#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:34:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179851 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/47/7014777.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_7014777
loop_
_publ_author_name
'Cross, Warren B.'
'Daly, Christopher G.'
'Ackerman, Rachel L.'
'George, Ian R.'
'Singh, Kuldip'
_publ_section_title
;
 N-heterocyclic carbene tethered amido complexes of palladium and
 platinum.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              495
_journal_page_last               505
_journal_paper_doi               10.1039/c0dt01149e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C24 H26 I N5 Pd,2(C6 H6)'
_chemical_formula_sum            'C36 H38 I N5 Pd'
_chemical_formula_weight         774.01
_chemical_name_common            '[CNC-i-Pr]PdI (7a)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8012(19)
_cell_length_b                   19.746(4)
_cell_length_c                   15.230(3)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.537
_cell_measurement_theta_min      3.379
_cell_volume                     3248.3(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex 2000 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13040
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 10643 reflections(SADABS);Rint 0.0932 before
correction and 0.0291 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0260
_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)+(0.0362P)²+2.6372P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                3149
_reflns_number_total             3336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01149E.TXT
_cod_data_source_block           09075n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        3248.2(10)
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7014777
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 0.0000 0.664516(12) 0.7500 0.01718(8) Uani 1 2 d S . .
I1 I 0.0000 0.795617(11) 0.7500 0.03443(9) Uani 1 2 d S . .
N1 N 0.0000 0.56204(14) 0.7500 0.0194(6) Uani 1 2 d S . .
N2 N 0.1165(2) 0.60700(13) 0.90727(17) 0.0219(5) Uani 1 1 d . . .
N3 N -0.0034(4) 0.68626(12) 0.95424(15) 0.0247(4) Uani 1 1 d . . .
C1 C 0.1008(3) 0.52836(15) 0.7837(2) 0.0242(7) Uani 1 1 d . . .
C2 C 0.1682(3) 0.55467(16) 0.8555(2) 0.0227(6) Uani 1 1 d . . .
C3 C 0.2827(3) 0.52693(18) 0.8782(2) 0.0297(7) Uani 1 1 d . . .
H3 H 0.3308 0.5477 0.9229 0.036 Uiso 1 1 calc R . .
C4 C 0.3273(3) 0.46995(18) 0.8367(3) 0.0342(8) Uani 1 1 d . . .
H4 H 0.4048 0.4510 0.8531 0.041 Uiso 1 1 calc R . .
C5 C 0.2569(3) 0.44072(18) 0.7707(2) 0.0369(10) Uani 1 1 d . . .
H5 H 0.2859 0.4007 0.7428 0.044 Uiso 1 1 calc R . .
C6 C 0.1468(3) 0.46822(14) 0.7450(4) 0.0312(7) Uani 1 1 d . . .
H6 H 0.1001 0.4466 0.7002 0.037 Uiso 1 1 calc R . .
C7 C 0.0371(3) 0.65612(15) 0.8798(2) 0.0208(6) Uani 1 1 d . . .
C8 C 0.1261(3) 0.60808(18) 0.9985(2) 0.0271(7) Uani 1 1 d . . .
H8 H 0.1758 0.5790 1.0335 0.033 Uiso 1 1 calc R . .
C9 C 0.0530(3) 0.6574(2) 1.0276(2) 0.0327(8) Uani 1 1 d . . .
H9 H 0.0414 0.6706 1.0870 0.039 Uiso 1 1 calc R . .
C10 C -0.0991(3) 0.73945(17) 0.9613(2) 0.0275(7) Uani 1 1 d . . .
H10 H -0.1319 0.7491 0.9012 0.033 Uiso 1 1 calc R . .
C11 C -0.2046(4) 0.7140(2) 1.0177(3) 0.0421(10) Uani 1 1 d . . .
H11A H -0.2500 0.6787 0.9859 0.063 Uiso 1 1 calc R . .
H11B H -0.2607 0.7516 1.0312 0.063 Uiso 1 1 calc R . .
H11C H -0.1715 0.6953 1.0724 0.063 Uiso 1 1 calc R . .
C12 C -0.0437(4) 0.8040(2) 0.9980(3) 0.0409(10) Uani 1 1 d . . .
H12A H -0.0080 0.7949 1.0560 0.061 Uiso 1 1 calc R . .
H12B H -0.1085 0.8385 1.0034 0.061 Uiso 1 1 calc R . .
H12C H 0.0212 0.8204 0.9584 0.061 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'
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
N1 Pd1 C7 85.30(9) . . ?
N1 Pd1 C7 85.30(9) . 3_556 ?
C7 Pd1 C7 170.61(17) . 3_556 ?
N1 Pd1 I1 180.0 . . ?
C7 Pd1 I1 94.70(9) . . ?
C7 Pd1 I1 94.70(9) 3_556 . ?
C1 N1 C1 122.2(3) 3_556 . ?
C1 N1 Pd1 118.92(16) 3_556 . ?
