Chalcogens-Induced Ag<sub>6</sub>Z<sub>4</sub>@Ag<sub>36</sub> (Z = S or Se) Core-Shell Nanoclusters: Enlarged Tetrahedral Core and Homochiral Crystallization.
Wang, Zhi; Liu, Jia-Wei; Su, Hai-Feng; Zhao, Quan-Qin; Kurmoo, Mohamedally; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Zheng, Lan-Sun; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09460

data_4127295
_publ_section_title
;
 Chalcogens-Induced Ag<sub>6</sub>Z<sub>4</sub>@Ag<sub>36</sub> (Z = S or
 Se) Core-Shell Nanoclusters: Enlarged Tetrahedral Core and Homochiral
 Crystallization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09460
_journal_year                    2019
_chemical_formula_moiety         'C252 H312 Ag42 F18 O24 S24 Se4'
_chemical_formula_sum            'C252 H312 Ag42 F18 O24 S24 Se4'
_chemical_formula_weight         9682.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9548(6)
_cell_length_b                   33.9141(5)
_cell_length_c                   35.3758(6)
_cell_measurement_reflns_used    20968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.2130
_cell_measurement_theta_min      3.7640
_cell_volume                     37137.7(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.845
_diffrn_measured_fraction_theta_max 0.992
_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    -11.00  74.00   1.00    1.00    --    1.09  37.00 -60.00   85
  2  \w     77.00 147.00   1.00   40.00    --   87.84  37.00 -90.00   70
  3  \w     33.00  99.00   1.00   40.00    --   87.84 -37.00-150.00   66
  4  \w     16.00 104.00   1.00   40.00    --   87.84-105.00  87.00   88
  5  \w    -38.00 -13.00   1.00   40.00    --  -85.65  91.00 -68.00   25
  6  \w    -91.00 -65.00   1.00   40.00    --  -85.65  38.00  95.00   26
  7  \w   -113.00 -61.00   1.00   40.00    --  -85.65  91.00 -68.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0267045000
_diffrn_orient_matrix_UB_12      0.0209516000
_diffrn_orient_matrix_UB_13      0.0307590000
_diffrn_orient_matrix_UB_21      -0.0367260000
_diffrn_orient_matrix_UB_22      0.0068016000
_diffrn_orient_matrix_UB_23      -0.0287359000
_diffrn_orient_matrix_UB_31      -0.0203638000
_diffrn_orient_matrix_UB_32      -0.0396857000
_diffrn_orient_matrix_UB_33      0.0113148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.845
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            99779
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.168
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             18688
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 11991 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.096(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1654
_refine_ls_number_reflns         53592
_refine_ls_number_restraints     1005
_refine_ls_restrained_S_all      27.186
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1639P)^2^+5.4768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2693
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    0.744
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                34206
_reflns_number_total             53592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09460_si_002.cif
_cod_data_source_block           Ag42bCCCC
_cod_database_code               4127295
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         AgCSFO
_diffrn_oxdiff_ac3_digest_frames
;
013f2818e616ac013791e2ae965cec4a0e00412d4c2
