#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179471 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/68/4336838.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_4336838
loop_
_publ_author_name
'Michael G. Campbell'
'Shao-Liang Zheng'
'Tobias Ritter'
_publ_section_title
;
 One-Dimensional Palladium Wires: Influence of Molecular Changes on
 Supramolecular Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13295
_journal_page_last               13297
_journal_paper_doi               10.1021/ic4019635
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C101 H88 Cl22 F16 N6 O12 P2 Pd6'
_chemical_formula_weight         3362.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   25.4572(6)
_cell_length_b                   25.4572(6)
_cell_length_c                   16.5136(4)
_cell_measurement_reflns_used    19384
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      19.49
_cell_measurement_theta_min      2.22
_cell_volume                     9268.2(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85555
_diffrn_reflns_theta_full        29.59
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.9315
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       needle
_exptl_crystal_F_000             4968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5797
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0349
_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)+(0.0402P)²+32.4348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                5390
_reflns_number_total             5797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019635_si_002.cif
_cod_data_source_block           zsl
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4336838
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
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 0.326415(10) 0.316732(9) 0.585100(13) 0.01307(6) Uani 1 1 d . . .
O1 O 0.38737(12) 0.40993(11) 0.59229(14) 0.0219(5) Uani 1 1 d . . .
O2 O 0.41214(11) 0.40890(11) 0.72221(15) 0.0208(5) Uani 1 1 d . . .
N1 N 0.39206(13) 0.29739(14) 0.55641(16) 0.0189(6) Uani 1 1 d . . .
C1 C 0.45068(16) 0.33574(17) 0.5396(2) 0.0204(7) Uani 1 1 d . . .
H1 H 0.4656 0.3782 0.5401 0.024 Uiso 1 1 calc R . .
C2 C 0.48990(17) 0.31416(18) 0.5214(2) 0.0237(7) Uani 1 1 d . . .
H2 H 0.5313 0.3420 0.5096 0.028 Uiso 1 1 calc R . .
C3 C 0.46896(17) 0.25213(19) 0.5204(2) 0.0258(8) Uani 1 1 d . . .
H3 H 0.4960 0.2376 0.5085 0.031 Uiso 1 1 calc R . .
C4 C 0.40789(17) 0.21140(17) 0.5369(2) 0.0218(7) Uani 1 1 d . . .
C5 C 0.3800(2) 0.14628(19) 0.5368(3) 0.0300(9) Uani 1 1 d . . .
H5 H 0.4043 0.1283 0.5269 0.036 Uiso 1 1 calc R . .
C6 C 0.3197(2) 0.10995(18) 0.5506(2) 0.0296(8) Uani 1 1 d . . .
H6 H 0.3028 0.0672 0.5490 0.035 Uiso 1 1 calc R . .
C7 C 0.28088(18) 0.13434(17) 0.5676(2) 0.0244(7) Uani 1 1 d . . .
C8 C 0.21804(19) 0.10022(15) 0.5811(2) 0.0300(8) Uani 1 1 d . . .
H8 H 0.1983 0.0572 0.5815 0.036 Uiso 1 1 calc R . .
C9 C 0.18483(17) 0.12877(18) 0.5940(2) 0.0268(8) Uani 1 1 d . . .
H9 H 0.1423 0.1052 0.6026 0.032 Uiso 1 1 calc R . .
C10 C 0.21346(17) 0.19284(18) 0.5944(2) 0.0229(7) Uani 1 1 d . . .
H10 H 0.1902 0.2120 0.6038 0.028 Uiso 1 1 calc R . .
C11 C 0.27395(14) 0.22684(14) 0.58152(18) 0.0141(6) Uani 1 1 d . . .
C12 C 0.30743(16) 0.19811(16) 0.5686(2) 0.0173(6) Uani 1 1 d . . .
C13 C 0.37069(15) 0.23590(16) 0.55410(19) 0.0174(7) Uani 1 1 d . . .
C14 C 0.41770(15) 0.43491(15) 0.6550(2) 0.0180(6) Uani 1 1 d . . .
C15 C 0.4651(2) 0.50092(18) 0.6496(3) 0.0342(9) Uani 1 1 d . . .
H15A H 0.4459 0.5246 0.6344 0.051 Uiso 1 1 calc R . .
H15B H 0.4953 0.5064 0.6086 0.051 Uiso 1 1 calc R . .
H15C H 0.4851 0.5149 0.7022 0.051 Uiso 1 1 calc R . .
P1 P 0.6667 0.3333 0.57123(11) 0.0243(3) Uani 1 3 d S . .
F1 F 0.70854(11) 0.39069(11) 0.62728(16) 0.0357(6) Uani 1 1 d . . .
