# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_beata7new
_database_code_depnum_ccdc_archive 'CCDC 1056668'
_audit_update_record             
;
2015-05-12 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C130.60 H98.40 Mo4 N48 Ni8 O14.60'
_chemical_formula_weight         3427.21

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1796(5)
_cell_length_b                   15.6667(7)
_cell_length_c                   21.9922(9)
_cell_angle_alpha                95.044(3)
_cell_angle_beta                 107.310(3)
_cell_angle_gamma                109.261(3)
_cell_volume                     4308.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      25.0

_exptl_crystal_description       needle-like
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             1727
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.196
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7728
_exptl_absorpt_correction_T_max  0.8986
_exptl_absorpt_process_details   'X-red and X-Shape (STOE, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32078
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.407
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             15040
_reflns_number_gt                11128
_reflns_threshold_expression     'I > 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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'

_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)+(0.0984P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         15040
_refine_ls_number_parameters     947
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1630
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Mo1 Mo 0.26907(3) 0.30114(3) 0.54470(2) 0.04647(13) Uani 1 1 d . . . . .
C1 C 0.2806(4) 0.3510(4) 0.6432(3) 0.0541(13) Uani 1 1 d . . . . .
N1 N 0.2944(3) 0.3800(3) 0.6961(2) 0.0549(11) Uani 1 1 d . . . . .
C2 C 0.1365(4) 0.1947(4) 0.5590(3) 0.0523(12) Uani 1 1 d . . . . .
N2 N 0.0668(4) 0.1396(3) 0.5645(3) 0.0648(13) Uani 1 1 d . . . . .
C3 C 0.3566(4) 0.4482(4) 0.5625(3) 0.0525(12) Uani 1 1 d . . . . .
N3 N 0.4013(3) 0.5254(3) 0.5724(2) 0.0564(11) Uani 1 1 d . . . . .
C4 C 0.1687(4) 0.2562(4) 0.4440(3) 0.0530(12) Uani 1 1 d . . . . .
N4 N 0.1156(4) 0.2319(3) 0.3899(3) 0.0602(12) Uani 1 1 d . . . . .
C5 C 0.4156(4) 0.3064(4) 0.6122(3) 0.0522(12) Uani 1 1 d . . . . .
N5 N 0.4977(3) 0.3088(3) 0.6452(2) 0.0570(11) Uani 1 1 d . . . . .
C6 C 0.3742(4) 0.3246(3) 0.4882(3) 0.0520(12) Uani 1 1 d . . . . .
N6 N 0.4299(3) 0.3332(3) 0.4590(2) 0.0556(11) Uani 1 1 d . . . . .
C7 C 0.1531(4) 0.3666(4) 0.5314(3) 0.0563(13) Uani 1 1 d . . . . .
N7 N 0.0924(4) 0.4012(4) 0.5245(3) 0.0721(14) Uani 1 1 d . . . . .
C8 C 0.2798(4) 0.1684(4) 0.5208(3) 0.0542(13) Uani 1 1 d . . . . .
N8 N 0.2856(4) 0.0981(3) 0.5082(2) 0.0589(11) Uani 1 1 d . . . . .
Mo2 Mo 0.73033(3) 0.65311(3) 0.82861(2) 0.05188(14) Uani 1 1 d . . . . .
C11 C 0.8260(4) 0.7133(4) 0.7725(3) 0.0601(14) Uani 1 1 d . . . . .
N11 N 0.8789(4) 0.7445(4) 0.7438(2) 0.0683(14) Uani 1 1 d . . . . .
C12 C 0.5695(4) 0.5626(4) 0.8163(3) 0.0609(14) Uani 1 1 d . . . . .
N12 N 0.4869(3) 0.5104(3) 0.8099(2) 0.0618(12) Uani 1 1 d . . . . .
C13 C 0.6323(4) 0.6535(4) 0.7326(3) 0.0574(14) Uani 1 1 d . . . . .
N13 N 0.5844(3) 0.6568(3) 0.6811(2) 0.0549(11) Uani 1 1 d . . . . .
C14 C 0.7346(4) 0.6139(4) 0.9206(3) 0.0586(14) Uani 1 1 d . . . . .
N14 N 0.7405(4) 0.5906(4) 0.9691(3) 0.0726(15) Uani 1 1 d . . . . .
C15 C 0.8481(5) 0.7793(4) 0.8954(3) 0.0650(15) Uani 1 1 d . . . . .
N15 N 0.9114(5) 0.8460(4) 0.9312(3) 0.0869(17) Uani 1 1 d . . . . .
C16 C 0.8759(4) 0.6267(4) 0.8654(3) 0.0612(14) Uani 1 1 d . . . . .
N16 N 0.9537(4) 0.6118(4) 0.8832(3) 0.0685(14) Uani 1 1 d . . . . .
C17 C 0.7039(4) 0.5217(4) 0.7774(3) 0.0575(14) Uani 1 1 d . . . . .
N17 N 0.6870(3) 0.4487(4) 0.7480(3) 0.0612(12) Uani 1 1 d . . . . .
C18 C 0.6546(6) 0.7478(6) 0.8445(3) 0.0781(18) Uani 1 1 d . . . . .
N18 N 0.6124(6) 0.7957(7) 0.8516(4) 0.116(3) Uani 1 1 d . . . . .
Ni1 Ni 0.47885(5) 0.66402(4) 0.59757(3) 0.05016(18) Uani 1 1 d . . . . .
N21 N 0.3893(3) 0.6840(3) 0.6538(2) 0.0593(12) Uani 1 1 d . . . . .
N22 N 0.5437(3) 0.8082(3) 0.6255(2) 0.0551(11) Uani 1 1 d . . . . .
C21 C 0.3178(5) 0.6205(5) 0.6704(4) 0.0792(19) Uani 1 1 d . . . . .
H21 H 0.2983 0.5570 0.6528 0.095 Uiso 1 1 calc R U . . .
C22 C 0.2705(6) 0.6446(6) 0.7132(4) 0.092(2) Uani 1 1 d . . . . .
H22 H 0.2195 0.5981 0.7243 0.111 Uiso 1 1 calc R U . . .
C23 C 0.2982(6) 0.7353(6) 0.7386(5) 0.097(2) Uani 1 1 d . . . . .
H23 H 0.2652 0.7517 0.7671 0.117 Uiso 1 1 calc R U . . .
C24 C 0.3748(5) 0.8055(5) 0.7236(4) 0.0753(18) Uani 1 1 d . . . . .
C25 C 0.4089(6) 0.8991(6) 0.7476(4) 0.086(2) Uani 1 1 d . . . . .
H25 H 0.3792 0.9195 0.7767 0.103 Uiso 1 1 calc R U . . .
C26 C 0.4838(5) 0.9636(5) 0.7311(4) 0.084(2) Uani 1 1 d . . . . .
H26 H 0.5044 1.0275 0.7481 0.101 Uiso 1 1 calc R U . . .
C27 C 0.5313(5) 0.9352(4) 0.6884(3) 0.0684(16) Uani 1 1 d . . . . .
C28 C 0.6108(5) 0.9977(4) 0.6719(4) 0.0760(18) Uani 1 1 d . . . . .
H28 H 0.6321 1.0624 0.6862 0.091 Uiso 1 1 calc R U . . .
C29 C 0.6582(5) 0.9631(4) 0.6341(4) 0.0763(19) Uani 1 1 d . . . . .
H29 H 0.7145 1.0038 0.6233 0.092 Uiso 1 1 calc R U . . .
C30 C 0.6224(5) 0.8686(4) 0.6124(3) 0.0672(16) Uani 1 1 d . . . . .
H30 H 0.6557 0.8458 0.5868 0.081 Uiso 1 1 calc R U . . .
C31 C 0.4990(4) 0.8400(4) 0.6629(3) 0.0610(14) Uani 1 1 d . . . . .
C32 C 0.4175(4) 0.7737(4) 0.6798(3) 0.0619(14) Uani 1 1 d . . . . .
Ni2 Ni 0.65850(5) 0.33937(5) 0.68037(4) 0.05538(19) Uani 1 1 d . . . . .
N41 N 0.6497(3) 0.2378(3) 0.6098(2) 0.0597(11) Uani 1 1 d . . . . .
N42 N 0.8204(3) 0.3680(3) 0.6997(2) 0.0584(11) Uani 1 1 d . . . . .
C41 C 0.5637(5) 0.1737(4) 0.5650(3) 0.0654(15) Uani 1 1 d . . . . .
H41 H 0.4953 0.1681 0.5658 0.078 Uiso 1 1 calc R U . . .
C42 C 0.5711(6) 0.1148(4) 0.5173(4) 0.0756(18) Uani 1 1 d . . . . .
H42 H 0.5078 0.0692 0.4866 0.091 Uiso 1 1 calc R U . . .
C43 C 0.6671(6) 0.1210(4) 0.5135(4) 0.0760(18) Uani 1 1 d . . . . .
H43 H 0.6714 0.0813 0.4800 0.091 Uiso 1 1 calc R U . . .
C44 C 0.7607(5) 0.1884(4) 0.5607(3) 0.0655(15) Uani 1 1 d . . . . .
C45 C 0.8658(5) 0.2034(5) 0.5619(4) 0.0748(17) Uani 1 1 d . . . . .
