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_7718921
_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         'C33 H39 F Fe N4 O9, C16 H36 N'
_chemical_formula_sum            'C49 H75 F Fe N5 O9'
_chemical_formula_weight         952.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-12-16
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_audit_update_record
;
2025-02-07 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9191(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0306(4)
_cell_length_b                   23.0834(3)
_cell_length_c                   15.06554(17)
_cell_measurement_reflns_used    16979
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      69.7920
_cell_measurement_theta_min      2.4640
_cell_volume                     9973.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-015 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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   -121.00 -35.00   0.50   16.00    --  -47.28 -29.00 -86.00  172
  2  \w     -2.00  47.00   0.50   16.00    --   47.28 -29.00 -86.00   98
  3  \w     -2.00  47.00   0.50   16.00    --   47.28 -29.00 -86.00   98
  4  \w     58.00 102.00   0.50   16.00    --   47.28  29.00  74.00   88
  5  \w   -117.00 -79.00   0.50   32.00    --  -91.75 -29.00 -86.00   76
  6  \w    110.00 168.00   0.50   32.00    --  108.47  29.00  74.00  116
  7  \w    -84.00 -40.00   0.50   16.00    --  -47.28 125.00-150.00   88
  8  \w    -21.00  27.00   0.50   16.00    --  -47.28  29.00  74.00   96
  9  \w     -2.00  28.00   0.50   16.00    --  -47.28  19.00 -90.00   60
 10  \w    -10.00  23.00   0.50   16.00    --  -47.28  19.00-150.00   66
 11  \w    -56.00 -30.00   0.50   32.00    --  -91.75  61.00 150.00   52
 12  \w    -55.00 -20.00   0.50   32.00    --  -91.75  61.00 -90.00   70
 13  \w    -54.00 -27.00   0.50   32.00    --  -91.75  61.00-180.00   54
 14  \w    -52.00 -20.00   0.50   32.00    --  -91.75  61.00-150.00   64
 15  \w    -54.00 -20.00   0.50   32.00    --  -91.75  61.00-120.00   68
 16  \w    -53.00 -27.00   0.50   32.00    --  -91.75  61.00  60.00   52
 17  \w     49.00  75.00   0.50   32.00    --  108.47-125.00-180.00   52
 18  \w     47.00  84.00   0.50   32.00    --  108.47 -61.00 -60.00   74
 19  \w     37.00  64.00   0.50   32.00    --  108.47 -45.00 -90.00   54
 20  \w     82.00 111.00   0.50   32.00    --  108.47-125.00-180.00   58
 21  \w     37.00  63.00   0.50   32.00    --  108.47 -45.00 150.00   52
 22  \w     42.00  84.00   0.50   32.00    --  108.47 -61.00 120.00   84
 23  \w     39.00 111.00   0.50   32.00    --  108.47-125.00 150.00  144
 24  \w     37.00  62.00   0.50   32.00    --  108.47 -45.00-180.00   50
 25  \w     37.00  62.00   0.50   32.00    --  108.47 -45.00 -30.00   50
 26  \w     37.00  62.00   0.50   32.00    --  108.47 -45.00   0.00   50
 27  \w     36.00 101.00   0.50   32.00    --  108.47 -77.00 -60.00  130
 28  \w     38.00  64.00   0.50   32.00    --  108.47 -45.00-120.00   52
 29  \w     39.00  66.00   0.50   32.00    --  108.47 -61.00   0.00   54
 30  \w     37.00  62.00   0.50   32.00    --  108.47 -61.00 -30.00   50
;
_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      0.0033192000
_diffrn_orient_matrix_UB_12      0.0254241000
_diffrn_orient_matrix_UB_13      -0.0933471000
_diffrn_orient_matrix_UB_21      0.0536104000
_diffrn_orient_matrix_UB_22      -0.0030070000
_diffrn_orient_matrix_UB_23      0.0209993000
_diffrn_orient_matrix_UB_31      -0.0012339000
_diffrn_orient_matrix_UB_32      -0.0616206000
_diffrn_orient_matrix_UB_33      -0.0395010000
_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  0.0686
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75017
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.170
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       needle
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1540
_refine_ls_number_reflns         18819
_refine_ls_number_restraints     659
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+1.1386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12855
_reflns_number_total             18819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01284h8.cif
_cod_data_source_block           brblh06
_cod_depositor_comments
'Adding full bibliography for 7718917--7718921.cif.'
