(1<i>S</i>,3<i>R</i>,8<i>R</i>)-9-(1-Aminoethylidene)-2,2-dichloro-3,7,7-trimethyltricyclo[6.4.0.0^1,3^]undecan-10-one
Benharref, Ahmed; Lassaba, Essêdiya; Avignant, Daniel; Oudahmane, Abdelghani; Berraho, Moha; Acta Crystallographica Section E 67 (2011) o645–o646; doi:10.1107/S1600536811005307

data_2229376
_publ_section_title
;
 (1<i>S</i>,3<i>R</i>,8<i>R</i>)-9-(1-Aminoethylidene)-2,2-dichloro-3,7,7-trimethyltricyclo[6.4.0.0^1,3^]undecan-10-one
;
_journal_coeditor_code           FJ2396
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o645
_journal_page_last               o646
_journal_paper_doi               10.1107/S1600536811005307
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H23 Cl2 N O'
_chemical_formula_moiety         'C16 H23 Cl2 N O'
_chemical_formula_sum            'C16 H23 Cl2 N O'
_chemical_formula_weight         316.25
_chemical_name_systematic
;
(1<i>S</i>,3<i>R</i>,8<i>R</i>)-9-(1-Aminoethylidene)-2,2-dichloro-3,7,7-
trimethyltricyclo[6.4.0.0^1,3^]undecan-10-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.432(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7570(7)
_cell_length_b                   9.7041(9)
_cell_length_c                   10.6901(10)
_cell_measurement_reflns_used    4954
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      3.4
_cell_volume                     803.25(13)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2009)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4954
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.224
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), <b>614</b> Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2355
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                2297
_reflns_number_total             2355
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2396.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2229376
_cod_database_fobs_code          2229376