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_7709363
_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         'C78 H108 Ag12 F18 N6 O12 S6'
_chemical_formula_sum            'C78 H108 Ag12 F18 N6 O12 S6'
_chemical_formula_weight         3150.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_formula_units_Z            4
_cell_length_a                   29.633(14)
_cell_length_b                   18.580(9)
_cell_length_c                   19.796(10)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.1098
_cell_measurement_theta_min      2.4217
_cell_volume                     10899(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.448
_diffrn_reflns_theta_min         2.422
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       block
_exptl_crystal_F_000             6144
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6288
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+15.0237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4828
_reflns_number_total             6288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00016d2.cif
_cod_data_source_block           cmca
_cod_depositor_comments
'Adding full bibliography for 7709363--7709369.cif.'
_cod_original_cell_volume        10900(9)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7709363
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.620
_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
 F3-C5 \\sim F3A-C5A
 with sigma of 0.02
 F5-C6 \\sim F5A-C6
 with sigma of 0.04
 F4-C6 \\sim F4A-C6
 with sigma of 0.04
 F4-C5 \\sim F4A-C5A
 with sigma of 0.02
 F5-C5 \\sim F5A-C5A
 with sigma of 0.02
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6
 with sigma of 0.02
 F3-F4 \\sim F3A-F4A
 with sigma of 0.04
 F3-F5 \\sim F3A-F5A
 with sigma of 0.04
 F3-C6 \\sim F3A-C6
 with sigma of 0.04
 F1-C14 \\sim F1A-C14
 with sigma of 0.02
 F2-C14 \\sim F2A-C14
 with sigma of 0.02
3. Rigid bond restraints
 F1, F1A, F2A, F2, C22, F5A, F3, F4, F3A, F4A, F5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F4A \\sim F4 \\sim F3A \\sim F3 \\sim F5A \\sim F5 \\sim F1A \\sim F1 \\sim F2
\\sim F2A \\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
5. Rigid body (RIGU) restrains
 O3, O4, C6, F3A, F4A, F5A, C5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3, F4, F5, O3, O4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3, F4, F5, O3, O4, C5, C6, F3A, F4A, F5A, C5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(C5A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(C5)=FVAR(1)
 Sof(F2A)=1-FVAR(2)
 Sof(F1A)=0.5*(1-FVAR(3))
 Sof(F1)=0.5*FVAR(3)
 Sof(F2)=FVAR(2)
 Fixed Sof: H8A(0.5) H8B(0.5) H8C(0.5)
7.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C16(H16), C17(H17), C20(H20)
7.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              74005
_olex2_submission_special_instructions 'No special instructions were received'