Preparation of hydrido [CNC]-pincer cobalt complexes via selective C‒H/C‒F bond activation and their catalytic performances
Yang, Fei; Wang, Yangyang; Lu, Faguan; Xie, Shangqing; Qi, Xinghao; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; New Journal of Chemistry 42 (2018) 15578–; doi:10.1039/C8NJ02979B

data_7057623
_publ_section_title
;
 Preparation of hydrido [CNC]-pincer cobalt complexes via selective
 C--H/C--F bond activation and their catalytic performances
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15578
_journal_paper_doi               10.1039/C8NJ02979B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C23 H27 Co F2 I N P2'
_chemical_formula_sum            'C23 H27 Co F2 I N P2'
_chemical_formula_weight         603.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-04-27 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.600(2)
_cell_length_b                   15.531(2)
_cell_length_c                   19.029(3)
_cell_measurement_reflns_used    3473
_cell_measurement_temperature    298
_cell_measurement_theta_max      21.546
_cell_measurement_theta_min      2.467
_cell_volume                     4906.0(12)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2003)'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detactor'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27459
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  0.7855
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.486
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                3288
_reflns_number_total             5567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj02979b2.cif
_cod_data_source_block           complex11
_cod_depositor_comments
'Adding full bibliography for 7057621--7057623.cif.'
_cod_database_code               7057623
_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 Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C5(H5), C9(H9), C14(H14), C10(H10), C3(H3), C11(H11),
 C16(H16)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'