Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'ProfD Roland Kraemer'
_publ_contact_author_address     
;
Anorganisch-Chemisches Institut
Im Neuenheimer Feld 270
Heidelberg
69120
GERMANY
;

_publ_contact_author_email       ROLAND.KRAEMER@URZ.UNI-HEIDELBERG.DE

_publ_section_title              
;
Synthesis, structure and magnetism of a new
ferromagnetic hexanuclear nickel cluster with a dicubane-like core
;
loop_
_publ_author_name
'Roland Kraemer'
'Igor O. Fritsky'
'Hans Pritzkow'
'Stefan Woerl'

data_sw45
_database_code_depnum_ccdc_archive 'CCDC 252084'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H54 N4 Ni6 O28, 2( C6 H16 N), 5( C2 H3 N), 2.6( H2 O)'
_chemical_formula_sum            'C106 H106 N11 Ni6 O31'
_chemical_formula_weight         2382.28

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_H-M   P2(1)/n

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                   17.9912(11)
_cell_length_b                   12.7070(8)
_cell_length_c                   22.8638(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2850(10)
_cell_angle_gamma                90.00
_cell_volume                     5225.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2470
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      103(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  'CCD area detector'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70348
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.31
_reflns_number_total             12638
_reflns_number_gt                9285
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;

As one solvent molecule (CH3CN ?) in a special position could not be
described satisfactorily,a correction with SQUEEZE(PLATON) was used for
it. The Et3NH-cation was disordered over two orientations (ca. 2:1 ).
For the latter orientation a peak was located, which probably belongs to
an additional H2O molecule.

Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0579P)^2^+11.7700P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'difmap and geom'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12638
_refine_ls_number_parameters     836
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1375
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.025
_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 0.42767(2) 0.34233(3) 0.44919(2) 0.02145(12) Uani 1 1 d . . .
Ni2 Ni 0.42366(2) 0.54425(3) 0.51591(2) 0.01926(11) Uani 1 1 d . . .
Ni3 Ni 0.27957(2) 0.61339(4) 0.57960(2) 0.02375(12) Uani 1 1 d . . .
O1 O 0.44749(14) 0.18983(19) 0.46089(13) 0.0302(6) Uani 1 1 d . . .
O2 O 0.40777(19) 0.0254(2) 0.45125(17) 0.0481(9) Uani 1 1 d . . .
O3 O 0.39182(13) 0.48720(18) 0.43519(11) 0.0221(5) Uani 1 1 d . . .
O4 O 0.3268(2) 0.6189(2) 0.39798(14) 0.0450(8) Uani 1 1 d . . .
O5 O 0.52734(13) 0.37888(19) 0.41239(12) 0.0225(5) Uani 1 1 d . . .
O6 O 0.63253(14) 0.3280(2) 0.37176(12) 0.0284(6) Uani 1 1 d . . .
O7 O 0.32900(13) 0.48044(19) 0.55179(12) 0.0232(5) Uani 1 1 d . . .
O8 O 0.33078(14) 0.3314(2) 0.49948(13) 0.0288(6) Uani 1 1 d . . .
O9 O 0.25073(14) 0.5508(2) 0.65469(13) 0.0326(6) Uani 1 1 d . . .
O10 O 0.18279(19) 0.5365(3) 0.73297(16) 0.0568(10) Uani 1 1 d . . .
O11 O 0.22714(14) 0.7505(2) 0.57344(13) 0.0297(6) Uani 1 1 d . . .
O12 O 0.1667(2) 0.8672(3) 0.51832(18) 0.0546(10) Uani 1 1 d . . .
O13 O 0.48041(13) 0.40601(18) 0.51929(12) 0.0200(5) Uani 1 1 d . . .
O14 O 0.34770(14) 0.6682(2) 0.50655(13) 0.0244(5) Uani 1 1 d . . .
O15 O 0.4052(2) 0.8545(2) 0.52370(18) 0.0397(8) Uani 1 1 d . . .
N1 N 0.39273(17) 0.2980(2) 0.35974(15) 0.0261(7) Uani 1 1 d . . .
N2 N 0.16802(17) 0.5497(3) 0.55113(15) 0.0295(7) Uani 1 1 d . . .
N3 N 0.3536(3) 0.8607(5) 0.2473(3) 0.0801(18) Uani 1 1 d . . .
N4 N 0.4815(4) 0.2767(4) 0.6321(3) 0.090(2) Uani 1 1 d . . .
C1 C 0.3240(2) 0.2456(3) 0.37760(19) 0.0281(8) Uani 1 1 d . . .
C2 C 0.3278(2) 0.1599(3) 0.4167(2) 0.0303(9) Uani 1 1 d . . .
C3 C 0.2624(2) 0.1112(3) 0.4324(2) 0.0367(10) Uani 1 1 d . . .
C4 C 0.1938(2) 0.1477(4) 0.4137(2) 0.0440(12) Uani 1 1 d . . .
C5 C 0.1907(2) 0.2330(4) 0.3767(2) 0.0431(11) Uani 1 1 d . . .
C6 C 0.2554(2) 0.2815(4) 0.3575(2) 0.0358(10) Uani 1 1 d . . .
C7 C 0.3990(2) 0.1210(3) 0.4442(2) 0.0347(9) Uani 1 1 d . . .
C8 C 0.3808(2) 0.3836(3) 0.31650(19) 0.0318(9) Uani 1 1 d . . .
C9 C 0.3631(3) 0.4877(3) 0.3323(2) 0.0397(10) Uani 1 1 d . . .
C10 C 0.3474(4) 0.5594(4) 0.2871(3) 0.0659(19) Uani 1 1 d . . .
C11 C 0.3516(5) 0.5345(5) 0.2297(3) 0.075(2) Uani 1 1 d . . .
C12 C 0.3692(4) 0.4328(4) 0.2142(3) 0.0540(14) Uani 1 1 d . . .
