PCU-type copper-rich open-framework chalcogenides: pushing up the length limit of the connection mode and the first mixed-metal [Cu7GeSe13] cluster
Luo, Min; Hu, Dandan; Yang, Huajun; Li, Dongsheng; Wu, Tao; Inorganic Chemistry Frontiers 4 (2017) 387–; doi:10.1039/C6QI00482B

data_4349606
_publ_section_title
;
 PCU-type copper-rich open-framework chalcogenides: pushing up the length
 limit of the connection mode and the first mixed-metal [Cu7GeSe13]
 cluster
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              387
_journal_paper_doi               10.1039/C6QI00482B
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_formula_sum            'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_formula_weight         6855.29
_chemical_melting_point          'C12 H Cl3 Cu32 Ge24 N12 Ni6 S72'
_chemical_name_common            1c
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-10-17 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.7454(6)
_cell_length_b                   22.7454(6)
_cell_length_c                   22.7454(6)
_cell_measurement_reflns_used    9459
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.53
_cell_volume                     11767.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29719
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    6.986
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8976
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                1382
_reflns_number_total             1870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00482b2.cif
_cod_data_source_block           a_sq_d_sq_d
_cod_database_code               4349606