#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312925.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_4312925
loop_
_publ_author_name
'Intyaj Pasha'
'Amitava Choudhury'
'C. N. R. Rao'
_publ_section_title
;
 Organically Templated Vanadyl Selenites with Layered Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              409
_journal_page_last               415
_journal_paper_doi               10.1021/ic020479r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C3 H10 N O8 Se2 V'
_chemical_formula_weight         396.98
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.3152(3)
_cell_length_b                   18.1918(8)
_cell_length_c                   17.7172(8)
_cell_measurement_reflns_used    4507
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.00
_cell_volume                     2035.44(16)
_computing_cell_refinement       SAINT(Siemens,1996)
_computing_data_collection       SMART(Siemens,1996)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL v5.0'
_computing_publication_material  'SHELXTL v5.0'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens CCD-diffractometer'
_diffrn_measurement_method       Ω
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7620
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    8.152
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.644917
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.591
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.00170(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_obs          0.0274
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0226P)²+5.9637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0619
_refine_ls_wR_factor_obs         0.0583
_reflns_number_observed          1242
_reflns_number_total             1458
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020479r_1.cif
_cod_data_source_block           sad1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+5.9637P] 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^)+(0.0226P)^2^+5.9637P] 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        2035.4(2)
_cod_database_code               4312925
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Se1 Se 0.20660(8) 0.48831(3) 0.43210(3) 0.0153(2) Uani 1 d . .
Se2 Se -0.50423(8) 0.67839(3) 0.51322(3) 0.0135(2) Uani 1 d . .
V1 V -0.02129(14) 0.64717(5) 0.46120(5) 0.0140(2) Uani 1 d . .
O1 O 0.1033(6) 0.4048(2) 0.4256(2) 0.0204(8) Uani 1 d . .
O2 O -0.0150(5) 0.5415(2) 0.4257(2) 0.0174(8) Uani 1 d . .
O3 O 0.2912(6) 0.5015(2) 0.3381(2) 0.0326(10) Uani 1 d . .
H8 H 0.3773(6) 0.4695(2) 0.3269(2) 0.049 Uiso 1 calc R .
O4 O -0.7258(5) 0.6300(2) 0.4960(2) 0.0276(10) Uani 1 d . .
O5 O -0.3405(5) 0.6400(2) 0.4489(2) 0.0173(8) Uani 1 d . .
O6 O -0.5589(5) 0.7625(2) 0.4725(2) 0.0150(8) Uani 1 d . .
O7 O 0.0221(6) 0.6898(2) 0.3832(2) 0.0262(9) Uani 1 d . .
N1 N -0.5424(7) 0.7671(2) 0.3185(2) 0.0218(11) Uani 1 d . .
H1 H -0.5732(7) 0.7667(2) 0.3687(2) 0.026 Uiso 1 calc R .
C1 C -0.7105(10) 0.8087(3) 0.2777(3) 0.032(2) Uani 1 d . .
H2 H -0.7099(10) 0.8598(3) 0.2936(3) 0.039 Uiso 1 calc R .
H3 H -0.8485(10) 0.7880(3) 0.2889(3) 0.039 Uiso 1 calc R .
C2 C -0.3343(9) 0.8036(3) 0.3070(3) 0.0293(14) Uani 1 d . .
H4 H -0.2236(9) 0.7755(3) 0.3317(3) 0.035 Uiso 1 calc R .
H5 H -0.3368(9) 0.8524(3) 0.3290(3) 0.035 Uiso 1 calc R .
C3 C -0.5335(11) 0.6899(3) 0.2905(3) 0.037(2) Uani 1 d . .
H6 H -0.6717(11) 0.6671(3) 0.2954(3) 0.044 Uiso 1 calc R .
H7 H -0.4333(11) 0.6618(3) 0.3204(3) 0.044 Uiso 1 calc R .
O10A O 0.2972(11) 0.4829(8) 0.1782(4) 0.034(3) Uiso 0.69(3) d P .
O10 O 0.3050(24) 0.5184(16) 0.1845(8) 0.033(6) Uiso 0.31(3) d P .
