#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:33:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179729 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/25/7002547.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_7002547
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            'C14 H24 B F4 N3 Pd'
_chemical_formula_weight         427.57
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 100.5540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6589(2)
_cell_length_b                   7.3818(2)
_cell_length_c                   22.3551(6)
_cell_measurement_reflns_used    34684
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1891.41(8)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13190
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1135P)²+1.0605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                3081
_reflns_number_total             4270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912068h.txt
_cod_data_source_block           ic12052
_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_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7002547
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.13964(3) 0.38892(5) 0.086125(17) 0.0601(2) Uani 1 1 d . . .
F1 F 0.6786(9) 0.3554(18) 0.0958(4) 0.256(7) Uani 1 1 d . . .
F2 F 0.5002(6) 0.3013(17) 0.0993(5) 0.255(5) Uani 1 1 d . . .
F3 F 0.6151(10) 0.4127(15) 0.1743(5) 0.267(6) Uani 1 1 d . . .
F4 F 0.6358(10) 0.1606(12) 0.1523(5) 0.243(5) Uani 1 1 d . . .
N1 N 0.0645(3) 0.4681(6) 0.15701(19) 0.0616(9) Uani 1 1 d . . .
N2 N 0.2855(3) 0.5371(6) 0.13934(17) 0.0574(9) Uani 1 1 d . . .
H2B H 0.3511 0.4763 0.1346 0.069 Uiso 1 1 calc R . .
N3 N 0.2241(4) 0.3016(7) 0.0215(2) 0.0767(12) Uani 1 1 d . . .
C1 C -0.0023(5) 0.2481(9) 0.0449(3) 0.0907(18) Uani 1 1 d . . .
H1A H -0.0015 0.2388 0.0021 0.136 Uiso 1 1 calc R . .
H1B H -0.0719 0.3099 0.0508 0.136 Uiso 1 1 calc R . .
H1C H -0.0008 0.1289 0.0622 0.136 Uiso 1 1 calc R . .
C2 C -0.0510(4) 0.4751(8) 0.1588(3) 0.0739(14) Uani 1 1 d . . .
H2A H -0.1046 0.4460 0.1240 0.089 Uiso 1 1 calc R . .
C3 C -0.0906(5) 0.5238(9) 0.2102(3) 0.0861(18) Uani 1 1 d . . .
H3A H -0.1703 0.5277 0.2103 0.103 Uiso 1 1 calc R . .
C4 C -0.0126(7) 0.5664(9) 0.2613(4) 0.089(2) Uani 1 1 d . . .
H4A H -0.0382 0.5971 0.2970 0.107 Uiso 1 1 calc R . .
C5 C 0.1042(6) 0.5637(8) 0.2594(3) 0.0761(15) Uani 1 1 d . . .
H5A H 0.1585 0.5954 0.2937 0.091 Uiso 1 1 calc R . .
C6 C 0.1411(4) 0.5136(7) 0.2065(2) 0.0615(11) Uani 1 1 d . . .
C7 C 0.2703(4) 0.5027(7) 0.2030(2) 0.0638(12) Uani 1 1 d . . .
H7A H 0.3132 0.5946 0.2299 0.077 Uiso 1 1 calc R . .
C8 C 0.3165(5) 0.3173(10) 0.2233(3) 0.0845(17) Uani 1 1 d . . .
H8A H 0.3981 0.3111 0.2216 0.127 Uiso 1 1 calc R . .
H8B H 0.2751 0.2270 0.1969 0.127 Uiso 1 1 calc R . .
H8C H 0.3056 0.2959 0.2642 0.127 Uiso 1 1 calc R . .
C9 C 0.3050(4) 0.7329(7) 0.1234(2) 0.0662(12) Uani 1 1 d . . .
C10 C 0.3229(6) 0.7301(9) 0.0569(3) 0.0834(16) Uani 1 1 d . . .
H10A H 0.2541 0.6832 0.0314 0.125 Uiso 1 1 calc R . .
H10B H 0.3884 0.6545 0.0536 0.125 Uiso 1 1 calc R . .
H10C H 0.3373 0.8510 0.0443 0.125 Uiso 1 1 calc R . .
C11 C 0.1979(6) 0.8458(8) 0.1290(4) 0.0857(17) Uani 1 1 d . . .
