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_4332712
_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         'C38 H39 Fe2 N8 O3, 3(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C41 H43 F9 Fe2 N8 O14 S3'
_chemical_formula_weight         1250.71
_chemical_name_common            02190
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                82.545(6)
_cell_angle_beta                 74.449(6)
_cell_angle_gamma                65.580(6)
_cell_formula_units_Z            2
_cell_length_a                   12.177(4)
_cell_length_b                   13.460(5)
_cell_length_c                   17.924(6)
_cell_measurement_reflns_used    3127
_cell_measurement_temperature    173(2)
_cell_volume                     2576.4(15)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25438
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.7933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'intense green'
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular needle'
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0860P)^2^+1.6322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                6272
_reflns_number_total             9144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060740usup1.cif
_cod_data_source_block           02190
_cod_original_cell_volume        2576(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332712