#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/18/7101879.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_7101879
loop_
_publ_author_name
'Zheng, Shou-Tian'
'Yuan, Da-Qiang'
'Jia, Hong-Peng'
'Zhang, Jie'
'Yang, Guo-Yu'
_publ_section_title
;
 Combination between lacunary polyoxometalates and high-nuclear
 transition metal clusters under hydrothermal conditions: I. from
 isolated cluster to 1-D chain.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1858
_journal_page_last               1860
_journal_paper_doi               10.1039/b617191e
_journal_year                    2007
_chemical_formula_moiety         'C12 H46 N9 Ni6 P W9 O39, 4(H2 O)'
_chemical_formula_sum            'C12 H54 N9 Ni6 O43 P W9'
_chemical_formula_weight         3050.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   16.4477(3)
_cell_length_b                   19.4046(3)
_cell_length_c                   16.22210(10)
_cell_measurement_reflns_used    304
_cell_measurement_temperature    274(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.48
_cell_volume                     5177.46(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      274(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29016
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.171
_exptl_absorpt_correction_T_max  0.11
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    3.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.276
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0254P)²+124.9408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                4708
_reflns_number_total             5419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b617191e.txt
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     -P2ac2n
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7101879
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Ni1 Ni 0.11745(14) 0.2500 2.10622(14) 0.0291(5) Uani 1 2 d S . .
Ni2 Ni 0.07780(9) 0.32820(7) 1.94713(9) 0.0183(3) Uani 1 1 d . . .
Ni3 Ni 0.04489(11) 0.2500 1.78897(12) 0.0139(4) Uani 1 2 d S . .
Ni4 Ni 0.05116(9) 0.40962(7) 1.78784(9) 0.0201(3) Uani 1 1 d . . .
W1 W -0.28699(4) 0.2500 1.83664(4) 0.01498(14) Uani 1 2 d S . .
W2 W -0.25203(3) 0.34380(2) 2.02508(3) 0.01759(11) Uani 1 1 d . . .
W3 W -0.13474(3) 0.33538(2) 1.74328(3) 0.01524(11) Uani 1 1 d . . .
W4 W -0.09826(3) 0.42745(2) 1.93202(3) 0.01711(11) Uani 1 1 d . . .
W5 W -0.06415(3) 0.34262(2) 2.10523(3) 0.02011(12) Uani 1 1 d . . .
P1 P -0.0931(2) 0.2500 1.9262(2) 0.0098(7) Uani 1 2 d S . .
O1 O 0.1104(5) 0.3267(4) 1.8314(5) 0.0195(16) Uani 1 1 d . . .
H1A H 0.1690 0.3246 1.8204 0.023 Uiso 1 1 calc R . .
O2 O 0.1417(7) 0.2500 1.9852(7) 0.022(2) Uani 1 2 d S . .
H2C H 0.1994 0.2500 1.9699 0.027 Uiso 1 2 calc SR . .
O3 O 0.0309(5) 0.3230(4) 2.0623(5) 0.0230(18) Uani 1 1 d . . .
O4 O -0.0048(6) 0.2500 1.9081(6) 0.014(2) Uani 1 2 d S . .
O5 O -0.0001(4) 0.3994(4) 1.9035(5) 0.0181(16) Uani 1 1 d . . .
O6 O -0.0283(4) 0.3280(4) 1.7549(5) 0.0173(16) Uani 1 1 d . . .
O7 O -0.0412(6) 0.3739(5) 2.1979(5) 0.032(2) Uani 1 1 d . . .
O8 O -0.1164(5) 0.3130(4) 1.9753(5) 0.0181(16) Uani 1 1 d . . .
O9 O -0.1812(5) 0.3531(4) 2.1101(5) 0.0199(17) Uani 1 1 d . . .
O10 O -0.0828(7) 0.2500 2.1309(6) 0.020(2) Uani 1 2 d S . .
O11 O -0.1403(6) 0.2500 1.8475(6) 0.013(2) Uani 1 2 d S . .