;
_diffrn_oxdiff_ac3_digest_hkl
;
010541de054ce0d34ea658ca81399b34feb081
;
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C87-C89
 1.55 with sigma of 0.001
 C157-C159
 1.55 with sigma of 0.001
 C167-C168
 1.55 with sigma of 0.001
 C107-C108
 1.55 with sigma of 0.001
 C57-C59
 1.55 with sigma of 0.001
 C187-C185
 1.55 with sigma of 0.01
 C117-C114
 1.55 with sigma of 0.02
 C117-C119
 1.55 with sigma of 0.001
 C114-C119
 2.35 with sigma of 0.001
 C214-C217
 1.55 with sigma of 0.001
 C147-C144
 2.35 with sigma of 0.001
 C146-C147
 2.35 with sigma of 0.001
 C217-C213
 2.35 with sigma of 0.001
 C215-C217
 2.35 with sigma of 0.001
 C211-S21
 1.82 with sigma of 0.001
 S21-C212
 2.75 with sigma of 0.001
 S21-C216
 2.75 with sigma of 0.001
 C191-S18
 1.82 with sigma of 0.001
 C197-C195
 1.55 with sigma of 0.001
 C197-C194
 1.55 with sigma of 0.001
 C197-C193
 2.35 with sigma of 0.001
 C195-C197
 2.35 with sigma of 0.001
 C187-C184
 2.35 with sigma of 0.001
 C187-C186
 2.35 with sigma of 0.001
 S14-C23
 2.8 with sigma of 0.001
 S14-C22
 2.8 with sigma of 0.001
 C27-C24
 2.35 with sigma of 0.01
 C27-C26
 2.35 with sigma of 0.01
 C27-C29
 1.55 with sigma of 0.001
 C29-C25
 2.35 with sigma of 0.001
 C201-S19
 1.82 with sigma of 0.001
 C206-C207
 1.55 with sigma of 0.001
 C207-C209
 1.55 with sigma of 0.001
 C207-C208
 1.55 with sigma of 0.001
 C209-C206
 2.35 with sigma of 0.001
 C206-C208
 2.35 with sigma of 0.001
 C207-C205
 2.35 with sigma of 0.001
 C207-C204
 2.35 with sigma of 0.001
 C208-C209
 2.35 with sigma of 0.001
 O9-C245
 1.25 with sigma of 0.001
 O10-C245
 1.25 with sigma of 0.001
 C245-C246
 1.55 with sigma of 0.001
 C246-F18
 1.45 with sigma of 0.001
 C246-F16
 1.45 with sigma of 0.001
 C246-F17
 1.45 with sigma of 0.001
 F18-F16
 2.4 with sigma of 0.001
 F16-F17
 2.4 with sigma of 0.001
 F17-F18
 2.4 with sigma of 0.001
 F18-C245
 2.35 with sigma of 0.001
 C245-F16
 2.35 with sigma of 0.001
 C245-F17
 2.35 with sigma of 0.001
 C248-C247
 1.55 with sigma of 0.001
 C247-O3
 1.25 with sigma of 0.001
 C247-O4
 1.25 with sigma of 0.001
 O3-C248
 2.3 with sigma of 0.02
 C248-O4
 2.3 with sigma of 0.02
 C248-F8
 1.45 with sigma of 0.001
 F9-C248
 1.45 with sigma of 0.001
 F8-C248
 1.45 with sigma of 0.001
 F9-F8
 2.4 with sigma of 0.001
 C248-F7
 1.45 with sigma of 0.001
 F8-F7
 2.4 with sigma of 0.001
 F9-F7
 2.4 with sigma of 0.001
 C37-C36
 2.35 with sigma of 0.001
 C34-C37
 2.35 with sigma of 0.001
 C35-C40
 2.35 with sigma of 0.001
 C37-C35
 1.55 with sigma of 0.001
 C37-C40
 1.55 with sigma of 0.001
 C40-C35
 2.35 with sigma of 0.001
 C244-O2
 2.35 with sigma of 0.001
 C244-O1
 2.35 with sigma of 0.001
 C244-F13
 1.45 with sigma of 0.001
 C244-F15
 1.45 with sigma of 0.001
 F13-F15
 2.4 with sigma of 0.001
 C250-F10
 1.45 with sigma of 0.001
 C250-F11
 1.45 with sigma of 0.001
 F11-F10
 2.4 with sigma of 0.001
 C249-O5
 1.25 with sigma of 0.001
 C249-O6
 1.25 with sigma of 0.001
 C249-C250
 1.55 with sigma of 0.001
 C250-F12
 1.45 with sigma of 0.001
 F10-F12
 2.4 with sigma of 0.001
 F11-F12
 2.4 with sigma of 0.001
 C249-F12
 2.4 with sigma of 0.001
 C249-F10
 2.4 with sigma of 0.001
 C249-F11
 2.4 with sigma of 0.001
 C247-F9
 2.4 with sigma of 0.001
 C247-F7
 2.4 with sigma of 0.001
 C247-F8
 2.4 with sigma of 0.001
 C19-C17
 2.35 with sigma of 0.001
 C18-C17
 1.55 with sigma of 0.001
 C17-C19
