#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:35:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179191 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/33/4313368.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_4313368
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            'C4 H14 N2 O10 S2 V'
_chemical_formula_weight         365.23
_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
_cell_angle_alpha                90.46(2)
_cell_angle_beta                 90.47(2)
_cell_angle_gamma                115.68(2)
_cell_formula_units_Z            2
_cell_length_a                   6.2558(10)
_cell_length_b                   7.0663(14)
_cell_length_c                   15.592(4)
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.00
_cell_volume                     621.1(2)
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2620
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.753914
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Bluish-green
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       Rod
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0244(24)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         1755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_obs          0.0279
_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)+(0.0399P)²+0.4644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0753
_refine_ls_wR_factor_obs         0.0735
_reflns_number_observed          1566
_reflns_number_total             1755
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020645v_3.cif
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0399P)^2^+0.4644P] 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^)+(0.0399P)^2^+0.4644P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313368
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.05218(8) 0.93409(7) 0.26590(3) 0.0154(2) Uani 1 d . .
S1 S 0.23656(13) 1.29811(11) 0.16901(5) 0.0172(2) Uani 1 d . .
S2 S 0.54494(12) 0.92382(11) 0.30028(4) 0.0163(2) Uani 1 d . .
O1 O 0.0472(4) 0.9073(3) 0.36658(13) 0.0271(5) Uani 1 d . .
O2 O -0.2623(4) 0.9331(3) 0.24223(13) 0.0240(5) Uani 1 d . .
O3 O -0.0943(5) 0.6421(4) 0.2176(2) 0.0367(7) Uani 1 d . .
O4 O 0.3640(3) 0.9324(3) 0.23853(12) 0.0217(5) Uani 1 d . .
O5 O 0.2148(4) 1.2552(3) 0.26339(12) 0.0218(5) Uani 1 d . .
O6 O 0.1149(4) 1.0850(3) 0.12913(12) 0.0206(5) Uani 1 d . .
O7 O 0.1149(4) 1.4242(3) 0.14439(14) 0.0283(5) Uani 1 d . .
O8 O 0.4852(4) 1.3969(3) 0.14480(14) 0.0293(5) Uani 1 d . .
O9 O 0.6303(4) 1.1023(4) 0.3575(2) 0.0450(7) Uani 1 d . .
O10 O 0.4468(5) 0.7275(4) 0.3444(2) 0.0460(7) Uani 1 d . .
C1 C -0.3084(6) 1.2083(5) -0.0008(2) 0.0266(7) Uani 1 d . .
N1 N -0.3553(6) 1.0709(4) 0.0756(2) 0.0245(6) Uani 1 d . .
C2 C -0.4668(6) 0.8454(5) 0.0506(2) 0.0259(7) Uani 1 d . .
C3 C -0.7238(6) 0.3284(5) 0.4744(2) 0.0296(8) Uani 1 d . .
N2 N -0.5100(5) 0.3973(5) 0.4197(2) 0.0276(7) Uani 1 d . .
C4 C -0.2859(6) 0.4906(5) 0.4713(2) 0.0270(8) Uani 1 d . .
H1 H -0.4467(69) 1.0906(56) 0.1035(23) 0.031(11) Uiso 1 d . .
H2 H -0.2175(74) 1.1113(57) 0.0997(23) 0.033(10) Uiso 1 d . .
H3 H -0.1899(66) 1.1870(54) -0.0332(23) 0.034(10) Uiso 1 d . .
H4 H -0.2555(59) 1.3509(58) 0.0135(21) 0.028(9) Uiso 1 d . .
H5 H -0.3500(59) 0.8157(48) 0.0141(20) 0.022(8) Uiso 1 d . .
H6 H -0.5031(59) 0.7675(52) 0.0970(22) 0.025(9) Uiso 1 d . .
H7 H -0.5152(64) 0.4897(60) 0.3850(24) 0.033(10) Uiso 1 d . .
H8 H -0.5098(66) 0.2959(63) 0.3933(23) 0.036(11) Uiso 1 d . .
H9 H -0.7297(65) 0.2191(60) 0.5079(24) 0.038(10) Uiso 1 d . .
H10 H -0.8696(77) 0.2712(62) 0.4417(25) 0.047(11) Uiso 1 d . .
H11 H -0.2762(57) 0.3784(53) 0.5050(21) 0.025(8) Uiso 1 d . .
H12 H -0.1563(66) 0.5393(53) 0.4314(22) 0.033(9) Uiso 1 d . .
H13 H -0.0314(83) 0.5850(69) 0.2061(28) 0.048(15) Uiso 1 d . .
H14 H -0.2243(98) 0.5769(75) 0.2044(30) 0.063(16) 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 O2 101.94(10) . . ?
O1 V1 O3 105.22(12) . . ?
O2 V1 O3 85.52(11) . . ?
O1 V1 O4 100.81(10) . . ?
O2 V1 O4 157.06(8) . . ?
O3 V1 O4 85.72(11) . . ?
O1 V1 O5 98.00(10) . . ?
O2 V1 O5 90.79(9) . . ?
O3 V1 O5 156.76(11) . . ?
O4 V1 O5 88.96(9) . . ?
O1 V1 O6 162.07(10) . . ?
