#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:58:05 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180204 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/98/7109873.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_7109873
loop_
_publ_author_name
'Dao-Peng Zhang'
'Li-Fang Zhang'
'Guo-Ling Li'
'Zhong-Hai Ni'
_publ_section_title
;
 Water-controlled synthesis and single-crystal structural transformations
 of a cyanide-bridged W(IV)-Ni(II) molecular wheel complex and 3D networks
;
_journal_name_full               Chem.Commun.
_journal_page_first              9582
_journal_paper_doi               10.1039/c3cc46063k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C228 H352 N96 Ni12 O42 W6'
_chemical_formula_weight         6917.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   33.5208(19)
_cell_length_b                   33.5208(19)
_cell_length_c                   24.994(3)
_cell_measurement_reflns_used    2871
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.861
_cell_measurement_theta_min      2.761
_cell_volume                     24322(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40039
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    2.868
_exptl_absorpt_correction_T_max  0.7068
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             10524
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9484
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0514P)²+88.1983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7298
_reflns_number_total             9484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46063k.txt
_cod_data_source_block           1
_cod_original_cell_volume        24322(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7109873
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.955967(7) 0.198497(8) 0.363537(8) 0.03193(9) Uani 1 1 d .
Ni1 Ni 0.94212(2) 0.28260(3) 0.19027(3) 0.03948(19) Uani 1 1 d .
Ni2 Ni 0.86979(3) 0.11547(2) 0.53646(3) 0.03913(18) Uani 1 1 d .
O1 O 0.95028(15) 0.33314(14) 0.12802(16) 0.0509(11) Uani 1 1 d .
H1O1 H 0.9658 0.3445 0.0995 0.040(17) Uiso 1 1 d R
H2O1 H 0.9265 0.3358 0.1260 0.05(2) Uiso 1 1 d R
O2 O 0.86849(19) 0.30950(18) 0.0758(2) 0.0868(18) Uani 1 1 d .
H1O2 H 0.8931 0.3111 0.0872 0.07(2) Uiso 1 1 d R
H2O2 H 0.8556 0.2866 0.0546 0.046(19) Uiso 1 1 d R
O3 O 0.7809(3) 0.2136(4) 0.3885(5) 0.190(5) Uani 1 1 d .
H103 H 0.7692 0.1893 0.4035 0.228 Uiso 1 1 d R
H203 H 0.7952 0.2396 0.4030 0.228 Uiso 1 1 d R
O4 O 0.9925(4) 0.1444(4) 0.8021(5) 0.213(5) Uani 1 1 d .
H204 H 0.9757 0.1513 0.8298 0.255 Uiso 1 1 d R
H104 H 1.0255 0.1583 0.8064 0.255 Uiso 1 1 d R
O5 O 0.9308(6) 0.0639(6) 0.2569(7) 0.321(10) Uani 1 1 d .
H1O5 H 0.9064 0.0646 0.2634 0.385 Uiso 1 1 d R
H2O5 H 0.9521 0.0838 0.2769 0.385 Uiso 1 1 d R
O6 O 0.0000 0.0000 0.073(5) 1.13(19) Uani 1 3 d SD
H106 H 0.0105 0.0292 0.0452 1.359 Uiso 1 1 d RD
H206 H 0.0000 0.0000 0.1065 1.359 Uiso 1 3 d SRD
O7 O 0.0000 0.0000 0.5000 0.29(2) Uani 1 6 d S
H1O7 H 0.0270 0.0219 0.5066 0.343 Uiso 0.33 1 d PR
O8 O 0.9699(6) 0.0269(5) 0.3830(13) 0.48(2) Uani 1 1 d .
H208 H 0.9893 0.0318 0.4090 0.579 Uiso 1 1 d R
H108 H 0.9438 0.0207 0.3915 0.579 Uiso 1 1 d R
O9 O 0.0551(8) 0.1504(7) 0.2067(9) 0.193(8) Uani 0.50 1 d PU
H109 H 0.0553 0.1716 0.1730 0.232 Uiso 0.50 1 d PR
H209 H 0.0724 0.1579 0.2307 0.232 Uiso 0.50 1 d PR
N1 N 0.93808(17) 0.24084(18) 0.25267(19) 0.0461(12) Uani 1 1 d .
