#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/03/4110369.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_4110369
loop_
_publ_author_name
'Chandra Shekhar Purohit'
'Sandeep Verma'
_publ_section_title
;
 A Luminescent Silver-Adenine Metallamacrocyclic Quartet
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              400
_journal_page_last               401
_journal_paper_doi               10.1021/ja056452z
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C9 H9 Ag N6 O3.50'
_chemical_formula_sum            'C9 H9 Ag N6 O3.5'
_chemical_formula_weight         365.09
_chemical_melting_point          380
_chemical_name_common            '9-allyl adenine silver nirtate complex'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.6668(15)
_cell_length_b                   26.0509(15)
_cell_length_c                   7.5084(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     4824.8(5)
_computing_cell_refinement       'SMART 5.628 (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT+ 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'DIAMOND 2.1 e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area Detector'
_diffrn_measurement_method       'Phi-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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            7870
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.05
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.7855
_exptl_absorpt_correction_T_min  0.7284
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2277
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0251
_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)+(0.0442P)²+13.7938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                2261
_reflns_number_total             2277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056452zsi20050920_025024.cif
_cod_data_source_block           6decb
_cod_original_formula_sum        'C9 H9 Ag N6 O3.50'
_cod_database_code               4110369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
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 0.449822(9) 1.175159(9) 1.75062(6) 0.01987(8) Uani 1 1 d .
O2 O 0.27260(12) 1.14862(15) 2.0156(6) 0.0480(10) Uani 1 1 d .
O3 O 0.19409(11) 1.13599(13) 2.1321(5) 0.0327(7) Uani 1 1 d .
N9 N 0.40081(11) 1.03510(11) 2.0153(5) 0.0217(6) Uani 1 1 d .
N7 N 0.41402(12) 1.10313(11) 1.8398(4) 0.0188(6) Uani 1 1 d .
N3 N 0.31588(12) 1.00344(12) 1.8879(5) 0.0211(6) Uani 1 1 d .
N6 N 0.33323(13) 1.12619(12) 1.5379(5) 0.0277(8) Uani 1 1 d .
H6A H 0.3084 1.1307 1.4589 0.033 Uiso 1 1 calc R
H6B H 0.3612 1.1459 1.5399 0.033 Uiso 1 1 calc R
N14 N 0.24350(13) 1.12788(13) 2.1276(5) 0.0244(7) Uani 1 1 d .
C5 C 0.36640(14) 1.07828(12) 1.7911(5) 0.0174(7) Uani 1 1 d .
N1 N 0.28374(12) 1.05764(12) 1.6514(5) 0.0219(6) Uani 1 1 d .
C4 C 0.35823(14) 1.03616(13) 1.8992(5) 0.0193(7) Uani 1 1 d .
C10 C 0.41248(15) 0.99828(15) 2.1585(6) 0.0255(8) Uani 1 1 d .
H10A H 0.4479 1.0059 2.2081 0.031 Uiso 1 1 calc R
H10B H 0.4139 0.9640 2.1082 0.031 Uiso 1 1 calc R
C8 C 0.43248(14) 1.07618(13) 1.9746(6) 0.0201(8) Uani 1 1 d .
H8 H 0.4640 1.0844 2.0361 0.024 Uiso 1 1 calc R
C11 C 0.37188(17) 0.99903(15) 2.3036(6) 0.0272(8) Uani 1 1 d .
H11 H 0.3550 1.0300 2.3304 0.033 Uiso 1 1 calc R
C6 C 0.32836(13) 1.08834(13) 1.6577(5) 0.0186(7) Uani 1 1 d .
C1 C 0.28037(12) 1.01797(13) 1.7628(7) 0.0228(7) Uani 1 1 d .
H1 H 0.2494 0.9978 1.7524 0.027 Uiso 1 1 calc R
C12 C 0.35837(17) 0.95810(17) 2.3970(6) 0.0304(9) Uani 1 1 d .
H12A H 0.3746 0.9267 2.3729 0.037 Uiso 1 1 calc R
H12B H 0.3326 0.9607 2.4869 0.037 Uiso 1 1 calc R
O1 O 0.26511(11) 1.09759(10) 2.2413(5) 0.0288(6) Uani 1 1 d .
OM O 0.5000 1.0000 2.6338(18) 0.110(3) Uiso 1 2 d S
C' C 0.5281(4) 1.0201(4) 2.7900(16) 0.100(3) Uiso 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'
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
N7 Ag1 N3 146.02(12) . 11_554
N7 Ag1 N1 111.42(12) . 4_575
N3 Ag1 N1 99.05(11) 11_554 4_575
N7 Ag1 O1 106.58(10) . 4_574
N3 Ag1 O1 91.81(11) 11_554 4_574
N1 Ag1 O1 82.04(11) 4_575 4_574
C8 N9 C4 106.4(3) . .
C8 N9 C10 124.5(3) . .
C4 N9 C10 129.1(3) . .
