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_7718920
_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         'C45 H63 Fe K N4 O15'
_chemical_formula_sum            'C45 H63 Fe K N4 O15'
_chemical_formula_weight         994.94
_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             2025-02-07
_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                 91.7336(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.52253(5)
_cell_length_b                   20.51441(12)
_cell_length_c                   21.90377(12)
_cell_measurement_reflns_used    43543
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.1980
_cell_measurement_theta_min      4.0150
_cell_volume                     4726.06(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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 -69.00   0.50    0.35    --  -47.32-132.00  61.00  100
  2  \w    -91.00 -17.00   0.50    0.35    --  -47.32 132.00 131.00  148
  3  \w   -119.00 -65.00   0.50    0.35    --  -47.32-138.00-114.00  108
  4  \w     42.00 102.00   0.50    0.35    --   47.32-138.00-114.00  120
  5  \w     38.00  99.00   0.50    0.35    --   47.32-132.00  61.00  122
  6  \w   -162.00 -69.00   0.50    1.41    --  -91.75-132.00  61.00  186
  7  \w     42.00 121.00   0.50    1.41    --  113.25-138.00-114.00  158
  8  \w     87.00 175.00   0.50    1.41    --  113.25 138.00 -52.00  176
  9  \w     91.00 178.00   0.50    1.41    --  113.25 132.00 131.00  174
 10  \w     42.00 117.00   0.50    1.41    --  113.25-132.00  61.00  150
 11  \w   -119.00 -32.00   0.50    0.35    --  -47.32 -57.00 150.00  174
 12  \w    -16.00  28.00   0.50    0.35    --  -47.32  19.00  60.00   88
 13  \w    -16.00  28.00   0.50    0.35    --  -47.32  19.00 150.00   88
 14  \w    -16.00  28.00   0.50    0.35    --  -47.32  19.00  30.00   88
 15  \w   -163.00 -74.00   0.50    1.41    --  -91.75 -65.00 137.76  178
 16  \w     42.00 136.00   0.50    1.41    --  113.25 -77.00-120.00  188
 17  \w     42.00 111.00   0.50    1.41    --  113.25-125.00 -30.00  138
 18  \w     42.00 111.00   0.50    1.41    --  113.25-125.00 -90.00  138
 19  \w    101.00 178.00   0.50    1.41    --  113.25  30.00  60.00  154
 20  \w    101.00 178.00   0.50    1.41    --  113.25  45.00 -60.00  154
 21  \w    101.00 178.00   0.50    1.41    --  113.25  30.00 -60.00  154
 22  \w    101.00 178.00   0.50    1.41    --  113.25  30.00 150.00  154
 23  \w     42.00 106.00   0.50    1.41    --  113.25 -94.00-150.00  128
 24  \w     42.00  79.00   0.50    1.41    --  113.25 -61.00 -60.00   74
 25  \w     42.00 106.00   0.50    1.41    --  113.25 -94.00  90.00  128
 26  \w     42.00 106.00   0.50    1.41    --  113.25 -94.00-120.00  128
 27  \w     42.00 106.00   0.50    1.41    --  113.25 -94.00 -30.00  128
 28  \w     42.00  79.00   0.50    1.41    --  113.25 -61.00-180.00   74
 29  \w     91.00 178.00   0.50    1.41    --  113.25  77.00  30.00  174
 30  \w     42.00 106.00   0.50    1.41    --  113.25 -94.00 120.00  128
 31  \w   -119.00 -25.00   0.50    0.35    --  -47.32 -77.00 -90.00  188
 32  \w   -119.00 -25.00   0.50    0.35    --  -47.32 -77.00  30.00  188
 33  \w   -119.00 -32.00   0.50    0.35    --  -47.32 -57.00 -60.00  174
 34  \w    -16.00  28.00   0.50    0.35    --  -47.32  19.00  90.00   88
 35  \w   -119.00 -25.00   0.50    0.35    --  -47.32 -77.00  90.00  188
 36  \w     25.00 120.00   0.50    0.35    --   47.32  77.00-150.00  190
;
_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      -0.0201495000
_diffrn_orient_matrix_UB_12      -0.0083197000
_diffrn_orient_matrix_UB_13      -0.0695224000
_diffrn_orient_matrix_UB_21      0.0008214000
_diffrn_orient_matrix_UB_22      0.0746127000
_diffrn_orient_matrix_UB_23      -0.0079225000
_diffrn_orient_matrix_UB_31      0.1450818000
_diffrn_orient_matrix_UB_32      -0.0015409000
_diffrn_orient_matrix_UB_33      -0.0074608000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80553
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.420
_diffrn_reflns_theta_min         4.038
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         10163
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0409P)^2^+2.6934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9477
_reflns_number_total             10163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01284h8.cif
_cod_data_source_block           brbcdh15
_cod_depositor_comments
'Adding full bibliography for 7718917--7718921.cif.'
_cod_database_code               7718920
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.477
_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
 C39-O13 \\sim C39-O13' \\sim O15-C44 \\sim O15'-C44
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
4. Same fragment restrains
{O13, C40, C41, O14, C42, C43, O15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13', C40', C41', O14', C42', C43', O15'}
{O15, C43, C42, O14, C41, C40, O13} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13, C40, C41, O14, C42, C43, O15}
5. Others
 Sof(H39C)=Sof(H39D)=Sof(H44C)=Sof(H44D)=Sof(O13')=Sof(C40')=Sof(H40C)=
 Sof(H40D)=Sof(C41')=Sof(H41C)=Sof(H41D)=Sof(O14')=Sof(C42')=Sof(H42C)=
 Sof(H42D)=Sof(C43')=Sof(H43C)=Sof(H43D)=Sof(O15')=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(O13)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(O14)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(O15)=Sof(H44A)=Sof(H44B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39(H39C,H39D), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C44(H44C,H44D), 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), C45(H45A,H45B),
  C40'(H40C,H40D), C41'(H41C,H41D), C42'(H42C,H42D), C43'(H43C,H43D)
6.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)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              94307
_shelx_hkl_checksum              7802
_olex2_submission_original_sample_id brbcdh15
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.799