A Remarkable Skeletal Rearrangement of a Coordinated Tetrapyrrole: Chemical Consequences of Palladium π-Coordination to a Bilindione
Pamela A. Lord; Bruce C. Noll; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 123 (2001) 10554–10559; doi:10.1021/ja010647z

data_4115734
_publ_section_title
;
 A Remarkable Skeletal Rearrangement of a Coordinated Tetrapyrrole:
 Chemical Consequences of Palladium \p-Coordination to a Bilindione
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10554
_journal_page_last               10559
_journal_paper_doi               10.1021/ja010647z
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C35 H42 N4 O3 Pd'
_chemical_formula_weight         673.13
_chemical_name_common            'Compound 2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.527(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.868(3)
_cell_length_b                   14.966(2)
_cell_length_c                   15.018(2)
_cell_measurement_reflns_used    6784
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      1.9
_cell_volume                     3113.9(9)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28078
_diffrn_reflns_theta_full        31.29
_diffrn_reflns_theta_max         31.29
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.8441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
' Blessing, R. H., Acta Cryst. (1995). A51, 33-38.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00014(7)
_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   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+5.2675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                6813
_reflns_number_total             9436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010647z.cif
_cod_data_source_block           mn890
_cod_database_code               4115734