Electron-density analysis of halide...halide through-space magnetic exchange
Scatena, Rebecca; Manson, Zachary E.; Villa, Danielle Y.; Manson, Jamie L.; Allan, David R.; Goddard, Paul A.; Johnson, Roger D.; Journal of Applied Crystallography 58 (2025) 363–373; doi:10.1107/S1600576725000536

data_2300753
_publ_section_title
;
 Electron-density analysis of halide...halide through-space magnetic
 exchange
;
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              363
_journal_page_last               373
_journal_paper_doi               10.1107/S1600576725000536
_journal_volume                  58
_journal_year                    2025
_chemical_formula_moiety         '0.25(C28 H36 I2 N4 Ni)'
_chemical_formula_sum            'C7 H9 I0.5 N Ni0.25'
_chemical_formula_weight         185.282
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_symmetry_Int_Tables_number      126
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-07
_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                   12.0231
_cell_length_b                   12.0231
_cell_length_c                   9.9896
_cell_measurement_reflns_used    98354
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.79873556464521
_cell_measurement_theta_min      2.316174643601404
_cell_volume                     1444.046
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            236805
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9994
_diffrn_reflns_theta_full        24.4148
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         2.32
_diffrn_source                   Synchrotron
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    2.621
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9476121068048929
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.10.2-1-g02720afcd-release
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             731.087
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.3492
_refine_diff_density_min         -0.3652
_refine_diff_density_rms         0.0400
_refine_ls_d_res_high            0.6001
_refine_ls_d_res_low             8.5016
_refine_ls_goodness_of_fit_ref   1.0444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0444
_refine_ls_R_factor_all          0.0082
_refine_ls_R_factor_gt           0.0078
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0052P)^2^+0.2242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0194
_refine_ls_wR_factor_ref         0.0196
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1674
_reflns_number_total             1764
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            NiI2lut4_HAR.cif
_cod_data_source_block           NiI2lut4_HAR
_cod_depositor_comments
'Adding full bibliography for 2300750--2300753.cif.'
_cod_original_cell_volume        1444.045965
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_original_formula_sum        'C7 H9 I0.50 N Ni0.25'
_cod_database_code               2300753
_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
;
_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:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      x2c-TZVP
   CHARGE:         0
   MULTIPLICITY:   3
   RELATIVISTIC:   DKH2
   DATE:           2024-10-07_14-52-01
;
_olex2_submission_special_instructions 'No special instructions were received'