#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:43:26 +0100 (vie 25 de mar de 2016) $
#$Revision: 179986 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028004.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_7028004
loop_
_publ_author_name
'Stelzig, Lutz'
'Kötte, Stephan'
'Krebs, Bernt'
_publ_section_title
;
 Molybdenum complexes with tridentate NS2 ligands. Synthesis, crystal
 structures and spectroscopic properties
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2921
_journal_paper_doi               10.1039/a802334d
_journal_year                    1998
_chemical_formula_sum            'C57 H48 Cl6 Mo2 N6 O3 S4'
_chemical_formula_weight         1397.83
_chemical_name_common
;
(2-oxo)Bis(1-mercaptobenzaldehyde)
-4-triphenylmethylthiosemicarbazone-S,S,N)-oxo-molybdenum(V) 
;
_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                 121.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.449(4)
_cell_length_b                   19.763(4)
_cell_length_c                   18.450(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6041(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24807
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         5.30
_exptl_absorpt_coefficient_mu    0.867
_exptl_crystal_colour            'deep red to violet'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.686
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_obs          0.0672
_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)+(0.0889P)²+19.4345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2131
_refine_ls_wR_factor_obs         0.1657
_reflns_number_observed          4575
_reflns_number_total             6700
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            D802334sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+19.4345P] 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^)+(0.0889P)^2^+19.4345P] 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        6040.8(22)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028004
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
Mo1 Mo 0.05650(3) 0.07819(2) 0.05525(3) 0.0600(2) Uani 1 d .
S1 S -0.04466(9) 0.13978(7) -0.06361(9) 0.0665(4) Uani 1 d .
S2 S 0.07307(11) 0.02404(7) 0.17726(11) 0.0749(5) Uani 1 d .
O1 O 0.0000 0.0000 0.0000 0.078(2) Uani 1 d S
O2 O 0.1419(3) 0.0797(3) 0.0558(4) 0.0920(15) Uani 1 d .
N1 N 0.0568(3) 0.1735(2) 0.1124(3) 0.0594(11) Uani 1 d .
N2 N 0.0386(3) 0.2321(2) 0.0610(3) 0.0651(12) Uani 1 d .
N3 N -0.0325(3) 0.2713(2) -0.0760(3) 0.0603(11) Uani 1 d .
H3N H -0.0603(3) 0.2604(2) -0.1316(3) 0.080 Uiso 1 d R
C1 C 0.1038(4) 0.0769(3) 0.2648(4) 0.0661(14) Uani 1 d .
C2 C 0.1291(4) 0.0455(4) 0.3418(4) 0.083(2) Uani 1 d .
H2A H 0.1341(4) -0.0029(4) 0.3446(4) 0.080 Uiso 1 d R
C3 C 0.1461(5) 0.0810(4) 0.4129(5) 0.089(2) Uani 1 d .
H3A H 0.1624(5) 0.0577(4) 0.4652(5) 0.080 Uiso 1 d R
C4 C 0.1410(4) 0.1504(4) 0.4097(4) 0.087(2) Uani 1 d .
H4A H 0.1516(4) 0.1757(4) 0.4589(4) 0.080 Uiso 1 d R
C5 C 0.1188(4) 0.1835(4) 0.3359(4) 0.083(2) Uani 1 d .
H5A H 0.1172(4) 0.2320(4) 0.3340(4) 0.080 Uiso 1 d R
C6 C 0.1000(4) 0.1478(3) 0.2611(4) 0.0665(14) Uani 1 d .
C7 C 0.0755(4) 0.1893(3) 0.1882(4) 0.0685(14) Uani 1 d .
H7A H 0.0712(4) 0.2366(3) 0.1970(4) 0.080 Uiso 1 d R
C8 C -0.0083(3) 0.2201(3) -0.0196(4) 0.0606(13) Uani 1 d .
C9 C -0.0177(3) 0.3443(2) -0.0541(3) 0.0527(11) Uani 1 d .
C10 C -0.0391(3) 0.3603(2) 0.0135(3) 0.0562(12) Uani 1 d .
C11 C -0.1114(4) 0.3351(3) 0.0010(4) 0.0672(14) Uani 1 d .
H11A H -0.1452(4) 0.3079(3) -0.0483(4) 0.080 Uiso 1 d R
C12 C -0.1352(4) 0.3495(4) 0.0582(4) 0.080(2) Uani 1 d .
