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_7708813
_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         'C44 H55 B F5 Fe2 N2 P S2'
_chemical_formula_sum            'C44 H55 B F5 Fe2 N2 P S2'
_chemical_formula_weight         924.49
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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                97.2170(10)
_cell_angle_beta                 97.8230(10)
_cell_angle_gamma                103.6040(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1726(6)
_cell_length_b                   11.9179(7)
_cell_length_c                   18.6830(11)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      25.990
_cell_measurement_theta_min      2.194
_cell_volume                     2151.6(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42504
_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         26.371
_diffrn_reflns_theta_min         1.941
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1086 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.9030.
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    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(14)
_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     1052
_refine_ls_number_reflns         17536
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      2.181
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0307P)^2^+0.5811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                13772
_reflns_number_total             17536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03482k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H110 B2 F10 Fe4 N4 P2 S4'
_cod_original_formula_weight         1848.99
_cod_original_formula_moiety         '2(C44 H55 B F5 Fe2 N2 P S2)'
_cod_original_formula_units_Z            1
_cod_database_code               7708813
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.979(14)
 0.021(14)
2. 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
3. Restrained distances
 H23A-H8B
 2.06 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C65(H65A,H65B), C67(H67A,H67B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C84(H84), C40(H40), C38(H38), C88(H88), C72(H72), C79(H79), C44(H44),
 C78(H78), C32(H32), C86(H86), C76(H76), C43(H43), C41(H41), C80(H80), C31(H31),
  C85(H85), C75(H75), C29(H29), C82(H82), C30(H30), C34(H34), C81(H81),
 C37(H37), C28(H28), C73(H73), C35(H35), C87(H87), C74(H74), C36(H36), C42(H42)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C6(H6A,H6B,
 H6C), C64(H64A,H64B,H64C), C50(H50A,H50B,H50C), C19(H19A,H19B,H19C), C18(H18A,
 H18B,H18C), C52(H52A,H52B,H52C), C68(H68A,H68B,H68C), C7(H7A,H7B,H7C),
 C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
  C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C51(H51A,H51B,H51C), C22(H22A,H22B,
 H22C), C66(H66A,H66B,H66C), C8(H8A,H8B,H8C), C53(H53A,H53B,H53C), C24(H24A,
 H24B,H24C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              44572
_shelx_hkl_checksum              59784
_olex2_submission_special_instructions 'No special instructions were received'