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#$Date: 2022-06-22 12:02:36 +0300 (Wed, 22 Jun 2022) $
#$Revision: 276147 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/54/8105448.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_8105448
loop_
_publ_author_name
'Zhang, Gang'
'Luan, Jian'
'Wang, Xiao-Jie'
_publ_section_title
;
 The crystal structure of tetrakis(1-methylimidazole-κ1
 N)-oxido-(sulfato-κ1 O)vanadium(IV), C16H24N8O5SV
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1295
_journal_page_last               1296
_journal_paper_doi               10.1515/ncrs-2020-0276
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C16 H24 N8 O5 S V'
_chemical_formula_sum            'C16 H24 N8 O5 S V'
_chemical_formula_weight         491.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 121.630(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6165(6)
_cell_length_b                   16.6705(10)
_cell_length_c                   15.2726(7)
_cell_measurement_reflns_used    4569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.46
_cell_volume                     2084.7(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015) [1]'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [3]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [3]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015) [2]'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10187
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.986
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.8854
_exptl_absorpt_correction_T_min  0.8350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs,bruker(2005)
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0417
_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)+(0.0780P)²+2.5004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3133
_reflns_number_total             3651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0276_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P  21/c '
_cod_database_code               8105448
_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_max   0.885
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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 0.50579(6) 0.77526(3) 0.11581(4) 0.01267(19) Uani 1 1 d . . . . .
S1 S 0.80278(9) 0.62433(4) 0.24080(6) 0.0127(2) Uani 1 1 d . . . . .
O1 O 0.3724(3) 0.84460(13) 0.05802(17) 0.0183(5) Uani 1 1 d . . . . .
O2 O 0.7289(3) 0.55996(13) 0.26855(17) 0.0213(5) Uani 1 1 d . . . . .
O3 O 0.9476(3) 0.65760(14) 0.33209(18) 0.0220(5) Uani 1 1 d . . . . .
O4 O 0.8404(3) 0.59672(14) 0.16410(17) 0.0202(5) Uani 1 1 d . . . . .
O5 O 0.6772(3) 0.69056(13) 0.19261(16) 0.0164(5) Uani 1 1 d . . . . .
N1 N 0.3949(3) 0.69623(16) -0.0104(2) 0.0183(6) Uani 1 1 d . . . . .
N2 N 0.2074(3) 0.63784(18) -0.1529(2) 0.0257(7) Uani 1 1 d . . . . .
N3 N 0.6551(3) 0.81985(15) 0.06266(19) 0.0147(6) Uani 1 1 d . . . . .
N4 N 0.7624(3) 0.91064(15) 0.0106(2) 0.0154(6) Uani 1 1 d . . . . .
N5 N 0.3681(3) 0.72253(16) 0.1715(2) 0.0184(6) Uani 1 1 d . . . . .
N6 N 0.2796(3) 0.64710(16) 0.2498(2) 0.0187(6) Uani 1 1 d . . . . .
N7 N 0.6375(3) 0.84482(15) 0.2526(2) 0.0165(6) Uani 1 1 d . . . . .
N8 N 0.7013(4) 0.93930(17) 0.3687(2) 0.0235(6) Uani 1 1 d . . . . .
C1 C 0.2434(4) 0.7015(2) -0.0905(3) 0.0227(7) Uani 1 1 d . . . . .
H1 H 0.171946 0.743368 -0.101929 0.027 Uiso 1 1 calc R . . . .
C2 C 0.0536(5) 0.6208(3) -0.2479(3) 0.0385(10) Uani 1 1 d . . . . .
H2A H -0.019515 0.665336 -0.264551 0.058 Uiso 1 1 calc GR . . . .
H2B H 0.005456 0.573432 -0.239168 0.058 Uiso 1 1 calc GR . . . .
H2C H 0.073431 0.612549 -0.302657 0.058 Uiso 1 1 calc GR . . . .
C3 C 0.3448(5) 0.5912(2) -0.1147(3) 0.0310(9) Uani 1 1 d . . . . .
H3 H 0.356555 0.544384 -0.143281 0.037 Uiso 1 1 calc R . . . .
C4 C 0.4602(5) 0.6277(2) -0.0264(3) 0.0272(8) Uani 1 1 d . . . . .
H4 H 0.566485 0.609458 0.016572 0.033 Uiso 1 1 calc R . . . .
