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_7122456
_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_formula_sum            'C34 H44 N4 O4'
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_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
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_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                78.245(5)
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_cell_measurement_temperature    300(2)
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_point_group_measured_fraction_full 0.965
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_exptl_absorpt_coefficient_mu    0.627
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.150
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_refine_diff_density_min         -0.111
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_refine_ls_abs_structure_details
;
 Flack x determined using 2373 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5616
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0391P)^2^+0.0448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                5291
_reflns_number_total             5616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07567k2.cif
_cod_data_source_block           cu_20180508_zh_1_0m
_cod_depositor_comments
'Adding full bibliography for 7122454--7122457.cif.'
_cod_database_code               7122456
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              64963