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#$Date: 2016-03-23 02:30:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179183 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/30/4313068.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_4313068
loop_
_publ_author_name
'Zhimin Dai'
'Xiaobo Chen'
'Zhan Shi'
'Dong Zhang'
'Guanghua Li'
'Shouhua Feng'
_publ_contact_author
;
      Feng,Shouhua
      Department of Chemistry
      Jilin University
      Changchun, 130023
      P. R. China
;
_publ_contact_author_email       shfeng@mail.jlu.edu.cn
_publ_contact_author_fax         86-431-5671974
_publ_contact_author_phone       86-431-5671974
_publ_section_title
;
 Hydrothermal Syntheses and Crystal Structures of Complex-Linked
 Three-Dimensional Coordination Vanadium Selenites:
 M(4,4'-bipy)(H2O)V2Se2O10 (M = Co, Ni)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              908
_journal_page_last               912
_journal_paper_doi               10.1021/ic026037x
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H10 Co N2 O11 Se2 V2'
_chemical_formula_weight         652.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.704(2)
_cell_angle_beta                 73.5180(10)
_cell_angle_gamma                75.645(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9665(3)
_cell_length_b                   8.1974(3)
_cell_length_c                   13.8096(4)
_cell_measurement_temperature    293(2)
_cell_volume                     837.76(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4118
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    6.481
_exptl_absorpt_correction_T_max  0.5634
_exptl_absorpt_correction_T_min  0.4431
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Dark_red
_exptl_crystal_density_diffrn    2.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0263P)²+2.1504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                2167
_reflns_number_total             2396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026037x-2_s1_2.cif
_cod_data_source_block           CoVSe
_cod_database_code               4313068
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.21860(8) -0.48923(8) 0.14850(4) 0.01610(16) Uani 1 1 d . . .
V1 V 0.47144(10) -0.20308(9) 0.02777(5) 0.01146(18) Uani 1 1 d . . .
V2 V -0.04316(10) -0.15268(10) 0.28313(5) 0.01468(19) Uani 1 1 d . . .
Se1 Se 0.13495(6) 0.12505(6) 0.13059(3) 0.01675(14) Uani 1 1 d . . .
Se2 Se -0.34476(6) -0.01652(6) 0.15598(3) 0.01822(14) Uani 1 1 d . . .
O1 O 0.3171(4) -0.2742(4) 0.1176(2) 0.0184(7) Uani 1 1 d . . .
O2 O 0.0103(4) -0.3588(4) 0.2635(2) 0.0212(7) Uani 1 1 d . . .
O3 O 0.0653(5) -0.3807(5) 0.0421(3) 0.0395(10) Uani 1 1 d D . .
O4 O 0.5941(4) -0.3771(4) -0.0328(2) 0.0191(7) Uani 1 1 d . . .
O5 O 0.3688(4) 0.0534(4) 0.0870(2) 0.0149(7) Uani 1 1 d . . .
O6 O 0.1029(5) 0.3128(4) 0.1783(3) 0.0326(9) Uani 1 1 d . . .
O7 O 0.0970(4) 0.0148(4) 0.2416(2) 0.0193(7) Uani 1 1 d . . .
O8 O -0.1290(4) -0.0798(4) 0.1639(2) 0.0219(7) Uani 1 1 d . . .
O9 O -0.3072(4) 0.1222(4) 0.0585(2) 0.0189(7) Uani 1 1 d . . .
O10 O -0.3481(4) -0.1943(4) 0.1001(2) 0.0198(7) Uani 1 1 d . . .
O11 O -0.2308(4) -0.1062(4) 0.3705(2) 0.0251(8) Uani 1 1 d . . .
N1 N 0.3886(5) -0.5777(5) 0.2459(3) 0.0241(9) Uani 1 1 d . . .
N2 N 0.8889(5) -0.8034(5) 0.6062(3) 0.0218(9) Uani 1 1 d . . .
C1 C 0.5526(8) -0.5516(8) 0.2294(4) 0.0405(15) Uani 1 1 d . . .
H1 H 0.5998 -0.4994 0.1691 0.080 Uiso 1 1 calc . . .
