Stepwise deprotonation of truxene: structures, metal complexation, and charge-dependent optical properties.
Guo, Yumeng; Torchon, Herdya S.; Zhu, Yikun; Wei, Zheng; Zhang, Zhenyi; Han, Haixiang; Petrukhina, Marina A.; Zhou, Zheng; Chemical science 14 (2023) 13219–13227; doi:10.1039/d3sc04885c

data_1570225
_publ_section_title
;
 Stepwise deprotonation of truxene: structures, metal complexation, and
 charge-dependent optical properties.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              13219
_journal_page_last               13227
_journal_paper_doi               10.1039/d3sc04885c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C51 H63 K2 O12, C20 H40 K O8, C4 H8 O'
_chemical_formula_sum            'C75 H111 K3 O21'
_chemical_formula_weight         1465.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-18 deposited with the CCDC.	2023-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4467(7)
_cell_length_b                   15.8867(9)
_cell_length_c                   18.3239(10)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.675
_cell_measurement_theta_min      2.184
_cell_volume                     3823.3(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector
;
DECTRIS PILATUS3 X 1M(CdTe) pixel array detector
;
_diffrn_detector_area_resol_mean 30
_diffrn_detector_type            'CMOS pixel array detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Huber 4-circle diffractometer'
_diffrn_measurement_method       'phi rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Si(111) & Si(311)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            139675
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         16.694
_diffrn_reflns_theta_min         0.902
_diffrn_source                   synchrotron
_diffrn_source_current           103.0
_diffrn_source_power             103.0
_diffrn_source_type
;
Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab
;
_diffrn_source_voltage           1000.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.1487 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.7694.
The \l/2 correction factor is not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1673
_refine_ls_number_reflns         21383
_refine_ls_number_restraints     4175
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1693P)^2^+0.5693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2668
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                17459
_reflns_number_total             21383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04885c2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1570220--1570225.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1570225
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(17)
