#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:20:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179105 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/67/4306741.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_4306741
loop_
_publ_author_name
'Alen Hadzovic'
'Datong Song'
_publ_section_title
;
Syntheses, Structures, and Reactivities of Novel Palladium
β-Diiminato-Acetate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12010
_journal_page_last               12017
_journal_paper_doi               10.1021/ic801557c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C38 H40 N4 O4 Pd2'
_chemical_formula_weight         829.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9268(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0440(5)
_cell_length_b                   11.5241(4)
_cell_length_c                   18.4938(4)
_cell_measurement_reflns_used    13552
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     3597.78(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24340
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.725
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+0.9443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                5914
_reflns_number_total             8169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801557c_si_001_1.cif
_cod_data_source_block           Complex_1a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_database_code               4306741
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.668430(14) 0.77074(2) 0.041228(12) 0.02328(8) Uani 1 1 d . . .
Pd2 Pd 0.833012(14) 0.77903(2) -0.000357(12) 0.02254(8) Uani 1 1 d . . .
N1 N 0.64220(16) 0.6104(2) 0.06961(13) 0.0276(6) Uani 1 1 d . . .
N2 N 0.60799(16) 0.7464(2) -0.05752(14) 0.0270(6) Uani 1 1 d . . .
N3 N 0.84351(15) 0.6120(2) -0.02555(14) 0.0257(6) Uani 1 1 d . . .
N4 N 0.83630(15) 0.8265(2) -0.10305(13) 0.0258(6) Uani 1 1 d . . .
O1 O 0.73314(14) 0.7971(2) 0.14260(11) 0.0295(5) Uani 1 1 d . . .
O2 O 0.84997(14) 0.7427(2) 0.10944(11) 0.0291(5) Uani 1 1 d . . .
O3 O 0.68512(13) 0.94324(19) 0.01995(12) 0.0292(5) Uani 1 1 d . . .
O4 O 0.81785(13) 0.95082(19) 0.02548(11) 0.0270(5) Uani 1 1 d . . .
C1 C 0.6086(2) 0.4042(3) 0.0522(2) 0.0368(8) Uani 1 1 d . . .
H1A H 0.6514 0.3846 0.0913 0.055 Uiso 1 1 calc R . .
H1B H 0.6074 0.3473 0.0126 0.055 Uiso 1 1 calc R . .
H1C H 0.5579 0.4031 0.0714 0.055 Uiso 1 1 calc R . .
C2 C 0.62288(18) 0.5242(3) 0.02311(18) 0.0296(7) Uani 1 1 d . . .
C3 C 0.61242(19) 0.5388(3) -0.05274(17) 0.0321(8) Uani 1 1 d . . .
H3A H 0.6143 0.4709 -0.0816 0.039 Uiso 1 1 calc R . .
C4 C 0.59945(19) 0.6437(3) -0.08974(17) 0.0310(8) Uani 1 1 d . . .
C5 C 0.5699(2) 0.6372(3) -0.17076(17) 0.0397(9) Uani 1 1 d . . .
H5A H 0.5209 0.6823 -0.1816 0.060 Uiso 1 1 calc R . .
H5B H 0.5594 0.5560 -0.1848 0.060 Uiso 1 1 calc R . .
H5C H 0.6101 0.6689 -0.1983 0.060 Uiso 1 1 calc R . .
C6 C 0.6376(2) 0.5952(3) 0.14660(17) 0.0298(7) Uani 1 1 d . . .
C7 C 0.7020(2) 0.5555(3) 0.19410(18) 0.0362(8) Uani 1 1 d . . .
H7A H 0.7493 0.5340 0.1759 0.043 Uiso 1 1 calc R . .
C8 C 0.6975(2) 0.5471(3) 0.26770(19) 0.0427(9) Uani 1 1 d . . .
H8A H 0.7421 0.5210 0.3001 0.051 Uiso 1 1 calc R . .
C9 C 0.6287(2) 0.5763(3) 0.29477(19) 0.0445(10) Uani 1 1 d . . .
H9A H 0.6258 0.5700 0.3456 0.053 Uiso 1 1 calc R . .
C10 C 0.5642(2) 0.6147(3) 0.24783(19) 0.0417(9) Uani 1 1 d . . .
