#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:35:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179191 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/33/4313369.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_4313369
loop_
_publ_author_name
'Geo Paul'
'Amitava Choudhury'
'R. Nagarajan'
'C. N. R. Rao'
_publ_section_title
;
 Amine-Templated Linear Vanadium Sulfates with Different Chain Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2004
_journal_page_last               2013
_journal_paper_doi               10.1021/ic020645v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C6 H15 N2 O10 S2 V'
_chemical_formula_weight         390.26
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.441(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.666(2)
_cell_length_b                   12.0098(12)
_cell_length_c                   12.4810(12)
_cell_measurement_reflns_used    2207
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.05
_cell_volume                     2654.3(5)
_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  0.0873
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5438
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.473159
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.993
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0744P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1394
_refine_ls_wR_factor_obs         0.1178
_reflns_number_observed          1264
_reflns_number_total             1909
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020645v_4.cif
_cod_data_source_block           junk
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0744P)^2^+0.0000P] 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^)+(0.0744P)^2^+0.0000P] 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        2654.3(4)
_cod_database_code               4313369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.0000 0.13684(13) 0.7500 0.0176(5) Uani 1 d S .
V2 V 0.0000 0.0000 0.5000 0.0171(4) Uani 1 d S .
S1 S 0.14745(9) 0.03867(14) 0.92810(14) 0.0214(5) Uani 1 d . .
S2 S 0.04458(9) 0.26124(14) 0.54901(14) 0.0188(5) Uani 1 d . .
O1 O 0.0304(3) 0.0216(4) 0.6621(4) 0.0200(11) Uani 1 d . .
O2 O 0.1054(2) 0.1367(4) 0.8625(4) 0.0213(11) Uani 1 d . .
O3 O 0.0342(3) 0.2584(4) 0.6625(4) 0.0255(12) Uani 1 d . .
O4 O -0.1116(2) 0.0090(4) 0.4843(3) 0.0227(11) Uani 1 d . .
O5 O -0.0001(2) 0.1689(3) 0.4791(3) 0.0198(11) Uani 1 d . .
O6 O 0.2245(2) 0.0705(4) 0.9831(4) 0.0336(13) Uani 1 d . .
O7 O 0.1415(3) -0.0549(4) 0.8507(4) 0.0321(13) Uani 1 d . .
O8 O 0.1238(2) 0.2522(4) 0.5612(4) 0.0305(12) Uani 1 d . .
O9 O 0.0138(3) 0.3669(4) 0.4938(4) 0.0263(12) Uani 1 d . .
O100 O -0.0785(6) 0.4494(8) 0.6307(9) 0.158(5) Uani 1 d . .
N2 N 0.3790(3) 0.1477(5) 0.8344(5) 0.030(2) Uani 1 d . .
C1 C 0.2672(5) 0.0386(6) 0.7345(8) 0.030(2) Uani 1 d . .
C5 C 0.2547(5) 0.2348(8) 0.7819(8) 0.038(2) Uani 1 d . .
C2 C 0.3439(5) 0.0353(7) 0.8225(8) 0.040(2) Uani 1 d . .
C3 C 0.3878(5) 0.1832(9) 0.7242(8) 0.039(2) Uani 1 d . .
C4 C 0.3115(4) 0.1841(7) 0.6354(7) 0.033(2) Uani 1 d . .
C6 C 0.3292(5) 0.2289(10) 0.8710(9) 0.045(3) Uani 1 d . .
N1 N 0.2531(4) 0.1536(5) 0.6888(5) 0.0256(15) Uani 1 d . .
H1 H 0.2072(33) 0.1620(47) 0.6466(47) 0.002(16) Uiso 1 d . .
H2 H 0.2066(52) 0.2108(81) 0.8091(73) 0.084(31) Uiso 1 d . .
H3 H 0.2454(41) 0.2973(62) 0.7500(60) 0.033(23) Uiso 1 d . .
H4 H 0.3238(40) 0.2007(64) 0.9430(68) 0.046(25) Uiso 1 d . .
H5 H 0.3474(48) 0.2843(76) 0.8766(74) 0.044(33) Uiso 1 d . .
