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_7715377
_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         'C67.796 H75.776 F4 Lu N16 O16, 0.204(C H3)'
_chemical_formula_sum            'C68 H77 F4 Lu N16 O16'
_chemical_formula_weight         1625.42
_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   mixed
_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                95.281(3)
_cell_angle_beta                 108.174(4)
_cell_angle_gamma                112.712(4)
_cell_formula_units_Z            2
_cell_length_a                   15.1258(6)
_cell_length_b                   17.7696(7)
_cell_length_c                   21.3790(8)
_cell_measurement_reflns_used    20027
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      28.7664
_cell_measurement_theta_min      2.8697
_cell_volume                     4886.0(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      150.00(14)
_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  -13.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686  -99.0000    0.0000 37

  2 omega  -14.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686  -99.0000 -180.0000 34

  3 omega   14.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623   57.0000  -30.0000 41

  4 omega  -53.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623  -38.0000   30.0000 100

  5 omega   11.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623   57.0000  150.0000 71

  6 omega    5.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623   57.0000    0.0000 76

  7 omega   11.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623   38.0000 -120.0000 46

  8 omega   35.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.3623 -178.0000  -30.0000 60

  9 omega  -96.00  -71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686 -178.0000 -150.0000 25

 10 omega  -96.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2686 -178.0000   60.0000 61
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0167628000
_diffrn_orient_matrix_UB_12      0.0334161000
_diffrn_orient_matrix_UB_13      0.0282166000
_diffrn_orient_matrix_UB_21      0.0408657000
_diffrn_orient_matrix_UB_22      0.0250681000
_diffrn_orient_matrix_UB_23      -0.0094465000
_diffrn_orient_matrix_UB_31      -0.0326258000
_diffrn_orient_matrix_UB_32      0.0156481000
_diffrn_orient_matrix_UB_33      -0.0202507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0571
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48286
_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         25.681
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63439
_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    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         18535
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0554P)^2^+2.0682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15414
_reflns_number_total             18535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           0103-lyc-xyj-7
_cod_database_code               7715377
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.739
_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 C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C8
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(N2) = Uanis(N2A)
4. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(N2A)=1-FVAR(1)
 Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(H9AA)=Sof(H9AB)=
 Sof(N2)=Sof(H2)=FVAR(1)
5.a Riding coordinates:
 C69(H69A,H69B,H69C)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N12(H12), N16(H16)
5.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B),
 C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B),
  C29(H29A,H29B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,
 H44B), C46(H46A,H46B), C57(H57A,H57B), C58(H58A,H58B), C60(H60A,H60B),
 C61(H61A,H61B), C63(H63A,H63B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C20(H20), C32(H32), C37(H37), C49(H49), C54(H54), C66(H66)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C30(H30A,H30B,
 H30C), C42(H42A,H42B,H42C), C47(H47A,H47B,H47C), C59(H59A,H59B,H59C), C64(H64A,
 H64B,H64C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87235
_shelx_fab_checksum              2798
_olex2_submission_special_instructions 'No special instructions were received'