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_7717676
_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         'C26 H33 Cl N3 Ni2 O P S2'
_chemical_formula_sum            'C26 H33 Cl N3 Ni2 O P S2'
_chemical_formula_weight         651.51
_chemical_properties_physical    Air-sensitive,Oxygen-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             2024-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-29 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.798(2)
_cell_angle_beta                 93.041(2)
_cell_angle_gamma                92.763(2)
_cell_formula_units_Z            4
_cell_length_a                   9.7816(4)
_cell_length_b                   15.5698(6)
_cell_length_c                   18.7752(7)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      66.756
_cell_measurement_theta_min      3.603
_cell_volume                     2848.29(19)
_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 2018/2 (Sheldrick, 2018)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            90413
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.872
_diffrn_reflns_theta_max         66.872
_diffrn_reflns_theta_min         2.360
_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    4.601
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0747 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.8661.
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    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         10058
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0677
_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^)+18.2623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8468
_reflns_number_total             10058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03174a2.cif
_cod_data_source_block           as_ni_dame_fe_co_0m
_cod_depositor_comments
'Adding full bibliography for 7717671--7717676.cif.'
_cod_database_code               7717676
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.339
_shelx_estimated_absorpt_t_min   0.207
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N5-C33A \\sim N5-C33B
 with sigma of 0.02
 C34B-C33B \\sim C34A-C33A
 with sigma of 0.02
 Ni4-Cl2B \\sim Ni4-Cl2A
 with sigma of 0.02
 C31B-C30B \\sim C31A-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34A) = Uanis(C34B)
Uanis(C33B) = Uanis(C33A)
Uanis(C30B) = Uanis(C30A)
Uanis(C31B) = Uanis(C31A)
Uanis(N4B) = Uanis(N4A)
Uanis(N4A) = Uanis(N4B) = Uanis(N5)
Uanis(C31B) = Uanis(C31A) = Uanis(C5)
Uanis(C33B) = Uanis(C33A) = Uanis(C7)
Uanis(S4A) = Uanis(S4B)
Uanis(C30B) = Uanis(C30A) = Uanis(C5)
Uanis(C32) = Uanis(C29)
4. Others
 Sof(S4B)=Sof(Cl2B)=Sof(N4B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(H28C)=Sof(H28D)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=
 Sof(H34C)=Sof(H34D)=Sof(C30B)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(S4A)=Sof(Cl2A)=Sof(N4A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(H28A)=Sof(H28B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=
 Sof(H34A)=Sof(H34B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C7(H7A,H7B), C2(H2A,H2B), C5(H5A,H5B), C1(H1A,H1B),
 C31A(H31A,H31B), C31B(H31C,H31D), C27(H27A,H27B), C28(H28A,H28B), C28(H28C,
 H28D), C33A(H33A,H33B), C33B(H33C,H33D), C34A(H34A,H34B), C34B(H34C,H34D),
 C30A(H30A,H30B), C30B(H30C,H30D)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C16(H16), C10(H10), C14(H14), C13(H13), C17(H17), C22(H22),
 C26(H26), C19(H19), C40(H40), C12(H12), C18(H18), C48(H48), C23(H23), C11(H11),
  C50(H50), C25(H25), C24(H24), C52(H52), C49(H49), C46(H46), C36(H36),
 C39(H39), C38(H38), C42(H42), C51(H51), C43(H43), C44(H44), C37(H37), C45(H45)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C),
 C29(H29D,H29E,H29F)
;
_shelx_res_checksum              3580
_shelx_hkl_checksum              11650
_olex2_submission_special_instructions 'No special instructions were received'