 0.17(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C36-C37
 1.54 with sigma of 0.02
 C39-C38 = C28-C29 = C31-C30 = C33-C32 = C35-C34 = C36-C37
 1.54 with sigma of 0.02
 O6-C38 = O6-C37 = O5-C36 = O5-C35 = O4-C34 = O4-C33 = O3-C32 = O3-C31 = O2-
 C30 = O2-C29 = O1-C28 = O1-C39
 1.43 with sigma of 0.02
 O20-C71 = O20-C68
 1.43 with sigma of 0.02
 C70-C71 = C69-C68 = C69-C70
 1.54 with sigma of 0.02
 C71-C68
 2.4 with sigma of 0.02
 C46-C47 = C48-C49 = C51-C50 = C41-C40 = C43-C42 = C45-C44
 1.54 with sigma of 0.02
 O10-C45 = O10-C46 = O9-C44 = O9-C43 = O8-C42 = O8-C41 = O7-C40 = O7-C51 = O12-
 C50 = O12-C49 = O11-C48 = O11-C47
 1.43 with sigma of 0.02
 C46-C45
 2.4 with sigma of 0.02
 C47-O10
 2.4 with sigma of 0.02
 C50-C49
 2.4 with sigma of 0.02
 C61X-C62X
 2.4 with sigma of 0.02
 O13X-C63X = O13X-C52X
 1.43 with sigma of 0.02
 C63X-C52X
 2.4 with sigma of 0.02
 C70X-C69X = C70X-C71X = C69X-C68X
 1.54 with sigma of 0.02
 O20X-C71X = O20X-C68X
 1.43 with sigma of 0.02
 O6-O1 \\sim O1-O2 \\sim O2-O3 \\sim O3-O4 \\sim O4-O5 \\sim O5-O6
 with sigma of 0.02
 O12-O11 \\sim O11-O10 \\sim O10-O9 \\sim O9-O8 \\sim O8-O7 \\sim O7-O12
 with sigma of 0.02
 O4-C34 \\sim O4X-C34X
 with sigma of 0.02
 O4-C33 \\sim O4X-C33X
 with sigma of 0.02
 O1-C39 \\sim O1X-C39X
 with sigma of 0.02
 O1-C28 \\sim O1X-C28X
 with sigma of 0.02
 O6-C38 \\sim O6X-C38X
 with sigma of 0.02
 O6-C37 \\sim O6X-C37X
 with sigma of 0.02
 C34-C35 \\sim C34X-C35X
 with sigma of 0.02
 O3-C31 \\sim O3X-C31X
 with sigma of 0.02
 O3-C32 \\sim O3X-C32X
 with sigma of 0.02
 C30-C31 \\sim C30X-C31X
 with sigma of 0.02
 C30-O2 \\sim C30X-O2X
 with sigma of 0.02
 O5-C35 \\sim O5X-C35X
 with sigma of 0.02
 O5-C36 \\sim O5X-C36X
 with sigma of 0.02
 C29-C28 \\sim C29X-C28X
 with sigma of 0.02
 C29-O2 \\sim C29X-O2X
 with sigma of 0.02
 C39-C38 \\sim C39X-C38X
 with sigma of 0.02
 C37-C36 \\sim C37X-C36X
 with sigma of 0.02
 C33-C32 \\sim C33X-C32X
 with sigma of 0.02
 O4-C35 \\sim O4X-C35X
 with sigma of 0.04
 O4-C32 \\sim O4X-C32X
 with sigma of 0.04
 O1-C29 \\sim O1X-C29X
 with sigma of 0.04
 O1-C38 \\sim O1X-C38X
 with sigma of 0.04
 O6-C39 \\sim O6X-C39X
 with sigma of 0.04
 O6-C36 \\sim O6X-C36X
 with sigma of 0.04
 C34-O5 \\sim C34X-O5X
 with sigma of 0.04
 C34-C33 \\sim C34X-C33X
 with sigma of 0.04
 O3-C30 \\sim O3X-C30X
 with sigma of 0.04
 O3-C33 \\sim O3X-C33X
 with sigma of 0.04
 C30-C29 \\sim C30X-C29X
 with sigma of 0.04
 O5-C37 \\sim O5X-C37X
 with sigma of 0.04
 C31-C32 \\sim C31X-C32X
 with sigma of 0.04
 C31-O2 \\sim C31X-O2X
 with sigma of 0.04
 C39-C28 \\sim C39X-C28X
 with sigma of 0.04
 C38-C37 \\sim C38X-C37X
 with sigma of 0.04
 C28-O2 \\sim C28X-O2X
 with sigma of 0.04
 C35-C36 \\sim C35X-C36X
