Novel Chloride-Centered Discrete CuI8 Cubic Clusters Containing Diselenophosphate Ligands. Syntheses and Structures of {Cu8(μ8-Cl)[Se2P(OR)2]6}(PF6) (R = Et, Pr,iPr)1
C. W. Liu; Chiu-Mine Hung; Bidyut Kumar Santra; Hsiu-Chih Chen; Hsueh; Ju-Chung Wang; Inorganic Chemistry 42 (2003) 3216–3220; doi:10.1021/ic020732n

data_4313621
_publ_section_title
;
 Novel Chloride-Centered Discrete CuI8 Cubic Clusters Containing
 Diselenophosphate Ligands. Syntheses and Structures of
 {Cu8(\m8-Cl)[Se2P(OR)2]6}(PF6) (R = Et, Pr,iPr)1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3216
_journal_page_last               3220
_journal_paper_doi               10.1021/ic020732n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24.5 H60.5 Cl2.5 Cu8 F6 O12 P7 Se12'
_chemical_formula_weight         2422.48
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   17.7054(17)
_cell_length_b                   17.7054(17)
_cell_length_c                   73.576(10)
_cell_measurement_temperature    293(2)
_cell_volume                     19975(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            19888
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    9.392
_exptl_absorpt_correction_T_max  0.95454
_exptl_absorpt_correction_T_min  0.24343
_exptl_absorpt_correction_type   empircial
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13740
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0310P)^2^+197.2490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                2913
_reflns_number_total             3902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020732n_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C24.50 H60.50 Cl2.50 Cu8 F6 O12 P7 Se12'
_cod_database_code               4313621