# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Darren Bradshaw'
_publ_contact_author_email       DEG5Y@LIV.AC.UK

_publ_section_title              
;
Triply interpenetrated (3,4)- and (3,5)-connected
binodal metal-organic networks prepared from 1,3,5-benzenetrisbenzoate
and 4,4'-bipyridyl
;
loop_
_publ_author_name
'Darren Bradshaw'
'John Bacsa'
'Romain Heck'
'Matthew J Rosseinsky'
'John E Warren'

# Attachment 'Submission.cif'

data_mjr458
_database_code_depnum_ccdc_archive 'CCDC 692026'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            MJR458
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H48 N4 Ni2 O12'
_chemical_formula_weight         1302.58

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_as_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                   14.4662(18)
_cell_length_b                   30.099(4)
_cell_length_c                   16.497(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.872(2)
_cell_angle_gamma                90.00
_cell_volume                     7179.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2131
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      19.88

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9714
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_process_details   'SADABS V2008-1 (Bruker, 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.67100
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS, Station 16.2SMX'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31162
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         21.15
_reflns_number_total             9277
_reflns_number_gt                5805
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_reduction        'APEXII (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1051P)²+0.1652P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9274
_refine_ls_number_parameters     894
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2074
_refine_ls_wR_factor_gt          0.1901
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.50631(5) 0.22767(3) 1.09802(5) 0.0319(2) Uani 1 1 d D . .
N1 N 0.5975(4) 0.23334(18) 1.0031(4) 0.0454(16) Uani 1 1 d . . .
C1 C 0.5055(4) 0.5017(2) 1.1190(4) 0.0343(16) Uani 1 1 d . . .
Ni2 Ni -0.04005(5) 0.72238(2) 0.93817(5) 0.0248(2) Uani 1 1 d . . .
N2 N 0.9106(3) 0.27225(16) 0.6890(3) 0.0357(14) Uani 1 1 d . . .
C2 C 0.5820(4) 0.5271(2) 1.1436(4) 0.0380(17) Uani 1 1 d . . .
H2 H 0.6400 0.5128 1.1526 0.046 Uiso 1 1 calc R . .
N3 N 0.3643(3) 0.77007(16) 0.5305(3) 0.0303(13) Uani 1 1 d . . .
C3 C 0.5759(4) 0.5729(2) 1.1555(4) 0.0317(15) Uani 1 1 d . . .
N4 N 0.0536(3) 0.72098(15) 0.8432(3) 0.0258(12) Uani 1 1 d . . .
C4 C 0.4922(4) 0.5938(2) 1.1418(4) 0.0338(16) Uani 1 1 d . . .
H4 H 0.4879 0.6251 1.1491 0.041 Uiso 1 1 calc R . .
C5 C 0.4141(4) 0.5700(2) 1.1174(4) 0.0346(16) Uani 1 1 d . . .
C6 C 0.4222(4) 0.5238(2) 1.1048(4) 0.0387(17) Uani 1 1 d . . .
H6 H 0.3695 0.5075 1.0860 0.046 Uiso 1 1 calc R . .
C7 C 0.5106(4) 0.4526(2) 1.1104(4) 0.0337(16) Uani 1 1 d . . .
C8 C 0.4469(4) 0.4299(2) 1.0602(4) 0.0323(16) Uani 1 1 d . . .
H8 H 0.4042 0.4462 1.0270 0.039 Uiso 1 1 calc R . .
C9 C 0.4454(4) 0.3838(2) 1.0584(4) 0.0368(17) Uani 1 1 d . . .
H9 H 0.4010 0.3690 1.0244 0.044 Uiso 1 1 calc R . .
C10 C 0.5078(4) 0.3591(2) 1.1058(4) 0.0359(17) Uani 1 1 d . . .
C11 C 0.5739(4) 0.3821(2) 1.1542(4) 0.0398(18) Uani 1 1 d . . .
H11 H 0.6189 0.3660 1.1854 0.048 Uiso 1 1 calc R . .
C12 C 0.5738(4) 0.4275(2) 1.1566(4) 0.0352(17) Uani 1 1 d . . .
H12 H 0.6181 0.4423 1.1907 0.042 Uiso 1 1 calc R . .
C13 C 0.5059(4) 0.3095(2) 1.1048(4) 0.0364(17) Uani 1 1 d . . .
O1 O 0.4455(3) 0.28985(14) 1.0603(3) 0.0392(11) Uani 1 1 d . . .
O2 O 0.5639(3) 0.28749(13) 1.1468(3) 0.0350(11) Uani 1 1 d . . .
C14 C 0.6599(4) 0.5988(2) 1.1844(4) 0.0355(17) Uani 1 1 d . . .
C15 C 0.7432(5) 0.5941(2) 1.1507(5) 0.0486(19) Uani 1 1 d . . .
H15 H 0.7472 0.5765 1.1032 0.058 Uiso 1 1 calc R . .
C16 C 0.8235(5) 0.6141(2) 1.1824(5) 0.049(2) Uani 1 1 d . . .
H16 H 0.8813 0.6100 1.1576 0.059 Uiso 1 1 calc R . .
C17 C 0.8163(5) 0.6401(2) 1.2515(4) 0.0428(18) Uani 1 1 d . . .
C18 C 0.7316(4) 0.6469(2) 1.2851(5) 0.0455(19) Uani 1 1 d . . .
H18 H 0.7262 0.6656 1.3311 0.055 Uiso 1 1 calc R . .
C19 C 0.6552(4) 0.6264(2) 1.2513(4) 0.0405(18) Uani 1 1 d . . .
H19 H 0.5969 0.6313 1.2746 0.049 Uiso 1 1 calc R . .
C20 C 0.9029(4) 0.6588(2) 1.2905(5) 0.0421(18) Uani 1 1 d . . .
O3 O 0.9791(3) 0.6419(2) 1.2676(4) 0.0710(17) Uani 1 1 d D . .
O4 O 0.8967(3) 0.68921(14) 1.3423(3) 0.0374(11) Uani 1 1 d . . .
C21 C 0.3215(4) 0.5916(2) 1.1019(4) 0.0324(16) Uani 1 1 d . . .
C22 C 0.2423(5) 0.5744(3) 1.1315(5) 0.061(2) Uani 1 1 d . . .
H22 H 0.2460 0.5489 1.1653 0.073 Uiso 1 1 calc R . .
C23 C 0.1568(4) 0.5930(2) 1.1135(4) 0.050(2) Uani 1 1 d . . .
H23 H 0.1028 0.5804 1.1352 0.060 Uiso 1 1 calc R . .
C24 C 0.1498(4) 0.6302(2) 1.0638(4) 0.0339(16) Uani 1 1 d . . .
C25 C 0.2301(4) 0.6485(2) 1.0367(4) 0.0419(18) Uani 1 1 d . . .
H25 H 0.2269 0.6753 1.0064 0.050 Uiso 1 1 calc R . .
C26 C 0.3162(4) 0.6288(2) 1.0524(4) 0.0387(17) Uani 1 1 d . . .
H26 H 0.3703 0.6407 1.0295 0.046 Uiso 1 1 calc R . .
C27 C 0.0577(4) 0.6488(2) 1.0375(4) 0.0327(16) Uani 1 1 d . . .
O5 O 0.0535(3) 0.68493(13) 1.0018(2) 0.0314(10) Uani 1 1 d . . .
O6 O -0.0112(3) 0.62357(15) 1.0472(3) 0.0456(13) Uani 1 1 d . . .
C28 C 0.5016(4) 0.5073(2) 0.3747(4) 0.0321(16) Uani 1 1 d . . .
C29 C 0.4282(4) 0.4836(2) 0.3395(4) 0.0363(17) Uani 1 1 d . . .
H29 H 0.3721 0.4987 0.3262 0.044 Uiso 1 1 calc R . .
C30 C 0.4346(4) 0.43897(18) 0.3233(4) 0.0306(16) Uani 1 1 d . . .
C31 C 0.5153(4) 0.4161(2) 0.3475(4) 0.0364(17) Uani 1 1 d . . .
H31 H 0.5194 0.3850 0.3380 0.044 Uiso 1 1 calc R . .
C32 C 0.5898(4) 0.4382(2) 0.3854(4) 0.0330(16) Uani 1 1 d D . .
