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_4128521
_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 Co5 N30, Cl, 9(B F4), 3(C2 H3 N), C2 N, C7 H8'
_chemical_formula_sum            'C275 H237 B9 Cl Co5 F36 N34'
_chemical_formula_weight         5129.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2017-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                61.443(7)
_cell_angle_beta                 87.521(6)
_cell_angle_gamma                67.458(7)
_cell_formula_units_Z            2
_cell_length_a                   22.1116(17)
_cell_length_b                   28.081(2)
_cell_length_c                   28.5729(17)
_cell_measurement_reflns_used    13254
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.0600
_cell_measurement_theta_min      1.5330
_cell_volume                     14176(2)
_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 0.583
_diffrn_measured_fraction_theta_max 0.989
_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
  5  \w   -120.00  49.00   1.00    0.20    --   55.00   0.00   0.00  169
  6  \w   -120.00  49.00   1.00    0.20    --   55.00   0.00 120.00  169
  7  \w   -120.00  49.00   1.00    0.20    --   55.00   0.00 240.00  169
  8  \f      0.00 179.00   1.00    0.20   0.00  55.00   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      -0.0098814000
_diffrn_orient_matrix_UB_12      0.0209985000
_diffrn_orient_matrix_UB_13      0.0080394000
_diffrn_orient_matrix_UB_21      -0.0091697000
_diffrn_orient_matrix_UB_22      0.0223470000
_diffrn_orient_matrix_UB_23      -0.0266829000
_diffrn_orient_matrix_UB_31      -0.0314819000
_diffrn_orient_matrix_UB_32      0.0006904000
_diffrn_orient_matrix_UB_33      0.0000170000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.583
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            126225
_diffrn_reflns_point_group_measured_fraction_full 0.583
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         20.273
_diffrn_reflns_theta_min         1.453
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79295
_exptl_absorpt_correction_type   multi-scan
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       plate
_exptl_crystal_F_000             5292
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3458
_refine_ls_number_reflns         29908
_refine_ls_number_restraints     2510
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.1195
_refine_ls_shift/su_max          0.004
_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          0.3161
_refine_ls_wR_factor_ref         0.3584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14833
_reflns_number_total             29908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12548_si_002.cif
_cod_data_source_block           m_copk_collection_
_cod_original_cell_volume        14177(2)
