#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/14/7031426.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_7031426
loop_
_publ_author_name
'Sun, Xiao-Lu'
'Zhu, Qin-Yu'
'Mu, Wen-Qin'
'Qian, Li-Wen'
'Yu, Lan'
'Wu, Jing'
'Bian, Guo-Qing'
'Dai, Jie'
_publ_section_title
;
 Ion pair charge-transfer thiogermanate salts [MV]2Ge4S10·xSol:
 solvent induced crystal transformation and photocurrent responsive
 properties.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12582
_journal_page_last               12589
_journal_paper_doi               10.1039/c4dt01289e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C24 H40 Ge4 N4 O6 S10'
_chemical_formula_weight         1091.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.997(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2968(15)
_cell_length_b                   21.035(3)
_cell_length_c                   21.516(4)
_cell_measurement_reflns_used    7762
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     4115.7(12)
_computing_cell_refinement       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_collection       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku Corporation, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_sigmaI/netI    0.1177
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10142
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_T_max  0.8467
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0876
_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)+(0.0306P)²+15.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                2349
_reflns_number_total             3600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01289e4.cif
_cod_data_source_block           1'
_cod_depositor_comments
'Adding full bibliography for 7031425--7031427.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c  '
_cod_database_code               7031426
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Ge1 Ge 0.65051(12) 0.54049(5) 0.31758(5) 0.0306(3) Uani 1 1 d .
Ge2 Ge 0.63107(11) 0.66121(5) 0.19839(5) 0.0294(3) Uani 1 1 d .
S1 S 0.7965(3) 0.48179(15) 0.38255(13) 0.0512(9) Uani 1 1 d .
S2 S 0.5000 0.47835(17) 0.2500 0.0335(9) Uani 1 2 d S
S3 S 0.7864(3) 0.60118(13) 0.26719(11) 0.0342(7) Uani 1 1 d .
S4 S 0.5184(3) 0.60024(13) 0.37187(10) 0.0322(6) Uani 1 1 d .
S5 S 0.7532(3) 0.72197(13) 0.14961(13) 0.0429(7) Uani 1 1 d .
S6 S 0.5000 0.72373(17) 0.2500 0.0350(9) Uani 1 2 d S
N1 N 0.8572(9) 0.5747(5) 0.6189(4) 0.053(3) Uani 1 1 d .
N2 N 0.9590(9) 0.7963(5) 0.3899(4) 0.044(2) Uani 1 1 d .
C1 C 0.8521(13) 0.5563(6) 0.5586(5) 0.059(4) Uani 1 1 d .
H1 H 0.8332 0.5135 0.5473 0.071 Uiso 1 1 calc R
C2 C 0.8737(12) 0.5988(6) 0.5134(5) 0.050(3) Uani 1 1 d .
H2 H 0.8696 0.5848 0.4716 0.060 Uiso 1 1 calc R
C3 C 0.9015(11) 0.6621(6) 0.5284(5) 0.042(3) Uani 1 1 d .
C4 C 0.9081(12) 0.6794(6) 0.5915(5) 0.051(3) Uani 1 1 d .
H4 H 0.9275 0.7218 0.6042 0.061 Uiso 1 1 calc R
C5 C 0.8863(11) 0.6340(7) 0.6357(5) 0.058(4) Uani 1 1 d .
H5 H 0.8924 0.6461 0.6782 0.069 Uiso 1 1 calc R
C6 C 0.8932(13) 0.7415(6) 0.3715(5) 0.052(3) Uani 1 1 d .
H6 H 0.8593 0.7333 0.3280 0.063 Uiso 1 1 calc R
C7 C 0.8741(13) 0.6963(6) 0.4160(5) 0.052(3) Uani 1 1 d .
H7 H 0.8279 0.6575 0.4021 0.063 Uiso 1 1 calc R
C8 C 0.9221(11) 0.7073(5) 0.4807(5) 0.035(3) Uani 1 1 d .
C9 C 0.9911(14) 0.7645(5) 0.4959(5) 0.058(4) Uani 1 1 d .
H9 H 1.0288 0.7739 0.5390 0.069 Uiso 1 1 calc R
C10 C 1.0073(13) 0.8086(6) 0.4508(5) 0.058(4) Uani 1 1 d .
H10 H 1.0530 0.8477 0.4634 0.070 Uiso 1 1 calc R
C11 C 0.8394(14) 0.5264(7) 0.6673(5) 0.073(4) Uani 1 1 d .
H11A H 0.8158 0.5476 0.7040 0.110 Uiso 1 1 calc R
H11B H 0.9302 0.5027 0.6802 0.110 Uiso 1 1 calc R
H11C H 0.7605 0.4975 0.6493 0.110 Uiso 1 1 calc R
C12 C 0.9781(12) 0.8429(5) 0.3415(5) 0.051(3) Uani 1 1 d .
H12A H 1.0185 0.8819 0.3621 0.076 Uiso 1 1 calc R
H12B H 0.8837 0.8516 0.3139 0.076 Uiso 1 1 calc R
H12C H 1.0449 0.8258 0.3165 0.076 Uiso 1 1 calc R
O1 O 0.6922(8) 0.8600(4) 0.2186(3) 0.052(2) Uani 1 1 d .
O2 O 0.9090(18) 0.0473(5) 0.5184(5) 0.154(6) Uani 1 1 d .
O3 O 0.6587(17) 0.1037(5) 0.4350(7) 0.174(7) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 Ge1 S2 108.51(12) . .
S1 Ge1 S3 107.64(12) . .
S2 Ge1 S3 111.23(9) . .
