#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327454.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_4327454
loop_
_publ_author_name
'Yangguang Li'
'Na Hao'
'Enbo Wang'
'Mei Yuan'
'Changwen Hu'
'Ninghai Hu'
'Hengqing Jia'
_publ_section_title
;
 New High-Dimensional Networks Based on Polyoxometalate and Crown Ether
 Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2729
_journal_page_last               2735
_journal_paper_doi               10.1021/ic026172+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H57 Mo6 N Na2 O34'
_chemical_formula_weight         1741.51
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           127
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2ab'
_symmetry_space_group_name_H-M   'P 4/m b m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9701(6)
_cell_length_b                   16.9701(6)
_cell_length_c                   14.2676(4)
_cell_measurement_reflns_used    4876
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.40
_cell_volume                     4108.8(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4876
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.40
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       tetragonal
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.543
_exptl_crystal_size_min          0.203
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0667
_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)+(0.1200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1997
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                1768
_reflns_number_total             2558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0261722B_1.cif
_cod_data_source_block           m136
_cod_database_code               4327454
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-y-1/2, -x-1/2, z'
'y-1/2, x-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
Mo1 Mo 0.02108(5) 0.13482(5) 0.5000 0.0447(3) Uani 1 2 d S . .
Mo2 Mo 0.0000 0.0000 0.33711(6) 0.0442(3) Uani 1 4 d S . .
Na Na 0.2008(3) -0.2992(3) 0.0000 0.0765(18) Uani 1 4 d S . .
C1 C 0.1063(9) -0.1320(8) 0.0819(9) 0.118(5) Uani 1 1 d . . .
C2 C 0.0923(10) -0.1790(9) 0.1605(8) 0.149(7) Uani 1 1 d . A .
O1 O 0.0376(5) 0.2313(4) 0.5000 0.0648(19) Uani 1 2 d S . .
O2 O -0.0918(4) 0.1256(4) 0.5000 0.0491(15) Uani 1 2 d S . .
O3 O 0.0000 0.0000 0.2200(6) 0.063(3) Uani 1 4 d S . .
O4 O 0.0174(3) 0.1083(3) 0.3684(3) 0.0491(11) Uani 1 1 d . . .
O5 O 0.0000 0.0000 0.5000 0.033(2) Uani 1 8 d S . .
O6 O 0.0947(6) -0.1781(5) 0.0000 0.079(3) Uani 1 2 d S . .
O7 O 0.1323(10) -0.2599(9) 0.1664(11) 0.073(4) Uani 0.50 1 d P A 1
C3 C 0.1203(12) -0.3225(11) 0.2361(10) 0.078(5) Uani 0.50 1 d P A 1
C4 C 0.0664(13) -0.3213(14) 0.3010(12) 0.089(6) Uani 0.50 1 d P A 1
C5 C 0.0631(13) -0.3811(13) 0.3682(11) 0.089(6) Uani 0.50 1 d P A 1
O7' O 0.1668(10) -0.2271(10) 0.1586(11) 0.074(4) Uani 0.50 1 d P A 2
C3' C 0.1706(10) -0.2696(12) 0.2415(8) 0.072(5) Uani 0.50 1 d P A 2
C4' C 0.1257(12) -0.2598(12) 0.3235(10) 0.076(5) Uani 0.50 1 d P A 2
C5' C 0.1342(12) -0.3041(13) 0.3969(9) 0.083(6) Uani 0.50 1 d P A 2
C6 C 0.2911(11) -0.2089(11) 0.3339(15) 0.028(5) Uiso 0.25 2 d SPD . .
C7 C 0.335(2) -0.165(2) 0.261(3) 0.100(18) Uiso 0.25 2 d SPD . .
N1 N 0.2668(13) -0.2332(13) 0.4072(17) 0.059(8) Uiso 0.25 2 d SPD . .
O1W O 0.1039(14) -0.3961(14) 0.0000 0.101(9) Uiso 0.50 4 d SP A .
O2W O 0.2970(9) -0.2030(9) -0.0390(12) 0.097(6) Uiso 0.50 2 d SP . .
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'
Na Na 0.0362 0.0249 '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'
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
O1 Mo1 O2 102.7(4) . 11_556
O1 Mo1 O2 104.4(3) . .
O2 Mo1 O2 152.9(3) 11_556 .
O1 Mo1 O4 103.60(14) . .
O2 Mo1 O4 86.62(16) 11_556 .
