#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318016.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_4318016
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)(AsO4)].H2O'
_chemical_formula_sum            'C15 H15 As N3 O9 V2'
_chemical_formula_weight         558.10
_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                113.4640(10)
_cell_angle_beta                 95.5600(10)
_cell_angle_gamma                94.5850(10)
_cell_formula_units_Z            2
_cell_length_a                   7.8843(6)
_cell_length_b                   10.3686(7)
_cell_length_c                   12.2606(9)
_cell_measurement_temperature    295(2)
_cell_volume                     907.35(11)
_computing_molecular_graphics    'Diamond', 'SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0265
_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       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9045
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0001(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0245
_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)+(0.0368P)²+0.5957P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                3673
_reflns_number_total             4057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0111841_2.cif
_cod_data_source_block           vbpyas
_cod_database_code               4318016
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 -0.50851(4) 0.23661(4) 0.69348(3) 0.02035(10) Uani 1 1 d . . .
V2 V 0.06511(5) 0.15091(4) 0.37045(3) 0.01949(10) Uani 1 1 d . . .
As1 As -0.23884(3) 0.05803(2) 0.509242(18) 0.01703(7) Uani 1 1 d . . .
O1 O -0.3937(2) 0.16437(18) 0.55002(14) 0.0252(3) Uani 1 1 d . . .
O2 O -0.0643(2) 0.15393(17) 0.49891(14) 0.0248(3) Uani 1 1 d . . .
O3 O 0.1840(2) 0.00038(19) 0.38516(15) 0.0287(4) Uani 1 1 d . . .
O4 O -0.6854(2) 0.07406(18) 0.62441(14) 0.0286(4) Uani 1 1 d . . .
O5 O -0.3515(2) 0.2570(2) 0.79733(15) 0.0336(4) Uani 1 1 d . . .
O6 O -0.5301(2) 0.39052(19) 0.69236(16) 0.0330(4) Uani 1 1 d . . .
O7 O 0.1511(3) 0.3155(2) 0.43269(17) 0.0413(5) Uani 1 1 d . . .
O8 O -0.0907(2) 0.1291(2) 0.26589(16) 0.0380(5) Uani 1 1 d . . .
O9 O -0.3772(4) 0.3939(3) 0.4638(3) 0.0844(10) Uani 1 1 d . . .
N1 N -0.6792(2) 0.2804(2) 0.83517(17) 0.0251(4) Uani 1 1 d . . .
N2 N -0.1728(3) 0.4513(3) 0.3097(2) 0.0396(5) Uani 1 1 d . . .
N3 N 0.2354(2) 0.1043(2) 0.23099(16) 0.0228(4) Uani 1 1 d . . .
C1 C -0.8511(3) 0.2557(3) 0.8121(2) 0.0305(5) Uani 1 1 d . . .
C2 C -0.6089(3) 0.3432(3) 0.9513(2) 0.0314(5) Uani 1 1 d . . .
C3 C -0.9560(3) 0.2899(3) 0.9017(2) 0.0305(5) Uani 1 1 d . . .
C4 C -0.8819(3) 0.3562(2) 0.0219(2) 0.0248(5) Uani 1 1 d . . .
C5 C -0.7029(3) 0.3828(3) 0.0450(2) 0.0328(6) Uani 1 1 d . . .
C6 C -0.9861(3) 0.3933(2) 0.1222(2) 0.0258(5) Uani 1 1 d . . .
C7 C -0.1587(3) 0.3370(3) 0.1029(2) 0.0370(6) Uani 1 1 d . . .
C8 C -0.2483(4) 0.3669(4) 0.1993(3) 0.0439(7) Uani 1 1 d . . .
C9 C -0.0101(4) 0.5104(3) 0.3318(2) 0.0429(7) Uani 1 1 d . . .
C10 C -0.9138(4) 0.4823(3) 0.2387(2) 0.0388(6) Uani 1 1 d . . .
C11 C 0.4001(3) 0.0865(3) 0.2534(2) 0.0318(6) Uani 1 1 d . . .
C12 C 0.1767(3) 0.0833(3) 0.1182(2) 0.0285(5) Uani 1 1 d . . .
C13 C 0.5075(3) 0.0471(3) 0.1664(2) 0.0323(6) Uani 1 1 d . . .
C14 C 0.2750(3) 0.0434(3) 0.0261(2) 0.0304(5) Uani 1 1 d . . .
C15 C 0.4455(3) 0.0224(3) 0.04845(19) 0.0236(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 -1.0768 0.2661 0.8657 0.050 Uiso 1 1 d . . .
H4 H -1.2206 0.2733 1.0203 0.050 Uiso 1 1 d . . .
H5 H -1.3727 0.3275 1.1786 0.050 Uiso 1 1 d . . .
H6 H -0.7970 0.5217 1.2633 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 1.1254 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 1.4168 0.050 Uiso 1 1 d . . .
H13 H -1.2444 0.4914 1.3824 0.050 Uiso 1 1 d . . .
H14 H -1.4569 0.3634 1.4191 0.050 Uiso 1 1 d . . .
H15 H -1.3732 0.4783 1.4994 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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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 108.36(10) . . ?
O6 V1 O4 124.26(9) . . ?
O5 V1 O4 124.24(9) . . ?
O6 V1 O1 96.59(8) . . ?
O5 V1 O1 100.70(8) . . ?
O4 V1 O1 91.04(7) . . ?
O6 V1 N1 89.49(8) . . ?
