Highly reactive meso-like positions of dipyrihexaphyrin
Jun-ichiro Setsune; Kyohei Yamato; Chem.Commun. 48 (2012) 4447–; doi:10.1039/c2cc30981e

data_7107615
_publ_section_title
;
 Highly reactive meso-like positions of dipyrihexaphyrin
;
_journal_name_full               Chem.Commun.
_journal_page_first              4447
_journal_paper_doi               10.1039/c2cc30981e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C45 H51 N7'
_chemical_formula_sum            'C47 H57 Cl2 N7 O'
_chemical_formula_weight         806.90
_chemical_name_common
;
8,9,13,14,22,23,27,28-octaethyl-11-cyano-29,30,31,32,33, 34-
hexaaza-heptacyclo(24,2,1,12,6,17,10,112,15,116,20,121,24)
tetratriaconta-1(28),2(34),3,5,7,9,12,14,16(31),17,19,21(30), 22,24,26-
pentadecaene
;
_chemical_name_systematic
;
8,9,13,14,22,23,27,28-octaethyl-11-cyano-29,30,31,32,33,
34-hexaaza-heptacyclo(24,2,1,12,6,17,10,112,15,116,20,121,24)
tetratriaconta-1(28),2(34),3,5,7,9,12,14,16(31),17,19,21(30),
22,24,26-pentadecaene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.589(4)
_cell_angle_beta                 86.948(4)
_cell_angle_gamma                77.737(4)
_cell_formula_units_Z            2
_cell_length_a                   11.025(3)
_cell_length_b                   14.059(4)
_cell_length_c                   15.430(4)
_cell_measurement_reflns_used    1874
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      2.189
_cell_measurement_theta_min      21.3805
_cell_volume                     2217.2(10)
_computing_cell_refinement       'APEXII (Bruker AXS, 2006)'
_computing_data_collection       'APEXII (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'Bruker XSHELL ver. 6.3.1'
_computing_publication_material  'Bruker XSHELL ver. 6.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11027
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         7995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0604
_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^)+(0.1000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                4080
_reflns_number_total             7995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30981e.txt
_cod_data_source_block           7a
_cod_original_cell_volume        2217.3(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107615