Trialkylphosphine-Stabilized Copper(I) Gallium(III) Phenylchalcogenolate Complexes: Crystal Structures and Generation of Ternary Semiconductors by Thermolysis
Oliver Kluge; Harald Krautscheid; Inorganic Chemistry 51 (2012) 6655–6666; doi:10.1021/ic300278v

data_4329467
_publ_section_title
;
 Trialkylphosphine-Stabilized Copper(I) Gallium(III) Phenylchalcogenolate
 Complexes: Crystal Structures and Generation of Ternary Semiconductors by
 Thermolysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6655
_journal_page_last               6666
_journal_paper_doi               10.1021/ic300278v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C46 H60 Cu4 Ga P3 Se6, 1.5 (C4 O), 0.5(C5)'
_chemical_formula_sum            'C54.5 H60 Cu4 Ga O1.5 P3 Se6'
_chemical_formula_weight         1629.57
_chemical_name_systematic
;
tris(\m~3~-phenylselenido)-tris(\m~2~-phenylselenido)-tris(trimethylphosphine)
-methyl-tetra-copper-gallium pentane solvate tetrahydrofuran solvate
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   16.3325(7)
_cell_length_b                   16.3325(7)
_cell_length_c                   27.1616(15)
_cell_measurement_reflns_used    22345
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.44
_cell_volume                     6274.7(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      ' 165 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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27174
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.44
_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    5.350
_exptl_absorpt_correction_T_max  0.5033
_exptl_absorpt_correction_T_min  0.3046
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3577
_reflns_number_total             4088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300278v_si_002_15.cif
_cod_data_source_block           15
_cod_original_formula_sum        'C54.50 H60 Cu4 Ga O1.50 P3 Se6'
_cod_database_code               4329467