#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:37:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179730 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/26/7002665.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_7002665
loop_
_publ_author_name
'Zhang, Xiao'
'Yi, Zhihui'
'Zhao, Liyan'
'Chen, Qian'
'Gu, Xianmo'
'Xu, Jiqing'
'Wang, Xiaolin'
'Yang, Chao'
'Xu, Xianzhu'
'Xia, Wujiong'
_publ_section_title
;
 Steric hindrance-dependent rational design and synthesis of three new
 Keggin-based supramolecular networks
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9198
_journal_paper_doi               10.1039/b906313g
_journal_year                    2009
_chemical_formula_sum            'C18 H70 N12 Ni3 O45 P W12'
_chemical_formula_weight         3588.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   CONSTR
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.1790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6446(9)
_cell_length_b                   22.0180(15)
_cell_length_c                   22.6442(16)
_cell_measurement_reflns_used    3869
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.54
_cell_volume                     6299.8(8)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_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 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       'ω 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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16617
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    22.811
_exptl_absorpt_correction_T_max  0.4623
_exptl_absorpt_correction_T_min  0.2626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6436
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.880
_refine_diff_density_min         -2.133
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                4330
_reflns_number_total             5561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906313g.txt
_cod_data_source_block           yi
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to
'constr' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002665
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
N2 N 0.5799(11) 0.3766(6) 0.6156(5) 0.033(3) Uani 1 1 d . . .
W1 W 0.49238(5) 0.21518(3) 0.36209(3) 0.02584(17) Uani 1 1 d . . .
W2 W 0.69325(5) 0.21256(3) 0.24811(3) 0.02652(18) Uani 1 1 d . . .
W3 W 0.70100(5) 0.33327(3) 0.36145(3) 0.02746(18) Uani 1 1 d . . .
W4 W 0.69709(5) 0.32263(3) 0.14458(3) 0.02647(18) Uani 1 1 d . . .
W5 W 0.69627(6) 0.44258(3) 0.25784(3) 0.0342(2) Uani 1 1 d . . .
W6 W 0.48715(6) 0.43973(3) 0.13920(3) 0.03093(19) Uani 1 1 d . . .
P1 P 0.5000 0.3279(2) 0.2500 0.0178(12) Uani 1 2 d SD . .
Ni1 Ni 1.0000 0.48714(12) 0.2500 0.0339(7) Uani 1 2 d S . .
Ni2 Ni 0.47534(17) 0.32122(8) 0.57075(8) 0.0252(5) Uani 1 1 d . . .
O1 O 0.4308(7) 0.2868(4) 0.2888(3) 0.016(2) Uani 1 1 d D . .
O2 O 0.5881(8) 0.1919(4) 0.3017(4) 0.022(2) Uani 1 1 d . . .
O3 O 0.5864(8) 0.3770(4) 0.1210(4) 0.020(2) Uani 1 1 d . . .
O4 O 0.6181(8) 0.2593(4) 0.1010(4) 0.024(2) Uani 1 1 d . . .
O5 O 0.7669(7) 0.2587(4) 0.1887(4) 0.021(2) Uani 1 1 d . . .
O6 O 0.5911(8) 0.2777(4) 0.3821(4) 0.021(2) Uani 1 1 d . . .
O7 O 0.6186(8) 0.4821(4) 0.3185(4) 0.027(2) Uani 1 1 d . . .
O8 O 0.7364(8) 0.3800(4) 0.2048(4) 0.025(2) Uani 1 1 d . . .
O9 O 0.5707(7) 0.3678(3) 0.2894(3) 0.015(2) Uani 1 1 d D . .
O10 O 0.3765(8) 0.3947(4) 0.0981(4) 0.022(2) Uani 1 1 d . . .
O11 O 0.7880(9) 0.3356(4) 0.0918(4) 0.032(3) Uani 1 1 d . . .
O12 O 0.7329(8) 0.2765(4) 0.3022(4) 0.023(2) Uani 1 1 d . . .
O13 O 0.7925(9) 0.4950(5) 0.2452(4) 0.040(3) Uani 1 1 d . . .
O14 O 0.6164(7) 0.1728(3) 0.1853(4) 0.017(2) Uani 1 1 d . . .
O15 O 0.5184(8) 0.1622(4) 0.4162(4) 0.026(2) Uani 1 1 d . . .
O16 O 0.7711(8) 0.3961(4) 0.3198(4) 0.023(2) Uani 1 1 d . . .
O17 O 0.7897(9) 0.1596(4) 0.2636(4) 0.035(3) Uani 1 1 d . . .
O18 O 0.5888(8) 0.4621(4) 0.2009(4) 0.025(2) Uani 1 1 d . . .
O19 O 0.7983(9) 0.3165(4) 0.4136(4) 0.031(3) Uani 1 1 d . . .
O20 O 0.5115(10) 0.4916(4) 0.0854(4) 0.037(3) Uani 1 1 d . . .
