Towards stable analogues of inositol phosphates: stereoselective syntheses of (α,α-difluoromethyl)phosphonic acid (DFMPA)-containing cyclohexanes
Butt, Afshan H.; Kariuki, B. M.; Percy, Jonathan M.; Spencer, Neil S.; Chemical Communications  (2002) 682–; doi:10.1039/b200560n

data_7111203
_publ_section_title
;
 Towards stable analogues of inositol phosphates: stereoselective
 syntheses of (\a,\a-difluoromethyl)phosphonic acid (DFMPA)-containing
 cyclohexanes
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              682
_journal_paper_doi               10.1039/b200560n
_journal_year                    2002
_chemical_formula_moiety         'C17 H23 F2 O6 P S'
_chemical_formula_sum            'C17 H23 F2 O6 P S'
_chemical_formula_weight         424.38
_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                 104.776(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9968(6)
_cell_length_b                   16.8039(14)
_cell_length_c                   12.5119(11)
_cell_measurement_reflns_used    2947
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      1.68
_cell_volume                     2032.3(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et. al. 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku R-axis IIc'
_diffrn_measurement_method       'Image plate scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11831
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9193
_exptl_absorpt_correction_T_min  0.8705
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.021(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+1.3904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                2947
_reflns_number_total             3531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200560nsup1.cif
_cod_data_source_block           ahb2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7111203