Tetra- and hexanuclear string complexes of the coinage metals
Dahlen, Milena; Seifert, Tim P.; Lebedkin, Sergei; Gamer, Michael T.; Kappes, Manfred M.; Roesky, Peter W.; Chemical Communications  (2021) –; doi:10.1039/D1CC06034A

data_7129281
_publ_section_title
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 Tetra- and hexanuclear string complexes of the coinage metals
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06034A
_journal_year                    2021
_chemical_formula_moiety         'C41 H37 Au4 Cl3 N2 P2 S, 1.5(C4 H8 O)'
_chemical_formula_sum            'C47 H49 Au4 Cl3 N2 O1.5 P2 S'
_chemical_formula_weight         1654.10
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-10-26 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.695(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.7643(13)
_cell_length_b                   12.9640(4)
_cell_length_c                   31.9939(16)
_cell_measurement_reflns_used    37939
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.46
_cell_volume                     10842.1(9)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48035
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.206
_diffrn_reflns_theta_min         2.463
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.071
_exptl_absorpt_correction_T_max  0.5931
_exptl_absorpt_correction_T_min  0.0814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE XRED, XSHAPE & LANA'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       plate
_exptl_crystal_F_000             6160
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.037
_refine_diff_density_max         5.783
_refine_diff_density_min         -4.358
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         24014
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0803
_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^)+(0.1451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15146
_reflns_number_total             24014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06034a2.cif
_cod_data_source_block           md126
_cod_original_formula_sum        'C47 H49 Au4 Cl3 N2 O1.50 P2 S'
_cod_database_code               7129281
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.093
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C20, C22, C21, C23, C24, N2, P2, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim N2: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,
 H93B), C94(H94A,H94B)
4.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C1(H1),
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
  C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53744
_shelx_hkl_checksum              19667
_shelx_fab_checksum              604
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'