#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:07:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180169 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/65/7106570.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_7106570
loop_
_publ_author_name
'Jin Jin'
'Weiyin Wang'
'Yanhua Liu'
'Hongwei Hou'
'Yaoting Fan'
_publ_section_title
;
 A precise hexagonal octadecanuclear Ag macrocycle with significant
 luminescent properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              7461
_journal_paper_doi               10.1039/c1cc12142a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C45 H42 Ag3 Cl2 N18 O15'
_chemical_formula_weight         1469.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 108.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.978(2)
_cell_length_b                   14.054(3)
_cell_length_c                   18.062(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2877.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0230
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.183
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          3.742
_refine_ls_shift/su_mean         0.069
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1337P)²+5.9721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.2680
_reflns_number_gt                4783
_reflns_number_total             5287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12142a.txt
_cod_data_source_block           a
_cod_original_cell_volume        2877.9(10)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7106570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.32780(7) 0.49480(5) 0.46861(4) 0.0869(3) Uani 1 1 d . . .
Ag2 Ag -0.15034(11) 0.7500 0.39891(7) 0.1370(7) Uani 1 2 d S . .
N1 N 0.3547(6) 0.4893(5) 0.5904(4) 0.0718(17) Uani 1 1 d . . .
N2 N 0.3613(6) 0.5239(4) 0.7075(3) 0.0653(15) Uani 1 1 d . . .
N3 N 0.4098(8) 0.4369(6) 0.7125(4) 0.095(2) Uani 1 1 d . . .
N4 N 0.3127(7) 0.4883(4) 0.3482(4) 0.0745(18) Uani 1 1 d . . .
N5 N 0.2937(5) 0.5241(4) 0.2290(3) 0.0578(14) Uani 1 1 d . . .
N6 N 0.3378(7) 0.4350(4) 0.2397(4) 0.0802(19) Uani 1 1 d . . .
N7 N -0.1505(10) 0.7500 0.5168(7) 0.108(4) Uani 1 2 d S . .
N8 N -0.0943(8) 0.7500 0.6427(6) 0.080(3) Uani 1 2 d S . .
N9 N -0.2162(10) 0.7500 0.6163(9) 0.101(4) Uani 1 2 d S . .
N10 N -0.1735(11) 0.7500 0.2757(7) 0.124(5) Uani 1 2 d S . .
N11 N -0.1527(8) 0.7500 0.1619(6) 0.087(3) Uani 1 2 d S . .
N12 N -0.2694(12) 0.7500 0.1466(9) 0.191(11) Uani 1 2 d S . .
Cl1 Cl 0.0164(13) 0.5232(12) 0.4776(7) 0.188(5) Uani 0.50 1 d P . .
Cl2 Cl 0.4118(3) 0.7500 0.4847(2) 0.0873(9) Uani 1 2 d S . .
O1 O 0.5563(4) 0.4236(4) 0.0097(4) 0.093(2) Uani 1 1 d . . .
O2 O 0.7223(5) 0.5039(3) 0.0401(4) 0.0779(17) Uani 1 1 d . . .
O3 O 1.0946(4) 0.3292(3) 0.0778(3) 0.0645(12) Uani 1 1 d . . .
O4 O 0.326(2) 0.7500 0.514(2) 0.293(15) Uani 1 2 d S . .
O5 O 0.364(3) 0.7500 0.4061(10) 0.274(14) Uani 1 2 d S . .
O6 O 0.4770(9) 0.6661(8) 0.5046(7) 0.169(4) Uani 1 1 d . . .
O7 O 0.3210(11) 0.3418(5) 0.0638(5) 0.165(4) Uani 1 1 d . . .
O8 O 0.0933(19) 0.552(6) 0.414(3) 0.92(10) Uani 0.50 1 d P . .
H8 H 0.0961 0.5060 0.3871 1.387 Uiso 0.50 1 calc PR . .
O9 O 0.074(2) 0.599(3) 0.505(3) 0.34(3) Uani 0.50 1 d P . .
O10 O -0.0767(17) 0.547(3) 0.4326(19) 0.238(18) Uani 0.50 1 d P . .
C1 C 1.0435(8) 0.2500 0.0733(5) 0.0497(19) Uani 1 2 d S . .
C2 C 0.9133(6) 0.2500 0.0611(4) 0.0381(16) Uani 1 2 d S . .
C3 C 0.8522(5) 0.3345(4) 0.0538(3) 0.0402(12) Uani 1 1 d . . .
H3 H 0.8931 0.3917 0.0588 0.048 Uiso 1 1 calc R . .
C4 C 0.7316(5) 0.3365(4) 0.0392(3) 0.0410(12) Uani 1 1 d . . .
