#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:17:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179239 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/59/4315914.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_4315914
loop_
_publ_author_name
'Pei-Xin Li'
'Fang Kong'
'Chun-Li Hu'
'Na Zhao'
'Jiang-Gao Mao'
_publ_section_title
;
 A Series of New Phases Containing Three Different Asymmetric Building
 Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5943
_journal_page_last               5952
_journal_paper_doi               10.1021/ic100462r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'O18 Pb2 Se5 V3'
_chemical_formula_weight         1250.00
_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   none
_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                   17.013(3)
_cell_length_b                   10.7097(15)
_cell_length_c                   9.0590(13)
_cell_measurement_reflns_used    4308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.2471
_cell_volume                     1650.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10721
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    33.088
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3523
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    5.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         1.541
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0198
_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)+(0.0284P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                1720
_reflns_number_total             1898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100462r_si_001_2.cif
_cod_data_source_block           Pb2V3Se5O18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315914
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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
Pb1 Pb -0.217739(13) -0.2500 0.14402(2) 0.01173(8) Uani 1 2 d S . .
Pb2 Pb -0.191777(15) 0.2500 0.13269(3) 0.02076(9) Uani 1 2 d S . .
V1 V -0.02130(5) -0.2500 0.02022(10) 0.00778(19) Uani 1 2 d S . .
V2 V -0.15734(4) -0.00755(6) 0.47289(8) 0.01070(15) Uani 1 1 d . . .
Se1 Se 0.06221(3) -0.2500 0.39478(6) 0.00958(13) Uani 1 2 d S . .
Se2 Se -0.31307(2) 0.01895(4) 0.32682(5) 0.01095(10) Uani 1 1 d . . .
Se3 Se -0.04552(2) 0.01878(3) 0.18350(4) 0.00834(10) Uani 1 1 d . . .
O1 O 0.0421(3) -0.2500 0.2177(5) 0.0247(10) Uani 1 2 d S . .
O2 O 0.1292(2) -0.1309(3) 0.3963(4) 0.0278(8) Uani 1 1 d . . .
O3 O -0.28442(19) 0.0633(3) 0.1531(3) 0.0180(7) Uani 1 1 d . . .
O4 O -0.24885(19) -0.1019(3) 0.3646(3) 0.0163(6) Uani 1 1 d . . .
O5 O -0.25779(17) 0.1227(3) 0.4207(3) 0.0163(6) Uani 1 1 d . . .
O6 O -0.11913(16) 0.0821(2) 0.2867(3) 0.0132(6) Uani 1 1 d . . .
O7 O -0.05804(16) 0.1164(2) 0.0352(3) 0.0129(6) Uani 1 1 d . . .
O8 O -0.08872(17) -0.1137(2) 0.1181(3) 0.0129(6) Uani 1 1 d . . .
O9 O -0.0706(3) -0.2500 -0.1296(5) 0.0190(10) Uani 1 2 d S . .
O10 O -0.0869(2) -0.1050(3) 0.4687(4) 0.0331(9) Uani 1 1 d . . .
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
O5 Pb1 O5 66.85(14) 8 2_454 ?
O5 Pb1 O4 158.14(10) 8 . ?
O5 Pb1 O4 104.93(10) 2_454 . ?
O5 Pb1 O4 104.93(10) 8 7 ?
O5 Pb1 O4 158.14(10) 2_454 7 ?
O4 Pb1 O4 74.98(14) . 7 ?
O5 Pb1 O8 111.77(9) 8 . ?
O5 Pb1 O8 76.31(9) 2_454 . ?
O4 Pb1 O8 84.31(9) . . ?
O4 Pb1 O8 124.90(9) 7 . ?
O5 Pb1 O8 76.31(9) 8 7 ?
O5 Pb1 O8 111.77(9) 2_454 7 ?
O4 Pb1 O8 124.90(9) . 7 ?
O4 Pb1 O8 84.31(9) 7 7 ?
O8 Pb1 O8 66.94(12) . 7 ?
O3 Pb2 O3 103.12(16) . 7_565 ?
O3 Pb2 O6 143.09(9) . 7_565 ?
O3 Pb2 O6 73.26(10) 7_565 7_565 ?
O3 Pb2 O6 73.26(10) . . ?
O3 Pb2 O6 143.09(9) 7_565 . ?
O6 Pb2 O6 87.94(13) 7_565 . ?
O9 V1 O7 97.97(14) . 5_557 ?
O9 V1 O7 97.97(14) . 3_547 ?
O7 V1 O7 89.64(16) 5_557 3_547 ?
O9 V1 O8 94.24(14) . . ?
O7 V1 O8 88.70(11) 5_557 . ?
O7 V1 O8 167.79(12) 3_547 . ?
O9 V1 O8 94.24(14) . 7 ?
O7 V1 O8 167.79(12) 5_557 7 ?
O7 V1 O8 88.70(11) 3_547 7 ?
