#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:33:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179729 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/25/7002549.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_7002549
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            'C15 H18 B F4 N3 Pd'
_chemical_formula_weight         433.53
_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                 102.2370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9543(2)
_cell_length_b                   9.4463(2)
_cell_length_c                   18.9653(3)
_cell_measurement_reflns_used    18690
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1742.81(6)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10796
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.720
_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    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0039(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   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0299
_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)+(0.0322P)²+0.6758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                3070
_reflns_number_total             3966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912068h.txt
_cod_data_source_block           ic11059
_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               7002549
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 0.201887(19) 0.02930(2) 0.458474(10) 0.04126(9) Uani 1 1 d . . .
N1 N 0.0339(2) 0.1395(2) 0.40900(11) 0.0435(5) Uani 1 1 d . . .
N2 N 0.1692(2) -0.0679(3) 0.35162(12) 0.0425(5) Uani 1 1 d . . .
H2 H 0.185(3) -0.145(3) 0.3562(13) 0.035(8) Uiso 1 1 d . . .
N3 N 0.3531(2) -0.0987(3) 0.50627(12) 0.0534(6) Uani 1 1 d . . .
C1 C 0.2242(3) 0.1354(4) 0.55196(15) 0.0660(9) Uani 1 1 d . . .
H1A H 0.2654 0.0744 0.5911 0.099 Uiso 1 1 calc R . .
H1B H 0.1358 0.1661 0.5586 0.099 Uiso 1 1 calc R . .
H1C H 0.2822 0.2162 0.5509 0.099 Uiso 1 1 calc R . .
C2 C -0.0169(3) 0.2581(3) 0.43282(15) 0.0547(7) Uani 1 1 d . . .
H2A H 0.0308 0.2993 0.4754 0.066 Uiso 1 1 calc R . .
C3 C -0.1363(3) 0.3207(4) 0.39676(18) 0.0641(8) Uani 1 1 d . . .
H3A H -0.1695 0.4019 0.4150 0.077 Uiso 1 1 calc R . .
C4 C -0.2054(3) 0.2618(4) 0.33384(17) 0.0632(8) Uani 1 1 d . . .
H4A H -0.2870 0.3021 0.3090 0.076 Uiso 1 1 calc R . .
C5 C -0.1539(3) 0.1427(3) 0.30728(15) 0.0557(7) Uani 1 1 d . . .
H5A H -0.1989 0.1033 0.2637 0.067 Uiso 1 1 calc R . .
C6 C -0.0347(3) 0.0823(3) 0.34608(13) 0.0436(6) Uani 1 1 d . . .
C7 C 0.0207(3) -0.0529(3) 0.32281(15) 0.0497(7) Uani 1 1 d . . .
H7A H -0.0269 -0.1320 0.3391 0.060 Uiso 1 1 calc R . .
H7B H 0.0030 -0.0559 0.2705 0.060 Uiso 1 1 calc R . .
C8 C 0.2598(3) -0.0080(3) 0.31007(13) 0.0403(6) Uani 1 1 d . . .
C9 C 0.2173(3) 0.0942(3) 0.25895(16) 0.0582(8) Uani 1 1 d . . .
H9A H 0.1279 0.1288 0.2510 0.070 Uiso 1 1 calc R . .
C10 C 0.3085(4) 0.1460(4) 0.21908(18) 0.0713(9) Uani 1 1 d . . .
H10A H 0.2795 0.2157 0.1846 0.086 Uiso 1 1 calc R . .
C11 C 0.4393(3) 0.0965(4) 0.22959(17) 0.0647(8) Uani 1 1 d . . .
H11A H 0.4989 0.1302 0.2018 0.078 Uiso 1 1 calc R . .
C12 C 0.4822(3) -0.0035(3) 0.28155(17) 0.0581(8) Uani 1 1 d . . .
H12A H 0.5720 -0.0368 0.2895 0.070 Uiso 1 1 calc R . .
C13 C 0.3941(3) -0.0554(3) 0.32224(14) 0.0477(7) Uani 1 1 d . . .