C13 C 0.3831(3) 0.3593(4) 0.2577(2) 0.0403(11) Uani 1 1 d . . .
C14 C 0.3592(2) 0.5339(3) 0.39241(19) 0.0314(9) Uani 1 1 d . . .
C15 C 0.4469(2) 0.2223(3) 0.33643(19) 0.0285(8) Uani 1 1 d . . .
C16 C 0.5241(2) 0.2395(3) 0.34051(18) 0.0275(8) Uani 1 1 d . . .
C17 C 0.5709(3) 0.1718(3) 0.3101(2) 0.0384(10) Uani 1 1 d . . .
C18 C 0.5426(3) 0.0879(4) 0.2768(2) 0.0457(12) Uani 1 1 d . . .
C19 C 0.4670(3) 0.0710(3) 0.2744(2) 0.0423(11) Uani 1 1 d . . .
C20 C 0.4197(3) 0.1360(3) 0.3046(2) 0.0359(10) Uani 1 1 d . . .
C21 C 0.5644(2) 0.3214(3) 0.37705(17) 0.0251(8) Uani 1 1 d . . .
C22 C 0.1620(2) 0.4343(3) 0.5579(2) 0.0337(9) Uani 1 1 d . . .
C23 C 0.2220(2) 0.3654(3) 0.55010(19) 0.0308(9) Uani 1 1 d . . .
C24 C 0.2100(2) 0.2563(3) 0.5557(2) 0.0363(10) Uani 1 1 d . . .
C25 C 0.1406(3) 0.2169(4) 0.5693(2) 0.0473(12) Uani 1 1 d . . .
C26 C 0.0823(3) 0.2848(5) 0.5772(3) 0.0543(14) Uani 1 1 d . . .
C27 C 0.0925(2) 0.3911(4) 0.5711(2) 0.0454(12) Uani 1 1 d . . .
C28 C 0.29900(19) 0.3945(3) 0.53167(18) 0.0248(8) Uani 1 1 d . . .
C29 C 0.1143(2) 0.6041(4) 0.5874(2) 0.0356(10) Uani 1 1 d . . .
C30 C 0.1231(2) 0.6066(4) 0.6484(2) 0.0389(10) Uani 1 1 d . . .
C31 C 0.0695(3) 0.6540(5) 0.6816(3) 0.0521(14) Uani 1 1 d . . .
C32 C 0.0076(3) 0.7008(6) 0.6558(3) 0.0669(18) Uani 1 1 d . . .
C33 C -0.0010(3) 0.6968(6) 0.5959(3) 0.0635(17) Uani 1 1 d . . .
C34 C 0.0503(2) 0.6479(4) 0.5617(3) 0.0464(12) Uani 1 1 d . . .
C35 C 0.1901(2) 0.5615(4) 0.6808(2) 0.0380(10) Uani 1 1 d . . .
C36 C 0.1659(2) 0.5864(3) 0.49083(19) 0.0315(9) Uani 1 1 d . . .
C37 C 0.1739(2) 0.6949(4) 0.4801(2) 0.0359(9) Uani 1 1 d . . .
C38 C 0.1660(3) 0.7304(4) 0.4228(2) 0.0453(11) Uani 1 1 d . . .
C39 C 0.1522(3) 0.6614(5) 0.3769(3) 0.0588(15) Uani 1 1 d . . .
C40 C 0.1461(3) 0.5546(5) 0.3879(3) 0.0531(13) Uani 1 1 d . . .
C41 C 0.1518(2) 0.5175(4) 0.4446(2) 0.0406(11) Uani 1 1 d . . .
C42 C 0.1903(2) 0.7770(3) 0.5276(2) 0.0359(10) Uani 1 1 d . . .
C49 C 0.3411(3) 0.8634(4) 0.2960(3) 0.0508(13) Uani 1 1 d . . .
C50 C 0.3258(3) 0.8663(4) 0.3561(3) 0.0572(14) Uani 1 1 d . . .
H50A H 0.2770 0.8985 0.3617 0.127(13) Uiso 1 1 calc R . .
H50B H 0.3640 0.9079 0.3768 0.127(13) Uiso 1 1 calc R . .
H50C H 0.3258 0.7945 0.3718 0.127(13) Uiso 1 1 calc R . .
C51 C 0.4625(3) 0.1952(5) 0.6180(3) 0.0565(15) Uani 1 1 d . . .
C52 C 0.4390(4) 0.0919(5) 0.5988(3) 0.0712(18) Uani 1 1 d . . .
H52A H 0.4028 0.0988 0.5664 0.127(13) Uiso 1 1 calc R . .
H52B H 0.4162 0.0547 0.6313 0.127(13) Uiso 1 1 calc R . .
H52C H 0.4822 0.0522 0.5856 0.127(13) Uiso 1 1 calc R . .
N5 N 0.3202(3) 0.4695(3) 0.77025(19) 0.0539(11) Uani 1 1 d D . .
