Comparative spectroscopic and theoretical studies on the conformation of some α-diethoxyphosphoryl carbonyl compounds and their α-ethylsulfonyl analogues 1
Olivato, Paulo R.; Filho, Rubens Ruiz; Zukerman-Schpector, Julio; Dal Colle, Maurizio; Distefano, Giuseppe; Journal of the Chemical Society, Perkin Transactions 2  (2001) 97–; doi:10.1039/b005501h

data_7213414
_publ_section_title
;
 Comparative spectroscopic and theoretical studies on the conformation of
 some \a-diethoxyphosphoryl carbonyl compounds and their \a-ethylsulfonyl
 analogues&#x200A;1
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              97
_journal_paper_doi               10.1039/b005501h
_journal_year                    2001
_chemical_formula_sum            'C6 H15 O5 P S'
_chemical_formula_weight         230.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 108.46(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.074(1)
_cell_length_b                   8.3570(9)
_cell_length_c                   13.991(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      9.23
_cell_volume                     1117.3(2)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software'
_computing_data_reduction        MolEN
_computing_molecular_graphics    ZORTEP
_computing_publication_material  'PARST95, WinGX'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CAD4 Mach3'
_diffrn_measurement_method       \t/2\t
_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  0.0083
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2040
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        -1.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0743P)^2^+0.6371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                1463
_reflns_number_total             1958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005501hsup1.cif
_cod_data_source_block           s97
_cod_database_code               7213414