S1 Ge1 S4 109.02(10) . .
S2 Ge1 S4 109.35(9) . .
S3 Ge1 S4 111.02(10) . .
S5 Ge2 S3 109.24(11) . .
S5 Ge2 S4 109.39(10) . 2_655
S3 Ge2 S4 110.47(11) . 2_655
S5 Ge2 S6 107.06(12) . .
S3 Ge2 S6 110.31(8) . .
S4 Ge2 S6 110.29(9) 2_655 .
Ge1 S2 Ge1 107.92(16) 2_655 .
Ge1 S3 Ge2 107.03(11) . .
Ge2 S4 Ge1 107.44(10) 2_655 .
Ge2 S6 Ge2 108.03(16) 2_655 .
C5 N1 C1 120.2(10) . .
C5 N1 C11 120.2(11) . .
C1 N1 C11 119.5(11) . .
C10 N2 C6 120.6(10) . .
C10 N2 C12 120.5(10) . .
C6 N2 C12 118.9(9) . .
N1 C1 C2 121.2(12) . .
N1 C1 H1 119.4 . .
C2 C1 H1 119.4 . .
C1 C2 C3 120.8(11) . .
C1 C2 H2 119.6 . .
C3 C2 H2 119.6 . .
C2 C3 C4 116.6(11) . .
C2 C3 C8 120.9(10) . .
C4 C3 C8 122.5(11) . .
C5 C4 C3 120.2(12) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
N1 C5 C4 121.0(11) . .
N1 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
N2 C6 C7 120.4(10) . .
N2 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C6 C7 C8 121.1(10) . .
C6 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C9 C8 C7 115.0(10) . .
C9 C8 C3 122.2(10) . .
C7 C8 C3 122.8(10) . .
C8 C9 C10 122.6(11) . .
C8 C9 H9 118.7 . .
C10 C9 H9 118.7 . .
N2 C10 C9 120.3(11) . .
N2 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N2 C12 H12A 109.5 . .
N2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 S1 2.129(3) .
Ge1 S2 2.221(2) .
Ge1 S3 2.229(3) .
Ge1 S4 2.247(3) .
Ge2 S5 2.126(3) .
Ge2 S3 2.232(3) .
Ge2 S4 2.233(3) 2_655
Ge2 S6 2.238(2) .
S2 Ge1 2.221(2) 2_655
S4 Ge2 2.233(3) 2_655
S6 Ge2 2.238(2) 2_655
N1 C5 1.312(15) .
N1 C1 1.346(13) .
N1 C11 1.488(13) .
N2 C10 1.319(12) .
N2 C6 1.326(13) .
N2 C12 1.468(12) .
C1 C2 1.365(14) .
C1 H1 0.9400 .
C2 C3 1.383(15) .
C2 H2 0.9400 .
C3 C4 1.393(14) .
C3 C8 1.441(14) .
C4 C5 1.392(15) .
C4 H4 0.9400 .
C5 H5 0.9400 .
C6 C7 1.387(14) .
C6 H6 0.9400 .
C7 C8 1.390(13) .
C7 H7 0.9400 .
C8 C9 1.371(14) .
C9 C10 1.373(14) .
C9 H9 0.9400 .
C10 H10 0.9400 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 H11C 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 H12C 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
S1 Ge1 S2 Ge1 -179.73(10) . 2_655
S3 Ge1 S2 Ge1 -61.50(8) . 2_655
S4 Ge1 S2 Ge1 61.47(8) . 2_655
S1 Ge1 S3 Ge2 179.18(11) . .
S2 Ge1 S3 Ge2 60.43(13) . .
S4 Ge1 S3 Ge2 -61.58(13) . .
S5 Ge2 S3 Ge1 178.88(11) . .
S4 Ge2 S3 Ge1 -60.74(13) 2_655 .
S6 Ge2 S3 Ge1 61.47(14) . .
S1 Ge1 S4 Ge2 179.56(13) . 2_655
S2 Ge1 S4 Ge2 -61.95(14) . 2_655
S3 Ge1 S4 Ge2 61.15(14) . 2_655
S5 Ge2 S6 Ge2 179.71(10) . 2_655
S3 Ge2 S6 Ge2 -61.53(8) . 2_655
S4 Ge2 S6 Ge2 60.79(8) 2_655 2_655
C5 N1 C1 C2 -1.3(18) . .
C11 N1 C1 C2 -177.4(11) . .
N1 C1 C2 C3 0.0(19) . .
C1 C2 C3 C4 0.9(17) . .
C1 C2 C3 C8 -179.1(10) . .
C2 C3 C4 C5 -0.5(16) . .
C8 C3 C4 C5 179.5(10) . .
C1 N1 C5 C4 1.8(17) . .
C11 N1 C5 C4 177.9(10) . .
C3 C4 C5 N1 -0.9(17) . .
C10 N2 C6 C7 0.1(18) . .
C12 N2 C6 C7 179.6(10) . .
N2 C6 C7 C8 0.4(19) . .
C6 C7 C8 C9 -1.5(17) . .
C6 C7 C8 C3 178.6(11) . .
C2 C3 C8 C9 -160.3(11) . .
C4 C3 C8 C9 19.8(17) . .
C2 C3 C8 C7 19.7(17) . .
C4 C3 C8 C7 -160.3(11) . .
C7 C8 C9 C10 2.1(19) . .
C3 C8 C9 C10 -178.0(11) . .
C6 N2 C10 C9 0.5(18) . .
C12 N2 C10 C9 -179.0(11) . .
C8 C9 C10 N2 -2(2) . .
