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#$Date: 2022-04-21 01:59:29 +0300 (Thu, 21 Apr 2022) $
#$Revision: 274612 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/00/7710096.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_7710096
loop_
_publ_author_name
'Duan, Shuping'
'Xu, Ya'
'Zhou, Jian'
'Xiao, Zunhong'
'Zou, Hua-Hong'
_publ_section_title
;
 Rare examples of hybrid chalcogenoarsenate(III) incorporating trivalent
 vanadium complexes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt00251e
_journal_year                    2022
_chemical_formula_moiety         'C12 H48 N12 O V2, As2 Se5'
_chemical_formula_sum            'C12 H48 As2 N12 O Se5 V2'
_chemical_formula_weight         1023.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-08 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                105.82(3)
_cell_angle_beta                 107.08(5)
_cell_angle_gamma                111.27(3)
_cell_formula_units_Z            1
_cell_length_a                   9.166(4)
_cell_length_b                   9.983(7)
_cell_length_c                   10.470(7)
_cell_measurement_reflns_used    3693
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.65
_cell_volume                     772.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10106
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         3.344
_exptl_absorpt_coefficient_mu    8.654
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.009
_exptl_transmission_factor_max   0.937
_exptl_transmission_factor_min   0.775
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2735
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0281
_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)+(0.0077P)²+0.3454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2243
_reflns_number_total             2735
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00251e2.cif
_cod_data_source_block           5
_cod_original_cell_volume        772.2(9)
_cod_database_code               7710096
_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   0.711
_shelx_estimated_absorpt_t_max   0.939
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.57652(6) 0.18286(5) 0.44562(4) 0.03934(13) Uani 1 1 d . . . . .
Se2 Se 0.33685(5) 0.22282(5) 0.11903(4) 0.02833(11) Uani 1 1 d . . . . .
Se3 Se 0.64129(11) 0.57629(9) 0.51117(9) 0.0335(2) Uani 0.5 1 d . . P . .
V1 V 0.19319(7) 0.66962(6) 0.03990(6) 0.01538(14) Uani 1 1 d . . . . .
As1 As 0.41179(11) 0.30101(9) 0.37414(7) 0.0228(3) Uani 0.5009(15) 1 d . . P A 1
As1' As 0.53148(11) 0.36799(9) 0.36690(8) 0.0213(3) Uani 0.4991(15) 1 d . . P A
2
O1 O 0.0000 0.5000 0.0000 0.0176(7) Uani 1 2 d S . P . .
N1 N 0.4564(4) 0.8655(3) 0.1121(3) 0.0213(7) Uani 1 1 d . . . . .
H1A H 0.4781 0.8621 0.0341 0.026 Uiso 1 1 calc R U . . .
H1B H 0.4609 0.9584 0.1533 0.026 Uiso 1 1 calc R U . . .
N2 N 0.3593(4) 0.6006(3) 0.1667(3) 0.0239(7) Uani 1 1 d . . . . .
H2A H 0.3633 0.6264 0.2564 0.029 Uiso 1 1 calc R U . . .
H2B H 0.3158 0.4957 0.1232 0.029 Uiso 1 1 calc R U . . .
N3 N 0.0878(4) 0.7861(4) -0.0751(3) 0.0260(7) Uani 1 1 d D . . . .
H3A H -0.0251 0.7470 -0.0976 0.031 Uiso 1 1 calc R U . . .
H3B H 0.1412 0.8896 -0.0170 0.031 Uiso 1 1 calc R U . . .
N4 N 0.2024(4) 0.5724(4) -0.1676(3) 0.0260(7) Uani 1 1 d D . . . .
H4A H 0.3114 0.6183 -0.1565 0.031 Uiso 1 1 calc R U . . .
H4B H 0.1642 0.4684 -0.1979 0.031 Uiso 1 1 calc R U . . .
N5 N 0.1989(4) 0.8129(3) 0.2359(3) 0.0222(7) Uani 1 1 d . . . . .
H5A H 0.1953 0.7607 0.2926 0.027 Uiso 1 1 calc R U . . .
H5B H 0.3016 0.9008 0.2840 0.027 Uiso 1 1 calc R U . . .
N6 N -0.0063(5) 0.7737(4) 0.4039(4) 0.0380(9) Uani 1 1 d D . . . .
C1 C 0.5887(5) 0.8513(5) 0.2190(4) 0.0307(9) Uani 1 1 d . . . . .
