Catalytic enantioselective ene-type reactions of vinylogous hydrazone: construction of α-methylene-γ-butyrolactone derivatives.
Zhang, Hang; Yao, Qian; Cao, Weidi; Ge, Shulin; Xu, Jinxiu; Liu, Xiaohua; Feng, Xiaoming; Chemical communications (Cambridge, England) 54 (2018) 12511–12514; doi:10.1039/c8cc07567k

data_7122457
_publ_section_title
;
 Catalytic enantioselective ene-type reactions of vinylogous hydrazone:
 construction of \a-methylene-\g-butyrolactone derivatives.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12511
_journal_page_last               12514
_journal_paper_doi               10.1039/c8cc07567k
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C44 H71 N5 O5 Zn, 2(C2 F6 N O4 S2), C2 H3 N [+ solvent]'
_chemical_formula_sum            'C50 H74 F12 N8 O13 S4 Zn'
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_space_group_name_Hall           'P 2yb'
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_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
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_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
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_diffrn_reflns_limit_h_min       -24
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_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.224
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_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2944.0
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_refine_diff_density_min         -0.891
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_refine_ls_abs_structure_details
;
 Flack x determined using 10976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(7)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         27566
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_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+6.3940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                25246
_reflns_number_total             27566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07567k2.cif
_cod_data_source_block           fxm-zh-c1-140k_sq
_cod_depositor_comments
'Adding full bibliography for 7122454--7122457.cif.'
_cod_original_cell_volume        7559.14(12)
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_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              73497
_shelx_fab_checksum              63497