C33 C 0.5820(4) 0.4845(2) 0.3965(4) 0.0350(16) Uani 1 1 d . . .
H33 H 0.6332 0.5005 0.4193 0.042 Uiso 1 1 calc R . .
C34 C 0.4952(4) 0.5560(2) 0.3883(4) 0.0336(16) Uani 1 1 d . . .
C35 C 0.5487(4) 0.5776(2) 0.4474(4) 0.0345(16) Uani 1 1 d . . .
H35 H 0.5911 0.5609 0.4804 0.041 Uiso 1 1 calc R . .
C36 C 0.5414(4) 0.6237(2) 0.4594(4) 0.0369(17) Uani 1 1 d . . .
H36 H 0.5791 0.6379 0.4999 0.044 Uiso 1 1 calc R . .
C37 C 0.4800(4) 0.64844(19) 0.4129(4) 0.0284(15) Uani 1 1 d . . .
C38 C 0.4245(4) 0.6269(2) 0.3546(4) 0.0374(17) Uani 1 1 d . . .
H38 H 0.3797 0.6433 0.3238 0.045 Uiso 1 1 calc R . .
C39 C 0.4341(4) 0.5818(2) 0.3414(4) 0.0390(18) Uani 1 1 d . . .
H39 H 0.3981 0.5680 0.2992 0.047 Uiso 1 1 calc R . .
C40 C 0.4705(4) 0.6970(2) 0.4257(4) 0.0300(15) Uani 1 1 d . . .
O7 O 0.5240(3) 0.71699(12) 0.4765(3) 0.0326(11) Uani 1 1 d . . .
O8 O 0.4097(3) 0.71831(13) 0.3858(2) 0.0317(10) Uani 1 1 d . . .
C41 C 0.3607(4) 0.4168(2) 0.2724(4) 0.0348(17) Uani 1 1 d . . .
C42 C 0.3069(4) 0.4416(2) 0.2176(4) 0.0402(18) Uani 1 1 d . . .
H42 H 0.3148 0.4730 0.2166 0.048 Uiso 1 1 calc R . .
C43 C 0.2430(4) 0.4228(2) 0.1651(4) 0.0358(17) Uani 1 1 d . . .
H43 H 0.2105 0.4407 0.1262 0.043 Uiso 1 1 calc R . .
C44 C 0.2261(4) 0.37802(19) 0.1691(4) 0.0298(15) Uani 1 1 d . . .
C45 C 0.2752(4) 0.3528(2) 0.2249(4) 0.0435(19) Uani 1 1 d . . .
H45 H 0.2636 0.3218 0.2281 0.052 Uiso 1 1 calc R . .
C46 C 0.3409(5) 0.3717(2) 0.2763(5) 0.048(2) Uani 1 1 d . . .
H46 H 0.3732 0.3536 0.3150 0.058 Uiso 1 1 calc R . .
C47 C 0.1574(4) 0.3566(2) 0.1103(4) 0.0343(16) Uani 1 1 d . . .
O9 O 0.1428(3) 0.37899(15) 0.0454(3) 0.0494(13) Uani 1 1 d D . .
O10 O 0.1227(3) 0.32042(13) 0.1258(2) 0.0302(10) Uani 1 1 d . . .
C48A C 0.6783(5) 0.4126(4) 0.4023(8) 0.026(3) Uani 0.524(5) 1 d PDU . 1
C49A C 0.6742(8) 0.3710(4) 0.4411(9) 0.038(4) Uani 0.524(5) 1 d PD . 1
H49A H 0.6159 0.3578 0.4508 0.046 Uiso 0.524(5) 1 calc PR . 1
C50A C 0.7550(9) 0.3493(5) 0.4651(14) 0.040(4) Uani 0.524(5) 1 d PD . 1
H50A H 0.7500 0.3213 0.4912 0.048 Uiso 0.524(5) 1 calc PR . 1
C51A C 0.8437(7) 0.3662(4) 0.4530(8) 0.032(3) Uani 0.524(5) 1 d PD . 1
C52A C 0.8466(7) 0.4082(4) 0.4204(8) 0.044(4) Uani 0.524(5) 1 d PD . 1
H52A H 0.9047 0.4225 0.4160 0.053 Uiso 0.524(5) 1 calc PR . 1
C53A C 0.7668(7) 0.4302(4) 0.3937(8) 0.039(3) Uani 0.524(5) 1 d PD . 1
H53A H 0.7727 0.4585 0.3686 0.047 Uiso 0.524(5) 1 calc PR . 1
C54A C 0.9301(8) 0.3445(4) 0.4862(8) 0.045(4) Uani 0.524(5) 1 d PD . 1
O11A O 0.9187(9) 0.3088(4) 0.5272(7) 0.036(2) Uani 0.524(5) 1 d PD . 1
O12A O 1.0066(6) 0.3626(3) 0.4723(8) 0.082(4) Uani 0.524(5) 1 d PD . 1
C48B C 0.6682(8) 0.4153(4) 0.4318(8) 0.026(3) Uani 0.476(5) 1 d PDU . 2
C49B C 0.6988(10) 0.3744(5) 0.4052(9) 0.038(4) Uani 0.476(5) 1 d PD . 2
H49B H 0.6705 0.3605 0.3590 0.046 Uiso 0.476(5) 1 calc PR . 2
C50B C 0.7715(12) 0.3543(6) 0.4474(15) 0.040(4) Uani 0.476(5) 1 d PD . 2
H50B H 0.7932 0.3261 0.4305 0.048 Uiso 0.476(5) 1 calc PR . 2
C51B C 0.8131(8) 0.3751(4) 0.5141(9) 0.035(4) Uani 0.476(5) 1 d PD . 2
C52B C 0.7781(8) 0.4155(4) 0.5425(8) 0.043(4) Uani 0.476(5) 1 d PD . 2
H52B H 0.8033 0.4286 0.5907 0.052 Uiso 0.476(5) 1 calc PR . 2
C53B C 0.7061(9) 0.4360(4) 0.4993(9) 0.048(4) Uani 0.476(5) 1 d PD . 2
H53B H 0.6833 0.4640 0.5162 0.058 Uiso 0.476(5) 1 calc PR . 2
C54B C 0.8851(8) 0.3519(4) 0.5657(8) 0.037(4) Uani 0.476(5) 1 d PD . 2
O11B O 0.9258(11) 0.3184(4) 0.5363(9) 0.036(2) Uani 0.476(5) 1 d PD . 2
O12B O 0.8990(6) 0.3698(3) 0.6345(5) 0.037(3) Uani 0.476(5) 1 d PD . 2
C55 C 0.9342(5) 0.2665(3) 0.7701(4) 0.054(2) Uani 1 1 d . . .
H55 H 0.9982 0.2688 0.7845 0.065 Uiso 1 1 calc R . .
C56 C 0.8807(4) 0.2586(3) 0.8275(5) 0.057(2) Uani 1 1 d . . .
H56 H 0.9051 0.2524 0.8804 0.069 Uiso 1 1 calc R . .
C57 C 0.7858(4) 0.2590(2) 0.8120(4) 0.0331(16) Uani 1 1 d . . .
C58 C 0.7562(4) 0.2679(2) 0.7332(4) 0.0379(17) Uani 1 1 d . . .
H58 H 0.6920 0.2699 0.7196 0.045 Uiso 1 1 calc R . .
C59 C 0.8207(4) 0.27375(19) 0.6744(5) 0.0405(18) Uani 1 1 d . . .
H59 H 0.7990 0.2792 0.6203 0.049 Uiso 1 1 calc R . .
C60 C 0.5758(4) 0.2590(3) 0.9372(5) 0.052(2) Uani 1 1 d . . .
H60 H 0.5165 0.2725 0.9345 0.062 Uiso 1 1 calc R . .
C61 C 0.6323(4) 0.2666(2) 0.8754(4) 0.048(2) Uani 1 1 d . . .
H61 H 0.6108 0.2838 0.8304 0.057 Uiso 1 1 calc R . .
C62 C 0.7209(4) 0.24968(19) 0.8765(4) 0.0315(16) Uani 1 1 d . . .
C63 C 0.7449(4) 0.2228(2) 0.9434(4) 0.0387(17) Uani 1 1 d . . .
H63 H 0.8040 0.2091 0.9472 0.046 Uiso 1 1 calc R . .
C64 C 0.6831(5) 0.2163(2) 1.0031(5) 0.048(2) Uani 1 1 d . . .
H64 H 0.7023 0.1985 1.0481 0.057 Uiso 1 1 calc R . .
C65 C 0.2742(4) 0.77912(19) 0.5236(4) 0.0292(15) Uani 1 1 d . . .
H65 H 0.2510 0.7925 0.4749 0.035 Uiso 1 1 calc R . .
C66 C 0.2130(4) 0.76993(19) 0.5839(4) 0.0316(16) Uani 1 1 d . . .
H66 H 0.1499 0.7781 0.5765 0.038 Uiso 1 1 calc R . .
C67 C 0.2422(4) 0.74908(19) 0.6545(4) 0.0278(15) Uani 1 1 d . . .
C68 C 0.3341(4) 0.7381(2) 0.6608(4) 0.0468(19) Uani 1 1 d . . .
H68 H 0.3583 0.7233 0.7077 0.056 Uiso 1 1 calc R . .
C69 C 0.3911(4) 0.7488(3) 0.5982(4) 0.047(2) Uani 1 1 d . . .
H69 H 0.4543 0.7404 0.6038 0.056 Uiso 1 1 calc R . .
C70 C 0.0311(4) 0.7175(2) 0.7659(4) 0.0322(16) Uani 1 1 d . . .
H70 H -0.0310 0.7092 0.7528 0.039 Uiso 1 1 calc R . .
C71 C 0.0912(5) 0.7249(2) 0.6971(4) 0.0405(18) Uani 1 1 d . . .
H71 H 0.0715 0.7215 0.6419 0.049 Uiso 1 1 calc R . .
C72 C 0.1780(4) 0.73726(18) 0.7212(4) 0.0279(15) Uani 1 1 d . . .
C73 C 0.2062(4) 0.73959(19) 0.8023(4) 0.0331(16) Uani 1 1 d . . .
H73 H 0.2682 0.7471 0.8174 0.040 Uiso 1 1 calc R . .
C74 C 0.1433(4) 0.73089(18) 0.8600(4) 0.0303(15) Uani 1 1 d . . .
H74 H 0.1637 0.7319 0.9153 0.036 Uiso 1 1 calc R . .
H9A H 0.091(2) 0.375(3) 0.014(3) 0.08(3) Uiso 1 1 d D . .
H3A H 1.030(2) 0.642(3) 1.301(3) 0.093 Uiso 1 1 d D . .


