6AB \\sim C1H \\sim C1I:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F131 \\sim F202 \\sim F212 \\sim B149 \\sim F5AA \\sim B1 \\sim F2 \\sim F3
\\sim F5 \\sim F5AB: within 2A with sigma of 0.002 and sigma for terminal atoms
of 0.004
F4 \\sim F7AA \\sim F6AA \\sim F8AA \\sim B199: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
C162 \\sim C7BB \\sim C4HB \\sim C2EB \\sim C4CB \\sim C5CB \\sim C16A \\sim
C6DA: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C52 \\sim C46 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C47 \\sim
C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54 \\sim C53 \\sim C50 \\sim C51 \\sim
C48 \\sim C49 \\sim C1LA \\sim C8KA \\sim C8CA \\sim C9KA \\sim C0LA \\sim C63
\\sim C9CA \\sim C3LA \\sim C3FB \\sim C8IA \\sim C2LA \\sim C70 \\sim C9CB
\\sim C1FB \\sim C2FB \\sim C2DB \\sim C1DB \\sim C0DB: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C168 \\sim C167 \\sim C166 \\sim C4CB \\sim C2EB \\sim C165 \\sim C16A \\sim
C164 \\sim C163 \\sim C6DA \\sim C5CB: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004
C3 \\sim C4 \\sim C6 \\sim C5 \\sim N1 \\sim C2: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
C270 \\sim C271 \\sim C272 \\sim C267 \\sim N268 \\sim C269: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C175 \\sim C180 \\sim C179 \\sim N177 \\sim C176 \\sim C178: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C7KA \\sim C173 \\sim C7CA \\sim C172 \\sim C4BB \\sim C171 \\sim C170 \\sim
C169 \\sim C174 \\sim C5BB \\sim C6BB \\sim C7BB: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
C273 \\sim C1D \\sim C278 \\sim C8DB \\sim C274 \\sim C275 \\sim C9DB \\sim
C276 \\sim C8EB \\sim C277 \\sim C2IB \\sim C3HB \\sim C270: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uiso(B109) = Uiso(F23) = Uiso(F2AA) = Uiso(F4AA) = Uiso(F44)
6. Rigid body (RIGU) restrains
 N80, C84, C79, C83, C81, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N147, C146, N152, C153, C154, C148, C145, C150, C155, C149, C156, C151
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N89, C88, C87, C92, C91, C90, C97, C98, C93, N94, C95, C96, C86, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C125, N124, C123, C130, C127, C128, C117, C118, N119, C120, C121, C122, C126,
 C129
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C250, N249, C256, C251, C253, C257, C255, C259, N254, C248, C245, C258, C252,
 C247, C246
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C245, C236, C237, C238, C233, C234, N235, C244, C239, N240, C241, C242, C243
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, C67, C68, C69, N70, C65, C66, C59, C60, C61, C62, N63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N133, C134, C131, C136, C141, C140, C139, N138, C137, C142, C130, C135, C132
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F92, F176, F182, F219, F221, B21, F47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F41, F101, F124, F207, B44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N191, N196, C192, C195, C197, C199, C200, C194, C190, C189, C198
