Polyoxometalate-mediated syntheses of three structurally new silver clusters.
Zhang, Jing; Dong, Yuanyuan; Deng, Lan; Chi, Manzhou; Feng, Yeqin; Zhao, Mengyun; Lv, Hongjin; Yang, Guo-Yu; Nanoscale 16 (2024) 11518–11523; doi:10.1039/d4nr02016b

data_1571726
_publ_section_title
;
 Polyoxometalate-mediated syntheses of three structurally new silver
 clusters.
;
_journal_issue                   24
_journal_name_full               Nanoscale
_journal_page_first              11518
_journal_page_last               11523
_journal_paper_doi               10.1039/d4nr02016b
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety
'C195 H232 Ag24 Cl O52 P12 S11 Si W15, 0.606(O17 W6), C195 H234 Ag24 Cl O41.093 P12 S11 Si W11.364, 2(O Si0.5)'
_chemical_formula_sum            'C390 H466 Ag48 Cl2 O105.39 P24 S22 Si3 W30'
_chemical_formula_weight         19136.95
_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   mixed
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                86.9110(10)
_cell_angle_beta                 86.8350(10)
_cell_angle_gamma                80.0060(10)
_cell_formula_units_Z            2
_cell_length_a                   21.7876(2)
_cell_length_b                   21.8079(2)
_cell_length_c                   59.0524(4)
_cell_measurement_reflns_used    171894
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.6480
_cell_measurement_theta_min      2.1450
_cell_volume                     27562.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -82.00 -56.00   0.25    2.00    --   -6.91 -18.00 -21.00  104
  2  \w    -20.00  68.00   0.25    2.00    --   -6.91  18.00 146.00  352
  3  \w    -11.00  37.00   0.25    2.00    --    3.47 -99.00  30.00  192
  4  \w     43.00  69.00   0.25    2.00    --    3.47  38.00-180.00  104
  5  \w    -18.00  12.00   0.25    2.00    --   -6.91 -99.00  60.00  120
  6  \w    -18.00  26.00   0.25    2.00    --   -6.91 -99.00 -90.00  176
  7  \w    -17.00  22.00   0.25    2.00    --   -6.91 -99.00-150.00  156
  8  \w     -8.00  26.00   0.25    2.00    --   -6.91 -99.00   0.00  136
  9  \w    -28.00  65.00   0.25    2.00    --   -6.91  77.00-180.00  372
 10  \w    -23.00   2.00   0.25    2.00    --   -6.91 -18.00 -21.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0300070000
_diffrn_orient_matrix_UB_12      0.0185562000
_diffrn_orient_matrix_UB_13      0.0013020000
_diffrn_orient_matrix_UB_21      0.0138875000
_diffrn_orient_matrix_UB_22      0.0257567000
_diffrn_orient_matrix_UB_23      0.0025654000
_diffrn_orient_matrix_UB_31      0.0012836000
_diffrn_orient_matrix_UB_32      0.0092610000
_diffrn_orient_matrix_UB_33      -0.0116940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            359565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.991
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_description       block
_exptl_crystal_F_000             17826
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.201
_refine_diff_density_min         -3.544
_refine_diff_density_rms         0.497
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6311
_refine_ls_number_reflns         96956
_refine_ls_number_restraints     17199
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.1503
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+6551.4736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3286
_refine_ls_wR_factor_ref         0.3312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                88361
_reflns_number_total             96956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02016b2.cif
_cod_data_source_block           20220928
_cod_depositor_comments
'Adding full bibliography for 1571724--1571726.cif.'
