Nonheme Oxoiron(IV) Complexes of Tris(2-pyridylmethyl)amine withcis-Monoanionic Ligands
Rohde, Jan-Uwe; Stubna, Audria; Bominaar, Emile L.; Münck, Eckard; Nam, Wonwoo; Que, Lawrence; Inorganic Chemistry 45 (2006) 6435–6445; doi:10.1021/ic060740u

data_4332713
_publ_section_title
;
 Nonheme Oxoiron(IV) Complexes of Tris(2-pyridylmethyl)amine
 withcis-Monoanionic Ligands
;
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6435
_journal_page_last               6445
_journal_paper_doi               10.1021/ic060740u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C8 H20 N, Br4 Fe'
_chemical_formula_sum            'C8 H20 Br4 Fe N'
_chemical_formula_weight         505.74
_chemical_name_common            04140
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.3774(11)
_cell_length_b                   8.3774(11)
_cell_length_c                   13.631(4)
_cell_measurement_reflns_used    3105
_cell_measurement_temperature    293(2)
_cell_volume                     828.5(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7320
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    10.529
_exptl_absorpt_correction_T_max  0.2812
_exptl_absorpt_correction_T_min  0.1678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         757
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.4360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                577
_reflns_number_total             757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060740usup2.cif
_cod_data_source_block           04140
_cod_original_sg_symbol_H-M      P6(3)mc
_cod_database_code               4332713