Polymorphism of levofloxacin: structure, properties and phase transformation
Wei, Ning; Jia, Lina; Shang, Zeren; Gong, Junbo; Wu, Songgu; Wang, Jingkang; Tang, Weiwei; CrystEngComm 21 (2019) 6196–; doi:10.1039/C9CE00847K

data_7233525
_publ_section_title
;
 Polymorphism of levofloxacin: structure, properties and phase
 transformation
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6196
_journal_paper_doi               10.1039/C9CE00847K
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         '4(C18 H20 F N3 O4)'
_chemical_formula_sum            'C72 H80 F4 N12 O16'
_chemical_formula_weight         1445.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2019-08-10 deposited with the CCDC.    2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.22(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.067(5)
_cell_length_b                   9.2924(19)
_cell_length_c                   34.377(7)
_cell_measurement_reflns_used    7447
_cell_measurement_temperature    128.15
_cell_measurement_theta_max      27.9263
_cell_measurement_theta_min      1.6341
_cell_volume                     8304(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      128.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.1390
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29443
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.188
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear(Rigaku, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 1619 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(10)
_refine_ls_extinction_coef       0.0042(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         14506
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.1109
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1547P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2776
_refine_ls_wR_factor_ref         0.3122
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                8749
_reflns_number_total             14506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00847k2.cif
_cod_data_source_block           shelxl_sq
_cod_depositor_comments
'Adding full bibliography for 7233523--7233525.cif.'
_cod_database_code               7233525
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C11A(H11A), C11C(H11C), C11B(H11B), C11D(H11D)
2.b Secondary CH2 refined with riding coordinates:
 C16A(H16A,H16B), C17A(H17A,H17B), C14A(H14A,H14B), C15A(H15A,H15B), C12A(H12A,
 H12B), C16C(H16C,H16D), C17C(H17C,H17D), C14C(H14C,H14D), C15C(H15C,H15D),
 C12C(H12C,H12D), C16B(H16E,H16F), C17B(H17E,H17F), C14B(H14E,H14F), C15B(H15E,
 H15F), C12B(H12E,H12F), C16D(H16G,H16H), C17D(H17G,H17H), C14D(H14G,H14H),
 C15D(H15G,H15H), C12D(H12G,H12H)
2.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C1A(H1AA), C4C(H4C), C1C(H1CA), C4B(H4B), C1B(H1BA), C4D(H4D),
 C1D(H1DA)
2.d Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C13A(H13A,H13B,H13C), C18C(H18D,H18E,H18F), C13C(H13D,
 H13E,H13F), C18B(H18G,H18H,H18I), C13B(H13G,H13H,H13I), C18D(H18J,H18K,H18L),
 C13D(H13J,H13K,H13L)
2.e Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1C(H1C), O1B(H1B), O1D(H1D)
;
_shelx_res_checksum              85242
_shelx_fab_checksum              75
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'