#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323441.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_4323441
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: SO2 + Mo(N2)2(dppee)2'
_chemical_formula_analytical     'FAB mass spec: M+ - SO'
_chemical_formula_moiety         'C52 H44 Mo O4 P4 S2'
_chemical_formula_structural
;
  'Mo (S O2)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2' 
;
_chemical_formula_sum            'C52 H44 Mo O4 P4 S2'
_chemical_formula_weight         1016.81
_chemical_name_common            trans-Mo(η-SO₂)₂(dppee)₂
_chemical_name_systematic
; 
trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')
                   -bis-(η₂(S,O)-sulfur dioxide)molybdenum (0) 
;
_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                 118.480(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.534(6)
_cell_length_b                   12.4271(13)
_cell_length_c                   19.550(5)
_cell_measurement_reflns_used    '197 (4 times 50, 3 skipped)'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      14.1
_cell_volume                     4598.6(19)
_computing_cell_refinement       'LCR out of ULM package'
_computing_data_collection       'CAD4 - software'
_computing_data_reduction        STP
_computing_molecular_graphics    'ORTEP out of ULM package'
_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       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω/2/6θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5064
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   'empirical \Y-scan correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    'CH-free, Ph-H AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_obs          0.0299
_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)+(0.0355P)²+7.7181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0806
_refine_ls_wR_factor_obs         0.0751
_reflns_number_observed          3418
_reflns_number_total             4036
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_8.cif
_cod_data_source_block           MoSO2_2_dppee2_8
_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 (13 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 (26 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
(39 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^)+(0.0355P)^2^+7.7181P] 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^)+(0.0355P)^2^+7.7181P] 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        4598.4(18)
_cod_database_code               4323441
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
_atom_site_disorder_group
Mo1 Mo 0.5000 0.1594 0.7500 0.02708(10) Uani 1 d S .
S1 S 0.37745(3) 0.21632(6) 0.69913(4) 0.0392(2) Uani 1 d . .
O1 O 0.39794(9) 0.12625(15) 0.65769(10) 0.0373(4) Uani 1 d . .
O2 O 0.34279(11) 0.1753(2) 0.74289(13) 0.0537(5) Uani 1 d . .
P1 P 0.46965(4) 0.02379(6) 0.82796(4) 0.0346(2) Uani 1 d . .
P2 P 0.50503(4) 0.27982(6) 0.85649(4) 0.0346(2) Uani 1 d . .
C1 C 0.4680(2) 0.0963(3) 0.9076(2) 0.0448(7) Uani 1 d . .
H1 H 0.4578(16) 0.0608(25) 0.9420(18) 0.051(9) Uiso 1 d . .
C1A C 0.38632(14) -0.0504(2) 0.7832(2) 0.0428(7) Uani 1 d . .
C1B C 0.3423(2) -0.0585(3) 0.8169(2) 0.0698(10) Uani 1 d . .
H1B H 0.3543(2) -0.0234(3) 0.8635(2) 0.078(3) Uiso 1 calc R .
C1C C 0.2812(2) -0.1180(4) 0.7815(3) 0.0854(14) Uani 1 d . .
H1C H 0.2522(2) -0.1226(4) 0.8045(3) 0.078(3) Uiso 1 calc R .
C1D C 0.2623(2) -0.1705(3) 0.7128(3) 0.0789(13) Uani 1 d . .
H1D H 0.2210(2) -0.2109(3) 0.6894(3) 0.078(3) Uiso 1 calc R .
C1E C 0.3042(2) -0.1629(3) 0.6795(2) 0.0710(11) Uani 1 d . .
H1E H 0.2918(2) -0.1985(3) 0.6329(2) 0.078(3) Uiso 1 calc R .
C1F C 0.3661(2) -0.1024(3) 0.7141(2) 0.0595(9) Uani 1 d . .
H1F H 0.3941(2) -0.0973(3) 0.6899(2) 0.078(3) Uiso 1 calc R .
C1G C 0.53257(15) -0.0823(2) 0.8862(2) 0.0410(6) Uani 1 d . .
C1H C 0.5982(2) -0.0532(3) 0.9471(2) 0.0483(7) Uani 1 d . .
H1H H 0.6102(2) 0.0192(3) 0.9566(2) 0.078(3) Uiso 1 calc R .
