#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:28:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179580 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/45/4504579.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_4504579
loop_
_publ_author_name
'An, Haiyan'
'Li, Yangguang'
'Xiao, Dongrong'
'Wang, Enbo'
'Sun, Chunyan'
_publ_section_title
;
 Self-Assembly of Extended High-Dimensional Architectures from
 Anderson-type Polyoxometalate Clusters
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1107
_journal_paper_doi               10.1021/cg050326p
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C24 H44 I La2 Mo6 N5 O47'
_chemical_formula_weight         2135.00
_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                103.72(3)
_cell_angle_beta                 99.96(3)
_cell_angle_gamma                115.21(3)
_cell_formula_units_Z            1
_cell_length_a                   10.544(2)
_cell_length_b                   10.677(2)
_cell_length_c                   14.528(3)
_cell_measurement_reflns_used    13485
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.04
_cell_volume                     1365.9(8)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0653
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13485
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.548
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0520P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                5313
_reflns_number_total             6181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050326psi20050711_085249.cif
_cod_data_source_block           aa162c
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1365.8(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4504579
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
I1 I 1.0000 0.0000 1.0000 0.00965(10) Uani 1 2 d S
Mo1 Mo 0.67059(4) -0.15447(5) 0.83793(3) 0.01209(10) Uani 1 1 d .
Mo2 Mo 0.80450(4) -0.36583(5) 0.89308(3) 0.01414(10) Uani 1 1 d .
Mo3 Mo 0.86320(4) 0.21027(5) 0.94286(3) 0.01182(10) Uani 1 1 d .
La1 La 0.55762(3) -0.21833(3) 0.530309(17) 0.01122(9) Uani 1 1 d .
O1 O 0.9688(4) 0.1527(4) 1.0694(2) 0.0129(7) Uani 1 1 d .
O2 O 0.9166(3) 0.0194(4) 0.8821(2) 0.0109(6) Uani 1 1 d .
O3 O 1.1913(3) 0.1471(4) 1.0177(2) 0.0124(7) Uani 1 1 d .
O4 O 0.6938(3) 0.0265(4) 0.9269(2) 0.0139(7) Uani 1 1 d .
O5 O 0.7392(4) -0.2904(4) 0.7976(2) 0.0150(7) Uani 1 1 d .
O6 O 0.9269(4) -0.3324(4) 1.0216(2) 0.0135(7) Uani 1 1 d .
O7 O 0.8174(4) 0.3212(4) 1.0190(3) 0.0216(8) Uani 1 1 d .
O8 O 0.8160(4) 0.2167(4) 0.8262(2) 0.0203(8) Uani 1 1 d .
O9 O 0.5100(4) -0.2641(4) 0.8542(2) 0.0200(8) Uani 1 1 d .
O10 O 0.6288(4) -0.1326(4) 0.7241(2) 0.0194(8) Uani 1 1 d .
O11 O 0.8454(5) -0.4789(5) 0.8141(3) 0.0264(9) Uani 1 1 d .
O12 O 0.6429(4) -0.4756(5) 0.9068(3) 0.0265(9) Uani 1 1 d .
O13 O 0.4041(4) -0.1025(4) 0.5688(2) 0.0183(7) Uani 1 1 d .
O14 O 0.4564(4) 0.1328(4) 0.6152(2) 0.0202(8) Uani 1 1 d .
O15 O 0.3798(4) -0.4171(4) 0.5843(2) 0.0202(8) Uani 1 1 d .
O16 O 0.4666(4) -0.5708(4) 0.5991(2) 0.0190(8) Uani 1 1 d .
O17 O 0.0775(10) -0.3690(11) 0.4844(7) 0.039(2) Uani 0.50 1 d PDU
O18 O -0.0371(10) -0.4304(13) 0.5882(7) 0.048(3) Uani 0.50 1 d PDU
O19 O 0.0595(16) -0.3884(17) 0.5385(9) 0.066(4) Uani 0.50 1 d PDU
C1 C 0.4590(6) 0.1393(7) 0.9031(4) 0.0239(12) Uani 1 1 d .
H1A H 0.5028 0.2253 0.9586 0.029 Uiso 1 1 calc R
C2 C 0.4813(5) 0.1457(6) 0.8134(3) 0.0159(10) Uani 1 1 d .
H2A H 0.5399 0.2356 0.8074 0.019 Uiso 1 1 calc R
C3 C 0.4145(5) 0.0152(6) 0.7319(3) 0.0151(9) Uani 1 1 d .
