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_4350672
_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_absolute_configuration unk
_chemical_formula_moiety         'C23 H24 Fe N8 O2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C25 H27 F12 Fe N9 O2 P2'
_chemical_formula_weight         831.38
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      159
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   20.6829(3)
_cell_length_b                   20.6829(3)
_cell_length_c                   27.1011(5)
_cell_measurement_reflns_used    9185
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3553
_cell_measurement_theta_min      2.3948
_cell_volume                     10040.2(3)
_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 0.993
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            306292
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         0.75
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.465
_exptl_crystal_size_min          0.440
_platon_squeeze_details
;
The unit cell contains 3 acetonitrile molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions 
by SQUEEZE/PLATON since they are located on a special position and could not
be refined.
;
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         12376
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0766P)^2^+9.5389P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                11787
_reflns_number_total             12376
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            ic500959m_si_002.cif
_cod_data_source_block           compound_2a
_cod_original_cell_volume        10040.2(4)
_cod_database_code               4350672