#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323440.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_4323440
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        'data were measured by Sanjay K. Mandel'
_chemical_formula_moiety         'C52 H44 Mo O P4 S'
_chemical_formula_sum            'C52 H44 Mo O P4 S'
_chemical_formula_weight         936.75
_chemical_name_common            trans-Mo(O)(S)(dppee)₂
_chemical_name_systematic
; 
 trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')-oxo-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                75.300(10)
_cell_angle_beta                 85.930(10)
_cell_angle_gamma                63.210(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0400(10)
_cell_length_b                   10.5630(10)
_cell_length_c                   12.162(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.5
_cell_measurement_theta_min      29
_cell_volume                     1112.3(3)
_computing_cell_refinement       'TEXSAN-TEXRAY, MSC 1985'
_computing_data_collection       'TEXSAN-TEXRAY, MSC 1985'
_computing_data_reduction        'TEXSAN-TEXRAY, MSC 1985'
_computing_molecular_graphics    'ORTEP, ULM 1992'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'MSC-Rigaku AFC5R'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3313
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        unknown
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  'based on count'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   'empirical \Y-scan corrections'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    'AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0299
_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)+(0.0000P)²+0.7276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0981
_refine_ls_wR_factor_obs         0.0980
_reflns_number_observed          3293
_reflns_number_total             3313
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_7.cif
_cod_data_source_block           MoOSdppee2_7
_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 (11 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 (19 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 done' 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^)+(0.0000P)^2^+0.7276P] 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^)+(0.0000P)^2^+0.7276P] 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        1112.3(2)
_cod_database_code               4323440
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 0.5000 0.5000 0.5000 0.02735(13) Uani 1 d S .
S1 S 0.5412(3) 0.2684(3) 0.5797(2) 0.0393(6) Uani 0.50 d P .
O1 O 0.4756(7) 0.6881(7) 0.4387(6) 0.033(2) Uiso 0.50 d P .
P1 P 0.33104(8) 0.51325(8) 0.35088(6) 0.0319(2) Uani 1 d . .
P2 P 0.25814(8) 0.58648(8) 0.59861(6) 0.0319(2) Uani 1 d . .
C1 C 0.1459(3) 0.5642(3) 0.4074(3) 0.0363(6) Uani 1 d . .
H1 H 0.0711(36) 0.5634(34) 0.3570(27) 0.035(8) Uiso 1 d . .
C1A C 0.3666(3) 0.3426(3) 0.3163(3) 0.0376(7) Uani 1 d . .
C1B C 0.4345(4) 0.3099(4) 0.2171(3) 0.0559(9) Uani 1 d . .
H1B H 0.4566(4) 0.3779(4) 0.1644(3) 0.077(3) Uiso 1 calc R .
C1C C 0.4696(5) 0.1744(5) 0.1969(4) 0.0703(12) Uani 1 d . .
H1C H 0.5145(5) 0.1524(5) 0.1302(4) 0.077(3) Uiso 1 calc R .
C1D C 0.4385(5) 0.0741(4) 0.2741(4) 0.0667(11) Uani 1 d . .
H1D H 0.4625(5) -0.0159(4) 0.2598(4) 0.077(3) Uiso 1 calc R .
C1E C 0.3722(4) 0.1049(4) 0.3726(4) 0.0593(9) Uani 1 d . .
H1E H 0.3515(4) 0.0359(4) 0.4252(4) 0.077(3) Uiso 1 calc R .
C1F C 0.3361(4) 0.2394(4) 0.3933(3) 0.0469(8) Uani 1 d . .
H1F H 0.2906(4) 0.2604(4) 0.4601(3) 0.077(3) Uiso 1 calc R .
C1G C 0.2826(3) 0.6448(3) 0.2112(2) 0.0399(7) Uani 1 d . .
C1H C 0.3524(4) 0.7352(4) 0.1783(3) 0.0590(10) Uani 1 d . .
H1H H 0.4257(4) 0.7276(4) 0.2257(3) 0.077(3) Uiso 1 calc R .
