Crystal structure of 4-methyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane
Said, Musa A.; Al Belewi, Bayan L.; Hughes, David L.; Acta Crystallographica Section E 72 (2016) 1021–1024; doi:10.1107/S2056989016009993

data_2241748
_publ_section_title
;
 Crystal structure of 4-methyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane
;
_journal_coeditor_code           LH5816
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1021
_journal_page_last               1024
_journal_paper_doi               10.1107/S2056989016009993
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C5 H9 O3 P'
_chemical_formula_moiety         'C5 H9 O3 P'
_chemical_formula_structural     P(OCH2)3CMe
_chemical_formula_sum            'C5 H9 O3 P'
_chemical_formula_weight         148.09
_chemical_name_systematic
;
4-Methyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4408(6)
_cell_length_b                   6.2129(5)
_cell_length_c                   10.5052(5)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      32.2821
_cell_measurement_theta_min      3.2724
_cell_volume                     681.45(7)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
ORTEPIII (Johnson, 1976) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      140.0(10)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10309
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.810
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.120
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 605 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1561
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0459P)^2^+0.0252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                1405
_reflns_number_total             1561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5816sup1.cif
_cod_data_source_block           I
_cod_database_code               2241748
_cod_database_fobs_code          2241748
_shelx_hkl_checksum              19337
_shelx_res_checksum              23965