(1<i>S</i>,2<i>R</i>,8<i>R</i>)-2,2-Dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1,3^]dodec-10-en-9-one
Benharref, Ahmed; El Ammari, Lahcen; Berraho, Moha; Acta Crystallographica Section E 66 (2010) o2911–; doi:10.1107/S1600536810040213

data_2227658
_publ_section_title
;
 (1<i>S</i>,2<i>R</i>,8<i>R</i>)-2,2-Dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1,3^]dodec-10-en-9-one
;
_journal_coeditor_code           IM2235
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2911
_journal_paper_doi               10.1107/S1600536810040213
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C16 H22 Cl2 O'
_chemical_formula_moiety         'C16 H22 Cl2 O'
_chemical_formula_sum            'C16 H22 Cl2 O'
_chemical_formula_weight         301.24
_chemical_name_common            6\a,7\a-dichlorocarbene-himachal-3-en-2-one
_chemical_name_systematic
;
(1<i>S</i>,2<i>R</i>,8<i>R</i>)-2,2-Dichloro-3,7,7,10-
tetramethyltricyclo[6.4.0.0^1,3^]dodec-10-en-9-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                 90.430(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6680(7)
_cell_length_b                   18.7760(16)
_cell_length_c                   12.7696(12)
_cell_measurement_reflns_used    11524
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.29
_cell_volume                     1598.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia,1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXS97 (Sheldrick,2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick,2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11524
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.174
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), 1791 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                4348
_reflns_number_total             5817
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2235.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2227658
_cod_database_fobs_code          2227658