#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305216.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_4305216
loop_
_publ_author_name
'Jie-Sheng Huang'
'Jin Xie'
'Steven C. F. Kui'
'Guo-Su Fang'
'Nianyong Zhu'
'Chi-Ming Che'
_publ_section_title
;
Self-Assembly of a Cyclic Metalladecapyridine from the Reaction of
2,6-Bis(bis(2-pyridyl)methoxymethane)pyridine with Silver(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5727
_journal_page_last               5735
_journal_paper_doi               10.1021/ic8000043
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H40 Ag1 S1'
_chemical_formula_sum            'C74 H72 Ag2 N10 O12 S2'
_chemical_formula_weight         1573.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-02-08T10:59:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                118.08(3)
_cell_angle_beta                 98.90(3)
_cell_angle_gamma                91.28(3)
_cell_formula_units_Z            1
_cell_length_a                   11.922(2)
_cell_length_b                   12.941(3)
_cell_length_c                   12.986(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1736.0(8)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9095
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                4479
_reflns_number_total             5636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8000043-file002.cif
_cod_data_source_block           Complex1_2MeOH
_cod_original_cell_volume        1736.0(6)
_cod_database_code               4305216
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
Ag1 Ag 0.548766(19) 0.34470(2) -0.093471(19) 0.03834(10) Uani 1 1 d . . .
O1 O 0.89639(16) 0.42204(17) 0.17604(16) 0.0336(4) Uani 1 1 d . . .
O2 O 0.77810(17) 0.81955(17) 0.40500(18) 0.0385(5) Uani 1 1 d . . .
N1 N 0.7402(2) 0.2711(2) -0.1262(2) 0.0393(6) Uani 1 1 d . . .
N2 N 0.5943(2) 0.3394(2) 0.0773(2) 0.0315(5) Uani 1 1 d . . .
N3 N 0.73062(19) 0.58547(19) 0.18025(19) 0.0270(5) Uani 1 1 d . . .
N4 N 0.5506(2) 0.8610(2) 0.2118(2) 0.0400(6) Uani 1 1 d . . .
N5 N 0.5046(2) 0.6467(2) 0.26190(19) 0.0305(5) Uani 1 1 d . . .
C1 C 0.7493(3) 0.1762(3) -0.2287(3) 0.0538(9) Uani 1 1 d . . .
H1 H 0.7008 0.1636 -0.2978 0.065 Uiso 1 1 calc R . .
C2 C 0.8260(4) 0.0970(4) -0.2368(3) 0.0701(12) Uani 1 1 d . . .
H2 H 0.8302 0.0326 -0.3096 0.084 Uiso 1 1 calc R . .
C3 C 0.8956(4) 0.1152(4) -0.1358(4) 0.0847(15) Uani 1 1 d . . .
H3 H 0.9482 0.0625 -0.1383 0.102 Uiso 1 1 calc R . .
C4 C 0.8885(3) 0.2127(3) -0.0286(3) 0.0577(10) Uani 1 1 d . . .
H4 H 0.9362 0.2263 0.0414 0.069 Uiso 1 1 calc R . .
C5 C 0.8095(2) 0.2888(2) -0.0277(2) 0.0311(6) Uani 1 1 d . . .
C6 C 0.7945(2) 0.3945(2) 0.0894(2) 0.0280(6) Uani 1 1 d . . .
C7 C 0.7011(2) 0.3588(2) 0.1386(2) 0.0266(6) Uani 1 1 d . . .
C8 C 0.7256(3) 0.3435(3) 0.2374(3) 0.0381(7) Uani 1 1 d . . .
H8 H 0.8005 0.357 0.2778 0.046 Uiso 1 1 calc R . .
C9 C 0.6384(3) 0.3080(3) 0.2760(3) 0.0475(8) Uani 1 1 d . . .
H9 H 0.6536 0.2977 0.3429 0.057 Uiso 1 1 calc R . .
C10 C 0.5271(3) 0.2876(3) 0.2133(3) 0.0441(8) Uani 1 1 d . . .
H10 H 0.4666 0.2636 0.2373 0.053 Uiso 1 1 calc R . .
C11 C 0.5088(3) 0.3040(3) 0.1150(3) 0.0390(7) Uani 1 1 d . . .
H11 H 0.4347 0.2901 0.0727 0.047 Uiso 1 1 calc R . .
