#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:48:10 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223612 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/24/7232487.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_7232487
loop_
_publ_author_name
'Zhang, Zhong'
'Wang, Yue-Lin'
'Li, Hai-Lou'
'Sun, Ke-Ning'
'Yang, Guo-Yu'
_publ_section_title
;
 Syntheses, structures and properties of three organic--inorganic hybrid
 polyoxotungstates constructed from {Ni6PW9} building blocks: from
 isolated clusters to 2-D layers
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2641
_journal_paper_doi               10.1039/C9CE00194H
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C16.67 H32 N6.67 Ni5 O33.67 P0.67 W6'
_chemical_formula_weight         2281.78
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-09-21 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   21.5089(16)
_cell_length_b                   21.5089(16)
_cell_length_c                   58.751(5)
_cell_measurement_temperature    296(2)
_cell_volume                     23539(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            74581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.040
_exptl_absorpt_coefficient_mu    15.000
_exptl_crystal_density_diffrn    2.897
_exptl_crystal_F_000             18756
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         6.018
_refine_diff_density_min         -3.364
_refine_diff_density_rms         0.461
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9272
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1061P)²+5053.5005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7287
_reflns_number_total             9272
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00194h1.cif
_cod_data_source_block           3_a
_cod_depositor_comments
'Adding full bibliography for 7232485--7232487.cif.'
_cod_original_cell_volume        23539(4)
_cod_database_code               7232487
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.153
_shelx_estimated_absorpt_t_max   0.198
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ni1 Ni 0.91708(11) 1.00209(11) 0.67462(4) 0.0197(5) Uani 1 1 d . . .
Ni2 Ni 0.83218(12) 0.84391(12) 0.67866(5) 0.0248(6) Uani 1 1 d . . .
Ni3 Ni 0.50150(12) 0.67830(12) 0.76053(4) 0.0218(5) Uani 1 1 d . . .
Ni4 Ni 0.33464(11) 0.58359(11) 0.76483(4) 0.0180(5) Uani 1 1 d . . .
Ni5 Ni 0.5927(2) 0.5804(3) 0.87244(7) 0.0819(15) Uani 1 1 d . . .
P1 P 1.000000 1.000000 0.62769(12) 0.0105(14) Uani 1 3 d S T P
P2 P 0.333333 0.666667 0.81161(11) 0.0066(13) Uani 1 3 d S T P
W1 W 0.52289(4) 0.76691(4) 0.81323(2) 0.0247(2) Uani 1 1 d . . .
W2 W 0.90579(4) 1.09697(4) 0.62736(2) 0.0272(2) Uani 1 1 d . . .
W3 W 0.42776(4) 0.56964(4) 0.81219(2) 0.0248(2) Uani 1 1 d . . .
W4 W 0.80987(4) 0.91354(4) 0.62642(2) 0.0278(2) Uani 1 1 d . . .
W5 W 0.33679(5) 0.56871(5) 0.86111(2) 0.0306(2) Uani 1 1 d . . .
W6 W 0.90296(5) 1.00545(5) 0.57853(2) 0.0432(3) Uani 1 1 d . . .
C1 C 0.7453(9) 0.7057(11) 0.7015(3) 0.047(5) Uani 1 1 d D U .
C2 C 0.7224(13) 0.6932(10) 0.6768(3) 0.045(5) Uani 1 1 d D U .
C3 C 0.6054(17) 0.6305(14) 0.7634(5) 0.068(6) Uani 1 1 d D U .
C4 C 0.5773(11) 0.6144(19) 0.7392(5) 0.078(7) Uani 1 1 d D U .
C5 C 0.7848(11) 0.9406(11) 0.7003(4) 0.032(3) Uani 1 1 d . U .
C6 C 0.7229(10) 0.9441(10) 0.7099(4) 0.027(3) Uani 1 1 d . U .
