#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:22:05 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/65/7046597.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_7046597
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 H62 K N4 Nd2 O69 P Ti2 W10'
_chemical_formula_weight         3803.53
_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                 133.528(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.916(13)
_cell_length_b                   30.097(19)
_cell_length_c                   15.243(9)
_cell_measurement_reflns_used    18523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.449
_cell_volume                     7290(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.992
_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  0.1022
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18523
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.449
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.516
_exptl_absorpt_correction_T_max  0.086
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    3.466
_exptl_crystal_description       'block '
_exptl_crystal_F_000             6894
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.967
_refine_diff_density_min         -2.911
_refine_diff_density_rms         0.469
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         6503
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0540
_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)+(0.0361P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4931
_reflns_number_total             6503
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00389k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7046596--7046601.cif.'
_cod_database_code               7046597
_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 0.35876(4) 0.24005(2) -0.21809(6) 0.01124(18) Uani 1 1 d . . . . .
W2 W 0.28603(4) 0.32205(2) -0.15177(6) 0.00969(17) Uani 1 1 d . . . . .
W3 W 0.41678(4) 0.23915(2) 0.05445(6) 0.01054(18) Uani 1 1 d . . . . .
W4 W 0.55588(4) 0.32795(2) 0.28121(6) 0.00960(17) Uani 1 1 d . . . . .
W5 W 0.42674(5) 0.40899(2) 0.07180(7) 0.00857(19) Uani 0.78 1 d . . P A 1
Ti1 Ti 0.42674(5) 0.40899(2) 0.07180(7) 0.00857(19) Uani 0.22 1 d . . P A 2
W6 W 0.62789(9) 0.40769(4) 0.21493(14) 0.0064(3) Uani 0.22 1 d . . P A 3
Ti2 Ti 0.62789(9) 0.40769(4) 0.21493(14) 0.0064(3) Uani 0.78 1 d . . P A 4
Nd1 Nd 0.81335(7) 0.5000 0.38297(11) 0.0113(3) Uani 1 2 d S T P A .
Nd2 Nd 0.28405(8) 0.5000 0.08113(12) 0.0161(3) Uani 1 2 d S T P A .
K1 K 0.6027(4) 0.5000 0.3484(6) 0.0342(15) Uani 1 2 d S T P A .
P1 P 0.5000 0.32448(15) 0.0000 0.0058(11) Uani 1 2 d S T P A .
O1 O 0.5192(6) 0.3530(3) 0.0979(9) 0.009(2) Uani 1 1 d . U . . .
O2 O 0.4244(6) 0.2944(3) -0.0543(9) 0.010(2) Uani 1 1 d . U . . .
O3 O 0.3991(6) 0.4241(3) -0.0689(9) 0.011(2) Uani 1 1 d . . . . .
O4 O 0.3446(6) 0.3600(3) -0.0201(9) 0.012(2) Uani 1 1 d . U . . .
O5 O 0.7037(6) 0.4458(3) 0.3129(9) 0.010(2) Uani 1 1 d . U . . .
O6 O 0.2726(7) 0.2735(3) -0.2497(9) 0.012(2) Uani 1 1 d . . . . .
O7 O 0.5323(6) 0.4349(3) 0.1716(9) 0.010(2) Uani 1 1 d . U . . .
O8 O 0.3716(6) 0.4466(3) 0.0790(9) 0.011(2) Uani 1 1 d . U . . .
O9 O 0.5794(7) 0.3154(3) 0.4109(10) 0.015(2) Uani 1 1 d . U . . .
O10 O 0.3010(7) 0.2010(3) -0.3297(10) 0.017(2) Uani 1 1 d . U . . .
O11 O 0.1837(7) 0.3297(3) -0.2239(10) 0.015(2) Uani 1 1 d . . . . .
O12 O 0.3947(7) 0.1996(3) 0.1117(10) 0.018(3) Uani 1 1 d . . . . .
O13 O 0.6286(6) 0.2846(3) 0.2906(9) 0.010(2) Uani 1 1 d . U . . .
O14 O 0.5276(6) 0.2242(3) 0.1275(9) 0.009(2) Uani 1 1 d . U . . .
O15 O 0.4701(6) 0.2851(3) 0.1722(9) 0.012(2) Uani 1 1 d . U . . .
O16 O 0.3162(7) 0.2742(3) -0.0410(9) 0.013(2) Uani 1 1 d . . . . .
O17 O 0.4740(7) 0.3714(3) 0.2137(10) 0.014(2) Uani 1 1 d . . . . .
O18 O 0.3002(7) 0.3613(3) -0.2290(9) 0.013(2) Uani 1 1 d . . . . .
O19 O 0.6375(6) 0.3701(3) 0.3329(9) 0.011(2) Uani 1 1 d . . . . .
O20 O 0.3737(6) 0.2111(3) -0.0899(9) 0.012(2) Uani 1 1 d . U . . .