C43 C 0.3484(4) 0.3922(6) 0.7304(3) 0.0475(19) Uani 0.676(6) 1 d PD A 1
H43A H 0.3921 0.3581 0.7494 0.059(9) Uiso 0.676(6) 1 calc PR A 1
H43B H 0.3662 0.4296 0.6954 0.059(9) Uiso 0.676(6) 1 calc PR A 1
C44 C 0.2958(6) 0.3075(7) 0.7103(5) 0.070(3) Uani 0.676(6) 1 d PD A 1
H44A H 0.2862 0.2596 0.7428 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H44B H 0.3179 0.2681 0.6782 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H44C H 0.2490 0.3394 0.6966 0.090(11) Uiso 0.676(6) 1 calc PR A 1
C45 C 0.3014(5) 0.4253(7) 0.8302(4) 0.061(2) Uani 0.676(6) 1 d PD A 1
H45A H 0.2835 0.3522 0.8247 0.059(9) Uiso 0.676(6) 1 calc PR A 1
H45B H 0.3479 0.4219 0.8541 0.059(9) Uiso 0.676(6) 1 calc PR A 1
C46 C 0.2444(4) 0.4840(7) 0.8647(3) 0.052(2) Uani 0.676(6) 1 d PD A 1
H46A H 0.2619 0.5559 0.8722 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H46B H 0.2369 0.4480 0.9020 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H46C H 0.1973 0.4864 0.8424 0.090(11) Uiso 0.676(6) 1 calc PR A 1
C47 C 0.3553(4) 0.5722(5) 0.7737(4) 0.0472(19) Uani 0.676(6) 1 d PD A 1
H47A H 0.3291 0.6162 0.8024 0.059(9) Uiso 0.676(6) 1 calc PR A 1
H47B H 0.3510 0.6072 0.7351 0.059(9) Uiso 0.676(6) 1 calc PR A 1
C48 C 0.4370(5) 0.5638(8) 0.7918(5) 0.078(3) Uani 0.676(6) 1 d PD A 1
H48A H 0.4415 0.5276 0.8296 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H48B H 0.4584 0.6345 0.7953 0.090(11) Uiso 0.676(6) 1 calc PR A 1
H48C H 0.4637 0.5239 0.7622 0.090(11) Uiso 0.676(6) 1 calc PR A 1
C43A C 0.3846(9) 0.4469(13) 0.7246(7) 0.058(5) Uiso 0.324(6) 1 d PD A 2
H43C H 0.3668 0.3904 0.6980 0.059(9) Uiso 0.324(6) 1 calc PR A 2
H43D H 0.3904 0.5110 0.7006 0.059(9) Uiso 0.324(6) 1 calc PR A 2
C44A C 0.4579(8) 0.4170(16) 0.7466(9) 0.065(5) Uiso 0.324(6) 1 d PD A 2
H44D H 0.4716 0.4612 0.7802 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H44E H 0.4942 0.4264 0.7157 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H44F H 0.4572 0.3430 0.7587 0.090(11) Uiso 0.324(6) 1 calc PR A 2
C45A C 0.3079(9) 0.3689(9) 0.8010(7) 0.048(4) Uiso 0.324(6) 1 d PD A 2
H45C H 0.2733 0.3805 0.8334 0.059(9) Uiso 0.324(6) 1 calc PR A 2
H45D H 0.3557 0.3436 0.8180 0.059(9) Uiso 0.324(6) 1 calc PR A 2
C46A C 0.2754(10) 0.2840(11) 0.7593(9) 0.058(5) Uiso 0.324(6) 1 d PD A 2
H46d H 0.2317 0.3124 0.7383 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H46e H 0.2608 0.2223 0.7821 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H46f H 0.3130 0.2635 0.7312 0.090(11) Uiso 0.324(6) 1 calc PR A 2
C47A C 0.3540(9) 0.5509(11) 0.8109(7) 0.048(4) Uiso 0.324(6) 1 d PD A 2
H47C H 0.3978 0.5198 0.8313 0.059(9) Uiso 0.324(6) 1 calc PR A 2
H47D H 0.3173 0.5693 0.8409 0.059(9) Uiso 0.324(6) 1 calc PR A 2
C48A C 0.3778(9) 0.6511(10) 0.7801(8) 0.051(4) Uiso 0.324(6) 1 d PD A 2
H48D H 0.4298 0.6446 0.7687 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H48E H 0.3727 0.7111 0.8066 0.090(11) Uiso 0.324(6) 1 calc PR A 2
H48F H 0.3463 0.6621 0.7451 0.090(11) Uiso 0.324(6) 1 calc PR A 2
O16 O 0.2285(5) 0.4877(7) 0.9273(4) 0.037(2) Uiso 0.324(6) 1 d P A 2
H5N H 0.263(5) 0.491(6) 0.753(4) 0.12(3) Uiso 1 1 d . . .
H13O H 0.482(2) 0.369(4) 0.552(2) 0.030(12) Uiso 1 1 d . . .
H14O H 0.361(4) 0.739(6) 0.517(4) 0.11(3) Uiso 1 1 d . . .
H14P H 0.329(3) 0.665(4) 0.467(3) 0.056(16) Uiso 1 1 d . . .
H15O H 0.447(4) 0.850(5) 0.523(3) 0.054(18) Uiso 1 1 d . . .
H15P H 0.397(4) 0.895(5) 0.498(3) 0.06(2) Uiso 1 1 d . . .
H3 H 0.268(3) 0.063(4) 0.455(2) 0.034(14) Uiso 1 1 d . . .
H4 H 0.148(3) 0.111(4) 0.430(3) 0.059(16) Uiso 1 1 d . . .
H5 H 0.146(3) 0.249(4) 0.361(2) 0.039(13) Uiso 1 1 d . . .
H6 H 0.254(2) 0.330(3) 0.3293(19) 0.019(10) Uiso 1 1 d . . .
H10 H 0.339(4) 0.622(6) 0.297(3) 0.10(3) Uiso 1 1 d . . .
H11 H 0.352(4) 0.583(5) 0.195(3) 0.08(2) Uiso 1 1 d . . .
H12 H 0.379(3) 0.416(4) 0.177(2) 0.038(13) Uiso 1 1 d . . .
H13 H 0.398(3) 0.294(4) 0.247(2) 0.036(12) Uiso 1 1 d . . .
H17 H 0.626(3) 0.177(4) 0.313(2) 0.034(12) Uiso 1 1 d . . .
H18 H 0.573(3) 0.050(4) 0.258(3) 0.057(17) Uiso 1 1 d . . .
H19 H 0.443(4) 0.017(5) 0.251(3) 0.08(2) Uiso 1 1 d . . .
H20 H 0.371(3) 0.123(3) 0.302(2) 0.030(11) Uiso 1 1 d . . .
