Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Talal Mallah'
_publ_contact_author_address     
;
Universite Paris-Sud, Bat. 420
Laboratoire de Chimie Inorganique
UMR CNRS 8613
Orsay
91405
FRANCE
;

_publ_contact_author_email       MALLAH@ICMO.U-PSUD.FR

_publ_section_title              
;
Magnetic anisotropy of two trinuclear and tetranuclear
CrIIINiII cyanide-bridged complexes with spin ground states S = 4 and 5
;
loop_
_publ_author_name
'Talal Mallah'
'Anne-Laure Barra'
'Laure Catala'
'Gaelle Charron'
'Regis Guillot'
'Jean-Noel Rebilly'
;
E.Riviere
;
'Guillaume Rogez'

# Attachment 'Mallah_cr2ni2_cif.txt'

data_GuillotICMMO
_database_code_depnum_ccdc_archive 'CCDC 292375'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H60 N11 O8 Cl2 Cr1 Ni1'
_chemical_formula_weight         1052.65

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.471(3)
_cell_length_b                   14.195(3)
_cell_length_c                   15.050(3)
_cell_angle_alpha                109.18(3)
_cell_angle_beta                 94.03(3)
_cell_angle_gamma                91.87(3)
_cell_volume                     2505.9(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(1)
_cell_measurement_reflns_used    4455
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.35

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1102
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      160(1)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'X8 APEX II Bruker'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22418
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         26.89
_reflns_number_total             9652
_reflns_number_gt                7503
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
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.

The hydrogen atoms of methyl are placed on the residual peaks of the difference
Fourier map. The geometry obtained is a little distant from a carbon CH3
(angles being in the 89.7 to 117.2 degree range).
;

_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^)+(0.0675P)^2^+6.7927P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_number_reflns         7352
_refine_ls_number_parameters     629
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1489
_refine_ls_wR_factor_gt          0.1287
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.010

