#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/65/2236545.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2236545
loop_
_publ_author_name
'Ou, Guang-Chuan'
'Yuan, Xian-You'
'Li, Zhi-Zhang'
_publ_section_title
;
 catena-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ⁴N)nickel(II)]-μ-oxido-[dioxidotungstate(VI)]-μ-oxido]
 tetrahydrate]
;
_journal_coeditor_code           PV2574
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1173
_journal_paper_doi               10.1107/S1600536812034538
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni W O4 (C16 H36 N4)], 4H2 O'
_chemical_formula_moiety         'C16 H36 N4 Ni O4 W, 4(H2 O)'
_chemical_formula_sum            'C16 H44 N4 Ni O8 W'
_chemical_formula_weight         663.11
_chemical_name_systematic
;
catena-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-
tetraazacyclotetradecane-κ⁴N)nickel(II)]-μ-oxido-
[dioxidotungstate(VI)]-μ-oxido] tetrahydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                107.163(2)
_cell_angle_beta                 102.529(3)
_cell_angle_gamma                104.984(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8402(14)
_cell_length_b                   11.7653(18)
_cell_length_c                   13.931(2)
_cell_measurement_reflns_used    3766
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.93
_cell_volume                     1268.1(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7631
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.318
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.2894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0382
_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)+(0.0498P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                4330
_reflns_number_total             5397
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2574.cif
_cod_data_source_block           I
_cod_database_code               2236545
_cod_database_fobs_code          2236545
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
W W1 0.86432(3) 0.90496(2) 0.70182(2) 0.01423(9) Uani d . 1 1
O O4 0.9085(5) 0.9844(4) 0.8399(3) 0.0187(9) Uani d . 1 1
O O1 0.9900(5) 0.9988(4) 0.6505(3) 0.0201(10) Uani d . 1 1
O O3 0.6535(5) 0.8719(4) 0.6342(4) 0.0231(10) Uani d . 1 1
O O2 0.9049(6) 0.7611(4) 0.6806(4) 0.0258(11) Uani d . 1 1
Ni Ni1 1.0000 1.0000 1.0000 0.0130(2) Uani d S 1 2
