#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:22:05 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/65/7046598.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_7046598
loop_
_publ_author_name
'An, Haiyan'
'Zhang, Yumeng'
'Hou, Yujiao'
'Hu, Tao'
'Yang, Wei'
'Chang, Shenzhen'
'Zhang, Jianjun'
_publ_section_title
;
 Hybrid dimers based on metal-substituted Keggin polyoxometalates (metal =
 Ti, Ln) for cyanosilylation catalysis.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9079
_journal_page_last               9089
_journal_paper_doi               10.1039/c8dt00389k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C24 H54 K N4 O65 P Sm2 Ti2 W10'
_chemical_formula_weight         3743.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.421(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.889(4)
_cell_length_b                   30.183(6)
_cell_length_c                   15.327(3)
_cell_measurement_reflns_used    19022
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.490
_cell_volume                     7355(2)
_computing_data_collection       'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19022
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.490
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.539
_exptl_absorpt_correction_T_max  0.145
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.381
_exptl_crystal_description       'block '
_exptl_crystal_F_000             6752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         6.541
_refine_diff_density_min         -3.918
_refine_diff_density_rms         0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0659P)²+203.1434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5214
_reflns_number_total             6577
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00389k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7046596--7046601.cif.'
_cod_original_cell_volume        7355(3)
_cod_database_code               7046598
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.41615(4) 0.23948(2) 0.55422(6) 0.01723(18) Uani 1 1 d . . . . .
W2 W 0.35903(4) 0.24037(2) 0.28287(6) 0.01804(19) Uani 1 1 d . . . . .
W3 W 0.28531(4) 0.32233(2) 0.34778(6) 0.01567(18) Uani 1 1 d . . . . .
W4 W 0.44419(4) 0.32833(2) 0.21935(5) 0.01480(18) Uani 1 1 d . . . . .
W5 W 0.42648(5) 0.40928(2) 0.57103(6) 0.0139(2) Uani 0.8 1 d . . P A 1
Ti1 Ti 0.42648(5) 0.40928(2) 0.57103(6) 0.0139(2) Uani 0.2 1 d . . P A 2
W6 W 0.37091(10) 0.40805(5) 0.28465(13) 0.0093(3) Uani 0.2 1 d . . P A 3
Ti2 Ti 0.37091(10) 0.40805(5) 0.28465(13) 0.0093(3) Uani 0.8 1 d . . P A 4
Sm1 Sm 0.18751(7) 0.5000 0.11798(11) 0.0206(3) Uani 1 2 d S T P A .
Sm2 Sm 0.28500(9) 0.5000 0.57979(13) 0.0319(3) Uani 1 2 d S T P A .
K1 K 0.3988(5) 0.5000 0.1556(7) 0.0555(19) Uani 1 2 d S T P A .
P1 P 0.5000 0.32489(17) 0.5000 0.0089(11) Uani 1 2 d S TU P A .
O1 O 0.4813(6) 0.3540(3) 0.4024(9) 0.015(2) Uani 1 1 d . U . . .
O2 O 0.4240(6) 0.2945(3) 0.4446(8) 0.013(2) Uani 1 1 d . . . . .
O3 O 0.3952(7) 0.2003(4) 0.6120(10) 0.025(3) Uani 1 1 d . U . . .
O4 O 0.3021(8) 0.2018(4) 0.1727(11) 0.032(3) Uani 1 1 d . . . . .
O5 O 0.3730(7) 0.2116(3) 0.4097(10) 0.022(2) Uani 1 1 d . . . . .
O6 O 0.4195(8) 0.3165(4) 0.0903(10) 0.025(3) Uani 1 1 d . . . . .
O7 O 0.2745(7) 0.2741(3) 0.2519(9) 0.022(2) Uani 1 1 d . . . . .
O8 O 0.5326(7) 0.4356(4) 0.6700(9) 0.020(2) Uani 1 1 d . U . . .
O9 O 0.2960(7) 0.4466(3) 0.1878(9) 0.019(2) Uani 1 1 d . . . . .
O10 O 0.1821(7) 0.3295(4) 0.2750(10) 0.023(3) Uani 1 1 d . . . . .
O11 O 0.3990(6) 0.4238(3) 0.4302(9) 0.017(2) Uani 1 1 d . . . . .