N2 N 0.92211(16) 0.17013(16) 0.48870(19) 0.0416(11) Uani 1 1 d .
N3 N 0.81930(18) 0.05783(17) 0.5787(2) 0.0492(13) Uani 1 1 d .
N4 N 0.86380(19) 0.2096(2) 0.3840(2) 0.0570(14) Uani 1 1 d .
N5 N 0.9985(2) 0.30849(19) 0.3935(2) 0.0557(14) Uani 1 1 d .
N6 N 1.0257(3) 0.2007(3) 0.2690(3) 0.089(2) Uani 1 1 d .
N7 N 0.8702(2) 0.10309(19) 0.3128(2) 0.0619(15) Uani 1 1 d .
N8 N 0.9646(2) 0.1062(2) 0.3878(3) 0.0680(17) Uani 1 1 d .
N9 N 0.91232(17) 0.23502(16) 0.13585(19) 0.0431(12) Uani 1 1 d .
N10 N 0.99727(16) 0.28065(17) 0.15917(19) 0.0442(12) Uani 1 1 d .
N11 N 0.97412(19) 0.33862(18) 0.2370(2) 0.0531(13) Uani 1 1 d .
H11 H 0.9796 0.3625 0.2152 0.064 Uiso 1 1 d R
N12 N 0.87454(18) 0.26603(19) 0.1996(2) 0.0525(14) Uani 1 1 d .
N13 N 0.88131(17) 0.15954(16) 0.59393(19) 0.0444(12) Uani 1 1 d .
N14 N 0.91769(17) 0.10906(17) 0.5802(2) 0.0481(13) Uani 1 1 d .
N15 N 0.86116(18) 0.07374(17) 0.4737(2) 0.0528(14) Uani 1 1 d .
H15 H 0.8819 0.0919 0.4485 0.063 Uiso 1 1 d R
N16 N 0.82419(17) 0.13740(17) 0.5181(2) 0.0464(12) Uani 1 1 d .
C1 C 0.94412(19) 0.2260(2) 0.2911(2) 0.0379(13) Uani 1 1 d .
C2 C 0.93569(18) 0.18192(18) 0.4460(2) 0.0346(12) Uani 1 1 d .
C3 C 0.7980(2) 0.0230(2) 0.5990(2) 0.0393(13) Uani 1 1 d .
C4 C 0.8955(2) 0.2055(2) 0.3773(2) 0.0403(13) Uani 1 1 d .
C5 C 0.9835(2) 0.2707(2) 0.3823(2) 0.0395(13) Uani 1 1 d .
C6 C 1.0015(2) 0.1998(2) 0.3012(3) 0.0540(16) Uani 1 1 d .
C7 C 0.8998(2) 0.1369(2) 0.3296(2) 0.0425(14) Uani 1 1 d .
C8 C 0.9625(2) 0.1386(2) 0.3804(2) 0.0447(14) Uani 1 1 d .
C9 C 0.9389(2) 0.2254(2) 0.1055(2) 0.0516(16) Uani 1 1 d .
C10 C 0.9196(3) 0.1953(2) 0.0627(3) 0.064(2) Uani 1 1 d .
H10 H 0.9376 0.1882 0.0408 0.077 Uiso 1 1 d R
C11 C 0.8737(3) 0.1766(3) 0.0539(3) 0.075(2) Uani 1 1 d .
H11A H 0.8603 0.1562 0.0255 0.090 Uiso 1 1 d R
C12 C 0.8465(3) 0.1867(2) 0.0855(3) 0.071(2) Uani 1 1 d .
H12 H 0.8150 0.1733 0.0792 0.085 Uiso 1 1 d R
C13 C 0.8678(2) 0.2183(2) 0.1282(2) 0.0497(16) Uani 1 1 d .
C14 C 0.8465(2) 0.2362(2) 0.1666(3) 0.0522(17) Uani 1 1 d .
