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_4329470
_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         'C55 H78 Cu4 Ga P3 Te6'
_chemical_formula_sum            'C55 H78 Cu4 Ga P3 Te6'
_chemical_formula_weight         1921.56
_chemical_name_systematic
;
tris(\m~3~-phenyltellurido)-tris(\m~2~-phenyltellurido)
-tris(triethylphosphine)-methyl-tetra-copper-gallium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 111.598(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.2628(8)
_cell_length_b                   13.1277(5)
_cell_length_c                   23.5164(9)
_cell_measurement_reflns_used    40715
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      1.77
_cell_volume                     6677.4(4)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      ' 225 frames, detector distance = 110 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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46762
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         1.75
_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    4.325
_exptl_absorpt_correction_T_max  0.5959
_exptl_absorpt_correction_T_min  0.2788
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         13124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0395
_reflns_number_gt                9888
_reflns_number_total             13124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300278v_si_002_18.cif
_cod_data_source_block           18
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329470