_cod_database_code               1571726
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag Si W O P S'
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.563
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 W3-O1 = W1-O1
 1.9 with sigma of 0.01
 H91A-H376
 2.1 with sigma of 0.01
 C103-C411 = C411-C413
 1.46 with sigma of 0.01
 C103-C413
 2.5 with sigma of 0.01
 C205-C255 = C313-C255
 1.46 with sigma of 0.01
 C226-C158 = C330-C226
 1.48 with sigma of 0.01
 C313-C205
 2.5 with sigma of 0.01
 S24-C219
 1.8 with sigma of 0.01
 C330-C158
 2.5 with sigma of 0.01
 C56-C356 = C56-C352
 1.48 with sigma of 0.01
 O19-O22 = O22-O21
 2.5 with sigma of 0.01
 C381-C19
 2.5 with sigma of 0.01
 C354-C272 = C350-C272
 1.48 with sigma of 0.01
 C19-S24 = S24-C381
 2.6 with sigma of 0.01
 C160-C74 = C346-C74
 1.48 with sigma of 0.01
 Ag23-S21 = Ag21-S21 = Ag41-S21
 2.3 with sigma of 0.01
 C88-C394 = C394-C176
 1.48 with sigma of 0.01
 O20-O19 = O19-O22
 2.5 with sigma of 0.01
 C303-C191 = C191-C189
 1.48 with sigma of 0.01
 C34-C390 = C384-C390
 1.48 with sigma of 0.01
 C39-C201 = C201-C115
 1.48 with sigma of 0.01
 C240-C252 = C328-C240
 1.48 with sigma of 0.01
 C409-C155 = C155-C51
 1.48 with sigma of 0.01
 Si1-O19 = Si1-O22 = Si1-O20 = Si1-O21
 1.5 with sigma of 0.01
 C152-S26 = S26-C70
 2.6 with sigma of 0.01
 W9A-O1B
 1.9 with sigma of 0.01
 C405-C251 = C127-C251
 1.48 with sigma of 0.01
 C19-C219 = C219-C381
 1.48 with sigma of 0.01
 O20-O21 = O21-O22
 2.5 with sigma of 0.01
 C34-S2 = S2-C384
 2.6 with sigma of 0.01
 C407-C101 = C311-C101
 1.48 with sigma of 0.01
 C152-C66 = C70-C66
 1.48 with sigma of 0.01
 C356-S30 = S30-C352
 2.6 with sigma of 0.01
 O40-O43 = O43-O41
 2.5 with sigma of 0.01
 C303-S3 = S3-C189
 2.6 with sigma of 0.01
 O43-O41 = O41-O42
 2.5 with sigma of 0.01
 C407-S23 = S23-C311
 2.6 with sigma of 0.01
 C356-C352
 2.5 with sigma of 0.01
 S2-C390
 1.8 with sigma of 0.01
 C39-S11 = S11-C115
 2.6 with sigma of 0.01
 C127-S13 = S13-C405
 2.6 with sigma of 0.01
 W11A-O28A = W10A-O28A
 1.9 with sigma of 0.01
 C402-C396 = C408-C396
 1.48 with sigma of 0.01
 S25-C409 = C409-C51
 2.6 with sigma of 0.01
 W7A-O39A
 1.9 with sigma of 0.01
 C92-C180 = C182-C92
 1.48 with sigma of 0.01
 C51-C409
 2.5 with sigma of 0.01
 W10A-O27A = W9A-O27A
 1.9 with sigma of 0.01
 C412-C38 = C400-C38
 1.48 with sigma of 0.01
 C127-C405
 2.5 with sigma of 0.01
 C394-C176 = C88-C394
 1.48 with sigma of 0.01
 O40-O42 = O42-O43
 2.5 with sigma of 0.01
 S7-C38 = S29-C396 = S27-C394 = S31-C92 = S15-C1
 1.8 with sigma of 0.01
 C115-C39
 2.5 with sigma of 0.01
 W4-O9 = W2-O9
 1.9 with sigma of 0.01
 C196-C1 = C404-C1
 1.48 with sigma of 0.01
 O42-O43 = O43-O41
 2.5 with sigma of 0.01
 S13-C251
 1.9 with sigma of 0.01
 S23-C101
 1.9 with sigma of 0.01
 C88-S27 = S27-C176
 2.6 with sigma of 0.01
 Si2-O40 = Si2-O41 = Si2-O42 = Si2-O43
 1.5 with sigma of 0.01
 S25-C155
 1.9 with sigma of 0.01
 C180-C182
 2.5 with sigma of 0.01
 W9A-O26A = W11A-O26A
 1.9 with sigma of 0.01
 W10-O30 = W11-O30
 1.9 with sigma of 0.01
 C404-C196
 2.5 with sigma of 0.01
 S3-C191
 1.9 with sigma of 0.01
