#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:04:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178633 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/44/4074449.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4074449
loop_
_publ_author_name
'Tian, Xin'
'Goddard, Richard'
'Pörschke, Klaus-Richard'
_publ_section_title
;
 (β-Diketiminato)palladium Complexes
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5854
_journal_paper_doi               10.1021/om0606486
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'pentane at -40 degrees'
_chemical_formula_moiety         'C22 H42 N4 Pd'
_chemical_formula_sum            'C22 H42 N4 Pd'
_chemical_formula_weight         469.00
_chemical_name_systematic
; 
 bis[2-(isopropylamino)-4-(isopropylimino)-pent-2-ene-N,N']
 palladium(ii)
;
_chemical_temperature_decomposition 426
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2006-07-04
_cell_angle_alpha                78.659(1)
_cell_angle_beta                 82.887(1)
_cell_angle_gamma                65.204(1)
_cell_formula_units_Z            2
_cell_length_a                   8.1121(2)
_cell_length_b                   9.6711(3)
_cell_length_c                   16.6998(4)
_cell_measurement_reflns_used    22243
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.91
_cell_volume                     1164.88(5)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD ω-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26528
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.7480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack, Otwinowski (1997)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0285
_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/[σ²(Fo²)+(0.0274P)²+1.4660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                7091
_reflns_number_total             7540
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0606486si20060718_110644.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '426
decomposition'. The value '426 decomposition' was changed to
'426'.

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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               4074449
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.8280(2) -0.1745(2) 0.32226(11) 0.0182(3) Uani 1 1 d .
H1A H 0.9482 -0.2314 0.3010 0.027 Uiso 1 1 calc R
H1B H 0.7533 -0.1081 0.2781 0.027 Uiso 1 1 calc R
H1C H 0.7767 -0.2451 0.3501 0.027 Uiso 1 1 calc R
C2 C 0.8370(2) -0.07782(17) 0.38169(9) 0.0113(2) Uani 1 1 d .
C3 C 0.6711(2) 0.01351(18) 0.41907(10) 0.0125(3) Uani 1 1 d .
H3 H 0.5787 -0.0215 0.4307 0.015 Uiso 1 1 calc R
C4 C 0.64331(19) 0.15678(17) 0.43907(9) 0.0108(2) Uani 1 1 d .
C5 C 0.4488(2) 0.27696(19) 0.43967(11) 0.0166(3) Uani 1 1 d .
H5A H 0.4457 0.3691 0.4544 0.025 Uiso 1 1 calc R
H5B H 0.3754 0.2376 0.4787 0.025 Uiso 1 1 calc R
H5C H 0.4022 0.3002 0.3863 0.025 Uiso 1 1 calc R
C6 C 1.1474(2) -0.12038(18) 0.33444(9) 0.0133(3) Uani 1 1 d .
H6 H 1.0995 -0.1126 0.2819 0.016 Uiso 1 1 calc R
C7 C 1.2345(3) -0.0051(2) 0.32416(12) 0.0225(3) Uani 1 1 d .
H7A H 1.1439 0.0976 0.3098 0.034 Uiso 1 1 calc R
H7B H 1.3286 -0.0273 0.2816 0.034 Uiso 1 1 calc R
H7C H 1.2858 -0.0130 0.3745 0.034 Uiso 1 1 calc R
C8 C 1.2899(3) -0.2842(2) 0.35659(11) 0.0240(4) Uani 1 1 d .
H8A H 1.2339 -0.3559 0.3626 0.036 Uiso 1 1 calc R
H8B H 1.3416 -0.2935 0.4071 0.036 Uiso 1 1 calc R
H8C H 1.3839 -0.3065 0.3140 0.036 Uiso 1 1 calc R
C9 C 0.7655(2) 0.34864(17) 0.43124(9) 0.0108(2) Uani 1 1 d .
H9 H 0.6562 0.4162 0.4591 0.013 Uiso 1 1 calc R
C10 C 0.9301(2) 0.36416(19) 0.45625(11) 0.0169(3) Uani 1 1 d .
