#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/70/7027090.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027090
loop_
_publ_author_name
'Sokolov, Maxim'
'Imoto, Hideo'
'Saito, Taro'
'Fedorov, Vladimir'
_publ_section_title
;
 Substitution of bridging S2 ligands in the [Nb2(μ-S2)2]4+ core: a simple
 route to [Nb2(Se2)2]4+, [Nb2(S)(Te2)]4+ and [Nb2(S)2]4+
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              85
_journal_paper_doi               10.1039/a806627b
_journal_year                    1999
_chemical_formula_moiety         'C20 H28 Nb2 O8 S4 '
_chemical_formula_structural     '[Nb2 (S2)2 (CH3 CO CH CO CH3)4]'
_chemical_formula_sum            'C20 H28 Nb2 O8 S4'
_chemical_formula_weight         710.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Sun May  3 22:50:29 1998'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             ' May 7 1998'
_cell_angle_alpha                90
_cell_angle_beta                 121.036(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.923(3)
_cell_length_b                   7.868(3)
_cell_length_c                   17.819(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      10.6
_cell_volume                     2873.9(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.00879
_diffrn_orient_matrix_UB_12      -0.08194
_diffrn_orient_matrix_UB_13      0.04778
_diffrn_orient_matrix_UB_21      0.00980
_diffrn_orient_matrix_UB_22      0.09704
_diffrn_orient_matrix_UB_23      0.04123
_diffrn_orient_matrix_UB_31      -0.04698
_diffrn_orient_matrix_UB_32      0.00491
_diffrn_orient_matrix_UB_33      -0.01753
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.111
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3634
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0.11
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1432.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.327
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     210
_refine_ls_number_reflns         1917
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.0292
_refine_ls_shift/esd_mean        0.0016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + (1/4)(0.003|Fo|)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0243
_reflns_number_observed          1917
_reflns_number_total             3547
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            806627Bsup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
(1/4)(0.003|Fo|)^2^]' 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) + (1/4)(0.003|Fo|)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2873(1)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C20 H28 Nb2 O8 S4 '
_cod_database_code               7027090
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_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_calc_flag
_atom_site_occupancy
Nb 0.19218(2) 0.24843(8) 0.00704(3) 0.0314(1) Uani d 1.00
S(1) 0.19172(6) 0.2765(2) -0.13499(8) 0.0421(4) Uani d 1.00
S(2) 0.21560(7) 0.0431(2) -0.08023(9) 0.0393(4) Uani d 1.00
O(1) 0.1461(2) 0.4904(4) -0.0422(2) 0.042(1) Uani d 1.00
O(2) 0.0935(2) 0.1674(4) -0.0706(2) 0.046(1) Uani d 1.00
O(3) 0.1671(2) 0.3272(4) 0.1004(2) 0.043(1) Uani d 1.00