C12 C 0.7681(2) 0.5074(2) 0.0839(2) 0.0264(6) Uani 1 1 d . . .
C13 C 0.7924(2) 0.5339(3) -0.0027(3) 0.0343(7) Uani 1 1 d . . .
H13 H 0.8161 0.4772 -0.07 0.041 Uiso 1 1 calc R . .
C14 C 0.7806(3) 0.6456(3) 0.0130(3) 0.0382(7) Uani 1 1 d . . .
H14 H 0.7983 0.6661 -0.0428 0.046 Uiso 1 1 calc R . .
C15 C 0.7423(2) 0.7270(3) 0.1121(3) 0.0361(7) Uani 1 1 d . . .
H15 H 0.734 0.8031 0.1244 0.043 Uiso 1 1 calc R . .
C16 C 0.7163(2) 0.6932(2) 0.1930(2) 0.0279(6) Uani 1 1 d . . .
C17 C 0.6806(2) 0.7756(2) 0.3107(2) 0.0288(6) Uani 1 1 d . . .
C18 C 0.6193(2) 0.8796(2) 0.3119(3) 0.0317(6) Uani 1 1 d . . .
C19 C 0.6290(3) 0.9855(3) 0.4171(3) 0.0434(8) Uani 1 1 d . . .
H19 H 0.6776 0.9964 0.4855 0.052 Uiso 1 1 calc R . .
C20 C 0.5657(3) 1.0739(3) 0.4187(3) 0.0516(9) Uani 1 1 d . . .
H20 H 0.571 1.1452 0.4882 0.062 Uiso 1 1 calc R . .
C21 C 0.4943(3) 1.0553(3) 0.3158(3) 0.0513(9) Uani 1 1 d . . .
H21 H 0.4505 1.1133 0.3142 0.062 Uiso 1 1 calc R . .
C22 C 0.4900(3) 0.9492(3) 0.2164(3) 0.0480(8) Uani 1 1 d . . .
H22 H 0.4419 0.9369 0.1471 0.058 Uiso 1 1 calc R . .
C23 C 0.6002(2) 0.7052(2) 0.3417(2) 0.0266(6) Uani 1 1 d . . .
C24 C 0.6249(3) 0.7039(2) 0.4488(2) 0.0335(7) Uani 1 1 d . . .
H24 H 0.6909 0.7459 0.5036 0.04 Uiso 1 1 calc R . .
C25 C 0.5489(3) 0.6384(3) 0.4729(3) 0.0393(7) Uani 1 1 d . . .
H25 H 0.5642 0.6348 0.5435 0.047 Uiso 1 1 calc R . .
C26 C 0.4508(3) 0.5791(3) 0.3910(3) 0.0396(7) Uani 1 1 d . . .
H26 H 0.3985 0.5354 0.4055 0.048 Uiso 1 1 calc R . .
C27 C 0.4322(3) 0.5858(3) 0.2879(3) 0.0361(7) Uani 1 1 d . . .
H27 H 0.3657 0.5459 0.2328 0.043 Uiso 1 1 calc R . .
S1 S 1.19138(7) 0.26455(7) 0.24399(7) 0.03990(19) Uani 1 1 d . . .
O3 O 1.13135(19) 0.2039(2) 0.12126(19) 0.0546(6) Uani 1 1 d . . .
O4 O 1.27763(19) 0.1988(2) 0.26880(19) 0.0542(6) Uani 1 1 d . . .
O5 O 1.2340(2) 0.3850(2) 0.2822(2) 0.0656(7) Uani 1 1 d . . .
C28 C 1.0870(2) 0.2718(3) 0.3307(3) 0.0349(7) Uani 1 1 d . . .
C29 C 0.9940(3) 0.1879(3) 0.2842(3) 0.0415(7) Uani 1 1 d . . .
H29 H 0.9836 0.1285 0.2056 0.05 Uiso 1 1 calc R . .
C30 C 0.9159(3) 0.1917(3) 0.3543(3) 0.0476(8) Uani 1 1 d . . .
H30 H 0.8536 0.1344 0.3222 0.057 Uiso 1 1 calc R . .
C31 C 0.9289(3) 0.2785(3) 0.4704(3) 0.0482(8) Uani 1 1 d . . .
C32 C 1.0219(3) 0.3619(3) 0.5152(3) 0.0601(10) Uani 1 1 d . . .