C15 C 0.7957(2) 0.2185(3) 0.1627(3) 0.073(2) Uani 1 1 d .
H15A H 0.7830 0.2147 0.1980 0.110 Uiso 1 1 d R
H15B H 0.7811 0.1893 0.1446 0.110 Uiso 1 1 d R
H15C H 0.7905 0.2400 0.1431 0.110 Uiso 1 1 d R
C16 C 0.8617(3) 0.2869(3) 0.2421(3) 0.071(2) Uani 1 1 d .
H16A H 0.8524 0.2670 0.2732 0.085 Uiso 1 1 d R
H16B H 0.8354 0.2894 0.2306 0.085 Uiso 1 1 d R
C17 C 0.8999(3) 0.3338(3) 0.2578(3) 0.078(2) Uani 1 1 d .
H17A H 0.9075 0.3535 0.2266 0.093 Uiso 1 1 d R
H17B H 0.8876 0.3459 0.2844 0.093 Uiso 1 1 d R
C18 C 0.9437(3) 0.3392(3) 0.2793(3) 0.066(2) Uani 1 1 d .
H18A H 0.9598 0.3680 0.2987 0.079 Uiso 1 1 d R
H18B H 0.9366 0.3144 0.3044 0.079 Uiso 1 1 d R
C19 C 1.0200(2) 0.3482(2) 0.2539(3) 0.0596(18) Uani 1 1 d .
H19A H 1.0168 0.3237 0.2774 0.072 Uiso 1 1 d R
H19B H 1.0348 0.3767 0.2740 0.072 Uiso 1 1 d R
C20 C 1.0503(2) 0.3520(2) 0.2071(3) 0.0573(18) Uani 1 1 d .
H20A H 1.0821 0.3694 0.2189 0.069 Uiso 1 1 d R
H20B H 1.0463 0.3702 0.1796 0.069 Uiso 1 1 d R
C21 C 1.0433(2) 0.3081(2) 0.1811(3) 0.0552(17) Uani 1 1 d .
H21A H 1.0657 0.3158 0.1527 0.066 Uiso 1 1 d R
H21B H 1.0486 0.2899 0.2075 0.066 Uiso 1 1 d R
C22 C 0.9880(2) 0.2507(2) 0.1225(3) 0.0505(16) Uani 1 1 d .
C23 C 1.0210(3) 0.2401(3) 0.0964(4) 0.084(3) Uani 1 1 d .
H23A H 1.0438 0.2668 0.0776 0.126 Uiso 1 1 d R
H23B H 1.0050 0.2152 0.0716 0.126 Uiso 1 1 d R
H23C H 1.0359 0.2313 0.1230 0.126 Uiso 1 1 d R
C24 C 0.9145(2) 0.1672(2) 0.6291(2) 0.0511(16) Uani 1 1 d .
C25 C 0.9268(3) 0.2014(2) 0.6663(3) 0.067(2) Uani 1 1 d .
H25 H 0.9499 0.2076 0.6910 0.080 Uiso 1 1 d R
C26 C 0.9047(3) 0.2264(3) 0.6667(3) 0.067(2) Uani 1 1 d .
H26 H 0.9126 0.2492 0.6924 0.081 Uiso 1 1 d R
C27 C 0.8713(3) 0.2186(2) 0.6301(3) 0.0607(19) Uani 1 1 d .
H27 H 0.8566 0.2359 0.6305 0.073 Uiso 1 1 d R
C28 C 0.8599(2) 0.1842(2) 0.5922(2) 0.0484(15) Uani 1 1 d .
C29 C 0.8258(2) 0.1688(2) 0.5479(3) 0.0498(16) Uani 1 1 d .
C30 C 0.7962(3) 0.1900(3) 0.5423(3) 0.081(2) Uani 1 1 d .
H30A H 0.8014 0.2047 0.5080 0.122 Uiso 1 1 d R
H30B H 0.8036 0.2125 0.5701 0.122 Uiso 1 1 d R
H30C H 0.7644 0.1666 0.5453 0.122 Uiso 1 1 d R
C31 C 0.7908(2) 0.1150(3) 0.4750(3) 0.066(2) Uani 1 1 d .
