#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:32:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179795 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/91/7009144.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_7009144
loop_
_publ_author_name
'Zhou, Xiang-Ge'
'Huang, Jie-Sheng'
'Yu, Xiao-Qi'
'Zhou, Zhong-Yuan'
'Che, Chi-Ming'
_publ_section_title
;
 Binaphthyl Schiff base complexes of palladium(II). Structures and
 reactivities toward alkene epoxidation
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1075
_journal_paper_doi               10.1039/a908917i
_journal_year                    2000
_chemical_formula_sum            'C38 H34 Cl4 N2 O4 Pd'
_chemical_formula_weight         830.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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_method           SHELXL-97
_cell_angle_alpha                98.88(3)
_cell_angle_beta                 93.85(3)
_cell_angle_gamma                102.00(3)
_cell_formula_units_Z            2
_cell_length_a                   10.317(2)
_cell_length_b                   13.332(3)
_cell_length_c                   13.668(3)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      5
_cell_volume                     1807.3(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.565
_diffrn_measured_fraction_theta_max 0.565
_diffrn_measurement_device_type  P4
_diffrn_measurement_method       'OMEGA SCAN '
_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    0.0449
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4142
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        1.82
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.7722
_exptl_absorpt_correction_type   SEMI-EMPERICAL
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         3825
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.374
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                3825
_reflns_number_total             3825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908917i.txt
_cod_data_source_block           pdn
_cod_original_cell_volume        1807.3(6)
_cod_database_code               7009144
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.004405(14) 0.256555(9) 0.557677(8) 0.04780(4) Uani 1 1 d D . .
Cl1 Cl -0.21715(8) 0.23307(6) 0.85114(4) 0.0894(2) Uani 1 1 d . . .
Cl2 Cl -0.68006(8) 0.05778(6) 0.62622(5) 0.0878(2) Uani 1 1 d . . .
Cl3 Cl 0.31827(15) 0.36854(10) 0.85177(7) 0.0773(4) Uani 0.50 1 d P A 1
Cl3' Cl 0.30420(15) 0.38853(11) 0.85139(8) 0.0746(4) Uani 0.50 1 d P A 2
Cl4 Cl 0.70563(7) 0.48708(6) 0.62513(5) 0.0794(2) Uani 1 1 d . A .
N1 N -0.14781(19) 0.25360(12) 0.45708(10) 0.0558(5) Uani 1 1 d D . .
N2 N 0.12670(18) 0.22502(12) 0.45613(10) 0.0530(5) Uani 1 1 d D . .
O1 O -0.11517(16) 0.27093(10) 0.66585(9) 0.0579(4) Uani 1 1 d D . .
O2 O 0.15392(16) 0.28130(11) 0.66546(9) 0.0570(4) Uani 1 1 d D . .
C1 C -0.0150(2) 0.16278(14) 0.29939(12) 0.0507(5) Uani 1 1 d . . .
C2 C 0.0685(2) 0.14377(13) 0.37270(12) 0.0537(6) Uani 1 1 d . . .
C3 C 0.0961(2) 0.04640(15) 0.37223(16) 0.0599(6) Uani 1 1 d . . .
H3A H 0.1561 0.0360 0.4215 0.072 Uiso 1 1 calc R . .
C4 C 0.0326(3) -0.03648(15) 0.29681(17) 0.0730(8) Uani 1 1 d . . .
H4A H 0.0478 -0.1027 0.2978 0.088 Uiso 1 1 calc R . .
C5 C -0.0515(2) -0.02048(15) 0.22171(15) 0.0611(6) Uani 1 1 d D . .
C6 C -0.1155(3) -0.11108(16) 0.14295(17) 0.0788(9) Uani 1 1 d D . .
H6A H -0.0456 -0.1379 0.1108 0.095 Uiso 1 1 calc R . .
H6B H -0.1636 -0.1654 0.1750 0.095 Uiso 1 1 calc R . .
C7 C -0.2089(4) -0.0908(2) 0.0645(3) 0.1563(14) Uani 1 1 d D . .
H7A H -0.1655 -0.0927 0.0036 0.188 Uiso 1 1 calc R . .
H7B H -0.2859 -0.1486 0.0527 0.188 Uiso 1 1 calc R . .
C8 C -0.2582(4) 0.0048(3) 0.0792(3) 0.1343(14) Uani 1 1 d D . .
H8A H -0.2673 0.0259 0.0148 0.161 Uiso 1 1 calc R . .
