#------------------------------------------------------------------------------
#$Date: 2018-01-28 01:56:17 +0200 (Sun, 28 Jan 2018) $
#$Revision: 205782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/21/7012187.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_7012187
loop_
_publ_author_name
'Guzei, Ilia A.'
'Li, Kelin'
'Bikzhanova, Galina A.'
'Darkwa, James'
'Mapolie, Selwyn F.'
_publ_section_title
;
 Benzenedicarbonyl and benzenetricarbonyl linker pyrazolyl complexes of
 palladium(II): synthesis, X-ray structures and evaluation as ethylene
 polymerisation catalysts
;
_journal_coden_ASTM              DTARAF
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              715
_journal_page_last               722
_journal_paper_doi               10.1039/b208376k
_journal_year                    2003
_chemical_formula_sum            'C24.5 H25 Cl1.5 N6 O3'
_chemical_formula_weight         504.68
_space_group_IT_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.1070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.360(2)
_cell_length_b                   17.3164(15)
_cell_length_c                   16.6335(15)
_cell_measurement_temperature    296(2)
_cell_volume                     5294.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4148
_diffrn_reflns_theta_full        23.99
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.9360
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0550
_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/[σ²(Fo²)+(0.0587P)²+5.9411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                3185
_reflns_number_total             4148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208376k.txt
_cod_data_source_block           daro
_cod_original_formula_sum        'C24.50 H25 Cl1.50 N6 O3'
_cod_database_code               7012187
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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.06156(9) 0.44196(10) 0.21575(13) 0.0344(4) Uani 1 1 d . . .
O2 O 1.08397(10) 0.14795(10) 0.02846(15) 0.0445(5) Uani 1 1 d . . .
O3 O 0.88915(9) 0.16008(10) 0.16572(14) 0.0349(4) Uani 1 1 d . . .
N1 N 1.07477(10) 0.44492(11) 0.09227(14) 0.0234(5) Uani 1 1 d . . .
N2 N 1.06335(11) 0.40956(12) 0.00900(15) 0.0288(5) Uani 1 1 d . . .
N3 N 0.97390(10) 0.09020(11) -0.07014(15) 0.0284(5) Uani 1 1 d . . .
N4 N 0.90379(11) 0.08412(13) -0.10173(17) 0.0362(5) Uani 1 1 d . . .
N5 N 0.83496(10) 0.27772(11) 0.11694(14) 0.0253(5) Uani 1 1 d . . .
N6 N 0.82181(10) 0.34529(11) 0.06303(15) 0.0268(5) Uani 1 1 d . . .
C1 C 1.01716(12) 0.33157(13) 0.11063(17) 0.0228(5) Uani 1 1 d . . .
C2 C 1.03294(12) 0.27362(13) 0.06935(17) 0.0257(6) Uani 1 1 d . . .
H2 H 1.0669 0.2827 0.0584 0.031 Uiso 1 1 calc R . .
C3 C 0.99862(12) 0.20189(13) 0.04399(18) 0.0243(6) Uani 1 1 d . . .
C4 C 0.94969(12) 0.18791(14) 0.06375(17) 0.0250(5) Uani 1 1 d . . .
H4 H 0.9277 0.1397 0.0492 0.030 Uiso 1 1 calc R . .
C5 C 0.93350(12) 0.24563(13) 0.10523(17) 0.0236(5) Uani 1 1 d . . .
C6 C 0.96698(12) 0.31752(13) 0.12799(17) 0.0225(5) Uani 1 1 d . . .
H6 H 0.9557 0.3563 0.1549 0.027 Uiso 1 1 calc R . .
C7 C 1.05296(12) 0.40956(14) 0.14484(18) 0.0249(5) Uani 1 1 d . . .
C8 C 1.12394(15) 0.57157(15) 0.1921(2) 0.0396(7) Uani 1 1 d . . .
H8A H 1.1481 0.6163 0.1919 0.059 Uiso 1 1 calc R . .
H8B H 1.1551 0.5464 0.2573 0.059 Uiso 1 1 calc R . .