H24 H 0.256(3) 0.202(4) 0.548(2) 0.040(13) Uiso 1 1 d . . .
H25 H 0.137(3) 0.146(4) 0.575(2) 0.043(14) Uiso 1 1 d . . .
H26 H 0.037(3) 0.269(4) 0.591(3) 0.056(16) Uiso 1 1 d . . .
H27 H 0.055(3) 0.439(4) 0.578(2) 0.034(12) Uiso 1 1 d . . .
H31 H 0.074(3) 0.655(4) 0.723(2) 0.033(12) Uiso 1 1 d . . .
H32 H -0.022(3) 0.739(4) 0.677(3) 0.059(17) Uiso 1 1 d . . .
H33 H -0.037(4) 0.719(6) 0.581(3) 0.09(3) Uiso 1 1 d . . .
H34 H 0.043(2) 0.649(4) 0.516(2) 0.034(12) Uiso 1 1 d . . .
H38 H 0.172(2) 0.809(4) 0.415(2) 0.031(11) Uiso 1 1 d . . .
H39 H 0.150(3) 0.687(4) 0.340(3) 0.048(15) Uiso 1 1 d . . .
H40 H 0.135(3) 0.516(5) 0.357(3) 0.064(18) Uiso 1 1 d . . .
H41 H 0.150(4) 0.449(6) 0.456(3) 0.10(2) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0185(2) 0.0139(2) 0.0318(3) -0.00121(18) -0.00356(18) -0.00417(16)
Ni2 0.0153(2) 0.01418(19) 0.0282(3) -0.00052(17) -0.00137(17) -0.00357(15)
Ni3 0.0164(2) 0.0262(2) 0.0286(3) 0.00173(19) -0.00015(18) -0.00089(17)
O1 0.0272(13) 0.0154(11) 0.0476(18) 0.0002(11) -0.0077(12) -0.0042(10)
O2 0.057(2) 0.0125(13) 0.074(3) 0.0027(14) -0.0141(18) -0.0046(12)
O3 0.0205(11) 0.0174(11) 0.0281(14) -0.0025(10) -0.0048(10) -0.0010(9)
O4 0.067(2) 0.0285(15) 0.0385(19) -0.0016(13) -0.0170(16) 0.0198(15)
O5 0.0193(11) 0.0195(11) 0.0286(14) -0.0036(10) -0.0016(10) -0.0029(9)
O6 0.0234(13) 0.0294(14) 0.0322(16) -0.0020(11) -0.0015(11) -0.0022(10)
O7 0.0186(11) 0.0210(12) 0.0299(15) 0.0019(10) -0.0005(10) -0.0048(9)
O8 0.0229(12) 0.0240(13) 0.0392(17) -0.0008(12) -0.0012(11) -0.0094(10)
O9 0.0228(13) 0.0421(16) 0.0330(16) 0.0068(13) 0.0035(11) -0.0006(11)
O10 0.0387(18) 0.088(3) 0.044(2) 0.030(2) 0.0107(15) 0.0039(18)
O11 0.0249(13) 0.0301(14) 0.0340(16) -0.0015(12) -0.0006(11) 0.0056(11)
O12 0.054(2) 0.0380(18) 0.071(3) 0.0028(17) -0.0198(18) 0.0178(15)
O13 0.0185(11) 0.0133(11) 0.0282(15) 0.0021(10) -0.0020(10) -0.0022(9)
O14 0.0241(12) 0.0178(12) 0.0312(16) 0.0011(11) -0.0016(11) -0.0009(10)
O15 0.0329(17) 0.0205(14) 0.065(3) 0.0058(15) -0.0029(16) -0.0054(12)
N1 0.0255(15) 0.0174(14) 0.0349(19) -0.0049(13) -0.0079(13) -0.0008(11)
N2 0.0195(14) 0.0374(18) 0.0314(19) 0.0042(15) -0.0008(13) -0.0050(13)
N3 0.061(3) 0.117(5) 0.063(4) -0.020(3) 0.000(3) -0.040(3)
N4 0.134(6) 0.048(3) 0.088(5) 0.022(3) 0.006(4) -0.004(3)
C1 0.0246(17) 0.0200(17) 0.040(2) -0.0109(16) -0.0035(16) -0.0048(14)
C2 0.0294(19) 0.0191(17) 0.042(2) -0.0102(16) -0.0044(17) -0.0054(14)
C3 0.034(2) 0.026(2) 0.049(3) -0.009(2) -0.002(2) -0.0121(17)
C4 0.027(2) 0.049(3) 0.056(3) -0.019(2) 0.005(2) -0.0114(19)
C5 0.023(2) 0.059(3) 0.047(3) -0.015(2) -0.0074(19) 0.0052(19)
C6 0.032(2) 0.035(2) 0.041(3) -0.010(2) -0.0077(18) 0.0057(17)
C7 0.036(2) 0.0194(17) 0.048(3) -0.0008(17) -0.0031(19) -0.0034(15)
C8 0.032(2) 0.0268(19) 0.036(2) -0.0043(17) -0.0121(17) -0.0028(16)
C9 0.057(3) 0.026(2) 0.035(3) -0.0005(18) -0.015(2) 0.0022(19)
C10 0.128(6) 0.031(3) 0.038(3) -0.002(2) -0.026(3) 0.018(3)
C11 0.144(7) 0.043(3) 0.037(3) 0.004(2) -0.026(4) 0.016(3)
C12 0.080(4) 0.046(3) 0.035(3) -0.007(2) -0.014(3) 0.005(3)
C13 0.050(3) 0.031(2) 0.040(3) -0.0067(19) -0.013(2) -0.0004(19)
C14 0.039(2) 0.0231(18) 0.032(2) -0.0001(16) -0.0086(17) -0.0013(16)
