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_2008139
_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~Cl~4~(C~18~H~15~O~3~P)~4~]'
_chemical_formula_moiety         'C72 H60 Cl4 Cu4 O12 P4'
_chemical_formula_structural     '[Cu Cl (P (O C6 H5)3)]4'
_chemical_formula_sum            'C72 H60 Cl4 Cu4 O12 P4'
_chemical_formula_weight         1637.15
_chemical_melting_point          558
_chemical_name_common
'cuprous chloride triphenylphosphite cubane tetramer'
_chemical_name_systematic
;
tetra-\m~3~-chloro-tetrakis[(triphenyl phosphite-P)copper(I)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.4340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6643(2)
_cell_length_b                   22.6409(3)
_cell_length_c                   22.66450(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1.9
_cell_volume                     7179.23(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.066
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56312
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        -0.6
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type
'empirical (SADABS; Blessing, 1995; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.619
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.100
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0214P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                7760
_reflns_number_total             12671
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1019.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0214P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0214P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7179.20(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008139