H8C H 1.0797 0.5871 0.1799 0.059 Uiso 1 1 calc R . .
C9 C 1.10665(12) 0.51724(14) 0.11031(18) 0.0274(6) Uani 1 1 d . . .
C10 C 1.11621(13) 0.52613(14) 0.03873(19) 0.0307(6) Uani 1 1 d . . .
H10 H 1.1367 0.5686 0.0309 0.037 Uiso 1 1 calc R . .
C11 C 1.08907(13) 0.45840(14) -0.02252(19) 0.0292(6) Uani 1 1 d . . .
C12 C 1.08657(16) 0.43802(18) -0.1115(2) 0.0449(7) Uani 1 1 d . . .
H12A H 1.1344 0.4240 -0.0879 0.067 Uiso 1 1 calc R . .
H12B H 1.0696 0.4816 -0.1565 0.067 Uiso 1 1 calc R . .
H12C H 1.0541 0.3953 -0.1474 0.067 Uiso 1 1 calc R . .
C13 C 1.02270(13) 0.14515(14) 0.0024(2) 0.0299(6) Uani 1 1 d . . .
C14 C 1.05645(15) 0.02868(16) -0.1039(2) 0.0399(7) Uani 1 1 d . . .
H14A H 1.0526 -0.0129 -0.1452 0.060 Uiso 1 1 calc R . .
H14B H 1.0955 0.0183 -0.0333 0.060 Uiso 1 1 calc R . .
H14C H 1.0661 0.0760 -0.1237 0.060 Uiso 1 1 calc R . .
C15 C 0.98690(13) 0.03602(14) -0.11876(19) 0.0299(6) Uani 1 1 d . . .
C16 C 0.92483(14) -0.00460(16) -0.1798(2) 0.0362(6) Uani 1 1 d . . .
H16 H 0.9163 -0.0454 -0.2223 0.043 Uiso 1 1 calc R . .
C17 C 0.87510(14) 0.02646(16) -0.1670(2) 0.0392(7) Uani 1 1 d . . .
C18 C 0.79907(16) -0.0002(2) -0.2168(3) 0.0646(10) Uani 1 1 d . . .
H18A H 0.8004 -0.0490 -0.1883 0.097 Uiso 1 1 calc R . .
H18B H 0.7735 -0.0058 -0.2889 0.097 Uiso 1 1 calc R . .
H18C H 0.7745 0.0371 -0.2051 0.097 Uiso 1 1 calc R . .
C19 C 0.88536(12) 0.22334(14) 0.13178(17) 0.0248(5) Uani 1 1 d . . .
C20 C 0.78929(15) 0.20490(17) 0.2008(2) 0.0408(7) Uani 1 1 d . . .
H20A H 0.7580 0.2165 0.2183 0.061 Uiso 1 1 calc R . .
H20B H 0.8377 0.1952 0.2620 0.061 Uiso 1 1 calc R . .
H20C H 0.7715 0.1600 0.1579 0.061 Uiso 1 1 calc R . .
C21 C 0.79038(13) 0.27162(15) 0.14534(18) 0.0293(6) Uani 1 1 d . . .
C22 C 0.74965(14) 0.33656(15) 0.1099(2) 0.0338(6) Uani 1 1 d . . .
H22 H 0.7145 0.3501 0.1172 0.041 Uiso 1 1 calc R . .
C23 C 0.77039(13) 0.38014(14) 0.05970(19) 0.0296(6) Uani 1 1 d . . .
C24 C 0.74047(14) 0.45628(15) 0.0060(2) 0.0412(7) Uani 1 1 d . . .
H24A H 0.7661 0.4727 -0.0191 0.062 Uiso 1 1 calc R . .
H24B H 0.7465 0.4940 0.0530 0.062 Uiso 1 1 calc R . .
H24C H 0.6897 0.4507 -0.0502 0.062 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'
Cl Cl 0.1484 0.1585 '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 N1 C9 111.20(18) . . ?
N2 N1 C7 120.95(18) . . ?
C9 N1 C7 127.8(2) . . ?
C11 N2 N1 105.12(19) . . ?
N4 N3 C15 111.17(19) . . ?