C4 C 0.3299(6) -0.1181(7) 0.7431(4) 0.0253(12) Uani 1 1 d .
H4A H 0.2857 -0.2066 0.6897 0.030 Uiso 1 1 calc R
C5 C 0.3130(7) -0.1162(7) 0.8347(4) 0.0306(13) Uani 1 1 d .
H5A H 0.2577 -0.2042 0.8442 0.037 Uiso 1 1 calc R
C6 C 0.4268(5) 0.0161(6) 0.6296(3) 0.0140(10) Uani 1 1 d .
C7 C 0.1333(6) -0.5404(7) 0.7734(4) 0.0240(12) Uani 1 1 d .
H7A H 0.0596 -0.5166 0.7806 0.029 Uiso 1 1 calc R
C8 C 0.1994(6) -0.5115(6) 0.7025(3) 0.0206(11) Uani 1 1 d .
H8A H 0.1726 -0.4651 0.6623 0.025 Uiso 1 1 calc R
C9 C 0.3071(5) -0.5512(5) 0.6898(3) 0.0138(9) Uani 1 1 d .
C10 C 0.3400(6) -0.6242(7) 0.7485(4) 0.0245(12) Uani 1 1 d .
H10A H 0.4060 -0.6583 0.7384 0.029 Uiso 1 1 calc R
C11 C 0.2764(7) -0.6465(8) 0.8212(4) 0.0326(14) Uani 1 1 d .
H11A H 0.3024 -0.6914 0.8630 0.039 Uiso 1 1 calc R
C12 C 0.3906(5) -0.5087(6) 0.6176(3) 0.0142(10) Uani 1 1 d .
N1 N 0.3756(5) 0.0113(6) 0.9099(3) 0.0236(10) Uani 1 1 d .
H1B H 0.3607 0.0098 0.9661 0.028 Uiso 1 1 calc R
N2 N 0.1757(5) -0.6032(6) 0.8321(3) 0.0221(10) Uani 1 1 d .
H2B H 0.1371 -0.6166 0.8789 0.027 Uiso 1 1 calc R
N3 N -0.0065(15) -0.4737(13) 0.5128(9) 0.035(3) Uiso 0.50 1 d PD
OW1 O 0.7276(4) 0.0704(4) 0.6161(2) 0.0235(8) Uani 1 1 d .
OW2 O 0.7282(4) -0.3103(5) 0.6048(2) 0.0212(8) Uani 1 1 d .
OW3 O 0.2897(4) -0.3656(6) 0.4009(3) 0.0337(11) Uani 1 1 d .
OW4 O 0.7996(4) -0.1280(5) 0.4891(3) 0.0271(9) Uani 1 1 d .
OW5 O 0.9315(4) 0.1150(5) 0.4350(3) 0.0340(10) Uani 1 1 d .
OW6A O 1.0235(12) 0.0439(14) 0.7171(7) 0.055(3) Uani 0.50 1 d P
OW6B O 1.0611(15) -0.0564(19) 0.7560(7) 0.070(4) Uani 0.50 1 d P
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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 I1 O3 180.000(1) 2_757 .
O3 I1 O2 86.49(15) 2_757 .
O3 I1 O2 93.51(15) . .
O3 I1 O2 93.51(15) 2_757 2_757
O3 I1 O2 86.49(15) . 2_757
O2 I1 O2 180.000(2) . 2_757
O3 I1 O1 87.34(15) 2_757 2_757
O3 I1 O1 92.66(15) . 2_757
O2 I1 O1 93.37(15) . 2_757
O2 I1 O1 86.63(14) 2_757 2_757
O3 I1 O1 92.66(15) 2_757 .
O3 I1 O1 87.34(15) . .
O2 I1 O1 86.63(14) . .
O2 I1 O1 93.37(15) 2_757 .
O1 I1 O1 180.00(18) 2_757 .
O9 Mo1 O10 107.99(18) . .
O9 Mo1 O5 101.33(18) . .
O10 Mo1 O5 97.11(16) . .
O9 Mo1 O4 94.11(17) . .
O10 Mo1 O4 100.31(16) . .
O5 Mo1 O4 151.86(13) . .
O9 Mo1 O3 92.16(15) . 2_757
O10 Mo1 O3 159.37(15) . 2_757
O5 Mo1 O3 73.99(13) . 2_757
O4 Mo1 O3 82.13(13) . 2_757
O9 Mo1 O2 157.69(13) . .
O10 Mo1 O2 92.82(15) . .
O5 Mo1 O2 83.47(14) . .