C5 C 0.6718(7) 0.2500 0.0320(5) 0.0432(18) Uani 1 2 d S . .
H5 H 0.5907 0.2500 0.0223 0.052 Uiso 1 2 calc SR . .
C6 C 0.6678(5) 0.4289(4) 0.0295(4) 0.0521(15) Uani 1 1 d . . .
C7 C 0.4038(9) 0.7500 0.1839(7) 0.078(3) Uani 1 2 d S . .
H7A H 0.4347 0.7020 0.2229 0.117 Uiso 0.50 1 calc PR . .
H7B H 0.4333 0.8112 0.2049 0.117 Uiso 0.50 1 calc PR . .
H7C H 0.4280 0.7368 0.1391 0.117 Uiso 0.50 1 calc PR . .
C8 C 0.2720(7) 0.7500 0.1599(5) 0.0491(19) Uani 1 2 d S . .
C9 C 0.2087(5) 0.6644(4) 0.1480(3) 0.0477(13) Uani 1 1 d . . .
C10 C 0.2730(8) 0.5716(5) 0.1532(4) 0.0679(19) Uani 1 1 d . . .
H10A H 0.2274 0.5298 0.1117 0.082 Uiso 1 1 calc R . .
H10B H 0.3482 0.5831 0.1453 0.082 Uiso 1 1 calc R . .
C11 C 0.0866(6) 0.6640(4) 0.1290(3) 0.0505(14) Uani 1 1 d . . .
C12 C 0.0221(9) 0.5681(7) 0.1170(5) 0.093(3) Uani 1 1 d . . .
H12A H -0.0408 0.5708 0.1390 0.140 Uiso 1 1 calc R . .
H12B H 0.0765 0.5188 0.1424 0.140 Uiso 1 1 calc R . .
H12C H -0.0097 0.5545 0.0621 0.140 Uiso 1 1 calc R . .
C13 C 0.0265(7) 0.7500 0.1211(5) 0.052(2) Uani 1 2 d S . .
C14 C -0.1095(9) 0.7500 0.0966(7) 0.091(4) Uani 1 2 d S . .
H14A H -0.1396 0.8058 0.0648 0.109 Uiso 0.50 1 calc PR . .
H14B H -0.1396 0.6942 0.0648 0.109 Uiso 0.50 1 calc PR . .
C15 C -0.1026(12) 0.7500 0.2358(8) 0.121(6) Uani 1 2 d S . .
C16 C -0.2774(14) 0.7500 0.2206(11) 0.188(13) Uani 1 2 d S . .
C17 C 0.2794(7) 0.5546(6) 0.2942(4) 0.071(2) Uani 1 1 d . . .
H17 H 0.2502 0.6141 0.3011 0.085 Uiso 1 1 calc R . .
C18 C 0.3468(9) 0.4163(6) 0.3124(5) 0.083(2) Uani 1 1 d . . .
H18 H 0.3743 0.3586 0.3366 0.100 Uiso 1 1 calc R . .
C19 C 0.3288(8) 0.5537(6) 0.6341(4) 0.074(2) Uani 1 1 d . . .
H19 H 0.2928 0.6118 0.6164 0.089 Uiso 1 1 calc R . .
C20 C 0.4038(8) 0.4203(7) 0.6395(5) 0.086(2) Uani 1 1 d . . .
H20 H 0.4317 0.3646 0.6240 0.103 Uiso 1 1 calc R . .
C21 C -0.0611(13) 0.7500 0.5805(8) 0.120(6) Uani 1 2 d S . .
C22 C -0.2406(13) 0.7500 0.5411(9) 0.092(4) Uani 1 2 d S . .
C23 C -0.0298(13) 0.7500 0.7281(8) 0.116(5) Uani 1 2 d S . .
H23A H -0.0513 0.6941 0.7519 0.139 Uiso 0.50 1 calc PR . .
H23B H -0.0513 0.8059 0.7519 0.139 Uiso 0.50 1 calc PR . .
C24 C 0.1058(10) 0.7500 0.7424(6) 0.078(4) Uani 1 2 d S . .
C25 C 0.1012(10) 0.5704(8) 0.7412(6) 0.108(3) Uani 1 1 d . . .
H25A H 0.1404 0.5233 0.7200 0.161 Uiso 1 1 calc R . .
H25B H 0.0216 0.5781 0.7070 0.161 Uiso 1 1 calc R . .
H25C H 0.1005 0.5504 0.7919 0.161 Uiso 1 1 calc R . .
C26 C 0.1652(7) 0.6632(7) 0.7485(4) 0.075(2) Uani 1 1 d . . .
C27 C 0.2853(7) 0.6646(6) 0.7626(4) 0.0659(18) Uani 1 1 d . . .