Ni Ni2 1.0000 1.0000 0.5000 0.0139(2) Uani d S 1 2
N N1 0.9427(7) 1.1622(5) 1.0653(4) 0.0170(11) Uani d . 1 1
H H1C 0.9860 1.1842 1.1380 0.020 Uiso calc R 1 1
N N2 1.2351(6) 1.1000(5) 1.0097(4) 0.0158(11) Uani d . 1 1
H H2C 1.3028 1.1227 1.0785 0.019 Uiso calc R 1 1
N N4 0.7426(6) 0.9212(5) 0.4386(4) 0.0183(11) Uani d . 1 1
H H4D 0.7043 0.9048 0.4920 0.022 Uiso calc R 1 1
N N3 1.0343(7) 0.8257(5) 0.4733(4) 0.0195(12) Uani d . 1 1
H H3A 1.0258 0.8088 0.5334 0.023 Uiso calc R 1 1
C C6 1.0127(9) 1.2828(6) 1.0490(5) 0.0219(15) Uani d . 1 1
C C11 0.6783(9) 0.7997(7) 0.3458(6) 0.0298(17) Uani d . 1 1
H H11 0.7226 0.8148 0.2887 0.036 Uiso calc R 1 1
C C5 1.1979(9) 1.3084(6) 1.0670(6) 0.0264(16) Uani d . 1 1
H H5A 1.2466 1.3084 1.1380 0.032 Uiso calc R 1 1
H H5B 1.2477 1.3953 1.0694 0.032 Uiso calc R 1 1
C C9 1.2125(8) 0.8541(7) 0.4833(6) 0.0271(16) Uani d . 1 1
H H9A 1.2321 0.8652 0.4188 0.033 Uiso calc R 1 1
H H9B 1.2474 0.7833 0.4922 0.033 Uiso calc R 1 1
C C10 0.6896(9) 1.0242(7) 0.4200(6) 0.0295(17) Uani d . 1 1
H H10A 0.5698 1.0036 0.4095 0.035 Uiso calc R 1 1
H H10B 0.7109 1.0349 0.3558 0.035 Uiso calc R 1 1
C C14 0.9159(9) 0.7086(6) 0.3836(6) 0.0266(16) Uani d . 1 1
C C16 0.9464(10) 0.7001(7) 0.2778(6) 0.0359(19) Uani d . 1 1
H H16A 0.9446 0.7773 0.2649 0.054 Uiso calc R 1 1
H H16B 0.8597 0.6263 0.2204 0.054 Uiso calc R 1 1
H H16C 1.0543 0.6912 0.2805 0.054 Uiso calc R 1 1
C C13 0.7386(9) 0.7023(6) 0.3763(6) 0.0313(18) Uani d . 1 1
H H13A 0.6640 0.6175 0.3245 0.038 Uiso calc R 1 1
H H13B 0.7252 0.7078 0.4461 0.038 Uiso calc R 1 1
C C15 0.9397(11) 0.5905(7) 0.4055(7) 0.041(2) Uani d . 1 1
H H15A 0.8627 0.5129 0.3469 0.061 Uiso calc R 1 1
H H15B 0.9180 0.5911 0.4717 0.061 Uiso calc R 1 1
H H15C 1.0533 0.5934 0.4117 0.061 Uiso calc R 1 1
C C12 0.4873(10) 0.7496(8) 0.3017(7) 0.045(2) Uani d . 1 1
H H12A 0.4416 0.7344 0.3568 0.068 Uiso calc R 1 1
H H12B 0.4495 0.6701 0.2403 0.068 Uiso calc R 1 1
H H12C 0.4499 0.8125 0.2803 0.068 Uiso calc R 1 1
C C3 1.2531(9) 1.2195(6) 0.9881(6) 0.0256(16) Uani d . 1 1
H H3 1.1785 1.1969 0.9150 0.031 Uiso calc R 1 1
C C8 0.9959(10) 1.3946(6) 1.1322(6) 0.0283(16) Uani d . 1 1
H H8A 0.8787 1.3813 1.1227 0.042 Uiso calc R 1 1
H H8B 1.0477 1.4736 1.1233 0.042 Uiso calc R 1 1
H H8C 1.0506 1.4000 1.2034 0.042 Uiso calc R 1 1
C C7 0.9231(9) 1.2735(7) 0.9384(6) 0.0298(17) Uani d . 1 1
