Protonated N-Confused Porphyrin Dimer: Formation, Structure, and Guest Binding
Piotr J. Chmielewski; Marta Siczek; Ludmiła Szterenberg; Inorganic Chemistry 50 (2011) 6719–6736; doi:10.1021/ic200742d

data_4325681
_publ_section_title
;
 Protonated N-Confused Porphyrin Dimer: Formation, Structure, and Guest
 Binding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6719
_journal_page_last               6736
_journal_paper_doi               10.1021/ic200742d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C96 H76 N8, 2Cl, 5(C H Cl3)'
_chemical_formula_sum            'C101 H81 Cl17 N8'
_chemical_formula_weight         2009.39
_chemical_name_systematic
'3,3-bis(meso-tetratolyl-2-aza-21-carbaporphyrin) dihydrochloride'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.088(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.632(3)
_cell_length_b                   19.729(3)
_cell_length_c                   23.833(3)
_cell_measurement_reflns_used    1540
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.93
_cell_measurement_theta_min      3.43
_cell_volume                     9520(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.686
_diffrn_measured_fraction_theta_max 0.686
_diffrn_measurement_device_type  'Xcalibur with Onyx CCD'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1318
_diffrn_reflns_av_sigmaI/netI    0.1547
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8908
_diffrn_reflns_theta_full        62.93
_diffrn_reflns_theta_max         62.93
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00019(3)
_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_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         5282
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                2777
_reflns_number_total             5282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200742d_si_002_1.cif
_cod_data_source_block           swi11dc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4325681