H8B H -0.3472 -0.0127 0.0997 0.161 Uiso 1 1 calc R . .
C9 C -0.1844(3) 0.09556(19) 0.14921(15) 0.0767(8) Uani 1 1 d D . .
H9A H -0.2481 0.1270 0.1849 0.092 Uiso 1 1 calc R . .
H9B H -0.1399 0.1458 0.1111 0.092 Uiso 1 1 calc R . .
C10 C -0.0825(2) 0.07835(14) 0.22420(13) 0.0562(6) Uani 1 1 d D . .
C11 C -0.0414(2) 0.26872(12) 0.30126(12) 0.0503(5) Uani 1 1 d . . .
C12 C 0.0095(2) 0.32673(15) 0.22975(12) 0.0546(6) Uani 1 1 d D . .
C13 C 0.0971(3) 0.2878(2) 0.15680(14) 0.0762(8) Uani 1 1 d D . .
H13A H 0.1832 0.2902 0.1915 0.091 Uiso 1 1 calc R . .
H13B H 0.0578 0.2158 0.1281 0.091 Uiso 1 1 calc R . .
C14 C 0.1164(4) 0.3500(2) 0.0757(2) 0.1471(12) Uani 1 1 d D . .
H14A H 0.0411 0.3229 0.0255 0.176 Uiso 1 1 calc R . .
H14B H 0.1949 0.3369 0.0453 0.176 Uiso 1 1 calc R . .
C15 C 0.1319(4) 0.4668(2) 0.0996(2) 0.1038(11) Uani 1 1 d D . .
H15A H 0.2184 0.4979 0.1363 0.125 Uiso 1 1 calc R . .
H15B H 0.1284 0.4943 0.0381 0.125 Uiso 1 1 calc R . .
C16 C 0.0273(3) 0.49542(16) 0.15880(15) 0.0870(10) Uani 1 1 d D . .
H16A H -0.0489 0.4958 0.1133 0.104 Uiso 1 1 calc R . .
H16B H 0.0600 0.5660 0.1945 0.104 Uiso 1 1 calc R . .
C17 C -0.0204(2) 0.42675(13) 0.23322(13) 0.0566(6) Uani 1 1 d D . .
C18 C -0.0944(3) 0.46285(15) 0.30623(16) 0.0620(6) Uani 1 1 d . . .
H18A H -0.1147 0.5277 0.3067 0.074 Uiso 1 1 calc R . .
C19 C -0.1386(3) 0.40634(16) 0.37762(14) 0.0631(6) Uani 1 1 d . . .
H19A H -0.1865 0.4330 0.4267 0.076 Uiso 1 1 calc R . .
C20 C -0.1107(2) 0.30834(14) 0.37561(12) 0.0536(5) Uani 1 1 d . . .
C21 C -0.2678(2) 0.22866(14) 0.47112(12) 0.0526(5) Uani 1 1 d . . .
H21A H -0.3297 0.2322 0.4198 0.063 Uiso 1 1 calc R . .
C22 C -0.3203(2) 0.19485(14) 0.55887(14) 0.0520(5) Uani 1 1 d . . .
C23 C -0.2388(2) 0.22167(15) 0.65161(14) 0.0557(6) Uani 1 1 d . . .
C24 C -0.3065(2) 0.20143(15) 0.73464(13) 0.0572(6) Uani 1 1 d . . .
C25 C -0.4409(2) 0.15316(17) 0.72992(16) 0.0628(6) Uani 1 1 d . . .
H25A H -0.4812 0.1433 0.7876 0.075 Uiso 1 1 calc R . .
C26 C -0.5152(3) 0.11921(16) 0.63406(16) 0.0656(7) Uani 1 1 d . . .
C27 C -0.4551(3) 0.14275(15) 0.55207(16) 0.0619(6) Uani 1 1 d . . .
H27A H -0.5044 0.1239 0.4900 0.074 Uiso 1 1 calc R . .
C28 C 0.2533(2) 0.25864(13) 0.46834(14) 0.0526(5) Uani 1 1 d . . .
H28A H 0.3010 0.2400 0.4157 0.063 Uiso 1 1 calc R . .
C29 C 0.3288(2) 0.32362(14) 0.55795(12) 0.0512(5) Uani 1 1 d . . .
C30 C 0.2736(2) 0.32372(12) 0.65172(13) 0.0522(5) Uani 1 1 d . A .
C31 C 0.3673(3) 0.37714(16) 0.73457(14) 0.0603(6) Uani 1 1 d . . .
