#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/11/7031193.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_7031193
loop_
_publ_author_name
'Sureshbabu, Bemineni'
'Ramkumar, Venkatachalam'
'Sankararaman, Sethuraman'
_publ_section_title
;
 Facile base-free in situ generation and palladation of mesoionic and
 normal N-heterocyclic carbenes at ambient conditions.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10710
_journal_page_last               10712
_journal_paper_doi               10.1039/c4dt01112k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C30 H26 I2 N6 Pd'
_chemical_formula_sum            'C30 H26 I2 N6 Pd'
_chemical_formula_weight         830.77
_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                100.783(2)
_cell_angle_beta                 90.525(2)
_cell_angle_gamma                116.372(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0912(4)
_cell_length_b                   9.6479(5)
_cell_length_c                   9.7378(4)
_cell_measurement_reflns_used    4005
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.14
_cell_volume                     747.57(6)
_computing_cell_refinement       'APEX2 and SAINT (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        'SAINT and XPREP (Bruker-Nonius, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0302
_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            8349
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.6862
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0387
_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)+(0.0432P)²+2.4979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                1895
_reflns_number_total             2543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01112k2.cif
_cod_data_source_block           new
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031193--7031196.cif.
;
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031193
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
C1 C 0.3421(8) 0.7656(7) 0.9614(7) 0.0477(16) Uani 1 1 d .
C2 C 0.3276(8) 0.6480(7) 1.0315(8) 0.0490(16) Uani 1 1 d .
C3 C 0.4178(9) 0.6588(8) 1.1594(9) 0.0593(19) Uani 1 1 d .
C4 C 0.4738(14) 0.7938(12) 1.2650(10) 0.096(3) Uani 1 1 d .
H4 H 0.4533 0.8773 1.2529 0.115 Uiso 1 1 calc R
C5 C 0.5602(17) 0.8064(15) 1.3883(12) 0.118(4) Uani 1 1 d .
H5 H 0.5984 0.8982 1.4582 0.142 Uiso 1 1 calc R
C6 C 0.5891(13) 0.6838(15) 1.4072(12) 0.096(3) Uani 1 1 d .
H6 H 0.6453 0.6921 1.4910 0.115 Uiso 1 1 calc R
C7 C 0.5391(14) 0.5546(15) 1.3091(12) 0.098(3) Uani 1 1 d .
H7 H 0.5620 0.4731 1.3231 0.118 Uiso 1 1 calc R
C8 C 0.4512(11) 0.5384(11) 1.1835(10) 0.078(2) Uani 1 1 d .
H8 H 0.4149 0.4454 1.1153 0.093 Uiso 1 1 calc R
C9 C 0.1299(15) 0.3450(12) 0.9684(15) 0.130(5) Uani 1 1 d .
H9A H 0.0212 0.2865 0.9189 0.195 Uiso 1 1 calc R
H9B H 0.1234 0.3445 1.0666 0.195 Uiso 1 1 calc R
H9C H 0.1980 0.2970 0.9319 0.195 Uiso 1 1 calc R
C10 C 0.1786(9) 0.7378(10) 0.7345(9) 0.065(2) Uani 1 1 d .
C11 C 0.2011(18) 0.682(2) 0.6016(13) 0.141(6) Uani 1 1 d .
H11 H 0.2534 0.6179 0.5865 0.169 Uiso 1 1 calc R
C12 C 0.146(2) 0.722(2) 0.4872(14) 0.168(7) Uani 1 1 d .
H12 H 0.1570 0.6818 0.3956 0.201 Uiso 1 1 calc R
C13 C 0.0746(16) 0.821(2) 0.5136(14) 0.133(5) Uani 1 1 d .
H13 H 0.0415 0.8527 0.4396 0.159 Uiso 1 1 calc R
C14 C 0.0525(16) 0.8718(19) 0.6422(15) 0.134(5) Uani 1 1 d .
H14 H -0.0003 0.9359 0.6577 0.161 Uiso 1 1 calc R
C15 C 0.1060(14) 0.8322(14) 0.7558(11) 0.102(3) Uani 1 1 d .
H15 H 0.0913 0.8715 0.8467 0.122 Uiso 1 1 calc R
I1 I 0.29289(6) 1.06884(6) 1.14742(6) 0.0699(2) Uani 1 1 d .
N1 N 0.2017(8) 0.5082(7) 0.9495(9) 0.075(2) Uani 1 1 d .
N2 N 0.1394(8) 0.5291(8) 0.8410(9) 0.079(2) Uani 1 1 d .
N3 N 0.2239(7) 0.6831(7) 0.8468(7) 0.0597(16) Uani 1 1 d .
Pd1 Pd 0.5000 1.0000 1.0000 0.0459(2) Uani 1 2 d S
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'
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'
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
N3 C1 C2 103.1(6) . .
N3 C1 Pd1 125.5(5) . .
C2 C1 Pd1 131.4(5) . .
C1 C2 N1 104.5(6) . .
C1 C2 C3 130.0(6) . .
N1 C2 C3 125.5(6) . .
C4 C3 C8 117.0(8) . .
C4 C3 C2 119.9(7) . .
C8 C3 C2 123.0(8) . .
