#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:42:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179343 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324017.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_4324017
loop_
_publ_author_name
'Patricia C. Secrest'
'Steven J. Geib'
'N. John Cooper'
_publ_section_title
;
 Conversion of Dinuclear, Diamagnetic [MoV2O3(NCS)8]4- into Mononuclear,
 Paramagnetic [MoVO(NCS)5]2- through Photolytic Ligand Redistribution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4182
_journal_page_last               4186
_journal_paper_doi               10.1021/ic9607898
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C27 H54 Mo2 N12 O4 S8'
_chemical_formula_weight         1059.18
_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                110.52(3)
_cell_angle_beta                 105.17(3)
_cell_angle_gamma                98.63(3)
_cell_formula_units_Z            1
_cell_length_a                   9.455(2)
_cell_length_b                   11.831(2)
_cell_length_c                   12.772(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1244.4(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3979
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.7425
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_obs          0.0617
_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)+(0.0798P)²+0.8876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1655
_refine_ls_wR_factor_obs         0.1392
_reflns_number_observed          2549
_reflns_number_total             3913
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9607898.cif
_cod_data_source_block           pat3c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.8876P] 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^)+(0.0798P)^2^+0.8876P] 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        1244.4(4)
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               4324017
_cod_database_fobs_code          4324017
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
Mo Mo 0.29963(9) 0.41201(6) 0.45045(5) 0.0652(3) Uani 1 d . .
S1 S 0.1493(4) 0.4412(3) 0.0735(2) 0.1121(9) Uani 1 d . .
S2 S -0.1189(3) 0.0427(3) 0.2671(3) 0.1216(10) Uani 1 d . .
S3 S 0.3376(3) 0.2470(3) 0.7467(2) 0.1051(9) Uani 1 d . .
S4 S 0.4833(4) 0.0418(3) 0.2710(2) 0.1171(10) Uani 1 d . .
O1 O 0.5000 0.5000 0.5000 0.085(2) Uani 1 d S .
O2 O 0.2250(9) 0.5260(6) 0.5114(5) 0.117(2) Uani 1 d . .
O3 O -0.1031(20) 0.1177(19) -0.0157(17) 0.165(7) Uani 0.50 d P .
N1 N 0.2528(7) 0.4265(5) 0.2878(5) 0.070(2) Uani 1 d . .
N2 N 0.0957(9) 0.2683(8) 0.3723(6) 0.079(2) Uani 1 d . .
N3 N 0.3425(8) 0.3574(6) 0.5912(5) 0.075(2) Uani 1 d . .
N4 N 0.3816(7) 0.2471(5) 0.3643(5) 0.063(2) Uani 1 d . .
N5 N 0.3537(8) 0.6911(6) 0.8890(5) 0.072(2) Uani 1 d . .
N6 N 0.1847(7) 0.8108(6) 0.3659(5) 0.069(2) Uani 1 d . .
C1 C 0.2109(8) 0.4316(6) 0.1983(6) 0.062(2) Uani 1 d . .
C2 C 0.0072(11) 0.1735(10) 0.3276(8) 0.077(2) Uani 1 d . .
C3 C 0.3410(8) 0.3107(6) 0.6560(6) 0.057(2) Uani 1 d . .
C4 C 0.4199(8) 0.1615(7) 0.3239(6) 0.058(2) Uani 1 d . .
C6 C -0.0340(30) 0.0472(26) -0.0020(17) 0.108(8) Uani 0.50 d P .
C7 C 0.1202(15) 0.0906(11) 0.0538(10) 0.135(4) Uani 1 d . .
C51 C 0.2358(21) 0.6610(19) 0.7800(12) 0.261(11) Uani 1 d . .
H51A H 0.2694(21) 0.7079(19) 0.7389(12) 0.392 Uiso 1 calc R .
H51B H 0.1472(21) 0.6818(19) 0.7962(12) 0.392 Uiso 1 calc R .
H51C H 0.2113(21) 0.5730(19) 0.7314(12) 0.392 Uiso 1 calc R .
C52 C 0.3126(22) 0.6262(20) 0.9536(17) 0.280(13) Uani 1 d . .
H52A H 0.2814(22) 0.5379(20) 0.9050(17) 0.420 Uiso 1 calc R .
