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_7019015
_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 H16 F30 N6'
_chemical_formula_sum            'C66 H16 F30 N6'
_chemical_formula_weight         1462.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.955(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3440(4)
_cell_length_b                   23.6138(7)
_cell_length_c                   19.8359(6)
_cell_measurement_reflns_used    30288
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.3
_cell_volume                     6190.2(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70388
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  0.8713
_exptl_absorpt_correction_T_min  0.8156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Higashi, T. (1995). Program for Absorption Correction.

Rigaku Corporation, Tokyo, Japan.

;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         11179
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0854
_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^)+(0.1743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2455
_refine_ls_wR_factor_ref         0.2735
_reflns_number_gt                7420
_reflns_number_total             11179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30306j.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7019015