O5 V1 N1 86.80(8) . . ?
O4 V1 N1 77.25(7) . . ?
O1 V1 N1 168.26(7) . . ?
O8 V2 O7 110.10(11) . . ?
O8 V2 O3 125.08(10) . . ?
O7 V2 O3 121.86(10) . . ?
O8 V2 O2 100.40(8) . . ?
O7 V2 O2 97.38(8) . . ?
O3 V2 O2 89.98(7) . . ?
O8 V2 N3 86.93(8) . . ?
O7 V2 N3 90.88(8) . . ?
O3 V2 N3 76.32(7) . . ?
O2 V2 N3 166.26(7) . . ?
O3 As1 O4 112.64(9) 2_556 2_456 ?
O3 As1 O2 107.65(8) 2_556 . ?
O4 As1 O2 110.55(8) 2_456 . ?
O3 As1 O1 109.95(8) 2_556 . ?
O4 As1 O1 107.57(8) 2_456 . ?
O2 As1 O1 108.42(8) . . ?
As1 O1 V1 133.89(9) . . ?
As1 O2 V2 135.68(9) . . ?
As1 O3 V2 137.92(10) 2_556 . ?
As1 O4 V1 139.27(10) 2_456 . ?
C1 N1 C2 117.0(2) . . ?
C1 N1 V1 123.75(15) . . ?
C2 N1 V1 119.13(15) . . ?
C8 N2 C9 122.1(2) . . ?
C12 N3 C11 116.98(19) . . ?
C12 N3 V2 121.53(15) . . ?
C11 N3 V2 121.35(15) . . ?
N1 C1 C3 123.1(2) . . ?
N1 C1 H1 118.4 . . ?
C3 C1 H1 118.5 . . ?
N1 C2 C5 123.7(2) . 1_556 ?
N1 C2 H2 101.3 . . ?
C5 C2 H2 135.0 1_556 . ?
C1 C3 C4 119.5(2) . 1_556 ?
C1 C3 H3 109.9 . . ?
C4 C3 H3 130.5 1_556 . ?
C5 C4 C3 117.0(2) . 1_554 ?
C5 C4 C6 120.6(2) . . ?
C3 C4 C6 122.4(2) 1_554 . ?
C2 C5 C4 119.7(2) 1_554 . ?
C10 C6 C7 117.8(2) . 1_455 ?
C10 C6 C4 121.0(2) . . ?
C7 C6 C4 121.2(2) 1_455 . ?
C8 C7 C6 119.5(3) . 1_655 ?
N2 C8 C7 120.6(3) . . ?
N2 C9 C10 119.8(3) . 1_655 ?
C9 C10 C6 120.3(3) 1_455 . ?
N3 C11 C13 123.1(2) . . ?
N3 C11 H7 118.7 . . ?
C13 C11 H7 118.2 . . ?
N3 C12 C14 123.5(2) . . ?
N3 C12 H8 111.4 . . ?
C14 C12 H8 124.7 . . ?
C11 C13 C15 119.9(2) . . ?
C11 C13 H9 112.0 . . ?
C15 C13 H9 128.0 . . ?
C12 C14 C15 119.7(2) . . ?
C12 C14 H11 117.3 . . ?
C15 C14 H11 123.0 . . ?
C13 C15 C14 116.7(2) . . ?
C13 C15 C15 121.9(3) . 2_655 ?
C14 C15 C15 121.4(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 O6 1.6236(18) . ?
V1 O5 1.6237(17) . ?
V1 O4 1.9397(17) . ?
V1 O1 1.9603(16) . ?
V1 N1 2.2263(19) . ?
V2 O8 1.6194(17) . ?
V2 O7 1.6221(19) . ?
V2 O3 1.9422(17) . ?
V2 O2 1.9494(15) . ?
V2 N3 2.2024(18) . ?
As1 O3 1.6697(16) 2_556 ?
As1 O4 1.6763(16) 2_456 ?
As1 O2 1.6774(15) . ?
As1 O1 1.6882(15) . ?
O3 As1 1.6697(16) 2_556 ?
O4 As1 1.6763(15) 2_456 ?
N1 C1 1.340(3) . ?
N1 C2 1.345(3) . ?
N2 C8 1.330(4) . ?
N2 C9 1.330(4) . ?
N3 C12 1.340(3) . ?
N3 C11 1.344(3) . ?
C1 C3 1.389(3) . ?
C1 H1 1.0700 . ?
C2 C5 1.370(3) 1_556 ?
C2 H2 0.9986 . ?
C3 C4 1.395(3) 1_556 ?
C3 H3 0.9781 . ?
C4 C5 1.395(3) . ?
C4 C3 1.395(3) 1_554 ?
C4 C6 1.485(3) . ?
C5 C2 1.370(3) 1_554 ?
C6 C10 1.388(4) . ?
C6 C7 1.396(4) 1_455 ?
C7 C8 1.376(4) . ?
C7 C6 1.396(4) 1_655 ?
C9 C10 1.380(4) 1_655 ?
C10 C9 1.380(4) 1_455 ?
C11 C13 1.380(3) . ?
C11 H7 1.0658 . ?
C12 C14 1.376(3) . ?
C12 H8 0.9741 . ?
C13 C15 1.394(3) . ?
C13 H9 1.0118 . ?
C14 C15 1.397(3) . ?
C14 H11 0.9895 . ?
C15 C15 1.479(4) 2_655 ?