H H7A 0.9179 1.1950 0.8854 0.045 Uiso calc R 1 1
H H7B 0.9832 1.3464 0.9246 0.045 Uiso calc R 1 1
H H7C 0.8109 1.2731 0.9343 0.045 Uiso calc R 1 1
C C4 1.4286(10) 1.2865(8) 0.9937(8) 0.051(3) Uani d . 1 1
H H4A 1.5007 1.3220 1.0674 0.077 Uiso calc R 1 1
H H4B 1.4304 1.3550 0.9671 0.077 Uiso calc R 1 1
H H4C 1.4677 1.2257 0.9504 0.077 Uiso calc R 1 1
C C1 0.7623(8) 1.1146(6) 1.0442(5) 0.0213(14) Uani d . 1 1
H H1A 0.7047 1.1009 0.9702 0.026 Uiso calc R 1 1
H H1B 0.7301 1.1780 1.0919 0.026 Uiso calc R 1 1
C C2 1.2872(8) 1.0076(6) 0.9384(5) 0.0188(14) Uani d . 1 1
H H2A 1.4084 1.0407 0.9539 0.023 Uiso calc R 1 1
H H2B 1.2336 0.9936 0.8636 0.023 Uiso calc R 1 1
O O2W 0.3988(7) 0.6388(5) 0.5720(5) 0.0422(14) Uani d D 1 1
H H2WA 0.389(10) 0.589(5) 0.510(3) 0.051 Uiso d D 1 1
H H2WB 0.458(9) 0.714(3) 0.582(5) 0.051 Uiso d D 1 1
O O4W 0.5200(7) 0.9166(6) 0.8089(4) 0.0441(15) Uani d D 1 1
H H4WB 0.461(7) 0.842(3) 0.797(4) 0.053 Uiso d D 1 1
H H4WA 0.564(9) 0.915(6) 0.759(5) 0.053 Uiso d D 1 1
O O1W 0.6501(8) 0.5326(5) 0.6291(5) 0.0447(15) Uani d D 1 1
H H1WA 0.729(5) 0.599(5) 0.639(7) 0.054 Uiso d D 1 1
H H1WB 0.560(4) 0.547(7) 0.617(7) 0.054 Uiso d D 1 1
O O3W 0.2150(7) 0.7401(6) 0.6956(5) 0.0504(17) Uani d D 1 1
H H3WA 0.109(3) 0.714(8) 0.681(5) 0.061 Uiso d D 1 1
H H3WB 0.234(7) 0.706(8) 0.638(3) 0.061 Uiso d D 1 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 W1 O2 . . 108.7(2)
O1 W1 O4 . . 110.9(2)
O2 W1 O4 . . 108.7(2)
O1 W1 O3 . . 108.9(2)
O2 W1 O3 . . 109.7(2)
O4 W1 O3 . . 109.9(2)
W1 O4 Ni1 . . 151.1(2)
W1 O1 Ni2 . . 137.9(2)
N2 Ni1 N2 . 2_777 180.0000(10)
N2 Ni1 N1 . 2_777 85.46(19)
N2 Ni1 N1 2_777 2_777 94.5(2)
N2 Ni1 N1 . . 94.5(2)
N2 Ni1 N1 2_777 . 85.46(19)
N1 Ni1 N1 2_777 . 180.000(3)
N2 Ni1 O4 . . 90.57(18)
N2 Ni1 O4 2_777 . 89.43(18)
N1 Ni1 O4 2_777 . 85.20(18)
N1 Ni1 O4 . . 94.80(18)
N2 Ni1 O4 . 2_777 89.43(18)
N2 Ni1 O4 2_777 2_777 90.57(18)
N1 Ni1 O4 2_777 2_777 94.80(18)
N1 Ni1 O4 . 2_777 85.20(18)
O4 Ni1 O4 . 2_777 180.000(2)
N3 Ni2 N3 2_776 . 180.000(2)
N3 Ni2 N4 2_776 2_776 94.6(2)
N3 Ni2 N4 . 2_776 85.4(2)
N3 Ni2 N4 2_776 . 85.4(2)
N3 Ni2 N4 . . 94.6(2)
N4 Ni2 N4 2_776 . 180.0000(10)
N3 Ni2 O1 2_776 2_776 86.13(19)
N3 Ni2 O1 . 2_776 93.87(19)
N4 Ni2 O1 2_776 2_776 90.23(18)
N4 Ni2 O1 . 2_776 89.77(18)
N3 Ni2 O1 2_776 . 93.87(19)
N3 Ni2 O1 . . 86.13(19)
