#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:51:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179350 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/47/4324709.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_4324709
loop_
_publ_author_name
'Yanping Zhang'
'Lili Li'
'Tao Sun'
'Bin Liu'
'Huaiming Hu'
'Ganglin Xue'
_publ_section_title
;
 A Cagelike Polyanion with a Ag+ Enwrapped, [AgAs2Mo15O54]11-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2613
_journal_page_last               2618
_journal_paper_doi               10.1021/ic102459r
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C4 H62 Ag As2 Mo15 N13 O60'
_chemical_formula_weight         2949.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   none
_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            4
_cell_length_a                   25.144(8)
_cell_length_b                   19.410(6)
_cell_length_c                   13.355(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6518(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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_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  0.0902
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30654
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    4.203
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.006
_exptl_crystal_description       block
_exptl_crystal_F_000             5600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.355
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0606
_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)+(0.0870P)²+9.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                3159
_reflns_number_total             5926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102459r_si_002.cif
_cod_data_source_block           xb2782
_cod_database_code               4324709
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Mo1 Mo 0.13530(4) 0.16909(6) 0.70652(10) 0.0410(3) Uani 1 1 d .
Mo2 Mo 0.17368(4) 0.07729(6) 0.48762(11) 0.0448(4) Uani 1 1 d .
Mo3 Mo 0.20503(5) 0.15780(7) 0.29351(11) 0.0534(4) Uani 1 1 d .
Mo4 Mo 0.31605(4) 0.09189(6) 0.45073(10) 0.0455(4) Uani 1 1 d .
Mo5 Mo 0.24431(6) 0.2500 0.83448(14) 0.0421(5) Uani 1 2 d S
Mo6 Mo 0.37330(5) 0.16505(6) 0.87348(11) 0.0494(4) Uani 1 1 d .
Mo7 Mo 0.40920(5) 0.07207(6) 0.65489(11) 0.0510(4) Uani 1 1 d .
Mo8 Mo 0.45209(5) 0.15775(7) 0.45829(11) 0.0523(4) Uani 1 1 d .
Ag1 Ag 0.27487(6) 0.2500 0.56732(15) 0.0626(5) Uani 1 2 d S
As1 As 0.17885(7) 0.2500 0.50029(16) 0.0364(5) Uani 1 2 d S
As2 As 0.36803(7) 0.2500 0.63265(16) 0.0383(5) Uani 1 2 d S
O1 O 0.1613(4) 0.1292(5) 0.8087(8) 0.057(3) Uani 1 1 d .
O2 O 0.1054(4) 0.2500 0.7690(10) 0.045(3) Uani 1 2 d S
O3 O 0.0776(3) 0.1274(5) 0.6839(8) 0.052(3) Uani 1 1 d .
O4 O 0.1281(4) 0.2500 0.5925(10) 0.039(3) Uani 1 2 d S
O5 O 0.1809(3) 0.1311(4) 0.6081(7) 0.041(2) Uani 1 1 d .
O6 O 0.2037(4) 0.2500 0.7239(10) 0.041(3) Uani 1 2 d S
O7 O 0.1567(3) 0.1809(4) 0.4259(7) 0.041(2) Uani 1 1 d .
O8 O 0.1119(3) 0.0469(5) 0.5046(8) 0.058(3) Uani 1 1 d .
O9 O 0.2160(4) 0.0123(5) 0.5248(8) 0.063(3) Uani 1 1 d .
O10 O 0.1790(3) 0.0711(4) 0.3463(8) 0.055(3) Uani 1 1 d .
O11 O 0.1591(5) 0.1714(5) 0.2023(8) 0.079(4) Uani 1 1 d .
O12 O 0.2591(4) 0.1258(6) 0.2304(10) 0.085(4) Uani 1 1 d .
O13 O 0.2283(5) 0.2500 0.3187(12) 0.059(4) Uani 1 2 d S
O14 O 0.2533(3) 0.1351(4) 0.4410(8) 0.051(3) Uani 1 1 d .
O15 O 0.3158(3) 0.0153(5) 0.3848(9) 0.065(3) Uani 1 1 d .
O16 O 0.3285(3) 0.0773(5) 0.5744(7) 0.052(3) Uani 1 1 d .
O17 O 0.3651(4) 0.1458(6) 0.4027(8) 0.061(3) Uani 1 1 d .
O18 O 0.2074(6) 0.2500 0.9392(11) 0.070(5) Uani 1 2 d S
O19 O 0.2839(3) 0.1767(4) 0.8365(8) 0.055(3) Uani 1 1 d .
