#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:20:00 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223757 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/03/7700377.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_7700377
loop_
_publ_author_name
'Luo, Hai-Ying'
'Zhou, Jian'
'Cao, Shumei'
_publ_section_title
;
 A series of new hybrid chalcogenogermanates: the rare examples of
 chalcogenogermanates combined with trivalent vanadium complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10907
_journal_page_last               10914
_journal_paper_doi               10.1039/c9dt02077b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H48 N12 O V2, Ge2 Se6'
_chemical_formula_sum            'C12 H48 Ge2 N12 O Se6 V2'
_chemical_formula_weight         1097.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-20 deposited with the CCDC.    2019-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                109.090(4)
_cell_angle_beta                 104.169(4)
_cell_angle_gamma                111.520(5)
_cell_formula_units_Z            1
_cell_length_a                   9.4480(12)
_cell_length_b                   10.1780(13)
_cell_length_c                   10.4361(12)
_cell_measurement_reflns_used    2858
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.52
_cell_volume                     802.73(18)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14287
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.554
_diffrn_reflns_theta_min         2.519
_exptl_absorpt_coefficient_mu    9.250
_exptl_absorpt_correction_T_max  0.207
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0204P)²+0.5551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3262
_reflns_number_total             4422
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02077b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7700373--7700378.cif.'
_cod_original_cell_volume        802.73(17)
_cod_database_code               7700377
_shelx_shelxl_version_number     2018/3
_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   0.139
_shelx_estimated_absorpt_t_max   0.303
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Se1 Se 0.27219(5) 0.39005(5) 0.62389(4) 0.02729(10) Uani 1 1 d . . .
Se2 Se 0.31569(4) 0.39936(5) 1.01750(4) 0.02425(10) Uani 1 1 d . . .
Se3 Se 0.37482(5) 0.76764(5) 0.96041(4) 0.02743(10) Uani 1 1 d . . .
Ge1 Ge 0.39727(4) 0.54173(4) 0.87994(4) 0.01643(9) Uani 1 1 d . . .
V1 V 0.34397(7) 0.86991(7) 0.53619(6) 0.01747(13) Uani 1 1 d . . .
O1 O 0.500000 1.000000 0.500000 0.0220(8) Uani 1 2 d S . P
N1 N 0.3065(4) 1.0607(4) 0.6626(3) 0.0238(7) Uani 1 1 d . . .
H1A H 0.389428 1.120919 0.753427 0.029 Uiso 1 1 calc R U .
H1B H 0.307393 1.121749 0.617870 0.029 Uiso 1 1 calc R U .
N2 N 0.1591(3) 0.7486(3) 0.6143(3) 0.0211(6) Uani 1 1 d . . .
H2A H 0.062064 0.675718 0.536486 0.025 Uiso 1 1 calc R U .
H2B H 0.196301 0.699340 0.658766 0.025 Uiso 1 1 calc R U .
N3 N 0.3195(4) 0.6364(4) 0.4165(3) 0.0271(7) Uani 1 1 d . . .
H3A H 0.397599 0.646047 0.381342 0.033 Uiso 1 1 calc R U .
H3B H 0.332703 0.593990 0.477823 0.033 Uiso 1 1 calc R U .
N4 N 0.1282(4) 0.7724(4) 0.3305(3) 0.0252(7) Uani 1 1 d . . .
H4A H 0.036078 0.748211 0.347003 0.030 Uiso 1 1 calc R U .
H4B H 0.140833 0.844108 0.296997 0.030 Uiso 1 1 calc R U .
N5 N 0.5300(3) 0.9119(4) 0.7326(3) 0.0220(7) Uani 1 1 d . . .
H5A H 0.593096 1.016909 0.788601 0.026 Uiso 1 1 calc R U .
H5B H 0.477359 0.874980 0.783405 0.026 Uiso 1 1 calc R U .
N6 N 0.8898(4) 1.1009(5) 0.8940(4) 0.0353(8) Uani 1 1 d D . .
C1 C 0.1440(4) 0.9935(5) 0.6741(4) 0.0254(8) Uani 1 1 d . . .
