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_7715379
_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 H74 F4 N16 O16 Tb'
_chemical_formula_sum            'C68 H74 F4 N16 O60 Tb'
_chemical_formula_weight         2310.35
_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                69.465(5)
_cell_angle_beta                 73.894(5)
_cell_angle_gamma                66.707(5)
_cell_formula_units_Z            2
_cell_length_a                   15.0450(9)
_cell_length_b                   18.2526(9)
_cell_length_c                   21.3124(10)
_cell_measurement_reflns_used    11292
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5478
_cell_measurement_theta_min      2.9734
_cell_volume                     4968.1(5)
_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   11.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889   38.0000    0.0000 32

  2 omega -100.00  -74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889 -178.0000  -60.0000 26

  3 omega  -19.00   24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000  120.0000 43

  4 omega   -1.00   66.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389   38.0000 -180.0000 67

  5 omega  -50.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389  -77.0000  -30.0000 101

  6 omega   -7.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389   38.0000   90.0000 101

  7 omega   -2.00   27.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389   57.0000  -30.0000 29

  8 omega   76.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389  178.0000 -120.0000 25

  9 omega   -2.00   76.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389   57.0000 -120.0000 78

 10 omega   35.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389  178.0000    0.0000 66

 11 omega  -52.00   -2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389  -38.0000    0.0000 50

 12 omega  -52.00   53.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       21.5389  -38.0000   90.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0447487000
_diffrn_orient_matrix_UB_12      0.0076637000
_diffrn_orient_matrix_UB_13      -0.0060514000
_diffrn_orient_matrix_UB_21      0.0182237000
_diffrn_orient_matrix_UB_22      -0.0374655000
_diffrn_orient_matrix_UB_23      0.0249526000
_diffrn_orient_matrix_UB_31      0.0192464000
_diffrn_orient_matrix_UB_32      -0.0217255000
_diffrn_orient_matrix_UB_33      -0.0252489000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61871
_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         26.370
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49184
_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    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             2350
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         20290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0800
_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^)+(0.1229P)^2^+7.8069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13164
_reflns_number_total             20290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           1123-czf-xyj-tb
_cod_database_code               7715379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.759
_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:
 N4(H4), N12(H12), N16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C21(H21A,H21B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B), C56(H56A,
 H56B), C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C20(H20), C30(H30), C37(H37), C39(H39), C48(H48), C54(H54),
 C65(H65)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C55(H55A,H55B,H55C), C61(H61A,
 H61B,H61C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89289
_shelx_fab_checksum              8915
_olex2_submission_special_instructions 'No special instructions were received'