_cod_database_code               4128521
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         CoFClPCNOH
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.966
_reflns_odcompleteness_completeness 51.57
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F05M-B34 = F04J-B34 = F04Z-B34 = F07Y-B34
 1.35 with sigma of 0.02
 F05M-F07Y
 2.2 with sigma of 0.02
 F05M-F04Z
 2.2 with sigma of 0.02
 F04Z-F07Y
 2.2 with sigma of 0.02
 F04J-F07Y
 2.2 with sigma of 0.02
 F04Z-F04J
 2.2 with sigma of 0.02
 F05M-F04J
 2.2 with sigma of 0.02
 F01E-B075 = F015-B075 = F02P-B075 = F01H-B075
 1.35 with sigma of 0.02
 F4-B16
 1.35 with sigma of 0.02
 F5-F10
 2.2 with sigma of 0.02
 F5-F13
 2.2 with sigma of 0.02
 F4-F5
 2.2 with sigma of 0.02
 F10-F13
 2.2 with sigma of 0.02
 F4-F13
 2.2 with sigma of 0.02
 F4-F10
 2.2 with sigma of 0.02
 F1-B54 = F2-B54 = F7-B54 = F3-B54
 1.35 with sigma of 0.02
 F10-B16 = F4-B16 = F13-B16 = F5-B16
 1.35 with sigma of 0.02
 C169-C167
 2.4 with sigma of 0.02
 C50-C49
 1.35 with sigma of 0.02
 C283-C282
 1.35 with sigma of 0.02
 C107-C108
 1.35 with sigma of 0.02
 C167-C166
 1.35 with sigma of 0.02
 C165-C166 = C167-C168
 1.45 with sigma of 0.02
 F34A-F18A
 2.2 with sigma of 0.02
 F18-F08T
 2.2 with sigma of 0.02
 F18-F34
 2.2 with sigma of 0.02
 F34-F08T
 2.2 with sigma of 0.02
 F08T-F09O
 2.2 with sigma of 0.02
 F18-F09O
 2.2 with sigma of 0.02
 F34-F09O
 2.2 with sigma of 0.02
 F18-B09A = F34-B09A = F09O-B09A = F08T-B09A
 1.35 with sigma of 0.02
 F08U-F34A
 2.2 with sigma of 0.02
 F08U-F18A
 2.2 with sigma of 0.02
 F34A-F09P
 2.2 with sigma of 0.02
 F18A-F09P
 2.2 with sigma of 0.02
 F18A-B09B = F08U-B09B = F34A-B09B = F09P-B09B
 1.35 with sigma of 0.02
 F08U-F09P
 2.2 with sigma of 0.02
 C511-C170
 2.4 with sigma of 0.02
 C510-C508
 2.4 with sigma of 0.02
 C111-C109
 2.4 with sigma of 0.02
 C108-C110
 2.4 with sigma of 0.02
 C108-C106
 2.4 with sigma of 0.02
 C105-C107
 2.4 with sigma of 0.02
 C584-C582
 2.4 with sigma of 0.02
 C583-C585
 2.4 with sigma of 0.02
 C51A-C49A
 2.4 with sigma of 0.02
 C48A-C46
 2.4 with sigma of 0.02
 C562-C106
 2.4 with sigma of 0.02
 C567-C105
 2.4 with sigma of 0.02
 C105-C563
 2.4 with sigma of 0.02
 C48A-C50A
 2.4 with sigma of 0.02
 C586-C584
 2.4 with sigma of 0.02
 C508-C506
 2.4 with sigma of 0.02
 C509-C507
 2.4 with sigma of 0.02
 C225-C227
 2.4 with sigma of 0.02
 C223-C225
 2.4 with sigma of 0.02
 C226-C224
 2.4 with sigma of 0.002
 C224-C225
 1.35 with sigma of 0.02
 C527-C525
 2.4 with sigma of 0.02
 C225-C223
 2.4 with sigma of 0.02
 C225-C224
 1.35 with sigma of 0.02
 C527-C529
 2.4 with sigma of 0.02
 C528-C526
 2.4 with sigma of 0.02
 C530-C529
 1.35 with sigma of 0.02
 C224-C223 = C226-C225
 1.45 with sigma of 0.02
 C3BA-C6AA
 2.4 with sigma of 0.02
 C3BA-C9AA
 2.4 with sigma of 0.02
 C0BA-C3BA
 1.45 with sigma of 0.02
 C109-C107
