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_4508365
_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
'2(C42 H37 Mo N4 O2 P2), 2(C32 H12 B F24), C5 H12'
_chemical_formula_sum            'C153 H110 B2 F48 Mo2 N8 O4 P4'
_chemical_formula_weight         3373.87
_chemical_name_systematic
;Tris(acetonitrile)(nitrosyl)[(oxydibenzene-2,1-diyl)bis(diphenylphosphane-\k<i>P</i>)]molybdenum tetrakis[3'5-bis(trifluoromethyl)phenyl]borate
hemipentane solvate
;
_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                88.382(2)
_cell_angle_beta                 81.163(2)
_cell_angle_gamma                87.527(1)
_cell_formula_units_Z            1
_cell_length_a                   12.4979(2)
_cell_length_b                   15.4233(3)
_cell_length_c                   19.7740(4)
_cell_measurement_reflns_used    33262
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.67
_cell_measurement_theta_min      2.64
_cell_volume                     3761.96(12)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66387
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
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            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1702
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         22919
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                17440
_reflns_number_total             22919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs4004276_si_003.cif
_cod_data_source_block           3(CCDC-921394)
_cod_database_code               4508365