#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/72/4507258.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_4507258
loop_
_publ_author_name
'Yang, Guang'
'Baran, Peter'
'Martínez, Angel R.'
'Raptis, Raphael G.'
_publ_section_title
;
 Substituent Effects on the Supramolecular Aggregation of AgI-Pyrazolato
 Trimers
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              264
_journal_paper_doi               10.1021/cg301411j
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C46.5 H36.5 Ag3 N6'
_chemical_formula_weight         1002.93
_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                100.076(7)
_cell_angle_beta                 101.519(7)
_cell_angle_gamma                107.103(7)
_cell_formula_units_Z            2
_cell_length_a                   11.806(7)
_cell_length_b                   13.182(8)
_cell_length_c                   14.862(9)
_cell_measurement_temperature    298(2)
_cell_volume                     2098(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12369
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.6825
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             997
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8687
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0441
_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)+(0.0588P)²+1.6710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                7153
_reflns_number_total             8687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301411j_si_002.cif
_cod_data_source_block           yg151-New
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46.50 H36.50 Ag3 N6'
_cod_database_code               4507258
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.13669(3) 0.68183(2) 0.794394(19) 0.04403(10) Uani 1 1 d . . .
Ag2 Ag 0.04920(3) 0.41856(2) 0.82445(2) 0.04937(10) Uani 1 1 d . . .
Ag3 Ag -0.11186(3) 0.48809(2) 0.64457(2) 0.04833(10) Uani 1 1 d . . .
C1 C 0.2322(4) 0.9032(3) 1.1042(3) 0.0533(10) Uani 1 1 d . . .
H1 H 0.1951 0.8658 1.1440 0.064 Uiso 1 1 calc R . .
C2 C 0.2535(5) 1.0152(4) 1.1178(4) 0.0640(12) Uani 1 1 d . . .
H2 H 0.2311 1.0519 1.1669 0.077 Uiso 1 1 calc R . .
C3 C 0.3080(5) 1.0723(4) 1.0585(4) 0.0655(13) Uani 1 1 d . . .
H3 H 0.3206 1.1468 1.0670 0.079 Uiso 1 1 calc R . .
C4 C 0.3442(5) 1.0164(4) 0.9848(4) 0.0607(12) Uani 1 1 d . . .
H4 H 0.3818 1.0542 0.9454 0.073 Uiso 1 1 calc R . .
C5 C 0.3229(4) 0.9039(3) 0.9721(3) 0.0487(9) Uani 1 1 d . . .
H5 H 0.3467 0.8671 0.9239 0.058 Uiso 1 1 calc R . .
C6 C 0.2661(3) 0.8460(3) 1.0312(3) 0.0403(8) Uani 1 1 d . . .
C7 C 0.2371(3) 0.7256(3) 1.0181(3) 0.0388(8) Uani 1 1 d . . .
C8 C 0.2417(4) 0.6670(3) 1.0878(3) 0.0431(8) Uani 1 1 d . . .
H8 H 0.2688 0.6954 1.1532 0.052 Uiso 1 1 calc R . .
C9 C 0.1965(3) 0.5557(3) 1.0380(3) 0.0404(8) Uani 1 1 d . . .
C10 C 0.1850(4) 0.4592(3) 1.0800(3) 0.0408(8) Uani 1 1 d . . .
C11 C 0.2752(5) 0.4694(4) 1.1623(3) 0.0580(11) Uani 1 1 d . . .
H11 H 0.3407 0.5349 1.1885 0.070 Uiso 1 1 calc R . .
C12 C 0.2673(5) 0.3817(4) 1.2055(4) 0.0644(12) Uani 1 1 d . . .
H12 H 0.3271 0.3892 1.2599 0.077 Uiso 1 1 calc R . .
C13 C 0.1694(5) 0.2833(4) 1.1662(4) 0.0612(12) Uani 1 1 d . . .
H13 H 0.1637 0.2253 1.1947 0.073 Uiso 1 1 calc R . .
C14 C 0.0801(5) 0.2715(4) 1.0844(4) 0.0625(12) Uani 1 1 d . . .
H14 H 0.0160 0.2051 1.0579 0.075 Uiso 1 1 calc R . .
C15 C 0.0866(4) 0.3594(4) 1.0417(3) 0.0513(10) Uani 1 1 d . . .
H15 H 0.0256 0.3516 0.9879 0.062 Uiso 1 1 calc R . .
C16 C 0.0278(4) 0.1498(4) 0.8049(4) 0.0613(12) Uani 1 1 d . . .
H16 H 0.0522 0.2218 0.8404 0.074 Uiso 1 1 calc R . .
