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#$Date: 2022-03-25 09:56:23 +0200 (Fri, 25 Mar 2022) $
#$Revision: 273970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/48/8104856.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_8104856
loop_
_publ_author_name
'Yang, Bingchuan'
'Lv, Xueyan'
'Liu, Gang'
'Liu, Rutao'
_publ_section_title
;
 Crystal structure of
 catena-poly[(5H-pyrrolo[3,2-b:4,5-b′]dipyridine-κ2
 N,N′)-(μ4-hexaoxidodivanadato)dizinc(II)],C10H9N3O6V2Zn
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              447
_journal_page_last               449
_journal_paper_doi               10.1515/ncrs-2020-0604
_journal_volume                  236
_journal_year                    2021
_chemical_formula_sum            'C10 H9 N3 O6 V2 Zn'
_chemical_formula_weight         434.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 95.025(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.0106(17)
_cell_length_b                   29.957(6)
_cell_length_c                   12.050(3)
_cell_measurement_reflns_used    1574
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.640
_cell_measurement_theta_min      2.996
_cell_volume                     2880.6(11)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.937
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8830
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.479
_diffrn_reflns_theta_min         2.174
_exptl_absorpt_coefficient_mu    2.953
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   0602
_exptl_transmission_factor_min   0.548
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0512
_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)+(0.1132P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2282
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0604_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        2880.6(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8104856
_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   0.550
_shelx_estimated_absorpt_t_max   0.604
loop_
_space_group_symop_operation_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_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
C1 C 0.1988(9) 0.4502(2) 0.3684(6) 0.0461(16) Uani 1 1 d . . . . .
H1 H 0.166675 0.452583 0.440473 0.055 Uiso 1 1 calc R U . . .
C2 C 0.2184(10) 0.4881(2) 0.3096(7) 0.0539(19) Uani 1 1 d . . . . .
H2 H 0.199601 0.515954 0.340344 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2672(10) 0.4844(2) 0.2026(7) 0.0514(18) Uani 1 1 d . . . . .
H3 H 0.283273 0.509899 0.160769 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2919(10) 0.4428(2) 0.1584(6) 0.0484(17) Uani 1 1 d . . . . .
H4 H 0.322859 0.439859 0.086116 0.058 Uiso 1 1 calc R U . . .
C5 C 0.2700(8) 0.40536(19) 0.2227(5) 0.0325(13) Uani 1 1 d . . . . .
C6 C 0.2759(9) 0.3203(2) 0.2089(5) 0.0380(15) Uani 1 1 d . . . . .
C7 C 0.3209(9) 0.2870(2) 0.1342(5) 0.0414(15) Uani 1 1 d . . . . .
H7 H 0.361140 0.294659 0.066710 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3040(10) 0.2428(2) 0.1632(6) 0.0505(18) Uani 1 1 d . . . . .
H8 H 0.335352 0.220193 0.116422 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2387(10) 0.2325(2) 0.2644(6) 0.0474(17) Uani 1 1 d . . . . .
H9 H 0.220103 0.203135 0.285055 0.057 Uiso 1 1 calc R U . . .
C10 C 0.2044(9) 0.2669(2) 0.3300(5) 0.0409(15) Uani 1 1 d . . . . .
H10 H 0.165389 0.260178 0.398522 0.049 Uiso 1 1 calc R U . . .
N1 N 0.2245(6) 0.40826(16) 0.3260(4) 0.0327(11) Uani 1 1 d . . . . .
N2 N 0.2216(6) 0.31022(17) 0.3049(4) 0.0316(11) Uani 1 1 d . . . . .
N3 N 0.2993(8) 0.36405(17) 0.1734(4) 0.0462(15) Uani 1 1 d . . . . .
H3A H 0.339045 0.366013 0.109544 0.055 Uiso 1 1 calc R U . . .
O1 O 0.4147(7) 0.34645(18) 0.5235(4) 0.0611(16) Uani 1 1 d . . . . .
O2 O 0.7334(7) 0.3766(3) 0.5800(5) 0.085(2) Uani 1 1 d . . . . .
O3 O 0.4566(8) 0.43049(18) 0.5876(5) 0.0686(16) Uani 1 1 d . . . . .
O4 O 0.500000 0.3646(3) 0.750000 0.0564(19) Uani 1 2 d S T P . .
O5 O 0.0329(6) 0.34579(15) 0.5204(4) 0.0446(11) Uani 1 1 d . . . . .
