A centrosymmetric polymorph of chloridotris(triphenylphosphine-κ<i>P</i>)copper(I) at 150K
Machado, Aline; Manzoni de Oliveira, Gelson N.; Fenner, Herton; Burrow, Robert A.; Acta Crystallographica Section C 64 (2008) m233–m236; doi:10.1107/S0108270108011232

data_2016628
_publ_section_title
;
 A centrosymmetric polymorph of
 chloridotris(triphenylphosphine-\k<i>P</i>)copper(I) at 150K
;
_journal_coeditor_code           BG3066
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m233
_journal_page_last               m236
_journal_paper_doi               10.1107/S0108270108011232
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu Cl (C18 H15)3]'
_chemical_formula_moiety         'C54 H45 Cl Cu P3'
_chemical_formula_sum            'C54 H45 Cl Cu P3'
_chemical_formula_weight         885.80
_chemical_name_systematic
;
chloridotris(triphenylphosphine-\kP)copper(I)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.496(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   43.253(3)
_cell_length_b                   9.9863(8)
_cell_length_c                   44.354(3)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      2.225
_cell_volume                     17570(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection
;
APEX2 (Bruker, 2006), COSMO (Bruker, 2006) and BIS (Bruker, 2006)
;
_computing_data_reduction
;
SAINT (Bruker, 2006), XPREP (Bruker, 2006) and SADABS (Bruker, 2006)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            191602
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.92671
_exptl_absorpt_correction_T_min  0.8438
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
[XPREP (Bruker, 2006) was used to perform the Gaussian numeric
absorption
correction based on the face-indexed crystal size; SADABS (Bruker,
2006) was
used to perform further processing]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.723
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         25640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0583P)^2^+28.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                17309
_reflns_number_total             25640
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3066.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2016628
_cod_database_fobs_code          2016628