Ru(ii)-Catalyzed spirocyclization of aryl N-sulfonyl ketimines with aryl isocyanates through an aromatic C-H bond activation.
K, Nagarjuna Reddy; U, Subhadra; B, Sridhar; B V, Subba Reddy; Organic & biomolecular chemistry 16 (2018) 2522–2526; doi:10.1039/C7OB03198J

data_7156155
_publ_section_title
;
 Ru(ii)-Catalyzed spirocyclization of aryl N-sulfonyl ketimines with aryl
 isocyanates through an aromatic C-H bond activation.
;
_journal_issue                   14
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2522
_journal_page_last               2526
_journal_paper_doi               10.1039/C7OB03198J
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C21 H15 N3 O6 S'
_chemical_formula_sum            'C21 H15 N3 O6 S'
_chemical_formula_weight         437.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-09 deposited with the CCDC.
2018-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2970(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.26140(10)
_cell_length_b                   11.3690(2)
_cell_length_c                   10.8661(2)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.65
_cell_volume                     979.58(3)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  '<i>SHELXL2014</i> (Sheldrick, 2015)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28348
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.570
_diffrn_reflns_theta_min         2.569
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2016'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       needle
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 2540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5670
_reflns_number_total             5995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob03198j2.cif
_cod_data_source_block           KA238_0m
_cod_depositor_comments          'Adding full bibliography for 7156155.cif.'
_cod_database_code               7156155
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              70063