C1 C 0.7605(15) 0.4200(8) 0.6097(9) 0.054(5) Uani 1 1 d U . .
H1A H 0.8144 0.3944 0.6272 0.080 Uiso 1 1 calc R . .
H1B H 0.7320 0.4456 0.6395 0.080 Uiso 1 1 calc R . .
H1C H 0.7906 0.4449 0.5798 0.080 Uiso 1 1 calc R . .
C2 C 0.6940(15) 0.3380(9) 0.5450(9) 0.063(7) Uani 1 1 d . . .
H2A H 0.7423 0.3097 0.5648 0.076 Uiso 1 1 calc R . .
H2B H 0.7311 0.3557 0.5125 0.076 Uiso 1 1 calc R . .
C3 C 0.6743(19) 0.3816(11) 0.5824(11) 0.086(7) Uani 1 1 d U . .
H3 H 0.6474 0.4114 0.5534 0.103 Uiso 1 1 calc R . .
C4 C 0.3027(16) 0.4025(9) 0.5330(8) 0.051(5) Uani 1 1 d . . .
H4 H 0.2612 0.3693 0.5148 0.062 Uiso 1 1 calc R . .
C5 C 0.2927(17) 0.3961(8) 0.5977(9) 0.058(6) Uani 1 1 d . . .
H5A H 0.3210 0.4322 0.6171 0.069 Uiso 1 1 calc R . .
H5B H 0.2184 0.3931 0.6064 0.069 Uiso 1 1 calc R . .
C6 C 0.2570(15) 0.4610(7) 0.5071(8) 0.049(5) Uani 1 1 d . . .
H6A H 0.3015 0.4945 0.5190 0.073 Uiso 1 1 calc R . .
H6B H 0.1872 0.4673 0.5213 0.073 Uiso 1 1 calc R . .
H6C H 0.2534 0.4583 0.4648 0.073 Uiso 1 1 calc R . .
C7 C 1.0219(15) 0.4595(8) 0.3724(8) 0.044(5) Uani 1 1 d . . .
H7 H 1.0984 0.4657 0.3779 0.053 Uiso 1 1 calc R . .
C8 C 0.9717(16) 0.5182(8) 0.3669(8) 0.053(5) Uani 1 1 d . . .
H8A H 0.8957 0.5133 0.3687 0.063 Uiso 1 1 calc R . .
H8B H 0.9953 0.5437 0.3998 0.063 Uiso 1 1 calc R . .
C9 C 0.9845(16) 0.4235(9) 0.4235(8) 0.057(6) Uani 1 1 d . . .
H9A H 0.9897 0.4478 0.4587 0.086 Uiso 1 1 calc R . .
H9B H 1.0277 0.3879 0.4287 0.086 Uiso 1 1 calc R . .
H9C H 0.9122 0.4116 0.4160 0.086 Uiso 1 1 calc R . .
N1 N 0.6055(11) 0.3032(6) 0.5200(6) 0.034(3) Uani 1 1 d . . .
H1D H 0.6206 0.2633 0.5209 0.041 Uiso 1 1 calc R . .
H1E H 0.5918 0.3142 0.4822 0.041 Uiso 1 1 calc R . .
H2C H 0.5512 0.4134 0.6202 0.041 Uiso 1 1 d R . .
H2D H 0.5961 0.3609 0.6514 0.041 Uiso 1 1 d R . .
N3 N 0.3484(11) 0.3426(5) 0.6217(6) 0.035(4) Uani 1 1 d . . .
H3A H 0.3036 0.3109 0.6223 0.042 Uiso 1 1 calc R . .
H3B H 0.3716 0.3502 0.6590 0.042 Uiso 1 1 calc R . .
N4 N 0.4126(10) 0.3922(5) 0.5170(5) 0.024(3) Uani 1 1 d . . .
H4A H 0.4508 0.4263 0.5229 0.029 Uiso 1 1 calc R . .
H4B H 0.4150 0.3819 0.4786 0.029 Uiso 1 1 calc R . .
N5 N 1.0014(12) 0.4280(5) 0.3148(6) 0.042(4) Uani 1 1 d . . .
H5C H 0.9387 0.4087 0.3151 0.051 Uiso 1 1 calc R . .
H5D H 1.0521 0.4001 0.3093 0.051 Uiso 1 1 calc R . .
N6 N 0.9958(11) 0.5479(6) 0.3122(6) 0.043(4) Uani 1 1 d . . .
H6D H 1.0588 0.5668 0.3161 0.052 Uiso 1 1 calc R . .
H6E H 0.9461 0.5759 0.3029 0.052 Uiso 1 1 calc R . .
O1W O 0.3805(10) 0.2567(5) 0.5213(4) 0.040(3) Uani 1 1 d . . .
O2W O 0.5133(10) 0.2440(5) 0.6284(5) 0.049(3) Uani 1 1 d . . .