H10A H 0.5165 0.6338 0.2663 0.050 Uiso 1 1 calc R . .
C11 C 0.5684(2) 0.6257(3) 0.17359(18) 0.0343(8) Uani 1 1 d . . .
H11A H 0.5242 0.6539 0.1415 0.041 Uiso 1 1 calc R . .
C12 C 0.57770(19) 0.8493(3) -0.09526(16) 0.0304(8) Uani 1 1 d . . .
C13 C 0.6173(2) 0.9019(3) -0.14648(18) 0.0396(9) Uani 1 1 d . . .
H13A H 0.6649 0.8691 -0.1587 0.048 Uiso 1 1 calc R . .
C14 C 0.5868(3) 1.0036(4) -0.1802(2) 0.0514(11) Uani 1 1 d . . .
H14A H 0.6137 1.0397 -0.2159 0.062 Uiso 1 1 calc R . .
C15 C 0.5187(3) 1.0521(4) -0.1623(2) 0.0566(12) Uani 1 1 d . . .
H15A H 0.4988 1.1223 -0.1849 0.068 Uiso 1 1 calc R . .
C16 C 0.4792(3) 0.9986(4) -0.1115(2) 0.0526(11) Uani 1 1 d . . .
H16A H 0.4314 1.0311 -0.0997 0.063 Uiso 1 1 calc R . .
C17 C 0.5084(2) 0.8982(4) -0.07761(18) 0.0401(9) Uani 1 1 d . . .
H17A H 0.4811 0.8623 -0.0421 0.048 Uiso 1 1 calc R . .
C18 C 0.8147(2) 0.4408(3) -0.1047(2) 0.0386(9) Uani 1 1 d . . .
H18A H 0.8584 0.4029 -0.0735 0.058 Uiso 1 1 calc R . .
H18B H 0.8190 0.4246 -0.1560 0.058 Uiso 1 1 calc R . .
H18C H 0.7641 0.4109 -0.0930 0.058 Uiso 1 1 calc R . .
C19 C 0.81857(19) 0.5707(3) -0.09178(17) 0.0282(7) Uani 1 1 d . . .
C20 C 0.80086(19) 0.6395(3) -0.15417(17) 0.0306(8) Uani 1 1 d . . .
H20A H 0.7746 0.6025 -0.1966 0.037 Uiso 1 1 calc R . .
C21 C 0.81795(19) 0.7572(3) -0.16016(17) 0.0274(7) Uani 1 1 d . . .
C22 C 0.8202(2) 0.8052(3) -0.23626(17) 0.0382(9) Uani 1 1 d . . .
H22A H 0.8730 0.8371 -0.2394 0.057 Uiso 1 1 calc R . .
H22B H 0.7805 0.8667 -0.2463 0.057 Uiso 1 1 calc R . .
H22C H 0.8088 0.7429 -0.2722 0.057 Uiso 1 1 calc R . .
C23 C 0.87326(19) 0.5363(3) 0.03319(17) 0.0277(7) Uani 1 1 d . . .
C24 C 0.8255(2) 0.4536(3) 0.05978(19) 0.0357(8) Uani 1 1 d . . .
H24A H 0.7715 0.4466 0.0391 0.043 Uiso 1 1 calc R . .
C25 C 0.8564(2) 0.3812(3) 0.11659(19) 0.0435(9) Uani 1 1 d . . .
H25A H 0.8239 0.3238 0.1343 0.052 Uiso 1 1 calc R . .
C26 C 0.9348(3) 0.3927(4) 0.1473(2) 0.0487(10) Uani 1 1 d . . .
H26A H 0.9564 0.3424 0.1857 0.058 Uiso 1 1 calc R . .
C27 C 0.9815(2) 0.4775(4) 0.1222(2) 0.0462(10) Uani 1 1 d . . .
H27A H 1.0349 0.4867 0.1442 0.055 Uiso 1 1 calc R . .
C28 C 0.9510(2) 0.5488(3) 0.06534(18) 0.0341(8) Uani 1 1 d . . .
H28A H 0.9836 0.6067 0.0482 0.041 Uiso 1 1 calc R . .
C29 C 0.87106(19) 0.9384(3) -0.11271(16) 0.0266(7) Uani 1 1 d . . .
