#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302765.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_4302765
loop_
_publ_author_name
'Jitendra Kumar'
'Sandeep Verma'
_publ_section_title
;
Silver-Adenine Metallamacrocyclic Hexamer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6350
_journal_page_last               6352
_journal_paper_doi               10.1021/ic900811k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C48 H48 Ag12 Cl6 N30 O46'
_chemical_formula_weight         3288.30
_chemical_name_common            '9-(carboxypropyl)adenine_AgClO4 complex'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :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            3
_cell_length_a                   18.5055(14)
_cell_length_b                   18.5055(14)
_cell_length_c                   22.556(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.2
_cell_volume                     6689.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND 3.1 d'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11322
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.864
_exptl_absorpt_correction_T_max  0.5982
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4740
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.135
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0441
_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)+(0.0637P)²+35.8612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                4844
_reflns_number_total             5173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900811k_si_002.cif
_cod_data_source_block           mou
_cod_original_cell_volume        6689.4(10)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4302765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
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 0.89287(4) 0.14668(4) 0.34571(3) 0.02343(19) Uani 1 1 d . . .
N9 N 0.6295(4) -0.1854(5) 0.4631(3) 0.0143(15) Uani 1 1 d . . .
C6 C 0.7141(6) -0.0001(6) 0.3789(4) 0.019(2) Uani 1 1 d . . .
C10 C 0.6291(6) -0.2513(5) 0.4988(4) 0.0162(19) Uani 1 1 d . . .
H10A H 0.6853 -0.2455 0.4978 0.019 Uiso 1 1 calc R . .
H10B H 0.5892 -0.3062 0.4814 0.019 Uiso 1 1 calc R . .
N7 N 0.5745(4) -0.1170(4) 0.4179(4) 0.0165(17) Uani 1 1 d . . .
O1 O 0.6400(4) -0.1598(4) 0.6458(3) 0.0233(14) Uani 1 1 d . . .
N6 N 0.6897(5) 0.0477(5) 0.3518(4) 0.0231(18) Uani 1 1 d . . .
H6A H 0.7266 0.0939 0.3340 0.028 Uiso 1 1 calc R . .
H6B H 0.6366 0.0332 0.3516 0.028 Uiso 1 1 calc R . .
C12 C 0.6633(6) -0.1689(6) 0.5957(4) 0.018(2) Uani 1 1 d . . .
C4 C 0.6937(5) -0.1186(6) 0.4364(4) 0.0141(18) Uani 1 1 d . . .
C11 C 0.6047(6) -0.2484(5) 0.5631(4) 0.019(2) Uani 1 1 d . . .
H11A H 0.5480 -0.2555 0.5636 0.023 Uiso 1 1 calc R . .
H11B H 0.6022 -0.2962 0.5847 0.023 Uiso 1 1 calc R . .
C5 C 0.6603(6) -0.0755(6) 0.4087(4) 0.0151(18) Uani 1 1 d . . .
N3 N 0.7759(5) -0.0955(4) 0.4350(3) 0.0145(16) Uani 1 1 d . . .
Ag2 Ag 1.09912(4) 0.57309(4) 0.38519(3) 0.01992(17) Uani 1 1 d . . .
C11' C 1.1798(7) 0.2810(7) 0.1706(4) 0.025(2) Uani 1 1 d . . .
H11C H 1.2234 0.2789 0.1466 0.030 Uiso 1 1 calc R . .
H11D H 1.1265 0.2288 0.1632 0.030 Uiso 1 1 calc R . .
O3 O 1.2145(5) 0.4246(5) 0.1731(3) 0.0323(18) Uani 1 1 d . . .
O4 O 1.1182(5) 0.3432(6) 0.1112(4) 0.047(2) Uani 1 1 d . . .
C12' C 1.1710(6) 0.3553(8) 0.1500(5) 0.028(2) Uani 1 1 d . . .
Ag3 Ag 1.33060(4) 0.48405(5) 0.26535(3) 0.02529(19) Uani 1 1 d . . .
Ag4 Ag 0.83540(5) -0.16090(5) 0.47339(3) 0.0275(2) Uani 1 1 d . . .
O2 O 0.7311(4) -0.1212(4) 0.5705(3) 0.0254(15) Uani 1 1 d . . .
