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#$Date: 2016-03-21 09:02:51 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178616 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/27/4072756.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_4072756
loop_
_publ_author_name
'Liao, Chuang-Yi'
'Chan, Kai-Ting'
'Zeng, Jing-Yao'
'Hu, Ching-Han'
'Tu, Cheng-Yi'
'Lee, Hon Man'
_publ_section_title
;
 Nonchelate and Chelate Complexes of Palladium(II) with N-Heterocyclic
 Carbene Ligands of Amido Functionality
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1692
_journal_paper_doi               10.1021/om0610041
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C36 H30 F2 N6 O2 Pd, 2(C H4 O)'
_chemical_formula_sum            'C38 H38 F2 N6 O4 Pd'
_chemical_formula_weight         787.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.505(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9128(3)
_cell_length_b                   17.8089(5)
_cell_length_c                   9.3293(3)
_cell_measurement_temperature    396(2)
_cell_volume                     1698.23(9)
_computing_cell_refinement       'APEX2 v1.0-22'
_computing_data_collection       'APEX2 v1.0-22 (Bruker, 2004)'
_computing_data_reduction        'APEX2 v1.0-22'
_computing_molecular_graphics    'SHELXTL 5.1'
_computing_publication_material  'SHELXTL 5.1'
_computing_structure_refinement  'SHELXTL 5.1'
_computing_structure_solution    'SHELXTL 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23701
_diffrn_reflns_theta_full        28.66
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         1.99
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.8432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.853
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0736P)²+1.1137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                3069
_reflns_number_total             4367
_reflns_threshold_expression     I>2σ
_cod_data_source_file            om0610041si20061221_100443.cif
_cod_data_source_block           trans-6b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072756
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.4985(3) 0.03946(17) 0.2019(4) 0.0208(7) Uani 1 1 d .
C2 C 0.5392(4) 0.0836(2) 0.4405(4) 0.0279(8) Uani 1 1 d .
H2 H 0.5789 0.0902 0.5455 0.034 Uiso 1 1 calc R
C3 C 0.4345(4) 0.1202(2) 0.3484(4) 0.0279(8) Uani 1 1 d .
H3 H 0.3872 0.1571 0.3767 0.033 Uiso 1 1 calc R
C4 C 0.6942(4) -0.01491(19) 0.4035(4) 0.0277(8) Uani 1 1 d .
H4A H 0.6694 -0.0659 0.3692 0.033 Uiso 1 1 calc R
H4B H 0.7275 -0.0151 0.5145 0.033 Uiso 1 1 calc R
C5 C 0.8012(4) 0.0105(2) 0.3470(4) 0.0288(8) Uani 1 1 d .
C6 C 0.8769(4) -0.0432(3) 0.3094(5) 0.0396(10) Uani 1 1 d .
H6 H 0.8582 -0.0938 0.3150 0.047 Uiso 1 1 calc R
C7 C 0.9797(5) -0.0226(3) 0.2636(6) 0.0543(13) Uani 1 1 d .
H7 H 1.0305 -0.0586 0.2387 0.065 Uiso 1 1 calc R
C8 C 1.0043(4) 0.0508(3) 0.2562(5) 0.0501(13) Uani 1 1 d .
C9 C 0.9326(4) 0.1074(3) 0.2906(6) 0.0500(12) Uani 1 1 d .
H9 H 0.9523 0.1578 0.2832 0.060 Uiso 1 1 calc R
C10 C 0.8297(4) 0.0857(2) 0.3368(5) 0.0360(9) Uani 1 1 d .
H10 H 0.7792 0.1222 0.3612 0.043 Uiso 1 1 calc R
C11 C 0.3105(4) 0.1172(2) 0.0611(4) 0.0267(8) Uani 1 1 d .
H11A H 0.2566 0.1551 0.0847 0.032 Uiso 1 1 calc R
H11B H 0.2546 0.0750 0.0139 0.032 Uiso 1 1 calc R
C12 C 0.3693(3) 0.14957(18) -0.0520(4) 0.0206(7) Uani 1 1 d .
C13 C 0.5505(3) 0.14222(17) -0.1423(4) 0.0194(7) Uani 1 1 d .
C14 C 0.6812(4) 0.1192(2) -0.0874(4) 0.0263(8) Uani 1 1 d .
H14 H 0.7077 0.0823 -0.0123 0.032 Uiso 1 1 calc R
C15 C 0.7716(4) 0.1501(2) -0.1426(5) 0.0315(8) Uani 1 1 d .
H15 H 0.8582 0.1341 -0.1039 0.038 Uiso 1 1 calc R
C16 C 0.7348(4) 0.2046(2) -0.2548(5) 0.0310(8) Uani 1 1 d .
H16 H 0.7962 0.2258 -0.2913 0.037 Uiso 1 1 calc R
C17 C 0.6060(4) 0.2273(2) -0.3120(4) 0.0307(8) Uani 1 1 d .
H17 H 0.5805 0.2639 -0.3879 0.037 Uiso 1 1 calc R
C18 C 0.5132(4) 0.19629(19) -0.2578(4) 0.0250(7) Uani 1 1 d .
H18 H 0.4263 0.2116 -0.2987 0.030 Uiso 1 1 calc R
C19 C 0.0410(9) 0.2610(5) 0.0979(11) 0.114(3) Uani 1 1 d .
