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_7215693
_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         '6(C18 H21 F N3 O4), 3(C2 O4), 11(O)'
_chemical_formula_sum            'C114 H126 F6 N18 O47'
_chemical_formula_weight         2614.33
_chemical_name_systematic        ?
_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                67.254(8)
_cell_angle_beta                 86.503(12)
_cell_angle_gamma                77.145(11)
_cell_formula_units_Z            1
_cell_length_a                   9.984(2)
_cell_length_b                   17.199(3)
_cell_length_c                   19.058(4)
_cell_measurement_reflns_used    4294
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.1
_cell_volume                     2941.2(10)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_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: 44.9735
              2theta: -19.6234
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: 44.9735
              2theta: -19.6234
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: 44.9735
              2theta: -19.6234
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: 44.9735
              2theta: -19.6234

;
_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      0.095410
_diffrn_orient_matrix_UB_12      -0.032654
_diffrn_orient_matrix_UB_13      -0.019822
_diffrn_orient_matrix_UB_21      0.010324
_diffrn_orient_matrix_UB_22      0.057910
_diffrn_orient_matrix_UB_23      0.026634
_diffrn_orient_matrix_UB_31      -0.004399
_diffrn_orient_matrix_UB_32      -0.041398
_diffrn_orient_matrix_UB_33      0.038813
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23164
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_transf_matrix_11  0.095410
_diffrn_reflns_transf_matrix_12  -0.032654
_diffrn_reflns_transf_matrix_13  -0.019822
_diffrn_reflns_transf_matrix_21  0.010324
_diffrn_reflns_transf_matrix_22  0.057910
_diffrn_reflns_transf_matrix_23  0.026634
_diffrn_reflns_transf_matrix_31  -0.004399
_diffrn_reflns_transf_matrix_32  -0.041398
_diffrn_reflns_transf_matrix_33  0.038813
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1736
_refine_ls_number_reflns         13485
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0714P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                11244
_reflns_number_total             13485
_reflns_shell_number_unique_all  13485
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ce00263f2.cif
_cod_data_source_block           LevoOxalicAcid100K
_cod_depositor_comments
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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        2941.3(10)
_cod_database_code               7215693