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_7718918
_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         'C36 H46 Fe N5 O10, 3(C H2 Cl2)'
_chemical_formula_sum            'C39 H52 Cl6 Fe N5 O10'
_chemical_formula_weight         1019.40
_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             2023-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-02-07 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.120(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5162(2)
_cell_length_b                   13.9489(3)
_cell_length_c                   26.6627(4)
_cell_measurement_reflns_used    14275
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.7560
_cell_measurement_theta_min      3.3430
_cell_volume                     4636.39(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.962
_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    -77.00 -52.00   0.50    9.05    --  -47.31 130.00 -70.00   50
  2  \w   -118.00 -73.00   0.50    9.05    --  -47.31-130.00-142.00   90
  3  \w    -93.00 -67.00   0.50    9.05    --  -47.31-140.00  43.00   52
  4  \w     53.00  96.00   0.50    9.05    --   47.31-130.00-142.00   86
  5  \w     51.00  97.00   0.50    9.05    --   47.31-140.00  43.00   92
  6  \w     -8.00  27.00   0.50    9.05    --  -47.31  19.00 -30.00   70
  7  \w     -9.00  28.00   0.50    9.05    --  -47.31  19.00 -90.00   74
  8  \w    -30.00  23.00   0.50    9.05    --  -47.31  38.00-150.00  106
  9  \w     -6.00  26.00   0.50    9.05    --  -47.31  19.00 120.00   64
 10  \w     -1.00  26.00   0.50    9.05    --  -47.31  19.00-180.00   54
 11  \w   -113.00 -86.00   0.50   36.20    --  -91.75-140.00  43.00   54
 12  \w   -163.00 -77.00   0.50   36.20    --  -91.75 -54.00-114.26  172
 13  \w     46.00 116.00   0.50   36.20    --  113.25-130.00-142.00  140
 14  \w     80.00 123.00   0.50   36.20    --  113.25-140.00  43.00   86
 15  \w    111.00 136.00   0.50   36.20    --  113.25 130.00 -70.00   50
 16  \w     86.00 141.00   0.50   36.20    --  113.25 140.00 102.00  110
 17  \w    120.00 146.00   0.50   36.20    --  113.25  45.00-150.00   52
 18  \w    100.00 127.00   0.50   36.20    --  113.25  15.00 -60.00   54
 19  \w     51.00  77.00   0.50   36.20    --  113.25 -61.00  60.00   52
 20  \w     48.00 108.00   0.50   36.20    --  113.25-125.00  90.00  120
 21  \w     42.00  80.00   0.50   36.20    --  113.25 -61.00 120.00   76
 22  \w    135.00 178.00   0.50   36.20    --  113.25  15.00 -60.00   86
 23  \w    118.00 177.00   0.50   36.20    --  113.25   0.00-120.00  118
 24  \w     42.00  78.00   0.50   36.20    --  113.25 -94.00  30.00   72
 25  \w     49.00 106.00   0.50   36.20    --  113.25 -94.00-120.00  114
 26  \w     56.00 105.00   0.50   36.20    --  113.25-125.00 -60.00   98
 27  \w     46.00  82.00   0.50   36.20    --  113.25 -61.00  90.00   72
 28  \w     80.00 105.00   0.50   36.20    --  113.25 -94.00-180.00   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      -0.1175131000
_diffrn_orient_matrix_UB_12      0.0324190000
_diffrn_orient_matrix_UB_13      -0.0107544000
_diffrn_orient_matrix_UB_21      0.0353988000
_diffrn_orient_matrix_UB_22      0.1055265000
_diffrn_orient_matrix_UB_23      0.0054917000
_diffrn_orient_matrix_UB_31      0.0144966000
_diffrn_orient_matrix_UB_32      0.0041059000
_diffrn_orient_matrix_UB_33      -0.0567216000
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35514
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.430
_diffrn_reflns_theta_min         3.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         9764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0686P)^2^+4.3910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7498
_reflns_number_total             9764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01284h8.cif
_cod_data_source_block           brblh02
_cod_depositor_comments
'Adding full bibliography for 7718917--7718921.cif.'
_cod_database_code               7718918
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C38(H38A,H38B), C37(H37A,H37B), C39(H39A,H39B)
2.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), C34(H34)
2.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), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              55435
_shelx_hkl_checksum              60788
_olex2_submission_original_sample_id brblh02
_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 1.966
_oxdiff_exptl_absorpt_empirical_full_min 0.605