In situ insertion of copper to form heteroanionic D3h-symmetric [Cu3Mo8O32]10− for a templated Ag55 nanocluster
Gao, Jin-Ping; Qi, Zhikai; Zhang, Fu-Qiang; Zhang, Xian-Ming; Nanoscale  (2022) –; doi:10.1039/D2NR00078D

data_1566580
_publ_section_title
;
 &#x000D; In situ insertion of copper to form heteroanionic D3h-symmetric
 [Cu3Mo8O32]10&#x2212; for a templated Ag55 nanocluster
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D2NR00078D
_journal_year                    2022
_chemical_formula_moiety         'C261 H468 Ag55 Cu3 F3 Mo8 O36 S43, 2(O)'
_chemical_formula_sum            'C261 H476 Ag55 Cu3 F3 Mo8 O38 S43'
_chemical_formula_weight         12548.96
_chemical_name_systematic        1
_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     iterative
_audit_creation_date             2021-12-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2021-12-27 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                73.3300(10)
_cell_angle_beta                 75.2360(10)
_cell_angle_gamma                73.6330(10)
_cell_formula_units_Z            2
_cell_length_a                   23.3674(3)
_cell_length_b                   23.7497(4)
_cell_length_c                   38.3998(5)
_cell_measurement_reflns_used    56765
_cell_measurement_temperature    150
_cell_measurement_theta_max      78.7400
_cell_measurement_theta_min      3.6480
_cell_volume                     19233.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.949
_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     -3.00  83.00   0.50    7.00    --   52.30 -77.00   0.00  172
  2  \w    -36.00  19.00   0.50    7.00    --   52.30 -57.00 -90.00  110
  3  \w    111.00 142.00   0.50    7.00    --   52.30  82.00 -30.00   62
  4  \w    105.00 142.00   0.50    7.00    --   52.30  77.00 -60.00   74
  5  \w    -37.00  65.00   0.50    7.00    --   52.30 -37.00  60.00  204
  6  \w     44.00  75.00   0.50    7.00    --   52.30 -57.00 -90.00   62
  7  \w    107.00 138.00   0.50    7.00    --   52.30  82.00   0.00   62
  8  \w     16.00  76.00   0.50    7.00    --   52.30 -82.00 -90.00  120
  9  \w    139.00 197.00   0.50   32.00    --  109.10  82.00   0.00  116
 10  \w    112.00 138.00   0.50   32.00    --  109.10  82.00   0.00   52
 11  \w     28.00 139.00   0.50   32.00    --  109.10 -77.00 -30.00  222
 12  \w     21.00 105.00   0.50   32.00    --  109.10 -57.00 -30.00  168
 13  \w     81.00 108.00   0.50   32.00    --  109.10 -82.00 -90.00   54
 14  \w     64.00  90.00   0.50   32.00    --  109.10 -82.00-180.00   52
 15  \w     49.00 120.00   0.50   32.00    --  109.10 -57.00  90.00  142
 16  \w    106.00 195.00   0.50   32.00    --  109.10  37.00-180.00  178
 17  \w     95.00 121.00   0.50   32.00    --  109.10 -82.00   0.00   52
 18  \w     96.00 141.00   0.50   32.00    --  109.10 -82.00-180.00   90
 19  \w    122.00 198.00   0.50   32.00    --  109.10  19.00  90.00  152
