#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:17:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179718 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/20/7002008.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_7002008
loop_
_publ_author_name
'Zamora, Matthew T.'
'Ferguson, Michael J.'
'McDonald, Robert'
'Cowie, Martin'
_publ_section_title
;
 Carbene-anchored/pendent-imidazolium species as precursors to
 di-N-heterocyclic carbene-bridged mixed-metal complexes
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7269
_journal_paper_doi               10.1039/b906884h
_journal_year                    2009
_chemical_formula_moiety         'C23 H36 I2 N4 P Pd, I'
_chemical_formula_sum            'C23 H36 I3 N4 P Pd'
_chemical_formula_weight         886.63
_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                91.9746(12)
_cell_angle_beta                 100.9332(12)
_cell_angle_gamma                103.9630(12)
_cell_formula_units_Z            2
_cell_length_a                   9.4861(11)
_cell_length_b                   12.0320(13)
_cell_length_c                   14.0083(16)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.39
_cell_volume                     1518.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11967
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.732
_exptl_absorpt_correction_T_max  0.6405
_exptl_absorpt_correction_T_min  0.2626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.306
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00110(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0251
_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)+(0.0310P)²+4.1569P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                5815
_reflns_number_total             6159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906884h.txt
_cod_data_source_block           11b
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7002008
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
I1 I 0.41463(3) 0.25196(2) 0.320636(19) 0.02614(8) Uani 1 1 d . . .
I2 I -0.14776(3) 0.22052(2) 0.30385(2) 0.03133(8) Uani 1 1 d . . .
I3 I -0.13572(3) 0.65748(3) 0.06535(2) 0.03669(9) Uani 1 1 d . . .
Pd Pd 0.13349(3) 0.22879(2) 0.32139(2) 0.01982(8) Uani 1 1 d . . .
P P 0.08586(13) 0.04213(9) 0.25440(8) 0.0305(2) Uani 1 1 d . . .
N11 N 0.2072(3) 0.4500(3) 0.4645(2) 0.0200(6) Uani 1 1 d . . .
N12 N 0.1723(3) 0.4834(3) 0.3137(2) 0.0200(6) Uani 1 1 d . . .
N13 N 0.2566(3) 0.5365(3) 0.1669(2) 0.0213(6) Uani 1 1 d . . .
N14 N 0.3707(3) 0.6593(3) 0.0811(2) 0.0209(6) Uani 1 1 d . . .
C1A C 0.2059(5) 0.4677(4) 0.6405(3) 0.0328(9) Uani 1 1 d . . .
H1AA H 0.2761 0.5436 0.6503 0.039 Uiso 1 1 calc R . .
H1AB H 0.2165 0.4294 0.7011 0.039 Uiso 1 1 calc R . .
H1AC H 0.1044 0.4764 0.6222 0.039 Uiso 1 1 calc R . .
C1B C 0.4012(5) 0.3937(4) 0.5804(3) 0.0342(10) Uani 1 1 d . . .
H1BA H 0.4633 0.4725 0.5958 0.041 Uiso 1 1 calc R . .
H1BB H 0.4244 0.3590 0.5229 0.041 Uiso 1 1 calc R . .
H1BC H 0.4207 0.3485 0.6360 0.041 Uiso 1 1 calc R . .
C1C C 0.1371(7) 0.2749(4) 0.5510(3) 0.0484(13) Uani 1 1 d . . .
H1CA H 0.1552 0.2408 0.6133 0.058 Uiso 1 1 calc R . .
H1CB H 0.1578 0.2275 0.4996 0.058 Uiso 1 1 calc R . .
H1CC H 0.0332 0.2784 0.5346 0.058 Uiso 1 1 calc R . .
C1D C 0.2660(5) 0.7982(4) -0.0161(3) 0.0325(9) Uani 1 1 d . . .
H1DA H 0.1809 0.7380 -0.0512 0.039 Uiso 1 1 calc R . .
H1DB H 0.2878 0.8615 -0.0575 0.039 Uiso 1 1 calc R . .
H1DC H 0.2428 0.8267 0.0439 0.039 Uiso 1 1 calc R . .
C1E C 0.5375(5) 0.8421(4) 0.0591(4) 0.0375(10) Uani 1 1 d . . .
