#------------------------------------------------------------------------------
#$Date: 2025-04-05 05:56:02 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717470.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717470
loop_
_publ_author_name
'Duffin, Rebekah N.'
'Kelderman, Jenisi T. A.'
'Herdman, Megan E.'
'Andrews, Philip C.'
_publ_section_title
;
 Highly selective organo-gallium hydroxamate mediated inhibition of
 antibiotic resistant Klebsiella pneumoniae.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              649
_journal_page_last               661
_journal_paper_doi               10.1039/d4dt02440k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C6.5 H5 Fe0.17 N0.5 O'
_chemical_formula_sum            'C6.5 H5 Fe0.17 N0.5 O'
_chemical_formula_weight         115.42
_chemical_name_systematic        'Iron tris-N-benzyl-N-phenylhydroxamate'
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-07 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   13.4603(9)
_cell_length_b                   13.4603(9)
_cell_length_c                   10.2309(8)
_cell_measurement_reflns_used    3823
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      28.6680
_cell_measurement_theta_min      3.4920
_cell_volume                     1605.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00   4.00   0.50    6.00    --   -8.90 -27.00-157.00  176
  2  ω    -23.00  25.00   0.50    6.00    --   -8.90 -99.00-120.00   96
  3  ω    -21.00  64.00   0.50    6.00    --   -8.90  38.00  30.00  170
  4  ω      7.00  43.00   0.50    6.00    --    9.22-112.00 116.00   72
  5  ω    -23.00   2.00   0.50    6.00    --    9.22 -99.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295897000
_diffrn_orient_matrix_UB_12      0.0606595000
_diffrn_orient_matrix_UB_13      -0.0055668000
_diffrn_orient_matrix_UB_21      -0.0488377000
_diffrn_orient_matrix_UB_22      0.0009722000
_diffrn_orient_matrix_UB_23      0.0243822000
_diffrn_orient_matrix_UB_31      0.0209618000
_diffrn_orient_matrix_UB_32      0.0049181000
_diffrn_orient_matrix_UB_33      0.0646527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11699
_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         25.960
_diffrn_reflns_theta_min         3.496
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull reddish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       needle
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.737
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1060
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1572P)²+2.5728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                829
_reflns_number_total             1060
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02440k2.cif
_cod_data_source_block           jk_a33_auto
_cod_depositor_comments
'Adding full bibliography for 7717469--7717476.cif.'
_cod_original_formula_sum        'C6.50 H5 Fe0.17 N0.50 O'
_cod_database_code               7717470
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe C H N O'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.884
_diffrn_oxdiff_digest_frames
;
0182e12329f96f5cc2124e0bc8590319d100564fd3f
;
_diffrn_oxdiff_digest_hkl
;
01602dce3652c27348480b1d22cfba2ba4a081
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N1, C1}
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C1) = Uanis(N1)
4. Others
 Fixed Sof: C1(0.5) N1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C3(H3), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.521
_oxdiff_exptl_absorpt_empirical_full_min 0.643
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.2500 0.0319(6) Uani 1 6 d S T P A .
O1 O 0.1416(3) 0.0888(3) 0.3580(3) 0.0341(8) Uani 1 1 d . U . . .
C1 C 0.2171(3) 0.1879(3) 0.3050(3) 0.0298(9) Uani 0.5 1 d . U . A .
C7 C 0.4289(3) 0.3066(3) 0.3120(4) 0.0259(9) Uani 1 1 d . . . . .
H7 H 0.4319 0.3004 0.2198 0.031 Uiso 1 1 calc R . . . .
C2 C 0.3233(3) 0.2543(3) 0.3767(4) 0.0267(9) Uani 1 1 d . . . . .
C6 C 0.5290(3) 0.3674(3) 0.3834(4) 0.0309(10) Uani 1 1 d . . . . .
H6 H 0.6011 0.4032 0.3401 0.037 Uiso 1 1 calc R . . . .
C5 C 0.5239(4) 0.3759(4) 0.5187(4) 0.0361(11) Uani 1 1 d . . . . .
H5 H 0.5926 0.4189 0.5674 0.043 Uiso 1 1 calc R . . . .
C3 C 0.3187(4) 0.2611(4) 0.5118(4) 0.0355(10) Uani 1 1 d . . . . .
H3 H 0.2470 0.2240 0.5559 0.043 Uiso 1 1 calc R . . . .
C4 C 0.4201(4) 0.3225(4) 0.5819(4) 0.0396(11) Uani 1 1 d . . . . .
H4 H 0.4175 0.3276 0.6743 0.048 Uiso 1 1 calc R . . . .
N1 N 0.2171(3) 0.1879(3) 0.3050(3) 0.0298(9) Uani 0.5 1 d . U . A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 92.45(12) 5 4 ?
O1 Fe1 O1 98.36(18) 6 2 ?
O1 Fe1 O1 92.45(12) 3 . ?
O1 Fe1 O1 92.45(12) 5 6 ?
O1 Fe1 O1 98.36(18) 4 . ?
O1 Fe1 O1 92.45(12) 4 6 ?
O1 Fe1 O1 166.06(17) 4 2 ?
O1 Fe1 O1 98.36(18) 5 3 ?
O1 Fe1 O1 92.45(12) 3 2 ?
O1 Fe1 O1 78.38(16) 4 3 ?
O1 Fe1 O1 78.38(16) 6 . ?
O1 Fe1 O1 166.06(17) 6 3 ?
O1 Fe1 O1 92.45(12) 2 . ?
O1 Fe1 O1 78.38(16) 5 2 ?
O1 Fe1 O1 166.06(17) 5 . ?
C1 O1 Fe1 113.5(2) . . ?
O1 C1 C2 116.0(3) . . ?
C1 C1 O1 117.3(2) 6 . ?
C1 C1 C2 126.7(2) 6 . ?
N1 C1 O1 117.3(2) 6 . ?
N1 C1 C1 0.0 6 6 ?
N1 C1 C2 126.7(2) 6 . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C2 119.5(4) . . ?
C7 C2 C1 120.8(4) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C7 120.4(4) . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0(4) . . ?
C5 C6 H6 120.0 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5 119.9 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(4) . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.001(3) 5 ?
Fe1 O1 2.001(3) 2 ?
Fe1 O1 2.001(3) 3 ?
Fe1 O1 2.001(3) 4 ?
Fe1 O1 2.001(3) 6 ?
Fe1 O1 2.001(3) . ?
O1 C1 1.322(5) . ?
C1 C1 1.315(7) 6 ?
C1 C2 1.450(5) . ?
C1 N1 1.315(7) 6 ?
C7 H7 0.9500 . ?
C7 C2 1.398(5) . ?
C7 C6 1.384(6) . ?
C2 C3 1.389(6) . ?
C6 H6 0.9500 . ?
C6 C5 1.394(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.372(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.390(7) . ?
C4 H4 0.9500 . ?
