Cobalt catalyzed sp3C‒H amination utilizing aryl azides
Villanueva, Omar; Weldy, Nina Mace; Blakey, Simon B.; MacBeth, Cora E.; Chem. Sci. 6 (2015) 6672–; doi:10.1039/C5SC01162K

data_1529314
_publ_section_title
;
 Cobalt catalyzed sp3C--H amination utilizing aryl azides
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6672
_journal_paper_doi               10.1039/C5SC01162K
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
'C32 H16 Co2 F12 N6 O4, 2(C8 H20 N), C4 H10 O'
_chemical_formula_sum            'C52 H66 Co2 F12 N8 O5'
_chemical_formula_weight         1229.00
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-03-31 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.28(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.072(2)
_cell_length_b                   38.683(8)
_cell_length_c                   14.706(3)
_cell_measurement_reflns_used    7688
_cell_measurement_theta_max      21.773
_cell_measurement_theta_min      2.299
_cell_volume                     5670(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            101432
_diffrn_reflns_theta_full        28.6994
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'"SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0677 before and 0.0616 after correction. The Ratio of minimum to maximum transmission is 0.8908. The \l/2 correction factor is 0.00. {Info from /Users/ovilla05/Desktop/OV-B2-290.abs}'
_exptl_crystal_density_diffrn    1.4396
_exptl_crystal_F_000             2548.4051
_refine_diff_density_max         1.4134
_refine_diff_density_min         -0.9101
_refine_diff_density_rms         0.1582
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             11.6288
_refine_ls_goodness_of_fit_ref   1.0361
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    102
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0361
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.0075
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+4.3447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              52
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -9
_reflns_number_gt                8612
_reflns_number_total             14606
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5sc01162k2.cif
_cod_data_source_block           OV-B2-290
_cod_depositor_comments
'Adding full bibliography for 1529314--1529316.cif.'
_cod_database_code               1529314
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'