O3W O 0.0000 0.0924(8) 0.2500 0.072(7) Uani 1 2 d S . .
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'
Ni Ni 0.3393 1.1124 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C3 N2 Ni2 108.7(11) . . ?
C3 N2 H2C 109.7 . . ?
Ni2 N2 H2C 110.0 . . ?
C3 N2 H2D 109.6 . . ?
Ni2 N2 H2D 110.0 . . ?
H2C N2 H2D 108.8 . . ?
O15 W1 O6 102.5(4) . . ?
O15 W1 O4 99.0(4) . 2_655 ?
O6 W1 O4 90.7(4) . 2_655 ?
O15 W1 O2 102.6(4) . . ?
O6 W1 O2 86.4(4) . . ?
O4 W1 O2 158.4(4) 2_655 . ?
O15 W1 O14 100.4(4) . 2_655 ?
O6 W1 O14 157.0(4) . 2_655 ?
O4 W1 O14 88.4(4) 2_655 2_655 ?
O2 W1 O14 86.1(4) . 2_655 ?
O15 W1 O1 172.1(4) . . ?
O6 W1 O1 83.2(3) . . ?
O4 W1 O1 75.3(3) 2_655 . ?
O2 W1 O1 83.1(3) . . ?
O14 W1 O1 74.3(3) 2_655 . ?
O17 W2 O2 102.6(4) . . ?
O17 W2 O14 100.3(4) . . ?
O2 W2 O14 91.0(4) . . ?
O17 W2 O12 101.6(5) . . ?
O2 W2 O12 86.5(4) . . ?
O14 W2 O12 158.0(4) . . ?
O17 W2 O5 98.1(4) . . ?
O2 W2 O5 159.1(4) . . ?
O14 W2 O5 88.2(4) . . ?
O12 W2 O5 86.4(4) . . ?
O17 W2 O1 171.0(4) . 2_655 ?
O2 W2 O1 85.5(3) . 2_655 ?
O14 W2 O1 75.2(3) . 2_655 ?
O12 W2 O1 82.8(3) . 2_655 ?
O5 W2 O1 74.2(3) . 2_655 ?
O19 W3 O12 100.3(4) . . ?
O19 W3 O16 99.3(4) . . ?
O12 W3 O16 90.8(4) . . ?
O19 W3 O6 101.7(4) . . ?
O12 W3 O6 85.8(4) . . ?
O16 W3 O6 159.0(4) . . ?
O19 W3 O10 100.9(4) . 2_655 ?
O12 W3 O10 158.5(4) . 2_655 ?
O16 W3 O10 88.9(4) . 2_655 ?
O6 W3 O10 86.9(4) . 2_655 ?
O19 W3 O9 173.9(4) . . ?
O12 W3 O9 83.5(4) . . ?
O16 W3 O9 75.7(3) . . ?
O6 W3 O9 83.3(3) . . ?
O10 W3 O9 75.6(3) 2_655 . ?
O11 W4 O3 101.9(4) . . ?
O11 W4 O8 102.9(4) . . ?
O3 W4 O8 87.3(4) . . ?
O11 W4 O5 100.2(4) . . ?
O3 W4 O5 157.7(4) . . ?
O8 W4 O5 90.6(4) . . ?
O11 W4 O4 96.3(4) . . ?
O3 W4 O4 87.2(4) . . ?
O8 W4 O4 160.7(4) . . ?
O5 W4 O4 87.5(4) . . ?
O11 W4 O1 169.9(4) . 2_655 ?
O3 W4 O1 82.9(3) . 2_655 ?
O8 W4 O1 86.1(3) . 2_655 ?
O5 W4 O1 74.8(3) . 2_655 ?
O4 W4 O1 74.8(3) . 2_655 ?
O13 W5 O18 103.3(5) . . ?
O13 W5 O8 100.0(4) . . ?
O18 W5 O8 86.3(4) . . ?
O13 W5 O7 101.6(4) . . ?
O18 W5 O7 90.6(4) . . ?
O8 W5 O7 158.3(4) . . ?
O13 W5 O16 98.3(5) . . ?
O18 W5 O16 158.1(4) . . ?
O8 W5 O16 86.6(4) . . ?
O7 W5 O16 88.3(4) . . ?
O13 W5 O9 172.1(4) . . ?
O18 W5 O9 83.9(3) . . ?
O8 W5 O9 83.5(3) . . ?
O7 W5 O9 74.8(3) . . ?
O16 W5 O9 74.7(3) . . ?
O20 W6 O7 100.3(4) . 2_655 ?
O20 W6 O3 101.0(4) . . ?
O7 W6 O3 158.6(4) 2_655 . ?
O20 W6 O18 102.3(5) . . ?
O7 W6 O18 88.4(4) 2_655 . ?
O3 W6 O18 85.2(4) . . ?
O20 W6 O10 98.5(5) . . ?
O7 W6 O10 89.1(4) 2_655 . ?
O3 W6 O10 89.7(4) . . ?