N4 Ni2 O1 2_776 . 89.77(18)
N4 Ni2 O1 . . 90.23(18)
O1 Ni2 O1 2_776 . 180.000(2)
C1 N1 C6 . . 116.7(5)
C1 N1 Ni1 . . 104.6(4)
C6 N1 Ni1 . . 122.1(4)
C1 N1 H1C . . 103.7
C6 N1 H1C . . 103.7
Ni1 N1 H1C . . 103.7
C2 N2 C3 . . 113.8(5)
C2 N2 Ni1 . . 105.4(4)
C3 N2 Ni1 . . 115.3(4)
C2 N2 H2C . . 107.3
C3 N2 H2C . . 107.3
Ni1 N2 H2C . . 107.3
C10 N4 C11 . . 115.2(5)
C10 N4 Ni2 . . 104.7(4)
C11 N4 Ni2 . . 114.5(4)
C10 N4 H4D . . 107.3
C11 N4 H4D . . 107.3
Ni2 N4 H4D . . 107.3
C9 N3 C14 . . 116.5(5)
C9 N3 Ni2 . . 104.7(4)
C14 N3 Ni2 . . 121.3(4)
C9 N3 H3A . . 104.1
C14 N3 H3A . . 104.1
Ni2 N3 H3A . . 104.1
N1 C6 C7 . . 110.9(6)
N1 C6 C5 . . 107.7(5)
C7 C6 C5 . . 111.8(6)
N1 C6 C8 . . 110.2(5)
C7 C6 C8 . . 108.9(5)
C5 C6 C8 . . 107.4(6)
N4 C11 C13 . . 109.7(6)
N4 C11 C12 . . 111.8(6)
C13 C11 C12 . . 110.3(6)
N4 C11 H11 . . 108.3
C13 C11 H11 . . 108.3
C12 C11 H11 . . 108.3
C6 C5 C3 . . 119.3(6)
C6 C5 H5A . . 107.5
C3 C5 H5A . . 107.5
C6 C5 H5B . . 107.5
C3 C5 H5B . . 107.5
H5A C5 H5B . . 107.0
N3 C9 C10 . 2_776 107.7(5)
N3 C9 H9A . . 110.2
C10 C9 H9A 2_776 . 110.2
N3 C9 H9B . . 110.2
C10 C9 H9B 2_776 . 110.2
H9A C9 H9B . . 108.5
N4 C10 C9 . 2_776 108.0(6)
N4 C10 H10A . . 110.1
C9 C10 H10A 2_776 . 110.1
N4 C10 H10B . . 110.1
C9 C10 H10B 2_776 . 110.1
H10A C10 H10B . . 108.4
N3 C14 C13 . . 109.8(5)
N3 C14 C16 . . 112.3(6)
C13 C14 C16 . . 110.8(6)
N3 C14 C15 . . 108.7(6)
C13 C14 C15 . . 108.1(6)
C16 C14 C15 . . 106.9(6)
C14 C16 H16A . . 109.5
C14 C16 H16B . . 109.5
H16A C16 H16B . . 109.5
C14 C16 H16C . . 109.5
H16A C16 H16C . . 109.5
H16B C16 H16C . . 109.5
C11 C13 C14 . . 118.9(6)
C11 C13 H13A . . 107.6
C14 C13 H13A . . 107.6
C11 C13 H13B . . 107.6
C14 C13 H13B . . 107.6
H13A C13 H13B . . 107.0
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
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
N2 C3 C4 . . 112.5(6)
N2 C3 C5 . . 109.4(5)
C4 C3 C5 . . 110.3(6)
N2 C3 H3 . . 108.2
C4 C3 H3 . . 108.2
C5 C3 H3 . . 108.2
C6 C8 H8A . . 109.5
C6 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C6 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
C6 C7 H7A . . 109.5
C6 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C6 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
N1 C1 C2 . 2_777 109.7(5)
N1 C1 H1A . . 109.7
C2 C1 H1A 2_777 . 109.7
N1 C1 H1B . . 109.7
C2 C1 H1B 2_777 . 109.7
H1A C1 H1B . . 108.2
