Unusual reactions of N-allylic difluoroenamines under thermal conditions
Amii, Hideki; Ichihara, Yutaka; Nakagawa, Takashi; Kobayashi, Takeshi; Uneyama, Kenji; Chemical Communications  (2003) 2902–; doi:10.1039/b309696c

data_7113803
_publ_section_title
;
 Unusual reactions of N-allylic difluoroenamines under thermal conditions
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2902
_journal_paper_doi               10.1039/b309696c
_journal_year                    2003
_chemical_formula_moiety         'C18 H17 F2 N O '
_chemical_formula_sum            'C18 H17 F2 N O'
_chemical_formula_weight         301.34
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_date             'Wed Jun 26 23:37:34 2003'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 107.690(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4898(5)
_cell_length_b                   21.309(1)
_cell_length_c                   7.9275(3)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1527.28(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku RAXIS-IV'
_diffrn_measurement_method       =20
_diffrn_orient_matrix_UB_11      -0.09328
_diffrn_orient_matrix_UB_12      -0.02520
_diffrn_orient_matrix_UB_13      -0.03599
_diffrn_orient_matrix_UB_21      0.05926
_diffrn_orient_matrix_UB_22      -0.03955
_diffrn_orient_matrix_UB_23      0.02792
_diffrn_orient_matrix_UB_31      -0.00452
_diffrn_orient_matrix_UB_32      0.00158
_diffrn_orient_matrix_UB_33      0.12432
_diffrn_radiation_detector       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1688
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.255
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             632.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.09
_refine_diff_density_min         -0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.375
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0398
_refine_ls_shift/esd_max         0.0020
_refine_ls_shift/esd_mean        0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w == 1/[\s^2^(Fo) + 0.00090|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          1490
_reflns_number_total             1688
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            b309696c.txt
_cod_data_source_block           Compound_4c_(R3==Ph)
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w == 1/[=A5s^2^(Fo) +
0.00090|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w == 1/[=A5s^2^(Fo) + 0.00090|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1527.3(1)
_cod_original_sg_symbol_H-M      'C c          '
_cod_original_formula_sum        'C18 H17 F2 N O '
_cod_database_code               7113803