#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:13:32 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180417 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/86/7208617.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_7208617
loop_
_publ_author_name
'Chen, Yan'
'Liu, Tao'
'He, Cheng'
'Duan, Chunying'
_publ_section_title
;
 Mild hydrothermal synthesis, structure and characterization of the
 vanadyl phosphate hydrate Pb(VOPO4)2·3H2O: the formation of spin
 dimers in a three dimensional crystal structure
;
_journal_issue                   37
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              19872
_journal_paper_doi               10.1039/c2jm32976j
_journal_volume                  22
_journal_year                    2012
_chemical_formula_sum            'O18 P3 Pb3 V3'
_chemical_formula_weight         1155.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7136(19)
_cell_length_b                   13.824(3)
_cell_length_c                   11.003(2)
_cell_measurement_reflns_used    816
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.37
_cell_volume                     1477.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1763
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    36.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.206
_refine_diff_density_min         -4.740
_refine_diff_density_rms         0.424
_refine_ls_extinction_coef       0.00056(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1763
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0385
_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)+(0.0308P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                1374
_reflns_number_total             1763
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2jm32976j.txt
_cod_data_source_block           difabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'p n m a'
_cod_database_code               7208617
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Pb01 Pb 0.91064(4) 0.10977(3) 0.11898(4) 0.01229(16) Uani 1 1 d U
Pb02 Pb 1.03632(8) 0.2500 0.48906(9) 0.0333(2) Uani 1 2 d SU
V003 V 1.28959(17) 0.01844(12) 0.09632(18) 0.0086(4) Uani 1 1 d U
V004 V 1.1218(3) -0.2500 0.1854(3) 0.0139(6) Uani 1 2 d SU
P005 P 1.1035(3) -0.04952(19) 0.3256(3) 0.0069(5) Uani 1 1 d U
P006 P 1.2178(4) 0.2500 0.2110(4) 0.0072(8) Uani 1 2 d SU
O007 O 1.0694(10) 0.2500 0.1715(12) 0.013(2) Uani 1 2 d SU
O008 O 1.2224(10) 0.2500 0.3534(11) 0.013(2) Uani 1 2 d SU
O009 O 0.9935(7) 0.0282(5) 0.3175(7) 0.0108(15) Uani 1 1 d U
O010 O 1.2879(11) -0.2500 0.1881(15) 0.032(3) Uani 1 2 d SU
O011 O 1.0510(7) -0.1403(6) 0.2552(8) 0.0176(18) Uani 1 1 d U
O012 O 1.0773(13) -0.2500 0.0425(11) 0.023(3) Uani 1 2 d SU
O013 O 1.3230(7) -0.0909(5) 0.0442(8) 0.0129(16) Uani 1 1 d U
O014 O 1.2389(6) -0.0149(5) 0.2701(7) 0.0096(15) Uani 1 1 d U
O015 O 1.1307(7) 0.0321(5) 0.0502(8) 0.0135(16) Uani 1 1 d U
O017 O 1.1256(7) -0.0844(5) 0.4573(7) 0.0105(15) Uani 1 1 d U
O018 O 1.3012(7) 0.1607(5) 0.1701(8) 0.0133(16) Uani 1 1 d U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Pb Pb -3.3944 10.1111 '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
O015 Pb01 O007 83.0(3) . .
O015 Pb01 O009 78.6(2) . .
O007 Pb01 O009 87.2(3) . .
O015 Pb01 O012 94.2(3) . 5_755
O007 Pb01 O012 64.2(4) . 5_755
O009 Pb01 O012 151.3(3) . 5_755
O015 Pb01 O018 136.1(2) . 6_556
O007 Pb01 O018 80.9(3) . 6_556
O009 Pb01 O018 60.0(2) . 6_556
O012 Pb01 O018 114.4(3) 5_755 6_556
O015 Pb01 O008 157.6(3) . 6_556
O007 Pb01 O008 80.6(2) . 6_556
O009 Pb01 O008 115.6(3) . 6_556
O012 Pb01 O008 64.8(3) 5_755 6_556
O018 Pb01 O008 55.6(3) 6_556 6_556
O015 Pb01 O014 113.0(2) . 6_556
O007 Pb01 O014 139.5(3) . 6_556
O009 Pb01 O014 62.0(2) . 6_556
O012 Pb01 O014 143.6(3) 5_755 6_556
O018 Pb01 O014 61.6(2) 6_556 6_556
O008 Pb01 O014 89.4(2) 6_556 6_556
O015 Pb01 O015 67.2(3) . 5_755
O007 Pb01 O015 142.2(3) . 5_755
O009 Pb01 O015 108.0(2) . 5_755
O012 Pb01 O015 94.3(3) 5_755 5_755
O018 Pb01 O015 136.8(2) 6_556 5_755
O008 Pb01 O015 119.7(3) 6_556 5_755
O014 Pb01 O015 76.0(2) 6_556 5_755
O008 Pb02 O013 75.5(2) . 7_866
O008 Pb02 O013 75.5(2) . 2_755
O013 Pb02 O013 111.6(3) 7_866 2_755
O015 V003 O013 100.6(4) . .
