Ligand solid-solution tuning of magnetic and mechanical properties of the van der Waals metal-organic magnet NiCl<sub>2</sub>(btd)<sub>1-<i>x</i></sub>(bod)<sub><i>x</i></sub>.
Myatt, Emily; Lata, Simrun; Pitcairn, Jem; Daisenberger, Dominik; Kronawitter, Silva M.; Hallweger, Sebastian A.; Kieslich, Gregor; Argent, Stephen P.; Tidey, Jeremiah P.; Cliffe, Matthew J.; Chemical communications (Cambridge, England) 60 (2024) 14427–14430; doi:10.1039/d4cc04214j

data_7133890
_publ_section_title
;
 Ligand solid-solution tuning of magnetic and mechanical properties of the
 van der Waals metal-organic magnet
 NiCl<sub>2</sub>(btd)<sub>1-<i>x</i></sub>(bod)<sub><i>x</i></sub>.
;
_journal_issue                   97
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14427
_journal_page_last               14430
_journal_paper_doi               10.1039/d4cc04214j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C6 H4 Cl2 N2 Ni O'
_chemical_formula_sum            'C6 H4 Cl2 N2 Ni O'
_chemical_formula_weight         249.710
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_Int_Tables_number      13
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-26
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-07-26 deposited with the CCDC.	2024-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.05(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.52(7)
_cell_length_b                   8.96(9)
_cell_length_c                   12.17(8)
_cell_measurement_reflns_used    705
_cell_measurement_temperature    293(5)
_cell_measurement_theta_max      1.0220
_cell_measurement_theta_min      0.0990
_cell_volume                     383(9)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.106a 64-bit (release 01-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac6-020 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.9815
_diffrn_measured_fraction_theta_max 0.9462
_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    -70.00  70.00   0.25    0.25    --    0.00   0.00   0.00  560
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016296000
_diffrn_orient_matrix_UB_12      0.0018558000
_diffrn_orient_matrix_UB_13      -0.0014940000
_diffrn_orient_matrix_UB_21      -0.0025315000
_diffrn_orient_matrix_UB_22      -0.0020708000
_diffrn_orient_matrix_UB_23      -0.0012228000
_diffrn_orient_matrix_UB_31      -0.0064847000
_diffrn_orient_matrix_UB_32      0.0003296000
_diffrn_orient_matrix_UB_33      0.0007318000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02510
_diffrn_reflns_av_R_equivalents  0.1561
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.9815
_diffrn_reflns_Laue_measured_fraction_max 0.9462
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1836
_diffrn_reflns_point_group_measured_fraction_full 0.9815
_diffrn_reflns_point_group_measured_fraction_max 0.9462
_diffrn_reflns_theta_full        0.8629
_diffrn_reflns_theta_max         1.03
_diffrn_reflns_theta_min         0.08
_diffrn_source                   'electron diffractometer'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_description       'irregular, submicron grain'
_exptl_crystal_F_000             79.686
_refine_diff_density_max         1.3754
_refine_diff_density_min         -1.2734
_refine_diff_density_rms         0.3134
_refine_ls_d_res_high            0.6992
_refine_ls_d_res_low             8.9611
_refine_ls_extinction_coef       21403(3253)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.7474
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.7300
_refine_ls_R_factor_all          0.1782
_refine_ls_R_factor_gt           0.1621
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4313
_refine_ls_wR_factor_ref         0.4444
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              4
_reflns_limit_h_min              -4
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                1479
_reflns_number_total             1836
_reflns_threshold_expression     I>=2u(I)
_twin_special_details
;
Component 2 rotated by 179.9636\% 
around [-0.00 -0.00 1.00] (reciprocal) or [0.17 -0.00 0.98] (direct)
;
_cod_data_source_file            d4cc04214j2.cif
_cod_data_source_block           exp_659_S0E0_L07_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7133888--7133890.cif.'
_cod_database_code               7133890
_chemical_oxdiff_formula         'Ni Cl2 C6 H4 N2 O'
_chemical_oxdiff_usercomment
'2024NCS0083, S009256, EMMJCA, Matt Cliffe sample - light grind on holey carbon at RT'
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.567(8)
 0.433(8)
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
;
_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 1.585
_oxdiff_exptl_absorpt_empirical_full_min 0.558
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2