O21 O 0.9089(7) 0.5533(4) 0.5431(11) 0.022(3) Uani 1 1 d . U . . .
O22 O 1.0325(8) 0.5807(4) 0.6358(13) 0.038(3) Uani 1 1 d . U . . .
O23 O 0.3349(9) 0.4215(4) 0.3593(12) 0.033(3) Uani 1 1 d . . . . .
O24 O 0.2870(8) 0.4386(4) 0.1785(11) 0.024(3) Uani 1 1 d . . . . .
N1 N 0.8077(10) 0.6767(5) 0.4787(14) 0.028(4) Uani 1 1 d . . . . .
H1A H 0.7542 0.6798 0.4319 0.034 Uiso 1 1 calc R U . . .
N2 N 0.3156(9) 0.3087(5) 0.1300(14) 0.021(3) Uani 1 1 d . U . . .
H2A H 0.3038 0.3009 0.0654 0.026 Uiso 1 1 calc R U . . .
C1 C 0.9582(10) 0.5839(5) 0.5818(15) 0.016(4) Uani 1 1 d . U . . .
C2 C 0.9251(10) 0.6299(5) 0.5681(14) 0.016(4) Uani 1 1 d . U . . .
C3 C 0.8400(10) 0.6367(5) 0.5022(16) 0.021(4) Uani 1 1 d . . . . .
H3A H 0.8050 0.6122 0.4741 0.026 Uiso 1 1 calc R U . . .
C4 C 0.8557(11) 0.7117(5) 0.5253(15) 0.021(4) Uani 1 1 d . U . . .
H4A H 0.8321 0.7394 0.5130 0.025 Uiso 1 1 calc R U . . .
C5 C 0.9418(11) 0.7088(5) 0.5932(16) 0.020(4) Uani 1 1 d . . . . .
H5A H 0.9745 0.7343 0.6207 0.025 Uiso 1 1 calc R U . . .
C6 C 0.9760(11) 0.6687(5) 0.6177(16) 0.023(4) Uani 1 1 d . . . . .
H6A H 1.0339 0.6661 0.6680 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3156(11) 0.4130(6) 0.2621(19) 0.028(5) Uani 1 1 d . . . . .
C8 C 0.3227(12) 0.3626(5) 0.2452(16) 0.022(4) Uani 1 1 d . . . . .
C9 C 0.3018(11) 0.3506(5) 0.1414(17) 0.024(4) Uani 1 1 d . U . . .
H9A H 0.2784 0.3711 0.0797 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3470(11) 0.2789(6) 0.2155(15) 0.022(4) Uani 1 1 d . . . . .
H10A H 0.3562 0.2500 0.2053 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3660(11) 0.2899(6) 0.3178(17) 0.025(4) Uani 1 1 d . U . . .
H11A H 0.3874 0.2691 0.3782 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3523(12) 0.3329(5) 0.3288(17) 0.023(4) Uani 1 1 d . . . . .
H12A H 0.3644 0.3413 0.3981 0.027 Uiso 1 1 calc R U . . .
O1W O 0.8190(7) 0.5721(3) 0.2926(11) 0.020(3) Uani 1 1 d . U . . .
H1WA H 0.7813 0.5919 0.2611 0.024 Uiso 1 1 d R U . A .
H1WB H 0.8583 0.5756 0.2945 0.024 Uiso 1 1 d R U . . .
O2W O 0.7899(11) 0.5000 0.5236(16) 0.024(4) Uani 1 2 d S T P A .
O3W O 0.7073(10) 0.5000 0.1547(14) 0.018(4) Uani 1 2 d S TU P . .
H3WA H 0.6550 0.5000 0.1144 0.021 Uiso 1 2 d R U P A .
H3WB H 0.7239 0.5000 0.1182 0.021 Uiso 1 2 d R U P . .
O4W O 0.9190(10) 0.5000 0.3708(17) 0.027(4) Uani 1 2 d S T P . .
H4WA H 0.9665 0.5179 0.4227 0.032 Uiso 0.5 1 calc R U P A .
H4WB H 0.9116 0.4821 0.3143 0.032 Uiso 0.5 1 calc R U P . .
O5W O 0.4210(13) 0.5000 0.2848(17) 0.036(5) Uani 1 2 d S T P A .
O6W O 0.1927(9) 0.4489(5) -0.0898(12) 0.040(4) Uani 1 1 d . . . . .
H6WA H 0.2140 0.4290 -0.1015 0.048 Uiso 1 1 d R U . A .
H6WB H 0.1395 0.4510 -0.1376 0.048 Uiso 1 1 d R U . . .
O7W O 0.1458(11) 0.5000 0.0176(15) 0.028(4) Uani 1 2 d S TU P . .
H7WA H 0.1149 0.4770 -0.0148 0.034 Uiso 0.5 1 d R U P A .
