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#$Date: 2016-02-04 01:06:32 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175484 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/45/4344543.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_4344543
loop_
_publ_author_name
'Akine, Shigehisa'
'Utsuno, Fumihiko'
'Piao, Shunjin'
'Orita, Hideo'
'Tsuzuki, Seiji'
'Nabeshima, Tatsuya'
_publ_section_title
;
 Synthesis, Ion Recognition Ability, and Metal-Assisted Aggregation
 Behavior of Dinuclear Metallohosts Having a Bis(Saloph) Macrocyclic
 Ligand.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              810
_journal_page_last               821
_journal_paper_doi               10.1021/acs.inorgchem.5b02288
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         C44H36N4O8Pd2S2
_chemical_formula_sum            'C44 H36 N4 O8 Pd2 S2'
_chemical_formula_weight         1025.69
_chemical_name_common            '[LPd2]_2DMSO'
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.9893(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7324(6)
_cell_length_b                   15.3932(7)
_cell_length_c                   11.6479(7)
_cell_measurement_temperature    120(2)
_cell_volume                     1910.00(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17672
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.8966
_exptl_absorpt_correction_T_min  0.6639
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0426
_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)+(0.0437P)²+3.8852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                3335
_reflns_number_total             4159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02288_si_004.cif
_cod_data_source_block           uts122
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4344543
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 0.19732(3) 0.106086(19) 0.48134(3) 0.01935(11) Uani 1 1 d .
C1 C 0.5463(3) 0.2239(3) 0.5963(4) 0.0225(8) Uani 1 1 d .
C2 C 0.4133(4) 0.2112(3) 0.5730(3) 0.0216(8) Uani 1 1 d .
C3 C 0.3381(4) 0.2887(3) 0.5679(4) 0.0237(9) Uani 1 1 d .
C4 C 0.3952(4) 0.3718(3) 0.5831(4) 0.0276(9) Uani 1 1 d .
H1 H 0.3439 0.4219 0.5846 0.033 Uiso 1 1 calc R
C5 C 0.5231(4) 0.3806(3) 0.5956(4) 0.0275(9) Uani 1 1 d .
H2 H 0.5605 0.4366 0.6000 0.033 Uiso 1 1 calc R
C6 C 0.5983(4) 0.3054(3) 0.6016(4) 0.0263(9) Uani 1 1 d .
H3 H 0.6870 0.3113 0.6097 0.032 Uiso 1 1 calc R
O1 O 0.3712(2) 0.13206(18) 0.5559(2) 0.0242(6) Uani 1 1 d .
C7 C 0.2053(4) 0.2894(3) 0.5394(4) 0.0246(9) Uani 1 1 d .
H4 H 0.1637 0.3428 0.5495 0.030 Uiso 1 1 calc R
N1 N 0.1353(3) 0.2241(2) 0.5010(3) 0.0223(7) Uani 1 1 d .
C8 C 0.0047(3) 0.2337(3) 0.4583(3) 0.0228(8) Uani 1 1 d .
C9 C -0.0613(4) 0.3115(3) 0.4616(4) 0.0277(9) Uani 1 1 d .
H5 H -0.0222 0.3613 0.4981 0.033 Uiso 1 1 calc R
C10 C -0.1847(4) 0.3149(3) 0.4110(4) 0.0301(10) Uani 1 1 d .
H6 H -0.2302 0.3679 0.4115 0.036 Uiso 1 1 calc R
C11 C -0.2430(4) 0.2412(3) 0.3592(4) 0.0293(10) Uani 1 1 d .
H7 H -0.3280 0.2443 0.3253 0.035 Uiso 1 1 calc R
C12 C -0.1782(4) 0.1642(3) 0.3569(4) 0.0247(9) Uani 1 1 d .
H8 H -0.2182 0.1139 0.3223 0.030 Uiso 1 1 calc R
C13 C -0.0528(3) 0.1607(3) 0.4063(3) 0.0216(8) Uani 1 1 d .
N2 N 0.0266(3) 0.0859(2) 0.4038(3) 0.0208(7) Uani 1 1 d .
C14 C -0.0084(3) 0.0157(3) 0.3463(3) 0.0221(8) Uani 1 1 d .