C5 C 0.6740(4) 0.89763(19) 0.0542(2) 0.0160(6) Uani 1 1 d . . . . .
H5 H 0.631661 0.937955 0.075667 0.019 Uiso 1 1 calc R . . . .
C6 C 0.8144(4) 0.98916(19) -0.0042(3) 0.0218(7) Uani 1 1 d . . . . .
H6A H 0.920460 1.001536 0.053923 0.033 Uiso 1 1 calc GR . . . .
H6B H 0.737673 1.029221 -0.010888 0.033 Uiso 1 1 calc GR . . . .
H6C H 0.819165 0.988312 -0.065425 0.033 Uiso 1 1 calc GR . . . .
C7 C 0.8012(4) 0.8373(2) -0.0112(3) 0.0209(7) Uani 1 1 d . . . . .
H7 H 0.861352 0.827462 -0.041884 0.025 Uiso 1 1 calc R . . . .
C8 C 0.7340(4) 0.7815(2) 0.0212(3) 0.0211(7) Uani 1 1 d . . . . .
H8 H 0.740619 0.726223 0.016014 0.025 Uiso 1 1 calc R . . . .
C9 C 0.4067(4) 0.66668(19) 0.2410(2) 0.0169(7) Uani 1 1 d . . . . .
H9 H 0.509709 0.643517 0.279412 0.020 Uiso 1 1 calc R . . . .
C10 C 0.2757(4) 0.5875(2) 0.3184(3) 0.0243(8) Uani 1 1 d . . . . .
H10A H 0.384547 0.578330 0.375426 0.036 Uiso 1 1 calc GR . . . .
H10B H 0.231170 0.538257 0.281635 0.036 Uiso 1 1 calc GR . . . .
H10C H 0.208683 0.606834 0.343404 0.036 Uiso 1 1 calc GR . . . .
C11 C 0.1479(5) 0.6904(2) 0.1767(3) 0.0371(10) Uani 1 1 d . . . . .
H11 H 0.042089 0.688716 0.163813 0.045 Uiso 1 1 calc R . . . .
C12 C 0.2014(5) 0.7358(2) 0.1275(3) 0.0352(10) Uani 1 1 d . . . . .
H12 H 0.137608 0.770270 0.072948 0.042 Uiso 1 1 calc R . . . .
C13 C 0.5871(4) 0.91200(19) 0.2748(3) 0.0204(7) Uani 1 1 d . . . . .
H13 H 0.486995 0.936637 0.231559 0.024 Uiso 1 1 calc R . . . .
C14 C 0.6895(6) 1.0101(3) 0.4212(3) 0.0390(10) Uani 1 1 d . . . . .
H14A H 0.581819 1.032532 0.381222 0.059 Uiso 1 1 calc GR . . . .
H14B H 0.768476 1.049237 0.429095 0.059 Uiso 1 1 calc GR . . . .
H14C H 0.710395 0.994894 0.487685 0.059 Uiso 1 1 calc GR . . . .
C15 C 0.8289(4) 0.8874(2) 0.4076(3) 0.0211(7) Uani 1 1 d . . . . .
H15 H 0.925535 0.891026 0.471292 0.025 Uiso 1 1 calc R . . . .
C16 C 0.7891(4) 0.8295(2) 0.3362(3) 0.0209(7) Uani 1 1 d . . . . .
H16 H 0.854570 0.786020 0.343002 0.025 Uiso 1 1 calc R . . . .
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'
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
O1 V1 O5 178.07(11) . .
O1 V1 N1 94.14(11) . .
O1 V1 N3 92.48(11) . .
O1 V1 N5 91.86(11) . .
O1 V1 N7 92.29(11) . .
O5 V1 N1 87.79(10) . .
O5 V1 N3 87.54(10) . .
O5 V1 N5 88.16(10) . .
O5 V1 N7 85.78(10) . .
N1 V1 N3 89.33(10) . .
N1 V1 N7 173.57(10) . .
N3 V1 N7 90.62(10) . .
N5 V1 N1 89.13(11) . .
N5 V1 N3 175.49(10) . .
N5 V1 N7 90.43(10) . .
O2 S1 O3 111.35(14) . .
O2 S1 O4 111.11(13) . .
O2 S1 O5 106.89(13) . .
O3 S1 O4 111.59(13) . .
O3 S1 O5 107.71(13) . .