O20 O 0.3572(5) 0.2500 0.9413(10) 0.051(4) Uani 1 2 d S
O21 O 0.3523(4) 0.1109(5) 0.9630(9) 0.072(3) Uani 1 1 d .
O22 O 0.4401(4) 0.1653(5) 0.8856(10) 0.071(3) Uani 1 1 d .
O23 O 0.3750(4) 0.2500 0.7596(11) 0.045(3) Uani 1 2 d S
O24 O 0.3669(3) 0.1082(4) 0.7602(8) 0.049(2) Uani 1 1 d .
O25 O 0.3972(5) -0.0142(5) 0.6668(9) 0.076(3) Uani 1 1 d .
O26 O 0.4084(3) 0.1808(4) 0.5987(7) 0.043(2) Uani 1 1 d .
O27 O 0.4698(4) 0.0843(5) 0.7089(8) 0.071(3) Uani 1 1 d .
O28 O 0.5105(4) 0.1717(5) 0.5199(9) 0.064(3) Uani 1 1 d .
O29 O 0.4346(5) 0.2500 0.4273(10) 0.050(4) Uani 1 2 d S
O30 O 0.4318(4) 0.0701(4) 0.5158(8) 0.056(3) Uani 1 1 d .
O31 O 0.4716(4) 0.1262(6) 0.3460(9) 0.076(3) Uani 1 1 d .
O101 O 0.2394(4) 0.9595(6) 0.2459(9) 0.078(3) Uiso 1 1 d .
O102 O 0.9960(7) 0.2500 0.7746(13) 0.091(5) Uiso 1 2 d S
O103 O 0.1066(9) 0.2500 0.0265(17) 0.129(8) Uiso 1 2 d S
O104 O 0.3507(7) 0.2500 0.2745(15) 0.106(6) Uiso 1 2 d S
O105 O 0.4492(7) 0.9016(9) 0.8033(12) 0.137(6) Uiso 1 1 d .
O106 O 0.2767(7) 0.8936(9) 0.5161(13) 0.147(6) Uiso 1 1 d .
O107 O 0.5015(8) 0.0263(10) 0.9021(15) 0.174(7) Uiso 1 1 d .
O108 O 0.0540(10) 0.2500 0.234(2) 0.164(10) Uiso 1 2 d S
O109 O 0.5286(9) 0.1830(13) 0.0288(18) 0.224(10) Uiso 1 1 d .
O110 O 0.3895(10) 0.8964(13) 0.5132(19) 0.226(10) Uiso 1 1 d .
O111 O 0.2964(15) 0.2500 0.097(3) 0.235(16) Uiso 1 2 d S
C1 C 0.4078(5) 0.0188(7) 0.2728(9) 0.038(3) Uiso 1 1 d D
C2 C 0.3826(10) 0.0561(13) 0.1894(16) 0.152(10) Uiso 1 1 d D
N1 N 0.4261(7) -0.0150(9) 0.3380(12) 0.118(6) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
H H 0.0000 0.0000 '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
O3 Mo1 O1 104.8(5) . .
O3 Mo1 O5 102.1(4) . .
O1 Mo1 O5 98.5(4) . .
O3 Mo1 O2 97.7(4) . .
O1 Mo1 O2 100.0(5) . .
O5 Mo1 O2 148.5(4) . .
O3 Mo1 O4 98.5(4) . .
O1 Mo1 O4 156.1(4) . .
O5 Mo1 O4 81.2(4) . .
O2 Mo1 O4 71.7(4) . .
O3 Mo1 O6 166.1(4) . .
O1 Mo1 O6 86.8(4) . .
O5 Mo1 O6 83.4(4) . .
O2 Mo1 O6 72.4(4) . .
O4 Mo1 O6 69.5(4) . .
O3 Mo1 Mo1 118.7(3) . 7_565
O1 Mo1 Mo1 117.1(3) . 7_565
O5 Mo1 Mo1 112.9(3) . 7_565
O2 Mo1 Mo1 35.6(3) . 7_565
O4 Mo1 Mo1 44.3(2) . 7_565
O6 Mo1 Mo1 47.84(17) . 7_565
O8 Mo2 O9 106.0(5) . .
O8 Mo2 O10 100.2(4) . .
O9 Mo2 O10 101.3(5) . .
O8 Mo2 O5 99.5(4) . .
O9 Mo2 O5 95.7(4) . .
O10 Mo2 O5 149.2(4) . .