H31A H 0.7848 0.1376 0.4582 0.079 Uiso 1 1 d R
H31B H 0.7621 0.0912 0.4903 0.079 Uiso 1 1 d R
C32 C 0.8062(2) 0.0937(2) 0.4328(3) 0.0633(19) Uani 1 1 d .
H32A H 0.8343 0.1181 0.4170 0.076 Uiso 1 1 d R
H32B H 0.7830 0.0818 0.4049 0.076 Uiso 1 1 d R
C33 C 0.8153(2) 0.0553(2) 0.4489(3) 0.0639(19) Uani 1 1 d .
H33A H 0.7918 0.0350 0.4740 0.077 Uiso 1 1 d R
H33B H 0.8133 0.0374 0.4175 0.077 Uiso 1 1 d R
C34 C 0.8730(2) 0.0378(2) 0.4871(3) 0.0605(19) Uani 1 1 d .
H34A H 0.8714 0.0207 0.4550 0.073 Uiso 1 1 d R
H34B H 0.8507 0.0163 0.5125 0.073 Uiso 1 1 d R
C35 C 0.9207(2) 0.0584(2) 0.5108(3) 0.0632(19) Uani 1 1 d .
H35A H 0.9409 0.0855 0.4900 0.076 Uiso 1 1 d R
H35B H 0.9312 0.0364 0.5057 0.076 Uiso 1 1 d R
C36 C 0.9279(2) 0.0723(2) 0.5691(3) 0.0621(19) Uani 1 1 d .
H36A H 0.9081 0.0457 0.5910 0.075 Uiso 1 1 d R
H36B H 0.9595 0.0825 0.5789 0.075 Uiso 1 1 d R
C37 C 0.9323(2) 0.1342(2) 0.6219(3) 0.0562(17) Uani 1 1 d .
C38 C 0.9633(3) 0.1323(3) 0.6634(4) 0.097(3) Uani 1 1 d .
H38A H 0.9742 0.1121 0.6516 0.146 Uiso 1 1 d R
H38B H 0.9466 0.1208 0.6963 0.146 Uiso 1 1 d R
H38C H 0.9891 0.1626 0.6691 0.146 Uiso 1 1 d R
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'
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
C7 W1 C2 96.7(2) . .
C7 W1 C1 79.6(2) . .
C2 W1 C1 144.2(2) . .
C7 W1 C6 90.4(2) . .
C2 W1 C6 145.3(2) . .
C1 W1 C6 70.5(2) . .
C7 W1 C8 68.6(2) . .
C2 W1 C8 74.9(2) . .
C1 W1 C8 133.3(2) . .
C6 W1 C8 76.3(2) . .
C7 W1 C5 146.6(2) . .
C2 W1 C5 89.1(2) . .
C1 W1 C5 76.7(2) . .
C6 W1 C5 103.3(2) . .
C8 W1 C5 144.0(2) . .
C7 W1 C3 142.4(2) . 11_666
C2 W1 C3 79.7(2) . 11_666
C1 W1 C3 124.1(2) . 11_666
C6 W1 C3 74.2(2) . 11_666
C8 W1 C3 74.4(2) . 11_666
C5 W1 C3 71.0(2) . 11_666
C7 W1 C4 75.5(2) . .
C2 W1 C4 71.7(2) . .
C1 W1 C4 72.9(2) . .
C6 W1 C4 142.6(2) . .
C8 W1 C4 126.8(2) . .
C5 W1 C4 75.2(2) . .
C3 W1 C4 135.7(2) 11_666 .
N9 Ni1 N11 170.9(2) . .
N9 Ni1 N10 79.0(2) . .
N11 Ni1 N10 100.5(2) . .
N9 Ni1 N1 98.1(2) . .
N11 Ni1 N1 91.0(2) . .
N10 Ni1 N1 91.1(2) . .
N9 Ni1 N12 79.3(2) . .