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N191, N196, C192, C195, C197, C199, C193, C200, C194, C190, C189, C198
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N210, C211, C212, C213, C214, C209, N205, C207, C203, C204, C206, C208
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, F56, F117, B24, F42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, N12, C7, C8, C13, N1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Sof(C7KA)=Sof(C7CA)=Sof(H7CA)=Sof(C4BB)=Sof(H4BB)=Sof(C5BB)=Sof(H5BB)=
 Sof(C6BB)=Sof(H6BB)=Sof(C7BB)=Sof(C4HB)=Sof(H4HA)=Sof(H4HB)=Sof(C2EB)=
 Sof(H2EA)=Sof(H2EB)=Sof(C4CB)=Sof(H4CB)=Sof(C5CB)=Sof(H5CB)=Sof(C16A)=
 Sof(H16I)=Sof(H16J)=Sof(C6DA)=Sof(H6DA)=Sof(H6DB)=1-FVAR(1)
 Sof(C174)=Sof(C169)=Sof(C170)=Sof(H170)=Sof(C171)=Sof(H171)=Sof(C172)=
 Sof(H172)=Sof(C173)=Sof(H173)=Sof(C163)=Sof(H16A)=Sof(H16B)=Sof(C165)=
 Sof(H165)=Sof(C164)=Sof(H16C)=Sof(H16D)=Sof(C166)=Sof(H166)=Sof(C167)=
 Sof(H16E)=Sof(H16F)=Sof(C168)=Sof(H16G)=Sof(H16H)=FVAR(1)
 Sof(C1LA)=Sof(C8KA)=Sof(C8CA)=Sof(H8CA)=Sof(C9KA)=Sof(H9KA)=Sof(C0LA)=
 Sof(H0LA)=Sof(C63)=Sof(H63)=Sof(C9CA)=Sof(H9CA)=Sof(H9CB)=Sof(C3LA)=Sof(H3LA)=
 Sof(C3FB)=Sof(H3FA)=Sof(H3FB)=Sof(C8IA)=Sof(H8IA)=Sof(H8IB)=Sof(C2LA)=
 Sof(H2LA)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C9CB)=Sof(C1FB)=Sof(C2FB)=Sof(H2FB)=
 Sof(C2DB)=Sof(H2DB)=Sof(C1DB)=Sof(H1DB)=Sof(C0DB)=Sof(H0DB)=1-FVAR(2)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C46)=Sof(C41)=Sof(C42)=Sof(H42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(C58)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56)=Sof(C55)=Sof(H55)=Sof(C54)=
 Sof(H54)=Sof(C53)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49)=FVAR(2)
 Sof(C0FB)=Sof(C4GB)=Sof(C6GB)=Sof(H6GB)=Sof(C5GB)=Sof(H5GB)=Sof(C0IA)=
 Sof(H0IA)=Sof(C3GB)=Sof(H3GB)=Sof(C6JA)=Sof(H6JA)=Sof(H6JB)=Sof(C2JB)=
 Sof(H2JA)=Sof(H2JB)=Sof(C3CB)=Sof(H3CB)=Sof(C2CB)=Sof(H2CB)=Sof(C7IB)=
 Sof(H7IA)=Sof(H7IB)=Sof(C1CB)=Sof(H1CA)=Sof(H1CB)=Sof(C1B)=Sof(C3BB)=Sof(C2BB)=
 Sof(H2BB)=Sof(C34A)=Sof(H34A)=Sof(C1BB)=Sof(H1BB)=Sof(C1A)=Sof(H1A)=1-FVAR(3)
 Sof(C226)=Sof(H22A)=Sof(H22B)=Sof(C220)=Sof(C215)=Sof(C216)=Sof(H216)=
 Sof(C217)=Sof(H217)=Sof(C218)=Sof(H218)=Sof(C219)=Sof(H219)=Sof(C221)=
 Sof(H22C)=Sof(H22D)=Sof(C224)=Sof(H224)=Sof(C223)=Sof(H223)=Sof(C232)=
 Sof(C227)=Sof(C228)=Sof(H228)=Sof(C229)=Sof(H229)=Sof(C230)=Sof(H230)=
 Sof(C231)=Sof(H231)=Sof(C222)=Sof(H22E)=Sof(H22F)=Sof(C225)=Sof(H22G)=
 Sof(H22H)=FVAR(3)
 Sof(C83A)=Sof(C3EB)=Sof(H3EB)=Sof(C3IB)=Sof(H3IB)=Sof(C2HB)=Sof(H2HB)=
 Sof(C5DB)=Sof(H5DB)=Sof(C5EB)=Sof(C1C)=Sof(H1C)=Sof(C7FB)=Sof(H7FA)=Sof(H7FB)=
 Sof(C1GB)=Sof(H1GA)=Sof(H1GB)=Sof(C9FB)=Sof(H9FA)=Sof(H9FB)=Sof(C2IB)=
 Sof(H2IB)=Sof(C3HB)=Sof(C1D)=Sof(C8DB)=Sof(H8DB)=Sof(C9DB)=Sof(H9DB)=Sof(C8EB)=
 Sof(H8EB)=Sof(C4JB)=Sof(H4JB)=Sof(C3JB)=Sof(H3JA)=Sof(H3JB)=1-FVAR(4)
