meso-Unsubstituted Porphyrinogens and Hexaphyrinogens: The First X-ray Characterization
Hidemitsu Uno; Takashi Inoue; Yumiko Fumoto; Motoo Shiro; Noboru Ono; Journal of the American Chemical Society 122 (2000) 6773–6774; doi:10.1021/ja000482e

data_4116087
_publ_contact_author_address
;
    Advanced Instrumentation Center for Chemical Analysis
    Ehime University
    Matsuyama 790-8577
    Japan
;
_publ_contact_author_email       ' uno@dpc.ehime-u.ac.jp '
_publ_contact_author_fax         ' 81(89927)9663 '
_publ_contact_author_name        ' Dr. Hidemitsu Uno '
_publ_contact_author_phone       ' 81(89927)9663 '
_publ_section_title
;
 meso-Unsubstituted Porphyrinogens and Hexaphyrinogens: The First X-ray
 Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6773
_journal_page_last               6774
_journal_paper_doi               10.1021/ja000482e
_journal_volume                  122
_journal_year                    2000
_chemical_formula_analytical     'C103 H115 Cl3 N6 O12 '
_chemical_formula_moiety         'C102 H114 N6 O12 (C H Cl3)'
_chemical_formula_sum            'C103 H115 Cl3 N6 O12'
_chemical_formula_weight         1735.43
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   43.981(2)
_cell_length_b                   43.981(1)
_cell_length_c                   17.017(1)
_cell_measurement_reflns_used    47075
_cell_measurement_temperature    143.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     28506(2)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXsan for Windows (MSC, 1997-1998)'
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'teXsan for Windows (MSC, 1997-1998)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997-1998)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      143.2
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measured_fraction_theta_max 0.9908
_diffrn_measurement_device       'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00001
_diffrn_orient_matrix_UB_12      -0.02079
_diffrn_orient_matrix_UB_13      -0.02379
_diffrn_orient_matrix_UB_21      0.02622
_diffrn_orient_matrix_UB_22      0.01263
_diffrn_orient_matrix_UB_23      0.00281
_diffrn_orient_matrix_UB_31      -0.00137
_diffrn_orient_matrix_UB_32      -0.00988
_diffrn_orient_matrix_UB_33      0.05366
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37057
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             11064.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.50
_refine_ls_extinction_coef       0.000434
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method
;
Zachariasen (1967) type 2 gaussian isotropic
;
_refine_ls_goodness_of_fit_ref   1.739
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     765
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.01000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                6480
_reflns_number_total             14403
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja000482e_2.cif
_cod_data_source_block           '_Hexaphyrinogen-4a__'
_cod_original_cell_volume        28507(2)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C103 H115 Cl3 N6 O12 '
_cod_database_code               4116087