1H NMR Investigations of Triphenylporphyrin Metal Complexes and Electronic Interactions in Iron(III) Complexes of meso-meso-Linked 5,5'-Bis(10,15,20-triphenylporphyrin)
Jacek Wojaczyński; Lechosław Latos-Grażyński; Piotr J. Chmielewski; Pamela Van Calcar; Alan L. Balch; Inorganic Chemistry 38 (1999) 3040–3050; doi:10.1021/ic990038g

data_4322117
_publ_section_title
;
 1H NMR Investigations of Triphenylporphyrin Metal Complexes and
 Electronic Interactions in Iron(III) Complexes of meso-meso-Linked
 5,5'-Bis(10,15,20-triphenylporphyrin)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3040
_journal_page_last               3050
_journal_paper_doi               10.1021/ic990038g
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C41.4 H30.8 Cl0.8 N4 O3 Zn'
_chemical_formula_weight         726.03
_chemical_name_common
;
5,10,15-tris(p-methoxyphenyl)porphyrin Zn^II^
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.770(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.744(9)
_cell_length_b                   9.090(2)
_cell_length_c                   15.571(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     6743(2)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.03 (Sheldrick, 1995) XP'
_computing_publication_material  'SHELXTL 5.03 (Sheldrick, 1995) XCIF'
_computing_structure_refinement  'SHELXTL 5.03 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL 5.03 (Sheldrick, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5553
_diffrn_reflns_theta_max         55.81
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
 B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2998
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.520
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         4361
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_obs          0.0756
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+52.1270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2530
_refine_ls_wR_factor_obs         0.2169
_reflns_number_observed          3179
_reflns_number_total             4366
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990038g.cif
_cod_data_source_block           pv47
_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^)+(0.1270P)^2^+52.1270P] 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^)+(0.1270P)^2^+52.1270P] 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        6743.1(20)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C41.40 H30.80 Cl0.80 N4 O3 Zn'
_cod_database_code               4322117