5,5-Dimethoxy-2-phenoxy-1,3,2-dioxaphosphorinane 2-oxide
Ślepokura, Katarzyna; Lis, Tadeusz; Acta Crystallographica Section C 60 (2004) o315–o317; doi:10.1107/S0108270104006110

data_2013963
_publ_section_title
;
 5,5-Dimethoxy-2-phenoxy-1,3,2-dioxaphosphorinane 2-oxide
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o315
_journal_page_last               o317
_journal_paper_doi               10.1107/S0108270104006110
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C11 H15 O6 P'
_chemical_formula_moiety         'C11 H15 O6 P'
_chemical_formula_sum            'C11 H15 O6 P'
_chemical_formula_weight         274.20
_chemical_name_systematic
;
5,5-dimethoxy-2-phenoxy-1,3,2-dioxaphosphorinan-2-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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.024(2)
_cell_length_b                   10.371(3)
_cell_length_c                   9.917(3)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.41
_cell_measurement_theta_min      3.75
_cell_volume                     614.2(3)
_computing_cell_refinement       'KM-4 CCD Software'
_computing_data_collection
'KM-4 CCD Software (Oxford Diffraction, 1995--2003)'
_computing_data_reduction        'KM-4 CCD Software'
_computing_molecular_graphics
'PLATON (Spek, 2003) and SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'KUMA KM-4 CCD \k-geometry diffractometer'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10758
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         37.41
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(8)
_refine_ls_extinction_coef       0.015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                4232
_reflns_number_total             4632
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1743.cif
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     'P  2yb'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013963