#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:05:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179276 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/96/4319674.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_4319674
loop_
_publ_author_name
'Ching-Hui Huang'
'Li-Hsun Huang'
'Kwang-Hwa Lii'
_publ_contact_author
;
Kwang-Hwa Lii,
Department of Chemistry,
National Central University,
Chungli, Taiwan 320
;
_publ_contact_author_email       liikh@cc.ncu.edu.tw
_publ_section_title
;
 Synthesis and Structure of (4,4'-H2bpy)[V2(HPO4)4(4,4'-bpy)2], a Novel
 Two-Dimensional Network Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2625
_journal_page_last               2627
_journal_paper_doi               10.1021/ic001169g
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_structural     (4,4'H2bpy)[V2(HPO4)4(4,4'-bpy)2]
_chemical_formula_sum            'C30 H30 N6 O16 P4 V2'
_chemical_formula_weight         956.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           3
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.060(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   8.1434(9)
_cell_length_b                   11.4343(12)
_cell_length_c                   10.0905(11)
_cell_measurement_reflns_used    911
_cell_measurement_temperature    296(2)
_cell_volume                     898.22(17)
_computing_molecular_graphics    ATOMS
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens Smart CCD'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5942
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.938
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_extinction_coef       0.0000(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3986
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_obs          0.0449
_refine_ls_shift/esd_max         -0.575
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0530P)²+0.2984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1096
_refine_ls_wR_factor_obs         0.1034
_reflns_number_observed          3354
_reflns_number_total             3986
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001169g.cif
_cod_data_source_block           mr06m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        898.2(2)
_cod_database_code               4319674
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 1.0000 0.55888(9) 0.5000 0.0125(3) Uani 1 d S .
V2 V 1.0000 0.62928(9) 1.0000 0.0131(3) Uani 1 d S .
P1 P 0.72026(14) 0.60465(12) 1.18604(12) 0.0149(3) Uani 1 d . .
P2 P 0.7161(2) 0.58921(12) 0.68200(13) 0.0182(4) Uani 1 d . .
O1 O 0.5713(5) 0.5190(3) 1.1266(3) 0.0200(8) Uani 1 d . .
O2 O 0.8042(4) 0.6372(4) 1.0775(3) 0.0204(9) Uani 1 d . .
O3 O 0.8420(4) 0.5522(4) 1.3132(3) 0.0254(9) Uani 1 d . .
O4 O 0.6422(5) 0.7217(3) 1.2241(4) 0.0267(9) Uani 1 d . .
O5 O 0.8368(4) 0.6369(3) 0.8157(3) 0.0209(8) Uani 1 d . .
O6 O 0.5742(5) 0.6835(4) 0.6252(4) 0.0245(9) Uani 1 d . .
O7 O 0.8050(4) 0.5578(4) 0.5752(3) 0.0228(9) Uani 1 d . .
O8 O 0.6293(5) 0.4740(4) 0.7101(4) 0.0310(10) Uani 1 d . .
N1 N 1.0000 0.7482(6) 0.5000 0.019(2) Uani 1 d S .
N2 N 1.0000 0.3715(6) 0.5000 0.023(2) Uani 1 d S .
N3 N 1.0000 0.8181(6) 1.0000 0.0167(14) Uani 1 d S .
N4 N 1.0000 0.4386(6) 1.0000 0.022(2) Uani 1 d S .
N5 N 0.6134(6) 1.1135(5) 1.1832(5) 0.0531(12) Uani 1 d . .
C1 C 0.9815(6) 0.8099(4) 0.6076(4) 0.0229(9) Uani 1 d . .
C2 C 0.9800(6) 0.9312(4) 0.6120(4) 0.0255(10) Uani 1 d . .
C3 C 1.0000 0.9977(7) 0.5000 0.019(2) Uani 1 d S .
C4 C 1.0000 1.1218(9) 0.5000 0.029(2) Uani 1 d S .
C5 C 0.9581(7) 0.3097(4) 0.5986(5) 0.0306(11) Uani 1 d . .
C6 C 0.9586(7) 0.1886(4) 0.6032(5) 0.0320(11) Uani 1 d . .
C7 C 0.8528(6) 0.8784(4) 0.9703(5) 0.0305(10) Uani 1 d . .
C8 C 0.8477(6) 0.9980(4) 0.9712(5) 0.0319(11) Uani 1 d . .
C9 C 1.0000 1.0612(6) 1.0000 0.017(2) Uani 1 d S .
C10 C 1.0000 1.1950(8) 1.0000 0.023(2) Uani 1 d S .
C11 C 0.8610(6) 0.3766(4) 1.0041(5) 0.0264(9) Uani 1 d . .
C12 C 0.8564(6) 1.2562(4) 1.0046(5) 0.0293(10) Uani 1 d . .
C13 C 0.5955(8) 1.0133(6) 1.2459(7) 0.055(2) Uani 1 d . .
