Cp*Co(III)-Catalyzed C-H Alkenylation/Annulation to Afford Spiro Indenyl Benzosultam.
Liu, Hui; Li, Jie; Xiong, Miao; Jiang, Jijun; Wang, Jun; The Journal of organic chemistry 81 (2016) 6093–6099; doi:10.1021/acs.joc.6b00976

data_4036925
_publ_section_title
;
 Cp*Co(III)-Catalyzed C-H Alkenylation/Annulation to Afford Spiro Indenyl
 Benzosultam.
;
_journal_issue                   14
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6093
_journal_page_last               6099
_journal_paper_doi               10.1021/acs.joc.6b00976
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C28 H21 N O3 S, C H Cl3'
_chemical_formula_sum            'C29 H22 Cl3 N O3 S'
_chemical_formula_weight         570.88
_chemical_name_common            3ha
_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   geom
_audit_creation_date             2016-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5388(4)
_cell_length_b                   19.2355(6)
_cell_length_c                   13.3088(5)
_cell_measurement_reflns_used    5918
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     2616.74(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20633
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.373
_exptl_crystal_size_min          0.326
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0661P)^2^+2.9526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4886
_reflns_number_total             5918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00976_si_002.cif
_cod_data_source_block           3ga
_cod_database_code               4036925
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C29(H29)
2.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C26(H26), C27(H27)
;
_shelx_res_checksum              72031
_shelx_hkl_checksum              34760
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'