O12 O -0.0705(5) 0.4235(4) 2.0429(5) 0.0210(17) Uani 1 1 d . . .
O13 O -0.0965(5) 0.5119(4) 1.9111(5) 0.0238(18) Uani 1 1 d . . .
O14 O -0.1405(5) 0.3940(4) 1.8326(4) 0.0154(15) Uani 1 1 d . . .
O15 O -0.1383(6) 0.2500 1.6888(6) 0.014(2) Uani 1 2 d S . .
O16 O -0.2822(5) 0.3143(4) 1.9190(4) 0.0188(16) Uani 1 1 d . . .
O17 O -0.2482(4) 0.3156(4) 1.7641(5) 0.0160(16) Uani 1 1 d . . .
O18 O -0.1451(5) 0.3914(4) 1.6653(5) 0.0254(18) Uani 1 1 d . . .
O19 O -0.3385(5) 0.3768(5) 2.0611(5) 0.029(2) Uani 1 1 d . . .
O20 O -0.2072(5) 0.4192(4) 1.9757(5) 0.0202(17) Uani 1 1 d . . .
O21 O -0.3873(6) 0.2500 1.8145(7) 0.018(2) Uani 1 2 d S . .
O22 O -0.2607(6) 0.2500 2.0475(7) 0.019(2) Uani 1 2 d S . .
N1 N 0.1899(10) 0.3291(9) 2.1426(10) 0.072(5) Uani 1 1 d DU . .
H1D H 0.1802 0.3661 2.1108 0.086 Uiso 1 1 d R A .
H1E H 0.2427 0.3172 2.1360 0.086 Uiso 1 1 d R . .
N2 N 0.0865(10) 0.2500 2.2284(9) 0.033(4) Uani 1 2 d S . .
H2E H 0.0320 0.2500 2.2329 0.040 Uiso 1 2 d SR A .
N3 N 0.1395(7) 0.4763(6) 1.8233(7) 0.036(3) Uani 1 1 d . . .
H3C H 0.1177 0.5090 1.8558 0.043 Uiso 1 1 calc R . .
H3D H 0.1772 0.4535 1.8529 0.043 Uiso 1 1 calc R . .
N4 N 0.1023(7) 0.4220(5) 1.6751(6) 0.030(2) Uani 1 1 d . . .
H4C H 0.1174 0.3798 1.6561 0.036 Uiso 1 1 calc R . .
N5 N -0.0229(6) 0.4876(5) 1.7451(6) 0.026(2) Uani 1 1 d . . .
H5C H -0.0750 0.4733 1.7456 0.031 Uiso 1 1 calc R . .
H5D H -0.0189 0.5243 1.7788 0.031 Uiso 1 1 calc R . .
C1 C 0.194(2) 0.3345(18) 2.2323(18) 0.061(7) Uani 0.62(4) 1 d PDU A 1
H1B H 0.2073 0.3814 2.2485 0.073 Uiso 0.62(4) 1 calc PR A 1
H1C H 0.2361 0.3041 2.2537 0.073 Uiso 0.62(4) 1 calc PR A 1
C2 C 0.1115(17) 0.3139(18) 2.266(2) 0.046(7) Uani 0.62(4) 1 d PDU A 1
H2A H 0.1145 0.3084 2.3253 0.055 Uiso 0.62(4) 1 calc PR A 1
H2B H 0.0720 0.3496 2.2538 0.055 Uiso 0.62(4) 1 calc PR A 1
C1A C 0.154(4) 0.356(2) 2.220(2) 0.061(7) Uani 0.38(4) 1 d PD . 2
H1AA H 0.1101 0.3868 2.2068 0.073 Uiso 0.38(4) 1 calc PR A 2
H1AB H 0.1954 0.3817 2.2497 0.073 Uiso 0.38(4) 1 calc PR A 2
C2A C 0.123(4) 0.297(3) 2.274(4) 0.046(7) Uani 0.38(4) 1 d PD . 2
H2AA H 0.1679 0.2767 2.3040 0.055 Uiso 0.38(4) 1 calc PR A 2
H2AB H 0.0848 0.3157 2.3142 0.055 Uiso 0.38(4) 1 calc PR A 2
C3 C 0.1762(13) 0.5069(10) 1.7565(10) 0.071(5) Uani 1 1 d DU . .