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 0.45288(5) 0.35422(4) 0.75700(4) 0.02100(18) Uani 1 1 d . . .
Cr1 Cr 0.75177(6) 0.35069(5) 1.02117(5) 0.0210(2) Uani 1 1 d . . .
Cl2 Cl 0.76788(13) 0.26873(12) 0.43969(11) 0.0537(4) Uani 1 1 d . . .
Cl1 Cl 0.83282(12) 0.87411(10) 0.84375(11) 0.0472(4) Uani 1 1 d . . .
C110 C 0.8230(4) 0.4773(4) 0.9985(3) 0.0218(10) Uani 1 1 d . . .
C100 C 0.3323(3) 0.5425(3) 0.8857(3) 0.0202(9) Uani 1 1 d . . .
N2 N 0.8951(3) 0.3412(3) 1.1068(3) 0.0258(9) Uani 1 1 d . . .
N1 N 0.8134(3) 0.2266(3) 0.9142(3) 0.0273(9) Uani 1 1 d . . .
N200 N 0.5260(3) 0.4566(3) 0.7034(3) 0.0254(9) Uani 1 1 d . . .
N3 N 0.6843(3) 0.2363(3) 1.0724(3) 0.0269(9) Uani 1 1 d . . .
N201 N 0.3390(3) 0.3504(3) 0.6471(2) 0.0248(9) Uani 1 1 d . . .
N110 N 0.8488(3) 0.5475(4) 0.9966(3) 0.0385(11) Uani 1 1 d . . .
N203 N 0.5128(3) 0.2190(3) 0.6766(2) 0.0242(9) Uani 1 1 d . . .
C213 C 0.2269(4) 0.2006(3) 0.8775(3) 0.0306(11) Uani 1 1 d . . .
H3 H 0.1749 0.2190 0.9204 0.037 Uiso 1 1 calc R . .
O8 O 0.8226(4) 0.3216(4) 0.3888(3) 0.0737(14) Uani 1 1 d . . .
C205 C 0.4578(4) 0.4865(3) 0.6453(3) 0.0241(10) Uani 1 1 d . . .
N120 N 0.5742(3) 0.3650(3) 0.8618(3) 0.0259(9) Uani 1 1 d . . .
C200 C 0.6184(4) 0.5120(3) 0.7385(3) 0.0313(11) Uani 1 1 d . . .
H106 H 0.6660 0.4918 0.7782 0.038 Uiso 1 1 calc R . .
O1 O 0.8764(6) 0.8017(5) 0.7738(6) 0.156(3) Uani 1 1 d . . .
C214 C 0.2430(4) 0.1001(3) 0.8334(3) 0.0309(11) Uani 1 1 d . . .
C211 C 0.2492(4) 0.2903(3) 0.6175(3) 0.0298(11) Uani 1 1 d . . .
H5 H 0.2387 0.2385 0.6416 0.036 Uiso 1 1 calc R . .
C216 C 0.3237(4) 0.0769(3) 0.7715(3) 0.0303(11) Uani 1 1 d . . .
H1 H 0.3372 0.0106 0.7406 0.036 Uiso 1 1 calc R . .
N100 N 0.3796(3) 0.4767(3) 0.8432(3) 0.0248(8) Uani 1 1 d . . .
C201 C 0.6461(4) 0.5977(4) 0.7185(4) 0.0373(12) Uani 1 1 d . . .
H105 H 0.7112 0.6334 0.7442 0.045 Uiso 1 1 calc R . .
C207 C 0.2787(4) 0.4403(4) 0.5456(3) 0.0327(12) Uani 1 1 d . . .
H4 H 0.2904 0.4926 0.5225 0.039 Uiso 1 1 calc R . .
C202 C 0.5766(4) 0.6300(3) 0.6601(4) 0.0350(12) Uani 1 1 d . . .
N202 N 0.3648(3) 0.2506(3) 0.7978(2) 0.0244(9) Uani 1 1 d . . .
C11 C 0.8218(5) 0.2316(4) 0.8138(3) 0.0335(12) Uani 1 1 d . . .
C31 C 0.5662(4) 0.2376(4) 1.0940(4) 0.0338(12) Uani 1 1 d . . .
C6 C 0.7295(4) 0.1452(3) 0.9071(3) 0.0334(12) Uani 1 1 d . . .
H30A H 0.7530 0.0818 0.8674 0.040 Uiso 1 1 calc R . .
H30B H 0.6628 0.1581 0.8770 0.040 Uiso 1 1 calc R . .
C217 C 0.3841(4) 0.1534(3) 0.7561(3) 0.0238(10) Uani 1 1 d . . .
C4 C 0.7514(4) 0.2575(4) 1.1653(3) 0.0301(12) Uani 1 1 d . . .
H32A H 0.7289 0.3185 1.2102 0.036 Uiso 1 1 calc R . .
H32B H 0.7374 0.2036 1.1899 0.036 Uiso 1 1 calc R . .
C5 C 0.7082(4) 0.1372(3) 1.0020(3) 0.0337(12) Uani 1 1 d . . .
H33A H 0.6476 0.0897 0.9939 0.040 Uiso 1 1 calc R . .
H33B H 0.7707 0.1118 1.0269 0.040 Uiso 1 1 calc R . .
C208 C 0.1846(4) 0.3786(4) 0.5147(3) 0.0364(12) Uani 1 1 d . . .
C218 C 0.4736(4) 0.1359(3) 0.6927(3) 0.0244(10) Uani 1 1 d . . .
C219 C 0.5152(4) 0.0436(3) 0.6529(3) 0.0307(11) Uani 1 1 d . . .
H36 H 0.4875 -0.0118 0.6657 0.037 Uiso 1 1 calc R . .
C220 C 0.5987(4) 0.0331(3) 0.5936(3) 0.0305(11) Uani 1 1 d . . .
C1 C 0.9209(4) 0.2058(4) 0.9537(3) 0.0337(12) Uani 1 1 d . . .
H38A H 0.9690 0.1862 0.9036 0.040 Uiso 1 1 calc R . .
H38B H 0.9117 0.1506 0.9776 0.040 Uiso 1 1 calc R . .
C2 C 0.9709(4) 0.2963(3) 1.0322(3) 0.0293(11) Uani 1 1 d . . .
H39A H 1.0345 0.2773 1.0616 0.035 Uiso 1 1 calc R . .
H39B H 0.9936 0.3465 1.0055 0.035 Uiso 1 1 calc R . .
O5 O 0.6970(5) 0.3350(4) 0.4977(4) 0.0945(19) Uani 1 1 d . . .
C22 C 1.0669(4) 0.4273(4) 1.2092(4) 0.0382(13) Uani 1 1 d . . .
H41A H 1.1071 0.3977 1.1558 0.057 Uiso 1 1 calc R . .
H41B H 1.0660 0.3849 1.2475 0.057 Uiso 1 1 calc R . .
H41C H 1.1000 0.4916 1.2459 0.057 Uiso 1 1 calc R . .
C120 C 0.6339(4) 0.3573(3) 0.9201(3) 0.0202(9) Uani 1 1 d . . .
C3 C 0.8703(4) 0.2687(4) 1.1577(3) 0.0320(12) Uani 1 1 d . . .
H43A H 0.8962 0.2041 1.1239 0.038 Uiso 1 1 calc R . .
H43B H 0.9075 0.2922 1.2205 0.038 Uiso 1 1 calc R . .
C212 C 0.2873(4) 0.2724(3) 0.8581(3) 0.0294(11) Uani 1 1 d . . .
H44 H 0.2744 0.3392 0.8878 0.035 Uiso 1 1 calc R . .
C222 C 0.6353(4) 0.1176(3) 0.5761(3) 0.0321(11) Uani 1 1 d . . .
H45 H 0.6895 0.1137 0.5358 0.038 Uiso 1 1 calc R . .
C210 C 0.1716(4) 0.3024(4) 0.5523(3) 0.0365(12) Uani 1 1 d . . .
H46 H 0.1104 0.2591 0.5336 0.044 Uiso 1 1 calc R . .
C13 C 0.9011(5) 0.3132(4) 0.8112(4) 0.0517(16) Uani 1 1 d . . .
H47A H 0.8838 0.3759 0.8552 0.078 Uiso 1 1 calc R . .
H47B H 0.8973 0.3175 0.7488 0.078 Uiso 1 1 calc R . .
H47C H 0.9726 0.2981 0.8281 0.078 Uiso 1 1 calc R . .
C223 C 0.5912(4) 0.2085(3) 0.6186(3) 0.0291(11) Uani 1 1 d . . .
H48 H 0.6175 0.2645 0.6061 0.035 Uiso 1 1 calc R . .
C204 C 0.4811(4) 0.5717(3) 0.6229(3) 0.0319(12) Uani 1 1 d . . .
H49 H 0.4327 0.5903 0.5827 0.038 Uiso 1 1 calc R . .
C206 C 0.3553(4) 0.4247(3) 0.6104(3) 0.0256(10) Uani 1 1 d . . .
O4 O 0.9055(5) 0.9468(4) 0.9004(5) 0.125(3) Uani 1 1 d . . .
C21 C 0.9512(4) 0.4392(4) 1.1748(3) 0.0317(12) Uani 1 1 d . . .
C221 C 0.6488(4) -0.0663(3) 0.5528(4) 0.0379(13) Uani 1 1 d . . .
H53A H 0.6127 -0.1159 0.5725 0.057 Uiso 1 1 calc R . .
H53B H 0.7237 -0.0596 0.5749 0.057 Uiso 1 1 calc R . .
H53C H 0.6418 -0.0863 0.4851 0.057 Uiso 1 1 calc R . .
O7 O 0.8408(4) 0.2408(5) 0.5021(4) 0.1000(19) Uani 1 1 d . . .
C215 C 0.1751(5) 0.0196(4) 0.8512(4) 0.0489(15) Uani 1 1 d . . .
H55A H 0.1979 -0.0447 0.8152 0.073 Uiso 1 1 calc R . .
H55B H 0.1009 0.0248 0.8325 0.073 Uiso 1 1 calc R . .
H55C H 0.1831 0.0274 0.9171 0.073 Uiso 1 1 calc R . .
C12 C 0.8492(5) 0.1319(4) 0.7424(4) 0.0467(14) Uani 1 1 d . . .
H56A H 0.7983 0.0800 0.7430 0.070 Uiso 1 1 calc R . .
H56B H 0.9204 0.1161 0.7593 0.070 Uiso 1 1 calc R . .
H56C H 0.8461 0.1372 0.6804 0.070 Uiso 1 1 calc R . .
N300 N 0.8838(5) 0.9288(5) 0.3956(5) 0.086(2) Uani 1 1 d . . .
C23 C 0.8881(4) 0.4871(4) 1.2581(4) 0.0422(13) Uani 1 1 d . . .
H10A H 0.8159 0.4950 1.2361 0.063 Uiso 1 1 calc R . .
H10B H 0.9218 0.5514 1.2942 0.063 Uiso 1 1 calc R . .
H10C H 0.8864 0.4455 1.2971 0.063 Uiso 1 1 calc R . .
C203 C 0.6005(5) 0.7243(4) 0.6372(4) 0.0495(15) Uani 1 1 d . . .
H60A H 0.5427 0.7332 0.5958 0.074 Uiso 1 1 calc R . .
H60B H 0.6664 0.7189 0.6070 0.074 Uiso 1 1 calc R . .
H60C H 0.6077 0.7806 0.6945 0.074 Uiso 1 1 calc R . .
C209 C 0.1013(5) 0.3943(5) 0.4446(4) 0.0552(16) Uani 1 1 d . . .
H61A H 0.0430 0.3446 0.4321 0.083 Uiso 1 1 calc R . .
H61B H 0.1332 0.3887 0.3870 0.083 Uiso 1 1 calc R . .
H61C H 0.0745 0.4595 0.4700 0.083 Uiso 1 1 calc R . .
C300 C 0.9356(6) 0.9941(5) 0.3905(5) 0.0607(17) Uani 1 1 d . . .
C32 C 0.4882(5) 0.2184(5) 1.0076(4) 0.0541(16) Uani 1 1 d . . .
H63A H 0.5056 0.2647 0.9756 0.081 Uiso 1 1 calc R . .
H63B H 0.4162 0.2271 1.0263 0.081 Uiso 1 1 calc R . .
H63C H 0.4934 0.1514 0.9658 0.081 Uiso 1 1 calc R . .
C33 C 0.5365(5) 0.1637(4) 1.1452(4) 0.0467(14) Uani 1 1 d . . .
H64A H 0.5848 0.1761 1.2008 0.070 Uiso 1 1 calc R . .
H64B H 0.5421 0.0966 1.1039 0.070 Uiso 1 1 calc R . .
H64C H 0.4640 0.1725 1.1627 0.070 Uiso 1 1 calc R . .
O2 O 0.7454(7) 0.9100(4) 0.8046(7) 0.183(4) Uani 1 1 d . . .
O3 O 0.7872(7) 0.8226(9) 0.8937(5) 0.210(5) Uani 1 1 d . . .
C301 C 1.0035(8) 1.0765(6) 0.3834(7) 0.069(2) Uani 1 1 d . . .
O6 O 0.7087(6) 0.1847(4) 0.3761(4) 0.125(3) Uani 1 1 d . . .
H102 H 0.556(3) 0.307(3) 1.137(3) 0.017(11) Uiso 1 1 d . . .
H100 H 0.754(4) 0.243(3) 0.796(3) 0.009(11) Uiso 1 1 d . . .
H101 H 0.954(3) 0.480(3) 1.142(3) 0.017(11) Uiso 1 1 d . . .
H104 H 0.969(8) 1.129(7) 0.393(7) 0.12(4) Uiso 1 1 d . . .
H110 H 1.076(8) 1.080(6) 0.434(7) 0.13(3) Uiso 1 1 d . . .
H111 H 1.017(8) 1.079(7) 0.330(7) 0.13(4) 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 0.0245(4) 0.0165(3) 0.0221(3) 0.0063(2) 0.0020(2) 0.0030(2)
Cr1 0.0216(5) 0.0190(4) 0.0229(4) 0.0072(3) 0.0023(3) 0.0051(3)
Cl2 0.0572(11) 0.0608(10) 0.0613(10) 0.0404(8) 0.0202(7) 0.0195(7)
Cl1 0.0508(10) 0.0305(7) 0.0620(9) 0.0158(6) 0.0104(7) 0.0098(6)
C110 0.017(3) 0.024(3) 0.019(2) 0.0000(19) -0.0038(17) 0.010(2)
C100 0.020(3) 0.020(2) 0.021(2) 0.0090(18) -0.0021(18) 0.0022(18)
N2 0.024(3) 0.029(2) 0.028(2) 0.0151(17) 0.0011(16) 0.0029(16)
N1 0.030(3) 0.024(2) 0.029(2) 0.0091(16) 0.0047(17) 0.0082(16)
N200 0.022(3) 0.023(2) 0.031(2) 0.0085(16) 0.0028(16) 0.0014(16)
N3 0.028(3) 0.025(2) 0.030(2) 0.0117(17) 0.0043(17) 0.0022(16)
N201 0.028(3) 0.0202(19) 0.024(2) 0.0048(16) 0.0004(16) 0.0005(16)
N110 0.031(3) 0.053(3) 0.037(3) 0.020(2) 0.0103(19) 0.008(2)
N203 0.030(3) 0.0207(19) 0.0205(19) 0.0052(15) 0.0039(16) 0.0013(16)
C213 0.029(3) 0.031(3) 0.038(3) 0.016(2) 0.013(2) 0.007(2)
O8 0.076(4) 0.094(4) 0.068(3) 0.048(3) 0.021(2) -0.007(3)
C205 0.028(3) 0.022(2) 0.023(2) 0.0076(18) 0.0057(19) 0.0050(19)
N120 0.031(3) 0.0176(19) 0.029(2) 0.0058(16) 0.0065(18) 0.0051(16)
C200 0.023(3) 0.031(3) 0.040(3) 0.013(2) 0.000(2) 0.003(2)
O1 0.118(6) 0.101(5) 0.189(8) -0.036(5) 0.013(5) 0.051(4)
C214 0.025(3) 0.035(3) 0.039(3) 0.021(2) 0.004(2) 0.002(2)
C211 0.031(3) 0.026(3) 0.029(3) 0.006(2) 0.000(2) 0.001(2)
C216 0.033(3) 0.021(2) 0.039(3) 0.013(2) 0.003(2) 0.006(2)
N100 0.024(2) 0.025(2) 0.026(2) 0.0103(17) -0.0005(16) 0.0024(17)
C201 0.026(3) 0.030(3) 0.055(3) 0.014(2) 0.006(2) -0.005(2)
C207 0.037(4) 0.035(3) 0.028(3) 0.013(2) 0.000(2) 0.006(2)
C202 0.042(4) 0.026(3) 0.042(3) 0.016(2) 0.016(2) 0.005(2)
N202 0.027(3) 0.021(2) 0.025(2) 0.0070(16) 0.0043(16) 0.0047(15)
C11 0.036(4) 0.037(3) 0.028(3) 0.010(2) 0.006(2) 0.017(2)
C31 0.031(4) 0.035(3) 0.040(3) 0.018(2) 0.004(2) -0.001(2)
C6 0.041(3) 0.022(2) 0.035(3) 0.005(2) 0.002(2) 0.005(2)
C217 0.028(3) 0.021(2) 0.023(2) 0.0080(18) 0.0000(18) 0.0027(18)
C4 0.029(4) 0.032(3) 0.034(3) 0.018(2) 0.004(2) 0.004(2)
C5 0.038(3) 0.021(2) 0.042(3) 0.010(2) 0.005(2) 0.002(2)
C208 0.040(4) 0.042(3) 0.027(3) 0.011(2) 0.001(2) 0.011(2)
C218 0.030(3) 0.021(2) 0.022(2) 0.0075(18) 0.0004(19) 0.0004(18)
C219 0.037(3) 0.023(2) 0.035(3) 0.011(2) 0.008(2) 0.003(2)
C220 0.039(3) 0.022(2) 0.028(3) 0.004(2) 0.006(2) 0.005(2)
C1 0.029(3) 0.036(3) 0.038(3) 0.013(2) 0.008(2) 0.015(2)
C2 0.019(3) 0.040(3) 0.032(3) 0.015(2) 0.002(2) 0.008(2)
O5 0.115(5) 0.108(4) 0.111(4) 0.087(4) 0.070(3) 0.066(3)
C22 0.032(3) 0.049(3) 0.036(3) 0.019(2) -0.007(2) -0.001(2)
C120 0.022(3) 0.016(2) 0.022(2) 0.0061(18) 0.0032(19) 0.0049(17)
C3 0.035(4) 0.030(3) 0.038(3) 0.020(2) 0.001(2) 0.005(2)
C212 0.029(3) 0.027(3) 0.032(3) 0.009(2) 0.005(2) 0.005(2)
C222 0.036(3) 0.031(3) 0.029(3) 0.009(2) 0.013(2) 0.003(2)
C210 0.031(3) 0.036(3) 0.033(3) 0.001(2) -0.005(2) -0.004(2)
C13 0.074(5) 0.046(3) 0.037(3) 0.013(3) 0.020(3) -0.001(3)
C223 0.037(3) 0.028(3) 0.026(3) 0.013(2) 0.009(2) 0.001(2)
C204 0.038(3) 0.031(3) 0.032(3) 0.017(2) 0.004(2) 0.004(2)
C206 0.033(3) 0.022(2) 0.022(2) 0.0074(19) 0.0041(19) 0.0056(19)
O4 0.084(5) 0.074(4) 0.174(7) -0.012(4) -0.002(4) -0.033(3)
C21 0.036(4) 0.031(3) 0.030(3) 0.014(2) -0.004(2) 0.001(2)
C221 0.046(4) 0.025(3) 0.042(3) 0.008(2) 0.015(2) 0.012(2)
O7 0.086(4) 0.153(5) 0.094(4) 0.078(4) 0.022(3) 0.061(4)
C215 0.049(4) 0.039(3) 0.072(4) 0.033(3) 0.020(3) 0.004(3)
C12 0.053(4) 0.049(3) 0.035(3) 0.007(3) 0.012(3) 0.016(3)
N300 0.084(5) 0.091(5) 0.085(5) 0.039(4) -0.013(4) -0.033(4)
C23 0.038(4) 0.043(3) 0.037(3) 0.002(2) -0.005(2) 0.006(2)
C203 0.055(4) 0.039(3) 0.063(4) 0.026(3) 0.019(3) -0.002(3)
C209 0.052(4) 0.071(4) 0.042(3) 0.022(3) -0.016(3) 0.007(3)
C300 0.057(5) 0.060(4) 0.054(4) 0.005(3) 0.005(3) -0.004(3)
C32 0.031(4) 0.088(5) 0.056(4) 0.043(3) -0.004(3) -0.013(3)
C33 0.039(4) 0.058(4) 0.057(4) 0.036(3) 0.013(3) -0.003(3)
O2 0.204(8) 0.043(3) 0.253(10) 0.010(4) -0.124(7) 0.024(4)
O3 0.161(8) 0.355(14) 0.117(6) 0.102(8) -0.002(5) -0.136(9)
C301 0.073(6) 0.048(4) 0.079(6) 0.009(4) 0.012(5) 0.000(4)
O6 0.183(7) 0.086(4) 0.096(4) 0.026(4) -0.006(4) -0.064(4)

