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_4135076
_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         'C150 H138 Au12 N6 P12 S4, 4(Cl), 2(C H4 O)'
_chemical_formula_sum            'C152 H146 Au12 Cl4 N6 O2 P12 S4'
_chemical_formula_weight         5094.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                103.56(3)
_cell_angle_beta                 110.52(3)
_cell_angle_gamma                107.89(3)
_cell_formula_units_Z            1
_cell_length_a                   16.755(3)
_cell_length_b                   16.845(3)
_cell_length_c                   18.531(4)
_cell_measurement_reflns_used    93523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      0.474
_cell_volume                     4304(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.057
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_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_number            14855
_diffrn_reflns_point_group_measured_fraction_full 0.937
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_diffrn_reflns_theta_full        29.730
_diffrn_reflns_theta_max         30.009
_diffrn_reflns_theta_min         2.562
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    15.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowgreen
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.562
_refine_diff_density_min         -2.019
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+11.8072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                14660
_reflns_number_total             14855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04677_si_003.cif
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_cod_depositor_comments
'Adding full bibliography for 4135076--4135079.cif.'
_cod_original_cell_volume        4304.2(19)
_cod_database_code               4135076
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Rigid bond restraints
 C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C56) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C30(H30), C29(H29), C28(H28), C25(H25), C24(H24),
 C23(H23), C22(H22), C21(H21), C38(H38), C37(H37), C36(H36), C35(H35), C34(H34),
  C68(H68), C67(H67), C66(H66), C65(H65), C64(H64), C71(H71), C19(H19),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C44(H44), C43(H43), C42(H42),
  C41(H41), C40(H40), C57(H57), C56(H56), C55(H55), C54(H54), C53(H53),
 C72(H72), C15(H15), C74(H74), C75(H75), C73(H73), C16(H16), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C7(H7), C6(H6), C5(H5), C4(H4), C3(H3),
 C18(H18), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17)
4.b Fitted hexagon refined as free rotating group:
 C27(C32,C31,C30,C29,C28), C20(C25,C24,C23,C22,C21), C33(C38,C37,C36,C35,C34),
 C69(C68,C67,C66,C65,C64), C58(C59,C60,C61,C62,C63), C39(C44,C43,C42,C41,C40),
 C52(C57,C56,C55,C54,C53), C45(C46,C47,C48,C49,C50), C2(C7,C6,C5,C4,C3), C8(C9,
 C10,C11,C12,C13)
4.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C77(H77A,H77B,H77C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              75017
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_olex2_submission_special_instructions 'No special instructions were received'