H12A H -0.1851(4) 0.3318(4) 0.0491(4) 0.080 Uiso 1 d R
C13 C -0.0874(5) 0.3887(4) 0.1281(5) 0.088(2) Uani 1 d .
H13A H -0.1032(5) 0.3987(4) 0.1683(5) 0.080 Uiso 1 d R
C14 C -0.0162(5) 0.4133(3) 0.1406(4) 0.078(2) Uani 1 d .
H14A H 0.0170(5) 0.4417(3) 0.1888(4) 0.080 Uiso 1 d R
C15 C 0.0087(4) 0.3989(3) 0.0852(3) 0.0612(13) Uani 1 d .
H15A H 0.0599(4) 0.4150(3) 0.0963(3) 0.080 Uiso 1 d R
C16 C -0.0746(3) 0.3824(2) -0.1380(3) 0.0546(11) Uani 1 d .
C17 C -0.0661(4) 0.3707(3) -0.2066(4) 0.0697(15) Uani 1 d .
H17A H -0.0276(4) 0.3380(3) -0.2022(4) 0.080 Uiso 1 d R
C18 C -0.1149(5) 0.4055(4) -0.2824(4) 0.083(2) Uani 1 d .
H18A H -0.1086(5) 0.3982(4) -0.3300(4) 0.080 Uiso 1 d R
C19 C -0.1715(4) 0.4514(4) -0.2901(4) 0.079(2) Uani 1 d .
H19A H -0.2046(4) 0.4751(4) -0.3428(4) 0.080 Uiso 1 d R
C20 C -0.1796(4) 0.4626(3) -0.2226(5) 0.083(2) Uani 1 d .
H20A H -0.2193(4) 0.4944(3) -0.2280(5) 0.080 Uiso 1 d R
C21 C -0.1315(4) 0.4287(3) -0.1460(4) 0.0674(14) Uani 1 d .
H21A H -0.1373(4) 0.4369(3) -0.0982(4) 0.080 Uiso 1 d R
C22 C 0.0694(3) 0.3641(2) -0.0265(3) 0.0548(11) Uani 1 d .
C23 C 0.0904(4) 0.4315(3) -0.0186(4) 0.0622(13) Uani 1 d .
H23A H 0.0504(4) 0.4651(3) -0.0294(4) 0.080 Uiso 1 d R
C24 C 0.1672(4) 0.4523(3) 0.0033(4) 0.0687(14) Uani 1 d .
H24A H 0.1800(4) 0.4997(3) 0.0088(4) 0.080 Uiso 1 d R
C25 C 0.2246(4) 0.4049(3) 0.0170(4) 0.073(2) Uani 1 d .
H25A H 0.2779(4) 0.4191(3) 0.0328(4) 0.080 Uiso 1 d R
C26 C 0.2050(4) 0.3379(4) 0.0086(5) 0.081(2) Uani 1 d .
H26A H 0.2448(4) 0.3047(4) 0.0178(5) 0.080 Uiso 1 d R
C27 C 0.1285(4) 0.3170(3) -0.0133(4) 0.0690(15) Uani 1 d .
H27A H 0.1157(4) 0.2696(3) -0.0194(4) 0.080 Uiso 1 d R
C1L C 0.0000 -0.1319(6) 0.2500 0.100(3) Uani 1 d S
H1LA H -0.0078 -0.1034(6) 0.2873 0.080 Uiso 1 d R
Cl1 Cl -0.0832(2) -0.1800(2) 0.1915(2) 0.1760(14) Uani 1 d .
C2L C 0.2321(7) 0.3178(6) 0.2156(7) 0.134(4) Uani 1 d .
H2LA H 0.1802(7) 0.3212(6) 0.1641(7) 0.080 Uiso 1 d R
H2LB H 0.2680(7) 0.3483(6) 0.2108(7) 0.080 Uiso 1 d R
Cl3 Cl 0.2658(2) 0.23785(15) 0.2224(2) 0.1439(10) Uani 1 d .
Cl4 Cl 0.2221(2) 0.3434(2) 0.2984(2) 0.1571(12) Uani 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O2 Mo1 O1 108.7(2) .
O2 Mo1 N1 103.6(2) .
O1 Mo1 N1 147.42(13) .