_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
Ni1 O11A 2.018(13) 4_566 ?
Ni1 O11B 2.059(14) 4_566 ?
Ni1 O4 2.047(4) 2_647 ?
Ni1 N2 2.075(6) 4_566 ?
Ni1 N1 2.087(6) . ?
Ni1 O2 2.131(4) . ?
Ni1 O1 2.151(4) . ?
Ni1 C13 2.467(7) . ?
N1 C64 1.340(8) . ?
N1 C60 1.362(9) . ?
C1 C6 1.390(8) . ?
C1 C2 1.394(8) . ?
C1 C7 1.487(9) . ?
Ni2 O5 2.028(4) . ?
Ni2 O10 2.029(4) 3_566 ?
Ni2 O8 2.102(4) 4_576 ?
Ni2 N3 2.103(5) 4_576 ?
Ni2 N4 2.105(5) . ?
Ni2 O7 2.133(4) 4_576 ?
Ni2 C40 2.440(6) 4_576 ?
N2 C59 1.315(8) . ?
N2 C55 1.381(8) . ?
N2 Ni1 2.075(6) 4_665 ?
C2 C3 1.397(9) . ?
C2 H2 0.9500 . ?
N3 C65 1.334(7) . ?
N3 C69 1.333(8) . ?
N3 Ni2 2.103(5) 4_675 ?
C3 C4 1.377(8) . ?
C3 C14 1.506(8) . ?
N4 C70 1.311(7) . ?
N4 C74 1.350(7) . ?
C4 C5 1.386(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(9) . ?
C5 C21 1.504(8) . ?
C6 H6 0.9500 . ?
C7 C12 1.395(8) . ?
C7 C8 1.396(8) . ?
C8 C9 1.386(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.407(8) . ?
C10 C13 1.490(9) . ?
C11 C12 1.367(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O2 1.261(7) . ?
C13 O1 1.269(7) . ?
C14 C15 1.351(9) . ?
C14 C19 1.385(9) . ?
C15 C16 1.395(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(9) . ?
C17 C20 1.498(9) . ?
C18 C19 1.368(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 O4 1.258(8) . ?
C20 O3 1.281(8) . ?
O3 H3A 0.900(10) . ?
O4 Ni1 2.047(4) 2_657 ?
C21 C22 1.362(9) . ?
C21 C26 1.385(9) . ?
C22 C23 1.381(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.372(9) . ?
C24 C27 1.496(8) . ?
C25 C26 1.397(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 O5 1.237(7) . ?
C27 O6 1.267(7) . ?
C28 C33 1.389(8) . ?
C28 C29 1.391(8) . ?
C28 C34 1.485(8) . ?
C29 C30 1.373(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.402(8) . ?
C30 C41 1.495(8) . ?
C31 C32 1.397(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.412(8) . ?
C32 C48B 1.511(8) . ?
C32 C48A 1.512(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(8) . ?
C34 C39 1.392(8) . ?
C35 C36 1.407(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.373(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(8) . ?
C37 C40 1.485(8) . ?
C38 C39 1.384(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 O8 1.256(6) . ?
C40 O7 1.273(7) . ?
C40 Ni2 2.440(6) 4_675 ?
O7 Ni2 2.133(4) 4_675 ?
O8 Ni2 2.102(4) 4_675 ?
C41 C42 1.391(8) . ?
C41 C46 1.391(8) . ?
C42 C43 1.368(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.373(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.374(8) . ?
C44 C47 1.511(8) . ?
C45 C46 1.375(9) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 O10 1.229(7) . ?
C47 O9 1.277(8) . ?
O9 H9A 0.905(10) . ?
O10 Ni2 2.029(4) 3_566 ?
C48A C53A 1.398(13) . ?
C48A C49A 1.406(13) . ?
C49A C50A 1.387(13) . ?
C49A H49A 0.9500 . ?
C50A C51A 1.401(18) . ?
C50A H50A 0.9500 . ?
C51A C52A 1.373(14) . ?
C51A C54A 1.498(13) . ?
C52A C53A 1.391(13) . ?
C52A H52A 0.9500 . ?
C53A H53A 0.9500 . ?
C54A O11A 1.283(13) . ?
C54A O12A 1.262(13) . ?
O11A Ni1 2.019(13) 4_665 ?
C48B C53B 1.375(15) . ?
C48B C49B 1.386(14) . ?
C49B C50B 1.381(14) . ?
C49B H49B 0.9500 . ?
C50B C51B 1.386(19) . ?
C50B H50B 0.9500 . ?
C51B C52B 1.405(15) . ?
C51B C54B 1.496(14) . ?
C52B C53B 1.387(14) . ?
C52B H52B 0.9500 . ?
C53B H53B 0.9500 . ?
C54B O11B 1.273(15) . ?
C54B O12B 1.265(13) . ?
O11B Ni1 2.059(14) 4_665 ?
C55 C56 1.265(10) . ?
C55 H55 0.9500 . ?
C56 C57 1.388(8) . ?
C56 H56 0.9500 . ?
C57 C58 1.382(9) . ?
C57 C62 1.469(9) . ?
C58 C59 1.379(10) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C60 C61 1.346(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.377(9) . ?
C61 H61 0.9500 . ?
C62 C63 1.403(9) . ?
C63 C64 1.365(10) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.381(9) . ?
C65 H65 0.9500 . ?
C66 C67 1.377(8) . ?
C66 H66 0.9500 . ?
C67 C68 1.371(8) . ?
C67 C72 1.505(9) . ?
C68 C69 1.380(10) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C70 C71 1.469(9) . ?
C70 H70 0.9500 . ?
C71 C72 1.357(8) . ?
C71 H71 0.9500 . ?
C72 C73 1.388(9) . ?
C73 C74 1.363(9) . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?

