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_7215690
_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,  0.79(C3 O4),  0.21(C2 O2),  0.21(C O2), O'
_chemical_formula_sum            'C21 H21 F N3 O9'
_chemical_formula_weight         478.41
_chemical_name_common            'Levofloxacin Malonic Acid Hydrate'
_chemical_name_systematic        ?
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 99.282(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.856(3)
_cell_length_b                   6.989(1)
_cell_length_c                   36.502(7)
_cell_measurement_reflns_used    12863
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     4495.6(13)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 0.0000
                 XTD: 45.0000
              2theta: -20.0000
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 90.0000
                 XTD: 45.0000
              2theta: -20.0000
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 180.0000
                 XTD: 45.0000
              2theta: -20.0000
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 270.0000
                 XTD: 45.0000
              2theta: -20.0000

;
_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      0.002649
_diffrn_orient_matrix_UB_12      0.023438
_diffrn_orient_matrix_UB_13      0.027204
_diffrn_orient_matrix_UB_21      -0.056679
_diffrn_orient_matrix_UB_22      -0.000742
_diffrn_orient_matrix_UB_23      -0.003152
_diffrn_orient_matrix_UB_31      0.000738
_diffrn_orient_matrix_UB_32      -0.141150
_diffrn_orient_matrix_UB_33      0.004534
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.1307
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            18183
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_transf_matrix_11  0.002649
_diffrn_reflns_transf_matrix_12  0.023438
_diffrn_reflns_transf_matrix_13  0.027204
_diffrn_reflns_transf_matrix_21  -0.056679
_diffrn_reflns_transf_matrix_22  -0.000742
_diffrn_reflns_transf_matrix_23  -0.003152
_diffrn_reflns_transf_matrix_31  0.000738
_diffrn_reflns_transf_matrix_32  -0.141150
_diffrn_reflns_transf_matrix_33  0.004534
_diffrn_source                   MicroMax003_Mo
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9736
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1829
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.1692P)^2^] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2613
_refine_ls_wR_factor_ref         0.3253
_reflns_number_gt                4725
_reflns_number_total             9736
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ce00263f2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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_sg_symbol_H-M      'C 2'
_cod_database_code               7215690