#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:52:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179397 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/94/4329456.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4329456
loop_
_publ_author_name
'Oliver Kluge'
'Harald Krautscheid'
_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         'C19 H18 Ga Se3, C12 H36 Cu P4, 3(C H4 O)'
_chemical_formula_sum            'C34 H66 Cu Ga O3 P4 Se3'
_chemical_formula_weight         1016.89
_chemical_name_systematic
;
 tetrakis(trimethylphosphine)-copper tris(Phenylselenido)-methyl-gallium
 methanol solvate
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            2
_cell_length_a                   13.3170(12)
_cell_length_b                   13.3170(12)
_cell_length_c                   15.8022(15)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      1.76
_cell_volume                     2427.0(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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      ' 70 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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6423
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.77
_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    3.402
_exptl_absorpt_correction_T_max  0.4294
_exptl_absorpt_correction_T_min  0.3599
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       coloum
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0257
_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/[σ²(Fo²)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0468
_reflns_number_gt                2839
_reflns_number_total             3833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300278v_si_002_04.cif
_cod_data_source_block           04
_cod_database_code               4329456
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.3333 0.6667 0.34510(2) 0.02213(10) Uani 1 3 d S
Ga1 Ga 0.6667 0.3333 0.13832(2) 0.02236(9) Uani 1 3 d S
Se1 Se 0.785669(19) 0.520274(18) 0.206100(13) 0.02843(6) Uani 1 1 d .
P1 P 0.3333 0.6667 0.48890(6) 0.0381(2) Uani 1 3 d S
P2 P 0.37866(5) 0.53313(5) 0.29671(3) 0.02597(11) Uani 1 1 d .
C1 C 0.6667 0.3333 0.0124(2) 0.0350(9) Uani 1 3 d S
H1A H 0.7098 0.2981 -0.0079 0.052 Uiso 0.33 1 calc PR
H1B H 0.7019 0.4117 -0.0079 0.052 Uiso 0.33 1 calc PR
H1C H 0.5883 0.2902 -0.0079 0.052 Uiso 0.33 1 calc PR
C2 C 0.75307(18) 0.62606(17) 0.14467(12) 0.0248(4) Uani 1 1 d .
C3 C 0.65576(19) 0.5898(2) 0.09264(14) 0.0326(5) Uani 1 1 d .
H3 H 0.6032 0.5111 0.0863 0.039 Uiso 1 1 calc R
C4 C 0.6372(2) 0.6714(2) 0.05015(15) 0.0399(6) Uani 1 1 d .
H4 H 0.5732 0.6463 0.0149 0.048 Uiso 1 1 calc R
C5 C 0.7131(3) 0.7886(2) 0.06004(16) 0.0464(7) Uani 1 1 d .
H5 H 0.7000 0.8425 0.0320 0.056 Uiso 1 1 calc R
C6 C 0.8086(3) 0.8253(2) 0.11198(17) 0.0469(6) Uani 1 1 d .
H6 H 0.8592 0.9042 0.1196 0.056 Uiso 1 1 calc R
C7 C 0.8302(2) 0.74473(19) 0.15339(15) 0.0359(5) Uani 1 1 d .
H7 H 0.8962 0.7705 0.1867 0.043 Uiso 1 1 calc R
C8 C 0.4512(3) 0.6564(4) 0.5403(2) 0.0833(12) Uani 1 1 d .
H8A H 0.5244 0.7175 0.5200 0.125 Uiso 1 1 calc R
H8B H 0.4442 0.5827 0.5274 0.125 Uiso 1 1 calc R
H8C H 0.4467 0.6636 0.6005 0.125 Uiso 1 1 calc R
C9 C 0.3068(3) 0.3906(2) 0.34820(19) 0.0514(7) Uani 1 1 d .
H9A H 0.2245 0.3547 0.3403 0.077 Uiso 1 1 calc R
H9B H 0.3243 0.3999 0.4076 0.077 Uiso 1 1 calc R
H9C H 0.3341 0.3427 0.3236 0.077 Uiso 1 1 calc R
C10 C 0.5320(2) 0.5753(2) 0.30627(16) 0.0402(6) Uani 1 1 d .
