#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:19:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180387 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/56/7205603.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_7205603
loop_
_publ_author_name
'Dobrzańska, Liliana'
_publ_section_title
;
 Anion directed supramolecular architectures of silver(i) complexes
 with 1,3-bis(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene and a
 reversible, solvent-induced structural change during a
 single-crystal-to-single-crystal transformation
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2303
_journal_paper_doi               10.1039/c0ce00469c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C34 H40 Ag2 N10 O6'
_chemical_formula_weight         900.50
_chemical_name_common            work
_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           SHELXL-97
_cell_angle_alpha                94.1750(10)
_cell_angle_beta                 93.6960(10)
_cell_angle_gamma                107.1430(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5514(7)
_cell_length_b                   9.6731(8)
_cell_length_c                   11.5283(9)
_cell_measurement_reflns_used    5821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.503
_cell_volume                     905.12(13)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10477
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.7187
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.470
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0611
_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)+(0.0780P)²+4.3632P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                3886
_reflns_number_total             4168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00469c.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7205603
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 0.41164(4) 0.45787(4) 0.21053(4) 0.03503(16) Uani 1 1 d . . .
N1 N 0.2223(5) 0.5538(4) 0.2237(4) 0.0270(8) Uani 1 1 d . A .
C2 C 0.2051(6) 0.6559(5) 0.3006(4) 0.0274(9) Uani 1 1 d . . .
H2 H 0.2816 0.7011 0.3656 0.033 Uiso 1 1 calc R A .
N3 N 0.0647(5) 0.6867(4) 0.2739(3) 0.0257(8) Uani 1 1 d . . .
C4 C -0.0126(6) 0.6001(5) 0.1744(4) 0.0274(9) Uani 1 1 d . . .
H4 H -0.1144 0.5979 0.1347 0.033 Uiso 1 1 calc R A .
C5 C 0.0861(6) 0.5184(5) 0.1441(4) 0.0274(9) Uani 1 1 d . A .
H5 H 0.0646 0.4481 0.0784 0.033 Uiso 1 1 calc R . .
C6 C 0.0022(6) 0.7973(5) 0.3341(4) 0.0303(10) Uani 1 1 d . . .
H6A H -0.1116 0.7501 0.3529 0.036 Uiso 1 1 calc R A .
H6B H -0.0017 0.8718 0.2805 0.036 Uiso 1 1 calc R . .
C7 C 0.1053(5) 0.8711(5) 0.4452(4) 0.0253(9) Uani 1 1 d . . .
C8 C 0.2340(6) 0.9992(5) 0.4414(4) 0.0260(9) Uani 1 1 d . . .
C9 C 0.3210(6) 1.0718(5) 0.5452(4) 0.0273(9) Uani 1 1 d . . .
H9 H 0.4088 1.1585 0.5429 0.033 Uiso 1 1 calc R . .
C10 C 0.2815(5) 1.0194(5) 0.6536(4) 0.0245(8) Uani 1 1 d . . .
C11 C 0.1557(5) 0.8890(5) 0.6556(4) 0.0250(8) Uani 1 1 d . . .
C12 C 0.0690(5) 0.8126(5) 0.5514(4) 0.0255(9) Uani 1 1 d . . .
C13 C -0.0630(6) 0.6693(5) 0.5547(5) 0.0342(10) Uani 1 1 d . . .
H13A H -0.1663 0.6876 0.5720 0.051 Uiso 1 1 calc R . .
H13B H -0.0297 0.6153 0.6154 0.051 Uiso 1 1 calc R . .
H13C H -0.0786 0.6123 0.4787 0.051 Uiso 1 1 calc R . .
C14 C 0.2819(7) 1.0620(6) 0.3283(4) 0.0344(10) Uani 1 1 d . . .
H14A H 0.2975 0.9864 0.2729 0.052 Uiso 1 1 calc R . .
H14B H 0.3845 1.1422 0.3430 0.052 Uiso 1 1 calc R . .
H14C H 0.1947 1.0984 0.2953 0.052 Uiso 1 1 calc R . .
C15 C 0.3746(6) 1.1061(5) 0.7637(4) 0.0309(10) Uani 1 1 d . . .
H15A H 0.4518 1.1965 0.7439 0.046 Uiso 1 1 calc R . .
H15B H 0.4354 1.0491 0.8035 0.046 Uiso 1 1 calc R . .
H15C H 0.2971 1.1292 0.8152 0.046 Uiso 1 1 calc R . .
C16 C 0.1148(6) 0.8336(5) 0.7729(4) 0.0270(9) Uani 1 1 d . . .
H16A H 0.1078 0.9148 0.8277 0.032 Uiso 1 1 calc R A .
H16B H 0.0060 0.7587 0.7636 0.032 Uiso 1 1 calc R . .
N17 N 0.2388(5) 0.7709(4) 0.8225(3) 0.0254(7) Uani 1 1 d . A .