H6 H 0.4340(39) 0.1427(55) 0.9003(56) 0.032(19) Uiso 1 d . .
H7 H 0.4190(44) 0.1304(67) 0.7030(63) 0.048(25) Uiso 1 d . .
H8 H 0.4094(49) 0.2423(82) 0.7382(79) 0.064(34) Uiso 1 d . .
H9 H 0.3103(35) 0.1238(59) 0.5687(56) 0.033(20) Uiso 1 d . .
H10 H 0.2968(44) 0.2547(80) 0.5951(69) 0.065(28) Uiso 1 d . .
H11 H 0.2606(33) 0.0017(54) 0.6773(55) 0.010(19) Uiso 1 d . .
H12 H 0.2197(48) 0.0302(67) 0.7555(63) 0.059(26) Uiso 1 d . .
H13 H 0.3371(39) 0.0209(65) 0.8871(65) 0.038(24) Uiso 1 d . .
H14 H 0.3817(49) -0.0175(81) 0.8101(72) 0.075(32) Uiso 1 d . .
H15 H 0.0700(44) -0.0192(72) 0.7164(67) 0.059(26) Uiso 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'
S S 0.1246 0.1234 '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
O1 V1 O1 90.0(3) 2_556 . ?
O1 V1 O2 89.9(2) 2_556 2_556 ?
O1 V1 O2 90.0(2) . 2_556 ?
O1 V1 O2 90.0(2) 2_556 . ?
O1 V1 O2 89.9(2) . . ?
O2 V1 O2 179.9(3) 2_556 . ?
O1 V1 O3 90.6(2) 2_556 2_556 ?
O1 V1 O3 178.3(2) . 2_556 ?
O2 V1 O3 88.4(2) 2_556 2_556 ?
O2 V1 O3 91.7(2) . 2_556 ?
O1 V1 O3 178.3(2) 2_556 . ?
O1 V1 O3 90.6(2) . . ?
O2 V1 O3 91.7(2) 2_556 . ?
O2 V1 O3 88.4(2) . . ?
O3 V1 O3 88.8(2) 2_556 . ?
O1 V2 O1 180.0 . 5_556 ?
O1 V2 O4 92.6(2) . . ?
O1 V2 O4 87.4(2) 5_556 . ?
O1 V2 O4 87.4(2) . 5_556 ?
O1 V2 O4 92.6(2) 5_556 5_556 ?
O4 V2 O4 180.0 . 5_556 ?
O1 V2 O5 90.7(2) . 5_556 ?
O1 V2 O5 89.3(2) 5_556 5_556 ?
O4 V2 O5 91.4(2) . 5_556 ?
O4 V2 O5 88.6(2) 5_556 5_556 ?
O1 V2 O5 89.3(2) . . ?
O1 V2 O5 90.7(2) 5_556 . ?
O4 V2 O5 88.6(2) . . ?
O4 V2 O5 91.4(2) 5_556 . ?
O5 V2 O5 180.0 5_556 . ?
O6 S1 O7 112.0(3) . . ?
O6 S1 O4 109.1(3) . 2_556 ?
O7 S1 O4 110.0(3) . 2_556 ?
O6 S1 O2 108.8(3) . . ?
O7 S1 O2 108.9(3) . . ?
O4 S1 O2 107.9(3) 2_556 . ?
O8 S2 O9 110.5(3) . . ?
O8 S2 O3 109.6(3) . . ?
O9 S2 O3 108.4(3) . . ?
O8 S2 O5 111.8(3) . . ?
O9 S2 O5 107.7(3) . . ?
O3 S2 O5 108.8(2) . . ?
V2 O1 V1 129.7(2) . . ?
V2 O1 H15 124.9(47) . . ?
V1 O1 H15 105.0(48) . . ?
S1 O2 V1 127.1(3) . . ?
S2 O3 V1 133.0(3) . . ?
S1 O4 V2 128.7(3) 2_556 . ?
S2 O5 V2 133.2(3) . . ?
C2 N2 C3 109.9(7) . . ?
C2 N2 C6 108.8(7) . . ?
C3 N2 C6 110.5(7) . . ?
