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#$Date: 2016-03-25 09:58:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179736 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/32/7003226.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_7003226
loop_
_publ_author_name
'Huang, Yong-Qing'
'Shen, Zhong-Liang'
'Okamura, Taka-aki'
'Wang, Yan'
'Wang, Xiao-Feng'
'Sun, Wei-Yin'
'Yu, Jin-Quan'
'Ueyama, Norikazu'
_publ_section_title
;
 Silver(i) complexes with oxazoline-containing tripodal ligands:
 structure variation via counter anions and reaction conditions
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              204
_journal_page_last               213
_journal_paper_doi               10.1039/b714502k
_journal_year                    2008
_chemical_formula_moiety         'C36 H39 Ag3 Cl3 N9 O18'
_chemical_formula_sum            'C36 H39 Ag3 Cl3 N9 O18'
_chemical_formula_weight         1315.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.013(2)
_cell_length_b                   24.013(2)
_cell_length_c                   14.319(2)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.94
_cell_volume                     7150.5(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13663
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  0.9170
_exptl_absorpt_correction_T_min  0.5389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0769
_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)+(0.0942P)²+29.5321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.1916
_reflns_number_gt                3003
_reflns_number_total             3425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714502k.txt
_cod_data_source_block           7
_cod_original_cell_volume        7150.5(12)
_cod_original_sg_symbol_H-M      R3C
_cod_database_code               7003226
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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 0.81556(4) 0.96362(4) -0.09415(8) 0.0595(3) Uani 1 1 d . . .
Cl1 Cl 0.71031(12) 0.83339(12) -0.2540(2) 0.0595(6) Uani 1 1 d . . .
O1 O 0.8627(4) 0.8420(4) 0.0776(7) 0.066(2) Uani 1 1 d . . .
O2 O 0.9604(4) 1.1253(4) -0.2569(8) 0.077(3) Uani 1 1 d . . .
O3 O 0.6629(8) 0.8259(8) -0.3139(11) 0.135(5) Uiso 1 1 d . . .
O4 O 0.7055(9) 0.8677(9) -0.1774(16) 0.165(6) Uiso 1 1 d . . .
O5 O 0.7053(6) 0.7761(7) -0.2170(9) 0.114(4) Uiso 1 1 d . . .
O6 O 0.7703(10) 0.8847(10) -0.2709(16) 0.184(8) Uiso 1 1 d . . .
N1 N 0.8231(4) 0.8926(4) -0.0082(6) 0.0496(18) Uani 1 1 d . . .
N2 N 0.8755(4) 1.0483(4) -0.1823(7) 0.0529(19) Uani 1 1 d . . .
N3 N 0.7420(9) 0.9877(8) -0.0296(11) 0.106(4) Uani 1 1 d . . .
C1 C 0.9489(4) 1.0124(5) 0.0356(6) 0.046(2) Uani 1 1 d . . .
H1A H 0.9149 1.0203 0.0415 0.056 Uiso 1 1 calc R . .
C2 C 0.9369(4) 0.9483(5) 0.0311(6) 0.045(2) Uani 1 1 d . . .
C3 C 0.8710(5) 0.8934(4) 0.0315(7) 0.046(2) Uani 1 1 d . . .
C4 C 0.7674(6) 0.8269(5) 0.0103(9) 0.066(3) Uani 1 1 d . . .
H4A H 0.7326 0.8295 0.0403 0.079 Uiso 1 1 calc R . .
H4B H 0.7516 0.8028 -0.0474 0.079 Uiso 1 1 calc R . .
C5 C 0.7934(6) 0.7966(7) 0.0723(16) 0.099(5) Uani 1 1 d . . .
H5A H 0.7851 0.7557 0.0470 0.118 Uiso 1 1 calc R . .
H5B H 0.7740 0.7894 0.1338 0.118 Uiso 1 1 calc R . .
C6 C 0.9334(4) 0.9657(4) -0.2218(6) 0.0366(16) Uani 1 1 d . . .
H6A H 0.8888 0.9426 -0.2258 0.044 Uiso 1 1 calc R . .