C7 C 0.6643(10) 0.8839(10) 0.7184(3) 0.027(3) Uani 1 1 d . U .
H7 H 0.663895 0.840465 0.718254 0.01(4) Uiso 1 1 calc R . .
C8 C 0.6057(10) 0.8861(10) 0.7273(4) 0.028(3) Uani 1 1 d . U .
C9 C 0.6045(10) 0.9488(10) 0.7271(3) 0.027(3) Uani 1 1 d . U .
H9 H 0.564222 0.949938 0.732323 0.00(4) Uiso 1 1 calc R . .
C10 C 0.6646(10) 1.0121(11) 0.7190(4) 0.029(3) Uani 1 1 d . U .
H10 H 0.664822 1.055419 0.719224 0.08(10) Uiso 1 1 calc R . .
C11 C 0.7233(11) 1.0089(11) 0.7108(4) 0.030(3) Uani 1 1 d . U .
H11 H 0.763439 1.050713 0.705737 0.07(9) Uiso 1 1 calc R . .
C12 C 0.5462(10) 0.8200(10) 0.7382(4) 0.027(3) Uani 1 1 d . U .
C13 C 0.459(2) 0.4414(17) 0.8820(5) 0.089(8) Uani 1 1 d D U .
C14 C 0.4688(15) 0.4862(18) 0.9031(6) 0.084(8) Uani 1 1 d D U .
C15 C 0.9332(11) 0.9314(10) 0.7156(5) 0.0568(13) Uani 1 1 d D U .
C16 C 1.000000 1.000000 0.7232(6) 0.0568(11) Uani 1 3 d DS TU P
C17 C 0.2645(15) 0.6014(16) 0.7245(7) 0.0954(13) Uani 1 1 d D U .
C18 C 0.333333 0.666667 0.7163(8) 0.0954(12) Uani 1 3 d DS TU P
N1 N 0.8204(8) 0.7647(8) 0.7012(3) 0.037(4) Uani 1 1 d D . .
N2 N 0.7375(10) 0.7608(9) 0.6658(3) 0.042(5) Uani 1 1 d D U .
N3 N 0.5969(10) 0.6889(10) 0.7730(4) 0.048(5) Uani 1 1 d D . .
N4 N 0.5033(10) 0.6018(10) 0.7395(3) 0.038(4) Uani 1 1 d D . .
N5 N 0.492(2) 0.4915(19) 0.8628(6) 0.109(10) Uani 1 1 d D U .
N6 N 0.5466(15) 0.5376(16) 0.9044(6) 0.090(9) Uani 1 1 d D U .
N7 N 1.000000 1.000000 0.7482(6) 0.0570(13) Uani 1 3 d DS TU P
N8 N 0.333333 0.666667 0.6913(8) 0.0954(13) Uani 1 3 d DS TU P
O1 O 0.8430(6) 0.9222(6) 0.6555(2) 0.023(3) Uani 1 1 d . . .
O2 O 0.9287(6) 1.0900(6) 0.6568(2) 0.024(3) Uani 1 1 d . . .
O3 O 0.8766(7) 1.1574(7) 0.6287(3) 0.036(4) Uani 1 1 d . . .
O4 O 0.8185(7) 1.0071(7) 0.6291(3) 0.031(3) Uani 1 1 d . . .
O5 O 0.8931(8) 1.0767(8) 0.5941(2) 0.038(4) Uani 1 1 d . . .
O6 O 0.8188(8) 0.9334(8) 0.5938(3) 0.038(4) Uani 1 1 d . . .
O7 O 0.9972(7) 0.9307(6) 0.6187(2) 0.025(3) Uani 1 1 d . . .
O8 O 1.000000 1.000000 0.6541(3) 0.018(4) Uani 1 3 d S T P
O9 O 1.0025(9) 1.0695(9) 0.5753(3) 0.044(4) Uani 1 1 d . U .
O10 O 0.8737(11) 1.0079(11) 0.5518(4) 0.067(5) Uani 1 1 d . U .
