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_4116086
_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     'C62 H60 Cl8 N4 O10 '
_chemical_formula_moiety         'C56 H44 Cl8 N4 O8 2(C3 H8 O) '
_chemical_formula_sum            'C62 H60 Cl8 N4 O10'
_chemical_formula_weight         1304.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                100.63(4)
_cell_angle_beta                 95.88(4)
_cell_angle_gamma                112.38(4)
_cell_formula_units_Z            1
_cell_length_a                   12.571(6)
_cell_length_b                   14.418(7)
_cell_length_c                   9.414(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      25.68
_cell_volume                     1522.4(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997-1998)'
_computing_publication_material  'teXsan for Windows (MSC, 1997-1998)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997-1998)'
_computing_structure_solution
;
SIR97 (Altomare, et. al. 1997)
;
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w/2\q
_diffrn_orient_matrix_UB_11      -0.07777
_diffrn_orient_matrix_UB_12      -0.06057
_diffrn_orient_matrix_UB_13      -0.02739
_diffrn_orient_matrix_UB_21      -0.04036
_diffrn_orient_matrix_UB_22      0.04806
_diffrn_orient_matrix_UB_23      0.01040
_diffrn_orient_matrix_UB_31      -0.00115
_diffrn_orient_matrix_UB_32      0.00086
_diffrn_orient_matrix_UB_33      -0.10612
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.02440
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4997
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         61.59
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        -0.24
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.894
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
An empirical absorption correction based on azimuthal scans of five
reflections was applied. (North, Phillips, and Matthews, 1968)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             676.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       0.00956
_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_all   1.978
_refine_ls_goodness_of_fit_ref   1.980
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00048|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0690
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                3168
_reflns_number_total             4728
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja000482e_1.cif
_cod_data_source_block           '_Porphyrinogen-3b__'
_cod_original_cell_volume        1522(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C62 H60 Cl8 N4 O10 '
_cod_database_code               4116086