(1<i>R</i>,4<i>R</i>,6<i>S</i>,7<i>R</i>)-5,5-Dibromo-1,4,8,8-tetramethyltricyclo[5.4.1.0^4,6^]dodecan-12-one
Zaki, Mohamed; Benharref, Ahmed; Daran, Jean-Claude; Berraho, Moha; Acta Crystallographica Section E 70 (2014) o526–; doi:10.1107/S1600536814007351

data_2239310
_publ_section_title
;
 (1<i>R</i>,4<i>R</i>,6<i>S</i>,7<i>R</i>)-5,5-Dibromo-1,4,8,8-tetramethyltricyclo[5.4.1.0^4,6^]dodecan-12-one
;
_journal_coeditor_code           BT6972
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o526
_journal_paper_doi               10.1107/S1600536814007351
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C16 H24 Br2 O'
_chemical_formula_moiety         'C16 H24 Br2 O'
_chemical_formula_sum            'C16 H24 Br2 O'
_chemical_formula_weight         392.17
_chemical_name_systematic
;
(1<i>R</i>,4<i>R</i>,6<i>S</i>,7<i>R</i>)-5,5-Dibromo-1,4,8,8-tetramethyltricyclo[5.4.1.0^4,6^]dodecan-12-one
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.008(6)
_cell_angle_beta                 83.921(6)
_cell_angle_gamma                89.511(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6550(3)
_cell_length_b                   9.4142(4)
_cell_length_c                   12.9389(13)
_cell_measurement_reflns_used    2828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.6430
_cell_measurement_theta_min      3.7250
_cell_volume                     804.13(10)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur (Eos, Gemini ultra)'
_diffrn_measurement_method       '\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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11451
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    5.032
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.624
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), 3035 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6327
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                5209
_reflns_number_total             6327
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6972sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        804.13(9)
_cod_database_code               2239310
_cod_database_fobs_code          2239310