# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_b_sq
_database_code_depnum_ccdc_archive 'CCDC 1587891'
_audit_update_record             
;
2018-03-01 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_1_b_sq              
;
PROBLEM: Check Calcd Positive Resid. Density on        W2       2.89 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT035_1_b_sq              
;
PROBLEM: _chemical_absolute_configuration Info  Not Given     Please Do !
RESPONSE: Refined as inversion twin with BASF 0.24
;
_vrf_PLAT413_1_b_sq              
;
PROBLEM: Short Inter XH3 .. XHn     H5B      ..H11A             1.90 Ang.
RESPONSE: Disordered DMF molecules
;
# Added during the CSD deposition process: Thursday 01 March 2018 06:25 AM
# end Validation Reply Form

# complex 2 [Co(DMF)6]2[PW11NbO40]*2.6DMF
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H84 Co2 N12 O52 P W12'
_chemical_formula_weight         3872.18

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'
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'
Co Co 0.3494 0.9721 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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.
;

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'

_cell_length_a                   15.8751(6)
_cell_length_b                   15.8751(6)
_cell_length_c                   31.9698(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6977.6(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2417
_cell_measurement_theta_min      3.8190
_cell_measurement_theta_max      29.0750

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_F_000             5271
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    15.221
_shelx_estimated_absorpt_T_min   0.135
_shelx_estimated_absorpt_T_max   0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.14441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            6745
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.514
_diffrn_reflns_theta_max         29.556
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4974
_reflns_number_gt                4549
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.830
_reflns_Friedel_fraction_full    0.994