C14 C 0.5484(8) 1.0072(5) 1.3669(7) 0.0513(15) Uani 1 d . .
C15 C 0.5210(6) 1.1099(5) 1.4327(5) 0.0411(12) Uani 1 d . .
C16 C 0.5401(9) 1.2142(6) 1.3668(7) 0.057(2) Uani 1 d . .
C17 C 0.5838(9) 1.2101(5) 1.2436(7) 0.058(2) Uani 1 d . .
H4O H 0.5672 0.7057 0.2770 0.050 Uiso 1 d . .
H8O H 0.5689 0.4836 0.7772 0.050 Uiso 1 d . .
H1C H 0.9531 0.7695 0.6783 0.050 Uiso 1 d . .
H2C H 0.9549 0.9609 0.6983 0.050 Uiso 1 d . .
H5C H 0.9407 0.3408 0.6783 0.050 Uiso 1 d . .
H6C H 0.8653 0.1387 0.6378 0.050 Uiso 1 d . .
H7C H 0.7501 0.8279 0.9575 0.050 Uiso 1 d . .
H8C H 0.7561 0.0409 0.9776 0.050 Uiso 1 d . .
H11C H 0.7557 0.4210 0.9976 0.050 Uiso 1 d . .
H12C H 0.7473 0.2159 0.9976 0.050 Uiso 1 d . .
H14C H 0.5424 0.9211 0.3969 0.050 Uiso 1 d . .
H16C H 0.5062 0.2809 0.4233 0.050 Uiso 1 d . .
H17C H 0.6022 0.2764 0.1972 0.050 Uiso 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
O3 V1 O3 175.5(3) 2_757 1_554 ?
O3 V1 O7 89.67(15) 2_757 2_756 ?
O3 V1 O7 90.30(15) 1_554 2_756 ?
O3 V1 O7 90.30(15) 2_757 . ?
O3 V1 O7 89.67(15) 1_554 . ?
O7 V1 O7 179.2(3) 2_756 . ?
O3 V1 N2 87.75(13) 2_757 . ?
O3 V1 N2 87.75(13) 1_554 . ?
O7 V1 N2 89.62(13) 2_756 . ?
O7 V1 N2 89.62(13) . . ?
O3 V1 N1 92.25(13) 2_757 . ?
O3 V1 N1 92.25(13) 1_554 . ?
O7 V1 N1 90.38(13) 2_756 . ?
O7 V1 N1 90.38(13) . . ?
N2 V1 N1 180.000(2) . . ?
O5 V2 O5 174.9(2) 2_757 . ?
O5 V2 O2 91.37(14) 2_757 . ?
O5 V2 O2 88.39(14) . . ?
O5 V2 O2 88.39(14) 2_757 2_757 ?
O5 V2 O2 91.37(14) . 2_757 ?
O2 V2 O2 174.8(2) . 2_757 ?
O5 V2 N3 87.44(12) 2_757 . ?
O5 V2 N3 87.44(12) . . ?
O2 V2 N3 87.38(12) . . ?
O2 V2 N3 87.38(12) 2_757 . ?
O5 V2 N4 92.56(12) 2_757 . ?
O5 V2 N4 92.56(12) . . ?
O2 V2 N4 92.62(12) . . ?
O2 V2 N4 92.62(12) 2_757 . ?
N3 V2 N4 180.000(2) . . ?
O3 P1 O2 113.3(2) . . ?
O3 P1 O1 109.1(2) . . ?
O2 P1 O1 110.5(2) . . ?
O3 P1 O4 110.1(2) . . ?
O2 P1 O4 105.7(2) . . ?
O1 P1 O4 107.9(2) . . ?
O7 P2 O5 113.5(2) . . ?
O7 P2 O8 105.5(2) . . ?
O5 P2 O8 110.6(2) . . ?
O7 P2 O6 111.2(2) . . ?
O5 P2 O6 107.2(2) . . ?
O8 P2 O6 108.9(2) . . ?
P1 O2 V2 150.9(2) . . ?
P1 O3 V1 153.8(3) . 1_556 ?
P2 O5 V2 156.4(3) . . ?
P2 O7 V1 153.3(3) . . ?
P2 O8 H8O 112.8(3) . . ?
C1 N1 C1 116.4(6) . 2_756 ?
C1 N1 V1 121.8(3) . . ?
C1 N1 V1 121.8(3) 2_756 . ?
C5 N2 C5 116.6(6) 2_756 . ?
C5 N2 V1 121.7(3) 2_756 . ?
C5 N2 V1 121.7(3) . . ?
C7 N3 C7 118.0(6) 2_757 . ?
C7 N3 V2 121.0(3) 2_757 . ?
C7 N3 V2 121.0(3) . . ?
C11 N4 C11 116.5(6) 2_757 . ?
C11 N4 V2 121.7(3) 2_757 . ?
