Construction of three-dimensional anionic molecular frameworks based on hydrogen-bonded metal dithiolene complexes and the crystal solvent effect
Yokomori, So; Ueda, Akira; Higashino, Toshiki; Kumai, Reiji; Murakami, Youichi; Mori, Hatsumi; CrystEngComm 21 (2019) 2940–; doi:10.1039/C9CE00364A

data_7232622
_publ_section_title
;
 Construction of three-dimensional anionic molecular frameworks based on
 hydrogen-bonded metal dithiolene complexes and the crystal solvent effect
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2940
_journal_paper_doi               10.1039/C9CE00364A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C40 H38 Au O5 P S4'
_chemical_formula_sum            'C40 H38 Au O5 P S4'
_chemical_formula_weight         954.92
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-04-01 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                65.051(8)
_cell_angle_beta                 80.380(13)
_cell_angle_gamma                79.305(14)
_cell_formula_units_Z            2
_cell_length_a                   10.783(3)
_cell_length_b                   14.172(4)
_cell_length_c                   16.481(5)
_cell_measurement_reflns_used    5326
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.11
_cell_volume                     2232.7(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16221
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.566
_exptl_absorpt_correction_T_max  0.490
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             952.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/diethyl ether'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.01
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8926
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0474P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6222
_reflns_number_total             8926
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9ce00364a2.cif
_cod_data_source_block           SY70720_4_20170722
_cod_depositor_comments
'Adding full bibliography for 7232619--7232622.cif.'
_cod_original_cell_volume        2232.8(11)
_cod_database_code               7232622
_shelx_res_checksum              16198
_shelx_fab_checksum              27282