Crystal structure of diethyl 2-(4,5-dihydroxy-2-methyl-sulfanyl-3,4,5,6- tetrahydro-4H-thiopyranyl)difluoro-methylphosphonate, C~11~H~21~F~2~O~5~PS~2~, a thioglycoside analogue bearing a difluorophosphonate group
Pfund, E.; Barbey, C.; Lequeux, T.; Navaza, A.; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 629–630; doi:

data_8101893
_publ_section_title
;
Crystal structure of diethyl 2-(4,5-dihydroxy-2-methyl-sulfanyl-3,4,5,6-
tetrahydro-4H-thiopyranyl)difluoro-methylphosphonate, C~11~H~21~F~2~O~5~PS~2~, 
a thioglycoside analogue bearing a difluorophosphonate group
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              629
_journal_page_last               630
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         'C11 H21 F2 O5 P S2'
_chemical_formula_sum            'C11 H21 F2 O5 P S2'
_chemical_formula_weight         366.37
_chemical_name_systematic
; 
 diethyl 2-(4,5-dihydroxy-2-methylsulfanyl-3,4,5,6-tetrahydro-
 4H-thiopyranyl)-difluoromethylphosphonate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6070(15)
_cell_length_b                   7.7110(15)
_cell_length_c                   26.981(5)
_cell_measurement_temperature    113(2)
_cell_volume                     1570.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4150
_diffrn_reflns_theta_full        23.84
_diffrn_reflns_theta_max         23.84
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+1.7483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                1722
_reflns_number_total             2338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1683.cff
_cod_data_source_block           CB-dedhmsthtpdfmp
_cod_original_sg_symbol_H-M      P12(1)/c1
_cod_database_code               8101893