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_7052796
_publ_section_title
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 Tetrahalidocuprates(ii)---structure and EPR spectroscopy. Part 1:
 Tetrabromidocuprates(ii)
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_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(C25 H22 P), Cu Br4, 2(C H Cl3)'
_chemical_formula_sum            'C52 H46 Br4 Cl6 Cu P2'
_chemical_formula_weight         1328.71
_chemical_melting_point          414.5(5)
_chemical_name_systematic
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Bis(benzyltriphenylphosphonium)tetrabromocuprate(II) chloroform solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.612(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6843(11)
_cell_length_b                   10.2238(6)
_cell_length_c                   28.5236(15)
_cell_measurement_reflns_used    24443
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      1.33
_cell_volume                     5446.6(5)
_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 = 3 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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34342
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_T_max  0.3129
_exptl_absorpt_correction_T_min  0.2976
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'X-RED (Stoe, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00077(5)
_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    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                6886
_reflns_number_total             9574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20271e.txt
_cod_data_source_block           thiel2
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '414-415' was changed to '414.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7052796