Phosphine catalyzed Rauhut−Currier reaction of γ-alkyl allenoate and trapped by Diels-Alder reaction
Zhang, Juan; Hao, Wei; Chen, Ying; Wang, Zhen; Yao, Jinzhong; Yao, Weijun; Chemical Communications  (2023) –; doi:10.1039/D3CC03151A

data_7132069
_publ_section_title
;
 Phosphine catalyzed Rauhut&#x2212;Currier reaction of \g-alkyl allenoate
 and trapped by Diels-Alder reaction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03151A
_journal_year                    2023
_chemical_formula_sum            'C22 H22 Br N2 O5'
_chemical_formula_weight         474.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.058(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.095(4)
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_cell_length_c                   21.347(3)
_cell_measurement_reflns_used    4825
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.33
_cell_volume                     4260.9(11)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19336
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    1.965
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3493
_reflns_number_total             4870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03151a2.cif
_cod_data_source_block           2J11262_0m
_cod_original_cell_volume        4260.9(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7132069
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              51078
_shelx_hkl_checksum              91617