H3A H 0.2328 0.5157 1.7695 0.085 Uiso 1 1 calc R . .
H3B H 0.1503 0.5510 1.7461 0.085 Uiso 1 1 calc R . .
C4 C 0.1717(9) 0.4637(8) 1.6793(8) 0.040(4) Uani 1 1 d D . .
H4A H 0.1725 0.4940 1.6317 0.048 Uiso 1 1 calc R . .
H4B H 0.2196 0.4346 1.6765 0.048 Uiso 1 1 calc R . .
C5 C 0.0412(8) 0.4489(7) 1.6212(8) 0.033(3) Uani 1 1 d . . .
H5A H 0.0022 0.4131 1.6079 0.040 Uiso 1 1 calc R . .
H5B H 0.0660 0.4646 1.5703 0.040 Uiso 1 1 calc R . .
C6 C -0.0008(8) 0.5077(6) 1.6629(9) 0.031(3) Uani 1 1 d . . .
H6A H 0.0349 0.5474 1.6648 0.038 Uiso 1 1 calc R . .
H6B H -0.0492 0.5203 1.6321 0.038 Uiso 1 1 calc R . .
OW1 O 0.1569(5) 0.4014(5) 1.9839(6) 0.034(2) Uani 1 1 d . . .
OW2 O 0.296(4) 0.467(3) 1.962(3) 0.102(11) Uani 0.50 1 d PU . .
OW2A O 0.309(4) 0.442(3) 1.987(3) 0.102(11) Uani 0.50 1 d P . .
OW3 O 0.3068(11) 0.2500 1.9716(11) 0.070(5) Uani 1 2 d SU . .
OW4 O -0.500(3) 0.337(3) 2.048(3) 0.056(9) Uani 0.25 1 d PU . .
OW4A O -0.483(3) 0.312(3) 2.003(3) 0.056(9) Uani 0.25 1 d 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'
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'
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
O2 Ni1 N1 99.7(5) . . ?
N1 Ni1 N1 98.2(10) . 7_565 ?
O2 Ni1 N2 177.1(6) . . ?
N1 Ni1 N2 82.2(6) . . ?
O2 Ni1 O3 78.8(3) . 7_565 ?
N1 Ni1 O3 172.6(6) . 7_565 ?
N1 Ni1 O3 89.3(6) 7_565 7_565 ?
N2 Ni1 O3 99.1(4) . 7_565 ?
O2 Ni1 O3 78.8(3) . . ?
N1 Ni1 O3 89.3(6) . . ??
N2 Ni1 O3 99.1(4) . . ?
O3 Ni1 O3 83.3(5) 7_565 . ?
O2 Ni2 O1 98.3(4) . . ?
O2 Ni2 O5 172.1(3) . . ?
O1 Ni2 O5 81.2(3) . . ?
O2 Ni2 OW1 96.1(4) . . ?
O1 Ni2 OW1 96.8(4) . . ?
O5 Ni2 OW1 91.8(4) . . ?
O2 Ni2 O3 82.8(4) . . ?
O1 Ni2 O3 172.5(3) . . ?
O5 Ni2 O3 96.7(3) . . ?
OW1 Ni2 O3 90.4(4) . . ?
O2 Ni2 O4 83.3(3) . . ?
O1 Ni2 O4 83.0(3) . . ?
O5 Ni2 O4 88.8(3) . . ?
OW1 Ni2 O4 179.4(3) . . ?
O3 Ni2 O4 89.8(4) . . ?
O1 Ni3 O1 98.6(5) . 7_565 ?
O1 Ni3 O6 174.8(3) . 7_565 ?
