One-pot Synthesis of Multi-substituted Conjugated Dienones by Trapping Allene Carbocation with Active Ylides
Ni, Dan; Song, Longlong; Zhao, Yun; Liu, Shunying; Chemical Communications  (2022) –; doi:10.1039/D1CC06405C

data_7129546
_publ_section_title
;
 One-pot Synthesis of Multi-substituted Conjugated Dienones by Trapping
 Allene Carbocation with Active Ylides
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06405C
_journal_year                    2022
_chemical_formula_sum            'C40 H37 Br N2 O2'
_chemical_formula_weight         657.62
_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
;
2021-09-20 deposited with the CCDC.	2022-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                107.6090(10)
_cell_angle_beta                 96.1770(10)
_cell_angle_gamma                104.8480(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9024(2)
_cell_length_b                   10.9990(3)
_cell_length_c                   16.8991(5)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.455
_cell_measurement_theta_min      5.163
_cell_volume                     1661.18(8)
_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      293(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  0.0412
_diffrn_reflns_av_unetI/netI     0.0328
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32963
_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         25.999
_diffrn_reflns_theta_min         2.676
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0422P)^2^+0.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4465
_reflns_number_total             6520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06405c2.cif
_cod_data_source_block           mo_d8v21356_0m
_cod_database_code               7129546
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2013-4
_shelx_res_checksum              93129
_shelx_hkl_checksum              40445