C8 N7 C5 104.3(3) . .
C8 N7 Ag1 123.8(2) . .
C5 N7 Ag1 131.5(2) . .
C1 N3 C4 111.8(3) . .
C1 N3 Ag1 114.1(2) . 15_545
C4 N3 Ag1 133.1(3) . 15_545
O2 N14 O3 121.2(4) . .
O2 N14 O1 118.9(3) . .
O3 N14 O1 119.8(4) . .
C4 C5 N7 109.8(3) . .
C4 C5 C6 118.2(3) . .
N7 C5 C6 132.0(3) . .
C1 N1 C6 119.0(3) . .
C1 N1 Ag1 112.8(2) . 12_474
C6 N1 Ag1 127.1(2) . 12_474
N3 C4 N9 128.5(3) . .
N3 C4 C5 125.3(3) . .
N9 C4 C5 106.2(3) . .
N9 C10 C11 113.4(3) . .
N7 C8 N9 113.2(3) . .
C12 C11 C10 123.5(4) . .
N6 C6 N1 118.8(3) . .
N6 C6 C5 124.0(3) . .
N1 C6 C5 117.2(3) . .
N1 C1 N3 128.2(3) . .
N14 O1 Ag1 112.5(2) . 12_475
C' OM C' 73.0(11) . 2_675
OM C' C' 53.5(6) . 2_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N7 2.179(3) .
Ag1 N3 2.242(3) 11_554
Ag1 N1 2.402(3) 4_575
Ag1 O1 2.595(3) 4_574
O2 N14 1.231(5) .
O3 N14 1.237(4) .
N9 C8 1.360(4) .
N9 C4 1.365(5) .
N9 C10 1.470(5) .
N7 C8 1.313(5) .
N7 C5 1.390(4) .
N3 C1 1.339(5) .
N3 C4 1.351(4) .
N3 Ag1 2.242(3) 15_545
N6 C6 1.340(5) .
N14 O1 1.279(4) .
C5 C4 1.380(5) .
C5 C6 1.397(5) .
N1 C1 1.332(5) .
N1 C6 1.361(5) .
N1 Ag1 2.402(3) 12_474
C10 C11 1.480(6) .
C11 C12 1.319(6) .
O1 Ag1 2.595(3) 12_475
OM C' 1.459(15) .
OM C' 1.459(14) 2_675
C' C' 1.74(2) 2_675
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_4
N3 Ag1 N7 C8 -144.0(3) 11_554 .
N1 Ag1 N7 C8 8.1(3) 4_575 .
O1 Ag1 N7 C8 95.9(3) 4_574 .
N3 Ag1 N7 C5 27.5(5) 11_554 .
N1 Ag1 N7 C5 179.7(3) 4_575 .
O1 Ag1 N7 C5 -92.5(3) 4_574 .
C8 N7 C5 C4 -0.7(4) . .
Ag1 N7 C5 C4 -173.5(3) . .
C8 N7 C5 C6 179.9(4) . .
Ag1 N7 C5 C6 7.2(6) . .
C1 N3 C4 N9 176.9(4) . .
Ag1 N3 C4 N9 -14.8(7) 15_545 .
C1 N3 C4 C5 -3.1(6) . .
Ag1 N3 C4 C5 165.2(3) 15_545 .
C8 N9 C4 N3 -179.6(4) . .
C10 N9 C4 N3 0.3(7) . .
C8 N9 C4 C5 0.4(4) . .
C10 N9 C4 C5 -179.7(4) . .
N7 C5 C4 N3 -179.8(4) . .
C6 C5 C4 N3 -0.4(6) . .
N7 C5 C4 N9 0.2(4) . .
C6 C5 C4 N9 179.6(3) . .
C8 N9 C10 C11 114.9(4) . .
C4 N9 C10 C11 -64.9(6) . .
C5 N7 C8 N9 1.0(4) . .
Ag1 N7 C8 N9 174.5(3) . .
C4 N9 C8 N7 -1.0(5) . .
C10 N9 C8 N7 179.2(4) . .
N9 C10 C11 C12 147.8(4) . .
C1 N1 C6 N6 175.8(4) . .
Ag1 N1 C6 N6 -17.3(5) 12_474 .
C1 N1 C6 C5 -4.5(6) . .
Ag1 N1 C6 C5 162.4(3) 12_474 .
C4 C5 C6 N6 -176.0(4) . .
N7 C5 C6 N6 3.3(7) . .
C4 C5 C6 N1 4.3(5) . .
N7 C5 C6 N1 -176.4(4) . .
C6 N1 C1 N3 0.9(7) . .
Ag1 N1 C1 N3 -167.8(4) 12_474 .
C4 N3 C1 N1 2.9(7) . .
Ag1 N3 C1 N1 -167.8(4) 15_545 .
O2 N14 O1 Ag1 167.6(3) . 12_475
O3 N14 O1 Ag1 -12.1(4) . 12_475
