Synthesis and enzymatic evaluation of ketose phosphonates: the interplay between mutarotation, monofluorination and acidity
Forget, Stephanie M.; Bhattasali, Debabrata; Hart, V. Catherine; Cameron, T. Stanley; Syvitski, Ray T.; Jakeman, David L.; Chemical Science 3 (2012) 1866–; doi:10.1039/c2sc01077a

data_1515172
_publ_section_title
;
 Synthesis and enzymatic evaluation of ketose phosphonates: the interplay
 between mutarotation, monofluorination and acidity
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              1866
_journal_paper_doi               10.1039/c2sc01077a
_journal_volume                  3
_journal_year                    2012
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C49 H50 F O9 P '
_chemical_formula_sum            'C49 H50 F O9 P'
_chemical_formula_weight         832.90
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.661(3)
_cell_length_b                   27.676(3)
_cell_length_c                   6.5393(7)
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.2
_cell_volume                     4463.2(9)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      296.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.161
_diffrn_measurement_device_type  'Rigaku RAXIS-UNKNOWN'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            32722
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         35.75
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.12
_refine_diff_density_min         -0.13
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 3964 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.09(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.317
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8707
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0310P)^2^+2.9672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2291
_reflns_number_gt                8707
_reflns_number_total             9192
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2sc01077a.txt
_cod_data_source_block           '__Jack1'
_cod_depositor_comments
;
 Changing the values of data items related to the _atom_site_label data item
 (e. g. _geom_bond_atom_site_label_*) to match the _atom_site_label values.

 Antanas Vaitkus,
 2017-01-06
;
_cod_original_cell_volume        4463.1(9)
_cod_original_formula_sum        'C49 H50 F O9 P '
_cod_database_code               1515172