Trialkylphosphine-Stabilized Copper(I) Phenylchalcogenolate Complexes - Crystal Structures and Copper-Chalcogenolate Bonding
Oliver Kluge; Katharina Grummt; Ralf Biedermann; Harald Krautscheid; Inorganic Chemistry 50 (2011) 4742–4752; doi:10.1021/ic102249g

data_4325144
_publ_section_title
;
 Trialkylphosphine-Stabilized Copper(I) Phenylchalcogenolate Complexes -
 Crystal Structures and Copper-Chalcogenolate Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4742
_journal_page_last               4752
_journal_paper_doi               10.1021/ic102249g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C66 H105 Cu6 P5 Se6, C2.5'
_chemical_formula_sum            'C68.5 H105 Cu6 P5 Se6'
_chemical_formula_weight         1938.38
_chemical_name_common
pentakis(triethylphosphino)-hexakis(copper-phenylselenolate)
_chemical_name_systematic
;
pentakis(\m~3~-phenylselenido)-(\m~2~-phenylselenido)-
pentakis(triethylphosphine)-hexa-copper pentane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.005(3)
_cell_angle_beta                 103.197(3)
_cell_angle_gamma                114.376(3)
_cell_formula_units_Z            2
_cell_length_a                   13.6847(6)
_cell_length_b                   14.9342(6)
_cell_length_c                   22.3746(10)
_cell_measurement_reflns_used    53856
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.70
_cell_volume                     4011.8(3)
_computing_cell_refinement       'stoe x-area'
_computing_data_collection       'stoe x-area'
_computing_data_reduction        'stoe x-red'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    sir-92
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            stoe
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 322 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'stoe ipds 2t'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'mo k\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35350
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.70
_diffrn_source
'sealed x-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.419
_exptl_absorpt_correction_T_max  0.3297
_exptl_absorpt_correction_T_min  0.2171
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'stoe x-red'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             1929
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         15758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                12943
_reflns_number_total             15758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102249g_si_002_05.cif
_cod_data_source_block           05
_cod_original_formula_sum        'C68.50 H105 Cu6 P5 Se6'
_cod_database_code               4325144