Synthesis and Characterization of Palladium Complexes Supported by an NPN-Phosphido Ancillary Ligand
MacInnis, Morgan C.; McDonald, Robert; Turculet, Laura; Organometallics 30 (2011) 6408–; doi:10.1021/om200701h

data_4065303
_publ_section_title
;
 Synthesis and Characterization of Palladium Complexes Supported by an
 NPN-Phosphido Ancillary Ligand
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6408
_journal_paper_doi               10.1021/om200701h
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H46 N4 O4 P2 Pd2, C6 H6'
_chemical_formula_sum            'C42 H52 N4 O4 P2 Pd2'
_chemical_formula_weight         951.62
_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                91.9195(18)
_cell_angle_beta                 96.8964(18)
_cell_angle_gamma                95.3691(17)
_cell_formula_units_Z            2
_cell_length_a                   11.7857(15)
_cell_length_b                   11.8320(15)
_cell_length_c                   15.682(2)
_cell_measurement_reflns_used    5536
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.22
_cell_volume                     2159.3(5)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14929
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.8253
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;

Attempts to refine peaks of residual electron density as solvent benzene

carbon atoms were unsuccessful.  The data were corrected for disordered

electron density through use of the SQUEEZE procedure (Sluis, P. van der;

Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in

PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34.  PLATON - a

multipurpose crystallographic tool.  Utrecht University, Utrecht, The

Netherlands).  A total solvent-accessible void volume of 374.8 A^3^ with

a total electron count of 99 (consistent with two molecules of solvent

benzene, or one molecule per formula unit of the dipalladium complex ion)

was found in the unit cell.

;
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                6448
_reflns_number_total             8723
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200701h_si_001.cif
_cod_data_source_block           dal0711
_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 
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_cod_database_code               4065303