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_4135078
_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         'C104 H100 Au10 N4 P8 S4, 2(Cl)'
_chemical_formula_sum            'C104 H100 Au10 Cl2 N4 P8 S4'
_chemical_formula_weight         3822.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.431(5)
_cell_length_b                   32.431(5)
_cell_length_c                   24.806(5)
_cell_measurement_reflns_used    302120
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      0.474
_cell_volume                     26090(8)
_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 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82657
_diffrn_reflns_av_R_equivalents  0.1407
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            88367
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        29.732
_diffrn_reflns_theta_max         30.166
_diffrn_reflns_theta_min         1.745
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    16.820
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowgreen
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_description       block
_exptl_crystal_F_000             14080
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.976
_refine_diff_density_min         -4.273
_refine_diff_density_rms         0.330
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.539(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         24247
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1358P)^2^+104.2959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                23960
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04677_si_005.cif
_cod_data_source_block           cc_sq
_cod_depositor_comments
'Adding full bibliography for 4135076--4135079.cif.'
_cod_original_cell_volume        26090(10)
_cod_database_code               4135078
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.461(9)
 0.539(9)
2. 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
3. Restrained distances
 N1-C1
 1.5 with sigma of 0.02
 C1-C2
 1.515 with sigma of 0.02
 C27-N2
 1.5 with sigma of 0.02
 C27-C28
 1.515 with sigma of 0.02
 C53-N3
 1.5 with sigma of 0.02
 C53-C54
 1.515 with sigma of 0.02
 C79-N4
 1.5 with sigma of 0.02
 C80-C79
 1.515 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C95) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C80) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C28) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C27) \\sim Ueq, Uanis(C97) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(C88) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C104) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C96) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C97) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cl3(0.5)
6.a Riding coordinates:
 C2(H2A,H2B,H2C)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C1(H1A,H1B), C53(H53A,H53B), C79(H79A,H79B)
6.c Aromatic/amide H refined with riding coordinates:
 C72(H72), C71(H71), C70(H70), C69(H69), C68(H68), C66(H66), C65(H65),
 C64(H64), C63(H63), C62(H62), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
  C60(H60), C59(H59), C58(H58), C57(H57), C56(H56), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C20(H20), C19(H19), C18(H18), C17(H17), C16(H16),
  C104(H104), C103(H103), C102(H102), C101(H101), C100(H100), C92(H92),
 C91(H91), C90(H90), C89(H89), C88(H88), C36(H36), C37(H37), C38(H38), C39(H39),
  C40(H40), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C10(H10),
 C11(H11), C12(H12), C13(H13), C14(H14), C86(H86), C85(H85), C84(H84), C83(H83),
  C82(H82), C98(H98), C97(H97), C96(H96), C95(H95), C94(H94), C26(H26),
 C25(H25), C24(H24), C23(H23), C22(H22), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C8(H8), C7(H7), C6(H6), C5(H5), C4(H4)
6.d Fitted hexagon refined as free rotating group:
 C67(C72,C71,C70,C69,C68), C61(C66,C65,C64,C63,C62), C73(C74,C75,C76,C77,C78),
 C55(C60,C59,C58,C57,C56), C41(C42,C43,C44,C45,C46), C15(C20,C19,C18,C17,C16),
 C99(C104,C103,C102,C101,C100), C87(C92,C91,C90,C89,C88), C35(C36,C37,C38,C39,
 C40), C47(C48,C49,C50,C51,C52), C9(C10,C11,C12,C13,C14), C81(C86,C85,C84,C83,
 C82), C93(C98,C97,C96,C95,C94), C21(C26,C25,C24,C23,C22), C29(C30,C31,C32,C33,
 C34), C3(C8,C7,C6,C5,C4)
6.e Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C28(H28A,H28B,H28C), C80(H80A,H80B,H80C)
;
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_olex2_submission_special_instructions 'No special instructions were received'