_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 N120 2.071(4) . ?
Ni1 N100 2.081(4) . ?
Ni1 N202 2.081(4) . ?
Ni1 N201 2.088(4) . ?
Ni1 N200 2.093(4) . ?
Ni1 N203 2.098(4) . ?
Cr1 C120 2.067(5) . ?
Cr1 C100 2.068(4) 2_667 ?
Cr1 C110 2.115(5) . ?
Cr1 N2 2.163(4) . ?
Cr1 N1 2.165(4) . ?
Cr1 N3 2.182(4) . ?
Cl2 O6 1.406(5) . ?
Cl2 O7 1.419(5) . ?
Cl2 O8 1.425(4) . ?
Cl2 O5 1.432(5) . ?
Cl1 O3 1.348(8) . ?
Cl1 O1 1.366(6) . ?
Cl1 O4 1.366(5) . ?
Cl1 O2 1.392(6) . ?
C110 N110 1.047(6) . ?
C100 N100 1.151(5) . ?
C100 Cr1 2.068(4) 2_667 ?
N2 C3 1.508(6) . ?
N2 C2 1.510(6) . ?
N2 C21 1.540(6) . ?
N1 C1 1.506(6) . ?
N1 C6 1.506(6) . ?
N1 C11 1.547(6) . ?
N200 C200 1.345(6) . ?
N200 C205 1.353(6) . ?
N3 C5 1.511(6) . ?
N3 C4 1.512(6) . ?
N3 C31 1.531(7) . ?
N201 C211 1.341(6) . ?
N201 C206 1.358(6) . ?
N203 C223 1.335(6) . ?
N203 C218 1.363(5) . ?
C213 C212 1.368(6) . ?
C213 C214 1.390(6) . ?
C205 C204 1.386(6) . ?
C205 C206 1.487(6) . ?
N120 C120 1.147(5) . ?
C200 C201 1.385(7) . ?
C214 C216 1.393(7) . ?
C214 C215 1.505(7) . ?
C211 C210 1.384(7) . ?
C216 C217 1.392(6) . ?
C201 C202 1.385(7) . ?
C207 C206 1.392(6) . ?
C207 C208 1.395(7) . ?
C202 C204 1.398(7) . ?
C202 C203 1.514(7) . ?
N202 C212 1.346(6) . ?
N202 C217 1.352(5) . ?
C11 C13 1.510(8) . ?
C11 C12 1.536(7) . ?
C31 C32 1.512(7) . ?
C31 C33 1.541(7) . ?
C6 C5 1.510(7) . ?
C217 C218 1.493(6) . ?
C4 C3 1.502(7) . ?
C208 C210 1.386(7) . ?
C208 C209 1.502(7) . ?
C218 C219 1.385(6) . ?
C219 C220 1.399(7) . ?
C220 C222 1.380(6) . ?
C220 C221 1.516(6) . ?
C1 C2 1.511(7) . ?
C22 C21 1.531(7) . ?
C222 C223 1.389(6) . ?
C21 C23 1.506(7) . ?
N300 C300 1.139(8) . ?
C300 C301 1.459(11) . ?

