#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179163 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/24/4312474.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_4312474
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 Cu N2 O8 Te V2'
_chemical_formula_weight         601.22
_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                 97.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2193(18)
_cell_length_b                   7.9853(16)
_cell_length_c                   21.401(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      1.92
_cell_volume                     1561.9(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 '100x100 microns'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5746
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_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    4.400
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.864
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0270
_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)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                2870
_reflns_number_total             3494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034272psi20030424_091810.cif
_cod_data_source_block           x17b
_cod_database_code               4312474
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 0.22045(3) 0.52924(4) 0.226058(12) 0.01747(9) Uani 1 1 d . . .
Cu Cu 0.42301(5) 0.41129(7) 0.12656(2) 0.01698(13) Uani 1 1 d . . .
V2 V 0.60752(7) 0.64759(9) 0.25267(3) 0.01717(16) Uani 1 1 d . . .
V1 V -0.06961(7) 0.43732(9) 0.30216(3) 0.01797(16) Uani 1 1 d . . .
O8 O 0.2272(3) 0.4366(4) 0.14744(13) 0.0205(6) Uani 1 1 d . . .
O5 O 0.4880(3) 0.5700(4) 0.19282(14) 0.0241(7) Uani 1 1 d . . .
O1 O 0.0343(3) 0.4383(4) 0.23577(15) 0.0275(7) Uani 1 1 d . . .
O4 O 0.7464(4) 0.4983(5) 0.27484(16) 0.0352(9) Uani 1 1 d . . .
O6 O 0.5160(3) 0.6847(4) 0.31138(14) 0.0240(7) Uani 1 1 d . . .
O2 O 0.6856(3) 0.8352(4) 0.22728(14) 0.0273(7) Uani 1 1 d . . .
O7 O -0.0759(3) 0.2436(4) 0.33059(15) 0.0308(8) Uani 1 1 d . . .
O3 O 0.0057(4) 0.5574(5) 0.35699(17) 0.0412(9) Uani 1 1 d . . .
N2 N 0.3485(4) 0.2778(5) 0.05041(16) 0.0198(7) Uani 1 1 d . . .
N1 N 0.6111(4) 0.4015(5) 0.08844(16) 0.0210(8) Uani 1 1 d . . .
C11 C 0.4504(4) 0.2537(5) 0.01130(19) 0.0178(8) Uani 1 1 d . . .
C12 C 0.5922(4) 0.3210(6) 0.03172(19) 0.0196(8) Uani 1 1 d . . .
C4 C 0.7056(5) 0.3000(6) -0.0053(2) 0.0241(9) Uani 1 1 d . . .
C3 C 0.8431(5) 0.3652(7) 0.0186(2) 0.0303(11) Uani 1 1 d . . .
H3A H 0.9206 0.3574 -0.0050 0.036 Uiso 1 1 calc R . .
C1 C 0.7439(5) 0.4573(6) 0.1099(2) 0.0280(10) Uani 1 1 d . . .
H1A H 0.7581 0.5103 0.1490 0.034 Uiso 1 1 calc R . .
C5 C 0.6754(5) 0.2141(6) -0.0645(2) 0.0300(11) Uani 1 1 d . . .
H5A H 0.7491 0.2022 -0.0899 0.036 Uiso 1 1 calc R . .
C7 C 0.4235(5) 0.1671(6) -0.0459(2) 0.0238(9) Uani 1 1 d . . .
C8 C 0.2813(5) 0.1028(6) -0.0620(2) 0.0299(11) Uani 1 1 d . . .
H8A H 0.2570 0.0455 -0.0998 0.036 Uiso 1 1 calc R . .
C9 C 0.1796(5) 0.1248(6) -0.0220(2) 0.0323(11) Uani 1 1 d . . .
H9A H 0.0858 0.0818 -0.0323 0.039 Uiso 1 1 calc R . .
C2 C 0.8635(5) 0.4398(7) 0.0762(2) 0.0323(11) Uani 1 1 d . . .
H2A H 0.9555 0.4786 0.0930 0.039 Uiso 1 1 calc R . .
C10 C 0.2161(5) 0.2125(6) 0.0347(2) 0.0274(10) Uani 1 1 d . . .
H10A H 0.1461 0.2252 0.0619 0.033 Uiso 1 1 calc R . .
C6 C 0.5407(5) 0.1499(6) -0.0838(2) 0.0307(11) Uani 1 1 d . . .
H6A H 0.5238 0.0937 -0.1221 0.037 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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 94.89(13) . . ?
O8 Te O2 94.66(13) . 2_645 ?
O1 Te O2 89.27(14) . 2_645 ?
