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_1572372
_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         'Fe, 3(C5 H7 O2)'
_chemical_formula_sum            'C15 H21 Fe O6'
_chemical_formula_weight         353.175
_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             2023-12-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1898(3)
_cell_length_b                   13.3897(2)
_cell_length_c                   16.3685(3)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.90
_cell_measurement_theta_min      2.70
_cell_volume                     3329.14(10)
_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      100.04
_diffrn_measured_fraction_theta_full 0.9877
_diffrn_measured_fraction_theta_max 0.9616
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.9877
_diffrn_reflns_Laue_measured_fraction_max 0.9616
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30371
_diffrn_reflns_point_group_measured_fraction_full 0.9877
_diffrn_reflns_point_group_measured_fraction_max 0.9616
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         70.32
_diffrn_reflns_theta_min         5.17
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.493
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1477.249
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.2181
_refine_diff_density_min         -0.2868
_refine_diff_density_rms         0.0427
_refine_ls_d_res_high            0.8187
_refine_ls_d_res_low             8.5610
_refine_ls_extinction_coef       0.00072(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0437
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0437
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+1.2642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2819
_reflns_number_total             3056
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jf5002.cif
_cod_data_source_block           XRD_TAAM-ligand
_cod_database_code               1572372
_shelx_estimated_absorpt_t_min   0.102
_shelx_estimated_absorpt_t_max   0.373
_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:
 C2(H2), C7(H7), C12(H12)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c)
;
_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:       discambMATTS2tsc   v. 2.101
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2023-12-22_10-03-58
;
_olex2_submission_special_instructions 'No special instructions were received'