H1C H 0.5999 0.9011 0.3174 0.037 Uiso 1 1 calc R U . . .
H1D H 0.7006 0.9053 0.2190 0.037 Uiso 1 1 calc R U . . .
C2 C 0.5376(5) 0.6807(5) 0.1792(4) 0.0314(9) Uani 1 1 d . . . . .
H2C H 0.5396 0.6332 0.0860 0.038 Uiso 1 1 calc R U . . .
H2D H 0.6180 0.6700 0.2547 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1114(7) 0.7621(5) -0.2101(4) 0.0501(13) Uani 1 1 d D . . . .
H3C H 0.2265 0.8416 -0.1873 0.060 Uiso 1 1 calc R U . . .
H3D H 0.0261 0.7744 -0.2797 0.060 Uiso 1 1 calc R U . . .
C4 C 0.0913(7) 0.6026(5) -0.2771(4) 0.0497(13) Uani 1 1 d D . . . .
H4C H 0.1225 0.5934 -0.3587 0.060 Uiso 1 1 calc R U . . .
H4D H -0.0295 0.5235 -0.3157 0.060 Uiso 1 1 calc R U . . .
C5 C 0.0639(5) 0.8618(5) 0.2248(4) 0.0279(9) Uani 1 1 d . . . . .
H5C H -0.0471 0.7749 0.1467 0.034 Uiso 1 1 calc R U . . .
H5D H 0.0925 0.9511 0.1989 0.034 Uiso 1 1 calc R U . . .
C6 C 0.0480(5) 0.9082(4) 0.3672(4) 0.0305(9) Uani 1 1 d D . . . .
H6D H 0.1593 0.9939 0.4459 0.037 Uiso 1 1 calc R U . . .
H6E H -0.0365 0.9460 0.3579 0.037 Uiso 1 1 calc R U . . .
H6B H -0.068(5) 0.780(5) 0.449(4) 0.045(13) Uiso 1 1 d D . . . .
H6A H 0.081(5) 0.772(6) 0.464(5) 0.070(18) 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
_geom_angle_publ_flag
As1 Se3 Se3 69.91(8) 2_666 2_666 ?
As1' Se3 Se3 68.38(7) . 2_666 ?
As1' Se3 As1' 114.13(6) . 2_666 ?
Se3 Se3 As1' 45.75(5) 2_666 2_666 ?
As1 Se3 As1 113.17(7) 2_666 . ?
Se3 Se3 As1 43.27(5) 2_666 . ?
O1 V1 N5 93.56(11) . . ?
O1 V1 N2 92.68(10) . . ?
N5 V1 N2 90.36(12) . . ?
O1 V1 N3 101.57(10) . . ?
N5 V1 N3 89.49(12) . . ?
N2 V1 N3 165.74(12) . . ?
O1 V1 N4 96.00(11) . . ?
N5 V1 N4 166.98(12) . . ?
N2 V1 N4 97.99(12) . . ?
N3 V1 N4 79.95(12) . . ?
O1 V1 N1 170.45(8) . . ?
N5 V1 N1 86.01(13) . . ?
N2 V1 N1 77.79(12) . . ?
N3 V1 N1 87.97(12) . . ?
N4 V1 N1 86.02(13) . . ?
Se3 As1 Se1 126.65(6) 2_666 . ?
Se3 As1 Se2 129.12(6) 2_666 . ?
Se1 As1 Se2 104.23(5) . . ?
Se3 As1 Se3 66.83(7) 2_666 . ?
Se1 As1 Se3 98.12(7) . . ?
Se2 As1 Se3 109.20(7) . . ?
Se3 As1' Se2 138.15(6) . . ?
Se3 As1' Se1 116.58(7) . . ?
Se2 As1' Se1 105.12(6) . . ?
Se3 As1' Se3 65.87(6) . 2_666 ?
Se2 As1' Se3 104.48(6) . 2_666 ?
Se1 As1' Se3 100.46(5) . 2_666 ?
V1 O1 V1 180.0 . 2_565 ?
C1 N1 V1 110.3(2) . . ?
C1 N1 H1A 109.6 . . ?
V1 N1 H1A 109.6 . . ?
C1 N1 H1B 109.6 . . ?
V1 N1 H1B 109.6 . . ?
H1A N1 H1B 108.1 . . ?
C2 N2 V1 110.5(2) . . ?
C2 N2 H2A 109.6 . . ?
V1 N2 H2A 109.6 . . ?
