#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:04:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178633 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/44/4074450.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_4074450
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
_chemical_formula_moiety         'C34 H48 N2 O2 Pd'
_chemical_formula_sum            'C34 H48 N2 O2 Pd'
_chemical_formula_weight         623.14
_chemical_melting_point          500
_chemical_name_systematic
; 
 (2-(2,6-di-isopropylphenylimino)-4-
 (2,6-di-isopropylphenylimino)pent-2-ene-N,N')-acetylacetonate-
 palladium(ii)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.00
_cell_angle_beta                 121.351(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.0185(5)
_cell_length_b                   10.6251(1)
_cell_length_c                   20.5768(3)
_cell_measurement_reflns_used    62632
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.91
_cell_volume                     6538.29(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            89328
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack, Otwinowski (1997)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         10856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0291P)²+10.4890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                9510
_reflns_number_total             10856
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0606486si20060718_110709.cif
_cod_data_source_block           4
_cod_depositor_comments
;
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_original_cell_volume        6538.29(15)
_cod_database_code               4074450
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
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 0.11535(5) -0.10419(14) -0.47493(8) 0.0166(3) Uani 1 1 d .
H1A H 0.0847 -0.1048 -0.5161 0.025 Uiso 1 1 calc R
H1B H 0.1230 -0.1853 -0.4509 0.025 Uiso 1 1 calc R
H1C H 0.1344 -0.0852 -0.4943 0.025 Uiso 1 1 calc R
C2 C 0.12148(5) -0.00556(13) -0.41752(8) 0.0120(2) Uani 1 1 d .
C3 C 0.13664(5) -0.04693(13) -0.34319(8) 0.0135(2) Uani 1 1 d .
H3 H 0.1390 -0.1336 -0.3357 0.016 Uiso 1 1 calc R
C4 C 0.14859(5) 0.02696(13) -0.27913(8) 0.0125(2) Uani 1 1 d .
C5 C 0.16703(5) -0.04083(14) -0.20393(8) 0.0184(3) Uani 1 1 d .
H5A H 0.1961 -0.0081 -0.1680 0.028 Uiso 1 1 calc R
H5B H 0.1693 -0.1292 -0.2111 0.028 Uiso 1 1 calc R
H5C H 0.1474 -0.0282 -0.1850 0.028 Uiso 1 1 calc R
C6 C 0.09974(5) 0.14650(13) -0.51624(8) 0.0123(2) Uani 1 1 d .
C7 C 0.13262(5) 0.18836(14) -0.53088(8) 0.0149(3) Uani 1 1 d .
C8 C 0.11900(5) 0.23357(15) -0.60360(9) 0.0189(3) Uani 1 1 d .
H8 H 0.1403 0.2617 -0.6142 0.023 Uiso 1 1 calc R
C9 C 0.07403(6) 0.23697(16) -0.66017(9) 0.0223(3) Uani 1 1 d .
H9 H 0.0653 0.2693 -0.7079 0.027 Uiso 1 1 calc R
C10 C 0.04208(5) 0.19192(16) -0.64525(9) 0.0205(3) Uani 1 1 d .
H10 H 0.0121 0.1927 -0.6838 0.025 Uiso 1 1 calc R
C11 C 0.05417(5) 0.14541(14) -0.57344(8) 0.0144(3) Uani 1 1 d .
C12 C 0.18207(5) 0.18774(16) -0.46949(9) 0.0200(3) Uani 1 1 d .
H12 H 0.1853 0.1438 -0.4250 0.024 Uiso 1 1 calc R
C13 C 0.19928(7) 0.3222(2) -0.44536(12) 0.0334(4) Uani 1 1 d .
H13A H 0.2304 0.3200 -0.4066 0.050 Uiso 1 1 calc R
H13B H 0.1828 0.3627 -0.4258 0.050 Uiso 1 1 calc R
H13C H 0.1954 0.3682 -0.4885 0.050 Uiso 1 1 calc R
C14 C 0.21008(6) 0.11722(18) -0.49540(11) 0.0271(4) Uani 1 1 d .
H14A H 0.2410 0.1187 -0.4554 0.041 Uiso 1 1 calc R
H14B H 0.2068 0.1572 -0.5399 0.041 Uiso 1 1 calc R
H14C H 0.2000 0.0316 -0.5071 0.041 Uiso 1 1 calc R
C15 C 0.01836(5) 0.09902(15) -0.55850(8) 0.0170(3) Uani 1 1 d .
H15 H 0.0334 0.0520 -0.5105 0.020 Uiso 1 1 calc R
C16 C -0.00626(7) 0.20888(19) -0.54885(13) 0.0318(4) Uani 1 1 d .