O(4) 0.1907(2) 0.0058(4) 0.0606(2) 0.039(1) Uani d 1.00
C(1) 0.0764(5) 0.719(1) -0.1126(7) 0.079(3) Uani d 1.00
C(2) 0.0882(3) 0.5318(8) -0.0924(4) 0.057(2) Uani d 1.00
C(3) 0.0360(4) 0.418(1) -0.1296(7) 0.110(3) Uani d 1.00
C(4) 0.0406(3) 0.244(1) -0.1157(4) 0.074(2) Uani d 1.00
C(5) -0.0210(5) 0.139(2) -0.156(1) 0.133(5) Uani d 1.00
C(6) 0.1411(6) 0.353(1) 0.2102(8) 0.078(4) Uani d 1.00
C(7) 0.1595(2) 0.2476(9) 0.1554(3) 0.045(2) Uani d 1.00
C(8) 0.1660(3) 0.0718(8) 0.1682(4) 0.054(2) Uani d 1.00
C(9) 0.1800(2) -0.0401(7) 0.1189(3) 0.036(2) Uani d 1.00
C(10) 0.1805(5) -0.226(1) 0.1350(6) 0.064(3) Uani d 1.00
H(1) 0.061(3) 0.739(9) -0.077(3) 0.06(2) Uiso calc 1.00
H(2) 0.097(3) 0.754(10) -0.141(4) 0.08(2) Uiso calc 1.00
H(3) 0.039(3) 0.73(1) -0.162(4) 0.16(4) Uiso calc 1.00
H(4) -0.001(3) 0.465(7) -0.166(3) 0.05(2) Uiso calc 1.00
H(5) -0.060(3) 0.20(1) -0.173(5) 0.14(3) Uiso calc 1.00
H(6) -0.016(5) 0.10(1) -0.204(6) 0.16(6) Uiso calc 1.00
H(7) -0.020(3) 0.042(8) -0.116(4) 0.08(2) Uiso calc 1.00
H(8) 0.158(3) 0.448(8) 0.224(4) 0.08(3) Uiso calc 1.00
H(9) 0.103(3) 0.412(8) 0.177(4) 0.07(2) Uiso calc 1.00
H(10) 0.138(3) 0.290(9) 0.248(4) 0.12(3) Uiso calc 1.00
H(11) 0.159(3) 0.028(7) 0.209(3) 0.06(2) Uiso calc 1.00
H(12) 0.190(2) -0.248(8) 0.188(3) 0.06(2) Uiso calc 1.00
H(13) 0.154(3) -0.287(9) 0.087(4) 0.10(3) Uiso calc 1.00
H(14) 0.217(3) -0.264(10) 0.136(4) 0.09(3) Uiso calc 1.00
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 80 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 112 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 32 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Nb 0 8 -2.073 0.621
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S 0 16 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and
 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-8 0 6
-5 -1 5
-2 0 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_2
_geom_angle_site_symmetry_3
Nb Nb S(1) 55.04(3) 7_555 1_555 1_555
Nb Nb S(1) 55.06(3) 7_555 1_555 7_555
Nb Nb S(2) 54.71(4) 7_555 1_555 1_555
Nb Nb S(2) 54.39(4) 7_555 1_555 7_555
Nb Nb O(1) 105.6(1) 7_555 1_555 1_555
Nb Nb O(2) 137.2(1) 7_555 1_555 1_555
Nb Nb O(3) 136.8(1) 7_555 1_555 1_555
Nb Nb O(4) 106.33(9) 7_555 1_555 1_555
S(1) Nb S(1) 110.10(4) 1_555 1_555 7_555
S(1) Nb S(2) 47.30(5) 1_555 1_555 1_555
S(1) Nb S(2) 90.69(5) 1_555 1_555 7_555
S(1) Nb O(1) 77.17(10) 1_555 1_555 1_555
S(1) Nb O(2) 86.8(1) 1_555 1_555 1_555
S(1) Nb O(3) 153.67(10) 1_555 1_555 1_555
S(1) Nb O(4) 122.00(10) 1_555 1_555 1_555
S(1) Nb S(2) 90.94(5) 7_555 1_555 1_555
S(1) Nb S(2) 47.21(5) 7_555 1_555 7_555
S(1) Nb O(1) 122.0(1) 7_555 1_555 1_555
S(1) Nb O(2) 153.6(1) 7_555 1_555 1_555
S(1) Nb O(3) 86.5(1) 7_555 1_555 1_555
S(1) Nb O(4) 78.00(10) 7_555 1_555 1_555
S(2) Nb S(2) 109.10(4) 1_555 1_555 7_555
S(2) Nb O(1) 123.49(10) 1_555 1_555 1_555
S(2) Nb O(2) 86.0(1) 1_555 1_555 1_555
S(2) Nb O(3) 156.60(10) 1_555 1_555 1_555
S(2) Nb O(4) 76.21(9) 1_555 1_555 1_555
S(2) Nb O(1) 76.2(1) 7_555 1_555 1_555
S(2) Nb O(2) 156.6(1) 7_555 1_555 1_555
S(2) Nb O(3) 86.0(1) 7_555 1_555 1_555
S(2) Nb O(4) 124.26(10) 7_555 1_555 1_555
O(1) Nb O(2) 80.6(1) 1_555 1_555 1_555