C30 C 0.8251(2) 1.0328(3) -0.13830(18) 0.0352(8) Uani 1 1 d . . .
H30A H 0.7694 1.0246 -0.1503 0.042 Uiso 1 1 calc R . .
C31 C 0.8605(2) 1.1386(3) -0.14636(19) 0.0426(9) Uani 1 1 d . . .
H31A H 0.8288 1.2028 -0.1644 0.051 Uiso 1 1 calc R . .
C32 C 0.9414(2) 1.1528(4) -0.12864(18) 0.0407(9) Uani 1 1 d . . .
H32A H 0.9653 1.2260 -0.1348 0.049 Uiso 1 1 calc R . .
C33 C 0.9870(2) 1.0593(3) -0.10195(18) 0.0364(9) Uani 1 1 d . . .
H33A H 1.0426 1.0681 -0.0893 0.044 Uiso 1 1 calc R . .
C34 C 0.95171(19) 0.9520(3) -0.09352(17) 0.0316(8) Uani 1 1 d . . .
H34A H 0.9832 0.8881 -0.0745 0.038 Uiso 1 1 calc R . .
C35 C 0.8046(2) 0.7686(3) 0.15570(17) 0.0267(7) Uani 1 1 d . . .
C36 C 0.8427(2) 0.7627(3) 0.23444(18) 0.0384(9) Uani 1 1 d . . .
H36A H 0.8020 0.7727 0.2666 0.058 Uiso 1 1 calc R . .
H36B H 0.8823 0.8245 0.2439 0.058 Uiso 1 1 calc R . .
H36C H 0.8684 0.6871 0.2438 0.058 Uiso 1 1 calc R . .
C37 C 0.7501(2) 0.9953(3) 0.02299(15) 0.0264(7) Uani 1 1 d . . .
C38 C 0.7455(2) 1.1267(3) 0.0234(2) 0.0409(9) Uani 1 1 d . . .
H38A H 0.7114 1.1532 -0.0205 0.061 Uiso 1 1 calc R . .
H38B H 0.7988 1.1591 0.0240 0.061 Uiso 1 1 calc R . .
H38C H 0.7234 1.1525 0.0668 0.061 Uiso 1 1 calc R . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N1 90.25(11) . . ?
N2 Pd1 O3 91.64(10) . . ?
N1 Pd1 O3 172.77(10) . . ?
N2 Pd1 O1 178.78(9) . . ?
N1 Pd1 O1 90.49(10) . . ?
O3 Pd1 O1 87.74(9) . . ?
N4 Pd2 N3 91.55(11) . . ?
N4 Pd2 O2 169.55(10) . . ?
N3 Pd2 O2 91.67(10) . . ?
N4 Pd2 O4 88.75(10) . . ?
N3 Pd2 O4 177.95(9) . . ?
O2 Pd2 O4 88.39(9) . . ?
C2 N1 C6 120.4(3) . . ?
C2 N1 Pd1 124.7(2) . . ?
C6 N1 Pd1 114.6(2) . . ?
C4 N2 C12 120.6(3) . . ?
C4 N2 Pd1 123.4(2) . . ?
C12 N2 Pd1 115.8(2) . . ?
C19 N3 C23 121.1(3) . . ?
C19 N3 Pd2 122.2(2) . . ?
C23 N3 Pd2 116.4(2) . . ?
C21 N4 C29 119.7(3) . . ?
C21 N4 Pd2 124.2(2) . . ?
C29 N4 Pd2 115.58(18) . . ?
C35 O1 Pd1 121.4(2) . . ?
C35 O2 Pd2 127.2(2) . . ?
C37 O3 Pd1 126.9(2) . . ?
C37 O4 Pd2 121.8(2) . . ?
N1 C2 C3 123.1(3) . . ?
N1 C2 C1 119.4(3) . . ?
C3 C2 C1 117.5(3) . . ?
C4 C3 C2 125.9(3) . . ?
N2 C4 C3 123.7(3) . . ?
N2 C4 C5 119.4(3) . . ?
C3 C4 C5 116.8(3) . . ?
C7 C6 C11 119.6(3) . . ?
C7 C6 N1 121.2(3) . . ?
C11 C6 N1 119.2(3) . . ?
C8 C7 C6 120.2(3) . . ?
C7 C8 C9 120.5(4) . . ?