C15 0.0286(19) 0.0209(17) 0.036(2) -0.0050(16) -0.0020(16) -0.0005(14)
C16 0.0268(18) 0.0233(17) 0.032(2) -0.0061(16) 0.0007(16) -0.0009(14)
C17 0.036(2) 0.034(2) 0.045(3) -0.0103(19) 0.0032(19) -0.0005(18)
C18 0.046(3) 0.038(2) 0.053(3) -0.021(2) 0.005(2) 0.001(2)
C19 0.050(3) 0.028(2) 0.049(3) -0.015(2) -0.001(2) -0.0031(19)
C20 0.038(2) 0.0250(19) 0.045(3) -0.0082(18) -0.0073(19) -0.0059(16)
C21 0.0217(17) 0.0271(18) 0.027(2) -0.0021(15) 0.0012(14) -0.0032(14)
C22 0.0248(18) 0.037(2) 0.039(3) 0.0076(18) -0.0028(17) -0.0111(16)
C23 0.0239(18) 0.036(2) 0.033(2) 0.0054(17) -0.0001(16) -0.0110(15)
C24 0.035(2) 0.036(2) 0.038(3) 0.0076(19) -0.0001(18) -0.0155(18)
C25 0.043(3) 0.044(3) 0.055(3) 0.012(2) -0.001(2) -0.025(2)
C26 0.029(2) 0.065(3) 0.068(4) 0.016(3) 0.004(2) -0.025(2)
C27 0.022(2) 0.054(3) 0.060(3) 0.012(2) 0.002(2) -0.010(2)
C28 0.0186(16) 0.0218(17) 0.034(2) 0.0018(15) 0.0038(15) -0.0109(13)
C29 0.0164(17) 0.048(2) 0.042(3) 0.006(2) 0.0017(16) -0.0018(16)
C30 0.0185(18) 0.053(3) 0.046(3) 0.007(2) 0.0072(17) -0.0023(17)
C31 0.029(2) 0.087(4) 0.040(3) 0.011(3) 0.008(2) 0.000(2)
C32 0.028(2) 0.106(5) 0.068(4) -0.002(4) 0.011(3) 0.018(3)
C33 0.026(2) 0.104(5) 0.060(4) 0.006(3) -0.002(2) 0.010(3)
C34 0.0195(19) 0.066(3) 0.053(3) 0.001(3) -0.0022(19) -0.0001(19)
C35 0.030(2) 0.045(2) 0.039(3) 0.011(2) 0.0070(18) -0.0053(18)
C36 0.0194(17) 0.042(2) 0.033(2) 0.0046(18) -0.0055(16) -0.0026(15)
C37 0.0272(19) 0.040(2) 0.040(3) 0.0031(19) -0.0061(18) 0.0037(17)
C38 0.043(3) 0.045(3) 0.047(3) 0.013(2) -0.011(2) -0.001(2)
C39 0.069(4) 0.066(4) 0.040(3) 0.017(3) -0.025(3) -0.006(3)
C40 0.062(3) 0.058(3) 0.038(3) -0.002(3) -0.020(3) -0.006(3)
C41 0.033(2) 0.043(3) 0.046(3) 0.003(2) -0.009(2) -0.0074(19)
C42 0.028(2) 0.035(2) 0.044(3) 0.0039(19) 0.0001(18) 0.0076(16)
C49 0.046(3) 0.056(3) 0.051(4) -0.009(3) 0.002(2) -0.024(2)
C50 0.073(4) 0.038(3) 0.061(4) -0.005(2) 0.009(3) -0.011(2)
C51 0.050(3) 0.048(3) 0.072(4) 0.025(3) 0.014(3) 0.009(2)
C52 0.066(4) 0.060(4) 0.088(5) 0.015(3) 0.008(3) -0.013(3)
N5 0.066(3) 0.047(2) 0.047(3) 0.015(2) -0.013(2) -0.006(2)
C43 0.027(3) 0.053(4) 0.062(5) 0.016(4) 0.000(3) -0.001(3)
C44 0.069(6) 0.047(5) 0.091(8) 0.008(5) -0.020(5) -0.006(4)
C45 0.055(5) 0.072(6) 0.056(6) 0.024(5) -0.001(4) 0.018(4)
C46 0.052(4) 0.060(5) 0.044(5) 0.020(4) 0.004(3) -0.004(4)
C47 0.035(4) 0.052(4) 0.053(5) 0.010(4) -0.004(3) -0.008(3)
C48 0.055(5) 0.082(7) 0.095(8) -0.012(6) -0.018(5) -0.006(5)

_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 O3 1.974(2) . ?
Ni1 O1 1.987(3) . ?
Ni1 O13 2.014(3) . ?
Ni1 O5 2.051(2) . ?
Ni1 O8 2.114(3) . ?
Ni1 N1 2.199(3) . ?
Ni1 Ni2 2.9867(6) . ?
Ni2 O13 2.022(2) 3_666 ?
Ni2 O13 2.032(2) . ?
Ni2 O3 2.052(3) . ?
Ni2 O7 2.072(2) . ?
Ni2 O5 2.087(3) 3_666 ?
Ni2 O14 2.093(3) . ?
Ni3 O9 1.972(3) . ?
Ni3 O11 1.985(3) . ?
Ni3 O7 2.018(3) . ?
Ni3 O6 2.053(3) 3_666 ?
Ni3 O14 2.206(3) . ?
Ni3 N2 2.247(3) . ?
O1 C7 1.287(5) . ?
O2 C7 1.235(5) . ?
O3 C14 1.276(5) . ?
O4 C14 1.234(5) . ?
O5 C21 1.286(4) . ?
O5 Ni2 2.087(3) 3_666 ?
O6 C21 1.237(4) . ?
O6 Ni3 2.053(3) 3_666 ?
O7 C28 1.298(4) . ?
O8 C28 1.237(5) . ?
O9 C35 1.263(5) . ?
O10 C35 1.243(6) . ?
O11 C42 1.272(5) . ?
O12 C42 1.238(5) . ?
O13 Ni2 2.022(2) 3_666 ?
