Photochemical behavior of 2,5-di-tert-butyl-3H-azepine: unexpected formation of a dicyclopenta[b,e]pyridine derivative and a cis,cis-cyclodeca-1,6-diene derivative
Satake, Kyosuke; Tawada, Yuko; Takami, Shizuka; Kimura, Masaru; Chemical Communications  (2001) 1382–; doi:10.1039/b101225h

data_7114735
_publ_section_title
;
 Photochemical behavior of 2,5-di-tert-butyl-3H-azepine: unexpected
 formation of a dicyclopenta[b,e]pyridine derivative and a
 cis,cis-cyclodeca-1,6-diene derivative
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1382
_journal_paper_doi               10.1039/b101225h
_journal_year                    2001
_chemical_formula_moiety         'C28 H47 N O2 '
_chemical_formula_sum            'C28 H47 N O2'
_chemical_formula_weight         429.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.400(2)
_cell_length_b                   21.835(6)
_cell_length_c                   10.935(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      11.1
_cell_volume                     2721.9(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_publication_material  'teXsan for Windows version 1.06'
_computing_structure_refinement  'teXsan for Windows version 1.06'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.06821
_diffrn_orient_matrix_UB_12      -0.01780
_diffrn_orient_matrix_UB_13      0.04530
_diffrn_orient_matrix_UB_21      -0.03314
_diffrn_orient_matrix_UB_22      0.04204
_diffrn_orient_matrix_UB_23      0.01160
_diffrn_orient_matrix_UB_31      -0.04410
_diffrn_orient_matrix_UB_32      -0.00404
_diffrn_orient_matrix_UB_33      -0.07878
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3138
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        3.92
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type
;
psi-scan (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'not determined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.149
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.164
_refine_ls_R_factor_gt           0.089
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.178
_refine_ls_wR_factor_ref         0.178
_reflns_number_gt                1468
_reflns_number_total             2743
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b101225h.txt
_cod_data_source_block           3H-azepine_photodimer
_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 
;
_cod_original_cell_volume        2721.9(12)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C28 H47 N O2 '
_cod_database_code               7114735