H7WB H 0.1290 0.5230 0.0281 0.034 Uiso 0.5 1 d R U P . .
OW1 O 0.2473(13) 0.4174(5) 0.4360(18) 0.064(5) Uani 1 1 d . . . . .
OW2 O 0.0864(12) 0.3944(6) -0.1072(19) 0.073(6) Uani 1 1 d . . . . .
OW3 O 0.5259(13) 0.5694(5) 0.4002(15) 0.075(6) Uani 1 1 d . . . . .
OW4 O 0.6962(18) 0.5000 0.601(2) 0.068(7) Uani 1 2 d S T P A .
OW6 O 0.920(2) 0.5821(10) 0.779(3) 0.060(10) Uani 0.5 1 d . . P . .
OW5 O 0.110(3) 0.3854(13) 0.099(3) 0.190(15) Uani 1 1 d . U . . .
OW7 O 0.9874(18) 0.5000 0.789(2) 0.100(11) Uani 1 2 d S T P . .
OW8 O 0.863(2) 0.5000 0.810(3) 0.121(12) Uani 1 2 d S TU 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'
Nd Nd -0.1943 3.0179 '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'
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
O10 W1 O13 102.4(5) . 2_655
O10 W1 O6 100.9(5) . .
O13 W1 O6 89.7(4) 2_655 .
O10 W1 O14 104.6(5) . 2_655
O13 W1 O14 87.5(4) 2_655 2_655
O6 W1 O14 154.3(4) . 2_655
O10 W1 O20 100.9(5) . .
O13 W1 O20 156.7(4) 2_655 .
O6 W1 O20 86.7(4) . .
O14 W1 O20 85.8(4) 2_655 .
O10 W1 O2 170.2(4) . .
O13 W1 O2 84.3(4) 2_655 .
O6 W1 O2 71.7(4) . .
O14 W1 O2 82.6(4) 2_655 .
O20 W1 O2 72.7(4) . .
O11 W2 O18 103.1(5) . .
O11 W2 O4 103.8(5) . .
O18 W2 O4 90.1(4) . .
O11 W2 O16 99.8(5) . .
O18 W2 O16 156.9(5) . .
O4 W2 O16 87.0(4) . .
O11 W2 O6 99.7(5) . .
O18 W2 O6 89.6(4) . .
O4 W2 O6 155.9(4) . .
O16 W2 O6 83.9(4) . .
O11 W2 O2 167.8(4) . .
O18 W2 O2 85.5(4) . .
O4 W2 O2 84.6(4) . .
O16 W2 O2 71.5(4) . .
O6 W2 O2 71.3(4) . .
O12 W3 O20 101.0(5) . .
O12 W3 O15 103.2(5) . .
O20 W3 O15 155.9(4) . .
O12 W3 O14 103.3(5) . .
O20 W3 O14 89.3(4) . .
O15 W3 O14 85.0(4) . .
O12 W3 O16 100.8(5) . .
O20 W3 O16 88.4(4) . .
O15 W3 O16 87.4(4) . .
O14 W3 O16 155.9(4) . .
O12 W3 O2 171.0(4) . .
O20 W3 O2 74.1(4) . .
O15 W3 O2 82.0(4) . .
O14 W3 O2 84.4(4) . .
O16 W3 O2 71.9(4) . .
O9 W4 O17 101.7(5) . .
O9 W4 O19 103.0(5) . .
O17 W4 O19 92.0(4) . .
O9 W4 O15 100.9(5) . .
O17 W4 O15 89.8(4) . .
O19 W4 O15 155.2(4) . .
O9 W4 O13 100.6(5) . .
O17 W4 O13 157.4(5) . .
O19 W4 O13 85.9(4) . .
O15 W4 O13 83.1(4) . .
O9 W4 O1 174.5(4) . .
O17 W4 O1 73.5(4) . .
O19 W4 O1 74.8(4) . .
O15 W4 O1 82.1(4) . .
O13 W4 O1 84.3(4) . .
O8 W5 O3 103.3(5) . .
O8 W5 O7 101.9(5) . .
O3 W5 O7 94.3(4) . .
O8 W5 O4 101.6(5) . .
O3 W5 O4 87.2(4) . .
O7 W5 O4 155.5(4) . .
O8 W5 O17 99.7(5) . .
O3 W5 O17 156.4(4) . .
O7 W5 O17 85.8(4) . .
O4 W5 O17 83.3(4) . .
O8 W5 O1 170.3(4) . .
O3 W5 O1 86.0(4) . .
O7 W5 O1 74.4(4) . .
O4 W5 O1 81.3(4) . .
O17 W5 O1 71.3(4) . .
O5 W6 O7 101.0(5) . .
O5 W6 O3 100.2(5) . 2_655
O7 W6 O3 95.7(4) . 2_655
O5 W6 O18 99.0(5) . 2_655
O7 W6 O18 159.7(4) . 2_655
O3 W6 O18 84.0(4) 2_655 2_655
O5 W6 O19 99.0(4) . .