O13 H13O 0.88(5) . ?
O14 H14O 0.96(8) . ?
O14 H14P 0.95(6) . ?
O15 H15O 0.76(6) . ?
O15 H15P 0.80(7) . ?
N1 C1 1.470(5) . ?
N1 C15 1.477(5) . ?
N1 C8 1.482(5) . ?
N2 C36 1.455(5) . ?
N2 C29 1.461(5) . ?
N2 C22 1.479(5) . ?
N3 C49 1.140(7) . ?
N4 C51 1.137(8) . ?
C1 C6 1.386(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.383(6) . ?
C2 C7 1.498(6) . ?
C3 C4 1.378(7) . ?
C3 H3 0.80(5) . ?
C4 C5 1.376(8) . ?
C4 H4 1.02(6) . ?
C5 C6 1.395(7) . ?
C5 H5 0.89(5) . ?
C6 H6 0.90(4) . ?
C8 C13 1.381(7) . ?
C8 C9 1.409(6) . ?
C9 C10 1.401(7) . ?
C9 C14 1.499(6) . ?
C10 C11 1.355(8) . ?
C10 H10 0.83(8) . ?
C11 C12 1.379(8) . ?
C11 H11 1.00(7) . ?
C12 C13 1.382(7) . ?
C12 H12 0.90(5) . ?
C13 H13 0.91(5) . ?
C15 C20 1.398(5) . ?
C15 C16 1.408(5) . ?
C16 C17 1.398(6) . ?
C16 C21 1.510(5) . ?
C17 C18 1.399(6) . ?
C17 H17 1.00(5) . ?
C18 C19 1.377(7) . ?
C18 H18 0.85(6) . ?
C19 C20 1.382(6) . ?
C19 H19 0.97(7) . ?
C20 H20 0.90(5) . ?
C22 C23 1.404(6) . ?
C22 C27 1.405(5) . ?
C23 C24 1.409(6) . ?
C23 C28 1.504(5) . ?
C24 C25 1.387(6) . ?
C24 H24 1.09(5) . ?
C25 C26 1.373(8) . ?
C25 H25 0.91(5) . ?
C26 C27 1.370(7) . ?
C26 H26 0.89(6) . ?
C27 H27 0.92(5) . ?
C29 C34 1.397(6) . ?
C29 C30 1.401(7) . ?
C30 C31 1.380(7) . ?
C30 C35 1.513(6) . ?
C31 C32 1.382(8) . ?
C31 H31 0.94(5) . ?
C32 C33 1.377(9) . ?
C32 H32 0.87(6) . ?
C33 C34 1.372(8) . ?
C33 H33 0.77(8) . ?
C34 H34 1.06(5) . ?
C36 C41 1.392(7) . ?
C36 C37 1.409(6) . ?
C37 C38 1.389(7) . ?
C37 C42 1.531(7) . ?
C38 C39 1.386(8) . ?
C38 H38 1.02(5) . ?
C39 C40 1.385(8) . ?
C39 H39 0.90(6) . ?
C40 C41 1.380(8) . ?
C40 H40 0.87(6) . ?
C41 H41 0.90(7) . ?
C49 C50 1.409(8) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.443(9) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N5 C43 1.440(8) . ?
N5 C47 1.452(7) . ?
N5 C45A 1.478(11) . ?
N5 C47A 1.509(11) . ?
N5 C45 1.526(8) . ?
N5 C43A 1.603(11) . ?
N5 H5N 1.13(9) . ?
C43 C44 1.498(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.506(11) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.522(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C43A C44A 1.45(2) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?
C45A C46A 1.54(2) . ?
C45A H45C 0.9900 . ?
C45A H45D 0.9900 . ?
C46A H46d 0.9800 . ?
C46A H46e 0.9800 . ?
C46A H46f 0.9800 . ?
C47A C48A 1.52(2) . ?
C47A H47C 0.9900 . ?
C47A H47D 0.9900 . ?
C48A H48D 0.9800 . ?
C48A H48E 0.9800 . ?
C48A H48F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 O1 171.10(10) . . ?
O3 Ni1 O13 84.30(10) . . ?
O1 Ni1 O13 101.82(11) . . ?
O3 Ni1 O5 90.45(10) . . ?
O1 Ni1 O5 96.90(11) . . ?
O13 Ni1 O5 80.49(10) . . ?
O3 Ni1 O8 83.05(10) . . ?
O1 Ni1 O8 90.60(11) . . ?
O13 Ni1 O8 88.45(10) . . ?
O5 Ni1 O8 167.70(10) . . ?
O3 Ni1 N1 90.14(11) . . ?
O1 Ni1 N1 85.54(12) . . ?
O13 Ni1 N1 164.30(11) . . ?
O5 Ni1 N1 84.89(11) . . ?
O8 Ni1 N1 105.48(11) . . ?
O13 Ni2 O13 81.53(10) 3_666 . ?
O13 Ni2 O3 88.63(10) 3_666 . ?
O13 Ni2 O3 81.88(10) . . ?
O13 Ni2 O7 175.14(10) 3_666 . ?
O13 Ni2 O7 93.64(10) . . ?
O3 Ni2 O7 90.15(10) . . ?
O13 Ni2 O5 79.45(10) 3_666 3_666 ?
O13 Ni2 O5 99.89(10) . 3_666 ?
O3 Ni2 O5 167.50(10) . 3_666 ?
O7 Ni2 O5 102.04(10) . 3_666 ?
O13 Ni2 O14 106.57(10) 3_666 . ?
O13 Ni2 O14 168.68(10) . . ?
O3 Ni2 O14 90.31(11) . . ?
O7 Ni2 O14 78.13(10) . . ?
O5 Ni2 O14 89.51(11) 3_666 . ?
O9 Ni3 O11 106.37(12) . . ?
O9 Ni3 O7 93.61(11) . . ?
O11 Ni3 O7 157.58(12) . . ?