_cod_database_code               7718921
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.322
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-O5 \\sim C12-O5A
 with sigma of 0.02
 O5-C15 \\sim O5A-C15A
 with sigma of 0.02
 C12-C15 \\sim C12-C15A
 with sigma of 0.04
 C58-C59 \\sim C58-C59A
 with sigma of 0.02
 O17-C65 \\sim O18-C66 \\sim O17A-C65A \\sim O18A-C66A \\sim O14-C48 \\sim
O14A-C48A
 with sigma of 0.02
 C61-O17 \\sim C63-O18 \\sim C61A-O17A \\sim C63A-O18A \\sim C45-O14 \\sim
C45-O14A
 with sigma of 0.02
 C61-C65 \\sim C63-C66 \\sim C61A-C65A \\sim C63A-C66A \\sim C45-C48 \\sim
C45-C48A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
All non-hydrogen atoms have similar U: within 0.4A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 0.4A
Uanis(C97) \\sim Ueq, Uanis(C97A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C59A) \\sim Ueq, Uanis(C65A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C12, O5A, C15A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N10A, C91, C92, C93, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10A, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10A, C91A, C92A, C93A, C94A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10A, C95A, C96A, C97A, C98A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C75, C76A, C77A, C78A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C59, C60, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C59A, C60A, C61A, C62A, C63A, C64A}
{C79, C80A, C81A, C82A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C79, C80, C81, C82}
{C59, C64, C63, C62, C61, C60} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C59, C60, C61, C62, C63, C64}
{C75, C76A, C77A, C78A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C75, C76, C77, C78}
{N10, C87, C88, C89, C90} sigma for 1-2: 0.02, 1-3: 0.04
{N10, C91, C92, C93, C94} sigma for 1-2: 0.02, 1-3: 0.04
{N10, C95, C96, C97, C98} sigma for 1-2: 0.02, 1-3: 0.04
{N10A, C83A, C84A, C85A, C86A} sigma for 1-2: 0.02, 1-3: 0.04
{N10A, C87A, C88A, C89A, C90A} sigma for 1-2: 0.02, 1-3: 0.04
{N10A, C91A, C92A, C93A, C94A} sigma for 1-2: 0.02, 1-3: 0.04
{N10A, C95A, C96A, C97A, C98A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N10, C83, C84, C85, C86}
6. Others
 Sof(O17A)=Sof(O18A)=Sof(C59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(C62A)=
 Sof(H62A)=Sof(C63A)=Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65D)=Sof(H65E)=
 Sof(H65F)=Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=1-FVAR(1)
 Sof(O17)=Sof(O18)=Sof(C59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(C62)=Sof(H62)=
 Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=
 Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(1)
 Sof(O14A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(O14)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(2)
 Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)=Sof(C77A)=Sof(H77C)=
 Sof(H77D)=Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(3)
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(3)
 Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=Sof(C81A)=Sof(H81C)=
 Sof(H81D)=Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=1-FVAR(4)
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C81)=Sof(H81A)=Sof(H81B)=
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(4)
 Sof(N10A)=Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=
 Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C85A)=
 Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86D)=Sof(H86E)=Sof(H86F)=Sof(C91A)=
 Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(H93C)=
 Sof(H93D)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C95A)=Sof(H95C)=
 Sof(H95D)=Sof(C96A)=Sof(H96C)=Sof(H96D)=Sof(C97A)=Sof(H97C)=Sof(H97D)=
 Sof(C98A)=Sof(H98D)=Sof(H98E)=Sof(H98F)=1-FVAR(5)
 Sof(N10)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=
 Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C87)=Sof(H87A)=
 Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=
 Sof(H90A)=Sof(H90B)=Sof(H90C)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=
 Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=
 Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=FVAR(5)
 Sof(O5A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(6)
 Sof(O5)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(6)
7.a Secondary CH2 refined with riding coordinates:
 C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C87(H87A,H87B), C88(H88A,
 H88B), C89(H89A,H89B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B),
 C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C87A(H87C,H87D), C88A(H88C,
 H88D), C89A(H89C,H89D), C83A(H83C,H83D), C84A(H84C,H84D), C85A(H85C,H85D),
 C91A(H91C,H91D), C92A(H92C,H92D), C93A(H93C,H93D), C95A(H95C,H95D), C96A(H96C,
 H96D), C97A(H97C,H97D), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C67(H67A,H67B), C68(H68A,H68B),
  C69(H69A,H69B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C75(H75A,
 H75B), C75(H75C,H75D), C76(H76A,H76B), C77(H77A,H77B), C79(H79A,H79B),
 C79(H79C,H79D), C80(H80A,H80B), C81(H81A,H81B), C76A(H76C,H76D), C77A(H77C,
 H77D), C80A(H80C,H80D), C81A(H81C,H81D)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C18(H18), C20(H20), C22(H22), C27(H27), C29(H29),
 C31(H31), C42(H42), C44(H44), C46(H46), C51(H51), C53(H53), C55(H55), C60(H60),
  C62(H62), C64(H64), C60A(H60A), C62A(H62A), C64A(H64A)
7.c Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C90(H90A,H90B,H90C), C94(H94A,H94B,H94C), C98(H98A,H98B,
 H98C), C90A(H90D,H90E,H90F), C86A(H86D,H86E,H86F), C94A(H94D,H94E,H94F),
 C98A(H98D,H98E,H98F), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C47(H47A,
 H47B,H47C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C70(H70A,H70B,H70C),
 C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C48(H48A,H48B,
 H48C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C48A(H48D,H48E,H48F),
 C65A(H65D,H65E,H65F), C66A(H66D,H66E,H66F), C78A(H78D,H78E,H78F), C82A(H82D,
 H82E,H82F), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              87223
_shelx_hkl_checksum              11666
_olex2_submission_original_sample_id brblh06
_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 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.426