5-Bromo-5-bromomethyl-2-phenoxy-1,3,2-dioxaphosphorinan-2-one
Fun, Hoong-Kun; Chantrapromma, Suchada; Adak, Avijit Kr.; Maity, Annada C.; Goswami, Shyamaprosad; Acta Crystallographica Section E 64 (2008) o2228–o2229; doi:10.1107/S1600536808033631

data_2219907
_publ_section_title
;
 5-Bromo-5-bromomethyl-2-phenoxy-1,3,2-dioxaphosphorinan-2-one
;
_journal_coeditor_code           IS2349
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2228
_journal_page_last               o2229
_journal_paper_doi               10.1107/S1600536808033631
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C10 H11 Br2 O4 P'
_chemical_formula_moiety         'C10 H11 Br2 O4 P'
_chemical_formula_sum            'C10 H11 Br2 O4 P'
_chemical_formula_weight         385.96
_chemical_melting_point_gt       361
_chemical_melting_point_lt       362
_chemical_name_systematic
;
5-Bromo-5-bromomethyl-2-phenoxy-1,3,2-dioxaphosphorinan-2-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.196(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1315(3)
_cell_length_b                   6.30950(10)
_cell_length_c                   16.8901(3)
_cell_measurement_reflns_used    3756
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.41
_cell_volume                     1291.88(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16007
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.397
_exptl_absorpt_correction_T_max  0.7255
_exptl_absorpt_correction_T_min  0.1561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.913
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.3299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                1952
_reflns_number_total             3756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2349.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2219907
_cod_database_fobs_code          2219907