H45 H 0.8753 0.1655 0.5300 0.090 Uiso 1 1 calc R U . . .
C46 C 0.9513(5) 0.2689(5) 0.6064(4) 0.0748(18) Uani 1 1 d . . . . .
H46 H 1.0203 0.2774 0.6054 0.090 Uiso 1 1 calc R U . . .
C47 C 0.9396(5) 0.3267(4) 0.6557(3) 0.0664(16) Uani 1 1 d . . . . .
C48 C 1.0268(5) 0.3959(5) 0.7057(4) 0.0746(18) Uani 1 1 d . . . . .
H48 H 1.0977 0.4060 0.7079 0.089 Uiso 1 1 calc R U . . .
C49 C 1.0084(5) 0.4479(5) 0.7507(4) 0.0762(19) Uani 1 1 d . . . . .
H49 H 1.0662 0.4939 0.7847 0.091 Uiso 1 1 calc R U . . .
C50 C 0.9033(4) 0.4326(4) 0.7460(3) 0.0679(16) Uani 1 1 d . . . . .
H50 H 0.8909 0.4697 0.7770 0.081 Uiso 1 1 calc R U . . .
C51 C 0.8378(4) 0.3157(4) 0.6559(3) 0.0578(13) Uani 1 1 d . . . . .
C52 C 0.7470(4) 0.2447(4) 0.6076(3) 0.0575(13) Uani 1 1 d . . . . .
Ni3 Ni 0.35785(5) 0.39248(5) 0.79482(4) 0.05508(19) Uani 1 1 d . . . . .
N61 N 0.2302(4) 0.2747(3) 0.7922(2) 0.0602(12) Uani 1 1 d . . . . .
N62 N 0.4119(3) 0.3735(3) 0.8901(2) 0.0597(12) Uani 1 1 d . . . . .
C61 C 0.1414(5) 0.2278(4) 0.7437(3) 0.0700(17) Uani 1 1 d . . . . .
H61 H 0.1336 0.2422 0.7019 0.084 Uiso 1 1 calc R U . . .
C62 C 0.0576(5) 0.1572(5) 0.7516(4) 0.083(2) Uani 1 1 d . . . . .
H62 H -0.0056 0.1240 0.7153 0.100 Uiso 1 1 calc R U . . .
C63 C 0.0668(5) 0.1364(5) 0.8108(4) 0.086(2) Uani 1 1 d . . . . .
H63 H 0.0094 0.0894 0.8166 0.104 Uiso 1 1 calc R U . . .
C64 C 0.1608(5) 0.1838(4) 0.8637(3) 0.0677(16) Uani 1 1 d . . . . .
C65 C 0.1793(6) 0.1632(5) 0.9272(4) 0.083(2) Uani 1 1 d . . . . .
H65 H 0.1242 0.1165 0.9352 0.099 Uiso 1 1 calc R U . . .
C66 C 0.2731(6) 0.2084(5) 0.9761(4) 0.0811(19) Uani 1 1 d . . . . .
H66 H 0.2846 0.1922 1.0176 0.097 Uiso 1 1 calc R U . . .
C67 C 0.3562(5) 0.2817(5) 0.9649(3) 0.0686(16) Uani 1 1 d . . . . .
C68 C 0.4574(5) 0.3331(5) 1.0136(3) 0.0781(19) Uani 1 1 d . . . . .
H68 H 0.4730 0.3206 1.0562 0.094 Uiso 1 1 calc R U . . .
C69 C 0.5313(5) 0.3997(6) 0.9990(4) 0.083(2) Uani 1 1 d . . . . .
H69 H 0.5999 0.4326 1.0307 0.100 Uiso 1 1 calc R U . . .
C70 C 0.5061(5) 0.4200(5) 0.9368(3) 0.0690(17) Uani 1 1 d . . . . .
H70 H 0.5578 0.4684 0.9276 0.083 Uiso 1 1 calc R U . . .
C71 C 0.3386(4) 0.3042(4) 0.9035(3) 0.0624(14) Uani 1 1 d . . . . .
C72 C 0.2409(4) 0.2541(4) 0.8522(3) 0.0577(13) Uani 1 1 d . . . . .
Ni4 Ni 0.98164(5) 0.82142(6) 0.70446(4) 0.0615(2) Uani 1 1 d . . . . .
N81 N 1.0968(4) 0.8854(4) 0.7972(3) 0.0701(14) Uani 1 1 d . . . . .
N82 N 1.1004(4) 0.9141(4) 0.6788(3) 0.0675(14) Uani 1 1 d . . . . .
C81 C 1.0950(5) 0.8720(6) 0.8554(3) 0.084(2) Uani 1 1 d . . . . .
H81 H 1.0345 0.8247 0.8577 0.101 Uiso 1 1 calc R U . . .
C82 C 1.1756(6) 0.9225(7) 0.9129(4) 0.097(2) Uani 1 1 d . . . . .
H82 H 1.1698 0.9109 0.9536 0.116 Uiso 1 1 calc R U . . .
C83 C 1.2640(6) 0.9896(7) 0.9101(4) 0.096(2) Uani 1 1 d . . . . .
H83 H 1.3227 1.0227 0.9488 0.115 Uiso 1 1 calc R U . . .
C84 C 1.2672(5) 1.0084(5) 0.8514(4) 0.0776(18) Uani 1 1 d . . . . .
C85 C 1.3542(5) 1.0843(5) 0.8434(5) 0.094(3) Uani 1 1 d . . . . .
H85 H 1.4124 1.1232 0.8807 0.113 Uiso 1 1 calc R U . . .
C86 C 1.3518(5) 1.0994(5) 0.7832(6) 0.098(3) Uani 1 1 d . . . . .
H86 H 1.4088 1.1490 0.7794 0.118 Uiso 1 1 calc R U . . .
C87 C 1.2681(5) 1.0442(5) 0.7265(4) 0.078(2) Uani 1 1 d . . . . .
C88 C 1.2633(6) 1.0551(5) 0.6623(5) 0.092(3) Uani 1 1 d . . . . .
H88 H 1.3187 1.1035 0.6560 0.110 Uiso 1 1 calc R U . . .
C89 C 1.1813(6) 0.9979(6) 0.6107(4) 0.085(2) Uani 1 1 d . . . . .
H89 H 1.1782 1.0058 0.5680 0.101 Uiso 1 1 calc R U . . .
C90 C 1.1004(5) 0.9264(5) 0.6201(4) 0.080(2) Uani 1 1 d . . . . .
H90 H 1.0434 0.8853 0.5831 0.096 Uiso 1 1 calc R U . . .
C91 C 1.1823(4) 0.9712(4) 0.7312(4) 0.0688(16) Uani 1 1 d . . . . .
C92 C 1.1833(4) 0.9557(4) 0.7953(3) 0.0666(15) Uani 1 1 d . . . . .
O1 O 0.3576(3) 0.6722(3) 0.5148(2) 0.0596(9) Uani 1 1 d . . . . .
O2 O 0.6466(3) 0.2466(3) 0.7430(2) 0.0678(11) Uani 1 1 d . . . . .
O3 O 0.6700(4) 0.4289(3) 0.6095(2) 0.0778(12) Uani 1 1 d . . . . .
C95 C 0.6345(10) 0.4958(9) 0.6017(6) 0.097(3) Uani 0.7 1 d . . P A 1
H95A H 0.6515 0.5234 0.5661 0.146 Uiso 0.7 1 calc R U P A 1
H95B H 0.5571 0.4711 0.5912 0.146 Uiso 0.7 1 calc R U P A 1
H95C H 0.6682 0.5430 0.6420 0.146 Uiso 0.7 1 calc R U P A 1
C95' C 0.7343(16) 0.5166(14) 0.6152(10) 0.065(5) Uani 0.3 1 d . . P A 2
H95D H 0.7168 0.5344 0.5729 0.098 Uiso 0.3 1 calc R U P A 2
H95E H 0.7244 0.5577 0.6470 0.098 Uiso 0.3 1 calc R U P A 2
H95F H 0.8087 0.5215 0.6300 0.098 Uiso 0.3 1 calc R U P A 2
O4 O 0.4467(3) 0.3169(3) 0.7732(2) 0.0621(10) Uani 1 1 d . . . . .
O5 O 0.2737(3) 0.4709(3) 0.8179(2) 0.0620(10) Uani 1 1 d . . . . .
O6 O 0.9230(4) 0.9268(3) 0.7084(2) 0.0710(12) Uani 1 1 d . . . . .
C96 C 0.862(2) 0.9222(18) 0.7331(18) 0.115(13) Uani 0.3 1 d . . P . .
H96A H 0.8431 0.9768 0.7307 0.172 Uiso 0.3 1 calc R U P . .
H96B H 0.7984 0.8665 0.7110 0.172 Uiso 0.3 1 calc R U P . .
H96C H 0.8926 0.9194 0.7788 0.172 Uiso 0.3 1 calc R U P . .
O7 O 1.0461(3) 0.7188(4) 0.6999(2) 0.0809(13) Uani 1 1 d . . . . .
O8 O 0.8496(17) 0.5615(17) 0.6190(18) 0.161(12) Uani 0.3 1 d . . P B 1


_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
Mo1 C5 2.135(6) . ?
Mo1 C4 2.149(6) . ?
Mo1 C3 2.160(5) . ?