O18 W6 O10 159.2(4) . . ?
O20 W6 O9 172.5(5) . 2_655 ?
O7 W6 O9 75.4(3) 2_655 2_655 ?
O3 W6 O9 83.6(3) . 2_655 ?
O18 W6 O9 83.8(3) . 2_655 ?
O10 W6 O9 75.6(3) . 2_655 ?
O9 P1 O9 109.3(7) . 2_655 ?
O9 P1 O1 109.6(4) . . ?
O9 P1 O1 109.7(5) 2_655 . ?
O9 P1 O1 109.7(5) . 2_655 ?
O9 P1 O1 109.6(4) 2_655 2_655 ?
O1 P1 O1 108.8(6) . 2_655 ?
N6 Ni1 N6 93.0(8) . 2_755 ?
N6 Ni1 N5 85.1(5) . . ?
N6 Ni1 N5 177.2(6) 2_755 . ?
N6 Ni1 N5 177.2(6) . 2_755 ?
N6 Ni1 N5 85.1(5) 2_755 2_755 ?
N5 Ni1 N5 96.8(7) . 2_755 ?
N6 Ni1 O13 86.0(5) . . ?
N6 Ni1 O13 88.8(5) 2_755 . ?
N5 Ni1 O13 93.2(5) . . ?
N5 Ni1 O13 91.8(5) 2_755 . ?
N2 Ni2 N3 95.0(5) . . ?
N2 Ni2 N1 83.0(5) . . ?
N3 Ni2 N1 177.7(5) . . ?
N2 Ni2 N4 93.8(5) . . ?
N3 Ni2 N4 82.5(5) . . ?
N1 Ni2 N4 96.3(5) . . ?
N2 Ni2 O1W 173.5(5) . . ?
N3 Ni2 O1W 90.7(5) . . ?
N1 Ni2 O1W 91.4(5) . . ?
N4 Ni2 O1W 89.9(5) . . ?
N2 Ni2 O2W 92.5(5) . . ?
N3 Ni2 O2W 90.1(5) . . ?
N1 Ni2 O2W 91.2(5) . . ?
N4 Ni2 O2W 170.7(5) . . ?
O1W Ni2 O2W 84.4(4) . . ?
P1 O1 W4 125.0(4) . 2_655 ?
P1 O1 W2 125.1(4) . 2_655 ?
W4 O1 W2 89.8(3) 2_655 2_655 ?
P1 O1 W1 126.8(5) . . ?
W4 O1 W1 89.5(2) 2_655 . ?
W2 O1 W1 89.1(3) 2_655 . ?
W2 O2 W1 150.1(5) . . ?
W4 O3 W6 150.6(5) . . ?
W1 O4 W4 120.4(4) 2_655 . ?
W4 O5 W2 121.2(5) . . ?
W1 O6 W3 151.3(5) . . ?
W6 O7 W5 121.4(4) 2_655 . ?
W5 O8 W4 149.1(6) . . ?
P1 O9 W6 126.2(5) . 2_655 ?
P1 O9 W3 126.1(5) . . ?
W6 O9 W3 88.3(3) 2_655 . ?
P1 O9 W5 126.9(4) . . ?
W6 O9 W5 88.3(3) 2_655 . ?
W3 O9 W5 88.6(3) . . ?
W3 O10 W6 120.4(5) 2_655 . ?
W3 O12 W2 151.7(5) . . ?
W5 O13 Ni1 131.7(6) . . ?
W2 O14 W1 121.4(4) . 2_655 ?
W3 O16 W5 120.9(5) . . ?
W5 O18 W6 151.7(5) . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 118.4(18) . . ?
C3 C2 H2A 107.7 . . ?
N1 C2 H2A 107.7 . . ?
C3 C2 H2B 107.7 . . ?
N1 C2 H2B 107.7 . . ?
H2A C2 H2B 107.1 . . ?
C2 C3 N2 117.5(19) . . ?
C2 C3 C1 122(2) . . ?
N2 C3 C1 115.8(17) . . ?
C2 C3 H3 97.3 . . ?
N2 C3 H3 97.3 . . ?
C1 C3 H3 97.3 . . ?
N4 C4 C5 110.2(16) . . ?
N4 C4 C6 112.7(14) . . ?
C5 C4 C6 114.5(16) . . ?
N4 C4 H4 106.3 . . ?
C5 C4 H4 106.3 . . ?
C6 C4 H4 106.3 . . ?
N3 C5 C4 112.7(15) . . ?
N3 C5 H5A 109.1 . . ?
C4 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N5 106.3(15) . . ?
C8 C7 C9 113.0(16) . . ?
N5 C7 C9 112.5(14) . . ?
C8 C7 H7 108.3 . . ?
N5 C7 H7 108.3 . . ?
C9 C7 H7 108.3 . . ?
N6 C8 C7 111.9(14) . . ?