C32 C 0.4961(3) 0.42408(17) 0.72627(16) 0.0640(7) Uani 1 1 d . A .
H32A H 0.5536 0.4551 0.7832 0.077 Uiso 1 1 calc R . .
C33 C 0.5410(2) 0.42551(18) 0.63337(15) 0.0621(7) Uani 1 1 d . . .
C34 C 0.4584(2) 0.37411(15) 0.54935(15) 0.0593(6) Uani 1 1 d . A .
O3 O 0.4729(4) 0.2322(3) 0.30334(19) 0.1434(15) Uani 1 1 d . . .
O4 O 0.4851(4) 0.2077(2) 0.14314(19) 0.1204(11) Uani 1 1 d . . .
C35 C 0.3596(9) 0.0768(4) 0.2074(3) 0.174(3) Uani 1 1 d . . .
H35A H 0.3323 0.0601 0.2698 0.260 Uiso 1 1 calc R . .
H35B H 0.4073 0.0271 0.1784 0.260 Uiso 1 1 calc R . .
H35C H 0.2824 0.0749 0.1632 0.260 Uiso 1 1 calc R . .
C36 C 0.4511(4) 0.1875(3) 0.2250(2) 0.1092(13) Uani 1 1 d . . .
C37 C 0.5739(6) 0.3106(4) 0.1496(4) 0.145(2) Uani 1 1 d D . .
H37A H 0.5298 0.3638 0.1789 0.174 Uiso 1 1 calc R . .
H37B H 0.6539 0.3146 0.1929 0.174 Uiso 1 1 calc R . .
C38 C 0.6087(9) 0.3297(6) 0.0569(4) 0.201(3) Uani 1 1 d D . .
H38A H 0.6666 0.3974 0.0640 0.301 Uiso 1 1 calc R . .
H38B H 0.5298 0.3271 0.0143 0.301 Uiso 1 1 calc R . .
H38C H 0.6538 0.2779 0.0282 0.301 Uiso 1 1 calc R . .
H34A H 0.4757(18) 0.3615(12) 0.4831(11) 0.027(4) Uiso 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'
Cl Cl 0.1484 0.1585 '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 O2 90.05(7) . . ?
N2 Pd1 O1 172.40(7) . . ?
O2 Pd1 O1 86.97(6) . . ?
N2 Pd1 N1 94.46(7) . . ?
O2 Pd1 N1 171.42(6) . . ?
O1 Pd1 N1 89.41(7) . . ?
C21 N1 C20 119.43(19) . . ?
C21 N1 Pd1 124.27(13) . . ?
C20 N1 Pd1 114.50(14) . . ?
C28 N2 C2 118.97(18) . . ?
C28 N2 Pd1 124.34(12) . . ?
C2 N2 Pd1 115.64(14) . . ?
C23 O1 Pd1 120.36(12) . . ?
C30 O2 Pd1 121.09(12) . . ?
C2 C1 C10 118.87(18) . . ?
C2 C1 C11 120.60(15) . . ?
C10 C1 C11 120.44(17) . . ?
C1 C2 C3 121.83(16) . . ?
C1 C2 N2 120.22(18) . . ?
C3 C2 N2 117.90(18) . . ?
C2 C3 C4 119.5(2) . . ?
C5 C4 C3 120.4(2) . . ?
C4 C5 C10 119.79(17) . . ?
C4 C5 C6 118.3(2) . . ?
C10 C5 C6 121.8(2) . . ?
C7 C6 C5 116.4(2) . . ?
C8 C7 C6 119.9(3) . . ?
C9 C8 C7 120.3(3) . . ?
C8 C9 C10 117.3(3) . . ?
C5 C10 C1 119.27(19) . . ?
C5 C10 C9 121.15(17) . . ?
C1 C10 C9 119.58(19) . . ?
C20 C11 C12 122.04(17) . . ?
C20 C11 C1 119.12(16) . . ?
C12 C11 C1 118.79(17) . . ?
C11 C12 C17 116.84(18) . . ?
C11 C12 C13 121.5(2) . . ?
C17 C12 C13 121.59(19) . . ?
C14 C13 C12 112.2(3) . . ?
C13 C14 C15 119.4(2) . . ?
C16 C15 C14 111.8(3) . . ?
C15 C16 C17 116.5(2) . . ?
C18 C17 C12 119.83(18) . . ?
C18 C17 C16 118.7(2) . . ?