O4 Mo1 O2 73.80(13) . .
O3 Mo1 O2 68.00(12) 2_757 .
O12 Mo2 O11 106.6(2) . .
O12 Mo2 O6 95.85(17) . .
O11 Mo2 O6 101.70(16) . .
O12 Mo2 O5 100.92(17) . .
O11 Mo2 O5 96.81(16) . .
O6 Mo2 O5 150.26(15) . .
O12 Mo2 O1 157.66(16) . 2_757
O11 Mo2 O1 94.61(17) . 2_757
O6 Mo2 O1 72.67(14) . 2_757
O5 Mo2 O1 82.89(14) . 2_757
O12 Mo2 O3 92.96(18) . 2_757
O11 Mo2 O3 159.16(18) . 2_757
O6 Mo2 O3 82.81(13) . 2_757
O5 Mo2 O3 72.02(13) . 2_757
O1 Mo2 O3 67.06(12) 2_757 2_757
O7 Mo3 O8 107.50(18) . .
O7 Mo3 O6 101.77(17) . 2_757
O8 Mo3 O6 98.13(16) . 2_757
O7 Mo3 O4 95.53(17) . .
O8 Mo3 O4 99.49(17) . .
O6 Mo3 O4 150.25(15) 2_757 .
O7 Mo3 O1 94.84(15) . .
O8 Mo3 O1 157.40(15) . .
O6 Mo3 O1 73.41(14) 2_757 .
O4 Mo3 O1 81.23(14) . .
O7 Mo3 O2 159.55(16) . .
O8 Mo3 O2 91.26(15) . .
O6 Mo3 O2 83.00(14) 2_757 .
O4 Mo3 O2 72.86(13) . .
O1 Mo3 O2 67.20(11) . .
O16 La1 O13 137.63(12) 2_646 .
O16 La1 O14 80.14(12) 2_646 2_656
O13 La1 O14 82.43(12) . 2_656
O16 La1 OW4 73.58(13) 2_646 .
O13 La1 OW4 133.06(14) . .
O14 La1 OW4 68.22(13) 2_656 .
O16 La1 O15 84.03(12) 2_646 .
O13 La1 O15 82.52(13) . .
O14 La1 O15 136.31(12) 2_656 .
OW4 La1 O15 143.49(14) . .
O16 La1 OW2 70.60(12) 2_646 .
O13 La1 OW2 144.11(11) . .
O14 La1 OW2 131.08(11) 2_656 .
OW4 La1 OW2 66.38(13) . .
O15 La1 OW2 79.24(12) . .
O16 La1 O10 134.12(13) 2_646 .
O13 La1 O10 76.63(11) . .
O14 La1 O10 143.95(13) 2_656 .
OW4 La1 O10 106.33(13) . .
O15 La1 O10 69.56(12) . .
OW2 La1 O10 68.11(11) . .
O16 La1 OW3 70.01(14) 2_646 .
O13 La1 OW3 67.67(13) . .
O14 La1 OW3 67.77(14) 2_656 .
OW4 La1 OW3 126.31(12) . .
O15 La1 OW3 68.56(13) . .
OW2 La1 OW3 130.84(15) . .
O10 La1 OW3 127.36(12) . .
O16 La1 OW1 140.78(12) 2_646 .
O13 La1 OW1 70.44(12) . .
O14 La1 OW1 77.97(13) 2_656 .
OW4 La1 OW1 68.20(13) . .
O15 La1 OW1 133.26(11) . .
OW2 La1 OW1 100.89(13) . .
O10 La1 OW1 67.53(13) . .
OW3 La1 OW1 128.25(15) . .
I1 O1 Mo3 103.54(13) . .
I1 O1 Mo2 102.92(14) . 2_757
Mo3 O1 Mo2 90.37(13) . 2_757
I1 O2 Mo1 102.47(15) . .
I1 O2 Mo3 102.63(13) . .
Mo1 O2 Mo3 90.53(12) . .
I1 O3 Mo1 103.04(15) . 2_757
I1 O3 Mo2 102.69(14) . 2_757
Mo1 O3 Mo2 90.14(11) 2_757 2_757
Mo3 O4 Mo1 117.51(16) . .
Mo1 O5 Mo2 119.24(16) . .
Mo3 O6 Mo2 118.62(17) 2_757 .
Mo1 O10 La1 153.6(2) . .
C6 O13 La1 135.3(3) . .
C6 O14 La1 137.7(3) . 2_656
C12 O15 La1 132.8(3) . .
