#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/36/4503617.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_4503617
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            'C19 H17 N4 O7 Pd0.5'
_chemical_formula_weight         466.57
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3065(5)
_cell_length_b                   14.7815(9)
_cell_length_c                   15.1488(9)
_cell_measurement_reflns_used    2110
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.69
_cell_volume                     1857.72(19)
_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 0.998
_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  0.0841
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11352
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0451
_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)+(0.0546P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                2470
_reflns_number_total             4054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800140s-file002.cif
_cod_data_source_block           Pd(ppma)2(H2tma)2(CH3OH)2
_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 2.4.1 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      P2(1)/n
_cod_original_formula_sum        'C19 H17 N4 O7 Pd0.50'
_cod_database_code               4503617
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.0000 0.5000 0.5000 0.01434(15) Uani 1 2 d S
N1 N 0.0170(5) 0.5514(3) 0.6231(3) 0.0163(9) Uani 1 1 d .
N2 N -0.0826(6) 0.6613(3) 0.7212(3) 0.0289(11) Uani 1 1 d .
N3 N -0.0804(5) 0.6929(3) 0.5730(3) 0.0181(10) Uani 1 1 d .
H3B H -0.1599 0.7313 0.5797 0.022 Uiso 1 1 calc R
N4 N 0.0617(5) 0.6244(3) 0.4589(3) 0.0161(9) Uani 1 1 d .
O1 O 0.4191(4) 0.5030(2) 0.8207(2) 0.0231(7) Uani 1 1 d .
O2 O 0.6184(5) 0.4531(3) 0.7408(2) 0.0307(9) Uani 1 1 d .
O3 O 0.6760(4) 0.5830(2) 0.4417(2) 0.0220(8) Uani 1 1 d .
O4 O 0.5700(5) 0.7185(2) 0.4111(2) 0.0323(10) Uani 1 1 d .
H4 H 0.5960 0.7086 0.3655 0.039 Uiso 1 1 d R
O5 O 0.2118(4) 0.8635(2) 0.6206(2) 0.0220(8) Uani 1 1 d .
H5 H 0.1536 0.9117 0.6495 0.026 Uiso 1 1 d R
O6 O 0.2118(5) 0.8106(2) 0.7584(2) 0.0307(9) Uani 1 1 d .
O7 O -0.2214(5) 0.8568(2) 0.6168(3) 0.0348(10) Uani 1 1 d .
H7 H -0.1879 0.8759 0.6591 0.042 Uiso 1 1 d R
C1 C 0.0726(5) 0.5018(4) 0.6939(3) 0.0212(10) Uani 1 1 d .
H1A H 0.1298 0.4473 0.6841 0.025 Uiso 1 1 calc R
C2 C 0.0485(6) 0.5281(3) 0.7780(3) 0.0210(12) Uani 1 1 d .
H2A H 0.0887 0.4935 0.8271 0.025 Uiso 1 1 calc R
C3 C -0.0361(6) 0.6067(4) 0.7895(3) 0.0255(12) Uani 1 1 d .
H3A H -0.0630 0.6234 0.8475 0.031 Uiso 1 1 calc R
C4 C -0.0480(6) 0.6331(3) 0.6405(3) 0.0185(11) Uani 1 1 d .
C5 C -0.0004(7) 0.6989(3) 0.4953(4) 0.0173(10) Uani 1 1 d .
C6 C 0.0150(6) 0.7834(3) 0.4589(3) 0.0195(11) Uani 1 1 d .
H6A H -0.0347 0.8345 0.4840 0.023 Uiso 1 1 calc R
C7 C 0.1032(6) 0.7922(4) 0.3860(4) 0.0269(13) Uani 1 1 d .
H7A H 0.1146 0.8499 0.3595 0.032 Uiso 1 1 calc R
C8 C 0.1764(7) 0.7174(4) 0.3504(4) 0.0271(13) Uani 1 1 d .
H8A H 0.2413 0.7231 0.3007 0.032 Uiso 1 1 calc R
C9 C 0.1527(6) 0.6356(3) 0.3886(3) 0.0222(12) Uani 1 1 d .
H9A H 0.2026 0.5840 0.3646 0.027 Uiso 1 1 calc R
C10 C 0.5062(6) 0.5063(4) 0.7550(3) 0.0193(10) Uani 1 1 d .
C11 C 0.4746(6) 0.5819(3) 0.6897(3) 0.0155(11) Uani 1 1 d .
C12 C 0.3762(6) 0.6543(3) 0.7112(3) 0.0159(11) Uani 1 1 d .
H12A H 0.3277 0.6550 0.7667 0.019 Uiso 1 1 calc R
C13 C 0.3483(6) 0.7256(3) 0.6524(3) 0.0159(11) Uani 1 1 d .
