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#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335589.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_4335589
loop_
_publ_author_name
'Yu-Kun Chen'
'Mei-Chun Chen'
'Liu-Jiang Zhou'
'Ling Chen'
'Li-Ming Wu'
_publ_section_title
;
 Syntheses, Structures, and Nonlinear Optical Properties of Quaternary
 Chalcogenides: Pb4Ga4GeQ12 (Q = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8334
_journal_page_last               8341
_journal_paper_doi               10.1021/ic400995z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Ga4 Ge Pb4 S12'
_chemical_formula_weight         1564.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6726(15)
_cell_length_b                   12.6726(15)
_cell_length_c                   6.1281(14)
_cell_measurement_reflns_used    2262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4663
_cell_measurement_theta_min      2.2729
_cell_volume                     984.1(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7490
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    42.222
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5617
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            lawnblue
_exptl_crystal_density_diffrn    5.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.335
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_coef       0.00069(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1120
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+32.5200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                1026
_reflns_number_total             1120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400995z_si_002.cif
_cod_data_source_block           a
_cod_database_code               4335589
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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
Pb Pb 0.68605(7) 0.98940(6) 0.58822(15) 0.0321(3) Uani 1 1 d U
Ge Ge 1.0000 1.0000 1.0000 0.0165(8) Uani 1 4 d S
Ga Ga 0.85183(15) 0.76449(15) 0.9509(4) 0.0153(5) Uani 1 1 d .
S1 S 0.9824(4) 0.6401(3) 0.9641(8) 0.0173(10) Uani 1 1 d .
S2 S 0.9043(4) 0.9067(4) 0.7612(8) 0.0162(10) Uani 1 1 d .
S3 S 0.7030(3) 0.6912(4) 0.8044(8) 0.0175(10) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb 0.0408(5) 0.0252(4) 0.0303(5) -0.0037(4) 0.0001(4) 0.0030(3)
Ge 0.0167(11) 0.0167(11) 0.016(2) 0.000 0.000 0.000
Ga 0.0167(9) 0.0149(9) 0.0142(11) -0.0008(9) 0.0011(9) 0.0001(8)
S1 0.016(2) 0.016(2) 0.019(3) -0.0001(19) 0.000(2) 0.0041(18)
S2 0.020(2) 0.017(2) 0.012(3) 0.000(2) -0.004(2) -0.0030(19)
S3 0.015(2) 0.027(2) 0.010(3) -0.001(2) -0.0010(18) -0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S1 Pb S1 82.62(11) 3_577 5_656
S1 Pb S3 77.01(14) 3_577 5_656
S1 Pb S3 78.81(12) 5_656 5_656
S1 Pb S1 89.75(12) 3_577 6_466
S1 Pb S1 73.75(13) 5_656 6_466
S3 Pb S1 150.86(12) 5_656 6_466
S2 Ge S2 98.4(3) . 2_775
S2 Ge S2 115.30(15) . 3_577
S2 Ge S2 115.30(14) 2_775 3_577
S2 Ge S2 115.30(15) . 4_757
S2 Ge S2 115.30(15) 2_775 4_757
S2 Ge S2 98.4(3) 3_577 4_757
S2 Ga S3 114.82(18) . 7_665
S2 Ga S3 111.5(2) . .
S3 Ga S3 104.49(17) 7_665 .
S2 Ga S1 110.94(18) . .
S3 Ga S1 105.37(19) 7_665 .
S3 Ga S1 109.30(18) . .
Ga S1 Pb 89.06(16) . 4_757
Ga S1 Pb 85.24(15) . 5_646
Pb S1 Pb 109.76(16) 4_757 5_646
Ga S1 Pb 166.3(2) . 6_566
Pb S1 Pb 96.03(14) 4_757 6_566
Pb S1 Pb 104.87(13) 5_646 6_566
Ge S2 Ga 104.2(2) . .
Ga S3 Ga 108.8(2) 7_664 .
Ga S3 Pb 85.37(15) 7_664 5_646
Ga S3 Pb 82.72(15) . 5_646
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb S1 2.827(5) 3_577
Pb S1 2.882(5) 5_656
Pb S3 2.991(5) 5_656
Pb S1 3.075(4) 6_466
Ge S2 2.239(5) .
Ge S2 2.239(5) 2_775
Ge S2 2.239(5) 3_577
Ge S2 2.239(5) 4_757
Ga S2 2.245(5) .
Ga S3 2.271(6) 7_665
Ga S3 2.286(5) .
Ga S1 2.287(5) .
S1 Pb 2.827(5) 4_757
S1 Pb 2.882(5) 5_646
S1 Pb 3.075(4) 6_566
S3 Ga 2.271(6) 7_664
S3 Pb 2.991(5) 5_646
