Confusion of Möbius aromaticity: disruption of annulenic pathway in singly N-confused [28]hexaphyrin and its mono-Pd(ii) complex
Gokulnath, Sabapathi; Toganoh, Motoki; Yamaguchi, Keisuke; Mori, Shigeki; Uno, Hidemitsu; Furuta, Hiroyuki; Dalton Transactions 41 (2012) 6283–; doi:10.1039/c2dt30306j

data_7019016
_publ_section_title
;
 Confusion of M\"obius aromaticity: disruption of annulenic pathway in
 singly N-confused [28]hexaphyrin and its mono-Pd(ii) complex
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              6283
_journal_paper_doi               10.1039/c2dt30306j
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C66 H14 F30 N6 Pd, C7 H16 '
_chemical_formula_sum            'C73 H30 F30 N6 Pd'
_chemical_formula_weight         1667.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.727(3)
_cell_angle_beta                 90.851(2)
_cell_angle_gamma                93.498(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6108(2)
_cell_length_b                   17.3675(8)
_cell_length_c                   24.9638(11)
_cell_measurement_reflns_used    8471
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3223.6(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  'SHELXL97 and Platon squeeze'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Mercury-8'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34080
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0038(4)
_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   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         14684
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+4.9988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                12112
_reflns_number_total             14684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30306j.txt
_cod_data_source_block           '__PdNCHex'
_cod_original_formula_sum        'C73 H30 F30 N6 Pd '
_cod_database_code               7019016