The Electronic Configuration and Ligand Nature of Five Coordinate Iron Porphyrin Carbene Complexes: An Experimental Study.
Liu, Yulong; Xu, Wei; Zhang, Jing; Fuller, William; Schulz, Charles E.; Li, Jianfeng; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b01722

data_4126289
_publ_section_title
;
 The Electronic Configuration and Ligand Nature of Five Coordinate Iron
 Porphyrin Carbene Complexes: An Experimental Study.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b01722
_journal_year                    2017
_chemical_formula_moiety         'C49 H36 Cl2 Fe N4, 1.5(C6 H6)'
_chemical_formula_sum            'C29 H22.5 Cl Fe0.5 N2'
_chemical_formula_weight         462.36
_chemical_name_common            '[Fe(TTP)(CCl2)]1.5C6H6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                74.813(2)
_cell_angle_beta                 78.417(2)
_cell_angle_gamma                81.985(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6869(10)
_cell_length_b                   13.4548(10)
_cell_length_c                   14.0726(10)
_cell_measurement_reflns_used    9747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1188
_cell_measurement_theta_min      2.4404
_cell_volume                     2261.5(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2013; Sheldrick, 2015)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'XCIF (Sheldrick, 2015)/enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Brucker D8 QUEST System'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49238
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.141
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (2008) SADABS. University of G\"ottingen, Germany.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.790
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0373P)^2^+1.9438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8802
_reflns_number_total             9962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01722_si_004.cif
_cod_data_source_block           FeTTPCCl2_20150922
_cod_original_formula_sum        'C29 H22.50 Cl Fe0.50 N2'
_cod_database_code               4126289
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.826
_shelxl_version_number           2014/6
_shelx_res_checksum              86489
_shelx_hkl_checksum              96930