Palladium Vacataporphyrin Reveals Conformational Rearrangements Involving Hückel and Möbius Macrocyclic Topologies
Ewa Pacholska-Dudziak; Janusz Skonieczny; Miłosz Pawlicki; Ludmiła Szterenberg; Zbigniew Ciunik; Lechosław Latos-Grażyński; Journal of the American Chemical Society 130 (2008) 6182–6195; doi:10.1021/ja711039c

data_4107761
_publ_section_title
;
 Palladium Vacataporphyrin Reveals Conformational Rearrangements Involving
 H\"uckel and M\"obius Macrocyclic Topologies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6182
_journal_page_last               6195
_journal_paper_doi               10.1021/ja711039c
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C46 H34 Cl N3 Pd, C H2 Cl2'
_chemical_formula_sum            'C47 H36 Cl3 N3 Pd'
_chemical_formula_weight         855.54
_chemical_name_common            'palladium vacataporphyrin'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 106.885(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9744(6)
_cell_length_b                   23.6761(9)
_cell_length_c                   11.9400(6)
_cell_measurement_reflns_used    7450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.96
_cell_measurement_theta_min      3.73
_cell_volume                     3780.2(3)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction,Poland Sp. z o.o)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction,Poland Sp. z o.o)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction,Poland Sp. z o.o)'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35486
_diffrn_reflns_theta_full        73.96
_diffrn_reflns_theta_max         73.96
_diffrn_reflns_theta_min         3.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.210
_exptl_absorpt_correction_T_max  0.6994
_exptl_absorpt_correction_T_min  0.5563
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'(Instruction, Oxford Diffraction,Poland Sp. z o.o)'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.252
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.00077(11)
_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   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                5826
_reflns_number_total             7396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711039c-file001.cif
_cod_data_source_block           v2cuabs
_cod_database_code               4107761