O11 O 0.8410(7) 0.8460(7) 0.6199(3) 0.031(3) Uani 1 1 d . . .
O12 O 0.7181(7) 0.8573(7) 0.6292(3) 0.037(4) Uani 1 1 d . . .
O13 O 0.9230(7) 0.9234(7) 0.6922(2) 0.022(3) Uani 1 1 d . U .
O14 O 0.7757(8) 0.8770(7) 0.6988(3) 0.047(5) Uani 1 1 d . . .
O15 O 0.8386(7) 0.9969(6) 0.6945(2) 0.028(3) Uani 1 1 d . . .
O16 O 0.4933(7) 0.8243(7) 0.7447(3) 0.029(3) Uani 1 1 d . . .
O17 O 0.5568(7) 0.7675(7) 0.7402(3) 0.032(3) Uani 1 1 d . . .
O18 O 0.4910(6) 0.7450(6) 0.7838(2) 0.020(3) Uani 1 1 d . U .
O19 O 0.6136(7) 0.8003(8) 0.8114(2) 0.032(3) Uani 1 1 d . . .
O20 O 0.5139(7) 0.7798(7) 0.8456(2) 0.023(3) Uani 1 1 d . U .
O21 O 0.4913(7) 0.6694(7) 0.8200(3) 0.031(3) Uani 1 1 d . . .
O22 O 0.4212(6) 0.5931(6) 0.7828(2) 0.018(3) Uani 1 1 d . . .
O23 O 0.3362(7) 0.6003(6) 0.8203(2) 0.025(3) Uani 1 1 d . . .
O24 O 0.333333 0.666667 0.7858(3) 0.015(4) Uani 1 3 d S T P
O25 O 0.4085(7) 0.5581(7) 0.8456(2) 0.028(3) Uani 1 1 d . U .
O26 O 0.4029(8) 0.6693(8) 0.8644(2) 0.033(3) Uani 1 1 d . U .
O27 O 0.3381(9) 0.5379(10) 0.8883(3) 0.049(4) Uani 1 1 d . . .
O28 O 0.2565(7) 0.5899(7) 0.7473(2) 0.022(3) Uani 1 1 d . U .
O29 O 0.3366(8) 0.4828(7) 0.8111(2) 0.028(3) Uani 1 1 d . . .
O30 O 0.4871(8) 0.5386(8) 0.8110(3) 0.036(4) Uani 1 1 d . . .
O1W O 0.5458(13) 0.6431(13) 0.8712(4) 0.085(7) Uani 1 1 d . U .
O2W O 0.6235(15) 0.5964(12) 0.8380(4) 0.088(7) Uani 1 1 d . . .
O3W O 0.6937(17) 0.6729(18) 0.8826(4) 0.112(10) Uani 1 1 d . . .
O4W O 0.650(2) 0.522(2) 0.8735(6) 0.138(12) Uani 1 1 d . U .
O5W O 0.6976(10) 0.7334(10) 0.8188(4) 0.066(6) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O13 Ni1 O1 171.9(5) 3_675 .
O13 Ni1 O15 97.7(6) 3_675 .
O1 Ni1 O15 89.6(5) . .
O13 Ni1 O13 90.3(7) 3_675 .
O1 Ni1 O13 85.7(5) . .
O15 Ni1 O13 93.4(5) . .
O13 Ni1 O2 82.8(5) 3_675 .
O1 Ni1 O2 100.4(5) . .
O15 Ni1 O2 93.4(5) . .
O13 Ni1 O2 170.9(5) . .
O13 Ni1 O8 83.6(5) 3_675 .
O1 Ni1 O8 88.9(5) . .
O15 Ni1 O8 175.8(4) . .
O13 Ni1 O8 82.6(5) . .
O2 Ni1 O8 90.7(5) . .
O13 Ni1 Ni2 132.5(4) 3_675 .