C2 N2 H2B 109.6 . . ?
V1 N2 H2B 109.6 . . ?
H2A N2 H2B 108.1 . . ?
C3 N3 V1 110.1(2) . . ?
C3 N3 H3A 109.6 . . ?
V1 N3 H3A 109.6 . . ?
C3 N3 H3B 109.6 . . ?
V1 N3 H3B 109.6 . . ?
H3A N3 H3B 108.1 . . ?
C4 N4 V1 108.2(2) . . ?
C4 N4 H4A 110.1 . . ?
V1 N4 H4A 110.1 . . ?
C4 N4 H4B 110.1 . . ?
V1 N4 H4B 110.1 . . ?
H4A N4 H4B 108.4 . . ?
C5 N5 V1 119.5(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 H6B 110(3) . . ?
C6 N6 H6A 113(4) . . ?
H6B N6 H6A 105(4) . . ?
N1 C1 C2 109.7(3) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C2 C1 107.6(3) . . ?
N2 C2 H2C 110.2 . . ?
C1 C2 H2C 110.2 . . ?
N2 C2 H2D 110.2 . . ?
C1 C2 H2D 110.2 . . ?
H2C C2 H2D 108.5 . . ?
N3 C3 C4 110.4(3) . . ?
N3 C3 H3C 109.6 . . ?
C4 C3 H3C 109.6 . . ?
N3 C3 H3D 109.6 . . ?
C4 C3 H3D 109.6 . . ?
H3C C3 H3D 108.1 . . ?
C3 C4 N4 110.8(3) . . ?
C3 C4 H4C 109.5 . . ?
N4 C4 H4C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
N4 C4 H4D 109.5 . . ?
H4C C4 H4D 108.1 . . ?
N5 C5 C6 111.7(3) . . ?
N5 C5 H5C 109.3 . . ?
C6 C5 H5C 109.3 . . ?
N5 C5 H5D 109.3 . . ?
C6 C5 H5D 109.3 . . ?
H5C C5 H5D 107.9 . . ?
N6 C6 C5 110.6(3) . . ?
N6 C6 H6D 109.5 . . ?
C5 C6 H6D 109.5 . . ?
N6 C6 H6E 109.5 . . ?
C5 C6 H6E 109.5 . . ?
H6D C6 H6E 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 As1 2.3111(13) . ?
Se1 As1' 2.3345(16) . ?
Se2 As1' 2.318(2) . ?
Se2 As1 2.369(2) . ?
Se3 As1 1.7755(14) 2_666 ?
Se3 As1' 1.869(2) . ?
Se3 Se3 2.382(2) 2_666 ?
Se3 As1' 2.4262(15) 2_666 ?
Se3 As1 2.433(3) . ?
V1 O1 1.7839(14) . ?
V1 N5 2.131(3) . ?
V1 N2 2.151(3) . ?
V1 N3 2.152(3) . ?
V1 N4 2.165(3) . ?
V1 N1 2.217(3) . ?
As1 Se3 1.7755(14) 2_666 ?
As1' Se3 2.4262(15) 2_666 ?
O1 V1 1.7839(14) 2_565 ?
N1 C1 1.469(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C2 1.482(5) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C3 1.461(4) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C4 1.472(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C5 1.472(4) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N6 C6 1.451(5) . ?
N6 H6B 0.84(3) . ?
N6 H6A 0.87(3) . ?
C1 C2 1.488(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.471(5) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.503(5) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6D 0.9700 . ?
C6 H6E 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Se3 Se3 As1' Se2 84.87(9) 2_666 . . . ?
As1' Se3 As1' Se2 84.86(9) 2_666 . . . ?
Se3 Se3 As1' Se1 -89.90(7) 2_666 . . . ?
As1' Se3 As1' Se1 -89.90(7) 2_666 . . . ?
As1' Se3 As1' Se3 -0.001(0) 2_666 . . 2_666 ?
V1 N1 C1 C2 35.7(3) . . . . ?
V1 N2 C2 C1 46.2(3) . . . . ?
N1 C1 C2 N2 -54.0(4) . . . . ?
V1 N3 C3 C4 35.9(4) . . . . ?
N3 C3 C4 N4 -51.5(5) . . . . ?
V1 N4 C4 C3 40.1(4) . . . . ?
V1 N5 C5 C6 159.3(3) . . . . ?
N5 C5 C6 N6 -62.8(4) . . . . ?