N11 Ni1 N12 100.8(2) . .
N10 Ni1 N12 158.3(2) . .
N1 Ni1 N12 92.4(2) . .
N9 Ni1 O1 87.26(17) . .
N11 Ni1 O1 83.64(19) . .
N10 Ni1 O1 89.39(18) . .
N1 Ni1 O1 174.66(19) . .
N12 Ni1 O1 89.11(18) . .
N13 Ni2 N15 175.9(2) . .
N13 Ni2 N14 79.5(2) . .
N15 Ni2 N14 101.0(2) . .
N13 Ni2 N16 78.2(2) . .
N15 Ni2 N16 101.5(2) . .
N14 Ni2 N16 157.5(2) . .
N13 Ni2 N3 95.1(2) . .
N15 Ni2 N3 89.0(2) . .
N14 Ni2 N3 87.1(2) . .
N16 Ni2 N3 92.3(2) . .
N13 Ni2 N2 89.74(19) . .
N15 Ni2 N2 86.13(19) . .
N14 Ni2 N2 92.14(19) . .
N16 Ni2 N2 90.39(19) . .
N3 Ni2 N2 174.9(2) . .
Ni1 O1 H1O1 138.0 . .
Ni1 O1 H2O1 111.1 . .
H1O1 O1 H2O1 107.6 . .
H1O2 O2 H2O2 107.6 . .
H103 O3 H203 126.4 . .
H204 O4 H104 117.1 . .
H1O5 O5 H2O5 107.9 . .
H206 O6 H106 129.1 . .
H206 O6 H106 129.1 . .
H106 O6 H106 0.0 . .
H206 O6 H206 0.0 . .
H106 O6 H206 129.1 . .
H106 O6 H206 129.1 . .
H208 O8 H108 117.1 . .
H109 O9 H209 128.0 . .
C1 N1 Ni1 165.2(5) . .
C2 N2 Ni2 145.1(4) . .
C3 N3 Ni2 165.4(5) . .
C13 N9 C9 124.6(6) . .
C13 N9 Ni1 117.2(5) . .
C9 N9 Ni1 117.8(4) . .
C22 N10 C21 122.1(6) . .
C22 N10 Ni1 115.5(4) . .
C21 N10 Ni1 122.0(4) . .
C19 N11 C18 116.5(5) . .
C19 N11 Ni1 112.5(4) . .
C18 N11 Ni1 112.3(4) . .
C19 N11 H11 104.7 . .
C18 N11 H11 104.7 . .
Ni1 N11 H11 104.7 . .
C14 N12 C16 125.0(6) . .
C14 N12 Ni1 114.7(5) . .
C16 N12 Ni1 120.3(5) . .
C24 N13 C28 123.6(6) . .
C24 N13 Ni2 117.3(4) . .
C28 N13 Ni2 118.6(4) . .
C37 N14 C36 122.6(6) . .
C37 N14 Ni2 115.5(5) . .
C36 N14 Ni2 121.1(4) . .
C33 N15 C34 113.6(5) . .
C33 N15 Ni2 111.9(4) . .
C34 N15 Ni2 112.4(4) . .
C33 N15 H15 106.0 . .
C34 N15 H15 106.0 . .
Ni2 N15 H15 106.0 . .
C29 N16 C31 124.2(6) . .
C29 N16 Ni2 115.9(4) . .
C31 N16 Ni2 119.8(4) . .
N1 C1 W1 179.6(7) . .
N2 C2 W1 174.9(5) . .
N3 C3 W1 178.9(5) . 12_546
N4 C4 W1 179.0(6) . .
N5 C5 W1 178.0(5) . .
N6 C6 W1 179.2(6) . .
N7 C7 W1 177.3(5) . .
N8 C8 W1 177.1(6) . .
N9 C9 C10 119.4(7) . .
N9 C9 C22 112.6(6) . .
C10 C9 C22 128.0(7) . .
C11 C10 C9 118.0(8) . .
C11 C10 H10 121.0 . .
C9 C10 H10 121.0 . .
