Thermodynamic, Kinetic, and Mechanistic Study of Oxygen Atom Transfer from Mesityl Nitrile Oxide to Phosphines and to a Terminal Metal Phosphido Complex
Xiaochen Cai; Subhojit Majumdar; George C. Fortman; Luis Manuel Frutos; Manuel Temprado; Christopher R. Clough; Christopher C. Cummins; Meaghan E. Germain; Taryn Palluccio; Elena V. Rybak-Akimova; Burjor Captain; Carl D. Hoff; Inorganic Chemistry 50 (2011) 9620–9630; doi:10.1021/ic2013599

data_4326384
_publ_section_title
;
 Thermodynamic, Kinetic, and Mechanistic Study of Oxygen Atom Transfer
 from Mesityl Nitrile Oxide to Phosphines and to a Terminal Metal
 Phosphido Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9620
_journal_page_last               9630
_journal_paper_doi               10.1021/ic2013599
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40.5 H53 N3 O'
_chemical_formula_weight         597.86
_chemical_name_systematic
; 
 ? 
;
_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                 96.425(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3510(17)
_cell_length_b                   12.9808(13)
_cell_length_c                   16.5439(16)
_cell_measurement_reflns_used    1932
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.70
_cell_measurement_theta_min      2.25
_cell_volume                     3702.8(6)
_computing_cell_refinement       'SAINT+  V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+  V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       '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  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29404
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0041(12)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6507
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1450P)^2^+0.4829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2708
_reflns_number_gt                3207
_reflns_number_total             6507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2013599_si_002.cif
_cod_data_source_block           p21c
_cod_original_formula_sum        'C40.50 H53 N3 O'
_cod_database_code               4326384