Mixed valence triiron complexes from the conjugation of [Fe<sup>I</sup>Fe<sup>I</sup>] and [Fe<sup>II</sup>] complexes <i>via</i> intermolecular carbyne/alkyne coupling.
Bresciani, Giulio; Ciancaleoni, Gianluca; Zacchini, Stefano; Biancalana, Lorenzo; Pampaloni, Guido; Funaioli, Tiziana; Marchetti, Fabio; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4299–4313; doi:10.1039/d4dt00079j

data_7715133
_publ_section_title
;
 Mixed valence triiron complexes from the conjugation of
 [Fe<sup>I</sup>Fe<sup>I</sup>] and [Fe<sup>II</sup>] complexes <i>via</i>
 intermolecular carbyne/alkyne coupling.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4299
_journal_page_last               4313
_journal_paper_doi               10.1039/d4dt00079j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C20 H17 Fe N O2'
_chemical_formula_weight         359.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2024-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.963(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0498(13)
_cell_length_b                   15.316(3)
_cell_length_c                   13.650(2)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.832
_cell_measurement_theta_min      2.9015
_cell_volume                     1652.2(5)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6656
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1414 (selected reflections only, before parameter refinement)
 R(int) =  0.0536 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0326P)^2^+1.2421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3391
_reflns_number_total             3607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00079j4.cif
_cod_data_source_block           4a1
_cod_depositor_comments
'Adding full bibliography for 7715132--7715133.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7715133
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.874
_shelx_res_checksum              16434