H1C H 0.052120 0.948541 0.578691 0.030 Uiso 1 1 calc R U .
H1D H 0.137323 1.076458 0.747288 0.030 Uiso 1 1 calc R U .
C2 C 0.1340(5) 0.8669(5) 0.7201(4) 0.0288(9) Uani 1 1 d . . .
H2C H 0.219141 0.914450 0.819861 0.035 Uiso 1 1 calc R U .
H2D H 0.025505 0.814792 0.720971 0.035 Uiso 1 1 calc R U .
C3 C 0.1507(5) 0.5322(5) 0.2916(4) 0.0302(9) Uani 1 1 d . . .
H3C H 0.067813 0.494017 0.328981 0.036 Uiso 1 1 calc R U .
H3D H 0.147785 0.440813 0.220028 0.036 Uiso 1 1 calc R U .
C4 C 0.1126(5) 0.6274(5) 0.2182(4) 0.0329(9) Uani 1 1 d . . .
H4C H 0.189713 0.657322 0.173376 0.039 Uiso 1 1 calc R U .
H4D H -0.000059 0.563376 0.140084 0.039 Uiso 1 1 calc R U .
C5 C 0.6438(5) 0.8454(5) 0.7183(4) 0.0291(9) Uani 1 1 d . . .
H5C H 0.672847 0.851609 0.636671 0.035 Uiso 1 1 calc R U .
H5D H 0.586598 0.733975 0.694539 0.035 Uiso 1 1 calc R U .
C6 C 0.8006(5) 0.9324(5) 0.8582(4) 0.0321(9) Uani 1 1 d . . .
H6A H 0.772838 0.923644 0.939683 0.038 Uiso 1 1 calc R U .
H6B H 0.871682 0.885120 0.844981 0.038 Uiso 1 1 calc R U .
H6D H 0.9998(15) 1.149(5) 0.944(4) 0.046(13) Uiso 1 1 d D . .
H6C H 0.851(6) 1.156(5) 0.946(5) 0.065(17) Uiso 1 1 d 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'
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'
Se Se -0.0929 2.2259 '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
Ge1 Se2 Ge1 86.692(17) 2_667 .
Se3 Ge1 Se1 113.79(2) . .
Se3 Ge1 Se2 111.38(2) . 2_667
Se1 Ge1 Se2 111.53(2) . 2_667
Se3 Ge1 Se2 109.85(2) . .
Se1 Ge1 Se2 115.28(2) . .
Se2 Ge1 Se2 93.309(17) 2_667 .
O1 V1 N5 91.69(8) . .
O1 V1 N1 92.46(8) . .
N5 V1 N1 91.98(12) . .
O1 V1 N4 98.65(8) . .
N5 V1 N4 166.95(12) . .
N1 V1 N4 95.49(12) . .
O1 V1 N3 103.87(8) . .
N5 V1 N3 89.91(12) . .
N1 V1 N3 163.51(11) . .
N4 V1 N3 79.93(12) . .
O1 V1 N2 169.67(8) . .
N5 V1 N2 85.43(11) . .
N1 V1 N2 77.75(11) . .
N4 V1 N2 85.71(11) . .
N3 V1 N2 86.07(11) . .
V1 O1 V1 180.0 . 2_676
C1 N1 V1 110.0(2) . .
C1 N1 H1A 109.7 . .
V1 N1 H1A 109.7 . .
C1 N1 H1B 109.7 . .
V1 N1 H1B 109.7 . .
H1A N1 H1B 108.2 . .
C2 N2 V1 110.0(2) . .
C2 N2 H2A 109.7 . .
V1 N2 H2A 109.7 . .
C2 N2 H2B 109.7 . .
V1 N2 H2B 109.7 . .
H2A N2 H2B 108.2 . .
C3 N3 V1 108.5(2) . .
C3 N3 H3A 110.0 . .
V1 N3 H3A 110.0 . .
C3 N3 H3B 110.0 . .
V1 N3 H3B 110.0 . .
H3A N3 H3B 108.4 . .
C4 N4 V1 108.9(2) . .
C4 N4 H4A 109.9 . .
V1 N4 H4A 109.9 . .
C4 N4 H4B 109.9 . .