 O40-O41 = O41-O42
 2.5 with sigma of 0.01
 C77-C99 = C99-C197
 1.48 with sigma of 0.01
 C412-S7 = S7-C400
 2.6 with sigma of 0.01
 C408-C402
 2.5 with sigma of 0.01
 C209-C125 = C125-C95
 1.48 with sigma of 0.01
 W7-O31 = W10-O31
 1.9 with sigma of 0.01
 C239-C13 = C157-C13
 1.48 with sigma of 0.01
 W12A-O30A = W8A-O30A
 1.9 with sigma of 0.01
 C299-C379 = C379-C377
 1.48 with sigma of 0.01
 O33A-W12A_$1
 1.9 with sigma of 0.01
 W7-O25 = W9-O25
 1.9 with sigma of 0.01
 S19-C43
 1.9 with sigma of 0.01
 C63-C43 = C43-C151
 1.48 with sigma of 0.01
 W8-O24 = W9-O24
 1.9 with sigma of 0.01
 C404-S15 = S15-C196
 2.6 with sigma of 0.01
 S9-C99
 1.9 with sigma of 0.01
 W5-O10 = W4-O10
 1.9 with sigma of 0.01
 C72-C68 = C68-C426
 1.48 with sigma of 0.01
 C396-C176
 3.1 with sigma of 0.01
 W7-O23 = O23-W8
 1.9 with sigma of 0.01
 S17-C379
 1.9 with sigma of 0.01
 W7A-O24A = W8A-O24A
 1.9 with sigma of 0.01
 S9-C77 = C77-C197
 2.6 with sigma of 0.01
 C88-C176
 2.5 with sigma of 0.01
 S21-C13
 1.9 with sigma of 0.01
 W3-O11 = W5-O11
 1.9 with sigma of 0.01
 C282-C172 = C386-C282
 1.46 with sigma of 0.01
 W9A-O23A = W7A-O23A
 1.9 with sigma of 0.01
 C239-S21 = S21-C157
 2.6 with sigma of 0.01
 C63-S19 = S19-C151
 2.6 with sigma of 0.01
 W3-O6 = W6-O6
 1.9 with sigma of 0.01
 C419-C107
 2.5 with sigma of 0.01
 W8A-O25A = W9A-O25A
 1.9 with sigma of 0.01
 W4A-O7A = W5A-O7A = W5A-O5 = W6-O5 = W6-O12 = W5-O12
 1.9 with sigma of 0.01
 H133-H34L
 3.2 with sigma of 0.01
 C107-C55
 1.5 with sigma of 0.01
 S24A-C55
 1.8 with sigma of 0.01
 W2-O7 = W3-O7
 1.9 with sigma of 0.01
 W2-O2 = W1-O2
 1.9 with sigma of 0.01
 W1A-O1A = O1A-W2A
 1.9 with sigma of 0.01
 W3A-O10A = O10A-W2A
 1.9 with sigma of 0.01
 O1-O7
 2.7 with sigma of 0.01
 W2-O8 = W6_$2-O8
 1.9 with sigma of 0.01
 W1-O3 = W5_$2-O3
 1.9 with sigma of 0.01
 W4_$2-O4 = W1-O4
 1.9 with sigma of 0.01
 W1A-O2A = W3A-O2A
 1.9 with sigma of 0.01
 W5A-O6A = O6A-W6A
 1.9 with sigma of 0.01
 W5A-O4A = W1A-O4A
 1.9 with sigma of 0.01
 O1A-O4A
 2.7 with sigma of 0.01
 W2A-O8A = W4A-O8A
 1.9 with sigma of 0.01
 W3A-O12A = W4A_$2-O12A
 1.9 with sigma of 0.01
 W3A-O11A = W5A_$2-O11A
 1.9 with sigma of 0.01
 W2A-O10A = W3A-O10A
 1.9 with sigma of 0.01
 W1A-O3A = W6A-O3A
 1.9 with sigma of 0.01
 W1A-O13A
 1.9 with sigma of 0.01
 W3A-O18A
 1.9 with sigma of 0.01
 W2A-O9A
 1.9 with sigma of 0.01
 O9A-O10A = O10A-O1A
 2.7 with sigma of 0.01
 W2A-O17A
 1.9 with sigma of 0.01
 W5A-O14A
 1.9 with sigma of 0.01
 W6A-O15A
 1.9 with sigma of 0.01
 W4A-O16A
 1.9 with sigma of 0.01
 O10_$2-O3 = O3-O4
 2.7 with sigma of 0.01
 O2-O3 = O3-O12_$2
 2.7 with sigma of 0.01
 W3-O15
 1.9 with sigma of 0.01
 W1-O14
 1.9 with sigma of 0.01
 W2-O16
 1.9 with sigma of 0.01
 W6-O13
 1.9 with sigma of 0.01
 W5-O18
 1.9 with sigma of 0.01
 W4-O17
 1.9 with sigma of 0.01
 W11-O28 = W12-O28
 1.9 with sigma of 0.01
 W11-O27 = O27-W9
 1.9 with sigma of 0.01
 W9-O26 = W12-O26
 1.9 with sigma of 0.01
 O26A-O27A = O27A-O23A
 2.7 with sigma of 0.01
 O28A-O27A = O27A-O26A
 2.7 with sigma of 0.01
 O25A-O23A = O23A-O24A
 2.7 with sigma of 0.01
 W12-O29
 1.9 with sigma of 0.01
