#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323435.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_4323435
loop_
_publ_author_name
'F. Albert Cotton'
'Günter Schmid'
_publ_section_title
;
 Mononuclear Molybdenum(IV) Complexes with Two Multiply Bonded Chalcogen
 Ligands in Trans Configuration and Chelating Biphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2267
_journal_page_last               2278
_journal_paper_doi               10.1021/ic961071v
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
 Reaction: Mo(N2)2(dppee)2, 2 Bz2S3 in toluene
;
_chemical_formula_analytical     'FAB mass spectrum: 954u + 3u (NBA)'
_chemical_formula_moiety         'C52 H44 Mo P4 S2'
_chemical_formula_structural
;
 Mo (S)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2
;
_chemical_formula_sum            'C52 H44 Mo P4 S2'
_chemical_formula_weight         952.81
_chemical_melting_point          530(3)
_chemical_name_common            trans-Mo(S)₂(dppee)₂
_chemical_name_systematic
;
trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')-bis-sulfido-
molybdenum(IV)
;
_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                100.95(3)
_cell_angle_beta                 95.04(4)
_cell_angle_gamma                117.81(2)
_cell_formula_units_Z            1
_cell_length_a                   10.102(4)
_cell_length_b                   10.722(4)
_cell_length_c                   12.195(3)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      13.1
_cell_volume                     1123.1(8)
_computing_cell_refinement       'LCR from System ULM'
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        STP
_computing_molecular_graphics    'ORTEP from System ULM'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Mo on 0.0 0.0 0.0'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5205
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_count 'based on time, every 60 minutes'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  'Mode FLAT'
_exptl_absorpt_correction_T_min  'Mode FLAT'
_exptl_absorpt_correction_type   'Mode FLAT, CAD4-Diffractometer'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not determined'
_exptl_crystal_description       'rhombic plate'
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_hydrogen_treatment    'all hydrogens refined, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_obs          0.0366
_refine_ls_shift/esd_max         -0.038
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0691P)²+0.2770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1029
_refine_ls_wR_factor_obs         0.0969
_reflns_number_observed          3651
_reflns_number_total             4166
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_2.cif
_cod_data_source_block           MoS2dppee_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (10 times).

'_geom_bond_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (24
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (14 times).

'_geom_angle_publ_flag'
value 'N' changed to 'n' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(38 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not determined' 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 'calc
w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.2770P] 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^)+(0.0691P)^2^+0.2770P] 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        1123.1(7)
_cod_database_code               4323435
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
Mo1 Mo 0.0000 0.0000 0.0000 0.03159(12) Uani 1 d S .
S1 S 0.18308(8) 0.23011(7) 0.07925(6) 0.0427(2) Uani 1 d . .
P2 P 0.15469(7) -0.01437(7) -0.14618(5) 0.0358(2) Uani 1 d . .
P1 P 0.15614(7) -0.08535(7) 0.10174(6) 0.0369(2) Uani 1 d . .
C1 C 0.2874(3) -0.0967(3) 0.0117(2) 0.0421(6) Uani 1 d . .
H1 H 0.3500(35) -0.1287(32) 0.0405(26) 0.046(8) Uiso 1 d . .
C1A C 0.0812(3) -0.2625(3) 0.1361(2) 0.0438(6) Uani 1 d . .
C1B C -0.0734(4) -0.3512(3) 0.1262(3) 0.0543(7) Uani 1 d . .
H1B H -0.1375(44) -0.3170(43) 0.1011(34) 0.078(5) Uiso 1 d . .
C1C C -0.1266(5) -0.4835(4) 0.1541(3) 0.0694(10) Uani 1 d . .
H1C H -0.2146(46) -0.5304(46) 0.1562(36) 0.078(5) Uiso 1 d . .
C1D C -0.0290(5) -0.5271(4) 0.1925(3) 0.0688(10) Uani 1 d . .
H1D H -0.0614(45) -0.6173(45) 0.2095(33) 0.078(5) Uiso 1 d . .
C1E C 0.1255(5) -0.4392(4) 0.2040(4) 0.0722(10) Uani 1 d . .
H1E H 0.1883(44) -0.4719(44) 0.2295(35) 0.078(5) Uiso 1 d . .