O1 Ni1 Ni2 44.7(4) . .
O15 Ni1 Ni2 82.6(4) . .
O13 Ni1 Ni2 42.6(4) . .
O2 Ni1 Ni2 144.7(4) . .
O8 Ni1 Ni2 93.54(9) . .
O13 Ni2 O14 88.2(6) . .
O13 Ni2 N2 178.1(7) . .
O14 Ni2 N2 90.7(7) . .
O13 Ni2 N1 96.6(6) . .
O14 Ni2 N1 93.8(7) . .
N2 Ni2 N1 81.9(7) . .
O13 Ni2 O1 84.4(5) . .
O14 Ni2 O1 86.7(6) . .
N2 Ni2 O1 97.1(6) . .
N1 Ni2 O1 178.9(7) . .
O13 Ni2 O2 80.2(5) . 2_765
O14 Ni2 O2 165.2(5) . 2_765
N2 Ni2 O2 101.0(7) . 2_765
N1 Ni2 O2 96.8(6) . 2_765
O1 Ni2 O2 82.9(5) . 2_765
O13 Ni2 Ni1 43.5(4) . .
O14 Ni2 Ni1 77.3(4) . .
N2 Ni2 Ni1 137.7(5) . .
N1 Ni2 Ni1 138.5(5) . .
O1 Ni2 Ni1 42.6(4) . .
O2 Ni2 Ni1 87.9(3) 2_765 .
O28 Ni3 O17 88.0(5) 2_665 .
O28 Ni3 N4 94.3(6) 2_665 .
O17 Ni3 N4 99.4(7) . .
O28 Ni3 O18 84.6(5) 2_665 .
O17 Ni3 O18 87.2(5) . .
N4 Ni3 O18 173.3(7) . .
O28 Ni3 N3 177.7(7) 2_665 .
O17 Ni3 N3 91.4(8) . .
N4 Ni3 N3 83.6(7) . .
O18 Ni3 N3 97.7(6) . .
O28 Ni3 O22 79.4(5) 2_665 .
O17 Ni3 O22 164.5(5) . .
N4 Ni3 O22 90.6(6) . .
O18 Ni3 O22 82.7(5) . .
N3 Ni3 O22 101.6(7) . .
O28 Ni3 Ni4 43.4(4) 2_665 2_665
O17 Ni3 Ni4 77.2(4) . 2_665
N4 Ni3 Ni4 137.2(5) . 2_665
O18 Ni3 Ni4 42.9(3) . 2_665
N3 Ni3 Ni4 138.5(5) . 2_665
O22 Ni3 Ni4 87.4(3) . 2_665
O28 Ni4 O16 96.5(5) 2_665 3_565
O28 Ni4 O18 172.3(5) 2_665 3_565
O16 Ni4 O18 90.4(5) 3_565 3_565
O28 Ni4 O28 90.4(7) 2_665 .
O16 Ni4 O28 93.6(5) 3_565 .
O18 Ni4 O28 85.6(5) 3_565 .
O28 Ni4 O22 83.4(5) 2_665 .
O16 Ni4 O22 92.5(5) 3_565 .
O18 Ni4 O22 99.9(5) 3_565 .
O28 Ni4 O22 171.7(5) . .
O28 Ni4 O24 84.1(5) 2_665 .
O16 Ni4 O24 176.8(5) 3_565 .
O18 Ni4 O24 88.9(5) 3_565 .
O28 Ni4 O24 83.3(5) . .
O22 Ni4 O24 90.6(4) . .
O28 Ni4 Ni3 132.7(4) 2_665 3_565
O16 Ni4 Ni3 83.1(4) 3_565 3_565
O18 Ni4 Ni3 44.6(4) 3_565 3_565
O28 Ni4 Ni3 42.8(4) . 3_565
O22 Ni4 Ni3 143.9(4) . 3_565
O24 Ni4 Ni3 94.26(9) . 3_565
O1W Ni5 O2W 94.4(10) . .
