Syntheses, Structures, and Reactivity of Low Spin Iron(III) Complexes Containing a Single Carboxamido Nitrogen in a [FeN5L] Chromophore
John M. Rowland; Marilyn Olmstead; Pradip K. Mascharak; Inorganic Chemistry 40 (2001) 2810–2817; doi:10.1021/ic001127s

data_4319735
_publ_section_title
;
 Syntheses, Structures, and Reactivity of Low Spin Iron(III) Complexes
 Containing a Single Carboxamido Nitrogen in a [FeN5L] Chromophore
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2810
_journal_page_last               2817
_journal_paper_doi               10.1021/ic001127s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H26 Cl2 Fe N7 O5'
_chemical_formula_weight         619.27
_chemical_name_common            '[Fe(III)(PaPy3)Cl)]ClO4.2CH3CN'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.8510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4292(3)
_cell_length_b                   14.1990(5)
_cell_length_c                   11.3770(4)
_cell_measurement_reflns_used    7242
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.3
_cell_volume                     1345.46(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12918
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.9777
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, Sheldrick, G.M. An empirical absorption correction program based 
 on the method of Blessing, R. H., Acta Cryst. (1995). A51, 33-38.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6717
_reflns_number_total             7385
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic001127s_2.cif
_cod_data_source_block           djn145
_cod_original_cell_volume        1345.45(8)
_cod_database_code               4319735