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_7709367
_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         'C72 H100 Ag12 F18 N6 O14 S6'
_chemical_formula_sum            'C72 H100 Ag12 F18 N6 O14 S6'
_chemical_formula_weight         3102.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-24
_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                 90.30
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.995(5)
_cell_length_b                   17.314(6)
_cell_length_c                   18.391(6)
_cell_measurement_reflns_used    8156
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.2625
_cell_measurement_theta_min      2.3525
_cell_volume                     5093(3)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27240
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.353
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.094
_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     758
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     1066
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0359P)^2^+9.5775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6951
_reflns_number_total             9430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00016d2.cif
_cod_data_source_block           p21
_cod_depositor_comments
'Adding full bibliography for 7709363--7709369.cif.'
_cod_database_code               7709367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C9-C10
 1.52 with sigma of 0.001
 Ag5-N2 \\sim Ag5-N2A
 with sigma of 0.02
 N2-C20 \\sim N2A-C20A
 with sigma of 0.02
 N2-C24 \\sim N2A-C24A
 with sigma of 0.02
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C20-C24 \\sim C20A-C24A
 with sigma of 0.04
 Ag5-C20 \\sim Ag5-C20A
 with sigma of 0.04
 Ag5-C24 \\sim Ag5-C24A
 with sigma of 0.04
 N2-C19 \\sim N2A-C19A
 with sigma of 0.04
 N2-C21 \\sim N2A-C21A
 with sigma of 0.04
 N2-C23 \\sim N2A-C23A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12
 with sigma of 0.02
 F3-C32 \\sim F3A-C32
 with sigma of 0.02
 F1-C32 \\sim F1A-C32
 with sigma of 0.02
 F2-C32 \\sim F2A-C32
 with sigma of 0.02
 F6-C34 \\sim F6A-C34
 with sigma of 0.02
 F4-C34 \\sim F4A-C34
 with sigma of 0.02
 F5-C34 \\sim F5A-C34
 with sigma of 0.02
3. 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
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
5. Rigid body (RIGU) restrains
 N2, C18, C19, C20, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2A, C20A, C21A, C22A, C23A, C24A, C18A, C19A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C12, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(N2A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(N2)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=
 Sof(H24)=FVAR(1)
 Sof(H12C)=Sof(H12D)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(H12A)=Sof(H12B)=FVAR(2)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(5)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(5)
7.a Free rotating group:
 O7(H7A,H7B)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C26(H26), C29(H29)
7.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C12(H12C,H12D), C19(H19A,H19B), C19A(H19C,H19D)
7.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C17(H17),
 C21(H21), C22(H22), C23(H23), C24(H24), C21A(H21A), C22A(H22A), C23A(H23A),
 C24A(H24A)
7.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C18A(H18D,H18E,H18F), C11A(H11D,H11E,H11F)
;
_shelx_res_checksum              82000
_olex2_submission_special_instructions 'No special instructions were received'