 20  \w     20.00 125.00   0.50   32.00    --  109.10 -82.00-150.00  210
 21  \w     93.00 198.00   0.50   32.00    --  109.10  82.00  30.00  210
 22  \w     37.00 117.00   0.50   32.00    --  109.10 -82.00  90.00  160
 23  \w     82.00 197.00   0.50   32.00    --  109.10  19.00 150.00  230
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0040838000
_diffrn_orient_matrix_UB_12      0.0205839000
_diffrn_orient_matrix_UB_13      -0.0422566000
_diffrn_orient_matrix_UB_21      0.0677392000
_diffrn_orient_matrix_UB_22      -0.0320661000
_diffrn_orient_matrix_UB_23      -0.0057822000
_diffrn_orient_matrix_UB_31      -0.0170761000
_diffrn_orient_matrix_UB_32      -0.0581218000
_diffrn_orient_matrix_UB_33      0.0000457000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            214510
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.582
_diffrn_reflns_theta_min         3.671
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             12138
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.39304
_refine_diff_density_max         3.268
_refine_diff_density_min         -3.979
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2588
_refine_ls_number_reflns         80132
_refine_ls_number_restraints     497
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.148
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1334P)^2^+454.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2827
_refine_ls_wR_factor_ref         0.3083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                52747
_reflns_number_total             80132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr00078d2.cif
_cod_data_source_block           cu-1_auto
_cod_database_code               1566580
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C O S Ag Mo Cu'
_shelx_estimated_absorpt_t_max   0.257
_shelx_estimated_absorpt_t_min   0.108
_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
 C25-C26
 1.54 with sigma of 0.02
 C26-C27
 1.54 with sigma of 0.02
 C27-C28
 1.54 with sigma of 0.02
 C28-C29
 1.54 with sigma of 0.02
 C29-C30
 1.54 with sigma of 0.02
 C30-C25
 1.54 with sigma of 0.02
 C25-C27
 2.52 with sigma of 0.02
 C26-C28
 2.52 with sigma of 0.02
 C27-C29
 2.52 with sigma of 0.02
 C28-C30
 2.52 with sigma of 0.02
 C29-C25
 2.52 with sigma of 0.02
 C30-C26
 2.52 with sigma of 0.02
 C13-C14
 1.54 with sigma of 0.02
 C56-C17
 2.52 with sigma of 0.02
 C13-C56
 2.52 with sigma of 0.02
 C14-C56
 1.54 with sigma of 0.02
 C17-C13
 2.52 with sigma of 0.02
 C56-C16
 1.54 with sigma of 0.02
 C14-C16
 2.52 with sigma of 0.02
 C16-C17
 1.54 with sigma of 0.02
 C16-C18
 2.52 with sigma of 0.02
 C17-C18
 1.54 with sigma of 0.02
 C18-C14
 2.52 with sigma of 0.02
 C18-C13
 1.54 with sigma of 0.02
 C97-C102
 1.54 with sigma of 0.02
 C102-C101
 1.54 with sigma of 0.02
 C101-C100
 1.54 with sigma of 0.02
 C100-C99
 1.54 with sigma of 0.02
 C99-C98
 1.54 with sigma of 0.02
 C98-C97
 1.54 with sigma of 0.02
 C97-C101
