#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318015.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_4318015
loop_
_publ_author_name
'Li-Hsun Huang'
'Hsien-Ming Kao'
'Kwang-Hwa Lii'
_publ_section_title
;
 Novel Vanadium(V) Compounds with a Layer Structure: Synthesis, Crystal
 Structures, and Solid State NMR Spectroscopy of
 [(VO2)2(4,4'-bpy)0.5(4,4'-Hbpy)(XO4)].H2O (X = P and As)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2936
_journal_page_last               2940
_journal_paper_doi               10.1021/ic0111841
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[(VO2)2(4,4'-bpy)0.5(4,4'-Hbpy)(PO4)].H2O'
_chemical_formula_sum            'C15 H15 N3 O9 P V2'
_chemical_formula_weight         514.15
_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                113.4652(7)
_cell_angle_beta                 95.7231(7)
_cell_angle_gamma                94.4447(7)
_cell_formula_units_Z            2
_cell_length_a                   7.9063(3)
_cell_length_b                   10.2201(4)
_cell_length_c                   12.1336(5)
_cell_measurement_temperature    294(2)
_cell_volume                     887.46(6)
_computing_molecular_graphics    'Diamond', 'SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  '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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9430
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0352P)²+0.9049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                3671
_reflns_number_total             4209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0111841_1.cif
_cod_data_source_block           4044all
_cod_database_code               4318015
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 -0.50456(5) 0.23104(4) 0.68868(3) 0.01926(10) Uani 1 1 d . . .
V2 V 0.05923(5) 0.14390(4) 0.37062(3) 0.01854(10) Uani 1 1 d . . .
P1 P -0.23977(7) 0.05627(6) 0.50890(5) 0.01677(13) Uani 1 1 d . . .
O1 O -0.3771(2) 0.15739(18) 0.55160(14) 0.0233(3) Uani 1 1 d . . .
O2 O -0.0848(2) 0.14108(18) 0.49111(15) 0.0233(3) Uani 1 1 d . . .
O3 O 0.1827(2) -0.0018(2) 0.39465(15) 0.0268(4) Uani 1 1 d . . .
O4 O -0.6833(2) 0.06865(19) 0.61098(15) 0.0279(4) Uani 1 1 d . . .
O5 O -0.3537(2) 0.2515(2) 0.79720(16) 0.0318(4) Uani 1 1 d . . .
O6 O -0.5228(2) 0.3877(2) 0.68738(17) 0.0322(4) Uani 1 1 d . . .
O7 O 0.1397(3) 0.3114(2) 0.43463(18) 0.0390(5) Uani 1 1 d . . .
O8 O -0.0913(2) 0.1211(2) 0.26150(17) 0.0374(5) Uani 1 1 d . . .
O9 O -0.3677(4) 0.3943(3) 0.4655(3) 0.0769(9) Uani 1 1 d . . .
N1 N -0.6797(2) 0.2762(2) 0.82886(17) 0.0234(4) Uani 1 1 d . . .
N2 N -0.1726(3) 0.4533(3) 0.3076(2) 0.0386(6) Uani 1 1 d . . .
N3 N 0.2347(2) 0.0997(2) 0.23280(17) 0.0216(4) Uani 1 1 d . . .
C1 C -0.8507(3) 0.2496(3) 0.8049(2) 0.0272(5) Uani 1 1 d . . .
C2 C -0.6106(3) 0.3409(3) 0.9465(2) 0.0312(6) Uani 1 1 d . . .
C3 C -0.9560(3) 0.2851(3) 0.8954(2) 0.0279(5) Uani 1 1 d . . .
C4 C -0.8833(3) 0.3535(3) 0.0168(2) 0.0236(5) Uani 1 1 d . . .
C5 C -0.7054(3) 0.3824(3) 0.0410(2) 0.0319(6) Uani 1 1 d . . .
C6 C -0.9877(3) 0.3918(3) 0.1177(2) 0.0243(5) Uani 1 1 d . . .
C7 C -1.1598(3) 0.3375(3) 0.0986(3) 0.0344(6) Uani 1 1 d . . .
C8 C -1.2493(4) 0.3692(4) 0.1959(3) 0.0412(7) Uani 1 1 d . . .
C9 C -1.0097(4) 0.5104(4) 0.3298(3) 0.0419(7) Uani 1 1 d . . .
