Concentration- and Solvation-Induced Reversible Structural Transformation and Assembly of Polynuclear Gold(I) Sulfido Complexes.
Yan, Liang-Liang; Yao, Liao-Yuan; Yam, Vivian Wing-Wah; Journal of the American Chemical Society 142 (2020) 11560–11568; doi:10.1021/jacs.0c04677

data_4135077
_publ_section_title
;
 Concentration- and Solvation-Induced Reversible Structural Transformation
 and Assembly of Polynuclear Gold(I) Sulfido Complexes.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11560
_journal_page_last               11568
_journal_paper_doi               10.1021/jacs.0c04677
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C100 H92 Au10 N4 P8 S4, 4(C H2 Cl2), 2(Cl)'
_chemical_formula_sum            'C104 H100 Au10 Cl10 N4 P8 S4'
_chemical_formula_weight         4106.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.927(3)
_cell_length_b                   11.430(2)
_cell_length_c                   32.513(7)
_cell_measurement_reflns_used    67437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      0.526
_cell_volume                     6213(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            19787
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         29.978
_diffrn_reflns_theta_min         2.072
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.904
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowgreen
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.679
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_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11239
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_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1194P)^2^+10.7145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10252
_reflns_number_total             11239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04677_si_002.cif
_cod_data_source_block           p2n_sq
_cod_depositor_comments
'Adding full bibliography for 4135076--4135079.cif.'
_cod_database_code               4135077
_shelx_shelxl_version_number     2018/3
_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.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C53(H53A,H53B)
2.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C38(H38), C32(H32), C16(H16), C7(H7), C31(H31), C29(H29), C13(H13),
 C44(H44), C28(H28), C11(H11), C6(H6), C20(H20), C37(H37), C4(H4), C9(H9),
 C30(H30), C22(H22), C10(H10), C25(H25), C26(H26), C23(H23), C36(H36), C43(H43),
  C3(H3), C34(H34), C41(H41), C12(H12), C42(H42), C35(H35), C50(H50), C46(H46),
 C5(H5), C24(H24), C19(H19), C18(H18), C17(H17), C47(H47), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              35749
_shelx_hkl_checksum              36275
_shelx_fab_checksum              39481
_olex2_submission_special_instructions 'No special instructions were received'