#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:52:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179132 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309456.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_4309456
loop_
_publ_author_name
'Haiyan An'
'Yangguang Li'
'Enbo Wang'
'Dongrong Xiao'
'Chunyan Sun'
'Lin Xu'
_publ_section_title
;
Self-Assembly of a Series of Extended Architectures Based on
Polyoxometalate Clusters and Silver Coordination Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6062
_journal_page_last               6070
_journal_paper_doi               10.1021/ic050636x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H36 Ag Cr Mo6 N4 O36'
_chemical_formula_weight         1692.08
_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                97.40(3)
_cell_angle_beta                 112.38(3)
_cell_angle_gamma                113.59(3)
_cell_formula_units_Z            1
_cell_length_a                   10.458(2)
_cell_length_b                   10.644(2)
_cell_length_c                   12.295(3)
_cell_measurement_reflns_used    10692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.27
_cell_volume                     1094.1(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_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_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP diffractomete'
_diffrn_measurement_method       'Oscillation 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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10692
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.458
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             819
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0156(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0268
_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)+(0.0460P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                4431
_reflns_number_total             4942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050636xsi20050617_052340.cif
_cod_data_source_block           aa110b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1094.0(4)
_cod_database_code               4309456
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
Cr1 Cr 0.0000 0.0000 0.0000 0.01342(12) Uani 1 2 d S . .
Mo1 Mo 0.16498(2) 0.32021(2) 0.212368(19) 0.01655(8) Uani 1 1 d . . .
Mo2 Mo -0.08466(3) 0.02151(3) 0.23530(2) 0.01889(8) Uani 1 1 d . . .
Mo3 Mo -0.24941(2) -0.29970(2) 0.02118(2) 0.01772(8) Uani 1 1 d . . .
Ag1 Ag 0.0000 0.5000 0.0000 0.04820(14) Uani 1 2 d S . .
O1 O 0.1178(2) 0.0824(2) 0.18418(16) 0.0167(4) Uani 1 1 d . . .
H1 H 0.181(6) 0.054(6) 0.214(5) 0.075(16) Uiso 1 1 d . . .
O2 O -0.1894(2) -0.0685(2) 0.02512(17) 0.0170(4) Uani 1 1 d . . .
H2 H -0.255(4) -0.058(4) -0.012(3) 0.030(10) Uiso 1 1 d . . .
O3 O -0.0363(2) -0.19700(19) -0.00898(16) 0.0154(4) Uani 1 1 d . . .
H3 H 0.061(5) -0.193(5) 0.045(4) 0.046(11) Uiso 1 1 d . . .
O4 O -0.0356(2) 0.2052(2) 0.20563(18) 0.0207(4) Uani 1 1 d . . .
O5 O -0.1077(2) -0.1724(2) 0.19359(17) 0.0214(4) Uani 1 1 d . . .
O6 O -0.3237(2) -0.3406(2) -0.15885(16) 0.0197(4) Uani 1 1 d . . .
O7 O 0.1365(2) 0.4636(2) 0.18435(19) 0.0252(4) Uani 1 1 d . . .
O8 O 0.2893(2) 0.3783(2) 0.36831(18) 0.0291(5) Uani 1 1 d . . .
O9 O -0.2641(3) -0.0191(3) 0.2254(2) 0.0327(5) Uani 1 1 d . . .
O10 O 0.0439(3) 0.0757(3) 0.39016(19) 0.0322(5) Uani 1 1 d . . .
O11 O -0.4288(2) -0.3404(3) 0.0113(2) 0.0317(5) Uani 1 1 d . . .
O12 O -0.2192(2) -0.4442(2) 0.04266(19) 0.0288(5) Uani 1 1 d . . .
O13 O 0.1931(3) 0.7648(2) 0.1049(2) 0.0374(6) Uani 1 1 d . . .
O14 O 0.2876(3) 0.9439(3) 0.2797(2) 0.0384(6) Uani 1 1 d . . .
O15 O 0.2613(3) -1.5214(3) -0.3850(2) 0.0380(6) Uani 1 1 d . . .
O16 O 0.4627(3) -1.2928(3) -0.3041(2) 0.0364(6) Uani 1 1 d . . .
H16 H 0.532(5) -1.332(5) -0.253(5) 0.071(15) Uiso 1 1 d . . .
C1 C 0.5726(4) 0.7758(4) 0.4705(3) 0.0351(7) Uani 1 1 d . . .
H1A H 0.608(4) 0.779(4) 0.552(4) 0.033(9) Uiso 1 1 d . . .
