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_4349603
_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_sum            'C4.5 H0 Cu5.25 Ge3 N3 Se9.75'
_chemical_formula_weight         1417.29
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-03-28 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            8
_cell_length_a                   13.2540(6)
_cell_length_b                   13.2540(6)
_cell_length_c                   30.366(3)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      3.07
_cell_volume                     4619.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20220
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    23.944
_exptl_absorpt_correction_T_max  0.1237
_exptl_absorpt_correction_T_min  0.1237
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             5022
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1712
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0005P)^2^+54.6222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0363
_refine_ls_wR_factor_ref         0.0370
_reflns_number_gt                1706
_reflns_number_total             1712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00482b2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Hexagonal' was changed to
'hexagonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      R3c
_cod_original_formula_sum        'C4.50 H0 Cu5.25 Ge3 N3 Se9.75'
_cod_database_code               4349603