On the structure refinement of metal complexes against 3D electron diffraction data using multipolar scattering factors.
Pacoste, Laura; Ignat'ev, Vladislav Mikhailovich; Dominiak, Paulina Maria; Zou, Xiaodong; IUCrJ 11 (2024) –; doi:10.1107/S2052252524006730

data_1572370
_publ_section_title
;
 On the structure refinement of metal complexes against 3D electron
 diffraction data using multipolar scattering factors.
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524006730
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C15 H21 Fe O6'
_chemical_formula_sum            'C15 H21 Fe O6'
_chemical_formula_weight         353.172
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_audit_creation_date             2024-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.35(5)
_cell_length_b                   13.56(7)
_cell_length_c                   16.50(5)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      69.90
_cell_measurement_theta_min      2.70
_cell_volume                     3434(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.9205
_diffrn_measured_fraction_theta_max 0.9186
_diffrn_measurement_device_type
'ThermoFisher Scientific Titan Krios cryo-Transmission Electron Microscope'
_diffrn_measurement_method       \b\
_diffrn_radiation_source         'Electron Schottky Gun'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.01967
_diffrn_reflns_av_R_equivalents  0.2170
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.9205
_diffrn_reflns_Laue_measured_fraction_max 0.9186
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37312
_diffrn_reflns_point_group_measured_fraction_full 0.9205
_diffrn_reflns_point_group_measured_fraction_max 0.9186
_diffrn_reflns_theta_full        0.6634
_diffrn_reflns_theta_max         0.66
_diffrn_reflns_theta_min         0.07
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             542.168
_exptl_crystal_size_max          0.0005
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         1.0921
_refine_diff_density_min         -1.0145
_refine_diff_density_rms         0.2446
_refine_ls_d_res_high            0.8494
_refine_ls_d_res_low             8.6530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0440
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0440
_refine_ls_R_factor_all          0.2101
_refine_ls_R_factor_gt           0.1749
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1483P)^2^+5.0209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4009
_refine_ls_wR_factor_ref         0.4208
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2007
_reflns_number_total             2687
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jf5002.cif
_cod_data_source_block           3DED_TAAM-ligand-FeIII
_cod_original_cell_volume        3434(23)
_cod_database_code               1572370
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C010(H010), C012(H012), C013(H013)
2.b Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C008(H00d,H00e,H00f), C009(H00g,H00h,H00i), C011(H01a,
 H01b,H01c), C014(H01d,H01e,H01f), C015(H01g,H01h,H01i)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       discambMATTS
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2024-02-20_16-19-08
;
_olex2_submission_special_instructions 'No special instructions were received'