 W10-O32
 1.9 with sigma of 0.01
 W11-O38
 1.9 with sigma of 0.01
 O32-O30 = O30-O38
 2.7 with sigma of 0.01
 O30-O31 = O31-O29_$1
 2.7 with sigma of 0.01
 O29_$1-O32 = O32-O30
 2.7 with sigma of 0.01
 O27-O30 = O30-O31
 2.7 with sigma of 0.01
 O38-O30 = O30-O32
 2.7 with sigma of 0.01
 W7-O34
 1.9 with sigma of 0.01
 O30-O27 = O27-O25
 2.7 with sigma of 0.01
 O28-O27 = O27-O26
 2.7 with sigma of 0.01
 W7A-O32A = W7A-O33A
 1.9 with sigma of 0.01
 W8A-O31A
 1.9 with sigma of 0.01
 O24A-O31A = O31A_$1-O28A
 2.7 with sigma of 0.01
 O26A-O29A = O29A-O30A
 2.7 with sigma of 0.01
 O24A-O32A = O32A_$1-O28A
 2.7 with sigma of 0.01
 O33A_$1-O29A = O29A-O32A_$1
 2.7 with sigma of 0.01
 O30A-O29A = O29A-O26A
 2.7 with sigma of 0.01
 O32A_$1-O29A = O29A-O33A_$1
 2.7 with sigma of 0.01
 W11A-O37A
 1.9 with sigma of 0.01
 W8A-O35A
 1.9 with sigma of 0.01
 W12A-O36A
 1.9 with sigma of 0.01
 W11A-O29A = W12A-O29A
 2.1 with sigma of 0.01
 W10A-O34A
 1.9 with sigma of 0.01
 W7-O35
 1.9 with sigma of 0.01
 W10-O33
 1.9 with sigma of 0.01
 O32-O33 = O33-O31
 2.7 with sigma of 0.01
 W11-O37
 1.9 with sigma of 0.01
 W9-O36
 1.9 with sigma of 0.01
 W12-O39
 1.9 with sigma of 0.01
 W8A-O31A = O31A_$1-W10A
 1.9 with sigma of 0.01
 W12A_$1-O38A = O38A-W10A
 1.9 with sigma of 0.01
 O23A-O33A = O33A-O38A
 2.7 with sigma of 0.01
 O23A-O27A = O27A-O38A
 2.7 with sigma of 0.01
 Ag23-Ag21
 3.5 with sigma of 0.01
 Ag3-Ag51
 3.5 with sigma of 0.01
 P5-C224
 1.8 with sigma of 0.01
 S27-C394
 1.8 with sigma of 0.01
 S11-C201
 1.9 with sigma of 0.01
 S5-C125
 1.9 with sigma of 0.01
 C378-C265
 3 with sigma of 0.01
 C68-S26A
 1.8 with sigma of 0.01
 C62-C416 = C416-C278
 1.48 with sigma of 0.01
 C265-C380
 3.1 with sigma of 0.01
 P11-C423
 1.6 with sigma of 0.01
 C4-C348 = C4-C344
 1.46 with sigma of 0.01
 P15-C271
 1.7 with sigma of 0.01
 C399-C173 = C85-C399
 1.46 with sigma of 0.01
 H35N-H421 = H421-H35O
 2 with sigma of 0.01
 H38I-H139
 2 with sigma of 0.01
 H41J-H293 = H293-H41K
 2 with sigma of 0.01
 Cl2-C408
 2.5 with sigma of 0.01
 H247-H135
 2.1 with sigma of 0.01
 H17I-H247
 2.2 with sigma of 0.01
 O27A-O1B \\sim O1B-O25A
 with sigma of 0.01
 O23A-O39A \\sim O39A-O32A
 with sigma of 0.01
 C152-C66 \\sim C426-C68
 with sigma of 0.02
 C66-C70 \\sim C68-C72
 with sigma of 0.02
 C152-C70 \\sim C426-C72
 with sigma of 0.04
 O1A-O13A \\sim O13A-O3A
 with sigma of 0.01
 O4A-O13A \\sim O13A-O2A
 with sigma of 0.01
 O2A-O18A \\sim O18A-O11A
 with sigma of 0.01
 O12A-O18A \\sim O18A-O10A
 with sigma of 0.01
 O1A-O17A \\sim O17A-O9A
 with sigma of 0.01
 O10A-O17A \\sim O17A-O8A
 with sigma of 0.01
 O7A-O14A \\sim O14A-O6A
 with sigma of 0.01
 O6A-O15A \\sim O15A-O5A
 with sigma of 0.01
 O8A-O16A \\sim O16A-O7A
 with sigma of 0.01
 O7-O15 \\sim O15-O6
 with sigma of 0.01
 O1-O14 \\sim O14-O3
 with sigma of 0.01
 O7-O16 \\sim O16-O8
 with sigma of 0.01
 O5-O13 \\sim O13-O12
 with sigma of 0.01
 O12-O18 \\sim O18-O11
 with sigma of 0.01
 O10-O17 \\sim O17-O9
 with sigma of 0.01
 O28A-O37A \\sim O37A-O26A
 with sigma of 0.01
 O25A-O35A \\sim O35A-O31A
 with sigma of 0.01
 O29A-O36A \\sim O36A-O30A