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0706P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4974
_refine_ls_number_parameters     343
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1196
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4726(19) 1.0334(19) 0.3864(8) 0.036(6) Uani 1 1 d . . . . .
H1A H 0.477009 1.014916 0.357607 0.054 Uiso 1 1 calc R U . . .
H1B H 0.454849 0.977912 0.405034 0.054 Uiso 1 1 calc R U . . .
H1C H 0.422871 1.052639 0.388080 0.054 Uiso 1 1 calc R U . . .
C2 C 0.6474(18) 1.1564(19) 0.3678(9) 0.039(6) Uani 1 1 d . U . . .
H2A H 0.624634 1.118809 0.341817 0.059 Uiso 1 1 calc R U . . .
H2B H 0.666990 1.224454 0.362182 0.059 Uiso 1 1 calc R U . . .
H2C H 0.703211 1.152685 0.378650 0.059 Uiso 1 1 calc R U . . .
C3 C 0.7727(18) 1.2559(17) 0.5316(9) 0.038(6) Uani 1 1 d . . . . .
H3A H 0.723994 1.198755 0.518232 0.045 Uiso 1 1 calc R U . . .
C4 C 0.9190(19) 1.329(2) 0.5749(9) 0.046(7) Uani 1 1 d . . . . .
H4A H 0.952997 1.303960 0.592063 0.068 Uiso 1 1 calc R U . . .
H4B H 0.962603 1.370670 0.552773 0.068 Uiso 1 1 calc R U . . .
H4C H 0.899197 1.366451 0.592472 0.068 Uiso 1 1 calc R U . . .
C5 C 0.0394(15) 0.1796(16) 0.6292(8) 0.025(5) Uani 1 1 d . U . . .
H5A H 0.066382 0.220063 0.654164 0.038 Uiso 1 1 calc R U . . .
H5B H -0.021212 0.177531 0.621203 0.038 Uiso 1 1 calc R U . . .
H5C H 0.026171 0.113498 0.635096 0.038 Uiso 1 1 calc R U . . .
C10 C 0.1966(18) 0.3085(18) 0.6060(8) 0.034(6) Uani 1 1 d . . . . .
H10A H 0.193361 0.324142 0.635443 0.050 Uiso 1 1 calc R U . . .
H10B H 0.252659 0.299349 0.601907 0.050 Uiso 1 1 calc R U . . .
H10C H 0.203470 0.361911 0.588295 0.050 Uiso 1 1 calc R U . . .
C11 C 0.826(3) 1.153(3) 0.5652(11) 0.068(9) Uani 1 1 d . U . . .
H11A H 0.878688 1.164043 0.584309 0.103 Uiso 1 1 calc R U . . .
H11B H 0.763167 1.109378 0.578355 0.103 Uiso 1 1 calc R U . . .
H11C H 0.832006 1.123852 0.539223 0.103 Uiso 1 1 calc R U . . .
C12 C 0.5817(14) 1.1543(13) 0.4358(7) 0.017(4) Uani 1 1 d . . . . .
H12A H 0.529187 1.127691 0.455135 0.021 Uiso 1 1 calc R U . . .
O1 O 0.333333 0.666667 0.5419(7) 0.0161(15) Uani 1 3 d S TU P . .
O2 O 0.2983(11) 0.5582(11) 0.6059(5) 0.023(3) Uani 1 1 d . U . . .
O3 O 0.4888(13) 0.5981(13) 0.6262(6) 0.037(4) Uani 1 1 d . . . . .
O4 O 0.4959(11) 0.5884(11) 0.4813(5) 0.032(4) Uani 1 1 d . . . . .
O5 O 0.6943(11) 0.7352(11) 0.4949(5) 0.025(3) Uani 1 1 d . . . . .
O6 O 0.6128(11) 0.8565(11) 0.5009(5) 0.027(3) Uani 1 1 d . . . . .
O7 O 0.5781(10) 0.7478(10) 0.4333(5) 0.024(3) Uani 1 1 d . . . . .
O8 O 0.5389(9) 0.8912(10) 0.4328(5) 0.024(3) Uani 1 1 d . . . . .
O9 O 0.6115(12) 1.0296(11) 0.4981(5) 0.032(4) Uani 1 1 d . . . . .
O10 O 0.7729(12) 1.3320(12) 0.5241(6) 0.033(4) Uani 1 1 d . U . . .
O11 O 0.6618(12) 1.2256(11) 0.4476(5) 0.027(4) Uani 1 1 d . . . . .
O12 O -0.1023(12) 0.0124(12) 0.4715(5) 0.034(4) Uani 1 1 d D . . . .
O13 O 0.4055(10) 0.6323(10) 0.3973(5) 0.030(4) Uani 1 1 d . . . . .
O14 O 0.5397(13) 0.8101(13) 0.3573(7) 0.042(5) Uani 1 1 d . . . . .
O15 O 0.5322(11) 0.6981(10) 0.5467(5) 0.027(3) Uani 1 1 d . U . . .
O16 O 0.4829(11) 0.8717(11) 0.5475(5) 0.029(4) Uani 1 1 d . . . . .
O17 O 0.2617(9) 0.6987(9) 0.4777(4) 0.019(3) Uani 1 1 d . U . . .
C18 C 0.0910(19) 0.1809(17) 0.5585(8) 0.028(6) Uani 1 1 d . . . . .
H18A H 0.141844 0.209256 0.538393 0.033 Uiso 1 1 calc R U . . .
O19 O 0.0127(10) 0.1083(10) 0.5470(5) 0.018(3) Uani 1 1 d . . . . .
P1 P 0.333333 0.666667 0.4945(3) 0.0050(11) Uani 1 3 d S T P . .
Co1 Co 0.000000 0.000000 0.50802(17) 0.0218(12) Uani 1 3 d S T P A .
Co2 Co 0.666667 1.333333 0.48810(17) 0.0211(11) Uani 1 3 d S T P . .
W1 W 0.52986(7) 0.91034(7) 0.49364(3) 0.0255(2) Uani 1 1 d . . . . .
W2 W 0.48427(7) 0.77084(7) 0.40499(3) 0.0208(2) Uani 1 1 d . . . . .
W3 W 0.58101(7) 0.72416(7) 0.49196(3) 0.0253(3) Uani 1 1 d . . . . .
W4 W 0.43187(7) 0.62364(7) 0.58718(3) 0.0220(2) Uani 1 1 d . . . . .
N1 N 0.5674(13) 1.1156(13) 0.3993(6) 0.022(4) Uani 1 1 d . . . . .
N2 N 0.1090(15) 0.2206(14) 0.5950(6) 0.027(4) Uani 1 1 d . . . . .
N4 N 0.8318(15) 1.2461(14) 0.5558(7) 0.033(5) Uani 1 1 d . . . . .
C7A C -0.078(6) 0.089(9) 0.451(6) 0.08(10) Uiso 0.3 1 d D . P A 1
H7A H -0.013580 0.134928 0.442672 0.097 Uiso 0.3 1 calc R U P A 1
C8A C -0.234(7) 0.005(8) 0.422(4) 0.04(2) Uiso 0.3 1 d . . P A 1
H8AA H -0.227332 -0.048248 0.433871 0.062 Uiso 0.3 1 calc R U P A 1
H8AB H -0.301192 -0.009090 0.425543 0.062 Uiso 0.3 1 calc R U P A 1
H8AC H -0.218589 0.010654 0.391938 0.062 Uiso 0.3 1 calc R U P A 1
C9A C -0.161(6) 0.178(6) 0.434(3) 0.034(18) Uiso 0.3 1 d . . P A 1
H9AA H -0.111418 0.227665 0.452086 0.051 Uiso 0.3 1 calc R U P A 1
H9AB H -0.140506 0.194829 0.404475 0.051 Uiso 0.3 1 calc R U P A 1
H9AC H -0.223109 0.175085 0.438080 0.051 Uiso 0.3 1 calc R U P A 1
N3A N -0.170(6) 0.093(6) 0.442(3) 0.034(18) Uiso 0.3 1 d D . P A 1
C7B C -0.081(4) 0.093(3) 0.457(3) 0.06(3) Uiso 0.7 1 d D . P A 2
H7B H -0.019008 0.146508 0.464204 0.067 Uiso 0.7 1 calc R U P A 2
C8B C -0.236(3) 0.038(3) 0.4256(16) 0.048(12) Uiso 0.7 1 d . . P A 2
H8BA H -0.268135 0.062797 0.407086 0.072 Uiso 0.7 1 calc R U P A 2
H8BB H -0.236894 -0.018071 0.412532 0.072 Uiso 0.7 1 calc R U P A 2
H8BC H -0.270473 0.018769 0.452383 0.072 Uiso 0.7 1 calc R U P A 2
C9B C -0.104(3) 0.206(3) 0.4123(12) 0.044(9) Uiso 0.7 1 d . . P A 2
H9BA H -0.156462 0.204778 0.395830 0.065 Uiso 0.7 1 calc R U P A 2
H9BB H -0.082279 0.257372 0.433629 0.065 Uiso 0.7 1 calc R U P A 2
H9BC H -0.048866 0.220331 0.393792 0.065 Uiso 0.7 1 calc R U P A 2
N3B N -0.138(3) 0.113(3) 0.4324(13) 0.047(10) Uiso 0.7 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.48(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.49(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O10 1.23(3) . ?
C3 N4 1.28(3) . ?
C3 H3A 0.9500 . ?
C4 N4 1.48(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N2 1.45(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C10 N2 1.44(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.46(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 O11 1.26(2) . ?
C12 N1 1.29(3) . ?
C12 H12A 0.9500 . ?
O1 P1 1.51(3) . ?
O1 W4 2.466(14) . ?
O1 W4 2.466(14) 3_565 ?
O1 W4 2.466(14) 2_665 ?
O2 W4 1.875(14) 3_565 ?
O2 W4 1.931(15) . ?
O3 W4 1.704(18) . ?
O4 W1 1.897(16) 3_565 ?
O4 W3 1.917(16) . ?
O5 W3 1.721(15) . ?
O6 W1 1.909(15) . ?
O6 W3 1.921(14) . ?
O7 W3 1.917(15) . ?
O7 W2 1.927(14) . ?
O8 W2 1.881(14) . ?
O8 W1 1.984(15) . ?
O9 W1 1.682(15) . ?
O10 Co2 2.051(18) . ?
O11 Co2 2.116(16) . ?
O12 C7B 1.24(2) . ?
O12 C7A 1.25(2) . ?
O12 Co1 2.087(16) . ?
O13 W2 1.886(14) 3_565 ?
O13 W2 1.926(14) . ?
O14 W2 1.716(19) . ?
O15 W3 1.875(16) . ?
O15 W4 1.930(15) . ?
O16 W1 1.856(16) . ?
O16 W4 1.944(16) 2_665 ?
O17 P1 1.556(13) . ?
O17 W2 2.418(14) 2_665 ?
O17 W1 2.422(13) 2_665 ?
O17 W3 2.449(13) 2_665 ?
C18 O19 1.26(3) . ?
C18 N2 1.29(3) . ?
C18 H18A 0.9500 . ?
O19 Co1 2.050(14) . ?
C7A N3A 1.52(2) . ?
C7A H7A 0.9500 . ?
C8A N3A 1.42(13) . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A N3A 1.31(11) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C7B N3B 1.34(6) . ?
C7B H7B 0.9500 . ?
C8B N3B 1.43(6) . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B N3B 1.45(5) . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?