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
N120 Ni1 N100 92.05(14) . . ?
N120 Ni1 N202 90.72(15) . . ?
N100 Ni1 N202 94.29(14) . . ?
N120 Ni1 N201 175.28(15) . . ?
N100 Ni1 N201 88.31(14) . . ?
N202 Ni1 N201 93.95(15) . . ?
N120 Ni1 N200 96.26(15) . . ?
N100 Ni1 N200 85.45(14) . . ?
N202 Ni1 N200 173.02(15) . . ?
N201 Ni1 N200 79.08(15) . . ?
N120 Ni1 N203 88.43(14) . . ?
N100 Ni1 N203 172.35(14) . . ?
N202 Ni1 N203 78.07(14) . . ?
N201 Ni1 N203 91.84(14) . . ?
N200 Ni1 N203 102.09(14) . . ?
C120 Cr1 C100 84.98(16) . 2_667 ?
C120 Cr1 C110 84.33(16) . . ?
C100 Cr1 C110 82.64(16) 2_667 . ?
C120 Cr1 N2 169.40(15) . . ?
C100 Cr1 N2 103.27(15) 2_667 . ?
C110 Cr1 N2 90.07(15) . . ?
C120 Cr1 N1 88.03(15) . . ?
C100 Cr1 N1 170.35(16) 2_667 . ?
C110 Cr1 N1 103.30(15) . . ?
N2 Cr1 N1 84.50(14) . . ?
C120 Cr1 N3 102.93(16) . . ?
C100 Cr1 N3 90.12(15) 2_667 . ?
C110 Cr1 N3 169.31(15) . . ?
N2 Cr1 N3 83.93(14) . . ?
N1 Cr1 N3 84.97(14) . . ?
O6 Cl2 O7 111.1(4) . . ?
O6 Cl2 O8 109.8(3) . . ?
O7 Cl2 O8 111.3(3) . . ?
O6 Cl2 O5 110.1(4) . . ?
O7 Cl2 O5 106.3(3) . . ?
O8 Cl2 O5 108.1(3) . . ?
O3 Cl1 O1 103.3(7) . . ?
O3 Cl1 O4 110.7(5) . . ?
O1 Cl1 O4 114.5(4) . . ?
O3 Cl1 O2 103.7(7) . . ?
O1 Cl1 O2 109.1(5) . . ?
O4 Cl1 O2 114.3(4) . . ?
N110 C110 Cr1 169.2(4) . . ?
N100 C100 Cr1 170.5(4) . 2_667 ?
C3 N2 C2 109.6(3) . . ?
C3 N2 C21 111.3(4) . . ?
C2 N2 C21 107.2(4) . . ?
C3 N2 Cr1 108.5(3) . . ?
C2 N2 Cr1 101.4(3) . . ?
C21 N2 Cr1 118.2(3) . . ?
C1 N1 C6 111.1(4) . . ?
C1 N1 C11 110.2(4) . . ?
C6 N1 C11 107.6(4) . . ?
C1 N1 Cr1 107.6(3) . . ?
C6 N1 Cr1 100.3(3) . . ?
C11 N1 Cr1 119.5(3) . . ?
C200 N200 C205 117.8(4) . . ?
C200 N200 Ni1 126.6(3) . . ?
C205 N200 Ni1 113.1(3) . . ?
C5 N3 C4 111.5(4) . . ?
C5 N3 C31 111.2(4) . . ?
C4 N3 C31 106.9(4) . . ?
C5 N3 Cr1 106.0(3) . . ?
C4 N3 Cr1 101.3(3) . . ?
C31 N3 Cr1 119.6(3) . . ?
C211 N201 C206 118.7(4) . . ?
C211 N201 Ni1 127.1(3) . . ?
C206 N201 Ni1 113.9(3) . . ?
C223 N203 C218 117.8(4) . . ?
C223 N203 Ni1 126.3(3) . . ?
C218 N203 Ni1 115.6(3) . . ?
C212 C213 C214 120.2(4) . . ?
N200 C205 C204 121.6(4) . . ?
N200 C205 C206 115.9(4) . . ?
C204 C205 C206 122.4(4) . . ?
C120 N120 Ni1 169.2(4) . . ?
N200 C200 C201 123.2(5) . . ?
C213 C214 C216 117.4(4) . . ?
C213 C214 C215 121.2(4) . . ?
C216 C214 C215 121.4(4) . . ?
N201 C211 C210 122.5(5) . . ?
C217 C216 C214 119.8(4) . . ?
C100 N100 Ni1 174.7(4) . . ?
C200 C201 C202 119.7(5) . . ?
C206 C207 C208 121.1(5) . . ?
C201 C202 C204 117.0(4) . . ?
C201 C202 C203 122.5(5) . . ?
C204 C202 C203 120.5(5) . . ?
C212 N202 C217 118.2(4) . . ?
C212 N202 Ni1 125.2(3) . . ?
C217 N202 Ni1 116.5(3) . . ?
C13 C11 C12 109.2(5) . . ?
C13 C11 N1 113.1(4) . . ?
C12 C11 N1 113.0(4) . . ?
C32 C31 N3 113.3(4) . . ?
C32 C31 C33 108.9(4) . . ?
N3 C31 C33 113.1(4) . . ?
N1 C6 C5 112.9(4) . . ?
N202 C217 C216 121.7(4) . . ?
N202 C217 C218 114.8(4) . . ?
C216 C217 C218 123.5(4) . . ?
C3 C4 N3 113.5(4) . . ?
N3 C5 C6 112.4(4) . . ?
C210 C208 C207 116.6(4) . . ?
C210 C208 C209 121.6(5) . . ?
C207 C208 C209 121.8(5) . . ?
N203 C218 C219 121.6(4) . . ?
N203 C218 C217 114.5(4) . . ?
C219 C218 C217 123.8(4) . . ?
C218 C219 C220 120.4(4) . . ?
C222 C220 C219 117.1(4) . . ?
C222 C220 C221 121.6(4) . . ?
C219 C220 C221 121.2(4) . . ?
N1 C1 C2 111.5(4) . . ?
N2 C2 C1 113.0(4) . . ?
N120 C120 Cr1 174.8(4) . . ?
C4 C3 N2 111.2(4) . . ?
N202 C212 C213 122.7(4) . . ?
C220 C222 C223 120.1(4) . . ?
C211 C210 C208 120.4(5) . . ?
N203 C223 C222 123.0(4) . . ?
C205 C204 C202 120.7(4) . . ?
N201 C206 C207 120.7(4) . . ?
N201 C206 C205 115.4(4) . . ?
C207 C206 C205 123.9(4) . . ?
C23 C21 C22 109.8(4) . . ?
C23 C21 N2 112.6(4) . . ?
C22 C21 N2 113.4(4) . . ?
N300 C300 C301 178.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.890
_diffrn_reflns_theta_full        26.89
_diffrn_measured_fraction_theta_full 0.890
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.080