H19A H -0.0427 0.2796 0.0331 0.172 Uiso 1 1 calc R
H19B H 0.0459 0.2080 0.0819 0.172 Uiso 1 1 calc R
H19C H 0.1090 0.2863 0.0737 0.172 Uiso 1 1 calc R
F1 F 1.1066(3) 0.0711(2) 0.2104(4) 0.0808(11) Uani 1 1 d .
N1 N 0.5781(3) 0.03328(17) 0.3490(3) 0.0228(6) Uani 1 1 d .
N2 N 0.4102(3) 0.09224(15) 0.2024(3) 0.0214(6) Uani 1 1 d .
N3 N 0.4658(3) 0.10967(15) -0.0723(3) 0.0193(6) Uani 1 1 d .
O1 O 0.3247(2) 0.21095(13) -0.1126(3) 0.0284(6) Uani 1 1 d .
O2 O 0.0582(6) 0.2758(4) 0.2668(8) 0.1153(19) Uani 1 1 d .
H2A H 0.1359 0.2731 0.3196 0.173 Uiso 1 1 calc R
Pd1 Pd 0.5000 0.0000 0.0000 0.01759(12) 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'
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'
F F 0.0171 0.0103 '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
N2 C1 N1 105.1(3) . .
N2 C1 Pd1 119.1(2) . .
N1 C1 Pd1 135.2(3) . .
C3 C2 N1 107.1(3) . .
C3 C2 H2 126.4 . .
N1 C2 H2 126.4 . .
C2 C3 N2 106.4(3) . .
C2 C3 H3 126.8 . .
N2 C3 H3 126.8 . .
N1 C4 C5 112.6(3) . .
N1 C4 H4A 109.1 . .
C5 C4 H4A 109.1 . .
N1 C4 H4B 109.1 . .
C5 C4 H4B 109.1 . .
H4A C4 H4B 107.8 . .
C10 C5 C6 118.8(4) . .
C10 C5 C4 122.3(3) . .
C6 C5 C4 118.9(3) . .
C7 C6 C5 121.0(4) . .
C7 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C8 C7 C6 118.3(5) . .
C8 C7 H7 120.9 . .
C6 C7 H7 120.9 . .
C7 C8 F1 118.2(5) . .
C7 C8 C9 124.1(4) . .
F1 C8 C9 117.8(5) . .
C8 C9 C10 116.9(5) . .
C8 C9 H9 121.5 . .
C10 C9 H9 121.5 . .
C5 C10 C9 121.0(4) . .
C5 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
N2 C11 C12 112.3(3) . .
N2 C11 H11A 109.1 . .
C12 C11 H11A 109.1 . .
N2 C11 H11B 109.1 . .
C12 C11 H11B 109.1 . .
H11A C11 H11B 107.9 . .
O1 C12 N3 127.0(3) . .
O1 C12 C11 116.9(3) . .
N3 C12 C11 116.1(3) . .
C18 C13 C14 118.0(3) . .
C18 C13 N3 125.0(3) . .
C14 C13 N3 117.0(3) . .
C15 C14 C13 121.3(3) . .
C15 C14 H14 119.4 . .
C13 C14 H14 119.4 . .
C14 C15 C16 120.5(4) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C17 C16 C15 119.1(3) . .
C17 C16 H16 120.5 . .
C15 C16 H16 120.5 . .
C16 C17 C18 121.0(3) . .
C16 C17 H17 119.5 . .
C18 C17 H17 119.5 . .
C17 C18 C13 120.1(3) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
O2 C19 H19A 109.5 . .
O2 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
O2 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C1 N1 C2 110.0(3) . .
C1 N1 C4 124.9(3) . .
C2 N1 C4 124.9(3) . .
C1 N2 C3 111.3(3) . .
C1 N2 C11 121.3(3) . .
C3 N2 C11 127.3(3) . .
C12 N3 C13 121.1(3) . .
C12 N3 Pd1 121.2(2) . .
C13 N3 Pd1 117.6(2) . .
C19 O2 H2A 109.5 . .
C1 Pd1 C1 180.0 . 3_655
C1 Pd1 N3 85.16(12) . .
C1 Pd1 N3 94.84(12) 3_655 .
C1 Pd1 N3 94.84(12) . 3_655
C1 Pd1 N3 85.16(12) 3_655 3_655
N3 Pd1 N3 180.0 . 3_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.347(4) .
C1 N1 1.348(5) .
C1 Pd1 2.016(3) .
C2 C3 1.334(5) .
C2 N1 1.402(4) .
C2 H2 0.9300 .
C3 N2 1.386(5) .
C3 H3 0.9300 .
C4 N1 1.465(5) .
C4 C5 1.509(5) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C10 1.385(5) .
C5 C6 1.387(6) .
C6 C7 1.382(7) .
C6 H6 0.9300 .
C7 C8 1.340(8) .
C7 H7 0.9300 .
C8 F1 1.376(5) .
C8 C9 1.382(7) .
C9 C10 1.392(6) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 N2 1.454(5) .
C11 C12 1.527(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 O1 1.248(4) .
C12 N3 1.339(4) .
C13 C18 1.395(5) .
C13 C14 1.398(5) .
C13 N3 1.427(4) .
C14 C15 1.377(5) .
C14 H14 0.9300 .
C15 C16 1.381(5) .
C15 H15 0.9300 .
C16 C17 1.378(6) .
C16 H16 0.9300 .
C17 C18 1.395(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 O2 1.543(10) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
N3 Pd1 2.057(3) .
O2 H2A 0.8200 .
Pd1 C1 2.016(3) 3_655
Pd1 N3 2.057(3) 3_655