C18 C 0.3203(6) 0.6946(5) 0.7635(4) 0.0278(9) Uani 1 1 d . . .
H18 H 0.3093 0.6747 0.6809 0.033 Uiso 1 1 calc R A .
N19 N 0.4188(5) 0.6502(5) 0.8358(4) 0.0315(9) Uani 1 1 d . . .
C20 C 0.3953(7) 0.7002(7) 0.9468(5) 0.0395(12) Uani 1 1 d . . .
H20 H 0.4491 0.6848 1.0172 0.047 Uiso 1 1 calc R A .
C21 C 0.2837(6) 0.7743(6) 0.9396(4) 0.0346(11) Uani 1 1 d . A .
H21 H 0.2444 0.8194 1.0026 0.042 Uiso 1 1 calc R . .
N22 N 0.5315(6) 0.5120(7) 0.4871(6) 0.028(2) Uani 0.50 1 d PDU A -2
O23 O 0.5629(13) 0.5803(8) 0.3953(7) 0.057(2) Uani 0.50 1 d PDU A -2
O24 O 0.4644(13) 0.5625(13) 0.5658(9) 0.077(4) Uani 0.50 1 d PDU A -2
O25 O 0.5696(9) 0.3987(7) 0.4933(8) 0.0402(17) Uani 0.50 1 d PD A -2
N26 N 0.0890(8) 0.1086(7) 0.0026(7) 0.0337(19) Uani 0.50 1 d PD B -1
O27 O 0.1876(6) 0.2324(5) 0.0169(4) 0.0111(9) Uani 0.50 1 d PDU B -1
O28 O 0.1054(12) 0.0073(11) 0.0590(7) 0.0414(18) Uani 0.50 1 d P B -1
O29 O -0.0272(10) 0.0835(9) -0.0745(6) 0.0354(15) Uani 0.50 1 d P B -1
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'
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
N19 Ag1 N1 169.00(16) 2_666 . ?
N19 Ag1 O23 96.2(3) 2_666 . ?
N1 Ag1 O23 94.6(3) . . ?
C2 N1 C5 106.2(4) . . ?
C2 N1 Ag1 131.0(3) . . ?
C5 N1 Ag1 122.8(3) . . ?
N1 C2 N3 110.7(4) . . ?
N1 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
C2 N3 C4 107.8(4) . . ?
C2 N3 C6 128.1(4) . . ?
C4 N3 C6 124.1(4) . . ?
C5 C4 N3 106.1(4) . . ?
C5 C4 H4 126.9 . . ?
N3 C4 H4 126.9 . . ?
C4 C5 N1 109.2(4) . . ?
C4 C5 H5 125.4 . . ?
N1 C5 H5 125.4 . . ?
N3 C6 C7 113.3(4) . . ?
N3 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
N3 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C12 120.7(4) . . ?
C8 C7 C6 119.6(4) . . ?
C12 C7 C6 119.7(4) . . ?
C9 C8 C7 119.1(4) . . ?
C9 C8 C14 118.6(4) . . ?
C7 C8 C14 122.3(4) . . ?
C8 C9 C10 121.3(4) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 118.9(4) . . ?
C11 C10 C15 122.1(4) . . ?
C9 C10 C15 119.0(4) . . ?
C10 C11 C12 120.6(4) . . ?
C10 C11 C16 118.3(4) . . ?
C12 C11 C16 121.1(4) . . ?
C7 C12 C11 119.3(4) . . ?
C7 C12 C13 120.7(4) . . ?
C11 C12 C13 120.0(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N17 C16 C11 111.9(4) . . ?
N17 C16 H16A 109.2 . . ?
C11 C16 H16A 109.2 . . ?
N17 C16 H16B 109.2 . . ?
C11 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 N17 C21 108.0(4) . . ?
C18 N17 C16 126.6(4) . . ?
C21 N17 C16 125.2(4) . . ?
N19 C18 N17 110.8(4) . . ?
N19 C18 H18 124.6 . . ?
N17 C18 H18 124.6 . . ?
C18 N19 C20 105.7(4) . . ?
C18 N19 Ag1 126.8(3) . 2_666 ?
C20 N19 Ag1 127.3(3) . 2_666 ?
C21 C20 N19 109.5(5) . . ?
C21 C20 H20 125.3 . . ?
N19 C20 H20 125.3 . . ?
C20 C21 N17 106.0(4) . . ?
C20 C21 H21 127.0 . . ?
N17 C21 H21 127.0 . . ?
O25 N22 O24 122.7(7) . . ?
O25 N22 O23 118.3(7) . . ?
O24 N22 O23 119.0(8) . . ?
N22 O23 Ag1 116.9(4) . . ?
O27 N26 O29 118.1(8) . . ?
O27 N26 O28 122.7(8) . . ?
O29 N26 O28 119.2(7) . . ?
