Palladium N(CH2CH2PiPr2)2-Dialkylamides: Synthesis, Structural Characterization, and Reactivity
Alexander N. Marziale; Eberhardt Herdtweck; Jörg Eppinger; Sven Schneider; Inorganic Chemistry 48 (2009) 3699–3709; doi:10.1021/ic802286u

data_4301966
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl f\"ur Anorganische Chemie,
       Technische Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Dr. Eberhardt Herdtweck
;
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
Palladium N(CH2CH2PiPr2)2-Dialkylamides: Synthesis, Structural
Characterization, and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3699
_journal_page_last               3709
_journal_paper_doi               10.1021/ic802286u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C21 H45 N2 P2 Pd, F6 P'
_chemical_formula_sum            'C21 H45 F6 N2 P3 Pd'
_chemical_formula_weight         638.88
_chemical_name_systematic        ?
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5853(1)
_cell_length_b                   15.7998(2)
_cell_length_c                   19.5797(2)
_cell_measurement_reflns_used    43961
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      25.61
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_computing_cell_refinement       'CrysAlis (Oxford, 2005)'
_computing_data_collection       'CrysAlis (Oxford, 2005)'
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_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      153(1)
_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur \k-CCD diffractometer'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube, Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_max         25.61
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_exptl_absorpt_coefficient_mu    0.837
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
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_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
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_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0302P)^2^+6.6563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                2551
_reflns_number_total             2881
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic802286u_si_001_6.cif
_cod_data_source_block           SVER-1116-153
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4301966