C1I C 0.6455(2) -0.1306(3) 0.9933(2) 0.0602(9) Uani 1 d . .
H1I H 0.6890(2) -0.1100(3) 1.0340(2) 0.078(3) Uiso 1 calc R .
C1L C 0.5652(2) -0.2673(3) 0.9202(2) 0.0730(11) Uani 1 d . .
H1L H 0.5543(2) -0.3400(3) 0.9110(2) 0.078(3) Uiso 1 calc R .
C1K C 0.6289(2) -0.2369(3) 0.9797(2) 0.0726(11) Uani 1 d . .
H1K H 0.6610(2) -0.2887(3) 1.0110(2) 0.078(3) Uiso 1 calc R .
C1M C 0.5166(2) -0.1910(3) 0.8734(2) 0.0586(9) Uani 1 d . .
H1M H 0.4732(2) -0.2128(3) 0.8332(2) 0.078(3) Uiso 1 calc R .
C2 C 0.4837(2) 0.1984(3) 0.9197(2) 0.0449(7) Uani 1 d . .
H2 H 0.4883(16) 0.2302(26) 0.9613(19) 0.052(9) Uiso 1 d . .
C2A C 0.45024(14) 0.3997(2) 0.8411(2) 0.0394(6) Uani 1 d . .
C2B C 0.4241(2) 0.4562(3) 0.7736(2) 0.0691(10) Uani 1 d . .
H2B H 0.4318(2) 0.4309(3) 0.7335(2) 0.078(3) Uiso 1 calc R .
C2C C 0.3863(3) 0.5503(3) 0.7629(2) 0.0879(14) Uani 1 d . .
H2C H 0.3702(3) 0.5887(3) 0.7167(2) 0.078(3) Uiso 1 calc R .
C2D C 0.3728(2) 0.5863(3) 0.8198(2) 0.0780(12) Uani 1 d . .
H2D H 0.3461(2) 0.6483(3) 0.8125(2) 0.078(3) Uiso 1 calc R .
C2E C 0.3983(2) 0.5311(3) 0.8874(3) 0.0821(13) Uani 1 d . .
H2E H 0.3898(2) 0.5564(3) 0.9269(3) 0.078(3) Uiso 1 calc R .
C2F C 0.4366(2) 0.4386(3) 0.8986(2) 0.0680(10) Uani 1 d . .
H2F H 0.4535(2) 0.4017(3) 0.9455(2) 0.078(3) Uiso 1 calc R .
C2G C 0.59159(14) 0.3328(2) 0.9285(2) 0.0413(6) Uani 1 d . .
C2H C 0.6128(2) 0.4348(3) 0.9208(2) 0.0535(8) Uani 1 d . .
H2H H 0.5820(2) 0.4786(3) 0.8802(2) 0.078(3) Uiso 1 calc R .
C2I C 0.6792(2) 0.4727(3) 0.9727(2) 0.0649(9) Uani 1 d . .
H2I H 0.6932(2) 0.5410(3) 0.9661(2) 0.078(3) Uiso 1 calc R .
C2K C 0.7239(2) 0.4105(3) 1.0332(2) 0.0722(11) Uani 1 d . .
H2K H 0.7684(2) 0.4363(3) 1.0684(2) 0.078(3) Uiso 1 calc R .
C2L C 0.7034(2) 0.3096(3) 1.0424(2) 0.0692(11) Uani 1 d . .
H2L H 0.7339(2) 0.2674(3) 1.0843(2) 0.078(3) Uiso 1 calc R .
C2M C 0.6383(2) 0.2705(3) 0.9905(2) 0.0549(8) Uani 1 d . .