H52B H 0.2301(22) 0.6515(20) 0.9775(17) 0.420 Uiso 1 calc R .
H52C H 0.3981(22) 0.6445(20) 1.0229(17) 0.420 Uiso 1 calc R .
C53 C 0.3981(31) 0.8196(14) 0.9649(15) 0.300(14) Uani 1 d . .
H53A H 0.4275(31) 0.8680(14) 0.9237(15) 0.449 Uiso 1 calc R .
H53B H 0.4826(31) 0.8356(14) 1.0340(15) 0.449 Uiso 1 calc R .
H53C H 0.3146(31) 0.8426(14) 0.9886(15) 0.449 Uiso 1 calc R .
C54 C 0.4819(18) 0.6577(17) 0.8587(17) 0.260(11) Uani 1 d . .
H54A H 0.5104(18) 0.7022(17) 0.8142(17) 0.391 Uiso 1 calc R .
H54B H 0.4553(18) 0.5692(17) 0.8116(17) 0.391 Uiso 1 calc R .
H54C H 0.5656(18) 0.6792(17) 0.9301(17) 0.391 Uiso 1 calc R .
C61 C 0.1060(11) 0.7838(10) 0.2400(7) 0.115(4) Uani 1 d . .
H61A H 0.1644(11) 0.8374(10) 0.2160(7) 0.172 Uiso 1 calc R .
H61B H 0.0072(11) 0.7985(10) 0.2307(7) 0.172 Uiso 1 calc R .
H61C H 0.0953(11) 0.6979(10) 0.1915(7) 0.172 Uiso 1 calc R .
C62 C 0.2070(12) 0.9455(8) 0.4411(8) 0.107(3) Uani 1 d . .
H62A H 0.2655(12) 0.9970(8) 0.4152(8) 0.161 Uiso 1 calc R .
H62B H 0.2601(12) 0.9632(8) 0.5226(8) 0.161 Uiso 1 calc R .
H62C H 0.1098(12) 0.9629(8) 0.4339(8) 0.161 Uiso 1 calc R .
C63 C 0.3356(10) 0.7854(9) 0.3794(9) 0.108(3) Uani 1 d . .
H63A H 0.3952(10) 0.8383(9) 0.3555(9) 0.163 Uiso 1 calc R .
H63B H 0.3227(10) 0.6992(9) 0.3303(9) 0.163 Uiso 1 calc R .
H63C H 0.3865(10) 0.8020(9) 0.4610(9) 0.163 Uiso 1 calc R .
C64 C 0.0959(13) 0.7292(11) 0.4027(11) 0.133(4) Uani 1 d . .
H64A H 0.1471(13) 0.7468(11) 0.4845(11) 0.200 Uiso 1 calc R .
H64B H 0.0851(13) 0.6432(11) 0.3543(11) 0.200 Uiso 1 calc R .
H64C H -0.0029(13) 0.7438(11) 0.3935(11) 0.200 Uiso 1 calc R .
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'
Mo Mo -1.6832 0.6857 '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'
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
O2 Mo O1 100.7(3) . . ?
O2 Mo N3 95.5(3) . . ?
O1 Mo N3 91.8(2) . . ?
O2 Mo N1 95.4(3) . . ?
O1 Mo N1 92.0(2) . . ?
N3 Mo N1 167.6(2) . . ?
O2 Mo N2 95.8(3) . . ?
O1 Mo N2 163.5(2) . . ?
N3 Mo N2 86.1(3) . . ?
N1 Mo N2 87.0(3) . . ?
O2 Mo N4 175.2(3) . . ?
O1 Mo N4 84.1(2) . . ?
N3 Mo N4 83.6(2) . . ?
N1 Mo N4 85.1(2) . . ?
N2 Mo N4 79.4(2) . . ?
Mo O1 Mo 180.0 2_666 . ?
C1 N1 Mo 172.4(7) . . ?
C2 N2 Mo 164.4(7) . . ?
C3 N3 Mo 167.3(6) . . ?
C4 N4 Mo 176.7(6) . . ?
C52 N5 C53 106.7(13) . . ?
C52 N5 C51 112.6(13) . . ?
C53 N5 C51 113.0(13) . . ?
C52 N5 C54 109.2(13) . . ?