O8 Te O7 84.75(12) . 2 ?
O1 Te O7 82.99(13) . 2 ?
O2 Te O7 172.16(12) 2_645 2 ?
O8 Cu O5 88.35(12) . . ?
O8 Cu N2 90.74(13) . . ?
O5 Cu N2 171.50(14) . . ?
O8 Cu N1 169.02(13) . . ?
O5 Cu N1 97.00(14) . . ?
N2 Cu N1 82.55(14) . . ?
O8 Cu O6 96.63(12) . 2_645 ?
O5 Cu O6 93.66(12) . 2_645 ?
N2 Cu O6 94.84(13) . 2_645 ?
N1 Cu O6 92.62(13) . 2_645 ?
O6 V2 O5 107.37(16) . . ?
O6 V2 O4 110.23(16) . . ?
O5 V2 O4 109.42(17) . . ?
O6 V2 O2 110.70(15) . . ?
O5 V2 O2 109.07(15) . . ?
O4 V2 O2 110.00(17) . . ?
O3 V1 O7 108.69(18) . . ?
O3 V1 O4 112.22(18) . 1_455 ?
O7 V1 O4 107.20(17) . 1_455 ?
O3 V1 O1 110.41(18) . . ?
O7 V1 O1 109.69(16) . . ?
O4 V1 O1 108.56(15) 1_455 . ?
Te O8 Cu 113.45(14) . . ?
V2 O5 Cu 154.3(2) . . ?
V1 O1 Te 131.63(18) . . ?
V2 O4 V1 153.4(2) . 1_655 ?
V2 O6 Cu 118.84(16) . 2_655 ?
V2 O2 Te 132.31(16) . 2_655 ?
V1 O7 Te 121.44(17) . 2_545 ?
C10 N2 C11 118.5(4) . . ?
C10 N2 Cu 128.5(3) . . ?
C11 N2 Cu 112.9(3) . . ?
C1 N1 C12 118.1(4) . . ?
C1 N1 Cu 130.6(3) . . ?
C12 N1 Cu 111.2(3) . . ?
N2 C11 C7 123.6(4) . . ?
N2 C11 C12 116.1(4) . . ?
C7 C11 C12 120.3(4) . . ?
N1 C12 C4 122.7(4) . . ?
N1 C12 C11 117.1(4) . . ?
C4 C12 C11 120.2(4) . . ?
C12 C4 C3 117.0(4) . . ?
C12 C4 C5 118.9(4) . . ?
C3 C4 C5 124.1(4) . . ?
C2 C3 C4 120.3(4) . . ?
N1 C1 C2 122.7(4) . . ?
C6 C5 C4 120.9(4) . . ?
C11 C7 C8 116.5(4) . . ?
C11 C7 C6 118.6(4) . . ?
C8 C7 C6 124.9(4) . . ?
C9 C8 C7 119.7(4) . . ?
C8 C9 C10 120.1(4) . . ?
C3 C2 C1 119.0(4) . . ?
N2 C10 C9 121.5(4) . . ?
C5 C6 C7 121.2(4) . . ?
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 1.847(3) . ?
Te O1 1.900(3) . ?
Te O2 1.980(3) 2_645 ?
Te O7 2.399(3) 2 ?
Cu O8 1.927(3) . ?
Cu O5 1.937(3) . ?
Cu N2 1.993(3) . ?
Cu N1 2.013(3) . ?
Cu O6 2.271(3) 2_645 ?
V2 O6 1.630(3) . ?
V2 O5 1.693(3) . ?
V2 O4 1.768(3) . ?
V2 O2 1.778(3) . ?
V1 O3 1.601(4) . ?
V1 O7 1.666(3) . ?
V1 O4 1.787(3) 1_455 ?
V1 O1 1.815(3) . ?
O4 V1 1.787(3) 1_655 ?
O6 Cu 2.271(3) 2_655 ?
O2 Te 1.980(3) 2_655 ?
O7 Te 2.399(3) 2_545 ?
N2 C10 1.330(6) . ?
N2 C11 1.351(5) . ?
N1 C1 1.327(5) . ?
N1 C12 1.364(5) . ?
C11 C7 1.401(6) . ?
C11 C12 1.427(6) . ?
C12 C4 1.402(6) . ?
C4 C3 1.404(6) . ?
C4 C5 1.435(6) . ?
C3 C2 1.360(7) . ?
C1 C2 1.402(6) . ?
C5 C6 1.357(7) . ?
C7 C8 1.408(6) . ?
C7 C6 1.439(6) . ?
C8 C9 1.362(7) . ?
C9 C10 1.403(6) . ?