H9 H -0.0938 0.0128 0.3134 0.027 Uiso 1 1 calc R
C15 C 0.0690(3) -0.0578(3) 0.3278(3) 0.0213(8) Uani 1 1 d .
C16 C 0.1948(3) -0.0685(2) 0.3805(3) 0.0180(8) Uani 1 1 d .
C17 C 0.2615(3) -0.1422(3) 0.3457(3) 0.0211(8) Uani 1 1 d .
C18 C 0.2109(4) -0.1962(3) 0.2580(4) 0.0250(9) Uani 1 1 d .
H10 H 0.2607 -0.2410 0.2310 0.030 Uiso 1 1 calc R
C19 C 0.0853(4) -0.1853(3) 0.2079(4) 0.0280(9) Uani 1 1 d .
H11 H 0.0490 -0.2242 0.1499 0.034 Uiso 1 1 calc R
C20 C 0.0167(4) -0.1180(3) 0.2441(4) 0.0250(9) Uani 1 1 d .
H12 H -0.0685 -0.1116 0.2121 0.030 Uiso 1 1 calc R
O2 O 0.2541(2) -0.01543(17) 0.4571(2) 0.0233(6) Uani 1 1 d .
O3 O 0.3845(2) -0.14714(18) 0.3998(3) 0.0266(7) Uani 1 1 d .
S1 S 0.47789(10) 0.01189(7) 0.78313(10) 0.0270(2) Uani 1 1 d .
O4 O 0.3843(3) -0.0340(2) 0.8494(3) 0.0338(7) Uani 1 1 d .
C21 C 0.4896(4) -0.0502(3) 0.6567(4) 0.0276(9) Uani 1 1 d .
H13 H 0.5026 -0.1114 0.6777 0.041 Uiso 1 1 calc R
H14 H 0.5607 -0.0293 0.6190 0.041 Uiso 1 1 calc R
H15 H 0.4120 -0.0441 0.6035 0.041 Uiso 1 1 calc R
C22 C 0.6304(4) -0.0140(4) 0.8575(4) 0.0409(12) Uani 1 1 d .
H16 H 0.6352 0.0052 0.9381 0.061 Uiso 1 1 calc R
H17 H 0.6951 0.0156 0.8196 0.061 Uiso 1 1 calc R
H18 H 0.6438 -0.0769 0.8552 0.061 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'
S S 0.1246 0.1234 '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 N2 83.62(13) . .
N1 Pd1 O2 177.63(12) . .
N2 Pd1 O2 94.04(12) . .
N1 Pd1 O1 94.38(12) . .
N2 Pd1 O1 177.17(13) . .
O2 Pd1 O1 87.95(11) . .
C6 C1 O3 124.2(3) . 3_656
C6 C1 C2 121.6(4) . .
O3 C1 C2 113.9(3) 3_656 .
O1 C2 C1 118.4(3) . .
O1 C2 C3 125.9(3) . .
C1 C2 C3 115.8(4) . .
C4 C3 C7 115.3(4) . .
C4 C3 C2 120.7(4) . .
C7 C3 C2 123.8(4) . .
C5 C4 C3 121.0(4) . .
C5 C4 H1 119.5 . .
C3 C4 H1 119.5 . .
C4 C5 C6 119.0(4) . .
C4 C5 H2 120.5 . .
C6 C5 H2 120.5 . .
C1 C6 C5 121.5(4) . .
C1 C6 H3 119.3 . .
C5 C6 H3 119.3 . .
C2 O1 Pd1 122.7(2) . .
N1 C7 C3 126.5(4) . .
N1 C7 H4 116.8 . .
C3 C7 H4 116.8 . .
C7 N1 C8 122.5(3) . .
C7 N1 Pd1 124.5(3) . .
C8 N1 Pd1 112.7(3) . .
C13 C8 C9 120.5(4) . .
C13 C8 N1 115.6(3) . .
C9 C8 N1 123.8(4) . .
C10 C9 C8 119.0(4) . .
C10 C9 H5 120.5 . .
C8 C9 H5 120.5 . .
C9 C10 C11 120.5(4) . .
C9 C10 H6 119.7 . .
C11 C10 H6 119.7 . .
C12 C11 C10 120.5(4) . .
