5,5-Dimethyl-2-methylseleno-1,3,2-dioxaphosphorinan-2-one
Cholewinski, Grzegorz; Chojnacki, Jaroslaw; Pikies, Jerzy; Rachon, Janusz; Acta Crystallographica Section E 66 (2010) o856–; doi:10.1107/S1600536810008330

data_2225509
_publ_section_title
;
 5,5-Dimethyl-2-methylseleno-1,3,2-dioxaphosphorinan-2-one
;
_journal_coeditor_code           DN2544
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o856
_journal_paper_doi               10.1107/S1600536810008330
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C6 H13 O3 P1 Se1'
_chemical_formula_moiety         'C6 H13 O3 P1 Se1'
_chemical_formula_sum            'C6 H13 O3 P Se'
_chemical_formula_weight         243.09
_chemical_melting_point          364.0(10)
_chemical_name_systematic
;
5,5-Dimethyl-2-methylseleno-1,3,2-dioxaphosphorinan-2-one
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.078(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2252(4)
_cell_length_b                   9.4842(4)
_cell_length_c                   11.4160(6)
_cell_measurement_reflns_used    3018
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5921
_cell_measurement_theta_min      3.0999
_cell_volume                     980.22(8)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material
;
WinGX (Farrugia, 1999), PLATON (Spek, 2009) and publCIF (Westrip,
2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Oxford Diffraction KM-4-CCD'
_diffrn_measurement_method       '\w scans, 0.8\% width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Mo Ka radiation'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3146
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  0.372
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2009), using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needless
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.409
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.326
_refine_ls_abs_structure_details 'Flack (1983), 189 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1238
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.065
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                1214
_reflns_number_total             1238
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            dn2544.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2225509
_cod_database_fobs_code          2225509