C2 N2 H6 107.7(36) . . ?
C3 N2 H6 111.0(34) . . ?
C6 N2 H6 109.1(35) . . ?
N1 C1 C2 108.4(6) . . ?
N1 C1 H11 102.1(45) . . ?
C2 C1 H11 117.9(44) . . ?
N1 C1 H12 97.6(47) . . ?
C2 C1 H12 121.4(45) . . ?
H11 C1 H12 105.9(63) . . ?
C6 C5 N1 109.3(7) . . ?
C6 C5 H2 114.9(47) . . ?
N1 C5 H2 104.5(49) . . ?
C6 C5 H3 113.7(53) . . ?
N1 C5 H3 105.2(51) . . ?
H2 C5 H3 108.3(74) . . ?
N2 C2 C1 109.6(6) . . ?
N2 C2 H13 106.1(53) . . ?
C1 C2 H13 107.1(49) . . ?
N2 C2 H14 106.4(53) . . ?
C1 C2 H14 117.4(52) . . ?
H13 C2 H14 109.6(71) . . ?
N2 C3 C4 109.0(7) . . ?
N2 C3 H7 108.6(47) . . ?
C4 C3 H7 108.6(48) . . ?
N2 C3 H8 104.0(68) . . ?
C4 C3 H8 116.5(67) . . ?
H7 C3 H8 109.8(78) . . ?
N1 C4 C3 108.9(6) . . ?
N1 C4 H9 109.5(35) . . ?
C3 C4 H9 110.0(34) . . ?
N1 C4 H10 108.4(47) . . ?
C3 C4 H10 115.5(50) . . ?
H9 C4 H10 104.3(61) . . ?
C5 C6 N2 108.9(7) . . ?
C5 C6 H4 110.7(43) . . ?
N2 C6 H4 107.6(45) . . ?
C5 C6 H5 108.7(73) . . ?
N2 C6 H5 107.5(68) . . ?
H4 C6 H5 113.3(85) . . ?
C1 N1 C4 109.5(6) . . ?
C1 N1 C5 110.3(6) . . ?
C4 N1 C5 110.3(6) . . ?
C1 N1 H1 111.4(39) . . ?
C4 N1 H1 115.2(37) . . ?
C5 N1 H1 99.7(38) . . ?
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 O1 1.959(4) 2_556 ?
V1 O1 1.959(4) . ?
V1 O2 2.023(4) 2_556 ?
V1 O2 2.023(4) . ?
V1 O3 2.043(4) 2_556 ?
V1 O3 2.043(4) . ?
V2 O1 1.938(4) . ?
V2 O1 1.938(4) 5_556 ?
V2 O4 2.033(4) . ?
V2 O4 2.033(4) 5_556 ?
V2 O5 2.045(4) 5_556 ?
V2 O5 2.045(4) . ?
S1 O6 1.436(5) . ?
S1 O7 1.463(5) . ?
S1 O4 1.494(4) 2_556 ?
S1 O2 1.505(5) . ?
S2 O8 1.442(5) . ?
S2 O9 1.471(4) . ?
S2 O3 1.489(4) . ?
S2 O5 1.492(4) . ?
O1 H15 0.96(8) . ?
O4 S1 1.494(4) 2_556 ?
N2 C2 1.487(10) . ?
N2 C3 1.497(10) . ?
N2 C6 1.514(11) . ?
N2 H6 1.09(7) . ?
C1 N1 1.485(9) . ?
C1 C2 1.505(11) . ?
C1 H11 0.82(6) . ?
C1 H12 1.01(8) . ?
C5 C6 1.483(13) . ?
C5 N1 1.509(10) . ?
C5 H2 1.09(9) . ?
C5 H3 0.84(7) . ?
C2 H13 0.87(7) . ?
C2 H14 1.00(9) . ?
C3 C4 1.502(12) . ?
C3 H7 0.95(8) . ?
C3 H8 0.81(9) . ?
C4 N1 1.492(9) . ?
C4 H9 1.10(7) . ?
C4 H10 0.98(9) . ?
C6 H4 1.00(8) . ?
C6 H5 0.74(9) . ?
N1 H1 0.86(6) . ?