C28 C 0.3456(10) 0.7500 0.7667(5) 0.067(3) Uani 1 2 d S . .
C29 C 0.3557(8) 0.5725(6) 0.7790(4) 0.081(2) Uani 1 1 d . . .
H29A H 0.4354 0.5864 0.8125 0.097 Uiso 1 1 calc R . .
H29B H 0.3206 0.5297 0.8074 0.097 Uiso 1 1 calc R . .
C30 C 0.4767(10) 0.7500 0.7735(8) 0.085(3) Uani 1 2 d S . .
H30A H 0.5236 0.7373 0.8266 0.128 Uiso 0.50 1 calc PR . .
H30B H 0.4976 0.8110 0.7580 0.128 Uiso 0.50 1 calc PR . .
H30C H 0.4908 0.7017 0.7400 0.128 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'
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
N1 Ag1 N4 174.2(2) . . ?
N7 Ag2 N10 173.0(4) . . ?
C19 N1 C20 104.2(7) . . ?
C19 N1 Ag1 128.1(5) . . ?
C20 N1 Ag1 127.7(6) . . ?
C19 N2 N3 109.7(7) . . ?
C19 N2 C29 130.2(7) . . ?
N3 N2 C29 120.1(6) . . ?
C20 N3 N2 102.2(6) . . ?
C17 N4 C18 104.2(7) . . ?
C17 N4 Ag1 129.4(5) . . ?
C18 N4 Ag1 126.2(5) . . ?
C17 N5 N6 109.4(6) . . ?
C17 N5 C10 130.9(6) . . ?
N6 N5 C10 119.7(5) . . ?
C18 N6 N5 103.4(6) . . ?
C21 N7 C22 103.9(12) . . ?
C21 N7 Ag2 128.4(9) . . ?
C22 N7 Ag2 127.6(10) . . ?
C21 N8 N9 106.5(11) . . ?
C21 N8 C23 133.7(11) . . ?
N9 N8 C23 119.7(10) . . ?
C22 N9 N8 102.6(11) . . ?
C15 N10 C16 102.2(13) . . ?
C15 N10 Ag2 134.1(10) . . ?
C16 N10 Ag2 123.7(10) . . ?
C15 N11 N12 108.9(12) . . ?
C15 N11 C14 133.6(11) . . ?
N12 N11 C14 117.5(10) . . ?
N11 N12 C16 101.4(13) . . ?
O10 Cl1 Cl1 100(2) . 3_566 ?
O10 Cl1 O9 108(2) . . ?
Cl1 Cl1 O9 116(3) 3_566 . ?
O10 Cl1 O8 94(2) . . ?
Cl1 Cl1 O8 159(3) 3_566 . ?
O9 Cl1 O8 74(3) . . ?
O10 Cl1 O10 139.8(17) . 3_566 ?
Cl1 Cl1 O10 39.9(12) 3_566 3_566 ?
O9 Cl1 O10 95(3) . 3_566 ?
O8 Cl1 O10 125(2) . 3_566 ?
O10 Cl1 O9 85(2) . 3_566 ?
Cl1 Cl1 O9 33.2(16) 3_566 3_566 ?
O9 Cl1 O9 149.3(19) . 3_566 ?
O8 Cl1 O9 134(2) . 3_566 ?
O10 Cl1 O9 60.5(12) 3_566 3_566 ?
O4 Cl2 O5 108(2) . . ?
O4 Cl2 O6 110.1(9) . 4_575 ?
O5 Cl2 O6 106.4(9) . 4_575 ?
O4 Cl2 O6 110.1(9) . . ?
O5 Cl2 O6 106.4(9) . . ?
O6 Cl2 O6 115.3(10) 4_575 . ?
Cl1 O9 Cl1 30.7(19) . 3_566 ?
Cl1 O10 Cl1 40.2(17) . 3_566 ?
O3 C1 O3 124.0(8) . 4_565 ?
O3 C1 C2 118.0(4) . . ?
O3 C1 C2 118.0(4) 4_565 . ?
C3 C2 C3 118.9(7) 4_565 . ?
C3 C2 C1 120.5(3) 4_565 . ?
C3 C2 C1 120.5(3) . . ?
C4 C3 C2 121.7(5) . . ?
C3 C4 C5 118.2(5) . . ?
C3 C4 C6 120.4(5) . . ?
C5 C4 C6 121.4(5) . . ?
C4 C5 C4 121.2(7) . 4_565 ?
O2 C6 O1 123.8(6) . . ?
O2 C6 C4 120.4(5) . . ?
O1 C6 C4 115.8(5) . . ?
C9 C8 C9 118.3(7) . 4_575 ?
C9 C8 C7 120.8(4) . . ?
C9 C8 C7 120.8(4) 4_575 . ?
