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_7232619
_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         'C84 H68 Au Br1.74 Cl0.26 O4 P3 S4'
_chemical_formula_sum            'C84 H68 Au Br1.74 Cl0.26 O4 P3 S4'
_chemical_formula_weight         1707.84
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.464(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.636(3)
_cell_length_b                   14.5547(19)
_cell_length_c                   27.872(4)
_cell_measurement_reflns_used    13100
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.01
_cell_volume                     7553.1(19)
_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 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            56560
_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         27.487
_diffrn_reflns_theta_min         3.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.111
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3429.28
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF/diethyl ether'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.89
_refine_diff_density_min         -1.92
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     887
_refine_ls_number_reflns         17275
_refine_ls_number_restraints     792
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0545P)^2^+6.0439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11084
_reflns_number_total             17275
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9ce00364a2.cif
_cod_data_source_block           SY70428_20170510
_cod_depositor_comments
'Adding full bibliography for 7232619--7232622.cif.'
_cod_original_cell_volume        7553.0(17)
_cod_database_code               7232619
_shelx_res_checksum              61069