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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O10 C3 N4 126(2) . . ?
O10 C3 H3A 116.8 . . ?
N4 C3 H3A 116.8 . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O11 C12 N1 124(2) . . ?
O11 C12 H12A 118.1 . . ?
N1 C12 H12A 118.1 . . ?
P1 O1 W4 126.0(4) . . ?
P1 O1 W4 126.0(4) . 3_565 ?
W4 O1 W4 89.0(6) . 3_565 ?
P1 O1 W4 126.0(4) . 2_665 ?
W4 O1 W4 89.0(6) . 2_665 ?
W4 O1 W4 89.0(6) 3_565 2_665 ?
W4 O2 W4 130.5(8) 3_565 . ?
W1 O4 W3 149.9(9) 3_565 . ?
W1 O6 W3 127.5(8) . . ?
W3 O7 W2 126.4(8) . . ?
W2 O8 W1 125.9(7) . . ?
C3 O10 Co2 121.4(16) . . ?
C12 O11 Co2 121.3(14) . . ?
C7B O12 Co1 119(3) . . ?
C7A O12 Co1 120(6) . . ?
W2 O13 W2 149.7(8) 3_565 . ?
W3 O15 W4 152.2(9) . . ?
W1 O16 W4 151.4(9) . 2_665 ?
P1 O17 W2 126.2(8) . 2_665 ?
P1 O17 W1 125.2(7) . 2_665 ?
W2 O17 W1 90.7(4) 2_665 2_665 ?
P1 O17 W3 124.3(7) . 2_665 ?
W2 O17 W3 89.7(4) 2_665 2_665 ?
W1 O17 W3 89.7(4) 2_665 2_665 ?
O19 C18 N2 126(2) . . ?
O19 C18 H18A 117.0 . . ?
N2 C18 H18A 117.0 . . ?
C18 O19 Co1 125.7(14) . . ?
O1 P1 O17 110.2(6) . 2_665 ?
O1 P1 O17 110.2(6) . . ?
O17 P1 O17 108.7(6) 2_665 . ?
O1 P1 O17 110.2(6) . 3_565 ?
O17 P1 O17 108.7(6) 2_665 3_565 ?
O17 P1 O17 108.7(6) . 3_565 ?
O19 Co1 O19 86.9(6) . 2 ?
O19 Co1 O19 86.9(6) . 3 ?
O19 Co1 O19 86.9(6) 2 3 ?
O19 Co1 O12 176.5(7) . 2 ?
O19 Co1 O12 90.9(6) 2 2 ?
O19 Co1 O12 90.3(6) 3 2 ?
O19 Co1 O12 90.3(6) . 3 ?
O19 Co1 O12 176.5(7) 2 3 ?
O19 Co1 O12 90.9(6) 3 3 ?
O12 Co1 O12 91.8(7) 2 3 ?
O19 Co1 O12 90.9(6) . . ?
O19 Co1 O12 90.3(6) 2 . ?
O19 Co1 O12 176.5(7) 3 . ?
O12 Co1 O12 91.8(7) 2 . ?
O12 Co1 O12 91.8(7) 3 . ?
O10 Co2 O10 91.6(7) . 3_575 ?
O10 Co2 O10 91.6(7) . 2_775 ?
O10 Co2 O10 91.6(7) 3_575 2_775 ?
O10 Co2 O11 91.9(7) . . ?
O10 Co2 O11 90.0(7) 3_575 . ?
O10 Co2 O11 176.1(7) 2_775 . ?
O10 Co2 O11 90.0(7) . 2_775 ?
O10 Co2 O11 176.1(7) 3_575 2_775 ?
O10 Co2 O11 91.9(7) 2_775 2_775 ?
O11 Co2 O11 86.4(7) . 2_775 ?
O10 Co2 O11 176.1(7) . 3_575 ?
O10 Co2 O11 91.9(7) 3_575 3_575 ?
O10 Co2 O11 90.0(7) 2_775 3_575 ?
O11 Co2 O11 86.4(7) . 3_575 ?
O11 Co2 O11 86.4(7) 2_775 3_575 ?
O9 W1 O16 104.5(8) . . ?
O9 W1 O4 104.0(8) . 2_665 ?
O16 W1 O4 87.5(7) . 2_665 ?
O9 W1 O6 100.2(8) . . ?
O16 W1 O6 89.5(7) . . ?
O4 W1 O6 155.6(7) 2_665 . ?
O9 W1 O8 100.4(7) . . ?
O16 W1 O8 155.1(6) . . ?
O4 W1 O8 86.5(6) 2_665 . ?
O6 W1 O8 86.0(6) . . ?
O9 W1 O17 168.2(7) . 3_565 ?
O16 W1 O17 84.6(6) . 3_565 ?
O4 W1 O17 83.8(6) 2_665 3_565 ?
O6 W1 O17 71.8(5) . 3_565 ?
O8 W1 O17 70.8(5) . 3_565 ?
O14 W2 O8 99.2(8) . . ?
O14 W2 O13 102.0(8) . 2_665 ?
O8 W2 O13 90.0(6) . 2_665 ?
O14 W2 O13 103.0(8) . . ?
O8 W2 O13 157.9(7) . . ?
O13 W2 O13 85.6(9) 2_665 . ?
O14 W2 O7 100.5(8) . . ?
O8 W2 O7 87.9(6) . . ?
O13 W2 O7 157.5(7) 2_665 . ?
O13 W2 O7 88.0(6) . . ?
O14 W2 O17 168.8(8) . 3_565 ?
O8 W2 O17 72.5(5) . 3_565 ?
O13 W2 O17 85.8(6) 2_665 3_565 ?
O13 W2 O17 85.6(6) . 3_565 ?
O7 W2 O17 72.2(5) . 3_565 ?
O5 W3 O15 105.5(7) . . ?
O5 W3 O4 103.7(7) . . ?
O15 W3 O4 86.4(7) . . ?
O5 W3 O7 99.2(7) . . ?
O15 W3 O7 155.3(6) . . ?
O4 W3 O7 88.5(7) . . ?
O5 W3 O6 101.0(7) . . ?
O15 W3 O6 87.5(6) . . ?
O4 W3 O6 155.2(7) . . ?
O7 W3 O6 87.1(6) . . ?
O5 W3 O17 167.8(6) . 3_565 ?
O15 W3 O17 83.8(6) . 3_565 ?
O4 W3 O17 84.5(6) . 3_565 ?
O7 W3 O17 71.6(5) . 3_565 ?
O6 W3 O17 71.0(5) . 3_565 ?
O3 W4 O2 102.0(8) . 2_665 ?
O3 W4 O15 105.2(8) . . ?
O2 W4 O15 88.4(6) 2_665 . ?
O3 W4 O2 102.4(8) . . ?
O2 W4 O2 87.7(9) 2_665 . ?
O15 W4 O2 152.3(6) . . ?
O3 W4 O16 105.5(7) . 3_565 ?
O2 W4 O16 152.4(7) 2_665 3_565 ?
O15 W4 O16 85.4(6) . 3_565 ?
O2 W4 O16 85.4(6) . 3_565 ?
O3 W4 O1 168.9(8) . . ?
O2 W4 O1 70.5(5) 2_665 . ?
O15 W4 O1 83.1(6) . . ?
O2 W4 O1 69.7(5) . . ?
O16 W4 O1 82.1(6) 3_565 . ?
C12 N1 C1 122(2) . . ?
C12 N1 C2 120(2) . . ?
C1 N1 C2 118(2) . . ?
C18 N2 C10 124(2) . . ?
C18 N2 C5 122(2) . . ?
C10 N2 C5 113.6(19) . . ?
C3 N4 C11 124(2) . . ?
C3 N4 C4 124(2) . . ?
C11 N4 C4 112(2) . . ?
O12 C7A N3A 107(6) . . ?
O12 C7A H7A 126.3 . . ?
N3A C7A H7A 126.3 . . ?
N3A C8A H8AA 109.5 . . ?
N3A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
N3A C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
N3A C9A H9AA 109.5 . . ?
N3A C9A H9AB 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
N3A C9A H9AC 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C9A N3A C8A 125(8) . . ?
C9A N3A C7A 118(7) . . ?
C8A N3A C7A 106(10) . . ?
O12 C7B N3B 126(5) . . ?
O12 C7B H7B 117.0 . . ?
N3B C7B H7B 117.0 . . ?
N3B C8B H8BA 109.5 . . ?
N3B C8B H8BB 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
N3B C8B H8BC 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
N3B C9B H9BA 109.5 . . ?
N3B C9B H9BB 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
N3B C9B H9BC 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C7B N3B C8B 119(4) . . ?
C7B N3B C9B 123(4) . . ?
C8B N3B C9B 118(4) . . ?