O9 Ni3 O6 83.63(12) . 3_666 ?
O11 Ni3 O6 94.54(11) . 3_666 ?
O7 Ni3 O6 97.73(10) . 3_666 ?
O9 Ni3 O14 161.38(11) . . ?
O11 Ni3 O14 86.59(11) . . ?
O7 Ni3 O14 76.68(10) . . ?
O6 Ni3 O14 82.03(11) 3_666 . ?
O9 Ni3 N2 81.73(12) . . ?
O11 Ni3 N2 82.86(12) . . ?
O7 Ni3 N2 90.24(11) . . ?
O6 Ni3 N2 163.74(12) 3_666 . ?
O14 Ni3 N2 113.72(12) . . ?
C7 O1 Ni1 120.3(3) . . ?
C14 O3 Ni1 134.5(2) . . ?
C14 O3 Ni2 129.7(2) . . ?
Ni1 O3 Ni2 95.74(11) . . ?
C21 O5 Ni1 126.8(2) . . ?
C21 O5 Ni2 122.9(2) . 3_666 ?
Ni1 O5 Ni2 98.14(11) . 3_666 ?
C21 O6 Ni3 136.4(3) . 3_666 ?
C28 O7 Ni3 129.3(2) . . ?
C28 O7 Ni2 121.9(2) . . ?
Ni3 O7 Ni2 99.73(10) . . ?
C28 O8 Ni1 132.8(2) . . ?
C35 O9 Ni3 128.0(3) . . ?
C42 O11 Ni3 121.9(3) . . ?
Ni1 O13 Ni2 101.54(12) . 3_666 ?
Ni1 O13 Ni2 95.15(11) . . ?
Ni2 O13 Ni2 98.47(10) 3_666 . ?
Ni1 O13 H13O 118(3) . . ?
Ni2 O13 H13O 119(3) 3_666 . ?
Ni2 O13 H13O 120(3) . . ?
Ni2 O14 Ni3 93.30(10) . . ?
Ni2 O14 H14O 122(5) . . ?
Ni3 O14 H14O 104(5) . . ?
Ni2 O14 H14P 106(3) . . ?
Ni3 O14 H14P 120(3) . . ?
H14O O14 H14P 111(6) . . ?
H15O O15 H15P 102(6) . . ?
C1 N1 C15 111.7(3) . . ?
C1 N1 C8 114.0(3) . . ?
C15 N1 C8 108.9(3) . . ?
C1 N1 Ni1 94.7(2) . . ?
C15 N1 Ni1 109.0(2) . . ?
C8 N1 Ni1 117.8(2) . . ?
C36 N2 C29 112.5(3) . . ?
C36 N2 C22 114.7(3) . . ?
C29 N2 C22 111.0(3) . . ?
C36 N2 Ni3 99.4(2) . . ?
C29 N2 Ni3 105.3(2) . . ?
C22 N2 Ni3 113.2(2) . . ?
C6 C1 C2 119.6(4) . . ?
C6 C1 N1 120.5(4) . . ?
C2 C1 N1 119.8(3) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C7 117.9(4) . . ?
C1 C2 C7 123.3(3) . . ?
C4 C3 C2 122.1(5) . . ?
C4 C3 H3 123(4) . . ?
C2 C3 H3 114(4) . . ?
C5 C4 C3 118.6(4) . . ?
C5 C4 H4 124(3) . . ?
C3 C4 H4 117(3) . . ?
C4 C5 C6 121.2(4) . . ?
C4 C5 H5 116(3) . . ?
C6 C5 H5 122(3) . . ?
C1 C6 C5 119.6(5) . . ?
C1 C6 H6 119(3) . . ?
C5 C6 H6 121(3) . . ?
O2 C7 O1 123.1(4) . . ?
O2 C7 C2 119.0(4) . . ?
O1 C7 C2 117.9(3) . . ?
C13 C8 C9 118.0(4) . . ?
C13 C8 N1 118.6(4) . . ?
C9 C8 N1 123.2(4) . . ?
C10 C9 C8 117.7(4) . . ?
C10 C9 C14 114.0(4) . . ?
C8 C9 C14 128.2(4) . . ?
C11 C10 C9 123.2(5) . . ?
C11 C10 H10 119(6) . . ?
C9 C10 H10 117(6) . . ?
C10 C11 C12 119.1(5) . . ?
C10 C11 H11 128(4) . . ?
C12 C11 H11 112(4) . . ?
C11 C12 C13 119.2(5) . . ?
C11 C12 H12 121(3) . . ?
C13 C12 H12 119(3) . . ?
C8 C13 C12 122.7(4) . . ?
C8 C13 H13 119(3) . . ?
C12 C13 H13 118(3) . . ?
O4 C14 O3 122.5(4) . . ?
O4 C14 C9 118.0(4) . . ?
O3 C14 C9 119.4(4) . . ?
C20 C15 C16 119.3(4) . . ?
C20 C15 N1 118.2(3) . . ?
C16 C15 N1 122.2(3) . . ?
C17 C16 C15 118.4(4) . . ?
C17 C16 C21 114.4(3) . . ?
C15 C16 C21 127.2(3) . . ?
C16 C17 C18 121.6(4) . . ?
C16 C17 H17 122(3) . . ?
C18 C17 H17 116(3) . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 123(4) . . ?
C17 C18 H18 118(4) . . ?
C18 C19 C20 120.4(4) . . ?
C18 C19 H19 124(4) . . ?
C20 C19 H19 116(4) . . ?
C19 C20 C15 121.1(4) . . ?
C19 C20 H20 118(3) . . ?
C15 C20 H20 121(3) . . ?
O6 C21 O5 123.5(3) . . ?
O6 C21 C16 117.2(3) . . ?
O5 C21 C16 119.3(3) . . ?
C23 C22 C27 118.3(4) . . ?
C23 C22 N2 123.1(3) . . ?
