#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:33:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179729 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/25/7002548.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_7002548
loop_
_publ_author_name
'Lin, Ya-Chi'
'Yu, Kuo-Hsuan'
'Huang, Shou-Ling'
'Liu, Yi-Hung'
'Wang, Yu'
'Liu, Shiuh-Tzung'
'Chen, Jwu-Ting'
_publ_section_title
;
 Alternating ethylene-norbornene copolymerization catalyzed by cationic
 organopalladium complexes bearing hemilabile bidentate ligands of
 α-amino-pyridines
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              9058
_journal_page_last               9067
_journal_paper_doi               10.1039/b912068h
_journal_year                    2009
_chemical_formula_sum            'C13 H15 Cl N2 Pd'
_chemical_formula_weight         341.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                93.8870(10)
_cell_angle_beta                 110.9020(10)
_cell_angle_gamma                113.4540(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2253(2)
_cell_length_b                   9.1194(2)
_cell_length_c                   10.6977(2)
_cell_measurement_reflns_used    14090
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     666.77(3)
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_collection       'COLLECT (Nonius BV)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_method       CCD
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5239
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_process_details
;
mu_exptl_absorpt_correction_type 'multi-scan'
lti-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0303P)²+0.4056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                2731
_reflns_number_total             3008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912068h.txt
_cod_data_source_block           ic10676
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_sg_symbol_H-M      P-1
_cod_database_code               7002548
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 0.38226(3) 0.41478(2) 0.199422(19) 0.04113(12) Uani 1 1 d . . .
Cl1 Cl 0.47405(12) 0.26710(9) 0.35340(8) 0.05479(19) Uani 1 1 d . . .
N1 N 0.3059(3) 0.5565(3) 0.0711(2) 0.0457(5) Uani 1 1 d . . .
N2 N 0.5465(4) 0.6573(3) 0.3499(2) 0.0455(5) Uani 1 1 d . . .
C1 C 0.2236(5) 0.2038(4) 0.0499(3) 0.0622(8) Uani 1 1 d . . .
H1A H 0.1605 0.2259 -0.0360 0.093 Uiso 1 1 calc R . .
H1B H 0.1268 0.1257 0.0735 0.093 Uiso 1 1 calc R . .
H1C H 0.3079 0.1593 0.0409 0.093 Uiso 1 1 calc R . .
C2 C 0.2301(5) 0.5190(4) -0.0670(3) 0.0608(8) Uani 1 1 d . . .
H2A H 0.2055 0.4172 -0.1132 0.073 Uiso 1 1 calc R . .
C3 C 0.1871(6) 0.6239(5) -0.1430(4) 0.0785(11) Uani 1 1 d . . .
H3A H 0.1338 0.5936 -0.2389 0.094 Uiso 1 1 calc R . .
C4 C 0.2243(7) 0.7752(5) -0.0748(4) 0.0850(12) Uani 1 1 d . . .
H4A H 0.1942 0.8481 -0.1238 0.102 Uiso 1 1 calc R . .
C5 C 0.3065(6) 0.8163(4) 0.0667(4) 0.0716(10) Uani 1 1 d . . .
H5A H 0.3352 0.9189 0.1144 0.086 Uiso 1 1 calc R . .
C6 C 0.3464(4) 0.7061(4) 0.1379(3) 0.0506(6) Uani 1 1 d . . .
C7 C 0.4292(5) 0.7430(4) 0.2935(3) 0.0549(7) Uani 1 1 d . . .
H7A H 0.5099 0.8608 0.3311 0.066 Uiso 1 1 calc R . .
H7B H 0.3229 0.7098 0.3220 0.066 Uiso 1 1 calc R . .
C8 C 0.7476(4) 0.7342(3) 0.3710(3) 0.0457(6) Uani 1 1 d . . .
C9 C 0.8183(5) 0.8558(4) 0.3076(3) 0.0550(7) Uani 1 1 d . . .
H9A H 0.7355 0.8920 0.2492 0.066 Uiso 1 1 calc R . .
C10 C 1.0141(5) 0.9242(4) 0.3314(4) 0.0665(9) Uani 1 1 d . . .
H10A H 1.0620 1.0067 0.2889 0.080 Uiso 1 1 calc R . .
C11 C 1.1368(5) 0.8716(4) 0.4165(4) 0.0721(10) Uani 1 1 d . . .
H11A H 1.2676 0.9180 0.4319 0.086 Uiso 1 1 calc R . .
C12 C 1.0661(5) 0.7496(4) 0.4793(4) 0.0745(10) Uani 1 1 d . . .
H12A H 1.1488 0.7129 0.5370 0.089 Uiso 1 1 calc R . .
C13 C 0.8719(5) 0.6816(4) 0.4565(4) 0.0603(8) Uani 1 1 d . . .
H13A H 0.8247 0.5994 0.4994 0.072 Uiso 1 1 calc R . .
H2 H 0.552(5) 0.648(4) 0.427(4) 0.060(10) 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'
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
C1 Pd1 N1 94.40(11) . . ?
C1 Pd1 N2 174.96(11) . . ?
N1 Pd1 N2 80.56(9) . . ?
C1 Pd1 Cl1 88.57(9) . . ?
N1 Pd1 Cl1 176.93(6) . . ?
N2 Pd1 Cl1 96.47(7) . . ?
C2 N1 C6 118.4(3) . . ?
C2 N1 Pd1 127.5(2) . . ?
C6 N1 Pd1 114.07(19) . . ?
C8 N2 C7 117.6(2) . . ?
C8 N2 Pd1 111.13(16) . . ?
C7 N2 Pd1 103.04(17) . . ?
C8 N2 H2 104(2) . . ?
C7 N2 H2 109(2) . . ?
Pd1 N2 H2 112(2) . . ?
Pd1 C1 H1A 109.5 . . ?
Pd1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Pd1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 122.9(3) . . ?
N1 C2 H2A 118.6 . . ?
C3 C2 H2A 118.6 . . ?
C2 C3 C4 118.7(3) . . ?
C2 C3 H3A 120.6 . . ?
C4 C3 H3A 120.6 . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
N1 C6 C5 121.1(3) . . ?
N1 C6 C7 116.8(2) . . ?
C5 C6 C7 122.0(3) . . ?
N2 C7 C6 112.2(2) . . ?
N2 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C13 C8 C9 119.4(3) . . ?
C13 C8 N2 118.2(3) . . ?
C9 C8 N2 122.4(3) . . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C8 C13 C12 120.7(3) . . ?
C8 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
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 C1 2.015(3) . ?
Pd1 N1 2.055(2) . ?
Pd1 N2 2.212(2) . ?
Pd1 Cl1 2.3065(7) . ?
N1 C2 1.339(4) . ?
N1 C6 1.349(4) . ?
N2 C8 1.438(4) . ?
N2 C7 1.468(4) . ?
N2 H2 0.82(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.367(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.378(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.373(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.510(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.377(4) . ?
C8 C9 1.378(4) . ?
C9 C10 1.391(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.367(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.376(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.381(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 Cl1 0.82(3) 3.26(3) 3.371(2) 91(2) .