C8 C9 C11 121.0(6) . . ?
C8 C9 C10 119.6(6) . . ?
C11 C9 C10 119.3(6) . . ?
N5 C10 C9 112.3(5) . . ?
C13 C11 C9 119.4(6) . . ?
C13 C11 C12 121.9(7) . . ?
C9 C11 C12 118.7(7) . . ?
C11 C13 C11 120.8(8) 4_575 . ?
C11 C13 C14 119.5(4) 4_575 . ?
C11 C13 C14 119.5(4) . . ?
N11 C14 C13 113.1(9) . . ?
N10 C15 N11 114.6(13) . . ?
N10 C16 N12 112.9(14) . . ?
N5 C17 N4 109.7(7) . . ?
N6 C18 N4 113.3(7) . . ?
N1 C19 N2 109.6(7) . . ?
N3 C20 N1 114.3(8) . . ?
N7 C21 N8 111.7(12) . . ?
N9 C22 N7 115.3(13) . . ?
N8 C23 C24 109.7(10) . . ?
C26 C24 C26 121.4(10) 4_575 . ?
C26 C24 C23 119.3(5) 4_575 . ?
C26 C24 C23 119.3(5) . . ?
C27 C26 C24 118.5(8) . . ?
C27 C26 C25 120.2(9) . . ?
C24 C26 C25 121.3(8) . . ?
C28 C27 C26 121.0(8) . . ?
C28 C27 C29 118.6(7) . . ?
C26 C27 C29 120.3(8) . . ?
C27 C28 C27 119.3(11) . 4_575 ?
C27 C28 C30 120.3(5) . . ?
C27 C28 C30 120.3(5) 4_575 . ?
N2 C29 C27 113.6(6) . . ?
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 2.120(7) . ?
Ag1 N4 2.126(7) . ?
Ag2 N7 2.129(11) . ?
Ag2 N10 2.153(12) . ?
N1 C19 1.303(11) . ?
N1 C20 1.316(10) . ?
N2 C19 1.323(9) . ?
N2 N3 1.343(10) . ?
N2 C29 1.482(10) . ?
N3 C20 1.317(11) . ?
N4 C17 1.314(9) . ?
N4 C18 1.334(10) . ?
N5 C17 1.316(9) . ?
N5 N6 1.349(8) . ?
N5 C10 1.470(8) . ?
N6 C18 1.308(10) . ?
N7 C21 1.294(18) . ?
N7 C22 1.291(18) . ?
N8 C21 1.308(16) . ?
N8 N9 1.382(15) . ?
N8 C23 1.485(17) . ?
N9 C22 1.295(19) . ?
N10 C15 1.279(18) . ?
N10 C16 1.32(2) . ?
N11 C15 1.274(16) . ?
N11 N12 1.335(16) . ?
N11 C14 1.432(14) . ?
N12 C16 1.37(2) . ?
Cl1 O10 1.19(3) . ?
Cl1 Cl1 1.20(2) 3_566 ?
Cl1 O9 1.29(4) . ?
Cl1 O8 1.74(7) . ?
Cl1 O10 1.83(4) 3_566 ?
Cl1 O9 2.11(6) 3_566 ?
Cl2 O4 1.306(19) . ?
Cl2 O5 1.348(17) . ?
Cl2 O6 1.396(10) 4_575 ?
Cl2 O6 1.396(10) . ?
O1 C6 1.268(8) . ?
O2 C6 1.221(8) . ?
O3 C1 1.261(6) . ?
O9 Cl1 2.11(5) 3_566 ?
O10 Cl1 1.83(4) 3_566 ?
C1 O3 1.261(6) 4_565 ?
C1 C2 1.502(11) . ?
C2 C3 1.380(7) 4_565 ?
C2 C3 1.380(7) . ?
C3 C4 1.382(7) . ?
C4 C5 1.396(6) . ?
C4 C6 1.488(8) . ?
C5 C4 1.396(6) 4_565 ?
C7 C8 1.497(13) . ?
C8 C9 1.402(7) . ?
C8 C9 1.402(7) 4_575 ?
C9 C11 1.390(9) . ?
C9 C10 1.503(9) . ?
C11 C13 1.391(8) . ?
C11 C12 1.534(10) . ?
C13 C11 1.391(8) 4_575 ?
C13 C14 1.545(13) . ?
C23 C24 1.560(18) . ?
C24 C26 1.398(11) 4_575 ?
C24 C26 1.398(10) . ?
C25 C26 1.497(13) . ?
C26 C27 1.378(11) . ?
C27 C28 1.390(10) . ?
C27 C29 1.521(12) . ?
C28 C27 1.390(9) 4_575 ?
C28 C30 1.535(16) . ?