 2.52 with sigma of 0.02
 C102-C100
 2.52 with sigma of 0.02
 C101-C99
 2.52 with sigma of 0.02
 C100-C98
 2.52 with sigma of 0.02
 C99-C97
 2.52 with sigma of 0.02
 C98-C102
 2.52 with sigma of 0.02
 C103-C108
 1.54 with sigma of 0.02
 C108-C107
 1.54 with sigma of 0.02
 C104-C103
 1.54 with sigma of 0.02
 C103-C107
 2.52 with sigma of 0.02
 C104-C108
 2.52 with sigma of 0.02
 C67-C68
 1.54 with sigma of 0.02
 C68-C69
 1.54 with sigma of 0.02
 C69-C70
 1.54 with sigma of 0.02
 C70-C71
 1.54 with sigma of 0.02
 C71-C72
 1.54 with sigma of 0.02
 C72-C67
 1.54 with sigma of 0.02
 C67-C69
 2.52 with sigma of 0.02
 C68-C70
 2.52 with sigma of 0.02
 C69-C71
 2.52 with sigma of 0.02
 C70-C72
 2.52 with sigma of 0.02
 C71-C67
 2.52 with sigma of 0.02
 C72-C68
 2.52 with sigma of 0.02
 C235-C236
 1.54 with sigma of 0.02
 C236-C237
 1.54 with sigma of 0.02
 C237-C238
 1.54 with sigma of 0.02
 C238-C239
 1.54 with sigma of 0.02
 C239-C240
 1.54 with sigma of 0.02
 C240-C235
 1.54 with sigma of 0.02
 C235-C237
 2.52 with sigma of 0.02
 C236-C238
 2.52 with sigma of 0.02
 C237-C239
 2.52 with sigma of 0.02
 C238-C240
 2.52 with sigma of 0.02
 C239-C235
 2.52 with sigma of 0.02
 C240-C236
 2.52 with sigma of 0.02
 C115-C120
 1.54 with sigma of 0.02
 C120-C119
 1.54 with sigma of 0.02
 C119-C118
 1.54 with sigma of 0.02
 C118-C117
 1.54 with sigma of 0.02
 C117-C116
 1.54 with sigma of 0.02
 C116-C115
 1.54 with sigma of 0.02
 C115-C119
 2.52 with sigma of 0.02
 C120-C118
 2.52 with sigma of 0.02
 C119-C117
 2.52 with sigma of 0.02
 C118-C116
 2.52 with sigma of 0.02
 C117-C115
 2.52 with sigma of 0.02
 C116-C120
 2.52 with sigma of 0.02
 C55-C60
 1.54 with sigma of 0.02
 C60-C59
 1.54 with sigma of 0.02
 C59-C58
 1.54 with sigma of 0.02
 C58-C57
 1.54 with sigma of 0.02
 C57-C15
 1.54 with sigma of 0.02
 C15-C55
 1.54 with sigma of 0.02
 C55-C59
 2.52 with sigma of 0.02
 C60-C58
 2.52 with sigma of 0.02
 C59-C57
 2.52 with sigma of 0.02
 C58-C15
 2.52 with sigma of 0.02
 C57-C55
 2.52 with sigma of 0.02
 C15-C60
 2.52 with sigma of 0.02
 C157-C162
 1.54 with sigma of 0.02
 C162-C161
 1.54 with sigma of 0.02
 C161-C160
 1.54 with sigma of 0.02
 C160-C159
 1.54 with sigma of 0.02
 C159-C158
 1.54 with sigma of 0.02
 C158-C157
 1.54 with sigma of 0.02
 C157-C161
 2.52 with sigma of 0.02
 C162-C160
 2.52 with sigma of 0.02
 C161-C159
 2.52 with sigma of 0.02
 C160-C158
 2.52 with sigma of 0.02
 C159-C157
 2.52 with sigma of 0.02
 C158-C162
 2.52 with sigma of 0.02
 C121-C122
 1.54 with sigma of 0.02
 C126-C121
 1.54 with sigma of 0.02
 C126-C122
 2.52 with sigma of 0.02
 C205-C206
 1.54 with sigma of 0.02
 C206-C207
 1.54 with sigma of 0.02
 C207-C208
 1.54 with sigma of 0.02
 C208-C209
 1.54 with sigma of 0.02
 C209-C210
 1.54 with sigma of 0.02
 C210-C205
 1.54 with sigma of 0.02
 C205-C207
 2.52 with sigma of 0.02
 C206-C208
 2.52 with sigma of 0.02
 C207-C209
 2.52 with sigma of 0.02
 C208-C210
 2.52 with sigma of 0.02