H11A H 0.1876 0.8469 0.1706 0.129 Uiso 1 1 calc R . .
H11B H 0.1301 0.7941 0.1039 0.129 Uiso 1 1 calc R . .
H11C H 0.2085 0.9676 0.1159 0.129 Uiso 1 1 calc R . .
C12 C 0.4142(6) 0.8066(10) 0.1638(3) 0.0897(18) Uani 1 1 d . . .
H12A H 0.4033 0.8080 0.2053 0.135 Uiso 1 1 calc R . .
H12B H 0.4287 0.9276 0.1513 0.135 Uiso 1 1 calc R . .
H12C H 0.4795 0.7308 0.1602 0.135 Uiso 1 1 calc R . .
C13 C 0.2765(6) 0.2510(9) -0.0127(3) 0.0834(16) Uani 1 1 d . . .
C14 C 0.3483(10) 0.1881(16) -0.0554(5) 0.141(3) Uani 1 1 d . . .
H14A H 0.4292 0.2000 -0.0373 0.211 Uiso 1 1 calc R . .
H14B H 0.3321 0.2595 -0.0919 0.211 Uiso 1 1 calc R . .
H14C H 0.3310 0.0633 -0.0652 0.211 Uiso 1 1 calc R . .
B1 B 0.6044(6) 0.3107(11) 0.1265(3) 0.0772(18) Uani 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N3 Pd1 C1 88.6(2) . . ?
N3 Pd1 N1 175.21(18) . . ?
C1 Pd1 N1 94.0(2) . . ?
N3 Pd1 N2 96.78(17) . . ?
C1 Pd1 N2 174.0(2) . . ?
N1 Pd1 N2 80.50(15) . . ?
C6 N1 C2 119.0(5) . . ?
C6 N1 Pd1 113.6(3) . . ?
C2 N1 Pd1 127.3(4) . . ?
C7 N2 C9 115.9(4) . . ?
C7 N2 Pd1 102.6(3) . . ?
C9 N2 Pd1 119.1(3) . . ?
C7 N2 H2B 106.1 . . ?
C9 N2 H2B 106.1 . . ?
Pd1 N2 H2B 106.1 . . ?
C13 N3 Pd1 176.6(5) . . ?
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 121.8(5) . . ?
N1 C2 H2A 119.1 . . ?
C3 C2 H2A 119.1 . . ?
C4 C3 C2 119.4(6) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 119.1(6) . . ?
C3 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
C4 C5 C6 119.8(6) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
N1 C6 C5 120.8(5) . . ?
N1 C6 C7 117.6(4) . . ?
C5 C6 C7 121.6(5) . . ?
N2 C7 C8 110.1(4) . . ?
N2 C7 C6 109.4(4) . . ?
C8 C7 C6 109.5(4) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C12 110.4(5) . . ?
N2 C9 C11 110.0(4) . . ?
C12 C9 C11 111.4(5) . . ?
N2 C9 C10 105.5(4) . . ?
C12 C9 C10 109.4(5) . . ?
C11 C9 C10 110.1(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 177.7(8) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
F1 B1 F2 117.1(9) . . ?
F1 B1 F4 108.0(10) . . ?
F2 B1 F4 110.1(10) . . ?
F1 B1 F3 109.2(10) . . ?
F2 B1 F3 111.7(9) . . ?
F4 B1 F3 99.1(9) . . ?
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 N3 1.998(5) . ?
Pd1 C1 2.028(5) . ?
Pd1 N1 2.032(4) . ?
Pd1 N2 2.182(4) . ?
F1 B1 1.244(10) . ?
F2 B1 1.257(9) . ?
F3 B1 1.294(11) . ?
F4 B1 1.271(10) . ?
N1 C6 1.332(6) . ?
N1 C2 1.354(6) . ?
N2 C7 1.489(6) . ?
N2 C9 1.515(7) . ?
N2 H2B 0.9100 . ?
N3 C13 1.127(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.363(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.360(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.381(7) . ?
C5 H5A 0.9300 . ?
C6 C7 1.524(7) . ?
C7 C8 1.509(8) . ?
C7 H7A 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C12 1.519(8) . ?
C9 C11 1.526(8) . ?
C9 C10 1.539(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.456(11) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
