Refinement of X-ray and electron diffraction crystal structures using analytical Fourier transforms of Slater-type atomic wavefunctions in <i>Olex2</i>.
Kleemiss, Florian; Peyerimhoff, Norbert; Bodensteiner, Michael; Journal of applied crystallography 57 (2024) 161–174; doi:10.1107/S1600576723010981

data_2300731
_publ_section_title
;
 Refinement of X-ray and electron diffraction crystal structures using
 analytical Fourier transforms of Slater-type atomic wavefunctions in
 <i>Olex2</i>.
;
_journal_issue                   'Pt 1'
_journal_name_full               'Journal of applied crystallography'
_journal_page_first              161
_journal_page_last               174
_journal_paper_doi               10.1107/S1600576723010981
_journal_volume                  57
_journal_year                    2024
_chemical_formula_moiety         'C16 H16 Co F6 N4 O4 S2'
_chemical_formula_sum            'C16 H16 Co F6 N4 O4 S2'
_chemical_formula_weight         565.386
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-01-23
_audit_creation_method
;
Olex2 1.5-dev
(compiled Jan 23 2023 09:41:20, GUI svn.r6410)
;
_cell_angle_alpha                82.625(1)
_cell_angle_beta                 81.527(1)
_cell_angle_gamma                81.726(1)
_cell_formula_units_Z            2
_cell_length_a                   7.9999(2)
_cell_length_b                   9.3718(3)
_cell_length_c                   14.7362(5)
_cell_volume                     1074.89(6)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9947
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9947
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11963
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9947
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.077
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             571.716
_refine_diff_density_max         0.5444
_refine_diff_density_min         -0.3576
_refine_diff_density_rms         0.0898
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             14.4877
_refine_ls_goodness_of_fit_ref   1.0443
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0443
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.5487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -11
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4121
_reflns_number_total             4897
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Co110_Thakkar.cif
_cod_data_source_block           Co110
_cod_depositor_comments
'Adding full bibliography for 2300730--2300733.cif.'
_cod_database_code               2300731
_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 and stretchable bonds:
 C22(H22a,H22b), C12(H12a,H12b)
2.b Aromatic/amide H refined with riding coordinates and stretchable bonds:
 C24(H24), C25(H25), C26(H26), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group with stretchable bonds:
 C28(H28a,H28b,H28c), C18(H18a,H18b,H18c)
;
_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:       Thakkar IAM
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2022-11-10_23-39-14
;
_olex2_submission_special_instructions 'No special instructions were received'