2',10'-Dibromospiro[cylohexane-1,6-dibenzo[<i>d</i>,<i>f</i>][1,3]dioxepine]
Zhang, Cheng-Bo; Zhang, Hai-Quan; Li, Qing-Shan; Xing, Guang-Zhong; Acta Crystallographica Section E 66 (2010) o1047–; doi:10.1107/S1600536810012535

data_2225935
_publ_section_title
;
 2',10'-Dibromospiro[cylohexane-1,6-dibenzo[<i>d</i>,<i>f</i>][1,3]dioxepine]
;
_journal_coeditor_code           NG2752
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1047
_journal_paper_doi               10.1107/S1600536810012535
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C18 H16 Br2 O2'
_chemical_formula_moiety         'C18 H16 Br2 O2'
_chemical_formula_sum            'C18 H16 Br2 O2'
_chemical_formula_weight         424.13
_chemical_name_systematic
;
2',10'-Dibromospiro[cylohexane-1,6-dibenzo[<i>d</i>,<i>f</i>][1,3]dioxepine]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.793(4)
_cell_length_b                   10.143(5)
_cell_length_c                   18.279(5)
_cell_measurement_reflns_used    3788
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      54.84
_cell_measurement_theta_min      2.23
_cell_volume                     3299(2)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29533
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.919
_exptl_absorpt_correction_T_max  0.6137
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.638
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+1.6141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2294
_reflns_number_total             3735
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng2752.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_database_code               2225935
_cod_database_fobs_code          2225935