O2 Mo1 O4 87.06(15) . .
O1 Mo1 O4 103.60(14) . 10_556
O2 Mo1 O4 86.62(16) 11_556 10_556
O2 Mo1 O4 87.06(15) . 10_556
O4 Mo1 O4 152.8(3) . 10_556
O1 Mo1 O5 179.1(3) . .
O2 Mo1 O5 76.5(2) 11_556 .
O2 Mo1 O5 76.42(19) . .
O4 Mo1 O5 76.40(14) . .
O4 Mo1 O5 76.40(14) 10_556 .
O3 Mo2 O4 103.50(13) . 2
O3 Mo2 O4 103.50(13) . 3
O4 Mo2 O4 86.88(6) 2 3
O3 Mo2 O4 103.50(13) . 4
O4 Mo2 O4 86.88(6) 2 4
O4 Mo2 O4 153.0(3) 3 4
O3 Mo2 O4 103.50(13) . .
O4 Mo2 O4 153.0(3) 2 .
O4 Mo2 O4 86.88(6) 3 .
O4 Mo2 O4 86.88(6) 4 .
O3 Mo2 O5 180.0 . .
O4 Mo2 O5 76.50(13) 2 .
O4 Mo2 O5 76.50(13) 3 .
O4 Mo2 O5 76.50(13) 4 .
O4 Mo2 O5 76.50(13) . .
O1W Na O2W 166.4(4) . 10
O1W Na O2W 166.4(4) . .
O2W Na O2W 27.1(8) 10 .
O1W Na O7' 100.0(5) . .
O2W Na O7' 68.3(6) 10 .
O2W Na O7' 91.9(6) . .
O1W Na O7' 100.0(5) . 16_655
O2W Na O7' 68.3(6) 10 16_655
O2W Na O7' 91.9(6) . 16_655
O7' Na O7' 57.8(7) . 16_655
O1W Na O7' 100.0(5) . 10
O2W Na O7' 91.9(6) 10 10
O2W Na O7' 68.3(6) . 10
O7' Na O7' 118.2(7) . 10
O7' Na O7' 160.0(9) 16_655 10
O1W Na O7' 100.0(5) . 7_545
O2W Na O7' 91.9(6) 10 7_545
O2W Na O7' 68.3(6) . 7_545
O7' Na O7' 160.0(9) . 7_545
O7' Na O7' 118.2(7) 16_655 7_545
O7' Na O7' 57.8(7) 10 7_545
O1W Na O7 82.6(4) . 10
O2W Na O7 109.2(6) 10 10
O2W Na O7 85.5(5) . 10
O7' Na O7 122.7(3) . 10
O7' Na O7 177.3(8) 16_655 10
O7' Na O7 17.4(4) 10 10
O7' Na O7 60.3(3) 7_545 10
O1W Na O7 82.6(4) . 7_545
O2W Na O7 109.2(6) 10 7_545
O2W Na O7 85.5(5) . 7_545
O7' Na O7 177.3(8) . 7_545
O7' Na O7 122.7(3) 16_655 7_545
O7' Na O7 60.3(3) 10 7_545
O7' Na O7 17.4(4) 7_545 7_545
O7 Na O7 56.6(7) 10 7_545
O1W Na O7 82.6(4) . .
O2W Na O7 85.5(5) 10 .
O2W Na O7 109.2(6) . .
O7' Na O7 17.4(4) . .
O7' Na O7 60.3(3) 16_655 .
O7' Na O7 122.7(3) 10 .
O7' Na O7 177.3(8) 7_545 .
O7 Na O7 121.1(7) 10 .
O7 Na O7 165.2(8) 7_545 .
O1W Na O7 82.6(4) . 16_655
O2W Na O7 85.5(5) 10 16_655
O2W Na O7 109.2(6) . 16_655
O7' Na O7 60.3(3) . 16_655
O7' Na O7 17.4(4) 16_655 16_655
O7' Na O7 177.3(8) 10 16_655
O7' Na O7 122.7(3) 7_545 16_655
O7 Na O7 165.2(8) 10 16_655
O7 Na O7 121.1(7) 7_545 16_655
O7 Na O7 56.6(7) . 16_655
O1W Na O6 93.8(3) . .
O2W Na O6 86.3(3) 10 .
O2W Na O6 86.3(3) . .
O7' Na O6 60.4(3) . .