Mo1 C8 2.165(7) . ?
Mo1 C7 2.172(7) . ?
Mo1 C6 2.174(6) . ?
Mo1 C1 2.177(7) . ?
Mo1 C2 2.188(5) . ?
C1 N1 1.143(7) . ?
N1 Ni3 2.052(5) . ?
C2 N2 1.124(6) . ?
C3 N3 1.131(7) . ?
N3 Ni1 2.021(4) . ?
C4 N4 1.151(7) . ?
N4 Ni4 2.034(5) 2_666 ?
C5 N5 1.159(7) . ?
N5 Ni2 2.048(4) . ?
C6 N6 1.140(7) . ?
N6 Ni1 2.038(5) 2_666 ?
C7 N7 1.142(8) . ?
C8 N8 1.147(8) . ?
Mo2 C17 2.117(7) . ?
Mo2 C11 2.147(5) . ?
Mo2 C13 2.156(6) . ?
Mo2 C14 2.156(5) . ?
Mo2 C18 2.158(8) . ?
Mo2 C15 2.169(6) . ?
Mo2 C16 2.171(6) . ?
Mo2 C12 2.172(5) . ?
C11 N11 1.138(7) . ?
N11 Ni4 2.023(5) . ?
C12 N12 1.145(7) . ?
N12 Ni3 2.042(4) . ?
C13 N13 1.150(7) . ?
N13 Ni1 2.035(5) . ?
C14 N14 1.145(7) . ?
C15 N15 1.155(8) . ?
C16 N16 1.163(7) . ?
C17 N17 1.175(8) . ?
N17 Ni2 2.011(6) . ?
C18 N18 1.131(10) . ?
Ni1 N6 2.038(5) 2_666 ?
Ni1 N21 2.090(5) . ?
Ni1 N22 2.092(4) . ?
Ni1 O1 2.148(4) . ?
N21 C21 1.332(7) . ?
N21 C32 1.346(8) . ?
N22 C30 1.329(7) . ?
N22 C31 1.332(8) . ?
C21 C22 1.398(11) . ?
C22 C23 1.359(12) . ?
C23 C24 1.410(10) . ?
C24 C25 1.382(11) . ?
C24 C32 1.416(9) . ?
C25 C26 1.366(10) . ?
C26 C27 1.426(10) . ?
C27 C28 1.392(9) . ?
C27 C31 1.413(9) . ?
C28 C29 1.390(11) . ?
C29 C30 1.382(10) . ?
C31 C32 1.443(7) . ?
Ni2 N41 2.067(5) . ?
Ni2 N42 2.087(4) . ?
Ni2 O2 2.091(4) . ?
Ni2 O3 2.192(4) . ?
N41 C41 1.330(8) . ?
N41 C52 1.364(7) . ?
N42 C50 1.328(8) . ?
N42 C51 1.340(8) . ?
C41 C42 1.388(10) . ?
C42 C43 1.361(10) . ?
C43 C44 1.420(9) . ?
C44 C52 1.397(9) . ?
C44 C45 1.421(9) . ?
C45 C46 1.333(10) . ?
C46 C47 1.435(10) . ?
C47 C51 1.398(8) . ?
C47 C48 1.417(10) . ?
C48 C49 1.364(11) . ?
C49 C50 1.399(9) . ?
C51 C52 1.435(8) . ?
Ni3 N62 2.091(5) . ?
Ni3 N61 2.098(4) . ?
Ni3 O5 2.099(4) . ?
Ni3 O4 2.112(4) . ?
N61 C61 1.309(8) . ?
N61 C72 1.363(7) . ?
N62 C70 1.334(7) . ?
N62 C71 1.356(7) . ?
C61 C62 1.397(8) . ?
C62 C63 1.351(10) . ?
C63 C64 1.397(10) . ?
C64 C72 1.400(7) . ?
C64 C65 1.430(9) . ?
C65 C66 1.350(10) . ?
C66 C67 1.449(9) . ?
C67 C71 1.395(8) . ?
C67 C68 1.424(10) . ?
C68 C69 1.352(9) . ?
C69 C70 1.399(9) . ?
C71 C72 1.417(8) . ?
Ni4 N4 2.034(5) 2_666 ?
Ni4 O6 2.085(5) . ?
Ni4 N82 2.087(4) . ?
Ni4 N81 2.100(5) . ?
Ni4 O7 2.104(5) . ?
N81 C81 1.320(8) . ?
N81 C92 1.367(7) . ?
N82 C90 1.321(8) . ?
N82 C91 1.347(9) . ?
C81 C82 1.378(10) . ?
C82 C83 1.366(12) . ?
C83 C84 1.361(11) . ?
C84 C92 1.384(9) . ?
C84 C85 1.470(10) . ?
C85 C86 1.357(13) . ?
C86 C87 1.402(12) . ?
C87 C91 1.405(8) . ?
C87 C88 1.421(12) . ?
C88 C89 1.338(12) . ?
C89 C90 1.396(9) . ?
C91 C92 1.449(9) . ?
O3 C95 1.308(13) . ?
O3 C95' 1.345(19) . ?
O6 C96 1.13(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 Mo1 C4 143.3(2) . . ?
C5 Mo1 C3 81.97(19) . . ?
C4 Mo1 C3 107.96(19) . . ?
C5 Mo1 C8 73.4(2) . . ?
C4 Mo1 C8 78.7(2) . . ?
C3 Mo1 C8 142.61(19) . . ?
C5 Mo1 C7 141.9(2) . . ?
C4 Mo1 C7 73.3(2) . . ?
C3 Mo1 C7 73.17(19) . . ?
C8 Mo1 C7 141.05(19) . . ?
C5 Mo1 C6 76.8(2) . . ?
C4 Mo1 C6 73.30(19) . . ?
C3 Mo1 C6 72.0(2) . . ?
C8 Mo1 C6 75.20(18) . . ?
C7 Mo1 C6 120.2(2) . . ?
C5 Mo1 C1 70.5(2) . . ?
C4 Mo1 C1 145.75(19) . . ?
C3 Mo1 C1 76.19(19) . . ?
C8 Mo1 C1 119.3(2) . . ?
C7 Mo1 C1 75.7(2) . . ?
C6 Mo1 C1 136.85(18) . . ?
C5 Mo1 C2 109.14(19) . . ?
C4 Mo1 C2 83.6(2) . . ?
C3 Mo1 C2 144.4(2) . . ?
C8 Mo1 C2 71.81(19) . . ?
C7 Mo1 C2 78.58(19) . . ?
C6 Mo1 C2 142.7(2) . . ?
C1 Mo1 C2 76.16(19) . . ?
N1 C1 Mo1 175.0(4) . . ?
C1 N1 Ni3 153.4(5) . . ?
N2 C2 Mo1 178.0(5) . . ?
N3 C3 Mo1 178.8(5) . . ?
C3 N3 Ni1 175.0(5) . . ?
N4 C4 Mo1 179.4(5) . . ?
C4 N4 Ni4 175.5(5) . 2_666 ?
N5 C5 Mo1 175.2(5) . . ?
C5 N5 Ni2 159.7(4) . . ?
N6 C6 Mo1 176.9(5) . . ?
C6 N6 Ni1 174.6(4) . 2_666 ?
N7 C7 Mo1 179.8(7) . . ?
N8 C8 Mo1 179.9(7) . . ?
C17 Mo2 C11 87.9(2) . . ?
C17 Mo2 C13 79.1(2) . . ?
C11 Mo2 C13 68.85(19) . . ?
C17 Mo2 C14 96.6(2) . . ?
C11 Mo2 C14 144.5(2) . . ?
C13 Mo2 C14 146.61(18) . . ?
C17 Mo2 C18 144.1(2) . . ?
C11 Mo2 C18 105.3(3) . . ?
C13 Mo2 C18 75.1(2) . . ?
C14 Mo2 C18 91.5(3) . . ?
C17 Mo2 C15 145.5(2) . . ?
C11 Mo2 C15 77.3(2) . . ?
C13 Mo2 C15 122.1(2) . . ?
C14 Mo2 C15 79.5(2) . . ?
C18 Mo2 C15 70.3(3) . . ?
C17 Mo2 C16 72.2(2) . . ?
C11 Mo2 C16 74.1(2) . . ?
C13 Mo2 C16 133.4(2) . . ?
C14 Mo2 C16 73.9(2) . . ?
C18 Mo2 C16 143.2(2) . . ?
C15 Mo2 C16 73.9(2) . . ?
C17 Mo2 C12 72.7(2) . . ?
C11 Mo2 C12 140.8(2) . . ?
C13 Mo2 C12 74.12(19) . . ?
C14 Mo2 C12 73.0(2) . . ?
C18 Mo2 C12 76.5(3) . . ?
C15 Mo2 C12 135.9(2) . . ?
C16 Mo2 C12 127.6(2) . . ?
N11 C11 Mo2 178.2(5) . . ?
C11 N11 Ni4 169.7(6) . . ?
N12 C12 Mo2 175.7(6) . . ?
C12 N12 Ni3 164.6(5) . . ?
N13 C13 Mo2 176.6(4) . . ?
C13 N13 Ni1 169.1(5) . . ?
N14 C14 Mo2 176.2(6) . . ?
N15 C15 Mo2 179.4(7) . . ?
