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_7715690
_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 O2 S4'
_chemical_formula_sum            'C22 H28 N2 Ni2 O2 S4'
_chemical_formula_weight         598.12
_chemical_name_systematic        Nibmedame-Nidpdt_O2
_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             2024-01-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.968(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8029(6)
_cell_length_b                   9.5412(5)
_cell_length_c                   25.5522(13)
_cell_measurement_reflns_used    20019
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.663
_cell_measurement_theta_min      2.279
_cell_volume                     2623.8(2)
_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  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57163
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.701
_diffrn_reflns_theta_min         2.117
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0849 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.9112. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic reddish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_preparation       'DCM/CH3CN and Et2O/Pentane'
_exptl_crystal_recrystallization_method layering
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0601P)^2^+4.8486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4284
_reflns_number_total             4978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00306c2.cif
_cod_data_source_block           nibmedamt_nidpdt_o2_q_0ma
_cod_depositor_comments
'Adding full bibliography for 7715688--7715691.cif.'
_cod_database_code               7715690
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.618
_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:
 C4(H4A,H4B), C10(H10A,H10B), C3(H3A,H3B), C6(H6A,H6B), C9(H9A,H9B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C13(H13), C21(H21), C16(H16), C22(H22), C15(H15),
 C18(H18), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              15055
_shelx_fab_checksum              72444
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'