O7 W6 O19 88.0(4) . .
O3 W6 O19 159.3(4) 2_655 .
O18 W6 O19 85.6(4) 2_655 .
O5 W6 O1 171.6(4) . .
O7 W6 O1 75.1(4) . .
O3 W6 O1 87.7(4) 2_655 .
O18 W6 O1 84.6(4) 2_655 .
O19 W6 O1 73.6(4) . .
O5 W6 K1 55.7(4) . .
O7 W6 K1 47.1(3) . .
O3 W6 K1 113.5(3) 2_655 .
O18 W6 K1 150.3(3) 2_655 .
O19 W6 K1 83.9(3) . .
O1 W6 K1 118.5(3) . .
O21 Nd1 O21 82.9(5) . 6_565
O21 Nd1 O5 141.7(4) . .
O21 Nd1 O5 84.7(3) 6_565 .
O21 Nd1 O5 84.7(3) . 6_565
O21 Nd1 O5 141.7(4) 6_565 6_565
O5 Nd1 O5 83.1(5) . 6_565
O21 Nd1 O4W 82.5(4) . .
O21 Nd1 O4W 82.5(4) 6_565 .
O5 Nd1 O4W 131.3(3) . .
O5 Nd1 O4W 131.3(3) 6_565 .
O21 Nd1 O3W 136.5(3) . .
O21 Nd1 O3W 136.5(3) 6_565 .
O5 Nd1 O3W 72.8(4) . .
O5 Nd1 O3W 72.8(4) 6_565 .
O4W Nd1 O3W 85.2(6) . .
O21 Nd1 O2W 71.7(4) . .
O21 Nd1 O2W 71.7(4) 6_565 .
O5 Nd1 O2W 70.1(4) . .
O5 Nd1 O2W 70.1(4) 6_565 .
O4W Nd1 O2W 145.2(6) . .
O3W Nd1 O2W 129.6(5) . .
O21 Nd1 O1W 139.2(4) . 6_565
O21 Nd1 O1W 70.1(4) 6_565 6_565
O5 Nd1 O1W 66.9(3) . 6_565
O5 Nd1 O1W 135.0(4) 6_565 6_565
O4W Nd1 O1W 64.6(3) . 6_565
O3W Nd1 O1W 66.9(3) . 6_565
O2W Nd1 O1W 123.9(2) . 6_565
O21 Nd1 O1W 70.1(4) . .
O21 Nd1 O1W 139.2(4) 6_565 .
O5 Nd1 O1W 135.0(3) . .
O5 Nd1 O1W 66.9(3) 6_565 .
O4W Nd1 O1W 64.6(3) . .
O3W Nd1 O1W 66.9(3) . .
O2W Nd1 O1W 123.9(2) . .
O1W Nd1 O1W 112.0(5) 6_565 .
O21 Nd1 K1 103.6(3) . .
O21 Nd1 K1 103.6(3) 6_565 .
O5 Nd1 K1 45.2(2) . .
O5 Nd1 K1 45.2(2) 6_565 .
O4W Nd1 K1 171.7(4) . .
O3W Nd1 K1 86.5(4) . .
O2W Nd1 K1 43.1(4) . .
O1W Nd1 K1 111.9(2) 6_565 .
O1W Nd1 K1 111.9(2) . .
O24 Nd2 O24 104.1(5) . 6_565
O24 Nd2 O5W 73.6(4) . .
O24 Nd2 O5W 73.6(4) 6_565 .
O24 Nd2 O6W 144.7(5) . 6_565
O24 Nd2 O6W 79.8(4) 6_565 6_565
O5W Nd2 O6W 138.7(4) . 6_565
O24 Nd2 O6W 79.8(4) . .
O24 Nd2 O6W 144.7(5) 6_565 .
O5W Nd2 O6W 138.7(4) . .
O6W Nd2 O6W 78.0(7) 6_565 .
O24 Nd2 O7W 74.9(4) . .
O24 Nd2 O7W 74.9(4) 6_565 .
O5W Nd2 O7W 127.6(6) . .
O6W Nd2 O7W 72.4(4) 6_565 .
O6W Nd2 O7W 72.4(4) . .
O24 Nd2 O8 79.4(4) . .
O24 Nd2 O8 145.3(4) 6_565 .
O5W Nd2 O8 74.5(4) . .
O6W Nd2 O8 117.4(4) 6_565 .
O6W Nd2 O8 70.0(4) . .
O7W Nd2 O8 137.4(3) . .