C10 C11 C12 122.1(7) . .
C10 C11 H11A 119.0 . .
C12 C11 H11A 119.0 . .
C11 C12 C13 118.0(7) . .
C11 C12 H12 121.0 . .
C13 C12 H12 121.0 . .
N9 C13 C12 117.8(7) . .
N9 C13 C14 113.8(6) . .
C12 C13 C14 128.5(7) . .
N12 C14 C13 114.9(6) . .
N12 C14 C15 126.6(7) . .
C13 C14 C15 118.5(6) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N12 C16 C17 113.2(6) . .
N12 C16 H16A 108.9 . .
C17 C16 H16A 108.9 . .
N12 C16 H16B 108.9 . .
C17 C16 H16B 108.9 . .
H16A C16 H16B 107.8 . .
C18 C17 C16 119.6(7) . .
C18 C17 H17A 107.4 . .
C16 C17 H17A 107.4 . .
C18 C17 H17B 107.4 . .
C16 C17 H17B 107.4 . .
H17A C17 H17B 106.9 . .
N11 C18 C17 112.7(6) . .
N11 C18 H18A 109.0 . .
C17 C18 H18A 109.0 . .
N11 C18 H18B 109.0 . .
C17 C18 H18B 109.0 . .
H18A C18 H18B 107.8 . .
N11 C19 C20 112.4(5) . .
N11 C19 H19A 109.1 . .
C20 C19 H19A 109.1 . .
N11 C19 H19B 109.1 . .
C20 C19 H19B 109.1 . .
H19A C19 H19B 107.9 . .
C19 C20 C21 118.5(6) . .
C19 C20 H20A 107.7 . .
C21 C20 H20A 107.7 . .
C19 C20 H20B 107.7 . .
C21 C20 H20B 107.7 . .
H20A C20 H20B 107.1 . .
N10 C21 C20 112.0(5) . .
N10 C21 H21A 109.2 . .
C20 C21 H21A 109.2 . .
N10 C21 H21B 109.2 . .
C20 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
N10 C22 C23 126.2(7) . .
N10 C22 C9 114.7(6) . .
C23 C22 C9 119.1(6) . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N13 C24 C25 118.7(7) . .
N13 C24 C37 112.2(5) . .
C25 C24 C37 129.2(7) . .
C26 C25 C24 119.3(7) . .
C26 C25 H25 120.3 . .
C24 C25 H25 120.3 . .
C27 C26 C25 121.3(7) . .
C27 C26 H26 119.3 . .
C25 C26 H26 119.3 . .
C26 C27 C28 118.4(7) . .
C26 C27 H27 120.8 . .
C28 C27 H27 120.8 . .
N13 C28 C27 118.7(7) . .
N13 C28 C29 111.6(5) . .
C27 C28 C29 129.7(7) . .
N16 C29 C28 115.4(6) . .
N16 C29 C30 125.5(7) . .
C28 C29 C30 119.1(6) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
N16 C31 C32 113.9(6) . .
N16 C31 H31A 108.8 . .
C32 C31 H31A 108.8 . .
N16 C31 H31B 108.8 . .
C32 C31 H31B 108.8 . .
H31A C31 H31B 107.7 . .
C31 C32 C33 118.7(6) . .
C31 C32 H32A 107.6 . .
C33 C32 H32A 107.6 . .
C31 C32 H32B 107.6 . .
C33 C32 H32B 107.6 . .
H32A C32 H32B 107.1 . .
N15 C33 C32 111.4(5) . .
N15 C33 H33A 109.4 . .
C32 C33 H33A 109.4 . .
N15 C33 H33B 109.4 . .
C32 C33 H33B 109.4 . .
H33A C33 H33B 108.0 . .
N15 C34 C35 111.6(5) . .
N15 C34 H34A 109.3 . .
C35 C34 H34A 109.3 . .
N15 C34 H34B 109.3 . .
C35 C34 H34B 109.3 . .
H34A C34 H34B 108.0 . .
C34 C35 C36 119.2(6) . .
C34 C35 H35A 107.5 . .