 2.4 with sigma of 0.02
 H50B_$1-H4
 2 with sigma of 0.02
 C2BA-C8
 1.45 with sigma of 0.02
 C5AA-C2BA
 2.4 with sigma of 0.02
 C2BA-C1
 2.4 with sigma of 0.02
 H20-H2BA
 2 with sigma of 0.002
 C59-C58A
 1.45 with sigma of 0.02
 C511-C509
 2.4 with sigma of 0.02
 C158-C154 \\sim C154-C501 \\sim C176-C175
 with sigma of 0.02
 C170-C512 \\sim C170-C169 \\sim C164-C163 \\sim C506-C507
 with sigma of 0.02
 C165-C164 \\sim C507-C508 \\sim C511-C510 \\sim C168-C167
 with sigma of 0.02
 C166-C165 \\sim C508-C509 \\sim C511-C510 \\sim C168-C167
 with sigma of 0.02
 C164-C163 \\sim C507-C506 \\sim C512-C170 \\sim C170-C169
 with sigma of 0.02
 C169-C168 \\sim C512-C511 \\sim C165-C164 \\sim C508-C507
 with sigma of 0.02
 C166-C165 \\sim C509-C508 \\sim C511-C510 \\sim C168-C167
 with sigma of 0.02
 C167-C166 \\sim C510-C509
 with sigma of 0.02
 C52A-C51A \\sim C52-C51 \\sim C48A-C47A \\sim C48-C47
 with sigma of 0.02
 C49A-C48A \\sim C49-C48 \\sim C51-C50 \\sim C51A-C50A
 with sigma of 0.02
 C50-C49 \\sim C50A-C49A
 with sigma of 0.02
 C117-C550 \\sim C117-C116 \\sim C567-C96
 with sigma of 0.02
 C555-C556 \\sim C111-C110 \\sim C562-C561 \\sim C105-C562
 with sigma of 0.02
 C556-C557 \\sim C110-C109 \\sim C561-C560 \\sim C106-C105
 with sigma of 0.02
 C560-C559 \\sim C107-C106 \\sim C109-C108 \\sim C557-C558
 with sigma of 0.02
 C559-C558 \\sim C108-C107
 with sigma of 0.02
 C285-C284 \\sim C582-C581 \\sim C281-C280 \\sim C586-C585
 with sigma of 0.02
 C284-C283 \\sim C583-C582 \\sim C585-C584 \\sim C282-C281
 with sigma of 0.02
 C283-C282 \\sim C584-C583
 with sigma of 0.02
 C116-C110 \\sim C110-C112
 with sigma of 0.02
 C153-C501 \\sim C501-C155
 with sigma of 0.02
 C115-C117 \\sim C117-C111
 with sigma of 0.002
 C122-C116 \\sim C116-C118
 with sigma of 0.002
 C521-C234 \\sim C234-C233
 with sigma of 0.02
 C229-C228 \\sim C233-C232 \\sim C231-C230 \\sim C526-C525 \\sim C524-C523
\\sim C522-C521
 with sigma of 0.02
 C527-C526 \\sim C228-C227 \\sim C222-C221 \\sim C532-C221
 with sigma of 0.02
 C521-C527 \\sim C527-C525
 with sigma of 0.02
 C531-C530 \\sim C224-C223 \\sim C529-C528 \\sim C226-C225
 with sigma of 0.02
 C530-C529 \\sim C225-C224
 with sigma of 0.02
 C528-C527 \\sim C227-C226 \\sim C532-C531 \\sim C223-C222
 with sigma of 0.02
 C286-C285 \\sim C581-C580 \\sim C586-C279 \\sim C280-C279
 with sigma of 0.02
 C3-C291 \\sim C575-C3 \\sim C274-C271
 with sigma of 0.02
 C580-C3 \\sim C3-C576
 with sigma of 0.02
 C501-C507 \\sim C507-C505
 with sigma of 0.02
 C53A-C52A \\sim C53-C52 \\sim C47A-C46 \\sim C47-C46
 with sigma of 0.02
 C502-C154 \\sim C154-C506
 with sigma of 0.02
3. Restrained planarity
 C562, C563, C564, C565, C566, C567, C105
 with sigma of 0.1
 C110, C111, C112, C113, C114, C115, C116
 with sigma of 0.1
 C154, C501, C502, C503, C504, C505, C506, C507
 with sigma of 0.1