N16 C16 Mo2 177.9(6) . . ?
N17 C17 Mo2 178.4(5) . . ?
C17 N17 Ni2 166.5(5) . . ?
N18 C18 Mo2 178.1(7) . . ?
N3 Ni1 N13 92.70(18) . . ?
N3 Ni1 N6 94.39(19) . 2_666 ?
N13 Ni1 N6 96.91(19) . 2_666 ?
N3 Ni1 N21 94.31(18) . . ?
N13 Ni1 N21 86.77(19) . . ?
N6 Ni1 N21 170.38(18) 2_666 . ?
N3 Ni1 N22 173.48(19) . . ?
N13 Ni1 N22 89.57(18) . . ?
N6 Ni1 N22 91.40(18) 2_666 . ?
N21 Ni1 N22 79.71(18) . . ?
N3 Ni1 O1 87.15(17) . . ?
N13 Ni1 O1 174.39(17) . . ?
N6 Ni1 O1 88.70(17) 2_666 . ?
N21 Ni1 O1 87.64(17) . . ?
N22 Ni1 O1 89.98(17) . . ?
C21 N21 C32 118.6(6) . . ?
C21 N21 Ni1 128.3(5) . . ?
C32 N21 Ni1 112.7(3) . . ?
C30 N22 C31 118.4(5) . . ?
C30 N22 Ni1 129.0(4) . . ?
C31 N22 Ni1 112.5(3) . . ?
N21 C21 C22 121.8(7) . . ?
C23 C22 C21 119.3(7) . . ?
C22 C23 C24 121.3(8) . . ?
C25 C24 C23 125.5(7) . . ?
C25 C24 C32 119.7(6) . . ?
C23 C24 C32 114.8(7) . . ?
C26 C25 C24 122.5(7) . . ?
C25 C26 C27 120.1(7) . . ?
C28 C27 C31 118.3(7) . . ?
C28 C27 C26 122.4(6) . . ?
C31 C27 C26 119.2(6) . . ?
C29 C28 C27 118.3(6) . . ?
C30 C29 C28 119.1(6) . . ?
N22 C30 C29 123.3(7) . . ?
N22 C31 C27 122.4(5) . . ?
N22 C31 C32 118.1(6) . . ?
C27 C31 C32 119.4(6) . . ?
N21 C32 C24 124.1(5) . . ?
N21 C32 C31 116.8(6) . . ?
C24 C32 C31 119.0(6) . . ?
N17 Ni2 N5 93.62(19) . . ?
N17 Ni2 N41 171.86(18) . . ?
N5 Ni2 N41 93.03(19) . . ?
N17 Ni2 N42 92.94(19) . . ?
N5 Ni2 N42 170.3(2) . . ?
N41 Ni2 N42 79.90(19) . . ?
N17 Ni2 O2 94.46(19) . . ?
N5 Ni2 O2 93.35(17) . . ?
N41 Ni2 O2 89.83(19) . . ?
N42 Ni2 O2 93.25(17) . . ?
N17 Ni2 O3 89.53(19) . . ?
N5 Ni2 O3 86.78(18) . . ?
N41 Ni2 O3 86.16(19) . . ?
N42 Ni2 O3 86.15(18) . . ?
O2 Ni2 O3 175.99(19) . . ?
C41 N41 C52 118.0(6) . . ?
C41 N41 Ni2 128.8(4) . . ?
C52 N41 Ni2 113.0(4) . . ?
C50 N42 C51 119.0(5) . . ?
C50 N42 Ni2 128.5(5) . . ?
C51 N42 Ni2 112.4(4) . . ?
N41 C41 C42 121.8(6) . . ?
C43 C42 C41 121.4(6) . . ?
C42 C43 C44 118.3(7) . . ?
C52 C44 C43 117.0(6) . . ?
C52 C44 C45 118.7(6) . . ?
C43 C44 C45 124.3(7) . . ?
C46 C45 C44 122.3(7) . . ?
C45 C46 C47 120.2(6) . . ?
C51 C47 C48 116.8(6) . . ?
C51 C47 C46 119.7(6) . . ?
C48 C47 C46 123.5(6) . . ?
C49 C48 C47 119.7(6) . . ?
C48 C49 C50 119.2(6) . . ?
N42 C50 C49 122.2(7) . . ?
N42 C51 C47 123.1(6) . . ?
N42 C51 C52 117.9(5) . . ?
C47 C51 C52 119.0(6) . . ?
N41 C52 C44 123.5(5) . . ?
N41 C52 C51 116.4(5) . . ?
C44 C52 C51 120.2(5) . . ?
N12 Ni3 N1 95.89(18) . . ?
N12 Ni3 N62 93.90(18) . . ?
N1 Ni3 N62 167.3(2) . . ?
N12 Ni3 N61 172.8(2) . . ?
N1 Ni3 N61 91.16(18) . . ?
N62 Ni3 N61 79.36(18) . . ?
N12 Ni3 O5 90.49(18) . . ?
N1 Ni3 O5 94.98(18) . . ?
N62 Ni3 O5 92.98(18) . . ?
N61 Ni3 O5 87.25(18) . . ?
N12 Ni3 O4 87.97(18) . . ?
N1 Ni3 O4 85.82(18) . . ?
N62 Ni3 O4 86.49(18) . . ?
N61 Ni3 O4 94.20(18) . . ?
O5 Ni3 O4 178.33(16) . . ?
C61 N61 C72 118.8(5) . . ?
C61 N61 Ni3 128.8(4) . . ?
C72 N61 Ni3 112.0(4) . . ?
C70 N62 C71 118.7(5) . . ?
C70 N62 Ni3 128.4(4) . . ?
C71 N62 Ni3 113.0(4) . . ?
N61 C61 C62 122.2(6) . . ?
C63 C62 C61 119.7(6) . . ?
C62 C63 C64 120.0(5) . . ?
C63 C64 C72 117.0(6) . . ?
C63 C64 C65 123.6(5) . . ?
C72 C64 C65 119.3(6) . . ?
C66 C65 C64 121.5(6) . . ?
C65 C66 C67 119.5(6) . . ?
C71 C67 C68 117.0(5) . . ?
C71 C67 C66 119.7(6) . . ?
C68 C67 C66 123.3(6) . . ?
C69 C68 C67 119.7(6) . . ?
C68 C69 C70 119.7(6) . . ?
N62 C70 C69 122.1(6) . . ?
N62 C71 C67 122.7(5) . . ?
N62 C71 C72 117.2(5) . . ?
C67 C71 C72 120.1(5) . . ?
N61 C72 C64 122.3(5) . . ?
N61 C72 C71 117.8(5) . . ?
C64 C72 C71 119.8(5) . . ?
N11 Ni4 N4 95.98(19) . 2_666 ?
N11 Ni4 O6 91.4(2) . . ?
N4 Ni4 O6 90.8(2) 2_666 . ?
N11 Ni4 N82 170.8(2) . . ?
N4 Ni4 N82 92.80(19) 2_666 . ?
O6 Ni4 N82 85.9(2) . . ?
N11 Ni4 N81 91.16(19) . . ?
N4 Ni4 N81 172.81(18) 2_666 . ?
O6 Ni4 N81 89.7(2) . . ?
N82 Ni4 N81 80.1(2) . . ?
N11 Ni4 O7 90.8(2) . . ?
N4 Ni4 O7 89.6(2) 2_666 . ?
O6 Ni4 O7 177.73(17) . . ?
N82 Ni4 O7 91.9(2) . . ?
N81 Ni4 O7 89.6(2) . . ?
C81 N81 C92 116.8(6) . . ?
C81 N81 Ni4 130.5(4) . . ?
C92 N81 Ni4 112.6(4) . . ?
C90 N82 C91 118.9(5) . . ?
C90 N82 Ni4 128.6(5) . . ?
C91 N82 Ni4 112.3(4) . . ?
N81 C81 C82 124.0(7) . . ?
C83 C82 C81 118.5(8) . . ?
C84 C83 C82 119.4(7) . . ?
C83 C84 C92 119.2(6) . . ?
C83 C84 C85 123.7(7) . . ?
C92 C84 C85 117.0(7) . . ?
C86 C85 C84 120.5(7) . . ?
C85 C86 C87 122.3(6) . . ?
C86 C87 C91 119.7(8) . . ?
C86 C87 C88 124.5(7) . . ?
C91 C87 C88 115.8(7) . . ?
C89 C88 C87 120.5(6) . . ?
C88 C89 C90 119.7(7) . . ?
N82 C90 C89 122.1(8) . . ?
N82 C91 C87 123.0(7) . . ?
N82 C91 C92 118.6(5) . . ?
C87 C91 C92 118.4(6) . . ?
N81 C92 C84 121.9(6) . . ?
N81 C92 C91 116.0(5) . . ?
C84 C92 C91 122.1(6) . . ?
C95 O3 Ni2 128.1(6) . . ?
C95' O3 Ni2 132.0(9) . . ?
C96 O6 Ni4 119.8(13) . . ?

_refine_diff_density_max         0.724
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.093
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.082 0.418 0.500 961.1 211.4
2 0.500 1.000 1.000 174.2 45.4
3 0.406 0.511 0.096 13.5 7.5
4 0.593 0.489 0.904 13.5 8.1
_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_beata2new
_database_code_depnum_ccdc_archive 'CCDC 1056669'
_audit_update_record             
;
2015-03-27 deposited with the CCDC.
