2-Hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinan-2-one monohydrate
Samas, Brian; Groendyke, Todd; Blackburn, Anthony C; Godrej, Delara B; Acta Crystallographica Section E 63 (2007) o1276–o1278; doi:10.1107/S1600536807006496

data_2212485
_publ_section_title
;
 2-Hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinan-2-one
 monohydrate
;
_journal_coeditor_code           BT2265
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1276
_journal_page_last               o1278
_journal_paper_doi               10.1107/S1600536807006496
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C11 H15 O4 P, H2 O'
_chemical_formula_moiety         'C11 H15 O4 P, H2 O'
_chemical_formula_sum            'C11 H17 O5 P'
_chemical_formula_weight         260.22
_chemical_melting_point          86.5
_chemical_name_common            '(S)-phencyphos monohydrate'
_chemical_name_systematic
;
2-Hydroxy-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphorinan-2-one monohydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.017(2)
_cell_length_b                   8.219(3)
_cell_length_c                   25.475(10)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.60
_cell_volume                     1259.8(8)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'MERCURY (Bruno <i>et al.</i>,  2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23045
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.8611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.227
_refine_ls_abs_structure_details 'Flack (1983), 1213 friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0515P)^2^+0.1668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                2899
_reflns_number_total             3004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2265.cif
_cod_data_source_block           I
_cod_original_cell_volume        1259.7(8)
_cod_database_code               2212485
_cod_database_fobs_code          2212485