Hydrosulfide (HS-) Coordination in Iron Porphyrinates
Jeffrey W. Pavlik; Bruce C. Noll; Allen G. Oliver; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 49 (2010) 1017–1026; doi:10.1021/ic901853p

data_4314668
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
University of Notre Dame,
Notre Dame, IN 46556
USA
;
_publ_contact_author_email       scheidt.1@nd.edu
_publ_contact_author_fax         '+1 574 631 6652'
_publ_contact_author_name        'W. Robert Scheidt'
_publ_contact_author_phone       '+1 574 631 5939'
_publ_section_title
;
 Hydrosulfide (HS-) Coordination in Iron Porphyrinates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1017
_journal_page_last               1026
_journal_paper_doi               10.1021/ic901853p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C72 H78 Cl Fe N6 Na O10 S'
_chemical_formula_weight         1333.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.392(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3987(5)
_cell_length_b                   25.3197(10)
_cell_length_c                   21.7450(8)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.3203
_cell_measurement_theta_min      2.3044
_cell_volume                     6796.2(5)
_computing_cell_refinement       'BRUKER APEX2/SAINT'
_computing_data_collection       'BRUKER APEX2'
_computing_data_reduction        'BRUKER SHELXL'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'KAPPA APEX II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            90934
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.8901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.386
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         11972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1205P)^2^+13.2662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2164
_reflns_number_gt                8963
_reflns_number_total             11972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901853p_si_002_2.cif
_cod_data_source_block           feiitpomepphs
_cod_database_code               4314668