#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:06:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179826 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/22/7012247.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_7012247
loop_
_publ_author_name
'Tulloch, Arran A. D.'
'Winston, Scott'
'Danopoulos, Andreas A.'
'Eastham, Graham'
'Hursthouse, Michael B.'
_publ_section_title
;
 Functionalised and chelate heterocyclic carbene complexes of
 palladium; synthesis and structural studiesElectronic supplementary
 information (ESI) available: crystallographic data and ORTEP plots for
 complexes 4, 7, 8 and 13. See
 http://www.rsc.org/suppdata/dt/b2/b209231j/
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              699
_journal_paper_doi               10.1039/b209231j
_journal_year                    2003
_chemical_formula_moiety         'C34 H48 Cl2 N4 O2 Pd'
_chemical_formula_sum            'C34 H48 Cl2 N4 O2 Pd'
_chemical_formula_weight         722.11
_chemical_name_common            01sw053
_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                74.5110(10)
_cell_angle_beta                 78.0540(10)
_cell_angle_gamma                79.5380(10)
_cell_formula_units_Z            1
_cell_length_a                   8.1120(2)
_cell_length_b                   9.1241(2)
_cell_length_c                   12.5173(4)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     865.61(4)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'Denzo a. Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'Phi and omega scans to fill ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_sigmaI/netI    0.0825
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12165
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.27946
_exptl_absorpt_correction_T_min  0.84709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sortav
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.577
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0352P)²+0.2474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                3492
_reflns_number_total             3868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b209231j.txt
_cod_data_source_block           Compound11
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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               7012247
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 0.5000 0.0000 0.5000 0.01589(10) Uani 1 2 d S . .
Cl1 Cl 0.28973(8) 0.19418(7) 0.53904(5) 0.02344(15) Uani 1 1 d . . .
O1 O 0.8419(3) 0.3493(2) 0.40803(15) 0.0320(5) Uani 1 1 d . . .
N1 N 0.7825(3) 0.1302(2) 0.55341(16) 0.0196(4) Uani 1 1 d . . .
N2 N 0.6392(2) 0.0140(2) 0.70587(15) 0.0158(4) Uani 1 1 d . . .
C1 C 0.6480(3) 0.0512(3) 0.59302(18) 0.0174(5) Uani 1 1 d . . .
C2 C 0.7660(3) 0.0711(3) 0.7357(2) 0.0234(5) Uani 1 1 d . . .
H2 H 0.7854 0.0607 0.8081 0.039(9) Uiso 1 1 d R . .
C3 C 0.8556(3) 0.1448(3) 0.6398(2) 0.0241(5) Uani 1 1 d . . .
H3 H 0.9480 0.1956 0.6329 0.020(7) Uiso 1 1 d R . .
C4 C 0.8487(4) 0.1908(3) 0.4342(2) 0.0256(6) Uani 1 1 d . . .
H4A H 0.7832 0.1628 0.3879 0.019(7) Uiso 1 1 d R . .
H4B H 0.9657 0.1449 0.4174 0.029(8) Uiso 1 1 d R . .
C5 C 0.6772(5) 0.4269(4) 0.4015(3) 0.0533(10) Uani 1 1 d . . .
H5A H 0.5992 0.3836 0.4640 0.085(15) Uiso 1 1 d R . .
H5B H 0.6761 0.5302 0.4010 0.049(10) Uiso 1 1 d R . .
H5C H 0.6257 0.3968 0.3450 0.14(3) Uiso 1 1 d R . .
C6 C 0.5215(3) -0.0829(3) 0.78422(18) 0.0181(5) Uani 1 1 d . . .
C7 C 0.3695(3) -0.0124(3) 0.83461(19) 0.0197(5) Uani 1 1 d . . .
C8 C 0.2567(3) -0.1102(3) 0.9069(2) 0.0265(6) Uani 1 1 d . . .
H8 H 0.1533 -0.0679 0.9419 0.015(6) Uiso 1 1 d R . .
C9 C 0.2967(4) -0.2663(3) 0.9266(2) 0.0303(6) Uani 1 1 d . . .
H9 H 0.2188 -0.3286 0.9733 0.030(8) Uiso 1 1 d R . .
C10 C 0.4511(4) -0.3329(3) 0.8774(2) 0.0278(6) Uani 1 1 d . . .
H10 H 0.4768 -0.4392 0.8932 0.024(7) Uiso 1 1 d R . .
C11 C 0.5694(3) -0.2422(3) 0.80458(19) 0.0210(5) Uani 1 1 d . . .
C12 C 0.3294(3) 0.1598(3) 0.8183(2) 0.0224(5) Uani 1 1 d . . .
H12 H 0.3873 0.2070 0.7434 0.017(7) Uiso 1 1 d R . .
C13 C 0.3990(4) 0.2126(4) 0.9047(2) 0.0357(7) Uani 1 1 d . . .
