#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/43/4324362.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_4324362
loop_
_publ_author_name
'Kelly J. Kilpin'
'Martin L. Gower'
'Shane G. Telfer'
'Geoffrey B. Jameson'
'James D. Crowley'
_publ_section_title
;
 Toward the Self-Assembly of Metal-Organic Nanotubes Using Metal-Metal and
 π-Stacking Interactions: Bis(pyridylethynyl) Silver(I)
 Metallo-macrocycles and Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1123
_journal_page_last               1134
_journal_paper_doi               10.1021/ic1020059
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '[C20 H12 Ag N2] [Cl O4] 1.5[H2 O]'
_chemical_formula_sum            'C20 H15 Ag Cl N2 O5.5'
_chemical_formula_weight         514.66
_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                112.223(1)
_cell_angle_beta                 102.814(1)
_cell_angle_gamma                106.508(1)
_cell_formula_units_Z            2
_cell_length_a                   9.920(1)
_cell_length_b                   10.875(1)
_cell_length_c                   11.678(1)
_cell_measurement_reflns_used    6889
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.974
_cell_measurement_theta_min      3.067
_cell_volume                     1038.38(17)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21794
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.8758
_exptl_absorpt_correction_T_min  0.4489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2004/1 (Bruker,2004) was used for absorption correction.
_exptl_special_details 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       Needle
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0350
_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)+(0.0571P)²+1.8189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                3528
_reflns_number_total             3745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1020059_si_002_1.cif
_cod_data_source_block           mg13
_cod_original_cell_volume        1038.4(4)
_cod_original_formula_sum        'C20 H15 Ag Cl N2 O5.50'
_cod_database_code               4324362
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
Ag1 Ag 0.84976(3) 0.96456(3) 0.88975(3) 0.03180(12) Uani 1 1 d .
N1 N 0.9809(3) 1.1289(3) 0.8521(3) 0.0261(6) Uani 1 1 d .
N2 N 0.7035(3) 0.7805(3) 0.8952(3) 0.0259(6) Uani 1 1 d .
C1 C 0.9748(4) 1.2587(4) 0.8945(3) 0.0282(7) Uani 1 1 d .
H1 H 0.9263 1.2846 0.9559 0.034 Uiso 1 1 calc R
C2 C 1.0357(4) 1.3567(4) 0.8533(4) 0.0319(8) Uani 1 1 d .
H2 H 1.0295 1.4484 0.8863 0.038 Uiso 1 1 calc R
C3 C 1.1058(4) 1.3209(4) 0.7639(4) 0.0313(8) Uani 1 1 d .
H3 H 1.1473 1.3868 0.7333 0.038 Uiso 1 1 calc R
C4 C 1.1147(4) 1.1854(4) 0.7189(3) 0.0267(7) Uani 1 1 d .
C5 C 1.0503(4) 1.0940(4) 0.7660(3) 0.0269(7) Uani 1 1 d .
H5 H 1.0554 1.0018 0.7358 0.032 Uiso 1 1 calc R
C6 C 1.1850(4) 1.1387(4) 0.6221(4) 0.0301(8) Uani 1 1 d .
C7 C 1.2411(4) 1.1019(4) 0.5487(4) 0.0295(8) Uani 1 1 d .
C8 C 1.3130(3) 1.0551(4) 0.4538(3) 0.0229(6) Uani 1 1 d .
C9 C 1.3914(4) 1.1497(4) 0.4157(3) 0.0290(7) Uani 1 1 d .
H9 H 1.3972 1.2462 0.4506 0.035 Uiso 1 1 calc R
C10 C 1.4615(4) 1.1062(4) 0.3278(3) 0.0242(7) Uani 1 1 d .
H10 H 1.5154 1.1729 0.3030 0.029 Uiso 1 1 calc R
C11 C 1.4537(4) 0.9669(4) 0.2757(3) 0.0274(7) Uani 1 1 d .
H11 H 1.5027 0.9374 0.2155 0.033 Uiso 1 1 calc R
C12 C 0.6266(4) 0.1311(4) 0.6885(3) 0.0241(7) Uani 1 1 d .
C13 C 1.3040(3) 0.9135(4) 0.4008(3) 0.0250(7) Uani 1 1 d .
H13 H 1.2501 0.8472 0.4259 0.030 Uiso 1 1 calc R
C14 C 0.6330(4) 0.2762(4) 0.7423(3) 0.0280(7) Uani 1 1 d .
C15 C 0.6327(4) 0.3933(4) 0.7860(4) 0.0294(7) Uani 1 1 d .
C16 C 0.7174(4) 0.6538(4) 0.8474(3) 0.0267(7) Uani 1 1 d .
H16 H 0.7998 0.6498 0.8197 0.032 Uiso 1 1 calc R
C17 C 0.6163(4) 0.5281(4) 0.8367(3) 0.0280(7) Uani 1 1 d .
C18 C 0.4957(4) 0.5364(4) 0.8767(4) 0.0339(8) Uani 1 1 d .
H18 H 0.4227 0.4523 0.8690 0.041 Uiso 1 1 calc R
C19 C 0.4827(4) 0.6677(4) 0.9276(4) 0.0364(8) Uani 1 1 d .