C1 N1 Pd1 118.92(16) . . ?
C7 N2 C8 110.0(3) . . ?
C7 N2 C2 126.7(3) . . ?
C8 N2 C2 122.5(3) . . ?
C7 N3 C9 110.5(3) . . ?
C7 N3 C10 126.9(3) . . ?
C9 N3 C10 122.5(3) . . ?
N1 C1 C2 121.3(3) . . ?
N1 C1 C6 121.9(3) . . ?
C2 C1 C6 116.7(3) . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 N2 119.9(3) . . ?
C1 C2 N2 119.8(3) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
N3 C7 N2 105.0(3) . . ?
N3 C7 Pd1 135.9(2) . . ?
N2 C7 Pd1 118.9(2) . . ?
C9 C8 N2 107.3(3) . . ?
C9 C8 H8 126.3 . . ?
N2 C8 H8 126.3 . . ?
C8 C9 N3 107.0(3) . . ?
C8 C9 H9 126.5 . . ?
N3 C9 H9 126.5 . . ?
N3 C10 C11 109.4(3) . . ?
N3 C10 C12 110.4(3) . . ?
C11 C10 C12 111.5(3) . . ?
N3 C10 H10 108.5 . . ?
C11 C10 H10 108.5 . . ?
C12 C10 H10 108.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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
Pd1 N1 2.024(3) . ?
Pd1 C7 2.024(3) . ?
Pd1 C7 2.024(3) 3_556 ?
Pd1 I1 2.5887(6) . ?
N1 C1 1.375(3) 3_556 ?
N1 C1 1.375(3) . ?
N2 C7 1.361(4) . ?
N2 C8 1.394(4) . ?
N2 C2 1.414(4) . ?
N3 C7 1.353(4) . ?
N3 C9 1.393(5) . ?
N3 C10 1.478(4) . ?
C1 C2 1.413(4) . ?
C1 C6 1.416(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.377(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.330(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.513(5) . ?
C10 C12 1.516(5) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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
C7 Pd1 N1 C1 126.68(17) . . . 3_556 ?
C7 Pd1 N1 C1 -53.32(17) 3_556 . . 3_556 ?
C7 Pd1 N1 C1 -53.32(17) . . . . ?
C7 Pd1 N1 C1 126.68(17) 3_556 . . . ?
C1 N1 C1 C2 -145.8(3) 3_556 . . . ?
Pd1 N1 C1 C2 34.2(3) . . . . ?
C1 N1 C1 C6 38.3(2) 3_556 . . . ?
Pd1 N1 C1 C6 -141.7(2) . . . . ?
N1 C1 C2 C3 -167.9(3) . . . . ?
C6 C1 C2 C3 8.3(4) . . . . ?
N1 C1 C2 N2 15.3(4) . . . . ?
C6 C1 C2 N2 -168.6(3) . . . . ?
C7 N2 C2 C3 152.4(3) . . . . ?
C8 N2 C2 C3 -38.2(4) . . . . ?
C7 N2 C2 C1 -30.7(4) . . . . ?
C8 N2 C2 C1 138.6(3) . . . . ?
C1 C2 C3 C4 -6.0(5) . . . . ?
N2 C2 C3 C4 170.8(3) . . . . ?
C2 C3 C4 C5 0.9(5) . . . . ?
C3 C4 C5 C6 1.6(5) . . . . ?
C4 C5 C6 C1 1.0(6) . . . . ?
N1 C1 C6 C5 170.2(3) . . . . ?
C2 C1 C6 C5 -5.9(5) . . . . ?
C9 N3 C7 N2 1.7(4) . . . . ?
C10 N3 C7 N2 -174.8(3) . . . . ?
C9 N3 C7 Pd1 177.6(3) . . . . ?
C10 N3 C7 Pd1 1.1(5) . . . . ?
C8 N2 C7 N3 -1.1(3) . . . . ?
C2 N2 C7 N3 169.3(3) . . . . ?
C8 N2 C7 Pd1 -177.9(2) . . . . ?
C2 N2 C7 Pd1 -7.4(4) . . . . ?
N1 Pd1 C7 N3 -136.0(3) . . . . ?
I1 Pd1 C7 N3 44.0(3) . . . . ?
N1 Pd1 C7 N2 39.5(2) . . . . ?
I1 Pd1 C7 N2 -140.5(2) . . . . ?
C7 N2 C8 C9 0.1(4) . . . . ?
C2 N2 C8 C9 -170.8(3) . . . . ?
N2 C8 C9 N3 0.9(4) . . . . ?
C7 N3 C9 C8 -1.6(4) . . . . ?
C10 N3 C9 C8 175.0(3) . . . . ?
C7 N3 C10 C11 119.7(4) . . . . ?
C9 N3 C10 C11 -56.4(4) . . . . ?
C7 N3 C10 C12 -117.2(4) . . . . ?
C9 N3 C10 C12 66.7(4) . . . . ?