O24 Nd2 O8 145.3(4) . 6_565
O24 Nd2 O8 79.4(4) 6_565 6_565
O5W Nd2 O8 74.5(4) . 6_565
O6W Nd2 O8 70.0(4) 6_565 6_565
O6W Nd2 O8 117.4(4) . 6_565
O7W Nd2 O8 137.4(3) . 6_565
O8 Nd2 O8 79.2(5) . 6_565
O7 K1 O7 89.4(4) . 6_565
O7 K1 OW4 135.2(2) . .
O7 K1 OW4 135.2(2) 6_565 .
O7 K1 O2W 111.7(3) . .
O7 K1 O2W 111.7(3) 6_565 .
OW4 K1 O2W 61.6(7) . .
O7 K1 O5 56.2(3) . .
O7 K1 O5 100.8(3) 6_565 .
OW4 K1 O5 107.5(5) . .
O2W K1 O5 56.3(3) . .
O7 K1 O5 100.8(3) . 6_565
O7 K1 O5 56.2(3) 6_565 6_565
OW4 K1 O5 107.5(5) . 6_565
O2W K1 O5 56.3(3) . 6_565
O5 K1 O5 63.9(4) . 6_565
O7 K1 OW3 133.1(5) . .
O7 K1 OW3 74.8(4) 6_565 .
OW4 K1 OW3 70.7(5) . .
O2W K1 OW3 115.2(4) . .
O5 K1 OW3 168.7(4) . .
O5 K1 OW3 105.6(4) 6_565 .
O7 K1 OW3 74.8(4) . 6_565
O7 K1 OW3 133.1(5) 6_565 6_565
OW4 K1 OW3 70.7(5) . 6_565
O2W K1 OW3 115.2(4) . 6_565
O5 K1 OW3 105.6(4) . 6_565
O5 K1 OW3 168.7(4) 6_565 6_565
OW3 K1 OW3 84.5(6) . 6_565
O7 K1 O5W 88.0(3) . .
O7 K1 O5W 88.0(3) 6_565 .
OW4 K1 O5W 89.8(7) . .
O2W K1 O5W 151.5(5) . .
O5 K1 O5W 142.6(3) . .
O5 K1 O5W 142.6(3) 6_565 .
OW3 K1 O5W 48.5(4) . .
OW3 K1 O5W 48.5(4) 6_565 .
O7 K1 Ti2 100.8(3) . 6_565
O7 K1 Ti2 29.9(2) 6_565 6_565
OW4 K1 Ti2 120.0(3) . 6_565
O2W K1 Ti2 81.8(3) . 6_565
O5 K1 Ti2 84.5(2) . 6_565
O5 K1 Ti2 27.08(18) 6_565 6_565
OW3 K1 Ti2 87.0(3) . 6_565
OW3 K1 Ti2 163.0(4) 6_565 6_565
O5W K1 Ti2 115.7(2) . 6_565
O7 K1 W6 100.8(3) . 6_565
O7 K1 W6 29.9(2) 6_565 6_565
OW4 K1 W6 120.0(3) . 6_565
O2W K1 W6 81.8(3) . 6_565
O5 K1 W6 84.5(2) . 6_565
O5 K1 W6 27.08(18) 6_565 6_565
OW3 K1 W6 87.0(3) . 6_565
OW3 K1 W6 163.0(4) 6_565 6_565
O5W K1 W6 115.7(2) . 6_565
O7 K1 W6 29.9(2) . .
O7 K1 W6 100.8(3) 6_565 .
OW4 K1 W6 120.0(3) . .
O2W K1 W6 81.8(3) . .
O5 K1 W6 27.08(18) . .
O5 K1 W6 84.5(2) 6_565 .
OW3 K1 W6 163.0(4) . .
OW3 K1 W6 87.0(3) 6_565 .
O5W K1 W6 115.7(2) . .
W6 K1 W6 97.22(16) 6_565 .
O1 P1 O1 110.6(8) 2_655 .
O1 P1 O2 109.3(5) 2_655 2_655
O1 P1 O2 109.9(5) . 2_655
O1 P1 O2 109.9(5) 2_655 .
O1 P1 O2 109.3(5) . .
O2 P1 O2 107.8(8) 2_655 .
P1 O1 W6 125.8(6) . .
P1 O1 W4 127.3(5) . .
W6 O1 W4 89.1(3) . .
P1 O1 W5 126.6(6) . .
W4 O1 W5 89.0(3) . .
P1 O2 W2 123.9(5) . .
P1 O2 W3 126.2(6) . .
W2 O2 W3 90.5(3) . .
P1 O2 W1 126.8(6) . .
W2 O2 W1 89.8(3) . .
W3 O2 W1 88.3(3) . .
W2 O4 W5 147.3(6) . .
W6 O5 Nd1 154.3(6) . .
W6 O5 K1 97.2(4) . .
Nd1 O5 K1 100.3(3) . .
W1 O6 W2 127.2(5) . .
W5 O7 K1 129.5(5) . .
W6 O7 K1 103.0(4) . .
W5 O8 Nd2 177.2(6) . .
