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_4325149
_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         'C72 H114 Cu6 P4 Se6, C5'
_chemical_formula_sum            'C72 H114 Cu6 P4 Se6'
_chemical_formula_weight         2018.56
_chemical_name_common
tetrakis(triisopropylphosphino)-hexakis(copper-phenylselenolate)
_chemical_name_systematic
;
tris(\m~3~-phenylselenido)-tris(\m~2~-phenylselenido)
-tetrakis(triisopropylphosphine)-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                71.435(3)
_cell_angle_beta                 88.298(4)
_cell_angle_gamma                71.704(4)
_cell_formula_units_Z            4
_cell_length_a                   14.9225(7)
_cell_length_b                   24.3620(11)
_cell_length_c                   27.1525(12)
_cell_measurement_reflns_used    46771
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.41
_cell_volume                     8857.3(8)
_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    SIR92
_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      ' 294 frames, detector distance = 120 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  0.0991
_diffrn_reflns_av_sigmaI/netI    0.1308
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            81963
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.41
_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    3.989
_exptl_absorpt_correction_T_max  0.6111
_exptl_absorpt_correction_T_min  0.4063
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1672
_refine_ls_number_reflns         34780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                18618
_reflns_number_total             34780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102249g_si_002_10.cif
_cod_data_source_block           09xpentane
_cod_original_cell_volume        8857.3(7)
_cod_database_code               4325149