C12 C11 H7 119.8 . .
C10 C11 H7 119.8 . .
C11 C12 C13 119.2(4) . .
C11 C12 H8 120.4 . .
C13 C12 H8 120.4 . .
C8 C13 C12 120.3(4) . .
C8 C13 N2 115.2(3) . .
C12 C13 N2 124.5(4) . .
C14 N2 C13 122.8(3) . .
C14 N2 Pd1 124.2(3) . .
C13 N2 Pd1 112.7(2) . .
N2 C14 C15 126.5(3) . .
N2 C14 H9 116.7 . .
C15 C14 H9 116.7 . .
C20 C15 C16 119.9(4) . .
C20 C15 C14 115.6(3) . .
C16 C15 C14 124.3(4) . .
O2 C16 C15 125.2(3) . .
O2 C16 C17 117.9(3) . .
C15 C16 C17 116.9(3) . .
C18 C17 O3 124.7(4) . .
C18 C17 C16 121.6(3) . .
O3 C17 C16 113.3(3) . .
C17 C18 C19 120.4(4) . .
C17 C18 H10 119.8 . .
C19 C18 H10 119.8 . .
C20 C19 C18 119.0(4) . .
C20 C19 H11 120.5 . .
C18 C19 H11 120.5 . .
C19 C20 C15 121.8(4) . .
C19 C20 H12 119.1 . .
C15 C20 H12 119.1 . .
C16 O2 Pd1 123.1(2) . .
C17 O3 C1 122.2(3) . 3_656
O4 S1 C21 106.9(2) . .
O4 S1 C22 105.8(2) . .
C21 S1 C22 97.4(2) . .
S1 C21 H13 109.5 . .
S1 C21 H14 109.5 . .
H13 C21 H14 109.5 . .
S1 C21 H15 109.5 . .
H13 C21 H15 109.5 . .
H14 C21 H15 109.5 . .
S1 C22 H16 109.5 . .
S1 C22 H17 109.5 . .
H16 C22 H17 109.5 . .
S1 C22 H18 109.5 . .
H16 C22 H18 109.5 . .
H17 C22 H18 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 1.957(3) .
Pd1 N2 1.966(3) .
Pd1 O2 1.998(3) .
Pd1 O1 2.000(3) .
C1 C6 1.371(6) .
C1 O3 1.394(5) 3_656
C1 C2 1.434(5) .
C2 O1 1.306(5) .
C2 C3 1.437(6) .
C3 C4 1.420(6) .
C3 C7 1.424(5) .
C4 C5 1.369(6) .
C4 H1 0.9500 .
C5 C6 1.408(6) .
C5 H2 0.9500 .
C6 H3 0.9500 .
C7 N1 1.301(5) .
C7 H4 0.9500 .
N1 C8 1.436(5) .
C8 C13 1.385(6) .
C8 C9 1.394(6) .
C9 C10 1.384(6) .
C9 H5 0.9500 .
C10 C11 1.397(6) .
C10 H6 0.9500 .
C11 C12 1.377(6) .
C11 H7 0.9500 .
C12 C13 1.399(5) .
C12 H8 0.9500 .
C13 N2 1.435(5) .
N2 C14 1.304(5) .
C14 C15 1.435(5) .
C14 H9 0.9500 .
C15 C20 1.411(6) .
C15 C16 1.423(5) .
C16 O2 1.315(4) .
C16 C17 1.427(5) .
C17 C18 1.376(6) .
C17 O3 1.393(4) .
C18 C19 1.412(5) .
C18 H10 0.9500 .
C19 C20 1.367(6) .
C19 H11 0.9500 .
C20 H12 0.9500 .
O3 C1 1.394(5) 3_656
S1 O4 1.514(3) .
S1 C21 1.773(4) .
S1 C22 1.801(5) .
C21 H13 0.9800 .
C21 H14 0.9800 .
C21 H15 0.9800 .
C22 H16 0.9800 .
C22 H17 0.9800 .
C22 H18 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C6 C1 C2 O1 172.2(4) . .
O3 C1 C2 O1 -1.4(5) 3_656 .
C6 C1 C2 C3 -6.3(6) . .
O3 C1 C2 C3 -179.9(3) 3_656 .