 2.35 with sigma of 0.001
 C17-C15
 2.35 with sigma of 0.001
 C15-C19
 2.35 with sigma of 0.001
 C234-C233 = C234-C235
 1.55 with sigma of 0.01
 C239-C234
 1.55 with sigma of 0.001
 C231-S20
 1.8 with sigma of 0.001
 C232-S20
 2.7 with sigma of 0.001
 S20-C236
 2.7 with sigma of 0.001
 Ag38-O11W
 2.5 with sigma of 0.001
 Ag24-O10W
 2.5 with sigma of 0.001
 Ag13-O6W
 2.5 with sigma of 0.001
 Ag10-O1W
 2.5 with sigma of 0.001
 Ag19-O3W
 2.5 with sigma of 0.001
 Ag23-O12W
 2.5 with sigma of 0.001
 Ag27-O8W
 2.5 with sigma of 0.001
 Ag16-O9W
 2.5 with sigma of 0.001
 Ag31-O7W
 2.5 with sigma of 0.001
 Ag20-O2W
 2.5 with sigma of 0.001
 Ag35-O5W
 2.5 with sigma of 0.001
 O4W-Ag39
 2.5 with sigma of 0.001
 C242-O7
 2.2 with sigma of 0.001
 C242-O8
 2.2 with sigma of 0.001
 F1-C242
 1.45 with sigma of 0.02
 C242-F2
 1.45 with sigma of 0.02
 F1-F2
 2.4 with sigma of 0.001
 C242-C241
 1.55 with sigma of 0.001
 C241-O7
 1.25 with sigma of 0.001
 C241-O8
 1.25 with sigma of 0.001
 C242-F3
 1.45 with sigma of 0.02
 F1-F3
 2.4 with sigma of 0.001
 F3-F2
 2.4 with sigma of 0.001
 F3-C241
 2.4 with sigma of 0.001
 F2-C241
 2.4 with sigma of 0.001
 F1-C241
 2.4 with sigma of 0.001
 C251-O11
 1.25 with sigma of 0.001
 O12-C251
 1.25 with sigma of 0.001
 C251-C252
 1.55 with sigma of 0.001
 O11-C252
 2.35 with sigma of 0.001
 C252-O12
 2.35 with sigma of 0.001
 F4-F5
 2.4 with sigma of 0.001
 F5-F6
 2.4 with sigma of 0.001
 F4-C252
 1.45 with sigma of 0.001
 F6-C252
 1.45 with sigma of 0.001
 C252-F5
 1.45 with sigma of 0.001
 C244-C243
 1.55 with sigma of 0.001
 C243-O2
 1.25 with sigma of 0.001
 C243-O1
 1.25 with sigma of 0.001
 C244-F14
 1.45 with sigma of 0.001
 F14-F13
 2.4 with sigma of 0.001
 F14-F15
 2.4 with sigma of 0.001
 C243-F13
 2.4 with sigma of 0.001
 C243-F15
 2.4 with sigma of 0.001
 C243-F14
 2.4 with sigma of 0.001
 C47-C49
 1.55 with sigma of 0.001
 C49-C50
 2.35 with sigma of 0.01
 C50-C48
 2.35 with sigma of 0.01
 C49-C48
 2.35 with sigma of 0.01
 C67-C65
 1.55 with sigma of 0.001
 S1-C63
 2.8 with sigma of 0.001
 S1-C61
 2.8 with sigma of 0.001
 C185-C190
 2.35 with sigma of 0.01
 C187-C190
 1.55 with sigma of 0.01
 C97-C100
 1.55 with sigma of 0.001
 C100-C95
 2.35 with sigma of 0.001
 C98-C100
 2.35 with sigma of 0.001
 C98-C95
 2.35 with sigma of 0.001
 C95-C100
 2.35 with sigma of 0.001
 C97-C98
 1.55 with sigma of 0.001
 C35-C38
 2.35 with sigma of 0.001
 C38-C40
 2.35 with sigma of 0.001
 C37-C38
 1.55 with sigma of 0.001
 C38-C35
 2.35 with sigma of 0.001
 C8-C10
 1.55 with sigma of 0.001
 C35-C39
 2.35 with sigma of 0.001
 C39-C40
 2.35 with sigma of 0.001
 C37-C39
 1.55 with sigma of 0.001
 C39-C35
 2.35 with sigma of 0.001
 C38-C39
 2.35 with sigma of 0.001
 S8-C172
 2.85 with sigma of 0.001
 S8-C173
 2.85 with sigma of 0.001
 C176-C177
 1.55 with sigma of 0.001
 C177-C180
 1.55 with sigma of 0.001
 C177-C174
 2.35 with sigma of 0.001
 C175-C177
 2.35 with sigma of 0.001
 C176-C180
 2.35 with sigma of 0.001
 C180-C178
 2.35 with sigma of 0.001
 C177-C178
 1.55 with sigma of 0.001
 C176-C178
 2.35 with sigma of 0.001
 C229-C228
 2.35 with sigma of 0.001
 C207-C210
 1.55 with sigma of 0.001
 C206-C210
 2.35 with sigma of 0.001
 C208-C210
 2.35 with sigma of 0.001
 C210-C209
 2.35 with sigma of 0.001
 C217-C220
 1.55 with sigma of 0.001
 C220-C214
 2.35 with sigma of 0.001
 C214-C220
 2.35 with sigma of 0.001
 C19-C20