C27 C22 N2 118.5(4) . . ?
C22 C23 C24 118.8(4) . . ?
C22 C23 C28 126.7(4) . . ?
C24 C23 C28 114.3(4) . . ?
C25 C24 C23 121.1(5) . . ?
C25 C24 H24 120(3) . . ?
C23 C24 H24 119(3) . . ?
C26 C25 C24 119.8(5) . . ?
C26 C25 H25 123(3) . . ?
C24 C25 H25 117(3) . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26 112(4) . . ?
C25 C26 H26 127(4) . . ?
C26 C27 C22 121.9(5) . . ?
C26 C27 H27 122(3) . . ?
C22 C27 H27 116(3) . . ?
O8 C28 O7 124.2(3) . . ?
O8 C28 C23 116.7(3) . . ?
O7 C28 C23 119.1(3) . . ?
C34 C29 C30 118.9(4) . . ?
C34 C29 N2 120.0(4) . . ?
C30 C29 N2 120.9(4) . . ?
C31 C30 C29 119.6(4) . . ?
C31 C30 C35 117.0(4) . . ?
C29 C30 C35 123.4(4) . . ?
C30 C31 C32 121.3(5) . . ?
C30 C31 H31 121(3) . . ?
C32 C31 H31 118(3) . . ?
C33 C32 C31 118.7(6) . . ?
C33 C32 H32 121(4) . . ?
C31 C32 H32 120(4) . . ?
C34 C33 C32 121.5(5) . . ?
C34 C33 H33 119(6) . . ?
C32 C33 H33 119(6) . . ?
C33 C34 C29 119.9(5) . . ?
C33 C34 H34 120(2) . . ?
C29 C34 H34 120(2) . . ?
O10 C35 O9 122.5(4) . . ?
O10 C35 C30 117.8(4) . . ?
O9 C35 C30 119.7(4) . . ?
C41 C36 C37 120.1(4) . . ?
C41 C36 N2 121.2(4) . . ?
C37 C36 N2 118.6(4) . . ?
C38 C37 C36 118.3(4) . . ?
C38 C37 C42 117.5(4) . . ?
C36 C37 C42 124.2(4) . . ?
C39 C38 C37 121.4(5) . . ?
C39 C38 H38 120(3) . . ?
C37 C38 H38 118(3) . . ?
C40 C39 C38 119.8(5) . . ?
C40 C39 H39 122(4) . . ?
C38 C39 H39 119(4) . . ?
C41 C40 C39 120.0(5) . . ?
C41 C40 H40 125(4) . . ?
C39 C40 H40 115(4) . . ?
C40 C41 C36 120.4(5) . . ?
C40 C41 H41 126(5) . . ?
C36 C41 H41 113(5) . . ?
O12 C42 O11 123.8(4) . . ?
O12 C42 C37 116.7(4) . . ?
O11 C42 C37 119.5(4) . . ?
N3 C49 C50 179.8(8) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N4 C51 C52 178.8(7) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C43 N5 C47 119.2(5) . . ?
C45A N5 C47A 111.3(8) . . ?
C43 N5 C45 113.9(5) . . ?
C47 N5 C45 112.8(5) . . ?
C45A N5 C43A 105.8(8) . . ?
C47A N5 C43A 103.7(8) . . ?
C43 N5 H5N 106(4) . . ?
C47 N5 H5N 101(4) . . ?
C45A N5 H5N 103(4) . . ?
C47A N5 H5N 114(4) . . ?
C45 N5 H5N 101(4) . . ?
C43A N5 H5N 119(4) . . ?
N5 C43 C44 117.1(6) . . ?
N5 C43 H43A 108.0 . . ?
C44 C43 H43A 108.0 . . ?
N5 C43 H43B 108.0 . . ?
C44 C43 H43B 108.0 . . ?
H43A C43 H43B 107.3 . . ?
C46 C45 N5 117.1(6) . . ?
C46 C45 H45A 108.0 . . ?
N5 C45 H45A 108.0 . . ?
C46 C45 H45B 108.0 . . ?
N5 C45 H45B 108.0 . . ?
H45A C45 H45B 107.3 . . ?
N5 C47 C48 111.6(6) . . ?
N5 C47 H47A 109.3 . . ?
C48 C47 H47A 109.3 . . ?
N5 C47 H47B 109.3 . . ?
C48 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C44A C43A N5 119.1(13) . . ?
C44A C43A H43C 107.5 . . ?
N5 C43A H43C 107.5 . . ?
C44A C43A H43D 107.5 . . ?
N5 C43A H43D 107.5 . . ?
H43C C43A H43D 107.0 . . ?
C43A C44A H44D 109.5 . . ?
C43A C44A H44E 109.5 . . ?
H44D C44A H44E 109.5 . . ?
C43A C44A H44F 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
N5 C45A C46A 111.7(12) . . ?
N5 C45A H45C 109.3 . . ?
C46A C45A H45C 109.3 . . ?
N5 C45A H45D 109.3 . . ?
C46A C45A H45D 109.3 . . ?
H45C C45A H45D 107.9 . . ?
C45A C46A H46d 109.5 . . ?
C45A C46A H46e 109.5 . . ?
H46d C46A H46e 109.5 . . ?
C45A C46A H46f 109.5 . . ?
H46d C46A H46f 109.5 . . ?
H46e C46A H46f 109.5 . . ?
N5 C47A C48A 113.8(12) . . ?
N5 C47A H47C 108.8 . . ?
C48A C47A H47C 108.8 . . ?
N5 C47A H47D 108.8 . . ?
C48A C47A H47D 108.8 . . ?
H47C C47A H47D 107.7 . . ?
C47A C48A H48D 109.5 . . ?
C47A C48A H48E 109.5 . . ?
H48D C48A H48E 109.5 . . ?
C47A C48A H48F 109.5 . . ?
H48D C48A H48F 109.5 . . ?
H48E C48A H48F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.101