 with sigma of 0.01
 O38A-O34A \\sim O34A-O27A
 with sigma of 0.01
 O34-O35 \\sim O35-O25
 with sigma of 0.01
 O30-O37 \\sim O37-O27
 with sigma of 0.01
 O30-O37 \\sim O37-O38
 with sigma of 0.01
 O27-O36 \\sim O36-O24
 with sigma of 0.01
 O25-O36 \\sim O36-O26
 with sigma of 0.01
 O28-O39 \\sim O39-O29
 with sigma of 0.01
 O29A-O37A \\sim O37A-O28A
 with sigma of 0.01
 O28A-O34A \\sim O34A-O38A
 with sigma of 0.01
 O31A_$1-O34A \\sim O34A-O27A
 with sigma of 0.01
 C293-P11 \\sim P11-C297
 with sigma of 0.01
 Ag30-C66 \\sim Ag30-C68
 with sigma of 0.04
 C67-P19 \\sim P19-C33
 with sigma of 0.01
 C211-P11 \\sim P11-C53
 with sigma of 0.01
 C17-P15 \\sim P15-C135
 with sigma of 0.01
3. Restrained planarity
 P5, C372, C380, C382
 with sigma of 0.01
 C211, C423, C53, P11
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(Si1) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O19)
\\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(W1A)=Sof(W2A)=Sof(W3A)=Sof(W4A)=Sof(W5A)=Sof(W6A)=Sof(O1A)=Sof(O2A)=
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=
 Sof(O11A)=Sof(O12A)=Sof(O13A)=Sof(O14A)=Sof(O15A)=Sof(O16A)=Sof(O17A)=
 Sof(O18A)=1-FVAR(1)
 Sof(W1)=Sof(W2)=Sof(W3)=Sof(W4)=Sof(W5)=Sof(W6)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(O17)=Sof(O18)=FVAR(1)
 Sof(W7A)=Sof(W8A)=Sof(W9A)=Sof(W10A)=Sof(W11A)=Sof(W12A)=Sof(O1B)=Sof(O23A)=
 Sof(O24A)=Sof(O25A)=Sof(O26A)=Sof(O27A)=Sof(O28A)=Sof(O29A)=Sof(O30A)=
 Sof(O31A)=Sof(O32A)=Sof(O33A)=Sof(O34A)=Sof(O35A)=Sof(O36A)=Sof(O37A)=
 Sof(O38A)=Sof(O39A)=1-FVAR(2)
 Sof(W7)=Sof(W8)=Sof(W9)=Sof(W10)=Sof(W11)=Sof(W12)=Sof(O23)=Sof(O24)=Sof(O25)=
 Sof(O26)=Sof(O27)=Sof(O28)=Sof(O29)=Sof(O30)=Sof(O31)=Sof(O32)=Sof(O33)=
 Sof(O34)=Sof(O35)=Sof(O36)=Sof(O37)=Sof(O38)=Sof(O39)=FVAR(2)
 Sof(Ag5)=Sof(Ag19)=Sof(Ag21)=Sof(Ag23)=Sof(Ag39)=Sof(S5)=Sof(S9)=Sof(S17)=
 Sof(S19)=Sof(S21)=Sof(C239)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C125)=Sof(H125)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C299)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C151)=Sof(H15K)=Sof(H15L)=Sof(H15M)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C157)=Sof(H15N)=Sof(H15O)=Sof(H15P)=Sof(C43)=Sof(H43)=Sof(C377)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=Sof(C379)=Sof(H379)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=
 Sof(C197)=Sof(H19G)=Sof(H19H)=Sof(H19I)=Sof(C99)=Sof(H99)=Sof(C13)=Sof(H13)=
 Sof(C209)=Sof(H20I)=Sof(H20J)=Sof(H20K)=1-FVAR(3)
 Sof(Ag3)=Sof(Ag13)=Sof(Ag25)=Sof(Ag49)=Sof(Ag51)=Sof(S3)=Sof(S11)=Sof(S13)=
 Sof(S23)=Sof(S25)=Sof(C115)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C251)=Sof(H251)=
 Sof(C127)=Sof(H12E)=Sof(H12F)=Sof(H12G)=Sof(C303)=Sof(H30C)=Sof(H30D)=
 Sof(H30E)=Sof(C155)=Sof(H155)=Sof(C311)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C189)=Sof(H18G)=Sof(H18H)=Sof(H18I)=
 Sof(C191)=Sof(H191)=Sof(C201)=Sof(H201)=Sof(C101)=Sof(H101)=Sof(C405)=
 Sof(H40L)=Sof(H40M)=Sof(H40N)=Sof(C407)=Sof(H40O)=Sof(H40P)=Sof(H40Q)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C409)=Sof(H40R)=Sof(H40S)=Sof(H40T)=FVAR(3)
