#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/36/4503616.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_4503616
loop_
_publ_author_name
'Kwon, Soon Sik'
'Cha, Moon Soon'
'Lee, Ji Eun'
'Lee, Shim Sung'
'Jung, Ok-Sang'
_publ_section_title
;
 Subtle Ligand Effects on the Formation and Behavior of Inorganic
 Guest-Organic Host Supramolecular System
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2073
_journal_page_last               2075
_journal_paper_doi               10.1021/cg800140s
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C27 H19 N4 O12 Pd0.5'
_chemical_formula_weight         644.66
_chemical_name_systematic        ?
_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
_audit_creation_method           SHELXTL
_cell_angle_alpha                65.2670(10)
_cell_angle_beta                 88.5900(10)
_cell_angle_gamma                82.4400(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2400(5)
_cell_length_b                   11.8761(6)
_cell_length_c                   12.9567(7)
_cell_measurement_reflns_used    6026
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.73
_cell_volume                     1279.42(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11134
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.072
_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     399
_refine_ls_number_reflns         5497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0338
_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)+(0.0367P)²+0.2573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                4956
_reflns_number_total             5497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800140s-file002.cif
_cod_data_source_block           Pd(ppma)2(H2tma)2(H3tma)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C27 H19 N4 O12 Pd0.50'
_cod_database_code               4503616
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
Pd1 Pd 0.5000 0.5000 0.5000 0.01601(8) Uani 1 2 d S
N1 N 0.51182(19) 0.37780(17) 0.66566(15) 0.0186(4) Uani 1 1 d .
N2 N 0.5071(2) 0.20606(18) 0.61860(16) 0.0226(4) Uani 1 1 d .
H2A H 0.5606 0.1354 0.6274 0.027 Uiso 1 1 calc R
N3 N 0.37511(19) 0.38519(17) 0.47401(15) 0.0170(4) Uani 1 1 d .
N4 N 0.5710(2) 0.16662(19) 0.80150(17) 0.0291(5) Uani 1 1 d .
C1 C 0.5113(2) 0.4170(2) 0.75027(19) 0.0214(5) Uani 1 1 d .
H1A H 0.4879 0.5036 0.7327 0.026 Uiso 1 1 calc R
C2 C 0.5441(3) 0.3335(2) 0.8606(2) 0.0257(5) Uani 1 1 d .
H2B H 0.5423 0.3602 0.9203 0.031 Uiso 1 1 calc R
C3 C 0.5799(3) 0.2083(2) 0.8819(2) 0.0301(6) Uani 1 1 d .
H3A H 0.6120 0.1501 0.9565 0.036 Uiso 1 1 calc R
C4 C 0.5299(2) 0.2535(2) 0.69660(19) 0.0202(5) Uani 1 1 d .
C5 C 0.4068(2) 0.2601(2) 0.52714(19) 0.0188(4) Uani 1 1 d .
C6 C 0.3426(2) 0.1797(2) 0.49451(19) 0.0216(5) Uani 1 1 d .
H6A H 0.3722 0.0919 0.5298 0.026 Uiso 1 1 calc R
C7 C 0.2357(3) 0.2305(2) 0.4101(2) 0.0243(5) Uani 1 1 d .
H7A H 0.1907 0.1778 0.3858 0.029 Uiso 1 1 calc R
C8 C 0.1933(2) 0.3586(2) 0.3603(2) 0.0234(5) Uani 1 1 d .
H8A H 0.1167 0.3943 0.3039 0.028 Uiso 1 1 calc R
C9 C 0.2637(2) 0.4325(2) 0.39366(19) 0.0213(5) Uani 1 1 d .
H9A H 0.2341 0.5203 0.3597 0.026 Uiso 1 1 calc R
O1 O 0.2549(2) 0.62269(16) -0.04211(16) 0.0361(5) Uani 1 1 d .
H1 H 0.2254 0.6969 -0.0871 0.054 Uiso 1 1 calc R
O2 O 0.09044(19) 0.58544(16) -0.14384(15) 0.0311(4) Uani 1 1 d .
O3 O 0.54458(18) 0.26344(15) 0.26345(14) 0.0243(4) Uani 1 1 d .
H3 H 0.6033 0.2277 0.3197 0.037 Uiso 1 1 calc R
O4 O 0.50371(19) 0.06760(15) 0.30396(14) 0.0307(4) Uani 1 1 d .
