#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:00:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179821 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/17/7011714.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_7011714
loop_
_publ_author_name
'Lu, Ying'
'Wang, Enbo'
'Yuan, Mei'
'Luan, Guoyou'
'Li, Yangguang'
'Zhang, Hong'
'Hu, Changwen'
'Yao, Yuangen'
'Qin, Yeyan'
'Chen, Yubiao'
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of a layered vanadium
 phosphate with a directly coordinated organonitrogen ligand:
 [V4O7(HPO4)2(2,2'-bipy)2]
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3029
_journal_paper_doi               10.1039/b203324k
_journal_year                    2002
_chemical_formula_sum            'C20 H18 N4 O15 P2 V4'
_chemical_formula_weight         820.08
_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                97.04(3)
_cell_angle_beta                 109.91(3)
_cell_angle_gamma                99.01(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3682(17)
_cell_length_b                   9.2153(18)
_cell_length_c                   9.5991(19)
_cell_measurement_temperature    293(2)
_cell_volume                     675.0(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP diffractometer'
_diffrn_measurement_method       'Oscillation scans'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5006
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.545
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0422
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                2336
_reflns_number_total             2863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203324k.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        675.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011714
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
V1 V 0.47245(6) 0.68487(5) 0.98109(6) 0.01974(16) Uani 1 1 d . . .
V2 V 0.05808(6) 0.77876(5) 0.87825(5) 0.01977(16) Uani 1 1 d . . .
P1 P -0.27831(9) 0.91890(8) 0.88116(8) 0.01868(19) Uani 1 1 d . . .
O1 O -0.1352(3) 0.8867(2) 0.8278(3) 0.0263(5) Uani 1 1 d . . .
O2 O 0.2236(3) 0.9742(2) 0.9691(2) 0.0260(5) Uani 1 1 d . . .
O3 O 0.6100(3) 0.7694(3) 0.8868(3) 0.0319(5) Uani 1 1 d . . .
O4 O -0.3989(3) 0.9860(3) 0.7524(3) 0.0339(6) Uani 1 1 d . . .
H1 H -0.4245 1.0596 0.7898 0.051 Uiso 1 1 calc R . .
O5 O 0.2668(3) 0.6831(3) 0.8826(3) 0.0291(5) Uani 1 1 d . . .
O6 O 0.5262(3) 0.7872(3) 1.1456(3) 0.0309(5) Uani 1 1 d . . .
O7 O 0.5000 0.5000 1.0000 0.0376(8) Uani 1 2 d S . .
O8 O 0.0330(3) 0.7120(3) 1.0171(3) 0.0341(6) Uani 1 1 d . . .
N1 N -0.1224(3) 0.5954(3) 0.7128(3) 0.0226(5) Uani 1 1 d . . .
N2 N 0.0698(3) 0.8112(3) 0.6516(3) 0.0228(5) Uani 1 1 d . . .
C1 C -0.1533(4) 0.5907(3) 0.5654(3) 0.0233(6) Uani 1 1 d . . .
C2 C -0.2787(5) 0.4779(4) 0.4541(4) 0.0345(8) Uani 1 1 d . . .
H2 H -0.290(6) 0.473(5) 0.352(5) 0.044(12) Uiso 1 1 d . . .
C3 C -0.3760(5) 0.3693(4) 0.4971(4) 0.0384(9) Uani 1 1 d . . .
H3 H -0.462(6) 0.310(5) 0.412(5) 0.042(11) Uiso 1 1 d . . .
C4 C -0.3467(5) 0.3751(4) 0.6470(5) 0.0381(8) Uani 1 1 d . . .
H4 H -0.415(6) 0.302(5) 0.689(5) 0.056(13) Uiso 1 1 d . . .
C5 C -0.2188(5) 0.4883(4) 0.7521(4) 0.0293(7) Uani 1 1 d . . .
H5 H -0.198(5) 0.498(5) 0.870(5) 0.042(12) Uiso 1 1 d . . .
C6 C -0.0441(4) 0.7105(4) 0.5292(3) 0.0236(6) Uani 1 1 d . . .
C7 C -0.0508(5) 0.7226(4) 0.3844(4) 0.0329(8) Uani 1 1 d . . .
H6 H -0.131(5) 0.661(4) 0.298(4) 0.030(10) Uiso 1 1 d . . .
C8 C 0.0616(5) 0.8371(4) 0.3656(4) 0.0378(8) Uani 1 1 d . . .