 C234, C521, C522, C523, C524, C525, C526
 with sigma of 0.1
 N236, C234, C235, C237, C238, C239, C521
 with sigma of 0.1
 C521, C522, C523, C524, C525, C526, C527
 with sigma of 0.1
 C223, C224, C225, C226
 with sigma of 0.1
 C528, C529, C530, C531
 with sigma of 0.1
 C3BA, C0BA, C6AA, C1BA, C8AA, C7AA, C9AA
 with sigma of 0.1
 C512, C170, C171, C172, C173, C174, C175
 with sigma of 0.1
 C52A, C53A, C54A, C55A, C56A, C57A, C58A
 with sigma of 0.1
 C2BA, C5AA, C2AA, C1AA, C0AA, C1, C8
 with sigma of 0.1
 C511, C510, C509, C508
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F7 \\sim B54: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C164 \\sim C165 \\sim C166 \\sim C167 \\sim C168 \\sim C169 \\sim C507 \\sim
C508 \\sim C509 \\sim C510 \\sim C511 \\sim C512: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C158 \\sim C159 \\sim C160 \\sim C161 \\sim C162 \\sim C163 \\sim C501 \\sim
C502 \\sim C503 \\sim C504 \\sim C505 \\sim C506: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C47A \\sim C48A
\\sim C49A \\sim C50A \\sim C51A \\sim C52A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C556 \\sim
C557 \\sim C558 \\sim C559 \\sim C560 \\sim C561: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C550 \\sim
C551 \\sim C552 \\sim C553 \\sim C554 \\sim C555: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C280 \\sim C281 \\sim C282 \\sim C283 \\sim C284 \\sim C285 \\sim C581 \\sim
C582 \\sim C583 \\sim C584 \\sim C585 \\sim C586: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227 \\sim C527 \\sim
C528 \\sim C529 \\sim C530 \\sim C531 \\sim C532: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C291 \\sim C575: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C1 \\sim C8 \\sim C0AA \\sim C5AA \\sim C1AA \\sim C2AA: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C0BA \\sim C9AA \\sim C6AA \\sim C3BA \\sim C7AA \\sim C1BA \\sim C8AA: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C53A \\sim C58A \\sim C57A \\sim C56A \\sim C55A \\sim C54A \\sim C53 \\sim C58
\\sim C57 \\sim C56 \\sim C55 \\sim C54: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
C2BA \\sim C8 \\sim C5AA \\sim C2AA \\sim C1AA \\sim C1 \\sim C0AA: within 2A
with sigma of 0.002 and sigma for terminal atoms of 0.004
Uiso(F08U) = Uiso(F34A) = Uiso(F18A) = Uiso(F18) = Uiso(F09O) = Uiso(F08T) =
Uiso(B09A) = Uiso(B09B) = Uiso(F09P)
Uiso(B16) = Uiso(F4) = Uiso(F5) = Uiso(F10) = Uiso(F13)
Uanis(C576) = Uanis(C290)
5. Rigid body (RIGU) restrains
 F01E, F01H, F02P, F015, B075
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N36, C35, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F08T, F09O, F18, F34, B09A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N178, C170, C171, C172, C173, C174, C175, C176, C177, C179, C180, C181