 Sof(Ag7)=Sof(Ag27)=Sof(Ag29)=Sof(Ag55)=Sof(Ag57)=Sof(S7)=Sof(S15)=Sof(S27)=
 Sof(S29)=Sof(S31)=Sof(C1)=Sof(H1)=Sof(C38)=Sof(H38)=Sof(C88)=Sof(H88A)=
 Sof(H88B)=Sof(H88C)=Sof(C92)=Sof(H92)=Sof(C176)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C180)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C182)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C196)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C394)=Sof(H394)=
 Sof(C396)=Sof(H396)=Sof(C400)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C402)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C404)=Sof(H40G)=Sof(H40H)=Sof(H40I)=
 Sof(C408)=Sof(H40J)=Sof(H40K)=Sof(H2)=Sof(C412)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(Ag53)=1-FVAR(4)
 Sof(Ag2)=Sof(Ag15)=Sof(Ag17)=Sof(Ag35)=Sof(Ag45)=Sof(S2)=Sof(S14)=Sof(S28)=
 Sof(S30)=Sof(S32)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C56)=Sof(H56)=
 Sof(C74)=Sof(H74)=Sof(C160)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C240)=Sof(H240)=
 Sof(C252)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C272)=Sof(H272)=Sof(C328)=
 Sof(H32E)=Sof(H32F)=Sof(H32G)=Sof(C346)=Sof(H34G)=Sof(H34H)=Sof(H34I)=
 Sof(C350)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C352)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C354)=Sof(H35G)=Sof(H35H)=Sof(H35I)=Sof(C356)=Sof(H35J)=
 Sof(H35K)=Sof(H35L)=Sof(C384)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C390)=
 Sof(H390)=Sof(Ag58)=FVAR(4)
 Sof(Ag1A)=Sof(Ag9A)=Sof(S26A)=Sof(C68)=Sof(H68)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=Sof(C426)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(5)
 Sof(Ag9)=Sof(Ag33)=Sof(S26)=Sof(C66)=Sof(H66)=Sof(C70)=Sof(H70A)=Sof(H70B)=
 Sof(H70C)=Sof(C152)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(5)
 Sof(Ag)=1-FVAR(6)
 Sof(Ag37)=FVAR(6)
 Sof(Ag60)=1-FVAR(7)
 Sof(Ag43)=FVAR(7)
 Sof(Ag61)=1-FVAR(8)
 Sof(Ag44)=FVAR(8)
 Sof(Ag1B)=Sof(Ag62)=Sof(S24A)=Sof(C107)=Sof(H10E)=Sof(H10F)=Sof(H10G)=
 Sof(C55)=Sof(H55)=Sof(C419)=Sof(H41I)=Sof(H41J)=Sof(H41K)=1-FVAR(9)
 Sof(Ag11)=Sof(Ag41)=Sof(S24)=Sof(C219)=Sof(H219)=Sof(C19)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C381)=Sof(H38G)=Sof(H38H)=Sof(H38I)=FVAR(9)
 Fixed Sof: O19(0.25) O20(0.25) O21(0.25) O22(0.25) O40(0.25) O41(0.25)
 O42(0.25) O43(0.25)
 Fixed X: C396(-0.374579) C357(-0.64518) C203(-0.69244) C205(-0.95094) C103(-
 1.23926) C413(-1.20699)
 Fixed Y: C396(1.10682) C357(1.153161) C203(1.09557) C205(0.59489)
 C103(1.325281) C413(1.34072)
 Fixed Z: C396(0.81097) C357(0.528181) C203(0.499469) C205(0.68487)
 C103(0.681141) C413(0.63846)
7.a Riding coordinates:
 C34(H34A,H34B,H34C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C88(H88A,H88B,
 H88C), C98(H98A,H98B,H98C), C152(H15A,H15B,H15C), C158(H15F,H15G,H15H),
 C160(H16A,H16B,H16C), C172(H17A,H17B,H17C), C176(H17D,H17E,H17F), C180(H18A,
 H18B,H18C), C182(H18D,H18E,H18F), C196(H19A,H19B,H19C), C252(H25A,H25B,H25C),
 C328(H32E,H32F,H32G), C330(H33A,H33B,H33C), C346(H34G,H34H,H34I), C348(H34J,
 H34K,H34L), C350(H35A,H35B,H35C), C352(H35D,H35E,H35F), C354(H35G,H35H,H35I),
 C356(H35J,H35K,H35L), C370(H37A,H37B,H37C), C384(H38A,H38B,H38C), C386(H38D,