 with sigma of 0.04
 O7-C51 \\sim O12X-C49X
 with sigma of 0.02
 O7-C40 \\sim O12X-C50X
 with sigma of 0.02
 C41-O8 \\sim C51X-O7X
 with sigma of 0.02
 C41-C40 \\sim C51X-C50X
 with sigma of 0.02
 O8-C42 \\sim O7X-C40X
 with sigma of 0.02
 C51-C50 \\sim C49X-C48X
 with sigma of 0.02
 C45-C44 \\sim C43X-C42X
 with sigma of 0.02
 C45-O10 \\sim C43X-O9X
 with sigma of 0.02
 C44-O9 \\sim C42X-O8X
 with sigma of 0.02
 O9-C43 \\sim O8X-C41X
 with sigma of 0.02
 C42-C43 \\sim C40X-C41X
 with sigma of 0.02
 O10-C46 \\sim O9X-C44X
 with sigma of 0.02
 C50-O12 \\sim C48X-O11X
 with sigma of 0.02
 O12-C49 \\sim O11X-C47X
 with sigma of 0.02
 O11-C48 \\sim O10X-C46X
 with sigma of 0.02
 O11-C47 \\sim O10X-C45X
 with sigma of 0.02
 C48-C49 \\sim C46X-C47X
 with sigma of 0.02
 C47-C46 \\sim C45X-C44X
 with sigma of 0.02
 O7-C41 \\sim O12X-C51X
 with sigma of 0.04
 O7-C50 \\sim O12X-C48X
 with sigma of 0.04
 C41-C42 \\sim C51X-C40X
 with sigma of 0.04
 O8-C43 \\sim O7X-C41X
 with sigma of 0.04
 O8-C40 \\sim O7X-C50X
 with sigma of 0.04
 C51-O12 \\sim C49X-O11X
 with sigma of 0.04
 C51-C40 \\sim C49X-C50X
 with sigma of 0.04
 C45-O9 \\sim C43X-O8X
 with sigma of 0.04
 C45-C46 \\sim C43X-C44X
 with sigma of 0.04
 C44-O10 \\sim C42X-O9X
 with sigma of 0.04
 C44-C43 \\sim C42X-C41X
 with sigma of 0.04
 O9-C42 \\sim O8X-C40X
 with sigma of 0.04
 O10-C47 \\sim O9X-C45X
 with sigma of 0.04
 C50-C49 \\sim C48X-C47X
 with sigma of 0.04
 O12-C48 \\sim O11X-C46X
 with sigma of 0.04
 O11-C49 \\sim O10X-C47X
 with sigma of 0.04
 O11-C46 \\sim O10X-C44X
 with sigma of 0.04
 C48-C47 \\sim C46X-C45X
 with sigma of 0.04
 O20-C71 \\sim O20X-C68X
 with sigma of 0.02
 O20-C68 \\sim O20X-C71X
 with sigma of 0.02
 C71-C70 \\sim C68X-C69X
 with sigma of 0.02
 C70-C69 \\sim C69X-C70X
 with sigma of 0.02
 C69-C68 \\sim C70X-C71X
 with sigma of 0.02
 O20-C70 \\sim O20X-C69X
 with sigma of 0.04
 O20-C69 \\sim O20X-C70X
 with sigma of 0.04
 C71-C69 \\sim C68X-C70X
 with sigma of 0.04
 C71-C68 \\sim C68X-C71X
 with sigma of 0.04
 C70-C68 \\sim C69X-C71X
 with sigma of 0.04
 O16-C57 \\sim O16X-C57X
 with sigma of 0.02
 O16-C58 \\sim O16X-C58X
 with sigma of 0.02
 O18-C61 \\sim O18X-C61X
 with sigma of 0.02
 O18-C62 \\sim O18X-C62X
 with sigma of 0.02
 O14-C54 \\sim O14X-C54X
 with sigma of 0.02
 O14-C53 \\sim O14X-C53X
 with sigma of 0.02
 C57-C56 \\sim C57X-C56X
 with sigma of 0.02
 C58-C59 \\sim C58X-C59X
 with sigma of 0.02
 C61-C60 \\sim C61X-C60X
 with sigma of 0.02
 C62-C63 \\sim C62X-C63X
 with sigma of 0.02
 O17-C59 \\sim O17X-C59X
 with sigma of 0.02
 O17-C60 \\sim O17X-C60X
 with sigma of 0.02
 C54-C55 \\sim C54X-C55X
 with sigma of 0.02
 O15-C56 \\sim O15X-C56X
 with sigma of 0.02
 O15-C55 \\sim O15X-C55X