O8 V1 O8 90.37(16) . 7 ?
O9 V1 O1 179.4(2) . . ?
O7 V1 O1 82.44(14) 5_557 . ?
O7 V1 O1 82.44(14) 3_547 . ?
O8 V1 O1 85.35(14) . . ?
O8 V1 O1 85.35(14) 7 . ?
O10 V2 O2 109.08(19) . 5_558 ?
O10 V2 O3 101.37(16) . 2_455 ?
O2 V2 O3 81.56(13) 5_558 2_455 ?
O10 V2 O6 92.78(15) . . ?
O2 V2 O6 93.79(12) 5_558 . ?
O3 V2 O6 165.85(13) 2_455 . ?
O10 V2 O4 103.42(17) . . ?
O2 V2 O4 145.99(14) 5_558 . ?
O3 V2 O4 82.53(12) 2_455 . ?
O6 V2 O4 94.38(12) . . ?
O10 V2 O5 166.41(17) . . ?
O2 V2 O5 81.02(13) 5_558 . ?
O3 V2 O5 88.88(13) 2_455 . ?
O6 V2 O5 77.17(11) . . ?
O4 V2 O5 68.79(11) . . ?
O10 V2 Se2 136.34(15) . . ?
O2 V2 Se2 114.52(12) 5_558 . ?
O3 V2 Se2 87.15(10) 2_455 . ?
O6 V2 Se2 82.62(8) . . ?
O4 V2 Se2 34.69(8) . . ?
O5 V2 Se2 34.24(7) . . ?
O1 Se1 O2 98.41(17) . . ?
O1 Se1 O2 98.41(17) . 7 ?
O2 Se1 O2 96.5(3) . 7 ?
O5 Se2 O3 97.00(15) . . ?
O5 Se2 O4 92.37(14) . . ?
O3 Se2 O4 102.11(15) . . ?
O5 Se2 V2 48.84(10) . . ?
O3 Se2 V2 100.46(11) . . ?
O4 Se2 V2 43.74(10) . . ?
O6 Se3 O8 101.84(14) . . ?
O6 Se3 O7 95.50(13) . . ?
O8 Se3 O7 100.47(14) . . ?
Se1 O1 V1 160.9(3) . . ?
Se1 O2 V2 137.10(19) . 5_558 ?
Se2 O3 V2 121.68(16) . 2_454 ?
Se2 O3 Pb2 117.32(14) . . ?
V2 O3 Pb2 118.73(13) 2_454 . ?
Se2 O4 V2 101.58(14) . . ?
Se2 O4 Pb1 115.62(14) . . ?
V2 O4 Pb1 120.05(13) . . ?
Se2 O5 V2 96.92(13) . . ?
Se2 O5 Pb1 132.97(15) . 2_455 ?
V2 O5 Pb1 107.27(12) . 2_455 ?
Se3 O6 V2 119.93(15) . . ?
Se3 O6 Pb2 109.36(13) . . ?
V2 O6 Pb2 128.17(12) . . ?
Se3 O7 V1 122.74(15) . 5_557 ?
Se3 O8 V1 120.00(15) . . ?
Se3 O8 Pb1 141.82(14) . . ?
V1 O8 Pb1 96.28(10) . . ?
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
Pb1 O5 2.474(3) 8 ?
Pb1 O5 2.474(3) 2_454 ?
Pb1 O4 2.605(3) . ?
Pb1 O4 2.605(3) 7 ?
Pb1 O8 2.646(3) . ?
Pb1 O8 2.646(3) 7 ?
Pb2 O3 2.552(3) . ?
Pb2 O3 2.552(3) 7_565 ?
Pb2 O6 2.590(3) 7_565 ?
Pb2 O6 2.590(3) . ?
V1 O9 1.595(4) . ?
V1 O7 2.030(3) 5_557 ?
V1 O7 2.030(3) 3_547 ?
V1 O8 2.057(3) . ?
V1 O8 2.057(3) 7 ?
V1 O1 2.089(5) . ?
V2 O10 1.590(3) . ?
V2 O2 1.958(3) 5_558 ?
V2 O3 2.001(3) 2_455 ?
V2 O6 2.047(3) . ?
V2 O4 2.100(3) . ?
V2 O5 2.256(3) . ?
V2 Se2 2.9750(9) . ?
Se1 O1 1.640(5) . ?
Se1 O2 1.711(3) . ?
Se1 O2 1.711(3) 7 ?
Se2 O5 1.686(3) . ?
Se2 O3 1.715(3) . ?
Se2 O4 1.728(3) . ?
Se3 O6 1.704(3) . ?
Se3 O8 1.704(3) . ?
Se3 O7 1.715(3) . ?
O2 V2 1.958(3) 5_558 ?
O3 V2 2.001(3) 2_454 ?
O5 Pb1 2.474(3) 2_455 ?
O7 V1 2.030(3) 5_557 ?