_refine_diff_density_max         3.509
_refine_diff_density_min         -4.374
_refine_diff_density_rms         0.370


_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1587892'
_audit_update_record             
;
2017-11-28 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_1_a                 
;
PROBLEM: Check Calcd Resid. Dens.  0.62A   From O16             2.55 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT975_1_a_2               
;
PROBLEM: Check Calcd Resid. Dens.  0.54A   From O15             2.46 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT975_1_a_3               
;
PROBLEM: Check Calcd Resid. Dens.  0.60A   From O20             2.05 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT110_1_a                 
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: Thermal ellipsoids and refinement of CH3CN/H2O disordering is better in P2(1)/n then in I2/m
;
_vrf_PLAT112_1_a                 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         I        100 %Fit
RESPONSE: Thermal ellipsoids and refinement of CH3CN/H2O disordering is better in P2(1)/n then in I2/m
;
_vrf_PLAT113_1_a                 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       I2/m Check
RESPONSE: Thermal ellipsoids and refinement of CH3CN/H2O disordering is better in P2(1)/n then in I2/m
;
_vrf_PLAT971_1_a                 
;
PROBLEM: Check Calcd Resid. Dens.  0.62A   From O16             2.55 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT973_1_a                 
;
PROBLEM: Check Calcd Positive Resid. Density on        W5       1.76 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT975_1_a_4               
;
PROBLEM: Check Calcd Resid. Dens.  0.64A   From O15             1.95 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT975_1_a_5               
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From O2              1.93 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_2               
;
PROBLEM: Check Calcd Resid. Dens.  0.54A   From O15             2.46 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_3               
;
PROBLEM: Check Calcd Resid. Dens.  0.96A   From W5              2.11 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_4               
;
PROBLEM: Check Calcd Resid. Dens.  1.50A   From N6              2.07 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_5               
;
PROBLEM: Check Calcd Resid. Dens.  0.60A   From O20             2.05 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_6               
;
PROBLEM: Check Calcd Resid. Dens.  1.10A   From W3              2.04 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_7               
;
PROBLEM: Check Calcd Resid. Dens.  1.07A   From W1              2.00 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_8               
;
PROBLEM: Check Calcd Resid. Dens.  1.10A   From C15B            2.00 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_9               
;
PROBLEM: Check Calcd Resid. Dens.  0.64A   From O15             1.95 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_10              
;
PROBLEM: Check Calcd Resid. Dens.  1.01A   From W3              1.94 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_11              
;
PROBLEM: Check Calcd Resid. Dens.  0.66A   From O17             1.94 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_12              
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From O21             1.93 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_13              
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From O2              1.93 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_14              
;
PROBLEM: Check Calcd Resid. Dens.  0.25A   From W3              1.85 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_15              
;
PROBLEM: Check Calcd Resid. Dens.  0.64A   From O16             1.85 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_16              
;
PROBLEM: Check Calcd Resid. Dens.  0.94A   From O14             1.83 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_17              
;
PROBLEM: Check Calcd Resid. Dens.  0.32A   From W6              1.76 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_18              
;
PROBLEM: Check Calcd Resid. Dens.  0.80A   From O5              1.75 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_19              
;
PROBLEM: Check Calcd Resid. Dens.  0.97A   From O12             1.75 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_20              
;
PROBLEM: Check Calcd Resid. Dens.  1.13A   From O22             1.66 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_21              
;
PROBLEM: Check Calcd Resid. Dens.  0.63A   From C10B            1.65 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_22              
;
PROBLEM: Check Calcd Resid. Dens.  0.60A   From O20             1.64 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_23              
;
PROBLEM: Check Calcd Resid. Dens.  0.94A   From C10B            1.62 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT971_1_a_24              
;
PROBLEM: Check Calcd Resid. Dens.  0.29A   From W4              1.57 eA-3
RESPONSE: Residual density without any chemical sense
;
# Added during the CSD deposition process: Tuesday 28 November 2017 05:07 AM
# end Validation Reply Form

