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_7232620
_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         'C44 H44 Au O6 P S4'
_chemical_formula_sum            'C44 H44 Au O6 P S4'
_chemical_formula_weight         1025.01
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.0000
_cell_angle_beta                 110.8721(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.0138(4)
_cell_length_b                   7.3818(4)
_cell_length_c                   25.0096(7)
_cell_measurement_reflns_used    17586
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.19
_cell_measurement_theta_min      2.81
_cell_volume                     4142.4(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_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      100
_diffrn_measured_fraction_theta_full 0.829
_diffrn_measured_fraction_theta_max 0.652
_diffrn_measurement_device_type  'Rigaku imaging plate system'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68889
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.829
_diffrn_reflns_Laue_measured_fraction_max 0.652
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17508
_diffrn_reflns_point_group_measured_fraction_full 0.829
_diffrn_reflns_point_group_measured_fraction_max 0.652
_diffrn_reflns_theta_full        24.414
_diffrn_reflns_theta_max         37.169
_diffrn_reflns_theta_min         1.689
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.28
_refine_diff_density_min         -2.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5038
_reflns_number_total             7619
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9ce00364a2.cif
_cod_data_source_block           process_1
_cod_depositor_comments
'Adding full bibliography for 7232619--7232622.cif.'
_cod_database_code               7232620
_shelx_res_checksum              25821