#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:04:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180167 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/63/7106330.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_7106330
loop_
_publ_author_name
'Dario Braga'
'Simone d'Agostino'
'Eros D'Amen'
'Fabrizia Grepioni'
_publ_section_title
;
 Polymorphs from supramolecular gels: four crystal forms of the same
 silver(I) supergelator crystallized directly from its gels
;
_journal_name_full               Chem.Commun.
_journal_page_first              5154
_journal_paper_doi               10.1039/c1cc10305a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C32 H26 Ag N7 O5'
_chemical_formula_weight         696.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.587(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9972(7)
_cell_length_b                   9.1664(5)
_cell_length_c                   21.5610(13)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9697
_cell_measurement_theta_min      2.6188
_cell_volume                     2903.6(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1340
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_details
;
1 omega -7.00 36.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 18.0642 77.0000 150.0000 43

2 omega -39.00 6.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -18.5330 77.0000 -90.0000 45

3 omega -19.00 50.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -18.5330 77.0000 150.0000 69

4 omega -48.00 51.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -18.5330 77.0000 30.0000 99

;
_diffrn_measurement_device       '92mm CCD camera (sapphire) on κ-goniostat'
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.1208
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12854
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.04
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0456
_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)+(0.0572P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2575
_reflns_number_total             6146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10305a.txt
_cod_data_source_block           e_23_red2d
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7106330
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.09675(2) 0.10548(4) 0.054873(18) 0.06727(17) Uani 1 1 d . . .
O1 O 0.4593(2) -0.4410(3) 0.27658(14) 0.0659(9) Uani 1 1 d . . .
N1 N 0.2043(2) -0.0442(4) 0.05365(19) 0.0518(9) Uani 1 1 d . . .
N2 N 0.4187(3) -0.3900(5) 0.1716(2) 0.0553(11) Uani 1 1 d . . .
H2N H 0.436(2) -0.393(4) 0.1426(15) 0.011(11) Uiso 1 1 d . . .
N3 N 0.5376(3) -0.5408(4) 0.2072(2) 0.0556(11) Uani 1 1 d . . .
H3N H 0.538(2) -0.543(4) 0.1680(18) 0.042(13) Uiso 1 1 d . . .
C1 C 0.6836(4) -0.7188(6) 0.3447(3) 0.0894(18) Uani 1 1 d . . .
H1 H 0.6903 -0.7256 0.3885 0.107 Uiso 1 1 calc R . .
C2 C 0.7400(4) -0.7953(6) 0.3157(3) 0.0869(18) Uani 1 1 d . . .
H2 H 0.7869 -0.8503 0.3395 0.104 Uiso 1 1 calc R . .
C3 C 0.7283(3) -0.7920(6) 0.2517(3) 0.0807(16) Uani 1 1 d . . .
H3 H 0.7652 -0.8480 0.2311 0.097 Uiso 1 1 calc R . .
C4 C 0.6612(3) -0.7047(5) 0.2174(2) 0.0682(14) Uani 1 1 d . . .
H4 H 0.6545 -0.6999 0.1736 0.082 Uiso 1 1 calc R . .
C5 C 0.6042(3) -0.6249(5) 0.2465(2) 0.0499(11) Uani 1 1 d . . .
C6 C 0.6159(3) -0.6302(6) 0.3114(2) 0.0761(15) Uani 1 1 d . . .
H6 H 0.5790 -0.5754 0.3325 0.091 Uiso 1 1 calc R . .
C7 C 0.4709(3) -0.4573(5) 0.2232(2) 0.0458(11) Uani 1 1 d . . .
C8 C 0.3472(3) -0.2902(4) 0.1699(2) 0.0453(11) Uani 1 1 d . . .
C9 C 0.3073(3) -0.2643(5) 0.2204(2) 0.0526(12) Uani 1 1 d . . .
H9 H 0.3284 -0.3132 0.2583 0.063 Uiso 1 1 calc R . .
C10 C 0.2351(3) -0.1653(5) 0.2161(2) 0.0529(12) Uani 1 1 d . . .
H10 H 0.2096 -0.1485 0.2514 0.064 Uiso 1 1 calc R . .
C11 C 0.2019(3) -0.0935(5) 0.1614(2) 0.0548(12) Uani 1 1 d . . .
H11 H 0.1534 -0.0293 0.1592 0.066 Uiso 1 1 calc R . .
C12 C 0.2402(3) -0.1156(5) 0.1085(2) 0.0434(10) Uani 1 1 d . . .
C13 C 0.3135(3) -0.2159(4) 0.11135(19) 0.0398(10) Uani 1 1 d . . .
C14 C 0.3497(3) -0.2320(4) 0.0564(2) 0.0482(11) Uani 1 1 d . . .
H14 H 0.3993 -0.2933 0.0569 0.058 Uiso 1 1 calc R . .
C15 C 0.3127(3) -0.1582(5) 0.0027(2) 0.0554(12) Uani 1 1 d . . .
