#------------------------------------------------------------------------------
#$Date: 2016-02-10 10:06:24 +0200 (Wed, 10 Feb 2016) $
#$Revision: 176324 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/41/7224187.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_7224187
loop_
_publ_author_name
'Qian, Li-Wen'
'Zhao, Xiao-Wei'
'Su, Hu-Chao'
'Bian, Guo-Qing'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 Supramolecular hexagonal nano tubes assembled by vanadium diamine
 complexes with thiogermanates
;
_journal_issue                   20
_journal_name_full               'RSC Adv.'
_journal_page_first              16268
_journal_paper_doi               10.1039/C5RA27088J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C12 H40 Ge2 N8 O2 S6 V2'
_chemical_formula_weight         767.94
_space_group_crystal_system      hexagonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-05-21 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   38.284(5)
_cell_length_b                   38.284(5)
_cell_length_c                   11.170(2)
_cell_measurement_reflns_used    17116
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     14178(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45027
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.193
_exptl_absorpt_coefficient_mu    2.887
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       Block
_exptl_crystal_F_000             7020
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0894
_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
'w=1/[σ²(Fo²)+(0.0010P)²+550.5397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3559
_reflns_number_total             3623
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra27088j2.cif
_cod_data_source_block           2
_cod_original_cell_volume        14178(5)
_cod_database_code               7224187
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.256
_shelx_estimated_absorpt_t_max   0.761
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.07110(4) 0.55268(4) 0.06901(11) 0.0363(3) Uani 1 1 d . . . . .
Ge1 Ge 0.11080(3) 0.47879(2) 0.00838(6) 0.0347(2) Uani 1 1 d . . . . .
S1 S 0.07873(7) 0.50793(6) -0.06712(16) 0.0430(5) Uani 1 1 d . . . . .
S2 S 0.08505(7) 0.41838(7) -0.0833 0.0393(6) Uani 1 2 d S T P . .
S3 S 0.17184(8) 0.50517(8) -0.0833 0.0470(7) Uani 1 2 d S T P . .
S4 S 0.11254(8) 0.47598(7) 0.20004(16) 0.0494(6) Uani 1 1 d . . . . .
N1 N 0.0359(2) 0.5589(2) -0.0692(7) 0.0537(19) Uani 1 1 d . . . . .
H1A H 0.0490 0.5641 -0.1385 0.064 Uiso 1 1 calc R U . . .
H1B H 0.0126 0.5359 -0.0770 0.064 Uiso 1 1 calc R U . . .
N2 N 0.0631(2) 0.5999(2) 0.1436(6) 0.0492(17) Uani 1 1 d . . . . .
H2A H 0.0573 0.5952 0.2211 0.059 Uiso 1 1 calc R U . . .
H2B H 0.0860 0.6233 0.1367 0.059 Uiso 1 1 calc R U . . .
N3 N 0.1266(2) 0.6073(2) -0.0258(6) 0.0492(18) Uani 1 1 d . . . . .
H3A H 0.1239 0.6048 -0.1050 0.059 Uiso 1 1 calc R U . . .
H3B H 0.1282 0.6304 -0.0046 0.059 Uiso 1 1 calc R U . . .
N4 N 0.1223(2) 0.5675(2) 0.1778(5) 0.0398(15) Uani 1 1 d . . . . .
H4A H 0.1171 0.5729 0.2510 0.048 Uiso 1 1 calc R U . . .
H4B H 0.1246 0.5455 0.1836 0.048 Uiso 1 1 calc R U . . .
C1 C 0.0279(4) 0.5918(4) -0.0400(10) 0.090(4) Uani 1 1 d . . . . .
H1C H 0.0466 0.6156 -0.0850 0.108 Uiso 1 1 calc R U . . .
H1D H 0.0009 0.5841 -0.0669 0.108 Uiso 1 1 calc R U . . .
C2 C 0.0312(5) 0.6023(5) 0.0829(15) 0.118(6) Uani 1 1 d . . . . .