O12 O 0.2992(6) 0.3622(3) 0.2698(8) 0.016(2) Uani 1 1 d . . . . .
O13 O 0.3696(6) 0.4481(4) 0.5746(9) 0.021(2) Uani 1 1 d . U . . .
O14 O 0.5292(7) 0.2846(4) 0.3251(9) 0.022(3) Uani 1 1 d . . . . .
O15 O 0.3645(6) 0.3705(3) 0.1704(9) 0.018(2) Uani 1 1 d . . . . .
O16 O 0.3144(7) 0.2740(3) 0.4600(9) 0.020(2) Uani 1 1 d . . . . .
O17 O 0.5265(6) 0.3720(3) 0.2855(9) 0.016(2) Uani 1 1 d . U . . .
O18 O 0.5263(6) 0.2242(4) 0.6262(9) 0.017(2) Uani 1 1 d . U . . .
O19 O 0.3733(6) 0.2854(4) 0.2117(9) 0.021(2) Uani 1 1 d . . . . .
O20 O 0.3463(7) 0.3604(3) 0.4824(9) 0.020(2) Uani 1 1 d . . . . .
O21 O 0.0936(9) 0.4479(4) -0.0374(13) 0.045(4) Uani 1 1 d . . . . .
O22 O -0.0334(9) 0.4198(5) -0.1397(16) 0.061(4) Uani 1 1 d . U . . .
O23 O 0.2856(10) 0.4397(5) 0.6733(14) 0.051(4) Uani 1 1 d . . . . .
O24 O 0.3275(16) 0.4231(7) 0.850(2) 0.098(7) Uani 1 1 d . U . . .
C1 C 0.0439(11) 0.4164(6) -0.0793(17) 0.028(4) Uani 1 1 d . U . . .
C2 C 0.0778(11) 0.3709(6) -0.0637(15) 0.029(4) Uani 1 1 d . . . . .
C3 C 0.1623(11) 0.3652(6) 0.0015(17) 0.034(4) Uani 1 1 d . U . . .
H3A H 0.1985 0.3893 0.0325 0.040 Uiso 1 1 calc R U . . .
C4 C 0.1437(13) 0.2869(6) -0.0253(16) 0.033(5) Uani 1 1 d . . . . .
H4A H 0.1685 0.2592 -0.0079 0.040 Uiso 1 1 calc R U . . .
C5 C 0.0603(12) 0.2910(7) -0.0952(18) 0.040(5) Uani 1 1 d . . . . .
H5A H 0.0260 0.2660 -0.1306 0.048 Uiso 1 1 calc R U . . .
C6 C 0.0247(12) 0.3332(6) -0.115(2) 0.041(5) Uani 1 1 d . . . . .
H6A H -0.0326 0.3362 -0.1607 0.050 Uiso 1 1 calc R U . . .
C7 C 0.3085(15) 0.4123(8) 0.753(2) 0.048(6) Uani 1 1 d . U . . .
C8 C 0.3176(13) 0.3661(7) 0.7397(17) 0.039(5) Uani 1 1 d . U . . .
C9 C 0.3014(12) 0.3507(7) 0.6409(17) 0.035(4) Uani 1 1 d . . . . .
H9A H 0.2793 0.3701 0.5780 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3466(12) 0.2792(7) 0.7165(18) 0.037(5) Uani 1 1 d . U . . .
H10A H 0.3575 0.2504 0.7084 0.045 Uiso 1 1 calc R U . . .
C11 C 0.3615(13) 0.2923(7) 0.8169(18) 0.045(5) Uani 1 1 d . U . . .
H11A H 0.3810 0.2718 0.8767 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3477(16) 0.3343(7) 0.8273(18) 0.054(7) Uani 1 1 d . . . . .
H12A H 0.3586 0.3425 0.8953 0.065 Uiso 1 1 calc R U . . .
N1 N 0.1898(10) 0.3239(5) 0.0183(15) 0.041(4) Uani 1 1 d . . . . .
H1A H 0.2429 0.3207 0.0619 0.049 Uiso 1 1 calc R U . . .
N2 N 0.3159(10) 0.3099(6) 0.6327(15) 0.041(4) Uani 1 1 d . . . . .
H2A H 0.3050 0.3023 0.5691 0.050 Uiso 1 1 calc R U . . .
