#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/69/1516910.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_1516910
loop_
_publ_author_name
'Himansu Sekhar Sahoo'
'Debakanta Tripathy'
'Sabyasachi Chakrabortty'
'Satish Bhat'
'Avinash Kumbhar'
'Dillip Kumar Chand'
_publ_section_title
;
 Self-assembled mononuclear palladium(II) based molecular loopsOriginal
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              42
_journal_page_last               50
_journal_volume                  400
_journal_year                    2013
_chemical_formula_sum            'C36 H44 N6 O20 Pd'
_chemical_formula_weight         987.14
_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
_cell_angle_alpha                101.06(3)
_cell_angle_beta                 107.24(3)
_cell_angle_gamma                93.23(3)
_cell_formula_units_Z            1
_cell_length_a                   9.918(2)
_cell_length_b                   9.982(2)
_cell_length_c                   14.230(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1310.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0041
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5996
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.495
_refine_diff_density_min         -2.204
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0793
_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)+(0.1600P)²+4.0600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2491
_refine_ls_wR_factor_ref         0.2491
_reflns_number_gt                5996
_reflns_number_total             5996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-400-42-50-3.cif
_cod_data_source_block           plat
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1310.8(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1516910
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 1.0000 0.0000 0.0449(2) Uani 1 2 d S . 1
O1 O 0.7432(11) 0.4076(7) 0.0227(8) 0.137(3) Uani 1 1 d . A 1
O2 O 0.8066(9) 0.6084(7) 0.1311(7) 0.128(3) Uani 1 1 d . A 1
O3 O 1.0352(11) 0.7554(11) 0.2961(7) 0.145(4) Uani 1 1 d . A 1
O4 O 1.060(2) 1.0352(15) 0.3607(9) 0.236(9) Uani 1 1 d . A 1
O5 O 1.0426(6) 1.1831(8) 0.2045(5) 0.0955(18) Uani 1 1 d . A 1
O6 O 1.1727(7) 1.2159(10) 0.1052(7) 0.123(3) Uani 1 1 d . A 1
O7 O 0.7752(13) 0.8670(13) 0.2651(5) 1.672(18) Uani 1 1 d . B 4
O8 O 0.7565(18) 0.993(2) 0.278(3) 0.46(3) Uani 1 1 d . B 4
O9 O 0.764(6) 0.785(5) 0.3094(19) 1.57(8) Uani 1 1 d . C 3
O10 O 0.546(3) 0.776(3) 0.348(3) 0.57(3) Uani 1 1 d . D 4
N1 N 0.5298(5) 0.8020(4) -0.0510(4) 0.0487(9) Uani 1 1 d . A 1
N2 N 0.6776(5) 1.0700(4) -0.0289(4) 0.0506(10) Uani 1 1 d . A 1
N3 N 0.753(3) 0.952(3) 0.2287(9) 0.246(14) Uani 1 1 d . B 4
C1 C 0.4647(8) 0.7406(7) -0.1485(5) 0.0675(16) Uani 1 1 d . A 1
H1 H 0.4065 0.7886 -0.1911 0.081 Uiso 1 1 calc R A 1
