Structural and Electronic Comparison of 1st Row Transition Metal Complexes of a Tripodal Iminopyridine Ligand
Ashley M. McDaniel; Anthony K. Rappé; Matthew P. Shores; Inorganic Chemistry 51 (2012) 12493–12502; doi:10.1021/ic301909u

data_4331091
_publ_section_title
;
 Structural and Electronic Comparison of 1st Row Transition Metal
 Complexes of a Tripodal Iminopyridine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12493
_journal_page_last               12502
_journal_paper_doi               10.1021/ic301909u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H33 F6 Fe N7 O12 S2'
_chemical_formula_weight         941.62
_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           'Bruker SHELXTL'
_audit_update_record
;
2012-03-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.895(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6283(13)
_cell_length_b                   19.4132(16)
_cell_length_c                   14.4401(13)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.97
_cell_measurement_theta_min      2.82
_cell_volume                     3941.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            113816
_diffrn_reflns_theta_full        33.99
_diffrn_reflns_theta_max         33.99
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
SQUEEZE was used to treat disordered electron density located in the trigonal
 pocket formed by the ester groups of the ligand. A 144.8 Angstrom^3^ solvent
 void with 26 e-/unit cell was found, would could correspond to a partially
 occupied (62%) diethyl ether molecule. 
;
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         16017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+2.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                12958
_reflns_number_total             16017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301909u_si_002_3.cif
_cod_data_source_block           msn285
_cod_database_code               4331091