 Sof(C282)=Sof(H282)=Sof(C284)=Sof(H28C)=Sof(H28D)=Sof(C279)=Sof(H27C)=
 Sof(H27D)=Sof(C280)=Sof(H28E)=Sof(H28F)=Sof(C290)=Sof(C289)=Sof(H289)=
 Sof(C288)=Sof(H288)=Sof(C287)=Sof(H287)=Sof(C286)=Sof(H286)=Sof(C285)=
 Sof(C277)=Sof(H277)=Sof(C278)=Sof(C273)=Sof(C274)=Sof(H274)=Sof(C275)=
 Sof(H275)=Sof(C276)=Sof(H276)=Sof(C281)=Sof(H281)=Sof(C283)=Sof(H28G)=
 Sof(H28H)=FVAR(4)
 Sof(C4DB)=Sof(C3DB)=Sof(C8GB)=Sof(H8GB)=Sof(C9GB)=Sof(H9GB)=Sof(C5HB)=
 Sof(H5HB)=Sof(C1E)=Sof(H1E)=Sof(C5AB)=Sof(H5AB)=Sof(C9IB)=Sof(H9IA)=Sof(H9IB)=
 Sof(C9HB)=Sof(H9HB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C6EB)=Sof(H6EA)=Sof(H6EB)=
 Sof(C7EB)=Sof(H7EA)=Sof(H7EB)=Sof(C4AB)=Sof(C1G)=Sof(H1G)=Sof(C7AB)=Sof(H7AB)=
 Sof(C6AB)=Sof(H6AB)=Sof(C1H)=Sof(H1H)=Sof(C1I)=1-FVAR(5)
 Sof(C107)=Sof(H107)=Sof(C99)=Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=
 Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(C111)=Sof(C116)=
 Sof(C115)=Sof(H115)=Sof(C114)=Sof(H114)=Sof(C113)=Sof(H113)=Sof(C112)=
 Sof(H112)=Sof(C105)=Sof(H10A)=Sof(H10B)=Sof(C108)=Sof(H108)=Sof(C109)=
 Sof(H10C)=Sof(H10D)=Sof(C106)=Sof(H10E)=Sof(H10F)=Sof(C110)=Sof(H11A)=
 Sof(H11B)=FVAR(5)
 Sof(B1)=Sof(F2)=Sof(F3)=Sof(F5)=Sof(F5AB)=1-FVAR(6)
 Sof(F131)=Sof(F202)=Sof(F212)=Sof(B149)=Sof(F5AA)=FVAR(6)
 Fixed Sof: F92(0.5) F176(0.5) F182(0.5) F219(0.5) F221(0.5) F47(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C28(H28A,H28B), C27(H27A,H27B), C14(H14A,H14B), C259(H25A,
 H25B), C187(H18A,H18B), C245(H24A,H24B), C72(H72A,H72B), C260(H26A,H26B),
 C188(H18C,H18D), C130(H13C,H13D), C163(H16A,H16B), C52(H52A,H52B), C143(H14C,
 H14D), C71(H71A,H71B), C47(H47A,H47B), C201(H20A,H20B), C202(H20C,H20D),
 C226(H22A,H22B), C221(H22C,H22D), C164(H16C,H16D), C167(H16E,H16F), C51(H51A,
 H51B), C48(H48A,H48B), C284(H28C,H28D), C279(H27C,H27D), C280(H28E,H28F),
 C144(H14E,H14F), C168(H16G,H16H), C129(H12A,H12B), C86(H86A,H86B), C85(H85A,
 H85B), C246(H24C,H24D), C222(H22E,H22F), C105(H10A,H10B), C109(H10C,H10D),
 C106(H10E,H10F), C110(H11A,H11B), C283(H28G,H28H), C225(H22G,H22H), C4HB(H4HA,
 H4HB), C2EB(H2EA,H2EB), C16A(H16I,H16J), C6DA(H6DA,H6DB), C9CA(H9CA,H9CB),
 C3FB(H3FA,H3FB), C8IA(H8IA,H8IB), C70(H70A,H70B), C6JA(H6JA,H6JB), C2JB(H2JA,
 H2JB), C7IB(H7IA,H7IB), C1CB(H1CA,H1CB), C7FB(H7FA,H7FB), C1GB(H1GA,H1GB),
 C9FB(H9FA,H9FB), C3JB(H3JA,H3JB), C9IB(H9IA,H9IB), C1F(H1FA,H1FB), C6EB(H6EA,
 H6EB), C7EB(H7EA,H7EB)
8.b Aromatic/amide H refined with riding coordinates:
 C176(H176), C180(H180), C179(H179), C23(H23), C25(H25), C26(H26), C9(H9),
 C11(H11), C8(H8), C197(H197), C20(H20), C211(H211), C213(H213), C214(H214),
 C199(H199), C146(H146), C193(H193), C200(H200), C262(H262), C125(H125),
 C19(H19), C251(H251), C30(H30), C34(H34), C33(H33), C84(H84), C194(H194),
 C266(H266), C153(H153), C77(H77), C190(H190), C207(H207), C257(H257),
 C255(H255), C2(H2), C4(H4), C5(H5), C83(H83), C136(H136), C204(H204),
 C248(H248), C183(H183), C185(H185), C141(H141), C139(H139), C142(H142),