#complex 3 [Ni(CH3CN)5.5(H2O)0.5]2[PW11NbO40]*1.7CH3CN

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H33 N11 Ni2 O41 P W12'
_chemical_formula_weight         3522.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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'
C C 0.0033 0.0016 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6148(8)
_cell_length_b                   14.6506(7)
_cell_length_c                   19.8436(12)
_cell_angle_alpha                90
_cell_angle_beta                 105.190(6)
_cell_angle_gamma                90
_cell_volume                     3539.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3622
_cell_measurement_theta_min      3.5150
_cell_measurement_theta_max      27.0190

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.305
_exptl_crystal_F_000             3118
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    20.040
_shelx_estimated_absorpt_T_min   0.153
_shelx_estimated_absorpt_T_max   0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.32053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            27962
_diffrn_reflns_av_unetI/netI     0.1126
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.336
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6230
_reflns_number_gt                3763
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0581P)²+97.5865P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6230
_refine_ls_number_parameters     414
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0735
_refine_ls_wR_factor_ref         0.1819
_refine_ls_wR_factor_gt          0.1623
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1432(18) 0.8099(13) 0.3890(11) 0.056(6) Uani 1 1 d . . . . .
O2 O 0.2640(19) 0.8733(14) 0.5222(12) 0.064(6) Uani 1 1 d . U . . .
O3 O 0.2913(18) 0.8310(14) 0.6615(11) 0.061(7) Uani 1 1 d . . . . .
O4 O 0.4902(16) 0.9233(12) 0.6749(12) 0.055(6) Uani 1 1 d . . . . .
O5 O 0.3092(16) 1.0740(13) 0.3368(12) 0.056(6) Uani 1 1 d . . . . .
O6 O 0.4912(18) 1.3552(11) 0.4839(10) 0.049(5) Uani 1 1 d . . . . .
O7 O 0.5157(16) 0.8983(13) 0.3321(12) 0.053(6) Uani 1 1 d . . . . .
O8 O 0.2806(15) 1.1876(13) 0.6447(10) 0.046(5) Uani 1 1 d . . . . .
O10 O 0.1362(16) 1.1663(12) 0.3726(10) 0.041(5) Uani 1 1 d . U . . .
O11 O 0.2063(17) 0.9889(13) 0.4225(13) 0.059(6) Uani 1 1 d . . . . .
O12 O 0.3115(15) 1.0080(13) 0.6108(12) 0.054(6) Uani 1 1 d . . . . .
O13 O 0.3091(17) 0.8990(13) 0.3455(11) 0.049(5) Uani 1 1 d . . . . .
O14 O 0.4428(19) 0.7888(16) 0.5862(12) 0.076(8) Uani 1 1 d . . . . .
O15 O 0.352(2) 1.2091(17) 0.4271(13) 0.078(7) Uani 1 1 d . U . . .
O16 O 0.430(2) 1.2209(16) 0.5647(13) 0.075(7) Uani 1 1 d . U . . .
O17 O 0.251(2) 1.1256(17) 0.5063(14) 0.085(8) Uani 1 1 d . U . . .
O18 O 0.422(3) 1.084(2) 0.5004(17) 0.027(8) Uiso 0.5 1 d . . P . .
O19 O 0.425(2) 0.9143(17) 0.5060(14) 0.010(6) Uiso 0.5 1 d . . P . .
O20 O 0.6268(19) 1.2196(14) 0.5520(12) 0.062(6) Uani 1 1 d . U . . .
O21 O 0.354(2) 0.9778(17) 0.2250(15) 0.085(8) Uani 1 1 d . U . . .
O22 O 0.519(3) 0.997(2) 0.4287(19) 0.036(9) Uiso 0.5 1 d . . P . .
O23 O 0.406(3) 0.9946(19) 0.4410(16) 0.023(7) Uiso 0.5 1 d . . P . .
Ni1 Ni 0.3344(3) 0.5128(2) 0.67399(16) 0.0256(7) Uani 1 1 d . . . . .
W1 W 0.35238(10) 1.12807(7) 0.59856(6) 0.0325(3) Uani 1 1 d . . . . .
W2 W 0.25195(9) 1.11334(8) 0.41354(6) 0.0340(3) Uani 1 1 d . . . . .
W3 W 0.39876(9) 0.98436(7) 0.31422(5) 0.0273(3) Uani 1 1 d . . . . .
W4 W 0.36128(10) 0.88524(7) 0.61046(5) 0.0297(3) Uani 1 1 d . . . . .
W5 W 0.25840(9) 0.87085(7) 0.42592(6) 0.0313(3) Uani 1 1 d . . . . .
W6 W 0.49299(12) 1.24278(7) 0.48909(6) 0.0402(4) Uani 1 1 d . . . . .
P1 P 0.500000 1.000000 0.500000 0.0107(16) Uiso 1 2 d S . P . .
C1 C 0.534(2) 0.6531(17) 0.7003(13) 0.031(4) Uani 1 1 d . U . . .
C2 C 0.528(2) 0.3707(19) 0.6871(14) 0.037(4) Uani 1 1 d . U . . .
C3 C 0.402(2) 0.5041(17) 0.8403(14) 0.030(4) Uani 1 1 d . U . . .
C7 C 0.163(2) 0.667(2) 0.6898(15) 0.043(8) Uani 1 1 d . . . . .
C8 C 0.090(3) 0.730(3) 0.7013(16) 0.078(12) Uani 1 1 d . . . . .
H8A H 0.067748 0.770707 0.660760 0.117 Uiso 1 1 calc R U . . .