O2 Mo1 S2 111.5(2) .
O1 Mo1 S2 83.81(5) .
N1 Mo1 S2 88.05(13) .
O2 Mo1 S1 109.9(2) .
O1 Mo1 S1 87.36(5) .
N1 Mo1 S1 78.01(13) .
S2 Mo1 S1 138.34(7) .
C8 S1 Mo1 95.6(2) .
C1 S2 Mo1 114.9(2) .
Mo1 O1 Mo1 180.0 5
C7 N1 N2 111.1(4) .
C7 N1 Mo1 132.0(4) .
N2 N1 Mo1 116.8(3) .
C8 N2 N1 113.4(4) .
C8 N3 C9 125.5(4) .
C2 C1 C6 118.7(6) .
C2 C1 S2 116.5(5) .
C6 C1 S2 124.8(5) .
C3 C2 C1 122.1(7) .
C2 C3 C4 119.7(7) .
C5 C4 C3 120.1(7) .
C4 C5 C6 121.3(7) .
C1 C6 C5 118.0(6) .
C1 C6 C7 127.0(5) .
C5 C6 C7 114.9(6) .
N1 C7 C6 130.6(6) .
N2 C8 N3 120.0(5) .
N2 C8 S1 124.6(4) .
N3 C8 S1 115.4(4) .
N3 C9 C10 108.9(4) .
N3 C9 C22 111.0(4) .
C10 C9 C22 113.3(4) .
N3 C9 C16 105.4(4) .
C10 C9 C16 110.8(4) .
C22 C9 C16 107.0(4) .
C15 C10 C11 118.1(5) .
C15 C10 C9 123.9(5) .
C11 C10 C9 118.1(5) .
C12 C11 C10 120.8(6) .
C13 C12 C11 120.1(7) .
C14 C13 C12 119.2(6) .
C13 C14 C15 121.4(6) .
C14 C15 C10 120.4(6) .
C17 C16 C21 119.1(5) .
C17 C16 C9 118.0(5) .
C21 C16 C9 122.8(5) .
C16 C17 C18 119.5(6) .
C19 C18 C17 121.2(7) .
C20 C19 C18 119.0(6) .
C19 C20 C21 121.0(6) .
C16 C21 C20 120.1(6) .
C23 C22 C27 117.0(5) .
C23 C22 C9 119.6(5) .
C27 C22 C9 123.3(5) .
C22 C23 C24 122.0(6) .
C25 C24 C23 119.9(6) .
C26 C25 C24 119.1(6) .
C25 C26 C27 121.2(6) .
C26 C27 C22 120.7(5) .
Cl1 C1L Cl1 111.6(7) 2
Cl3 C2L Cl4 115.4(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.656(5) .
Mo1 O1 1.8604(6) .
Mo1 N1 2.158(4) .
Mo1 S2 2.357(2) .
Mo1 S1 2.375(2) .
S1 C8 1.754(5) .
S2 C1 1.745(7) .
O1 Mo1 1.8603(6) 5
N1 C7 1.286(7) .
N1 N2 1.417(6) .
N2 C8 1.296(7) .
N3 C8 1.348(6) .
N3 C9 1.485(6) .
C1 C2 1.384(9) .
C1 C6 1.402(8) .
C2 C3 1.368(10) .
C3 C4 1.374(10) .
C4 C5 1.360(9) .
C5 C6 1.416(9) .
C6 C7 1.427(8) .
C9 C10 1.541(7) .
C9 C22 1.542(8) .
C9 C16 1.546(7) .
C10 C15 1.382(7) .
C10 C11 1.393(8) .
C11 C12 1.385(9) .
C12 C13 1.368(10) .
C13 C14 1.369(10) .
C14 C15 1.370(9) .
C16 C17 1.379(8) .
C16 C21 1.383(8) .
C17 C18 1.393(9) .
C18 C19 1.374(10) .
C19 C20 1.353(10) .
C20 C21 1.391(8) .
C22 C23 1.379(7) .
C22 C27 1.398(7) .
C23 C24 1.390(8) .
C24 C25 1.377(9) .
C25 C26 1.364(9) .
C26 C27 1.385(9) .
C1L Cl1 1.690(7) 2
C1L Cl1 1.690(7) .
C2L Cl3 1.690(10) .
C2L Cl4 1.716(10) .