 C209-C205
 2.52 with sigma of 0.02
 C210-C206
 2.52 with sigma of 0.02
 C43-C48
 1.54 with sigma of 0.02
 C48-C47
 1.54 with sigma of 0.02
 C47-C46
 1.54 with sigma of 0.02
 C46-C45
 1.54 with sigma of 0.02
 C45-C44
 1.54 with sigma of 0.02
 C44-C43
 1.54 with sigma of 0.02
 C43-C47
 2.52 with sigma of 0.02
 C48-C46
 2.52 with sigma of 0.02
 C47-C45
 2.52 with sigma of 0.02
 C46-C44
 2.52 with sigma of 0.02
 C45-C43
 2.52 with sigma of 0.02
 C44-C48
 2.52 with sigma of 0.02
 C193-C198
 1.54 with sigma of 0.02
 C198-C197
 1.54 with sigma of 0.02
 C197-C196
 1.54 with sigma of 0.02
 C196-C195
 1.54 with sigma of 0.02
 C195-C194
 1.54 with sigma of 0.02
 C194-C193
 1.54 with sigma of 0.02
 C193-C197
 2.52 with sigma of 0.02
 C198-C196
 2.52 with sigma of 0.02
 C197-C195
 2.52 with sigma of 0.02
 C196-C194
 2.52 with sigma of 0.02
 C195-C193
 2.52 with sigma of 0.02
 C194-C198
 2.52 with sigma of 0.02
 C53-C52
 1.54 with sigma of 0.02
 C52-C51
 1.54 with sigma of 0.02
 C51-C50
 1.54 with sigma of 0.02
 C50-C49
 1.54 with sigma of 0.02
 C49-C53
 2.52 with sigma of 0.02
 C53-C51
 2.52 with sigma of 0.02
 C52-C50
 2.52 with sigma of 0.02
 C51-C49
 2.52 with sigma of 0.02
 C91-C96
 1.54 with sigma of 0.02
 C96-C95
 1.54 with sigma of 0.02
 C95-C94
 1.54 with sigma of 0.02
 C94-C93
 1.54 with sigma of 0.02
 C93-C92
 1.54 with sigma of 0.02
 C92-C91
 1.54 with sigma of 0.02
 C91-C95
 2.52 with sigma of 0.02
 C96-C94
 2.52 with sigma of 0.02
 C95-C93
 2.52 with sigma of 0.02
 C94-C92
 2.52 with sigma of 0.02
 C93-C91
 2.52 with sigma of 0.02
 C92-C96
 2.52 with sigma of 0.02
 C6-C2
 2.52 with sigma of 0.02
 C4-C6
 2.52 with sigma of 0.02
 C1-C2
 1.54 with sigma of 0.02
 C4-C5
 1.54 with sigma of 0.02
 C3-C5
 2.52 with sigma of 0.02
 C5-C6
 1.54 with sigma of 0.02
 C5-C1
 2.52 with sigma of 0.02
 C6-C1
 1.54 with sigma of 0.02
 C1-C3
 2.52 with sigma of 0.02
 C2-C3
 1.54 with sigma of 0.02
 C3-C4
 1.54 with sigma of 0.02
 C163-C168
 1.54 with sigma of 0.02
 C168-C167
 1.54 with sigma of 0.02
 C167-C166
 1.54 with sigma of 0.02
 C166-C165
 1.54 with sigma of 0.02
 C165-C164
 1.54 with sigma of 0.02
 C164-C163
 1.54 with sigma of 0.02
 C163-C167
 2.52 with sigma of 0.02
 C168-C166
 2.52 with sigma of 0.02
 C167-C165
 2.52 with sigma of 0.02
 C166-C164
 2.52 with sigma of 0.02
 C165-C163
 2.52 with sigma of 0.02
 C164-C168
 2.52 with sigma of 0.02
 C133-C138
 1.54 with sigma of 0.02
 C138-C137
 1.54 with sigma of 0.02
 C137-C136
 1.54 with sigma of 0.02
 C136-C135
 1.54 with sigma of 0.02
 C135-C134
 1.54 with sigma of 0.02
 C134-C133
 1.54 with sigma of 0.02
 C133-C137
 2.52 with sigma of 0.02
 C138-C136
 2.52 with sigma of 0.02
 C137-C135
 2.52 with sigma of 0.02
 C136-C134
 2.52 with sigma of 0.02
 C135-C133
 2.52 with sigma of 0.02
 C134-C138
 2.52 with sigma of 0.02
 C223-C228
 1.54 with sigma of 0.02
 C228-C227
 1.54 with sigma of 0.02
 C227-C226
 1.54 with sigma of 0.02
 C226-C225