H16A H -0.0286 0.1772 -0.5393 0.048 Uiso 1 1 calc R
H16B H -0.0203 0.2587 -0.5944 0.048 Uiso 1 1 calc R
H16C H 0.0146 0.2599 -0.5067 0.048 Uiso 1 1 calc R
C17 C -0.01481(6) 0.00974(19) -0.62078(10) 0.0278(4) Uani 1 1 d .
H17A H -0.0367 -0.0173 -0.6091 0.042 Uiso 1 1 calc R
H17B H 0.0009 -0.0622 -0.6234 0.042 Uiso 1 1 calc R
H17C H -0.0294 0.0527 -0.6688 0.042 Uiso 1 1 calc R
C18 C 0.16200(5) 0.21663(13) -0.20914(8) 0.0140(2) Uani 1 1 d .
C19 C 0.13304(5) 0.24308(14) -0.18281(8) 0.0171(3) Uani 1 1 d .
C20 C 0.15009(6) 0.30884(17) -0.11441(9) 0.0248(3) Uani 1 1 d .
H20 H 0.1314 0.3272 -0.0960 0.030 Uiso 1 1 calc R
C21 C 0.19439(6) 0.34727(18) -0.07346(10) 0.0282(4) Uani 1 1 d .
H21 H 0.2054 0.3903 -0.0278 0.034 Uiso 1 1 calc R
C22 C 0.22227(6) 0.32129(17) -0.10090(10) 0.0255(3) Uani 1 1 d .
H22 H 0.2519 0.3474 -0.0732 0.031 Uiso 1 1 calc R
C23 C 0.20671(5) 0.25678(15) -0.16923(9) 0.0188(3) Uani 1 1 d .
C24 C 0.08414(5) 0.20389(17) -0.22760(9) 0.0211(3) Uani 1 1 d .
H24 H 0.0799 0.1485 -0.2690 0.025 Uiso 1 1 calc R
C25 C 0.05334(6) 0.3176(2) -0.26343(12) 0.0358(5) Uani 1 1 d .
H25A H 0.0228 0.2899 -0.2913 0.054 Uiso 1 1 calc R
H25B H 0.0603 0.3594 -0.2973 0.054 Uiso 1 1 calc R
H25C H 0.0576 0.3748 -0.2241 0.054 Uiso 1 1 calc R
C26 C 0.07075(6) 0.13032(19) -0.17869(10) 0.0269(4) Uani 1 1 d .
H26A H 0.0398 0.1074 -0.2089 0.040 Uiso 1 1 calc R
H26B H 0.0754 0.1817 -0.1368 0.040 Uiso 1 1 calc R
H26C H 0.0887 0.0556 -0.1596 0.040 Uiso 1 1 calc R
C27 C 0.23735(6) 0.23608(19) -0.20018(11) 0.0283(4) Uani 1 1 d .
H27 H 0.2215 0.1823 -0.2453 0.034 Uiso 1 1 calc R
C28 C 0.24697(7) 0.3620(3) -0.22513(14) 0.0478(6) Uani 1 1 d .
H28A H 0.2662 0.3483 -0.2447 0.072 Uiso 1 1 calc R
H28B H 0.2613 0.4179 -0.1823 0.072 Uiso 1 1 calc R
H28C H 0.2194 0.3987 -0.2641 0.072 Uiso 1 1 calc R
C29 C 0.28084(7) 0.1695(2) -0.14284(13) 0.0351(4) Uani 1 1 d .
H29A H 0.2990 0.1582 -0.1647 0.053 Uiso 1 1 calc R
H29B H 0.2740 0.0889 -0.1303 0.053 Uiso 1 1 calc R
H29C H 0.2967 0.2196 -0.0976 0.053 Uiso 1 1 calc R
C30 C 0.05869(8) 0.54536(18) -0.54534(11) 0.0346(4) Uani 1 1 d .
H30A H 0.0730 0.5215 -0.5726 0.052 Uiso 1 1 calc R
H30B H 0.0589 0.6354 -0.5412 0.052 Uiso 1 1 calc R
H30C H 0.0284 0.5156 -0.5722 0.052 Uiso 1 1 calc R
C31 C 0.08357(6) 0.48815(15) -0.46684(9) 0.0204(3) Uani 1 1 d .
C32 C 0.09446(6) 0.56260(14) -0.40378(10) 0.0218(3) Uani 1 1 d .
H32 H 0.0859 0.6467 -0.4125 0.026 Uiso 1 1 calc R
C33 C 0.11720(6) 0.52077(14) -0.32852(10) 0.0197(3) Uani 1 1 d .
C34 C 0.12888(8) 0.61134(16) -0.26451(11) 0.0314(4) Uani 1 1 d .
H34A H 0.1213 0.5747 -0.2301 0.047 Uiso 1 1 calc R
H34B H 0.1125 0.6882 -0.2849 0.047 Uiso 1 1 calc R
H34C H 0.1604 0.6289 -0.2378 0.047 Uiso 1 1 calc R
N1 N 0.11279(4) 0.11365(11) -0.43947(6) 0.0112(2) Uani 1 1 d .