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 N19 2.096(4) 2_666 ?
Ag1 N1 2.098(4) . ?
Ag1 O23 2.447(8) . ?
N1 C2 1.326(6) . ?
N1 C5 1.377(6) . ?
C2 N3 1.342(6) . ?
C2 H2 0.9500 . ?
N3 C4 1.375(6) . ?
N3 C6 1.479(6) . ?
C4 C5 1.361(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.509(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.400(7) . ?
C7 C12 1.400(7) . ?
C8 C9 1.391(7) . ?
C8 C14 1.508(6) . ?
C9 C10 1.407(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(6) . ?
C10 C15 1.507(6) . ?
C11 C12 1.404(7) . ?
C11 C16 1.514(6) . ?
C12 C13 1.513(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N17 1.474(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
N17 C18 1.336(6) . ?
N17 C21 1.375(6) . ?
C18 N19 1.328(6) . ?
C18 H18 0.9500 . ?
N19 C20 1.383(7) . ?
N19 Ag1 2.096(4) 2_666 ?
C20 C21 1.354(7) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
N22 O25 1.238(5) . ?
N22 O24 1.249(5) . ?
N22 O23 1.289(10) . ?
N26 O27 1.237(5) . ?
N26 O29 1.245(11) . ?
N26 O28 1.251(11) . ?
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
N19 Ag1 N1 C2 -161.6(7) 2_666 . . . ?
O23 Ag1 N1 C2 6.1(5) . . . . ?
N19 Ag1 N1 C5 16.7(10) 2_666 . . . ?
O23 Ag1 N1 C5 -175.6(4) . . . . ?
C5 N1 C2 N3 0.2(5) . . . . ?
Ag1 N1 C2 N3 178.7(3) . . . . ?
N1 C2 N3 C4 -0.2(6) . . . . ?
N1 C2 N3 C6 -177.5(4) . . . . ?
C2 N3 C4 C5 0.1(5) . . . . ?
C6 N3 C4 C5 177.5(4) . . . . ?
N3 C4 C5 N1 0.1(5) . . . . ?
C2 N1 C5 C4 -0.2(5) . . . . ?
Ag1 N1 C5 C4 -178.8(3) . . . . ?
C2 N3 C6 C7 -6.4(7) . . . . ?
C4 N3 C6 C7 176.7(4) . . . . ?
N3 C6 C7 C8 91.4(5) . . . . ?
N3 C6 C7 C12 -90.1(5) . . . . ?
C12 C7 C8 C9 -2.9(6) . . . . ?
C6 C7 C8 C9 175.6(4) . . . . ?
C12 C7 C8 C14 177.2(4) . . . . ?
C6 C7 C8 C14 -4.3(6) . . . . ?
C7 C8 C9 C10 -0.3(7) . . . . ?
C14 C8 C9 C10 179.5(4) . . . . ?
C8 C9 C10 C11 2.2(7) . . . . ?
C8 C9 C10 C15 -177.2(4) . . . . ?
C9 C10 C11 C12 -0.8(6) . . . . ?
C15 C10 C11 C12 178.6(4) . . . . ?
C9 C10 C11 C16 179.9(4) . . . . ?
C15 C10 C11 C16 -0.8(6) . . . . ?
C8 C7 C12 C11 4.3(6) . . . . ?
C6 C7 C12 C11 -174.2(4) . . . . ?
C8 C7 C12 C13 -176.2(4) . . . . ?
C6 C7 C12 C13 5.3(6) . . . . ?
C10 C11 C12 C7 -2.4(6) . . . . ?
C16 C11 C12 C7 176.9(4) . . . . ?
C10 C11 C12 C13 178.1(4) . . . . ?
C16 C11 C12 C13 -2.6(6) . . . . ?
C10 C11 C16 N17 -75.1(5) . . . . ?
C12 C11 C16 N17 105.6(5) . . . . ?
C11 C16 N17 C18 -36.2(6) . . . . ?
C11 C16 N17 C21 147.9(5) . . . . ?
C21 N17 C18 N19 -1.3(6) . . . . ?
C16 N17 C18 N19 -177.8(4) . . . . ?
N17 C18 N19 C20 1.0(6) . . . . ?
N17 C18 N19 Ag1 -174.5(3) . . . 2_666 ?
C18 N19 C20 C21 -0.3(6) . . . . ?
Ag1 N19 C20 C21 175.1(4) 2_666 . . . ?
N19 C20 C21 N17 -0.5(7) . . . . ?
C18 N17 C21 C20 1.1(6) . . . . ?
C16 N17 C21 C20 177.7(5) . . . . ?
O25 N22 O23 Ag1 66.3(7) . . . . ?
O24 N22 O23 Ag1 -113.9(7) . . . . ?
N19 Ag1 O23 N22 -89.6(7) 2_666 . . . ?
N1 Ag1 O23 N22 92.7(7) . . . . ?