C12 C17 C16 121.5(2) . . ?
C19 C18 C17 122.2(2) . . ?
C18 C19 C20 118.9(2) . . ?
C11 C20 C19 120.04(18) . . ?
C11 C20 N1 121.73(18) . . ?
C19 C20 N1 118.08(18) . . ?
N1 C21 C22 126.71(19) . . ?
C27 C22 C23 121.37(19) . . ?
C27 C22 C21 118.69(18) . . ?
C23 C22 C21 119.75(18) . . ?
O1 C23 C24 118.80(17) . . ?
O1 C23 C22 126.04(19) . . ?
C24 C23 C22 114.78(19) . . ?
C25 C24 C23 124.54(18) . . ?
C25 C24 Cl1 116.91(16) . . ?
C23 C24 Cl1 118.49(17) . . ?
C24 C25 C26 118.3(2) . . ?
C27 C26 C25 118.9(2) . . ?
C27 C26 Cl2 121.84(18) . . ?
C25 C26 Cl2 119.16(18) . . ?
C26 C27 C22 121.8(2) . . ?
N2 C28 C29 125.36(19) . . ?
C34 C29 C30 122.95(16) . . ?
C34 C29 C28 116.94(18) . . ?
C30 C29 C28 119.72(18) . . ?
O2 C30 C31 120.32(17) . . ?
O2 C30 C29 126.62(16) . . ?
C31 C30 C29 113.05(19) . . ?
C32 C31 C30 123.9(2) . . ?
C32 C31 Cl3 118.70(16) . . ?
C30 C31 Cl3 117.00(18) . . ?
C32 C31 Cl3' 120.12(16) . . ?
C30 C31 Cl3' 115.81(18) . . ?
Cl3 C31 Cl3' 10.78(7) . . ?
C31 C32 C33 120.07(19) . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 Cl4 120.94(18) . . ?
C32 C33 Cl4 119.00(16) . . ?
C33 C34 C29 119.9(2) . . ?
C36 O4 C37 113.9(3) . . ?
O3 C36 O4 133.4(4) . . ?
O3 C36 C35 118.2(4) . . ?
O4 C36 C35 108.4(3) . . ?
C38 C37 O4 111.8(5) . . ?
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 1.9926(18) . ?
Pd1 O2 1.9980(15) . ?
Pd1 O1 2.0000(16) . ?
Pd1 N1 2.0064(18) . ?
Cl1 C24 1.731(2) . ?
Cl2 C26 1.716(3) . ?
Cl3 C31 1.725(2) . ?
Cl3' C31 1.761(2) . ?
Cl4 C33 1.745(2) . ?
N1 C21 1.249(3) . ?
N1 C20 1.453(2) . ?
N2 C28 1.280(3) . ?
N2 C2 1.446(2) . ?
O1 C23 1.294(3) . ?
O2 C30 1.285(3) . ?
C1 C2 1.365(3) . ?
C1 C10 1.424(2) . ?
C1 C11 1.490(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.403(3) . ?
C4 C5 1.370(4) . ?
C5 C10 1.415(3) . ?
C5 C6 1.492(3) . ?
C6 C7 1.488(5) . ?
C7 C8 1.457(5) . ?
C8 C9 1.457(4) . ?
C9 C10 1.496(3) . ?
C11 C20 1.383(3) . ?
C11 C12 1.401(3) . ?
C12 C17 1.424(3) . ?
C12 C13 1.496(3) . ?
C13 C14 1.484(4) . ?
C14 C15 1.512(4) . ?
C15 C16 1.470(5) . ?
C16 C17 1.511(3) . ?
C17 C18 1.385(3) . ?
C18 C19 1.368(3) . ?
C19 C20 1.392(3) . ?
C21 C22 1.445(3) . ?
C22 C27 1.409(3) . ?
C22 C23 1.426(3) . ?
C23 C24 1.404(3) . ?
C24 C25 1.394(3) . ?
C25 C26 1.431(3) . ?
C26 C27 1.364(3) . ?
C28 C29 1.456(2) . ?
C29 C34 1.388(3) . ?
C29 C30 1.437(3) . ?
C30 C31 1.429(3) . ?
C31 C32 1.366(3) . ?
C32 C33 1.382(3) . ?
C33 C34 1.378(3) . ?
O3 C36 1.126(4) . ?
O4 C36 1.246(4) . ?
O4 C37 1.468(6) . ?
C35 C36 1.551(7) . ?
C37 C38 1.387(9) . ?
