#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179471 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/68/4336839.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_4336839
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            'C30.58 H21.17 Cl3.17 F N2 O4 Pd2'
_chemical_formula_weight         824.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   23.8680(15)
_cell_length_b                   23.8680(15)
_cell_length_c                   11.2498(7)
_cell_measurement_reflns_used    18842
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.49
_cell_volume                     5550.2(6)
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            69099
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  0.8862
_exptl_absorpt_correction_T_min  0.7077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       needle
_exptl_crystal_F_000             2433
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0532
_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)+(0.1032P)²+28.9902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                2563
_reflns_number_total             3280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019635_si_003.cif
_cod_data_source_block           zsl
_cod_database_code               4336839
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6105(4) 0.4708(4) 0.3894(5) 0.0484(17) Uani 1 1 d . . .
H1 H 0.5800 0.4258 0.3862 0.058 Uiso 1 1 calc R . .
C2 C 0.6760(4) 0.4907(4) 0.3954(5) 0.057(2) Uani 1 1 d . . .
H2 H 0.6895 0.4595 0.3964 0.068 Uiso 1 1 calc R . .
C3 C 0.7209(4) 0.5550(4) 0.4000(6) 0.0556(19) Uani 1 1 d . . .
H3 H 0.7657 0.5686 0.4034 0.067 Uiso 1 1 calc R . .
C4 C 0.7003(4) 0.6013(4) 0.3996(5) 0.0477(17) Uani 1 1 d . . .
C5 C 0.7411(4) 0.6699(4) 0.4034(6) 0.0561(19) Uani 1 1 d . . .
H5 H 0.7867 0.6876 0.4053 0.067 Uiso 1 1 calc R . .
C6 C 0.7172(4) 0.7101(4) 0.4045(6) 0.0548(18) Uani 1 1 d . . .
H6 H 0.7460 0.7555 0.4060 0.066 Uiso 1 1 calc R . .
C7 C 0.6490(3) 0.6858(3) 0.4035(5) 0.0446(15) Uani 1 1 d . . .
C8 C 0.6183(4) 0.7234(4) 0.4047(6) 0.0519(18) Uani 1 1 d . . .
C9 C 0.5522(4) 0.6952(4) 0.4026(5) 0.0520(18) Uani 1 1 d . . .
H9 H 0.5333 0.7220 0.4050 0.062 Uiso 1 1 calc R . .
C10 C 0.5117(3) 0.6281(3) 0.3969(5) 0.0432(15) Uani 1 1 d . . .
H10 H 0.4661 0.6097 0.3956 0.052 Uiso 1 1 calc R . .
C11 C 0.5388(3) 0.5893(3) 0.3931(5) 0.0400(14) Uani 1 1 d . A .
C12 C 0.6071(3) 0.6192(3) 0.3982(5) 0.0389(14) Uani 1 1 d . . .
C13 C 0.6333(3) 0.5767(3) 0.3951(5) 0.0411(15) Uani 1 1 d . . .
C14 C 0.3752(4) 0.4664(4) 0.2626(6) 0.061(2) Uani 1 1 d D . .
C15 C 0.3093(7) 0.4624(14) 0.2694(13) 0.063(5) Uani 0.71(4) 1 d PD A 1
H15A H 0.2804 0.4320 0.2092 0.095 Uiso 0.71(4) 1 calc PR A 1
H15B H 0.3147 0.5053 0.2548 0.095 Uiso 0.71(4) 1 calc PR A 1
H15C H 0.2906 0.4473 0.3485 0.095 Uiso 0.71(4) 1 calc PR A 1
C15B C 0.3017(8) 0.431(3) 0.280(4) 0.063(5) Uani 0.29(4) 1 d PD A 2
H15D H 0.2881 0.4632 0.2953 0.095 Uiso 0.29(4) 1 calc PR A 2
H15E H 0.2897 0.4017 0.3474 0.095 Uiso 0.29(4) 1 calc PR A 2
H15F H 0.2803 0.4069 0.2078 0.095 Uiso 0.29(4) 1 calc PR A 2
N1 N 0.5893(3) 0.5127(3) 0.3879(4) 0.0410(13) Uani 1 1 d . A .
O1 O 0.4078(2) 0.4845(3) 0.3579(4) 0.0532(13) Uani 1 1 d D A .
O2 O 0.3952(2) 0.4591(3) 0.1640(4) 0.0559(13) Uani 1 1 d . A .
Cl1 Cl 0.66559(12) 0.80759(10) 0.4023(2) 0.0725(6) Uani 1 1 d . . .
Pd1 Pd 0.49754(2) 0.49546(2) 0.37115(3) 0.0338(3) Uani 1 1 d . . .
F1 F 0.3333 0.6667 0.7491(17) 0.036(2) Uani 0.114(4) 1 d PU B 1
F1B F 0.3883(7) 0.6598(7) 0.6567(15) 0.036(2) Uani 0.211(6) 1 d P C 2
F1C F 0.5925(8) 0.3367(8) 0.4535(18) 0.036(2) Uani 0.176(6) 1 d P D 3
Cl1S Cl 0.2846(5) 0.2215(4) 0.3009(8) 0.072(2) Uani 0.25 1 d PD . .