N6 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
N6 C8 H8B 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 N1 Ni2 107.3(10) . . ?
C2 N1 H1D 110.2 . . ?
Ni2 N1 H1D 110.2 . . ?
C2 N1 H1E 110.2 . . ?
Ni2 N1 H1E 110.2 . . ?
H1D N1 H1E 108.5 . . ?
C5 N3 Ni2 110.4(10) . . ?
C5 N3 H3A 109.6 . . ?
Ni2 N3 H3A 109.6 . . ?
C5 N3 H3B 109.6 . . ?
Ni2 N3 H3B 109.6 . . ?
H3A N3 H3B 108.1 . . ?
C4 N4 Ni2 108.1(9) . . ?
C4 N4 H4A 110.1 . . ?
Ni2 N4 H4A 110.1 . . ?
C4 N4 H4B 110.1 . . ?
Ni2 N4 H4B 110.1 . . ?
H4A N4 H4B 108.4 . . ?
C7 N5 Ni1 110.0(9) . . ?
C7 N5 H5C 109.7 . . ?
Ni1 N5 H5C 109.7 . . ?
C7 N5 H5D 109.7 . . ?
Ni1 N5 H5D 109.7 . . ?
H5C N5 H5D 108.2 . . ?
C8 N6 Ni1 108.8(10) . . ?
C8 N6 H6D 109.9 . . ?
Ni1 N6 H6D 109.9 . . ?
C8 N6 H6E 109.9 . . ?
Ni1 N6 H6E 109.9 . . ?
H6D N6 H6E 108.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C3 1.44(2) . ?
N2 Ni2 2.040(14) . ?
N2 H2C 0.8967 . ?
N2 H2D 0.8976 . ?
W1 O15 1.716(9) . ?
W1 O6 1.901(9) . ?
W1 O4 1.919(9) 2_655 ?
W1 O2 1.931(9) . ?
W1 O14 1.950(9) 2_655 ?
W1 O1 2.397(8) . ?
W2 O17 1.714(10) . ?
W2 O2 1.888(9) . ?
W2 O14 1.904(9) . ?
W2 O12 1.920(9) . ?
W2 O5 1.951(8) . ?
W2 O1 2.394(9) 2_655 ?
W3 O19 1.713(11) . ?
W3 O12 1.889(9) . ?
W3 O16 1.912(9) . ?
W3 O6 1.922(9) . ?
W3 O10 1.923(9) 2_655 ?
W3 O9 2.398(8) . ?
W4 O11 1.714(9) . ?
W4 O3 1.902(9) . ?
W4 O8 1.911(9) . ?
W4 O5 1.921(9) . ?
W4 O4 1.961(9) . ?
W4 O1 2.387(8) 2_655 ?
W5 O13 1.709(10) . ?
W5 O18 1.887(10) . ?
W5 O8 1.909(9) . ?
W5 O7 1.927(9) . ?
W5 O16 1.951(9) . ?
W5 O9 2.414(8) . ?
W6 O20 1.705(9) . ?
W6 O7 1.916(9) 2_655 ?
W6 O3 1.922(9) . ?
W6 O18 1.926(10) . ?
W6 O10 1.925(10) . ?
W6 O9 2.397(8) 2_655 ?
P1 O9 1.519(8) . ?
P1 O9 1.519(8) 2_655 ?
P1 O1 1.555(7) . ?
P1 O1 1.555(7) 2_655 ?
Ni1 N6 1.945(13) . ?
Ni1 N6 1.945(13) 2_755 ?
Ni1 N5 1.960(13) . ?
Ni1 N5 1.961(13) 2_755 ?
Ni1 O13 2.627(12) . ?
Ni2 N3 2.066(12) . ?
Ni2 N1 2.081(12) . ?
Ni2 N4 2.117(11) . ?
Ni2 O1W 2.146(11) . ?
Ni2 O2W 2.186(11) . ?
O1 W4 2.387(8) 2_655 ?
O1 W2 2.394(9) 2_655 ?
O4 W1 1.919(9) 2_655 ?
O7 W6 1.916(9) 2_655 ?
O9 W6 2.397(8) 2_655 ?
O10 W3 1.923(9) 2_655 ?
O14 W1 1.950(9) 2_655 ?
C1 C3 1.49(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.31(2) . ?
C2 N1 1.45(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3 0.9800 . ?
C4 N4 1.47(2) . ?
C4 C5 1.48(2) . ?
C4 C6 1.52(2) . ?
C4 H4 0.9800 . ?
C5 N3 1.46(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.44(2) . ?
C7 N5 1.49(2) . ?
C7 C9 1.50(2) . ?
C7 H7 0.9800 . ?
C8 N6 1.44(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 H5C 0.9000 . ?
N5 H5D 0.9000 . ?
N6 H6D 0.9000 . ?
N6 H6E 0.9000 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 Ni2 N3 -168.1(14) . . . . ?
C3 N2 Ni2 N1 10.7(14) . . . . ?
