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_2300750
_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         '0.5(F3.0 Sb0.5), C2 H2.25 F0.5 N Ni0.25'
_chemical_formula_sum            'C2 H2.25 F2 N Ni0.25 Sb0.25'
_chemical_formula_weight         123.184
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_symmetry_Int_Tables_number      129
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-08
_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                   9.9063
_cell_length_b                   9.9063
_cell_length_c                   6.4357
_cell_measurement_reflns_used    68780
_cell_measurement_temperature    100
_cell_measurement_theta_max      58.14029906584171
_cell_measurement_theta_min      1.9858890680957035
_cell_volume                     631.566
_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 0.9943
_diffrn_measured_fraction_theta_max 0.9978
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.9943
_diffrn_reflns_Laue_measured_fraction_max 0.9978
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            106972
_diffrn_reflns_point_group_measured_fraction_full 0.9943
_diffrn_reflns_point_group_measured_fraction_max 0.9978
_diffrn_reflns_theta_full        24.4148
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         2.82
_diffrn_source                   Synchrotron
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    3.435
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9442656493771946
_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            blue
_exptl_crystal_density_diffrn    2.591
_exptl_crystal_description       prism
_exptl_crystal_F_000             471.125
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.6197
_refine_diff_density_min         -0.4270
_refine_diff_density_rms         0.0758
_refine_ls_d_res_high            0.6007
_refine_ls_d_res_low             7.0048
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     38
_refine_ls_number_reflns         889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0413
_refine_ls_R_factor_all          0.0118
_refine_ls_R_factor_gt           0.0118
_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^)+(0.0161P)^2^+0.2874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0331
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                887
_reflns_number_total             889
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            NiHF2pyz2SbF6_IAM.cif
_cod_data_source_block           NiHF2pyz2SbF6_IAM
_cod_depositor_comments
'Adding full bibliography for 2300750--2300753.cif.'
_cod_original_cell_volume        631.566002
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_original_formula_sum        'C2 H2.25 F2.0 N Ni0.25 Sb0.25'
_cod_database_code               2300750
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(Sb01)=Sof(F005)=Sof(F006)=0.125*FVAR(2)
 Sof(F004)=0.5*FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C008(H008)
;
_olex2_submission_special_instructions 'No special instructions were received'