(<i>S</i>)-2-[1-(4-Bromophenyl)-1-hydroxyethyl]-5,5-dimethyl-1,3,2-dioxaphosphinane 2-oxide
Wang, Chubei; Peng, Hao; He, Hongwu; Acta Crystallographica Section E 67 (2011) o1739–; doi:10.1107/S1600536811020587

data_2230833
_publ_section_title
;
 (<i>S</i>)-2-[1-(4-Bromophenyl)-1-hydroxyethyl]-5,5-dimethyl-1,3,2-dioxaphosphinane
 2-oxide
;
_journal_coeditor_code           QK2003
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1739
_journal_paper_doi               10.1107/S1600536811020587
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C13 H18 Br O4 P'
_chemical_formula_moiety         'C13 H18 Br O4 P'
_chemical_formula_sum            'C13 H18 Br O4 P'
_chemical_formula_weight         349.15
_chemical_name_systematic
;
(<i>S</i>)-2-[1-(4-Bromophenyl)-1-hydroxyethyl]-5,5-dimethyl-1,3,2-
dioxaphosphinane 2-oxide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   11.0662(17)
_cell_length_b                   11.3149(18)
_cell_length_c                   11.9609(19)
_cell_measurement_reflns_used    3882
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      2.48
_cell_volume                     1497.7(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
;
PLATON (Spek, 2009) and SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10072
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.453
_refine_ls_abs_structure_details 'Flack (1983), with 1517 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.011(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                2691
_reflns_number_total             3627
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qk2003.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2230833
_cod_database_fobs_code          2230833