Synthesis, Structures, and Dearomatization by Deprotonation of Iron Complexes Featuring Bipyridine-based PNN Pincer Ligands
Thomas Zell; Robert Langer; Mark A. Iron; Leonid Konstantinovski; Linda J. W. Shimon; Yael Diskin-Posner; Gregory Leitus; Ekambaram Balaraman; Yehoshoa Ben-David; David Milstein; Inorganic Chemistry 52 (2013) 9636–9649; doi:10.1021/ic401432m

data_4335784
_publ_section_title
;
 Synthesis, Structures, and Dearomatization by Deprotonation of Iron
 Complexes Featuring Bipyridine-based PNN Pincer Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9636
_journal_page_last               9649
_journal_paper_doi               10.1021/ic401432m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C46 H38 Fe N4 P2), 2(Br4 Fe), C2 H3 N'
_chemical_formula_sum            'C94 H79 Br8 Fe4 N9 P4'
_chemical_formula_weight         2321.22
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.674(3)
_cell_length_b                   24.218(5)
_cell_length_c                   16.214(3)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     4728.0(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36027
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    4.099
_exptl_absorpt_correction_T_max  0.6846
_exptl_absorpt_correction_T_min  0.3727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+78.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                4957
_reflns_number_total             5413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401432m_si_001_5.cif
_cod_data_source_block           complex8
_cod_original_cell_volume        4728.1(19)
_cod_database_code               4335784