 1.54 with sigma of 0.02
 C225-C224
 1.54 with sigma of 0.02
 C224-C223
 1.54 with sigma of 0.02
 C223-C227
 2.52 with sigma of 0.02
 C228-C226
 2.52 with sigma of 0.02
 C227-C225
 2.52 with sigma of 0.02
 C226-C224
 2.52 with sigma of 0.02
 C225-C223
 2.52 with sigma of 0.02
 C224-C228
 2.52 with sigma of 0.02
 C257-C256
 1.54 with sigma of 0.02
 C256-C258
 2.52 with sigma of 0.02
 C257-C258
 1.54 with sigma of 0.02
 C254-C255
 1.54 with sigma of 0.02
 C258-C254
 2.52 with sigma of 0.02
 C257-C253
 2.52 with sigma of 0.02
 C253-C255
 2.52 with sigma of 0.02
 C258-C253
 1.54 with sigma of 0.02
 C254-C256
 2.52 with sigma of 0.02
 C255-C256
 1.54 with sigma of 0.02
 C255-C257
 2.52 with sigma of 0.02
 C253-C254
 1.54 with sigma of 0.02
 C250-C251
 1.54 with sigma of 0.02
 C250-C252
 2.52 with sigma of 0.02
 C251-C252
 1.54 with sigma of 0.02
 C248-C249
 1.54 with sigma of 0.02
 C252-C248
 2.52 with sigma of 0.02
 C251-C247
 2.52 with sigma of 0.02
 C247-C249
 2.52 with sigma of 0.02
 C252-C247
 1.54 with sigma of 0.02
 C248-C250
 2.52 with sigma of 0.02
 C249-C250
 1.54 with sigma of 0.02
 C249-C251
 2.52 with sigma of 0.02
 C247-C248
 1.54 with sigma of 0.02
 C123-C122
 1.54 with sigma of 0.02
 C125-C124
 1.54 with sigma of 0.02
 C123-C121
 2.52 with sigma of 0.02
 C122-C121
 1.54 with sigma of 0.02
 C124-C122
 2.52 with sigma of 0.02
 C121-C125
 2.52 with sigma of 0.02
 C122-C126
 2.52 with sigma of 0.02
 C126-C125
 1.54 with sigma of 0.02
 C124-C123
 1.54 with sigma of 0.02
 C125-C123
 2.52 with sigma of 0.02
 C126-C124
 2.52 with sigma of 0.02
 C121-C126
 1.54 with sigma of 0.02
 C81-C82
 1.54 with sigma of 0.02
 C218-C219
 1.54 with sigma of 0.02
 C81-C83
 2.52 with sigma of 0.02
 C79-C81
 2.52 with sigma of 0.02
 C83-C79
 2.52 with sigma of 0.02
 C219-C220
 1.54 with sigma of 0.02
 C83-C84
 1.54 with sigma of 0.02
 C79-C80
 1.54 with sigma of 0.02
 C80-C81
 1.54 with sigma of 0.02
 C217-C218
 1.54 with sigma of 0.02
 C82-C83
 1.54 with sigma of 0.02
 C222-C217
 1.54 with sigma of 0.02
 C84-C79
 1.54 with sigma of 0.02
 C217-C219
 2.52 with sigma of 0.02
 C80-C82
 2.52 with sigma of 0.02
 C218-C220
 2.52 with sigma of 0.02
 C82-C84
 2.52 with sigma of 0.02
 C219-C221
 2.52 with sigma of 0.02
 C84-C80
 2.52 with sigma of 0.02
 C220-C222
 2.52 with sigma of 0.02
 C220-C221
 1.54 with sigma of 0.02
 C221-C217
 2.52 with sigma of 0.02
 C221-C222
 1.54 with sigma of 0.02
 C222-C218
 2.52 with sigma of 0.02
 C141-C140
 1.54 with sigma of 0.02
 C139-C144
 1.54 with sigma of 0.02
 C141-C139
 2.52 with sigma of 0.02
 C140-C139
 1.54 with sigma of 0.02
 C143-C142
 1.54 with sigma of 0.02
 C139-C143
 2.52 with sigma of 0.02
 C140-C144
 2.52 with sigma of 0.02
 C144-C142
 2.52 with sigma of 0.02
 C144-C143
 1.54 with sigma of 0.02
 C143-C141
 2.52 with sigma of 0.02
 C142-C141
 1.54 with sigma of 0.02
 C142-C140
 2.52 with sigma of 0.02
 C73-C77
 2.52 with sigma of 0.02
 C77-C75
 2.52 with sigma of 0.02
