2-[(4-Chlorophenyl)(hydroxy)methyl]-5,5-dimethyl-1,3,2-dioxaphosphinan-2-one
Wang, Chubei; Peng, Hao; He, Hongwu; Acta Crystallographica Section E 67 (2011) o926–; doi:10.1107/S1600536811008944

data_2229876
_publ_section_title
;
 2-[(4-Chlorophenyl)(hydroxy)methyl]-5,5-dimethyl-1,3,2-dioxaphosphinan-2-one
;
_journal_coeditor_code           WN2424
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o926
_journal_paper_doi               10.1107/S1600536811008944
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C12 H16 Cl O4 P'
_chemical_formula_moiety         'C12 H16 Cl O4 P'
_chemical_formula_sum            'C12 H16 Cl O4 P'
_chemical_formula_weight         290.67
_chemical_name_systematic
;
2-[(4-Chlorophenyl)(hydroxy)methyl]-5,5-dimethyl-1,3,2-dioxaphosphinan-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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.6300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8965(11)
_cell_length_b                   9.4449(8)
_cell_length_c                   11.6425(10)
_cell_measurement_reflns_used    4935
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.68
_cell_volume                     1402.1(2)
_computing_cell_refinement       '<i>SAINT-Plus</i> (Bruker, 2001)'
_computing_data_collection       '<i>SMART</i> (Bruker, 2001)'
_computing_data_reduction        '<i>SAINT-Plus</i> (Bruker, 2001)'
_computing_molecular_graphics    '<i>PLATON</i> (Spek, 2009)'
_computing_publication_material  '<i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10123
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0581P)^2^+0.7742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                3141
_reflns_number_total             3463
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wn2424.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229876
_cod_database_fobs_code          2229876