N2 C2 C1 . 2_777 108.5(5)
N2 C2 H2A . . 110.0
C1 C2 H2A 2_777 . 110.0
N2 C2 H2B . . 110.0
C1 C2 H2B 2_777 . 110.0
H2A C2 H2B . . 108.4
H2WA O2W H2WB . . 109(3)
H4WB O4W H4WA . . 109(3)
H3WA O3W H3WB . . 107(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
W1 O1 . 1.772(4)
W1 O2 . 1.773(4)
W1 O4 . 1.775(4)
W1 O3 . 1.778(4)
O4 Ni1 . 2.135(4)
O1 Ni2 . 2.121(4)
Ni1 N2 . 2.059(5)
Ni1 N2 2_777 2.059(5)
Ni1 N1 2_777 2.098(5)
Ni1 N1 . 2.098(5)
Ni1 O4 2_777 2.135(4)
Ni2 N3 2_776 2.087(5)
Ni2 N3 . 2.087(5)
Ni2 N4 2_776 2.089(5)
Ni2 N4 . 2.089(5)
Ni2 O1 2_776 2.121(4)
N1 C1 . 1.477(8)
N1 C6 . 1.498(8)
N1 H1C . 0.9300
N2 C2 . 1.484(7)
N2 C3 . 1.499(8)
N2 H2C . 0.9300
N4 C10 . 1.478(8)
N4 C11 . 1.486(8)
N4 H4D . 0.9300
N3 C9 . 1.490(8)
N3 C14 . 1.492(8)
N3 H3A . 0.9300
C6 C7 . 1.530(9)
C6 C5 . 1.535(10)
C6 C8 . 1.539(9)
C11 C13 . 1.511(10)
C11 C12 . 1.548(10)
C11 H11 . 1.0000
C5 C3 . 1.536(9)
C5 H5A . 0.9900
C5 H5B . 0.9900
C9 C10 2_776 1.526(10)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 C9 2_776 1.526(10)
C10 H10A . 0.9900
C10 H10B . 0.9900
C14 C13 . 1.529(10)
C14 C16 . 1.534(9)
C14 C15 . 1.563(9)
C16 H16A . 0.9800
C16 H16B . 0.9800
C16 H16C . 0.9800
C13 H13A . 0.9900
C13 H13B . 0.9900
C15 H15A . 0.9800
C15 H15B . 0.9800
C15 H15C . 0.9800
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C3 C4 . 1.521(10)
C3 H3 . 1.0000
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C7 H7A . 0.9800
C7 H7B . 0.9800
C7 H7C . 0.9800
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
C1 C2 2_777 1.498(8)
C1 H1A . 0.9900
C1 H1B . 0.9900
C2 C1 2_777 1.498(8)
C2 H2A . 0.9900
C2 H2B . 0.9900
O2W H2WA . 0.85(2)
O2W H2WB . 0.86(2)
O4W H4WB . 0.845(19)
O4W H4WA . 0.86(2)
O1W H1WA . 0.86(2)
O1W H1WB . 0.85(2)
O3W H3WA . 0.87(2)
O3W H3WB . 0.863(19)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1C O2 2_777 0.93 2.32 3.253(7) 179.7
N2 H2C O4W 2_777 0.93 2.21 3.040(8) 149.0
O4W H4WB O3W . 0.845(19) 2.12(5) 2.720(8) 128(6)
O4W H4WA O3 . 0.86(2) 2.05(3) 2.900(7) 168(6)
O2W H2WA O1W 2_666 0.85(2) 1.94(2) 2.790(8) 175(7)
O3W H3WA O2 1_455 0.87(2) 2.01(5) 2.784(7) 148(8)
O1W H1WA O2 . 0.86(2) 1.95(2) 2.801(7) 172(8)
O2W H2WB O3 . 0.86(2) 1.99(3) 2.811(7) 160(8)
O3W H3WB O2W . 0.863(19) 2.08(4) 2.834(8) 145(6)
O1W H1WB O2W . 0.85(2) 2.10(4) 2.895(9) 157(7)
C16 H16A O1 2_776 0.98 2.40 3.241(9) 143.8