H8B H 0.124661 0.766259 0.742863 0.117 Uiso 1 1 calc R U . . .
H8C H 0.025326 0.698866 0.708588 0.117 Uiso 1 1 calc R U . . .
C9 C 0.632(2) 0.7096(17) 0.7158(13) 0.035(5) Uani 1 1 d . U . . .
H9A H 0.677091 0.696214 0.763060 0.052 Uiso 1 1 calc R U . . .
H9B H 0.611340 0.774154 0.712541 0.052 Uiso 1 1 calc R U . . .
H9C H 0.674909 0.696390 0.682060 0.052 Uiso 1 1 calc R U . . .
C11 C 0.626(2) 0.3181(19) 0.7003(15) 0.044(5) Uani 1 1 d . U . . .
H11A H 0.677993 0.346997 0.677931 0.066 Uiso 1 1 calc R U . . .
H11B H 0.608556 0.256523 0.681445 0.066 Uiso 1 1 calc R U . . .
H11C H 0.658815 0.314484 0.750824 0.066 Uiso 1 1 calc R U . . .
C12 C 0.157(3) 0.359(2) 0.6740(15) 0.051(9) Uani 1 1 d . . . . .
C13 C 0.072(3) 0.296(3) 0.6811(19) 0.085(13) Uani 1 1 d . . . . .
H13A H 0.027114 0.324606 0.708633 0.128 Uiso 1 1 calc R U . . .
H13B H 0.106437 0.240612 0.704813 0.128 Uiso 1 1 calc R U . . .
H13C H 0.025951 0.280234 0.634749 0.128 Uiso 1 1 calc R U . . .
C14 C 0.445(2) 0.4993(17) 0.9151(13) 0.035(5) Uani 1 1 d . U . . .
H14A H 0.481265 0.440414 0.927902 0.053 Uiso 1 1 calc R U . . .
H14B H 0.384195 0.505361 0.937388 0.053 Uiso 1 1 calc R U . . .
H14C H 0.497540 0.548805 0.930975 0.053 Uiso 1 1 calc R U . . .
C1S C 0.015(5) 0.767(4) 0.509(3) 0.067(17) Uiso 0.6 1 d . . P . .
C2S C -0.045(5) 0.720(4) 0.516(3) 0.065(17) Uiso 0.6 1 d . . P . .
C3S C 0.016(9) 0.671(8) 0.492(6) 0.06(3) Uiso 0.32 1 d . . P . .
C4S C -0.043(10) 0.616(7) 0.522(6) 0.06(3) Uiso 0.32 1 d . . P . .
C5S C 0.019(8) 0.592(6) 0.485(5) 0.05(2) Uiso 0.33 1 d . . P . .
C6S C -0.126(8) 0.660(6) 0.522(5) 0.05(3) Uiso 0.33 1 d . . P . .
N1 N 0.2222(17) 0.6140(14) 0.6798(11) 0.031(5) Uani 1 1 d . . . . .
N2 N 0.2175(18) 0.4146(15) 0.6686(11) 0.031(5) Uani 1 1 d . . . . .
N3 N 0.3777(17) 0.5038(13) 0.7847(12) 0.030(4) Uani 1 1 d . U . . .
N4 N 0.4532(19) 0.4163(15) 0.6774(11) 0.037(4) Uani 1 1 d . U . . .
N5 N 0.4594(19) 0.6077(14) 0.6876(11) 0.031(4) Uani 1 1 d . U . . .
C15B C 0.311(4) 0.521(3) 0.508(3) 0.035(13) Uiso 0.5 1 d . . P A 1
C10B C 0.271(7) 0.544(5) 0.450(4) 0.09(2) Uiso 0.5 1 d . . P A 1
H10A H 0.301252 0.604109 0.442152 0.130 Uiso 0.5 1 calc R U P A 1
H10B H 0.191520 0.549195 0.441988 0.130 Uiso 0.5 1 calc R U P A 1
H10C H 0.288114 0.499860 0.417268 0.130 Uiso 0.5 1 calc R U P A 1
N6 N 0.303(2) 0.5208(16) 0.5661(14) 0.062(7) Uiso 0.5 1 d . . P A 1
O1A O 0.303(2) 0.5208(16) 0.5661(14) 0.062(7) Uiso 0.5 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O1 W5 1.699(19) . ?
O2 W4 1.86(2) . ?
O2 W5 1.89(2) . ?
O3 W4 1.70(2) . ?
O4 W4 1.872(19) . ?
O4 W3 1.918(18) 3_676 ?
O5 W3 1.863(19) . ?
O5 W2 1.94(2) . ?
O6 W6 1.649(17) . ?
O7 W1 1.90(2) 3_676 ?
O7 W3 1.90(2) . ?
O8 W1 1.689(19) . ?
O10 W2 1.665(18) . ?
O11 W5 1.845(19) . ?
O11 W2 1.935(19) . ?
O12 W1 1.87(2) . ?
O12 W4 1.905(18) . ?
O13 W3 1.90(2) . ?
O13 W5 1.91(2) . ?
O14 W4 1.88(2) . ?
O14 W6 1.93(2) 3_676 ?
O15 W2 1.86(2) . ?
O15 W6 1.94(2) . ?
O16 W6 1.90(3) . ?
O16 W1 1.90(2) . ?
O17 W2 1.85(3) . ?
O17 W1 1.94(3) . ?
O18 P1 1.57(3) . ?
O18 O23 1.73(4) . ?
O18 W2 2.41(3) . ?
O18 W1 2.43(3) . ?
O18 W6 2.53(3) . ?
O19 P1 1.59(3) . ?
O19 O23 1.72(4) . ?
O19 W5 2.37(3) . ?
O19 W4 2.45(3) . ?
O19 W6 2.51(3) 3_676 ?
O20 W6 1.85(2) . ?
O20 W5 1.93(2) 3_676 ?
O21 W3 1.71(3) . ?
O22 P1 1.49(4) . ?
O22 O23 1.50(5) . ?
O22 W3 2.38(4) . ?
O23 P1 1.43(3) . ?
O23 W3 2.50(3) . ?
Ni1 N2 2.04(2) . ?
Ni1 N4 2.05(2) . ?
Ni1 N5 2.07(2) . ?
Ni1 N1 2.07(2) . ?
Ni1 O1A 2.08(3) . ?
Ni1 N6 2.08(3) . ?
Ni1 N3 2.12(2) . ?
C1 N5 1.12(3) . ?
C1 C9 1.46(4) . ?
C2 N4 1.13(3) . ?
C2 C11 1.42(4) . ?
C3 N3 1.06(3) . ?
C3 C14 1.44(3) . ?
C7 N1 1.13(3) . ?
C7 C8 1.36(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.14(3) . ?
C12 C13 1.45(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C1S C2S 1.06(7) . ?
C1S C3S 1.44(13) . ?
C2S C3S 1.23(12) . ?
C2S C6S 1.37(11) . ?
C2S C4S 1.53(12) . ?
C3S C5S 1.17(13) . ?
C3S C4S 1.35(15) . ?
C3S C6S 2.04(15) . ?
C4S C6S 1.24(13) . ?
C4S C5S 1.25(14) . ?
C15B C10B 1.18(9) . ?
C15B N6 1.19(6) . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?

