A sulfur-templated Ni-Ni' coordination polymer that relies on a polarizable nickel nitrosyl hub.
Jana, Manish; Hall, Michael B.; Darensbourg, Marcetta Y.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4927–4934; doi:10.1039/d4dt03174a

data_7717674
_publ_section_title
;
 A sulfur-templated Ni-Ni' coordination polymer that relies on a
 polarizable nickel nitrosyl hub.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4927
_journal_page_last               4934
_journal_paper_doi               10.1039/d4dt03174a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H28 N6 Ni2 O S2, 1[CH3OH]'
_chemical_formula_sum            'C22 H32 N6 Ni2 O2 S2'
_chemical_formula_weight         594.07
_chemical_properties_physical
Air-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.259(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0943(4)
_cell_length_b                   9.0239(3)
_cell_length_c                   12.9900(5)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      66.892
_cell_measurement_theta_min      4.208
_cell_volume                     1292.51(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34921
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.928
_diffrn_reflns_theta_max         66.928
_diffrn_reflns_theta_min         4.009
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0837 before and 0.0646 after correction. The Ratio of minimum to maximum transmission is 0.8302. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH Ether'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.32(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+3.8935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4462
_reflns_number_total             4583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03174a2.cif
_cod_data_source_block           ni_ni_no_n3_meoh2_0ma
_cod_depositor_comments
'Adding full bibliography for 7717671--7717676.cif.'
_cod_database_code               7717674
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.68(4)
 0.32(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C7)
Uanis(N5) = Uanis(N6)
Uanis(N5) = Uanis(N4A)
Uanis(C18) = Uanis(C6)
Uanis(C16) = Uanis(C8)
Uanis(C11) = Uanis(C10)
Uanis(C8) = Uanis(C5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C20(H20A,H20B), C12(H12A,H12B), C2(H2A,H2B), C3(H3A,H3B),
 C1(H1A,H1B), C10(H10A,H10B), C13(H13A,H13B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C7(H7), C19(H19), C16(H16), C8(H8), C5(H5), C6(H6), C9(H9),
 C17(H17), C18(H18)
;
_shelx_res_checksum              29238
_shelx_hkl_checksum              6991
_shelx_fab_checksum              68984
_olex2_submission_special_instructions 'No special instructions were received'