Formation of 2-Azaallyl Cobalt(I) Complexes by Csp3‒H Bond Activation
Xing, Junyang; Sun, Hongjian; Xue, Benjing; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; Organometallics 36 (2017) 975–; doi:10.1021/acs.organomet.6b00884

data_4089186
_publ_section_title
;
 Formation of 2-Azaallyl Cobalt(I) Complexes by Csp3--H Bond Activation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              975
_journal_paper_doi               10.1021/acs.organomet.6b00884
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C32 H38 Cl Co N P3'
_chemical_formula_sum            'C32 H38 Cl Co N P3'
_chemical_formula_weight         623.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                89.813(3)
_cell_angle_beta                 80.316(3)
_cell_angle_gamma                69.325(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5606(3)
_cell_length_b                   9.7857(4)
_cell_length_c                   19.9625(8)
_cell_measurement_reflns_used    20623
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      65.95
_cell_measurement_theta_min      2.25
_cell_volume                     1539.44(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '2.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'secondary plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.890
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12022
_diffrn_reflns_point_group_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         65.039
_diffrn_reflns_theta_min         4.502
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.802
_exptl_absorpt_correction_T_max  0.1033
_exptl_absorpt_correction_T_min  0.0099
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       needle
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1396P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4363
_reflns_number_total             4966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00884_si_002.cif
_cod_data_source_block           sun14
_cod_database_code               4089186
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C25(H25),
  C26(H26)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'