Synthesis and crystal structure of an iron triazole complex resulting from the unexpected ligand cleavage of a triazolium carbene precursor.
Pacholski, Roman; Durka, Krzysztof; Buchalski, Piotr; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624002973

data_2312471
_publ_section_title
;
 Synthesis and crystal structure of an iron triazole complex resulting
 from the unexpected ligand cleavage of a triazolium carbene precursor.
;
_journal_coeditor_code           OJ3018
_journal_issue                   5
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624002973
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'[Fe (C9 H9 N3)4 (C2 H3 N)2] [Fe2 Cl6 O], 2C2 H3 N'
_chemical_formula_moiety         'C40 H42 Fe N14 2+, Cl6 Fe2 O 2-, 2(C2 H3 N)'
_chemical_formula_sum            'C44 H48 Cl6 Fe3 N16 O'
_chemical_formula_weight         1197.23
_chemical_name_systematic
'Bis(acetonitrile)tetrakis(1-benzyl-1<i>H</i>-1,2,4-triazole-\k<i>N</i>^4^)iron(II) \m-oxido-bis[trichloridoferrate(III)] acetonitrile disolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                116.349(4)
_cell_angle_beta                 91.178(3)
_cell_angle_gamma                91.622(3)
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_cell_length_a                   8.9568(3)
_cell_length_b                   12.8555(4)
_cell_length_c                   12.8951(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.6040
_cell_measurement_theta_min      3.7990
_cell_volume                     1329.09(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova Dual source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20380
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.749
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.668
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.1552
_exptl_crystal_size_mid          0.1123
_exptl_crystal_size_min          0.0782
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.964
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5052
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1515P)^2^+2.6594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2377
_reflns_number_gt                4520
_reflns_number_total             5052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oj3018sup1.cif
_cod_data_source_block           I
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_shelx_hkl_checksum              29936
_shelx_res_checksum              17964
_shelxl_version_number           .2013
_cod_database_fobs_code 2312471