 2.35 with sigma of 0.001
 C20-C17
 2.35 with sigma of 0.001
 C17-C20
 2.35 with sigma of 0.001
 C20-C19
 2.35 with sigma of 0.001
 C15-C20
 2.35 with sigma of 0.001
 C78-C80
 1.55 with sigma of 0.001
 C197-C200
 1.55 with sigma of 0.001
 C194-C200
 2.35 with sigma of 0.001
 C27-C28
 1.55 with sigma of 0.001
 C28-C27
 1.55 with sigma of 0.001
 C25-C28
 2.35 with sigma of 0.01
 C29-C28
 2.35 with sigma of 0.001
 C28-C29
 2.35 with sigma of 0.001
 C117-C120
 1.55 with sigma of 0.001
 C119-C120
 2.35 with sigma of 0.001
 C114-C120
 2.35 with sigma of 0.001
 C218-C217
 1.55 with sigma of 0.001
 C218-C214
 2.35 with sigma of 0.001
 C214-C218
 2.35 with sigma of 0.001
 C218-C220
 2.35 with sigma of 0.001
 C95-C99
 2.35 with sigma of 0.001
 C99-C98
 2.35 with sigma of 0.001
 C99-C100
 2.35 with sigma of 0.001
 C98-C99
 2.35 with sigma of 0.001
 C100-C99
 2.35 with sigma of 0.001
 C99-C95
 2.35 with sigma of 0.001
 C97-C99
 1.55 with sigma of 0.001
 C239-C240
 1.55 with sigma of 0.001
 C234-C240
 2.35 with sigma of 0.001
 C239-C238
 1.55 with sigma of 0.001
 C234-C238
 2.35 with sigma of 0.001
 C240-C238
 2.35 with sigma of 0.001
 C239-C237
 1.55 with sigma of 0.001
 C234-C237
 2.35 with sigma of 0.001
 C237-C240
 2.35 with sigma of 0.001
 C237-C238
 2.35 with sigma of 0.001
 C197-C198
 1.55 with sigma of 0.001
 C194-C198
 2.35 with sigma of 0.001
 C200-C198
 2.35 with sigma of 0.001
 C198-C200
 2.35 with sigma of 0.001
 C228-C230
 2.35 with sigma of 0.001
 C227-C230
 1.55 with sigma of 0.001
 C229-C230
 2.35 with sigma of 0.001
 C27-C30
 1.55 with sigma of 0.001
 C25-C30
 2.35 with sigma of 0.01
 C30-C29
 1.55 with sigma of 0.001
 C29-C30
 2.35 with sigma of 0.001
 C28-C30
 1.55 with sigma of 0.001
 C30-C28
 2.35 with sigma of 0.01
 C217-C219
 1.55 with sigma of 0.001
 C214-C219
 2.35 with sigma of 0.001
 C220-C219
 2.35 with sigma of 0.001
 C218-C219
 2.35 with sigma of 0.001
 C145-C150
 2.35 with sigma of 0.001
 C127-C128
 1.55 with sigma of 0.001
 C59-C58
 2.35 with sigma of 0.001
 C189-C185
 2.35 with sigma of 0.01
 C189-C187
 1.55 with sigma of 0.01
 C190-C189
 2.35 with sigma of 0.001
 C137-C134 = C137-C138 = C137-C139 = C137-C140
 1.55 with sigma of 0.001
 C147-C149
 1.55 with sigma of 0.001
 C145-C149
 2.35 with sigma of 0.001
 C145-C148
 2.35 with sigma of 0.001
 C117-C118
 1.55 with sigma of 0.02
 C118-C119
 2.35 with sigma of 0.001
 C114-C118
 2.35 with sigma of 0.001
 C118-C120
 2.35 with sigma of 0.001
 C185-C188
 2.35 with sigma of 0.01
 C187-C188
 1.55 with sigma of 0.001
 C188-C187
 1.55 with sigma of 0.01
 C190-C188
 2.35 with sigma of 0.001
 C188-C189
 2.35 with sigma of 0.001
 C179-C177
 1.55 with sigma of 0.001
 C176-C179
 2.35 with sigma of 0.001
 C180-C179
 2.35 with sigma of 0.001
 C177-C176 = C177-C178 = C177-C179 = C177-C180
 1.55 with sigma of 0.001
 C178-C179
 2.35 with sigma of 0.001
 C197-C199
 1.55 with sigma of 0.001
 C194-C199
 2.35 with sigma of 0.001
 C200-C199
 2.35 with sigma of 0.001
 C198-C199
 2.35 with sigma of 0.001
 C79-C78
 1.55 with sigma of 0.001
 C80-C79
 2.35 with sigma of 0.001
 C65-C69
 2.35 with sigma of 0.001
 C67-C69
 1.55 with sigma of 0.001
 C69-C65
 2.35 with sigma of 0.001
 C67-C70
 1.55 with sigma of 0.001
 C65-C70
 2.35 with sigma of 0.001
 C67-C68
 1.55 with sigma of 0.001
 C69-C70
 2.35 with sigma of 0.0001
 C70-C68
 2.35 with sigma of 0.0001
 C68-C69
 2.35 with sigma of 0.0001
