Syntheses, Reactivity, and Stereochemistry of η3-Allyl Dithio-Molybdenum Complexes: Crystal Structures ofendo-[Mo(η3-C3H5)(η2-S2CNC4H8)(CO)(η2-dppe)],endo-[Mo(η3-C3H5){η2-S2P(OEt)2}(CO)(η2-dppe)],exo-,endo-[Mo(η3-C3H5)(η2-S2CNC4H8)(CO)(η2-dppm)], andendo-[Mo(η3-C3H5){η2-S2P(OEt)2}(CO)(η2-dppm)]
Yih, Kuang-Hway; Lee, Gene-Hsiang; Huang, Shou-Ling; Wang, Yu; Organometallics 21 (2002) 5767–; doi:10.1021/om0207156

data_4077133
_publ_section_title
;
 Syntheses, Reactivity, and Stereochemistry of \h3-Allyl Dithio-Molybdenum
 Complexes:&#x00A0; Crystal Structures
 ofendo-[Mo(\h3-C3H5)(\h2-S2CNC4H8)(CO)(\h2-dppe)],endo-[Mo(\h3-C3H5){\h2-S2P(OEt)2}(CO)(\h2-dppe)],exo-,endo-[Mo(\h3-C3H5)(\h2-S2CNC4H8)(CO)(\h2-dppm)],
 andendo-[Mo(\h3-C3H5){\h2-S2P(OEt)2}(CO)(\h2-dppm)]
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5767
_journal_paper_doi               10.1021/om0207156
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C68.5 H71 Cl Mo2 N2 O2 P4 S4'
_chemical_formula_weight         1433.72
_chemical_name_systematic
; 

 ? 

;
_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-97
_cell_angle_alpha                116.0641(3)
_cell_angle_beta                 92.4616(3)
_cell_angle_gamma                99.2887(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1526(1)
_cell_length_b                   15.8505(1)
_cell_length_c                   17.4172(1)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.31
_cell_volume                     3192.35(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81709
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1474
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0042(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         14649
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.6603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                12387
_reflns_number_total             14649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0207156.cif
_cod_data_source_block           ic8291
_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 2.4.1 from 2010-06-29.

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_measured' 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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C68.50 H71 Cl Mo2 N2 O2 P4 S4'
_cod_database_code               4077133