#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:23:36 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180336 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/05/7200589.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_7200589
loop_
_publ_author_name
'Niu, Cao-Yuan'
'Wu, Ben-Lai'
'Zheng, Xian-Fu'
'Wan, Xin-Sheng'
'Zhang, Hong-Yun'
'Niu, Yun-Yin'
'Meng, Lu-Yan'
_publ_section_title
;
 Counteranion's effects on the structures of supramolecular silver
 coordination compounds of one asymmetric and one biting organic
 ligands
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1373
_journal_paper_doi               10.1039/b818745b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C75 H66 Ag4 As4 F24 N18 O9'
_chemical_formula_weight         2550.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_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                   25.9571(7)
_cell_length_b                   25.9571(7)
_cell_length_c                   22.5629(12)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.02
_cell_volume                     13165.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23848
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.493
_exptl_absorpt_correction_T_max  0.5634
_exptl_absorpt_correction_T_min  0.3808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7482
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2740
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0349
_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)+(0.0670P)²+37.9821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                2421
_reflns_number_total             2740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818745b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7200589
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'
'-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-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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 0.3333 0.849046(16) -0.0833 0.05087(16) Uani 1 2 d S . .
Ag2 Ag 0.3333 0.6667 0.4167 0.0502(2) Uani 1 6 d S . .
C7 C 0.26386(13) 0.77401(13) 0.22637(12) 0.0325(6) Uani 1 1 d . . .
H7 H 0.2885 0.7594 0.2119 0.039 Uiso 1 1 calc R . .
C3 C 0.26222(14) 0.81080(13) 0.12369(12) 0.0321(6) Uani 1 1 d . . .
C10 C 0.20540(15) 0.81941(14) 0.20841(13) 0.0366(7) Uani 1 1 d . . .
C11 C 0.27299(14) 0.74241(15) 0.32599(14) 0.0369(7) Uani 1 1 d . . .
C9 C 0.21314(14) 0.79042(14) 0.30911(12) 0.0356(7) Uani 1 1 d . . .
C6 C 0.24218(14) 0.80015(13) 0.18689(12) 0.0330(6) Uani 1 1 d . . .
C8 C 0.25033(13) 0.76902(13) 0.28581(12) 0.0322(6) Uani 1 1 d . . .
N3 N 0.19230(12) 0.81374(12) 0.26701(11) 0.0374(6) Uani 1 1 d . . .
H1 H 0.1682 0.8262 0.2793 0.045 Uiso 1 1 calc R . .
O1 O 0.19840(12) 0.78835(12) 0.36166(9) 0.0492(6) Uani 1 1 d . . .
C2 C 0.30148(15) 0.86771(14) 0.10392(14) 0.0398(7) Uani 1 1 d . . .
H2 H 0.3158 0.9005 0.1304 0.048 Uiso 1 1 calc R . .
C4 C 0.24307(16) 0.76490(14) 0.08284(13) 0.0398(7) Uani 1 1 d . . .
H4 H 0.2156 0.7252 0.0942 0.048 Uiso 1 1 calc R . .
C5 C 0.26436(16) 0.77748(15) 0.02533(13) 0.0409(7) Uani 1 1 d D . .
H5 H 0.2514 0.7455 -0.0020 0.049 Uiso 1 1 calc RD . .
C1 C 0.31973(14) 0.87667(15) 0.04548(14) 0.0400(7) Uani 1 1 d . . .
H1A H 0.3460 0.9161 0.0324 0.048 Uiso 1 1 calc R . .
N2 N 0.29070(15) 0.72015(16) 0.35710(13) 0.0532(8) Uani 1 1 d . . .
N1 N 0.30202(12) 0.83218(12) 0.00667(11) 0.0363(6) Uani 1 1 d . . .
C12 C 0.1757(2) 0.84486(19) 0.17205(15) 0.0539(9) Uani 1 1 d . . .
H12A H 0.1474 0.8498 0.1967 0.081 Uiso 1 1 calc R . .
H12B H 0.1545 0.8179 0.1391 0.081 Uiso 1 1 calc R . .
H12C H 0.2057 0.8836 0.1564 0.081 Uiso 1 1 calc R . .
As1 As 0.3333 0.6667 0.1667 0.0379(2) Uani 1 6 d S . .
As2 As 0.3333 0.01620(3) 0.9167 0.0960(3) Uani 1 2 d S . .
F1 F 0.31218(14) 0.70675(13) 0.12387(14) 0.0868(9) Uani 1 1 d . . .
F2 F 0.2784(4) 0.0308(4) 0.9150(4) 0.256(5) Uani 1 1 d . . .
F3 F 0.3839(3) -0.0040(4) 0.9169(5) 0.257(5) Uani 1 1 d . . .