W1 O13 W4 149.7(6) 2_655 .
W1 O14 W3 150.8(5) 2_655 .
W3 O15 W4 155.3(6) . .
W3 O16 W2 126.1(6) . .
W4 O17 W5 125.8(6) . .
W2 O18 Ti2 147.8(6) . 2_655
W2 O18 W6 147.8(6) . 2_655
W4 O19 W6 121.7(5) . .
W3 O20 W1 124.8(5) . .
C1 O21 Nd1 148.3(12) . .
C7 O24 Nd2 157.4(12) . .
C4 N1 C3 120.8(16) . .
C4 N1 H1A 119.6 . .
C3 N1 H1A 119.6 . .
C10 N2 C9 121.6(16) . .
C10 N2 H2A 119.2 . .
C9 N2 H2A 119.2 . .
O21 C1 O22 126.3(15) . .
O21 C1 C2 116.5(15) . .
O22 C1 C2 117.1(14) . .
C3 C2 C6 115.7(14) . .
C3 C2 C1 120.7(14) . .
C6 C2 C1 123.7(15) . .
N1 C3 C2 122.1(15) . .
N1 C3 H3A 118.9 . .
C2 C3 H3A 118.9 . .
N1 C4 C5 121.7(15) . .
N1 C4 H4A 119.2 . .
C5 C4 H4A 119.2 . .
C6 C5 C4 118.5(16) . .
C6 C5 H5A 120.7 . .
C4 C5 H5A 120.7 . .
C5 C6 C2 120.8(17) . .
C5 C6 H6A 119.6 . .
C2 C6 H6A 119.6 . .
O24 C7 O23 127.7(17) . .
O24 C7 C8 118.4(17) . .
O23 C7 C8 113.7(16) . .
C12 C8 C9 119.8(16) . .
C12 C8 C7 122.9(17) . .
C9 C8 C7 117.2(15) . .
N2 C9 C8 118.5(16) . .
N2 C9 H9A 120.7 . .
C8 C9 H9A 120.7 . .
N2 C10 C11 120.7(17) . .
N2 C10 H10A 119.7 . .
C11 C10 H10A 119.7 . .
C10 C11 C12 117.2(16) . .
C10 C11 H11A 121.4 . .
C12 C11 H11A 121.4 . .
C8 C12 C11 122.2(17) . .
C8 C12 H12A 118.9 . .
C11 C12 H12A 118.9 . .
Nd1 O1W H1WA 120.0 . .
Nd1 O1W H1WB 120.0 . .
H1WA O1W H1WB 120.0 . .
Nd1 O2W K1 101.5(6) . .
Nd1 O3W H3WA 120.0 . .
Nd1 O3W H3WB 120.0 . .
H3WA O3W H3WB 120.0 . .
Nd1 O4W H4WA 120.0 . .
Nd1 O4W H4WB 120.0 . .
H4WA O4W H4WB 120.0 . .
Nd2 O5W K1 123.0(7) . .
Nd2 O6W H6WA 120.1 . .
Nd2 O6W H6WB 119.9 . .
H6WA O6W H6WB 120.0 . .
Nd2 O7W H7WA 120.0 . .
Nd2 O7W H7WB 120.0 . .
H7WA O7W H7WB 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O10 1.707(10) .
W1 O13 1.876(9) 2_655
W1 O6 1.887(11) .
W1 O14 1.898(10) 2_655
W1 O20 1.950(10) .
W1 O2 2.456(9) .
W2 O11 1.701(11) .
W2 O18 1.838(10) .
W2 O4 1.852(10) .
W2 O16 1.955(10) .
W2 O6 1.960(10) .
W2 O2 2.427(10) .
W3 O12 1.731(10) .
W3 O20 1.894(10) .
W3 O15 1.900(10) .
W3 O14 1.902(10) .
W3 O16 1.917(10) .
W3 O2 2.434(10) .
W4 O9 1.707(11) .
W4 O17 1.856(10) .
W4 O19 1.869(10) .
W4 O15 1.913(10) .
W4 O13 1.987(10) .
W4 O1 2.435(10) .
W5 O8 1.714(9) .
W5 O3 1.839(10) .
W5 O7 1.852(10) .
W5 O4 1.976(10) .
W5 O17 1.986(10) .
W5 O1 2.447(10) .
W6 O5 1.699(10) .
W6 O7 1.894(10) .
W6 O3 1.934(11) 2_655
W6 O18 2.004(10) 2_655
W6 O19 2.008(10) .
W6 O1 2.390(10) .
W6 K1 3.703(5) .
Nd1 O21 2.424(11) .
Nd1 O21 2.424(11) 6_565
Nd1 O5 2.458(10) .
Nd1 O5 2.458(10) 6_565
Nd1 O4W 2.446(17) .
Nd1 O3W 2.524(16) .
Nd1 O2W 2.525(17) .