O1W Ni5 N6 92.3(11) . .
O2W Ni5 N6 165.8(11) . .
O1W Ni5 N5 88.3(13) . .
O2W Ni5 N5 89.3(12) . .
N6 Ni5 N5 78.4(12) . .
O1W Ni5 O3W 90.2(12) . .
O2W Ni5 O3W 91.4(10) . .
N6 Ni5 O3W 101.1(11) . .
N5 Ni5 O3W 178.3(14) . .
O1W Ni5 O4W 175.6(13) . .
O2W Ni5 O4W 84.2(12) . .
N6 Ni5 O4W 90.0(13) . .
N5 Ni5 O4W 95.9(15) . .
O3W Ni5 O4W 85.7(14) . .
O8 P1 O7 109.9(6) . .
O8 P1 O7 109.9(6) . 2_765
O7 P1 O7 109.1(6) . 2_765
O8 P1 O7 109.9(6) . 3_675
O7 P1 O7 109.1(6) . 3_675
O7 P1 O7 109.1(6) 2_765 3_675
O24 P2 O23 109.2(6) . 3_565
O24 P2 O23 109.2(6) . 2_665
O23 P2 O23 109.7(6) 3_565 2_665
O24 P2 O23 109.2(6) . .
O23 P2 O23 109.7(6) 3_565 .
O23 P2 O23 109.7(6) 2_665 .
O19 W1 O18 104.5(6) . .
O19 W1 O21 100.4(6) . .
O18 W1 O21 91.9(6) . .
O19 W1 O29 101.5(6) . 2_665
O18 W1 O29 89.6(5) . 2_665
O21 W1 O29 157.0(6) . 2_665
O19 W1 O20 100.1(6) . .
O18 W1 O20 155.2(5) . .
O21 W1 O20 86.9(6) . .
O29 W1 O20 82.3(5) 2_665 .
O19 W1 O23 170.4(6) . 2_665
O18 W1 O23 82.7(5) . 2_665
O21 W1 O23 85.5(5) . 2_665
O29 W1 O23 71.9(5) 2_665 2_665
O20 W1 O23 72.5(5) . 2_665
O3 W2 O2 103.7(7) . .
O3 W2 O4 102.6(6) . .
O2 W2 O4 92.0(6) . .
O3 W2 O11 100.7(6) . 3_675
O2 W2 O11 91.2(6) . 3_675
O4 W2 O11 155.0(6) . 3_675
O3 W2 O5 98.6(7) . .
O2 W2 O5 157.7(6) . .
O4 W2 O5 82.8(7) . .
O11 W2 O5 84.9(7) 3_675 .
O3 W2 O7 168.8(6) . 3_675
O2 W2 O7 86.6(5) . 3_675
O4 W2 O7 72.3(5) . 3_675
O11 W2 O7 83.1(5) 3_675 3_675
O5 W2 O7 71.1(5) . 3_675
O30 W3 O22 104.2(7) . .
O30 W3 O29 102.5(6) . .
O22 W3 O29 93.2(5) . .
O30 W3 O21 101.0(6) . .
O22 W3 O21 91.6(6) . .
O29 W3 O21 154.0(6) . .
O30 W3 O25 98.0(7) . .
O22 W3 O25 157.8(5) . .
O29 W3 O25 82.2(6) . .
O21 W3 O25 83.8(6) . .
O30 W3 O23 169.2(6) . .
O22 W3 O23 85.7(5) . .
O29 W3 O23 72.3(5) . .
O21 W3 O23 82.6(5) . .
O25 W3 O23 72.2(5) . .
O12 W4 O1 103.5(7) . .
O12 W4 O11 101.4(6) . .
O1 W4 O11 89.8(6) . .
O12 W4 O4 101.6(6) . .
O1 W4 O4 89.3(6) . .