C14 C 0.2500(6) 0.8043(3) 0.6823(3) 0.0171(11) Uani 1 1 d .
C15 C 0.4170(6) 0.7248(3) 0.5700(3) 0.0159(11) Uani 1 1 d .
H15A H 0.3975 0.7729 0.5294 0.019 Uiso 1 1 calc R
C16 C 0.5147(6) 0.6520(3) 0.5484(3) 0.0142(10) Uani 1 1 d .
C17 C 0.5944(6) 0.6464(3) 0.4625(3) 0.0183(11) Uani 1 1 d .
C18 C 0.5419(6) 0.5821(3) 0.6088(3) 0.0157(11) Uani 1 1 d .
H18A H 0.6090 0.5331 0.5936 0.019 Uiso 1 1 calc R
C19 C -0.2820(9) 0.9208(4) 0.5536(5) 0.0529(19) Uani 1 1 d .
H19A H -0.3854 0.9444 0.5719 0.079 Uiso 1 1 calc R
H19B H -0.2974 0.8914 0.4958 0.079 Uiso 1 1 calc R
H19C H -0.2051 0.9707 0.5495 0.079 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 179.999(2) . 3_566
N1 Pd1 N4 93.77(16) . 3_566
N1 Pd1 N4 86.23(16) 3_566 3_566
N1 Pd1 N4 86.23(16) . .
N1 Pd1 N4 93.77(16) 3_566 .
N4 Pd1 N4 179.998(1) 3_566 .
C4 N1 C1 116.8(4) . .
C4 N1 Pd1 120.4(3) . .
C1 N1 Pd1 122.1(3) . .
C4 N2 C3 116.6(5) . .
C4 N3 C5 126.3(4) . .
C5 N4 C9 117.7(4) . .
C5 N4 Pd1 120.7(4) . .
C9 N4 Pd1 121.2(3) . .
C2 C1 N1 121.7(5) . .
C1 C2 C3 117.5(5) . .
N2 C3 C2 122.4(5) . .
N2 C4 N1 124.1(5) . .
N2 C4 N3 116.1(4) . .
N1 C4 N3 119.8(4) . .
N4 C5 C6 122.3(5) . .
N4 C5 N3 120.5(4) . .
C6 C5 N3 117.3(4) . .
C7 C6 C5 118.5(5) . .
C6 C7 C8 120.3(5) . .
C9 C8 C7 117.9(5) . .
N4 C9 C8 123.1(5) . .
O2 C10 O1 125.1(5) . .
O2 C10 C11 117.5(4) . .
O1 C10 C11 117.3(5) . .
C18 C11 C12 118.4(4) . .
C18 C11 C10 121.5(4) . .
C12 C11 C10 120.1(4) . .
C13 C12 C11 120.8(5) . .
C12 C13 C15 120.2(5) . .
C12 C13 C14 117.9(4) . .
C15 C13 C14 121.8(4) . .
O6 C14 O5 124.2(5) . .
O6 C14 C13 121.1(4) . .
O5 C14 C13 114.7(4) . .
C16 C15 C13 118.9(5) . .
C18 C16 C15 119.7(5) . .
C18 C16 C17 117.9(4) . .
C15 C16 C17 122.4(4) . .
O3 C17 O4 122.7(5) . .
O3 C17 C16 123.4(5) . .
O4 C17 C16 113.9(4) . .
C11 C18 C16 122.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.013(4) .
Pd1 N1 2.013(4) 3_566
Pd1 N4 2.016(4) 3_566
Pd1 N4 2.016(4) .
N1 C4 1.354(6) .
N1 C1 1.361(6) .
N2 C4 1.336(6) .
N2 C3 1.353(7) .
N3 C4 1.367(6) .
N3 C5 1.383(7) .
N4 C5 1.345(6) .
N4 C9 1.346(6) .
O1 C10 1.260(5) .
O2 C10 1.247(6) .
O3 C17 1.208(6) .
O4 C17 1.330(6) .
O5 C14 1.308(6) .
O6 C14 1.213(6) .
O7 C19 1.419(7) .
C1 C2 1.357(7) .
C2 C3 1.374(7) .
C5 C6 1.374(6) .
C6 C7 1.361(7) .
C7 C8 1.384(7) .
C8 C9 1.359(7) .
C10 C11 1.506(7) .
C11 C18 1.372(7) .
C11 C12 1.395(6) .
C12 C13 1.391(6) .
C13 C15 1.398(7) .
C13 C14 1.505(6) .
C15 C16 1.396(6) .
C16 C18 1.391(6) .
C16 C17 1.491(7) .
