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_7715381
_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 H73 F4 N16 O16 Y'
_chemical_formula_sum            'C68 H73 F4 N16 O16 Y'
_chemical_formula_weight         1535.33
_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     direct
_audit_creation_date             2023-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                95.794(8)
_cell_angle_beta                 107.599(7)
_cell_angle_gamma                113.372(8)
_cell_formula_units_Z            2
_cell_length_a                   15.0715(11)
_cell_length_b                   17.9090(18)
_cell_length_c                   21.361(2)
_cell_measurement_reflns_used    5203
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      28.8210
_cell_measurement_theta_min      2.9525
_cell_volume                     4881.5(9)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -82.00  -29.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4897  -57.0000 -150.0000 106

  2 omega  -86.00  -38.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4897 -178.0000   90.0000 96

  3 omega   17.00   60.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -99.0000 -150.0000 86

  4 omega   14.00   41.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -99.0000    0.0000 54

  5 omega   35.00   62.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  178.0000  150.0000 54

  6 omega   -3.00   38.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397   57.0000  -30.0000 82

  7 omega   57.00   84.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397   77.0000    0.0000 54

  8 omega   -8.00   26.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397   77.0000    0.0000 68

  9 omega  -10.00   89.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397   77.0000   90.0000 198

 10 omega  -20.00    8.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -99.0000 -150.0000 56

 11 omega  -54.00   44.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -38.0000  -60.0000 196

 12 omega  -94.00  -53.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4897  178.0000    0.0000 82
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0077117000
_diffrn_orient_matrix_UB_12      -0.0329416000
_diffrn_orient_matrix_UB_13      0.0127247000
_diffrn_orient_matrix_UB_21      0.0532356000
_diffrn_orient_matrix_UB_22      0.0281670000
_diffrn_orient_matrix_UB_23      0.0189023000
_diffrn_orient_matrix_UB_31      -0.0128412000
_diffrn_orient_matrix_UB_32      0.0104768000
_diffrn_orient_matrix_UB_33      0.0278738000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.2387
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46079
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55847
_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            yellow
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.733
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         17115
_refine_ls_number_restraints     3846
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.2257
_refine_ls_R_factor_gt           0.1238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1583P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3001
_refine_ls_wR_factor_ref         0.3591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5595
_reflns_number_total             17115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           0313-lyc-xyj-y-a
_cod_original_cell_volume        4881.4(8)
_cod_database_code               7715381
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 4A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 4A
2.a Ternary CH refined with riding coordinates:
 N16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B),
 C23(H23A,H23B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B),
  C39(H39A,H39B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,
 H51B), C56(H56A,H56B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B),
 C68(H68A,H68B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C20(H20), C27(H27), C37(H37), C43(H43), C54(H54), C60(H60)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C32(H32A,H32B,
 H32C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C), C55(H55A,H55B,H55C), C66(H66A,
 H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'