 H38E,H38F), C400(H40A,H40B,H40C), C402(H40D,H40E,H40F), C404(H40G,H40H,H40I),
 C408(H40J,H40K,H2), C412(H41A,H41B,H41C), C426(H42A,H42B,H42C), C107(H10E,H10F,
 H10G), C115(H11D,H11E,H11F), C239(H23A,H23B,H23C), C63(H63A,H63B,H63C),
 C127(H12E,H12F,H12G), C299(H29A,H29B,H29C), C151(H15K,H15L,H15M), C303(H30C,
 H30D,H30E), C19(H19D,H19E,H19F), C77(H77A,H77B,H77C), C311(H31A,H31B,H31C),
 C39(H39A,H39B,H39C), C313(H31D,H31E,H31F), C157(H15N,H15O,H15P), C357(H35M,
 H35N,H35O), C91(H91A,H91B,H91C), C377(H37D,H37E,H37F), C189(H18G,H18H,H18I),
 C95(H95A,H95B,H95C), C381(H38G,H38H,H38I), C197(H19G,H19H,H19I), C395(H39D,
 H39E,H39F), C397(H39G,H39H,H39I), C405(H40L,H40M,H40N), C203(H20A,H20B,H20C),
 C407(H40O,H40P,H40Q), C51(H51A,H51B,H51C), C409(H40R,H40S,H40T), C205(H20D,
 H20E,H20F), C103(H10J,H10K,H10L), C413(H41F,H41G,H41H), C209(H20I,H20J,H20K),
 C419(H41I,H41J,H41K)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C38(H38), C56(H56), C66(H66), C68(H68), C74(H74), C92(H92),
 C102(H102), C226(H226), C240(H240), C242(H242), C272(H272), C282(H282),
 C390(H390), C394(H394), C396(H396), C219(H219), C55(H55), C125(H125),
 C251(H251), C255(H255), C129(H129), C131(H131), C155(H155), C333(H333),
 C43(H43), C379(H379), C191(H191), C99(H99), C201(H201), C101(H101), C411(H411),
  C13(H13)
7.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C30(H30A,H30B), C32(H32A,H32B), C60(H60A,H60B), C62(H62A,
 H62B), C64(H64A,H64B), C94(H94A,H94B), C96(H96A,H96B), C100(H10A,H10B),
 C104(H10C,H10D), C122(H12A,H12B), C126(H12C,H12D), C156(H15D,H15E), C248(H24C,
 H24D), C270(H27A,H27B), C276(H27C,H27D), C278(H27E,H27F), C326(H32C,H32D),
 C416(H41D,H41E), C213(H21A,H21B), C215(H21C,H21D), C109(H10H,H10I), C15(H15I,
 H15J), C253(H25D,H25E), C259(H25F,H25G), C277(H27G,H27H), C283(H28A,H28B),
 C307(H30F,H30G), C309(H30H,H30I), C315(H31G,H31H), C79(H79A,H79B), C331(H33D,
 H33E), C85(H85A,H85B), C171(H17G,H17H), C173(H17I,H17J), C399(H39J,H39K),
 C207(H20G,H20H)
7.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C16(H16), C18(H18), C20(H20), C22(H22), C26(H26),
 C28(H28), C36(H36), C42(H42), C44(H44), C46(H46), C48(H48), C50(H50), C52(H52),
  C54(H54), C58(H58), C78(H78), C80(H80), C82(H82), C84(H84), C86(H86),
 C108(H108), C110(H110), C112(H112), C114(H114), C116(H116), C120(H120),
 C124(H124), C130(H130), C132(H132), C134(H134), C136(H136), C138(H138),
 C142(H142), C144(H144), C146(H146), C148(H148), C150(H150), C154(H154),
 C162(H162), C164(H164), C166(H166), C168(H168), C170(H170), C174(H174),
 C186(H186), C188(H188), C190(H190), C192(H192), C194(H194), C200(H200),
 C202(H202), C204(H204), C206(H206), C208(H208), C210(H210), C214(H214),
 C216(H216), C218(H218), C220(H220), C222(H222), C230(H230), C232(H232),
 C234(H234), C236(H236), C238(H238), C244(H244), C246(H246), C250(H250),
 C254(H254), C256(H256), C258(H258), C260(H260), C262(H262), C264(H264),
 C274(H274), C280(H280), C284(H284), C286(H286), C288(H288), C290(H290),
 C292(H292), C296(H296), C298(H298), C300(H300), C304(H304), C306(H306),
 C308(H308), C310(H310), C314(H314), C316(H316), C318(H318), C320(H320),
