#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:00:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179358 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/55/4325548.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_4325548
loop_
_publ_author_name
'Kelly J. Kilpin'
'Emma L. Gavey'
'C. John McAdam'
'Christopher B. Anderson'
'Samuel J. Lind'
'Courtney C. Keep'
'Keith C. Gordon'
'James D. Crowley'
_publ_section_title
;
 Palladium(II) Complexes of Readily Functionalized Bidentate
 2-Pyridyl-1,2,3-triazole "Click" Ligands: A Synthetic, Structural,
 Spectroscopic, and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6334
_journal_page_last               6346
_journal_paper_doi               10.1021/ic200789b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C28 H24 N8 Pd, 2(C2 H3 N), 2(B F4)'
_chemical_formula_sum            'C32 H30 B2 F8 N10 Pd'
_chemical_formula_weight         834.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.311(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.232(2)
_cell_length_b                   11.358(2)
_cell_length_c                   14.874(3)
_cell_measurement_reflns_used    5242
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      32.842
_cell_measurement_theta_min      2.5525
_cell_volume                     1718.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15411
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.8347
_exptl_absorpt_correction_T_min  0.7017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0202
_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)+(0.0173P)²+1.5930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                2957
_reflns_number_total             3192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200789b_si_001_05.cif
_cod_data_source_block           820910
_cod_original_cell_volume        1718.0(6)
_cod_database_code               4325548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.18469(16) -0.17749(15) 1.09915(11) 0.0138(3) Uani 1 1 d .
H1 H 0.1164 -0.1905 1.1364 0.017 Uiso 1 1 calc R
C2 C 0.30038(16) -0.24235(15) 1.11494(11) 0.0155(3) Uani 1 1 d .
H2 H 0.3115 -0.2974 1.1633 0.019 Uiso 1 1 calc R
C3 C 0.39890(16) -0.22583(15) 1.05955(11) 0.0151(3) Uani 1 1 d .
H3 H 0.4770 -0.2716 1.0677 0.018 Uiso 1 1 calc R
C4 C 0.38199(16) -0.14122(15) 0.99173(11) 0.0137(3) Uani 1 1 d .
H4 H 0.4489 -0.1274 0.9535 0.016 Uiso 1 1 calc R
C5 C 0.26611(15) -0.07757(14) 0.98079(10) 0.0110(3) Uani 1 1 d .
C6 C 0.23765(16) 0.01825(14) 0.91642(11) 0.0116(3) Uani 1 1 d .
C7 C 0.30132(16) 0.07559(15) 0.85290(11) 0.0126(3) Uani 1 1 d .
H7 H 0.3861 0.0592 0.8356 0.015 Uiso 1 1 calc R
C8 C 0.23395(16) 0.25401(15) 0.75361(11) 0.0148(3) Uani 1 1 d .
H8A H 0.1468 0.2832 0.7276 0.018 Uiso 1 1 calc R
H8B H 0.2791 0.2208 0.7038 0.018 Uiso 1 1 calc R
C9 C 0.31408(16) 0.35580(15) 0.79678(11) 0.0134(3) Uani 1 1 d .
C10 C 0.42876(16) 0.39153(15) 0.76226(11) 0.0143(3) Uani 1 1 d .
H10 H 0.4584 0.3509 0.7125 0.017 Uiso 1 1 calc R
C11 C 0.50041(16) 0.48721(15) 0.80077(12) 0.0163(4) Uani 1 1 d .
H11 H 0.5778 0.5120 0.7763 0.020 Uiso 1 1 calc R
C12 C 0.45949(17) 0.54613(16) 0.87423(12) 0.0189(4) Uani 1 1 d .
H12 H 0.5089 0.6107 0.9005 0.023 Uiso 1 1 calc R
C13 C 0.34516(18) 0.50992(16) 0.90933(13) 0.0202(4) Uani 1 1 d .
H13 H 0.3168 0.5496 0.9599 0.024 Uiso 1 1 calc R
C14 C 0.27255(17) 0.41582(16) 0.87044(12) 0.0178(4) Uani 1 1 d .
H14 H 0.1941 0.3922 0.8942 0.021 Uiso 1 1 calc R
N4 n 0.16675(13) -0.09713(12) 1.03286(9) 0.0114(3) Uani 1 1 d .
N3 n 0.11918(13) 0.07269(12) 0.91808(9) 0.0114(3) Uani 1 1 d .
N2 n 0.10534(13) 0.16044(12) 0.86016(9) 0.0127(3) Uani 1 1 d .
N1 n 0.21636(13) 0.16093(12) 0.82022(9) 0.0121(3) Uani 1 1 d .
Pd1 Pd 0.0000 0.0000 1.0000 0.00872(6) Uani 1 2 d S
B1 B 0.33808(19) 0.14512(19) 1.15817(14) 0.0184(4) Uani 1 1 d .
F1 F 0.32782(10) 0.18702(10) 1.06996(7) 0.0268(3) Uani 1 1 d .
