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_7062919
_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 H22 N'
_chemical_formula_sum            'C17 H22 N5 Ni S4'
_chemical_formula_weight         483.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-14 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.018(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5963(6)
_cell_length_b                   18.5456(12)
_cell_length_c                   14.2799(9)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      25.671
_cell_measurement_theta_min      2.919
_cell_volume                     2273.4(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker D8 Venture 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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0404
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.833
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0794 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.7605.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.6071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3514
_reflns_number_total             5216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02943c2.cif
_cod_data_source_block           2271346
_cod_depositor_comments
'Adding full bibliography for 7062919--7062922.cif.'
_cod_database_code               7062919
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N5 \\sim C9 \\sim C11 \\sim C13 \\sim C15 \\sim C9A \\sim C11A \\sim C13A \\sim
C15A \\sim C10 \\sim C12 \\sim C14 \\sim C16 \\sim C10A \\sim C12A \\sim C14A
\\sim C16A \\sim C17 \\sim C17A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Same fragment restrains
{N5, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A} sigma for 1-2: 0.02,
1-3: 0.04
as in
{N5, C9, C10, C11, C12, C13, C14, C15, C16, C17}
4. Others
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
 C9A(H9AA,H9AB), C11A(H11C,H11D), C13A(H13C,H13D), C15A(H15C,H15D), C16A(H16C,
 H16D)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C17(H17A,H17B,
 H17C), C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F),
 C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              37592
_shelx_hkl_checksum              79628
_olex2_submission_special_instructions 'No special instructions were received'