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_4314667
_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_moiety         'C36 H45 Fe N4 S, C18 H36 N2 Na O6, 0.5(C6 H6)'
_chemical_formula_sum            'C57 H84 Fe N6 Na O6 S6'
_chemical_formula_weight         1060.224
_chemical_melting_point          ?
_chemical_name_common            '[Na(222)][Fe(OEP)(SH)]0.5C6H6'
_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                 116.6760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.9682(4)
_cell_length_b                   23.7269(4)
_cell_length_c                   24.1203(6)
_cell_measurement_reflns_used    9147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6836
_cell_measurement_theta_min      2.2455
_cell_volume                     11234.2(4)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_data_reduction        'BRUKER SAINT/XPREP'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            398321
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.8859
_exptl_absorpt_correction_T_min  0.8463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal pill'
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         37293
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0556P)^2^+9.1657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                27137
_reflns_number_total             37293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901853p_si_002_1.cif
_cod_data_source_block           feiioephs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C114 H168 Fe2 N12 Na2 O12 S2'
_cod_original_formula_weight         2120.448
_cod_original_formula_moiety
'2(C36 H45 Fe N4 S), 2(C18 H36 N2 Na O6), C6 H6'
_cod_original_formula_units_Z            4
_cod_database_code               4314667