#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179163 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/24/4312475.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_4312475
loop_
_publ_author_name
'Dongrong Xiao'
'Yangguang Li'
'Enbo Wang'
'Shutao Wang'
'Yu Hou'
'Gejihu De'
'Changwen Hu'
_publ_section_title
;
 Two Novel Vanadium Tellurites Covalently Bonded with Metal-Organic
 Complex Moieties: M(phen)V2TeO8 (M = Cu, Ni)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7652
_journal_page_last               7657
_journal_paper_doi               10.1021/ic034272p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H8 N2 Ni O8 Te V2'
_chemical_formula_weight         596.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2163(18)
_cell_length_b                   7.9897(16)
_cell_length_c                   21.386(4)
_cell_measurement_reflns_used    6320
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.92
_cell_volume                     1561.2(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6320
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    4.246
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.678
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0433P)²+0.0786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                3199
_reflns_number_total             3578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034272psi20030424_092004.cif
_cod_data_source_block           xdr9a
_cod_original_cell_volume        1561.3(5)
_cod_database_code               4312475
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te Te 0.22046(2) 0.52925(3) 0.226028(8) 0.01735(8) Uani 1 1 d . . .
Ni Ni 0.42305(4) 0.41128(5) 0.126560(16) 0.01380(10) Uani 1 1 d . . .
V1 V -0.06963(5) 0.43754(7) 0.30212(2) 0.01792(12) Uani 1 1 d . . .
V2 V 0.60747(5) 0.64768(6) 0.25268(2) 0.01692(12) Uani 1 1 d . . .
O1 O 0.0340(3) 0.4385(3) 0.23600(11) 0.0285(5) Uani 1 1 d . . .
O2 O 0.6847(3) 0.8349(3) 0.22725(10) 0.0286(5) Uani 1 1 d . . .
O3 O 0.0064(3) 0.5569(3) 0.35710(13) 0.0408(7) Uani 1 1 d . . .
O4 O 0.7460(3) 0.4989(3) 0.27489(12) 0.0355(6) Uani 1 1 d . . .
O5 O 0.4878(2) 0.5708(3) 0.19292(10) 0.0245(5) Uani 1 1 d . . .
O6 O 0.5162(2) 0.6854(3) 0.31123(10) 0.0242(5) Uani 1 1 d . . .
O7 O -0.0758(3) 0.2430(3) 0.33039(11) 0.0305(5) Uani 1 1 d . . .
O8 O 0.2276(2) 0.4372(3) 0.14776(10) 0.0216(5) Uani 1 1 d . . .
C1 C 0.7446(4) 0.4572(5) 0.11011(16) 0.0287(7) Uani 1 1 d . . .
H1 H 0.7590 0.5099 0.1492 0.029 Uiso 1 1 calc R . .
C2 C 0.8637(4) 0.4399(5) 0.07627(17) 0.0333(8) Uani 1 1 d . . .
H2 H 0.9555 0.4796 0.0930 0.033 Uiso 1 1 calc R . .
C3 C 0.8444(4) 0.3646(5) 0.01867(17) 0.0305(8) Uani 1 1 d . . .
H3 H 0.9223 0.3556 -0.0047 0.030 Uiso 1 1 calc R . .
C4 C 0.7057(3) 0.3002(4) -0.00530(14) 0.0238(7) Uani 1 1 d . . .
C5 C 0.6747(4) 0.2147(5) -0.06449(15) 0.0302(8) Uani 1 1 d . . .
H5 H 0.7482 0.2034 -0.0901 0.030 Uiso 1 1 calc R . .
C6 C 0.5397(4) 0.1497(5) -0.08394(15) 0.0309(8) Uani 1 1 d . . .
H6 H 0.5228 0.0936 -0.1223 0.031 Uiso 1 1 calc R . .
C7 C 0.4237(4) 0.1668(4) -0.04594(14) 0.0236(7) Uani 1 1 d . . .
C8 C 0.2822(4) 0.1029(4) -0.06216(15) 0.0300(8) Uani 1 1 d . . .
H8 H 0.2581 0.0455 -0.0999 0.030 Uiso 1 1 calc R . .
C9 C 0.1797(4) 0.1256(5) -0.02197(17) 0.0321(8) Uani 1 1 d . . .
H9 H 0.0856 0.0832 -0.0324 0.032 Uiso 1 1 calc R . .
C10 C 0.2159(4) 0.2121(4) 0.03448(15) 0.0263(7) Uani 1 1 d . . .
H10 H 0.1457 0.2245 0.0617 0.026 Uiso 1 1 calc R . .
C11 C 0.4508(3) 0.2538(4) 0.01131(14) 0.0190(6) Uani 1 1 d . . .
C12 C 0.5931(3) 0.3209(4) 0.03159(13) 0.0191(6) Uani 1 1 d . . .
N1 N 0.6111(3) 0.4008(3) 0.08841(12) 0.0209(5) Uani 1 1 d . . .