 with sigma of 0.02
 C53-C52 \\sim C53X-C52X
 with sigma of 0.02
 C63-O13 \\sim C63X-O13X
 with sigma of 0.02
 O13-C52 \\sim O13X-C52X
 with sigma of 0.02
 O16-C56 \\sim O16X-C56X
 with sigma of 0.04
 O16-C59 \\sim O16X-C59X
 with sigma of 0.04
 O18-C63 \\sim O18X-C63X
 with sigma of 0.04
 O18-C60 \\sim O18X-C60X
 with sigma of 0.04
 O14-C55 \\sim O14X-C55X
 with sigma of 0.04
 O14-C52 \\sim O14X-C52X
 with sigma of 0.04
 C57-C58 \\sim C57X-C58X
 with sigma of 0.04
 C57-O15 \\sim C57X-O15X
 with sigma of 0.04
 C58-O17 \\sim C58X-O17X
 with sigma of 0.04
 C61-C62 \\sim C61X-C62X
 with sigma of 0.04
 C61-O17 \\sim C61X-O17X
 with sigma of 0.04
 C62-O13 \\sim C62X-O13X
 with sigma of 0.04
 C54-O15 \\sim C54X-O15X
 with sigma of 0.04
 C54-C53 \\sim C54X-C53X
 with sigma of 0.04
 C53-O13 \\sim C53X-O13X
 with sigma of 0.04
 C56-C55 \\sim C56X-C55X
 with sigma of 0.04
 C63-C52 \\sim C63X-C52X
 with sigma of 0.04
 C59-C60 \\sim C59X-C60X
 with sigma of 0.04
 O19-C64 \\sim O19X-C67X
 with sigma of 0.02
 O19-C67 \\sim O19X-C64X
 with sigma of 0.02
 C64-C65 \\sim C67X-C66X
 with sigma of 0.02
 C67-C66 \\sim C64X-C65X
 with sigma of 0.02
 C65-C66 \\sim C66X-C65X
 with sigma of 0.02
 O19-C65 \\sim O19X-C66X
 with sigma of 0.04
 O19-C66 \\sim O19X-C65X
 with sigma of 0.04
 C64-C67 \\sim C67X-C64X
 with sigma of 0.04
 C64-C66 \\sim C67X-C65X
 with sigma of 0.04
 C67-C65 \\sim C64X-C66X
 with sigma of 0.04
 C10-C11 \\sim C19X-C20X
 with sigma of 0.02
 C10-C18 \\sim C19X-C27X
 with sigma of 0.02
 C10-C9 \\sim C19X-C18X
 with sigma of 0.02
 C11-C12 \\sim C20X-C21X
 with sigma of 0.02
 C5-C4 \\sim C14X-C13X
 with sigma of 0.02
 C5-C6 \\sim C14X-C15X
 with sigma of 0.02
 C27-C26 \\sim C9X-C8X
 with sigma of 0.02
 C27-C1 \\sim C9X-C10X
 with sigma of 0.02
 C27-C19 \\sim C9X-C1X
 with sigma of 0.02
 C18-C19 \\sim C27X-C1X
 with sigma of 0.02
 C18-C17 \\sim C27X-C26X
 with sigma of 0.02
 C26-C21 \\sim C8X-C3X
 with sigma of 0.02
 C26-C25 \\sim C8X-C7X
 with sigma of 0.02
 C3-C4 \\sim C12X-C13X
 with sigma of 0.02
 C24-C23 \\sim C6X-C5X
 with sigma of 0.02
 C24-C25 \\sim C6X-C7X
 with sigma of 0.02
 C21-C22 \\sim C3X-C4X
 with sigma of 0.02
 C21-C20 \\sim C3X-C2X
 with sigma of 0.02
 C14-C15 \\sim C23X-C24X
 with sigma of 0.02
 C14-C13 \\sim C23X-C22X
 with sigma of 0.02
 C12-C17 \\sim C21X-C26X
 with sigma of 0.02
 C12-C13 \\sim C21X-C22X
 with sigma of 0.02
 C22-C23 \\sim C4X-C5X
 with sigma of 0.02
 C7-C8 \\sim C16X-C17X
 with sigma of 0.02
 C7-C6 \\sim C16X-C15X
 with sigma of 0.02
 C1-C2 \\sim C10X-C11X
 with sigma of 0.02
 C1-C9 \\sim C10X-C18X
 with sigma of 0.02
 C8-C9 \\sim C17X-C18X
 with sigma of 0.02
 C15-C16 \\sim C24X-C25X
 with sigma of 0.02
 C19-C20 \\sim C1X-C2X
 with sigma of 0.02
