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_7718917
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H27 F Fe N4 O9, C18 H36 K N2 O6'
_chemical_formula_sum            'C48 H63 F Fe K N6 O15'
_chemical_formula_weight         1077.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-05
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9303(3)
_cell_length_b                   12.0821(3)
_cell_length_c                   26.5119(8)
_cell_measurement_reflns_used    27606
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.7720
_cell_measurement_theta_min      1.6800
_cell_volume                     5102.8(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(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 0.901
_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    -62.00  29.00   0.50   47.91    --   11.04 -65.00 -61.00  182
  2  \w    -62.00  29.00   0.50   47.91    --   11.04 -65.00 -61.00  182
  3  \w     38.00  84.00   0.50   47.91    --   11.04-178.00 120.00   92
  4  \w     38.00  84.00   0.50   47.91    --   11.04-178.00-150.00   92
  5  \w     38.00  84.00   0.50   47.91    --   11.04-178.00  90.00   92
  6  \w     38.00  84.00   0.50   47.91    --   11.04-178.00 150.00   92
  7  \w     38.00  84.00   0.50   47.91    --   11.04-178.00 -30.00   92
  8  \w    -83.00   3.00   0.50   47.91    --  -11.98 -56.00 123.00  172
  9  \w     -4.00  21.00   0.50   47.91    --   11.04  57.00  60.00   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      -0.0287559000
_diffrn_orient_matrix_UB_12      -0.0436196000
_diffrn_orient_matrix_UB_13      -0.0047324000
_diffrn_orient_matrix_UB_21      -0.0078778000
_diffrn_orient_matrix_UB_22      -0.0047136000
_diffrn_orient_matrix_UB_23      0.0262462000
_diffrn_orient_matrix_UB_31      -0.0330666000
_diffrn_orient_matrix_UB_32      0.0390088000
_diffrn_orient_matrix_UB_33      -0.0021282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            91122
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         33.052
_diffrn_reflns_theta_min         1.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62783
_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    1.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 4399 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         16344
_refine_ls_number_restraints     634
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0758P)^2^+0.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.788
_reflns_number_gt                12042
_reflns_number_total             16344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01284h8.cif
_cod_data_source_block           brblh07
_cod_depositor_comments
'Adding full bibliography for 7718917--7718921.cif.'
_cod_database_code               7718917
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N5-C31 \\sim N5-C37 \\sim N5-C43 \\sim N6-C36 \\sim N6-C42 \\sim N6-C48 \\sim
N5'-C31' \\sim N5'-C37' ~
 N5'-C43' \\sim N6'-C36' \\sim N6'-C42' \\sim N6'-C48'
 with sigma of 0.02
 C31-C37 \\sim C31-C43 \\sim C37-C43 \\sim C31'-C37' \\sim C31'-C43' \\sim
C37'-C43'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1A
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
4. Rigid body (RIGU) restrains
 N5, C31, C32, O10, C33, C34, O11, C35, C36, C37, C38, O12, C39, C40, O13, C41,
  C42, C43, C44, O14, C45, C46, O15, C47, C48, N6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5', C31', C32', O10', C33', C34', O11', C35', C36', C37', C38', O12', C39',
 C40', O13', C41', C42', C43', C44', O14', C45', C46', O15', C47', C48', N6'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{N5', C37', C38', O12', C39', C40', O13', C41', C42'} sigma for 1-2: 0.02, 1-3:
0.04
{N5', C43', C44', O14', C45', C46', O15', C47', C48'} sigma for 1-2: 0.02, 1-3:
0.04
as in
{N5', C31', C32', O10', C33', C34', O11', C35', C36'}
{N5, C37, C38, O12, C39, C40, O13, C41, C42} sigma for 1-2: 0.02, 1-3: 0.04
{N5, C43, C44, O14, C45, C46, O15, C47, C48} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N5, C31, C32, O10, C33, C34, O11, C35, C36}
6. Others
 Sof(K1')=Sof(N5')=Sof(C31')=Sof(H31C)=Sof(H31D)=Sof(C32')=Sof(H32C)=Sof(H32D)=
 Sof(O10')=Sof(C33')=Sof(H33C)=Sof(H33D)=Sof(C34')=Sof(H34C)=Sof(H34D)=
 Sof(O11')=Sof(C35')=Sof(H35C)=Sof(H35D)=Sof(C36')=Sof(H36C)=Sof(H36D)=
 Sof(C37')=Sof(H37C)=Sof(H37D)=Sof(C38')=Sof(H38C)=Sof(H38D)=Sof(O12')=
 Sof(C39')=Sof(H39C)=Sof(H39D)=Sof(C40')=Sof(H40C)=Sof(H40D)=Sof(O13')=
 Sof(C41')=Sof(H41C)=Sof(H41D)=Sof(C42')=Sof(H42C)=Sof(H42D)=Sof(C43')=
 Sof(H43C)=Sof(H43D)=Sof(C44')=Sof(H44C)=Sof(H44D)=Sof(O14')=Sof(C45')=
 Sof(H45C)=Sof(H45D)=Sof(C46')=Sof(H46C)=Sof(H46D)=Sof(O15')=Sof(C47')=
 Sof(H47C)=Sof(H47D)=Sof(C48')=Sof(H48C)=Sof(H48D)=Sof(N6')=1-FVAR(1)
 Sof(K1)=Sof(N5)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(O10)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(O11)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(O12)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(O13)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(O14)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(O15)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(N6)=FVAR(1)
7.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),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B), C31'(H31C,H31D), C32'(H32C,H32D), C33'(H33C,
 H33D), C34'(H34C,H34D), C35'(H35C,H35D), C36'(H36C,H36D), C37'(H37C,H37D),
 C38'(H38C,H38D), C39'(H39C,H39D), C40'(H40C,H40D), C41'(H41C,H41D), C42'(H42C,
 H42D), C43'(H43C,H43D), C44'(H44C,H44D), C45'(H45C,H45D), C46'(H46C,H46D),
 C47'(H47C,H47D), C48'(H48C,H48D)
7.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              261
_shelx_hkl_checksum              77804
_olex2_submission_original_sample_id brblh07
_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 1.773
_oxdiff_exptl_absorpt_empirical_full_min 0.608