H7 H 0.055(4) 0.839(4) 0.274(4) 0.015(8) Uiso 1 1 d . . .
C9 C 0.1798(5) 0.9364(4) 0.4906(4) 0.0345(8) Uani 1 1 d . . .
H8 H 0.247(6) 1.011(5) 0.469(5) 0.048(13) Uiso 1 1 d . . .
C10 C 0.1785(4) 0.9211(4) 0.6309(4) 0.0289(7) Uani 1 1 d . . .
H9 H 0.244(4) 0.998(4) 0.721(4) 0.020(8) Uiso 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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
O6 V1 O5 108.44(12) . . ?
O6 V1 O7 109.82(9) . . ?
O5 V1 O7 110.21(9) . . ?
O6 V1 O3 108.33(12) . . ?
O5 V1 O3 109.22(12) . . ?
O7 V1 O3 110.76(9) . . ?
O8 V2 O1 99.84(12) . . ?
O8 V2 O2 105.33(12) . . ?
O1 V2 O2 88.87(10) . . ?
O8 V2 O5 94.73(12) . . ?
O1 V2 O5 165.38(10) . . ?
O2 V2 O5 88.42(10) . . ?
O8 V2 N1 93.92(12) . . ?
O1 V2 N1 85.83(10) . . ?
O2 V2 N1 160.64(10) . . ?
O5 V2 N1 92.04(10) . . ?
O8 V2 N2 165.31(11) . . ?
O1 V2 N2 85.47(10) . . ?
O2 V2 N2 88.36(10) . . ?
O5 V2 N2 80.10(10) . . ?
N1 V2 N2 72.68(10) . . ?
O1 P1 O2 116.86(13) . 2_577 ?
O1 P1 O3 109.73(13) . 1_455 ?
O2 P1 O3 109.24(13) 2_577 1_455 ?
O1 P1 O4 104.69(14) . . ?
O2 P1 O4 109.34(13) 2_577 . ?
O3 P1 O4 106.43(15) 1_455 . ?
P1 O1 V2 139.83(14) . . ?
P1 O2 V2 133.74(14) 2_577 . ?
P1 O3 V1 143.89(15) 1_655 . ?
V1 O5 V2 144.40(13) . . ?
V1 O7 V1 180.000(1) . 2_667 ?
C1 N1 C5 118.1(3) . . ?
C1 N1 V2 120.6(2) . . ?
C5 N1 V2 121.0(2) . . ?
C10 N2 C6 118.7(3) . . ?
C10 N2 V2 124.8(2) . . ?
C6 N2 V2 116.5(2) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 C6 115.7(3) . . ?
C2 C1 C6 122.3(3) . . ?
C3 C2 C1 118.8(3) . . ?
C4 C3 C2 119.3(3) . . ?
C3 C4 C5 119.2(3) . . ?
N1 C5 C4 122.6(3) . . ?
N2 C6 C7 121.1(3) . . ?
N2 C6 C1 114.2(3) . . ?
C7 C6 C1 124.7(3) . . ?
C8 C7 C6 119.3(3) . . ?
C7 C8 C9 119.2(3) . . ?
C10 C9 C8 119.1(3) . . ?
N2 C10 C9 122.6(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
V1 O6 1.614(2) . ?
V1 O5 1.654(2) . ?
V1 O7 1.7773(6) . ?
V1 O3 1.830(2) . ?
V2 O8 1.596(2) . ?
V2 O1 1.982(2) . ?
V2 O2 1.983(2) . ?
V2 O5 2.066(2) . ?
V2 N1 2.138(3) . ?
V2 N2 2.264(3) . ?
P1 O1 1.509(2) . ?
P1 O2 1.520(2) 2_577 ?
P1 O3 1.557(2) 1_455 ?
P1 O4 1.569(2) . ?
O2 P1 1.520(2) 2_577 ?
O3 P1 1.557(2) 1_655 ?
O7 V1 1.7773(6) 2_667 ?
N1 C1 1.343(4) . ?
N1 C5 1.347(4) . ?
N2 C10 1.333(4) . ?
N2 C6 1.357(4) . ?
C1 C2 1.395(4) . ?
C1 C6 1.472(4) . ?
C2 C3 1.382(5) . ?
C3 C4 1.368(6) . ?
C4 C5 1.382(5) . ?
C6 C7 1.391(4) . ?
C7 C8 1.372(5) . ?
C8 C9 1.376(5) . ?
C9 C10 1.375(5) . ?