C11 N4 V2 121.7(3) . . ?
C17 N5 C13 116.1(6) . . ?
N1 C1 C2 123.8(4) . . ?
N1 C1 H1C 118.0(4) . . ?
C2 C1 H1C 117.6(4) . . ?
C1 C2 C3 120.6(4) . . ?
C1 C2 H2C 111.7(4) . . ?
C3 C2 H2C 127.6(5) . . ?
C2 C3 C2 114.8(6) 2_756 . ?
C2 C3 C4 122.6(3) 2_756 . ?
C2 C3 C4 122.6(3) . . ?
C6 C4 C6 114.4(8) 1_565 2_766 ?
C6 C4 C3 122.8(4) 1_565 . ?
C6 C4 C3 122.8(4) 2_766 . ?
N2 C5 C6 123.4(5) . . ?
N2 C5 H5C 125.3(5) . . ?
C6 C5 H5C 110.7(4) . . ?
C5 C6 C4 121.1(5) . 1_545 ?
C5 C6 H6C 122.7(4) . . ?
C4 C6 H6C 107.1(5) 1_545 . ?
N3 C7 C8 122.7(5) . . ?
N3 C7 H7C 113.2(4) . . ?
C8 C7 H7C 123.8(4) . . ?
C7 C8 C9 119.6(4) . . ?
C8 C9 C8 117.4(6) 2_757 . ?
C8 C9 C10 121.3(3) 2_757 . ?
C8 C9 C10 121.3(3) . . ?
C12 C10 C12 118.9(7) 2_757 . ?
C12 C10 C9 120.6(4) 2_757 . ?
C12 C10 C9 120.6(4) . . ?
N4 C11 C12 123.4(5) . 1_545 ?
N4 C11 H11C 116.9(5) . . ?
C12 C11 H11C 119.5(4) 1_545 . ?
C10 C12 C11 118.9(5) . 1_565 ?
N5 C13 C14 123.8(6) . . ?
C13 C14 C15 120.0(6) . . ?
C16 C15 C14 115.8(5) . . ?
C16 C15 C15 121.3(3) . 2_658 ?
C14 C15 C15 122.8(3) . 2_658 ?
C17 C16 C15 119.4(6) . . ?
N5 C17 C16 124.8(6) . . ?
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 O3 1.947(3) 2_757 ?
V1 O3 1.947(3) 1_554 ?
V1 O7 1.950(3) 2_756 ?
V1 O7 1.950(3) . ?
V1 N2 2.143(7) . ?
V1 N1 2.164(7) . ?
V2 O5 1.945(3) 2_757 ?
V2 O5 1.945(3) . ?
V2 O2 1.973(3) . ?
V2 O2 1.973(3) 2_757 ?
V2 N3 2.159(7) . ?
V2 N4 2.181(7) . ?
P1 O3 1.498(4) . ?
P1 O2 1.498(3) . ?
P1 O1 1.537(4) . ?
P1 O4 1.577(4) . ?
P2 O7 1.508(3) . ?
P2 O5 1.518(3) . ?
P2 O8 1.560(4) . ?
P2 O6 1.561(4) . ?
O3 V1 1.947(3) 1_556 ?
O8 H8O 0.953(4) . ?
N1 C1 1.340(5) . ?
N1 C1 1.340(5) 2_756 ?
N2 C5 1.343(6) 2_756 ?
N2 C5 1.343(6) . ?
N3 C7 1.339(6) 2_757 ?
N3 C7 1.339(6) . ?
N4 C11 1.346(6) 2_757 ?
N4 C11 1.346(6) . ?
N5 C17 1.317(8) . ?
N5 C13 1.338(8) . ?
C1 C2 1.388(6) . ?
C1 H1C 0.934(4) . ?
C2 C3 1.410(6) . ?
C2 H2C 1.010(4) . ?
C3 C2 1.410(6) 2_756 ?
C3 C4 1.420(13) . ?
C4 C6 1.409(7) 1_565 ?
C4 C6 1.409(7) 2_766 ?
C5 C6 1.385(6) . ?
C5 H5C 0.927(4) . ?
C6 C4 1.409(7) 1_545 ?
C6 H6C 1.087(5) . ?
C7 C8 1.368(6) . ?
C7 H7C 0.993(4) . ?
C8 C9 1.390(6) . ?
C9 C8 1.390(6) 2_757 ?
C9 C10 1.530(11) . ?
C10 C12 1.375(6) 2_757 ?
C10 C12 1.375(6) . ?
C11 C12 1.378(6) 1_545 ?
C11 H11C 0.982(4) . ?
C12 C11 1.378(6) 1_565 ?
C13 C14 1.385(9) . ?
C14 C15 1.399(8) . ?
C15 C16 1.396(8) . ?
C15 C15 1.495(11) 2_658 ?
C16 C17 1.391(9) . ?
