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_7715376
_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 H77 Dy F4 N16 O16'
_chemical_formula_sum            'C68 H77 Dy F4 N16 O34'
_chemical_formula_weight         1900.95
_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                96.103(4)
_cell_angle_beta                 107.072(4)
_cell_angle_gamma                114.016(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0203(7)
_cell_length_b                   18.0734(8)
_cell_length_c                   21.3637(8)
_cell_measurement_reflns_used    9096
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5244
_cell_measurement_theta_min      2.9640
_cell_volume                     4891.8(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  -85.00  -57.80   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -77.0000  -30.0000 34

  2 omega  -20.00   24.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000  120.0000 55

  3 omega   -8.00   19.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000    0.0000 34

  4 omega  -16.00   12.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -77.0000  -30.0000 35

  5 omega -100.00  -52.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889 -178.0000  150.0000 60

  6 omega  -47.00   44.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -38.0000   60.0000 114

  7 omega   24.00   52.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -77.0000 -120.0000 35

  8 omega    7.00   35.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000  120.0000 35

  9 omega    0.00   91.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000    0.0000 114

 10 omega   31.00   75.00   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827   57.0000 -180.0000 55

 11 omega  -49.00   25.40   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -57.0000 -150.0000 93

 12 omega  -49.00   43.80   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3827  -57.0000    0.0000 116
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0458226000
_diffrn_orient_matrix_UB_12      -0.0043084000
_diffrn_orient_matrix_UB_13      0.0152190000
_diffrn_orient_matrix_UB_21      -0.0247946000
_diffrn_orient_matrix_UB_22      -0.0412074000
_diffrn_orient_matrix_UB_23      -0.0213007000
_diffrn_orient_matrix_UB_31      0.0196072000
_diffrn_orient_matrix_UB_32      0.0161757000
_diffrn_orient_matrix_UB_33      -0.0246451000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.1072
_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            51180
_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         26.371
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57775
_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    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1942
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.336
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         19964
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1061P)^2^+2.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11507
_reflns_number_total             19964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           1122-czf-xyj-dy-1
_cod_original_cell_volume        4891.8(4)
_cod_database_code               7715376
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.755
_reflns_odcompleteness_completeness 99.84
_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. Uiso/Uaniso restraints and constraints
N5 \\sim C19: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
3.a Ternary CH refined with riding coordinates:
 N1(H1), N5(H5), N9(H9), N10(H10), N13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C25(H25A,H25B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C48(H48A,H48B),
  C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C66(H66A,H66B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10A), C15(H15), C27(H27), C32(H32), C42(H42), C47(H47), C59(H59), C64(H64)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C),
 C35(H35A,H35B,H35C), C51(H51A,H51B,H51C), 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              49174
_shelx_fab_checksum              45141
_olex2_submission_special_instructions 'No special instructions were received'