 C76-C75
 1.54 with sigma of 0.02
 C76-C74
 2.52 with sigma of 0.02
 C75-C73
 2.52 with sigma of 0.02
 C77-C76
 1.54 with sigma of 0.02
 C75-C74
 1.54 with sigma of 0.02
 C74-C73
 1.54 with sigma of 0.02
 C105-C107
 2.52 with sigma of 0.02
 C103-C104
 1.54 with sigma of 0.02
 C49-C50
 1.54 with sigma of 0.02
 C105-C106
 1.54 with sigma of 0.02
 C50-C51
 1.54 with sigma of 0.02
 C103-C105
 2.52 with sigma of 0.02
 C53-C54
 1.54 with sigma of 0.02
 C107-C103
 2.52 with sigma of 0.02
 C54-C49
 1.54 with sigma of 0.02
 C107-C108
 1.54 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C78-C73
 1.54 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 C104-C105
 1.54 with sigma of 0.02
 C51-C53
 2.52 with sigma of 0.02
 C106-C107
 1.54 with sigma of 0.02
 C52-C54
 2.52 with sigma of 0.02
 C108-C103
 1.54 with sigma of 0.02
 C53-C49
 2.52 with sigma of 0.02
 C104-C106
 2.52 with sigma of 0.02
 C54-C50
 2.52 with sigma of 0.02
 C106-C108
 2.52 with sigma of 0.02
 C73-C74
 1.54 with sigma of 0.02
 C108-C104
 2.52 with sigma of 0.02
 C74-C75
 1.54 with sigma of 0.02
 C49-C51
 2.52 with sigma of 0.02
 C75-C76
 1.54 with sigma of 0.02
 C50-C52
 2.52 with sigma of 0.02
 C76-C77
 1.54 with sigma of 0.02
 C77-C78
 1.54 with sigma of 0.02
 H61-H68A
 2.3 with sigma of 0.04
 H74A-H84B
 2.3 with sigma of 0.04
 H74B-H84B
 2.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C153 \\sim C70 \\sim C163 \\sim C213 \\sim C239 \\sim C254 \\sim C249 \\sim
C238 \\sim C107 \\sim C73 \\sim C252 \\sim C61 \\sim C19 \\sim C140 \\sim C127
\\sim C192 \\sim C157 \\sim C259 \\sim C132 \\sim C175 \\sim C86 \\sim C39
\\sim C88 \\sim C1 \\sim C204 \\sim C38 \\sim C145 \\sim C205 \\sim C9 \\sim
C40 \\sim C251 \\sim C87 \\sim C228 \\sim C200 \\sim C128 \\sim C198 \\sim C62
\\sim C190 \\sim C217 \\sim C179 \\sim C137 \\sim C180 \\sim C13 \\sim C36
\\sim C64 \\sim C241 \\sim C150 \\sim C191 \\sim C25 \\sim C74 \\sim C203 \\sim
C176 \\sim C181 \\sim C14 \\sim C147 \\sim C76 \\sim C170 \\sim C136 \\sim C177
\\sim C97 \\sim C121 \\sim C102 \\sim C201 \\sim C158 \\sim C63 \\sim C33 \\sim
C35 \\sim C66 \\sim C246 \\sim C32 \\sim C111 \\sim C257 \\sim C69 \\sim C6
\\sim C186 \\sim C55 \\sim C216 \\sim C183 \\sim C178 \\sim C151 \\sim C149
\\sim C148 \\sim C41 \\sim C126 \\sim C197 \\sim C2 \\sim C211 \\sim C68 \\sim
C65 \\sim C235 \\sim C242 \\sim C3 \\sim C174 \\sim C115 \\sim C236 \\sim C72
\\sim C11 \\sim C71 \\sim C234 \\sim C244 \\sim C10 \\sim C112 \\sim C108 \\sim
C240 \\sim C195 \\sim C85 \\sim C199 \\sim C187 \\sim C37 \\sim C90 \\sim C189
\\sim C67 \\sim C134 \\sim C24 \\sim C188 \\sim C89 \\sim C21 \\sim C98 \\sim
C222 \\sim C146 \\sim C23 \\sim C42 \\sim C31 \\sim C110 \\sim C20 \\sim C109
\\sim C171 \\sim C99 \\sim C75 \\sim C182 \\sim C202 \\sim C169 \\sim C220
\\sim C120 \\sim C229 \\sim C218 \\sim C30 \\sim C129 \\sim C162 \\sim C12
\\sim C161 \\sim C22 \\sim C173 \\sim C219 \\sim C215 \\sim C214 \\sim C34
