Formation and Isolation of an Iron-Tripyrrole Complex from Heme Degradation
Sankar Prasad Rath; Marilyn M. Olmstead; Lechoslaw Latos-Grażyński; Alan L. Balch; Journal of the American Chemical Society 125 (2003) 12678–12679; doi:10.1021/ja036656k

data_4114278
_publ_section_title
;
 Formation and Isolation of an Iron-Tripyrrole Complex from Heme
 Degradation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12678
_journal_page_last               12679
_journal_paper_doi               10.1021/ja036656k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C52 H87 Cl Fe N4 O3.5'
_chemical_formula_weight         915.48
_chemical_name_common
'(n-Bu4N)[Fe(Tripyrrole)(Cl)].1.5Cyclohexane 0.5H2O'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.341(6)
_cell_length_b                   14.642(3)
_cell_length_c                   21.305(4)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      2.5
_cell_volume                     10401(3)
_computing_cell_refinement       'SMART 6.22 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SMART 6.22 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.086
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108728
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.8456
_exptl_crystal_colour            'Reddish black'
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         18850
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.1105
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1232P)^2^+44.4872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2769
_refine_ls_wR_factor_ref         0.3049
_reflns_number_gt                11691
_reflns_number_total             18850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja036656ksi20030612_051820.cif
_cod_data_source_block           sr29z
_cod_database_code               4114278