#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:43:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179986 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028002.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_7028002
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            'C22 H21 Mo N3 O2 S3'
_chemical_formula_weight         551.54
_chemical_name_common
;
cis-Dioxo-(S-benzyl-3-(2-mercapto-phenyl)-methylendithiocarbazate)
(4-methyl-pyridine)molybdenum(VI) 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.89(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.779(2)
_cell_length_b                   12.678(2)
_cell_length_c                   17.567(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2357.4(7)
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5446
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.846
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       needles
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.355
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.887
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_obs          0.0375
_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)+(0.0488P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0902
_refine_ls_wR_factor_obs         0.0839
_reflns_number_observed          3544
_reflns_number_total             5160
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            D802334sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0488P)^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^)+(0.0488P)^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_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028002
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.02184(3) 0.14935(2) 0.71801(2) 0.03958(9) Uani 1 d .
S1 S -0.13831(8) 0.02061(8) 0.72676(5) 0.0475(2) Uani 1 d .
S2 S 0.24639(10) 0.19700(8) 0.73525(6) 0.0569(3) Uani 1 d .
S3 S 0.46903(10) 0.06285(11) 0.77254(8) 0.0819(4) Uani 1 d .
O1 O -0.0154(3) 0.2523(2) 0.77149(13) 0.0595(7) Uani 1 d .
O2 O -0.0314(2) 0.1827(2) 0.62409(13) 0.0530(6) Uani 1 d .
N1 N 0.1168(2) 0.0024(2) 0.67947(14) 0.0355(6) Uani 1 d .
N2 N 0.2466(3) -0.0151(2) 0.7091(2) 0.0453(7) Uani 1 d .
N3 N 0.1026(2) 0.0690(2) 0.84288(14) 0.0371(6) Uani 1 d .
C1 C -0.1654(3) -0.0324(2) 0.6327(2) 0.0408(7) Uani 1 d .
C2 C -0.2918(4) -0.0450(3) 0.5972(2) 0.0573(10) Uani 1 d .
H2 H -0.3552(4) -0.0262(3) 0.6239(2) 0.069 Uiso 1 calc R
C3 C -0.3235(4) -0.0851(3) 0.5229(2) 0.0644(11) Uani 1 d .
H3 H -0.4081(4) -0.0936(3) 0.5001(2) 0.077 Uiso 1 calc R
C4 C -0.2314(4) -0.1123(3) 0.4829(2) 0.0584(10) Uani 1 d .
H4 H -0.2531(4) -0.1363(3) 0.4321(2) 0.070 Uiso 1 calc R
C5 C -0.1065(4) -0.1043(3) 0.5179(2) 0.0453(8) Uani 1 d .
H5 H -0.0447(4) -0.1255(3) 0.4908(2) 0.054 Uiso 1 calc R
C6 C -0.0695(3) -0.0649(2) 0.5937(2) 0.0376(7) Uani 1 d .
C7 C 0.0672(3) -0.0663(2) 0.6282(2) 0.0365(7) Uani 1 d .
C8 C 0.1472(4) -0.1502(3) 0.6005(2) 0.0574(9) Uani 1 d .
H8A H 0.2332(4) -0.1427(3) 0.6270(2) 0.069 Uiso 1 calc R
H8B H 0.1432(4) -0.1427(3) 0.5457(2) 0.069 Uiso 1 calc R
H8C H 0.1163(4) -0.2186(3) 0.6111(2) 0.069 Uiso 1 calc R
C9 C 0.3056(3) 0.0698(3) 0.7349(2) 0.0502(9) Uani 1 d .
C10 C 0.4993(4) -0.0783(4) 0.7762(3) 0.086(2) Uani 1 d .
H10A H 0.4535(4) -0.1100(4) 0.7289(3) 0.103 Uiso 1 calc R
H10B H 0.5886(4) -0.0898(4) 0.7776(3) 0.103 Uiso 1 calc R
C11 C 0.4628(4) -0.1337(4) 0.8438(3) 0.0680(12) Uani 1 d .
C12 C 0.3786(5) -0.2158(4) 0.8338(4) 0.094(2) Uani 1 d .
H12 H 0.3406(5) -0.2362(4) 0.7841(4) 0.112 Uiso 1 calc R
C13 C 0.3500(5) -0.2679(4) 0.8964(5) 0.110(2) Uani 1 d .
H13 H 0.2920(5) -0.3230(4) 0.8883(5) 0.132 Uiso 1 calc R
C14 C 0.4040(4) -0.2413(4) 0.9703(4) 0.092(2) Uani 1 d .
H14 H 0.3846(4) -0.2785(4) 1.0122(4) 0.110 Uiso 1 calc R
C15 C 0.4866(5) -0.1596(4) 0.9817(3) 0.0896(15) Uani 1 d .
H15 H 0.5250(5) -0.1403(4) 1.0317(3) 0.108 Uiso 1 calc R
C16 C 0.5136(4) -0.1052(4) 0.9187(3) 0.0869(15) Uani 1 d .