# Attachment 'Mallah_cr2ni_cif.txt'

data_210tm.cif
_database_code_depnum_ccdc_archive 'CCDC 292376'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H100 Cr2 N18 Ni O11'
_chemical_formula_weight         1244.15

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'
Cr Cr 0.3209 0.6236 '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   'C 2/c'

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

_cell_length_a                   17.623(4)
_cell_length_b                   9.6890(19)
_cell_length_c                   37.496(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.46(3)
_cell_angle_gamma                90.00
_cell_volume                     6296(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    15040
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'

_exptl_special_details           
;
Unit cell dimensions were determined from more than a thousand
reflections in all the angular range, taken from ten frames
with \f steps of 2\%.A 180\% range in \f was scanned during
data collection with 2\%\f steps and 10s exposure by frame.The
crystal to detector distance was 28mm.
;
_diffrn_ambient_temperature      123(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       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_diffrn_standards_number         none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15034
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_sigmaI/netI    0.1093
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.69
_reflns_number_total             5388
_reflns_number_gt                3393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'

_refine_special_details          
;
Structure solved by direct method and refined by full matrix
least-squares on F^2^ with anisotropic thermal parameters for all
non hydrogen atoms (except N and C atoms of the disordered
cyclam). Hydrogen atoms (except H atoms of water molecules
and disordered cyclam) were
introduced at calculated positions as riding atoms, with an
isotropic displacement parameter equal to 1.2 (CH, CH~2~) or
1.5 (CH~3~) times that of the parent atom.
The cyclam is found disordered on two positions with 0.5
occupancy factors.
;
_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^)+(0.1716P)^2^+21.4203P] where P=(Fo^2^+2Fc^2^)/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         5388
_refine_ls_number_parameters     360
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0935
_refine_ls_wR_factor_ref         0.2859
_refine_ls_wR_factor_gt          0.2455
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        25.69
_diffrn_measured_fraction_theta_full 0.900
_refine_diff_density_max         2.049
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.134