H1EA H 0.5643 0.8989 0.0128 0.045 Uiso 1 1 calc R . .
H1EB H 0.6202 0.8072 0.0806 0.045 Uiso 1 1 calc R . .
H1EC H 0.5158 0.8800 0.1156 0.045 Uiso 1 1 calc R . .
C1F C 0.4292(6) 0.6896(4) -0.0800(3) 0.0370(10) Uani 1 1 d . . .
H1FA H 0.3378 0.6341 -0.1133 0.044 Uiso 1 1 calc R . .
H1FB H 0.5069 0.6494 -0.0597 0.044 Uiso 1 1 calc R . .
H1FC H 0.4614 0.7471 -0.1245 0.044 Uiso 1 1 calc R . .
C10 C 0.2379(5) 0.3955(3) 0.5594(3) 0.0275(8) Uani 1 1 d . . .
C11 C 0.1772(4) 0.3974(3) 0.3736(3) 0.0192(7) Uani 1 1 d . . .
C12 C 0.2224(4) 0.5677(3) 0.4605(3) 0.0251(8) Uani 1 1 d . . .
H12 H 0.2451 0.6232 0.5147 0.030 Uiso 1 1 calc R . .
C13 C 0.1991(4) 0.5882(3) 0.3663(3) 0.0249(8) Uani 1 1 d . . .
H13 H 0.2008 0.6604 0.3406 0.030 Uiso 1 1 calc R . .
C14 C 0.1369(4) 0.4673(3) 0.2076(3) 0.0233(8) Uani 1 1 d . . .
H14A H 0.0437 0.4897 0.1828 0.028 Uiso 1 1 calc R . .
H14B H 0.1214 0.3851 0.1864 0.028 Uiso 1 1 calc R . .
C15 C 0.2421(4) 0.6199(3) 0.1083(3) 0.0223(7) Uani 1 1 d . . .
H15 H 0.1552 0.6465 0.0894 0.027 Uiso 1 1 calc R . .
C16 C 0.3979(4) 0.5208(4) 0.1751(3) 0.0266(8) Uani 1 1 d . . .
H16 H 0.4373 0.4662 0.2116 0.032 Uiso 1 1 calc R . .
C17 C 0.4690(4) 0.5978(4) 0.1217(3) 0.0269(8) Uani 1 1 d . . .
H17 H 0.5683 0.6078 0.1134 0.032 Uiso 1 1 calc R . .
C18 C 0.4004(4) 0.7488(3) 0.0094(3) 0.0252(8) Uani 1 1 d . . .
C21 C 0.2139(5) -0.0365(3) 0.3145(3) 0.0298(9) Uani 1 1 d . . .
C22 C 0.3199(6) -0.0669(4) 0.2706(3) 0.0426(11) Uani 1 1 d . . .
H22 H 0.3214 -0.0533 0.2043 0.051 Uiso 1 1 calc R . .
C23 C 0.4245(7) -0.1175(5) 0.3235(4) 0.0504(13) Uani 1 1 d . . .
H23 H 0.4965 -0.1387 0.2929 0.060 Uiso 1 1 calc R . .
C24 C 0.4240(6) -0.1369(4) 0.4190(4) 0.0429(11) Uani 1 1 d . . .
H24 H 0.4966 -0.1701 0.4549 0.052 Uiso 1 1 calc R . .
C25 C 0.3188(6) -0.1083(4) 0.4630(3) 0.0421(11) Uani 1 1 d . . .
H25 H 0.3174 -0.1229 0.5291 0.051 Uiso 1 1 calc R . .
C26 C 0.2140(5) -0.0579(4) 0.4111(3) 0.0362(10) Uani 1 1 d . . .
H26 H 0.1418 -0.0379 0.4421 0.043 Uiso 1 1 calc R . .
C27 C 0.0990(8) 0.0389(5) 0.1274(3) 0.0552(16) Uani 1 1 d . . .
H27A H 0.0801 -0.0410 0.1010 0.066 Uiso 1 1 calc R . .
H27B H 0.1987 0.0812 0.1216 0.066 Uiso 1 1 calc R . .
H27C H 0.0253 0.0746 0.0908 0.066 Uiso 1 1 calc R . .
C28 C -0.0942(6) -0.0551(4) 0.2528(5) 0.0559(15) Uani 1 1 d . . .