F4 F 0.3274(3) 0.0143(5) 0.9887(3) 0.271(5) Uani 1 1 d . . .
O2 O 0.4348(7) 0.1014(7) 0.0833 0.268(7) Uani 1 2 d SDU . .
C13 C 0.4512(12) 0.1366(10) 0.0338(9) 0.189(9) Uani 0.50 1 d PDU . .
H13A H 0.4211 0.1477 0.0249 0.284 Uiso 0.50 1 calc PR . .
H13B H 0.4548 0.1147 0.0002 0.284 Uiso 0.50 1 calc PR . .
H13C H 0.4896 0.1726 0.0408 0.284 Uiso 0.50 1 calc PR . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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 N1 178.33(14) 12_554 . ?
N2 Ag2 N2 173.66(16) 10_455 . ?
N2 Ag2 N2 90.08(15) 10_455 2_665 ?
N2 Ag2 N2 94.75(10) . 2_665 ?
N2 Ag2 N2 80.74(16) 10_455 3_565 ?
N2 Ag2 N2 94.75(10) . 3_565 ?
N2 Ag2 N2 94.75(10) 2_665 3_565 ?
N2 Ag2 N2 94.75(10) 10_455 11_565 ?
N2 Ag2 N2 90.08(15) . 11_565 ?
N2 Ag2 N2 80.74(16) 2_665 11_565 ?
N2 Ag2 N2 173.67(15) 3_565 11_565 ?
N2 Ag2 N2 94.75(10) 10_455 12 ?
N2 Ag2 N2 80.74(16) . 12 ?
N2 Ag2 N2 173.66(15) 2_665 12 ?
N2 Ag2 N2 90.08(15) 3_565 12 ?
N2 Ag2 N2 94.75(10) 11_565 12 ?
C8 C7 C6 121.4(3) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C2 C3 C4 117.3(3) . . ?
C2 C3 C6 120.5(3) . . ?
C4 C3 C6 122.2(3) . . ?
N3 C10 C6 119.3(3) . . ?
N3 C10 C12 115.4(3) . . ?
C6 C10 C12 125.2(3) . . ?
N2 C11 C8 178.4(4) . . ?
O1 C9 N3 120.0(3) . . ?
O1 C9 C8 126.0(3) . . ?
N3 C9 C8 114.0(2) . . ?
C10 C6 C7 118.3(3) . . ?
C10 C6 C3 120.8(3) . . ?
C7 C6 C3 120.7(3) . . ?
C7 C8 C11 121.0(3) . . ?
C7 C8 C9 120.7(3) . . ?
C11 C8 C9 118.2(3) . . ?
C10 N3 C9 126.1(3) . . ?
C10 N3 H1 116.9 . . ?
C9 N3 H1 116.9 . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C11 N2 Ag2 173.9(3) . . ?
C5 N1 C1 117.9(3) . . ?
C5 N1 Ag1 121.3(2) . . ?
C1 N1 Ag1 120.8(2) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
F1 As1 F1 179.996(1) 25_565 . ?
F1 As1 F1 89.11(16) 25_565 2_665 ?
F1 As1 F1 90.89(16) . 2_665 ?
F1 As1 F1 89.11(16) 25_565 3_565 ?
F1 As1 F1 90.89(16) . 3_565 ?
F1 As1 F1 90.89(16) 2_665 3_565 ?
F1 As1 F1 90.89(16) 25_565 26_455 ?
F1 As1 F1 89.11(16) . 26_455 ?
F1 As1 F1 180.00(18) 2_665 26_455 ?
F1 As1 F1 89.11(16) 3_565 26_455 ?
F1 As1 F1 90.89(16) 25_565 27 ?
F1 As1 F1 89.11(16) . 27 ?
F1 As1 F1 89.11(16) 2_665 27 ?
F1 As1 F1 179.997(1) 3_565 27 ?
F1 As1 F1 90.89(16) 26_455 27 ?
F4 As2 F4 178.1(9) 12_556 . ?
F4 As2 F3 93.8(6) 12_556 12_556 ?
F4 As2 F3 87.6(5) . 12_556 ?
F4 As2 F3 87.6(5) 12_556 . ?
F4 As2 F3 93.8(6) . . ?
F3 As2 F3 87.9(5) 12_556 . ?
F4 As2 F2 91.6(5) 12_556 . ?
F4 As2 F2 87.1(4) . . ?
F3 As2 F2 87.5(4) 12_556 . ?
F3 As2 F2 175.3(5) . . ?
F4 As2 F2 87.1(4) 12_556 12_556 ?
F4 As2 F2 91.6(5) . 12_556 ?