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
Ni Ni 0.2500 0.2500 0.0000 0.0249(4) Uani 1 2 d S . .
Cr Cr 0.12328(7) 0.21712(11) 0.11173(3) 0.0252(4) Uani 1 1 d . . .
O1 O -0.0975(6) 0.2539(8) 0.2293(3) 0.097(3) Uani 1 1 d . . .
O2 O -0.2027(5) 0.1661(8) 0.2034(3) 0.092(3) Uani 1 1 d . . .
O3 O -0.2024(4) 0.3455(8) 0.23739(19) 0.0669(19) Uani 1 1 d . . .
N1 N 0.2173(4) 0.1805(6) 0.15629(16) 0.0308(14) Uani 1 1 d . . .
N2 N 0.1122(3) 0.4087(6) 0.13898(17) 0.0284(14) Uani 1 1 d . . .
N3 N 0.0517(4) 0.1375(6) 0.14699(16) 0.0291(14) Uani 1 1 d . . .
N4 N 0.2303(4) 0.2820(6) 0.05372(17) 0.0306(14) Uani 1 1 d . . .
N5 N 0.1105(4) -0.0666(6) 0.06619(18) 0.0383(16) Uani 1 1 d . . .
N6 N -0.0015(5) 0.3068(7) 0.0427(2) 0.0510(19) Uani 1 1 d . . .
N7 N 0.2292(12) 0.039(2) 0.0099(6) 0.074(5) Uiso 0.50 1 d P . .
N8 N 0.3637(11) 0.2147(19) 0.0188(6) 0.071(5) Uiso 0.50 1 d P . .
N9 N 0.1615(7) 0.1082(11) -0.0073(3) 0.030(3) Uiso 0.50 1 d P . .
N10 N 0.3214(7) 0.0846(12) 0.0163(3) 0.028(3) Uiso 0.50 1 d P . .
N11 N -0.1686(5) 0.2535(7) 0.2226(2) 0.0459(19) Uani 1 1 d . . .
C1 C 0.2416(4) 0.3230(7) 0.1683(2) 0.0321(17) Uani 1 1 d . . .
H1A H 0.2697 0.3635 0.1509 0.039 Uiso 1 1 calc R . .
H1B H 0.2765 0.3179 0.1915 0.039 Uiso 1 1 calc R . .
C2 C 0.1744(4) 0.4165(7) 0.17220(19) 0.0287(16) Uani 1 1 d . . .
H2A H 0.1534 0.3891 0.1933 0.034 Uiso 1 1 calc R . .
H2B H 0.1924 0.5110 0.1758 0.034 Uiso 1 1 calc R . .
C3 C 0.0353(4) 0.3922(7) 0.1506(2) 0.0318(17) Uani 1 1 d . . .
H3A H -0.0055 0.3981 0.1295 0.038 Uiso 1 1 calc R . .
H3B H 0.0281 0.4668 0.1669 0.038 Uiso 1 1 calc R . .
C4 C 0.0296(5) 0.2547(7) 0.1696(2) 0.0320(17) Uani 1 1 d . . .
H4B H 0.0636 0.2555 0.1930 0.038 Uiso 1 1 calc R . .
H4C H -0.0228 0.2412 0.1735 0.038 Uiso 1 1 calc R . .
C5 C 0.1829(5) 0.1079(7) 0.1857(2) 0.0324(17) Uani 1 1 d . . .
H5A H 0.2184 0.0375 0.1970 0.039 Uiso 1 1 calc R . .
H5B H 0.1759 0.1742 0.2042 0.039 Uiso 1 1 calc R . .
C6 C 0.1058(5) 0.0416(7) 0.1704(2) 0.0361(19) Uani 1 1 d . . .
H6A H 0.1146 -0.0388 0.1563 0.043 Uiso 1 1 calc R . .
H6B H 0.0819 0.0103 0.1903 0.043 Uiso 1 1 calc R . .
C7 C 0.2888(5) 0.1046(8) 0.1486(2) 0.0389(19) Uani 1 1 d . . .
H7A H 0.3040 0.1485 0.1275 0.047 Uiso 1 1 calc R . .
C8 C 0.2724(6) -0.0494(9) 0.1392(3) 0.056(3) Uani 1 1 d . . .
H8A H 0.3186 -0.0925 0.1343 0.084 Uiso 1 1 calc R . .
H8B H 0.2326 -0.0563 0.1181 0.084 Uiso 1 1 calc R . .
H8C H 0.2560 -0.0950 0.1592 0.084 Uiso 1 1 calc R . .
C9 C 0.3571(5) 0.1149(9) 0.1798(2) 0.044(2) Uani 1 1 d . . .
H9A H 0.3681 0.2103 0.1855 0.067 Uiso 1 1 calc R . .
H9B H 0.4014 0.0722 0.1729 0.067 Uiso 1 1 calc R . .
H9C H 0.3449 0.0688 0.2007 0.067 Uiso 1 1 calc R . .
C10 C 0.1109(4) 0.5401(7) 0.11597(19) 0.0294(17) Uani 1 1 d . . .
H10A H 0.0795 0.5204 0.0922 0.035 Uiso 1 1 calc R . .
C11 C 0.0735(5) 0.6631(7) 0.1321(2) 0.043(2) Uani 1 1 d . . .
H11A H 0.0741 0.7424 0.1168 0.065 Uiso 1 1 calc R . .
H11B H 0.1020 0.6830 0.1559 0.065 Uiso 1 1 calc R . .
H11C H 0.0212 0.6405 0.1337 0.065 Uiso 1 1 calc R . .
C12 C 0.1907(5) 0.5819(7) 0.1098(2) 0.0356(19) Uani 1 1 d . . .
H12A H 0.2142 0.5056 0.0996 0.053 Uiso 1 1 calc R . .
H12B H 0.2220 0.6079 0.1325 0.053 Uiso 1 1 calc R . .
H12C H 0.1861 0.6587 0.0933 0.053 Uiso 1 1 calc R . .
C13 C -0.0207(5) 0.0556(8) 0.1292(2) 0.0376(19) Uani 1 1 d . . .
H13A H -0.0056 -0.0021 0.1102 0.045 Uiso 1 1 calc R . .
C14 C -0.0513(5) -0.0427(9) 0.1560(3) 0.049(2) Uani 1 1 d . . .
H14A H -0.0102 -0.1014 0.1676 0.074 Uiso 1 1 calc R . .
H14B H -0.0923 -0.0981 0.1431 0.074 Uiso 1 1 calc R . .
H14C H -0.0702 0.0108 0.1741 0.074 Uiso 1 1 calc R . .
C15 C -0.0867(5) 0.1465(9) 0.1111(3) 0.048(2) Uani 1 1 d . . .
H15A H -0.0685 0.2081 0.0945 0.071 Uiso 1 1 calc R . .
H15B H -0.1060 0.1991 0.1293 0.071 Uiso 1 1 calc R . .
H15C H -0.1272 0.0898 0.0982 0.071 Uiso 1 1 calc R . .
C16 C 0.1991(4) 0.2701(7) 0.07763(19) 0.0271(16) Uani 1 1 d . . .
C17 C 0.1170(5) 0.0306(7) 0.0842(2) 0.0319(17) Uani 1 1 d . . .
C18 C 0.0398(5) 0.2769(7) 0.0683(2) 0.0338(18) Uani 1 1 d . . .
C19 C 0.3095(15) -0.017(2) 0.0180(7) 0.066(6) Uiso 0.50 1 d P . .
C20 C 0.3692(10) 0.0756(17) 0.0419(4) 0.031(3) Uiso 0.50 1 d P . .
C21 C 0.4116(9) 0.3142(18) 0.0422(4) 0.027(3) Uiso 0.50 1 d P . .
C22 C 0.4041(16) 0.454(3) 0.0234(8) 0.087(7) Uiso 0.50 1 d P . .
C23 C 0.1747(12) -0.0182(17) -0.0149(5) 0.039(4) Uiso 0.50 1 d P . .
C24 C 0.2064(12) -0.0418(18) -0.0050(6) 0.042(4) Uiso 0.50 1 d P . .
C25 C 0.2668(13) -0.0358(18) 0.0221(5) 0.045(4) Uiso 0.50 1 d P . .
C26 C 0.3914(14) 0.128(3) 0.0479(7) 0.065(6) Uiso 0.50 1 d P . .
C27 C 0.4364(13) 0.229(2) 0.0401(6) 0.059(5) Uiso 0.50 1 d P . .
C28 C 0.3964(10) 0.378(2) 0.0393(5) 0.038(4) Uiso 0.50 1 d P . .
O1W O -0.1088(5) 0.3413(8) -0.0257(2) 0.025(2) Uani 0.50 1 d PU . .
O2W O 0.4407(4) 0.0262(7) 0.2684(2) 0.070(2) Uani 1 1 d U . .
O3W O 0.3616(9) 0.2490(15) 0.2752(5) 0.075(4) Uani 0.50 1 d PU . .
O4W O -0.1149(10) -0.0673(18) 0.2364(5) 0.087(5) Uani 0.50 1 d PU . .

