Cubane tetrameric complexes of copper(I) chloride and bromide with triphenyl phosphite
Pike, Robert D.; Starnes, William H. Jr; Carpenter, Gene B.; Acta Crystallographica Section C 55 (1999) 162–165; doi:10.1107/S0108270198012451

data_2008138
_publ_section_title
;
 Cubane tetrameric complexes of copper(I) chloride and bromide with
 triphenyl phosphite
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              162
_journal_page_last               165
_journal_paper_doi               10.1107/S0108270198012451
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Cu~4~Br~4~(C~18~H~15~O~3~P)~4~]'
_chemical_formula_moiety         'C72 H60 Br4 Cu4 O12 P4'
_chemical_formula_structural     '[Cu Br (P (O C6 H5)3)]4'
_chemical_formula_sum            'C72 H60 Br4 Cu4 O12 P4'
_chemical_formula_weight         1814.96
_chemical_melting_point          524.15
_chemical_name_common
'cuprous bromide triphenylphosphite cubane tetramer'
_chemical_name_systematic
;
tetra-\m~3~-bromo-tetrakis[(triphenyl phosphite-P)copper(I)]
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.16450(10)
_cell_length_b                   21.16450(10)
_cell_length_c                   28.93780(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      1.70
_cell_volume                     11225.67(8)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
'SAINT and SADABS (Blessing, 1995; Sheldrick, 1996)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.330
_diffrn_measured_fraction_theta_max 0.330
_diffrn_measurement_device_type  'Siemens P4 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18958
_diffrn_reflns_theta_full        24.89
_diffrn_reflns_theta_max         24.89
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.10
_exptl_absorpt_coefficient_mu    3.400
_exptl_absorpt_correction_T_max  0.507
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_type
'empirical (SADABS; Blessing, 1995; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.080
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0808P)^2^+3.6171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.147
_refine_ls_wR_factor_ref         0.147
_reflns_number_gt                3021
_reflns_number_total             4304
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1019.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '251 C' was changed to '524.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '251 C' was changed to '524.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        11225.66(8)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               2008138