V1 N4 H4B 109.9 . .
H4A N4 H4B 108.3 . .
C5 N5 V1 119.6(2) . .
C5 N5 H5A 107.4 . .
V1 N5 H5A 107.4 . .
C5 N5 H5B 107.4 . .
V1 N5 H5B 107.4 . .
H5A N5 H5B 107.0 . .
C6 N6 H6D 115(3) . .
C6 N6 H6C 111(3) . .
H6D N6 H6C 108(4) . .
N1 C1 C2 107.7(3) . .
N1 C1 H1C 110.2 . .
C2 C1 H1C 110.2 . .
N1 C1 H1D 110.2 . .
C2 C1 H1D 110.2 . .
H1C C1 H1D 108.5 . .
N2 C2 C1 109.5(3) . .
N2 C2 H2C 109.8 . .
C1 C2 H2C 109.8 . .
N2 C2 H2D 109.8 . .
C1 C2 H2D 109.8 . .
H2C C2 H2D 108.2 . .
N3 C3 C4 108.4(3) . .
N3 C3 H3C 110.0 . .
C4 C3 H3C 110.0 . .
N3 C3 H3D 110.0 . .
C4 C3 H3D 110.0 . .
H3C C3 H3D 108.4 . .
N4 C4 C3 109.7(3) . .
N4 C4 H4C 109.7 . .
C3 C4 H4C 109.7 . .
N4 C4 H4D 109.7 . .
C3 C4 H4D 109.7 . .
H4C C4 H4D 108.2 . .
N5 C5 C6 112.0(3) . .
N5 C5 H5C 109.2 . .
C6 C5 H5C 109.2 . .
N5 C5 H5D 109.2 . .
C6 C5 H5D 109.2 . .
H5C C5 H5D 107.9 . .
N6 C6 C5 109.7(3) . .
N6 C6 H6A 109.7 . .
C5 C6 H6A 109.7 . .
N6 C6 H6B 109.7 . .
C5 C6 H6B 109.7 . .
H6A C6 H6B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Ge1 2.3103(6) .
Se2 Ge1 2.4138(6) 2_667
Se2 Ge1 2.4161(5) .
Se3 Ge1 2.2845(6) .
V1 O1 1.7990(6) .
V1 N5 2.142(3) .
V1 N1 2.166(3) .
V1 N4 2.175(3) .
V1 N3 2.186(3) .
V1 N2 2.239(3) .
N1 C1 1.488(4) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N2 C2 1.481(5) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N3 C3 1.485(5) .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N4 C4 1.482(5) .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N5 C5 1.478(4) .
N5 H5A 0.8900 .
N5 H5B 0.8900 .
N6 C6 1.469(5) .
N6 H6D 0.886(10) .
N6 H6C 0.891(10) .
C1 C2 1.496(5) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 H2C 0.9700 .
C2 H2D 0.9700 .
C3 C4 1.504(5) .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 H4C 0.9700 .
C4 H4D 0.9700 .
C5 C6 1.498(5) .
C5 H5C 0.9700 .
C5 H5D 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Se3 0.89 2.80 3.666(3) 164.8 2_677 yes
N1 H1B Se1 0.89 2.85 3.623(3) 145.8 1_565 yes
N2 H2A Se1 0.89 2.89 3.647(3) 143.9 2_566 yes
N2 H2B Se3 0.89 2.89 3.590(3) 136.8 . yes
N3 H3B Se1 0.89 2.93 3.791(3) 163.2 . yes
N4 H4A Se1 0.89 2.87 3.752(3) 169.3 2_566 yes
N4 H4B N6 0.89 2.22 3.020(5) 149.1 2_676 yes
N5 H5A Se3 0.89 2.67 3.363(3) 135.5 2_677 yes
N5 H5A N6 0.89 2.43 2.893(4) 112.6 . yes
N5 H5B Se3 0.89 2.64 3.517(3) 169.1 . yes
N6 H6D Se2 0.886(10) 2.83(2) 3.607(3) 147(4) 1_665 yes
N6 H6C Se3 0.891(10) 2.80(2) 3.651(4) 160(4) 2_677 yes
