(2<i>R</i>,3a<i>S</i>,5a<i>R</i>,8a<i>R</i>,8b<i>S</i>)-4-Bromo-2-(4-methoxyphenyl)-7,7-dimethyl-3a,5a,8a,8b-tetrahydrobenzo[1,2-<i>d</i>:3,4-<i>d</i>']bis[1,3]dioxole
Martin G. Banwell; Okanya J. Kokas; Anthony C. Willis; Acta Crystallographica Section E 63 (2007) o3820–o3820; doi:10.1107/S1600536807039232

data_2215021
_publ_section_title
(2<i>R</i>,3a<i>S</i>,5a<i>R</i>,8a<i>R</i>,8b<i>S</i>)-4-Bromo-2-(4-methoxyphenyl)-7,7-dimethyl-3a,5a,8a,8b-tetrahydrobenzo[1,2-<i>d</i>:3,4-<i>d</i>']bis[1,3]dioxole
_journal_coeditor_code           BT2471
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3820
_journal_page_last               o3820
_journal_paper_doi               10.1107/S1600536807039232
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C17 H19 Br O5'
_chemical_formula_moiety         'C17 H19 Br O5'
_chemical_formula_sum            'C17 H19 Br O5'
_chemical_formula_weight         383.24
_chemical_name_systematic
;
(2<i>R</i>,3a<i>S</i>,5a<i>R</i>,8a<i>R</i>,8b<i>S</i>)-
4-Bromo-2-(4-methoxyphenyl)-7,7-dimethyl-3a,5a,8a,8b-tetrahydrobenzo[1,2-
<i>d</i>:3,4-<i>d</i>']bis[1,3]dioxole
;
_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
_audit_creation_method           CRYSTALS_ver_12.18
_cell_angle_alpha                90
_cell_angle_beta                 91.7226(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.22850(10)
_cell_length_b                   33.4467(9)
_cell_length_c                   9.4726(3)
_cell_measurement_reflns_used    55931
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.6
_cell_volume                     1655.78(8)
_computing_cell_refinement       'DENZO/SCALEPACK  (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation,
1997)
;
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20604
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.505
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (Mackay <i>et
al.</i>,  1999)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.82
_refine_ls_abs_structure_details 'Flack (1983), 2828 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.012(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9659
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5796
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + (0.03P)^2^ + 0.44P], where P=[max(Fo^2^,0) + 2Fc^2^]/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0777
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                4970
_reflns_number_total             5796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2471.cif
_cod_data_source_block           I
_cod_original_cell_volume        1655.78(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2215021
_cod_database_fobs_code          2215021