#------------------------------------------------------------------------------
#$Date: 2018-09-27 07:13:35 +0300 (Thu, 27 Sep 2018) $
#$Revision: 211196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/27/4332761.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332761
loop_
_publ_author_name
'Wang, Ruihu'
'Jin, Chuan-Ming'
'Twamley, Brendan'
'Shreeve, Jean'ne M.'
_publ_section_title
;
 Syntheses and Characterization of Unsymmetric Dicationic Salts
 Incorporating Imidazolium and Triazolium Functionalities
;
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6396
_journal_page_last               6403
_journal_paper_doi               10.1021/ic060822i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C28 H46 I4 N10 Pd2'
_chemical_formula_sum            'C28 H46 I4 N10 Pd2'
_chemical_formula_weight         1243.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.813(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8006(5)
_cell_length_b                   15.2620(9)
_cell_length_c                   15.8084(10)
_cell_measurement_reflns_used    6088
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.58
_cell_volume                     1875.4(2)
_computing_cell_refinement       'Bruker SAINT+ v. 6.45a'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.45a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      87(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28147
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.286
_exptl_absorpt_correction_T_max  0.8473
_exptl_absorpt_correction_T_min  0.3501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2004'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3403
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0444
_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)+(0.0397P)²+23.1888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                3115
_reflns_number_total             3403
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic060822isup1.cif
_cod_data_source_block           bt768
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.99750(6) 0.35668(3) 0.47562(3) 0.00837(14) Uani 1 1 d .
I1 I 1.26062(6) 0.37694(3) 0.38558(3) 0.01373(14) Uani 1 1 d .
I2 I 0.72520(6) 0.32839(3) 0.55707(3) 0.01371(14) Uani 1 1 d .
C1 C 1.4018(13) 0.0920(6) 0.4481(6) 0.035(2) Uani 1 1 d .
H1A H 1.3445 0.0352 0.4389 0.053 Uiso 1 1 calc R
H1B H 1.5267 0.0838 0.4501 0.053 Uiso 1 1 calc R
H1C H 1.3647 0.1318 0.4015 0.053 Uiso 1 1 calc R
C2 C 1.3550(10) 0.1305(5) 0.5311(5) 0.0199(17) Uani 1 1 d .
H2A H 1.4114 0.1883 0.5395 0.024 Uiso 1 1 calc R
H2B H 1.3996 0.0919 0.5783 0.024 Uiso 1 1 calc R
C3 C 1.1622(10) 0.1417(5) 0.5347(5) 0.0169(16) Uani 1 1 d .
H3A H 1.1180 0.1792 0.4867 0.020 Uiso 1 1 calc R
H3B H 1.1068 0.0836 0.5269 0.020 Uiso 1 1 calc R
C4 C 1.1087(9) 0.1817(5) 0.6164(5) 0.0163(16) Uani 1 1 d .
H4A H 0.9818 0.1866 0.6131 0.020 Uiso 1 1 calc R
H4B H 1.1451 0.1426 0.6646 0.020 Uiso 1 1 calc R
N5 N 1.1853(7) 0.2690(4) 0.6322(4) 0.0103(12) Uani 1 1 d .
C6 C 1.3070(9) 0.2871(5) 0.6988(5) 0.0130(15) Uani 1 1 d .
H6 H 1.3465 0.2463 0.7415 0.016 Uiso 1 1 calc R
N7 N 1.3598(8) 0.3681(4) 0.6946(4) 0.0170(14) Uani 1 1 d .
N8 N 1.2636(7) 0.4007(4) 0.6229(4) 0.0085(12) Uani 1 1 d .
C9 C 1.1578(9) 0.3413(5) 0.5834(5) 0.0111(14) Uani 1 1 d U
C10 C 0.9883(11) 0.0402(5) 0.3065(7) 0.033(2) Uani 1 1 d .
H10A H 1.0525 0.0761 0.2687 0.049 Uiso 1 1 calc R
H10B H 0.9907 -0.0212 0.2884 0.049 Uiso 1 1 calc R
H10C H 1.0411 0.0453 0.3648 0.049 Uiso 1 1 calc R
C11 C 0.8075(12) 0.0710(5) 0.3030(7) 0.033(2) Uani 1 1 d .
H11A H 0.7431 0.0299 0.3371 0.040 Uiso 1 1 calc R
H11B H 0.7582 0.0659 0.2435 0.040 Uiso 1 1 calc R
C12 C 0.7724(10) 0.1622(5) 0.3327(5) 0.0177(16) Uani 1 1 d .
H12A H 0.7904 0.1640 0.3954 0.021 Uiso 1 1 calc R
H12B H 0.6503 0.1767 0.3165 0.021 Uiso 1 1 calc R
C13 C 0.8863(9) 0.2315(4) 0.2959(5) 0.0121(15) Uani 1 1 d .
H13A H 1.0018 0.2302 0.3271 0.015 Uiso 1 1 calc R
H13B H 0.8998 0.2177 0.2356 0.015 Uiso 1 1 calc R
N14 N 0.8123(7) 0.3199(4) 0.3019(4) 0.0116(12) Uani 1 1 d .