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
O11A Ni1 O11B 9.5(8) 4_566 4_566 ?
O11A Ni1 O4 112.2(4) 4_566 2_647 ?
O11B Ni1 O4 103.0(5) 4_566 2_647 ?
O11A Ni1 N2 89.9(3) 4_566 4_566 ?
O11B Ni1 N2 88.8(3) 4_566 4_566 ?
O4 Ni1 N2 96.67(19) 2_647 4_566 ?
O11A Ni1 N1 90.6(3) 4_566 . ?
O11B Ni1 N1 92.6(3) 4_566 . ?
O4 Ni1 N1 88.1(2) 2_647 . ?
N2 Ni1 N1 174.6(2) 4_566 . ?
O11A Ni1 O2 155.2(4) 4_566 . ?
O11B Ni1 O2 164.6(5) 4_566 . ?
O4 Ni1 O2 92.43(16) 2_647 . ?
N2 Ni1 O2 89.29(18) 4_566 . ?
N1 Ni1 O2 88.01(19) . . ?
O11A Ni1 O1 93.6(4) 4_566 . ?
O11B Ni1 O1 103.0(5) 4_566 . ?
O4 Ni1 O1 153.98(17) 2_647 . ?
N2 Ni1 O1 86.09(19) 4_566 . ?
N1 Ni1 O1 88.5(2) . . ?
O2 Ni1 O1 61.66(15) . . ?
O11A Ni1 C13 124.5(4) 4_566 . ?
O11B Ni1 C13 133.9(5) 4_566 . ?
O4 Ni1 C13 123.09(19) 2_647 . ?
N2 Ni1 C13 87.9(2) 4_566 . ?
N1 Ni1 C13 87.4(2) . . ?
O2 Ni1 C13 30.73(16) . . ?
O1 Ni1 C13 30.94(16) . . ?
C64 N1 C60 113.9(7) . . ?
C64 N1 Ni1 125.1(5) . . ?
C60 N1 Ni1 120.7(5) . . ?
C6 C1 C2 117.5(6) . . ?
C6 C1 C7 120.3(6) . . ?
C2 C1 C7 122.1(5) . . ?
O5 Ni2 O10 106.75(16) . 3_566 ?
O5 Ni2 O8 154.24(16) . 4_576 ?
O10 Ni2 O8 97.81(16) 3_566 4_576 ?
O5 Ni2 N3 97.36(18) . 4_576 ?
O10 Ni2 N3 93.16(18) 3_566 4_576 ?
O8 Ni2 N3 88.81(17) 4_576 4_576 ?
O5 Ni2 N4 86.53(17) . . ?
O10 Ni2 N4 89.03(17) 3_566 . ?
O8 Ni2 N4 86.19(17) 4_576 . ?
N3 Ni2 N4 174.77(18) 4_576 . ?
O5 Ni2 O7 92.63(15) . 4_576 ?
O10 Ni2 O7 160.04(16) 3_566 4_576 ?
O8 Ni2 O7 62.37(15) 4_576 4_576 ?
N3 Ni2 O7 88.99(17) 4_576 4_576 ?
N4 Ni2 O7 87.34(17) . 4_576 ?
O5 Ni2 C40 123.63(18) . 4_576 ?
O10 Ni2 C40 128.67(18) 3_566 4_576 ?
O8 Ni2 C40 31.00(16) 4_576 4_576 ?
N3 Ni2 C40 89.9(2) 4_576 4_576 ?
N4 Ni2 C40 85.05(19) . 4_576 ?
O7 Ni2 C40 31.42(16) 4_576 4_576 ?
C59 N2 C55 113.2(6) . . ?
C59 N2 Ni1 123.1(5) . 4_665 ?
C55 N2 Ni1 123.5(4) . 4_665 ?
C1 C2 C3 122.0(6) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C65 N3 C69 115.2(5) . . ?
C65 N3 Ni2 125.4(4) . 4_675 ?
C69 N3 Ni2 118.6(4) . 4_675 ?
C4 C3 C2 119.1(6) . . ?
C4 C3 C14 120.8(5) . . ?
C2 C3 C14 120.1(5) . . ?
C70 N4 C74 115.0(5) . . ?
C70 N4 Ni2 125.5(4) . . ?
C74 N4 Ni2 118.7(4) . . ?
C3 C4 C5 121.1(6) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 118.8(6) . . ?
C4 C5 C21 122.6(6) . . ?
C6 C5 C21 118.6(5) . . ?
C1 C6 C5 121.5(6) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C12 C7 C8 117.8(6) . . ?
C12 C7 C1 121.3(5) . . ?
C8 C7 C1 120.7(5) . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 120.9(6) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C11 118.1(6) . . ?
C9 C10 C13 121.2(6) . . ?
C11 C10 C13 120.7(5) . . ?
C12 C11 C10 120.5(6) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C7 121.8(6) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 119.1 . . ?
O2 C13 O1 120.4(6) . . ?
O2 C13 C10 120.6(5) . . ?
O1 C13 C10 119.1(6) . . ?
O2 C13 Ni1 59.8(3) . . ?
O1 C13 Ni1 60.6(3) . . ?
C10 C13 Ni1 177.6(5) . . ?
C13 O1 Ni1 88.4(4) . . ?
C13 O2 Ni1 89.5(3) . . ?
C15 C14 C19 117.2(6) . . ?
C15 C14 C3 122.5(6) . . ?
C19 C14 C3 120.1(6) . . ?
C14 C15 C16 123.0(7) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C17 C16 C15 117.8(7) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
C18 C17 C16 120.3(6) . . ?
C18 C17 C20 121.0(6) . . ?
C16 C17 C20 118.6(6) . . ?
C19 C18 C17 119.2(7) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C14 122.4(7) . . ?
C18 C19 H19 118.8 . . ?
C14 C19 H19 118.8 . . ?
O4 C20 O3 124.7(6) . . ?
O4 C20 C17 119.2(6) . . ?
O3 C20 C17 116.1(6) . . ?
C20 O3 H3A 121(4) . . ?
C20 O4 Ni1 132.5(4) . 2_657 ?
C22 C21 C26 119.2(6) . . ?
C22 C21 C5 121.9(6) . . ?
C26 C21 C5 118.8(6) . . ?
C21 C22 C23 121.7(7) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C24 120.1(7) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 117.9(6) . . ?
C25 C24 C27 120.8(6) . . ?
C23 C24 C27 121.3(6) . . ?
C24 C25 C26 122.0(6) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C21 C26 C25 118.9(6) . . ?
C21 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
O5 C27 O6 124.0(6) . . ?
O5 C27 C24 119.7(6) . . ?
O6 C27 C24 115.9(6) . . ?
C27 O5 Ni2 139.2(4) . . ?
C33 C28 C29 118.4(6) . . ?
C33 C28 C34 120.3(5) . . ?
C29 C28 C34 121.3(5) . . ?
C30 C29 C28 121.9(6) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.0 . . ?
C29 C30 C31 119.1(5) . . ?
C29 C30 C41 119.6(5) . . ?
C31 C30 C41 121.0(5) . . ?
C32 C31 C30 121.1(5) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C33 117.7(5) . . ?
C31 C32 C48B 124.4(7) . . ?
C33 C32 C48B 116.4(7) . . ?
C31 C32 C48A 118.4(7) . . ?
C33 C32 C48A 123.4(7) . . ?
C48B C32 C48A 19.8(9) . . ?
C28 C33 C32 121.6(5) . . ?
C28 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C35 C34 C39 117.3(6) . . ?
C35 C34 C28 122.2(6) . . ?
C39 C34 C28 120.5(5) . . ?
C34 C35 C36 121.3(6) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C37 C36 C35 120.4(6) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 118.8(5) . . ?