O1W O 0.0843(11) 0.5000 0.1310(18) 0.038(5) Uani 1 2 d S T P . .
H1WA H 0.0368 0.5178 0.0797 0.046 Uiso 0.5 1 calc R U P A .
H1WB H 0.0918 0.4822 0.1872 0.046 Uiso 0.5 1 calc R U P . .
O2W O 0.2888(10) 0.5000 0.3419(14) 0.025(4) Uani 1 2 d S TU P . .
H2WA H 0.3415 0.5000 0.3838 0.030 Uiso 1 2 d R U P A .
H2WB H 0.2707 0.5000 0.3763 0.030 Uiso 1 2 d R U P . .
O3W O 0.2134(11) 0.5000 -0.0157(15) 0.027(4) Uani 1 2 d S T P A .
O4W O 0.1814(9) 0.4283(4) 0.2090(13) 0.047(4) Uani 1 1 d . . . . .
H4WA H 0.2193 0.4086 0.2411 0.056 Uiso 1 1 d R U . A .
H4WB H 0.1417 0.4248 0.2064 0.056 Uiso 1 1 d R U . . .
O6W O 0.1482(14) 0.5000 0.518(2) 0.070(7) Uani 1 2 d S T P . .
H6WA H 0.1169 0.4772 0.4848 0.084 Uiso 0.5 1 d R U P A .
H6WB H 0.1319 0.5228 0.5298 0.084 Uiso 0.5 1 d R U P . .
O7W O 0.1926(11) 0.4505(7) 0.4096(16) 0.085(6) Uani 1 1 d . . . . .
H7WA H 0.2133 0.4308 0.3966 0.101 Uiso 1 1 d R U . A .
H7WB H 0.1396 0.4528 0.3629 0.101 Uiso 1 1 d R U . . .
OW1 O 0.087(2) 0.3937(10) 0.389(3) 0.071(10) Uani 0.5 1 d . U P . .
OW2 O 0.497(3) 0.0000 1.287(4) 0.167(17) Uani 1 2 d S TU P . .
OW3 O 0.4838(18) 0.5728(8) 0.095(2) 0.127(9) Uani 1 1 d . U . . .
OW4 O 0.2626(19) 0.5807(9) -0.047(2) 0.133(9) Uani 1 1 d . U . . .
OW5 O 0.327(4) 0.5000 -0.082(4) 0.079(15) Uani 0.5 2 d S TU P A .
OW6 O -0.088(4) 0.414(2) 0.267(6) 0.16(2) Uani 0.5 1 d . U P . .
OW7 O 0.128(4) 0.5000 0.676(6) 0.10(2) Uani 0.5 2 d S TU P . .
O5W O 0.4048(17) 0.5000 0.750(3) 0.080(7) Uani 1 2 d S TU P . .
H5WA H 0.4201 0.5217 0.8054 0.096 Uiso 0.5 1 calc R U P A .
H5WB H 0.4433 0.4783 0.7716 0.096 Uiso 0.5 1 calc R U 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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 W1 O18 102.5(5) . .
O3 W1 O5 101.6(5) . .
O18 W1 O5 89.1(4) . .
O3 W1 O14 101.7(5) . 2_656
O18 W1 O14 84.9(4) . 2_656
O5 W1 O14 156.7(4) . 2_656
O3 W1 O16 100.3(5) . .
O18 W1 O16 157.1(4) . .
O5 W1 O16 88.5(5) . .
O14 W1 O16 88.4(4) 2_656 .
O3 W1 O2 171.5(4) . .
O18 W1 O2 84.5(4) . .
O5 W1 O2 73.4(4) . .
O14 W1 O2 83.6(4) 2_656 .
O16 W1 O2 73.1(4) . .
O4 W2 O7 101.5(5) . .
O4 W2 O19 102.6(5) . .
O7 W2 O19 89.4(5) . .
O4 W2 O18 104.4(5) . 2_656
O7 W2 O18 154.0(4) . 2_656
O19 W2 O18 87.1(4) . 2_656
O4 W2 O5 101.1(5) . .
O7 W2 O5 86.9(5) . .
O19 W2 O5 156.3(4) . .
O18 W2 O5 86.1(4) 2_656 .
O4 W2 O2 170.4(5) . .
O7 W2 O2 71.2(4) . .
O19 W2 O2 83.9(4) . .
