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_7235511
_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_formula_moiety         'C10 H13 N2 O5 P'
_chemical_formula_sum            'C10 H13 N2 O5 P'
_chemical_formula_weight         272.19
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 97.274(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8726(2)
_cell_length_b                   10.7546(3)
_cell_length_c                   14.0957(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    175
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1183.83(6)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.900
_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  0.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11529
_diffrn_reflns_theta_full        25.223
_diffrn_reflns_theta_max         28.992
_diffrn_reflns_theta_min         2.914
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.248
_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    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0002687
_refine_ls_shift/su_mean         0.0000337
_refine_ls_structure_factor_coef F
_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: 
 1.50 -1.07 0.922 -0.400 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0486
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0360
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1751
_reflns_number_total             2834
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      0.92
_oxford_refine_ls_r_factor_ref   0.0358
_oxford_refine_ls_scale          1.0700(18)
_oxford_reflns_number_all        2833
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c4ra00757c2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7235511
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   2,X'S) H   (   3,X'S) 
RIDE C   (   6,X'S) H   (  30,X'S) H   (  31,X'S) 
RIDE C   (   7,X'S) H   (  28,X'S) H   (  29,X'S) 
RIDE N   (   9,X'S) H   (  27,X'S) 
RIDE O   (  13,X'S) H   (  14,X'S) 
RIDE C   (  17,X'S) H   (  22,X'S) 
RIDE C   (  18,X'S) H   (  21,X'S) 
RIDE C   (  19,X'S) H   (  20,X'S) 
RIDE C   (  23,X'S) H   (  24,X'S) H   (  25,X'S) H   (  26,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                                                                             
;