N2 N 0.3483(3) 0.2774(3) 0.05036(12) 0.0194(5) 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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
O8 Te O1 95.17(10) . . ?
O8 Te O2 94.56(10) . 2_645 ?
O1 Te O2 89.44(11) . 2_645 ?
O8 Te O7 84.85(9) . 2 ?
O1 Te O7 82.92(10) . 2 ?
O2 Te O7 172.24(9) 2_645 2 ?
O8 Ni O5 87.99(9) . . ?
O8 Ni N2 90.93(10) . . ?
O5 Ni N2 171.41(10) . . ?
O8 Ni N1 169.19(10) . . ?
O5 Ni N1 97.18(10) . . ?
N2 Ni N1 82.54(11) . . ?
O8 Ni O6 96.57(9) . 2_645 ?
O5 Ni O6 93.71(9) . 2_645 ?
N2 Ni O6 94.88(10) . 2_645 ?
N1 Ni O6 92.58(9) . 2_645 ?
O3 V1 O7 108.69(14) . . ?
O3 V1 O4 112.39(14) . 1_455 ?
O7 V1 O4 107.26(13) . 1_455 ?
O3 V1 O1 110.27(14) . . ?
O7 V1 O1 109.46(12) . . ?
O4 V1 O1 108.69(12) 1_455 . ?
O6 V2 O5 107.31(12) . . ?
O6 V2 O4 110.31(13) . . ?
O5 V2 O4 109.66(13) . . ?
O6 V2 O2 110.43(12) . . ?
O5 V2 O2 108.85(11) . . ?
O4 V2 O2 110.23(13) . . ?
V1 O1 Te 131.82(14) . . ?
V2 O2 Te 132.34(12) . 2_655 ?
V2 O4 V1 153.49(18) . 1_655 ?
V2 O5 Ni 153.96(15) . . ?
V2 O6 Ni 119.09(12) . 2_655 ?
V1 O7 Te 121.62(12) . 2_545 ?
Te O8 Ni 113.81(11) . . ?
N1 C1 C2 122.5(3) . . ?
C3 C2 C1 119.6(3) . . ?
C2 C3 C4 119.7(3) . . ?
C12 C4 C3 117.2(3) . . ?
C12 C4 C5 118.6(3) . . ?
C3 C4 C5 124.1(3) . . ?
C6 C5 C4 121.3(3) . . ?
C5 C6 C7 120.7(3) . . ?
C8 C7 C11 116.8(3) . . ?
C8 C7 C6 124.4(3) . . ?
C11 C7 C6 118.8(3) . . ?
C9 C8 C7 119.5(3) . . ?
C8 C9 C10 120.2(3) . . ?
N2 C10 C9 121.6(3) . . ?
N2 C11 C7 123.3(3) . . ?
N2 C11 C12 116.6(3) . . ?
C7 C11 C12 120.1(3) . . ?
N1 C12 C4 123.2(3) . . ?
N1 C12 C11 116.4(3) . . ?
C4 C12 C11 120.3(3) . . ?
C1 N1 C12 117.8(3) . . ?
C1 N1 Ni 130.5(2) . . ?
C12 N1 Ni 111.7(2) . . ?
C10 N2 C11 118.6(3) . . ?
C10 N2 Ni 128.8(2) . . ?
C11 N2 Ni 112.6(2) . . ?
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
Te O8 1.837(2) . ?
Te O1 1.903(2) . ?
Te O2 1.987(2) 2_645 ?
Te O7 2.394(3) 2 ?
Ni O8 1.925(2) . ?
Ni O5 1.942(2) . ?
Ni N2 1.995(3) . ?
Ni N1 2.011(3) . ?
Ni O6 2.268(2) 2_645 ?
V1 O3 1.603(3) . ?
V1 O7 1.671(2) . ?
V1 O4 1.791(3) 1_455 ?
V1 O1 1.807(2) . ?
V2 O6 1.626(2) . ?
V2 O5 1.691(2) . ?
V2 O4 1.763(3) . ?
V2 O2 1.772(2) . ?
O2 Te 1.987(2) 2_655 ?
O4 V1 1.791(3) 1_655 ?
O6 Ni 2.268(2) 2_655 ?
O7 Te 2.394(3) 2_545 ?
C1 N1 1.336(4) . ?
C1 C2 1.398(5) . ?
C2 C3 1.362(5) . ?
C3 C4 1.411(5) . ?
C4 C12 1.393(4) . ?
C4 C5 1.434(5) . ?
C5 C6 1.362(5) . ?
C6 C7 1.432(5) . ?
C7 C8 1.401(5) . ?
C7 C11 1.402(4) . ?
C8 C9 1.370(5) . ?
C9 C10 1.393(5) . ?
C10 N2 1.330(4) . ?
C11 N2 1.353(4) . ?
C11 C12 1.431(4) . ?
C12 N1 1.364(4) . ?
