Cyclopalladated Complexes of Perylene Imine: Formation of Acetato-Bridged Dinuclear Complexes with 6,6- and 5,6-Membered Metallacycles
Lentijo, Sergio; Miguel, Jesús A.; Espinet, Pablo; Organometallics 30 (2011) 1059–; doi:10.1021/om1010929

data_4064032
_publ_section_title
;
 Cyclopalladated Complexes of Perylene Imine: Formation of Acetato-Bridged
 Dinuclear Complexes with 6,6- and 5,6-Membered Metallacycles
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1059
_journal_paper_doi               10.1021/om1010929
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C70 H62 N2 O6 Pd2'
_chemical_formula_weight         1240.02
_chemical_name_systematic
; 
 ? 
;
_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                85.326(4)
_cell_angle_beta                 76.814(4)
_cell_angle_gamma                80.801(4)
_cell_formula_units_Z            2
_cell_length_a                   12.024(3)
_cell_length_b                   14.667(3)
_cell_length_c                   16.540(3)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.818
_cell_volume                     2800.4(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      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23888
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.758780
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         11385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0577P)^2^+3.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                6821
_reflns_number_total             11385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1010929_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2800.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064032