C12 O16 La1 138.0(3) . 2_646
O19 O17 N3 37.8(10) . .
N3 O18 O19 36.6(7) . .
N3 O19 O17 100.1(17) . .
N3 O19 O18 65.1(14) . .
O17 O19 O18 148.3(16) . .
N3 O19 N3 26.9(15) . 2_546
O17 O19 N3 87.3(13) . 2_546
O18 O19 N3 88.1(14) . 2_546
N1 C1 C2 119.6(5) . .
C1 C2 C3 118.8(5) . .
C4 C3 C2 119.6(4) . .
C4 C3 C6 119.1(4) . .
C2 C3 C6 121.2(5) . .
C5 C4 C3 118.5(5) . .
N1 C5 C4 120.0(6) . .
O14 C6 O13 127.3(4) . .
O14 C6 C3 116.0(4) . .
O13 C6 C3 116.7(5) . .
N2 C7 C8 119.2(5) . .
C9 C8 C7 120.3(5) . .
C8 C9 C10 118.0(5) . .
C8 C9 C12 121.1(5) . .
C10 C9 C12 120.9(5) . .
C11 C10 C9 120.3(5) . .
N2 C11 C10 119.4(6) . .
O15 C12 O16 126.8(5) . .
O15 C12 C9 117.4(4) . .
O16 C12 C9 115.9(5) . .
C1 N1 C5 123.5(5) . .
C7 N2 C11 122.6(5) . .
O19 N3 N3 120(3) . 2_546
O19 N3 O18 78.3(15) . .
N3 N3 O18 144(3) 2_546 .
O19 N3 O17 42.1(12) . .
N3 N3 O17 96(2) 2_546 .
O18 N3 O17 114.9(11) . .
O19 N3 O19 153.1(15) . 2_546
N3 N3 O19 33.0(17) 2_546 2_546
O18 N3 O19 123.4(15) . 2_546
O17 N3 O19 121.6(10) . 2_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 O3 1.879(3) 2_757
I1 O3 1.879(3) .
I1 O2 1.885(3) .
I1 O2 1.885(3) 2_757
I1 O1 1.890(3) 2_757
I1 O1 1.890(3) .
Mo1 O9 1.695(4) .
Mo1 O10 1.733(3) .
Mo1 O5 1.900(4) .
Mo1 O4 1.941(4) .
Mo1 O3 2.301(3) 2_757
Mo1 O2 2.311(3) .
Mo2 O12 1.687(4) .
Mo2 O11 1.708(4) .
Mo2 O6 1.934(3) .
Mo2 O5 1.928(4) .
Mo2 O1 2.348(4) 2_757
Mo2 O3 2.364(4) 2_757
Mo3 O7 1.706(4) .
Mo3 O8 1.709(3) .
Mo3 O6 1.922(3) 2_757
Mo3 O4 1.936(4) .
Mo3 O1 2.325(3) .
Mo3 O2 2.355(4) .
La1 O16 2.450(4) 2_646
La1 O13 2.481(4) .
La1 O14 2.500(4) 2_656
La1 OW4 2.550(4) .
La1 O15 2.558(4) .
La1 OW2 2.589(4) .
La1 O10 2.605(3) .
La1 OW3 2.639(4) .
La1 OW1 2.639(4) .
O1 Mo2 2.348(4) 2_757
O3 Mo1 2.301(3) 2_757
O3 Mo2 2.364(3) 2_757
O6 Mo3 1.922(3) 2_757
O13 C6 1.256(6) .
O14 C6 1.228(7) .
O14 La1 2.500(4) 2_656
O15 C12 1.227(7) .
O16 C12 1.263(6) .
O16 La1 2.450(4) 2_646
O17 O19 0.889(15) .
O17 N3 1.305(14) .
O18 N3 1.235(12) .
O18 O19 1.333(19) .
O19 N3 0.813(13) .
O19 N3 1.29(2) 2_546
C1 N1 1.312(8) .
C1 C2 1.375(7) .
C2 C3 1.390(7) .
C3 C4 1.388(8) .
C3 C6 1.516(6) .
C4 C5 1.369(7) .
C5 N1 1.327(8) .
C7 N2 1.331(8) .
C7 C8 1.363(7) .
C8 C9 1.395(7) .
C9 C10 1.378(8) .
C9 C12 1.513(6) .
C10 C11 1.360(8) .
C11 N2 1.345(8) .
N3 N3 0.68(2) 2_546
N3 O19 1.29(2) 2_546
OW6A OW6B 1.482(19) .