C36 C35 H35A 107.5 . .
C34 C35 H35B 107.5 . .
C36 C35 H35B 107.5 . .
H35A C35 H35B 107.0 . .
N14 C36 C35 112.0(6) . .
N14 C36 H36A 109.2 . .
C35 C36 H36A 109.2 . .
N14 C36 H36B 109.2 . .
C35 C36 H36B 109.2 . .
H36A C36 H36B 107.9 . .
N14 C37 C38 125.8(7) . .
N14 C37 C24 114.9(6) . .
C38 C37 C24 119.2(7) . .
C37 C38 H38A 109.5 . .
C37 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C37 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C7 2.154(6) .
W1 C2 2.155(6) .
W1 C1 2.157(6) .
W1 C6 2.166(7) .
W1 C8 2.166(6) .
W1 C5 2.168(6) .
W1 C3 2.173(6) 11_666
W1 C4 2.181(6) .
Ni1 N9 1.949(5) .
Ni1 N11 2.006(5) .
Ni1 N10 2.037(5) .
Ni1 N1 2.054(5) .
Ni1 N12 2.058(5) .
Ni1 O1 2.214(4) .
Ni2 N13 1.955(5) .
Ni2 N15 2.024(5) .
Ni2 N14 2.040(5) .
Ni2 N16 2.052(5) .
Ni2 N3 2.108(5) .
Ni2 N2 2.155(5) .
O1 H1O1 0.8529 .
O1 H2O1 0.8480 .
O2 H1O2 0.8491 .
O2 H2O2 0.8518 .
O3 H103 0.7976 .
O3 H203 0.8390 .
O4 H204 0.9926 .
O4 H104 0.9668 .
O5 H1O5 0.8452 .
O5 H2O5 0.8523 .
O6 H206 0.8327 .
O6 H106 1.1000 .
O6 H106 1.1000 .
O6 H206 0.8327 .
O7 H1O7 0.8501 .
O8 H208 0.8747 .
O8 H108 0.8212 .
O9 H109 1.0991 .
O9 H209 0.7831 .
N1 C1 1.145(7) .
N2 C2 1.149(7) .
N3 C3 1.138(7) .
N4 C4 1.149(7) .
N5 C5 1.139(7) .
N6 C6 1.133(8) .
N7 C7 1.149(7) .
N8 C8 1.139(8) .
N9 C13 1.320(8) .
N9 C9 1.327(8) .
N10 C22 1.278(8) .
N10 C21 1.453(7) .
N11 C19 1.469(8) .
N11 C18 1.476(9) .
N11 H11 0.9100 .
N12 C14 1.275(8) .
N12 C16 1.451(9) .
N13 C24 1.337(8) .
N13 C28 1.339(8) .
N14 C37 1.274(8) .
N14 C36 1.461(8) .
N15 C33 1.477(8) .
N15 C34 1.486(8) .
N15 H15 0.9100 .
N16 C29 1.271(8) .
N16 C31 1.462(8) .
C3 W1 2.173(6) 12_546
C9 C10 1.388(9) .
C9 C22 1.488(9) .
C10 C11 1.358(11) .
C10 H10 0.9300 .
C11 C12 1.372(12) .
C11 H11A 0.9300 .
C12 C13 1.419(10) .
C12 H12 0.9300 .
C13 C14 1.488(10) .
C14 C15 1.501(9) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C17 1.499(11) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 C18 1.488(11) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.512(10) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 C21 1.518(9) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.474(10) .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.371(9) .
C24 C37 1.507(10) .
C25 C26 1.368(11) .
C25 H25 0.9300 .
C26 C27 1.365(10) .
C26 H26 0.9300 .
C27 C28 1.390(9) .
C27 H27 0.9300 .
C28 C29 1.487(9) .
C29 C30 1.488(10) .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 C32 1.503(10) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 C33 1.516(10) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 C35 1.509(10) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C35 C36 1.511(10) .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
C37 C38 1.495(10) .
C38 H38A 0.9600 .
C38 H38B 0.9600 .
C38 H38C 0.9600 .