H16 H 0.5678(4) -0.0475(4) 0.9272(3) 0.104 Uiso 1 calc R
C17 C 0.1368(3) 0.1339(2) 0.9037(2) 0.0429(8) Uani 1 d .
H17 H 0.1402(3) 0.2060(2) 0.8943(2) 0.051 Uiso 1 calc R
C18 C 0.1667(3) 0.0995(3) 0.9787(2) 0.0459(8) Uani 1 d .
H18 H 0.1894(3) 0.1479(3) 1.0187(2) 0.055 Uiso 1 calc R
C19 C 0.1634(3) -0.0079(3) 0.9956(2) 0.0388(7) Uani 1 d .
C20 C 0.1320(3) -0.0743(3) 0.9330(2) 0.0436(8) Uani 1 d .
H20 H 0.1306(3) -0.1468(3) 0.9408(2) 0.052 Uiso 1 calc R
C21 C 0.1027(3) -0.0344(2) 0.8592(2) 0.0410(7) Uani 1 d .
H21 H 0.0819(3) -0.0816(2) 0.8182(2) 0.049 Uiso 1 calc R
C22 C 0.1918(3) -0.0480(3) 1.0771(2) 0.0526(9) Uani 1 d .
H22A H 0.2115(3) 0.0102(3) 1.1122(2) 0.063 Uiso 1 calc R
H22B H 0.2626(3) -0.0952(3) 1.0832(2) 0.063 Uiso 1 calc R
H22C H 0.1195(3) -0.0849(3) 1.0882(2) 0.063 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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 Mo1 O1 105.97(11)
O2 Mo1 N1 90.16(10)
O1 Mo1 N1 162.53(10)
O2 Mo1 S1 96.69(9)
O1 Mo1 S1 103.82(10)
N1 Mo1 S1 80.37(7)
O2 Mo1 N3 169.29(10)
O1 Mo1 N3 84.51(10)
N1 Mo1 N3 79.73(8)
S1 Mo1 N3 78.26(7)
O2 Mo1 S2 101.72(9)
O1 Mo1 S2 94.18(10)
N1 Mo1 S2 75.62(7)
S1 Mo1 S2 149.58(3)
N3 Mo1 S2 79.32(7)
C1 S1 Mo1 101.18(11)
C9 S2 Mo1 97.21(12)
C9 S3 C10 102.8(2)
C7 N1 N2 113.6(3)
C7 N1 Mo1 127.2(2)
N2 N1 Mo1 119.0(2)
C9 N2 N1 112.8(3)
C21 N3 C17 116.1(3)
C21 N3 Mo1 126.0(2)
C17 N3 Mo1 117.4(2)
C2 C1 C6 119.6(3)
C2 C1 S1 116.1(3)
C6 C1 S1 124.3(2)
C3 C2 C1 120.7(4)
C4 C3 C2 120.3(4)
C3 C4 C5 119.8(3)
C4 C5 C6 121.9(3)
C1 C6 C5 117.5(3)
C1 C6 C7 124.7(3)
C5 C6 C7 117.7(3)
N1 C7 C6 121.6(3)
N1 C7 C8 120.9(3)
C6 C7 C8 117.5(3)
N2 C9 S2 128.3(3)
N2 C9 S3 118.9(3)
S2 C9 S3 112.8(2)
C11 C10 S3 114.7(3)
C12 C11 C16 117.1(5)
C12 C11 C10 121.5(5)
C16 C11 C10 121.4(4)
C13 C12 C11 120.6(5)
C14 C13 C12 121.8(5)
C15 C14 C13 118.8(6)
C14 C15 C16 119.6(5)
C11 C16 C15 122.0(5)
N3 C17 C18 123.4(3)
C17 C18 C19 120.4(3)
C20 C19 C18 116.1(3)
C20 C19 C22 122.1(3)
C18 C19 C22 121.8(3)
C21 C20 C19 120.5(3)
N3 C21 C20 123.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 O2 1.695(2)
Mo1 O1 1.700(2)
Mo1 N1 2.288(2)
Mo1 S1 2.4017(10)
Mo1 N3 2.426(2)
Mo1 S2 2.4572(11)
S1 C1 1.756(3)
S2 C9 1.735(4)
S3 C9 1.763(4)
S3 C10 1.818(6)
N1 C7 1.294(4)
N1 N2 1.415(4)
N2 C9 1.288(4)
N3 C21 1.342(4)
N3 C17 1.343(4)
C1 C2 1.396(5)
C1 C6 1.406(5)
C2 C3 1.382(5)
C3 C4 1.365(6)
C4 C5 1.374(5)
C5 C6 1.407(4)
C6 C7 1.483(4)
C7 C8 1.507(4)
C10 C11 1.494(7)
C11 C12 1.370(6)
C11 C16 1.375(6)
C12 C13 1.367(8)
C13 C14 1.360(8)
C14 C15 1.356(7)
C15 C16 1.381(7)
C17 C18 1.368(4)
C18 C19 1.395(5)
C19 C20 1.376(4)
C19 C22 1.496(4)
C20 C21 1.372(4)