C2 C 0.8225(6) -0.0244(6) 0.4060(4) 0.020(2) Uani 1 1 d . . .
H2 H 0.8807 -0.0050 0.4043 0.024 Uiso 1 1 calc R . .
C8' C 1.0610(6) 0.2256(5) 0.2844(4) 0.018(2) Uani 1 1 d . . .
H8' H 1.0416 0.1710 0.2694 0.022 Uiso 1 1 calc R . .
C5' C 1.0657(5) 0.3292(5) 0.3285(4) 0.0121(17) Uani 1 1 d . . .
N7' N 1.0149(5) 0.2444(5) 0.3165(3) 0.0156(15) Uani 1 1 d . . .
N6' N 0.9830(5) 0.3679(5) 0.3883(4) 0.0195(17) Uani 1 1 d . . .
H6'A H 0.9787 0.4071 0.4072 0.023 Uiso 1 1 calc R . .
H6'B H 0.9416 0.3160 0.3891 0.023 Uiso 1 1 calc R . .
C6' C 1.0515(6) 0.3868(5) 0.3588(4) 0.0137(19) Uani 1 1 d . . .
C4' C 1.1414(5) 0.3577(6) 0.3012(4) 0.0128(18) Uani 1 1 d . . .
N3' N 1.2064(5) 0.4367(5) 0.3025(4) 0.0171(16) Uani 1 1 d . . .
N1' N 1.1152(5) 0.4685(5) 0.3585(3) 0.0190(17) Uani 1 1 d . . .
N9' N 1.1384(5) 0.2891(5) 0.2737(3) 0.0160(16) Uani 1 1 d . . .
C2' C 1.1868(5) 0.4883(6) 0.3321(4) 0.0168(19) Uani 1 1 d . . .
H2' H 1.2294 0.5452 0.3343 0.020 Uiso 1 1 calc R . .
C10' C 1.2023(6) 0.2847(6) 0.2366(4) 0.020(2) Uani 1 1 d . . .
H10C H 1.2055 0.2345 0.2473 0.024 Uiso 1 1 calc R . .
H10D H 1.2576 0.3344 0.2439 0.024 Uiso 1 1 calc R . .
C8 C 0.5594(5) -0.1801(5) 0.4505(4) 0.0149(18) Uani 1 1 d . . .
H8 H 0.5052 -0.2191 0.4646 0.018 Uiso 1 1 calc R . .
N1 N 0.7960(5) 0.0229(5) 0.3789(3) 0.0173(17) Uani 1 1 d . . .
O15 O 0.8040(5) 0.2176(4) 0.3159(3) 0.0328(17) Uani 1 1 d . . .
Cl2 Cl 1.0000 0.0000 0.29855(19) 0.0189(8) Uani 1 3 d S . .
O9 O 1.0824(4) 0.0603(4) 0.2770(4) 0.0299(17) Uani 1 1 d . . .
O10 O 1.0000 0.0000 0.3620(6) 0.028(3) Uani 1 3 d S . .
Cl1 Cl 0.81815(18) 0.13679(17) 0.18113(12) 0.0361(6) Uani 1 1 d . . .
O6 O 0.8325(5) 0.1237(5) 0.1194(3) 0.0351(18) Uani 1 1 d . . .
O8 O 0.8685(5) 0.1174(5) 0.2177(3) 0.0395(19) Uani 1 1 d . . .
Cl3 Cl 1.0000 0.0000 0.54371(19) 0.0248(9) Uani 1 3 d S . .
Cl4 Cl 0.3333 -0.3333 0.4408(2) 0.0246(9) Uani 1 3 d S . .
O14 O 0.3897(4) -0.3608(4) 0.4603(4) 0.0298(18) Uani 1 1 d . . .
O12 O 1.0000 0.0000 0.4820(7) 0.043(3) Uani 1 3 d S . .
O13 O 0.3333 -0.3333 0.3763(7) 0.041(4) Uani 1 3 d S . .
O5 O 0.7330(5) 0.0836(5) 0.1991(3) 0.0390(18) Uani 1 1 d . . .
O7 O 0.8352(6) 0.2210(5) 0.1884(4) 0.045(2) Uani 1 1 d . . .
O11 O 1.0283(5) 0.0826(5) 0.5655(4) 0.0396(19) Uani 1 1 d . . .