C3 N2 Ni2 N4 -85.2(14) . . . . ?
C3 N2 Ni2 O1W 40(4) . . . . ?
C3 N2 Ni2 O2W 101.6(14) . . . . ?
O9 P1 O1 W4 62.4(7) . . . 2_655 ?
O9 P1 O1 W4 -57.7(7) 2_655 . . 2_655 ?
O1 P1 O1 W4 -177.6(7) 2_655 . . 2_655 ?
O9 P1 O1 W2 -178.5(5) . . . 2_655 ?
O9 P1 O1 W2 61.5(7) 2_655 . . 2_655 ?
O1 P1 O1 W2 -58.5(4) 2_655 . . 2_655 ?
O9 P1 O1 W1 -58.3(7) . . . . ?
O9 P1 O1 W1 -178.4(5) 2_655 . . . ?
O1 P1 O1 W1 61.7(4) 2_655 . . . ?
O15 W1 O1 P1 178(2) . . . . ?
O6 W1 O1 P1 41.6(6) . . . . ?
O4 W1 O1 P1 134.1(6) 2_655 . . . ?
O2 W1 O1 P1 -45.6(6) . . . . ?
O14 W1 O1 P1 -133.4(6) 2_655 . . . ?
O15 W1 O1 W4 43(3) . . . 2_655 ?
O6 W1 O1 W4 -93.7(3) . . . 2_655 ?
O4 W1 O1 W4 -1.1(3) 2_655 . . 2_655 ?
O2 W1 O1 W4 179.2(4) . . . 2_655 ?
O14 W1 O1 W4 91.3(3) 2_655 . . 2_655 ?
O15 W1 O1 W2 -47(3) . . . 2_655 ?
O6 W1 O1 W2 176.6(3) . . . 2_655 ?
O4 W1 O1 W2 -90.9(4) 2_655 . . 2_655 ?
O2 W1 O1 W2 89.4(4) . . . 2_655 ?
O14 W1 O1 W2 1.6(3) 2_655 . . 2_655 ?
O17 W2 O2 W1 129.2(11) . . . . ?
O14 W2 O2 W1 -130.0(11) . . . . ?
O12 W2 O2 W1 28.0(11) . . . . ?
O5 W2 O2 W1 -43(2) . . . . ?
O1 W2 O2 W1 -55.0(11) 2_655 . . . ?
O15 W1 O2 W2 -130.1(11) . . . . ?
O6 W1 O2 W2 -28.1(11) . . . . ?
O4 W1 O2 W2 54.6(19) 2_655 . . . ?
O14 W1 O2 W2 130.1(11) 2_655 . . . ?
O1 W1 O2 W2 55.5(11) . . . . ?
O11 W4 O3 W6 -130.4(11) . . . . ?
O8 W4 O3 W6 -27.7(11) . . . . ?
O5 W4 O3 W6 57.3(17) . . . . ?
O4 W4 O3 W6 133.7(11) . . . . ?
O1 W4 O3 W6 58.6(10) 2_655 . . . ?
O20 W6 O3 W4 129.1(11) . . . . ?
O7 W6 O3 W4 -45.7(19) 2_655 . . . ?
O18 W6 O3 W4 27.5(11) . . . . ?
O10 W6 O3 W4 -132.3(11) . . . . ?
O9 W6 O3 W4 -56.8(10) 2_655 . . . ?
O11 W4 O4 W1 173.4(6) . . . 2_655 ?
O3 W4 O4 W1 -85.0(6) . . . 2_655 ?
O8 W4 O4 W1 -11.4(16) . . . 2_655 ?
O5 W4 O4 W1 73.3(6) . . . 2_655 ?
O1 W4 O4 W1 -1.6(5) 2_655 . . 2_655 ?
O11 W4 O5 W2 -169.1(6) . . . . ?
O3 W4 O5 W2 3.2(14) . . . . ?
O8 W4 O5 W2 87.6(6) . . . . ?
O4 W4 O5 W2 -73.1(5) . . . . ?
O1 W4 O5 W2 1.9(5) 2_655 . . . ?
O17 W2 O5 W4 173.4(6) . . . . ?
O2 W2 O5 W4 -14.8(15) . . . . ?
O14 W2 O5 W4 73.2(6) . . . . ?
O12 W2 O5 W4 -85.4(6) . . . . ?
O1 W2 O5 W4 -1.9(5) 2_655 . . . ?
O15 W1 O6 W3 129.2(11) . . . . ?
O4 W1 O6 W3 -131.5(11) 2_655 . . . ?
O2 W1 O6 W3 27.1(11) . . . . ?
O14 W1 O6 W3 -43.9(17) 2_655 . . . ?
O1 W1 O6 W3 -56.4(11) . . . . ?
O19 W3 O6 W1 -126.3(11) . . . . ?
O12 W3 O6 W1 -26.6(11) . . . . ?
O16 W3 O6 W1 54.5(17) . . . . ?