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
Ni 0.0343(8) 0.0219(6) 0.0179(6) -0.0003(4) 0.0031(5) 0.0001(5)
Cr 0.0320(8) 0.0263(6) 0.0167(6) -0.0018(4) 0.0031(5) 0.0017(5)
O1 0.070(7) 0.084(6) 0.135(10) -0.023(5) 0.012(6) -0.015(4)
O2 0.113(7) 0.058(4) 0.087(6) -0.018(4) -0.031(5) -0.011(4)
O3 0.086(6) 0.077(5) 0.039(4) 0.005(3) 0.013(4) -0.010(4)
N1 0.041(4) 0.030(3) 0.023(3) 0.001(2) 0.010(3) 0.006(3)
N2 0.027(4) 0.028(3) 0.031(3) -0.002(2) 0.008(3) 0.000(2)
N3 0.035(4) 0.028(3) 0.025(3) -0.006(2) 0.007(3) -0.001(3)
N4 0.038(4) 0.030(3) 0.024(3) -0.002(2) 0.006(3) 0.004(3)
N5 0.055(5) 0.033(3) 0.030(4) -0.010(3) 0.015(3) -0.004(3)
N6 0.067(6) 0.045(4) 0.035(4) -0.002(3) -0.004(4) 0.010(4)
N11 0.057(6) 0.042(4) 0.039(4) 0.008(3) 0.010(4) -0.015(4)
C1 0.035(5) 0.038(4) 0.022(4) 0.000(3) 0.001(3) 0.000(3)
C2 0.031(5) 0.037(4) 0.016(3) 0.001(3) 0.000(3) 0.003(3)
C3 0.036(5) 0.031(4) 0.027(4) -0.001(3) 0.002(3) 0.002(3)
C4 0.040(5) 0.034(4) 0.024(4) -0.004(3) 0.009(3) -0.002(3)
C5 0.043(5) 0.034(4) 0.021(4) 0.003(3) 0.007(3) 0.003(3)
C6 0.057(6) 0.029(4) 0.022(4) -0.001(3) 0.006(4) 0.000(4)
C7 0.034(5) 0.053(5) 0.029(4) 0.010(3) 0.004(4) 0.020(4)
C8 0.058(6) 0.053(5) 0.049(6) -0.007(4) -0.011(5) 0.025(5)
C9 0.040(5) 0.045(4) 0.044(5) 0.007(4) -0.004(4) 0.008(4)
C10 0.040(5) 0.031(4) 0.016(3) -0.001(3) 0.001(3) 0.002(3)
C11 0.055(6) 0.030(4) 0.044(5) 0.000(3) 0.006(4) 0.008(4)
C12 0.051(5) 0.023(3) 0.033(4) -0.001(3) 0.009(4) -0.003(3)
C13 0.041(5) 0.041(4) 0.035(4) -0.013(3) 0.018(4) -0.011(4)
C14 0.051(6) 0.042(5) 0.057(6) -0.007(4) 0.015(5) -0.014(4)
C15 0.041(6) 0.051(5) 0.048(5) -0.009(4) -0.001(4) -0.010(4)
C16 0.032(4) 0.030(3) 0.017(4) -0.003(3) -0.001(3) 0.001(3)
C17 0.036(5) 0.030(4) 0.030(4) 0.006(3) 0.008(3) 0.003(3)
C18 0.043(5) 0.033(4) 0.024(4) -0.005(3) 0.001(4) 0.004(3)
O1W 0.034(4) 0.013(3) 0.021(4) -0.002(3) -0.015(3) 0.006(3)
O2W 0.086(4) 0.079(4) 0.044(3) 0.006(3) 0.005(3) -0.025(3)
O3W 0.062(6) 0.087(6) 0.075(6) -0.024(4) 0.009(4) 0.013(4)
O4W 0.093(6) 0.082(6) 0.086(6) 0.004(5) 0.014(5) 0.003(4)

_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
Ni N8 2.03(2) . ?
Ni N8 2.03(2) 7 ?
Ni N9 2.059(12) . ?
Ni N9 2.059(12) 7 ?
Ni N10 2.061(12) . ?
Ni N10 2.061(12) 7 ?
Ni N7 2.12(2) . ?
Ni N7 2.12(2) 7 ?
Ni N4 2.128(6) 7 ?
Ni N4 2.128(6) . ?
Cr C18 2.069(8) . ?
Cr C16 2.075(8) . ?
Cr C17 2.075(7) . ?
Cr N3 2.130(6) . ?
Cr N2 2.144(6) . ?
Cr N1 2.159(6) . ?
O1 N11 1.232(11) . ?
O2 N11 1.199(10) . ?
O3 N11 1.257(10) . ?
N1 C1 1.491(9) . ?
N1 C5 1.525(9) . ?
N1 C7 1.529(9) . ?
N2 C2 1.504(9) . ?
N2 C3 1.506(10) . ?
N2 C10 1.536(9) . ?
N3 C6 1.497(10) . ?
N3 C4 1.509(9) . ?
N3 C13 1.547(10) . ?
N4 C16 1.139(9) . ?
N5 C17 1.151(9) . ?
N6 C18 1.133(10) . ?
N7 C24 1.00(2) . ?
N7 C25 1.03(2) . ?
N7 C23 1.33(3) . ?
N7 N9 1.42(2) . ?
N7 C19 1.49(3) . ?
N7 N10 1.66(2) . ?
N8 C27 1.39(3) . ?
N8 C26 1.39(3) . ?
N8 N10 1.46(2) . ?
N8 C21 1.46(3) . ?
N8 C20 1.60(2) . ?
N8 N9 1.80(2) 7 ?
N8 C28 1.81(3) . ?
N9 C23 1.29(2) . ?
N9 C22 1.34(3) 7 ?
N9 C28 1.43(2) 7 ?
N9 C24 1.65(2) . ?
N9 N8 1.80(2) 7 ?
N9 C21 1.82(2) 7 ?
N10 C19 1.01(2) . ?
N10 C20 1.160(19) . ?
N10 C25 1.55(2) . ?
N10 C26 1.61(3) . ?
C1 C2 1.520(10) . ?
C3 C4 1.522(10) . ?
C5 C6 1.517(11) . ?
C7 C9 1.522(12) . ?
C7 C8 1.549(12) . ?
C10 C12 1.521(10) . ?
C10 C11 1.537(10) . ?
C13 C15 1.517(12) . ?
C13 C14 1.550(12) . ?
C19 C20 1.54(3) . ?
C21 C22 1.52(3) . ?
C22 N9 1.34(3) 7 ?
C22 C23 1.50(3) 7 ?
C23 C22 1.50(3) 7 ?
C24 C25 1.33(3) . ?
C26 C27 1.32(3) . ?
C27 C28 1.61(3) . ?
C28 N9 1.43(2) 7 ?