 C65-C68
 2.35 with sigma of 0.001
 S4-C72
 2.8 with sigma of 0.001
 S4-C76
 2.8 with sigma of 0.001
 C74-C80
 2.35 with sigma of 0.001
 C78-C74
 1.55 with sigma of 0.001
 C75-C78
 2.53 with sigma of 0.001
 C78-C73
 2.53 with sigma of 0.001
 C74-C77
 2.35 with sigma of 0.001
 C77-C80
 2.35 with sigma of 0.001
 C78-C77
 1.55 with sigma of 0.001
 C74-C79
 2.35 with sigma of 0.001
 C77-C79
 2.35 with sigma of 0.001
 C95-C97
 1.55 with sigma of 0.001
 C164-C170 \\sim C164-C169 \\sim C164-C168 \\sim C170-C169 \\sim C170-C168
\\sim C169-C168
 with sigma of 0.002
 C167-C164 \\sim C167-C170 \\sim C167-C169 \\sim C167-C168
 with sigma of 0.001
 C110-C106 \\sim C110-C109 \\sim C110-C108 \\sim C106-C109 \\sim C106-C108
\\sim C109-C108
 with sigma of 0.002
 C107-C110 \\sim C107-C106 \\sim C107-C109 \\sim C107-C108
 with sigma of 0.001
 C50-C48 \\sim C50-C45 \\sim C48-C45 \\sim C48-C49 \\sim C45-C49
 with sigma of 0.002
 C47-C50 \\sim C47-C48 \\sim C47-C45 \\sim C47-C49
 with sigma of 0.001
 C4-C10 \\sim C4-C9 \\sim C4-C7 \\sim C10-C9 \\sim C10-C7 \\sim C9-C7
 with sigma of 0.002
 C8-C4 \\sim C8-C10 \\sim C8-C9 \\sim C8-C7
 with sigma of 0.001
 C15-C20 \\sim C19-C20
 with sigma of 0.002
 C18-C15 \\sim C18-C17 \\sim C18-C19 \\sim C18-C20
 with sigma of 0.001
 C221-C229 \\sim C221-C228 \\sim C221-C230 \\sim C229-C228 \\sim C228-C230
 with sigma of 0.002
 C227-C221 \\sim C227-C229 \\sim C227-C228 \\sim C227-C230
 with sigma of 0.001
 C25-C28 \\sim C25-C30 \\sim C25-C29 \\sim C28-C30 \\sim C28-C29
 with sigma of 0.002
 C27-C25 \\sim C27-C28 \\sim C27-C30 \\sim C27-C29
 with sigma of 0.001
 C124-C129 \\sim C124-C130 \\sim C124-C128 \\sim C129-C130 \\sim C129-C128
\\sim C130-C128
 with sigma of 0.002
 C127-C124 \\sim C127-C129 \\sim C127-C130 \\sim C127-C128
 with sigma of 0.001
 C154-C158 \\sim C154-C159 \\sim C154-C160 \\sim C158-C159 \\sim C158-C160
\\sim C159-C160
 with sigma of 0.002
 C157-C154 \\sim C157-C158 \\sim C157-C159 \\sim C157-C160
 with sigma of 0.001
 C54-C60 \\sim C54-C59 \\sim C54-C58 \\sim C60-C59 \\sim C60-C58
 with sigma of 0.002
 C57-C54 \\sim C57-C60 \\sim C57-C59 \\sim C57-C58
 with sigma of 0.001
 C134-C138 \\sim C134-C139 \\sim C134-C140 \\sim C138-C139 \\sim C138-C140
\\sim C139-C140
 with sigma of 0.002
 C137-C134 \\sim C137-C138 \\sim C137-C139 \\sim C137-C140
 with sigma of 0.001
 C145-C148 \\sim C145-C149 \\sim C145-C150 \\sim C148-C149 \\sim C148-C150
\\sim C149-C150
 with sigma of 0.002
 C147-C145 \\sim C147-C148 \\sim C147-C149 \\sim C147-C150
 with sigma of 0.001
 C88-C85 \\sim C88-C89 \\sim C85-C89 \\sim C85-C90 \\sim C89-C90
 with sigma of 0.002
 C87-C88 \\sim C87-C85 \\sim C87-C89 \\sim C87-C90
 with sigma of 0.001
 C185-C190 \\sim C185-C189 \\sim C189-C188
 with sigma of 0.002
 C176-C178 \\sim C176-C179 \\sim C176-C180 \\sim C178-C179 \\sim C178-C180
 with sigma of 0.002
 C177-C176 \\sim C177-C178 \\sim C177-C179 \\sim C177-C180
 with sigma of 0.001
3. Restrained planarity
 C114, C113, C112, C111, C116, C115, C117, S23
 with sigma of 0.001
 C143, C141, C142, C146, C145, C144, C147
 with sigma of 0.001
 C214, C213, C212, C211, C216, C215, C217, S21
 with sigma of 0.001
 C191, C192, C193, C194, C195, C196, C197, S18
 with sigma of 0.001
 C183, C184, C185, C186, C181, C182, C187, S17
 with sigma of 0.001
 C26, C22, C21, C23, C24, C25, C27, S14
 with sigma of 0.001
 C202, C205, C206, C204, C203, C201, C207, S19
