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#$Date: 2016-03-21 06:17:59 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178502 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/40/4064002.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_4064002
loop_
_publ_author_name
'Poulain, Aurélie'
'Canseco-Gonzalez, Daniel'
'Hynes-Roche, Rachel'
'Müller-Bunz, Helge'
'Schuster, Oliver'
'Stoeckli-Evans, Helen'
'Neels, Antonia'
'Albrecht, Martin'
_publ_section_title
;
 Synthesis and Tunability of Abnormal 1,2,3-Triazolylidene Palladium and
 Rhodium Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1021
_journal_paper_doi               10.1021/om101076u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C22 H26 Cl2 N6 Pd'
_chemical_formula_sum            'C22 H26 Cl2 N6 Pd'
_chemical_formula_weight         551.79
_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                108.081(3)
_cell_angle_beta                 115.551(3)
_cell_angle_gamma                91.735(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2661(2)
_cell_length_b                   8.8875(3)
_cell_length_c                   9.3445(3)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5986
_cell_measurement_theta_min      5.6170
_cell_volume                     577.89(4)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0214
_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       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8246
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.80
_diffrn_reflns_theta_min         5.62
_exptl_absorpt_coefficient_mu    8.776
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.2705
_exptl_crystal_size_mid          0.1736
_exptl_crystal_size_min          0.1662
_refine_diff_density_max         1.716
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0032(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0714P)²+2.3112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                2401
_reflns_number_total             2401
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om101076u_si_002.cif
_cod_data_source_block           complex-4a
_cod_original_cell_volume        577.89(3)
_cod_database_code               4064002
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
Pd1 Pd 0.5000 0.5000 0.5000 0.01083(17) Uani 1 2 d S
Cl Cl 0.27856(11) 0.61269(11) 0.57094(10) 0.0153(2) Uani 1 1 d .
N1 N 0.2040(4) 0.2780(4) 0.1590(4) 0.0145(6) Uani 1 1 d .
N2 N 0.1008(5) 0.2475(4) -0.0065(4) 0.0186(7) Uani 1 1 d .
N3 N 0.1549(4) 0.3779(4) -0.0268(4) 0.0162(6) Uani 1 1 d .
C1 C 0.3209(5) 0.4227(4) 0.2476(4) 0.0123(7) Uani 1 1 d .
C2 C 0.2882(5) 0.4881(5) 0.1215(5) 0.0136(7) Uani 1 1 d .
C3 C 0.3822(5) 0.6425(5) 0.1416(5) 0.0147(7) Uani 1 1 d .
C4 C 0.0690(6) 0.3798(6) -0.2003(5) 0.0232(9) Uani 1 1 d .
H4A H 0.1468 0.3435 -0.2540 0.035 Uiso 1 1 calc R
H4B H 0.0534 0.4897 -0.1962 0.035 Uiso 1 1 calc R
H4C H -0.0506 0.3075 -0.2665 0.035 Uiso 1 1 calc R
C5 C 0.1795(6) 0.1553(5) 0.2273(5) 0.0200(8) Uani 1 1 d .
H5A H 0.2959 0.1619 0.3262 0.024 Uiso 1 1 calc R
H5B H 0.1478 0.0468 0.1395 0.024 Uiso 1 1 calc R
C6 C 0.0312(7) 0.1778(6) 0.2810(7) 0.0337(11) Uani 1 1 d .
H6A H 0.0631 0.2845 0.3691 0.051 Uiso 1 1 calc R
H6B H 0.0191 0.0945 0.3260 0.051 Uiso 1 1 calc R
H6C H -0.0848 0.1689 0.1827 0.051 Uiso 1 1 calc R
C7 C 0.4093(6) 0.6673(5) 0.0120(5) 0.0179(8) Uani 1 1 d .
H7 H 0.3579 0.5854 -0.0976 0.021 Uiso 1 1 calc R
C8 C 0.5111(6) 0.8115(5) 0.0437(6) 0.0214(8) Uani 1 1 d .
H8 H 0.5280 0.8280 -0.0450 0.026 Uiso 1 1 calc R
C9 C 0.5889(6) 0.9326(5) 0.2041(6) 0.0221(8) Uani 1 1 d .
H9 H 0.6608 1.0300 0.2254 0.027 Uiso 1 1 calc R
C10 C 0.5606(6) 0.9095(5) 0.3322(5) 0.0214(8) Uani 1 1 d .
H10 H 0.6122 0.9918 0.4415 0.026 Uiso 1 1 calc R
C11 C 0.4559(6) 0.7650(5) 0.3005(5) 0.0188(8) Uani 1 1 d .