C2 C 0.4838(10) 0.6050(9) -0.1867(7) 0.086(2) Uani 1 1 d . A 1
H2 H 0.4385 0.5622 -0.2538 0.104 Uiso 1 1 calc R A 1
C3 C 0.5740(9) 0.5354(7) -0.1201(7) 0.081(2) Uani 1 1 d . A 1
H3 H 0.5894 0.4457 -0.1429 0.097 Uiso 1 1 calc R A 1
C4 C 0.6371(7) 0.6006(6) -0.0236(6) 0.0601(14) Uani 1 1 d . A 1
C5 C 0.6155(6) 0.7369(5) 0.0103(4) 0.0485(11) Uani 1 1 d . A 1
H5 H 0.6622 0.7820 0.0767 0.058 Uiso 1 1 calc R A 1
C6 C 0.7353(9) 0.5268(7) 0.0457(8) 0.081(2) Uani 1 1 d . A 1
C7 C 0.900(2) 0.5491(16) 0.2086(15) 0.185(9) Uani 1 1 d . A 1
H7A H 0.8398 0.4972 0.2354 0.222 Uiso 1 1 calc R A 1
H7B H 0.9494 0.4838 0.1759 0.222 Uiso 1 1 calc R A 1
C8 C 0.987(3) 0.625(2) 0.2788(19) 0.31(2) Uani 1 1 d . A 1
H8A H 1.0718 0.5784 0.2878 0.369 Uiso 1 1 calc R A 1
H8B H 0.9551 0.6177 0.3360 0.369 Uiso 1 1 calc R A 1
C9 C 1.082(3) 0.834(3) 0.3905(12) 0.201(10) Uani 1 1 d . A 1
H9A H 1.0129 0.8006 0.4225 0.241 Uiso 1 1 d R A 1
H9B H 1.1558 0.7913 0.4305 0.241 Uiso 1 1 d R A 1
C10 C 1.139(2) 0.963(2) 0.4118(11) 0.153(6) Uani 1 1 d . A 1
H10A H 1.1007 1.0008 0.4650 0.184 Uiso 1 1 d R A 1
H10B H 1.2439 1.0042 0.4405 0.184 Uiso 1 1 d R A 1
C11 C 1.118(2) 1.168(2) 0.3798(9) 0.167(7) Uani 1 1 d . A 1
H11A H 1.2009 1.1899 0.4394 0.200 Uiso 1 1 d R A 1
H11B H 1.0474 1.2253 0.3920 0.200 Uiso 1 1 d R A 1
C12 C 1.1657(12) 1.2111(15) 0.2944(10) 0.128(4) Uani 1 1 d . A 1
H12A H 1.2012 1.3082 0.3130 0.153 Uiso 1 1 calc R A 1
H12B H 1.2409 1.1592 0.2823 0.153 Uiso 1 1 calc R A 1
C13 C 1.0614(7) 1.1894(8) 0.1174(7) 0.077(2) Uani 1 1 d . A 1
C14 C 0.9251(6) 1.1529(6) 0.0323(5) 0.0583(14) Uani 1 1 d . A 1
C15 C 0.8012(6) 1.1039(5) 0.0474(5) 0.0510(11) Uani 1 1 d . A 1
H15 H 0.8034 1.0942 0.1115 0.061 Uiso 1 1 calc R A 1
C16 C 0.6734(8) 1.0879(8) -0.1192(5) 0.0684(16) Uani 1 1 d . A 1
H16 H 0.5867 1.0686 -0.1705 0.082 Uiso 1 1 calc R A 1
C17 C 0.7931(11) 1.1345(9) -0.1407(7) 0.086(2) Uani 1 1 d . A 1
H17 H 0.7875 1.1432 -0.2057 0.103 Uiso 1 1 calc R A 1
C18 C 0.9191(9) 1.1671(8) -0.0645(7) 0.078(2) Uani 1 1 d . A 1
H18 H 1.0008 1.1988 -0.0769 0.094 Uiso 1 1 calc R A 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'
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 Pd1 N1 179.999(1) . 2_675
N1 Pd1 N2 89.72(17) . 2_675
N1 Pd1 N2 90.28(17) 2_675 2_675
N1 Pd1 N2 90.28(17) . .
N1 Pd1 N2 89.72(17) 2_675 .
N2 Pd1 N2 180.0 2_675 .
C6 O2 C7 118.2(9) . .
C8 O3 C9 121.6(16) . .
C10 O4 C11 113.2(17) . .
C13 O5 C12 118.7(8) . .
N3 O7 O8 35(2) . .
N3 O8 O7 58(3) . .
C5 N1 C1 120.7(5) . .
C5 N1 Pd1 120.2(4) . .
C1 N1 Pd1 119.1(4) . .
C16 N2 C15 119.3(5) . .
C16 N2 Pd1 121.7(5) . .
C15 N2 Pd1 118.9(4) . .
O8 N3 O7 87(3) . .
N1 C1 C2 120.8(7) . .
N1 C1 H1 119.6 . .
C2 C1 H1 119.6 . .
C1 C2 C3 118.1(7) . .
C1 C2 H2 120.9 . .
C3 C2 H2 120.9 . .
C4 C3 C2 119.2(6) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C3 C4 C5 120.3(6) . .
