New crystalline salt forms of levofloxacin: conformational analysis and attempts towards the crystal structure prediction of the anhydrous form
Singh, Shiv Shankar; Thakur, Tejender S.; CrystEngComm 16 (2014) 4215–; doi:10.1039/c4ce00263f

data_7215695
_publ_section_title
;
 New crystalline salt forms of levofloxacin: conformational analysis and
 attempts towards the crystal structure prediction of the anhydrous form
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              4215
_journal_paper_doi               10.1039/c4ce00263f
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C18 H21 F N3 O4, C7 H4 N2 O6, C7 H3 N2 O6'
_chemical_formula_sum            'C32 H28 F N7 O16'
_chemical_formula_weight         785.61
_chemical_name_common            'Levofloxacin 3,5-dinitrobenzoate 1:2'
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.910(13)
_cell_angle_beta                 78.135(14)
_cell_angle_gamma                73.833(13)
_cell_formula_units_Z            2
_cell_length_a                   9.135(2)
_cell_length_b                   12.008(3)
_cell_length_c                   16.533(5)
_cell_measurement_reflns_used    2732
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.6
_cell_volume                     1691.1(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_details
;
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 0.0000
                 XTD: 44.9003
              2theta: -19.6699
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 90.0000
                 XTD: 44.9003
              2theta: -19.6699
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 180.0000
                 XTD: 44.9003
              2theta: -19.6699
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 270.0000
                 XTD: 44.9003
              2theta: -19.6699

;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       XPlain
_diffrn_orient_matrix_UB_11      -0.075687
_diffrn_orient_matrix_UB_12      0.078474
_diffrn_orient_matrix_UB_13      0.038368
_diffrn_orient_matrix_UB_21      0.071209
_diffrn_orient_matrix_UB_22      0.046328
_diffrn_orient_matrix_UB_23      -0.020522
_diffrn_orient_matrix_UB_31      -0.021424
_diffrn_orient_matrix_UB_32      -0.007516
_diffrn_orient_matrix_UB_33      -0.058014
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13303
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_transf_matrix_11  -0.075687
_diffrn_reflns_transf_matrix_12  0.078474
_diffrn_reflns_transf_matrix_13  0.038368
_diffrn_reflns_transf_matrix_21  0.071209
_diffrn_reflns_transf_matrix_22  0.046328
_diffrn_reflns_transf_matrix_23  -0.020522
_diffrn_reflns_transf_matrix_31  -0.021424
_diffrn_reflns_transf_matrix_32  -0.007516
_diffrn_reflns_transf_matrix_33  -0.058014
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                6296
_reflns_number_total             7757
_reflns_shell_number_unique_all  6068
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ce00263f2.cif
_cod_data_source_block           Levo35DNBzAcid100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1691.2(8)
_cod_database_code               7215695