C7 C 0.9656(4) 1.0316(4) -0.2188(5) 0.0345(16) Uani 1 1 d . . .
C8 C 0.9305(4) 1.0680(5) -0.2173(7) 0.045(2) Uani 1 1 d . . .
C9 C 0.8609(6) 1.1008(5) -0.1961(11) 0.071(3) Uani 1 1 d . . .
H9A H 0.8540 1.1158 -0.1367 0.086 Uiso 1 1 calc R . .
H9B H 0.8228 1.0864 -0.2345 0.086 Uiso 1 1 calc R . .
C10 C 0.9187(6) 1.1525(7) -0.2441(12) 0.080 Uani 1 1 d . . .
H10A H 0.9072 1.1631 -0.3038 0.096 Uiso 1 1 calc R . .
H10B H 0.9395 1.1910 -0.2059 0.096 Uiso 1 1 calc R . .
C11 C 0.7165(7) 1.0017(7) 0.0293(11) 0.077(3) Uani 1 1 d . . .
C12 C 0.6855(6) 1.0160(7) 0.1001(10) 0.072(3) Uani 1 1 d . . .
H12A H 0.6424 1.0029 0.0810 0.108 Uiso 1 1 calc R . .
H12B H 0.7085 1.0614 0.1119 0.108 Uiso 1 1 calc R . .
H12C H 0.6845 0.9934 0.1560 0.108 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
N1 Ag1 N2 140.4(3) . . ?
N1 Ag1 N3 110.1(4) . . ?
N2 Ag1 N3 103.1(4) . . ?
O3 Cl1 O6 116.1(11) . . ?
O3 Cl1 O4 104.9(11) . . ?
O6 Cl1 O4 88.2(12) . . ?
O3 Cl1 O5 116.5(9) . . ?
O6 Cl1 O5 118.6(11) . . ?
O4 Cl1 O5 106.6(10) . . ?
C3 O1 C5 104.7(9) . . ?
C8 O2 C10 106.1(9) . . ?
C3 N1 C4 105.1(8) . . ?
C3 N1 Ag1 131.8(6) . . ?
C4 N1 Ag1 123.0(7) . . ?
C8 N2 C9 106.0(9) . . ?
C8 N2 Ag1 130.6(7) . . ?
C9 N2 Ag1 122.5(8) . . ?
C11 N3 Ag1 157.6(14) . . ?
C2 C1 C2 119.7(9) 3_675 . ?
C2 C1 H1A 120.1 3_675 . ?
C2 C1 H1A 120.1 . . ?
C1 C2 C1 119.9(9) 2_765 . ?
C1 C2 C3 118.7(9) 2_765 . ?
C1 C2 C3 121.1(8) . . ?
N1 C3 O1 119.6(8) . . ?
N1 C3 C2 124.8(9) . . ?
O1 C3 C2 115.6(9) . . ?
C5 C4 N1 104.6(10) . . ?
C5 C4 H4A 110.8 . . ?
N1 C4 H4A 110.8 . . ?
C5 C4 H4B 110.8 . . ?
N1 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C4 C5 O1 105.6(10) . . ?
C4 C5 H5A 110.6 . . ?
O1 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
O1 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
C7 C6 C7 119.1(8) . 2_765 ?
C7 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 2_765 . ?
C6 C7 C6 120.7(8) . 3_675 ?
C6 C7 C8 121.4(8) . . ?
C6 C7 C8 117.8(7) 3_675 . ?
N2 C8 O2 118.8(8) . . ?
N2 C8 C7 125.3(9) . . ?
O2 C8 C7 115.8(8) . . ?
N2 C9 C10 104.7(9) . . ?
N2 C9 H9A 110.8 . . ?
C10 C9 H9A 110.8 . . ?
N2 C9 H9B 110.8 . . ?
C10 C9 H9B 110.8 . . ?
H9A C9 H9B 108.9 . . ?
O2 C10 C9 104.3(9) . . ?
O2 C10 H10A 110.9 . . ?
C9 C10 H10A 110.9 . . ?
O2 C10 H10B 110.9 . . ?