F3 As2 F2 175.3(5) 12_556 12_556 ?
F3 As2 F2 87.5(4) . 12_556 ?
F2 As2 F2 97.1(7) . 12_556 ?
C13 O2 C13 121(3) . 16_544 ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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 2.149(2) 12_554 ?
Ag1 N1 2.150(2) . ?
Ag2 N2 2.548(3) 10_455 ?
Ag2 N2 2.548(3) . ?
Ag2 N2 2.548(3) 2_665 ?
Ag2 N2 2.548(3) 3_565 ?
Ag2 N2 2.549(3) 11_565 ?
Ag2 N2 2.549(3) 12 ?
C7 C8 1.376(4) . ?
C7 C6 1.397(4) . ?
C7 H7 0.9500 . ?
C3 C2 1.384(4) . ?
C3 C4 1.387(4) . ?
C3 C6 1.496(4) . ?
C10 N3 1.355(4) . ?
C10 C6 1.369(4) . ?
C10 C12 1.487(5) . ?
C11 N2 1.142(4) . ?
C11 C8 1.432(4) . ?
C9 O1 1.239(4) . ?
C9 N3 1.375(4) . ?
C9 C8 1.433(4) . ?
N3 H1 0.8800 . ?
C2 C1 1.381(4) . ?
C2 H2 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.327(4) . ?
C5 H5 0.9500 . ?
C1 N1 1.335(4) . ?
C1 H1A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
As1 F1 1.699(2) 25_565 ?
As1 F1 1.699(2) . ?
As1 F1 1.699(2) 2_665 ?
As1 F1 1.699(2) 3_565 ?
As1 F1 1.699(2) 26_455 ?
As1 F1 1.699(2) 27 ?
As2 F4 1.631(7) 12_556 ?
As2 F4 1.631(7) . ?
As2 F3 1.639(6) 12_556 ?
As2 F3 1.639(6) . ?
As2 F2 1.649(6) . ?
As2 F2 1.649(6) 12_556 ?
O2 C13 1.370(10) . ?
O2 C13 1.370(10) 16_544 ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H1 O1 0.88 2.02 2.874(3) 163.0 31_565
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
N3 C10 C6 C7 1.4(5) . . . . ?
C12 C10 C6 C7 -176.2(3) . . . . ?
N3 C10 C6 C3 -174.2(3) . . . . ?
C12 C10 C6 C3 8.1(5) . . . . ?
C8 C7 C6 C10 -1.9(5) . . . . ?
C8 C7 C6 C3 173.8(3) . . . . ?
C2 C3 C6 C10 69.5(4) . . . . ?
C4 C3 C6 C10 -111.0(4) . . . . ?
C2 C3 C6 C7 -106.0(4) . . . . ?
C4 C3 C6 C7 73.5(4) . . . . ?
C6 C7 C8 C11 -179.7(3) . . . . ?
C6 C7 C8 C9 0.3(5) . . . . ?
N2 C11 C8 C7 -45(13) . . . . ?
N2 C11 C8 C9 135(13) . . . . ?
O1 C9 C8 C7 -179.7(3) . . . . ?
N3 C9 C8 C7 1.7(4) . . . . ?
O1 C9 C8 C11 0.2(5) . . . . ?
N3 C9 C8 C11 -178.4(3) . . . . ?
C6 C10 N3 C9 0.7(5) . . . . ?
C12 C10 N3 C9 178.6(3) . . . . ?
O1 C9 N3 C10 179.1(3) . . . . ?
C8 C9 N3 C10 -2.2(5) . . . . ?
C4 C3 C2 C1 0.1(5) . . . . ?
C6 C3 C2 C1 179.7(3) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C6 C3 C4 C5 -178.5(3) . . . . ?
C3 C4 C5 N1 -1.1(5) . . . . ?
C3 C2 C1 N1 -1.5(5) . . . . ?
C8 C11 N2 Ag2 33(15) . . . . ?
N2 Ag2 N2 C11 92(3) 10_455 . . . ?
N2 Ag2 N2 C11 -48(3) 2_665 . . . ?
N2 Ag2 N2 C11 47(3) 3_565 . . . ?
N2 Ag2 N2 C11 -129(3) 11_565 . . . ?
N2 Ag2 N2 C11 137(3) 12 . . . ?
C4 C5 N1 C1 -0.1(5) . . . . ?
C4 C5 N1 Ag1 -179.8(3) . . . . ?
C2 C1 N1 C5 1.4(5) . . . . ?
C2 C1 N1 Ag1 -178.9(3) . . . . ?
N1 Ag1 N1 C5 -35.7(2) 12_554 . . . ?
N1 Ag1 N1 C1 144.7(2) 12_554 . . . ?