\\sim C100 \\sim C28 \\sim C77 \\sim C113 \\sim C8 \\sim C243 \\sim C130 \\sim
C7 \\sim C227 \\sim C18 \\sim C253 \\sim C172 \\sim C103 \\sim C29 \\sim C156
\\sim C131 \\sim C118 \\sim C114 \\sim C17 \\sim C27 \\sim C152 \\sim C5 \\sim
C212 \\sim C245 \\sim C230 \\sim C237 \\sim C16 \\sim C58 \\sim C221 \\sim C154
\\sim C104 \\sim C26 \\sim C248 \\sim C258 \\sim C231 \\sim C155 \\sim C101
\\sim C56 \\sim C117: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
C51 \\sim C53 \\sim C49 \\sim C52 \\sim C50: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C163 \\sim C165 \\sim C168 \\sim C166 \\sim C167 \\sim C164: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C254 \\sim C257 \\sim C255 \\sim C253 \\sim C258 \\sim C256: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(Ag0A)=Sof(Ag1D)=Sof(Ag4A)=Sof(Ag1E)=1-FVAR(1)
 Sof(Ag17)=Sof(Ag42)=Sof(Ag30)=Sof(Ag54)=FVAR(1)
 Sof(Ag1C)=1-FVAR(2)
 Sof(Ag24)=FVAR(2)
 Sof(Ag1F)=1-FVAR(3)
 Sof(Ag38)=FVAR(3)
 Sof(Ag1G)=1-FVAR(4)
 Sof(Ag20)=FVAR(4)
 Sof(Ag1H)=1-FVAR(5)
 Sof(Ag33)=FVAR(5)
 Sof(Ag1I)=1-FVAR(6)
 Sof(Ag22)=FVAR(6)
 Sof(Ag1A)=1-FVAR(7)
 Sof(Ag23)=FVAR(7)
 Sof(Ag26)=1-FVAR(8)
 Sof(Ag40)=FVAR(8)
 Sof(Ag8B)=1-FVAR(9)
 Sof(Ag32)=FVAR(9)
 Sof(Ag1J)=1-FVAR(10)
 Sof(Ag37)=FVAR(10)
 Sof(Ag1K)=1-FVAR(11)
 Sof(Ag57)=FVAR(11)
 Sof(Ag1L)=1-FVAR(12)
 Sof(Ag29)=FVAR(12)
 Sof(Ag)=1-FVAR(13)
 Sof(Ag53)=FVAR(13)
 Sof(Ag1M)=1-FVAR(14)
 Sof(Ag41)=FVAR(14)
 Sof(Ag7B)=1-FVAR(15)
 Sof(Ag45)=FVAR(15)
 Sof(Ag2C)=1-FVAR(16)
 Sof(Ag31)=FVAR(16)
 Sof(Ag1N)=1-FVAR(17)
 Sof(Ag48)=FVAR(17)
5.a Ternary CH refined with riding coordinates:
 C163(H163), C247(H247), C73(H73), C61(H61), C19(H19), C127(H127), C157(H157),
 C175(H175), C1(H1), C145(H145), C205(H205), C217(H217), C13(H13), C241(H241),
 C25(H25), C181(H181), C97(H97), C121(H121), C55(H55), C151(H151), C211(H211),
 C235(H235), C115(H115), C79(H79), C85(H85), C199(H199), C187(H187), C37(H37),
 C67(H67), C43(H43), C31(H31), C91(H91), C109(H109), C169(H169), C229(H229),
 C133(H133), C49(H49), C223(H223), C7(H7), C253(H253), C103(H103), C193(H193),
 C139(H139)
5.b Secondary CH2 refined with riding coordinates:
 C153(H15A,H15B), C70(H70A,H70B), C45(H45A,H45B), C213(H21A,H21B), C239(H23A,
 H23B), C165(H16A,H16B), C254(H25A,H25B), C48(H48A,H48B), C249(H24A,H24B),
 C144(H14A,H14B), C168(H16C,H16D), C238(H23C,H23D), C135(H13A,H13B), C107(H10A,
 H10B), C252(H25C,H25D), C106(H10C,H10D), C140(H14C,H14D), C192(H19A,H19B),
 C132(H13C,H13D), C86(H86A,H86B), C39(H39A,H39B), C88(H88A,H88B), C204(H20A,
 H20B), C38(H38A,H38B), C166(H16E,H16F), C9(H9A,H9B), C40(H40A,H40B), C251(H25E,
 H25F), C87(H87A,H87B), C228(H22A,H22B), C200(H20C,H20D), C128(H12A,H12B),
 C198(H19C,H19D), C62(H62A,H62B), C190(H19E,H19F), C179(H17A,H17B), C137(H13E,
 H13F), C180(H18A,H18B), C36(H36A,H36B), C64(H64A,H64B), C150(H15C,H15D),
 C191(H19G,H19H), C74(H74A,H74B), C203(H20E,H20F), C176(H17C,H17D), C14(H14E,
 H14F), C124(H12C,H12D), C147(H14G,H14H), C76(H76A,H76B), C170(H17E,H17F),