O6 O 0.0230(8) 0.42726(18) 0.6023(4) 0.0651(16) Uani 1 1 d . . . . .
O7 O 0.000000 0.3567(2) 0.750000 0.0457(17) Uani 1 2 d S T P . .
V1 V 0.52194(12) 0.38141(4) 0.61144(7) 0.0310(3) Uani 1 1 d . . . . .
V2 V -0.04763(12) 0.37835(3) 0.61285(8) 0.0291(3) Uani 1 1 d . . . . .
Zn1 Zn 0.21188(9) 0.35568(2) 0.42672(5) 0.0328(2) 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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O5 Zn1 O1 104.7(2) . .
O5 Zn1 N1 123.9(2) . .
O1 Zn1 N1 113.2(2) . .
O5 Zn1 N2 113.8(2) . .
O1 Zn1 N2 105.0(2) . .
N1 Zn1 N2 94.8(2) . .
O3 V1 O1 108.9(3) . .
O3 V1 O4 112.2(3) . .
O1 V1 O4 109.4(3) . .
O3 V1 O2 110.1(4) . .
O1 V1 O2 105.2(3) . .
O4 V1 O2 110.78(19) . .
O6 V2 O5 109.2(3) . .
O6 V2 O2 111.4(4) . 1_455
O5 V2 O2 105.7(3) . 1_455
O6 V2 O7 111.2(3) . .
O5 V2 O7 110.2(2) . .
O2 V2 O7 109.0(2) 1_455 .
C5 N1 C1 117.9(5) . .
C5 N1 Zn1 123.4(4) . .
C1 N1 Zn1 118.4(4) . .
V2 O5 Zn1 131.2(3) . .
N2 C6 N3 123.5(6) . .
N2 C6 C7 121.6(6) . .
N3 C6 C7 114.8(6) . .
V2 O7 V2 137.4(4) . 2_556
C6 N2 C10 118.1(6) . .
C6 N2 Zn1 121.9(4) . .
C10 N2 Zn1 118.6(4) . .
V1 O4 V1 146.9(5) 2_656 .
N1 C5 C4 122.0(6) . .
N1 C5 N3 121.6(5) . .
C4 C5 N3 116.3(6) . .
C4 C3 C2 119.7(7) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C6 N3 C5 131.8(6) . .
C6 N3 H3A 114.1 . .
C5 N3 H3A 114.1 . .
V1 O1 Zn1 130.5(3) . .
C2 C1 N1 122.8(7) . .
C2 C1 H1 118.6 . .
N1 C1 H1 118.6 . .
V2 O2 V1 154.0(4) 1_655 .
C9 C10 N2 125.4(6) . .
C9 C10 H10 117.3 . .
N2 C10 H10 117.3 . .
C3 C4 C5 119.2(7) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C8 C7 C6 118.7(6) . .
C8 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
C10 C9 C8 117.0(6) . .
C10 C9 H9 121.5 . .
C8 C9 H9 121.5 . .
C1 C2 C3 118.4(7) . .
C1 C2 H2 120.8 . .
C3 C2 H2 120.8 . .
C7 C8 C9 119.0(7) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 1.924(5) .
Zn1 O1 1.935(5) .
Zn1 N1 1.997(5) .
Zn1 N2 2.009(5) .
V1 O3 1.579(5) .
V1 O1 1.673(5) .
V1 O4 1.768(2) .
V1 O2 1.774(6) .
V2 O6 1.580(5) .
V2 O5 1.654(4) .
V2 O2 1.765(5) 1_455
V2 O7 1.785(3) .
N1 C5 1.330(7) .
N1 C1 1.379(8) .
C6 N2 1.306(8) .
C6 N3 1.397(8) .
C6 C7 1.412(9) .
N2 C10 1.342(8) .
C5 C4 1.383(9) .
C5 N3 1.401(8) .
C3 C4 1.377(10) .
C3 C2 1.384(11) .
C3 H3 0.9300 .
N3 H3A 0.8600 .
C1 C2 1.355(10) .
C1 H1 0.9300 .
C10 C9 1.342(9) .
C10 H10 0.9300 .
C4 H4 0.9300 .
C7 C8 1.378(10) .
C7 H7 0.9300 .
C9 C8 1.402(10) .
C9 H9 0.9300 .
C2 H2 0.9300 .
C8 H8 0.9300 .
