Trisannulation of benzamides and cyclohexadienone-tethered 1,1-disubstituted allenes initiated by Cp*Rh(iii)-catalyzed C–H activation
Kong, De-Shen; Wang, Yi-Fan; Tan, Yun-Xuan; Zhang, Jun-Li; Zhang, Jian-Ge; Tian, Ping; Lin, Guo-Qiang; Organic Chemistry Frontiers 6 (2019) 699–; doi:10.1039/C8QO01279B

data_1554560
_publ_section_title
;
 Trisannulation of benzamides and cyclohexadienone-tethered
 1,1-disubstituted allenes initiated by Cp*Rh(iii)-catalyzed C--H
 activation
;
_journal_issue                   5
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              699
_journal_paper_doi               10.1039/C8QO01279B
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C27 H31 N O4 Si'
_chemical_formula_weight         461.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                74.3930(10)
_cell_angle_beta                 85.5710(10)
_cell_angle_gamma                88.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9601(4)
_cell_length_b                   10.6766(3)
_cell_length_c                   11.8691(4)
_cell_measurement_reflns_used    8368
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.958
_cell_measurement_theta_min      4.567
_cell_volume                     1211.99(7)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20365
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.047
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4491
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+0.5223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3658
_reflns_number_total             4491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo01279b2.cif
_cod_data_source_block           mo_d8v17709_0m
_cod_database_code               1554560
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4
_shelx_res_checksum              42020
_shelx_hkl_checksum              92180