C1F C 0.1801(4) -0.3074(4) 0.1762(3) 0.0617(8) Uani 1 d . .
H1F H 0.2932(48) -0.2360(45) 0.1878(34) 0.078(5) Uiso 1 d . .
C1G C 0.2916(3) 0.0370(3) 0.2350(2) 0.0449(6) Uani 1 d . .
C1H C 0.2601(4) 0.0115(4) 0.3392(3) 0.0602(8) Uani 1 d . .
H1H H 0.1729(44) -0.0709(43) 0.3416(32) 0.072(5) Uiso 1 d . .
C1I C 0.3587(5) 0.1084(5) 0.4396(3) 0.0791(12) Uani 1 d . .
H1I H 0.3367(42) 0.0858(41) 0.5024(35) 0.072(5) Uiso 1 d . .
C1K C 0.4889(5) 0.2320(5) 0.4372(3) 0.0770(11) Uani 1 d . .
H1K H 0.5537(43) 0.2917(42) 0.5144(33) 0.072(5) Uiso 1 d . .
C1L C 0.5222(4) 0.2594(4) 0.3357(3) 0.0682(9) Uani 1 d . .
H1L H 0.6107(45) 0.3471(42) 0.3290(33) 0.072(5) Uiso 1 d . .
C1M C 0.4236(3) 0.1622(3) 0.2339(3) 0.0519(7) Uani 1 d . .
H1M H 0.4472(42) 0.1817(41) 0.1702(33) 0.072(5) Uiso 1 d . .
C2 C 0.2867(3) -0.0686(3) -0.0880(2) 0.0414(6) Uani 1 d . .
H2 H 0.3411(38) -0.0784(37) -0.1303(30) 0.056(10) Uiso 1 d . .
C2A C 0.2873(3) 0.1543(3) -0.1790(2) 0.0400(6) Uani 1 d . .
C2B C 0.2507(4) 0.1905(4) -0.2752(3) 0.0540(7) Uani 1 d . .
H2B H 0.1707(40) 0.1314(38) -0.3265(30) 0.059(4) Uiso 1 d . .
C2C C 0.3466(4) 0.3234(4) -0.2950(3) 0.0658(9) Uani 1 d . .
H2C H 0.3200(37) 0.3444(36) -0.3673(29) 0.059(4) Uiso 1 d . .
C2D C 0.4803(4) 0.4216(4) -0.2181(3) 0.0611(9) Uani 1 d . .
H2D H 0.5236(41) 0.4991(41) -0.2277(31) 0.059(4) Uiso 1 d . .
C2E C 0.5177(4) 0.3886(3) -0.1219(3) 0.0553(8) Uani 1 d . .
H2E H 0.6087(41) 0.4538(38) -0.0648(30) 0.059(4) Uiso 1 d . .
C2F C 0.4226(3) 0.2556(3) -0.1012(3) 0.0461(6) Uani 1 d . .
H2F H 0.4481(39) 0.2336(38) -0.0385(31) 0.059(4) Uiso 1 d . .
C2G C 0.0788(3) -0.1417(3) -0.2885(2) 0.0418(6) Uani 1 d . .
C2H C -0.0777(4) -0.2276(4) -0.3307(3) 0.0516(7) Uani 1 d . .
H2H H -0.1411(42) -0.2199(40) -0.2883(32) 0.067(5) Uiso 1 d . .
C2I C -0.1329(4) -0.3264(4) -0.4362(3) 0.0683(10) Uani 1 d . .
H2I H -0.2354(43) -0.3843(39) -0.4637(32) 0.067(5) Uiso 1 d . .
C2K C -0.0365(5) -0.3411(5) -0.5019(3) 0.0756(11) Uani 1 d . .
H2K H -0.0652(41) -0.3993(41) -0.5706(33) 0.067(5) Uiso 1 d . .
C2L C 0.1188(5) -0.2547(5) -0.4631(3) 0.0710(10) Uani 1 d . .
H2L H 0.1988(41) -0.2640(39) -0.5051(32) 0.067(5) Uiso 1 d . .
C2M C 0.1764(4) -0.1568(4) -0.3568(3) 0.0562(7) Uani 1 d . .
