(4a<i>R</i>,9<i>R</i>,9a<i>R</i>)-7-Bromo-9-nitromethyl-2,3,4,4a,9,9a-hexahydro-1<i>H</i>-xanthen-1-one
Wu, Chao; Guo, Yan-Jun; Xia, Ai-Bao; Acta Crystallographica Section E 69 (2013) o794–; doi:10.1107/S1600536813008659

data_2237827
_publ_section_title
;
 (4a<i>R</i>,9<i>R</i>,9a<i>R</i>)-7-Bromo-9-nitromethyl-2,3,4,4a,9,9a-hexahydro-1<i>H</i>-xanthen-1-one
;
_journal_coeditor_code           FY2090
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o794
_journal_paper_doi               10.1107/S1600536813008659
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C14 H14 Br N O4'
_chemical_formula_moiety         'C14 H14 Br N O4'
_chemical_formula_sum            'C14 H14 Br N O4'
_chemical_formula_weight         340.17
_chemical_name_systematic
(4a<i>R</i>,9<i>R</i>,9a<i>R</i>)-7-Bromo-9-nitromethyl-2,3,4,4a,9,9a-hexahydro-1<i>H</i>-xanthen-1-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                 102.849(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3457(7)
_cell_length_b                   5.4662(5)
_cell_length_c                   13.2446(12)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     730.25(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2007)'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6335
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.6732
_exptl_absorpt_correction_T_min  0.2236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.458
_refine_ls_abs_structure_details 'Flack (1983), 1058 Friedel pairs'
_refine_ls_abs_structure_Flack   0.021(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2655
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                1537
_reflns_number_total             2655
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fy2090.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2237827
_cod_database_fobs_code          2237827