C36 C37 C40 121.0(5) . . ?
C38 C37 C40 120.2(5) . . ?
C39 C38 C37 120.5(6) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C34 121.6(6) . . ?
C38 C39 H39 119.2 . . ?
C34 C39 H39 119.2 . . ?
O8 C40 O7 120.3(5) . . ?
O8 C40 C37 119.6(5) . . ?
O7 C40 C37 120.1(5) . . ?
O8 C40 Ni2 59.5(3) . 4_675 ?
O7 C40 Ni2 60.9(3) . 4_675 ?
C37 C40 Ni2 176.1(5) . 4_675 ?
C40 O7 Ni2 87.7(3) . 4_675 ?
C40 O8 Ni2 89.5(3) . 4_675 ?
C42 C41 C46 116.3(6) . . ?
C42 C41 C30 120.1(5) . . ?
C46 C41 C30 123.6(6) . . ?
C43 C42 C41 122.8(6) . . ?
C43 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C42 C43 C44 119.6(6) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C45 119.1(5) . . ?
C43 C44 C47 120.2(6) . . ?
C45 C44 C47 120.7(5) . . ?
C46 C45 C44 121.1(6) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C45 C46 C41 120.9(6) . . ?
C45 C46 H46 119.6 . . ?
C41 C46 H46 119.6 . . ?
O10 C47 O9 125.8(6) . . ?
O10 C47 C44 120.6(6) . . ?
O9 C47 C44 113.6(6) . . ?
C47 O9 H9A 121(5) . . ?
C47 O10 Ni2 133.8(4) . 3_566 ?
C53A C48A C49A 115.9(8) . . ?
C53A C48A C32 124.0(9) . . ?
C49A C48A C32 119.3(9) . . ?
C50A C49A C48A 120.1(12) . . ?
C50A C49A H49A 120.0 . . ?
C48A C49A H49A 119.9 . . ?
C49A C50A C51A 123.7(14) . . ?
C49A C50A H50A 118.1 . . ?
C51A C50A H50A 118.1 . . ?
C52A C51A C50A 115.5(10) . . ?
C52A C51A C54A 120.7(10) . . ?
C50A C51A C54A 123.0(11) . . ?
C51A C52A C53A 121.9(10) . . ?
C51A C52A H52A 119.1 . . ?
C53A C52A H52A 119.1 . . ?
C52A C53A C48A 122.6(10) . . ?
C52A C53A H53A 118.7 . . ?
C48A C53A H53A 118.7 . . ?
O11A C54A O12A 125.8(11) . . ?
O11A C54A C51A 116.1(11) . . ?
O12A C54A C51A 118.1(10) . . ?
C54A O11A Ni1 132.2(11) . 4_665 ?
C53B C48B C49B 122.4(9) . . ?
C53B C48B C32 118.5(9) . . ?
C49B C48B C32 119.1(10) . . ?
C50B C49B C48B 118.4(13) . . ?
C50B C49B H49B 120.8 . . ?
C48B C49B H49B 120.8 . . ?
C49B C50B C51B 120.4(15) . . ?
C49B C50B H50B 119.8 . . ?
C51B C50B H50B 119.8 . . ?
C50B C51B C52B 120.3(11) . . ?
C50B C51B C54B 121.2(10) . . ?
C52B C51B C54B 117.7(11) . . ?
C53B C52B C51B 119.1(12) . . ?
C53B C52B H52B 120.4 . . ?
C51B C52B H52B 120.5 . . ?
C48B C53B C52B 119.3(11) . . ?
C48B C53B H53B 120.4 . . ?
C52B C53B H53B 120.4 . . ?
O11B C54B O12B 128.1(12) . . ?
O11B C54B C51B 118.3(13) . . ?
O12B C54B C51B 113.6(10) . . ?
C54B O11B Ni1 127.4(11) . 4_665 ?
C56 C55 N2 127.6(6) . . ?
C56 C55 H55 116.2 . . ?
N2 C55 H55 116.2 . . ?
C55 C56 C57 119.1(7) . . ?
C55 C56 H56 120.4 . . ?
C57 C56 H56 120.4 . . ?
C58 C57 C56 116.6(7) . . ?
C58 C57 C62 122.2(5) . . ?
C56 C57 C62 121.1(6) . . ?
C59 C58 C57 119.4(6) . . ?
C59 C58 H58 120.3 . . ?
C57 C58 H58 120.3 . . ?
N2 C59 C58 123.7(6) . . ?
N2 C59 H59 118.2 . . ?
C58 C59 H59 118.2 . . ?
C61 C60 N1 124.8(6) . . ?
C61 C60 H60 117.6 . . ?
N1 C60 H60 117.6 . . ?
C60 C61 C62 121.0(7) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 H61 119.5 . . ?
C61 C62 C63 115.4(6) . . ?
C61 C62 C57 122.4(6) . . ?
C63 C62 C57 122.2(5) . . ?
C64 C63 C62 119.9(6) . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
N1 C64 C63 124.9(7) . . ?
N1 C64 H64 117.6 . . ?
C63 C64 H64 117.6 . . ?
N3 C65 C66 123.0(6) . . ?
N3 C65 H65 118.5 . . ?
C66 C65 H65 118.5 . . ?
C67 C66 C65 121.0(5) . . ?
C67 C66 H66 119.5 . . ?
C65 C66 H66 119.5 . . ?
C68 C67 C66 116.4(6) . . ?
C68 C67 C72 120.5(6) . . ?
C66 C67 C72 123.2(5) . . ?
C67 C68 C69 119.2(6) . . ?
C67 C68 H68 120.4 . . ?
C69 C68 H68 120.4 . . ?
N3 C69 C68 125.1(6) . . ?
N3 C69 H69 117.5 . . ?
C68 C69 H69 117.5 . . ?
N4 C70 C71 127.3(5) . . ?
N4 C70 H70 116.4 . . ?
C71 C70 H70 116.4 . . ?
C72 C71 C70 112.4(6) . . ?
C72 C71 H71 123.8 . . ?
C70 C71 H71 123.8 . . ?
C71 C72 C73 122.4(6) . . ?
C71 C72 C67 115.9(5) . . ?
C73 C72 C67 121.7(5) . . ?
C74 C73 C72 118.8(6) . . ?
C74 C73 H73 120.6 . . ?
C72 C73 H73 120.6 . . ?
N4 C74 C73 123.9(6) . . ?
N4 C74 H74 118.0 . . ?
C73 C74 H74 118.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O11A Ni1 N1 C64 -115.3(6) 4_566 . . . ?
O11B Ni1 N1 C64 -105.9(7) 4_566 . . . ?
O4 Ni1 N1 C64 -3.0(5) 2_647 . . . ?
N2 Ni1 N1 C64 149.4(19) 4_566 . . . ?
O2 Ni1 N1 C64 89.5(5) . . . . ?
O1 Ni1 N1 C64 151.1(5) . . . . ?
C13 Ni1 N1 C64 120.2(5) . . . . ?
O11A Ni1 N1 C60 70.7(6) 4_566 . . . ?
O11B Ni1 N1 C60 80.1(7) 4_566 . . . ?
O4 Ni1 N1 C60 -177.0(5) 2_647 . . . ?
N2 Ni1 N1 C60 -25(2) 4_566 . . . ?
O2 Ni1 N1 C60 -84.5(5) . . . . ?
O1 Ni1 N1 C60 -22.8(5) . . . . ?
C13 Ni1 N1 C60 -53.8(5) . . . . ?
C6 C1 C2 C3 1.4(10) . . . . ?
C7 C1 C2 C3 -176.8(6) . . . . ?
C1 C2 C3 C4 -0.7(10) . . . . ?
C1 C2 C3 C14 178.3(6) . . . . ?
O5 Ni2 N4 C70 141.4(5) . . . . ?
O10 Ni2 N4 C70 34.6(5) 3_566 . . . ?
O8 Ni2 N4 C70 -63.3(5) 4_576 . . . ?
N3 Ni2 N4 C70 -80(2) 4_576 . . . ?
O7 Ni2 N4 C70 -125.8(5) 4_576 . . . ?
C40 Ni2 N4 C70 -94.4(5) 4_576 . . . ?
O5 Ni2 N4 C74 -49.0(4) . . . . ?
O10 Ni2 N4 C74 -155.9(4) 3_566 . . . ?