C1S C 0.2921(16) 0.2921(16) 0.2500 0.072(2) Uani 0.25 2 d SPD . .
H1SA H 0.3243 0.3088 0.1849 0.086 Uiso 0.13 1 calc PR . .
H1SB H 0.3088 0.3243 0.3151 0.086 Uiso 0.13 1 calc PR . .
C2S C 0.6667 0.3333 0.578(3) 0.088(3) Uani 0.16667 1 d PD E -1
H2SA H 0.6887 0.3137 0.5346 0.105 Uiso 0.17 1 calc PR E -1
H2SB H 0.6490 0.3506 0.5177 0.105 Uiso 0.17 1 calc PR E -1
Cl3S Cl 0.7221(7) 0.3953(7) 0.6566(14) 0.088(3) Uani 0.16667 1 d PD E -1
Cl4S Cl 0.6002(7) 0.2705(7) 0.6578(13) 0.088(3) Uani 0.16667 1 d PD E -1
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'
Cl Cl 0.1484 0.1585 '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'
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'
Pd Pd -0.9988 1.0072 '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
N1 C1 C2 122.0(7) . .
C3 C2 C1 120.3(7) . .
C2 C3 C4 119.6(7) . .
C13 C4 C3 116.1(7) . .
C13 C4 C5 117.6(6) . .
C3 C4 C5 126.2(7) . .
C6 C5 C4 122.1(7) . .
C5 C6 C7 121.1(7) . .
C12 C7 C8 114.9(6) . .
C12 C7 C6 119.0(6) . .
C8 C7 C6 126.1(7) . .
C9 C8 C7 121.4(7) . .
C9 C8 Cl1 119.3(6) . .
C7 C8 Cl1 119.2(6) . .
C8 C9 C10 122.0(6) . .
C11 C10 C9 119.2(7) . .
C10 C11 C12 118.1(6) . .
C10 C11 Pd1 129.7(5) . .
C12 C11 Pd1 112.0(5) . .
C7 C12 C11 124.4(6) . .
C7 C12 C13 119.3(6) . .
C11 C12 C13 116.2(6) . .
N1 C13 C4 123.7(6) . .
N1 C13 C12 115.5(6) . .
C4 C13 C12 120.8(6) . .
O2 C14 O1 125.6(7) . .
O2 C14 C15 119.2(8) . .
O1 C14 C15 114.7(8) . .
O2 C14 C15B 116.6(18) . .
O1 C14 C15B 114.8(16) . .
C15 C14 C15B 25.6(17) . .
C1 N1 C13 118.3(6) . .
C1 N1 Pd1 129.0(5) . .
C13 N1 Pd1 112.6(4) . .
C14 O1 Pd1 122.4(5) . .
C14 O2 Pd1 122.0(5) . 4
C11 Pd1 N1 83.2(2) . .
C11 Pd1 O1 93.0(3) . .
N1 Pd1 O1 176.1(2) . .
C11 Pd1 O2 175.0(2) . 4
N1 Pd1 O2 93.5(2) . 4
O1 Pd1 O2 90.4(2) . 4
C11 Pd1 Pd1 96.23(16) . 4
N1 Pd1 Pd1 96.71(13) . 4
O1 Pd1 Pd1 84.34(12) . 4
O2 Pd1 Pd1 80.40(11) 4 4
C11 Pd1 Pd1 79.07(16) . 7_666
N1 Pd1 Pd1 83.86(13) . 7_666
O1 Pd1 Pd1 94.78(12) . 7_666
O2 Pd1 Pd1 104.36(12) 4 7_666
Pd1 Pd1 Pd1 175.18(3) 4 7_666
Cl1S C1S Cl1S 114(2) . 4
Cl3S C2S Cl4S 117(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.328(8) .
C1 C2 1.389(11) .
C2 C3 1.364(12) .
C3 C4 1.417(10) .
C4 C13 1.401(10) .
C4 C5 1.427(11) .
C5 C6 1.341(11) .
C6 C7 1.428(10) .
C7 C12 1.395(9) .
C7 C8 1.415(10) .
C8 C9 1.372(11) .
C8 Cl1 1.744(8) .
C9 C10 1.398(10) .
C10 C11 1.370(9) .
C11 C12 1.416(9) .
C11 Pd1 1.960(7) .
C12 C13 1.434(9) .
C13 N1 1.357(9) .
C14 O2 1.255(8) .
C14 O1 1.267(8) .
C14 C15 1.528(12) .
C14 C15B 1.531(18) .
N1 Pd1 2.025(6) .
O1 Pd1 2.029(5) .
O2 Pd1 2.128(5) 4
Pd1 O2 2.128(5) 4
Pd1 Pd1 2.7271(8) 4
Pd1 Pd1 2.9053(8) 7_666
Cl1S C1S 1.70(2) .
C1S Cl1S 1.70(2) 4
C2S Cl3S 1.66(2) .
C2S Cl4S 1.79(2) .