C17 C 0.0866(5) 0.0790(4) 0.8367(4) 0.0715(14) Uani 1 1 d . . .
H17 H 0.1489 0.1045 0.8931 0.086 Uiso 1 1 calc R . .
C18 C 0.0526(5) -0.0276(4) 0.7852(4) 0.0672(13) Uani 1 1 d . . .
H18 H 0.0919 -0.0740 0.8066 0.081 Uiso 1 1 calc R . .
C19 C -0.0418(5) -0.0663(4) 0.6999(4) 0.0617(12) Uani 1 1 d . . .
H19 H -0.0650 -0.1383 0.6648 0.074 Uiso 1 1 calc R . .
C20 C -0.1005(4) 0.0032(3) 0.6679(3) 0.0502(9) Uani 1 1 d . . .
H20 H -0.1625 -0.0229 0.6114 0.060 Uiso 1 1 calc R . .
C21 C -0.0673(4) 0.1137(3) 0.7204(3) 0.0422(8) Uani 1 1 d . . .
C22 C -0.1384(3) 0.1827(3) 0.6877(3) 0.0388(8) Uani 1 1 d . . .
C23 C -0.2567(3) 0.1476(3) 0.6241(3) 0.0403(8) Uani 1 1 d . . .
H23 H -0.3078 0.0758 0.5947 0.048 Uiso 1 1 calc R . .
C24 C -0.2807(3) 0.2435(3) 0.6148(3) 0.0397(8) Uani 1 1 d . . .
C25 C -0.3934(3) 0.2549(3) 0.5557(3) 0.0421(8) Uani 1 1 d . . .
C26 C -0.4643(4) 0.1736(4) 0.4719(3) 0.0517(10) Uani 1 1 d . . .
H26 H -0.4406 0.1136 0.4536 0.062 Uiso 1 1 calc R . .
C27 C -0.5708(5) 0.1822(5) 0.4156(4) 0.0689(14) Uani 1 1 d . . .
H27 H -0.6161 0.1288 0.3599 0.083 Uiso 1 1 calc R . .
C28 C -0.6078(5) 0.2713(5) 0.4437(4) 0.0767(16) Uani 1 1 d . . .
H28 H -0.6785 0.2767 0.4071 0.092 Uiso 1 1 calc R . .
C29 C -0.5395(5) 0.3514(5) 0.5259(4) 0.0725(14) Uani 1 1 d . . .
H29 H -0.5647 0.4105 0.5445 0.087 Uiso 1 1 calc R . .
C30 C -0.4319(4) 0.3442(4) 0.5818(4) 0.0585(11) Uani 1 1 d . . .
H30 H -0.3861 0.3991 0.6364 0.070 Uiso 1 1 calc R . .
C31 C -0.2242(5) 0.4755(4) 0.4184(4) 0.0682(13) Uani 1 1 d . . .
H31 H -0.1990 0.4403 0.4636 0.082 Uiso 1 1 calc R . .
C32 C -0.3273(6) 0.4148(5) 0.3412(4) 0.0858(18) Uani 1 1 d . . .
H32 H -0.3713 0.3424 0.3379 0.103 Uiso 1 1 calc R . .
C33 C -0.3620(6) 0.4622(7) 0.2721(4) 0.103(2) Uani 1 1 d . . .
H33 H -0.4287 0.4223 0.2201 0.124 Uiso 1 1 calc R . .
C34 C -0.2969(7) 0.5712(8) 0.2796(4) 0.115(3) Uani 1 1 d . . .
H34 H -0.3205 0.6039 0.2319 0.138 Uiso 1 1 calc R . .
C35 C -0.1968(5) 0.6329(6) 0.3574(4) 0.0857(19) Uani 1 1 d . . .
H35 H -0.1550 0.7061 0.3613 0.103 Uiso 1 1 calc R . .
C36 C -0.1592(4) 0.5843(4) 0.4298(3) 0.0490(9) Uani 1 1 d . . .
C37 C -0.0520(4) 0.6521(3) 0.5121(3) 0.0416(8) Uani 1 1 d . . .
C38 C 0.0411(4) 0.7483(4) 0.5163(3) 0.0477(9) Uani 1 1 d . . .
H38 H 0.0493 0.7837 0.4678 0.057 Uiso 1 1 calc R . .
C39 C 0.1206(4) 0.7815(3) 0.6088(3) 0.0419(8) Uani 1 1 d . . .
C40 C 0.2322(4) 0.8820(3) 0.6504(3) 0.0481(9) Uani 1 1 d . . .
C41 C 0.2393(5) 0.9756(4) 0.6145(4) 0.0643(12) Uani 1 1 d . . .
