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_7708811
_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 H40 F10 Fe2 N2 P2 S2'
_chemical_formula_sum            'C26 H40 F10 Fe2 N2 P2 S2'
_chemical_formula_weight         808.36
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.11 svn.re2ff6fc5 for OlexSys, GUI svn.r6348)
;
_audit_update_record
;
2021-09-22 deposited with the CCDC.	2021-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.836(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.479(3)
_cell_length_b                   19.104(5)
_cell_length_c                   17.747(5)
_cell_measurement_reflns_used    4787
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      29.998
_cell_measurement_theta_min      2.284
_cell_volume                     3417.9(16)
_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      298.0
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.956
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8048
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.284
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8720.
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    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0546P)^2^+8.1149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2502
_reflns_number_total             3108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03482k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3417.9(17)
_cod_database_code               7708811
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.804
_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
2. Restrained distances
 Fe1-C26 \\sim Fe1-N1
 with sigma of 0.02
 P1-N2 \\sim P1-C25
 with sigma of 0.02
 P1-C26 \\sim P1-N1
 with sigma of 0.04
 C26-N2 \\sim N1-C25
 with sigma of 0.02
 Fe1-N2 \\sim Fe1-C25
 with sigma of 0.04
3. Rigid bond restraints
 N2, P1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C25 \\sim N2 \\sim N1 \\sim C26: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(N1) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(N1)=Sof(C25)=1-FVAR(1)
 Sof(C26)=Sof(N2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
6.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16082
_shelx_hkl_checksum              22041
_shelx_fab_checksum              19997
_olex2_submission_special_instructions 'No special instructions were received'