H15 H 0.3357 -0.1696 -0.0340 0.066 Uiso 1 1 calc R . .
C16 C 0.2403(3) -0.0663(5) 0.0037(2) 0.0593(13) Uani 1 1 d . . .
H16 H 0.2153 -0.0166 -0.0333 0.071 Uiso 1 1 calc R . .
O2 O -0.2422(2) 0.7343(3) -0.13299(15) 0.0599(9) Uani 1 1 d . . .
N4 N -0.0159(2) 0.2435(4) 0.05455(19) 0.0571(10) Uani 1 1 d . . .
N5 N -0.2446(3) 0.5829(4) -0.05003(19) 0.0539(11) Uani 1 1 d . . .
H5N H -0.273(2) 0.555(4) -0.0228(17) 0.036(13) Uiso 1 1 d . . .
N6 N -0.3631(3) 0.7371(4) -0.0851(2) 0.0580(12) Uani 1 1 d . . .
H6N H -0.379(2) 0.708(3) -0.0566(14) 0.044(10) Uiso 1 1 d . . .
C17 C -0.5387(4) 1.0517(6) -0.1829(3) 0.0756(15) Uani 1 1 d . . .
H17 H -0.5785 1.1210 -0.2045 0.091 Uiso 1 1 calc R . .
C18 C -0.5450(3) 1.0114(5) -0.1226(3) 0.0755(15) Uani 1 1 d . . .
H18 H -0.5886 1.0534 -0.1030 0.091 Uiso 1 1 calc R . .
C19 C -0.4856(3) 0.9073(5) -0.0913(2) 0.0632(13) Uani 1 1 d . . .
H19 H -0.4901 0.8789 -0.0506 0.076 Uiso 1 1 calc R . .
C20 C -0.4743(4) 0.9905(5) -0.2109(2) 0.0727(15) Uani 1 1 d . . .
H20 H -0.4701 1.0190 -0.2517 0.087 Uiso 1 1 calc R . .
C21 C -0.4148(3) 0.8863(5) -0.1798(2) 0.0599(12) Uani 1 1 d . . .
H21 H -0.3716 0.8444 -0.1998 0.072 Uiso 1 1 calc R . .
C22 C -0.4199(3) 0.8450(5) -0.1193(2) 0.0519(12) Uani 1 1 d . . .
C23 C -0.2812(3) 0.6890(5) -0.0932(2) 0.0498(11) Uani 1 1 d . . .
C24 C -0.1698(3) 0.4939(4) -0.0527(2) 0.0444(11) Uani 1 1 d . . .
C25 C -0.1294(3) 0.4191(4) 0.0039(2) 0.0430(11) Uani 1 1 d . . .
C26 C -0.1365(3) 0.4734(5) -0.1066(2) 0.0531(12) Uani 1 1 d . . .
H26 H -0.1621 0.5235 -0.1434 0.064 Uiso 1 1 calc R . .
C27 C -0.0645(3) 0.3781(5) -0.1067(2) 0.0549(12) Uani 1 1 d . . .
H27 H -0.0425 0.3658 -0.1437 0.066 Uiso 1 1 calc R . .
C28 C -0.0256(3) 0.3026(5) -0.0541(2) 0.0543(12) Uani 1 1 d . . .
H28 H 0.0218 0.2381 -0.0556 0.065 Uiso 1 1 calc R . .
C29 C -0.0564(3) 0.3218(5) 0.0020(2) 0.0449(11) Uani 1 1 d . . .
C30 C -0.1552(3) 0.4370(5) 0.0624(2) 0.0526(12) Uani 1 1 d . . .
H30 H -0.2014 0.5023 0.0658 0.063 Uiso 1 1 calc R . .
C31 C -0.1139(3) 0.3607(5) 0.1139(2) 0.0658(14) Uani 1 1 d . . .
H31 H -0.1311 0.3729 0.1527 0.079 Uiso 1 1 calc R . .
C32 C -0.0447(3) 0.2628(5) 0.1073(2) 0.0679(14) Uani 1 1 d . . .
H32 H -0.0177 0.2083 0.1425 0.082 Uiso 1 1 calc R . .
N7 N 0.5815(3) 0.5523(7) 0.0544(2) 0.0783(14) Uani 1 1 d . . .
O3 O 0.5879(5) 0.6780(6) 0.0411(2) 0.185(3) Uani 1 1 d . . .
O4 O 0.5183(3) 0.5090(6) 0.07539(16) 0.1240(17) Uani 1 1 d . . .
O5 O 0.6397(3) 0.4772(6) 0.0465(2) 0.145(2) 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'
Ag Ag -0.8971 1.1015 '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'
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
N4 Ag1 N1 176.44(13) . . ?
C16 N1 C12 118.7(4) . . ?
C16 N1 Ag1 123.3(3) . . ?
C12 N1 Ag1 117.9(3) . . ?
C7 N2 C8 128.6(4) . . ?