H10A H 0.9422 0.3319 0.5142 0.025 Uiso 1 1 calc R
H10B H 0.9147 0.4699 0.4423 0.025 Uiso 1 1 calc R
H10C H 1.0374 0.3005 0.4280 0.025 Uiso 1 1 calc R
C11 C 0.7495(2) 0.40086(19) 0.33869(10) 0.0157(3) Uani 1 1 d .
H11A H 0.6457 0.3923 0.3219 0.024 Uiso 1 1 calc R
H11B H 0.8573 0.3368 0.3110 0.024 Uiso 1 1 calc R
H11C H 0.7355 0.5063 0.3252 0.024 Uiso 1 1 calc R
C12 C 0.2140(2) 0.93291(19) 0.08299(11) 0.0179(3) Uani 1 1 d .
H12A H 0.2996 0.9751 0.0580 0.027 Uiso 1 1 calc R
H12B H 0.1892 0.9484 0.1390 0.027 Uiso 1 1 calc R
H12C H 0.1033 0.9837 0.0543 0.027 Uiso 1 1 calc R
C13 C 0.2931(2) 0.76146(17) 0.07932(9) 0.0117(2) Uani 1 1 d .
C14 C 0.1854(2) 0.68069(18) 0.11321(10) 0.0129(3) Uani 1 1 d .
H14 H 0.0594 0.7325 0.1147 0.015 Uiso 1 1 calc R
C15 C 0.2660(2) 0.52124(18) 0.14512(9) 0.0119(3) Uani 1 1 d .
C16 C 0.1675(2) 0.4648(2) 0.21860(11) 0.0191(3) Uani 1 1 d .
H16A H 0.2341 0.3560 0.2353 0.029 Uiso 1 1 calc R
H16B H 0.0479 0.4842 0.2043 0.029 Uiso 1 1 calc R
H16C H 0.1583 0.5184 0.2627 0.029 Uiso 1 1 calc R
C17 C 0.6008(2) 0.74607(17) 0.05634(9) 0.0115(2) Uani 1 1 d .
H17 H 0.5581 0.8557 0.0328 0.014 Uiso 1 1 calc R
C18 C 0.6345(2) 0.7264(2) 0.14702(10) 0.0171(3) Uani 1 1 d .
H18A H 0.5227 0.7823 0.1754 0.026 Uiso 1 1 calc R
H18B H 0.7228 0.7655 0.1523 0.026 Uiso 1 1 calc R
H18C H 0.6789 0.6189 0.1702 0.026 Uiso 1 1 calc R
C19 C 0.7800(2) 0.6565(2) 0.01265(10) 0.0157(3) Uani 1 1 d .
H19A H 0.7612 0.6681 -0.0444 0.024 Uiso 1 1 calc R
H19B H 0.8238 0.5492 0.0361 0.024 Uiso 1 1 calc R
H19C H 0.8678 0.6958 0.0187 0.024 Uiso 1 1 calc R
C20 C 0.5354(2) 0.28113(18) 0.16569(9) 0.0139(3) Uani 1 1 d .
H20 H 0.5006 0.2903 0.2234 0.017 Uiso 1 1 calc R
C21 C 0.5117(3) 0.1409(2) 0.14830(11) 0.0202(3) Uani 1 1 d .
H21A H 0.3863 0.1567 0.1577 0.030 Uiso 1 1 calc R
H21B H 0.5851 0.0502 0.1839 0.030 Uiso 1 1 calc R
H21C H 0.5487 0.1278 0.0924 0.030 Uiso 1 1 calc R
C22 C 0.7351(2) 0.2559(2) 0.15167(11) 0.0184(3) Uani 1 1 d .
H22A H 0.7495 0.3436 0.1630 0.028 Uiso 1 1 calc R
H22B H 0.7733 0.2431 0.0959 0.028 Uiso 1 1 calc R
H22C H 0.8080 0.1650 0.1873 0.028 Uiso 1 1 calc R
N1 N 0.99291(17) -0.07534(15) 0.39484(7) 0.0098(2) Uani 1 1 d .
N2 N 0.78048(16) 0.18873(14) 0.45319(8) 0.0094(2) Uani 1 1 d .
N3 N 0.46049(17) 0.69059(15) 0.04782(8) 0.0100(2) Uani 1 1 d .
