Cyclic Metalloporphyrin Trimers: 1H NMR Identification of Trimeric Heterometallic (Iron(III), Gallium(III), Manganese(III)) 2-Hydroxy-5,10,15,20-tetraphenylporphyrins and X-ray Crystal Structure of the Iron(III) 2-Hydroxy-5,10,15,20-tetra-p-tolylporphyrin Trimer 1
Jacek Wojaczyński; Lechosław Latos-Grażyński; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 36 (1997) 4548–4554; doi:10.1021/ic970214q

data_4323591
_publ_section_title
;
 Cyclic Metalloporphyrin Trimers: 1H NMR Identification of Trimeric
 Heterometallic (Iron(III), Gallium(III), Manganese(III))
 2-Hydroxy-5,10,15,20-tetraphenylporphyrins and X-ray Crystal Structure of
 the Iron(III) 2-Hydroxy-5,10,15,20-tetra-p-tolylporphyrin Trimer 1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4548
_journal_page_last               4554
_journal_paper_doi               10.1021/ic970214q
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C168 H159 Fe3 N12 O3'
_chemical_formula_weight         2561.62
_chemical_name_common            '[2-O-FeTTP]~3~^.^3n-octane'
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.729(6)
_cell_length_b                   43.671(13)
_cell_length_c                   19.564(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      3.2
_cell_volume                     13751(8)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXTL v. 5 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL v. 5 (Sheldrick, 1994)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating Cu anode (15 kW)'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_sigmaI/netI    0.2081
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11646
_diffrn_reflns_theta_max         55.71
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.973
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5412
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.000039(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.228
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1612
_refine_ls_number_reflns         10818
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.224
_refine_ls_R_factor_all          0.2052
_refine_ls_R_factor_obs          0.0890
_refine_ls_shift/esd_max         -0.214
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2563
_refine_ls_wR_factor_obs         0.1848
_reflns_number_observed          5072
_reflns_number_total             10825
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970214q.cif
_cod_data_source_block           mn692
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        13750.7(81)
_cod_database_code               4323591