Silver(I) and Gold(I) Monothiocarbonate Complexes: Synthesis, Structure, Luminescence
Duminy, Welni; Pillay, Michael N.; van Zyl, Werner E.; Inorganics 10 (2022) 19–; doi:10.3390/inorganics10020019

data_1566562
_publ_section_title
;
 Silver(I) and Gold(I) Monothiocarbonate Complexes: Synthesis, Structure,
 Luminescence
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              19
_journal_paper_doi               10.3390/inorganics10020019
_journal_volume                  10
_journal_year                    2022
_chemical_formula_moiety         'C34 H38 Au2 O4 P2 S2'
_chemical_formula_sum            'C34 H38 Au2 O4 P2 S2'
_chemical_formula_weight         1030.63
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.882(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7462(9)
_cell_length_b                   39.197(3)
_cell_length_c                   15.6529(15)
_cell_measurement_reflns_used    8813
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.79
_cell_volume                     6858.7(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56967
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.039
_exptl_absorpt_coefficient_mu    8.798
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.5167.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.653
_refine_diff_density_min         -5.541
_refine_diff_density_rms         0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         15085
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+443.7759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11580
_reflns_number_total             15085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5gold_complex.cif
_cod_data_source_block           shelxt_a
_cod_database_code               1566562
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.444
_shelx_estimated_absorpt_t_min   0.227
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9985(4)
 0.0015(4)
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
 S2-C13
 1.81 with sigma of 0.02
 S4-C61
 1.81 with sigma of 0.02
 C57-O8
 1.2 with sigma of 0.02
 C57-S3
 1.78 with sigma of 0.02
 C65-O2
 1.2 with sigma of 0.02
 C65-S1
 1.78 with sigma of 0.02
 C65-O1
 1.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(O3) = Uanis(O4)
Uanis(S1) = Uanis(C65) = Uanis(O1) = Uanis(O2)
Uanis(C61) = Uanis(S4) = Uanis(O5) = Uanis(O6)
Uanis(O7) = Uanis(C57) = Uanis(O8) = Uanis(S3)
Uanis(C58) = Uanis(C60) = Uanis(C59)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C58(H58), C62(H62), C66(H66)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C43(H43A,H43B), C44(H44A,H44B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C)
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_shelx_res_checksum              59548
_shelx_hkl_checksum              50311
_olex2_submission_special_instructions 'No special instructions were received'