Site specific redox properties in ligand differentiated di-nickel complexes inspired by the acetyl CoA synthase active site.
Quiroz, Manuel; Jana, Manish; Liu, Kaiyang; Bhuvanesh, Nattamai; Hall, Michael B.; Darensbourg, Marcetta Y.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7414–7423; doi:10.1039/d4dt00306c

data_7715688
_publ_section_title
;
 Site specific redox properties in ligand differentiated di-nickel
 complexes inspired by the acetyl CoA synthase active site.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7414
_journal_page_last               7423
_journal_paper_doi               10.1039/d4dt00306c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H28 N2 Ni2 S4, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C24 H32 Cl4 N2 Ni2 S4'
_chemical_formula_weight         735.97
_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             2023-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.065(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.580(2)
_cell_length_b                   9.3786(10)
_cell_length_c                   18.147(2)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.317
_cell_volume                     2991.5(6)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62967
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.445
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1430 before and 0.0818 after correction. The Ratio of minimum to maximum transmission is 0.6957. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+4.3885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4839
_reflns_number_total             5250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00306c2.cif
_cod_data_source_block           nidameni
_cod_depositor_comments
'Adding full bibliography for 7715688--7715691.cif.'
_cod_database_code               7715688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.529
_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. Restrained distances
 Cl1T-C2T \\sim Cl1S-C2S \\sim Cl3S-C2S \\sim Cl3T-C2T
 with sigma of 0.02
 Cl1S-Cl3S \\sim Cl1T-Cl3T
 with sigma of 0.02
 Cl4T-C5T \\sim Cl4S-C5S \\sim Cl6T-C5T \\sim Cl6S-C5S
 with sigma of 0.02
 Cl4S-Cl6S \\sim Cl4T-Cl6T
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2T) = Uanis(C2S)
Uanis(Cl1T) = Uanis(Cl1S)
Uanis(Cl3S) = Uanis(Cl3T)
Uanis(Cl4T) = Uanis(Cl4S)
Uanis(Cl6T) = Uanis(Cl6S)
Uanis(C5S) = Uanis(C5T)
4. Others
 Sof(Cl1T)=Sof(C2T)=Sof(H2TA)=Sof(H2TB)=Sof(Cl3T)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=
 Sof(Cl4T)=Sof(Cl6T)=1-FVAR(1)
 Sof(Cl1S)=Sof(Cl3S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(Cl4S)=Sof(Cl6S)=Sof(C5S)=
 Sof(H5SA)=Sof(H5SB)=FVAR(1)
5.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),
 C2S(H2SA,H2SB), C5S(H5SA,H5SB), C2T(H2TA,H2TB), C5T(H5TA,H5TB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              35896
_olex2_submission_special_instructions 'No special instructions were received'