O18 W2 O2 82.8(4) 2_656 .
O5 W2 O2 72.7(4) . .
O10 W3 O12 103.0(5) . .
O10 W3 O20 105.1(5) . .
O12 W3 O20 90.2(4) . .
O10 W3 O7 100.4(5) . .
O12 W3 O7 89.3(5) . .
O20 W3 O7 154.0(5) . .
O10 W3 O16 98.7(5) . .
O12 W3 O16 158.2(4) . .
O20 W3 O16 86.3(4) . .
O7 W3 O16 84.7(4) . .
O10 W3 O2 167.1(4) . .
O12 W3 O2 85.9(4) . .
O20 W3 O2 84.0(4) . .
O7 W3 O2 70.0(4) . .
O16 W3 O2 72.4(4) . .
O6 W4 O15 102.5(5) . .
O6 W4 O17 101.4(5) . .
O15 W4 O17 91.3(4) . .
O6 W4 O14 100.8(5) . .
O15 W4 O14 155.7(4) . .
O17 W4 O14 90.7(4) . .
O6 W4 O19 100.8(5) . .
O15 W4 O19 86.8(5) . .
O17 W4 O19 157.7(4) . .
O14 W4 O19 82.2(4) . .
O6 W4 O1 173.7(4) . .
O15 W4 O1 74.0(4) . .
O17 W4 O1 73.6(4) . .
O14 W4 O1 83.4(4) . .
O19 W4 O1 84.5(4) . .
O13 W5 O11 102.2(5) . .
O13 W5 O8 101.8(5) . .
O11 W5 O8 94.2(4) . .
O13 W5 O20 102.2(5) . .
O11 W5 O20 87.2(4) . .
O8 W5 O20 155.1(4) . .
O13 W5 O17 100.5(5) . 2_656
O11 W5 O17 156.7(4) . 2_656
O8 W5 O17 86.2(4) . 2_656
O20 W5 O17 83.0(4) . 2_656
O13 W5 O1 171.6(4) . 2_656
O11 W5 O1 85.7(4) . 2_656
O8 W5 O1 74.3(4) . 2_656
O20 W5 O1 81.0(4) . 2_656
O17 W5 O1 72.0(4) 2_656 2_656
O9 W6 O8 100.5(5) . 2_656
O9 W6 O11 101.0(5) . .
O8 W6 O11 94.5(4) 2_656 .
O9 W6 O12 99.5(5) . .
O8 W6 O12 159.9(4) 2_656 .
O11 W6 O12 84.4(4) . .
O9 W6 O15 100.2(5) . .
O8 W6 O15 87.7(4) 2_656 .
O11 W6 O15 157.9(4) . .
O12 W6 O15 86.1(4) . .
O9 W6 O1 171.2(4) . .
O8 W6 O1 74.4(4) 2_656 .
O11 W6 O1 86.7(4) . .
O12 W6 O1 85.4(4) . .
O15 W6 O1 72.7(4) . .
O9 W6 K1 55.6(4) . .
O8 W6 K1 46.9(3) 2_656 .
O11 W6 K1 113.4(3) . .
O12 W6 K1 150.6(3) . .
O15 W6 K1 84.0(3) . .
O1 W6 K1 117.5(3) . .
O21 Sm1 O21 82.9(7) 6_565 .
O21 Sm1 O1W 82.4(5) 6_565 .
O21 Sm1 O1W 82.4(5) . .
O21 Sm1 O9 85.0(4) 6_565 6_565
O21 Sm1 O9 142.4(4) . 6_565
O1W Sm1 O9 130.9(3) . 6_565
O21 Sm1 O9 142.4(4) 6_565 .
O21 Sm1 O9 85.0(4) . .
O1W Sm1 O9 130.9(3) . .
O9 Sm1 O9 83.3(5) 6_565 .
O21 Sm1 O3W 72.7(5) 6_565 .
O21 Sm1 O3W 72.7(5) . .
O1W Sm1 O3W 146.5(6) . .
O9 Sm1 O3W 69.7(4) 6_565 .
O9 Sm1 O3W 69.7(4) . .
O21 Sm1 O2W 135.8(4) 6_565 .
O21 Sm1 O2W 135.8(4) . .
O1W Sm1 O2W 83.3(6) . .
