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_4515591
_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         'C72 H94 Co2 N6'
_chemical_formula_sum            'C72 H94 Co2 N6'
_chemical_formula_weight         1161.39
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 99.7220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1904(4)
_cell_length_b                   12.5885(3)
_cell_length_c                   22.6178(6)
_cell_measurement_reflns_used    8093
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.44
_cell_volume                     3140.42(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35406
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.656
_diffrn_reflns_theta_min         1.858
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.8718
_exptl_absorpt_correction_T_min  0.8412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         9435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0597P)^2^+0.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7209
_reflns_number_total             9435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00631_si_003.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515591
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.900
_shelx_res_checksum              67644
_shelx_hkl_checksum              72435