2015-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C116 H130 N48 Ni8 O29 W4'
_chemical_formula_weight         3865.75

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'

_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                   13.6083(3)
_cell_length_b                   20.4045(3)
_cell_length_c                   28.7109(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.4260(10)
_cell_angle_gamma                90
_cell_volume                     7785.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_F_000             3828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    3.963
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4894
_exptl_absorpt_correction_T_max  0.6093
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48958
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.234
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             13708
_reflns_number_gt                10336
_reflns_threshold_expression     'I > 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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0639P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13708
_refine_ls_number_parameters     953
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
W2 W 0.48645(3) 0.78261(2) 0.62657(2) 0.04074(10) Uani 1 1 d . . . . .
C11 C 0.3811(7) 0.7047(3) 0.6342(3) 0.049(2) Uani 1 1 d . . . . .
N11 N 0.3280(6) 0.6648(3) 0.6419(3) 0.0511(18) Uani 1 1 d . . . . .
C17 C 0.4134(7) 0.7649(3) 0.5546(3) 0.0426(19) Uani 1 1 d . . . . .
N17 N 0.3778(6) 0.7529(3) 0.5148(3) 0.0455(16) Uani 1 1 d . . . . .
C18 C 0.6356(9) 0.7905(4) 0.6709(3) 0.055(2) Uani 1 1 d . . . . .
N18 N 0.7162(8) 0.7952(4) 0.6946(3) 0.068(2) Uani 1 1 d . . . . .
C12 C 0.5867(6) 0.8043(3) 0.5791(3) 0.0392(17) Uani 1 1 d . . . . .
N12 N 0.6366(6) 0.8161(3) 0.5525(3) 0.0454(16) Uani 1 1 d . . . . .
C13 C 0.5545(7) 0.6883(3) 0.6205(3) 0.0426(18) Uani 1 1 d . . . . .
N13 N 0.5863(5) 0.6381(3) 0.6167(3) 0.0447(16) Uani 1 1 d . . . . .
C16 C 0.3399(8) 0.8259(3) 0.6201(3) 0.049(2) Uani 1 1 d . . . . .
N16 N 0.2583(7) 0.8473(3) 0.6179(3) 0.061(2) Uani 1 1 d . . . . .
C15 C 0.4715(8) 0.7846(4) 0.6996(3) 0.054(2) Uani 1 1 d . . . . .
N15 N 0.4596(8) 0.7819(4) 0.7379(3) 0.074(3) Uani 1 1 d . . . . .
C14 C 0.5072(7) 0.8883(4) 0.6321(3) 0.0464(19) Uani 1 1 d . . . . .
N14 N 0.5169(6) 0.9450(3) 0.6348(3) 0.056(2) Uani 1 1 d . . . . .
W1 W 0.35948(2) 0.38787(2) 0.58051(2) 0.03378(9) Uani 1 1 d . . . . .
C6 C 0.4820(6) 0.4573(3) 0.5868(3) 0.0387(17) Uani 1 1 d . . . . .
N6 N 0.5483(5) 0.4933(3) 0.5925(2) 0.0389(14) Uani 1 1 d . . . . .
C1 C 0.3057(6) 0.2988(3) 0.5435(3) 0.0385(17) Uani 1 1 d . . . . .
N1 N 0.2838(5) 0.2506(3) 0.5239(3) 0.0396(15) Uani 1 1 d . . . . .
C8 C 0.4464(7) 0.3742(3) 0.6524(3) 0.0435(19) Uani 1 1 d . . . . .
N8 N 0.4909(7) 0.3693(4) 0.6912(3) 0.062(2) Uani 1 1 d . . . . .
C2 C 0.2604(6) 0.3434(4) 0.6216(3) 0.0439(19) Uani 1 1 d . . . . .
N2 N 0.2052(6) 0.3206(4) 0.6418(3) 0.0550(19) Uani 1 1 d . . . . .
C5 C 0.4882(7) 0.3294(4) 0.5737(3) 0.047(2) Uani 1 1 d . . . . .
N5 N 0.5577(6) 0.3006(3) 0.5688(3) 0.0507(18) Uani 1 1 d . . . . .
C3 C 0.3679(7) 0.4119(4) 0.5084(3) 0.045(2) Uani 1 1 d . . . . .
N3 N 0.3654(6) 0.4225(3) 0.4696(3) 0.0506(18) Uani 1 1 d . . . . .
C4 C 0.3195(6) 0.4745(3) 0.6142(3) 0.0398(18) Uani 1 1 d . . . . .
N4 N 0.2994(6) 0.5213(3) 0.6328(3) 0.0456(17) Uani 1 1 d . . . . .
C7 C 0.2107(7) 0.4159(4) 0.5422(3) 0.054(2) Uani 1 1 d . . . . .
N7 N 0.1320(8) 0.4317(5) 0.5229(4) 0.090(3) Uani 1 1 d . . . . .
Ni4 Ni 0.25901(9) 0.59323(4) 0.67262(4) 0.0446(3) Uani 1 1 d . . . . .
N21 N 0.2054(6) 0.6562(3) 0.7180(3) 0.0504(18) Uani 1 1 d . . . . .
N22 N 0.1950(6) 0.5275(3) 0.7124(3) 0.0505(18) Uani 1 1 d . . . . .
C21 C 0.2085(8) 0.7218(4) 0.7167(4) 0.061(3) Uani 1 1 d . . . . .
H21 H 0.2353 0.7429 0.6926 0.073 Uiso 1 1 calc R U . . .
C22 C 0.1742(8) 0.7585(4) 0.7491(4) 0.065(3) Uani 1 1 d . . . . .
H22 H 0.1776 0.8049 0.7475 0.078 Uiso 1 1 calc R U . . .
C23 C 0.1345(8) 0.7296(4) 0.7844(4) 0.062(3) Uani 1 1 d . . . . .
H23 H 0.1120 0.7554 0.8075 0.075 Uiso 1 1 calc R U . . .
C24 C 0.1284(7) 0.6624(4) 0.7852(3) 0.053(2) Uani 1 1 d . . . . .
H24 H 0.0999 0.6408 0.8085 0.064 Uiso 1 1 calc R U . . .
C25 C 0.1647(7) 0.6263(4) 0.7511(3) 0.051(2) Uani 1 1 d . . . . .
C26 C 0.1607(7) 0.5540(4) 0.7489(3) 0.049(2) Uani 1 1 d . . . . .
C27 C 0.1264(8) 0.5143(4) 0.7814(3) 0.056(2) Uani 1 1 d . . . . .
H27 H 0.1036 0.5338 0.8073 0.067 Uiso 1 1 calc R U . . .
C28 C 0.1251(8) 0.4481(4) 0.7766(3) 0.057(2) Uani 1 1 d . . . . .
H28 H 0.1009 0.4211 0.7987 0.069 Uiso 1 1 calc R U . . .
C29 C 0.1593(7) 0.4207(4) 0.7394(4) 0.057(2) Uani 1 1 d . . . . .
H29 H 0.1601 0.3744 0.7356 0.068 Uiso 1 1 calc R U . . .
C30 C 0.1925(8) 0.4615(4) 0.7075(3) 0.058(2) Uani 1 1 d . . . . .
H30 H 0.2144 0.4426 0.6813 0.070 Uiso 1 1 calc R U . . .
O61 O 0.1227(5) 0.6065(3) 0.6207(3) 0.0638(17) Uani 1 1 d D . . . .
C61 C 0.0489(19) 0.5584(12) 0.6150(11) 0.102(8) Uiso 0.5 1 d D . P A 1
H61A H -0.0086 0.5717 0.5899 0.152 Uiso 0.5 1 calc R U P A 1
H61B H 0.0762 0.5170 0.6059 0.152 Uiso 0.5 1 calc R U P A 1
H61C H 0.0269 0.5525 0.6450 0.152 Uiso 0.5 1 calc R U P A 1
O1W O -0.025(3) 0.5135(17) 0.5700(13) 0.185(12) Uiso 0.5 1 d . . P B 2
O62 O 0.3895(6) 0.5802(4) 0.7271(3) 0.0697(19) Uani 1 1 d D . . . .
C62 C 0.4798(14) 0.6091(12) 0.7283(9) 0.081(6) Uiso 0.5 1 d D . P C 1
H62A H 0.5280 0.5952 0.7571 0.122 Uiso 0.5 1 calc R U P C 1
H62B H 0.5047 0.5961 0.7000 0.122 Uiso 0.5 1 calc R U P C 1
H62C H 0.4720 0.6568 0.7286 0.122 Uiso 0.5 1 calc R U P C 1
O2W O 0.581(2) 0.6437(14) 0.7341(10) 0.153(9) Uiso 0.5 1 d . . P D 2
Ni1 Ni 0.66374(8) 0.55803(4) 0.60155(4) 0.0394(2) Uani 1 1 d . . . . .
N31 N 0.7904(6) 0.6172(3) 0.6189(3) 0.0525(18) Uani 1 1 d . . . . .
N32 N 0.7140(6) 0.5369(3) 0.6737(3) 0.0505(18) Uani 1 1 d . . . . .
C31 C 0.8159(9) 0.6621(5) 0.5901(4) 0.070(3) Uani 1 1 d . . . . .