Nd1 O1W 2.618(11) 6_565
Nd1 O1W 2.618(11) .
Nd1 K1 4.272(7) .
Nd2 O24 2.344(12) .
Nd2 O24 2.344(12) 6_565
Nd2 O5W 2.411(19) .
Nd2 O6W 2.445(12) 6_565
Nd2 O6W 2.445(12) .
Nd2 O7W 2.465(18) .
Nd2 O8 2.520(10) .
Nd2 O8 2.520(10) 6_565
K1 O7 2.785(11) .
K1 O7 2.785(11) 6_565
K1 OW4 2.86(3) .
K1 O2W 2.979(19) .
K1 O5 3.083(12) .
K1 O5 3.083(12) 6_565
K1 OW3 3.11(2) .
K1 OW3 3.11(2) 6_565
K1 O5W 3.39(2) .
K1 Ti2 3.703(5) 6_565
K1 W6 3.703(5) 6_565
P1 O1 1.509(10) 2_655
P1 O1 1.509(10) .
P1 O2 1.536(10) 2_655
P1 O2 1.536(10) .
O3 Ti2 1.933(11) 2_655
O3 W6 1.933(11) 2_655
O13 W1 1.876(9) 2_655
O14 W1 1.898(10) 2_655
O18 Ti2 2.004(10) 2_655
O18 W6 2.004(10) 2_655
O21 C1 1.219(18) .
O22 C1 1.22(2) .
O23 C7 1.26(2) .
O24 C7 1.23(2) .
N1 C4 1.30(2) .
N1 C3 1.31(2) .
N1 H1A 0.8600 .
N2 C10 1.32(2) .
N2 C9 1.34(2) .
N2 H2A 0.8600 .
C1 C2 1.51(2) .
C2 C3 1.40(2) .
C2 C6 1.42(2) .
C3 H3A 0.9300 .
C4 C5 1.40(2) .
C4 H4A 0.9300 .
C5 C6 1.33(2) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 C8 1.56(2) .
C8 C12 1.31(2) .
C8 C9 1.36(2) .
C9 H9A 0.9300 .
C10 C11 1.35(2) .
C10 H10A 0.9300 .
C11 C12 1.37(2) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
O1W H1WA 0.8499 .
O1W H1WB 0.8498 .
O3W H3WA 0.8499 .
O3W H3WB 0.8500 .
O4W H4WA 0.9300 .
O4W H4WB 0.9300 .
O6W H6WA 0.8497 .
O6W H6WB 0.8502 .
O7W H7WA 0.8500 .
O7W H7WB 0.8499 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 P1 O1 W6_c -57.8(5) 2_655 .
O2 P1 O1 W6 63.0(8) 2_655 .
O2 P1 O1 W6 -178.9(6) . .
O1 P1 O1 W4 -179.5(8) 2_655 .
O2 P1 O1 W4 -58.8(8) 2_655 .
O2 P1 O1 W4 59.4(8) . .
O1 P1 O1 W5 58.1(5) 2_655 .
O2 P1 O1 W5 178.8(6) 2_655 .
O2 P1 O1 W5 -63.0(8) . .
O1 P1 O2 W2 -61.8(7) 2_655 .
O1 P1 O2 W2 59.8(8) . .
O2 P1 O2 W2 179.2(8) 2_655 .
O1 P1 O2 W3 178.1(6) 2_655 .
O1 P1 O2 W3 -60.4(8) . .
O2 P1 O2 W3 59.0(5) 2_655 .
O1 P1 O2 W1 58.0(8) 2_655 .
O1 P1 O2 W1 179.5(6) . .
O2 P1 O2 W1 -61.1(5) 2_655 .
O8 W5 O3 Ti2 -141.7(12) . 2_655
O7 W5 O3 Ti2 115.0(12) . 2_655
O4 W5 O3 Ti2 -40.4(12) . 2_655
O17 W5 O3 Ti2 26(2) . 2_655
O1 W5 O3 Ti2 41.1(12) . 2_655
O8 W5 O3 W6 -141.7(12) . 2_655
O7 W5 O3 W6 115.0(12) . 2_655
O4 W5 O3 W6 -40.4(12) . 2_655
O17 W5 O3 W6 26(2) . 2_655
O1 W5 O3 W6 41.1(12) . 2_655
O11 W2 O4 W5 -125.9(10) . .
O18 W2 O4 W5 -22.4(11) . .
O16 W2 O4 W5 134.7(11) . .
O6 W2 O4 W5 66.9(16) . .
O2 W2 O4 W5 63.1(10) . .
O7 W6 O5 Nd1 -119.2(12) . .
O3 W6 O5 Nd1 -21.2(13) 2_655 .
O18 W6 O5 Nd1 64.2(13) 2_655 .
O19 W6 O5 Nd1 151.1(12) . .
K1 W6 O5 Nd1 -132.7(14) . .