F2 F 0.65109(13) 0.37521(13) 0.51519(16) 0.0439(7) Uani 1 1 d . . .
C21 C 0.4520(3) 0.6178(3) 0.3712(3) 0.0464(12) Uani 1 1 d D . .
H21A H 0.4673 0.6619 0.3675 0.056 Uiso 1 1 calc R . .
H21B H 0.4071 0.5968 0.3731 0.056 Uiso 1 1 calc R . .
Cl1 Cl 0.47887(6) 0.60247(5) 0.46050(7) 0.0486(3) Uani 1 1 d D . .
Cl2 Cl 0.47452(7) 0.59416(5) 0.28474(7) 0.0490(3) Uani 1 1 d . . .
C22 C 0.6667 0.4360(5) 0.3333 0.084(3) Uani 1 2 d S . .
H22A H 0.6895 0.4336 0.3803 0.101 Uiso 0.50 1 d PR . .
H22B H 0.6851 0.4314 0.2830 0.101 Uiso 0.50 1 d PR . .
Cl3 Cl 0.57970(15) 0.37311(13) 0.34027(15) 0.0530(7) Uani 0.50 1 d P . .
Cl4 Cl 0.6667 0.50342(12) 0.3333 0.0724(6) Uani 1 2 d S . .
C23 C 0.6667 0.3333 0.8333 0.048(3) Uani 1 6 d S . .
H23 H 0.6442 0.3109 0.7866 0.058 Uiso 0.33 1 d PR . .
Cl5 Cl 0.6667 0.39724(11) 0.8333 0.0746(12) Uani 0.67 2 d SP . .
C24 C 0.3872(14) 0.0180(16) 0.2891(10) 0.066(3) Uani 0.17 1 d PDU A -1
H24A H 0.3651 -0.0233 0.2708 0.080 Uiso 0.17 1 d PR A -1
H24B H 0.4288 0.0339 0.2739 0.080 Uiso 0.17 1 d PR A -1
Cl7 Cl 0.3712(5) 0.0058(6) 0.3904(7) 0.066(3) Uani 0.17 1 d PD A -1
Cl6 Cl 0.3478(9) 0.0456(11) 0.2360(9) 0.066(3) Uani 0.17 1 d PD A -1
F3 F 0.3268(3) 0.0339(3) 0.3207(5) 0.0251(12) Uani 0.378(5) 1 d PU B -2
F4 F 0.3702(7) -0.0097(8) 0.5501(7) 0.0251(12) Uani 0.288(5) 1 d P B -3
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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
C11 Pd1 N1 82.77(13) . .
C11 Pd1 O2 93.15(12) . 11_556
N1 Pd1 O2 175.65(11) . 11_556
C11 Pd1 O1 175.18(12) . .
N1 Pd1 O1 93.14(11) . .
O2 Pd1 O1 91.00(10) 11_556 .
C11 Pd1 Pd1 95.45(8) . 11_556
N1 Pd1 Pd1 98.77(8) . 11_556
O2 Pd1 Pd1 83.08(7) 11_556 11_556
O1 Pd1 Pd1 82.60(6) . 11_556
C11 Pd1 Pd1 91.88(8) . 6_556
N1 Pd1 Pd1 84.69(8) . 6_556
O2 Pd1 Pd1 93.96(7) 11_556 6_556
O1 Pd1 Pd1 90.29(6) . 6_556
Pd1 Pd1 Pd1 172.233(5) 11_556 6_556
C14 O1 Pd1 122.7(2) . .
C14 O2 Pd1 122.8(2) . 11_556
C1 N1 C13 119.0(3) . .
C1 N1 Pd1 128.7(2) . .
C13 N1 Pd1 112.3(2) . .
N1 C1 C2 120.9(3) . .
N1 C1 H1 119.5 . .
C2 C1 H1 119.5 . .
C3 C2 C1 120.5(3) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C2 C3 C4 119.5(3) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C3 C4 C13 117.3(3) . .
C3 C4 C5 125.4(3) . .
C13 C4 C5 117.3(3) . .
C6 C5 C4 121.6(4) . .
C6 C5 H5 119.2 . .
C4 C5 H5 119.2 . .
C5 C6 C7 121.8(4) . .
C5 C6 H6 119.1 . .
C7 C6 H6 119.1 . .
C8 C7 C12 116.8(3) . .
C8 C7 C6 125.6(4) . .
C12 C7 C6 117.6(3) . .
C9 C8 C7 120.5(3) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 120.7(3) . .
C8 C9 H9 119.7 . .
C10 C9 H9 119.7 . .
C11 C10 C9 120.1(4) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C10 C11 C12 119.2(3) . .
C10 C11 Pd1 128.7(3) . .
C12 C11 Pd1 112.0(2) . .
C11 C12 C7 122.7(3) . .