H28A H -0.0968 -0.1313 0.2244 0.067 Uiso 1 1 calc R . .
H28B H -0.1720 -0.0256 0.2134 0.067 Uiso 1 1 calc R . .
H28C H -0.1107 -0.0607 0.3196 0.067 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 '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
C11 Pd P 176.92(10) . . ?
C11 Pd I2 87.45(10) . . ?
P Pd I2 93.00(3) . . ?
C11 Pd I1 90.49(10) . . ?
P Pd I1 88.70(3) . . ?
I2 Pd I1 173.030(14) . . ?
C27 P C21 106.6(2) . . ?
C27 P C28 103.3(3) . . ?
C21 P C28 102.7(2) . . ?
C27 P Pd 111.01(19) . . ?
C21 P Pd 113.35(13) . . ?
C28 P Pd 118.78(19) . . ?
C11 N11 C12 110.4(3) . . ?
C11 N11 C10 126.6(3) . . ?
C12 N11 C10 122.6(3) . . ?
C11 N12 C13 111.3(3) . . ?
C11 N12 C14 124.7(3) . . ?
C13 N12 C14 123.9(3) . . ?
C15 N13 C16 108.9(3) . . ?
C15 N13 C14 124.6(3) . . ?
C16 N13 C14 126.4(3) . . ?
C15 N14 C17 109.0(3) . . ?
C15 N14 C18 125.7(3) . . ?
C17 N14 C18 125.0(3) . . ?
N11 C10 C1C 109.8(3) . . ?
N11 C10 C1A 108.8(3) . . ?
C1C C10 C1A 108.9(4) . . ?
N11 C10 C1B 107.7(3) . . ?
C1C C10 C1B 111.3(4) . . ?
C1A C10 C1B 110.3(3) . . ?
N11 C11 N12 104.5(3) . . ?
N11 C11 Pd 133.0(3) . . ?
N12 C11 Pd 122.4(3) . . ?
C13 C12 N11 107.3(3) . . ?
C12 C13 N12 106.4(3) . . ?
N12 C14 N13 110.6(3) . . ?
N14 C15 N13 108.0(3) . . ?
C17 C16 N13 106.9(3) . . ?
C16 C17 N14 107.2(3) . . ?
N14 C18 C1F 107.3(3) . . ?
N14 C18 C1D 108.8(3) . . ?
C1F C18 C1D 111.5(4) . . ?
N14 C18 C1E 107.3(3) . . ?
C1F C18 C1E 110.9(4) . . ?
C1D C18 C1E 110.8(4) . . ?
C26 C21 C22 118.6(4) . . ?
C26 C21 P 118.5(3) . . ?
C22 C21 P 122.6(3) . . ?
C21 C22 C23 120.1(5) . . ?
C24 C23 C22 120.5(5) . . ?
C23 C24 C25 120.0(5) . . ?
C24 C25 C26 120.1(4) . . ?
C21 C26 C25 120.7(5) . . ?
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
I1 Pd 2.6158(5) . ?
I2 Pd 2.6095(5) . ?
Pd C11 2.049(4) . ?
Pd P 2.3093(11) . ?
P C27 1.806(5) . ?
P C21 1.816(4) . ?
P C28 1.818(5) . ?
N11 C11 1.350(5) . ?
N11 C12 1.393(5) . ?
N11 C10 1.513(5) . ?
N12 C11 1.359(5) . ?
N12 C13 1.380(5) . ?
N12 C14 1.456(5) . ?
N13 C15 1.334(5) . ?
N13 C16 1.382(5) . ?
N13 C14 1.459(4) . ?
N14 C15 1.329(5) . ?
N14 C17 1.379(5) . ?
N14 C18 1.511(5) . ?
C1A C10 1.525(6) . ?
C1B C10 1.527(6) . ?
C1C C10 1.520(6) . ?
C1D C18 1.521(5) . ?
C1E C18 1.527(6) . ?
C1F C18 1.520(6) . ?
C12 C13 1.339(6) . ?
C16 C17 1.346(6) . ?
C21 C26 1.385(6) . ?
C21 C22 1.386(7) . ?
C22 C23 1.395(7) . ?
C23 C24 1.367(7) . ?
C24 C25 1.371(8) . ?