H19 H 0.4025 0.6756 0.9575 0.044 Uiso 1 1 calc R
C20 C 0.5875(4) 0.7864(4) 0.9343(4) 0.0316(8) Uani 1 1 d .
H20 H 0.5774 0.8763 0.9679 0.038 Uiso 1 1 calc R
Cl1 Cl 0.16855(10) 0.78119(9) 0.83081(9) 0.0319(2) Uani 1 1 d .
O1 O 0.2382(5) 0.8263(5) 0.7529(5) 0.0832(13) Uani 1 1 d .
O2 O 0.1239(4) 0.6302(3) 0.7860(4) 0.0675(11) Uani 1 1 d .
O3 O 0.0387(3) 0.8140(3) 0.8256(3) 0.0467(7) Uani 1 1 d .
O4 O 0.2731(4) 0.8579(3) 0.9670(3) 0.0527(8) 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
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
N2 Ag1 N1 171.31(10) . .
N2 Ag1 Ag1 98.29(8) . 2_777
N1 Ag1 Ag1 87.80(8) . 2_777
C1 N1 C5 118.1(3) . .
C1 N1 Ag1 121.3(2) . .
C5 N1 Ag1 119.7(2) . .
C16 N2 C20 118.7(3) . .
C16 N2 Ag1 120.6(2) . .
C20 N2 Ag1 120.3(2) . .
N1 C1 C2 122.8(3) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C1 C2 C3 119.5(3) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C2 C3 C4 118.7(3) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C5 C4 C3 117.7(3) . .
C5 C4 C6 120.4(3) . .
C3 C4 C6 121.9(3) . .
N1 C5 C4 123.3(3) . .
N1 C5 H5 118.4 . .
C4 C5 H5 118.4 . .
C7 C6 C4 178.7(4) . .
C6 C7 C8 179.7(4) . .
C9 C8 C13 119.0(3) . .
C9 C8 C7 120.9(3) . .
C13 C8 C7 120.1(3) . .
C10 C9 C8 120.9(3) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C11 C10 C9 120.4(3) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C10 C11 C12 119.7(3) . 2_766
C10 C11 H11 120.2 . .
C12 C11 H11 120.2 2_766 .
C13 C12 C11 119.8(3) 2_766 2_766
C13 C12 C14 120.9(3) 2_766 .
C11 C12 C14 119.4(3) 2_766 .
C12 C13 C8 120.3(3) 2_766 .
C12 C13 H13 119.9 2_766 .
C8 C13 H13 119.9 . .
C15 C14 C12 177.5(4) . .
C14 C15 C17 174.1(4) . .
N2 C16 C17 122.7(3) . .
N2 C16 H16 118.7 . .
C17 C16 H16 118.7 . .
C16 C17 C18 117.6(3) . .
C16 C17 C15 122.2(3) . .
C18 C17 C15 120.2(3) . .
C19 C18 C17 119.6(3) . .
C19 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C20 C19 C18 118.9(3) . .
C20 C19 H19 120.6 . .
C18 C19 H19 120.6 . .
N2 C20 C19 122.5(3) . .
N2 C20 H20 118.8 . .
C19 C20 H20 118.8 . .
O1 Cl1 O2 111.5(3) . .
O1 Cl1 O3 109.5(2) . .
O2 Cl1 O3 109.2(2) . .
O1 Cl1 O4 109.4(3) . .
O2 Cl1 O4 108.4(2) . .
O3 Cl1 O4 108.81(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.146(3) .
Ag1 N1 2.147(3) .
Ag1 Ag1 3.1461(13) 2_777
N1 C1 1.332(5) .
N1 C5 1.340(5) .
N2 C16 1.337(5) .
N2 C20 1.337(5) .
C1 C2 1.372(5) .
C1 H1 0.9500 .
C2 C3 1.376(5) .
C2 H2 0.9500 .
C3 C4 1.401(5) .
C3 H3 0.9500 .
C4 C5 1.381(5) .
C4 C6 1.463(5) .
C5 H5 0.9500 .
C6 C7 1.132(5) .
C7 C8 1.459(5) .
C8 C9 1.382(5) .
C8 C13 1.392(5) .
C9 C10 1.377(5) .
C9 H9 0.9500 .
C10 C11 1.374(5) .
C10 H10 0.9500 .
C11 C12 1.396(5) 2_766
C11 H11 0.9500 .
C12 C13 1.387(5) 2_766
C12 C11 1.396(5) 2_766
C12 C14 1.436(5) .
C13 C12 1.387(5) 2_766
C13 H13 0.9500 .
C14 C15 1.181(5) .
C15 C17 1.431(5) .
C16 C17 1.388(5) .
C16 H16 0.9500 .
C17 C18 1.392(5) .
C18 C19 1.379(6) .
C18 H18 0.9500 .
C19 C20 1.371(5) .
C19 H19 0.9500 .
C20 H20 0.9500 .
Cl1 O1 1.404(4) .
Cl1 O2 1.415(3) .
Cl1 O3 1.426(3) .
Cl1 O4 1.440(3) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.031 0.500 0.500 181 24 ' '