C2 C 0.6566(8) -0.5963(8) 0.2953(5) 0.0421(15) Uani 1 1 d . . .
H2 H 0.7698 -0.5730 0.2798 0.080 Uiso 1 1 calc . . .
C3 C 0.5925(7) -0.6761(6) 0.3846(3) 0.0230(11) Uani 1 1 d . . .
C4 C 0.4281(9) -0.7142(12) 0.3989(5) 0.070(3) Uani 1 1 d . . .
H4 H 0.3821 -0.7754 0.4554 0.080 Uiso 1 1 calc . . .
C5 C 0.3320(9) -0.6610(11) 0.3288(5) 0.066(2) Uani 1 1 d . . .
H5 H 0.2200 -0.6857 0.3411 0.080 Uiso 1 1 calc . . .
C6 C 0.9550(10) -0.7417(13) 0.5175(5) 0.087(3) Uani 1 1 d . . .
H6 H 1.0707 -0.7244 0.5029 0.080 Uiso 1 1 calc . . .
C7 C 0.8648(10) -0.7005(14) 0.4441(5) 0.093(4) Uani 1 1 d . . .
H7 H 0.9205 -0.6577 0.3824 0.080 Uiso 1 1 calc . . .
C8 C 0.6956(6) -0.7219(6) 0.4613(4) 0.0231(11) Uani 1 1 d . . .
C9 C 0.6272(8) -0.7877(10) 0.5535(5) 0.055(2) Uani 1 1 d . . .
H9 H 0.5119 -0.8063 0.5699 0.080 Uiso 1 1 calc . . .
C10 C 0.7266(9) -0.8271(10) 0.6228(5) 0.055(2) Uani 1 1 d . . .
H10 H 0.6755 -0.8729 0.6845 0.080 Uiso 1 1 calc . . .
H3B H -0.035(7) -0.313(8) 0.070(5) 0.080 Uiso 1 1 d D . .
H3A H 0.056(9) -0.451(8) 0.013(6) 0.080 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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O6 Co1 O4 87.94(13) 1_545 2_645 ?
O6 Co1 O1 175.37(14) 1_545 . ?
O4 Co1 O1 94.83(12) 2_645 . ?
O6 Co1 O2 88.58(13) 1_545 . ?
O4 Co1 O2 175.21(12) 2_645 . ?
O1 Co1 O2 88.43(12) . . ?
O6 Co1 N1 93.65(16) 1_545 . ?
O4 Co1 N1 90.50(14) 2_645 . ?
O1 Co1 N1 90.04(14) . . ?
O2 Co1 N1 93.00(14) . . ?
O6 Co1 O3 92.45(16) 1_545 . ?
O4 Co1 O3 87.94(14) 2_645 . ?
O1 Co1 O3 83.95(14) . . ?
O2 Co1 O3 88.92(14) . . ?
N1 Co1 O3 173.65(16) . . ?
O4 V1 O1 102.06(16) . . ?
O4 V1 O9 99.52(14) . 2 ?
O1 V1 O9 93.49(14) . 2 ?
O4 V1 O10 93.49(14) . 1_655 ?
O1 V1 O10 101.86(14) . 1_655 ?
O9 V1 O10 157.36(13) 2 1_655 ?
O4 V1 O5 165.15(13) . . ?
O1 V1 O5 92.24(13) . . ?
O9 V1 O5 83.39(12) 2 . ?
O10 V1 O5 79.51(12) 1_655 . ?
O4 V1 O5 89.75(13) . 2_655 ?
O1 V1 O5 167.10(14) . 2_655 ?
O9 V1 O5 79.30(11) 2 2_655 ?
O10 V1 O5 82.33(12) 1_655 2_655 ?
O5 V1 O5 76.42(12) . 2_655 ?
O11 V2 O2 108.31(17) . . ?
O11 V2 O7 118.95(16) . . ?
O2 V2 O7 131.37(15) . . ?
O11 V2 O8 100.06(15) . . ?
O2 V2 O8 98.05(15) . . ?
O7 V2 O8 85.01(13) . . ?
O11 V2 N2 91.60(15) . 2_646 ?
O2 V2 N2 88.92(15) . 2_646 ?
O7 V2 N2 79.38(14) . 2_646 ?
