Formation of thiolate-bridged diiron complexes featuring anionic isocyanide originated from the activation of counterions in the outer sphere
Xu, Sunlin; Yang, Dawei; Zhao, Jinfeng; Wang, Baomin; Qu, Jingping; Dalton Transactions  (2021) –; doi:10.1039/D1DT03482K

data_7708815
_publ_section_title
;
 Formation of thiolate-bridged diiron complexes featuring anionic
 isocyanide originated from the activation of counterions in the outer
 sphere
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03482K
_journal_year                    2021
_chemical_formula_moiety         'C26 H39.678 Fe2 N2 S2'
_chemical_formula_sum            'C26 H39 Fe2 N2 S2'
_chemical_formula_weight         555.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.11 svn.re2ff6fc5 for OlexSys, GUI svn.r6348)
;
_audit_update_record
;
2021-07-24 deposited with the CCDC.	2021-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6910(8)
_cell_length_b                   14.4262(11)
_cell_length_c                   17.5493(13)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    300.16
_cell_measurement_theta_max      26.776
_cell_measurement_theta_min      2.328
_cell_volume                     2699.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            33469
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.328
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1383 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.7503.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0419P)^2^+1.5059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4566
_reflns_number_total             6195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03482k2.cif
_cod_data_source_block           2_CCDC1
_cod_database_code               7708815
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H23A,H23B,H23} of C23
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, {H7A,H7B,H7C} of C7, {H8A,H8B,H8C} of C8, {H10A,
  H10B,H10C} of C10, {H17A,H17B,H17C} of C17, {H9A,H9B,H9C} of C9, {H24A,H24B,
  H24C} of C24, {H22A,H22B,H22C} of C22, {H18A,H18B,H18C} of C18, {H16A,H16B,
  H16C} of C16, {H20A,H20B,H20C} of C20, {H6A,H6B,H6C} of C6, {H27A,H27B,H27C}
  of C27
2. Restrained distances
 C23-C24 \\sim C23-C27
 with sigma of 0.02
3. Others
 Sof(H23)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C),
  C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              78097
_shelx_hkl_checksum              43295
_olex2_submission_special_instructions 'No special instructions were received'