 C136(H13G,H13H), C177(H17G,H17H), C102(H10E,H10F), C201(H20G,H20H), C158(H15E,
 H15F), C63(H63A,H63B), C33(H33A,H33B), C35(H35A,H35B), C66(H66A,H66B),
 C246(H24C,H24D), C32(H32A,H32B), C111(H11A,H11B), C257(H25G,H25H), C69(H69A,
 H69B), C209(H20I,H20J), C6(H6A,H6B), C186(H18C,H18D), C216(H21C,H21D),
 C183(H18E,H18F), C178(H17I,H17J), C149(H14I,H14J), C148(H14K,H14L), C41(H41A,
 H41B), C126(H12E,H12F), C197(H19I,H19J), C2(H2A,H2B), C68(H68A,H68B), C65(H65A,
 H65B), C242(H24E,H24F), C3(H3A,H3B), C174(H17K,H17L), C236(H23E,H23F),
 C72(H72A,H72B), C11(H11C,H11D), C71(H71A,H71B), C244(H24G,H24H), C10(H10G,
 H10H), C83(H83A,H83B), C112(H11E,H11F), C255(H25I,H25J), C84(H84A,H84B),
 C108(H10I,H10J), C240(H24I,H24J), C195(H19K,H19L), C141(H14M,H14N), C44(H44A,
 H44B), C143(H14O,H14P), C92(H92A,H92B), C210(H21E,H21F), C93(H93A,H93B),
 C4(H4A,H4B), C206(H20K,H20L), C46(H46A,H46B), C47(H47A,H47B), C194(H19M,H19N),
 C90(H90A,H90B), C189(H18G,H18H), C134(H13I,H13J), C24(H24K,H24L), C188(H18I,
 H18J), C89(H89A,H89B), C119(H11G,H11H), C21(H21G,H21H), C98(H98A,H98B),
 C222(H22C,H22D), C167(H16G,H16H), C146(H14Q,H14R), C94(H94A,H94B), C23(H23I,
 H23J), C196(H19O,H19P), C42(H42A,H42B), C110(H11I,H11J), C20(H20M,H20N),
 C171(H17M,H17N), C99(H99A,H99B), C75(H75A,H75B), C182(H18K,H18L), C51(H51A,
 H51B), C202(H20O,H20P), C220(H22E,H22F), C120(H12G,H12H), C218(H21I,H21J),
 C30(H30A,H30B), C129(H12I,H12J), C53(H53A,H53B), C162(H16I,H16J), C12(H12K,
 H12L), C95(H95A,H95B), C116(H11K,H11L), C164(H16K,H16L), C138(H13K,H13L),
 C161(H16M,H16N), C22(H22G,H22H), C173(H17O,H17P), C219(H21K,H21L), C208(H20Q,
 H20R), C215(H21M,H21N), C214(H21O,H21P), C34(H34A,H34B), C100(H10K,H10L),
 C28(H28A,H28B), C77(H77A,H77B), C113(H11M,H11N), C8(H8A,H8B), C243(H24M,H24N),
 C130(H13M,H13N), C96(H96A,H96B), C184(H18M,H18N), C227(H22I,H22J), C18(H18O,
 H18P), C172(H17Q,H17R), C29(H29A,H29B), C156(H15G,H15H), C131(H13O,H13P),
 C52(H52A,H52B), C118(H11O,H11P), C114(H11Q,H11R), C17(H17S,H17T), C27(H27A,
 H27B), C152(H15I,H15J), C5(H5A,H5B), C212(H21Q,H21R), C245(H24O,H24P),
 C230(H23K,H23L), C82(H82A,H82B), C237(H23M,H23N), C16(H16O,H16P), C58(H58A,
 H58B), C221(H22K,H22L), C154(H15K,H15L), C123(H12M,H12N), C104(H10M,H10N),
 C26(H26D,H26E), C248(H24Q,H24R), C258(H25K,H25L), C207(H20S,H20T), C224(H22M,
 H22N), C15(H15M,H15N), C155(H15O,H15P), C81(H81A,H81B), C142(H14S,H14T),
 C80(H80A,H80B), C60(H60A,H60B), C122(H12O,H12P), C101(H10O,H10P), C57(H57A,
 H57B), C226(H22O,H22P), C185(H18Q,H18R), C56(H56A,H56B), C117(H11S,H11T),
 C225(H22Q,H22R), C160(H16Q,H16R), C256(H25M,H25N), C59(H59A,H59B), C250(H25O,
 H25P), C159(H15Q,H15R), C50(H50A,H50B), C125(H12Q,H12R), C78(H78A,H78B),
 C54(H54A,H54B), C105(H10Q,H10R)
5.c Idealised Me refined as rotating group:
 C261(H26A,H26B,H26C)
;
_shelx_res_checksum              87666
_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 2.639
_oxdiff_exptl_absorpt_empirical_full_min 0.345