Fosmidomycin analogues with N-hydroxyimidazole and N-hydroxyimidazolone as a chelating unit
Midrier, Camille; Montel, Sonia; Braun, Ralf; Haaf, Klaus; Willms, Lothar; van der Lee, Arie; Volle, Jean-Noël; Pirat, Jean-Luc; Virieux, David; RSC Adv. 4 (2014) 23770–; doi:10.1039/C4RA00757C

data_7235509
_publ_section_title
;
 Fosmidomycin analogues with N-hydroxyimidazole and N-hydroxyimidazolone
 as a chelating unit
;
_journal_issue                   45
_journal_name_full               'RSC Adv.'
_journal_page_first              23770
_journal_paper_doi               10.1039/C4RA00757C
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H13 N2 O5 P'
_chemical_formula_sum            'C8 H13 N2 O5 P'
_chemical_formula_weight         248.17
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 94.575(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.47500(10)
_cell_length_b                   13.8149(2)
_cell_length_c                   8.7194(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    175
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     537.330(19)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10395
_diffrn_reflns_theta_full        25.194
_diffrn_reflns_theta_max         28.959
_diffrn_reflns_theta_min         2.769
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details 'Flack (1983), 1231 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0405
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.0002867
_refine_ls_shift/su_mean         0.0000221
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 138. 178. 65.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0379
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0379
_reflns_limit_h_max              5
_reflns_limit_h_min              -6
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              -11
_reflns_number_gt                2382
_reflns_number_total             2568
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.67
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0262
_oxford_refine_ls_scale          5.84(4)
_oxford_reflns_number_all        2565
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c4ra00757c2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P n '
_cod_database_code               7235509
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE O   (   9,X'S) H   (  91,X'S) 
RIDE N   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;