Cyanide-alkene competition in a diiron complex and isolation of a multisite (cyano)alkylidene-alkene species.
Bresciani, Giulio; Schoch, Silvia; Biancalana, Lorenzo; Zacchini, Stefano; Bortoluzzi, Marco; Pampaloni, Guido; Marchetti, Fabio; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1936–1945; doi:10.1039/d1dt03781a

data_7709297
_publ_section_title
;
 Cyanide-alkene competition in a diiron complex and isolation of a
 multisite (cyano)alkylidene-alkene species.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1936
_journal_page_last               1945
_journal_paper_doi               10.1039/d1dt03781a
_journal_volume                  51
_journal_year                    2022
_chemical_formula_sum            'C18 H18 Fe2 N2 O2'
_chemical_formula_weight         406.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.513(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0058(12)
_cell_length_b                   24.672(3)
_cell_length_c                   7.7615(11)
_cell_measurement_reflns_used    5248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.573
_cell_measurement_theta_min      2.619
_cell_volume                     1569.1(4)
_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_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'PHOTON100 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7929
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.090
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.862
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.4037
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1488 (selected reflections only, before parameter refinement)
 R(int) =  0.0821 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.211
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2636
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0847
_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^)+(0.0264P)^2^+69.9229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                2252
_reflns_number_total             2636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03781a3.cif
_cod_data_source_block           cc
_cod_depositor_comments          'Adding full bibliography for 7709297.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7709297
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              31203
_shelx_hkl_checksum              93547