H31 H 0.7833 0.6621 0.5574 0.084 Uiso 1 1 calc R U . . .
C32 C 0.8894(10) 0.7090(5) 0.6069(6) 0.083(4) Uani 1 1 d . . . . .
H32 H 0.9053 0.7414 0.5859 0.099 Uiso 1 1 calc R U . . .
C33 C 0.9389(10) 0.7081(7) 0.6542(6) 0.097(5) Uani 1 1 d . . . . .
H33 H 0.9899 0.7392 0.6663 0.116 Uiso 1 1 calc R U . . .
C34 C 0.9125(9) 0.6610(6) 0.6835(5) 0.082(3) Uani 1 1 d . . . . .
H34 H 0.9466 0.6588 0.7160 0.098 Uiso 1 1 calc R U . . .
C35 C 0.8359(7) 0.6165(5) 0.6657(4) 0.060(2) Uani 1 1 d . . . . .
C36 C 0.8006(8) 0.5659(5) 0.6951(4) 0.059(2) Uani 1 1 d . . . . .
C37 C 0.8492(10) 0.5498(7) 0.7412(4) 0.080(3) Uani 1 1 d . . . . .
H37 H 0.9118 0.5695 0.7552 0.096 Uiso 1 1 calc R U . . .
C38 C 0.8068(12) 0.5055(7) 0.7664(4) 0.091(4) Uani 1 1 d . . . . .
H38 H 0.8395 0.4938 0.7980 0.109 Uiso 1 1 calc R U . . .
C39 C 0.7145(12) 0.4775(6) 0.7451(4) 0.086(4) Uani 1 1 d . . . . .
H39 H 0.6817 0.4480 0.7624 0.103 Uiso 1 1 calc R U . . .
C40 C 0.6727(9) 0.4932(5) 0.6991(4) 0.065(3) Uani 1 1 d . . . . .
H40 H 0.6114 0.4725 0.6842 0.077 Uiso 1 1 calc R U . . .
O71 O 0.7584(5) 0.4787(3) 0.5882(2) 0.0602(17) Uani 1 1 d . . . . .
H71A H 0.8197 0.4828 0.5880 0.090 Uiso 1 1 d R U . . .
H71B H 0.7310 0.4500 0.5687 0.090 Uiso 1 1 d R U . . .
Ni2 Ni 0.30934(8) 0.71653(4) 0.45176(4) 0.0410(2) Uani 1 1 d . . . . .
N41 N 0.1700(6) 0.7235(4) 0.4689(3) 0.062(2) Uani 1 1 d . . . . .
N42 N 0.2200(6) 0.6785(3) 0.3914(3) 0.0497(17) Uani 1 1 d . . . . .
C41 C 0.1516(9) 0.7475(7) 0.5094(4) 0.083(4) Uani 1 1 d . . . . .
H41 H 0.2063 0.7640 0.5327 0.100 Uiso 1 1 calc R U . . .
C42 C 0.0590(10) 0.7494(10) 0.5187(5) 0.114(6) Uani 1 1 d . . . . .
H42 H 0.0495 0.7676 0.5479 0.137 Uiso 1 1 calc R U . . .
C43 C -0.0201(10) 0.7257(10) 0.4870(6) 0.123(6) Uani 1 1 d . . . . .
H43 H -0.0862 0.7283 0.4927 0.147 Uiso 1 1 calc R U . . .
C44 C -0.0019(9) 0.6967(9) 0.4449(5) 0.108(5) Uani 1 1 d . . . . .
H44 H -0.0555 0.6780 0.4220 0.130 Uiso 1 1 calc R U . . .
C45 C 0.0962(8) 0.6961(7) 0.4377(4) 0.077(3) Uani 1 1 d . . . . .
C46 C 0.1229(8) 0.6706(6) 0.3933(4) 0.069(3) Uani 1 1 d . . . . .
C47 C 0.0550(10) 0.6426(8) 0.3563(5) 0.097(4) Uani 1 1 d . . . . .
H47 H -0.0121 0.6342 0.3591 0.116 Uiso 1 1 calc R U . . .
C48 C 0.0866(10) 0.6268(7) 0.3148(5) 0.089(4) Uani 1 1 d . . . . .
H48 H 0.0416 0.6073 0.2886 0.106 Uiso 1 1 calc R U . . .
C49 C 0.1850(9) 0.6400(6) 0.3126(4) 0.074(3) Uani 1 1 d . . . . .
H49 H 0.2076 0.6324 0.2840 0.088 Uiso 1 1 calc R U . . .
C50 C 0.2495(8) 0.6641(5) 0.3520(4) 0.060(2) Uani 1 1 d . . . . .
H50 H 0.3181 0.6707 0.3509 0.073 Uiso 1 1 calc R U . . .
O81 O 0.3192(8) 0.6189(3) 0.4813(2) 0.098(3) Uani 1 1 d D . . . .
C81 C 0.3776(19) 0.5900(10) 0.5198(7) 0.056(7) Uani 0.5 1 d D . P E 1
H81A H 0.3585 0.5439 0.5209 0.084 Uiso 0.5 1 calc R U P E 1
H81B H 0.4483 0.5930 0.5176 0.084 Uiso 0.5 1 calc R U P E 1
H81C H 0.3683 0.6123 0.5488 0.084 Uiso 0.5 1 calc R U P E 1
C81' C 0.337(3) 0.5985(15) 0.5272(7) 0.107(15) Uani 0.5 1 d D . P E 2
H81D H 0.3364 0.5505 0.5282 0.161 Uiso 0.5 1 calc R U P E 2
H81E H 0.4026 0.6147 0.5442 0.161 Uiso 0.5 1 calc R U P E 2
H81F H 0.2842 0.6156 0.5424 0.161 Uiso 0.5 1 calc R U P E 2
O82 O 0.2931(6) 0.8085(3) 0.4182(2) 0.0651(18) Uani 1 1 d . . . . .
H82A H 0.3141 0.8055 0.3929 0.098 Uiso 1 1 d R U . . .
H82B H 0.2321 0.8055 0.4194 0.098 Uiso 1 1 d R U . . .
Ni3 Ni 0.69808(8) 0.84415(4) 0.49682(4) 0.0398(2) Uani 1 1 d . . . . .
N51 N 0.7519(6) 0.8847(3) 0.4411(3) 0.0481(17) Uani 1 1 d . . . . .
N52 N 0.6727(6) 0.9432(3) 0.5062(3) 0.0506(18) Uani 1 1 d . . . . .
C51 C 0.7940(8) 0.8531(4) 0.4093(4) 0.056(2) Uani 1 1 d . . . . .
H51 H 0.7997 0.8068 0.4114 0.067 Uiso 1 1 calc R U . . .
C52 C 0.8289(8) 0.8845(4) 0.3740(4) 0.061(3) Uani 1 1 d . . . . .
H52 H 0.8587 0.8605 0.3522 0.074 Uiso 1 1 calc R U . . .
C53 C 0.8197(8) 0.9523(4) 0.3708(4) 0.061(2) Uani 1 1 d . . . . .
H53 H 0.8434 0.9754 0.3467 0.073 Uiso 1 1 calc R U . . .
C54 C 0.7765(7) 0.9855(4) 0.4023(3) 0.054(2) Uani 1 1 d . . . . .
H54 H 0.7695 1.0318 0.4003 0.064 Uiso 1 1 calc R U . . .
C55 C 0.7430(7) 0.9511(4) 0.4372(3) 0.049(2) Uani 1 1 d . . . . .
C56 C 0.6934(7) 0.9825(4) 0.4724(3) 0.047(2) Uani 1 1 d . . . . .
C57 C 0.6704(9) 1.0484(4) 0.4711(4) 0.064(3) Uani 1 1 d . . . . .
H57 H 0.6847 1.0756 0.4465 0.077 Uiso 1 1 calc R U . . .
C58 C 0.6263(11) 1.0745(4) 0.5061(4) 0.085(4) Uani 1 1 d . . . . .
H58 H 0.6102 1.1198 0.5063 0.102 Uiso 1 1 calc R U . . .
C59 C 0.6062(12) 1.0332(5) 0.5408(5) 0.099(5) Uani 1 1 d . . . . .
H59 H 0.5754 1.0497 0.5651 0.119 Uiso 1 1 calc R U . . .
C60 C 0.6309(10) 0.9679(4) 0.5400(4) 0.073(3) Uani 1 1 d . . . . .
H60 H 0.6175 0.9398 0.5643 0.087 Uiso 1 1 calc R U . . .
O91 O 0.5512(4) 0.8402(2) 0.4517(2) 0.0486(14) Uani 1 1 d . . . . .
H91A H 0.5487 0.8641 0.4276 0.073 Uiso 1 1 d R U . . .
H91B H 0.5405 0.8009 0.4434 0.073 Uiso 1 1 d R U . . .
O92 O 0.8404(5) 0.8483(3) 0.5426(3) 0.0631(17) Uani 1 1 d . . . . .
H92A H 0.8303 0.8515 0.5703 0.095 Uiso 1 1 d R U . . .
H92B H 0.8834 0.8768 0.5400 0.095 Uiso 1 1 d R U . . .
O3W O 0.5128(6) 0.9152(3) 0.3671(2) 0.0663(19) Uani 1 1 d . . . . .