 C17-C16 \\sim C26X-C25X
 with sigma of 0.02
 C10-C12 \\sim C19X-C21X
 with sigma of 0.04
 C10-C1 \\sim C19X-C10X
 with sigma of 0.04
 C10-C8 \\sim C19X-C17X
 with sigma of 0.04
 C10-C19 \\sim C19X-C1X
 with sigma of 0.04
 C10-C17 \\sim C19X-C26X
 with sigma of 0.04
 C11-C18 \\sim C20X-C27X
 with sigma of 0.04
 C11-C17 \\sim C20X-C26X
 with sigma of 0.04
 C11-C13 \\sim C20X-C22X
 with sigma of 0.04
 C11-C9 \\sim C20X-C18X
 with sigma of 0.04
 C5-C3 \\sim C14X-C12X
 with sigma of 0.04
 C5-C7 \\sim C14X-C16X
 with sigma of 0.04
 C27-C18 \\sim C9X-C27X
 with sigma of 0.04
 C27-C21 \\sim C9X-C3X
 with sigma of 0.04
 C27-C25 \\sim C9X-C7X
 with sigma of 0.04
 C27-C20 \\sim C9X-C2X
 with sigma of 0.04
 C27-C2 \\sim C9X-C11X
 with sigma of 0.04
 C27-C9 \\sim C9X-C18X
 with sigma of 0.04
 C18-C12 \\sim C27X-C21X
 with sigma of 0.04
 C18-C20 \\sim C27X-C2X
 with sigma of 0.04
 C18-C16 \\sim C27X-C25X
 with sigma of 0.04
 C18-C9 \\sim C27X-C18X
 with sigma of 0.04
 C26-C24 \\sim C8X-C6X
 with sigma of 0.04
 C26-C22 \\sim C8X-C4X
 with sigma of 0.04
 C26-C1 \\sim C8X-C10X
 with sigma of 0.04
 C26-C19 \\sim C8X-C1X
 with sigma of 0.04
 C26-C20 \\sim C8X-C2X
 with sigma of 0.04
 C3-C7 \\sim C12X-C16X
 with sigma of 0.04
 C3-C1 \\sim C12X-C10X
 with sigma of 0.04
 C3-C8 \\sim C12X-C17X
 with sigma of 0.04
 C3-C2 \\sim C12X-C11X
 with sigma of 0.04
 C3-C9 \\sim C12X-C18X
 with sigma of 0.04
 C24-C22 \\sim C6X-C4X
 with sigma of 0.04
 C21-C23 \\sim C3X-C5X
 with sigma of 0.04
 C21-C19 \\sim C3X-C1X
 with sigma of 0.04
 C21-C25 \\sim C3X-C7X
 with sigma of 0.04
 C14-C12 \\sim C23X-C21X
 with sigma of 0.04
 C14-C16 \\sim C23X-C25X
 with sigma of 0.04
 C12-C16 \\sim C21X-C25X
 with sigma of 0.04
 C22-C20 \\sim C4X-C2X
 with sigma of 0.04
 C7-C2 \\sim C16X-C11X
 with sigma of 0.04
 C7-C9 \\sim C16X-C18X
 with sigma of 0.04
 C1-C8 \\sim C10X-C17X
 with sigma of 0.04
 C1-C19 \\sim C10X-C1X
 with sigma of 0.04
 C8-C4 \\sim C17X-C13X
 with sigma of 0.04
 C8-C2 \\sim C17X-C11X
 with sigma of 0.04
 C8-C6 \\sim C17X-C15X
 with sigma of 0.04
 C15-C17 \\sim C24X-C26X
 with sigma of 0.04
 C15-C13 \\sim C24X-C22X
 with sigma of 0.04
 C23-C25 \\sim C5X-C7X
 with sigma of 0.04
 C19-C17 \\sim C1X-C26X
 with sigma of 0.04
 C17-C13 \\sim C26X-C22X
 with sigma of 0.04
 C4-C2 \\sim C13X-C11X
 with sigma of 0.04
 C4-C6 \\sim C13X-C15X
 with sigma of 0.04
 C2-C9 \\sim C11X-C18X
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O4 \\sim O1 \\sim O6 \\sim C34 \\sim O3 \\sim C30 \\sim O5 \\sim C31 \\sim C29
\\sim C39 \\sim C38 \\sim C28 \\sim C37 \\sim C35 \\sim C36 \\sim C33 \\sim C32
\\sim O2 \\sim O4X \\sim O1X \\sim O6X \\sim C34X \\sim O3X \\sim C30X \\sim
O5X \\sim C31X \\sim C29X \\sim C39X \\sim C38X \\sim C28X \\sim C37X \\sim
