Cobalt- and Iron-Catalyzed Isomerization‒Hydroboration of Branched Alkenes: Terminal Hydroboration with Pinacolborane and 1,3,2-Diazaborolanes
Ogawa, Takahiko; Ruddy, Adam J.; Sydora, Orson L.; Stradiotto, Mark; Turculet, Laura; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00823

data_4086862
_publ_section_title
;
 Cobalt- and Iron-Catalyzed Isomerization--Hydroboration of Branched
 Alkenes: Terminal Hydroboration with Pinacolborane and
 1,3,2-Diazaborolanes
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00823
_journal_year                    2016
_chemical_formula_moiety         'C39 H58 Co N3 P'
_chemical_formula_sum            'C39 H58 Co N3 P'
_chemical_formula_weight         658.78
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-06-24T10:30:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.9240(10)
_cell_angle_beta                 90.4010(10)
_cell_angle_gamma                101.4080(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9599(5)
_cell_length_b                   11.9389(5)
_cell_length_c                   14.9189(5)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.31
_cell_measurement_wavelength     0.71073
_cell_volume                     1898.65(13)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.001453
_diffrn_orient_matrix_UB_12      0.05358
_diffrn_orient_matrix_UB_13      -0.046767
_diffrn_orient_matrix_UB_21      -0.034899
_diffrn_orient_matrix_UB_22      0.054482
_diffrn_orient_matrix_UB_23      0.044042
_diffrn_orient_matrix_UB_31      0.086329
_diffrn_orient_matrix_UB_32      0.039713
_diffrn_orient_matrix_UB_33      0.020901
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            48909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         1.376
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.9245
_exptl_absorpt_correction_T_min  0.7893
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.586
_exptl_crystal_size_mid          0.444
_exptl_crystal_size_min          0.319
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     411
_refine_ls_number_reflns         9323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.5649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0
_reflns_number_gt                8612
_reflns_number_total             9323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00823_si_001.cif
_cod_data_source_block           CoLtBuNHdipp
_cod_database_code               4086862