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_7717675
_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_formula_moiety         '2(C21 H28 N2 Ni1.5 S2), Cl4 Ni, 2(C2 H3 N)'
_chemical_formula_sum            'C46 H62 Cl4 N6 Ni4 S4'
_chemical_formula_weight         1203.89
_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             2024-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.080(2)
_cell_angle_beta                 82.619(3)
_cell_angle_gamma                63.925(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1770(10)
_cell_length_b                   12.5543(10)
_cell_length_c                   18.8033(15)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      25.399
_cell_measurement_theta_min      2.261
_cell_volume                     2559.2(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54246
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.561
_diffrn_reflns_theta_min         2.081
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1644 before and 0.0853 after correction.
The Ratio of minimum to maximum transmission is 0.8336.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0487P)^2^+1.5027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7773
_reflns_number_total             9420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03174a2.cif
_cod_data_source_block           mj_ni_ni_cl_pph3_0m
_cod_depositor_comments
'Adding full bibliography for 7717671--7717676.cif.'
_cod_database_code               7717675
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.605
_shelx_estimated_absorpt_t_min   0.456
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00B), C00K(H00C,H00D), C00L(H00E,H00F), C00M(H00G,H00H), C00N(H00Q,
 H00R), C00Q(H00I,H00J), C00R(H00K,H00L), C00S(H00M,H00N), C00U(H00S,H00U),
 C00Y(H00O,H00P), C010(H01A,H01B), C012(H01F,H01G), C014(H01I,H01K), C016(H01L,
 H01M), C017(H01N,H01O), C019(H01P,H01Q), C01F(H01S,H01T), C01G(H01U,H01V)
2.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C011(H011),
 C013(H013), C015(H015), C018(H018), C01A(H01R), C01C(H01C), C01D(H01D),
 C01E(H01E), C01H(H01H), C01J(H01J), C01K(H01W), C01M(H01X), C01N(H01Y),
 C01P(H01Z), C01Q(H01)
2.c Idealised Me refined as rotating group:
 C01S(H2,H,HA), C01T(H1,HB,HC)
;
_shelx_res_checksum              7460
_shelx_hkl_checksum              10227
_olex2_submission_special_instructions 'No special instructions were received'