O4 S1 O5 107.96(13) . .
S1 O5 V1 174.75(15) . .
C1 N1 V1 126.0(2) . .
C1 N1 C4 105.8(3) . .
C4 N1 V1 128.2(2) . .
C1 N2 C2 127.5(3) . .
C1 N2 C3 108.2(3) . .
C3 N2 C2 124.2(3) . .
C5 N3 V1 122.4(2) . .
C5 N3 C8 105.8(3) . .
C8 N3 V1 131.4(2) . .
C5 N4 C6 125.3(3) . .
C5 N4 C7 107.5(3) . .
C7 N4 C6 127.1(3) . .
C9 N5 V1 130.8(2) . .
C9 N5 C12 105.6(3) . .
C12 N5 V1 123.2(2) . .
C9 N6 C10 127.4(3) . .
C9 N6 C11 106.9(3) . .
C11 N6 C10 125.5(3) . .
C13 N7 V1 126.8(2) . .
C13 N7 C16 105.7(3) . .
C16 N7 V1 127.5(2) . .
C13 N8 C14 126.9(3) . .
C13 N8 C15 107.2(3) . .
C15 N8 C14 125.8(3) . .
N1 C1 N2 110.6(3) . .
N1 C1 H1 124.7 . .
N2 C1 H1 124.7 . .
N2 C2 H2A 109.5 . .
N2 C2 H2B 109.5 . .
N2 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 H3 127.1 . .
C4 C3 N2 105.8(3) . .
C4 C3 H3 127.1 . .
N1 C4 H4 125.2 . .
C3 C4 N1 109.5(3) . .
C3 C4 H4 125.2 . .
N3 C5 N4 111.2(3) . .
N3 C5 H5 124.4 . .
N4 C5 H5 124.4 . .
N4 C6 H6A 109.5 . .
N4 C6 H6B 109.5 . .
N4 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N4 C7 H7 126.9 . .
C8 C7 N4 106.2(3) . .
C8 C7 H7 126.9 . .
N3 C8 H8 125.3 . .
C7 C8 N3 109.3(3) . .
C7 C8 H8 125.3 . .
N5 C9 N6 111.7(3) . .
N5 C9 H9 124.2 . .
N6 C9 H9 124.2 . .
N6 C10 H10A 109.5 . .
N6 C10 H10B 109.5 . .
N6 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N6 C11 H11 126.6 . .
C12 C11 N6 106.8(3) . .
C12 C11 H11 126.6 . .
N5 C12 H12 125.6 . .
C11 C12 N5 108.8(3) . .
C11 C12 H12 125.6 . .
N7 C13 N8 110.6(3) . .
N7 C13 H13 124.7 . .
N8 C13 H13 124.7 . .
N8 C14 H14A 109.5 . .
N8 C14 H14B 109.5 . .
N8 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N8 C15 H15 126.5 . .
C16 C15 N8 107.0(3) . .
C16 C15 H15 126.5 . .
N7 C16 H16 125.3 . .
C15 C16 N7 109.4(3) . .
C15 C16 H16 125.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.604(2) .
V1 O5 2.015(2) .
V1 N1 2.105(3) .
V1 N3 2.120(3) .
V1 N5 2.105(3) .
V1 N7 2.130(3) .
S1 O2 1.467(2) .
S1 O3 1.468(2) .
S1 O4 1.469(2) .
S1 O5 1.512(2) .
N1 C1 1.325(4) .
N1 C4 1.386(4) .
N2 C1 1.345(4) .
N2 C2 1.457(4) .
N2 C3 1.371(5) .
N3 C5 1.325(4) .
N3 C8 1.375(4) .
N4 C5 1.343(4) .
N4 C6 1.461(4) .
N4 C7 1.370(4) .
N5 C9 1.310(4) .
N5 C12 1.393(4) .
N6 C9 1.338(4) .
N6 C10 1.459(4) .
N6 C11 1.374(5) .
N7 C13 1.333(4) .
N7 C16 1.367(4) .
N8 C13 1.348(4) .
N8 C14 1.464(5) .
N8 C15 1.358(5) .
C1 H1 0.9300 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3 0.9300 .
C3 C4 1.360(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7 0.9300 .
C7 C8 1.364(5) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11 0.9300 .
C11 C12 1.344(5) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15 0.9300 .
C15 C16 1.352(5) .
C16 H16 0.9300 .