 with sigma of 0.001
 C33, C31, C32, C36, C35, C34, C37, S16
 with sigma of 0.001
 C249, C250, O5, O6
 with sigma of 0.01
 C247, C248, O3, O4
 with sigma of 0.01
 C234, C233, C232, C231, C236, C235, C239, S20
 with sigma of 0.001
 C224, C223, C222, C221, C226, C225, C227, S22
 with sigma of 0.001
 C241, C242, O7, O8
 with sigma of 0.01
 C243, C244, O1, O2
 with sigma of 0.01
 C62, C63, C64, C65, C66, C61, C67, S1
 with sigma of 0.001
 C132, C131, C136, C135, C134, C133, C137
 with sigma of 0.001
 C2, C3, C4, C5, C6, C1, C8, S13
 with sigma of 0.01
 C174, C176, C175, C172, C171, C173, C177, S8
 with sigma of 0.0001
 C76, C75, C74, C73, C72, C71, C78, S4
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C183 \\sim C184 \\sim C185 \\sim C186 \\sim C181 \\sim C182: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C114 \\sim C113 \\sim C112 \\sim C111 \\sim C116 \\sim C115: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C103 \\sim C102 \\sim C101 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C108 \\sim C109 \\sim C110: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C162 \\sim C161 \\sim C166 \\sim C165 \\sim C164 \\sim C163 \\sim C167 \\sim
C168 \\sim C169 \\sim C170: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C117: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C214 \\sim C213 \\sim C212 \\sim C211 \\sim C216 \\sim C215: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim C196: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim C196 \\sim C197: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C33 \\sim C31 \\sim C32 \\sim C36 \\sim C35 \\sim C34: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C202 \\sim C205 \\sim C206 \\sim C204 \\sim C203 \\sim C201: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C202 \\sim C205 \\sim C206 \\sim C204 \\sim C203 \\sim C201 \\sim C207 \\sim
S19: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O9 \\sim O10: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C245 \\sim C246 \\sim F16 \\sim F17 \\sim F18 \\sim O9 \\sim O10: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C247 \\sim C248 \\sim F7 \\sim F8 \\sim F9 \\sim O3 \\sim O4: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C33 \\sim C31 \\sim C32 \\sim C36 \\sim C35 \\sim C34 \\sim C37: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C249 \\sim C250 \\sim O5 \\sim O6: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C249 \\sim C250 \\sim F10 \\sim F11 \\sim F12 \\sim O5 \\sim O6: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C234 \\sim C233 \\sim C232 \\sim C231 \\sim C236 \\sim C235: within 1.7A with
sigma of 0.002 and sigma for terminal atoms of 0.002
C224 \\sim C223 \\sim C222 \\sim C221 \\sim C226 \\sim C225: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C241 \\sim C242 \\sim F1 \\sim F2 \\sim F3 \\sim O7 \\sim O8: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C251 \\sim C252 \\sim F4 \\sim F5 \\sim F6 \\sim O11 \\sim O12: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C243 \\sim C244 \\sim F13 \\sim F14 \\sim F15 \\sim O1 \\sim O2: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C44 \\sim C45 \\sim C46 \\sim C42 \\sim C41 \\sim C43 \\sim C47 \\sim C48 \\sim
C49 \\sim C50: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C95 \\sim C94 \\sim C93 \\sim C91 \\sim C92 \\sim C96: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1 \\sim C7 \\sim C8 \\sim C9