O5 O 0.1446(2) 0.00195(17) 0.06369(17) 0.0392(5) Uani 1 1 d .
O6 O -0.00353(18) 0.16866(15) -0.05630(14) 0.0277(4) Uani 1 1 d .
H6 H -0.0473 0.1132 -0.0610 0.033 Uiso 1 1 calc R
C10 C 0.1884(2) 0.5487(2) -0.06561(19) 0.0225(5) Uani 1 1 d .
C11 C 0.2269(2) 0.4129(2) 0.00171(19) 0.0198(5) Uani 1 1 d .
C12 C 0.3347(2) 0.3648(2) 0.08952(19) 0.0200(5) Uani 1 1 d .
H12A H 0.3843 0.4200 0.1072 0.024 Uiso 1 1 calc R
C13 C 0.3687(2) 0.2360(2) 0.15039(18) 0.0193(5) Uani 1 1 d .
C14 C 0.4817(2) 0.1806(2) 0.24751(19) 0.0208(5) Uani 1 1 d .
C15 C 0.2969(2) 0.1555(2) 0.12401(19) 0.0226(5) Uani 1 1 d .
H15A H 0.3219 0.0676 0.1644 0.027 Uiso 1 1 calc R
C16 C 0.1880(2) 0.2035(2) 0.03825(19) 0.0208(5) Uani 1 1 d .
C17 C 0.1082(2) 0.1158(2) 0.0153(2) 0.0230(5) Uani 1 1 d .
C18 C 0.1530(2) 0.3320(2) -0.02266(19) 0.0206(5) Uani 1 1 d .
H18A H 0.0785 0.3645 -0.0808 0.025 Uiso 1 1 calc R
O7 O 1.17938(19) -0.14027(16) 0.83335(15) 0.0319(4) Uani 1 1 d .
O8 O 1.01844(19) -0.17787(15) 0.72880(15) 0.0291(4) Uani 1 1 d .
H8 H 1.0478 -0.2522 0.7737 0.035 Uiso 1 1 calc R
O9 O 1.24006(17) 0.28867(16) 0.76340(14) 0.0260(4) Uani 1 1 d .
O10 O 1.08759(18) 0.44680(15) 0.63790(15) 0.0301(4) Uani 1 1 d .
H10 H 1.1491 0.4910 0.6422 0.036 Uiso 1 1 calc R
O11 O 0.75211(18) 0.37352(15) 0.38873(15) 0.0296(4) Uani 1 1 d .
O12 O 0.71852(17) 0.17700(15) 0.42949(14) 0.0243(4) Uani 1 1 d .
C19 C 1.0825(2) -0.1039(2) 0.75440(19) 0.0217(5) Uani 1 1 d .
C20 C 1.0398(2) 0.0323(2) 0.68959(19) 0.0201(5) Uani 1 1 d .
C21 C 1.1048(2) 0.1142(2) 0.71893(19) 0.0202(5) Uani 1 1 d .
H21A H 1.1789 0.0826 0.7773 0.024 Uiso 1 1 calc R
C22 C 1.0618(2) 0.2424(2) 0.66318(18) 0.0179(4) Uani 1 1 d .
C23 C 1.1392(2) 0.3267(2) 0.69447(19) 0.0202(5) Uani 1 1 d .
C24 C 0.9544(2) 0.2883(2) 0.57633(19) 0.0190(5) Uani 1 1 d .
H24A H 0.9242 0.3759 0.5387 0.023 Uiso 1 1 calc R
C25 C 0.8909(2) 0.2071(2) 0.54425(18) 0.0184(4) Uani 1 1 d .
C26 C 0.7786(2) 0.2586(2) 0.44609(19) 0.0202(5) Uani 1 1 d .
C27 C 0.9328(2) 0.0791(2) 0.60159(19) 0.0200(5) Uani 1 1 d .
H27A H 0.8888 0.0231 0.5812 0.024 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'
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 180.00(11) 2_666 .
N1 Pd1 N3 86.52(7) 2_666 2_666
N1 Pd1 N3 93.48(7) . 2_666
N1 Pd1 N3 93.48(7) 2_666 .
N1 Pd1 N3 86.52(7) . .
N3 Pd1 N3 180.000(1) 2_666 .
C4 N1 C1 117.09(19) . .
C4 N1 Pd1 121.18(15) . .
C1 N1 Pd1 121.61(15) . .
C4 N2 C5 125.72(19) . .
