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_7715375
_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         'C72 H75 Er F4 N12 O16'
_chemical_formula_sum            'C72 H73 Er F4 N12 O16'
_chemical_formula_weight         1605.68
_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     dual
_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                103.479(3)
_cell_angle_beta                 108.075(4)
_cell_angle_gamma                93.355(4)
_cell_formula_units_Z            2
_cell_length_a                   13.9930(7)
_cell_length_b                   15.1576(7)
_cell_length_c                   20.8128(6)
_cell_measurement_reflns_used    5351
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9291
_cell_measurement_theta_min      2.9799
_cell_volume                     4039.9(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -6.00   21.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3334   98.0000 -145.0000 54

  2 omega  -59.00  -32.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3334   98.0000 -145.0000 54

  3 omega    9.00   53.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -98.0000  108.0000 88

  4 omega  -35.00   49.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3334   57.0000   30.0000 168

  5 omega  -20.00   25.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3334  -99.0000 -150.0000 90

  6 omega  -54.00   44.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -38.0000   90.0000 196

  7 omega  -50.00   44.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -38.0000 -180.0000 188

  8 omega  -20.00   61.00   0.5000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7397  -99.0000  -34.0000 162
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0473112000
_diffrn_orient_matrix_UB_12      -0.0112938000
_diffrn_orient_matrix_UB_13      -0.0027538000
_diffrn_orient_matrix_UB_21      0.0205433000
_diffrn_orient_matrix_UB_22      0.0471058000
_diffrn_orient_matrix_UB_23      0.0124939000
_diffrn_orient_matrix_UB_31      0.0155199000
_diffrn_orient_matrix_UB_32      -0.0040464000
_diffrn_orient_matrix_UB_33      0.0349047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.1538
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36977
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.986
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70829
_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    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.517
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         16445
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0905P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9800
_reflns_number_total             16445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03343k2.cif
_cod_data_source_block           0720-lyc-xyj050729aaa
_cod_database_code               7715375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.664
_reflns_odcompleteness_completeness 99.44
_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
 N4-C73
 1.45 with sigma of 0.02
 C73-C25 = C73-C02X
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N4A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) = Uanis(N4A)
Uanis(C23) = Uanis(C02X)
Uanis(C24) = Uanis(C73)
4. Others
 Sof(C02X)=Sof(C02{)=Sof(H02{)=Sof(H25C)=Sof(H25D)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(H73C)=Sof(N4)=1-FVAR(1)
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(H25A)=
 Sof(H25B)=Sof(N4A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N3(H3A), N6(H6), N9(H9), N12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B),
 C25(H25A,H25B), C25(H25C,H25D), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B),
  C36(H36A,H36B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,
 H53B), C54(H54A,H54B), C66(H66A,H66B), C67(H67A,H67B), C70(H70A,H70B),
 C71(H71A,H71B)
5.c Aromatic/amide H refined with riding coordinates:
 C02{(H02{), C3(H3), C10(H10), C22(H22), C29(H29), C39(H39), C44(H44),
 C58(H58), C62(H62), C68(H68)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C34(H34A,H34B,
 H34C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C69(H69A,H69B,H69C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98271
_shelx_fab_checksum              19371
_olex2_submission_special_instructions 'No special instructions were received'