O10 W3 O6 W1 133.2(11) 2_655 . . . ?
O9 W3 O6 W1 57.3(11) . . . . ?
O13 W5 O7 W6 -169.7(6) . . . 2_655 ?
O18 W5 O7 W6 86.5(6) . . . 2_655 ?
O8 W5 O7 W6 4.9(16) . . . 2_655 ?
O16 W5 O7 W6 -71.5(6) . . . 2_655 ?
O9 W5 O7 W6 3.1(5) . . . 2_655 ?
O13 W5 O8 W4 -133.0(10) . . . . ?
O18 W5 O8 W4 -30.1(10) . . . . ?
O7 W5 O8 W4 52.4(17) . . . . ?
O16 W5 O8 W4 129.1(10) . . . . ?
O9 W5 O8 W4 54.1(10) . . . . ?
O11 W4 O8 W5 130.8(10) . . . . ?
O3 W4 O8 W5 29.3(10) . . . . ?
O5 W4 O8 W5 -128.5(10) . . . . ?
O4 W4 O8 W5 -44.3(18) . . . . ?
O1 W4 O8 W5 -53.8(10) 2_655 . . . ?
O9 P1 O9 W6 61.0(4) 2_655 . . 2_655 ?
O1 P1 O9 W6 -59.3(7) . . . 2_655 ?
O1 P1 O9 W6 -178.7(5) 2_655 . . 2_655 ?
O9 P1 O9 W3 -179.8(7) 2_655 . . . ?
O1 P1 O9 W3 59.9(6) . . . . ?
O1 P1 O9 W3 -59.5(6) 2_655 . . . ?
O9 P1 O9 W5 -59.1(4) 2_655 . . . ?
O1 P1 O9 W5 -179.4(5) . . . . ?
O1 P1 O9 W5 61.1(7) 2_655 . . . ?
O19 W3 O9 P1 171(3) . . . . ?
O12 W3 O9 P1 42.0(6) . . . . ?
O16 W3 O9 P1 134.4(6) . . . . ?
O6 W3 O9 P1 -44.5(6) . . . . ?
O10 W3 O9 P1 -133.0(6) 2_655 . . . ?
O19 W3 O9 W6 -54(4) . . . 2_655 ?
O12 W3 O9 W6 177.2(3) . . . 2_655 ?
O16 W3 O9 W6 -90.4(3) . . . 2_655 ?
O6 W3 O9 W6 90.6(3) . . . 2_655 ?
O10 W3 O9 W6 2.1(3) 2_655 . . 2_655 ?
O19 W3 O9 W5 34(4) . . . . ?
O12 W3 O9 W5 -94.5(3) . . . . ?
O16 W3 O9 W5 -2.0(3) . . . . ?
O6 W3 O9 W5 179.0(3) . . . . ?
O10 W3 O9 W5 90.5(3) 2_655 . . . ?
O13 W5 O9 P1 -163(3) . . . . ?
O18 W5 O9 P1 41.3(6) . . . . ?
O8 W5 O9 P1 -45.7(6) . . . . ?
O7 W5 O9 P1 133.6(7) . . . . ?
O16 W5 O9 P1 -133.9(7) . . . . ?
O13 W5 O9 W6 61(3) . . . 2_655 ?
O18 W5 O9 W6 -94.4(3) . . . 2_655 ?
O8 W5 O9 W6 178.6(4) . . . 2_655 ?
O7 W5 O9 W6 -2.1(4) . . . 2_655 ?
O16 W5 O9 W6 90.3(3) . . . 2_655 ?
O13 W5 O9 W3 -27(3) . . . . ?
O18 W5 O9 W3 177.2(3) . . . . ?
O8 W5 O9 W3 90.2(4) . . . . ?
O7 W5 O9 W3 -90.4(4) . . . . ?
O16 W5 O9 W3 2.0(3) . . . . ?
O20 W6 O10 W3 -172.3(6) . . . 2_655 ?
O7 W6 O10 W3 -72.0(5) 2_655 . . 2_655 ?
O3 W6 O10 W3 86.5(5) . . . 2_655 ?
O18 W6 O10 W3 11.1(14) . . . 2_655 ?
O9 W6 O10 W3 3.1(4) 2_655 . . 2_655 ?
O19 W3 O12 W2 128.1(11) . . . . ?
O16 W3 O12 W2 -132.3(11) . . . . ?
O6 W3 O12 W2 27.0(11) . . . . ?
O10 W3 O12 W2 -43.4(18) 2_655 . . . ?
O9 W3 O12 W2 -56.7(11) . . . . ?
O17 W2 O12 W3 -129.9(11) . . . . ?
O2 W2 O12 W3 -27.8(11) . . . . ?
O14 W2 O12 W3 56.3(17) . . . . ?
O5 W2 O12 W3 132.5(11) . . . . ?
O1 W2 O12 W3 58.1(11) 2_655 . . . ?