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C221, C222, C223, C224, C225, C226, C227, C228, C233, C232, C231, C230, C229,
 C216, C217, C218, C219, C220
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C116, C115, C114, C113, C112, C111, C110, C109, C108, C107, C106, C105, C562,
 C563, C564, C565, C566, C567
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C233, C232, C231, C230, C229, C228, C227, C226, C225, C224, C223, C222, C221,
 C220, C219, C218, C217, C216
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C521, C522, C523, C524, C525, C526, C527, C528, C530, C529, C531, C532, C221,
 C216, C217, C218, C219, C220
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C58, C57, C56, C55, C54, C53, C52, C51, C50, C49, C48, C47, C46, C45, C44,
 C43, C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C58, C57, C56, C55, C54, C53, C52, C51, C50, C49, C48, C47, C46, C45, C44,
 C43, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N22, C23, C24, C25, C26, C21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C575, C576, C577, C578, C579, C580, C581, C583, C585, C582, C584, C586, C279,
 C278, C277, C276, C275, C274
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C58A, C57A, C56A, C55A, C54A, C53A, C52A, C51A, C50A, C49A, C48A, C47A, C46,
 C45, C44, C43, C42, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(F08U)=Sof(F09P)=Sof(F18A)=Sof(F34A)=Sof(B09B)=1-FVAR(1)
 Sof(F08T)=Sof(F09O)=Sof(F18)=Sof(F34)=Sof(B09A)=FVAR(1)
 Sof(C501)=Sof(C502)=Sof(H502)=Sof(C503)=Sof(H503)=Sof(C504)=Sof(H504)=
 Sof(C505)=Sof(H505)=Sof(C506)=Sof(C507)=Sof(H50B)=Sof(H50C)=Sof(C508)=
 Sof(H50D)=Sof(H50E)=Sof(C509)=Sof(H509)=Sof(C510)=Sof(H510)=Sof(C511)=
 Sof(H51E)=Sof(H51F)=Sof(C512)=Sof(H51G)=Sof(H51H)=1-FVAR(2)
 Sof(C158)=Sof(C159)=Sof(H159)=Sof(C160)=Sof(H160)=Sof(C161)=Sof(H161)=
 Sof(C162)=Sof(H162)=Sof(C163)=Sof(C164)=Sof(H16A)=Sof(H16B)=Sof(C165)=
 Sof(H16C)=Sof(H16D)=Sof(C166)=Sof(H166)=Sof(C167)=Sof(H167)=Sof(C168)=
 Sof(H16E)=Sof(H16F)=Sof(C169)=Sof(H16G)=Sof(H16H)=FVAR(2)
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=
 Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C52A)=
 Sof(H52C)=Sof(H52D)=Sof(C58A)=Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=
 Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=1-FVAR(3)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(C53)=Sof(C58)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56)=Sof(C55)=Sof(H55)=
 Sof(C54)=Sof(H54)=FVAR(3)
 Sof(C521)=Sof(C522)=Sof(H522)=Sof(C523)=Sof(H523)=Sof(C524)=Sof(H524)=
 Sof(C525)=Sof(H525)=Sof(C526)=Sof(C527)=Sof(H52E)=Sof(H52F)=Sof(C528)=
 Sof(H52G)=Sof(H52H)=Sof(C529)=Sof(H529)=Sof(C530)=Sof(H530)=Sof(C531)=
 Sof(H53A)=Sof(H53B)=Sof(C532)=Sof(H53C)=Sof(H53D)=1-FVAR(4)
 Sof(C222)=Sof(H22A)=Sof(H22B)=Sof(C223)=Sof(H22C)=Sof(H22D)=Sof(C224)=
 Sof(H224)=Sof(C225)=Sof(H225)=Sof(C226)=Sof(H22E)=Sof(H22F)=Sof(C227)=