O015 V003 O017 95.8(4) . 2_754
O013 V003 O017 94.1(4) . 2_754
O015 V003 O014 95.1(3) . .
O013 V003 O014 99.6(4) . .
O017 V003 O014 160.5(3) 2_754 .
O015 V003 O018 93.5(3) . .
O013 V003 O018 165.5(3) . .
O017 V003 O018 81.1(3) 2_754 .
O014 V003 O018 82.2(3) . .
O015 V003 O009 167.5(3) . 6_656
O013 V003 O009 91.7(3) . 6_656
O017 V003 O009 86.0(3) 2_754 6_656
O014 V003 O009 80.0(3) . 6_656
O018 V003 O009 74.4(3) . 6_656
O010 V004 O012 106.4(8) . .
O010 V004 O011 111.6(4) . .
O012 V004 O011 107.7(4) . .
O010 V004 O011 111.6(4) . 8
O012 V004 O011 107.7(4) . 8
O011 V004 O011 111.6(6) . 8
O009 P005 O014 111.1(4) . .
O009 P005 O017 112.0(4) . .
O014 P005 O017 110.7(4) . .
O009 P005 O011 108.1(4) . .
O014 P005 O011 109.5(4) . .
O017 P005 O011 105.1(5) . .
O007 P006 O018 114.7(4) . 8_565
O007 P006 O018 114.7(4) . .
O018 P006 O018 106.2(6) 8_565 .
O007 P006 O008 108.4(7) . .
O018 P006 O008 106.1(4) 8_565 .
O018 P006 O008 106.1(4) . .
P006 O007 Pb01 130.24(17) . .
P006 O007 Pb01 130.24(17) . 8_565
Pb01 O007 Pb01 99.3(3) . 8_565
P006 O008 Pb02 127.9(6) . .
P006 O008 Pb01 97.6(4) . 3
Pb02 O008 Pb01 117.0(3) . 3
P006 O008 Pb01 97.6(4) . 6_656
Pb02 O008 Pb01 117.0(3) . 6_656
Pb01 O008 Pb01 92.6(3) 3 6_656
P005 O009 V003 124.4(4) . 6_556
P005 O009 Pb01 125.3(4) . .
V003 O009 Pb01 96.4(3) 6_556 .
P005 O011 V004 138.6(5) . .
V004 O012 Pb01 129.7(3) . 4_745
V004 O012 Pb01 129.7(3) . 5_755
Pb01 O012 Pb01 94.9(4) 4_745 5_755
V003 O013 Pb02 159.8(4) . 2_754
P005 O014 V003 131.1(5) . .
P005 O014 Pb01 123.6(4) . 6_656
V003 O014 Pb01 97.6(3) . 6_656
V003 O015 Pb01 139.4(4) . .
V003 O015 Pb01 105.5(3) . 5_755
Pb01 O015 Pb01 112.8(3) . 5_755
P005 O017 V003 130.2(5) . 2_755
P006 O018 V003 145.3(5) . .
P006 O018 Pb01 99.6(4) . 6_656
V003 O018 Pb01 96.3(3) . 6_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 O015 2.509(7) .
Pb01 O007 2.544(6) .
Pb01 O009 2.586(8) .
Pb01 O012 2.632(9) 5_755
Pb01 O018 2.648(9) 6_556
Pb01 O008 2.682(7) 6_556
Pb01 O014 2.692(7) 6_556
Pb01 O015 2.734(8) 5_755
Pb02 O008 2.344(11) .
Pb02 O013 2.659(7) 7_866
Pb02 O013 2.659(7) 2_755
V003 O015 1.635(7) .
V003 O013 1.649(7) .
V003 O017 1.962(8) 2_754
V003 O014 2.027(8) .
V003 O018 2.130(7) .
V003 O009 2.200(7) 6_656
V004 O010 1.613(11) .
V004 O012 1.631(13) .
V004 O011 1.834(8) .
V004 O011 1.834(8) 8
P005 O009 1.518(7) .
P005 O014 1.527(7) .
P005 O017 1.542(8) .
P005 O011 1.561(8) .
P006 O007 1.506(10) .
P006 O018 1.544(7) 8_565
P006 O018 1.544(7) .
P006 O008 1.567(12) .
O007 Pb01 2.544(6) 8_565
O008 Pb01 2.682(7) 3
O008 Pb01 2.682(7) 6_656
O009 V003 2.200(7) 6_556
O012 Pb01 2.632(9) 4_745
O012 Pb01 2.632(9) 5_755
O013 Pb02 2.659(7) 2_754
O014 Pb01 2.692(7) 6_656
O015 Pb01 2.734(8) 5_755
O017 V003 1.962(8) 2_755
O018 Pb01 2.648(9) 6_656
