A highly diastereoselective (5+1) annulation of allenoates and pyrazolones catalyzed by CH<sub>3</sub>OK.
Lai, Jingxiong; Huang, You; Chemical communications (Cambridge, England) 60 (2024) 2066–2069; doi:10.1039/d3cc05751h

data_7132790
_publ_section_title
;
 A highly diastereoselective (5+1) annulation of allenoates and
 pyrazolones catalyzed by CH<sub>3</sub>OK.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2066
_journal_page_last               2069
_journal_paper_doi               10.1039/d3cc05751h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C29 H32 N2 O5'
_chemical_formula_weight         488.56
_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-2018/3
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                85.779(3)
_cell_angle_beta                 79.152(3)
_cell_angle_gamma                85.444(3)
_cell_formula_units_Z            4
_cell_length_a                   11.4759(4)
_cell_length_b                   11.5363(3)
_cell_length_c                   19.7187(7)
_cell_measurement_temperature    113(2)
_cell_volume                     2551.20(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27119
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    0.087
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0087(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0624P)^2^+0.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7886
_reflns_number_total             10440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05751h2.cif
_cod_data_source_block           r20220919b
_cod_database_code               7132790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              10753
_shelx_hkl_checksum              81369