O11 W4 O4 156.5(6) . .
O12 W4 O6 101.4(7) . .
O1 W4 O6 155.0(6) . .
O11 W4 O6 86.4(6) . .
O4 W4 O6 84.6(6) . .
O12 W4 O7 171.2(6) . 3_675
O1 W4 O7 82.9(5) . 3_675
O11 W4 O7 84.4(5) . 3_675
O4 W4 O7 72.2(5) . 3_675
O6 W4 O7 72.1(6) . 3_675
O27 W5 O20 104.0(7) . 3_565
O27 W5 O25 103.0(7) . .
O20 W5 O25 88.8(6) 3_565 .
O27 W5 O26 101.4(8) . 3_565
O20 W5 O26 87.3(6) 3_565 3_565
O25 W5 O26 155.5(6) . 3_565
O27 W5 O26 101.2(8) . .
O20 W5 O26 154.4(6) 3_565 .
O25 W5 O26 89.7(6) . .
O26 W5 O26 83.5(9) 3_565 .
O27 W5 O23 173.0(7) . .
O20 W5 O23 71.6(5) 3_565 .
O25 W5 O23 71.8(5) . .
O26 W5 O23 84.1(5) 3_565 .
O26 W5 O23 83.7(5) . .
O10 W6 O5 103.3(8) . .
O10 W6 O9 100.7(9) . .
O5 W6 O9 90.2(7) . .
O10 W6 O6 104.0(8) . .
O5 W6 O6 89.2(7) . .
O9 W6 O6 154.8(7) . .
O10 W6 O9 101.6(9) . 2_765
O5 W6 O9 155.1(7) . 2_765
O9 W6 O9 83.4(10) . 2_765
O6 W6 O9 86.6(7) . 2_765
O10 W6 O7 173.5(8) . 3_675
O5 W6 O7 72.0(5) . 3_675
O9 W6 O7 84.0(6) . 3_675
O6 W6 O7 71.8(5) . 3_675
O9 W6 O7 83.3(6) 2_765 3_675
N1 C1 C2 104.9(17) . .
N2 C2 C1 110.8(17) . .
N3 C3 C4 110(2) . .
N4 C4 C3 107(2) . .
O15 C5 O14 126.5(19) . .
O15 C5 C6 118.8(18) . .
O14 C5 C6 114.7(17) . .
C7 C6 C11 118.3(18) . .
C7 C6 C5 121.1(17) . .
C11 C6 C5 120.7(18) . .
C6 C7 C8 121.8(18) . .
C6 C7 H7 119.1 . .
C8 C7 H7 119.1 . .
C9 C8 C7 119.9(18) . .
C9 C8 C12 120.9(18) . .
C7 C8 C12 119.1(17) . .
C8 C9 C10 119.7(18) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C11 C10 C9 119.3(18) . .
C11 C10 H10 120.4 . .
C9 C10 H10 120.4 . .
C10 C11 C6 120.9(19) . .
C10 C11 H11 119.6 . .
C6 C11 H11 119.6 . .
O16 C12 O17 128.0(18) . .
O16 C12 C8 116.0(16) . .
O17 C12 C8 115.9(17) . .
N5 C13 C14 107(3) . .
N6 C14 C13 105(3) . .
O13 C15 C16 115(2) . .
N7 C16 C15 106.9(17) . .
N7 C16 C15 106.9(17) . 2_765
C15 C16 C15 111.9(15) . 2_765
N7 C16 C15 106.9(16) . 3_675
C15 C16 C15 111.9(15) . 3_675
C15 C16 C15 111.9(15) 2_765 3_675
O28 C17 C18 117(4) . .
N8 C18 C17 108(2) . .
N8 C18 C17 108(2) . 3_565
C17 C18 C17 111(2) . 3_565
N8 C18 C17 108(2) . 2_665
C17 C18 C17 111(2) . 2_665
C17 C18 C17 111(2) 3_565 2_665
C1 N1 Ni2 110.5(14) . .
