Asymmetric catalytic [4+3] cycloaddition of ortho-quinone methides with oxiranes.
Tan, Qingfa; Yu, Han; Luo, Yao; Chang, Fenzhen; Liu, Xiaohua; Zhou, Yuqiao; Feng, Xiaoming; Chemical communications (Cambridge, England) 57 (2021) 3018–3021; doi:10.1039/d1cc00262g

data_7127990
_publ_section_title
;
 Asymmetric catalytic [4+3] cycloaddition of ortho-quinone methides with
 oxiranes.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3018
_journal_page_last               3021
_journal_paper_doi               10.1039/d1cc00262g
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H26 O9'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-01 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
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_cell_angle_beta                 90
_cell_angle_gamma                120
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_cell_length_c                   8.1020(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    144(2)
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_cell_measurement_theta_min      3.14
_cell_volume                     5550.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_diffrn_reflns_av_R_equivalents  0.1508
_diffrn_reflns_av_unetI/netI     0.1015
_diffrn_reflns_Laue_measured_fraction_full 0.964
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_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
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_diffrn_reflns_point_group_measured_fraction_full 0.838
_diffrn_reflns_point_group_measured_fraction_max 0.840
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_diffrn_reflns_theta_min         3.142
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6579
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_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
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'Re-crystallisation from solvent: MeOH, PE'
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_refine_ls_abs_structure_details
; 
 Flack x determined using 1437 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_coef       0.0136(15)
_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)'
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4103
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0972
_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^)+(0.1583P)^2^+1.5394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2310
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.712
_reflns_Friedel_fraction_max     0.714
_reflns_number_gt                3853
_reflns_number_total             4103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00262g2.cif
_cod_data_source_block           tqf003
_cod_depositor_comments
'Adding full bibliography for 7127989--7127990.cif.'
_cod_original_cell_volume        5550.5(4)
_cod_database_code               7127990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              5480