C53 N5 C54 108.5(14) . . ?
C51 N5 C54 106.7(12) . . ?
C64 N6 C61 109.6(8) . . ?
C64 N6 C63 108.5(8) . . ?
C61 N6 C63 109.3(7) . . ?
C64 N6 C62 111.1(7) . . ?
C61 N6 C62 109.7(7) . . ?
C63 N6 C62 108.7(7) . . ?
N1 C1 S1 178.5(7) . . ?
N2 C2 S2 178.5(8) . . ?
N3 C3 S3 179.3(6) . . ?
N4 C4 S4 177.1(7) . . ?
O3 C6 C7 118.8(29) . . ?
O3 C6 C6 173.1(38) . 2 ?
C7 C6 C6 67.4(19) . 2 ?
O3 C6 C7 117.7(26) . 2 ?
C7 C6 C7 123.4(15) . 2 ?
C6 C6 C7 56.0(20) 2 2 ?
C6 C7 C6 56.6(15) . 2 ?
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
Mo O2 1.661(5) . ?
Mo O1 1.8418(11) . ?
Mo N3 2.080(6) . ?
Mo N1 2.081(6) . ?
Mo N2 2.103(8) . ?
Mo N4 2.238(6) . ?
S1 C1 1.597(7) . ?
S2 C2 1.594(11) . ?
S3 C3 1.592(8) . ?
S4 C4 1.619(8) . ?
O1 Mo 1.8417(11) 2_666 ?
O3 C6 1.17(2) . ?
N1 C1 1.134(8) . ?
N2 C2 1.141(10) . ?
N3 C3 1.146(8) . ?
N4 C4 1.124(8) . ?
N5 C52 1.395(13) . ?
N5 C53 1.410(15) . ?
N5 C51 1.424(13) . ?
N5 C54 1.434(14) . ?
N6 C64 1.463(11) . ?
N6 C61 1.478(9) . ?
N6 C63 1.481(10) . ?
N6 C62 1.492(10) . ?
C6 C7 1.37(3) . ?
C6 C6 1.38(4) 2 ?
C6 C7 1.52(3) 2 ?
C7 C6 1.52(3) 2 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Mo O1 Mo 75.1(293) . . . 2_666 ?
N3 Mo O1 Mo -20.9(293) . . . 2_666 ?
N1 Mo O1 Mo 170.9(293) . . . 2_666 ?
N2 Mo O1 Mo -103.1(293) . . . 2_666 ?
N4 Mo O1 Mo -104.2(293) . . . 2_666 ?
O2 Mo N1 C1 -59.7(44) . . . . ?
O1 Mo N1 C1 -160.6(44) . . . . ?
N3 Mo N1 C1 92.0(46) . . . . ?
N2 Mo N1 C1 35.9(44) . . . . ?
N4 Mo N1 C1 115.6(44) . . . . ?
O2 Mo N2 C2 -164.7(27) . . . . ?
O1 Mo N2 C2 13.5(32) . . . . ?
N3 Mo N2 C2 -69.5(27) . . . . ?
N1 Mo N2 C2 100.2(27) . . . . ?
N4 Mo N2 C2 14.6(26) . . . . ?
O2 Mo N3 C3 97.1(27) . . . . ?
O1 Mo N3 C3 -162.0(27) . . . . ?
N1 Mo N3 C3 -54.5(33) . . . . ?
N2 Mo N3 C3 1.7(27) . . . . ?
N4 Mo N3 C3 -78.1(27) . . . . ?
O2 Mo N4 C4 -46.8(112) . . . . ?
O1 Mo N4 C4 124.9(100) . . . . ?
N3 Mo N4 C4 32.5(99) . . . . ?
N1 Mo N4 C4 -142.6(100) . . . . ?
N2 Mo N4 C4 -54.7(99) . . . . ?
Mo N1 C1 S1 50.0(299) . . . . ?
Mo N2 C2 S2 148.0(313) . . . . ?
Mo N3 C3 S3 -83.9(551) . . . . ?
Mo N4 C4 S4 -95.2(169) . . . . ?
O3 C6 C7 C6 -176.5(31) . . . 2 ?
C6 C6 C7 C6 0.0 2 . . 2 ?
C7 C6 C7 C6 0.004(2) 2 . . 2 ?
