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_7709369
_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
'C66 H84 Ag12 F18 N6 O12 S6, 0.45[C4H8O], 0.55[C4H8O]'
_chemical_formula_sum            'C70 H92 Ag12 F18 N6 O13 S6'
_chemical_formula_weight         3054.29
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   20.625(5)
_cell_length_b                   20.625(5)
_cell_length_c                   40.283(9)
_cell_measurement_reflns_used    9254
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.32
_cell_volume                     14840(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            30715
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.322
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1249 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.7595.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7591
_refine_ls_number_restraints     706
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0356P)^2^+21.9868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5356
_reflns_number_total             7591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00016d2.cif
_cod_data_source_block           20210318hl_02_0m_a
_cod_depositor_comments
'Adding full bibliography for 7709363--7709369.cif.'
_cod_original_cell_volume        14840(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7709369
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.631
_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
 C17-C16A \\sim C17-C16B
 with sigma of 0.02
 C64-F6 \\sim C64-F6A
 with sigma of 0.02
 C64-F4 \\sim C64-F4A
 with sigma of 0.02
 C64-F5 \\sim C64-F5A
 with sigma of 0.02
 C66-F8 \\sim C66-F8A
 with sigma of 0.02
 C66-F9 \\sim C66-F9A
 with sigma of 0.02
 C66-F7 \\sim C66-F7A
 with sigma of 0.02
3. Rigid bond restraints
 C16A, C16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F9A, F8, F8A, F7, F7A, F9, F5, F6A, F6, F5A, F4, F4A
 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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(1)
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1)
 Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C51(H51A,H51B)
7.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C13(H13), C15(H15), C18(H18), C20(H20)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C16B(H16A,H16B,H16C), C21(H21A,H21B,
 H21C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C16A(H16D,H16E,H16F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 243 electrons were 
found in a volume of 1179\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.45[C4H8O], 0.55[C4H8O] per Unit Cell 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35728
_shelx_fab_checksum              15425
_olex2_submission_special_instructions 'No special instructions were received'