Synthesis, characterization, and reactivity of furan- and thiophene-functionalized bis(N-heterocyclic carbene) complexes of iron(II).
Rieb, Julia; Raba, Andreas; Haslinger, Stefan; Kaspar, Manuel; Pöthig, Alexander; Cokoja, Mirza; Basset, Jean-Marie; Kühn, Fritz E; Inorganic chemistry 53 (2014) 9598–9606; doi:10.1021/ic500959m

data_4350673
_publ_section_title
;
 Synthesis, characterization, and reactivity of furan- and
 thiophene-functionalized bis(N-heterocyclic carbene) complexes of
 iron(II).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9598
_journal_page_last               9606
_journal_paper_doi               10.1021/ic500959m
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C23 H24 Fe N8 S2, 2(F6 P)'
_chemical_formula_sum            'C23 H24 F12 Fe N8 P2 S2'
_chemical_formula_weight         822.43
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 95.920(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0550(3)
_cell_length_b                   14.3291(3)
_cell_length_c                   18.8249(4)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3428
_cell_measurement_theta_min      2.3046
_cell_volume                     3502.73(13)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL2013 (Sheldrick, 2013), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0076
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            111677
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.582
_exptl_crystal_size_mid          0.538
_exptl_crystal_size_min          0.430
_platon_squeeze_details
;
The unit cell contains 4 acetonitrile molecules being positioned at a 
special position which have been treated as a diffuse contribution to 
the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         6439
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0457P)^2^+6.1789P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                6002
_reflns_number_total             6439
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            ic500959m_si_002.cif
_cod_data_source_block           compound_2b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4350673