N2 N 0.14530(4) 0.15156(11) -0.28034(6) 0.0114(2) Uani 1 1 d .
O1 O 0.09221(4) 0.37142(10) -0.46569(6) 0.0210(2) Uani 1 1 d .
O2 O 0.13027(4) 0.40870(10) -0.30585(6) 0.0203(2) Uani 1 1 d .
Pd1 Pd 0.120170(4) 0.259336(9) -0.372868(6) 0.01230(3) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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_publ_flag
N1 C2 C3 124.07(13) y
N1 C2 C1 118.87(12) y
C3 C2 C1 117.06(12) y
C4 C3 C2 127.55(13) y
N2 C4 C3 124.17(13) y
N2 C4 C5 118.71(13) y
C3 C4 C5 117.12(12) y
C7 C6 C11 121.50(13) y
C7 C6 N1 118.93(12) y
C11 C6 N1 119.38(12) y
C8 C7 C6 118.47(14) y
C8 C7 C12 119.79(13) y
C6 C7 C12 121.72(13) y
C9 C8 C7 120.84(14) y
C8 C9 C10 119.85(14) y
C9 C10 C11 121.26(15) y
C10 C11 C6 118.01(13) y
C10 C11 C15 120.01(13) y
C6 C11 C15 121.97(13) y
C7 C12 C13 110.57(14) y
C7 C12 C14 111.77(13) y
C13 C12 C14 110.72(14) y
C11 C15 C16 111.11(13) y
C11 C15 C17 112.21(13) y
C16 C15 C17 110.45(15) y
C23 C18 C19 121.54(13) y
C23 C18 N2 118.68(13) y
C19 C18 N2 119.73(13) y
C20 C19 C18 118.23(14) y
C20 C19 C24 120.25(14) y
C18 C19 C24 121.52(13) y
C21 C20 C19 121.07(16) y
C22 C21 C20 119.74(15) y
C21 C22 C23 121.33(16) y
C22 C23 C18 118.08(15) y
C22 C23 C27 120.14(15) y
C18 C23 C27 121.74(14) y
C19 C24 C26 112.06(13) y
C19 C24 C25 111.42(15) y
C26 C24 C25 109.91(15) y
C23 C27 C29 112.31(16) y
C23 C27 C28 109.87(17) y
C29 C27 C28 110.99(16) y
O1 C31 C32 126.04(15) y
O1 C31 C30 114.31(15) y
C32 C31 C30 119.64(15) y
C31 C32 C33 125.07(14) y
O2 C33 C32 126.37(15) y
O2 C33 C34 113.25(15) y
C32 C33 C34 120.38(14) y
C2 N1 C6 119.40(11) y
C2 N1 Pd1 125.66(9) y
C6 N1 Pd1 114.80(9) y
C4 N2 C18 118.30(12) y
C4 N2 Pd1 125.58(10) y
C18 N2 Pd1 116.10(9) y
C31 O1 Pd1 125.83(11) y
C33 O2 Pd1 125.84(10) y
N2 Pd1 N1 92.61(5) y
N2 Pd1 O2 88.03(5) y
N1 Pd1 O2 177.20(5) y
N2 Pd1 O1 177.06(5) y
N1 Pd1 O1 88.97(5) y
O2 Pd1 O1 90.51(5) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.5086(19) y
C2 N1 1.3258(17) y
C2 C3 1.4034(19) y
C3 C4 1.3981(19) y
C4 N2 1.3279(18) y
C4 C5 1.5134(19) y
C6 C7 1.406(2) y
C6 C11 1.406(2) y
C6 N1 1.4403(17) y
C7 C8 1.398(2) y
C7 C12 1.522(2) y
C8 C9 1.389(2) y
C9 C10 1.390(2) y
C10 C11 1.398(2) y
C11 C15 1.520(2) y
C12 C13 1.529(3) y
C12 C14 1.534(2) y
C15 C16 1.524(2) y
C15 C17 1.531(2) y
C18 C23 1.404(2) y
C18 C19 1.405(2) y
C18 N2 1.4404(18) y
C19 C20 1.397(2) y
C19 C24 1.521(2) y
C20 C21 1.387(3) y
C21 C22 1.386(3) y
C22 C23 1.395(2) y
C23 C27 1.522(2) y
C24 C26 1.528(2) y
C24 C25 1.529(3) y
C27 C29 1.530(3) y
C27 C28 1.532(3) y
C30 C31 1.508(2) y
C31 O1 1.2739(19) y
C31 C32 1.393(2) y
C32 C33 1.395(2) y
C33 O2 1.2739(19) y
C33 C34 1.506(2) y
N1 Pd1 1.9932(11) y
N2 Pd1 1.9919(11) y
O1 Pd1 2.0196(11) y
O2 Pd1 2.0094(11) y
