Characterization of a Six-Coordinate Ferrous High-Spin Heme with Both Intramolecular Axial Carboxylic Acid and Pyridine
Ismail Hijazi; Thierry Roisnel; Pascale Even-Hernandez; Eric Furet; Jean-François Halet; Olivier Cador; Bernard Boitrel; Journal of the American Chemical Society 132 (2010) 10652–10653; doi:10.1021/ja103825g

data_4102807
_publ_section_title
;
 Characterization of a Six-Coordinate Ferrous High-Spin Heme with Both
 Intramolecular Axial Carboxylic Acid and Pyridine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10652
_journal_page_last               10653
_journal_paper_doi               10.1021/ja103825g
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C84 H59 Fe N10 O6, 3(C H Cl3)'
_chemical_formula_sum            'C87 H62 Cl9 Fe N10 O6'
_chemical_formula_weight         1718.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-11-30T10:51:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.2420(10)
_cell_angle_beta                 69.0710(10)
_cell_angle_gamma                73.9570(10)
_cell_formula_units_Z            2
_cell_length_a                   16.1289(4)
_cell_length_b                   17.5960(5)
_cell_length_c                   17.6291(5)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.62
_cell_measurement_wavelength     0.71073
_cell_volume                     4305.1(2)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69278
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1762
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
;
_refine_diff_density_max         1.73
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         19147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+5.5817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2193
_reflns_number_gt                15802
_reflns_number_total             19147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103825g_si_002.cif
_cod_data_source_block           sq
_cod_database_code               4102807