C35X \\sim C36X \\sim C33X \\sim C32X \\sim O2X: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O7 \\sim C41 \\sim O8 \\sim C51 \\sim C45 \\sim C44 \\sim O9 \\sim C42 \\sim
O10 \\sim C43 \\sim C50 \\sim O12 \\sim O11 \\sim C48 \\sim C40 \\sim C47 \\sim
C49 \\sim C46 \\sim O12X \\sim C51X \\sim O7X \\sim C49X \\sim C43X \\sim C42X
\\sim O8X \\sim C40X \\sim O9X \\sim C41X \\sim C48X \\sim O11X \\sim O10X
\\sim C46X \\sim C50X \\sim C45X \\sim C47X \\sim C44X: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O20 \\sim C71 \\sim C70 \\sim C69 \\sim C68 \\sim O20X \\sim C68X \\sim C69X
\\sim C70X \\sim C71X: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O16 \\sim O18 \\sim O14 \\sim C57 \\sim C58 \\sim C61 \\sim C62 \\sim O17 \\sim
C54 \\sim O15 \\sim C53 \\sim C56 \\sim C63 \\sim O13 \\sim C59 \\sim C55 \\sim
C60 \\sim C52 \\sim O16X \\sim O18X \\sim O14X \\sim C57X \\sim C58X \\sim C61X
\\sim C62X \\sim O17X \\sim C54X \\sim O15X \\sim C53X \\sim C56X \\sim C63X
\\sim O13X \\sim C59X \\sim C55X \\sim C60X \\sim C52X: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O19 \\sim C64 \\sim C67 \\sim C65 \\sim C66 \\sim C64X \\sim O19X \\sim C67X
\\sim C65X \\sim C66X: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C10 \\sim C11 \\sim C5 \\sim C27 \\sim C18 \\sim C26 \\sim C3 \\sim C24 \\sim
C21 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C12 \\sim C13 \\sim C22 \\sim
C7 \\sim C1 \\sim C8 \\sim C23 \\sim C19 \\sim C4 \\sim C25 \\sim C20 \\sim C2
\\sim C9 \\sim C6 \\sim C19X \\sim C20X \\sim C14X \\sim C9X \\sim C27X \\sim
C8X \\sim C12X \\sim C6X \\sim C3X \\sim C23X \\sim C22X \\sim C21X \\sim C26X
\\sim C25X \\sim C24X \\sim C4X \\sim C16X \\sim C10X \\sim C17X \\sim C5X
\\sim C1X \\sim C13X \\sim C7X \\sim C2X \\sim C11X \\sim C18X \\sim C15X:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 O7, C41, O8, C51, C45, C44, O9, C42, O10, C43, C50, O12, O11, C48, C40, C47,
 C49, C46, O12X, C51X, O7X, C49X, C43X, C42X, O8X, C40X, O9X, C41X, C48X, O11X,
 O10X, C46X, C50X, C45X, C47X, C44X, O4, O1, O6, C34, O3, C30, O5, C31, C29,
 C39, C38, C28, C37, C35, C36, C33, C32, O2, O4X, O1X, O6X, C34X, O3X, C30X,
 O5X, C31X, C29X, C39X, C38X, C28X, C37X, C35X, C36X, C33X, C32X, O2X, C70X,
 O17X, O16X, O20, O19X, O19, O13, O15X, O15, O20X, O14, O18, O18X, C59X, C60X,
 C57X, C58X, C71, C68, C64X, C67X, C64, C67, C63, C52, C56X, C55X, C56, C55,
 C68X, C71X, C54, C53, C61, C62, C61X, C62X, C70, C69, C65X, C66X, C65, C66,
 C54X, C57, C69X, C60, C63X, O14X, O16, O17, O13X, C53X, C58, C59, C52X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O4X)=Sof(O1X)=Sof(O6X)=Sof(C34X)=Sof(H34C)=Sof(H34D)=Sof(O3X)=Sof(C30X)=
 Sof(H30C)=Sof(H30D)=Sof(O5X)=Sof(C31X)=Sof(H31C)=Sof(H31D)=Sof(C29X)=Sof(H29C)=