O8 Ni2 N4 C74 106.3(4) 4_576 . . . ?
N3 Ni2 N4 C74 89(2) 4_576 . . . ?
O7 Ni2 N4 C74 43.8(4) 4_576 . . . ?
C40 Ni2 N4 C74 75.2(4) 4_576 . . . ?
C2 C3 C4 C5 0.8(10) . . . . ?
C14 C3 C4 C5 -178.1(6) . . . . ?
C3 C4 C5 C6 -1.7(10) . . . . ?
C3 C4 C5 C21 179.9(6) . . . . ?
C2 C1 C6 C5 -2.3(10) . . . . ?
C7 C1 C6 C5 176.0(6) . . . . ?
C4 C5 C6 C1 2.4(10) . . . . ?
C21 C5 C6 C1 -179.1(6) . . . . ?
C6 C1 C7 C12 -150.1(6) . . . . ?
C2 C1 C7 C12 28.0(10) . . . . ?
C6 C1 C7 C8 24.7(10) . . . . ?
C2 C1 C7 C8 -157.2(6) . . . . ?
C12 C7 C8 C9 1.8(9) . . . . ?
C1 C7 C8 C9 -173.3(6) . . . . ?
C7 C8 C9 C10 -0.7(10) . . . . ?
C8 C9 C10 C11 -1.4(10) . . . . ?
C8 C9 C10 C13 179.4(6) . . . . ?
C9 C10 C11 C12 2.5(10) . . . . ?
C13 C10 C11 C12 -178.3(7) . . . . ?
C10 C11 C12 C7 -1.5(11) . . . . ?
C8 C7 C12 C11 -0.6(10) . . . . ?
C1 C7 C12 C11 174.3(6) . . . . ?
C9 C10 C13 O2 178.6(6) . . . . ?
C11 C10 C13 O2 -0.6(10) . . . . ?
C9 C10 C13 O1 -0.6(10) . . . . ?
C11 C10 C13 O1 -179.8(6) . . . . ?
C9 C10 C13 Ni1 82(12) . . . . ?
C11 C10 C13 Ni1 -97(12) . . . . ?
O11A Ni1 C13 O2 -179.4(5) 4_566 . . . ?
O11B Ni1 C13 O2 178.4(5) 4_566 . . . ?
O4 Ni1 C13 O2 -4.4(5) 2_647 . . . ?
N2 Ni1 C13 O2 92.2(4) 4_566 . . . ?
N1 Ni1 C13 O2 -90.4(4) . . . . ?
O1 Ni1 C13 O2 178.1(6) . . . . ?
O11A Ni1 C13 O1 2.5(6) 4_566 . . . ?
O11B Ni1 C13 O1 0.3(6) 4_566 . . . ?
O4 Ni1 C13 O1 177.5(3) 2_647 . . . ?
N2 Ni1 C13 O1 -85.9(4) 4_566 . . . ?
N1 Ni1 C13 O1 91.5(4) . . . . ?
O2 Ni1 C13 O1 -178.1(6) . . . . ?
O11A Ni1 C13 C10 -81(12) 4_566 . . . ?
O11B Ni1 C13 C10 -83(12) 4_566 . . . ?
O4 Ni1 C13 C10 94(12) 2_647 . . . ?
N2 Ni1 C13 C10 -170(12) 4_566 . . . ?
N1 Ni1 C13 C10 8(12) . . . . ?
O2 Ni1 C13 C10 98(12) . . . . ?
O1 Ni1 C13 C10 -84(12) . . . . ?
O2 C13 O1 Ni1 -1.9(6) . . . . ?
C10 C13 O1 Ni1 177.3(6) . . . . ?
O11A Ni1 O1 C13 -177.9(5) 4_566 . . . ?
O11B Ni1 O1 C13 -179.8(5) 4_566 . . . ?
O4 Ni1 O1 C13 -4.8(6) 2_647 . . . ?
N2 Ni1 O1 C13 92.4(4) 4_566 . . . ?
N1 Ni1 O1 C13 -87.4(4) . . . . ?
O2 Ni1 O1 C13 1.1(4) . . . . ?
O1 C13 O2 Ni1 1.9(6) . . . . ?
C10 C13 O2 Ni1 -177.3(6) . . . . ?
O11A Ni1 O2 C13 1.2(9) 4_566 . . . ?
O11B Ni1 O2 C13 -4.2(14) 4_566 . . . ?
O4 Ni1 O2 C13 176.3(4) 2_647 . . . ?
N2 Ni1 O2 C13 -87.0(4) 4_566 . . . ?
N1 Ni1 O2 C13 88.3(4) . . . . ?
O1 Ni1 O2 C13 -1.1(4) . . . . ?
C4 C3 C14 C15 -133.2(7) . . . . ?
C2 C3 C14 C15 47.9(9) . . . . ?
C4 C3 C14 C19 51.2(9) . . . . ?
C2 C3 C14 C19 -127.8(7) . . . . ?
C19 C14 C15 C16 3.0(11) . . . . ?
C3 C14 C15 C16 -172.7(6) . . . . ?
C14 C15 C16 C17 -0.5(11) . . . . ?
C15 C16 C17 C18 -2.2(11) . . . . ?
C15 C16 C17 C20 175.1(6) . . . . ?
C16 C17 C18 C19 2.4(11) . . . . ?
C20 C17 C18 C19 -174.9(6) . . . . ?
C17 C18 C19 C14 0.2(10) . . . . ?
C15 C14 C19 C18 -2.9(10) . . . . ?
C3 C14 C19 C18 173.0(6) . . . . ?
C18 C17 C20 O4 -16.9(10) . . . . ?
C16 C17 C20 O4 165.8(7) . . . . ?
C18 C17 C20 O3 163.1(7) . . . . ?
C16 C17 C20 O3 -14.2(10) . . . . ?
O3 C20 O4 Ni1 6.5(11) . . . 2_657 ?
C17 C20 O4 Ni1 -173.5(4) . . . 2_657 ?
C4 C5 C21 C22 -133.9(8) . . . . ?
C6 C5 C21 C22 47.8(10) . . . . ?
C4 C5 C21 C26 49.7(9) . . . . ?
C6 C5 C21 C26 -128.6(7) . . . . ?
C26 C21 C22 C23 -0.1(12) . . . . ?
C5 C21 C22 C23 -176.5(7) . . . . ?
C21 C22 C23 C24 0.3(12) . . . . ?
C22 C23 C24 C25 -2.7(11) . . . . ?
C22 C23 C24 C27 174.7(7) . . . . ?
C23 C24 C25 C26 5.1(10) . . . . ?
C27 C24 C25 C26 -172.3(6) . . . . ?
C22 C21 C26 C25 2.4(10) . . . . ?
C5 C21 C26 C25 178.9(6) . . . . ?
C24 C25 C26 C21 -5.0(10) . . . . ?
C25 C24 C27 O5 -11.6(9) . . . . ?
C23 C24 C27 O5 171.1(6) . . . . ?
C25 C24 C27 O6 161.9(6) . . . . ?
C23 C24 C27 O6 -15.4(9) . . . . ?
O6 C27 O5 Ni2 -4.9(11) . . . . ?
C24 C27 O5 Ni2 168.1(4) . . . . ?
O10 Ni2 O5 C27 -35.5(7) 3_566 . . . ?
O8 Ni2 O5 C27 162.8(6) 4_576 . . . ?
N3 Ni2 O5 C27 60.1(6) 4_576 . . . ?
N4 Ni2 O5 C27 -123.4(6) . . . . ?
O7 Ni2 O5 C27 149.4(6) 4_576 . . . ?
C40 Ni2 O5 C27 154.9(6) 4_576 . . . ?
C33 C28 C29 C30 -2.3(10) . . . . ?
C34 C28 C29 C30 177.1(6) . . . . ?
C28 C29 C30 C31 4.0(10) . . . . ?
C28 C29 C30 C41 -169.2(6) . . . . ?
C29 C30 C31 C32 -1.9(10) . . . . ?
C41 C30 C31 C32 171.2(6) . . . . ?
C30 C31 C32 C33 -1.7(10) . . . . ?
C30 C31 C32 C48B 164.0(9) . . . . ?
C30 C31 C32 C48A -173.9(8) . . . . ?
C29 C28 C33 C32 -1.6(10) . . . . ?
C34 C28 C33 C32 179.1(6) . . . . ?
C31 C32 C33 C28 3.5(10) . . . . ?
C48B C32 C33 C28 -163.4(9) . . . . ?
C48A C32 C33 C28 175.2(8) . . . . ?
C33 C28 C34 C35 -25.0(10) . . . . ?
C29 C28 C34 C35 155.7(6) . . . . ?
C33 C28 C34 C39 155.1(6) . . . . ?
C29 C28 C34 C39 -24.2(10) . . . . ?
C39 C34 C35 C36 0.1(10) . . . . ?
C28 C34 C35 C36 -179.8(6) . . . . ?
C34 C35 C36 C37 0.5(10) . . . . ?
C35 C36 C37 C38 0.9(10) . . . . ?
C35 C36 C37 C40 179.0(6) . . . . ?
C36 C37 C38 C39 -3.0(10) . . . . ?
C40 C37 C38 C39 178.9(6) . . . . ?
C37 C38 C39 C34 3.7(11) . . . . ?
C35 C34 C39 C38 -2.2(10) . . . . ?
C28 C34 C39 C38 177.7(6) . . . . ?