C7 N3 C5 128.8(4) . . ?
C2 C1 C6 122.0(5) . . ?
C1 C2 C3 119.7(5) . . ?
C2 C3 C4 119.3(5) . . ?
C5 C4 C3 121.3(5) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 N3 116.7(4) . . ?
C6 C5 N3 124.3(4) . . ?
C5 C6 C1 118.6(5) . . ?
O1 C7 N3 124.5(4) . . ?
O1 C7 N2 123.3(4) . . ?
N3 C7 N2 112.2(4) . . ?
C9 C8 N2 123.1(4) . . ?
C9 C8 C13 119.1(4) . . ?
N2 C8 C13 117.7(4) . . ?
C8 C9 C10 121.1(4) . . ?
C11 C10 C9 121.1(4) . . ?
C10 C11 C12 120.2(4) . . ?
N1 C12 C11 119.0(4) . . ?
N1 C12 C13 121.0(4) . . ?
C11 C12 C13 120.0(4) . . ?
C14 C13 C12 117.1(4) . . ?
C14 C13 C8 124.3(4) . . ?
C12 C13 C8 118.5(4) . . ?
C15 C14 C13 120.3(4) . . ?
C14 C15 C16 118.5(4) . . ?
N1 C16 C15 124.3(4) . . ?
C32 N4 C29 118.6(4) . . ?
C32 N4 Ag1 118.8(3) . . ?
C29 N4 Ag1 122.4(3) . . ?
C23 N5 C24 126.7(4) . . ?
C23 N6 C22 129.1(4) . . ?
C20 C17 C18 120.0(5) . . ?
C17 C18 C19 119.2(5) . . ?
C22 C19 C18 121.2(5) . . ?
C17 C20 C21 121.0(5) . . ?
C22 C21 C20 119.7(5) . . ?
C21 C22 C19 118.9(4) . . ?
C21 C22 N6 123.0(4) . . ?
C19 C22 N6 118.1(4) . . ?
O2 C23 N6 124.4(4) . . ?
O2 C23 N5 122.5(4) . . ?
N6 C23 N5 113.1(4) . . ?
C26 C24 N5 123.3(4) . . ?
C26 C24 C25 119.8(4) . . ?
N5 C24 C25 116.9(4) . . ?
C30 C25 C29 117.0(4) . . ?
C30 C25 C24 124.6(4) . . ?
C29 C25 C24 118.3(4) . . ?
C24 C26 C27 120.3(4) . . ?
C28 C27 C26 121.7(4) . . ?
C27 C28 C29 120.0(4) . . ?
N4 C29 C28 118.9(4) . . ?
N4 C29 C25 121.3(4) . . ?
C28 C29 C25 119.8(4) . . ?
C31 C30 C25 121.0(4) . . ?
C30 C31 C32 118.3(4) . . ?
N4 C32 C31 123.8(4) . . ?
O5 N7 O3 116.2(6) . . ?
O5 N7 O4 122.7(7) . . ?
O3 N7 O4 121.1(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 N4 2.109(4) . ?
Ag1 N1 2.122(3) . ?
O1 C7 1.208(5) . ?
N1 C16 1.313(5) . ?
N1 C12 1.364(5) . ?
N2 C7 1.371(5) . ?
N2 C8 1.404(5) . ?
N3 C7 1.359(5) . ?
N3 C5 1.405(5) . ?
C1 C2 1.346(7) . ?
C1 C6 1.383(6) . ?
C2 C3 1.357(7) . ?
C3 C4 1.379(6) . ?
C4 C5 1.369(6) . ?
C5 C6 1.376(6) . ?
C8 C9 1.365(5) . ?
C8 C13 1.434(5) . ?
C9 C10 1.401(5) . ?
C10 C11 1.356(5) . ?
C11 C12 1.391(5) . ?
C12 C13 1.424(5) . ?
C13 C14 1.406(5) . ?
C14 C15 1.360(5) . ?
C15 C16 1.378(6) . ?
O2 C23 1.206(5) . ?
N4 C32 1.307(5) . ?
N4 C29 1.375(5) . ?
N5 C23 1.381(5) . ?
N5 C24 1.397(5) . ?
N6 C23 1.348(5) . ?
N6 C22 1.413(5) . ?
C17 C20 1.360(6) . ?
C17 C18 1.373(7) . ?
C18 C19 1.385(6) . ?
C19 C22 1.378(6) . ?
C20 C21 1.384(6) . ?
C21 C22 1.376(6) . ?
C24 C26 1.367(5) . ?
C24 C25 1.425(5) . ?
C25 C30 1.401(5) . ?
C25 C29 1.420(5) . ?
C26 C27 1.388(6) . ?
C27 C28 1.355(6) . ?
C28 C29 1.390(5) . ?
C30 C31 1.353(5) . ?
C31 C32 1.402(6) . ?
N7 O5 1.150(5) . ?
N7 O3 1.196(6) . ?
N7 O4 1.197(5) . ?