 Sof(H29D)=Sof(C39X)=Sof(H39C)=Sof(H39D)=Sof(C38X)=Sof(H38C)=Sof(H38D)=
 Sof(C28X)=Sof(H28C)=Sof(H28D)=Sof(C37X)=Sof(H37C)=Sof(H37D)=Sof(C35X)=
 Sof(H35C)=Sof(H35D)=Sof(C36X)=Sof(H36C)=Sof(H36D)=Sof(C33X)=Sof(H33C)=
 Sof(H33D)=Sof(C32X)=Sof(H32C)=Sof(H32D)=Sof(O2X)=1-FVAR(1)
 Sof(O4)=Sof(O1)=Sof(O6)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(O3)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(O5)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(O2)=FVAR(1)
 Sof(O12X)=Sof(C51X)=Sof(H51C)=Sof(H51D)=Sof(O7X)=Sof(C49X)=Sof(H49C)=
 Sof(H49D)=Sof(C43X)=Sof(H43C)=Sof(H43D)=Sof(C42X)=Sof(H42C)=Sof(H42D)=Sof(O8X)=
 Sof(C40X)=Sof(H40C)=Sof(H40D)=Sof(O9X)=Sof(C41X)=Sof(H41C)=Sof(H41D)=Sof(C48X)=
 Sof(H48C)=Sof(H48D)=Sof(O11X)=Sof(O10X)=Sof(C46X)=Sof(H46C)=Sof(H46D)=
 Sof(C50X)=Sof(H50C)=Sof(H50D)=Sof(C45X)=Sof(H45C)=Sof(H45D)=Sof(C47X)=
 Sof(H47C)=Sof(H47D)=Sof(C44X)=Sof(H44C)=Sof(H44D)=1-FVAR(2)
 Sof(O7)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(O8)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(O9)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(O10)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C50)=Sof(H50A)=
 Sof(H50B)=Sof(O12)=Sof(O11)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=FVAR(2)
 Sof(O20X)=Sof(C68X)=Sof(H68C)=Sof(H68D)=Sof(C69X)=Sof(H69C)=Sof(H69D)=
 Sof(C70X)=Sof(H70C)=Sof(H70D)=Sof(C71X)=Sof(H71C)=Sof(H71D)=1-FVAR(3)
 Sof(O20)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(3)
 Sof(O16X)=Sof(O18X)=Sof(O14X)=Sof(C57X)=Sof(H57C)=Sof(H57D)=Sof(C58X)=
 Sof(H58C)=Sof(H58D)=Sof(C61X)=Sof(H61C)=Sof(H61D)=Sof(C62X)=Sof(H62C)=
 Sof(H62D)=Sof(O17X)=Sof(C54X)=Sof(H54C)=Sof(H54D)=Sof(O15X)=Sof(C53X)=
 Sof(H53C)=Sof(H53D)=Sof(C56X)=Sof(H56C)=Sof(H56D)=Sof(C63X)=Sof(H63C)=
 Sof(H63D)=Sof(O13X)=Sof(C59X)=Sof(H59C)=Sof(H59D)=Sof(C55X)=Sof(H55C)=
 Sof(H55D)=Sof(C60X)=Sof(H60C)=Sof(H60D)=Sof(C52X)=Sof(H52C)=Sof(H52D)=1-FVAR(4)
 Sof(O16)=Sof(O18)=Sof(O14)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(O17)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(O15)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C56)=
 Sof(H56A)=Sof(H56B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(O13)=Sof(C59)=Sof(H59A)=
 Sof(H59B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C52)=
 Sof(H52A)=Sof(H52B)=FVAR(4)
 Sof(C64X)=Sof(H64C)=Sof(H64D)=Sof(O19X)=Sof(C67X)=Sof(H67C)=Sof(H67D)=
 Sof(C65X)=Sof(H65C)=Sof(H65D)=Sof(C66X)=Sof(H66C)=Sof(H66D)=1-FVAR(5)
 Sof(O19)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C65)=
 Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=FVAR(5)
 Sof(C19X)=Sof(C20X)=Sof(H20X)=Sof(C14X)=Sof(H14X)=Sof(C9X)=Sof(C27X)=Sof(C8X)=
 Sof(C12X)=Sof(C6X)=Sof(H6X)=Sof(C3X)=Sof(C23X)=Sof(H23X)=Sof(C22X)=Sof(H22X)=