O(1) Nb O(3) 76.7(1) 1_555 1_555 1_555
O(1) Nb O(4) 148.1(1) 1_555 1_555 1_555
O(2) Nb O(3) 86.0(1) 1_555 1_555 1_555
O(2) Nb O(4) 75.8(1) 1_555 1_555 1_555
O(3) Nb O(4) 80.5(1) 1_555 1_555 1_555
Nb S(1) Nb 69.90(4) 1_555 1_555 7_555
Nb S(1) S(2) 65.40(5) 1_555 1_555 1_555
Nb S(1) S(2) 65.73(6) 7_555 1_555 1_555
Nb S(2) Nb 70.90(4) 1_555 1_555 7_555
Nb S(2) S(1) 67.30(6) 1_555 1_555 1_555
Nb S(2) S(1) 67.06(6) 7_555 1_555 1_555
Nb O(1) C(2) 132.2(4) 1_555 1_555 1_555
Nb O(2) C(4) 133.6(5) 1_555 1_555 1_555
Nb O(3) C(7) 132.7(4) 1_555 1_555 1_555
Nb O(4) C(9) 133.5(3) 1_555 1_555 1_555
C(2) C(1) H(1) 95(4) 1_555 1_555 1_555
C(2) C(1) H(2) 109(4) 1_555 1_555 1_555
C(2) C(1) H(3) 109(7) 1_555 1_555 1_555
H(1) C(1) H(2) 150(6) 1_555 1_555 1_555
H(1) C(1) H(3) 96(6) 1_555 1_555 1_555
H(2) C(1) H(3) 87(5) 1_555 1_555 1_555
O(1) C(2) C(1) 115.4(7) 1_555 1_555 1_555
O(1) C(2) C(3) 124.5(6) 1_555 1_555 1_555
C(1) C(2) C(3) 120.1(7) 1_555 1_555 1_555
C(2) C(3) C(4) 125.4(7) 1_555 1_555 1_555
C(2) C(3) H(4) 113(3) 1_555 1_555 1_555
C(4) C(3) H(4) 121(3) 1_555 1_555 1_555
O(2) C(4) C(3) 123.5(7) 1_555 1_555 1_555
O(2) C(4) C(5) 117.2(8) 1_555 1_555 1_555
C(3) C(4) C(5) 119.3(7) 1_555 1_555 1_555
C(4) C(5) H(5) 113(5) 1_555 1_555 1_555
C(4) C(5) H(6) 94(5) 1_555 1_555 1_555
C(4) C(5) H(7) 113(3) 1_555 1_555 1_555
H(5) C(5) H(6) 115(8) 1_555 1_555 1_555
H(5) C(5) H(7) 107(6) 1_555 1_555 1_555
H(6) C(5) H(7) 112(7) 1_555 1_555 1_555
C(7) C(6) H(8) 116(5) 1_555 1_555 1_555
C(7) C(6) H(9) 113(4) 1_555 1_555 1_555
C(7) C(6) H(10) 111(4) 1_555 1_555 1_555
H(8) C(6) H(9) 84(5) 1_555 1_555 1_555
H(8) C(6) H(10) 120(6) 1_555 1_555 1_555
H(9) C(6) H(10) 108(6) 1_555 1_555 1_555
O(3) C(7) C(6) 116.1(7) 1_555 1_555 1_555
O(3) C(7) C(8) 125.0(5) 1_555 1_555 1_555
C(6) C(7) C(8) 118.9(6) 1_555 1_555 1_555
C(7) C(8) C(9) 124.2(5) 1_555 1_555 1_555
C(7) C(8) H(11) 117(3) 1_555 1_555 1_555
C(9) C(8) H(11) 118(3) 1_555 1_555 1_555
O(4) C(9) C(8) 124.0(5) 1_555 1_555 1_555
O(4) C(9) C(10) 117.4(5) 1_555 1_555 1_555
C(8) C(9) C(10) 118.6(5) 1_555 1_555 1_555
C(9) C(10) H(12) 112(4) 1_555 1_555 1_555
C(9) C(10) H(13) 114(4) 1_555 1_555 1_555
C(9) C(10) H(14) 104(4) 1_555 1_555 1_555
H(12) C(10) H(13) 125(6) 1_555 1_555 1_555
H(12) C(10) H(14) 101(5) 1_555 1_555 1_555
H(13) C(10) H(14) 92(5) 1_555 1_555 1_555
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Nb Nb 2.9039(9) 1_555 7_555
Nb S(1) 2.535(1) 1_555 1_555
Nb S(1) 2.534(1) 1_555 7_555
Nb S(2) 2.498(1) 1_555 1_555
Nb S(2) 2.508(2) 1_555 7_555
Nb O(1) 2.147(4) 1_555 1_555
Nb O(2) 2.127(4) 1_555 1_555
Nb O(3) 2.131(3) 1_555 1_555
Nb O(4) 2.143(3) 1_555 1_555
S(1) S(2) 2.019(2) 1_555 1_555
O(1) C(2) 1.245(6) 1_555 1_555
O(2) C(4) 1.250(7) 1_555 1_555
O(3) C(7) 1.252(6) 1_555 1_555
O(4) C(9) 1.245(5) 1_555 1_555
C(1) C(2) 1.507(10) 1_555 1_555
C(2) C(3) 1.394(9) 1_555 1_555
C(3) C(4) 1.39(1) 1_555 1_555
C(4) C(5) 1.51(1) 1_555 1_555
C(6) C(7) 1.508(9) 1_555 1_555
C(7) C(8) 1.398(9) 1_555 1_555
C(8) C(9) 1.400(7) 1_555 1_555
C(9) C(10) 1.487(9) 1_555 1_555
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
O(1) C(10) 3.598(9) 1_555 1_565
O(2) C(1) 3.588(9) 1_555 1_545
O(3) C(10) 3.556(9) 1_555 1_565
