#------------------------------------------------------------------------------
#$Date: 2021-06-18 12:29:40 +0300 (Fri, 18 Jun 2021) $
#$Revision: 266564 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/35/1563583.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_1563583
loop_
_publ_author_name
'Gao, Yuanzhe'
'Xu, Yanqing'
'Han, Zhangang'
'Li, Chunhong'
'Cui, Fengyun'
'Chi, Yingnan'
'Hu, Changwen'
_publ_section_title
;
 Syntheses, structures and properties of 3D inorganic--organic hybrid
 frameworks constructed from lanthanide polymer and Keggin-type
 tungstosilicate
;
_journal_issue                   5
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1000
_journal_page_last               1006
_journal_paper_doi               10.1016/j.jssc.2010.03.006
_journal_volume                  183
_journal_year                    2010
_chemical_formula_moiety         'C28 H48 Ce4 N4 O74 Si W12'
_chemical_formula_sum            'C28 H48 Ce4 N4 O74 Si W12'
_chemical_formula_weight         4419.44
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            4
_cell_length_a                   21.999(2)
_cell_length_b                   21.999(2)
_cell_length_c                   16.7023(15)
_cell_measurement_reflns_used    3544
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.53
_cell_volume                     8083.2(13)
_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      298(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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16614
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    19.336
_exptl_absorpt_correction_T_max  0.141
_exptl_absorpt_correction_T_min  0.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             7880
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.279
_refine_diff_density_min         -2.269
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0578
_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)+(0.0450P)²+729.7845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                2893
_reflns_number_total             3543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-1000.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        8083.3(14)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               1563583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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
W1 W 0.96403(4) 0.64296(3) 1.02470(4) 0.0297(2) Uani 1 1 d . . .
W2 W 0.85355(3) 0.68547(4) 0.86709(4) 0.0287(2) Uani 1 1 d . . .
W3 W 0.89530(4) 0.79667(4) 1.02437(4) 0.0310(2) Uani 1 1 d . . .
Ce1 Ce 0.89141(5) 0.57438(6) 0.38457(6) 0.0383(3) Uani 1 1 d . . .
Si1 Si 1.0000 0.7500 0.8750 0.0100(16) Uani 1 4 d S . .
N1 N 1.1357(7) 0.5823(8) 0.2380(9) 0.035(4) Uani 1 1 d . . .
O1 O 1.0241(5) 0.6946(5) 0.9310(7) 0.022(3) Uani 1 1 d . . .
O2 O 0.9343(6) 0.7214(6) 1.0517(7) 0.029(3) Uani 1 1 d . . .
O3 O 0.9049(6) 0.6435(6) 0.9412(7) 0.030(3) Uani 1 1 d . . .
O4 O 0.8562(6) 0.7513(6) 0.9407(7) 0.031(3) Uani 1 1 d . . .
O5 O 1.0071(6) 0.5815(6) 0.9649(8) 0.032(3) Uani 1 1 d . . .
O6 O 1.0387(6) 0.6625(6) 1.0786(7) 0.032(3) Uani 1 1 d . . .
O7 O 0.9278(7) 0.5998(6) 1.0952(8) 0.043(4) Uani 1 1 d . . .
O8 O 0.8811(6) 0.6311(6) 0.7851(8) 0.035(3) Uani 1 1 d . . .
O9 O 0.7853(7) 0.6556(6) 0.8896(9) 0.041(3) Uani 1 1 d . . .
O10 O 0.8393(7) 0.8011(7) 1.0944(9) 0.050(4) Uani 1 1 d . . .
O11 O 1.2790(7) 0.5687(7) 0.1428(8) 0.044(4) Uani 1 1 d . . .
O12 O 1.2509(6) 0.6112(7) 0.2593(8) 0.043(4) Uani 1 1 d . . .
O13 O 0.9839(7) 0.5774(9) 0.2971(9) 0.060(5) Uani 1 1 d . . .
O14 O 1.0653(7) 0.6151(9) 0.3570(9) 0.057(5) Uani 1 1 d . . .
O15 O 0.9755(9) 0.6186(10) 0.4699(11) 0.084(6) Uani 1 1 d . . .
H15C H 1.0093 0.6136 0.4461 0.100 Uiso 1 1 d R . .
H15D H 0.9793 0.6079 0.5185 0.100 Uiso 1 1 d R . .
O16 O 0.9752(10) 0.4909(11) 0.4214(12) 0.096(8) Uani 1 1 d . . .
H16C H 0.9958 0.4753 0.3835 0.115 Uiso 1 1 d R . .
H16D H 0.9801 0.4688 0.4626 0.115 Uiso 1 1 d R . .
O17 O 0.8766(10) 0.4781(10) 0.3045(11) 0.085(6) Uani 1 1 d . . .
H17C H 0.8866 0.4748 0.2556 0.102 Uiso 1 1 d R . .
H17D H 0.8412 0.4633 0.3104 0.102 Uiso 1 1 d R . .
O18 O 0.8719(8) 0.6157(9) 0.2451(10) 0.070(5) Uani 1 1 d . . .