O7' Na O6 118.1(3) 16_655 .
O7' Na O6 60.4(3) 10 .
O7' Na O6 118.1(3) 7_545 .
O7 Na O6 62.3(3) 10 .
O7 Na O6 118.8(3) 7_545 .
O7 Na O6 62.3(3) . .
O7 Na O6 118.8(3) 16_655 .
C2 C1 O6 108.8(12) . .
C1 C2 O7' 98.7(13) . .
C1 C2 O7 118.7(11) . .
O7' C2 O7 31.1(7) . .
Mo1 O2 Mo1 117.1(3) 3 .
Mo2 O4 Mo1 117.1(2) . .
Mo1 O5 Mo1 180.0 9_556 .
Mo1 O5 Mo1 90.0 9_556 3
Mo1 O5 Mo1 90.0 . 3
Mo1 O5 Mo1 90.0 9_556 11_556
Mo1 O5 Mo1 90.0 . 11_556
Mo1 O5 Mo1 180.0 3 11_556
Mo1 O5 Mo2 90.0 9_556 9_556
Mo1 O5 Mo2 90.0 . 9_556
Mo1 O5 Mo2 90.0 3 9_556
Mo1 O5 Mo2 90.0 11_556 9_556
Mo1 O5 Mo2 90.0 9_556 .
Mo1 O5 Mo2 90.0 . .
Mo1 O5 Mo2 90.0 3 .
Mo1 O5 Mo2 90.0 11_556 .
Mo2 O5 Mo2 180.0 9_556 .
C1 O6 C1 110.7(15) 10 .
C1 O6 Na 108.9(6) 10 .
C1 O6 Na 108.9(6) . .
C3 O7 C2 128.5(13) . .
C3 O7 Na 118.2(10) . .
C2 O7 Na 111.1(9) . .
C4 C3 C3 120.5(12) . 16_655
C4 C3 O7 124.6(17) . .
C3 C3 O7 114.4(9) 16_655 .
C3 C4 C5 120.3(18) . .
C5 C5 C4 119.0(11) 16_655 .
C3' O7' C2 107.8(13) . .
C3' O7' Na 118.7(11) . .
C2 O7' Na 116.8(10) . .
O7' C3' C4' 128.5(15) . .
O7' C3' C3' 113.7(9) . 16_655
C4' C3' C3' 117.8(9) . 16_655
C5' C4' C3' 122.9(15) . .
C4' C5' C5' 119.3(10) . 16_655
N1 C6 C7 164(4) . .
O2W O2W Na 76.4(4) 10 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.661(7) .
Mo1 O2 1.918(6) 11_556
Mo1 O2 1.921(7) .
Mo1 O4 1.932(4) .
Mo1 O4 1.932(4) 10_556
Mo1 O5 2.3157(8) .
Mo2 O3 1.671(8) .
Mo2 O4 1.914(5) 2
Mo2 O4 1.914(5) 3
Mo2 O4 1.914(5) 4
Mo2 O4 1.914(5) .
Mo2 O5 2.3240(9) .
Na O1W 2.33(3) .
Na O2W 2.37(2) 10
Na O2W 2.37(2) .
Na O7' 2.636(16) .
Na O7' 2.636(16) 16_655
Na O7' 2.636(16) 10
Na O7' 2.636(16) 7_545
Na O7 2.726(14) 10
Na O7 2.726(14) 7_545
Na O7 2.726(14) .
Na O7 2.726(14) 16_655
Na O6 2.732(8) .
C1 C2 1.40(2) .
C1 O6 1.420(12) .
C2 O7' 1.505(18) .
C2 O7 1.535(18) .
O2 Mo1 1.918(6) 3
O5 Mo1 2.3157(8) 9_556
O5 Mo1 2.3157(8) 3
O5 Mo1 2.3157(8) 11_556
O5 Mo2 2.3240(9) 9_556
O6 C1 1.420(12) 10
O7 C3 1.47(2) .
C3 C4 1.30(2) .
C3 C3 1.37(4) 16_655
C4 C5 1.40(3) .
C5 C5 1.34(4) 16_655
O7' C3' 1.39(2) .
C3' C4' 1.41(2) .
C3' C3' 1.43(3) 16_655
C4' C5' 1.30(2) .
C5' C5' 1.48(4) 16_655
C6 N1 1.198(16) .
C6 C7 1.470(17) .
O2W O2W 1.11(3) 10