O16 O 0.8173(5) 0.3700(6) 0.3566(4) 0.050(2) Uani 1 1 d . . .
O17 O 0.6667 0.3333 0.3088(7) 0.052(4) Uani 1 3 d S . .
O18 O 0.9764(8) 0.0803(10) 0.1427(5) 0.090(4) 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
_geom_angle_publ_flag
N7' Ag1 N1 158.4(3) . . ?
N7' Ag1 O4 96.6(3) . 6_665 ?
N1 Ag1 O4 90.8(3) . 6_665 ?
C4 N9 C8 105.7(7) . . ?
C4 N9 C10 130.2(8) . . ?
C8 N9 C10 124.1(7) . . ?
N6 C6 N1 119.4(8) . . ?
N6 C6 C5 124.8(9) . . ?
N1 C6 C5 115.8(8) . . ?
N9 C10 C11 111.9(8) . . ?
C8 N7 C5 104.8(7) . . ?
C8 N7 Ag2 121.2(6) . 3_665 ?
C5 N7 Ag2 133.9(6) . 3_665 ?
O1 C12 O2 127.3(9) . . ?
O1 C12 C11 116.3(8) . . ?
O2 C12 C11 116.3(9) . . ?
N9 C4 N3 129.1(8) . . ?
N9 C4 C5 106.7(8) . . ?
N3 C4 C5 124.1(8) . . ?
C12 C11 C10 114.5(8) . . ?
C4 C5 N7 109.3(8) . . ?
C4 C5 C6 119.3(8) . . ?
N7 C5 C6 131.4(8) . . ?
C2 N3 C4 113.2(8) . . ?
C2 N3 Ag4 119.1(6) . . ?
C4 N3 Ag4 127.7(6) . . ?
N7 Ag2 N1' 165.1(3) 2_655 . ?
N7 Ag2 Ag3 82.8(2) 2_655 3_775 ?
N1' Ag2 Ag3 96.9(2) . 3_775 ?
C12' C11' C10' 113.6(8) . . ?
C12' O3 Ag4 107.2(7) . 7_554 ?
C12' O4 Ag1 111.9(7) . 8_644 ?
O3 C12' O4 121.7(10) . . ?
O3 C12' C11' 119.8(9) . . ?
O4 C12' C11' 118.5(11) . . ?
O2 Ag3 N3' 171.9(3) 8_644 . ?
O2 Ag3 Ag2 77.85(19) 8_644 2_755 ?
N3' Ag3 Ag2 97.1(2) . 2_755 ?
N3 Ag4 O3 172.1(3) . 4_445 ?
C12 O2 Ag3 125.7(6) . 6_665 ?
N3 C2 N1 126.9(9) . . ?
N7' C8' N9' 115.1(8) . . ?
C4' C5' N7' 109.3(8) . . ?
C4' C5' C6' 118.2(8) . . ?
N7' C5' C6' 132.4(8) . . ?
C8' N7' C5' 104.2(7) . . ?
C8' N7' Ag1 119.9(6) . . ?
C5' N7' Ag1 135.5(6) . . ?
N6' C6' N1' 118.5(8) . . ?
N6' C6' C5' 124.7(8) . . ?
N1' C6' C5' 116.8(8) . . ?
N3' C4' C5' 126.3(8) . . ?
N3' C4' N9' 127.3(8) . . ?
C5' C4' N9' 106.4(8) . . ?
C4' N3' C2' 111.5(7) . . ?
C4' N3' Ag3 128.0(6) . . ?
C2' N3' Ag3 120.4(6) . . ?
C2' N1' C6' 119.6(8) . . ?
C2' N1' Ag2 116.1(6) . . ?
C6' N1' Ag2 123.4(6) . . ?
C8' N9' C4' 104.8(8) . . ?
C8' N9' C10' 125.7(8) . . ?
C4' N9' C10' 129.3(8) . . ?
N1' C2' N3' 127.5(8) . . ?
N9' C10' C11' 110.1(8) . . ?
N7 C8 N9 113.4(8) . . ?
C2 N1 C6 120.7(8) . . ?
C2 N1 Ag1 117.1(6) . . ?
C6 N1 Ag1 121.7(6) . . ?
O10 Cl2 O9 109.5(4) . . ?
O10 Cl2 O9 109.5(4) . 3_765 ?
