Two heterodinuclear NiFe-based sulfenate complexes mimicking an S-oxygenated intermediate of an O2-tolerant [NiFe]-H2ase: synthesis, structures, and reactivity
Song, Li-Cheng; Chen, Wei; Feng, Li; New Journal of Chemistry 44 (2020) 14015–14023; doi:10.1039/D0NJ02586K

data_7059789
_publ_section_title
;
 Two heterodinuclear NiFe-based sulfenate complexes mimicking an
 S-oxygenated intermediate of an O2-tolerant [NiFe]-H2ase: synthesis,
 structures, and reactivity
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14015
_journal_page_last               14023
_journal_paper_doi               10.1039/D0NJ02586K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C13 H26 N2 Ni O S2, 2(C0.5 H Cl), H O0.5'
_chemical_formula_sum            'C14 H29 Cl2 N2 Ni O1.5 S2'
_chemical_formula_weight         443.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-20 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.079(5)
_cell_length_b                   14.047(3)
_cell_length_c                   12.304(3)
_cell_measurement_reflns_used    5766
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      1.6954
_cell_volume                     4003.8(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23673
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.871
_diffrn_reflns_theta_min         2.238
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0912P)^2^+8.1997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02586k2.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 7059789--7059793.cif.

 Adding full bibliography for 7059789--7059793.cif.
;
_cod_original_cell_volume        4003.9(15)
_cod_original_formula_sum        'C14 H29 Cl2 N2 Ni O1.50 S2'
_cod_database_code               7059789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 S1-O1 \\sim S1-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O1A)
4. Rigid body (RIGU) restrains
 C15, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1A)=1-FVAR(1)
 Sof(O1)=FVAR(1)
 Fixed Sof: H14A(0.5) H14B(0.5) H15A(0.5) H15B(0.5)
6.a Free rotating group:
 O2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C14(H14A,H14B), C15(H15A,H15B)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              15632
_olex2_submission_special_instructions 'No special instructions were received'