Marbofloxacin combined with heavy rare-earth ions makes better candidates for veterinary drugs: crystal structure and bio-activity studies.
Chen, Zhi-Chuan; Liu, Rui-Xue; Xie, Yan-Jie; Hu, Qin; Huang, Fu-Ping; Liu, Yan-Cheng; Liang, Hong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4204–4213; doi:10.1039/d3dt03343k

data_7715378
_publ_section_title
;
 Marbofloxacin combined with heavy rare-earth ions makes better candidates
 for veterinary drugs: crystal structure and bio-activity studies.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4204
_journal_page_last               4213
_journal_paper_doi               10.1039/d3dt03343k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C68 H75 F4 N16 O16 Tm'
_chemical_formula_sum            'C68 H85 F4 N16 O44 Tm'
_chemical_formula_weight         2075.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2023-12-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-18 deposited with the CCDC.	2024-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                69.501(4)
_cell_angle_beta                 74.423(4)
_cell_angle_gamma                67.627(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0283(6)
_cell_length_b                   18.2290(7)
_cell_length_c                   21.2597(9)
_cell_measurement_reflns_used    7655
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5287
_cell_measurement_theta_min      2.9327
_cell_volume                     4982.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -91.00  -63.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -57.0000  -90.0000 56

  2 omega   14.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889   57.0000  120.0000 70

  3 omega   -3.00   24.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000    0.0000 54

  4 omega  -58.00  -31.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -57.0000  -90.0000 54

  5 omega   -9.00   18.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000 -180.0000 54

  6 omega   -2.00   24.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000  -30.0000 52

  7 omega  -46.00    6.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -38.0000   60.0000 104

  8 omega   -1.00   90.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000 -120.0000 182

  9 omega  -12.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   77.0000    0.0000 202

 10 omega    6.00   35.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -57.0000 -120.0000 58

 11 omega   -3.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   55.0000  158.0000 190
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0408242000
_diffrn_orient_matrix_UB_12      0.0363569000
_diffrn_orient_matrix_UB_13      -0.0013214000
_diffrn_orient_matrix_UB_21      -0.0289337000
_diffrn_orient_matrix_UB_22      -0.0235879000
_diffrn_orient_matrix_UB_23      0.0239313000
_diffrn_orient_matrix_UB_31      0.0128981000
_diffrn_orient_matrix_UB_32      0.0064104000
_diffrn_orient_matrix_UB_33      0.0269438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.1275
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46844
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         6.627
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         20351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2593
_refine_ls_wR_factor_ref         0.2947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12433
_reflns_number_total             20351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           1122-czf-xyj-tm-1
_cod_database_code               7715378
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.723
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), N9(H9), N13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C31(H31A,H31B),
  C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C49(H49A,
 H49B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C66(H66A,H66B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C25(H25), C30(H30), C42(H42), C47(H47), C59(H59), C64(H64)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C65(H65A,
 H65B,H65C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54749
_shelx_fab_checksum              74115
_olex2_submission_special_instructions 'No special instructions were received'