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1 W1 O4 Ni1 . . -113.9(5)
O2 W1 O4 Ni1 . . 5.5(6)
O3 W1 O4 Ni1 . . 125.6(5)
O2 W1 O1 Ni2 . . 73.4(4)
O4 W1 O1 Ni2 . . -167.2(3)
O3 W1 O1 Ni2 . . -46.1(4)
W1 O4 Ni1 N2 . . 87.9(5)
W1 O4 Ni1 N2 . 2_777 -92.1(5)
W1 O4 Ni1 N1 . 2_777 2.5(5)
W1 O4 Ni1 N1 . . -177.5(5)
W1 O1 Ni2 N3 . 2_776 117.7(4)
W1 O1 Ni2 N3 . . -62.3(4)
W1 O1 Ni2 N4 . 2_776 -147.8(4)
W1 O1 Ni2 N4 . . 32.2(4)
N2 Ni1 N1 C1 . . 167.3(4)
N2 Ni1 N1 C1 2_777 . -12.7(4)
O4 Ni1 N1 C1 . . 76.4(4)
O4 Ni1 N1 C1 2_777 . -103.6(4)
N2 Ni1 N1 C6 . . 32.0(5)
N2 Ni1 N1 C6 2_777 . -148.0(5)
O4 Ni1 N1 C6 . . -58.9(5)
O4 Ni1 N1 C6 2_777 . 121.1(5)
N1 Ni1 N2 C2 2_777 . 16.8(4)
N1 Ni1 N2 C2 . . -163.2(4)
O4 Ni1 N2 C2 . . -68.4(4)
O4 Ni1 N2 C2 2_777 . 111.6(4)
N1 Ni1 N2 C3 2_777 . 143.2(5)
N1 Ni1 N2 C3 . . -36.8(5)
O4 Ni1 N2 C3 . . 58.0(4)
O4 Ni1 N2 C3 2_777 . -122.0(4)
N3 Ni2 N4 C10 2_776 . 16.1(4)
N3 Ni2 N4 C10 . . -163.9(4)
O1 Ni2 N4 C10 2_776 . -70.1(4)
O1 Ni2 N4 C10 . . 109.9(4)
N3 Ni2 N4 C11 2_776 . 143.2(5)
N3 Ni2 N4 C11 . . -36.8(5)
O1 Ni2 N4 C11 2_776 . 57.1(4)
O1 Ni2 N4 C11 . . -122.9(4)
N4 Ni2 N3 C9 2_776 . -15.4(4)
N4 Ni2 N3 C9 . . 164.6(4)
O1 Ni2 N3 C9 2_776 . 74.5(4)
O1 Ni2 N3 C9 . . -105.5(4)
N4 Ni2 N3 C14 2_776 . -149.8(5)
N4 Ni2 N3 C14 . . 30.2(5)
O1 Ni2 N3 C14 2_776 . -59.9(5)
O1 Ni2 N3 C14 . . 120.1(5)
C1 N1 C6 C7 . . -53.1(7)
Ni1 N1 C6 C7 . . 77.3(6)
C1 N1 C6 C5 . . -175.7(5)
Ni1 N1 C6 C5 . . -45.2(7)
C1 N1 C6 C8 . . 67.5(7)
Ni1 N1 C6 C8 . . -162.1(5)
C10 N4 C11 C13 . . -178.8(5)
Ni2 N4 C11 C13 . . 59.7(6)
C10 N4 C11 C12 . . -56.2(8)
Ni2 N4 C11 C12 . . -177.7(5)
N1 C6 C5 C3 . . 67.8(7)
C7 C6 C5 C3 . . -54.3(8)
C8 C6 C5 C3 . . -173.6(6)
C14 N3 C9 C10 . 2_776 -179.4(5)
Ni2 N3 C9 C10 . 2_776 43.7(6)
C11 N4 C10 C9 . 2_776 -171.2(5)
Ni2 N4 C10 C9 . 2_776 -44.5(6)
C9 N3 C14 C13 . . -172.9(5)
Ni2 N3 C14 C13 . . -43.5(7)
C9 N3 C14 C16 . . -49.2(8)
Ni2 N3 C14 C16 . . 80.2(7)
C9 N3 C14 C15 . . 69.0(7)
Ni2 N3 C14 C15 . . -161.6(5)
N4 C11 C13 C14 . . -78.2(8)
C12 C11 C13 C14 . . 158.4(6)
N3 C14 C13 C11 . . 66.9(8)
C16 C14 C13 C11 . . -57.8(8)
C15 C14 C13 C11 . . -174.6(6)
C2 N2 C3 C4 . . -56.5(8)
Ni1 N2 C3 C4 . . -178.5(5)
C2 N2 C3 C5 . . -179.3(5)
Ni1 N2 C3 C5 . . 58.7(7)
C6 C5 C3 N2 . . -77.9(8)
C6 C5 C3 C4 . . 157.9(6)
C6 N1 C1 C2 . 2_777 178.6(5)
Ni1 N1 C1 C2 . 2_777 40.5(6)
C3 N2 C2 C1 . 2_777 -170.8(6)
Ni1 N2 C2 C1 . 2_777 -43.5(6)