C11 C12 C13 117.0(3) . .
C7 C12 C13 120.3(3) . .
N1 C13 C4 122.8(3) . .
N1 C13 C12 115.7(3) . .
C4 C13 C12 121.5(3) . .
O1 C14 O2 125.4(3) . .
O1 C14 C15 117.6(3) . .
O2 C14 C15 117.1(3) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
F1 P1 F1 89.98(16) 3_665 2_655
F1 P1 F1 89.98(16) 3_665 .
F1 P1 F1 89.98(16) 2_655 .
F1 P1 F2 90.02(15) 3_665 3_665
F1 P1 F2 179.9(2) 2_655 3_665
F1 P1 F2 89.95(14) . 3_665
F1 P1 F2 89.95(14) 3_665 2_655
F1 P1 F2 90.03(15) 2_655 2_655
F1 P1 F2 179.9(2) . 2_655
F2 P1 F2 90.05(17) 3_665 2_655
F1 P1 F2 179.93(18) 3_665 .
F1 P1 F2 89.95(14) 2_655 .
F1 P1 F2 90.03(15) . .
F2 P1 F2 90.05(17) 3_665 .
F2 P1 F2 90.04(17) 2_655 .
Cl1 C21 Cl2 112.2(3) . .
Cl1 C21 H21A 109.2 . .
Cl2 C21 H21A 109.2 . .
Cl1 C21 H21B 109.2 . .
Cl2 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
Cl4 C22 Cl3 104.4(4) . .
Cl4 C22 Cl3 104.4(4) . 17_655
Cl3 C22 Cl3 151.1(7) . 17_655
Cl4 C22 H22A 110.8 . .
Cl3 C22 H22A 111.0 . .
Cl3 C22 H22A 57.6 17_655 .
Cl4 C22 H22B 110.8 . .
Cl3 C22 H22B 110.9 . .
Cl3 C22 H22B 57.7 17_655 .
H22A C22 H22B 108.9 . .
Cl3 Cl3 C22 133.3(3) 16 .
Cl5 C23 Cl5 120.0 3_665 2_655
Cl5 C23 Cl5 120.001(1) 3_665 .
Cl5 C23 Cl5 120.0 2_655 .
Cl5 C23 H23 107.3 3_665 .
Cl5 C23 H23 53.4 2_655 .
Cl5 C23 H23 107.3 . .
Cl7 C24 Cl6 115.9(11) . .
Cl7 C24 H24A 98.9 . .
Cl6 C24 H24A 98.3 . .
Cl7 C24 H24B 116.4 . .
Cl6 C24 H24B 116.0 . .
H24A C24 H24B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C11 1.992(3) .
Pd1 N1 2.020(3) .
Pd1 O2 2.067(2) 11_556
Pd1 O1 2.090(2) .
Pd1 Pd1 2.7112(4) 11_556
Pd1 Pd1 2.8428(4) 6_556
O1 C14 1.258(4) .
O2 C14 1.263(4) .
O2 Pd1 2.067(2) 11_556
N1 C1 1.342(5) .
N1 C13 1.377(4) .
C1 C2 1.392(5) .
C1 H1 0.9500 .
C2 C3 1.391(6) .
C2 H2 0.9500 .
C3 C4 1.398(5) .
C3 H3 0.9500 .
C4 C13 1.399(5) .
C4 C5 1.441(6) .
C5 C6 1.356(6) .
C5 H5 0.9500 .
C6 C7 1.434(6) .
C6 H6 0.9500 .
C7 C8 1.405(6) .
C7 C12 1.412(5) .
C8 C9 1.379(6) .
C8 H8 0.9500 .
C9 C10 1.415(6) .
C9 H9 0.9500 .
C10 C11 1.354(5) .
C10 H10 0.9500 .
C11 C12 1.389(5) .
C12 C13 1.424(5) .
C14 C15 1.504(5) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
P1 F1 1.603(3) 3_665
P1 F1 1.603(3) 2_655
P1 F1 1.603(3) .
P1 F2 1.604(3) 3_665
P1 F2 1.604(3) 2_655
P1 F2 1.604(3) .
C21 Cl1 1.750(5) .
C21 Cl2 1.754(5) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 Cl4 1.716(12) .
C22 Cl3 1.983(4) .
C22 Cl3 1.983(4) 17_655
C22 H22A 0.9900 .
C22 H22B 0.9900 .
Cl3 Cl3 1.769(5) 16
C23 Cl5 1.627(3) 3_665
C23 Cl5 1.627(3) 2_655
C23 Cl5 1.627(3) .
C23 H23 0.9601 .
C24 Cl7 1.713(10) .
C24 Cl6 1.724(10) .
C24 H24A 0.9598 .
C24 H24B 0.9600 .