H10A H 0.5423 0.5120 0.2888 0.060 Uiso 1 1 calc R
H10B H 0.5562 0.5946 0.3641 0.060 Uiso 1 1 calc R
H10C H 0.5779 0.6414 0.2710 0.060 Uiso 1 1 calc R
C11 C 0.3499(2) 0.4929(2) 0.18464(16) 0.0441(6) Uani 1 1 d .
H11A H 0.3756 0.4392 0.1711 0.066 Uiso 1 1 calc R
H11B H 0.3909 0.5611 0.1503 0.066 Uiso 1 1 calc R
H11C H 0.2682 0.4575 0.1739 0.066 Uiso 1 1 calc R
C1L C 0.8447(3) 0.7822(3) 0.3814(2) 0.0725(10) Uani 1 1 d .
H1L H 0.7909 0.8035 0.3591 0.109 Uiso 1 1 calc R
H2L H 0.8233 0.7055 0.3626 0.109 Uiso 1 1 calc R
H3L H 0.9215 0.8360 0.3617 0.109 Uiso 1 1 calc R
O1L O 0.8426(3) 0.7843(3) 0.46888(17) 0.1139(11) Uani 1 1 d .
H4L H 0.8545 0.8480 0.4848 0.171 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.1740
0 1 0 0.1490
1 0 0 0.1560
-1 0 0 0.1850
1 -1 0 0.1450
-1 1 0 0.1510
0 0 -1 0.1540
0 0 1 0.1780
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Cu1 P2 109.622(17) . 3_565
P1 Cu1 P2 109.622(17) . 2_665
P2 Cu1 P2 109.320(17) 3_565 2_665
P1 Cu1 P2 109.622(17) . .
P2 Cu1 P2 109.320(17) 3_565 .
P2 Cu1 P2 109.320(17) 2_665 .
C1 Ga1 Se1 116.139(10) . 3_665
C1 Ga1 Se1 116.139(10) . .
Se1 Ga1 Se1 102.056(12) 3_665 .
C1 Ga1 Se1 116.139(10) . 2_655
Se1 Ga1 Se1 102.056(12) 3_665 2_655
Se1 Ga1 Se1 102.056(12) . 2_655
C2 Se1 Ga1 104.86(6) . .
C8 P1 C8 101.83(14) 2_665 3_565
C8 P1 C8 101.83(14) 2_665 .
C8 P1 C8 101.83(14) 3_565 .
C8 P1 Cu1 116.33(12) 2_665 .
C8 P1 Cu1 116.33(12) 3_565 .
C8 P1 Cu1 116.33(12) . .
C10 P2 C9 101.83(13) . .
C10 P2 C11 101.94(12) . .
C9 P2 C11 101.63(14) . .
C10 P2 Cu1 115.01(8) . .
C9 P2 Cu1 117.03(9) . .
C11 P2 Cu1 117.00(9) . .
C7 C2 C3 118.6(2) . .
C7 C2 Se1 118.01(16) . .
C3 C2 Se1 123.37(16) . .
C4 C3 C2 120.3(2) . .
C5 C4 C3 120.7(2) . .
C4 C5 C6 119.4(2) . .
C5 C6 C7 120.7(2) . .
C2 C7 C6 120.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 P1 2.2725(11) .
Cu1 P2 2.2770(6) 3_565
Cu1 P2 2.2770(6) 2_665
Cu1 P2 2.2770(6) .
Ga1 C1 1.990(4) .
Ga1 Se1 2.4313(3) 3_665
Ga1 Se1 2.4313(3) .
Ga1 Se1 2.4313(3) 2_655
Se1 C2 1.931(2) .
P1 C8 1.832(3) 2_665
P1 C8 1.832(3) 3_565
P1 C8 1.832(3) .
P2 C10 1.834(2) .
P2 C9 1.834(3) .
P2 C11 1.834(2) .
C2 C7 1.396(3) .
C2 C3 1.401(3) .
C3 C4 1.400(3) .
C4 C5 1.380(4) .
C5 C6 1.382(4) .
C6 C7 1.404(3) .
C1L O1L 1.384(4) .