C36 C37 C40 O8 -175.5(6) . . . . ?
C38 C37 C40 O8 2.6(9) . . . . ?
C36 C37 C40 O7 5.0(9) . . . . ?
C38 C37 C40 O7 -176.9(6) . . . . ?
C36 C37 C40 Ni2 109(6) . . . 4_675 ?
C38 C37 C40 Ni2 -73(7) . . . 4_675 ?
O8 C40 O7 Ni2 -3.8(6) . . . 4_675 ?
C37 C40 O7 Ni2 175.7(5) . . . 4_675 ?
O7 C40 O8 Ni2 3.9(6) . . . 4_675 ?
C37 C40 O8 Ni2 -175.6(5) . . . 4_675 ?
C29 C30 C41 C42 24.3(10) . . . . ?
C31 C30 C41 C42 -148.7(7) . . . . ?
C29 C30 C41 C46 -155.4(7) . . . . ?
C31 C30 C41 C46 31.6(10) . . . . ?
C46 C41 C42 C43 -5.3(10) . . . . ?
C30 C41 C42 C43 175.0(6) . . . . ?
C41 C42 C43 C44 4.1(11) . . . . ?
C42 C43 C44 C45 -1.1(10) . . . . ?
C42 C43 C44 C47 -178.6(6) . . . . ?
C43 C44 C45 C46 -0.4(11) . . . . ?
C47 C44 C45 C46 177.1(7) . . . . ?
C44 C45 C46 C41 -1.0(12) . . . . ?
C42 C41 C46 C45 3.7(11) . . . . ?
C30 C41 C46 C45 -176.6(7) . . . . ?
C43 C44 C47 O10 -159.9(6) . . . . ?
C45 C44 C47 O10 22.6(9) . . . . ?
C43 C44 C47 O9 21.9(9) . . . . ?
C45 C44 C47 O9 -155.5(6) . . . . ?
O9 C47 O10 Ni2 5.2(10) . . . 3_566 ?
C44 C47 O10 Ni2 -172.7(4) . . . 3_566 ?
C31 C32 C48A C53A 140.9(11) . . . . ?
C33 C32 C48A C53A -30.8(16) . . . . ?
C48B C32 C48A C53A -106(3) . . . . ?
C31 C32 C48A C49A -49.8(15) . . . . ?
C33 C32 C48A C49A 138.6(11) . . . . ?
C48B C32 C48A C49A 63(2) . . . . ?
C53A C48A C49A C50A -3(2) . . . . ?
C32 C48A C49A C50A -172.9(14) . . . . ?
C48A C49A C50A C51A 0(3) . . . . ?
C49A C50A C51A C52A 5(3) . . . . ?
C49A C50A C51A C54A 174.1(15) . . . . ?
C50A C51A C52A C53A -6(2) . . . . ?
C54A C51A C52A C53A -176.0(12) . . . . ?
C51A C52A C53A C48A 4(2) . . . . ?
C49A C48A C53A C52A 1(2) . . . . ?
C32 C48A C53A C52A 170.7(11) . . . . ?
C52A C51A C54A O11A 168.9(13) . . . . ?
C50A C51A C54A O11A 0(2) . . . . ?
C52A C51A C54A O12A -11(2) . . . . ?
C50A C51A C54A O12A -179.6(16) . . . . ?
O12A C54A O11A Ni1 10(2) . . . 4_665 ?
C51A C54A O11A Ni1 -169.2(9) . . . 4_665 ?
C31 C32 C48B C53B -144.5(12) . . . . ?
C33 C32 C48B C53B 21.4(17) . . . . ?
C48A C32 C48B C53B 137(3) . . . . ?
C31 C32 C48B C49B 35.1(18) . . . . ?
C33 C32 C48B C49B -159.0(12) . . . . ?
C48A C32 C48B C49B -43.3(19) . . . . ?
C53B C48B C49B C50B -2(3) . . . . ?
C32 C48B C49B C50B 178.9(16) . . . . ?
C48B C49B C50B C51B -1(3) . . . . ?
C49B C50B C51B C52B 4(3) . . . . ?
C49B C50B C51B C54B 173.5(16) . . . . ?
C50B C51B C52B C53B -5(2) . . . . ?
C54B C51B C52B C53B -174.9(13) . . . . ?
C49B C48B C53B C52B 0(2) . . . . ?
C32 C48B C53B C52B 180.0(12) . . . . ?
C51B C52B C53B C48B 3(2) . . . . ?
C50B C51B C54B O11B 19(2) . . . . ?
C52B C51B C54B O11B -171.2(13) . . . . ?
C50B C51B C54B O12B -162.7(17) . . . . ?
C52B C51B C54B O12B 7.2(18) . . . . ?
O12B C54B O11B Ni1 16(2) . . . 4_665 ?
C51B C54B O11B Ni1 -166.1(10) . . . 4_665 ?
C59 N2 C55 C56 7.3(12) . . . . ?
Ni1 N2 C55 C56 -167.1(7) 4_665 . . . ?
N2 C55 C56 C57 -6.1(14) . . . . ?
C55 C56 C57 C58 0.6(11) . . . . ?
C55 C56 C57 C62 179.5(7) . . . . ?
C56 C57 C58 C59 2.8(9) . . . . ?
C62 C57 C58 C59 -176.1(6) . . . . ?
C55 N2 C59 C58 -3.2(9) . . . . ?
Ni1 N2 C59 C58 171.2(5) 4_665 . . . ?
C57 C58 C59 N2 -1.3(10) . . . . ?
C64 N1 C60 C61 1.5(10) . . . . ?
Ni1 N1 C60 C61 176.1(6) . . . . ?
N1 C60 C61 C62 -2.8(11) . . . . ?
C60 C61 C62 C63 3.1(10) . . . . ?
C60 C61 C62 C57 -177.0(6) . . . . ?
C58 C57 C62 C61 -28.5(9) . . . . ?
C56 C57 C62 C61 152.7(7) . . . . ?
C58 C57 C62 C63 151.4(6) . . . . ?
C56 C57 C62 C63 -27.4(9) . . . . ?
C61 C62 C63 C64 -2.4(9) . . . . ?
C57 C62 C63 C64 177.8(6) . . . . ?
C60 N1 C64 C63 -0.8(10) . . . . ?
Ni1 N1 C64 C63 -175.1(5) . . . . ?
C62 C63 C64 N1 1.3(10) . . . . ?
C69 N3 C65 C66 4.0(9) . . . . ?
Ni2 N3 C65 C66 174.2(4) 4_675 . . . ?
N3 C65 C66 C67 -2.4(9) . . . . ?
C65 C66 C67 C68 -0.2(9) . . . . ?
C65 C66 C67 C72 -178.4(5) . . . . ?
C66 C67 C68 C69 0.9(10) . . . . ?
C72 C67 C68 C69 179.1(6) . . . . ?
C65 N3 C69 C68 -3.4(10) . . . . ?
Ni2 N3 C69 C68 -174.3(6) 4_675 . . . ?
C67 C68 C69 N3 1.0(12) . . . . ?
C74 N4 C70 C71 -2.7(9) . . . . ?
Ni2 N4 C70 C71 167.2(5) . . . . ?
N4 C70 C71 C72 -0.9(9) . . . . ?
C70 C71 C72 C73 3.7(9) . . . . ?
C70 C71 C72 C67 -175.4(5) . . . . ?
C68 C67 C72 C71 -143.3(6) . . . . ?
C66 C67 C72 C71 34.9(8) . . . . ?
C68 C67 C72 C73 37.7(9) . . . . ?
C66 C67 C72 C73 -144.2(6) . . . . ?
C71 C72 C73 C74 -2.7(9) . . . . ?
C67 C72 C73 C74 176.3(5) . . . . ?
C70 N4 C74 C73 4.0(8) . . . . ?
Ni2 N4 C74 C73 -166.6(5) . . . . ?
C72 C73 C74 N4 -1.6(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O9 H9A O6 0.91(4) 1.50(4) 2.403(7) 169(6) 3_566 yes
C16 H16 O6 0.9500 2.4700 3.335(9) 152.00 1_655 yes
C58 H58 O8 0.9500 2.2700 3.080(8) 143.00 3_666 yes
C60 H60 O1 0.9500 2.4000 2.967(9) 118.00 . yes
C64 H64 O4 0.9500 2.3600 2.948(9) 120.00 2_647 yes
C69 H69 O7 0.9500 2.4600 2.984(8) 115.00 . yes
C70 H70 O10 0.9500 2.6000 3.116(7) 115.00 3_566 yes
C74 H74 O5 0.9500 2.5900 3.045(8) 110.00 . yes

