Rh(iii)-catalyzed C–H activation/[4 + 3] cycloaddition of benzamides and vinylcarbenoids: facile synthesis of azepinones
Cui, Sunliang; Zhang, Yan; Wang, Dahai; Wu, Qifan; Chemical Science 4 (2013) 3912–; doi:10.1039/c3sc51777b

data_1514526
_publ_section_title
;
 Rh(iii)-catalyzed C--H activation/[4 + 3] cycloaddition of benzamides and
 vinylcarbenoids: facile synthesis of azepinones
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3912
_journal_paper_doi               10.1039/c3sc51777b
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C17 H17 Cl3 N2 O3'
_chemical_formula_sum            'C17 H17 Cl3 N2 O3'
_chemical_formula_weight         403.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.745(8)
_cell_angle_beta                 71.023(9)
_cell_angle_gamma                89.009(8)
_cell_formula_units_Z            2
_cell_length_a                   9.7614(10)
_cell_length_b                   10.2988(10)
_cell_length_c                   10.4722(11)
_cell_measurement_reflns_used    1408
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5862
_cell_measurement_theta_min      3.3519
_cell_volume                     981.91(18)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6121
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.8845
_exptl_absorpt_correction_T_min  0.8488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.777
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.515
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3593
_refine_ls_wR_factor_ref         0.4023
_reflns_number_gt                2407
_reflns_number_total             3582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51777b.txt
_cod_data_source_block           130515_zy_4_27_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        981.92(17)
_cod_database_code               1514526