Highly Efficient Large Bite Angle Diphosphine Substituted Molybdenum Catalyst for Hydrosilylation
Chakraborty, Subrata; Blacque, Olivier; Fox, Thomas; Berke, Heinz; ACS Catalysis 3 (2013) 2208–; doi:10.1021/cs4004276

data_4508367
_publ_section_title
;
 Highly Efficient Large Bite Angle Diphosphine Substituted Molybdenum
 Catalyst for Hydrosilylation
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              2208
_journal_paper_doi               10.1021/cs4004276
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C38 H28 Cl Mo N O4 P2, C7 H8'
_chemical_formula_sum            'C45 H36 Cl Mo N O4 P2'
_chemical_formula_weight         848.08
_chemical_name_systematic
'Chloro(nitrosyl)(dicarbonyl)[(oxydibenzene-2,1-diyl)bis(diphenylphosphane-\k<i>P</i>)]molybdenum toluene solvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.155(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5883(1)
_cell_length_b                   13.8586(1)
_cell_length_c                   24.9475(2)
_cell_measurement_reflns_used    31110
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      2.57
_cell_volume                     3930.82(6)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_molecular_graphics
; ORTEP-3 for Windows.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97 -- Sheldrick, G. M (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            67377
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         12004
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                9437
_reflns_number_total             12004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs4004276_si_005.cif
_cod_data_source_block           5(CCDC-921395)
_cod_original_cell_volume        3930.82(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4508367