O1 Ni3 O6 81.6(3) 7_565 7_565 ?
O1 Ni3 O6 81.6(3) . . ?
O1 Ni3 O6 174.8(3) 7_565 . ?
O6 Ni3 O6 97.6(4) 7_565 . ?
O1 Ni3 O21 89.3(3) . 6_659 ?
O1 Ni3 O21 89.3(3) 7_565 6_659 ?
O6 Ni3 O21 95.9(3) 7_565 6_659 ?
O6 Ni3 O21 95.9(3) . 6_659 ?
O1 Ni3 O4 83.8(3) . . ?
O1 Ni3 O4 83.8(3) 7_565 . ?
O6 Ni3 O4 91.1(3) 7_565 . ?
O6 Ni3 O4 91.1(3) . . ?
O21 Ni3 O4 169.3(4) 6_659 . ?
O1 Ni4 N4 102.2(4) . . ?
O1 Ni4 N3 93.6(4) . . ?
N4 Ni4 N3 83.3(5) . . ?
O1 Ni4 N5 172.8(4) . . ?
N4 Ni4 N5 81.6(4) . . ?
N3 Ni4 N5 92.9(5) . . ?
O1 Ni4 O5 78.6(3) . . ?
N4 Ni4 O5 178.6(4) . . ?
N3 Ni4 O5 95.5(4) . . ?
N5 Ni4 O5 97.7(4) . . ?
O1 Ni4 O6 77.9(3) . . ?
N4 Ni4 O6 96.7(4) . . ?
N3 Ni4 O6 171.3(4) . . ?
N5 Ni4 O6 95.7(4) . . ?
O5 Ni4 O6 84.6(3) . . ?
O21 W1 O16 101.4(4) . . ?
O21 W1 O16 101.4(4) . 7_565 ?
O16 W1 O16 86.0(5) . 7_565 ?
O21 W1 O17 101.7(3) . 7_565 ?
O16 W1 O17 157.0(3) . 7_565 ?
O16 W1 O17 88.9(3) 7_565 7_565 ?
O21 W1 O17 101.7(3) . . ?
O16 W1 O17 88.9(3) . . ?
O16 W1 O17 157.0(3) 7_565 . ?
O17 W1 O17 87.1(5) 7_565 . ?
O21 W1 O11 171.9(4) . . ?
O16 W1 O11 84.5(3) . . ?
O16 W1 O11 84.5(3) 7_565 . ?
O17 W1 O11 72.6(3) 7_565 . ?
O17 W1 O11 72.6(3) . . ?
O19 W2 O9 104.1(4) . . ?
O19 W2 O20 101.0(4) . . ?
O9 W2 O20 89.7(4) . . ?
O19 W2 O22 104.0(5) . . ?
O9 W2 O22 89.9(4) . . ?
O20 W2 O22 154.3(4) . . ?
O19 W2 O16 102.3(4) . . ?
O9 W2 O16 153.6(3) . . ?
O20 W2 O16 87.1(3) . . ?
O22 W2 O16 82.0(4) . . ?
O19 W2 O8 171.3(4) . . ?
O9 W2 O8 72.0(3) . . ?
O20 W2 O8 71.5(3) . . ?
O22 W2 O8 84.0(4) . . ?
O16 W2 O8 82.2(3) . . ?
O18 W3 O6 103.5(4) . . ?
O18 W3 O14 100.8(4) . . ?
O6 W3 O14 91.0(3) . . ?
O18 W3 O15 102.4(4) . . ?
O6 W3 O15 90.6(4) . . ?
O14 W3 O15 155.7(4) . . ?
O18 W3 O17 99.3(4) . . ?
O6 W3 O17 157.1(3) . . ?
O14 W3 O17 86.3(3) . . ?
O15 W3 O17 83.0(4) . . ?
O18 W3 O11 171.1(4) . . ?
O6 W3 O11 84.6(3) . . ?
O14 W3 O11 82.5(3) . . ?
O15 W3 O11 73.6(3) . . ?