O9 Cl2 O9 109.4(4) . 3_765 ?
O10 Cl2 O9 109.5(4) . 2_645 ?
O9 Cl2 O9 109.4(4) . 2_645 ?
O9 Cl2 O9 109.4(4) 3_765 2_645 ?
O8 Cl1 O5 107.3(5) . . ?
O8 Cl1 O7 113.1(5) . . ?
O5 Cl1 O7 106.4(5) . . ?
O8 Cl1 O6 108.4(5) . . ?
O5 Cl1 O6 112.5(5) . . ?
O7 Cl1 O6 109.2(5) . . ?
O12 Cl3 O11 110.0(4) . . ?
O12 Cl3 O11 110.0(4) . 3_765 ?
O11 Cl3 O11 108.9(4) . 3_765 ?
O12 Cl3 O11 110.0(4) . 2_645 ?
O11 Cl3 O11 108.9(4) . 2_645 ?
O11 Cl3 O11 108.9(4) 3_765 2_645 ?
O14 Cl4 O14 111.1(4) 2_545 3_655 ?
O14 Cl4 O14 111.1(4) 2_545 . ?
O14 Cl4 O14 111.1(4) 3_655 . ?
O14 Cl4 O13 107.8(4) 2_545 . ?
O14 Cl4 O13 107.8(4) 3_655 . ?
O14 Cl4 O13 107.8(4) . . ?
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 N7' 2.172(8) . ?
Ag1 N1 2.217(8) . ?
Ag1 O4 2.571(8) 6_665 ?
N9 C4 1.353(12) . ?
N9 C8 1.380(12) . ?
N9 C10 1.459(11) . ?
C6 N6 1.328(12) . ?
C6 N1 1.353(12) . ?
C6 C5 1.415(13) . ?
C10 C11 1.527(13) . ?
N7 C8 1.287(12) . ?
N7 C5 1.392(11) . ?
N7 Ag2 2.174(7) 3_665 ?
O1 C12 1.251(11) . ?
C12 O2 1.252(12) . ?
C12 C11 1.513(12) . ?
C4 N3 1.359(12) . ?
C4 C5 1.378(13) . ?
N3 C2 1.328(12) . ?
N3 Ag4 2.182(7) . ?
Ag2 N7 2.174(7) 2_655 ?
Ag2 N1' 2.184(8) . ?
Ag2 Ag3 3.1148(11) 3_775 ?
C11' C12' 1.534(15) . ?
C11' C10' 1.537(14) . ?
O3 C12' 1.238(14) . ?
O3 Ag4 2.191(7) 7_554 ?
O4 C12' 1.246(13) . ?
O4 Ag1 2.571(8) 8_644 ?
Ag3 O2 2.144(7) 8_644 ?
Ag3 N3' 2.177(8) . ?
Ag3 Ag2 3.1148(11) 2_755 ?
Ag4 O3 2.191(7) 4_445 ?
O2 Ag3 2.144(7) 6_665 ?
C2 N1 1.347(13) . ?
C8' N7' 1.291(12) . ?
C8' N9' 1.345(12) . ?
C5' C4' 1.371(12) . ?
C5' N7' 1.395(12) . ?
C5' C6' 1.398(12) . ?
N6' C6' 1.314(12) . ?
C6' N1' 1.377(11) . ?
C4' N3' 1.352(12) . ?
C4' N9' 1.388(12) . ?
N3' C2' 1.354(12) . ?
N1' C2' 1.326(12) . ?
N9' C10' 1.484(11) . ?
Cl2 O10 1.430(13) . ?
Cl2 O9 1.451(7) . ?
Cl2 O9 1.451(7) 3_765 ?
Cl2 O9 1.451(7) 2_645 ?
Cl1 O8 1.417(8) . ?
Cl1 O5 1.436(8) . ?
Cl1 O7 1.437(8) . ?
Cl1 O6 1.461(7) . ?
Cl3 O12 1.393(16) . ?
Cl3 O11 1.431(8) . ?
Cl3 O11 1.431(8) 3_765 ?
Cl3 O11 1.431(8) 2_645 ?
Cl4 O14 1.439(7) 2_545 ?
Cl4 O14 1.439(7) 3_655 ?
Cl4 O14 1.439(7) . ?
Cl4 O13 1.455(16) . ?