H2 H 0.0066 0.5802 0.1182 0.142 Uiso 1 1 calc R U . A 1
C3 C 0.0264(5) 0.6392(5) 0.104(2) 0.094(8) Uani 0.66(2) 1 d . . P B 1
C3' C 0.0029(8) 0.5986(9) -0.121(2) 0.057(9) Uani 0.34(2) 1 d . . P B 2
C4 C 0.1625(3) 0.6068(3) 0.0110(9) 0.065(3) Uani 1 1 d . . . . .
H4C H 0.1862 0.6320 -0.0109 0.078 Uiso 1 1 calc R U . . .
H4D H 0.1638 0.5851 -0.0292 0.078 Uiso 1 1 calc R U . . .
C5 C 0.1616(3) 0.6011(3) 0.1404(9) 0.063(3) Uani 1 1 d . . . . .
H5 H 0.1634 0.6254 0.1757 0.076 Uiso 1 1 calc R U . . .
C6 C 0.1967(3) 0.5986(4) 0.1897(11) 0.085(4) Uani 1 1 d . . . . .
H6A H 0.1973 0.6012 0.2752 0.128 Uiso 1 1 calc R U . . .
H6B H 0.2213 0.6199 0.1565 0.128 Uiso 1 1 calc R U . . .
H6C H 0.1940 0.5730 0.1688 0.128 Uiso 1 1 calc R U . . .
O1 O 0.03769(17) 0.51903(18) 0.1554(5) 0.0521(15) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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'
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
O1 V1 N4 97.4(3) .
O1 V1 N1 103.2(3) .
N4 V1 N1 158.5(3) .
O1 V1 N2 92.9(3) .
N4 V1 N2 93.1(3) .
N1 V1 N2 79.9(3) .
O1 V1 N3 169.7(3) .
N4 V1 N3 73.7(2) .
N1 V1 N3 85.2(3) .
N2 V1 N3 82.7(3) .
O1 V1 S1 98.0(2) .
N4 V1 S1 97.26(18) .
N1 V1 S1 86.0(2) .
N2 V1 S1 163.8(2) .
N3 V1 S1 88.31(18) .
S4 Ge1 S1 116.57(8) .
S4 Ge1 S2 114.22(7) .
S1 Ge1 S2 106.10(6) .
S4 Ge1 S3 114.89(8) .
S1 Ge1 S3 108.20(7) .
S2 Ge1 S3 94.36(8) .
Ge1 S1 V1 114.51(8) .
Ge1 S2 Ge1 86.06(11) 10_454
Ge1 S3 Ge1 85.22(11) 10_454
C1 N1 V1 110.3(6) .
C2 N2 V1 110.8(6) .
C4 N3 V1 107.6(5) .
C5 N4 V1 118.3(5) .
C2 C1 N1 115.5(10) .
C1 C2 N2 113.1(11) .
C1 C2 C3 112.1(15) .
N2 C2 C3 119.1(12) .
N3 C4 C5 109.5(8) .
C4 C5 N4 110.5(8) .
C4 C5 C6 114.7(9) .
N4 C5 C6 113.4(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.606(6) .
V1 N4 2.128(6) .
V1 N1 2.140(7) .
V1 N2 2.146(7) .
V1 N3 2.359(7) .
V1 S1 2.415(2) .
Ge1 S4 2.1462(19) .
Ge1 S1 2.198(2) .
Ge1 S2 2.256(2) .
Ge1 S3 2.274(2) .
S2 Ge1 2.256(2) 10_454
S3 Ge1 2.274(2) 10_454
N1 C1 1.475(12) .
N2 C2 1.443(13) .
N3 C4 1.441(12) .
N4 C5 1.470(11) .
C1 C2 1.419(17) .
C2 C3 1.527(19) .
C4 C5 1.459(12) .
C5 C6 1.501(14) .
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
V1 N1 C1 C2 -21.6(16)
N1 C1 C2 N2 37(2)
N1 C1 C2 C3 174.6(13)
V1 N2 C2 C1 -32.5(17)
V1 N2 C2 C3 -167.3(15)
V1 N3 C4 C5 -46.3(10)
N3 C4 C5 N4 48.2(12)
N3 C4 C5 C6 177.9(9)
V1 N4 C5 C4 -25.9(11)
V1 N4 C5 C6 -156.3(7)