O8 Mo2 O7 101.0(4) . .
O9 Mo2 O7 153.0(4) . .
O10 Mo2 O7 72.6(4) . .
O5 Mo2 O7 80.6(3) . .
O8 Mo2 O14 168.9(4) . .
O9 Mo2 O14 84.3(4) . .
O10 Mo2 O14 73.1(4) . .
O5 Mo2 O14 83.3(3) . .
O7 Mo2 O14 68.7(3) . .
O11 Mo3 O12 104.0(6) . .
O11 Mo3 O13 100.9(5) . .
O12 Mo3 O13 100.5(5) . .
O11 Mo3 O10 99.6(5) . .
O12 Mo3 O10 97.6(5) . .
O13 Mo3 O10 148.4(6) . .
O11 Mo3 O7 99.8(5) . .
O12 Mo3 O7 155.4(5) . .
O13 Mo3 O7 80.6(5) . .
O10 Mo3 O7 72.4(4) . .
O11 Mo3 O14 168.2(5) . .
O12 Mo3 O14 86.2(5) . .
O13 Mo3 O14 82.5(5) . .
O10 Mo3 O14 73.0(4) . .
O7 Mo3 O14 69.5(3) . .
O16 Mo4 O15 110.5(5) . .
O16 Mo4 O17 109.1(4) . .
O15 Mo4 O17 109.4(5) . .
O16 Mo4 O14 108.0(4) . .
O15 Mo4 O14 111.3(4) . .
O17 Mo4 O14 108.4(5) . .
O18 Mo5 O19 107.7(4) . 7_565
O18 Mo5 O19 107.7(4) . .
O19 Mo5 O19 110.1(6) 7_565 .
O18 Mo5 O6 111.7(6) . .
O19 Mo5 O6 109.8(4) 7_565 .
O19 Mo5 O6 109.8(4) . .
O21 Mo6 O22 104.3(5) . .
O21 Mo6 O24 100.3(5) . .
O22 Mo6 O24 99.4(5) . .
O21 Mo6 O20 97.8(5) . .
O22 Mo6 O20 99.3(5) . .
O24 Mo6 O20 149.8(5) . .
O21 Mo6 O23 161.8(5) . .
O22 Mo6 O23 92.5(5) . .
O24 Mo6 O23 83.6(4) . .
O20 Mo6 O23 72.2(5) . .
O21 Mo6 O19 84.7(4) . .
O22 Mo6 O19 171.0(5) . .
O24 Mo6 O19 78.6(4) . .
O20 Mo6 O19 79.2(4) . .
O23 Mo6 O19 78.6(4) . .
O27 Mo7 O25 104.8(5) . .
O27 Mo7 O24 97.8(5) . .
O25 Mo7 O24 101.2(5) . .
O27 Mo7 O30 98.4(5) . .
O25 Mo7 O30 96.9(5) . .
O24 Mo7 O30 151.7(4) . .
O27 Mo7 O26 91.1(4) . .
O25 Mo7 O26 162.3(5) . .
O24 Mo7 O26 84.0(4) . .
O30 Mo7 O26 72.6(3) . .
O27 Mo7 O16 169.1(4) . .
O25 Mo7 O16 86.0(5) . .
O24 Mo7 O16 80.5(4) . .
O30 Mo7 O16 79.2(4) . .
O26 Mo7 O16 78.1(3) . .
O31 Mo8 O28 103.6(5) . .
O31 Mo8 O29 102.5(6) . .
O28 Mo8 O29 99.0(5) . .
O31 Mo8 O30 96.3(5) . .
O28 Mo8 O30 100.1(5) . .
O29 Mo8 O30 149.2(5) . .
O31 Mo8 O26 164.8(4) . .
O28 Mo8 O26 89.3(4) . .
O29 Mo8 O26 83.1(5) . .
O30 Mo8 O26 73.2(3) . .
O31 Mo8 O17 87.3(5) . .
O28 Mo8 O17 169.0(4) . .
O29 Mo8 O17 78.8(4) . .
O30 Mo8 O17 77.9(4) . .
O26 Mo8 O17 79.8(3) . .
As2 Ag1 As1 179.92(11) . .
O7 As1 O7 99.3(6) . 7_565
O7 As1 O4 99.5(4) . .
O7 As1 O4 99.5(4) 7_565 .
O7 As1 Ag1 119.5(3) . .
O7 As1 Ag1 119.5(3) 7_565 .
O4 As1 Ag1 115.7(4) . .
