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_2300732
_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_absolute_configuration unk
_chemical_formula_moiety         'C4 H8 Ca O8, 2(H2 O)'
_chemical_formula_sum            'C4 H12 Ca O10'
_chemical_formula_weight         260.212
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1718(4)
_cell_length_b                   9.5882(3)
_cell_length_c                   10.5502(4)
_cell_measurement_reflns_used    5018
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      37.3900
_cell_measurement_theta_min      2.8450
_cell_volume                     927.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_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_ambient_environment      N~2~
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0756
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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      0.00 110.00   1.00   11.80    --   37.95  19.00 120.00  110
  2  \w     35.00 112.00   1.00   11.80    --   37.95 178.00 -60.00   77
  3  \w     19.00 106.00   1.00   11.80    --   37.95  57.00 -30.00   87
  4  \w     16.00  67.00   1.00   11.80    --   37.95  38.00-150.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324559000
_diffrn_orient_matrix_UB_12      0.0602715000
_diffrn_orient_matrix_UB_13      -0.0268452000
_diffrn_orient_matrix_UB_21      -0.0536466000
_diffrn_orient_matrix_UB_22      -0.0423103000
_diffrn_orient_matrix_UB_23      -0.0294264000
_diffrn_orient_matrix_UB_31      -0.0451460000
_diffrn_orient_matrix_UB_32      0.0069405000
_diffrn_orient_matrix_UB_33      0.0542499000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10505
_diffrn_reflns_point_group_measured_fraction_full 0.9964
_diffrn_reflns_point_group_measured_fraction_max 0.9934
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7c (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_F_000             545.460
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.4214
_refine_diff_density_min         -0.3695
_refine_diff_density_rms         0.0816
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.002(18)
_refine_ls_d_res_high            0.6197
_refine_ls_d_res_low             7.0957
_refine_ls_goodness_of_fit_ref   0.9910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9910
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.985
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                3768
_reflns_number_total             4066
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            timmy_Thakkar.cif
_cod_data_source_block           timmy
_cod_depositor_comments
'Adding full bibliography for 2300730--2300733.cif.'
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               2300732
_chemical_oxdiff_formula         'C10 H10 O2'
_olex2_refinement_description
;
1.a Rotating group:
 O1L(H1La,H1Lb)
;
_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:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2022-11-10_23-38-32
;
_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 1.052
_oxdiff_exptl_absorpt_empirical_full_min 0.964