Conformation of Eight-Membered Benzoannulated Lactams by Combined NMR and DFT Studies
Agnieszka Witosińska; Bogdan Musielak; Paweł Serda; Maria Owińska; Barbara Rys; Journal of Organic Chemistry 77 (2012) 9784–9794; doi:10.1021/jo301859h

data_4027678
_publ_contact_author_address
;
Faculty of Chemistry
Jagiellonian University
Ingardena 3
30-060 Krak\'ow, Poland
;
_publ_contact_author_email       rys@chemia.uj.edu.pl
_publ_contact_author_name        'Rys, B.'
_publ_section_title
;
 Conformation of Eight-Membered Benzoannulated Lactams by Combined NMR and
 DFT Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9784
_journal_page_last               9794
_journal_paper_doi               10.1021/jo301859h
_journal_volume                  77
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C11 H13 N O'
_chemical_formula_sum            'C11 H13 N O'
_chemical_formula_weight         175.22
_chemical_name_common            ar99
_chemical_name_systematic
;
1,4,5,6-tetrahydro-2H-benzo[c]azocin-3-one
;
_space_group_IT_number           61
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_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   9.84720(10)
_cell_length_c                   25.9083(3)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     1913.02(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
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_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.264991E-1
_diffrn_orient_matrix_UB_12      0.46391E-2
_diffrn_orient_matrix_UB_13      0.13062
_diffrn_orient_matrix_UB_21      -0.332233E-1
_diffrn_orient_matrix_UB_22      -0.954291E-1
_diffrn_orient_matrix_UB_23      0.101119E-1
_diffrn_orient_matrix_UB_31      0.356607E-1
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_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_theta_max         26.07
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_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.078
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_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.35
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_refine_diff_density_max         0.134
_refine_diff_density_min         -0.123
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_refine_ls_extinction_coef       0.020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_matrix_type           full
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_refine_ls_R_factor_all          0.056
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                1461
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301859h_si_002.cif
_cod_data_source_block           ar99
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