H13A H 0.5185 0.1889 0.8946 0.065(12) Uiso 1 1 d R . .
H13B H 0.3693 0.3197 0.8961 0.053(10) Uiso 1 1 d R . .
H13C H 0.3523 0.1619 0.9779 0.062(12) Uiso 1 1 d R . .
C14 C 0.1399(4) 0.2196(4) 0.8247(2) 0.0335(7) Uani 1 1 d . . .
H14A H 0.0832 0.1894 0.9004 0.045(10) Uiso 1 1 d R . .
H14B H 0.1244 0.3288 0.8006 0.044(9) Uiso 1 1 d R . .
H14C H 0.0931 0.1777 0.7774 0.043(9) Uiso 1 1 d R . .
C15 C 0.7417(3) -0.3141(3) 0.7562(2) 0.0240(6) Uani 1 1 d . . .
H15 H 0.7813 -0.2432 0.6853 0.025(7) Uiso 1 1 d R . .
C16 C 0.8708(4) -0.3325(4) 0.8352(2) 0.0316(6) Uani 1 1 d . . .
H16A H 0.9801 -0.3755 0.8021 0.040(9) Uiso 1 1 d R . .
H16B H 0.8787 -0.2341 0.8461 0.042(9) Uiso 1 1 d R . .
H16C H 0.8345 -0.3995 0.9064 0.038(9) Uiso 1 1 d R . .
C17 C 0.7424(4) -0.4690(3) 0.7303(2) 0.0345(7) Uani 1 1 d . . .
H17A H 0.7204 -0.5453 0.7993 0.044(9) Uiso 1 1 d R . .
H17B H 0.6561 -0.4600 0.6860 0.027(8) Uiso 1 1 d R . .
H17C H 0.8513 -0.4988 0.6892 0.037(9) Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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 C1 180.000(1) . 2_656 ?
C1 Pd1 Cl1 91.09(7) . . ?
C1 Pd1 Cl1 88.91(7) 2_656 . ?
C1 Pd1 Cl1 88.91(7) . 2_656 ?
C1 Pd1 Cl1 91.09(7) 2_656 2_656 ?
Cl1 Pd1 Cl1 180.00(3) . 2_656 ?
C4 O1 C5 113.2(2) . . ?
C1 N1 C3 111.52(19) . . ?
C1 N1 C4 125.5(2) . . ?
C3 N1 C4 123.0(2) . . ?
C1 N2 C2 110.80(19) . . ?
C1 N2 C6 124.31(19) . . ?
C2 N2 C6 124.72(19) . . ?
N1 C1 N2 104.45(19) . . ?
N1 C1 Pd1 126.38(16) . . ?
N2 C1 Pd1 129.16(16) . . ?
C3 C2 N2 107.0(2) . . ?
C2 C3 N1 106.3(2) . . ?
O1 C4 N1 111.6(2) . . ?
C7 C6 C11 124.2(2) . . ?
C7 C6 N2 118.2(2) . . ?
C11 C6 N2 117.5(2) . . ?
C6 C7 C8 116.5(3) . . ?
C6 C7 C12 122.5(2) . . ?
C8 C7 C12 120.9(2) . . ?
C9 C8 C7 121.1(3) . . ?
C8 C9 C10 121.0(2) . . ?
C9 C10 C11 120.8(3) . . ?
C10 C11 C6 116.3(2) . . ?
C10 C11 C15 121.0(3) . . ?
C6 C11 C15 122.7(2) . . ?
C7 C12 C14 113.8(2) . . ?
C7 C12 C13 110.6(2) . . ?
C14 C12 C13 109.0(2) . . ?
C11 C15 C17 114.6(2) . . ?
C11 C15 C16 110.5(2) . . ?
C17 C15 C16 109.1(2) . . ?
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 2.022(2) . ?
Pd1 C1 2.022(2) 2_656 ?
Pd1 Cl1 2.3037(6) . ?
Pd1 Cl1 2.3037(6) 2_656 ?
O1 C4 1.388(3) . ?
O1 C5 1.402(4) . ?
N1 C1 1.351(3) . ?
N1 C3 1.383(3) . ?
N1 C4 1.468(3) . ?
N2 C1 1.352(3) . ?
N2 C2 1.388(3) . ?
N2 C6 1.453(3) . ?
C2 C3 1.344(3) . ?
C6 C7 1.393(4) . ?
C6 C11 1.402(4) . ?
C7 C8 1.405(3) . ?
C7 C12 1.512(4) . ?
C8 C9 1.368(4) . ?
C9 C10 1.387(4) . ?
C10 C11 1.400(3) . ?
C11 C15 1.510(4) . ?
C12 C14 1.528(4) . ?
C12 C13 1.534(4) . ?
C15 C17 1.531(4) . ?
C15 C16 1.542(4) . ?