C2 C 0.4690(4) 0.8227(4) 0.4120(3) 0.0297(6) Uani 1 1 d . . .
H2A H 0.457(5) 0.874(5) 0.454(4) 0.050(13) Uiso 1 1 d . . .
C3 C 0.4074(3) 0.7952(3) 0.2841(3) 0.0218(6) Uani 1 1 d . . .
C4 C 0.4553(3) 0.7248(3) 0.2198(3) 0.0268(6) Uani 1 1 d . . .
H4A H 0.423(4) 0.697(4) 0.143(3) 0.027(9) Uiso 1 1 d . . .
C5 C 0.5609(4) 0.6816(4) 0.2820(3) 0.0305(6) Uani 1 1 d . . .
H5A H 0.605(4) 0.647(4) 0.249(3) 0.023(8) Uiso 1 1 d . . .
C6 C 0.2867(3) 0.8407(3) 0.2195(3) 0.0271(6) Uani 1 1 d . . .
C7 C 0.1592(4) -1.1539(4) -0.5062(3) 0.0336(7) Uani 1 1 d . . .
H7A H 0.161(4) -1.069(4) -0.489(3) 0.017(8) Uiso 1 1 d . . .
C8 C 0.2478(4) -1.1996(4) -0.4241(3) 0.0304(7) Uani 1 1 d . . .
H8A H 0.318(5) -1.139(5) -0.352(4) 0.047(12) Uiso 1 1 d . . .
C9 C 0.2203(3) -1.3398(3) -0.4611(3) 0.0246(6) Uani 1 1 d . . .
C10 C 0.1015(4) -1.4336(4) -0.5806(3) 0.0298(6) Uani 1 1 d . . .
H10A H 0.079(3) -1.526(4) -0.599(3) 0.015(7) Uiso 1 1 d . . .
C11 C 0.0206(4) -1.3804(4) -0.6607(3) 0.0349(7) Uani 1 1 d . . .
H11A H -0.057(4) -1.436(4) -0.745(3) 0.023(8) Uiso 1 1 d . . .
C12 C 0.3166(3) -1.3956(4) -0.3787(3) 0.0270(6) Uani 1 1 d . . .
N1 N 0.6133(3) 0.7063(3) 0.4039(3) 0.0310(6) Uani 1 1 d . . .
H1B H 0.682(5) 0.687(4) 0.451(4) 0.041(10) Uiso 1 1 d . . .
N2 N 0.0516(3) -1.2442(3) -0.6221(2) 0.0321(6) Uani 1 1 d . . .
H2B H 0.000(5) -1.222(5) -0.677(4) 0.054(13) Uiso 1 1 d . . .
OW1 O -0.2750(4) 0.2869(4) 0.1402(4) 0.0669(10) Uani 1 1 d . . .
OW2 O -0.4449(3) -0.0416(3) -0.0934(3) 0.0556(8) 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'
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'
Cr Cr 0.3209 0.6236 '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'
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
O3 Cr1 O3 180.0 2 . ?
O3 Cr1 O1 95.74(9) 2 2 ?
O3 Cr1 O1 84.26(9) . 2 ?
O3 Cr1 O1 84.26(9) 2 . ?
O3 Cr1 O1 95.74(9) . . ?
O1 Cr1 O1 180.00(12) 2 . ?
O3 Cr1 O2 97.55(9) 2 . ?
O3 Cr1 O2 82.45(9) . . ?
O1 Cr1 O2 96.08(9) 2 . ?
O1 Cr1 O2 83.92(9) . . ?
O3 Cr1 O2 82.45(9) 2 2 ?
O3 Cr1 O2 97.55(9) . 2 ?
O1 Cr1 O2 83.92(9) 2 2 ?
O1 Cr1 O2 96.08(9) . 2 ?
O2 Cr1 O2 180.00(9) . 2 ?
O8 Mo1 O7 105.54(11) . . ?
O8 Mo1 O4 100.66(10) . . ?
O7 Mo1 O4 97.00(9) . . ?
O8 Mo1 O6 96.57(10) . 2 ?
O7 Mo1 O6 101.02(9) . 2 ?
O4 Mo1 O6 150.68(9) . 2 ?
O8 Mo1 O3 161.39(10) . 2 ?
O7 Mo1 O3 91.50(9) . 2 ?
O4 Mo1 O3 84.28(9) . 2 ?
O6 Mo1 O3 72.38(8) 2 2 ?