H5O H 0.4556 0.9007 0.3541 0.099 Uiso 1 1 d R U . . .
H6O H 0.5129 0.9530 0.3786 0.099 Uiso 1 1 d R U . . .
O4W O 0.8816(6) 0.7603(4) 0.7699(3) 0.079(2) Uani 1 1 d . . . . .
H7O H 0.8659 0.7918 0.7857 0.119 Uiso 1 1 d R U . . .
H8O H 0.8317 0.7584 0.7469 0.119 Uiso 1 1 d R U . . .
O5W O 0.0675(7) 0.2305(4) 0.6733(3) 0.093(3) Uani 1 1 d . . . . .
H9O H 0.1027 0.2614 0.6664 0.139 Uiso 1 1 d R U . . .
H10O H 0.0901 0.2344 0.7028 0.139 Uiso 1 1 d R U . . .
O6W O 0.8528(8) 0.6689(4) 0.8341(4) 0.104(3) Uani 1 1 d . . . . .
H11O H 0.8029 0.6682 0.8111 0.156 Uiso 1 1 d R U . . .
H12O H 0.8918 0.6990 0.8296 0.156 Uiso 1 1 d R U . . .
O7W O 0.4361(10) 0.4500(5) 0.7658(4) 0.052(3) Uani 0.5 1 d . . P . .
O8W O 0.0764(9) 0.8832(7) 0.6476(6) 0.073(4) Uani 0.5 1 d . . P . .
O9W O 0.8442(12) 0.8682(7) 0.6389(4) 0.071(4) Uani 0.5 1 d . . P . .
O10W O 0.0877(10) 0.8357(7) 0.3847(6) 0.079(4) Uani 0.5 1 d . . P . .
O11W O 0.1174(17) 0.5813(8) 0.5210(6) 0.107(7) Uani 0.5 1 d . . P . .


_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
W2 C17 2.122(10) . ?
W2 C15 2.150(9) . ?
W2 C16 2.152(10) . ?
W2 C18 2.157(12) . ?
W2 C13 2.159(7) . ?
W2 C12 2.171(8) . ?
W2 C14 2.177(7) . ?
W2 C11 2.184(8) . ?
C11 N11 1.140(10) . ?
N11 Ni4 2.037(7) . ?
C17 N17 1.167(11) . ?
N17 Ni2 1.992(8) . ?
C18 N18 1.163(13) . ?
C12 N12 1.150(10) . ?
N12 Ni3 2.041(7) . ?
C13 N13 1.126(10) . ?
N13 Ni1 2.042(7) . ?
C16 N16 1.183(12) . ?
C15 N15 1.147(12) . ?
C14 N14 1.164(10) . ?
W1 C4 2.141(7) . ?
W1 C1 2.152(7) . ?
W1 C3 2.154(9) . ?
W1 C7 2.163(9) . ?
W1 C5 2.163(9) . ?
W1 C8 2.166(9) . ?
W1 C6 2.166(8) . ?
W1 C2 2.172(8) . ?
C6 N6 1.148(10) . ?
N6 Ni1 2.025(6) . ?
C1 N1 1.140(9) . ?
N1 Ni3 2.053(6) 3_666 ?
C8 N8 1.151(11) . ?
C2 N2 1.141(10) . ?
C5 N5 1.147(11) . ?
N5 Ni2 2.050(8) 3_666 ?
C3 N3 1.128(10) . ?
N3 Ni1 2.036(8) 3_666 ?
C4 N4 1.156(9) . ?
N4 Ni4 2.008(6) . ?
C7 N7 1.141(13) . ?
Ni4 N22 2.071(7) . ?
Ni4 N21 2.072(7) . ?
Ni4 O62 2.115(8) . ?
Ni4 O61 2.132(7) . ?
N21 C21 1.340(10) . ?
N21 C25 1.345(11) . ?
N22 C26 1.347(10) . ?
N22 C30 1.353(10) . ?
C21 C22 1.353(13) . ?
C22 C23 1.380(15) . ?
C23 C24 1.374(13) . ?
C24 C25 1.396(11) . ?
C25 C26 1.478(11) . ?
C26 C27 1.391(12) . ?
C27 C28 1.358(13) . ?
C28 C29 1.373(13) . ?
C29 C30 1.384(12) . ?
O61 C61 1.388(17) . ?
O62 C62 1.357(16) . ?
Ni1 N3 2.036(8) 3_666 ?
Ni1 N31 2.075(7) . ?
Ni1 N32 2.081(7) . ?
Ni1 O71 2.154(6) . ?
N31 C31 1.327(13) . ?
N31 C35 1.353(13) . ?
N32 C36 1.344(12) . ?
N32 C40 1.350(12) . ?
C31 C32 1.393(15) . ?
C32 C33 1.38(2) . ?
C33 C34 1.37(2) . ?
C34 C35 1.394(15) . ?
C35 C36 1.478(15) . ?
C36 C37 1.387(15) . ?
C37 C38 1.361(18) . ?
C38 C39 1.40(2) . ?
C39 C40 1.359(15) . ?
Ni2 N42 2.043(8) . ?
Ni2 N5 2.050(8) 3_666 ?
Ni2 N41 2.064(8) . ?
Ni2 O82 2.099(6) . ?
Ni2 O81 2.158(6) . ?
N41 C45 1.318(14) . ?
N41 C41 1.335(14) . ?
N42 C50 1.314(12) . ?
N42 C46 1.342(13) . ?
C41 C42 1.343(16) . ?
C42 C43 1.34(2) . ?
C43 C44 1.42(2) . ?
C44 C45 1.395(16) . ?
C45 C46 1.491(16) . ?
C46 C47 1.373(16) . ?
C47 C48 1.389(18) . ?
C48 C49 1.381(17) . ?
C49 C50 1.366(15) . ?
O81 C81 1.349(16) . ?
O81 C81' 1.353(17) . ?
Ni3 N1 2.053(6) 3_666 ?
Ni3 N51 2.070(7) . ?
Ni3 N52 2.077(6) . ?
Ni3 O92 2.095(7) . ?
Ni3 O91 2.137(6) . ?
N51 C51 1.343(10) . ?
N51 C55 1.362(10) . ?
N52 C60 1.325(11) . ?
N52 C56 1.336(10) . ?
C51 C52 1.368(12) . ?
C52 C53 1.391(13) . ?
C53 C54 1.362(12) . ?
C54 C55 1.378(12) . ?
C55 C56 1.476(11) . ?
C56 C57 1.381(11) . ?
C57 C58 1.384(14) . ?
C58 C59 1.374(15) . ?
C59 C60 1.377(13) . ?

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
C17 W2 C15 146.1(4) . . ?
C17 W2 C16 75.8(3) . . ?
C15 W2 C16 78.2(4) . . ?
C17 W2 C18 140.4(3) . . ?
C15 W2 C18 72.4(4) . . ?
C16 W2 C18 139.2(3) . . ?
C17 W2 C13 83.6(3) . . ?
C15 W2 C13 103.1(3) . . ?
C16 W2 C13 139.8(3) . . ?
C18 W2 C13 75.4(3) . . ?
C17 W2 C12 69.5(3) . . ?
C15 W2 C12 144.3(3) . . ?
C16 W2 C12 123.9(3) . . ?
C18 W2 C12 73.5(3) . . ?
C13 W2 C12 78.1(3) . . ?
C17 W2 C14 105.5(3) . . ?
C15 W2 C14 87.0(3) . . ?
C16 W2 C14 72.7(3) . . ?
C18 W2 C14 78.0(3) . . ?
C13 W2 C14 147.0(3) . . ?
C12 W2 C14 75.8(3) . . ?
C17 W2 C11 78.1(3) . . ?
C15 W2 C11 73.4(3) . . ?
C16 W2 C11 72.0(3) . . ?
C18 W2 C11 123.4(4) . . ?
C13 W2 C11 70.2(3) . . ?
C12 W2 C11 136.6(3) . . ?
C14 W2 C11 142.4(3) . . ?
N11 C11 W2 174.8(8) . . ?
C11 N11 Ni4 164.8(8) . . ?
N17 C17 W2 176.2(7) . . ?
C17 N17 Ni2 169.1(6) . . ?
N18 C18 W2 179.4(9) . . ?
N12 C12 W2 177.3(8) . . ?
C12 N12 Ni3 168.2(7) . . ?
N13 C13 W2 177.3(8) . . ?
C13 N13 Ni1 167.3(7) . . ?
N16 C16 W2 176.8(7) . . ?
N15 C15 W2 175.4(8) . . ?
N14 C14 W2 179.1(9) . . ?
C4 W1 C1 145.9(3) . . ?
C4 W1 C3 108.5(3) . . ?
C1 W1 C3 78.5(3) . . ?
C4 W1 C7 73.1(3) . . ?
C1 W1 C7 77.9(3) . . ?
C3 W1 C7 71.9(4) . . ?
C4 W1 C5 141.8(3) . . ?
C1 W1 C5 71.7(3) . . ?
C3 W1 C5 80.0(3) . . ?
C7 W1 C5 142.0(3) . . ?
C4 W1 C8 79.4(3) . . ?
C1 W1 C8 114.8(3) . . ?
C3 W1 C8 144.5(3) . . ?
C7 W1 C8 141.1(3) . . ?
