Direct Access to Cobaltacycles via C-H Activation: N-Chloroamide-Enabled Room-Temperature Synthesis of Heterocycles.
Yu, Xiaolong; Chen, Kehao; Guo, Shan; Shi, Pengfei; Song, Chao; Zhu, Jin; Organic letters 19 (2017) 5348–5351; doi:10.1021/acs.orglett.7b02632

data_1547237
_publ_section_title
;
 Direct Access to Cobaltacycles via C-H Activation: N-Chloroamide-Enabled
 Room-Temperature Synthesis of Heterocycles.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5348
_journal_page_last               5351
_journal_paper_doi               10.1021/acs.orglett.7b02632
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C18 H18 Br Cl Co N O2, C H4 O'
_chemical_formula_sum            'C19 H22 Br Cl Co N O3'
_chemical_formula_weight         486.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 113.1250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3729(2)
_cell_length_b                   18.1458(4)
_cell_length_c                   14.1298(3)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.66
_cell_measurement_theta_min      4.18
_cell_volume                     1974.29(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18950
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.656
_diffrn_reflns_theta_max         66.656
_diffrn_reflns_theta_min         4.184
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    10.586
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.05
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_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0364P)^2^+1.4543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3367
_reflns_number_total             3471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02632_si_004.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1547236--1547237.cif.'
_cod_original_formula_sum        ' C19 H22 Br Cl Co N O3'
_cod_database_code               1547237
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              45833
_shelx_hkl_checksum              77627