F2 F 0.42621(12) 0.05011(12) 1.16598(9) 0.0389(3) Uani 1 1 d .
F3 F 0.21671(11) 0.10691(11) 1.17980(8) 0.0324(3) Uani 1 1 d .
F4 F 0.38499(12) 0.23393(11) 1.21670(8) 0.0352(3) Uani 1 1 d .
N5 n -0.06785(17) 0.33172(17) 1.07871(13) 0.0365(4) Uani 1 1 d .
C15 C 0.02923(19) 0.37874(17) 1.09896(13) 0.0240(4) Uani 1 1 d .
C16 C 0.1534(2) 0.4390(2) 1.12583(16) 0.0355(5) Uani 1 1 d .
H16A H 0.1538 0.5151 1.0949 0.053 Uiso 1 1 calc R
H16B H 0.2264 0.3907 1.1093 0.053 Uiso 1 1 calc R
H16C H 0.1634 0.4516 1.1914 0.053 Uiso 1 1 calc R
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'
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'
N N 0.0061 0.0033 '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
N4 C1 C2 121.95(15) . .
N4 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 119.32(16) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 119.04(16) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
C5 C4 C3 118.91(15) . .
C5 C4 H4 120.5 . .
C3 C4 H4 120.5 . .
N4 C5 C4 122.11(15) . .
N4 C5 C6 112.80(14) . .
C4 C5 C6 125.06(15) . .
N3 C6 C7 106.74(14) . .
N3 C6 C5 116.14(14) . .
C7 C6 C5 137.07(15) . .
N1 C7 C6 104.62(14) . .
N1 C7 H7 127.7 . .
C6 C7 H7 127.7 . .
N1 C8 C9 111.23(13) . .
N1 C8 H8A 109.4 . .
C9 C8 H8A 109.4 . .
N1 C8 H8B 109.4 . .
C9 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
C10 C9 C14 119.27(16) . .
C10 C9 C8 120.25(15) . .
C14 C9 C8 120.47(15) . .
C9 C10 C11 120.05(16) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C12 C11 C10 120.57(16) . .
C12 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C11 C12 C13 119.46(17) . .
C11 C12 H12 120.3 . .
C13 C12 H12 120.3 . .
C14 C13 C12 120.18(17) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C9 120.47(16) . .
C13 C14 H14 119.8 . .
C9 C14 H14 119.8 . .
C1 N4 C5 118.59(14) . .
C1 N4 Pd1 125.86(11) . .
C5 N4 Pd1 115.55(11) . .
N2 N3 C6 111.33(13) . .
N2 N3 Pd1 133.23(11) . .
C6 N3 Pd1 115.32(11) . .
N3 N2 N1 104.98(13) . .
N2 N1 C7 112.32(13) . .
N2 N1 C8 118.28(13) . .
C7 N1 C8 129.28(14) . .
N3 Pd1 N3 180.0 3_557 .
N3 Pd1 N4 100.41(5) 3_557 .
N3 Pd1 N4 79.59(5) . .
N3 Pd1 N4 79.59(5) 3_557 3_557
N3 Pd1 N4 100.41(5) . 3_557
N4 Pd1 N4 180.000(1) . 3_557
F4 B1 F3 109.87(15) . .
F4 B1 F1 109.25(16) . .
F3 B1 F1 110.49(15) . .
F4 B1 F2 109.47(16) . .
F3 B1 F2 108.91(16) . .
F1 B1 F2 108.84(15) . .
N5 C15 C16 179.4(2) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N4 1.341(2) .
C1 C2 1.392(2) .
C1 H1 0.9500 .
C2 C3 1.383(2) .
C2 H2 0.9500 .
C3 C4 1.390(2) .
C3 H3 0.9500 .
C4 C5 1.383(2) .
C4 H4 0.9500 .
C5 N4 1.362(2) .
C5 C6 1.457(2) .
C6 N3 1.363(2) .
C6 C7 1.370(2) .
C7 N1 1.356(2) .
C7 H7 0.9500 .
C8 N1 1.473(2) .
C8 C9 1.518(2) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.392(2) .
C9 C14 1.396(2) .
C10 C11 1.398(2) .
C10 H10 0.9500 .
C11 C12 1.385(3) .
C11 H11 0.9500 .
C12 C13 1.394(3) .
C12 H12 0.9500 .
C13 C14 1.391(3) .
C13 H13 0.9500 .
C14 H14 0.9500 .
N4 Pd1 2.0453(13) .
N3 N2 1.3148(19) .
N3 Pd1 1.9950(13) .
N2 N1 1.3385(19) .
Pd1 N3 1.9950(14) 3_557
Pd1 N4 2.0453(13) 3_557
B1 F4 1.383(2) .
B1 F3 1.386(2) .
B1 F1 1.389(2) .
B1 F2 1.403(2) .
N5 C15 1.139(3) .
C15 C16 1.460(3) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
