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_7708812
_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         'C27 H43 Fe2 N2 S2, F6 P'
_chemical_formula_sum            'C27 H43 F6 Fe2 N2 P S2'
_chemical_formula_weight         716.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-22
_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                 90.286(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.197(3)
_cell_length_b                   16.209(4)
_cell_length_c                   10.954(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      3.16
_cell_volume                     1632.9(8)
_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
'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.13
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24159
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.160
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6024
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1265 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.8079.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0253P)^2^+1.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2866
_reflns_number_total             3090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03482k2.cif
_cod_data_source_block           2
_cod_database_code               7708812
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6305(11)
 0.3695(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H8A(0.5) H8B(0.5) H8C(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
4.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C),
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              2438
_shelx_hkl_checksum              2391
_olex2_submission_special_instructions 'No special instructions were received'