H11 H 0.4350 0.7506 0.3881 0.023 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
C1 Pd1 C1 180.00(15) . 2_666
C1 Pd1 Cl 88.81(10) . 2_666
C1 Pd1 Cl 91.19(10) 2_666 2_666
C1 Pd1 Cl 91.19(10) . .
C1 Pd1 Cl 88.81(10) 2_666 .
Cl Pd1 Cl 179.999(1) 2_666 .
N2 N1 C1 115.4(3) . .
N2 N1 C5 117.9(3) . .
C1 N1 C5 126.8(3) . .
N3 N2 N1 103.1(3) . .
N2 N3 C2 112.5(3) . .
N2 N3 C4 116.6(3) . .
C2 N3 C4 130.8(3) . .
N1 C1 C2 102.5(3) . .
N1 C1 Pd1 124.3(3) . .
C2 C1 Pd1 133.1(3) . .
N3 C2 C1 106.5(3) . .
N3 C2 C3 126.2(3) . .
C1 C2 C3 127.3(3) . .
C11 C3 C7 119.2(4) . .
C11 C3 C2 117.7(3) . .
C7 C3 C2 123.1(3) . .
N3 C4 H4A 109.5 . .
N3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 C6 111.7(4) . .
N1 C5 H5A 109.3 . .
C6 C5 H5A 109.3 . .
N1 C5 H5B 109.3 . .
C6 C5 H5B 109.3 . .
H5A C5 H5B 107.9 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 C3 120.0(4) . .
C8 C7 H7 120.0 . .
C3 C7 H7 120.0 . .
C7 C8 C9 120.9(4) . .
C7 C8 H8 119.6 . .
C9 C8 H8 119.6 . .
C10 C9 C8 119.4(4) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C11 120.1(4) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C3 C11 C10 120.5(4) . .
C3 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 2.037(3) .
Pd1 C1 2.037(3) 2_666
Pd1 Cl 2.3534(8) 2_666
Pd1 Cl 2.3534(8) .
N1 N2 1.334(4) .
N1 C1 1.359(5) .
N1 C5 1.472(5) .
N2 N3 1.326(5) .
N3 C2 1.367(5) .
N3 C4 1.469(5) .
C1 C2 1.399(5) .
C2 C3 1.474(5) .
C3 C11 1.392(6) .
C3 C7 1.401(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.509(6) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.386(6) .
C7 H7 0.9500 .
C8 C9 1.394(6) .
C8 H8 0.9500 .
C9 C10 1.386(6) .
C9 H9 0.9500 .
C10 C11 1.400(6) .
C10 H10 0.9500 .
C11 H11 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C1 N1 N2 N3 0.8(4) .
C5 N1 N2 N3 -179.9(3) .
N1 N2 N3 C2 -0.1(4) .
N1 N2 N3 C4 178.3(3) .
N2 N1 C1 C2 -1.0(4) .
C5 N1 C1 C2 179.7(4) .
N2 N1 C1 Pd1 -178.2(3) .
C5 N1 C1 Pd1 2.5(5) .
C1 Pd1 C1 N1 24(7) 2_666
Cl Pd1 C1 N1 91.6(3) 2_666
Cl Pd1 C1 N1 -88.4(3) .
C1 Pd1 C1 C2 -153(7) 2_666
Cl Pd1 C1 C2 -84.7(4) 2_666
Cl Pd1 C1 C2 95.3(4) .
N2 N3 C2 C1 -0.5(4) .
C4 N3 C2 C1 -178.6(4) .
N2 N3 C2 C3 177.6(3) .
C4 N3 C2 C3 -0.5(6) .
N1 C1 C2 N3 0.8(4) .
Pd1 C1 C2 N3 177.7(3) .
N1 C1 C2 C3 -177.2(4) .
Pd1 C1 C2 C3 -0.4(6) .
N3 C2 C3 C11 154.7(4) .
C1 C2 C3 C11 -27.5(6) .
N3 C2 C3 C7 -29.1(6) .
C1 C2 C3 C7 148.6(4) .
N2 N1 C5 C6 -87.8(4) .
C1 N1 C5 C6 91.5(5) .
C11 C3 C7 C8 1.1(6) .
C2 C3 C7 C8 -175.0(4) .
C3 C7 C8 C9 0.6(6) .
C7 C8 C9 C10 -1.4(6) .
C8 C9 C10 C11 0.6(6) .
C7 C3 C11 C10 -1.9(6) .
C2 C3 C11 C10 174.4(4) .
C9 C10 C11 C3 1.1(6) .
