Assessing structure and dynamics of iron complexes supported by tris(amidate)amine ligands.
Huffman, Lucy S. X.; Seshadri, Anjana; Hastings, Christopher D.; Brennessel, William W.; Franco, Ignacio; Barnett, Brandon R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10719–10724; doi:10.1039/d5dt01284h

data_7718919
_publ_section_title
;
 Assessing structure and dynamics of iron complexes supported by
 tris(amidate)amine ligands.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10719
_journal_page_last               10724
_journal_paper_doi               10.1039/d5dt01284h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H27 Fe N4 O9, C H2 Cl2'
_chemical_formula_sum            'C31 H29 Cl2 Fe N4 O9'
_chemical_formula_weight         728.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-07 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.80990(10)
_cell_length_b                   15.73550(10)
_cell_length_c                   16.50520(10)
_cell_measurement_reflns_used    31857
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9480
_cell_measurement_theta_min      3.8760
_cell_volume                     2958.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -119.00 -28.00   0.50    0.50    --  -47.28 -69.00   2.00  182
  2  \w    -67.00  25.00   0.50    0.50    --  -47.28  69.00 135.00  184
  3  \w    -24.00  67.00   0.50    0.50    --   47.28 -69.00   2.00  182
  4  \w     28.00 120.00   0.50    0.50    --   47.28  69.00 135.00  184
  5  \w    -89.00 -19.00   0.50    2.00    --  -91.75  69.00 135.00  140
  6  \w   -163.00 -72.00   0.50    2.00    --  -91.75 -69.00   2.00  182
  7  \w     94.00 178.00   0.50    2.00    --  113.25  69.00 135.00  168
  8  \w     42.00  93.00   0.50    2.00    --  113.25 -69.00   2.00  102
  9  \w    -14.00  28.00   0.50    0.50    --  -47.28  19.00 -60.00   84
 10  \w     34.00  93.00   0.50    0.50    --   47.28-125.00-180.00  118
 11  \w    -72.00 -19.00   0.50    2.00    --  -91.75  61.00 -30.00  106
 12  \w    100.00 178.00   0.50    2.00    --  113.25  15.00  90.00  156
 13  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00 120.00   68
 14  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00  30.00   68
 15  \w     44.00 111.00   0.50    2.00    --  113.25-125.00  30.00  134
 16  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00 150.00   68
 17  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00-180.00   68
 18  \w     44.00 111.00   0.50    2.00    --  113.25-125.00 150.00  134
 19  \w     42.00 106.00   0.50    2.00    --  113.25 -94.00-120.00  128
 20  \w     95.00 178.00   0.50    2.00    --  113.25 125.00-180.00  166
 21  \w     44.00 111.00   0.50    2.00    --  113.25-125.00-150.00  134
 22  \w    100.00 178.00   0.50    2.00    --  113.25  15.00-150.00  156
 23  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00  60.00   68
 24  \w     95.00 178.00   0.50    2.00    --  113.25 125.00-150.00  166
 25  \w     42.00  76.00   0.50    2.00    --  113.25 -61.00 -90.00   68
 26  \w     42.00 106.00   0.50    2.00    --  113.25 -94.00-150.00  128
 27  \w   -119.00 -25.00   0.50    0.50    --  -47.28 -77.00 -90.00  188
 28  \w   -119.00 -32.00   0.50    0.50    --  -47.28 -57.00-180.00  174
 29  \w   -119.00 -32.00   0.50    0.50    --  -47.28 -57.00 -90.00  174
 30  \w   -120.00 -34.00   0.50    0.50    --  -47.28 -38.00  30.00  172
 31  \w   -119.00 -25.00   0.50    0.50    --  -47.28 -77.00 150.00  188
 32  \w     25.00 120.00   0.50    0.50    --   47.28  77.00   0.00  190
 33  \w   -163.00-134.00   0.50    2.00    --  -91.75 -77.00-120.00   58
 34  \w   -163.00 -69.00   0.50    2.00    --  -91.75 -77.00 120.00  188
 35  \w    100.00 178.00   0.50    2.00    --  113.25  15.00  30.00  156
 36  \w    101.00 178.00   0.50    2.00    --  113.25  45.00 -60.00  154
 37  \w    101.00 178.00   0.50    2.00    --  113.25  30.00 -90.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0643411000
_diffrn_orient_matrix_UB_12      0.0268705000
_diffrn_orient_matrix_UB_13      0.0658357000
_diffrn_orient_matrix_UB_21      -0.0630928000
_diffrn_orient_matrix_UB_22      0.0711544000
_diffrn_orient_matrix_UB_23      -0.0589597000
_diffrn_orient_matrix_UB_31      -0.1009342000
_diffrn_orient_matrix_UB_32      -0.0616200000
_diffrn_orient_matrix_UB_33      -0.0393988000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.205
_diffrn_reflns_theta_min         3.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6386
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0347
_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/[\s^2^(Fo^2^)+(0.0510P)^2^+2.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6088
_reflns_number_total             6386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01284h8.cif
_cod_data_source_block           brbbrb20
_cod_depositor_comments
'Adding full bibliography for 7718917--7718921.cif.'
_cod_original_cell_volume        2958.07(4)
_cod_database_code               7718919
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.398
_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
2. Restrained distances
 N1-C1 \\sim N1-C1A
 with sigma of 0.02
 N1-C3 \\sim N1-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4
 with sigma of 0.02
 N1-C5 \\sim N1-C5A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2
 with sigma of 0.02
 C5-C6 \\sim C5A-C6
 with sigma of 0.02
3. Others
 Sof(H2BC)=Sof(H2BD)=Sof(H4BC)=Sof(H4BD)=Sof(H6BC)=Sof(H6BD)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H2AA)=Sof(H2AB)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H6AA)=Sof(H6AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3A,H3B), C4(H4AA,H4AB),
 C4(H4BC,H4BD), C5(H5A,H5B), C6(H6AA,H6AB), C6(H6BC,H6BD), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C1A(H1AA,H1AB), C3A(H3AA,H3AB),
  C5A(H5AA,H5AB)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C16(H16), C18(H18), C20(H20), C23(H23), C25(H25),
 C27(H27)
;
_shelx_res_checksum              96704
_shelx_hkl_checksum              27598
_olex2_submission_original_sample_id brbbrb20
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.802