 Sof(C21X)=Sof(C26X)=Sof(C25X)=Sof(H25X)=Sof(C24X)=Sof(H24X)=Sof(C4X)=Sof(H4X)=
 Sof(C16X)=Sof(H16X)=Sof(C10X)=Sof(C17X)=Sof(C5X)=Sof(H5X)=Sof(C1X)=Sof(C13X)=
 Sof(H13X)=Sof(C7X)=Sof(H7X)=Sof(C2X)=Sof(H2X)=Sof(C11X)=Sof(H11X)=Sof(C18X)=
 Sof(C15X)=Sof(H15X)=1-FVAR(6)
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C5)=Sof(H5)=Sof(C27)=Sof(C18)=Sof(C26)=Sof(C3)=
 Sof(C24)=Sof(H24)=Sof(C21)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(C17)=Sof(C12)=Sof(C13)=Sof(H13)=Sof(C22)=Sof(H22)=Sof(C7)=Sof(H7)=
 Sof(C1)=Sof(C8)=Sof(C23)=Sof(H23)=Sof(C19)=Sof(C4)=Sof(H4)=Sof(C25)=Sof(H25)=
 Sof(C20)=Sof(H20)=Sof(C2)=Sof(H2)=Sof(C9)=Sof(C6)=Sof(H6)=FVAR(6)
7.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C54(H54A,
 H54B), C34(H34A,H34B), C64(H64A,H64B), C53(H53A,H53B), C56(H56A,H56B),
 C63(H63A,H63B), C71(H71A,H71B), C59(H59A,H59B), C30(H30A,H30B), C67(H67A,H67B),
  C55(H55A,H55B), C60(H60A,H60B), C31(H31A,H31B), C29(H29A,H29B), C52(H52A,
 H52B), C65(H65A,H65B), C39(H39A,H39B), C66(H66A,H66B), C70(H70A,H70B),
 C38(H38A,H38B), C69(H69A,H69B), C28(H28A,H28B), C37(H37A,H37B), C35(H35A,H35B),
  C36(H36A,H36B), C33(H33A,H33B), C32(H32A,H32B), C41(H41A,H41B), C51(H51A,
 H51B), C45(H45A,H45B), C44(H44A,H44B), C42(H42A,H42B), C43(H43A,H43B),
 C50(H50A,H50B), C68(H68A,H68B), C48(H48A,H48B), C40(H40A,H40B), C47(H47A,H47B),
  C49(H49A,H49B), C46(H46A,H46B), C34X(H34C,H34D), C30X(H30C,H30D), C31X(H31C,
 H31D), C29X(H29C,H29D), C39X(H39C,H39D), C38X(H38C,H38D), C28X(H28C,H28D),
 C37X(H37C,H37D), C35X(H35C,H35D), C36X(H36C,H36D), C33X(H33C,H33D), C32X(H32C,
 H32D), C51X(H51C,H51D), C49X(H49C,H49D), C43X(H43C,H43D), C42X(H42C,H42D),
 C40X(H40C,H40D), C41X(H41C,H41D), C48X(H48C,H48D), C46X(H46C,H46D), C50X(H50C,
 H50D), C45X(H45C,H45D), C47X(H47C,H47D), C44X(H44C,H44D), C68X(H68C,H68D),
 C69X(H69C,H69D), C70X(H70C,H70D), C71X(H71C,H71D), C57X(H57C,H57D), C58X(H58C,
 H58D), C61X(H61C,H61D), C62X(H62C,H62D), C54X(H54C,H54D), C53X(H53C,H53D),
 C56X(H56C,H56D), C63X(H63C,H63D), C59X(H59C,H59D), C55X(H55C,H55D), C60X(H60C,
 H60D), C52X(H52C,H52D), C64X(H64C,H64D), C67X(H67C,H67D), C65X(H65C,H65D),
 C66X(H66C,H66D)
7.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C24(H24), C14(H14), C15(H15), C16(H16), C13(H13), C22(H22),
 C7(H7), C23(H23), C4(H4), C25(H25), C20(H20), C2(H2), C6(H6), C20X(H20X),
 C14X(H14X), C6X(H6X), C23X(H23X), C22X(H22X), C25X(H25X), C24X(H24X), C4X(H4X),
  C16X(H16X), C5X(H5X), C13X(H13X), C7X(H7X), C2X(H2X), C11X(H11X), C15X(H15X)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15793
_shelx_hkl_checksum              62258
_shelx_fab_checksum              13843
_olex2_submission_special_instructions 'No special instructions were received'