O7 W6 O5 K1 13.5(4) . .
O3 W6 O5 K1 111.5(4) 2_655 .
O18 W6 O5 K1 -163.0(4) 2_655 .
O19 W6 O5 K1 -76.2(4) . .
O10 W1 O6 W2 173.7(6) . .
O13 W1 O6 W2 -83.7(7) 2_655 .
O14 W1 O6 W2 0.0(14) 2_655 .
O20 W1 O6 W2 73.3(7) . .
O2 W1 O6 W2 0.4(5) . .
O8 W5 O7 W6 174.5(6) . .
O3 W5 O7 W6 -80.9(6) . .
O4 W5 O7 W6 11.6(14) . .
O17 W5 O7 W6 75.5(6) . .
O1 W5 O7 W6 3.8(5) . .
O8 W5 O7 K1 19.0(7) . .
O3 W5 O7 K1 123.6(6) . .
O4 W5 O7 K1 -143.9(8) . .
O17 W5 O7 K1 -80.1(6) . .
O1 W5 O7 K1 -151.8(6) . .
O5 W6 O7 W5 -176.1(6) . .
O3 W6 O7 W5 82.2(6) 2_655 .
O18 W6 O7 W5 -5.9(17) 2_655 .
O19 W6 O7 W5 -77.3(6) . .
O1 W6 O7 W5 -3.8(5) . .
K1 W6 O7 W5 -160.8(8) . .
O5 W6 O7 K1 -15.3(5) . .
O3 W6 O7 K1 -116.9(4) 2_655 .
O18 W6 O7 K1 154.9(11) 2_655 .
O19 W6 O7 K1 83.5(4) . .
O1 W6 O7 K1 157.0(4) . .
O12 W3 O15 W4 131.2(14) . .
O20 W3 O15 W4 -48(2) . .
O14 W3 O15 W4 28.8(14) . .
O16 W3 O15 W4 -128.3(14) . .
O2 W3 O15 W4 -56.2(13) . .
O9 W4 O17 W5 170.6(6) . .
O19 W4 O17 W5 66.9(7) . .
O15 W4 O17 W5 -88.4(7) . .
O13 W4 O17 W5 -17.1(15) . .
O1 W4 O17 W5 -6.6(5) . .
O11 W2 O18 Ti2 135.7(11) . 2_655
O4 W2 O18 Ti2 31.5(11) . 2_655
O16 W2 O18 Ti2 -51.1(18) . 2_655
O6 W2 O18 Ti2 -124.4(11) . 2_655
O2 W2 O18 Ti2 -53.1(11) . 2_655
O11 W2 O18 W6 135.7(11) . 2_655
O4 W2 O18 W6 31.5(11) . 2_655
O16 W2 O18 W6 -51.1(18) . 2_655
O6 W2 O18 W6 -124.4(11) . 2_655
O2 W2 O18 W6 -53.1(11) . 2_655
O9 W4 O19 W6 -166.3(6) . .
O17 W4 O19 W6 -63.8(6) . .
O15 W4 O19 W6 30.0(13) . .
O13 W4 O19 W6 93.7(6) . .
O1 W4 O19 W6 8.6(5) . .
O12 W3 O20 W1 169.0(7) . .
O15 W3 O20 W1 -11.4(15) . .
O14 W3 O20 W1 -87.6(6) . .
O16 W3 O20 W1 68.4(7) . .
O2 W3 O20 W1 -3.3(6) . .
Nd1 O21 C1 O22 -83(3) . .
Nd1 O21 C1 C2 101(2) . .
O21 C1 C2 C3 -7(2) . .
O22 C1 C2 C3 176.6(17) . .
O21 C1 C2 C6 174.1(16) . .
O22 C1 C2 C6 -2(3) . .
C4 N1 C3 C2 -6(3) . .
C6 C2 C3 N1 6(3) . .
C1 C2 C3 N1 -173.2(17) . .
C3 N1 C4 C5 6(3) . .
N1 C4 C5 C6 -5(3) . .
C4 C5 C6 C2 5(3) . .
C3 C2 C6 C5 -5(3) . .
C1 C2 C6 C5 173.7(17) . .
Nd2 O24 C7 O23 63(4) . .
Nd2 O24 C7 C8 -123(3) . .
O24 C7 C8 C12 -180.0(18) . .
O23 C7 C8 C12 -5(3) . .
O24 C7 C8 C9 4(3) . .
O23 C7 C8 C9 179.2(16) . .
C10 N2 C9 C8 2(2) . .
C12 C8 C9 N2 -3(3) . .
C7 C8 C9 N2 173.0(15) . .
C9 N2 C10 C11 0(3) . .
N2 C10 C11 C12 -1(3) . .
C9 C8 C12 C11 2(3) . .
C7 C8 C12 C11 -173.3(16) . .
C10 C11 C12 C8 0(3) . .