O8 Mo1 O1 93.60(10) . . ?
O7 Mo1 O1 159.38(8) . . ?
O4 Mo1 O1 71.47(8) . . ?
O6 Mo1 O1 83.99(8) 2 . ?
O3 Mo1 O1 70.78(7) 2 . ?
O9 Mo2 O10 106.01(12) . . ?
O9 Mo2 O4 97.57(10) . . ?
O10 Mo2 O4 101.99(10) . . ?
O9 Mo2 O5 100.84(11) . . ?
O10 Mo2 O5 95.89(11) . . ?
O4 Mo2 O5 149.64(9) . . ?
O9 Mo2 O2 92.70(10) . . ?
O10 Mo2 O2 159.55(10) . . ?
O4 Mo2 O2 83.22(9) . . ?
O5 Mo2 O2 72.04(8) . . ?
O9 Mo2 O1 160.81(9) . . ?
O10 Mo2 O1 92.03(10) . . ?
O4 Mo2 O1 71.74(8) . . ?
O5 Mo2 O1 83.39(8) . . ?
O2 Mo2 O1 70.62(8) . . ?
O11 Mo3 O12 107.20(11) . . ?
O11 Mo3 O5 100.96(11) . . ?
O12 Mo3 O5 95.90(9) . . ?
O11 Mo3 O6 95.05(10) . . ?
O12 Mo3 O6 101.30(10) . . ?
O5 Mo3 O6 151.85(8) . . ?
O11 Mo3 O3 158.72(8) . . ?
O12 Mo3 O3 91.94(9) . . ?
O5 Mo3 O3 85.84(9) . . ?
O6 Mo3 O3 71.58(8) . . ?
O11 Mo3 O2 92.78(10) . . ?
O12 Mo3 O2 158.58(9) . . ?
O5 Mo3 O2 72.19(8) . . ?
O6 Mo3 O2 84.14(9) . . ?
O3 Mo3 O2 69.92(8) . . ?
O7 Ag1 O7 180.00(10) . 2_565 ?
O7 Ag1 O13 87.91(8) . . ?
O7 Ag1 O13 92.09(8) 2_565 . ?
O7 Ag1 O13 92.09(8) . 2_565 ?
O7 Ag1 O13 87.91(8) 2_565 2_565 ?
O13 Ag1 O13 180.0 . 2_565 ?
Cr1 O1 Mo2 102.12(8) . . ?
Cr1 O1 Mo1 100.34(8) . . ?
Mo2 O1 Mo1 92.23(8) . . ?
Cr1 O1 H1 112(4) . . ?
Mo2 O1 H1 118(4) . . ?
Mo1 O1 H1 128(4) . . ?
Cr1 O2 Mo3 103.09(9) . . ?
Cr1 O2 Mo2 103.28(9) . . ?
Mo3 O2 Mo2 94.32(8) . . ?
Cr1 O2 H2 120(3) . . ?
Mo3 O2 H2 117(3) . . ?
Mo2 O2 H2 116(3) . . ?
Cr1 O3 Mo1 104.57(8) . 2 ?
Cr1 O3 Mo3 104.52(9) . . ?
Mo1 O3 Mo3 95.42(8) 2 . ?
Cr1 O3 H3 109(2) . . ?
Mo1 O3 H3 121(3) 2 . ?
Mo3 O3 H3 120(2) . . ?
Mo1 O4 Mo2 119.99(10) . . ?
Mo3 O5 Mo2 117.38(9) . . ?
Mo1 O6 Mo3 115.58(9) 2 . ?
Mo1 O7 Ag1 132.53(12) . . ?
C6 O13 Ag1 131.5(2) . . ?
C12 O16 H16 112(3) . . ?
N1 C1 C2 119.1(3) . . ?
N1 C1 H1A 116(3) . . ?
C2 C1 H1A 125(3) . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2A 118(3) . . ?
C3 C2 H2A 122(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 C6 122.0(3) . . ?
C2 C3 C6 118.9(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4A 112(3) . . ?
C3 C4 H4A 128(3) . . ?
N1 C5 C4 119.3(3) . . ?
N1 C5 H5A 116(2) . . ?
C4 C5 H5A 124(2) . . ?
O14 C6 O13 127.0(3) . . ?
O14 C6 C3 119.1(3) . . ?
O13 C6 C3 113.8(3) . . ?
N2 C7 C8 119.5(3) . . ?
N2 C7 H7A 114(2) . . ?
C8 C7 H7A 126(2) . . ?
