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_7708814
_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         'C29 H49 F5 Fe2 N2 P S2 Si, F6 P'
_chemical_formula_sum            'C29 H48 F11 Fe2 N2 P2 S2 Si'
_chemical_formula_weight         899.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-13
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0907(10)
_cell_length_b                   15.7948(9)
_cell_length_c                   32.7765(18)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      25.512
_cell_measurement_theta_min      2.151
_cell_volume                     8847.8(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40160
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.151
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1356 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.8887.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         7855
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0754P)^2^+24.0053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4966
_reflns_number_total             7855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03482k2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7708814
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23-C25 \\sim C23-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C25 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
F9 \\sim F13 \\sim F12 \\sim F8 \\sim F17 \\sim F16 \\sim F6 \\sim F7 \\sim F14
\\sim F15 \\sim F10 \\sim F11: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C2, C1, C3, C5, C4, C6, C7, C10, C8, C9, C31, C35, C32, C34, C33, C40, C36,
 C39, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H23C)=Sof(H23D)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(F10)=Sof(F12)=Sof(F9)=Sof(F16)=Sof(F14)=Sof(F7)=1-FVAR(2)
 Sof(F6)=Sof(F13)=Sof(F8)=Sof(F17)=Sof(F11)=Sof(F15)=FVAR(2)
 Sof(C31)=Sof(C35)=Sof(C32)=Sof(C34)=Sof(C33)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=1-FVAR(3)
 Sof(C2)=Sof(C1)=Sof(C3)=Sof(C5)=Sof(C4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C23(H23C,H23D)
6.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C), C30(H30A,
 H30B,H30C), C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C),
 C24(H24A,H24B,H24C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C39(H39A,H39B,
 H39C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45172
_shelx_hkl_checksum              69796
_shelx_fab_checksum              45823
_olex2_submission_special_instructions 'No special instructions were received'