C10 C -0.9138(4) 0.4806(3) 0.2360(2) 0.0377(6) Uani 1 1 d . . .
C11 C 0.3991(3) 0.0846(3) 0.2561(2) 0.0284(5) Uani 1 1 d . . .
C12 C 0.1763(3) 0.0800(3) 0.1188(2) 0.0275(5) Uani 1 1 d . . .
C13 C 0.5074(3) 0.0468(3) 0.1684(2) 0.0286(5) Uani 1 1 d . . .
C14 C 0.2751(3) 0.0415(3) 0.0261(2) 0.0288(5) Uani 1 1 d . . .
C15 C 0.4453(3) 0.0222(3) 0.0489(2) 0.0227(5) Uani 1 1 d . . .
H1 H -0.9100 0.2036 0.7205 0.050 Uiso 1 1 d . . .
H2 H -0.4837 0.3452 0.9441 0.050 Uiso 1 1 d . . .
H3 H -0.0768 0.2661 0.8657 0.050 Uiso 1 1 d . . .
H4 H -0.2206 0.2733 0.0203 0.050 Uiso 1 1 d . . .
H5 H -0.3727 0.3275 0.1786 0.050 Uiso 1 1 d . . .
H6 H -0.7970 0.5217 0.2633 0.050 Uiso 1 1 d . . .
H7 H 0.4504 0.1022 0.3423 0.050 Uiso 1 1 d . . .
H8 H 0.0616 0.1100 0.1122 0.050 Uiso 1 1 d . . .
H9 H 0.6259 0.0369 0.1994 0.050 Uiso 1 1 d . . .
H10 H -0.6550 0.4203 0.1254 0.050 Uiso 1 1 d . . .
H11 H 0.2190 0.0294 -0.0543 0.050 Uiso 1 1 d . . .
H12 H -0.9546 0.5734 0.4168 0.050 Uiso 1 1 d . . .
H13 H -0.2444 0.4914 0.3824 0.050 Uiso 1 1 d . . .
H14 H -0.4569 0.3634 0.4191 0.050 Uiso 1 1 d . . .
H15 H -0.3732 0.4783 0.4994 0.050 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
O5 V1 O6 108.15(11) . . ?
O5 V1 O4 126.05(10) . . ?
O6 V1 O4 122.79(9) . . ?
O5 V1 O1 98.97(8) . . ?
O6 V1 O1 97.69(8) . . ?
O4 V1 O1 91.24(7) . . ?
O5 V1 N1 85.88(8) . . ?
O6 V1 N1 89.53(8) . . ?
O4 V1 N1 78.44(7) . . ?
O1 V1 N1 169.52(8) . . ?
O7 V2 O8 109.29(12) . . ?
O7 V2 O3 120.44(10) . . ?
O8 V2 O3 127.54(10) . . ?
O7 V2 O2 98.74(8) . . ?
O8 V2 O2 98.27(8) . . ?
O3 V2 O2 90.15(7) . . ?
O7 V2 N3 91.17(8) . . ?
O8 V2 N3 86.10(8) . . ?
O3 V2 N3 77.67(7) . . ?
O2 V2 N3 167.11(8) . . ?
O3 P1 O2 108.58(10) 2_556 . ?
O3 P1 O4 111.04(11) 2_556 2_456 ?
O2 P1 O4 110.49(9) . 2_456 ?
O3 P1 O1 110.00(9) 2_556 . ?
O2 P1 O1 108.51(10) . . ?
O4 P1 O1 108.19(10) 2_456 . ?
P1 O1 V1 139.06(11) . . ?
P1 O2 V2 142.64(11) . . ?
P1 O3 V2 141.95(11) 2_556 . ?
P1 O4 V1 144.90(11) 2_456 . ?
H14 O9 H15 103.8 . . ?
C1 N1 C2 116.9(2) . . ?
C1 N1 V1 124.75(16) . . ?
C2 N1 V1 118.32(15) . . ?
C9 N2 C8 122.0(2) 1_655 1_655 ?
C9 N2 H13 116.1 1_655 . ?
C8 N2 H13 121.3 1_655 . ?
C11 N3 C12 117.01(19) . . ?
C11 N3 V2 122.53(15) . . ?
