Stereoselective Three-component Cascade Synthesis of α-Substituted 2,4-Dienamide from gem-Difluorochloro Ethanes
Das, Shyamsundar; Ko, Nakeun; Lee, Eunsung; Kim, Sang Eun; Lee, Byung Chul; Chemical Communications  (2019) –; doi:10.1039/C9CC07100H

data_7124424
_publ_section_title
;
 Stereoselective Three-component Cascade Synthesis of \a-Substituted
 2,4-Dienamide from gem-Difluorochloro Ethanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07100H
_journal_year                    2019
_chemical_formula_sum            'C56 H68 N4 O4'
_chemical_formula_weight         861.14
_chemical_name_common            Z-24
_chemical_name_systematic        (Z)-N,5-dimethyl-2-phenylhexa-2,4-dienamide
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-04-22 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                89.994(3)
_cell_angle_beta                 89.985(3)
_cell_angle_gamma                90.048(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2925(9)
_cell_length_b                   9.7764(10)
_cell_length_c                   28.414(3)
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_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      17.87
_cell_measurement_theta_min      2.53
_cell_volume                     2581.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47325
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         0.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.872
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.601
_refine_ls_R_factor_all          0.3080
_refine_ls_R_factor_gt           0.1915
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4975
_refine_ls_wR_factor_ref         0.5484
_reflns_number_gt                3573
_reflns_number_total             8792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc07100h2.cif
_cod_data_source_block           output
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2581.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7124424