Halogen substitution effects on crystal structures and magnetic properties in nickel dithiolate molecular crystals
Chen, Xuan-Rong; Chen, Xiao-Yu; Wei, Yi-Ting; Yu, Yan-She; Xu, Jing-Wen; Lai, Jia; Yao, Yu-Feng; New Journal of Chemistry 48 (2024) 1678–1687; doi:10.1039/D3NJ02943C

data_7062920
_publ_section_title
;
 Halogen substitution effects on crystal structures and magnetic
 properties in nickel dithiolate molecular crystals
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1678
_journal_page_last               1687
_journal_paper_doi               10.1039/D3NJ02943C
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C8 N4 Ni S4, C9 H21 Br0.4 I0.6 N'
_chemical_formula_sum            'C17 H21 Br0.4 I0.6 N5 Ni S4'
_chemical_formula_weight         590.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-12 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                73.51(6)
_cell_angle_beta                 86.69(4)
_cell_angle_gamma                82.94(5)
_cell_formula_units_Z            2
_cell_length_a                   7.426(7)
_cell_length_b                   11.935(13)
_cell_length_c                   14.696(15)
_cell_measurement_reflns_used    9374
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.570
_cell_measurement_theta_min      2.765
_cell_volume                     1239(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II 293K'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12181
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         2.765
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1139 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7728.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       needle
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+2.1950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3734
_reflns_number_total             5466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02943c2.cif
_cod_data_source_block           2271349
_cod_depositor_comments
'Adding full bibliography for 7062919--7062922.cif.'
_cod_original_formula_sum        'C17 H21 Br0.40 I0.60 N5 Ni S4'
_cod_database_code               7062920
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.632
_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with polybutenes oil (CAS: 9003-29-6) on a glass slide. A suitable single crystal coated with polybutenes oil as less as possible was sealed in capillary tube filled with argon. The capillary tube with single crystal was mounted on copper pin with solid paraffin.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C16 \\sim I1 \\sim C15 \\sim Br1A \\sim C15A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: H16A(0.6) H16B(0.6) H16C(0.4) H16D(0.4) I1(0.6) C15(0.6) H15A(0.6)
 H15B(0.6) Br1A(0.4) C15A(0.4) H15C(0.4) H15D(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C16(H16C,
 H16D), C15(H15A,H15B), C17(H17A,H17B), C15A(H15C,H15D)
4.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              83783
_shelx_hkl_checksum              3980
_olex2_submission_special_instructions 'No special instructions were received'