H41 H 0.1736 0.9748 0.5676 0.077 Uiso 1 1 calc R . .
C42 C 0.3451(6) 1.0698(5) 0.6496(5) 0.0841(18) Uani 1 1 d . . .
H42 H 0.3494 1.1308 0.6253 0.101 Uiso 1 1 calc R . .
C43 C 0.4447(6) 1.0723(5) 0.7213(5) 0.090(2) Uani 1 1 d . . .
H43 H 0.5149 1.1346 0.7437 0.109 Uiso 1 1 calc R . .
C44 C 0.4382(5) 0.9815(5) 0.7588(4) 0.0764(15) Uani 1 1 d . . .
H44 H 0.5028 0.9838 0.8075 0.092 Uiso 1 1 calc R . .
C45 C 0.3337(4) 0.8869(4) 0.7226(3) 0.0585(11) Uani 1 1 d . . .
H45 H 0.3308 0.8259 0.7466 0.070 Uiso 1 1 calc R . .
N1 N 0.1923(3) 0.6537(2) 0.9302(2) 0.0404(7) Uani 1 1 d . . .
N2 N 0.1662(3) 0.5478(2) 0.9426(2) 0.0422(7) Uani 1 1 d . . .
N3 N -0.0945(3) 0.2944(2) 0.7151(2) 0.0415(7) Uani 1 1 d . . .
N4 N -0.1829(3) 0.3324(2) 0.6702(2) 0.0423(7) Uani 1 1 d . . .
N5 N -0.0306(3) 0.6280(3) 0.5989(2) 0.0418(7) Uani 1 1 d . . .
N6 N 0.0762(3) 0.7078(3) 0.6588(2) 0.0412(7) Uani 1 1 d . . .
C46 C 0.5762(19) 0.7071(13) 0.0912(16) 0.190(13) Uani 0.50 1 d PD A 1
C47 C 0.5346(18) 0.6211(16) 0.0149(10) 0.146(9) Uani 0.50 1 d PD . 1
C48 C 0.5241(10) 0.5235(11) 0.0398(7) 0.069(3) Uani 0.50 1 d PD . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N6 Ag1 N1 178.44(12) . .
N6 Ag1 Ag3 63.02(9) . .
N1 Ag1 Ag3 115.70(9) . .
N2 Ag2 N3 169.66(13) . .
N5 Ag3 N4 169.34(13) . .
N5 Ag3 Ag1 62.32(9) . .
N4 Ag3 Ag1 121.56(9) . .
C2 C1 C6 121.0(4) . .
C3 C2 C1 120.4(5) . .
C2 C3 C4 119.7(4) . .
C5 C4 C3 119.5(4) . .
C4 C5 C6 120.7(4) . .
C1 C6 C5 118.8(4) . .
C1 C6 C7 118.5(3) . .
C5 C6 C7 122.7(4) . .
N1 C7 C8 109.4(3) . .
N1 C7 C6 122.3(3) . .
C8 C7 C6 128.2(3) . .
C7 C8 C9 105.4(3) . .
N2 C9 C8 109.4(3) . .
N2 C9 C10 123.8(3) . .
C8 C9 C10 126.7(3) . .
C15 C10 C11 118.8(4) . .
C15 C10 C9 122.6(3) . .
C11 C10 C9 118.6(3) . .
C12 C11 C10 120.8(4) . .
C13 C12 C11 119.6(4) . .
C14 C13 C12 120.4(4) . .
C13 C14 C15 120.3(4) . .
C10 C15 C14 120.1(4) . .
C21 C16 C17 121.1(4) . .
C18 C17 C16 120.5(5) . .
C17 C18 C19 119.8(5) . .
C20 C19 C18 120.1(5) . .
C19 C20 C21 121.1(4) . .
C16 C21 C20 117.4(4) . .
C16 C21 C22 123.1(4) . .
C20 C21 C22 119.4(4) . .
N3 C22 C23 109.1(3) . .
N3 C22 C21 123.2(3) . .
C23 C22 C21 127.7(3) . .
C24 C23 C22 105.4(3) . .
N4 C24 C23 109.4(3) . .
N4 C24 C25 122.2(3) . .
C23 C24 C25 128.4(3) . .
C30 C25 C26 118.3(4) . .
C30 C25 C24 121.9(4) . .
C26 C25 C24 119.8(4) . .
C25 C26 C27 120.8(5) . .
C28 C27 C26 119.8(5) . .
C29 C28 C27 120.0(5) . .
C28 C29 C30 120.5(5) . .
C25 C30 C29 120.6(5) . .
C36 C31 C32 122.9(5) . .
C33 C32 C31 119.7(6) . .
