7-[(5,5-Dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl)oxy]-4-methyl-2<i>H</i>-chromen-2-one
Zhao, Yan-Ru; Hou, Xu-Feng; Xu, Zhi-Hong; Acta Crystallographica Section E 68 (2012) o1924–; doi:10.1107/S1600536812023513

data_2234976
_publ_section_title
;
 7-[(5,5-Dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl)oxy]-4-methyl-2<i>H</i>-chromen-2-one
;
_journal_coeditor_code           EZ2291
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1924
_journal_paper_doi               10.1107/S1600536812023513
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C15 H17 O6 P'
_chemical_formula_moiety         'C15 H17 O6 P'
_chemical_formula_sum            'C15 H17 O6 P'
_chemical_formula_weight         324.26
_chemical_name_systematic
;
7-[(5,5-Dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl)oxy]-4-methyl-2<i>H</i>-
chromen-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                 102.596(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.309(4)
_cell_length_b                   17.010(9)
_cell_length_c                   25.507(13)
_cell_measurement_reflns_used    1226
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.39
_cell_volume                     3095(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16892
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.9566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.233
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                2926
_reflns_number_total             6065
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ez2291.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234976
_cod_database_fobs_code          2234976