C1I C 0.3111(5) 0.8368(5) 0.0736(4) 0.0800(14) Uani 1 d . .
H1I H 0.3577(5) 0.8974(5) 0.0512(4) 0.077(3) Uiso 1 calc R .
C1K C 0.2047(5) 0.8498(5) 0.0037(4) 0.0828(15) Uani 1 d . .
H1K H 0.1784(5) 0.9191(5) -0.0659(4) 0.077(3) Uiso 1 calc R .
C1L C 0.1357(5) 0.7614(5) 0.0348(3) 0.0719(12) Uani 1 d . .
H1L H 0.0629(5) 0.7704(5) -0.0140(3) 0.077(3) Uiso 1 calc R .
C1M C 0.1732(4) 0.6583(4) 0.1385(3) 0.0529(8) Uani 1 d . .
H1M H 0.1257(4) 0.5985(4) 0.1594(3) 0.077(3) Uiso 1 calc R .
C2 C 0.1164(3) 0.5943(3) 0.5077(3) 0.0360(6) Uani 1 d . .
H2 H 0.0226(44) 0.6230(40) 0.5404(32) 0.052(10) Uiso 1 d . .
C2A C 0.1619(3) 0.7652(3) 0.6318(3) 0.0384(7) Uani 1 d . .
C2B C 0.2315(4) 0.8539(4) 0.6198(3) 0.0527(8) Uani 1 d . .
H2B H 0.3269(4) 0.8246(4) 0.5921(3) 0.077(3) Uiso 1 calc R .
C2C C 0.1596(5) 0.9871(4) 0.6489(4) 0.0685(11) Uani 1 d . .
H2C H 0.2074(5) 1.0463(4) 0.6413(4) 0.077(3) Uiso 1 calc R .
C2D C 0.0199(5) 1.0317(4) 0.6885(3) 0.0649(11) Uani 1 d . .
H2D H -0.0272(5) 1.1212(4) 0.7078(3) 0.077(3) Uiso 1 calc R .
C2E C -0.0518(5) 0.9461(5) 0.7002(4) 0.0715(12) Uani 1 d . .
H2E H -0.1478(5) 0.9776(5) 0.7266(4) 0.077(3) Uiso 1 calc R .
C2F C 0.0188(4) 0.8120(4) 0.6726(4) 0.0599(10) Uani 1 d . .
H2F H -0.0296(4) 0.7532(4) 0.6815(4) 0.077(3) Uiso 1 calc R .
C2G C 0.2439(3) 0.4643(3) 0.7312(3) 0.0378(7) Uani 1 d . .
C2H C 0.2463(5) 0.4938(4) 0.8353(3) 0.0604(10) Uani 1 d . .
H2H H 0.2509(5) 0.5789(4) 0.8384(3) 0.077(3) Uiso 1 calc R .
C2I C 0.2419(6) 0.3966(5) 0.9357(3) 0.0781(13) Uani 1 d . .
H2I H 0.2435(6) 0.4167(5) 1.0057(3) 0.077(3) Uiso 1 calc R .
C2K C 0.2353(5) 0.2703(5) 0.9310(4) 0.0724(12) Uani 1 d . .
H2K H 0.2317(5) 0.2056(5) 0.9978(4) 0.077(3) Uiso 1 calc R .
C2L C 0.2339(5) 0.2403(4) 0.8289(3) 0.0629(10) Uani 1 d . .
H2L H 0.2302(5) 0.1548(4) 0.8262(3) 0.077(3) Uiso 1 calc R .
C2M C 0.2382(4) 0.3364(4) 0.7291(3) 0.0483(8) Uani 1 d . .
