Rh(III)-Catalyzed Diastereoselective Cascade Annulation of Enone-Tethered Cyclohexadienones via a C(sp2)−H Bond Activation
Jadhav, Sandip B.; Maurya, Sundaram; Navaneetha, N.; Chegondi, Rambabu; Chemical Communications  (2021) –; doi:10.1039/D1CC05941F

data_7129285
_publ_section_title
;
 Rh(III)-Catalyzed Diastereoselective Cascade Annulation of Enone-Tethered
 Cyclohexadienones via a C(sp2)&#x2212;H Bond Activation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05941F
_journal_year                    2021
_chemical_formula_moiety         'C25 H24 Br N O5'
_chemical_formula_sum            'C25 H24 Br N O5'
_chemical_formula_weight         498.36
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.607(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.333(5)
_cell_length_b                   13.046(5)
_cell_length_c                   15.250(5)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.906
_cell_measurement_theta_min      2.327
_cell_volume                     2351.3(15)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37041
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.093
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane and Hexane (3:7)'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5393
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0421P)^2^+0.4928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4024
_reflns_number_total             5393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05941f2.cif
_cod_data_source_block           KB23_0m
_cod_original_cell_volume        2351.2(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7129285
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.751
_shelx_res_checksum              19879
_shelx_hkl_checksum              16054