Isomerism and Ligand Rearrangement within thecyclo-P2S3Middle Deck in Dimolybdenum Triple-Decker Complexes
Gröger, Christian; Kubicki, Marek M.; Meier, Walter; Pronold, Michael; Wachter, Joachim; Zabel, Manfred; Organometallics 28 (2009) 5633–; doi:10.1021/om900600t

data_4070076
_publ_section_title
;
 Isomerism and Ligand Rearrangement within thecyclo-P2S3Middle Deck in
 Dimolybdenum Triple-Decker Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5633
_journal_paper_doi               10.1021/om900600t
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C32 H34 Mo2 O10 P2 S3 W2, 2(C6 H6)'
_chemical_formula_sum            'C44 H46 Mo2 O10 P2 S3 W2'
_chemical_formula_weight         1452.52
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                91.496(4)
_cell_angle_beta                 96.043(5)
_cell_angle_gamma                91.882(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2880(8)
_cell_length_b                   12.4550(7)
_cell_length_c                   16.1132(7)
_cell_measurement_reflns_used    6791
_cell_measurement_temperature    123
_cell_measurement_theta_max      51.5699
_cell_measurement_theta_min      2.7521
_cell_volume                     2450.0(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -27.00   25.00   1.3000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.4688   45.0000  240.0000    0.0000    0.0000 40

  2 omega   24.00   74.70   1.3000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.4688   45.0000  240.0000    0.0000    0.0000 39

  3 omega  -26.00   26.00   1.3000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.4688   45.0000    0.0000    0.0000    0.0000 40

  4 phi    -61.00    2.70   1.3000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    0.4688    0.0000     -        0.0000    0.0000 49

  5 omega  -87.00  -35.00   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -61.8151  -45.0000    0.0000    0.0000    0.0000 40

  6 phi   -180.00 -118.90   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -61.8151    0.0000     -        0.0000    0.0000 47

  7 omega -111.00  -59.00   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -61.8151  114.0000  105.0000    0.0000    0.0000 40

  8 omega  -89.00  -37.00   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -61.8151   45.0000  240.0000    0.0000    0.0000 40

  9 omega -111.00  -56.40   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -61.8151  112.0000  214.0000    0.0000    0.0000 42

 10 omega   38.00   90.00   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -45.0000  120.0000    0.0000    0.0000 40

 11 omega  -14.00   41.90   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -75.0000  120.0000    0.0000    0.0000 43

 12 omega   83.00  140.20   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526   75.0000  240.0000    0.0000    0.0000 44

 13 omega   40.00   95.90   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -75.0000    0.0000    0.0000    0.0000 43

 14 omega   39.00   96.20   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -75.0000  240.0000    0.0000    0.0000 44

 15 omega   -7.00   41.10   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -45.0000  120.0000    0.0000    0.0000 37

 16 omega  -14.00   41.90   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -75.0000    0.0000    0.0000    0.0000 43

 17 omega  -15.00   43.50   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526  -75.0000  240.0000    0.0000    0.0000 45

 18 omega   83.00  136.30   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526   56.0000   -1.0000    0.0000    0.0000 41

 19 omega   54.00   86.50   1.3000    2.2000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.7526   62.0000  -35.0000    0.0000    0.0000 25

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13342
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        51.72
_diffrn_reflns_theta_max         51.72
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.816
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orange to red'
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       platelike
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                3808
_reflns_number_total             5320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900600t_si_003.cif
_cod_data_source_block           pme110
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4070076