C2 N2 Ni2 109.2(14) . .
C3 N3 Ni3 107.9(15) . .
C4 N4 Ni3 108.0(16) . .
C13 N5 Ni5 111(3) . .
C14 N6 Ni5 113(2) . .
W4 O1 Ni1 135.6(7) . .
W4 O1 Ni2 130.4(7) . .
Ni1 O1 Ni2 92.7(5) . .
W2 O2 Ni1 130.0(6) . .
W2 O2 Ni2 130.8(6) . 3_675
Ni1 O2 Ni2 94.7(5) . 3_675
W2 O4 W4 125.7(7) . .
W6 O5 W2 126.6(7) . .
W6 O6 W4 125.8(8) . .
P1 O7 W4 124.9(7) . 2_765
P1 O7 W2 125.1(7) . 2_765
W4 O7 W2 89.5(4) 2_765 2_765
P1 O7 W6 126.1(8) . 2_765
W4 O7 W6 89.9(4) 2_765 2_765
W2 O7 W6 90.1(4) 2_765 2_765
P1 O8 Ni1 123.7(5) . .
P1 O8 Ni1 123.7(5) . 3_675
Ni1 O8 Ni1 92.2(6) . 3_675
P1 O8 Ni1 123.7(5) . 2_765
Ni1 O8 Ni1 92.2(6) . 2_765
Ni1 O8 Ni1 92.2(6) 3_675 2_765
W6 O9 W6 153.5(10) . 3_675
W4 O11 W2 148.2(8) . 2_765
C15 O13 Ni1 115.9(13) . 2_765
C15 O13 Ni2 121.6(11) . .
Ni1 O13 Ni2 101.8(6) 2_765 .
C15 O13 Ni1 118.0(13) . .
Ni1 O13 Ni1 101.7(6) 2_765 .
Ni2 O13 Ni1 94.0(5) . .
C5 O14 Ni2 127.3(14) . .
C5 O15 Ni1 124.4(13) . .
C12 O16 Ni4 123.3(12) . 2_665
C12 O17 Ni3 127.4(12) . .
W1 O18 Ni4 135.6(7) . 2_665
W1 O18 Ni3 130.1(6) . .
Ni4 O18 Ni3 92.6(5) 2_665 .
W5 O20 W1 127.0(7) 2_665 .
W1 O21 W3 147.1(8) . .
W3 O22 Ni4 130.4(7) . .
W3 O22 Ni3 130.8(6) . .
Ni4 O22 Ni3 94.2(5) . .
P2 O23 W3 127.0(7) . .
P2 O23 W1 124.4(7) . 3_565
W3 O23 W1 90.0(4) . 3_565
P2 O23 W5 125.2(8) . .
W3 O23 W5 89.9(4) . .
W1 O23 W5 88.8(4) 3_565 .
P2 O24 Ni4 124.4(4) . .
P2 O24 Ni4 124.4(4) . 3_565
Ni4 O24 Ni4 91.2(6) . 3_565
P2 O24 Ni4 124.4(4) . 2_665
Ni4 O24 Ni4 91.2(6) . 2_665
Ni4 O24 Ni4 91.2(6) 3_565 2_665
W5 O25 W3 125.9(7) . .
W5 O26 W5 153.3(8) 2_665 .
C17 O28 Ni4 114.6(19) . 3_565
C17 O28 Ni3 122.0(14) . 3_565
Ni4 O28 Ni3 102.6(6) 3_565 3_565
C17 O28 Ni4 118.7(18) . .
Ni4 O28 Ni4 101.4(6) 3_565 .
Ni3 O28 Ni4 93.8(5) 3_565 .
W3 O29 W1 125.2(7) . 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O13 1.997(13) 3_675
Ni1 O1 2.004(13) .
Ni1 O15 2.009(13) .
