Tetrahalidocuprates(ii)—structure and EPR spectroscopy. Part 1: Tetrabromidocuprates(ii)
Farra, Ramzi; Thiel, Kerstin; Winter, Alette; Klamroth, Tillmann; Pöppl, Andreas; Kelling, Alexandra; Schilde, Uwe; Taubert, Andreas; Strauch, Peter; New Journal of Chemistry 35 (2011) 2793–; doi:10.1039/c1nj20271e

data_7052794
_publ_section_title
;
 Tetrahalidocuprates(ii)---structure and EPR spectroscopy. Part 1:
 Tetrabromidocuprates(ii)
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2793
_journal_paper_doi               10.1039/c1nj20271e
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         '2(C24 H20 P), Cu Br4'
_chemical_formula_sum            'C48 H40 Br4 Cu P2'
_chemical_formula_weight         1061.92
_chemical_melting_point          460.5(15)
_chemical_name_systematic
;
Bis(tetraphenylphosphonium)tetrabromocuprate(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 91.914(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8617(17)
_cell_length_b                   19.554(2)
_cell_length_c                   21.072(3)
_cell_measurement_reflns_used    8317
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      1.84
_cell_volume                     4473.0(11)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2005)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
180 frames, exposure time per frame = 5 min
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, 1.0 \%'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14297
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    4.165
_exptl_absorpt_correction_T_max  0.5282
_exptl_absorpt_correction_T_min  0.5199
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'X-RED (Stoe, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          1.1
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.763
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00048(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                2532
_reflns_number_total             3952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20271e.txt
_cod_data_source_block           farra6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '459-462' was changed to '460.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4473.1(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7052794