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_1554559
_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            'C28 H36 N2 O2 Si'
_chemical_formula_weight         460.68
_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   mixed
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                83.8910(10)
_cell_angle_beta                 69.7230(10)
_cell_angle_gamma                84.4990(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7904(3)
_cell_length_b                   10.7882(4)
_cell_length_c                   12.3517(4)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      68.2479
_cell_measurement_theta_min      3.8270
_cell_volume                     1214.36(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'D8  Venture'
_diffrn_radiation_type           'cu k\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            31749
_diffrn_reflns_theta_full        68.30
_diffrn_reflns_theta_max         68.30
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.312
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0389P)^2^+0.6308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                4272
_reflns_number_total             4415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo01279b2.cif
_cod_data_source_block           20181011kds
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1554559
_shelx_res_checksum              1284
_shelx_hkl_checksum              47897