O23 As2 O26 101.5(4) . 7_565
O23 As2 O26 101.5(4) . .
O26 As2 O26 100.9(6) 7_565 .
O23 As2 Ag1 116.4(4) . .
O26 As2 Ag1 117.0(3) 7_565 .
O26 As2 Ag1 117.0(3) . .
Mo1 O2 Mo1 108.9(6) . 7_565
As1 O4 Mo1 115.0(4) . 7_565
As1 O4 Mo1 115.0(4) . .
Mo1 O4 Mo1 91.3(5) 7_565 .
Mo1 O5 Mo2 137.2(4) . .
Mo5 O6 Mo1 120.0(4) . .
Mo5 O6 Mo1 120.0(4) . 7_565
Mo1 O6 Mo1 84.3(3) . 7_565
As1 O7 Mo3 115.9(4) . .
As1 O7 Mo2 114.9(4) . .
Mo3 O7 Mo2 90.4(3) . .
Mo2 O10 Mo3 109.3(4) . .
Mo3 O13 Mo3 138.6(8) . 7_565
Mo4 O14 Mo3 127.1(5) . .
Mo4 O14 Mo2 120.1(4) . .
Mo3 O14 Mo2 82.7(3) . .
Mo4 O16 Mo7 128.5(5) . .
Mo4 O17 Mo8 127.6(5) . .
Mo5 O19 Mo6 129.8(5) . .
Mo6 O20 Mo6 117.9(7) . 7_565
As2 O23 Mo6 132.2(3) . 7_565
As2 O23 Mo6 132.2(3) . .
Mo6 O23 Mo6 94.6(6) 7_565 .
Mo6 O24 Mo7 139.9(5) . .
As2 O26 Mo8 131.5(5) . .
As2 O26 Mo7 130.1(5) . .
Mo8 O26 Mo7 95.1(3) . .
Mo8 O29 Mo8 142.7(8) 7_565 .
Mo8 O30 Mo7 116.0(5) . .
N1 C1 C2 176(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.688(8) .
Mo1 O1 1.700(9) .
Mo1 O5 1.894(9) .
Mo1 O2 1.931(7) .
Mo1 O4 2.195(9) .
Mo1 O6 2.340(8) .
Mo1 Mo1 3.141(2) 7_565
Mo2 O8 1.678(9) .
Mo2 O9 1.724(9) .
Mo2 O10 1.896(10) .
Mo2 O5 1.927(9) .
Mo2 O7 2.215(9) .
Mo2 O14 2.379(9) .
Mo3 O11 1.700(12) .
Mo3 O12 1.716(10) .
Mo3 O13 1.913(5) .
Mo3 O10 1.938(9) .
Mo3 O7 2.192(9) .
Mo3 O14 2.356(10) .
Mo4 O16 1.705(10) .
Mo4 O15 1.728(9) .
Mo4 O17 1.740(9) .
Mo4 O14 1.790(8) .
Mo5 O18 1.679(17) .
Mo5 O19 1.736(8) 7_565
Mo5 O19 1.736(8) .
Mo5 O6 1.796(12) .
Mo6 O21 1.676(11) .
Mo6 O22 1.687(9) .
Mo6 O24 1.879(9) .
Mo6 O20 1.924(7) .
Mo6 O23 2.243(10) .
Mo6 O19 2.314(9) .
Mo7 O27 1.703(10) .
Mo7 O25 1.709(10) .
Mo7 O24 1.898(9) .
Mo7 O30 1.943(10) .
Mo7 O26 2.239(8) .
Mo7 O16 2.299(9) .
Mo8 O31 1.692(11) .
Mo8 O28 1.706(10) .
Mo8 O29 1.890(4) .
Mo8 O30 1.935(9) .
Mo8 O26 2.219(9) .
Mo8 O17 2.321(9) .
Ag1 As2 2.500(2) .
Ag1 As1 2.575(2) .
As1 O7 1.759(8) .
As1 O7 1.759(8) 7_565
As1 O4 1.773(11) .
As2 O23 1.705(15) .
As2 O26 1.744(8) 7_565
As2 O26 1.744(8) .
O2 Mo1 1.931(7) 7_565
O4 Mo1 2.195(9) 7_565
O6 Mo1 2.340(8) 7_565
O13 Mo3 1.913(5) 7_565
O20 Mo6 1.924(7) 7_565
O23 Mo6 2.243(10) 7_565
O29 Mo8 1.890(4) 7_565
C1 N1 1.183(9) .
C1 C2 1.472(10) .