C15 C 0.6912(9) 0.3545(5) 0.2422(5) 0.0131(15) Uani 1 1 d .
H15 H 0.6514 0.3284 0.1897 0.016 Uiso 1 1 calc R
C16 C 0.6408(9) 0.4308(4) 0.2718(4) 0.0100(14) Uani 1 1 d .
H16 H 0.5581 0.4696 0.2447 0.012 Uiso 1 1 calc R
N17 N 0.7320(7) 0.4428(4) 0.3494(4) 0.0101(12) Uani 1 1 d .
C18 C 0.8393(9) 0.3742(4) 0.3697(4) 0.0098(14) Uani 1 1 d U
C19 C 0.6966(9) 0.5123(4) 0.4082(4) 0.0101(14) Uani 1 1 d .
H19A H 0.7651 0.5020 0.4629 0.012 Uiso 1 1 calc R
H19B H 0.5734 0.5102 0.4190 0.012 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
C18 Pd1 C9 179.0(3) . .
C18 Pd1 I2 87.99(19) . .
C9 Pd1 I2 92.06(19) . .
C18 Pd1 I1 89.18(19) . .
C9 Pd1 I1 90.82(19) . .
I2 Pd1 I1 175.78(3) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C1 C2 C3 112.9(7) . .
C1 C2 H2A 109.0 . .
C3 C2 H2A 109.0 . .
C1 C2 H2B 109.0 . .
C3 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C4 C3 C2 114.9(7) . .
C4 C3 H3A 108.5 . .
C2 C3 H3A 108.5 . .
C4 C3 H3B 108.5 . .
C2 C3 H3B 108.5 . .
H3A C3 H3B 107.5 . .
N5 C4 C3 111.8(6) . .
N5 C4 H4A 109.3 . .
C3 C4 H4A 109.3 . .
N5 C4 H4B 109.3 . .
C3 C4 H4B 109.3 . .
H4A C4 H4B 107.9 . .
C9 N5 C6 109.7(6) . .
C9 N5 C4 126.8(6) . .
C6 N5 C4 123.4(6) . .
N7 C6 N5 110.4(6) . .
N7 C6 H6 124.8 . .
N5 C6 H6 124.8 . .
C6 N7 N8 103.2(6) . .
C9 N8 N7 113.8(6) . .
C9 N8 C19 126.7(6) . 3_766
N7 N8 C19 118.8(6) . 3_766
N8 C9 N5 102.9(6) . .
N8 C9 Pd1 128.3(5) . .
N5 C9 Pd1 128.8(5) . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C10 C11 C12 118.7(8) . .
C10 C11 H11A 107.6 . .
C12 C11 H11A 107.6 . .
C10 C11 H11B 107.6 . .
C12 C11 H11B 107.6 . .
H11A C11 H11B 107.1 . .
C11 C12 C13 113.3(6) . .
C11 C12 H12A 108.9 . .
C13 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
C13 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
N14 C13 C12 111.5(6) . .
N14 C13 H13A 109.3 . .
C12 C13 H13A 109.3 . .
N14 C13 H13B 109.3 . .
C12 C13 H13B 109.3 . .
H13A C13 H13B 108.0 . .
C18 N14 C15 111.0(6) . .
C18 N14 C13 125.1(6) . .
C15 N14 C13 123.6(6) . .
C16 C15 N14 107.5(6) . .
C16 C15 H15 126.3 . .
N14 C15 H15 126.3 . .
C15 C16 N17 106.5(6) . .
C15 C16 H16 126.8 . .
N17 C16 H16 126.8 . .
C18 N17 C16 111.7(6) . .
C18 N17 C19 123.8(6) . .
C16 N17 C19 123.7(6) . .
N14 C18 N17 103.4(6) . .
N14 C18 Pd1 128.3(5) . .
N17 C18 Pd1 128.3(5) . .
N17 C19 N8 113.0(5) . 3_766
N17 C19 H19A 109.0 . .
N8 C19 H19A 109.0 3_766 .
N17 C19 H19B 109.0 . .
N8 C19 H19B 109.0 3_766 .
H19A C19 H19B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C18 2.013(7) .
Pd1 C9 2.041(7) .
Pd1 I2 2.6105(7) .
Pd1 I1 2.6124(7) .
C1 C2 1.511(12) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.519(11) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.518(11) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 N5 1.473(9) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N5 C9 1.352(9) .
N5 C6 1.385(9) .
C6 N7 1.307(10) .
C6 H6 0.9500 .
N7 N8 1.396(8) .
N8 C9 1.344(9) .
N8 C19 1.459(9) 3_766
C10 C11 1.483(12) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.501(11) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.528(10) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N14 1.474(9) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
N14 C18 1.356(9) .
N14 C15 1.383(9) .
C15 C16 1.326(10) .
C15 H15 0.9500 .
C16 N17 1.378(9) .
C16 H16 0.9500 .
N17 C18 1.362(9) .
N17 C19 1.454(9) .
C19 N8 1.459(9) 3_766
C19 H19A 0.9900 .
C19 H19B 0.9900 .