O9 Sm1 O2W 73.6(4) 6_565 .
O9 Sm1 O2W 73.6(4) . .
O3W Sm1 O2W 130.2(5) . .
O21 Sm1 O4W 70.3(5) 6_565 6_565
O21 Sm1 O4W 138.8(4) . 6_565
O1W Sm1 O4W 64.0(4) . 6_565
O9 Sm1 O4W 67.0(4) 6_565 6_565
O9 Sm1 O4W 134.8(4) . 6_565
O3W Sm1 O4W 124.3(3) . 6_565
O2W Sm1 O4W 65.9(4) . 6_565
O21 Sm1 O4W 138.8(4) 6_565 .
O21 Sm1 O4W 70.3(5) . .
O1W Sm1 O4W 64.0(4) . .
O9 Sm1 O4W 134.8(4) 6_565 .
O9 Sm1 O4W 67.0(4) . .
O3W Sm1 O4W 124.3(3) . .
O2W Sm1 O4W 65.9(4) . .
O4W Sm1 O4W 110.9(7) 6_565 .
O21 Sm1 K1 104.3(3) 6_565 .
O21 Sm1 K1 104.3(3) . .
O1W Sm1 K1 170.9(5) . .
O9 Sm1 K1 45.3(2) 6_565 .
O9 Sm1 K1 45.3(2) . .
O3W Sm1 K1 42.6(4) . .
O2W Sm1 K1 87.6(4) . .
O4W Sm1 K1 112.1(3) 6_565 .
O4W Sm1 K1 112.1(3) . .
O5W Sm2 O23 75.8(5) . 6_565
O5W Sm2 O23 75.8(5) . .
O23 Sm2 O23 103.9(7) 6_565 .
O5W Sm2 O7W 139.0(5) . .
O23 Sm2 O7W 142.9(6) 6_565 .
O23 Sm2 O7W 80.0(6) . .
O5W Sm2 O7W 139.0(5) . 6_565
O23 Sm2 O7W 80.0(6) 6_565 6_565
O23 Sm2 O7W 142.9(6) . 6_565
O7W Sm2 O7W 76.1(10) . 6_565
O5W Sm2 O6W 129.9(8) . .
O23 Sm2 O6W 73.9(5) 6_565 .
O23 Sm2 O6W 73.9(5) . .
O7W Sm2 O6W 71.9(6) . .
O7W Sm2 O6W 71.9(6) 6_565 .
O5W Sm2 O13 73.3(5) . .
O23 Sm2 O13 146.6(5) 6_565 .
O23 Sm2 O13 80.6(4) . .
O7W Sm2 O13 70.3(5) . .
O7W Sm2 O13 116.5(5) 6_565 .
O6W Sm2 O13 137.3(3) . .
O5W Sm2 O13 73.3(5) . 6_565
O23 Sm2 O13 80.6(4) 6_565 6_565
O23 Sm2 O13 146.6(5) . 6_565
O7W Sm2 O13 116.5(5) . 6_565
O7W Sm2 O13 70.3(5) 6_565 6_565
O6W Sm2 O13 137.3(3) . 6_565
O13 Sm2 O13 78.7(5) . 6_565
O8 K1 O8 89.2(5) 5_666 2_656
O8 K1 OW5 134.6(3) 5_666 .
O8 K1 OW5 134.6(3) 2_656 .
O8 K1 O3W 111.1(4) 5_666 .
O8 K1 O3W 111.1(4) 2_656 .
OW5 K1 O3W 69.0(12) . .
O8 K1 O9 100.6(4) 5_666 .
O8 K1 O9 56.4(3) 2_656 .
OW5 K1 O9 112.8(10) . .
O3W K1 O9 55.4(3) . .
O8 K1 O9 56.4(3) 5_666 6_565
O8 K1 O9 100.6(4) 2_656 6_565
OW5 K1 O9 112.8(10) . 6_565
O3W K1 O9 55.4(3) . 6_565
O9 K1 O9 63.3(4) . 6_565
O8 K1 OW3 133.1(6) 5_666 6_565
O8 K1 OW3 76.9(4) 2_656 6_565
OW5 K1 OW3 64.6(9) . 6_565
O3W K1 OW3 115.7(5) . 6_565
O9 K1 OW3 107.7(4) . 6_565
O9 K1 OW3 169.5(5) 6_565 6_565
O8 K1 OW3 76.9(4) 5_666 .
