Molecular surface modification of silver chalcogenolate clusters.
Hu, Lei; Sheng, Ming-Ming; Qin, Shun-Shun; Shi, Hua-Tian; Strømme, Maria; Zhang, Qian-Feng; Xu, Chao; Dalton transactions (Cambridge, England : 2003) 51 (2022) 3241–3247; doi:10.1039/d2dt00016d

data_7709366
_publ_section_title
;
 Molecular surface modification of silver chalcogenolate clusters.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3241
_journal_page_last               3247
_journal_paper_doi               10.1039/d2dt00016d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C54 H148 Ag12 F18 N6 O18 S6'
_chemical_formula_sum            'C54 H148 Ag12 F18 N6 O18 S6'
_chemical_formula_weight         2998.58
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-24 deposited with the CCDC.	2022-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.8860(10)
_cell_length_b                   16.8860(10)
_cell_length_c                   28.799(3)
_cell_measurement_reflns_used    5220
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.567
_cell_measurement_theta_min      2.413
_cell_volume                     7111.5(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.412
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1061 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.8368.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_description       block
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1555
_refine_ls_number_restraints     469
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0592P)^2^+72.3842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1341
_reflns_number_total             1555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00016d2.cif
_cod_data_source_block           r-3m
_cod_depositor_comments
'Adding full bibliography for 7709363--7709369.cif.'
_cod_original_cell_volume        7111.4(12)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7709366
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.582
_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
 Ag1-O1 \\sim Ag1-O1A
 with sigma of 0.02
 O1-C7 \\sim O1A-C7A
 with sigma of 0.02
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 N1-C5 \\sim N1A-C5A
 with sigma of 0.02
 N1-C7 \\sim N1A-C7A
 with sigma of 0.02
 N1-C8 \\sim N1A-C8A
 with sigma of 0.04
 N1-C9 \\sim N1A-C9A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C5-C9 \\sim C5A-C9A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 Ag1-C7 \\sim Ag1-C7A
 with sigma of 0.04
 O1-N1 \\sim O1A-N1A
 with sigma of 0.04
 O1-C8 \\sim O1A-C8A
 with sigma of 0.04
 O2-C2 \\sim O2A-C2
 with sigma of 0.02
 F1-C1 \\sim F1A-C1
 with sigma of 0.02
 Ag2-O2 \\sim Ag2-O2A
 with sigma of 0.02
 F2-C1 \\sim F2A-C1
 with sigma of 0.02
3. Restrained planarity
 O1, N1, C5, C7, C8, C9, O1A, N1A, C5A, C7A, C8A, C9A
 with sigma of 0.001
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. 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
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O1, C8, C7, N1, C5, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5A, N1A, C7A, C9A, C8A, O1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1, F2, O2, C1, C2, F1A, F2A, O2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(F1A)=Sof(O2A)=1-FVAR(1)
 Sof(F2A)=0.5*(1-FVAR(2))
 Sof(F2)=0.5*FVAR(2)
 Sof(F1)=Sof(O2)=FVAR(1)
 Fixed Sof: O1(0.33333) N1(0.33333) C5(0.33333) H5A(0.66667) H5B(0.66667)
 H5C(0.66667) C7(0.33333) C8(0.33333) H8A(0.66667) H8B(0.66667) H8C(0.66667)
 C9(0.33333) H9A(0.66667) H9B(0.66667) H9C(0.66667) O1A(0.16667) N1A(0.16667)
 C5A(0.16667) H5AA(0.33333) H5AB(0.33333) H5AC(0.33333) C7A(0.16667)
 C8A(0.16667) H8AA(0.33333) H8AB(0.33333) H8AC(0.16667) C9A(0.16667)
 H9AA(0.33333) H9AB(0.33333) H9AC(0.33333)
8.a Riding coordinates:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C5A(H5AA,H5AB,H5AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC)
8.b Ternary CH refined with riding coordinates:
 C3(H3)
8.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              85003
_olex2_submission_special_instructions 'No special instructions were received'