 C150(H150), C155(H155), C258(H258), C16(H16), C78(H78), C208(H208), C88(H88),
 C92(H92), C91(H91), C135(H135), C127(H127), C149(H149), C37(H37), C39(H39),
 C40(H40), C265(H265), C170(H170), C171(H171), C172(H172), C173(H173),
 C186(H186), C237(H237), C238(H238), C234(H234), C252(H252), C132(H132),
 C271(H271), C269(H269), C272(H272), C128(H128), C42(H42), C43(H43), C44(H44),
 C45(H45), C244(H244), C241(H241), C243(H243), C81(H81), C67(H67), C69(H69),
 C66(H66), C60(H60), C61(H61), C64(H64), C118(H118), C121(H121), C122(H122),
 C282(H282), C159(H159), C160(H160), C161(H161), C158(H158), C107(H107),
 C100(H100), C101(H101), C102(H102), C103(H103), C216(H216), C217(H217),
 C218(H218), C219(H219), C156(H156), C224(H224), C223(H223), C97(H97), C98(H98),
  C95(H95), C165(H165), C57(H57), C56(H56), C55(H55), C54(H54), C166(H166),
 C115(H115), C114(H114), C113(H113), C112(H112), C50(H50), C228(H228),
 C229(H229), C230(H230), C231(H231), C49(H49), C289(H289), C288(H288),
 C287(H287), C286(H286), C74(H74), C108(H108), C277(H277), C274(H274),
 C275(H275), C276(H276), C281(H281), C7CA(H7CA), C4BB(H4BB), C5BB(H5BB),
 C6BB(H6BB), C4CB(H4CB), C5CB(H5CB), C8CA(H8CA), C9KA(H9KA), C0LA(H0LA),
 C63(H63), C3LA(H3LA), C2LA(H2LA), C2FB(H2FB), C2DB(H2DB), C1DB(H1DB),
 C0DB(H0DB), C6GB(H6GB), C5GB(H5GB), C0IA(H0IA), C3GB(H3GB), C3CB(H3CB),
 C2CB(H2CB), C2BB(H2BB), C34A(H34A), C1BB(H1BB), C1A(H1A), C3EB(H3EB),
 C3IB(H3IB), C2HB(H2HB), C5DB(H5DB), C1C(H1C), C2IB(H2IB), C8DB(H8DB),
 C9DB(H9DB), C8EB(H8EB), C4JB(H4JB), C8GB(H8GB), C9GB(H9GB), C5HB(H5HB),
 C1E(H1E), C5AB(H5AB), C9HB(H9HB), C1G(H1G), C7AB(H7AB), C6AB(H6AB), C1H(H1H)
8.c Fitted hexagon refined as free rotating group:
 N177(C176,C175,C180,C179,C178), N22(C23,C24,C25,C26,C21), C9(C10,C11,N12,C7,
 C8), N210(C211,C212,C213,C214,C209), C32(N31,C30,C29,C34,C33), N1(C2,C3,C4,C5,
 C6), C141(C140,C139,N138,C137,C142), N89(C88,C87,C92,C91,C90), C35(N36,C37,C38,
 C39,C40), C174(C169,C170,C171,C172,C173), C236(C237,C238,C233,C234,N235),
 C271(C270,C269,N268,C267,C272), C46(C41,C42,C43,C44,C45), C244(C239,N240,C241,
 C242,C243), C67(C68,C69,N70,C65,C66), C59(C60,C61,C62,N63,C64), C117(C118,N119,
 C120,C121,C122), C159(C160,C161,C162,C157,C158), C99(C100,C101,C102,C103,C104),
  C220(C215,C216,C217,C218,C219), C97(C98,C93,N94,C95,C96), C58(C57,C56,C55,C54,
 C53), C111(C116,C115,C114,C113,C112), C232(C227,C228,C229,C230,C231),
 C290(C289,C288,C287,C286,C285), C277(C278,C273,C274,C275,C276), C7KA(C7CA,C4BB,
 C5BB,C6BB,C7BB), C1LA(C8KA,C8CA,C9KA,C0LA,C63), C9CB(C1FB,C2FB,C2DB,C1DB,C0DB),
  C0FB(C4GB,C6GB,C5GB,C0IA,C3GB), C1B(C3BB,C2BB,C34A,C1BB,C1A), C83A(C3EB,C3IB,
 C2HB,C5DB,C5EB), C2IB(C3HB,C1D,C8DB,C9DB,C8EB), C4DB(C3DB,C8GB,C9GB,C5HB,C1E),
 C4AB(C1G,C7AB,C6AB,C1H,C1I)
;
_shelx_res_checksum              36118
_shelx_hkl_checksum              64626
_shelx_fab_checksum              70837
_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 2.933
_oxdiff_exptl_absorpt_empirical_full_min 0.522