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_2300752
_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 Cl2 N4 Ni)'
_chemical_formula_sum            'C7 H9 Cl0.5 N Ni0.25'
_chemical_formula_weight         139.556
_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
_audit_creation_date             2024-09-20
_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                   11.5371(1)
_cell_length_b                   11.5371(1)
_cell_length_c                   10.5513(2)
_cell_measurement_reflns_used    30943
_cell_measurement_temperature    100
_cell_measurement_theta_max      52.63877792848432
_cell_measurement_theta_min      2.4127722009639534
_cell_volume                     1404.43(3)
_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
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            109001
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        24.4148
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         2.42
_diffrn_source                   Synchrotron
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9219629582902182
_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            white
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             589.497
_exptl_crystal_size_max          0.008
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.5596
_refine_diff_density_min         -0.5456
_refine_diff_density_rms         0.0597
_refine_ls_d_res_high            0.6001
_refine_ls_d_res_low             8.1580
_refine_ls_goodness_of_fit_ref   1.0041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0041
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1450
_reflns_number_total             1711
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            NiCl2lut4_IAM.cif
_cod_data_source_block           NiCl2lut4_IAM
_cod_depositor_comments
'Adding full bibliography for 2300750--2300753.cif.'
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_original_formula_sum        'C7 H9 Cl0.50 N Ni0.25'
_cod_database_code               2300752
_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:
 C004(H004), C006(H006)
2.b Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c)
;
_olex2_submission_special_instructions 'No special instructions were received'