H32 H 1.032 0.4217 0.5935 0.072 Uiso 1 1 calc R . .
C33 C 1.1011(3) 0.3590(3) 0.4460(3) 0.0518(9) Uani 1 1 d . . .
H33 H 1.1635 0.4162 0.4781 0.062 Uiso 1 1 calc R . .
C34 C 0.8427(4) 0.2830(4) 0.5469(4) 0.0807(13) Uani 1 1 d . . .
H34A H 0.7847 0.2174 0.5017 0.121 Uiso 1 1 calc R . .
H34B H 0.8083 0.3552 0.5716 0.121 Uiso 1 1 calc R . .
H34C H 0.8808 0.2791 0.6156 0.121 Uiso 1 1 calc R . .
C35 C 1.2994(5) -0.0080(4) -0.0357(5) 0.0964(16) Uani 1 1 d . . .
C38 C 0.9921(3) 0.4731(3) 0.1565(3) 0.0462(8) Uani 1 1 d . . .
H38A H 1.0566 0.4887 0.2181 0.069 Uiso 1 1 calc R . .
H38B H 0.9746 0.5456 0.1575 0.069 Uiso 1 1 calc R . .
H38C H 1.01 0.4196 0.0808 0.069 Uiso 1 1 calc R . .
C48 C 0.8732(3) 0.8721(3) 0.3891(4) 0.0622(10) Uani 1 1 d . . .
H48A H 0.933 0.8979 0.4575 0.093 Uiso 1 1 calc R . .
H48B H 0.8522 0.9385 0.3792 0.093 Uiso 1 1 calc R . .
H48C H 0.8997 0.8158 0.3198 0.093 Uiso 1 1 calc R . .
O6 O 1.2110(3) 0.0427(3) -0.0720(3) 0.0960(11) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
C C 0.0033 0.0016 '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'
H H 0 0 '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
_geom_angle_publ_flag
N2 Ag1 N5 177.28(8) . 2_665 ?
N2 Ag1 N4 95.88(9) . 2_665 ?
N5 Ag1 N4 84.13(9) 2_665 2_665 ?
N2 Ag1 N1 83.77(8) . . ?
N5 Ag1 N1 98.95(8) 2_665 . ?
N4 Ag1 N1 91.45(9) 2_665 . ?
C38 O1 C6 114.7(2) . . ?
C48 O2 C17 116.9(2) . . ?
C5 N1 C1 118.1(3) . . ?
C5 N1 Ag1 113.91(17) . . ?
C1 N1 Ag1 119.9(2) . . ?
C7 N2 C11 118.3(2) . . ?
C7 N2 Ag1 124.50(18) . . ?
C11 N2 Ag1 116.97(19) . . ?
C12 N3 C16 118.4(2) . . ?
C18 N4 C22 117.2(3) . . ?
C18 N4 Ag1 113.19(17) . 2_665 ?
C22 N4 Ag1 117.3(2) . 2_665 ?
C27 N5 C23 118.3(2) . . ?
C27 N5 Ag1 117.32(19) . 2_665 ?
C23 N5 Ag1 124.22(17) . 2_665 ?
N1 C1 C2 123.6(3) . . ?
C3 C2 C1 117.9(3) . . ?
C2 C3 C4 119.9(3) . . ?
C5 C4 C3 118.7(3) . . ?
N1 C5 C4 121.8(3) . . ?
N1 C5 C6 117.5(2) . . ?
C4 C5 C6 120.6(3) . . ?
O1 C6 C7 105.00(19) . . ?
O1 C6 C12 107.9(2) . . ?
C7 C6 C12 109.2(2) . . ?
O1 C6 C5 108.9(2) . . ?
C7 C6 C5 109.2(2) . . ?
C12 C6 C5 116.1(2) . . ?
N2 C7 C8 122.1(3) . . ?
N2 C7 C6 115.9(2) . . ?
C8 C7 C6 121.9(2) . . ?
C7 C8 C9 119.5(3) . . ?
C8 C9 C10 119.0(3) . . ?
C11 C10 C9 118.4(3) . . ?
N2 C11 C10 122.7(3) . . ?
N3 C12 C13 122.4(2) . . ?
N3 C12 C6 112.3(2) . . ?
C13 C12 C6 124.9(2) . . ?
C14 C13 C12 118.7(3) . . ?
