Asymmetric synthesis of complex tricyclo[3.2.2.0]nonenes from racemic norcaradienes: kinetic resolution <i>via</i> Diels-Alder reaction.
Wang, Siyuan; Zhou, Yuqiao; Xiao, Wanlong; Li, Zegong; Liu, Xiaohua; Feng, Xiaoming; Chemical science 14 (2023) 1844–1851; doi:10.1039/d2sc06490a

data_1568269
_publ_section_title
;
 Asymmetric synthesis of complex tricyclo[3.2.2.0]nonenes from racemic
 norcaradienes: kinetic resolution <i>via</i> Diels-Alder reaction.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              1844
_journal_page_last               1851
_journal_paper_doi               10.1039/d2sc06490a
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C53 H84 Co N4 O6, 2(Cl O4), C4 H8 O'
_chemical_formula_sum            'C57 H92 Cl2 Co N4 O15'
_chemical_formula_weight         1203.17
_space_group_crystal_system      orthorhombic
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2022-10-12 deposited with the CCDC.	2023-01-12 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_cell_length_c                   41.707(3)
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_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.37
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_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, Hexane'
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; 
 Refined as an inversion twin. 
;
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+2.8464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1059
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_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10340
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_cod_data_source_block           waf014
_cod_depositor_comments
'Adding full bibliography for 1568266--1568269.cif.'
_cod_original_cell_volume        6208.1(7)
_cod_database_code               1568269
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.840
_shelx_res_checksum              23328
_shelx_hkl_checksum              52730