N4 N 0.42302(17) 0.42755(15) 0.11568(8) 0.0108(2) Uani 1 1 d .
Pd1 Pd 1.0000 0.0000 0.5000 0.00657(4) Uani 1 2 d S
Pd2 Pd 0.5000 0.5000 0.0000 0.00744(4) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C2 C3 121.96(14) . . y
N1 C2 C1 120.98(14) . . y
C3 C2 C1 117.00(13) . . y
C4 C3 C2 121.02(13) . . y
N2 C4 C3 122.16(13) . . y
N2 C4 C5 121.21(14) . . y
C3 C4 C5 116.56(13) . . y
N1 C6 C8 114.05(13) . . y
N1 C6 C7 108.34(13) . . y
C8 C6 C7 110.14(15) . . y
N2 C9 C10 111.59(12) . . y
N2 C9 C11 110.11(12) . . y
C10 C9 C11 108.37(13) . . y
N3 C13 C14 121.82(14) . . y
N3 C13 C12 120.94(14) . . y
C14 C13 C12 117.19(13) . . y
C13 C14 C15 120.86(14) . . y
N4 C15 C14 122.18(14) . . y
N4 C15 C16 121.26(14) . . y
C14 C15 C16 116.47(14) . . y
N3 C17 C19 111.36(12) . . y
N3 C17 C18 109.78(12) . . y
C19 C17 C18 108.49(13) . . y
N4 C20 C22 109.12(13) . . y
N4 C20 C21 113.57(13) . . y
C22 C20 C21 109.73(14) . . y
C2 N1 C6 120.42(13) . . y
C2 N1 Pd1 115.89(10) . . y
C6 N1 Pd1 123.67(10) . . y
C4 N2 C9 119.22(12) . . y
C4 N2 Pd1 113.95(10) . . y
C9 N2 Pd1 126.77(9) . . y
C13 N3 C17 119.05(12) . . y
C13 N3 Pd2 114.36(10) . . y
C17 N3 Pd2 126.38(9) . . y
C15 N4 C20 120.80(13) . . y
C15 N4 Pd2 116.10(10) . . y
C20 N4 Pd2 123.08(10) . . y
N2 Pd1 N2 179.998(1) . 2_756 y
N2 Pd1 N1 82.85(5) . . y
N2 Pd1 N1 97.15(5) 2_756 . y
N2 Pd1 N1 97.15(5) . 2_756 y
N2 Pd1 N1 82.85(5) 2_756 2_756 y
N1 Pd1 N1 180.00(8) . 2_756 y
N4 Pd2 N4 180.0 2_665 . n
N4 Pd2 N3 82.88(5) 2_665 2_665 y
N4 Pd2 N3 97.12(5) . 2_665 y
N4 Pd2 N3 97.12(5) 2_665 . y
N4 Pd2 N3 82.88(5) . . y
N3 Pd2 N3 180.0 2_665 . n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(2) . y
C2 N1 1.3208(19) . y
C2 C3 1.412(2) . y
C3 C4 1.408(2) . y
C4 N2 1.3309(18) . y
C4 C5 1.518(2) . y
C6 N1 1.4765(19) . y
C6 C8 1.524(2) . y
C6 C7 1.525(3) . y
C9 N2 1.4734(19) . y
C9 C10 1.521(2) . y
C9 C11 1.532(2) . y
C12 C13 1.517(2) . y
C13 N3 1.3320(18) . y
C13 C14 1.404(2) . y
C14 C15 1.417(2) . y
C15 N4 1.3181(19) . y
C15 C16 1.517(2) . y
C17 N3 1.4786(19) . y
C17 C19 1.525(2) . y
C17 C18 1.533(2) . y
C20 N4 1.475(2) . y
C20 C22 1.528(2) . y
C20 C21 1.533(2) . y
N1 Pd1 2.0449(12) . y
N2 Pd1 2.0423(12) . y
N3 Pd2 2.0391(12) . y
N4 Pd2 2.0369(12) . y
Pd1 N2 2.0423(12) 2_756 y
Pd1 N1 2.0450(12) 2_756 y
Pd2 N4 2.0369(12) 2_665 y
Pd2 N3 2.0391(12) 2_665 y