C3 C4 C5 120.8(10) . .
C3 C4 H4 119.6 . .
C5 C4 H4 119.6 . .
C6 C5 C4 119.8(11) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
C7 C6 C5 121.1(11) . .
C7 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C6 C7 C8 120.4(10) . .
C6 C7 H7 119.8 . .
C8 C7 H7 119.8 . .
C3 C8 C7 120.8(9) . .
C3 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C15 C10 C11 119.7(9) . .
C15 C10 N3 121.9(8) . .
C11 C10 N3 118.2(8) . .
C10 C11 C12 120.2(11) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C13 C12 C11 118.2(13) . .
C13 C12 H12 120.9 . .
C11 C12 H12 120.9 . .
C14 C13 C12 120.6(12) . .
C14 C13 H13 119.7 . .
C12 C13 H13 119.7 . .
C13 C14 C15 121.4(12) . .
C13 C14 H14 119.3 . .
C15 C14 H14 119.3 . .
C10 C15 C14 119.7(10) . .
C10 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
N2 N1 C2 113.9(6) . .
N2 N1 C9 115.3(8) . .
C2 N1 C9 130.8(9) . .
N1 N2 N3 103.9(6) . .
N2 N3 C1 114.6(6) . .
N2 N3 C10 115.1(7) . .
C1 N3 C10 130.3(6) . .
C1 Pd1 C1 180.000(1) 2_677 .
C1 Pd1 I1 88.49(18) 2_677 .
C1 Pd1 I1 91.51(18) . .
C1 Pd1 I1 91.51(18) 2_677 2_677
C1 Pd1 I1 88.49(18) . 2_677
I1 Pd1 I1 180.0 . 2_677
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N3 1.385(9) .
C1 C2 1.389(9) .
C1 Pd1 2.026(6) .
C2 N1 1.406(9) .
C2 C3 1.446(10) .
C3 C4 1.383(12) .
C3 C8 1.383(10) .
C4 C5 1.385(14) .
C4 H4 0.9300 .
C5 C6 1.363(15) .
C5 H5 0.9300 .
C6 C7 1.310(15) .
C6 H6 0.9300 .
C7 C8 1.399(13) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 N1 1.461(11) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C15 1.332(12) .
C10 C11 1.358(14) .
C10 N3 1.430(10) .
C11 C12 1.401(16) .
C11 H11 0.9300 .
C12 C13 1.361(19) .
C12 H12 0.9300 .
C13 C14 1.308(17) .
C13 H13 0.9300 .
C14 C15 1.385(14) .
C14 H14 0.9300 .
C15 H15 0.9300 .
I1 Pd1 2.6174(5) .
N1 N2 1.284(10) .
N2 N3 1.325(8) .
Pd1 C1 2.026(6) 2_677
Pd1 I1 2.6174(5) 2_677
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_4
N3 C1 C2 N1 0.1(7) .
Pd1 C1 C2 N1 -176.6(5) .
N3 C1 C2 C3 179.9(7) .
Pd1 C1 C2 C3 3.2(11) .
C1 C2 C3 C4 32.4(12) .
N1 C2 C3 C4 -147.8(8) .
C1 C2 C3 C8 -148.1(8) .
N1 C2 C3 C8 31.6(11) .
C8 C3 C4 C5 0.4(15) .
C2 C3 C4 C5 179.9(9) .
C3 C4 C5 C6 -0.7(18) .
C4 C5 C6 C7 1.3(19) .
C5 C6 C7 C8 -1.4(18) .
C4 C3 C8 C7 -0.5(13) .
C2 C3 C8 C7 -180.0(8) .
C6 C7 C8 C3 1.0(16) .
C15 C10 C11 C12 -1(2) .
N3 C10 C11 C12 174.6(13) .
C10 C11 C12 C13 2(3) .
C11 C12 C13 C14 -3(3) .
C12 C13 C14 C15 3(3) .
C11 C10 C15 C14 0.7(18) .
N3 C10 C15 C14 -174.8(10) .
C13 C14 C15 C10 -1(2) .
C1 C2 N1 N2 -0.6(8) .
C3 C2 N1 N2 179.6(7) .
C1 C2 N1 C9 -180.0(10) .
C3 C2 N1 C9 0.2(14) .
C2 N1 N2 N3 0.9(9) .
C9 N1 N2 N3 -179.7(8) .
N1 N2 N3 C1 -0.8(9) .
N1 N2 N3 C10 179.4(6) .
C2 C1 N3 N2 0.5(8) .
Pd1 C1 N3 N2 177.4(5) .
C2 C1 N3 C10 -179.8(7) .
Pd1 C1 N3 C10 -2.9(10) .
C15 C10 N3 N2 112.4(10) .
C11 C10 N3 N2 -63.1(12) .
C15 C10 N3 C1 -67.3(12) .
C11 C10 N3 C1 117.2(11) .
N3 C1 Pd1 C1 -119(84) 2_677
C2 C1 Pd1 C1 57(84) 2_677
N3 C1 Pd1 I1 91.1(5) .
C2 C1 Pd1 I1 -92.9(6) .
N3 C1 Pd1 I1 -88.9(5) 2_677
C2 C1 Pd1 I1 87.1(6) 2_677