H18C H 0.8871 0.6107 0.1988 0.084 Uiso 1 1 d R . .
H18D H 0.8334 0.6140 0.2413 0.084 Uiso 1 1 d R . .
O19 O 0.0000 0.7500 0.532(3) 0.140(16) Uani 1 2 d S . .
H19C H 0.0238 0.7605 0.5700 0.168 Uiso 0.50 1 d PR . .
H19D H -0.0151 0.7169 0.5152 0.168 Uiso 0.50 1 d PR . .
C1 C 1.2400(10) 0.5821(10) 0.1942(13) 0.043(5) Uani 1 1 d . . .
C2 C 1.1742(9) 0.5646(9) 0.1802(11) 0.035(4) Uani 1 1 d . . .
C3 C 1.1562(11) 0.5314(11) 0.1143(13) 0.047(6) Uani 1 1 d . . .
H3 H 1.1840 0.5208 0.0748 0.056 Uiso 1 1 calc R . .
C4 C 1.0959(9) 0.5141(11) 0.1083(13) 0.043(5) Uani 1 1 d . . .
H4 H 1.0823 0.4904 0.0658 0.052 Uiso 1 1 calc R . .
C5 C 1.0555(9) 0.5338(11) 0.1693(13) 0.043(5) Uani 1 1 d . . .
H5 H 1.0143 0.5249 0.1667 0.051 Uiso 1 1 calc R . .
C6 C 1.0788(9) 0.5662(11) 0.2317(12) 0.040(5) Uani 1 1 d . . .
C7 C 1.0387(10) 0.5868(12) 0.3005(13) 0.051(6) 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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
O7 W1 O2 100.4(6) . .
O7 W1 O3 100.9(6) . .
O2 W1 O3 86.1(5) . .
O7 W1 O6 101.5(6) . .
O2 W1 O6 88.9(5) . .
O3 W1 O6 157.6(5) . .
O7 W1 O5 101.3(6) . .
O2 W1 O5 158.2(5) . .
O3 W1 O5 87.7(5) . .
O6 W1 O5 88.8(6) . .
O7 W1 O1 172.9(6) . .
O2 W1 O1 85.0(5) . .
O3 W1 O1 83.9(5) . .
O6 W1 O1 73.9(4) . .
O5 W1 O1 73.5(5) . .
O9 W2 O4 100.4(6) . .
O9 W2 O3 101.2(6) . .
O4 W2 O3 86.0(5) . .
O9 W2 O8 101.4(6) . .
O4 W2 O8 158.1(5) . .
O3 W2 O8 88.6(5) . .
O9 W2 O5 101.0(6) . 10_677
O4 W2 O5 88.1(5) . 10_677
O3 W2 O5 157.7(5) . 10_677
O8 W2 O5 88.9(6) . 10_677
O9 W2 O1 172.8(5) . 10_677
O4 W2 O1 84.6(5) . 10_677
O3 W2 O1 84.3(5) . 10_677
O8 W2 O1 73.8(5) . 10_677
O5 W2 O1 73.8(5) 10_677 10_677
O10 W3 O8 101.1(7) . 10_677
O10 W3 O2 102.1(7) . .
O8 W3 O2 156.8(5) 10_677 .
O10 W3 O4 101.9(6) . .
O8 W3 O4 88.9(5) 10_677 .
O2 W3 O4 85.7(5) . .
O10 W3 O6 101.3(6) . 3_765
O8 W3 O6 88.8(6) 10_677 3_765
O2 W3 O6 87.4(5) . 3_765
O4 W3 O6 156.7(5) . 3_765
O10 W3 O1 171.8(6) . 3_765
O8 W3 O1 73.2(5) 10_677 3_765
O2 W3 O1 83.8(5) . 3_765
O4 W3 O1 84.2(5) . 3_765
O6 W3 O1 73.0(4) 3_765 3_765
O14 Ce1 O13 101.3(6) 10_676 .
O14 Ce1 O12 122.6(5) 10_676 10_676
O13 Ce1 O12 130.0(5) . 10_676
O14 Ce1 O11 80.2(6) 10_676 15_455
O13 Ce1 O11 133.9(5) . 15_455
O12 Ce1 O11 80.5(5) 10_676 15_455
O14 Ce1 O17 144.5(6) 10_676 .
O13 Ce1 O17 79.5(7) . .
O12 Ce1 O17 77.7(6) 10_676 .
O11 Ce1 O17 74.7(6) 15_455 .
O14 Ce1 O15 76.4(7) 10_676 .
O13 Ce1 O15 74.0(6) . .
O12 Ce1 O15 92.9(6) 10_676 .
O11 Ce1 O15 147.1(6) 15_455 .
O17 Ce1 O15 135.6(7) . .
O14 Ce1 O18 70.4(6) 10_676 .
O13 Ce1 O18 66.0(5) . .
O12 Ce1 O18 147.0(5) 10_676 .
O11 Ce1 O18 71.6(5) 15_455 .