\\sim C10: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C33 \\sim C31 \\sim C32 \\sim C36 \\sim C35 \\sim C34 \\sim C37 \\sim C38 \\sim
C39: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C33 \\sim C31 \\sim C32 \\sim C36 \\sim C35 \\sim C34 \\sim C37 \\sim C38 \\sim
C39 \\sim C40: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C174 \\sim C176 \\sim C175 \\sim C172 \\sim C171 \\sim C173: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C202 \\sim C205 \\sim C206 \\sim C204 \\sim C203 \\sim C201 \\sim C207 \\sim
C208 \\sim C209 \\sim C210: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C12 \\sim C11 \\sim C17 \\sim C18 \\sim
C19 \\sim C20: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C98 \\sim C99 \\sim C100: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C95 \\sim C94 \\sim C93 \\sim C91 \\sim C92 \\sim C96 \\sim C97 \\sim C98 \\sim
C99 \\sim C100: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C234 \\sim C233 \\sim C232 \\sim C231 \\sim C236 \\sim C235 \\sim C237 \\sim
C238 \\sim C239 \\sim C240: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C224 \\sim C223 \\sim C222 \\sim C221 \\sim C226 \\sim C225 \\sim C227 \\sim
C228 \\sim C229 \\sim C230: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C26 \\sim C22 \\sim C21 \\sim C23 \\sim C24 \\sim C25 \\sim C27 \\sim C28 \\sim
C29 \\sim C30: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C214 \\sim C213 \\sim C212 \\sim C211 \\sim C216 \\sim C215 \\sim C217 \\sim
C218 \\sim C219 \\sim C220: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C127 \\sim C128 \\sim C129 \\sim C130: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C124 \\sim C125 \\sim C126 \\sim C121 \\sim C122 \\sim C123 \\sim C127 \\sim
C128 \\sim C129 \\sim C130: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156 \\sim C151 \\sim C157 \\sim
C158 \\sim C159 \\sim C160: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C51 \\sim C52 \\sim C57 \\sim C58 \\sim
C59 \\sim C60: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C132 \\sim C131 \\sim C136 \\sim C135 \\sim C134 \\sim C133 \\sim C137 \\sim
C138 \\sim C139 \\sim C140: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C143 \\sim C141 \\sim C142 \\sim C146 \\sim C145 \\sim C144 \\sim C147 \\sim
C148 \\sim C149 \\sim C150: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C83 \\sim C81 \\sim C82 \\sim C86 \\sim C85 \\sim C84 \\sim C87 \\sim C88 \\sim
C89 \\sim C90: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C114 \\sim C113 \\sim C112 \\sim C111 \\sim C116 \\sim C115 \\sim C117 \\sim
C118 \\sim C119 \\sim C120: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C183 \\sim C184 \\sim C185 \\sim C186 \\sim C181 \\sim C182 \\sim C187 \\sim
C188 \\sim C189 \\sim C190: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C174 \\sim C176 \\sim C175 \\sim C172 \\sim C171 \\sim C173 \\sim C177 \\sim
C178 \\sim C179 \\sim C180: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C197 \\sim C198 \\sim C199 \\sim C200: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C61 \\sim C67 \\sim C68 \\sim
C69 \\sim C70: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C79 \\sim C78 \\sim C80 \\sim C77 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim
C71 \\sim C72: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