O8 V2 N2 163.71(14) . 2_646 ?
O6 Se1 O7 98.07(17) . . ?
O6 Se1 O5 104.75(15) . . ?
O7 Se1 O5 99.50(14) . . ?
O8 Se2 O9 97.18(15) . . ?
O8 Se2 O10 96.94(15) . . ?
O9 Se2 O10 104.26(15) . . ?
V1 O1 Co1 138.08(18) . . ?
V2 O2 Co1 126.33(17) . . ?
Co1 O3 H3B 113(5) . . ?
Co1 O3 H3A 109(6) . . ?
H3B O3 H3A 114(6) . . ?
V1 O4 Co1 154.64(19) . 2_645 ?
Se1 O5 V1 116.74(14) . . ?
Se1 O5 V1 119.93(15) . 2_655 ?
V1 O5 V1 103.58(12) . 2_655 ?
Se1 O6 Co1 137.9(2) . 1_565 ?
Se1 O7 V2 128.99(17) . . ?
Se2 O8 V2 128.69(18) . . ?
Se2 O9 V1 123.85(16) . 2 ?
Se2 O10 V1 123.40(17) . 1_455 ?
C5 N1 C1 115.7(4) . . ?
C5 N1 Co1 120.3(4) . . ?
C1 N1 Co1 124.0(3) . . ?
C6 N2 C10 115.5(5) . . ?
C6 N2 V2 119.7(4) . 2_646 ?
C10 N2 V2 124.7(3) . 2_646 ?
N1 C1 C2 124.3(5) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 116.4(5) . . ?
C2 C3 C8 122.3(5) . . ?
C4 C3 C8 121.4(5) . . ?
C3 C4 C5 119.6(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 124.2(5) . . ?
N1 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
N2 C6 C7 124.4(6) . . ?
N2 C6 H6 117.8 . . ?
C7 C6 H6 117.8 . . ?
C8 C7 C6 120.4(6) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 115.2(5) . . ?
C7 C8 C3 122.0(5) . . ?
C9 C8 C3 122.8(5) . . ?
C8 C9 C10 121.0(5) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
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
Co1 O6 2.019(3) 1_545 ?
Co1 O4 2.020(3) 2_645 ?
Co1 O1 2.070(3) . ?
Co1 O2 2.073(3) . ?
Co1 N1 2.137(4) . ?
Co1 O3 2.174(4) . ?
V1 O4 1.647(3) . ?
V1 O1 1.665(3) . ?
V1 O9 1.977(3) 2 ?
V1 O10 1.987(3) 1_655 ?
V1 O5 2.187(3) . ?
V1 O5 2.231(3) 2_655 ?
V2 O11 1.612(3) . ?
V2 O2 1.661(3) . ?
V2 O7 1.934(3) . ?
V2 O8 1.955(3) . ?
V2 N2 2.177(4) 2_646 ?
Se1 O6 1.653(3) . ?
Se1 O7 1.710(3) . ?
Se1 O5 1.747(3) . ?
Se2 O8 1.701(3) . ?
Se2 O9 1.704(3) . ?
Se2 O10 1.709(3) . ?
O3 H3B 0.86(4) . ?
O3 H3A 0.76(3) . ?
O4 Co1 2.020(3) 2_645 ?
O5 V1 2.231(3) 2_655 ?
O6 Co1 2.019(3) 1_565 ?
O9 V1 1.977(3) 2 ?
O10 V1 1.987(3) 1_455 ?
N1 C5 1.313(7) . ?
N1 C1 1.330(7) . ?
N2 C6 1.307(7) . ?
N2 C10 1.309(7) . ?
N2 V2 2.177(4) 2_646 ?
C1 C2 1.370(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(8) . ?
C3 C8 1.490(7) . ?
C4 C5 1.379(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.378(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.354(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.363(8) . ?
C9 C10 1.379(8) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
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
O3 H3B O8 0.86(4) 2.24(5) 2.926(5) 137(6) .
O3 H3B O10 0.86(4) 2.37(5) 3.164(5) 155(6) .
O3 H3A O3 0.76(3) 2.15(4) 2.880(7) 160(7) 2_545