H2M H 0.2888(42) -0.0929(39) -0.3245(32) 0.067(5) 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'
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'
P P 0.1023 0.0942 '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
S1 Mo1 P1 89.14(5) . . y
S1 Mo1 P1 90.86(5) . 2 y
S1 Mo1 P2 88.54(4) . . y
S1 Mo1 P2 91.46(4) . 2 y
P1 Mo1 P2 81.04(3) . . y
P1 Mo1 P2 98.96(3) . 2 y
C1 P1 C1A 100.46(13) . . y
C1 P1 C1G 100.48(13) . . y
C1A P1 C1G 100.81(14) . . y
Mo1 P1 C1 107.05(10) . . n
Mo1 P1 C1G 118.46(10) . . n
Mo1 P1 C1A 125.60(10) . . n
P1 C1 C2 122.3(2) . . y
P1 C1A C1B 120.9(2) . . n
P1 C1A C1F 120.4(2) . . n
P1 C1G C1H 120.9(2) . . n
P1 C1G C1M 120.6(2) . . n
C1F C1A C1B 118.6(3) . . n
C1A C1B C1C 119.7(3) . . n
C1B C1C C1D 121.3(4) . . n
C1C C1D C1E 119.7(3) . . n
C1D C1E C1F 119.7(4) . . n
C1E C1F C1A 121.0(3) . . n
C1M C1G C1H 118.5(3) . . n
C1G C1H C1I 120.6(4) . . n
C1H C1I C1K 120.3(4) . . n
C1I C1K C1L 120.1(3) . . n
C1K C1L C1M 120.0(4) . . n
C1L C1M C1G 120.5(3) . . n
C2 P2 C2A 100.99(13) . . y
C2 P2 C2G 99.90(13) . . y
C2A P2 C2G 100.91(13) . . y
Mo1 P2 C2 107.37(10) . . n
Mo1 P2 C2A 118.38(9) . . n
Mo1 P2 C2G 125.39(9) . . n
P2 C2 C1 122.2(2) . . y
P2 C2A C2B 121.2(2) . . n
P2 C2A C2F 120.1(2) . . n
P2 C2G C2H 121.0(2) . . n
P2 C2G C2M 120.9(2) . . n
C2F C2A C2B 118.4(3) . . n
C2A C2B C2C 120.9(3) . . n
C2B C2C C2D 120.0(3) . . n
C2C C2D C2E 120.0(3) . . n
C2D C2E C2F 120.4(3) . . n
C2E C2F C2A 120.2(3) . . n
C2M C2G C2H 118.1(3) . . n
C2G C2H C2I 120.3(3) . . n
C2H C2I C2K 121.1(3) . . n
C2I C2K C2L 119.6(3) . . n
C2K C2L C2M 120.2(3) . . n
C2L C2M C2G 120.7(3) . . n
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
Mo1 S1 2.2280(14) . y
Mo1 P1 2.5098(10) . y
Mo1 P2 2.5007(11) . y
P1 C1 1.826(3) . y
P1 C1A 1.836(3) . y
P1 C1G 1.833(3) . y
P2 C2 1.825(3) . y
P2 C2A 1.826(3) . y
P2 C2G 1.831(3) . y
C1 C2 1.308(4) . y
C1A C1B 1.377(4) . n
C1A C1F 1.387(4) . n
C1B C1C 1.386(5) . n
C1C C1D 1.357(6) . n
C1D C1E 1.372(6) . n
C1E C1F 1.379(5) . n
C1G C1H 1.383(4) . n
C1G C1M 1.385(4) . n
C1H C1I 1.381(5) . n
C1I C1K 1.371(6) . n
C1K C1L 1.361(6) . n
C1L C1M 1.394(5) . n
C2A C2B 1.376(4) . n
C2A C2F 1.394(4) . n
C2B C2C 1.383(5) . n
C2C C2D 1.374(5) . n
C2D C2E 1.360(5) . n
C2E C2F 1.386(4) . n
C2G C2H 1.390(4) . n
C2G C2M 1.390(4) . n
C2H C2I 1.376(5) . n
C2I C2K 1.359(6) . n
C2K C2L 1.375(6) . n
C2L C2M 1.379(5) . n
