Directly Pd(II)-Bridged Porphyrin Belts with Remarkable Curvatures
Jianxin Song; Naoki Aratani; Ji Haeng Heo; Dongho Kim; Hiroshi Shinokubo; Atsuhiro Osuka; Journal of the American Chemical Society 132 (2010) 11868–11869; doi:10.1021/ja1046654

data_4102960
_publ_section_title
;
 Directly Pd(II)-Bridged Porphyrin Belts with Remarkable Curvatures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11868
_journal_page_last               11869
_journal_paper_doi               10.1021/ja1046654
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'2(C134 H146 N10 Ni2), 3.44(C7 H8), 1.31(C7 H7), C7, 4.25(C2'
_chemical_formula_sum            'C316.74 H356.19 N20 Ni4 O6.75'
_chemical_formula_weight         4786.09
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.861(2)
_cell_angle_beta                 93.037(2)
_cell_angle_gamma                95.182(2)
_cell_formula_units_Z            1
_cell_length_a                   9.372(1)
_cell_length_b                   15.564(1)
_cell_length_c                   48.161(4)
_cell_measurement_reflns_used    8332
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      56.491
_cell_measurement_theta_min      4.925
_cell_volume                     6946.0(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            37670
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2566
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1981
_refine_ls_number_reflns         25351
_refine_ls_number_restraints     1918
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.123
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+6.2324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1973
_reflns_number_gt                16506
_reflns_number_total             25351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1046654_si_002.cif
_cod_data_source_block           81021so
_cod_database_code               4102960