C9 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
N3 C11 C12 178.0(16) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 N1 2.183(8) . ?
Ag1 N2 2.207(9) . ?
Ag1 N3 2.308(15) . ?
Cl1 O3 1.365(16) . ?
Cl1 O6 1.37(2) . ?
Cl1 O4 1.41(2) . ?
Cl1 O5 1.421(15) . ?
O1 C3 1.324(13) . ?
O1 C5 1.465(15) . ?
O2 C8 1.319(13) . ?
O2 C10 1.454(14) . ?
N1 C3 1.274(13) . ?
N1 C4 1.496(13) . ?
N2 C8 1.263(13) . ?
N2 C9 1.481(12) . ?
N3 C11 1.19(2) . ?
C1 C2 1.382(14) 3_675 ?
C1 C2 1.420(14) . ?
C1 H1A 0.9300 . ?
C2 C1 1.382(14) 2_765 ?
C2 C3 1.467(14) . ?
C4 C5 1.47(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.372(12) . ?
C6 C7 1.388(12) 2_765 ?
C6 H6A 0.9300 . ?
C7 C6 1.388(12) 3_675 ?
C7 C8 1.487(11) . ?
C9 C10 1.489(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.40(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ag1 N1 C3 21.8(12) . . . . ?
N3 Ag1 N1 C3 -123.4(10) . . . . ?
N2 Ag1 N1 C4 -154.1(7) . . . . ?
N3 Ag1 N1 C4 60.7(9) . . . . ?
N1 Ag1 N2 C8 15.9(12) . . . . ?
N3 Ag1 N2 C8 162.5(10) . . . . ?
N1 Ag1 N2 C9 -151.9(8) . . . . ?
N3 Ag1 N2 C9 -5.3(10) . . . . ?
N1 Ag1 N3 C11 48(4) . . . . ?
N2 Ag1 N3 C11 -110(4) . . . . ?
C2 C1 C2 C1 9.1(18) 3_675 . . 2_765 ?
C2 C1 C2 C3 -177.3(6) 3_675 . . . ?
C4 N1 C3 O1 -1.0(13) . . . . ?
Ag1 N1 C3 O1 -177.4(7) . . . . ?
C4 N1 C3 C2 179.2(9) . . . . ?
Ag1 N1 C3 C2 2.8(15) . . . . ?
C5 O1 C3 N1 -3.3(16) . . . . ?
C5 O1 C3 C2 176.6(11) . . . . ?
C1 C2 C3 N1 -150.0(10) 2_765 . . . ?
C1 C2 C3 N1 36.3(14) . . . . ?
C1 C2 C3 O1 30.2(13) 2_765 . . . ?
C1 C2 C3 O1 -143.5(9) . . . . ?
C3 N1 C4 C5 4.8(14) . . . . ?
Ag1 N1 C4 C5 -178.4(11) . . . . ?
N1 C4 C5 O1 -6.5(17) . . . . ?
C3 O1 C5 C4 6.0(17) . . . . ?
C7 C6 C7 C6 6.2(16) 2_765 . . 3_675 ?
C7 C6 C7 C8 -177.1(6) 2_765 . . . ?
C9 N2 C8 O2 -1.1(14) . . . . ?
Ag1 N2 C8 O2 -170.5(8) . . . . ?
C9 N2 C8 C7 179.3(9) . . . . ?
Ag1 N2 C8 C7 9.9(15) . . . . ?
C10 O2 C8 N2 2.5(15) . . . . ?
C10 O2 C8 C7 -177.9(10) . . . . ?
C6 C7 C8 N2 30.1(14) . . . . ?
C6 C7 C8 N2 -153.1(9) 3_675 . . . ?
C6 C7 C8 O2 -149.5(9) . . . . ?
C6 C7 C8 O2 27.3(12) 3_675 . . . ?
C8 N2 C9 C10 -0.7(14) . . . . ?
Ag1 N2 C9 C10 169.7(9) . . . . ?
C8 O2 C10 C9 -2.5(15) . . . . ?
N2 C9 C10 O2 1.9(15) . . . . ?
Ag1 N3 C11 C12 -71(48) . . . . ?