C25 C26 1.389(7) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 Pd P C27 1.2(19) . . . . ?
I2 Pd P C27 99.5(2) . . . . ?
I1 Pd P C27 -73.7(2) . . . . ?
C11 Pd P C21 121.1(19) . . . . ?
I2 Pd P C21 -140.57(16) . . . . ?
I1 Pd P C21 46.20(16) . . . . ?
C11 Pd P C28 -118.3(19) . . . . ?
I2 Pd P C28 -19.9(2) . . . . ?
I1 Pd P C28 166.8(2) . . . . ?
C11 N11 C10 C1C -38.8(5) . . . . ?
C12 N11 C10 C1C 148.3(4) . . . . ?
C11 N11 C10 C1A -157.9(3) . . . . ?
C12 N11 C10 C1A 29.2(5) . . . . ?
C11 N11 C10 C1B 82.6(4) . . . . ?
C12 N11 C10 C1B -90.3(4) . . . . ?
C12 N11 C11 N12 -0.7(4) . . . . ?
C10 N11 C11 N12 -174.3(3) . . . . ?
C12 N11 C11 Pd -177.3(3) . . . . ?
C10 N11 C11 Pd 9.1(6) . . . . ?
C13 N12 C11 N11 0.1(4) . . . . ?
C14 N12 C11 N11 -177.3(3) . . . . ?
C13 N12 C11 Pd 177.2(2) . . . . ?
C14 N12 C11 Pd -0.2(5) . . . . ?
P Pd C11 N11 -168.0(16) . . . . ?
I2 Pd C11 N11 93.6(3) . . . . ?
I1 Pd C11 N11 -93.1(3) . . . . ?
P Pd C11 N12 16(2) . . . . ?
I2 Pd C11 N12 -82.6(3) . . . . ?
I1 Pd C11 N12 90.8(3) . . . . ?
C11 N11 C12 C13 1.0(4) . . . . ?
C10 N11 C12 C13 174.9(3) . . . . ?
N11 C12 C13 N12 -0.9(4) . . . . ?
C11 N12 C13 C12 0.5(4) . . . . ?
C14 N12 C13 C12 178.0(3) . . . . ?
C11 N12 C14 N13 -123.2(4) . . . . ?
C13 N12 C14 N13 59.6(5) . . . . ?
C15 N13 C14 N12 -118.5(4) . . . . ?
C16 N13 C14 N12 67.5(5) . . . . ?
C17 N14 C15 N13 1.3(4) . . . . ?
C18 N14 C15 N13 175.7(3) . . . . ?
C16 N13 C15 N14 -1.4(4) . . . . ?
C14 N13 C15 N14 -176.4(3) . . . . ?
C15 N13 C16 C17 1.0(5) . . . . ?
C14 N13 C16 C17 175.8(4) . . . . ?
N13 C16 C17 N14 -0.2(5) . . . . ?
C15 N14 C17 C16 -0.7(5) . . . . ?
C18 N14 C17 C16 -175.2(4) . . . . ?
C15 N14 C18 C1F -113.3(4) . . . . ?
C17 N14 C18 C1F 60.3(5) . . . . ?
C15 N14 C18 C1D 7.5(5) . . . . ?
C17 N14 C18 C1D -178.9(4) . . . . ?
C15 N14 C18 C1E 127.5(4) . . . . ?
C17 N14 C18 C1E -59.0(5) . . . . ?
C27 P C21 C26 -173.1(4) . . . . ?
C28 P C21 C26 -64.8(4) . . . . ?
Pd P C21 C26 64.5(4) . . . . ?
C27 P C21 C22 12.7(5) . . . . ?
C28 P C21 C22 120.9(4) . . . . ?
Pd P C21 C22 -109.7(4) . . . . ?
C26 C21 C22 C23 -0.3(7) . . . . ?
P C21 C22 C23 173.9(4) . . . . ?
C21 C22 C23 C24 -0.4(8) . . . . ?
C22 C23 C24 C25 1.1(8) . . . . ?
C23 C24 C25 C26 -1.0(8) . . . . ?
C22 C21 C26 C25 0.4(7) . . . . ?
P C21 C26 C25 -174.1(4) . . . . ?
C24 C25 C26 C21 0.3(7) . . . . ?
