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_7709368
_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 H82 Ag12 F18 N6 O12 S6, 4(H2 O)'
_chemical_formula_sum            'C66 H90 Ag12 F18 N6 O16 S6'
_chemical_formula_weight         3052.23
_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             2022-01-23
_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                 98.596(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.933(3)
_cell_length_b                   28.031(8)
_cell_length_c                   15.304(4)
_cell_measurement_reflns_used    7018
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.81
_cell_measurement_theta_min      2.26
_cell_volume                     5062(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.256
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_description       block
_exptl_crystal_F_000             2956
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         8899
_refine_ls_number_restraints     876
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0627P)^2^+19.5220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5977
_reflns_number_total             8899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00016d2.cif
_cod_data_source_block           p21n
_cod_depositor_comments
'Adding full bibliography for 7709363--7709369.cif.'
_cod_original_cell_volume        5061(2)
_cod_database_code               7709368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.612
_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, All O(H,H) groups
2. Restrained distances
 C28-C29
 2.47 with sigma of 0.02
 N1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-N1
 1.39 with sigma of 0.01
 N1-C3 = C3-C5 = C5-N1 = C2-C4 = C4-C6 = C6-C2
 2.39 with sigma of 0.01
 F1-F2 = F2-F3 = F3-F1 = F4-F5 = F5-F6 = F6-F4 = F7-F8 = F8-F9 = F9-F7
 2.13 with sigma of 0.01
 C22-C24 \\sim C22A-C24A
 with sigma of 0.02
 C21-C24 \\sim C21A-C24A
 with sigma of 0.04
 C23-C24 \\sim C23A-C24A
 with sigma of 0.04
 F7-C36 \\sim F7A-C36
 with sigma of 0.02
 F5-C26 \\sim F5A-C26
 with sigma of 0.02
 F9-C36 \\sim F9A-C36
 with sigma of 0.02
 F4-C26 \\sim F4A-C26
 with sigma of 0.02
 F8-C36 \\sim F8A-C36
 with sigma of 0.02
 F6-C26 \\sim F6A-C26
 with sigma of 0.02
 C27-C30 \\sim C27A-C30A
 with sigma of 0.02
 S7-C27 \\sim S7-C27A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 S7-C30 \\sim S7-C30A
 with sigma of 0.04
 C27-C28 \\sim C27A-C28A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.02
 S8-C21 \\sim S8-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 S8-C22 \\sim S8-C22A
 with sigma of 0.04
 F1-C20 \\sim F1A-C20
 with sigma of 0.02
 F3-C20 \\sim F3A-C20
 with sigma of 0.02
 F2-C20 \\sim F2A-C20
 with sigma of 0.02
3. Restrained planarity
 N1, C2, C3, C4, C5, C6
 with sigma of 0.1
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
C2 \\sim C10 \\sim C9 \\sim C4 \\sim C6 \\sim C3 \\sim C11 \\sim C8 \\sim C5
\\sim C12 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20
\\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28
\\sim C29 \\sim C31 \\sim C32 \\sim C33 \\sim C36 \\sim C30 \\sim C34 \\sim C35
\\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C21A \\sim C22A \\sim C23A
\\sim C24A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
6. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(4)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(4)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(5)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(5)
7.a Free rotating group:
 O7(H7A,H7B), O6(H6A,H6B)
7.b Ternary CH refined with riding coordinates:
 C22(H22), C32(H32), C30(H30), C30A(H30A), C22A(H22A)
7.c Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C27(H27A,H27B), C31(H31A,H31B), C27A(H27C,H27D), C21A(H21C,
 H21D)
7.d Me refined with riding coordinates:
 C24A(H24D,H24E,H24F)
7.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C9(H9), C4(H4), C6(H6), C3(H3), C11(H11), C5(H5), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
7.f Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F), C23A(H23D,H23E,H23F)
;
_shelx_res_checksum              60366
_olex2_submission_special_instructions 'No special instructions were received'