C12 N3 V2 120.39(15) . . ?
N1 C1 C3 123.0(2) . . ?
N1 C1 H1 121.1 . . ?
C3 C1 H1 115.9 . . ?
N1 C2 C5 123.8(2) . 1_556 ?
N1 C2 H2 103.9 . . ?
C5 C2 H2 132.2 1_556 . ?
C4 C3 C1 119.7(2) 1_556 . ?
C5 C4 C3 117.0(2) . 1_554 ?
C5 C4 C6 120.4(2) . . ?
C3 C4 C6 122.5(2) 1_554 . ?
C2 C5 C4 119.6(2) 1_554 . ?
C2 C5 H10 123.3 1_554 . ?
C4 C5 H10 116.6 . . ?
C7 C6 C10 117.8(2) . . ?
C7 C6 C4 121.6(2) . . ?
C10 C6 C4 120.6(2) . . ?
C8 C7 C6 119.7(3) . . ?
N2 C8 C7 120.4(3) 1_455 . ?
N2 C9 C10 119.9(3) 1_455 . ?
N2 C9 H12 119.9 1_455 . ?
C10 C9 H12 120.1 . . ?
C9 C10 C6 120.2(3) . . ?
C9 C10 H6 112.5 . . ?
C6 C10 H6 127.2 . . ?
N3 C11 C13 123.2(2) . . ?
N3 C11 H7 119.8 . . ?
C13 C11 H7 117.0 . . ?
N3 C12 C14 123.5(2) . . ?
N3 C12 H8 112.1 . . ?
C14 C12 H8 123.8 . . ?
C11 C13 C15 119.8(2) . . ?
C11 C13 H9 113.7 . . ?
C15 C13 H9 126.4 . . ?
C12 C14 C15 119.9(2) . . ?
C12 C14 H11 116.7 . . ?
C15 C14 H11 123.4 . . ?
C14 C15 C13 116.6(2) . . ?
C14 C15 C15 121.6(3) . 2_655 ?
C13 C15 C15 121.8(3) . 2_655 ?
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 O5 1.6216(18) . ?
V1 O6 1.6251(19) . ?
V1 O4 1.9405(18) . ?
V1 O1 1.9503(15) . ?
V1 N1 2.2286(19) . ?
V2 O7 1.6160(19) . ?
V2 O8 1.6189(18) . ?
V2 O3 1.9416(17) . ?
V2 O2 1.9483(15) . ?
V2 N3 2.2095(19) . ?
P1 O3 1.5280(17) 2_556 ?
P1 O2 1.5284(16) . ?
P1 O4 1.5297(17) 2_456 ?
P1 O1 1.5410(16) . ?
O3 P1 1.5280(17) 2_556 ?
O4 P1 1.5297(17) 2_456 ?
O9 H14 0.8120 . ?
O9 H15 0.7980 . ?
N1 C1 1.338(3) . ?
N1 C2 1.345(3) . ?
N2 C9 1.328(4) 1_655 ?
N2 C8 1.331(4) 1_655 ?
N2 H13 1.0734 . ?
N3 C11 1.336(3) . ?
N3 C12 1.343(3) . ?
C1 C3 1.393(3) . ?
C1 H1 0.9883 . ?
C2 C5 1.375(3) 1_556 ?
C2 H2 1.0046 . ?
C3 C4 1.392(3) 1_556 ?
C4 C5 1.391(3) . ?
C4 C3 1.392(3) 1_554 ?
C4 C6 1.485(3) . ?
C5 C2 1.375(3) 1_554 ?
C5 H10 0.9671 . ?
C6 C7 1.389(4) . ?
C6 C10 1.392(4) . ?
C7 C8 1.377(4) . ?
C8 N2 1.331(4) 1_455 ?
C9 N2 1.328(4) 1_455 ?
C9 C10 1.377(4) . ?
C9 H12 1.0208 . ?
C10 H6 0.9525 . ?
C11 C13 1.386(3) . ?
C11 H7 1.0222 . ?
C12 C14 1.379(3) . ?
C12 H8 0.9854 . ?
C13 C15 1.399(3) . ?
C13 H9 1.0019 . ?
C14 C15 1.391(3) . ?
C14 H11 0.9863 . ?
C15 C15 1.483(4) 2_655 ?