O1 C2 C3 C4 -177.1(4) . .
C1 C2 C3 C4 1.2(6) . .
O1 C2 C3 C7 -2.0(7) . .
C1 C2 C3 C7 176.3(4) . .
C7 C3 C4 C5 -171.3(4) . .
C2 C3 C4 C5 4.2(7) . .
C3 C4 C5 C6 -4.6(7) . .
O3 C1 C6 C5 179.1(4) 3_656 .
C2 C1 C6 C5 6.1(7) . .
C4 C5 C6 C1 -0.5(7) . .
C1 C2 O1 Pd1 -162.8(3) . .
C3 C2 O1 Pd1 15.5(6) . .
N1 Pd1 O1 C2 -15.6(3) . .
N2 Pd1 O1 C2 29(3) . .
O2 Pd1 O1 C2 163.9(3) . .
C4 C3 C7 N1 166.5(4) . .
C2 C3 C7 N1 -8.8(7) . .
C3 C7 N1 C8 -170.5(4) . .
C3 C7 N1 Pd1 3.6(6) . .
N2 Pd1 N1 C7 -171.3(4) . .
O2 Pd1 N1 C7 -163(3) . .
O1 Pd1 N1 C7 6.7(4) . .
N2 Pd1 N1 C8 3.3(3) . .
O2 Pd1 N1 C8 11(3) . .
O1 Pd1 N1 C8 -178.7(3) . .
C7 N1 C8 C13 171.7(4) . .
Pd1 N1 C8 C13 -3.0(4) . .
C7 N1 C8 C9 -4.9(6) . .
Pd1 N1 C8 C9 -179.6(3) . .
C13 C8 C9 C10 -0.8(6) . .
N1 C8 C9 C10 175.7(4) . .
C8 C9 C10 C11 1.2(7) . .
C9 C10 C11 C12 -0.5(7) . .
C10 C11 C12 C13 -0.6(7) . .
C9 C8 C13 C12 -0.3(6) . .
N1 C8 C13 C12 -177.0(4) . .
C9 C8 C13 N2 177.3(4) . .
N1 C8 C13 N2 0.5(5) . .
C11 C12 C13 C8 1.0(6) . .
C11 C12 C13 N2 -176.4(4) . .
C8 C13 N2 C14 -171.6(4) . .
C12 C13 N2 C14 5.8(6) . .
C8 C13 N2 Pd1 2.2(4) . .
C12 C13 N2 Pd1 179.6(3) . .
N1 Pd1 N2 C14 170.7(3) . .
O2 Pd1 N2 C14 -8.9(3) . .
O1 Pd1 N2 C14 126(2) . .
N1 Pd1 N2 C13 -3.0(3) . .
O2 Pd1 N2 C13 177.3(3) . .
O1 Pd1 N2 C13 -48(3) . .
C13 N2 C14 C15 172.2(4) . .
Pd1 N2 C14 C15 -0.9(6) . .
N2 C14 C15 C20 -167.8(4) . .
N2 C14 C15 C16 6.8(7) . .
C20 C15 C16 O2 178.2(4) . .
C14 C15 C16 O2 3.8(6) . .
C20 C15 C16 C17 -0.9(6) . .
C14 C15 C16 C17 -175.3(4) . .
O2 C16 C17 C18 -173.6(4) . .
C15 C16 C17 C18 5.6(6) . .
O2 C16 C17 O3 -0.2(5) . .
C15 C16 C17 O3 179.0(3) . .
O3 C17 C18 C19 -179.3(4) . .
C16 C17 C18 C19 -6.7(6) . .
C17 C18 C19 C20 2.9(6) . .
C18 C19 C20 C15 1.8(6) . .
C16 C15 C20 C19 -2.7(6) . .
C14 C15 C20 C19 172.1(4) . .
C15 C16 O2 Pd1 -17.8(5) . .
C17 C16 O2 Pd1 161.3(3) . .
N1 Pd1 O2 C16 10(3) . .
N2 Pd1 O2 C16 17.9(3) . .
O1 Pd1 O2 C16 -160.1(3) . .
C18 C17 O3 C1 -25.1(6) . 3_656
C16 C17 O3 C1 161.8(4) . 3_656