H13A H 0.4249 -0.1224 0.3579 0.057 Uiso 1 1 calc R . .
C14 C 0.4264(3) -0.1824(3) 0.53360(15) 0.0541(7) Uani 1 1 d . . .
C15 C 0.5196(3) -0.2913(4) 0.56946(19) 0.0769(10) Uani 1 1 d . . .
H15A H 0.5458 -0.2704 0.6201 0.115 Uiso 1 1 calc R . .
H15B H 0.6001 -0.2937 0.5491 0.115 Uiso 1 1 calc R . .
H15C H 0.4746 -0.3816 0.5629 0.115 Uiso 1 1 calc R . .
B1 B 0.7939(4) 0.0497(4) 0.1023(2) 0.0598(9) Uani 1 1 d . . .
F1 F 0.6900(2) 0.1352(2) 0.11607(13) 0.0949(7) Uani 1 1 d . . .
F2 F 0.7612(3) 0.0016(3) 0.03327(11) 0.0899(6) Uani 1 1 d . . .
F3 F 0.9107(2) 0.1320(3) 0.11274(16) 0.1170(9) Uani 1 1 d . . .
F4 F 0.8131(3) -0.0618(2) 0.14844(12) 0.0978(7) 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'
N N 0.0061 0.0033 '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'
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 88.25(11) . . ?
N3 Pd1 N1 173.38(9) . . ?
C1 Pd1 N1 94.52(11) . . ?
N3 Pd1 N2 96.69(9) . . ?
C1 Pd1 N2 174.59(12) . . ?
N1 Pd1 N2 80.80(9) . . ?
C2 N1 C6 118.2(2) . . ?
C2 N1 Pd1 127.23(19) . . ?
C6 N1 Pd1 114.57(18) . . ?
C8 N2 C7 117.2(2) . . ?
C8 N2 Pd1 110.86(17) . . ?
C7 N2 Pd1 104.17(16) . . ?
C8 N2 H2 108(2) . . ?
C7 N2 H2 108(2) . . ?
Pd1 N2 H2 108(2) . . ?
C14 N3 Pd1 171.7(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 122.6(3) . . ?
N1 C2 H2A 118.7 . . ?
C3 C2 H2A 118.7 . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 H5A 120.4 . . ?
C6 C5 H5A 120.4 . . ?
N1 C6 C5 121.4(3) . . ?
N1 C6 C7 116.9(2) . . ?
C5 C6 C7 121.7(2) . . ?
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 . . ?
C9 C8 C13 119.3(2) . . ?
C9 C8 N2 122.1(2) . . ?
C13 C8 N2 118.6(2) . . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C12 119.1(3) . . ?
C10 C11 H11A 120.4 . . ?
C12 C11 H11A 120.4 . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C8 120.0(3) . . ?
C12 C13 H13A 120.0 . . ?
C8 C13 H13A 120.0 . . ?
N3 C14 C15 179.2(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
F4 B1 F2 109.6(3) . . ?
F4 B1 F3 110.2(3) . . ?
F2 B1 F3 110.5(3) . . ?
F4 B1 F1 109.9(3) . . ?
F2 B1 F1 110.0(3) . . ?
F3 B1 F1 106.6(3) . . ?
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 1.993(2) . ?
Pd1 C1 2.007(3) . ?
Pd1 N1 2.024(2) . ?
Pd1 N2 2.185(2) . ?
N1 C2 1.346(4) . ?
N1 C6 1.355(3) . ?
N2 C8 1.434(3) . ?
N2 C7 1.470(3) . ?
N2 H2 0.74(3) . ?
N3 C14 1.125(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.373(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.363(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.376(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.380(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.495(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.370(4) . ?
C8 C13 1.382(4) . ?
C9 C10 1.387(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.358(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.366(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.375(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.454(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
B1 F4 1.356(4) . ?
B1 F2 1.358(4) . ?
B1 F3 1.378(4) . ?
B1 F1 1.380(4) . ?