O17 W3 O11 72.5(3) . . ?
O13 W4 O5 103.5(4) . . ?
O13 W4 O12 103.5(4) . . ?
O5 W4 O12 90.9(3) . . ?
O13 W4 O14 99.8(4) . . ?
O5 W4 O14 90.4(3) . . ?
O12 W4 O14 155.7(3) . . ?
O13 W4 O20 99.9(4) . . ?
O5 W4 O20 156.6(3) . . ?
O12 W4 O20 82.5(3) . . ?
O14 W4 O20 86.7(3) . . ?
O13 W4 O8 171.4(3) . . ?
O5 W4 O8 84.4(3) . . ?
O12 W4 O8 72.7(3) . . ?
O14 W4 O8 83.2(3) . . ?
O20 W4 O8 72.2(3) . . ?
O7 W5 O3 103.6(4) . . ?
O7 W5 O10 100.8(4) . . ?
O3 W5 O10 91.5(4) . . ?
O7 W5 O12 101.2(4) . . ?
O3 W5 O12 91.0(4) . . ?
O10 W5 O12 156.6(4) . . ?
O7 W5 O9 98.7(4) . . ?
O3 W5 O9 157.7(3) . . ?
O10 W5 O9 85.9(4) . . ?
O12 W5 O9 83.0(3) . . ?
O7 W5 O8 169.5(4) . . ?
O3 W5 O8 85.2(3) . . ?
O10 W5 O8 84.5(4) . . ?
O12 W5 O8 72.6(3) . . ?
O9 W5 O8 72.5(3) . . ?
O4 P1 O11 109.9(6) . . ?
O4 P1 O8 110.7(4) . 7_565 ?
O11 P1 O8 108.6(4) . 7_565 ?
O4 P1 O8 110.7(4) . . ?
O11 P1 O8 108.6(4) . . ?
O8 P1 O8 108.3(6) 7_565 . ?
Ni2 O1 Ni3 101.4(3) . . ?
Ni2 O1 Ni4 101.1(3) . . ?
Ni3 O1 Ni4 102.6(4) . . ?
Ni2 O1 H1A 116.4 . . ?
Ni3 O1 H1A 116.4 . . ?
Ni4 O1 H1A 116.4 . . ?
Ni2 O2 Ni2 102.4(5) 7_565 . ?
Ni2 O2 Ni1 101.7(4) 7_565 . ?
Ni2 O2 Ni1 101.7(4) . . ?
Ni2 O2 H2C 116.2 7_565 . ?
Ni2 O2 H2C 116.2 . . ?
Ni1 O2 H2C 116.2 . . ?
W5 O3 Ni2 134.1(5) . . ?
W5 O3 Ni1 127.4(4) . . ?
Ni2 O3 Ni1 95.0(3) . . ?
P1 O4 Ni3 124.4(6) . . ?
P1 O4 Ni2 124.4(4) . . ?
Ni3 O4 Ni2 91.5(3) . . ?
P1 O4 Ni2 124.4(4) . 7_565 ?
Ni3 O4 Ni2 91.5(3) . 7_565 ?
Ni2 O4 Ni2 90.7(4) . 7_565 ?
W4 O5 Ni2 134.6(4) . . ?
W4 O5 Ni4 125.5(4) . . ?
Ni2 O5 Ni4 97.2(3) . . ?
W3 O6 Ni3 133.1(4) . . ?
W3 O6 Ni4 125.3(4) . . ?
Ni3 O6 Ni4 97.1(3) . . ?
P1 O8 W5 125.4(4) . . ?
P1 O8 W4 125.2(4) . . ?
W5 O8 W4 89.4(3) . . ?
P1 O8 W2 127.2(4) . . ?
W5 O8 W2 88.7(3) . . ?
W4 O8 W2 89.0(3) . . ?
W2 O9 W5 126.6(4) . . ?
W5 O10 W5 147.8(6) . 7_565 ?
P1 O11 W3 126.1(3) . 7_565 ?