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        21.15
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.085

data_rh195m
_database_code_depnum_ccdc_archive 'CCDC 692027'

_audit_update_record             
;
2007-11-08 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            RH195
_chemical_melting_point          ?
_chemical_formula_moiety         
'(Ni 2+)3, (C27 H15 O6 3-)2, (C2 H6 O2)3, (C10 H8 N2)3, (C7 H8)3'
_chemical_formula_sum            'C111 H96 N6 Ni3 O18'
_chemical_formula_weight         1978.07

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'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   31.053(2)
_cell_length_b                   31.053(2)
_cell_length_c                   16.9025(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14115.3(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1525
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      17.7

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6192
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8667
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_process_details   'SADABS-2007/4 (Sheldrick, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       'ω scans with a narrow frame width'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27213
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3603
_reflns_number_gt                2361
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_cell_refinement       'SAINT v6.45a (Bruker, 2005)'
_computing_data_reduction        'SAINT v6.45a (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0874P)²+0.0000P] 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         3598
_refine_ls_number_parameters     242
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1487
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.967
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.285576(16) 0.3333 0.0833 0.01564(18) Uani 1 2 d S . .
O1 O 0.24498(8) 0.25894(8) 0.10422(13) 0.0233(5) Uani 1 1 d . . .
O3 O 0.34345(8) 0.34646(9) 0.16035(13) 0.0261(5) Uani 1 1 d D . .
O2 O 0.26038(9) 0.22520(9) -0.00022(16) 0.0370(7) Uani 1 1 d . . .
N1 N 0.23886(9) 0.32776(10) -0.00910(15) 0.0198(6) Uani 1 1 d . . .
C1 C 0.23486(12) 0.22304(12) 0.0580(2) 0.0243(8) Uani 1 1 d . . .
C2 C 0.18833(12) 0.17470(12) 0.0764(2) 0.0251(8) Uani 1 1 d . . .
C9 C 0.04141(13) -0.00572(12) 0.1135(2) 0.0342(9) Uani 1 1 d . . .
H9 H 0.0699 -0.0095 0.1139 0.041 Uiso 1 1 calc R . .
C6 C 0.11027(13) 0.13031(13) 0.1472(2) 0.0350(9) Uani 1 1 d . . .
H6 H 0.0879 0.1302 0.1856 0.042 Uiso 1 1 calc R . .
C3 C 0.17671(12) 0.13136(12) 0.0370(2) 0.0282(8) Uani 1 1 d . . .
H3 H 0.1994 0.1312 -0.0005 0.034 Uiso 1 1 calc R . .
C8 C 0.04750(13) 0.04209(12) 0.1133(2) 0.0331(9) Uani 1 1 d . . .
C12 C 0.18169(12) 0.33186(13) -0.1340(2) 0.0294(8) Uani 1 1 d . . .
C5 C 0.09765(12) 0.08678(12) 0.1050(2) 0.0308(9) Uani 1 1 d . . .
C4 C 0.13233(12) 0.08799(12) 0.0514(2) 0.0314(9) Uani 1 1 d . . .
H4 H 0.1254 0.0584 0.0242 0.038 Uiso 1 1 calc R . .
C7 C 0.15515(12) 0.17366(12) 0.1336(2) 0.0291(8) Uani 1 1 d . . .
H7 H 0.1634 0.2028 0.1633 0.035 Uiso 1 1 calc R . .
C15 C 0.38373(17) 0.3483(2) 0.1183(3) 0.0624(14) Uani 1 1 d . . .
H11B H 0.4015 0.3369 0.1536 0.075 Uiso 1 1 calc R . .
H11A H 0.4073 0.3832 0.1036 0.075 Uiso 1 1 calc R . .
C11 C 0.16058(15) 0.3048(2) -0.0666(3) 0.092(2) Uani 1 1 d . . .
H11 H 0.1254 0.2869 -0.0612 0.110 Uiso 1 1 calc R . .
C10 C 0.19013(15) 0.30345(19) -0.0063(3) 0.0666(16) Uani 1 1 d . . .
H10 H 0.1743 0.2840 0.0392 0.080 Uiso 1 1 calc R . .
C14 C 0.25913(13) 0.35462(17) -0.0732(2) 0.0432(11) Uani 1 1 d . . .
H14 H 0.2944 0.3735 -0.0763 0.052 Uiso 1 1 calc R . .
C13 C 0.23174(10) 0.35663(13) -0.1360(2) 0.0363(10) Uani 1 1 d . . .
H13 H 0.2485 0.3758 -0.1814 0.044 Uiso 1 1 calc R . .
C2S C 0.49344(10) 0.33842(13) 0.1580(2) 0.035(3) Uani 0.50 1 d PRDU A -1
H2S H 0.4882 0.3310 0.2117 0.042 Uiso 0.50 1 d PR B -1
C3S C 0.4800(2) 0.3020(3) 0.1022(6) 0.063(3) Uani 0.50 1 d PDU A -1
H3S H 0.4647 0.2686 0.1206 0.076 Uiso 0.50 1 calc PR A -1
C1S C 0.5155(2) 0.3861(3) 0.1288(5) 0.073(4) Uani 0.50 1 d PDU A -1
C7S C 0.5303(4) 0.4261(4) 0.1885(6) 0.31(2) Uani 0.50 1 d PDU A -1
H7S1 H 0.5007 0.4269 0.2068 0.468 Uiso 0.50 1 calc PR A -1
H7S2 H 0.5537 0.4582 0.1646 0.468 Uiso 0.50 1 calc PR A -1
H7S3 H 0.5461 0.4196 0.2335 0.468 Uiso 0.50 1 calc PR A -1
C5S C 0.5102(3) 0.3611(5) -0.0020(6) 0.099(5) Uani 0.50 1 d PDU A -1
H5S H 0.5159 0.3687 -0.0568 0.118 Uiso 0.50 1 calc PR A -1
C6S C 0.5255(3) 0.4015(4) 0.0512(5) 0.070(3) Uani 0.50 1 d PDU A -1
H6S H 0.5409 0.4353 0.0352 0.084 Uiso 0.50 1 calc PR A -1
C4S C 0.4868(3) 0.30940(17) 0.0201(8) 0.100(6) Uani 0.50 1 d PDU A -1
H4S H 0.4770 0.2831 -0.0169 0.120 Uiso 0.50 1 calc PR A -1
H3O H 0.3571 0.3820 0.1735 0.14(3) Uiso 1 1 d RD . .


_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
Ni1 O1 2.034(2) . ?
Ni1 O1 2.034(2) 16_554 ?
Ni1 N1 2.079(2) 16_554 ?
Ni1 N1 2.080(2) . ?
Ni1 O3 2.088(2) . ?
Ni1 O3 2.088(2) 16_554 ?
O1 C1 1.266(4) . ?
O3 C15 1.415(5) . ?
O3 H3O 0.9900 . ?
O2 C1 1.244(4) . ?
N1 C10 1.311(4) . ?
N1 C14 1.320(4) . ?
C1 C2 1.506(5) . ?
C2 C3 1.379(5) . ?
C2 C7 1.401(5) . ?
C9 C8 1.382(5) 3 ?
C9 C8 1.400(5) . ?
C9 H9 0.9500 . ?
C6 C7 1.390(5) . ?
C6 C5 1.400(5) . ?
C6 H6 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C8 C9 1.382(5) 2 ?
C8 C5 1.487(5) . ?
C12 C13 1.347(4) . ?
C12 C11 1.372(5) . ?
C12 C12 1.478(6) 31_554 ?
C5 C4 1.393(5) . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C15 C15 1.430(8) 16_554 ?
C15 H11B 0.9900 . ?
C15 H11A 0.9900 . ?
C11 C10 1.386(6) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
C14 C13 1.381(5) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C2S C3S 1.368(10) . ?
C2S C1S 1.376(7) . ?
C2S H2S 0.9301 . ?
C3S C4S 1.405(14) . ?
C3S H3S 0.9500 . ?
C1S C6S 1.376(7) . ?
C1S C7S 1.484(5) . ?
C7S H7S1 0.9800 . ?
C7S H7S2 0.9800 . ?
C7S H7S3 0.9800 . ?
C5S C6S 1.419(14) . ?
C5S C4S 1.441(13) . ?
C5S H5S 0.9500 . ?
C6S H6S 0.9500 . ?
C4S H4S 0.9500 . ?

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
O1 Ni1 O1 174.04(13) . 16_554 ?
O1 Ni1 N1 84.62(10) . 16_554 ?
O1 Ni1 N1 91.47(10) 16_554 16_554 ?
O1 Ni1 N1 91.46(10) . . ?
O1 Ni1 N1 84.63(10) 16_554 . ?
N1 Ni1 N1 98.01(14) 16_554 . ?
O1 Ni1 O3 95.61(9) . . ?
O1 Ni1 O3 88.94(9) 16_554 . ?
N1 Ni1 O3 91.14(10) 16_554 . ?
N1 Ni1 O3 168.93(9) . . ?
O1 Ni1 O3 88.94(9) . 16_554 ?
O1 Ni1 O3 95.61(9) 16_554 16_554 ?
N1 Ni1 O3 168.93(9) 16_554 16_554 ?
N1 Ni1 O3 91.14(10) . 16_554 ?
O3 Ni1 O3 80.51(13) . 16_554 ?
C1 O1 Ni1 129.3(2) . . ?
C15 O3 Ni1 110.6(2) . . ?
C15 O3 H3O 101.0 . . ?
Ni1 O3 H3O 101.9 . . ?
C10 N1 C14 116.2(3) . . ?
C10 N1 Ni1 125.2(2) . . ?
C14 N1 Ni1 118.2(2) . . ?
O2 C1 O1 124.8(3) . . ?
O2 C1 C2 119.0(3) . . ?
O1 C1 C2 116.2(3) . . ?
C3 C2 C7 118.7(3) . . ?
C3 C2 C1 121.7(3) . . ?
C7 C2 C1 119.6(3) . . ?
C8 C9 C8 121.1(4) 3 . ?
C8 C9 H9 119.5 3 . ?
C8 C9 H9 119.5 . . ?
C7 C6 C5 120.8(3) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C9 C8 C9 118.9(4) 2 . ?
C9 C8 C5 119.9(3) 2 . ?
C9 C8 C5 120.9(3) . . ?
C13 C12 C11 115.6(3) . . ?
C13 C12 C12 122.0(4) . 31_554 ?
C11 C12 C12 122.4(4) . 31_554 ?
C4 C5 C6 117.8(3) . . ?
C4 C5 C8 121.4(3) . . ?
C6 C5 C8 120.7(3) . . ?
C3 C4 C5 121.4(3) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
O3 C15 C15 113.3(3) . 16_554 ?
O3 C15 H11B 108.9 . . ?
C15 C15 H11B 108.9 16_554 . ?
O3 C15 H11A 108.9 . . ?
C15 C15 H11A 108.9 16_554 . ?
H11B C15 H11A 107.7 . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
N1 C10 C11 123.2(4) . . ?
N1 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
N1 C14 C13 123.4(3) . . ?
N1 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
C12 C13 C14 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C3S C2S C1S 115.1(7) . . ?
C3S C2S H2S 121.6 . . ?
C1S C2S H2S 123.3 . . ?
C2S C3S C4S 125.9(7) . . ?
C2S C3S H3S 117.1 . . ?
C4S C3S H3S 117.1 . . ?
C2S C1S C6S 128.3(9) . . ?
C2S C1S C7S 115.9(5) . . ?
C6S C1S C7S 115.9(5) . . ?
C6S C5S C4S 125.4(9) . . ?
C6S C5S H5S 117.3 . . ?
C4S C5S H5S 117.3 . . ?
C1S C6S C5S 112.3(8) . . ?
C1S C6S H6S 123.8 . . ?
C5S C6S H6S 123.8 . . ?
C3S C4S C5S 112.9(8) . . ?
C3S C4S H4S 123.5 . . ?
C5S C4S H4S 123.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3O O2 0.9900 1.7000 2.651(4) 159.00 16_554 yes
C14 H14 O1 0.9500 2.5300 2.897(5) 103.00 16_554 yes

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.081