C13 C14 C15 119.4(3) . . ?
C14 C15 C16 118.6(3) . . ?
N3 C16 C15 122.4(2) . . ?
N3 C16 C17 112.8(2) . . ?
C15 C16 C17 124.6(2) . . ?
O2 C17 C23 105.3(2) . . ?
O2 C17 C16 109.8(2) . . ?
C23 C17 C16 109.3(2) . . ?
O2 C17 C18 109.5(2) . . ?
C23 C17 C18 107.5(2) . . ?
C16 C17 C18 115.0(2) . . ?
N4 C18 C19 122.0(3) . . ?
N4 C18 C17 117.6(2) . . ?
C19 C18 C17 120.1(3) . . ?
C20 C19 C18 119.3(3) . . ?
C19 C20 C21 119.1(3) . . ?
C22 C21 C20 118.0(3) . . ?
N4 C22 C21 124.4(3) . . ?
N5 C23 C24 121.9(3) . . ?
N5 C23 C17 117.3(2) . . ?
C24 C23 C17 120.8(3) . . ?
C23 C24 C25 118.6(3) . . ?
C26 C25 C24 119.3(3) . . ?
C27 C26 C25 118.4(3) . . ?
N5 C27 C26 123.5(3) . . ?
O4 S1 O5 112.92(17) . . ?
O4 S1 O3 112.64(14) . . ?
O5 S1 O3 112.69(16) . . ?
O4 S1 C28 105.91(13) . . ?
O5 S1 C28 106.39(15) . . ?
O3 S1 C28 105.55(14) . . ?
C33 C28 C29 119.4(3) . . ?
C33 C28 S1 119.8(2) . . ?
C29 C28 S1 120.7(2) . . ?
C28 C29 C30 120.1(3) . . ?
C31 C30 C29 121.2(3) . . ?
C30 C31 C32 117.9(3) . . ?
C30 C31 C34 121.1(3) . . ?
C32 C31 C34 121.0(3) . . ?
C31 C32 C33 121.5(3) . . ?
C28 C33 C32 119.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N2 2.234(2) . ?
Ag1 N5 2.236(2) 2_665 ?
Ag1 N4 2.509(3) 2_665 ?
Ag1 N1 2.512(2) . ?
O1 C38 1.420(3) . ?
O1 C6 1.431(3) . ?
O2 C48 1.400(4) . ?
O2 C17 1.431(3) . ?
N1 C5 1.326(4) . ?
N1 C1 1.343(4) . ?
N2 C7 1.342(3) . ?
N2 C11 1.354(4) . ?
N3 C12 1.338(3) . ?
N3 C16 1.343(3) . ?
N4 C18 1.335(4) . ?
N4 C22 1.347(4) . ?
N4 Ag1 2.509(3) 2_665 ?
N5 C27 1.338(4) . ?
N5 C23 1.343(4) . ?
N5 Ag1 2.236(2) 2_665 ?
C1 C2 1.366(5) . ?
C2 C3 1.352(5) . ?
C3 C4 1.388(5) . ?
C4 C5 1.376(4) . ?
C5 C6 1.534(4) . ?
C6 C7 1.529(4) . ?
C6 C12 1.534(4) . ?
C7 C8 1.378(4) . ?
C8 C9 1.379(4) . ?
C9 C10 1.393(5) . ?
C10 C11 1.375(4) . ?
C12 C13 1.386(4) . ?
C13 C14 1.376(4) . ?
C14 C15 1.379(4) . ?
C15 C16 1.385(4) . ?
C16 C17 1.530(4) . ?
C17 C23 1.529(4) . ?
C17 C18 1.541(4) . ?
C18 C19 1.392(4) . ?
C19 C20 1.379(4) . ?
C20 C21 1.380(5) . ?
C21 C22 1.365(5) . ?
C23 C24 1.384(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.376(4) . ?
C26 C27 1.367(4) . ?
S1 O4 1.442(2) . ?
S1 O5 1.447(3) . ?
S1 O3 1.454(2) . ?
S1 C28 1.778(3) . ?
C28 C33 1.366(4) . ?
C28 C29 1.377(4) . ?
C29 C30 1.386(4) . ?
C30 C31 1.373(5) . ?
C31 C32 1.374(5) . ?
C31 C34 1.519(5) . ?
C32 C33 1.390(5) . ?
C35 O6 1.390(6) . ?