C3 C4 C6 118.6(6) . .
C5 C4 C6 121.0(7) . .
N1 C5 C4 120.9(5) . .
N1 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
O1 C6 O2 125.7(8) . .
O1 C6 C4 122.3(9) . .
O2 C6 C4 112.0(6) . .
C8 C7 O2 118.7(14) . .
C8 C7 H7A 107.5 . .
O2 C7 H7A 107.6 . .
C8 C7 H7B 107.6 . .
O2 C7 H7B 107.8 . .
H7A C7 H7B 107.1 . .
C7 C8 O3 132.7(13) . .
C7 C8 H8A 104.1 . .
O3 C8 H8A 104.0 . .
C7 C8 H8B 104.2 . .
O3 C8 H8B 103.9 . .
H8A C8 H8B 105.4 . .
C10 C9 O3 123.6(16) . .
C10 C9 H9A 123.6 . .
O3 C9 H9A 102.5 . .
C10 C9 H9B 102.8 . .
O3 C9 H9B 107.9 . .
H9A C9 H9B 90.4 . .
O4 C10 C9 112.1(18) . .
O4 C10 H10A 85.3 . .
C9 C10 H10A 99.7 . .
O4 C10 H10B 113.6 . .
C9 C10 H10B 130.2 . .
H10A C10 H10B 102.8 . .
O4 C11 C12 115.8(14) . .
O4 C11 H11A 111.6 . .
C12 C11 H11A 106.2 . .
O4 C11 H11B 107.2 . .
C12 C11 H11B 107.7 . .
H11A C11 H11B 108.1 . .
O5 C12 C11 107.5(10) . .
O5 C12 H12A 110.2 . .
C11 C12 H12A 110.2 . .
O5 C12 H12B 110.2 . .
C11 C12 H12B 110.3 . .
H12A C12 H12B 108.5 . .
O6 C13 O5 125.4(9) . .
O6 C13 C14 122.7(9) . .
O5 C13 C14 111.9(6) . .
C15 C14 C18 118.3(6) . .
C15 C14 C13 120.8(6) . .
C18 C14 C13 120.8(6) . .
N2 C15 C14 121.4(6) . .
N2 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
N2 C16 C17 122.7(8) . .
N2 C16 H16 118.6 . .
C17 C16 H16 118.6 . .
C18 C17 C16 118.4(7) . .
C18 C17 H17 120.8 . .
C16 C17 H17 120.8 . .
C17 C18 C14 119.8(6) . .
C17 C18 H18 120.1 . .
C14 C18 H18 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.040(4) .
Pd1 N1 2.040(4) 2_675
Pd1 N2 2.041(4) 2_675
Pd1 N2 2.041(4) .
O1 C6 1.185(10) .
O2 C6 1.299(12) .
O2 C7 1.459(13) .
O3 C8 1.31(2) .
O3 C9 1.35(2) .
O4 C10 1.26(2) .
O4 C11 1.36(2) .
O5 C13 1.319(11) .
O5 C12 1.450(12) .
O6 C13 1.190(9) .
O7 N3 1.08(2) .
O7 O8 1.27(3) .
O8 N3 0.73(4) .
N1 C5 1.321(7) .
N1 C1 1.348(8) .
N2 C16 1.319(8) .
N2 C15 1.349(8) .
C1 C2 1.404(11) .
C1 H1 0.9300 .
C2 C3 1.414(13) .
C2 H2 0.9300 .
C3 C4 1.343(11) .
C3 H3 0.9300 .
C4 C5 1.404(7) .
C4 C6 1.501(10) .
C5 H5 0.9300 .
C7 C8 1.20(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.31(2) .
C9 H9A 1.0067 .
C9 H9B 0.9622 .
C10 H10A 0.9700 .
C10 H10B 1.0245 .
C11 C12 1.55(2) .
C11 H11A 0.9687 .
C11 H11B 0.9617 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.494(10) .
C14 C15 1.387(7) .
C14 C18 1.395(11) .
C15 H15 0.9300 .
C16 C17 1.389(11) .
C16 H16 0.9300 .
C17 C18 1.364(14) .
C17 H17 0.9300 .
C18 H18 0.9300 .
