Rotational Isomers of N-Alkylpyridylporphyrins and Their Metal Complexes. HPLC Separation, 1H NMR and X-ray Structural Characterization, Electrochemistry, and Catalysis of O2.- Disproportionation
Ivan Spasojević; Ramil Menzeleev; Peter S. White; Irwin Fridovich; Inorganic Chemistry 41 (2002) 5874–5881; doi:10.1021/ic025556x

data_4318782
_publ_section_title
;
 Rotational Isomers of N-Alkylpyridylporphyrins and Their Metal Complexes.
 HPLC Separation, 1H NMR and X-ray Structural Characterization,
 Electrochemistry, and Catalysis of O2.- Disproportionation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5874
_journal_page_last               5881
_journal_paper_doi               10.1021/ic025556x
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'Ivan Spasojevic, Biochemistry, Duke Univ.'
_chemical_formula_moiety         'C44 H38 N8 Cl4 O16 '
_chemical_formula_sum            'C44 H38 Cl4 N8 O16'
_chemical_formula_weight         1076.63
_chemical_name_common            'H2TM-2-PyP(4+) 4ClO4(-)'
_chemical_name_systematic
;
 meso-tetrakis(N-methylpyridinium-2-yl) porphyrin perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 95.374(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   14.2846(15)
_cell_length_b                   22.2158(24)
_cell_length_c                   29.369(3)
_cell_measurement_reflns_used    2810
_cell_measurement_temperature    193
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     9279.1(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41241
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown-red'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       'needle-like plate'
_exptl_crystal_F_000             4439.68
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.84
_refine_ls_goodness_of_fit_obs   1.66
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         5463
_refine_ls_R_factor_all          0.236
_refine_ls_R_factor_obs          0.077
_refine_ls_shift/esd_max         0.037
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(\s^2^(F)+0.0010F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.117
_refine_ls_wR_factor_obs         0.092
_reflns_number_observed          5473
_reflns_number_total             16078
_reflns_observed_criterion       'Inet > 3.0\s(Inet)'
_cod_data_source_file            ic025556x_s2.cif
_cod_data_source_block           c01111
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 144 times.

'_symmetry_cell_setting' value 'Monoclinic'
changed to 'monoclinic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0010F^2^)' 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^(F)+0.0010F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H38 N8 Cl4 O16 '
_cod_database_code               4318782