C5 W1 C8 74.3(3) . . ?
C4 W1 C6 71.8(3) . . ?
C1 W1 C6 140.1(3) . . ?
C3 W1 C6 74.5(3) . . ?
C7 W1 C6 119.3(3) . . ?
C5 W1 C6 75.2(3) . . ?
C8 W1 C6 75.6(3) . . ?
C4 W1 C2 81.5(3) . . ?
C1 W1 C2 74.4(3) . . ?
C3 W1 C2 141.7(3) . . ?
C7 W1 C2 76.3(4) . . ?
C5 W1 C2 115.4(3) . . ?
C8 W1 C2 72.8(3) . . ?
C6 W1 C2 141.7(3) . . ?
N6 C6 W1 176.6(7) . . ?
C6 N6 Ni1 178.9(7) . . ?
N1 C1 W1 175.4(6) . . ?
C1 N1 Ni3 156.9(6) . 3_666 ?
N8 C8 W1 177.2(8) . . ?
N2 C2 W1 177.3(8) . . ?
N5 C5 W1 176.9(7) . . ?
C5 N5 Ni2 157.6(7) . 3_666 ?
N3 C3 W1 174.9(8) . . ?
C3 N3 Ni1 170.7(8) . 3_666 ?
N4 C4 W1 178.9(8) . . ?
C4 N4 Ni4 171.2(6) . . ?
N7 C7 W1 178.4(9) . . ?
N4 Ni4 N11 93.9(3) . . ?
N4 Ni4 N22 92.3(2) . . ?
N11 Ni4 N22 172.2(3) . . ?
N4 Ni4 N21 171.1(3) . . ?
N11 Ni4 N21 94.9(3) . . ?
N22 Ni4 N21 78.9(3) . . ?
N4 Ni4 O62 92.3(3) . . ?
N11 Ni4 O62 91.1(3) . . ?
N22 Ni4 O62 84.1(3) . . ?
N21 Ni4 O62 88.1(3) . . ?
N4 Ni4 O61 89.9(3) . . ?
N11 Ni4 O61 91.1(3) . . ?
N22 Ni4 O61 93.5(3) . . ?
N21 Ni4 O61 89.4(3) . . ?
O62 Ni4 O61 176.8(3) . . ?
C21 N21 C25 119.7(7) . . ?
C21 N21 Ni4 125.7(6) . . ?
C25 N21 Ni4 114.6(5) . . ?
C26 N22 C30 118.3(7) . . ?
C26 N22 Ni4 115.2(5) . . ?
C30 N22 Ni4 126.2(6) . . ?
N21 C21 C22 121.0(9) . . ?
C21 C22 C23 121.0(8) . . ?
C24 C23 C22 118.3(8) . . ?
C23 C24 C25 118.9(9) . . ?
N21 C25 C24 121.1(8) . . ?
N21 C25 C26 116.1(7) . . ?
C24 C25 C26 122.8(8) . . ?
N22 C26 C27 120.8(7) . . ?
N22 C26 C25 114.7(7) . . ?
C27 C26 C25 124.5(7) . . ?
C28 C27 C26 120.6(8) . . ?
C27 C28 C29 119.0(8) . . ?
C28 C29 C30 118.9(8) . . ?
N22 C30 C29 122.4(8) . . ?
C61 O61 Ni4 119.5(14) . . ?
C62 O62 Ni4 125.1(12) . . ?
N6 Ni1 N3 91.2(3) . 3_666 ?
N6 Ni1 N13 97.3(3) . . ?
N3 Ni1 N13 93.4(3) 3_666 . ?
N6 Ni1 N31 172.4(3) . . ?
N3 Ni1 N31 95.7(3) 3_666 . ?
N13 Ni1 N31 85.6(3) . . ?
N6 Ni1 N32 94.1(3) . . ?
N3 Ni1 N32 172.1(3) 3_666 . ?
N13 Ni1 N32 91.6(3) . . ?
N31 Ni1 N32 78.7(3) . . ?
N6 Ni1 O71 88.0(2) . . ?
N3 Ni1 O71 87.9(3) 3_666 . ?
N13 Ni1 O71 174.5(3) . . ?
N31 Ni1 O71 89.0(3) . . ?
N32 Ni1 O71 86.6(3) . . ?
C31 N31 C35 120.0(9) . . ?
C31 N31 Ni1 124.6(7) . . ?
C35 N31 Ni1 114.3(6) . . ?
C36 N32 C40 118.0(9) . . ?
C36 N32 Ni1 115.6(6) . . ?
C40 N32 Ni1 126.1(7) . . ?
N31 C31 C32 121.6(12) . . ?
C33 C32 C31 119.4(12) . . ?
C34 C33 C32 118.4(11) . . ?
C33 C34 C35 120.3(13) . . ?
N31 C35 C34 120.2(11) . . ?
N31 C35 C36 116.1(8) . . ?
C34 C35 C36 123.7(11) . . ?
N32 C36 C37 121.6(10) . . ?
N32 C36 C35 114.0(9) . . ?
C37 C36 C35 124.4(10) . . ?
C38 C37 C36 119.7(12) . . ?
C37 C38 C39 118.9(12) . . ?
C40 C39 C38 118.6(13) . . ?
N32 C40 C39 123.1(12) . . ?
N17 Ni2 N42 171.2(3) . . ?
N17 Ni2 N5 93.2(3) . 3_666 ?
N42 Ni2 N5 95.3(3) . 3_666 ?
N17 Ni2 N41 91.8(3) . . ?
N42 Ni2 N41 79.5(3) . . ?
N5 Ni2 N41 173.4(3) 3_666 . ?
N17 Ni2 O82 93.8(3) . . ?
N42 Ni2 O82 88.1(3) . . ?
N5 Ni2 O82 91.9(3) 3_666 . ?
N41 Ni2 O82 92.1(3) . . ?
N17 Ni2 O81 90.6(3) . . ?
N42 Ni2 O81 87.5(3) . . ?
N5 Ni2 O81 88.3(4) 3_666 . ?
N41 Ni2 O81 87.3(4) . . ?
O82 Ni2 O81 175.6(3) . . ?
C45 N41 C41 119.3(9) . . ?
C45 N41 Ni2 114.4(7) . . ?
C41 N41 Ni2 126.0(7) . . ?
C50 N42 C46 119.6(9) . . ?
C50 N42 Ni2 125.3(7) . . ?
C46 N42 Ni2 115.0(7) . . ?
N41 C41 C42 122.9(12) . . ?
C43 C42 C41 120.4(13) . . ?
C42 C43 C44 117.9(12) . . ?
C45 C44 C43 118.7(12) . . ?
N41 C45 C44 120.5(12) . . ?
N41 C45 C46 116.0(9) . . ?
C44 C45 C46 123.2(11) . . ?
N42 C46 C47 121.5(11) . . ?
N42 C46 C45 114.5(9) . . ?
C47 C46 C45 123.9(11) . . ?
C46 C47 C48 118.6(12) . . ?
C49 C48 C47 118.5(12) . . ?
C50 C49 C48 119.3(11) . . ?
N42 C50 C49 122.2(11) . . ?
C81 O81 Ni2 134.4(11) . . ?
C81' O81 Ni2 130.4(14) . . ?
N12 Ni3 N1 93.4(2) . 3_666 ?
N12 Ni3 N51 172.3(2) . . ?
N1 Ni3 N51 93.9(2) 3_666 . ?
N12 Ni3 N52 93.6(3) . . ?
N1 Ni3 N52 170.8(3) 3_666 . ?
N51 Ni3 N52 78.9(3) . . ?
N12 Ni3 O92 90.0(3) . . ?
N1 Ni3 O92 93.8(3) 3_666 . ?
N51 Ni3 O92 92.0(3) . . ?
N52 Ni3 O92 92.1(3) . . ?
N12 Ni3 O91 88.7(3) . . ?
N1 Ni3 O91 86.8(2) 3_666 . ?
N51 Ni3 O91 89.2(3) . . ?
N52 Ni3 O91 87.5(3) . . ?
O92 Ni3 O91 178.6(3) . . ?
C51 N51 C55 117.7(7) . . ?
C51 N51 Ni3 127.4(5) . . ?
C55 N51 Ni3 114.9(5) . . ?
C60 N52 C56 119.7(7) . . ?
C60 N52 Ni3 125.1(6) . . ?
C56 N52 Ni3 114.9(5) . . ?
N51 C51 C52 123.1(8) . . ?
C51 C52 C53 118.3(8) . . ?
C54 C53 C52 119.7(8) . . ?
C53 C54 C55 119.2(8) . . ?
N51 C55 C54 121.9(8) . . ?
N51 C55 C56 114.9(7) . . ?
C54 C55 C56 123.2(7) . . ?
N52 C56 C57 121.4(8) . . ?
N52 C56 C55 115.9(7) . . ?
C57 C56 C55 122.7(8) . . ?
C56 C57 C58 119.2(9) . . ?
C59 C58 C57 118.3(8) . . ?
C58 C59 C60 119.7(10) . . ?
N52 C60 C59 121.7(9) . . ?

_refine_diff_density_max         1.672
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.128

_shelxl_version_number           2014-3

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.500 0.500 261.5 41.1
2 0.500 0.000 0.000 261.4 41.2
_platon_squeeze_details          
;
;

