Conformational Flexibility of 1,4-Naphthiporphyrin Promotes a Palladium-Mediated Contraction of Naphthalene to Isoindene
Szyszko, Bartosz; Latos-Grażyński, Lechosław; Organometallics 30 (2011) 4354–; doi:10.1021/om2004139

data_4063588
_publ_section_title
;
 Conformational Flexibility of 1,4-Naphthiporphyrin Promotes a
 Palladium-Mediated Contraction of Naphthalene to Isoindene
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4354
_journal_paper_doi               10.1021/om2004139
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         C50H33N3
_chemical_formula_sum            'C50 H33 N3'
_chemical_formula_weight         675.79
_chemical_name_systematic        1,4-naphthiporphyrin
_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                84.502(4)
_cell_angle_beta                 76.137(4)
_cell_angle_gamma                83.263(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4624(5)
_cell_length_b                   11.8931(6)
_cell_length_c                   14.8821(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1781.02(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.625
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_sigmaI/netI    0.2432
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22932
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         37.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.757
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         11325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.757
_refine_ls_R_factor_all          0.2216
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0394P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3562
_reflns_number_total             11325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2004139_si_002.cif
_cod_data_source_block           bs1
_cod_original_cell_volume        1781.02(14)
_cod_database_code               4063588