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
W4 O2 W5 142.3(14) . . ?
W4 O4 W3 140.0(13) . 3_676 ?
W3 O5 W2 140.7(13) . . ?
W1 O7 W3 139.4(11) 3_676 . ?
W5 O11 W2 140.8(11) . . ?
W1 O12 W4 141.8(11) . . ?
W3 O13 W5 140.7(12) . . ?
W4 O14 W6 138.2(14) . 3_676 ?
W2 O15 W6 139.3(14) . . ?
W6 O16 W1 139.6(13) . . ?
W2 O17 W1 139.9(16) . . ?
P1 O18 O23 51.0(14) . . ?
P1 O18 W2 125.2(17) . . ?
O23 O18 W2 74.2(15) . . ?
P1 O18 W1 124.8(17) . . ?
O23 O18 W1 138(2) . . ?
W2 O18 W1 94.8(12) . . ?
P1 O18 W6 118.9(17) . . ?
O23 O18 W6 128(2) . . ?
W2 O18 W6 92.3(10) . . ?
W1 O18 W6 92.0(10) . . ?
P1 O19 O23 51.1(13) . . ?
P1 O19 W5 126.9(14) . . ?
O23 O19 W5 75.9(14) . . ?
P1 O19 W4 122.2(14) . . ?
O23 O19 W4 138.0(18) . . ?
W5 O19 W4 95.1(10) . . ?
P1 O19 W6 118.6(14) . 3_676 ?
O23 O19 W6 129.2(17) . 3_676 ?
W5 O19 W6 93.7(9) . 3_676 ?
W4 O19 W6 91.8(9) . 3_676 ?
W6 O20 W5 141.2(12) . 3_676 ?
P1 O22 O23 57.1(18) . . ?
P1 O22 W3 133(2) . . ?
O23 O22 W3 76.4(19) . . ?
P1 O23 O22 61.3(19) . . ?
P1 O23 O19 60.0(14) . . ?
O22 O23 O19 101(2) . . ?
P1 O23 O18 58.7(15) . . ?
O22 O23 O18 99(2) . . ?
O19 O23 O18 92(2) . . ?
P1 O23 W3 129.3(18) . . ?
O22 O23 W3 68.0(18) . . ?
O19 O23 W3 132.6(17) . . ?
O18 O23 W3 134.2(19) . . ?
N2 Ni1 N4 91.5(9) . . ?
N2 Ni1 N5 175.2(8) . . ?
N4 Ni1 N5 86.2(9) . . ?
N2 Ni1 N1 90.7(8) . . ?
N4 Ni1 N1 174.7(9) . . ?
N5 Ni1 N1 91.2(8) . . ?
N2 Ni1 O1A 92.6(9) . . ?
N4 Ni1 O1A 90.7(9) . . ?
N5 Ni1 O1A 91.7(9) . . ?
N1 Ni1 O1A 93.9(9) . . ?
N2 Ni1 N6 92.6(9) . . ?
N4 Ni1 N6 90.7(9) . . ?
N5 Ni1 N6 91.7(9) . . ?
N1 Ni1 N6 93.9(9) . . ?
N2 Ni1 N3 89.8(8) . . ?
N4 Ni1 N3 86.3(8) . . ?
N5 Ni1 N3 85.8(8) . . ?
N1 Ni1 N3 88.9(8) . . ?
O1A Ni1 N3 176.2(9) . . ?
N6 Ni1 N3 176.2(9) . . ?
O8 W1 O12 102.1(10) . . ?
O8 W1 O7 101.8(9) . 3_676 ?
O12 W1 O7 86.2(8) . 3_676 ?
O8 W1 O16 102.9(10) . . ?
O12 W1 O16 155.0(10) . . ?
O7 W1 O16 88.0(10) 3_676 . ?
O8 W1 O17 101.9(10) . . ?
O12 W1 O17 88.2(10) . . ?
O7 W1 O17 156.3(10) 3_676 . ?
O16 W1 O17 87.4(11) . . ?
O8 W1 O18 158.7(10) . . ?
O12 W1 O18 91.3(10) . . ?
O7 W1 O18 95.4(10) 3_676 . ?
O16 W1 O18 65.0(10) . . ?
O17 W1 O18 61.7(11) . . ?
O10 W2 O17 101.9(11) . . ?
O10 W2 O15 101.2(10) . . ?
O17 W2 O15 87.9(11) . . ?
O10 W2 O11 103.9(9) . . ?
O17 W2 O11 85.4(10) . . ?
O15 W2 O11 154.9(10) . . ?
O10 W2 O5 102.4(9) . . ?
O17 W2 O5 155.7(11) . . ?
O15 W2 O5 87.7(10) . . ?
O11 W2 O5 88.5(8) . . ?
O10 W2 O18 159.1(10) . . ?
O17 W2 O18 62.9(12) . . ?
O15 W2 O18 65.8(10) . . ?
O11 W2 O18 89.8(10) . . ?
O5 W2 O18 93.6(10) . . ?
O21 W3 O5 103.4(11) . . ?
O21 W3 O13 103.7(11) . . ?
O5 W3 O13 86.3(8) . . ?
O21 W3 O7 100.7(11) . . ?
O5 W3 O7 155.8(10) . . ?
O13 W3 O7 90.1(8) . . ?
O21 W3 O4 101.0(11) . 3_676 ?
O5 W3 O4 86.9(8) . 3_676 ?
O13 W3 O4 155.3(10) . 3_676 ?
O7 W3 O4 86.5(8) . 3_676 ?
O21 W3 O22 160.8(13) . . ?
O5 W3 O22 89.5(11) . . ?
O13 W3 O22 91.2(10) . . ?
O7 W3 O22 66.7(10) . . ?
O4 W3 O22 65.0(11) 3_676 . ?
O21 W3 O23 163.5(12) . . ?
O5 W3 O23 65.2(10) . . ?
O13 W3 O23 65.1(9) . . ?
O7 W3 O23 91.7(10) . . ?
O4 W3 O23 90.6(10) 3_676 . ?
O22 W3 O23 35.7(11) . . ?
O3 W4 O2 101.5(10) . . ?
O3 W4 O4 103.0(10) . . ?
O2 W4 O4 155.5(10) . . ?
O3 W4 O14 101.8(12) . . ?
O2 W4 O14 87.6(9) . . ?
O4 W4 O14 87.9(9) . . ?
O3 W4 O12 102.4(10) . . ?
O2 W4 O12 87.5(9) . . ?
O4 W4 O12 86.8(8) . . ?
O14 W4 O12 155.8(11) . . ?
O3 W4 O19 157.0(10) . . ?
O2 W4 O19 60.2(10) . . ?