P1 O11 W3 126.1(3) . . ?
W3 O11 W3 88.8(3) 7_565 . ?
P1 O11 W1 125.5(6) . . ?
W3 O11 W1 89.3(3) 7_565 . ?
W3 O11 W1 89.3(3) . . ?
W4 O12 W5 124.8(4) . . ?
W3 O14 W4 150.6(4) . . ?
W3 O15 W3 123.8(5) . 7_565 ?
W1 O16 W2 152.5(5) . . ?
W1 O17 W3 125.5(4) . . ?
W2 O20 W4 127.0(4) . . ?
W1 O21 Ni3 135.9(6) . 6_559 ?
W2 O22 W2 155.8(7) 7_565 . ?
C1 N1 Ni1 111.9(14) . . ?
C1A N1 Ni1 106(2) . . ?
C1 N1 H1D 121.6 . . ?
C1A N1 H1D 97.9 . . ?
Ni1 N1 H1D 109.4 . . ?
C1 N1 H1E 95.1 . . ?
C1A N1 H1E 124.7 . . ?
Ni1 N1 H1E 109.6 . . ?
H1D N1 H1E 107.8 . . ?
C2A N2 C2A 88(5) . 7_565 ?
C2A N2 C2 103(3) 7_565 . ?
C2A N2 C2 103(3) . 7_565 ?
C2 N2 C2 119(3) . 7_565 ?
C2A N2 Ni1 116(2) . . ?
C2A N2 Ni1 116(2) 7_565 . ?
C2 N2 Ni1 109.8(15) . . ?
C2 N2 Ni1 109.8(15) 7_565 . ?
C2A N2 H2E 113.9 . . ?
C2A N2 H2E 113.9 7_565 . ?
C2 N2 H2E 104.4 . . ?
C2 N2 H2E 104.4 7_565 . ?
Ni1 N2 H2E 109.1 . . ?
C3 N3 Ni4 111.4(10) . . ?
C3 N3 H3C 109.3 . . ?
Ni4 N3 H3C 109.3 . . ?
C3 N3 H3D 109.3 . . ?
Ni4 N3 H3D 109.3 . . ?
H3C N3 H3D 108.0 . . ?
C4 N4 C5 113.1(11) . . ?
C4 N4 Ni4 111.3(8) . . ?
C5 N4 Ni4 107.7(8) . . ?
C4 N4 H4C 108.2 . . ?
C5 N4 H4C 108.2 . . ?
Ni4 N4 H4C 108.2 . . ?
C6 N5 Ni4 111.2(8) . . ?
C6 N5 H5C 109.4 . . ?
Ni4 N5 H5C 109.4 . . ?
C6 N5 H5D 109.4 . . ?
Ni4 N5 H5D 109.4 . . ?
H5C N5 H5D 108.0 . . ?
N1 C1 C2 107(3) . . ?
N1 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
N1 C1 H1C 110.3 . . ?
C2 C1 H1C 110.3 . . ?
H1B C1 H1C 108.6 . . ?
N2 C2 C1 109(2) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N1 C1A C2A 111(4) . . ?
N1 C1A H1AA 109.3 . . ?
C2A C1A H1AA 109.3 . . ?
N1 C1A H1AB 109.3 . . ?
C2A C1A H1AB 109.3 . . ?
H1AA C1A H1AB 108.0 . . ?
N2 C2A C1A 110(4) . . ?
N2 C2A C2A 46(2) . 7_565 ?
C1A C2A C2A 138(3) . 7_565 ?
N2 C2A H2AA 109.6 . . ?
C1A C2A H2AA 109.6 . . ?
C2A C2A H2AA 65.5 7_565 . ?
N2 C2A H2AB 109.6 . . ?
C1A C2A H2AB 109.6 . . ?
C2A C2A H2AB 111.4 7_565 . ?
H2AA C2A H2AB 108.1 . . ?
N3 C3 C4 113.1(13) . . ?
N3 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N3 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N4 C4 C3 113.6(12) . . ?