O17 Ce1 O18 78.0(7) . .
O15 Ce1 O18 120.2(6) . .
O14 Ce1 N1 61.2(5) 10_676 10_676
O13 Ce1 N1 149.3(5) . 10_676
O12 Ce1 N1 61.4(4) 10_676 10_676
O11 Ce1 N1 71.3(5) 15_455 10_676
O17 Ce1 N1 129.9(6) . 10_676
O15 Ce1 N1 77.2(6) . 10_676
O18 Ce1 N1 122.5(6) . 10_676
O14 Ce1 O16 144.5(7) 10_676 .
O13 Ce1 O16 65.9(6) . .
O12 Ce1 O16 64.4(6) 10_676 .
O11 Ce1 O16 133.2(7) 15_455 .
O17 Ce1 O16 68.6(7) . .
O15 Ce1 O16 68.3(7) . .
O18 Ce1 O16 125.0(6) . .
N1 Ce1 O16 112.5(6) 10_676 .
O1 Si1 O1 109.3(4) 3_765 12_757
O1 Si1 O1 109.3(4) 3_765 10_677
O1 Si1 O1 109.7(8) 12_757 10_677
O1 Si1 O1 109.7(8) 3_765 .
O1 Si1 O1 109.3(4) 12_757 .
O1 Si1 O1 109.3(4) 10_677 .
C6 N1 C2 118.0(17) . .
C6 N1 Ce1 121.1(13) . 12_756
C2 N1 Ce1 120.7(12) . 12_756
Si1 O1 W2 124.7(6) . 12_757
Si1 O1 W1 124.4(6) . .
W2 O1 W1 91.7(4) 12_757 .
Si1 O1 W3 124.2(6) . 3_765
W2 O1 W3 90.6(4) 12_757 3_765
W1 O1 W3 91.3(4) . 3_765
W1 O2 W3 151.8(7) . .
W1 O3 W2 151.5(7) . .
W2 O4 W3 151.7(7) . .
W2 O5 W1 121.0(6) 12_757 .
W1 O6 W3 121.8(6) . 3_765
W3 O8 W2 122.4(7) 12_757 .
C1 O11 Ce1 141.9(13) . 15
C1 O12 Ce1 127.2(13) . 12_756
C7 O13 Ce1 141.0(15) . .
C7 O14 Ce1 127.0(14) . 12_756
O11 C1 O12 125(2) . .
O11 C1 C2 119.3(18) . .
O12 C1 C2 115.8(18) . .
N1 C2 C3 123.0(19) . .
N1 C2 C1 114.8(17) . .
C3 C2 C1 122.2(19) . .
C2 C3 C4 119(2) . .
C3 C4 C5 118(2) . .
C6 C5 C4 118.3(19) . .
N1 C6 C5 124.3(19) . .
N1 C6 C7 114.5(19) . .
C5 C6 C7 121.1(19) . .
O13 C7 O14 125(2) . .
O13 C7 C6 119(2) . .
O14 C7 C6 116.1(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O7 1.710(13) .
W1 O2 1.900(13) .
W1 O3 1.907(12) .
W1 O6 1.921(12) .
W1 O5 1.929(13) .
W1 O1 2.341(11) .
W2 O9 1.681(15) .
W2 O4 1.900(12) .
W2 O3 1.914(13) .
W2 O8 1.916(13) .
W2 O5 1.925(13) 10_677
W2 O1 2.334(12) 10_677
W3 O10 1.702(14) .
W3 O8 1.899(14) 10_677
W3 O2 1.920(13) .
W3 O4 1.921(12) .
W3 O6 1.934(12) 3_765
W3 O1 2.369(11) 3_765
Ce1 O14 2.499(15) 10_676
Ce1 O13 2.505(15) .
Ce1 O12 2.515(14) 10_676
Ce1 O11 2.518(15) 15_455
Ce1 O17 2.53(2) .
Ce1 O15 2.53(2) .
Ce1 O18 2.537(17) .
Ce1 N1 2.645(15) 10_676
Ce1 O16 2.67(2) .
Si1 O1 1.626(11) 3_765
Si1 O1 1.626(11) 12_757
Si1 O1 1.626(11) 10_677
Si1 O1 1.626(11) .
N1 C6 1.30(2) .
N1 C2 1.34(2) .
N1 Ce1 2.645(15) 12_756
O1 W2 2.334(12) 12_757
O1 W3 2.369(11) 3_765
O5 W2 1.925(13) 12_757
O6 W3 1.934(12) 3_765
O8 W3 1.899(14) 12_757
O11 C1 1.25(2) .
O11 Ce1 2.518(15) 15
O12 C1 1.28(2) .
O12 Ce1 2.515(14) 12_756
O13 C7 1.22(3) .
O14 C7 1.27(3) .
O14 Ce1 2.499(15) 12_756
C1 C2 1.52(3) .
C2 C3 1.38(3) .
C3 C4 1.38(3) .
C4 C5 1.42(3) .
C5 C6 1.36(3) .
C6 C7 1.52(3) .