5.a Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C58(H58A,H58B,H58C), C77(H77A,H77B,H77C), C88(H88A,
 H88B,H88C), C90(H90A,H90B,H90C), C99(H99A,H99B,H99C), C118(H11D,H11E,H11F),
 C120(H12A,H12B,H12C), C128(H12D,H12E,H12F), C139(H13G,H13H,H13I), C140(H14A,
 H14B,H14C), C148(H14D,H14E,H14F), C149(H14G,H14H,H14I), C150(H15A,H15B,H15C),
 C160(H16A,H16B,H16C), C178(H17G,H17H,H17I), C179(H17J,H17K,H17L), C188(H18D,
 H18E,H18F), C189(H18G,H18H,H18I), C190(H19D,H19E,H19F), C198(H19G,H19H,H19I),
 C199(H19J,H19K,H19L), C200(H20D,H20E,H20F), C210(H21A,H21B,H21C), C218(H21D,
 H21E,H21F), C219(H21G,H21H,H21I), C220(H22A,H22B,H22C), C229(H22G,H22H,H22I),
 C230(H23A,H23B,H23C), C237(H23D,H23E,H23F), C238(H23G,H23H,H23I), C240(H24A,
 H24B,H24C), C79(H79A,H79B,H79C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C13(H13), C14(H14), C16(H16), C12(H12),
 C26(H26), C22(H22), C23(H23), C24(H24), C33(H33), C32(H32), C36(H36), C34(H34),
  C44(H44), C46(H46), C42(H42), C43(H43), C53(H53), C55(H55), C56(H56),
 C52(H52), C63(H63), C64(H64), C66(H66), C61(H61), C76(H76), C75(H75), C73(H73),
  C72(H72), C83(H83), C82(H82), C86(H86), C84(H84), C94(H94), C93(H93),
 C92(H92), C96(H96), C103(H103), C102(H102), C104(H104), C105(H105), C113(H113),
  C112(H112), C116(H116), C115(H115), C125(H125), C126(H126), C122(H122),
 C123(H123), C132(H132), C136(H136), C135(H135), C133(H133), C143(H143),
 C142(H142), C146(H146), C144(H144), C152(H152), C153(H153), C155(H155),
 C156(H156), C162(H162), C166(H166), C165(H165), C163(H163), C174(H174),
 C175(H175), C172(H172), C173(H173), C183(H183), C184(H184), C186(H186),
 C181(H181), C192(H192), C193(H193), C195(H195), C196(H196), C202(H202),
 C205(H205), C204(H204), C203(H203), C213(H213), C212(H212), C216(H216),
 C215(H215), C223(H223), C222(H222), C226(H226), C225(H225), C233(H233),
 C232(H232), C236(H236), C235(H235)
5.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C1), C13(C14,C15,C16,C12,C11), C26(C22,C21,C23,C24,C25),
 C33(C31,C32,C36,C35,C34), C44(C45,C46,C42,C41,C43), C53(C54,C55,C56,C51,C52),
 C62(C63,C64,C65,C66,C61), C76(C75,C74,C73,C72,C71), C83(C81,C82,C86,C85,C84),
 C95(C94,C93,C91,C92,C96), C103(C102,C101,C104,C105,C106), C114(C113,C112,C111,
 C116,C115), C124(C125,C126,C121,C122,C123), C132(C131,C136,C135,C134,C133),
 C143(C141,C142,C146,C145,C144), C152(C153,C154,C155,C156,C151), C162(C161,C166,
 C165,C164,C163), C174(C176,C175,C172,C171,C173), C183(C184,C185,C186,C181,
 C182), C191(C192,C193,C194,C195,C196), C202(C205,C206,C204,C203,C201),
 C214(C213,C212,C211,C216,C215), C224(C223,C222,C221,C226,C225), C234(C233,C232,
 C231,C236,C235)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C40(H40A,H40B,H40C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C80(H80A,H80B,H80C), C89(H89A,H89B,H89C), C98(H98A,H98B,H98C), C100(H10D,H10E,
 H10F), C108(H10G,H10H,H10I), C109(H10J,H10K,H10L), C110(H11A,H11B,H11C),
 C119(H11G,H11H,H11I), C129(H12G,H12H,H12I), C130(H13A,H13B,H13C), C138(H13D,
 H13E,H13F), C158(H15D,H15E,H15F), C159(H15G,H15H,H15I), C168(H16D,H16E,H16F),
 C169(H16G,H16H,H16I), C170(H17D,H17E,H17F), C180(H18A,H18B,H18C), C208(H20G,
 H20H,H20I), C209(H20J,H20K,H20L), C228(H22D,H22E,H22F)
;
_shelx_res_checksum              34001
_shelx_hkl_checksum              60333
_shelx_fab_checksum              43447
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.861
_oxdiff_exptl_absorpt_empirical_full_min 0.589