H2M H 0.6253(2) 0.2014(3) 0.9970(2) 0.078(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 0.0033 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'
O O 0.0106 0.0060 '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'
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
O1 Mo1 O1 157.54(10) . 2_656 y
S1 Mo1 S1 146.29(4) . 2_656 y
O1 Mo1 P1 85.60(5) . . y
O1 Mo1 P1 79.63(5) . 2_656 y
O1 Mo1 P2 115.96(5) . . y
O1 Mo1 P2 78.07(5) . 2_656 n
O1 Mo1 S1 39.35(5) . . y
O1 Mo1 S1 152.40(5) . 2_656 y
S1 Mo1 P1 84.25(3) . . y
S1 Mo1 P1 118.84(3) . 2_656 y
S1 Mo1 P2 77.11(3) . . y
S1 Mo1 P2 83.06(3) . 2_656 y
O1 S1 Mo1 59.06(7) . . y
O2 S1 Mo1 114.40(9) . . y
O2 S1 O1 113.61(12) . . y
P1 Mo1 P1 97.55(3) . 2_656 y
P2 Mo1 P1 79.74(3) . . y
P2 Mo1 P1 163.67(2) . 2_656 y
P2 Mo1 P2 107.27(4) . 2_656 y
C1 P1 C1A 104.18(14) . . y
C1 P1 C1G 97.76(13) . . y
C1A P1 C1G 101.50(13) . . y
Mo1 P1 C1 107.45(11) . . n
Mo1 P1 C1A 121.24(9) . . n
Mo1 P1 C1G 121.18(9) . . n
P1 C1 P2 121.9(2) . . y
P1 C1A C1B 123.0(3) . . n
P1 C1A C1F 119.3(2) . . n
P1 C1G C1H 119.3(2) . . n
P1 C1G C1M 122.7(2) . . n
C1F C1A C1B 117.7(3) . . n
C1A C1B C1C 120.3(4) . . n
C1B C1C C1D 121.0(4) . . n
C1C C1D C1E 119.2(4) . . n
C1D C1E C1F 120.7(4) . . n
C1E C1F C1A 121.1(3) . . n
C1M C1G C1H 118.1(3) . . n
C1G C1H C1I 120.7(3) . . n
C1H C1I C1K 120.4(3) . . n
C1I C1K C1L 120.0(3) . . n
C1K C1L C1M 120.7(4) . . n
C1L C1M C1G 120.2(3) . . n
C2 P2 C2A 102.25(13) . . y
C2 P2 C2G 99.84(14) . . y
C2A P2 C2G 99.95(13) . . y
Mo1 P2 C2 107.77(11) . . n
Mo1 P2 C2A 125.13(9) . . n
Mo1 P2 C2G 118.20(9) . . n
P2 C2 C1 123.1(2) . . y
P2 C2A C2B 121.0(2) . . n
P2 C2A C2F 121.5(2) . . n
P2 C2G C2H 120.8(2) . . n
P2 C2G C2M 121.2(2) . . n
C2F C2A C2B 117.4(3) . . n
C2A C2B C2C 121.7(3) . . n
C2B C2C C2D 119.8(4) . . n
C2C C2D C2E 119.3(3) . . n
C2D C2E C2F 121.1(4) . . n
C2E C2F C2A 120.7(3) . . n
C2M C2G C2H 118.0(3) . . n
C2G C2H C2I 120.9(3) . . n
C2H C2I C2K 120.1(4) . . n
C2I C2K C2L 119.8(3) . . n
C2K C2L C2M 120.6(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 2.4394(9) . y
Mo1 O1 2.115(2) . y
Mo1 P1 2.5573(7) . y
Mo1 P2 2.5239(8) . y
S1 O2 1.469(2) . y
S1 O1 1.564(2) . y
P1 C1 1.814(3) . y
P1 C1A 1.827(3) . y
P1 C1G 1.844(3) . y
P2 C2 1.817(3) . y
P2 C2A 1.834(3) . y
P2 C2G 1.840(3) . y
C1 C2 1.306(4) . y
C1A C1F 1.366(4) . n
C1A C1B 1.393(4) . n
C1B C1C 1.374(6) . n
C1C C1D 1.370(6) . n
C1D C1E 1.343(6) . n
C1E C1F 1.392(5) . n
C1G C1M 1.387(4) . n
C1G C1H 1.393(4) . n
C1H C1I 1.379(4) . n
C1I C1K 1.361(5) . n
C1L C1K 1.361(6) . n
C1L C1M 1.385(5) . n
C2A C2B 1.359(4) . n
C2A C2F 1.378(4) . n
C2B C2C 1.383(5) . n
C2C C2D 1.353(6) . n
C2D C2E 1.350(6) . n
C2E C2F 1.370(5) . n
C2G C2H 1.380(4) . n
C2G C2M 1.385(4) . n
C2H C2I 1.383(4) . n
C2I C2K 1.355(5) . n
C2K C2L 1.370(6) . n
C2L C2M 1.369(5) . n