O8 K1 OW3 133.1(6) 2_656 .
OW5 K1 OW3 64.6(9) . .
O3W K1 OW3 115.7(5) . .
O9 K1 OW3 169.5(5) . .
O9 K1 OW3 107.7(4) 6_565 .
OW3 K1 OW3 80.8(8) 6_565 .
O8 K1 OW4 158.6(5) 5_666 6_565
O8 K1 OW4 86.2(5) 2_656 6_565
OW5 K1 OW4 57.3(8) . 6_565
O3W K1 OW4 52.1(5) . 6_565
O9 K1 OW4 59.7(5) . 6_565
O9 K1 OW4 104.0(5) 6_565 6_565
OW3 K1 OW4 65.9(6) 6_565 6_565
OW3 K1 OW4 120.8(6) . 6_565
O8 K1 OW4 86.2(5) 5_666 .
O8 K1 OW4 158.6(5) 2_656 .
OW5 K1 OW4 57.3(8) . .
O3W K1 OW4 52.1(5) . .
O9 K1 OW4 104.0(5) . .
O9 K1 OW4 59.7(5) 6_565 .
OW3 K1 OW4 120.8(6) 6_565 .
OW3 K1 OW4 65.9(6) . .
OW4 K1 OW4 90.6(9) 6_565 .
O8 K1 W6 100.9(3) 5_666 .
O8 K1 W6 30.1(2) 2_656 .
OW5 K1 W6 122.9(5) . .
O3W K1 W6 81.0(2) . .
O9 K1 W6 27.2(2) . .
O9 K1 W6 84.2(3) 6_565 .
OW3 K1 W6 89.0(4) 6_565 .
OW3 K1 W6 162.9(5) . .
OW4 K1 W6 65.8(4) 6_565 .
OW4 K1 W6 131.2(5) . .
O1 P1 O1 109.8(8) 2_656 .
O1 P1 O2 110.1(5) 2_656 .
O1 P1 O2 109.9(5) . .
O1 P1 O2 109.9(5) 2_656 2_656
O1 P1 O2 110.0(5) . 2_656
O2 P1 O2 107.1(8) . 2_656
P1 O1 W6 125.5(5) . .
P1 O1 Ti1 126.8(5) . 2_656
P1 O1 W5 126.8(5) . 2_656
P1 O1 W4 126.4(6) . .
W6 O1 W4 89.1(3) . .
Ti1 O1 W4 89.6(3) 2_656 .
W5 O1 W4 89.6(3) 2_656 .
P1 O2 W3 123.3(6) . .
P1 O2 W2 127.6(5) . .
W3 O2 W2 90.0(3) . .
P1 O2 W1 125.6(5) . .
W3 O2 W1 90.3(3) . .
W2 O2 W1 88.7(3) . .
W1 O5 W2 125.1(5) . .
W2 O7 W3 128.8(6) . .
W5 O8 K1 129.1(5) . 5_666
Ti2 O8 K1 103.0(5) 2_656 5_666
W6 O8 K1 103.0(5) 2_656 5_666
W6 O9 Sm1 154.5(5) . .
W6 O9 K1 97.2(4) . .
Sm1 O9 K1 100.6(4) . .
W3 O12 W6 147.4(5) . .
W5 O13 Sm2 176.9(6) . .
W1 O14 W4 154.7(6) 2_656 .
W4 O15 W6 123.6(5) . .
W1 O16 W3 124.2(5) . .
W4 O17 Ti1 124.4(5) . 2_656
W4 O17 W5 124.4(5) . 2_656
W1 O18 W2 150.2(6) . 2_656
W2 O19 W4 151.0(6) . .
W3 O20 W5 147.1(6) . .
C1 O21 Sm1 150.8(14) . .
C7 O23 Sm2 161.4(16) . .
O21 C1 O22 125.2(17) . .
O21 C1 C2 117.2(16) . .
O22 C1 C2 117.4(16) . .
C3 C2 C6 118.8(17) . .
C3 C2 C1 119.9(16) . .
C6 C2 C1 121.3(16) . .
N1 C3 C2 117.4(18) . .
N1 C4 C5 117.8(18) . .
C4 C5 C6 120.0(18) . .
C5 C6 C2 118.9(17) . .
