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_4335785
_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         'C46 H36 Fe N4 P2, 1.5(C6 H6)'
_chemical_formula_sum            'C55 H45 Fe N4 P2'
_chemical_formula_weight         879.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.225(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2483(6)
_cell_length_b                   13.6776(5)
_cell_length_c                   18.6190(6)
_cell_measurement_reflns_used    46580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      1.86
_cell_volume                     4292.9(3)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'APEX 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_diffrn_measurement_method       'omega and phi 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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44751
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_correction_T_min  0.8452
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX 2'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+2.8223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                9354
_reflns_number_total             11470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401432m_si_001_6.cif
_cod_data_source_block           complex10
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4335785