C32 C33 C34 119.2(6) . .
C33 C34 C35 121.4(6) . .
C34 C35 C36 120.0(6) . .
C31 C36 C35 116.7(5) . .
C31 C36 C37 124.5(4) . .
C35 C36 C37 118.8(4) . .
N5 C37 C38 108.4(3) . .
N5 C37 C36 123.9(4) . .
C38 C37 C36 127.8(3) . .
C37 C38 C39 106.4(3) . .
N6 C39 C38 108.8(3) . .
N6 C39 C40 123.7(3) . .
C38 C39 C40 127.5(3) . .
C41 C40 C45 118.1(4) . .
C41 C40 C39 119.0(4) . .
C45 C40 C39 122.9(4) . .
C42 C41 C40 120.3(5) . .
C41 C42 C43 120.4(5) . .
C44 C43 C42 120.1(5) . .
C43 C44 C45 119.6(5) . .
C44 C45 C40 121.6(5) . .
C7 N1 N2 108.1(3) . .
C7 N1 Ag1 130.0(2) . .
N2 N1 Ag1 121.1(2) . .
C9 N2 N1 107.7(3) . .
C9 N2 Ag2 132.7(2) . .
N1 N2 Ag2 116.8(2) . .
C22 N3 N4 108.1(3) . .
C22 N3 Ag2 137.1(3) . .
N4 N3 Ag2 113.3(2) . .
C24 N4 N3 108.0(3) . .
C24 N4 Ag3 128.8(2) . .
N3 N4 Ag3 114.6(2) . .
C37 N5 N6 108.8(3) . .
C37 N5 Ag3 131.8(3) . .
N6 N5 Ag3 118.6(2) . .
C39 N6 N5 107.6(3) . .
C39 N6 Ag1 136.2(3) . .
N5 N6 Ag1 115.9(2) . .
C46 C47 C48 112.1(14) . .
C46 C47 C48 152.2(17) . 2_665
C48 C47 C48 40.7(10) . 2_665
C48 C48 C47 89.3(14) 2_665 .
C48 C48 C47 50.0(10) 2_665 2_665
C47 C48 C47 139.3(10) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N6 2.121(3) .
Ag1 N1 2.126(3) .
Ag1 Ag3 3.3293(13) .
Ag2 N2 2.120(3) .
Ag2 N3 2.129(3) .
Ag3 N5 2.107(3) .
Ag3 N4 2.109(3) .
C1 C2 1.393(6) .
C1 C6 1.403(6) .
C2 C3 1.390(7) .
C3 C4 1.419(7) .
C4 C5 1.400(6) .
C5 C6 1.406(5) .
C6 C7 1.490(5) .
C7 N1 1.371(5) .
C7 C8 1.398(5) .
C8 C9 1.410(5) .
C9 N2 1.369(5) .
C9 C10 1.496(5) .
C10 C15 1.407(6) .
C10 C11 1.409(6) .
C11 C12 1.406(6) .
C12 C13 1.394(7) .
C13 C14 1.391(7) .
C14 C15 1.407(6) .
C16 C21 1.406(6) .
C16 C17 1.409(7) .
C17 C18 1.375(8) .
C18 C19 1.410(8) .
C19 C20 1.393(6) .
C20 C21 1.423(6) .
C21 C22 1.487(5) .
C22 N3 1.363(5) .
C22 C23 1.413(5) .
C23 C24 1.399(5) .
C24 N4 1.368(5) .
C24 C25 1.504(5) .
C25 C30 1.402(6) .
C25 C26 1.410(6) .
C26 C27 1.411(7) .
C27 C28 1.395(8) .
C28 C29 1.383(8) .
C29 C30 1.411(7) .
C31 C36 1.375(7) .
C31 C32 1.409(7) .
C32 C33 1.348(10) .
C33 C34 1.389(11) .
C34 C35 1.398(9) .
C35 C36 1.409(7) .
C36 C37 1.493(6) .
C37 N5 1.375(5) .
C37 C38 1.395(6) .
C38 C39 1.412(5) .
C39 N6 1.371(5) .
C39 C40 1.495(6) .
C40 C41 1.414(6) .
C40 C45 1.417(6) .
C41 C42 1.406(7) .
C42 C43 1.409(9) .
C43 C44 1.394(9) .
C44 C45 1.401(7) .
N1 N2 1.392(4) .
N3 N4 1.391(5) .
N5 N6 1.390(4) .
C46 C47 1.346(17) .
C47 C48 1.378(17) .
C47 C48 1.80(3) 2_665
C48 C48 1.17(2) 2_665
C48 C47 1.80(3) 2_665