N4 N3 C13 121.53(19) . . ?
C15 N3 C13 127.3(2) . . ?
C17 N4 N3 104.65(19) . . ?
C21 N5 N6 111.76(19) . . ?
C21 N5 C19 127.8(2) . . ?
N6 N5 C19 120.37(18) . . ?
C23 N6 N5 104.26(19) . . ?
C2 C1 C6 119.4(2) . . ?
C2 C1 C7 125.5(2) . . ?
C6 C1 C7 115.0(2) . . ?
C1 C2 C3 121.0(2) . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 C13 126.4(2) . . ?
C2 C3 C13 114.5(2) . . ?
C3 C4 C5 120.4(2) . . ?
C6 C5 C4 119.8(2) . . ?
C6 C5 C19 123.4(2) . . ?
C4 C5 C19 116.5(2) . . ?
C1 C6 C5 120.3(2) . . ?
O1 C7 N1 120.2(2) . . ?
O1 C7 C1 120.4(2) . . ?
N1 C7 C1 119.3(2) . . ?
C10 C9 N1 105.7(2) . . ?
C10 C9 C8 129.4(2) . . ?
N1 C9 C8 124.9(2) . . ?
C9 C10 C11 107.2(2) . . ?
N2 C11 C10 110.8(2) . . ?
N2 C11 C12 119.7(2) . . ?
C10 C11 C12 129.5(2) . . ?
O2 C13 N3 119.2(2) . . ?
O2 C13 C3 120.4(2) . . ?
N3 C13 C3 120.4(2) . . ?
C16 C15 N3 105.7(2) . . ?
C16 C15 C14 129.6(2) . . ?
N3 C15 C14 124.7(2) . . ?
C15 C16 C17 106.9(2) . . ?
N4 C17 C16 111.5(2) . . ?
N4 C17 C18 121.2(2) . . ?
C16 C17 C18 127.3(2) . . ?
O3 C19 N5 120.0(2) . . ?
O3 C19 C5 121.4(2) . . ?
N5 C19 C5 118.5(2) . . ?
C22 C21 N5 105.2(2) . . ?
C22 C21 C20 129.7(2) . . ?
N5 C21 C20 125.0(2) . . ?
C21 C22 C23 107.2(2) . . ?
N6 C23 C22 111.5(2) . . ?
N6 C23 C24 120.4(2) . . ?
C22 C23 C24 128.0(2) . . ?
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
O1 C7 1.206(3) . ?
O2 C13 1.214(3) . ?
O3 C19 1.210(3) . ?
N1 N2 1.381(3) . ?
N1 C9 1.392(3) . ?
N1 C7 1.396(3) . ?
N2 C11 1.319(3) . ?
N3 N4 1.381(3) . ?
N3 C15 1.389(3) . ?
N3 C13 1.401(3) . ?
N4 C17 1.314(3) . ?
N5 C21 1.388(3) . ?
N5 N6 1.388(3) . ?
N5 C19 1.405(3) . ?
N6 C23 1.315(3) . ?
C1 C2 1.388(3) . ?
C1 C6 1.391(3) . ?
C1 C7 1.503(3) . ?
C2 C3 1.395(3) . ?
C3 C4 1.392(3) . ?
C3 C13 1.497(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.393(3) . ?
C5 C19 1.490(3) . ?
C8 C9 1.491(4) . ?
C9 C10 1.349(3) . ?
C10 C11 1.421(3) . ?
C11 C12 1.487(4) . ?
C14 C15 1.490(3) . ?
C15 C16 1.346(3) . ?
C16 C17 1.411(4) . ?
C17 C18 1.496(4) . ?
C20 C21 1.489(4) . ?
C21 C22 1.351(4) . ?
C22 C23 1.415(4) . ?
C23 C24 1.501(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 N2 C11 1.2(2) . . . . ?
C7 N1 N2 C11 179.1(2) . . . . ?
C15 N3 N4 C17 1.1(3) . . . . ?
C13 N3 N4 C17 -178.6(2) . . . . ?
C21 N5 N6 C23 0.6(2) . . . . ?