O4 W4 O19 96.1(10) . . ?
O14 W4 O19 65.8(10) . . ?
O12 W4 O19 91.2(9) . . ?
O1 W5 O11 102.7(10) . . ?
O1 W5 O2 104.3(10) . . ?
O11 W5 O2 86.4(10) . . ?
O1 W5 O13 100.9(9) . . ?
O11 W5 O13 87.8(9) . . ?
O2 W5 O13 154.8(10) . . ?
O1 W5 O20 104.1(10) . 3_676 ?
O11 W5 O20 153.2(10) . 3_676 ?
O2 W5 O20 87.5(9) . 3_676 ?
O13 W5 O20 86.7(9) . 3_676 ?
O1 W5 O19 160.0(10) . . ?
O11 W5 O19 91.1(10) . . ?
O2 W5 O19 61.7(10) . . ?
O13 W5 O19 94.0(9) . . ?
O20 W5 O19 63.2(9) 3_676 . ?
O6 W6 O20 102.8(10) . . ?
O6 W6 O16 102.5(10) . . ?
O20 W6 O16 86.0(10) . . ?
O6 W6 O14 101.1(10) . 3_676 ?
O20 W6 O14 89.1(9) . 3_676 ?
O16 W6 O14 156.4(11) . 3_676 ?
O6 W6 O15 102.6(11) . . ?
O20 W6 O15 154.6(10) . . ?
O16 W6 O15 87.4(11) . . ?
O14 W6 O15 87.2(10) 3_676 . ?
O6 W6 O19 156.2(10) . 3_676 ?
O20 W6 O19 60.8(9) . 3_676 ?
O16 W6 O19 93.8(9) . 3_676 ?
O14 W6 O19 63.9(9) 3_676 3_676 ?
O15 W6 O19 95.2(10) . 3_676 ?
O6 W6 O18 157.9(11) . . ?
O20 W6 O18 93.0(10) . . ?
O16 W6 O18 62.8(10) . . ?
O14 W6 O18 94.5(11) 3_676 . ?
O15 W6 O18 62.3(10) . . ?
O19 W6 O18 45.9(9) 3_676 . ?
O23 P1 O23 180(2) . 3_676 ?
O23 P1 O22 61.6(18) . . ?
O23 P1 O22 118.4(18) 3_676 . ?
O23 P1 O22 118.4(18) . 3_676 ?
O23 P1 O22 61.6(18) 3_676 3_676 ?
O22 P1 O22 180(3) . 3_676 ?
O23 P1 O18 70.4(16) . . ?
O23 P1 O18 109.6(16) 3_676 . ?
O22 P1 O18 106.5(17) . . ?
O22 P1 O18 73.5(17) 3_676 . ?
O23 P1 O18 109.6(16) . 3_676 ?
O23 P1 O18 70.4(16) 3_676 3_676 ?
O22 P1 O18 73.5(17) . 3_676 ?
O22 P1 O18 106.5(17) 3_676 3_676 ?
O18 P1 O18 179.999(12) . 3_676 ?
O23 P1 O19 111.1(15) . 3_676 ?
O23 P1 O19 68.9(15) 3_676 3_676 ?
O22 P1 O19 73.3(16) . 3_676 ?
O22 P1 O19 106.7(16) 3_676 3_676 ?
O18 P1 O19 76.6(15) . 3_676 ?
O18 P1 O19 103.4(15) 3_676 3_676 ?
O23 P1 O19 68.9(15) . . ?
O23 P1 O19 111.1(15) 3_676 . ?
O22 P1 O19 106.7(16) . . ?
O22 P1 O19 73.3(16) 3_676 . ?
O18 P1 O19 103.4(15) . . ?
O18 P1 O19 76.6(15) 3_676 . ?
O19 P1 O19 180.0 3_676 . ?
N5 C1 C9 178(3) . . ?
N4 C2 C11 177(3) . . ?
N3 C3 C14 174(3) . . ?
N1 C7 C8 179(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 C9 H9A 109.5 . . ?
C1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C11 H11A 109.5 . . ?
C2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C13 174(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C2S C1S C3S 57(6) . . ?
C1S C2S C3S 77(8) . . ?
C1S C2S C6S 177(9) . . ?
C3S C2S C6S 103(8) . . ?
C1S C2S C4S 131(8) . . ?
C3S C2S C4S 57(7) . . ?
C6S C2S C4S 50(6) . . ?
C5S C3S C2S 131(10) . . ?
C5S C3S C4S 59(8) . . ?
C2S C3S C4S 73(9) . . ?
C5S C3S C1S 173(10) . . ?
C2S C3S C1S 46(5) . . ?
C4S C3S C1S 116(10) . . ?
C5S C3S C6S 91(8) . . ?
C2S C3S C6S 41(5) . . ?
C4S C3S C6S 36(6) . . ?
C1S C3S C6S 87(7) . . ?
C6S C4S C5S 144(10) . . ?
C6S C4S C3S 104(10) . . ?
C5S C4S C3S 53(8) . . ?
C6S C4S C2S 58(7) . . ?
C5S C4S C2S 103(9) . . ?
C3S C4S C2S 50(6) . . ?
C3S C5S C4S 68(9) . . ?
C4S C6S C2S 72(8) . . ?
C4S C6S C3S 40(7) . . ?
C2S C6S C3S 36(5) . . ?
C7 N1 Ni1 173(2) . . ?
C12 N2 Ni1 172(2) . . ?
C3 N3 Ni1 176(2) . . ?
C2 N4 Ni1 170(2) . . ?
C1 N5 Ni1 172(2) . . ?
C10B C15B N6 146(7) . . ?
C15B C10B H10A 109.5 . . ?
C15B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C15B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C15B N6 Ni1 164(3) . . ?

_refine_diff_density_max         2.562
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.416

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

