Well-Defined β-Diketiminatocobalt(II) Complexes for Alkene Cyclohydroamination of Primary Amines
Lepori, Clément; Gómez-Orellana, Pablo; Ouharzoune, Allissa; Guillot, Régis; Lledós, Agusti; Ujaque, Gregori; Hannedouche, Jérôme; ACS Catalysis 8 (2018) 4446–; doi:10.1021/acscatal.8b00631

data_4515592
_publ_section_title
;
 Well-Defined \b-Diketiminatocobalt(II) Complexes for Alkene
 Cyclohydroamination of Primary Amines
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4446
_journal_paper_doi               10.1021/acscatal.8b00631
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C31 H48 Co N2 O Si'
_chemical_formula_sum            'C31 H48 Co N2 O Si'
_chemical_formula_weight         551.73
_chemical_properties_physical    'air-sensitive, oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 93.4830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0369(5)
_cell_length_b                   10.7343(3)
_cell_length_c                   17.0418(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.39
_cell_volume                     3110.83(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36866
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         9103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.8590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7117
_reflns_number_total             9103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00631_si_002.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515592
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              44156
_shelx_hkl_checksum              83934