N4 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
N4 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N4 C5 C6 109.0(11) . . ?
N4 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N4 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N5 C6 C5 109.3(10) . . ?
N5 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N5 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.003(12) .
Ni1 N1 2.031(15) .
Ni1 N2 2.046(15) .
Ni1 O3 2.131(8) .
Ni2 O2 1.947(7) .
Ni2 O1 1.953(8) .
Ni2 O5 2.013(8) .
Ni2 OW1 2.016(9) .
Ni2 O3 2.024(8) .
Ni2 O4 2.133(8) .
Ni3 O1 1.962(8) .
Ni3 O6 2.012(7) .
Ni3 O21 2.015(11) 6_659
Ni3 O4 2.098(10) .
Ni4 O1 2.010(8) .
Ni4 N4 2.027(10) .
Ni4 N3 2.029(11) .
Ni4 N5 2.063(10) .
Ni4 O5 2.067(8) .
Ni4 O6 2.121(8) .
W1 O21 1.688(10) .
W1 O16 1.829(7) .
W1 O17 1.847(7) .
W1 O11 2.419(10) .
W2 O19 1.665(8) .
W2 O9 1.814(8) .
W2 O20 1.824(8) .
W2 O22 1.862(2) .
W2 O16 1.881(7) .
W2 O8 2.447(8) .
W3 O18 1.677(8) .
W3 O6 1.766(7) .
W3 O14 1.845(7) .
W3 O15 1.878(5) .
W3 O17 1.935(7) .
W3 O11 2.369(7) .
W4 O13 1.673(7) .
W4 O5 1.765(7) .
W4 O12 1.858(8) .
W4 O14 1.872(7) .
W4 O20 1.933(8) .
W4 O8 2.349(8) .
W5 O7 1.665(8) .
W5 O3 1.753(8) .
W5 O10 1.870(3) .
W5 O12 1.870(8) .
W5 O9 1.938(8) .
W5 O8 2.349(8) .
P1 O4 1.482(11) .
P1 O11 1.495(10) .
P1 O8 1.508(8) .
O1 H1A 0.9800 .
O2 Ni2 1.947(7) 7_565
O2 H2C 0.9800 .
O4 Ni2 2.133(8) 7_565
O10 W5 1.870(3) 7_565
O11 W3 2.369(7) 7_565
O15 W3 1.878(5) 7_565
O21 Ni3 2.015(11) 6_559
O22 W2 1.862(2) 7_565
N1 C1 1.46(3) .
N1 C1A 1.475(10) .
N1 H1D 0.8989 .
N1 H1E 0.9043 .
N2 C2A 1.33(7) .
N2 C2 1.44(4) .
N2 H2E 0.8989 .
N3 C3 1.38(2) .
N3 H3C 0.9000 .
N3 H3D 0.9000 .
N4 C4 1.401(18) .
N4 C5 1.430(17) .
N4 H4C 0.9100 .
N5 C6 1.436(16) .
N5 H5C 0.9000 .
N5 H5D 0.9000 .
C1 C2 1.521(10) .
C1 H1B 0.9700 .
C1 H1C 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C1A H1AA 0.9700 .
C1A H1AB 0.9700 .
C2A H2AA 0.9700 .
C2A H2AB 0.9700 .
C3 C4 1.509(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.496(19) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C O12 0.90 2.24 3.126(14) 168.6 5_569
N3 H3D OW1 0.90 2.38 2.996(16) 126.1 .
N3 H3D OW2 0.90 2.64 3.42(6) 144.5 .
N4 H4C O16 0.91 2.41 3.211(13) 146.4 6_659
N4 H4C O21 0.91 2.57 3.347(11) 144.3 6_659
N5 H5C O14 0.90 2.35 3.010(12) 130.1 .
N5 H5C O18 0.90 2.36 3.034(14) 132.0 .
N5 H5D O7 0.90 2.24 3.030(13) 146.3 5_569
N5 H5D O13 0.90 2.51 2.989(13) 114.0 .