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'
Se Se -0.0929 2.2259 '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
O1 Se1 O2 101.1(2) . . ?
O1 Se1 O3 100.2(2) . . ?
O2 Se1 O3 96.3(2) . . ?
O4 Se2 O5 99.8(2) . . ?
O4 Se2 O6 102.8(2) . . ?
O5 Se2 O6 101.9(2) . . ?
O7 V1 O4 100.5(2) . 1_655 ?
O7 V1 O2 100.8(2) . . ?
O4 V1 O2 85.92(14) 1_655 . ?
O7 V1 O5 96.2(2) . . ?
O4 V1 O5 162.5(2) 1_655 . ?
O2 V1 O5 85.72(14) . . ?
O7 V1 O6 97.3(2) . 4_566 ?
O4 V1 O6 93.29(15) 1_655 4_566 ?
O2 V1 O6 161.71(14) . 4_566 ?
O5 V1 O6 89.86(14) . 4_566 ?
O7 V1 O1 174.8(2) . 5_566 ?
O4 V1 O1 82.83(15) 1_655 5_566 ?
O2 V1 O1 83.30(13) . 5_566 ?
O5 V1 O1 80.93(14) . 5_566 ?
O6 V1 O1 78.48(13) 4_566 5_566 ?
Se1 O1 V1 114.2(2) . 5_566 ?
Se1 O2 V1 122.3(2) . . ?
Se1 O3 H8 109.47(13) . . ?
Se2 O4 V1 139.0(2) . 1_455 ?
Se2 O5 V1 120.6(2) . . ?
Se2 O6 V1 116.8(2) . 4_466 ?
C2 N1 C3 110.0(5) . . ?
C2 N1 C1 109.7(4) . . ?
C3 N1 C1 110.2(5) . . ?
C2 N1 H1 109.0(3) . . ?
C3 N1 H1 109.0(3) . . ?
C1 N1 H1 109.0(3) . . ?
N1 C1 C2 108.2(5) . 3_455 ?
N1 C1 H2 110.1(3) . . ?
C2 C1 H2 110.1(3) 3_455 . ?
N1 C1 H3 110.1(3) . . ?
C2 C1 H3 110.1(3) 3_455 . ?
H2 C1 H3 108.4 . . ?
N1 C2 C1 108.9(4) . 3_455 ?
N1 C2 H4 109.9(3) . . ?
C1 C2 H4 109.9(3) 3_455 . ?
N1 C2 H5 109.9(3) . . ?
C1 C2 H5 109.9(3) 3_455 . ?
H4 C2 H5 108.3 . . ?
N1 C3 C3 109.2(3) . 3_455 ?
N1 C3 H6 109.8(3) . . ?
C3 C3 H6 109.8(5) 3_455 . ?
N1 C3 H7 109.8(3) . . ?
C3 C3 H7 109.8(5) 3_455 . ?
H6 C3 H7 108.3 . . ?
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
Se1 O1 1.657(3) . ?
Se1 O2 1.706(3) . ?
Se1 O3 1.765(4) . ?
Se2 O4 1.681(3) . ?
Se2 O5 1.689(3) . ?
Se2 O6 1.727(3) . ?
V1 O7 1.608(4) . ?
V1 O4 1.990(4) 1_655 ?
V1 O2 2.022(3) . ?
V1 O5 2.032(3) . ?
V1 O6 2.034(3) 4_566 ?
V1 O1 2.277(3) 5_566 ?
O1 V1 2.277(3) 5_566 ?
O3 H8 0.82 . ?
O4 V1 1.990(4) 1_455 ?
O6 V1 2.034(3) 4_466 ?
N1 C2 1.486(7) . ?
N1 C3 1.490(7) . ?
N1 C1 1.491(7) . ?
N1 H1 0.91 . ?
C1 C2 1.531(8) 3_455 ?
C1 H2 0.97 . ?
C1 H3 0.97 . ?
C2 C1 1.531(8) 3_455 ?
C2 H4 0.97 . ?
C2 H5 0.97 . ?
C3 C3 1.496(11) 3_455 ?
C3 H6 0.97 . ?
C3 H7 0.97 . ?
O10A O10 0.66(2) . ?