C5 N3 C9 117.42(18) . .
C5 N3 Pd1 121.45(14) . .
C9 N3 Pd1 120.85(15) . .
C3 N4 C4 116.3(2) . .
N1 C1 C2 120.9(2) . .
C1 C2 C3 117.5(2) . .
N4 C3 C2 122.6(2) . .
N4 C4 N1 124.8(2) . .
N4 C4 N2 114.7(2) . .
N1 C4 N2 120.5(2) . .
N3 C5 N2 120.08(19) . .
N3 C5 C6 122.6(2) . .
N2 C5 C6 117.4(2) . .
C7 C6 C5 118.3(2) . .
C6 C7 C8 120.0(2) . .
C9 C8 C7 118.8(2) . .
C8 C9 N3 122.6(2) . .
O2 C10 O1 123.4(2) . .
O2 C10 C11 118.2(2) . .
O1 C10 C11 118.4(2) . .
C18 C11 C12 120.0(2) . .
C18 C11 C10 118.47(19) . .
C12 C11 C10 121.5(2) . .
C13 C12 C11 119.8(2) . .
C15 C13 C12 120.0(2) . .
C15 C13 C14 118.6(2) . .
C12 C13 C14 121.32(19) . .
O4 C14 O3 126.1(2) . .
O4 C14 C13 120.2(2) . .
O3 C14 C13 113.72(19) . .
C13 C15 C16 120.1(2) . .
C18 C16 C15 120.2(2) . .
C18 C16 C17 120.7(2) . .
C15 C16 C17 119.1(2) . .
O5 C17 O6 124.0(2) . .
O5 C17 C16 121.1(2) . .
O6 C17 C16 114.9(2) . .
C11 C18 C16 119.9(2) . .
O7 C19 O8 123.8(2) . .
O7 C19 C20 118.1(2) . .
O8 C19 C20 118.16(19) . .
C21 C20 C27 119.9(2) . .
C21 C20 C19 118.96(19) . .
C27 C20 C19 121.11(19) . .
C20 C21 C22 120.2(2) . .
C21 C22 C24 119.6(2) . .
C21 C22 C23 118.16(19) . .
C24 C22 C23 122.2(2) . .
O9 C23 O10 123.9(2) . .
O9 C23 C22 122.9(2) . .
O10 C23 C22 113.18(18) . .
C25 C24 C22 120.7(2) . .
C27 C25 C24 119.34(19) . .
C27 C25 C26 120.43(19) . .
C24 C25 C26 120.2(2) . .
O11 C26 O12 124.9(2) . .
O11 C26 C25 119.72(19) . .
O12 C26 C25 115.4(2) . .
C25 C27 C20 120.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.0219(18) 2_666
Pd1 N1 2.0219(18) .
Pd1 N3 2.0302(17) 2_666
Pd1 N3 2.0302(17) .
N1 C4 1.346(3) .
N1 C1 1.358(3) .
N2 C4 1.379(3) .
N2 C5 1.391(3) .
N3 C5 1.344(3) .
N3 C9 1.368(3) .
N4 C3 1.336(3) .
N4 C4 1.343(3) .
C1 C2 1.369(3) .
C2 C3 1.388(3) .
C5 C6 1.393(3) .
C6 C7 1.372(3) .
C7 C8 1.385(3) .
C8 C9 1.365(3) .
O1 C10 1.272(3) .
O2 C10 1.268(3) .
O3 C14 1.294(3) .
O4 C14 1.222(3) .
O5 C17 1.231(3) .
O6 C17 1.308(3) .
C10 C11 1.475(3) .
C11 C18 1.387(3) .
C11 C12 1.406(3) .
C12 C13 1.391(3) .
C13 C15 1.386(3) .
C13 C14 1.516(3) .
C15 C16 1.395(3) .
C16 C18 1.390(3) .
C16 C17 1.480(3) .
O7 C19 1.268(3) .
O8 C19 1.274(3) .
O9 C23 1.209(3) .
O10 C23 1.328(3) .
O11 C26 1.244(3) .
O12 C26 1.271(3) .
C19 C20 1.480(3) .
C20 C21 1.388(3) .
C20 C27 1.403(3) .
C21 C22 1.389(3) .
C22 C24 1.396(3) .
C22 C23 1.490(3) .
C24 C25 1.394(3) .
C25 C27 1.388(3) .
C25 C26 1.521(3) .