Ni1 O13 2.040(12) .
Ni1 O2 2.065(13) .
Ni1 O8 2.172(12) .
Ni1 Ni2 2.959(3) .
Ni2 O13 2.007(13) .
Ni2 O14 2.060(15) .
Ni2 N2 2.07(2) .
Ni2 N1 2.069(18) .
Ni2 O1 2.085(13) .
Ni2 O2 2.158(13) 2_765
Ni3 O28 2.011(13) 2_665
Ni3 O17 2.060(14) .
Ni3 N4 2.073(17) .
Ni3 O18 2.075(12) .
Ni3 N3 2.081(19) .
Ni3 O22 2.210(12) .
Ni3 Ni4 2.954(3) 2_665
Ni4 O28 1.998(13) 2_665
Ni4 O16 2.001(13) 3_565
Ni4 O18 2.012(13) 3_565
Ni4 O28 2.034(13) .
Ni4 O22 2.059(12) .
Ni4 O24 2.183(11) .
Ni5 O1W 2.05(3) .
Ni5 O2W 2.11(3) .
Ni5 N6 2.11(3) .
Ni5 N5 2.12(4) .
Ni5 O3W 2.17(3) .
Ni5 O4W 2.17(4) .
P1 O8 1.55(2) .
P1 O7 1.554(12) .
P1 O7 1.554(12) 2_765
P1 O7 1.554(12) 3_675
P2 O24 1.52(2) .
P2 O23 1.545(12) 3_565
P2 O23 1.545(13) 2_665
P2 O23 1.546(12) .
W1 O19 1.713(13) .
W1 O18 1.830(12) .
W1 O21 1.895(14) .
W1 O29 1.938(15) 2_665
W1 O20 1.948(13) .
W1 O23 2.423(12) 2_665
W2 O3 1.704(14) .
W2 O2 1.822(14) .
W2 O4 1.909(13) .
W2 O11 1.918(13) 3_675
W2 O5 1.989(15) .
W2 O7 2.433(12) 3_675
W3 O30 1.712(14) .
W3 O22 1.826(12) .
W3 O29 1.917(14) .
W3 O21 1.938(13) .
W3 O25 1.997(14) .
W3 O23 2.417(13) .
W4 O12 1.731(13) .
W4 O1 1.825(13) .
W4 O11 1.917(14) .
W4 O4 1.933(13) .
W4 O6 1.954(15) .
W4 O7 2.421(12) 3_675
W5 O27 1.734(15) .
W5 O20 1.898(13) 3_565
W5 O25 1.900(14) .
W5 O26 1.905(14) 3_565
W5 O26 1.914(15) .
W5 O23 2.495(14) .
W6 O10 1.70(2) .
W6 O5 1.886(16) .
W6 O9 1.888(17) .
W6 O6 1.916(16) .
W6 O9 1.934(16) 2_765
W6 O7 2.458(14) 3_675
C1 N1 1.473(10) .
C1 C2 1.514(10) .
C2 N2 1.473(10) .
C3 N3 1.470(10) .
C3 C4 1.518(10) .
C4 N4 1.474(10) .
C5 O15 1.23(2) .
C5 O14 1.29(2) .
C5 C6 1.48(3) .
C6 C7 1.37(3) .
C6 C11 1.39(3) .
C7 C8 1.39(3) .
C7 H7 0.9300 .
C8 C9 1.36(3) .
C8 C12 1.50(3) .
C9 C10 1.41(3) .
C9 H9 0.9300 .
C10 C11 1.38(3) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 O16 1.25(2) .
C12 O17 1.26(2) .
C13 N5 1.471(10) .
C13 C14 1.521(10) .
C14 N6 1.476(10) .
C15 O13 1.39(3) .
C15 C16 1.522(10) .
C16 N7 1.471(10) .
C17 O28 1.36(4) .
C17 C18 1.521(10) .
C18 N8 1.471(10) .