O2 V1 O6 79.10(8) . . ?
O3 V1 O6 92.72(10) . . ?
O4 V1 O6 80.19(8) . . ?
O5 V1 O6 64.07(8) . . ?
O1 V1 S1 129.75(9) . . ?
O2 V1 S1 85.31(7) . . ?
O3 V1 S1 124.99(9) . . ?
O4 V1 S1 82.45(6) . . ?
O5 V1 S1 31.77(6) . . ?
O6 V1 S1 32.34(5) . . ?
O7 S1 O8 111.64(14) . . ?
O7 S1 O6 109.83(13) . . ?
O8 S1 O6 110.23(12) . . ?
O7 S1 O5 111.02(12) . . ?
O8 S1 O5 110.39(13) . . ?
O6 S1 O5 103.43(12) . . ?
O7 S1 V1 126.59(10) . . ?
O8 S1 V1 121.45(10) . . ?
O6 S1 V1 57.62(8) . . ?
O5 S1 V1 45.90(8) . . ?
O10 S2 O9 113.0(2) . . ?
O10 S2 O2 110.03(14) . 1_655 ?
O9 S2 O2 110.51(14) . 1_655 ?
O10 S2 O4 109.67(14) . . ?
O9 S2 O4 110.64(14) . . ?
O2 S2 O4 102.54(11) 1_655 . ?
S2 O2 V1 131.91(13) 1_455 . ?
V1 O3 H13 124.7(38) . . ?
V1 O3 H14 127.3(36) . . ?
H13 O3 H14 107.7(50) . . ?
S2 O4 V1 127.75(12) . . ?
S1 O5 V1 102.33(11) . . ?
S1 O6 V1 90.04(9) . . ?
N1 C1 C2 110.3(3) . 2_475 ?
N1 C1 H3 105.8(21) . . ?
C2 C1 H3 113.1(21) 2_475 . ?
N1 C1 H4 113.3(20) . . ?
C2 C1 H4 104.0(21) 2_475 . ?
H3 C1 H4 110.5(29) . . ?
C2 N1 C1 111.5(3) . . ?
C2 N1 H1 107.1(27) . . ?
C1 N1 H1 106.8(27) . . ?
C2 N1 H2 113.5(24) . . ?
C1 N1 H2 103.9(23) . . ?
H1 N1 H2 113.9(37) . . ?
N1 C2 C1 110.7(3) . 2_475 ?
N1 C2 H5 108.5(18) . . ?
C1 C2 H5 109.9(18) 2_475 . ?
N1 C2 H6 109.7(21) . . ?
C1 C2 H6 107.7(22) 2_475 . ?
H5 C2 H6 110.4(27) . . ?
N2 C3 C4 110.2(3) . 2_466 ?
N2 C3 H9 108.2(23) . . ?
C4 C3 H9 111.4(22) 2_466 . ?
N2 C3 H10 112.9(23) . . ?
C4 C3 H10 109.1(23) 2_466 . ?
H9 C3 H10 105.0(33) . . ?
C3 N2 C4 112.0(3) . . ?
C3 N2 H7 107.1(24) . . ?
C4 N2 H7 109.7(25) . . ?
C3 N2 H8 110.1(26) . . ?
C4 N2 H8 106.8(27) . . ?
H7 N2 H8 111.2(35) . . ?
N2 C4 C3 110.7(3) . 2_466 ?
N2 C4 H11 107.8(20) . . ?
C3 C4 H11 113.2(19) 2_466 . ?
N2 C4 H12 107.1(21) . . ?
C3 C4 H12 110.0(20) 2_466 . ?
H11 C4 H12 107.8(28) . . ?
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 1.582(2) . ?
V1 O2 1.996(2) . ?
V1 O3 1.997(3) . ?
V1 O4 2.005(2) . ?
V1 O5 2.046(2) . ?
V1 O6 2.351(2) . ?
V1 S1 2.7837(11) . ?
S1 O7 1.452(2) . ?
S1 O8 1.457(2) . ?
S1 O6 1.489(2) . ?
S1 O5 1.500(2) . ?
S2 O10 1.434(2) . ?
S2 O9 1.436(2) . ?
S2 O2 1.492(2) 1_655 ?
S2 O4 1.502(2) . ?
O2 S2 1.492(2) 1_455 ?
O3 H13 0.70(5) . ?
O3 H14 0.77(5) . ?
C1 N1 1.491(4) . ?
C1 C2 1.496(5) 2_475 ?
C1 H3 0.96(4) . ?
C1 H4 0.94(4) . ?
N1 C2 1.483(4) . ?
N1 H1 0.78(4) . ?
N1 H2 0.86(4) . ?
C2 C1 1.496(5) 2_475 ?
C2 H5 1.02(3) . ?
C2 H6 0.88(3) . ?
C3 N2 1.488(4) . ?
C3 C4 1.507(5) 2_466 ?
C3 H9 0.92(4) . ?
C3 H10 0.96(4) . ?
N2 C4 1.491(4) . ?
N2 H7 0.86(4) . ?
N2 H8 0.82(4) . ?
C4 C3 1.507(5) 2_466 ?
C4 H11 0.98(3) . ?
C4 H12 0.97(4) . ?
