Catalytic asymmetric synthesis of CF3-substituted tertiary propargylic alcohols via direct aldol reaction of α-N3 amide
Noda, Hidetoshi; Amemiya, Fuyuki; Weidner, Karin; Kumagai, Naoya; Shibasaki, Masakatsu; Chem. Sci. 8 (2017) 3260–; doi:10.1039/C7SC00330G

data_1545519
_publ_section_title
;
 Catalytic asymmetric synthesis of CF3-substituted tertiary propargylic
 alcohols via direct aldol reaction of \a-N3 amide
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              3260
_journal_paper_doi               10.1039/C7SC00330G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C20 H18 Cu F6 N10 O8 S2'
_chemical_formula_sum            'C20 H18 Cu F6 N10 O8 S2'
_chemical_formula_weight         768.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-08-13 deposited with the CCDC.
2017-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                110.106(8)
_cell_angle_beta                 95.309(7)
_cell_angle_gamma                106.922(8)
_cell_formula_units_Z            1
_cell_length_a                   7.3568(6)
_cell_length_b                   10.0126(8)
_cell_length_c                   10.8607(9)
_cell_measurement_reflns_used    4504
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.06
_cell_measurement_theta_min      4.44
_cell_volume                     702.02(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8326
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         4.439
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.472
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             387.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0745P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1615
_reflns_number_total             2514
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7sc00330g2.cif
_cod_data_source_block           160524Noda
_cod_depositor_comments
'Adding full bibliography for 1545518--1545520.cif.'
_cod_original_cell_volume        702.02(11)
_cod_database_code               1545519
_shelx_res_checksum              76740