O23 C7 O24 124(2) . .
O23 C7 C8 120.1(18) . .
O24 C7 C8 116(2) . .
C9 C8 C12 115(2) . .
C9 C8 C7 121.6(18) . .
C12 C8 C7 123.4(18) . .
N2 C9 C8 122.1(19) . .
N2 C10 C11 117(2) . .
C12 C11 C10 120.0(19) . .
C11 C12 C8 122(2) . .
C3 N1 C4 126.9(17) . .
C9 N2 C10 124.1(18) . .
Sm1 O3W K1 102.8(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O3 1.718(10) .
W1 O18 1.895(10) .
W1 O5 1.905(11) .
W1 O14 1.915(11) 2_656
W1 O16 1.927(11) .
W1 O2 2.450(10) .
W2 O4 1.693(12) .
W2 O7 1.866(11) .
W2 O19 1.897(11) .
W2 O18 1.916(10) 2_656
W2 O5 1.951(10) .
W2 O2 2.446(9) .
W3 O10 1.711(11) .
W3 O12 1.862(10) .
W3 O20 1.890(11) .
W3 O7 1.963(10) .
W3 O16 1.995(10) .
W3 O2 2.436(10) .
W4 O6 1.692(11) .
W4 O15 1.851(10) .
W4 O17 1.870(10) .
W4 O14 1.919(11) .
W4 O19 1.964(11) .
W4 O1 2.449(9) .
W5 O13 1.738(11) .
W5 O11 1.851(10) .
W5 O8 1.867(11) .
W5 O20 1.956(11) .
W5 O17 2.013(10) 2_656
W5 O1 2.427(10) 2_656
W6 O9 1.703(10) .
W6 O8 1.903(11) 2_656
W6 O11 1.923(10) .
W6 O12 1.985(10) .
W6 O15 2.008(10) .
W6 O1 2.400(10) .
W6 K1 3.695(5) .
Sm1 O21 2.374(14) 6_565
Sm1 O21 2.374(14) .
Sm1 O1W 2.401(17) .
Sm1 O9 2.426(10) 6_565
Sm1 O9 2.426(10) .
Sm1 O3W 2.473(15) .
Sm1 O2W 2.497(16) .
Sm1 O4W 2.627(13) 6_565
Sm1 O4W 2.627(13) .
Sm1 K1 4.250(8) .
Sm2 O5W 2.07(3) .
Sm2 O23 2.310(14) 6_565
Sm2 O23 2.310(14) .
Sm2 O7W 2.424(18) .
Sm2 O7W 2.424(18) 6_565
Sm2 O6W 2.44(2) .
Sm2 O13 2.468(11) .
Sm2 O13 2.468(11) 6_565
K1 O8 2.767(12) 5_666
K1 O8 2.767(12) 2_656
K1 OW5 2.80(4) .
K1 O3W 2.95(2) .
K1 O9 3.072(12) .
K1 O9 3.072(12) 6_565
K1 OW3 3.39(3) 6_565
K1 OW3 3.39(3) .
K1 OW4 3.43(3) 6_565
K1 OW4 3.43(3) .
P1 O1 1.529(10) 2_656
P1 O1 1.529(10) .
P1 O2 1.546(10) .
P1 O2 1.546(10) 2_656
O1 Ti1 2.427(10) 2_656
O1 W5 2.427(10) 2_656
O8 Ti2 1.903(11) 2_656
O8 W6 1.903(11) 2_656
O8 K1 2.767(12) 5_666
O14 W1 1.915(11) 2_656
O17 Ti1 2.013(10) 2_656
O17 W5 2.013(10) 2_656
O18 W2 1.916(10) 2_656
O21 C1 1.24(2) .
O22 C1 1.26(2) .
O23 C7 1.26(2) .
O24 C7 1.29(3) .
C1 C2 1.50(2) .
C2 C3 1.38(2) .
C2 C6 1.42(2) .
C3 N1 1.33(2) .
C4 N1 1.34(2) .
C4 C5 1.34(3) .
C5 C6 1.41(3) .
C7 C8 1.44(3) .
C8 C9 1.38(3) .
C8 C12 1.39(3) .
C9 N2 1.30(3) .
C10 N2 1.33(3) .
C10 C11 1.39(3) .
C11 C12 1.34(3) .