C10 C9 C8 119.6(3) . . ?
C9 C10 C11 120.4(3) . . ?
C6 C11 C10 119.6(3) . . ?
C13 C12 C17 119.8(3) . . ?
C13 C12 N2 121.4(3) . . ?
C17 C12 N2 118.8(3) . . ?
C12 C13 C14 119.4(3) . . ?
C15 C14 C13 120.7(4) . . ?
C14 C15 C16 119.5(4) . . ?
C15 C16 C17 120.6(4) . . ?
C16 C17 C12 120.0(4) . . ?
N3 C19 C20 124.3(3) . . ?
N3 C19 C18 120.1(3) . . ?
C20 C19 C18 115.5(3) . . ?
C21 C20 C19 126.4(3) . . ?
N4 C21 C20 123.4(3) . . ?
N4 C21 C22 119.1(3) . . ?
C20 C21 C22 117.4(3) . . ?
C28 C23 C24 119.6(3) . . ?
C28 C23 N3 118.7(3) . . ?
C24 C23 N3 121.6(3) . . ?
C23 C24 C25 120.1(3) . . ?
C26 C25 C24 119.9(4) . . ?
C27 C26 C25 119.9(4) . . ?
C28 C27 C26 120.3(4) . . ?
C27 C28 C23 120.2(4) . . ?
C34 C29 C30 119.7(3) . . ?
C34 C29 N4 118.8(3) . . ?
C30 C29 N4 121.5(3) . . ?
C31 C30 C29 119.8(3) . . ?
C30 C31 C32 121.1(4) . . ?
C33 C32 C31 119.1(4) . . ?
C32 C33 C34 120.2(3) . . ?
C29 C34 C33 120.1(3) . . ?
O1 C35 O2 126.9(3) . . ?
O1 C35 C36 118.4(3) . . ?
O2 C35 C36 114.8(3) . . ?
O3 C37 O4 127.3(3) . . ?
O3 C37 C38 115.7(3) . . ?
O4 C37 C38 117.0(3) . . ?
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
Pd1 N2 1.989(3) . ?
Pd1 N1 1.989(3) . ?
Pd1 O3 2.054(2) . ?
Pd1 O1 2.062(2) . ?
Pd2 N4 1.985(3) . ?
Pd2 N3 1.994(3) . ?
Pd2 O2 2.054(2) . ?
Pd2 O4 2.061(2) . ?
N1 C2 1.325(4) . ?
N1 C6 1.447(4) . ?
N2 C4 1.323(4) . ?
N2 C12 1.435(4) . ?
N3 C19 1.328(4) . ?
N3 C23 1.431(4) . ?
N4 C21 1.326(4) . ?
N4 C29 1.441(4) . ?
O1 C35 1.252(4) . ?
O2 C35 1.266(4) . ?
O3 C37 1.254(4) . ?
O4 C37 1.259(4) . ?
C1 C2 1.515(5) . ?
C2 C3 1.400(5) . ?
C3 C4 1.392(5) . ?
C4 C5 1.516(4) . ?
C6 C7 1.385(5) . ?
C6 C11 1.387(5) . ?
C7 C8 1.377(5) . ?
C8 C9 1.378(5) . ?
C9 C10 1.376(5) . ?
C10 C11 1.391(5) . ?
C12 C13 1.377(5) . ?
C12 C17 1.388(5) . ?
C13 C14 1.394(5) . ?
C14 C15 1.370(6) . ?
C15 C16 1.375(6) . ?
C16 C17 1.376(5) . ?
C18 C19 1.516(5) . ?
C19 C20 1.398(5) . ?
C20 C21 1.395(5) . ?
C21 C22 1.518(5) . ?
C23 C28 1.384(5) . ?
C23 C24 1.387(5) . ?
C24 C25 1.388(5) . ?
C25 C26 1.384(5) . ?
C26 C27 1.381(6) . ?
C27 C28 1.378(5) . ?
C29 C34 1.380(4) . ?
C29 C30 1.385(5) . ?
C30 C31 1.377(5) . ?
C31 C32 1.383(5) . ?
C32 C33 1.379(5) . ?
C33 C34 1.393(5) . ?
C35 C36 1.512(4) . ?
C37 C38 1.515(5) . ?