 Sof(H22G)=Sof(H22H)=Sof(C229)=Sof(H229)=Sof(C228)=Sof(C233)=Sof(C232)=
 Sof(H232)=Sof(C231)=Sof(H231)=Sof(C230)=Sof(H230)=FVAR(4)
 Sof(C550)=Sof(C551)=Sof(H551)=Sof(C552)=Sof(H552)=Sof(C553)=Sof(H553)=
 Sof(C554)=Sof(H554)=Sof(C555)=Sof(C556)=Sof(H55B)=Sof(H55C)=Sof(C557)=
 Sof(H55D)=Sof(H55E)=Sof(C558)=Sof(H558)=Sof(C559)=Sof(H559)=Sof(C560)=
 Sof(H56B)=Sof(H56C)=Sof(C561)=Sof(H56D)=Sof(H56E)=1-FVAR(5)
 Sof(C105)=Sof(H10A)=Sof(H10B)=Sof(C106)=Sof(H10C)=Sof(H10D)=Sof(C107)=
 Sof(H107)=Sof(C108)=Sof(H108)=Sof(C109)=Sof(H10E)=Sof(H10F)=Sof(C110)=
 Sof(H11A)=Sof(H11B)=Sof(C111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=
 Sof(C114)=Sof(H114)=Sof(C115)=Sof(H115)=Sof(C116)=FVAR(5)
 Sof(C575)=Sof(C576)=Sof(H576)=Sof(C577)=Sof(H577)=Sof(C578)=Sof(H578)=
 Sof(C579)=Sof(H579)=Sof(C580)=Sof(C581)=Sof(H58A)=Sof(H58B)=Sof(C582)=
 Sof(H58C)=Sof(H58D)=Sof(C583)=Sof(H583)=Sof(C584)=Sof(H584)=Sof(C585)=
 Sof(H58E)=Sof(H58F)=Sof(C586)=Sof(H58G)=Sof(H58H)=1-FVAR(6)
 Sof(C280)=Sof(H28C)=Sof(H28D)=Sof(C281)=Sof(H28E)=Sof(H28F)=Sof(C282)=
 Sof(H282)=Sof(C283)=Sof(H283)=Sof(C284)=Sof(H28G)=Sof(H28H)=Sof(C285)=
 Sof(H28I)=Sof(H28J)=Sof(C286)=Sof(C291)=Sof(C290)=Sof(H290)=Sof(C289)=
 Sof(H289)=Sof(C288)=Sof(H288)=Sof(C287)=Sof(H287)=FVAR(6)
 Fixed Sof: C1(0.5) H1(0.5) C8(0.5) C5AA(0.5) H5AA(0.5) C2AA(0.5) H2AA(0.5)
 C1AA(0.5) H1AA(0.5) C0AA(0.5) H0AA(0.5) C0BA(0.5) C9AA(0.5) H9AA(0.5)
 C7AA(0.5) H7AA(0.5) C8AA(0.5) H8AA(0.5) C1BA(0.5) H1BA(0.5) C6AA(0.5)
 H6AA(0.5) C3BA(0.5) H3BA(0.5) H3BB(0.5) H3BC(0.5) C2BA(0.5) H2BA(0.5)
 H2BB(0.5) H2BC(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C27(H27A,H27B), C28(H28A,H28B), C71(H71A,
 H71B), C72(H72A,H72B), C85(H85A,H85B), C86(H86A,H86B), C129(H12A,H12B),
 C130(H13C,H13D), C143(H14C,H14D), C144(H14E,H14F), C188(H18A,H18B), C189(H18C,
 H18D), C202(H20A,H20B), C203(H20C,H20D), C246(H24A,H24B), C247(H24C,H24D),
 C260(H26A,H26B), C261(H26C,H26D), C47(H47A,H47B), C48(H48A,H48B), C51(H51A,
 H51B), C52(H52A,H52B), C105(H10A,H10B), C106(H10C,H10D), C109(H10E,H10F),
 C110(H11A,H11B), C164(H16A,H16B), C165(H16C,H16D), C168(H16E,H16F), C169(H16G,
 H16H), C222(H22A,H22B), C223(H22C,H22D), C226(H22E,H22F), C227(H22G,H22H),
 C280(H28C,H28D), C281(H28E,H28F), C284(H28G,H28H), C285(H28I,H28J), C47A(H47C,
 H47D), C48A(H48C,H48D), C51A(H51C,H51D), C52A(H52C,H52D), C507(H50B,H50C),
 C508(H50D,H50E), C511(H51E,H51F), C512(H51G,H51H), C527(H52E,H52F), C528(H52G,
 H52H), C531(H53A,H53B), C532(H53C,H53D), C556(H55B,H55C), C557(H55D,H55E),
 C560(H56B,H56C), C561(H56D,H56E), C581(H58A,H58B), C582(H58C,H58D), C585(H58E,
 H58F), C586(H58G,H58H)
7.b Me refined with riding coordinates:
 C3BA(H3BA,H3BB,H3BC), C2BA(H2BA,H2BB,H2BC)
7.c Aromatic/amide H refined with riding coordinates:
 C156(H156), C155(H155), C153(H153), C2(H2), C4(H4), C5(H5), C9(H9), C11(H11),