H2M H 0.2372(4) 0.3148(4) 0.6597(3) 0.077(3) 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 0.0181 0.0091 '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 -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O1 Mo1 S1 176.8(2) . . y
O1 Mo1 P1 93.8(2) . . y
O1 Mo1 P1 86.2(2) . 2_666 y
O1 Mo1 P2 92.7(2) . . y
O1 Mo1 P2 87.3(2) . 2_666 y
S1 Mo1 P1 89.15(6) . . y
S1 Mo1 P1 90.85(6) . 2_666 y
S1 Mo1 P2 88.79(6) . . y
S1 Mo1 P2 91.21(6) . 2_666 y
P1 Mo1 P2 80.76(3) . . y
P1 Mo1 P2 99.24(2) . 2_666 y
C1 P1 C1A 100.82(14) . . y
C1 P1 C1G 100.10(14) . . y
C1A P1 C1G 102.84(14) . . y
Mo1 P1 C1 107.68(10) . . n
Mo1 P1 C1A 117.66(9) . . n
Mo1 P1 C1G 124.07(11) . . n
P1 C1 C2 121.9(2) . . y
P1 C1A C1B 120.9(3) . . n
P1 C1A C1F 119.9(2) . . n
P1 C1G C1H 119.9(3) . . n
P1 C1G C1M 120.7(3) . . n
C1F C1A C1B 119.0(3) . . n
C1A C1B C1C 119.6(4) . . n
C1B C1C C1D 120.5(4) . . n
C1C C1D C1E 120.5(4) . . n
C1D C1E C1F 119.6(4) . . n
C1E C1F C1A 120.9(3) . . n
C1M C1G C1H 119.3(3) . . n
C1G C1H C1I 119.0(4) . . n
C1H C1I C1K 121.4(4) . . n
C1I C1K C1L 120.2(4) . . n
C1K C1L C1M 120.5(4) . . n
C1L C1M C1G 119.6(4) . . n
C2 P2 C2A 101.22(14) . . y
C2 P2 C2G 100.67(14) . . y
C2A P2 C2G 101.71(14) . . y
Mo1 P2 C2 107.35(10) . . n
Mo1 P2 C2A 124.55(10) . . n
Mo1 P2 C2G 117.77(10) . . n
P2 C2 C1 122.2(2) . . y
P2 C2A C2B 120.5(2) . . n
P2 C2A C2F 120.6(3) . . n
P2 C2G C2H 120.9(3) . . n
P2 C2G C2M 120.2(2) . . n
C2F C2A C2B 118.9(3) . . n
C2A C2B C2C 120.0(4) . . n
C2B C2C C2D 120.6(4) . . n
C2C C2D C2E 120.4(4) . . n
C2D C2E C2F 119.9(4) . . n
C2E C2F C2A 120.2(4) . . n
C2M C2G C2H 118.8(3) . . n
C2G C2H C2I 120.2(4) . . n
C2H C2I C2K 119.8(4) . . n
C2I C2K C2L 120.2(4) . . n
C2K C2L C2M 120.3(4) . . n
C2L C2M C2G 120.7(4) . . 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 O1 1.843(6) . y
Mo1 S1 2.244(3) . y
Mo1 P1 2.5061(8) . y
Mo1 P2 2.5125(8) . y
P1 C1 1.823(3) . y
P1 C1A 1.827(3) . y
P1 C1G 1.834(3) . y
P2 C2 1.824(3) . y
P2 C2A 1.830(3) . y
P2 C2G 1.835(3) . y
C1 C2 1.318(4) . y
C1A C1F 1.379(5) . n
C1A C1B 1.386(5) . n
C1B C1C 1.395(6) . n
C1C C1D 1.361(6) . n
C1D C1E 1.368(6) . n
C1E C1F 1.385(5) . n
C1G C1H 1.390(5) . n
C1G C1M 1.393(5) . n
C1H C1I 1.387(6) . n
C1I C1K 1.350(7) . n
C1K C1L 1.364(7) . n
C1L C1M 1.385(5) . n
C2A C2B 1.376(5) . n
C2A C2F 1.392(5) . n
C2B C2C 1.389(5) . n
C2C C2D 1.357(6) . n
C2D C2E 1.365(6) . n
C2E C2F 1.386(6) . n
C2G C2H 1.383(5) . n
C2G C2M 1.385(5) . n
C2H C2I 1.395(6) . n
C2I C2K 1.381(7) . n
C2K C2L 1.359(6) . n
C2L C2M 1.383(5) . n
