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_4135079
_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         'C144 H126 Au12 N6 P12 S4, 4(Cl), 2(C H4 O)'
_chemical_formula_sum            'C146 H134 Au12 Cl4 N6 O2 P12 S4'
_chemical_formula_weight         5009.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 105.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.539(3)
_cell_length_b                   33.236(7)
_cell_length_c                   14.185(3)
_cell_measurement_reflns_used    154443
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      0.406
_cell_volume                     7501(3)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42526
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.177
_diffrn_reflns_theta_min         1.931
_exptl_absorpt_coefficient_mu    11.991
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowgreen
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.831
_refine_diff_density_min         -14.627
_refine_diff_density_rms         0.915
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         23696
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_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1201P)^2^+55.2518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.1859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23589
_reflns_number_total             23696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04677_si_004.cif
_cod_data_source_block           p1_sq
_cod_depositor_comments
'Adding full bibliography for 4135076--4135079.cif.'
_cod_database_code               4135079
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C73-O1
 1.41 with sigma of 0.02
3.a Riding coordinates:
 N2(H2), N1(H1), N3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C29(H29), C15(H15), C4(H4), C69(H69), C26(H26), C68(H68), C33(H33),
 C17(H17), C13(H13), C16(H16), C19(H19), C49(H49), C27(H27), C3(H3A), C71(H71),
 C41(H41), C8(H8), C65(H65), C28(H28), C25(H25), C10(H10), C34(H34), C35(H35),
 C63(H63), C21(H21), C51(H51), C52(H52), C20(H20), C53(H53), C44(H44), C9(H9),
 C46(H46), C62(H62), C31(H31), C45(H45), C5(H5), C59(H59), C22(H22), C11(H11),
 C2(H2A), C7(H7), C61(H61), C55(H55), C38(H38), C64(H64), C67(H67), C43(H43),
 C57(H57), C50(H50), C32(H32), C37(H37), C1(H1A), C40(H40), C58(H58), C70(H70),
 C23(H23), C56(H56), C39(H39), C47(H47)
3.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1B)
;
_shelx_res_checksum              51526
_shelx_hkl_checksum              20961
_shelx_fab_checksum              47921
_olex2_submission_special_instructions 'No special instructions were received'