Magnetic coupling between Fe(NO) spin probe ligands through diamagnetic Ni<sup>II</sup>, Pd<sup>II</sup> and Pt<sup>II</sup> tetrathiolate bridges.
Quiroz, Manuel; Lockart, Molly M.; Xue, Shan; Jones, Dakota; Guo, Yisong; Pierce, Brad S.; Dunbar, Kim R.; Hall, Michael B.; Darensbourg, Marcetta Y.; Chemical science 14 (2023) 9167–9174; doi:10.1039/d3sc01546g

data_1569666
_publ_section_title
;
 Magnetic coupling between Fe(NO) spin probe ligands through diamagnetic
 Ni<sup>II</sup>, Pd<sup>II</sup> and Pt<sup>II</sup> tetrathiolate
 bridges.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              9167
_journal_page_last               9174
_journal_paper_doi               10.1039/d3sc01546g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'2(C9 H18 Fe N3 Ni0.5 O S2), 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C22 H42 B2 F8 Fe2 N8 Ni O2 S4'
_chemical_formula_weight         922.90
_chemical_name_systematic        FeNiFe
_chemical_properties_physical    Air-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-19 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.406(2)
_cell_angle_beta                 89.714(2)
_cell_angle_gamma                82.273(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7964(6)
_cell_length_b                   11.2004(8)
_cell_length_c                   20.4101(14)
_cell_measurement_reflns_used    5275
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      24.883
_cell_measurement_theta_min      2.609
_cell_volume                     1760.4(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 4 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5987
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.070
_diffrn_reflns_theta_max         25.070
_diffrn_reflns_theta_min         1.841
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0886 before and 0.0441 after correction.
 
For component 2:
 wR2(int) was 0.0950 before and 0.0491 after correction.
 The Ratio of minimum to maximum transmission is 0.79.

Final HKLF 4 output contains 42174 reflections, Rint = 0.0817
 (20391 with I > 3sig(I), Rint = 0.0642)
;
_exptl_crystal_colour            'metallic greenish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_preparation       'CH3CN and Et2O,Magnetic properties'
_exptl_crystal_recrystallization_method 'vapor diffusion'
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0675
_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^)+28.4729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5045
_reflns_number_total             5987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01546g2.cif
_cod_data_source_block           fenife_073122_0m_4
_cod_depositor_comments
'Adding full bibliography for 1569666--1569668.cif.'
_cod_database_code               1569666
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54635
 0.45365
2. Restrained distances
 C13-C14 \\sim C13-C12
 with sigma of 0.02
 C4-C3 \\sim C4-C5
 with sigma of 0.02
 C7-C6 \\sim C16-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C7)
Uanis(C8) = Uanis(C9)
Uanis(C6) = Uanis(C15)
Uanis(C6) = Uanis(C7) = Uanis(C15)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
4.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C6S(H6SA,H6SB,H6SC)
;
_shelx_res_checksum              44317
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id MDB_MQ_221109_dQ_FeNiFe_073122
_olex2_submission_special_instructions 'No special instructions were received'