C19 N5 N6 C23 177.1(2) . . . . ?
C6 C1 C2 C3 0.7(3) . . . . ?
C7 C1 C2 C3 177.2(2) . . . . ?
C1 C2 C3 C4 -2.1(3) . . . . ?
C1 C2 C3 C13 -178.8(2) . . . . ?
C2 C3 C4 C5 2.0(3) . . . . ?
C13 C3 C4 C5 178.3(2) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C3 C4 C5 C19 -175.1(2) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C7 C1 C6 C5 -176.1(2) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
C19 C5 C6 C1 173.2(2) . . . . ?
N2 N1 C7 O1 -178.1(2) . . . . ?
C9 N1 C7 O1 -0.6(4) . . . . ?
N2 N1 C7 C1 0.6(3) . . . . ?
C9 N1 C7 C1 178.0(2) . . . . ?
C2 C1 C7 O1 -147.4(2) . . . . ?
C6 C1 C7 O1 29.2(3) . . . . ?
C2 C1 C7 N1 34.0(3) . . . . ?
C6 C1 C7 N1 -149.4(2) . . . . ?
N2 N1 C9 C10 -1.1(2) . . . . ?
C7 N1 C9 C10 -178.8(2) . . . . ?
N2 N1 C9 C8 177.9(2) . . . . ?
C7 N1 C9 C8 0.2(4) . . . . ?
N1 C9 C10 C11 0.4(3) . . . . ?
C8 C9 C10 C11 -178.4(2) . . . . ?
N1 N2 C11 C10 -0.9(3) . . . . ?
N1 N2 C11 C12 179.1(2) . . . . ?
C9 C10 C11 N2 0.3(3) . . . . ?
C9 C10 C11 C12 -179.7(3) . . . . ?
N4 N3 C13 O2 179.4(2) . . . . ?
C15 N3 C13 O2 -0.2(4) . . . . ?
N4 N3 C13 C3 -3.1(3) . . . . ?
C15 N3 C13 C3 177.3(2) . . . . ?
C4 C3 C13 O2 -146.9(3) . . . . ?
C2 C3 C13 O2 29.4(3) . . . . ?
C4 C3 C13 N3 35.6(4) . . . . ?
C2 C3 C13 N3 -148.0(2) . . . . ?
N4 N3 C15 C16 -0.8(3) . . . . ?
C13 N3 C15 C16 178.8(2) . . . . ?
N4 N3 C15 C14 178.2(2) . . . . ?
C13 N3 C15 C14 -2.1(4) . . . . ?
N3 C15 C16 C17 0.3(3) . . . . ?
C14 C15 C16 C17 -178.7(3) . . . . ?
N3 N4 C17 C16 -0.9(3) . . . . ?
N3 N4 C17 C18 178.2(3) . . . . ?
C15 C16 C17 N4 0.4(3) . . . . ?
C15 C16 C17 C18 -178.6(3) . . . . ?
C21 N5 C19 O3 6.4(4) . . . . ?
N6 N5 C19 O3 -169.5(2) . . . . ?
C21 N5 C19 C5 -173.4(2) . . . . ?
N6 N5 C19 C5 10.8(3) . . . . ?
C6 C5 C19 O3 -137.8(2) . . . . ?
C4 C5 C19 O3 36.4(3) . . . . ?
C6 C5 C19 N5 41.9(3) . . . . ?
C4 C5 C19 N5 -143.8(2) . . . . ?
N6 N5 C21 C22 -0.8(3) . . . . ?
C19 N5 C21 C22 -177.0(2) . . . . ?
N6 N5 C21 C20 177.9(2) . . . . ?
C19 N5 C21 C20 1.7(4) . . . . ?
N5 C21 C22 C23 0.6(3) . . . . ?
C20 C21 C22 C23 -178.0(3) . . . . ?
N5 N6 C23 C22 -0.2(3) . . . . ?
N5 N6 C23 C24 -179.5(2) . . . . ?
C21 C22 C23 N6 -0.3(3) . . . . ?
C21 C22 C23 C24 179.0(2) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 1030027