 C12(H12), C16(H16), C19(H19), C20(H20), C23(H23), C25(H25), C26(H26), C30(H30),
  C33(H33), C34(H34), C37(H37), C39(H39), C40(H40), C42(H42), C43(H43),
 C44(H44), C45(H45), C60(H60), C63(H63), C64(H64), C67(H67), C69(H69), C70(H70),
  C74(H74), C77(H77), C78(H78), C81(H81), C83(H83), C84(H84), C88(H88),
 C91(H91), C92(H92), C95(H95), C97(H97), C98(H98), C118(H118), C121(H121),
 C122(H122), C125(H125), C128(H128), C127(H127), C132(H132), C135(H135),
 C136(H136), C139(H139), C141(H141), C142(H142), C146(H146), C149(H149),
 C150(H150), C172(H172), C171(H171), C174(H174), C173(H173), C177(H177),
 C180(H180), C181(H181), C184(H184), C186(H186), C187(H187), C191(H191),
 C194(H194), C195(H195), C198(H198), C200(H200), C201(H201), C205(H205),
 C208(H208), C209(H209), C212(H212), C214(H214), C215(H215), C217(H217),
 C220(H220), C219(H219), C218(H218), C235(H235), C238(H238), C239(H239),
 C242(H242), C244(H244), C245(H245), C249(H249), C252(H252), C253(H253),
 C256(H256), C258(H258), C259(H259), C263(H263), C266(H266), C267(H267),
 C270(H270), C272(H272), C273(H273), C275(H275), C276(H276), C277(H277),
 C278(H278), C563(H563), C564(H564), C565(H565), C566(H566), C49(H49), C50(H50),
  C57(H57), C56(H56), C55(H55), C54(H54), C107(H107), C108(H108), C112(H112),
 C113(H113), C114(H114), C115(H115), C159(H159), C160(H160), C161(H161),
 C162(H162), C166(H166), C167(H167), C224(H224), C225(H225), C229(H229),
 C232(H232), C231(H231), C230(H230), C282(H282), C283(H283), C290(H290),
 C289(H289), C288(H288), C287(H287), C49A(H49A), C50A(H50A), C54A(H54A),
 C55A(H55A), C56A(H56A), C57A(H57A), C502(H502), C503(H503), C504(H504),
 C505(H505), C509(H509), C510(H510), C522(H522), C523(H523), C524(H524),
 C525(H525), C529(H529), C530(H530), C551(H551), C552(H552), C553(H553),
 C554(H554), C558(H558), C559(H559), C576(H576), C577(H577), C578(H578),
 C579(H579), C583(H583), C584(H584), C1(H1), C5AA(H5AA), C2AA(H2AA), C1AA(H1AA),
  C0AA(H0AA), C9AA(H9AA), C7AA(H7AA), C8AA(H8AA), C1BA(H1BA), C6AA(H6AA)
7.d Fitted hexagon refined as free rotating group:
 N152(C151,C156,C155,C154,C153), C126(C125,N124,C123,C128,C127), C172(C171,
 C170,C175,C174,C173), C217(C216,C221,C220,C219,C218), C53(C58,C57,C56,C55,C54),
  C111(C112,C113,C114,C115,C116), C158(C159,C160,C161,C162,C163), C229(C228,
 C233,C232,C231,C230), C286(C291,C290,C289,C288,C287), C58A(C53A,C54A,C55A,C56A,
 C57A), C501(C502,C503,C504,C505,C506), C521(C522,C523,C524,C525,C526),
 C550(C551,C552,C553,C554,C555), C575(C576,C577,C578,C579,C580), C1(C8,C5AA,
 C2AA,C1AA,C0AA), C0BA(C9AA,C7AA,C8AA,C1BA,C6AA)
7.e Idealised Me refined as rotating group:
 C4AA(H4AA,H4AB,H4AC), C076(H07A,H07B,H07C), C09C(H09A,H09B,H09C)
;
_shelx_res_checksum              5779
_shelx_hkl_checksum              63407
_shelx_fab_checksum              90515
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.545