O18 W5 O13 Ni1 -143.2(6) . . . . ?
O8 W5 O13 Ni1 -54.7(7) . . . . ?
O7 W5 O13 Ni1 123.3(6) . . . . ?
O16 W5 O13 Ni1 33.3(7) . . . . ?
O9 W5 O13 Ni1 61(3) . . . . ?
N6 Ni1 O13 W5 -118.1(8) . . . . ?
N6 Ni1 O13 W5 148.8(8) 2_755 . . . ?
N5 Ni1 O13 W5 -33.2(7) . . . . ?
N5 Ni1 O13 W5 63.8(7) 2_755 . . . ?
O17 W2 O14 W1 -169.7(5) . . . 2_655 ?
O2 W2 O14 W1 87.3(5) . . . 2_655 ?
O12 W2 O14 W1 4.1(13) . . . 2_655 ?
O5 W2 O14 W1 -71.8(5) . . . 2_655 ?
O1 W2 O14 W1 2.3(4) 2_655 . . 2_655 ?
O19 W3 O16 W5 -173.3(5) . . . . ?
O12 W3 O16 W5 86.1(6) . . . . ?
O6 W3 O16 W5 5.8(14) . . . . ?
O10 W3 O16 W5 -72.5(5) 2_655 . . . ?
O9 W3 O16 W5 3.0(4) . . . . ?
O13 W5 O16 W3 173.2(5) . . . . ?
O18 W5 O16 W3 -15.8(13) . . . . ?
O8 W5 O16 W3 -87.2(6) . . . . ?
O7 W5 O16 W3 71.7(5) . . . . ?
O9 W5 O16 W3 -2.9(4) . . . . ?
O13 W5 O18 W6 131.9(11) . . . . ?
O8 W5 O18 W6 32.5(11) . . . . ?
O7 W5 O18 W6 -126.0(11) . . . . ?
O16 W5 O18 W6 -38.9(18) . . . . ?
O9 W5 O18 W6 -51.4(11) . . . . ?
O20 W6 O18 W5 -131.8(11) . . . . ?
O7 W6 O18 W5 128.0(11) 2_655 . . . ?
O3 W6 O18 W5 -31.5(11) . . . . ?
O10 W6 O18 W5 44.8(19) . . . . ?
O9 W6 O18 W5 52.6(11) 2_655 . . . ?
N1 C2 C3 N2 26(4) . . . . ?
N1 C2 C3 C1 -179(2) . . . . ?
Ni2 N2 C3 C2 -23(3) . . . . ?
Ni2 N2 C3 C1 -179.0(17) . . . . ?
N4 C4 C5 N3 -45(2) . . . . ?
C6 C4 C5 N3 -173.3(16) . . . . ?
N5 C7 C8 N6 -47(2) . . . . ?
C9 C7 C8 N6 -170.6(15) . . . . ?
C3 C2 N1 Ni2 -15(3) . . . . ?
N2 Ni2 N1 C2 1.0(13) . . . . ?
N3 Ni2 N1 C2 33(15) . . . . ?
N4 Ni2 N1 C2 94.1(13) . . . . ?
O1W Ni2 N1 C2 -175.8(13) . . . . ?
O2W Ni2 N1 C2 -91.3(13) . . . . ?
C4 C5 N3 Ni2 28(2) . . . . ?
N2 Ni2 N3 C5 88.0(12) . . . . ?
N1 Ni2 N3 C5 56(14) . . . . ?
N4 Ni2 N3 C5 -5.2(12) . . . . ?
O1W Ni2 N3 C5 -95.0(12) . . . . ?
O2W Ni2 N3 C5 -179.5(12) . . . . ?
C5 C4 N4 Ni2 38.2(18) . . . . ?
C6 C4 N4 Ni2 167.5(12) . . . . ?
N2 Ni2 N4 C4 -112.8(11) . . . . ?
N3 Ni2 N4 C4 -18.2(11) . . . . ?
N1 Ni2 N4 C4 163.9(11) . . . . ?
O1W Ni2 N4 C4 72.5(11) . . . . ?
O2W Ni2 N4 C4 20(3) . . . . ?
C8 C7 N5 Ni1 34.2(17) . . . . ?
C9 C7 N5 Ni1 158.3(12) . . . . ?
N6 Ni1 N5 C7 -12.1(11) . . . . ?
N6 Ni1 N5 C7 36(13) 2_755 . . . ?
N5 Ni1 N5 C7 170.0(14) 2_755 . . . ?
O13 Ni1 N5 C7 -97.8(11) . . . . ?
C7 C8 N6 Ni1 37.3(19) . . . . ?
N6 Ni1 N6 C8 169.1(14) 2_755 . . . ?
N5 Ni1 N6 C8 -13.0(12) . . . . ?
N5 Ni1 N6 C8 121(12) 2_755 . . . ?
O13 Ni1 N6 C8 80.5(12) . . . . ?