 C322(H322), C334(H334), C336(H336), C338(H338), C340(H340), C342(H342),
 C358(H358), C360(H360), C364(H364), C366(H366), C368(H368), C372(H372),
 C374(H374), C376(H376), C378(H378), C380(H380), C388(H388), C392(H392),
 C398(H398), C406(H406), C410(H410), C414(H414), C418(H418), C420(H420),
 C422(H422), C27(H27), C221(H221), C111(H111), C7(H7), C225(H225), C113(H113),
 C227(H227), C57(H57), C229(H229), C29(H29), C233(H233), C117(H117), C235(H235),
  C59(H59), C119(H119), C243(H243), C61(H61), C245(H245), C123(H123),
 C247(H247), C31(H31), C249(H249), C257(H257), C65(H65), C261(H261), C33(H33),
 C265(H265), C133(H133), C267(H267), C67(H67), C269(H269), C135(H135), C17(H17),
  C273(H273), C137(H137), C139(H139), C279(H279), C35(H35), C281(H281),
 C71(H71), C143(H143), C287(H287), C9(H9), C289(H289), C145(H145), C291(H291),
 C293(H293), C147(H147), C295(H295), C37(H37), C297(H297), C149(H149),
 C301(H301), C153(H153), C317(H317), C159(H159), C319(H319), C5(H5), C321(H321),
  C161(H161), C81(H81), C163(H163), C327(H327), C41(H41), C329(H329),
 C165(H165), C167(H167), C335(H335), C21(H21), C337(H337), C169(H169),
 C339(H339), C341(H341), C343(H343), C345(H345), C347(H347), C87(H87),
 C349(H349), C351(H351), C11(H11), C353(H353), C177(H177), C355(H355), C89(H89),
  C359(H359), C45(H45), C361(H361), C181(H181), C363(H363), C183(H183),
 C367(H367), C23(H23), C369(H369), C185(H185), C93(H93), C373(H373), C187(H187),
  C375(H375), C47(H47), C383(H383), C3(H3), C385(H385), C387(H387), C97(H97),
 C389(H389), C195(H195), C391(H391), C393(H393), C199(H199), C25(H25),
 C401(H401), C403(H403), C415(H415), C417(H417), C105(H105), C421(H421),
 C211(H211), C53(H53), C425(H425)
7.e Fitted hexagon refined as free rotating group:
 C12(C14,C16,C18,C20,C22), C40(C42,C44,C46,C48,C50), C76(C78,C80,C82,C84,C86),
 C106(C108,C110,C112,C114,C116), C128(C130,C132,C134,C136,C138), C140(C142,C144,
 C146,C148,C150), C184(C186,C188,C190,C192,C194), C198(C200,C202,C204,C206,
 C208), C214(C216,C218,C220,C222,C224), C228(C230,C232,C234,C236,C238),
 C256(C258,C260,C262,C264,C266), C284(C286,C288,C290,C292,C294), C296(C298,C300,
 C302,C304,C306), C312(C314,C316,C318,C320,C322), C332(C334,C336,C338,C340,
 C342), C358(C360,C362,C364,C366,C368), C372(C374,C376,C378,C380,C382), C223(C7,
 C225,C113,C227,C57), C231(C29,C233,C117,C235,C59), C121(C243,C61,C245,C123,
 C247), C263(C33,C265,C133,C267,C67), C135(C271,C17,C273,C137,C275), C285(C143,
 C287,C9,C289,C145), C73(C293,C147,C295,C37,C297), C159(C319,C5,C321,C161,C323),
  C325(C163,C327,C41,C329,C165), C175(C351,C11,C353,C177,C355), C179(C359,C45,
 C361,C181,C363), C365(C183,C367,C23,C369,C185), C371(C93,C373,C187,C375,C47),
 C193(C387,C97,C389,C195,C391), C105(C421,C211,C423,C53,C425)
7.f Idealised Me refined as rotating group:
 C118(H11A,H11B,H11C), C268(H26A,H26B,H26C), C344(H34D,H34E,H34F), C49(H49A,
 H49B,H49C)
;
_shelx_res_checksum              47329
_shelx_hkl_checksum              70311
_shelx_fab_checksum              1460
_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 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.644