C7 C8 C9 119.6(3) . . ?
C7 C8 H8A 118(3) . . ?
C9 C8 H8A 122(3) . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 C12 122.6(3) . . ?
C10 C9 C12 118.0(3) . . ?
C11 C10 C9 118.6(3) . . ?
C11 C10 H10A 123.8(19) . . ?
C9 C10 H10A 117.5(19) . . ?
N2 C11 C10 120.2(3) . . ?
N2 C11 H11A 116(2) . . ?
C10 C11 H11A 124(2) . . ?
O15 C12 O16 126.2(3) . . ?
O15 C12 C9 122.0(3) . . ?
O16 C12 C9 111.8(3) . . ?
C1 N1 C5 123.4(3) . . ?
C1 N1 H1B 111(3) . . ?
C5 N1 H1B 126(3) . . ?
C11 N2 C7 122.6(3) . . ?
C11 N2 H2B 113(4) . . ?
C7 N2 H2B 124(4) . . ?
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
Cr1 O3 1.9556(18) 2 ?
Cr1 O3 1.9556(18) . ?
Cr1 O1 1.978(2) 2 ?
Cr1 O1 1.978(2) . ?
Cr1 O2 1.980(2) . ?
Cr1 O2 1.980(2) 2 ?
Mo1 O8 1.703(2) . ?
Mo1 O7 1.720(2) . ?
Mo1 O4 1.922(2) . ?
Mo1 O6 1.954(2) 2 ?
Mo1 O3 2.228(2) 2 ?
Mo1 O1 2.327(2) . ?
Mo2 O9 1.699(2) . ?
Mo2 O10 1.707(2) . ?
Mo2 O4 1.9344(19) . ?
Mo2 O5 1.954(2) . ?
Mo2 O2 2.272(2) . ?
Mo2 O1 2.306(2) . ?
Mo3 O11 1.698(2) . ?
Mo3 O12 1.722(2) . ?
Mo3 O5 1.946(2) . ?
Mo3 O6 1.9657(19) . ?
Mo3 O3 2.2545(19) . ?
Mo3 O2 2.272(2) . ?
Ag1 O7 2.352(2) . ?
Ag1 O7 2.352(2) 2_565 ?
Ag1 O13 2.492(3) . ?
Ag1 O13 2.492(3) 2_565 ?
O1 H1 0.82(6) . ?
O2 H2 0.73(4) . ?
O3 Mo1 2.228(2) 2 ?
O3 H3 0.96(4) . ?
O6 Mo1 1.954(2) 2 ?
O13 C6 1.273(4) . ?
O14 C6 1.237(4) . ?
O15 C12 1.206(4) . ?
O16 C12 1.307(4) . ?
O16 H16 1.03(5) . ?
C1 N1 1.328(5) . ?
C1 C2 1.368(4) . ?
C1 H1A 0.92(4) . ?
C2 C3 1.391(4) . ?
C2 H2A 0.78(6) . ?
C3 C4 1.374(5) . ?
C3 C6 1.511(3) . ?
C4 C5 1.367(4) . ?
C4 H4A 0.83(4) . ?
C5 N1 1.331(4) . ?
C5 H5A 0.87(4) . ?
C7 N2 1.335(5) . ?
C7 C8 1.374(4) . ?
C7 H7A 0.89(4) . ?
C8 C9 1.378(5) . ?
C8 H8A 0.85(4) . ?
C9 C10 1.392(4) . ?
C9 C12 1.499(4) . ?
C10 C11 1.378(4) . ?
C10 H10A 0.89(3) . ?
C11 N2 1.328(5) . ?
C11 H11A 0.95(3) . ?
N1 H1B 0.85(4) . ?
N2 H2B 0.82(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O14 0.82(6) 1.97(6) 2.768(3) 166(5) 1_545
O2 H2 OW2 0.73(4) 1.94(4) 2.665(3) 171(4) .
O3 H3 O13 0.96(4) 1.57(4) 2.501(3) 162(4) 1_545
O3 H3 O14 0.96(4) 2.64(4) 3.424(3) 139(4) 1_545
O16 H16 O6 1.03(5) 1.56(5) 2.557(3) 162(4) 1_645
N1 H1B O15 0.85(4) 2.23(5) 2.797(4) 125(4) 2_645
N1 H1B O8 0.85(4) 2.37(4) 2.984(3) 130(4) 2_666
N2 H2B O5 0.82(4) 1.85(4) 2.661(3) 175(5) 1_544