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
N8 Ni N8 179.999(1) . 7 ?
N8 Ni N9 127.6(6) . . ?
N8 Ni N9 52.4(6) 7 . ?
N8 Ni N9 52.4(6) . 7 ?
N8 Ni N9 127.6(6) 7 7 ?
N9 Ni N9 179.999(1) . 7 ?
N8 Ni N10 138.2(6) 7 . ?
N9 Ni N10 85.9(5) . . ?
N9 Ni N10 94.1(5) 7 . ?
N8 Ni N10 138.2(6) . 7 ?
N9 Ni N10 94.1(5) . 7 ?
N9 Ni N10 85.9(5) 7 7 ?
N10 Ni N10 179.999(1) . 7 ?
N8 Ni N7 88.2(8) . . ?
N8 Ni N7 91.8(8) 7 . ?
N9 Ni N7 140.4(6) 7 . ?
N10 Ni N7 133.3(6) 7 . ?
N8 Ni N7 91.8(8) . 7 ?
N8 Ni N7 88.2(8) 7 7 ?
N9 Ni N7 140.4(6) . 7 ?
N10 Ni N7 133.3(6) . 7 ?
N7 Ni N7 179.998(1) . 7 ?
N8 Ni N4 89.0(6) . 7 ?
N8 Ni N4 91.0(6) 7 7 ?
N9 Ni N4 91.5(4) . 7 ?
N9 Ni N4 88.5(4) 7 7 ?
N10 Ni N4 88.3(4) . 7 ?
N10 Ni N4 91.7(4) 7 7 ?
N7 Ni N4 95.1(6) . 7 ?
N7 Ni N4 84.9(6) 7 7 ?
N8 Ni N4 91.0(6) . . ?
N8 Ni N4 89.0(6) 7 . ?
N9 Ni N4 88.5(4) . . ?
N9 Ni N4 91.5(4) 7 . ?
N10 Ni N4 91.7(4) . . ?
N10 Ni N4 88.3(4) 7 . ?
N7 Ni N4 84.9(6) . . ?
N7 Ni N4 95.1(6) 7 . ?
N4 Ni N4 180.0 7 . ?
C18 Cr C16 83.7(3) . . ?
C18 Cr C17 83.5(3) . . ?
C16 Cr C17 83.7(3) . . ?
C18 Cr N3 100.0(3) . . ?
C16 Cr N3 172.8(2) . . ?
C17 Cr N3 90.6(3) . . ?
C18 Cr N2 91.1(3) . . ?
C16 Cr N2 101.8(2) . . ?
C17 Cr N2 171.9(3) . . ?
N3 Cr N2 84.4(2) . . ?
C18 Cr N1 172.5(3) . . ?
C16 Cr N1 91.6(3) . . ?
C17 Cr N1 101.9(3) . . ?
N3 Cr N1 85.3(2) . . ?
N2 Cr N1 84.1(2) . . ?
C1 N1 C5 109.8(5) . . ?
C1 N1 C7 107.5(6) . . ?
C5 N1 C7 111.3(5) . . ?
C1 N1 Cr 102.7(4) . . ?
C5 N1 Cr 106.6(4) . . ?
C7 N1 Cr 118.4(5) . . ?
C2 N2 C3 108.9(6) . . ?
C2 N2 C10 110.9(5) . . ?
C3 N2 C10 109.1(5) . . ?
C2 N2 Cr 108.8(4) . . ?
C3 N2 Cr 102.2(4) . . ?
C10 N2 Cr 116.3(4) . . ?
C6 N3 C4 109.9(6) . . ?
C6 N3 C13 108.8(6) . . ?
C4 N3 C13 110.5(6) . . ?
C6 N3 Cr 101.7(4) . . ?
C4 N3 Cr 108.5(4) . . ?
C13 N3 Cr 117.0(4) . . ?
C16 N4 Ni 156.2(6) . . ?
C24 N7 C25 82(2) . . ?
C25 N7 C23 110(2) . . ?
C24 N7 C19 96(2) . . ?
C23 N7 C19 122(2) . . ?
C26 N8 C21 81.0(18) . . ?
C27 N8 C20 79.1(15) . . ?
C21 N8 C20 105.0(16) . . ?
C27 N8 C28 58.7(12) . . ?
C26 N8 C28 98.9(18) . . ?
C20 N8 C28 121.8(15) . . ?
C23 N9 C22 69.5(16) . 7 ?
C23 N9 C28 91.9(14) . 7 ?
C22 N9 C24 89.7(15) 7 . ?
C28 N9 C24 112.9(13) 7 . ?
C23 N9 C21 111.4(13) . 7 ?
C24 N9 C21 132.1(12) . 7 ?
C19 N10 C20 90.1(19) . . ?
C20 N10 C25 101.7(14) . . ?
C19 N10 C26 110.5(19) . . ?
C25 N10 C26 120.5(14) . . ?
O2 N11 O1 120.3(10) . . ?
O2 N11 O3 122.7(10) . . ?
O1 N11 O3 117.0(8) . . ?
N1 C1 C2 113.3(6) . . ?
N2 C2 C1 110.7(6) . . ?
N2 C3 C4 111.5(6) . . ?
N3 C4 C3 110.5(6) . . ?
C6 C5 N1 111.6(6) . . ?
N3 C6 C5 112.9(6) . . ?
C9 C7 N1 112.8(7) . . ?
C9 C7 C8 109.1(6) . . ?
N1 C7 C8 112.4(7) . . ?
C12 C10 N2 112.8(6) . . ?
C12 C10 C11 109.1(6) . . ?
N2 C10 C11 112.6(6) . . ?
C15 C13 N3 113.6(6) . . ?
C15 C13 C14 108.6(7) . . ?
N3 C13 C14 113.1(7) . . ?
N4 C16 Cr 165.2(6) . . ?
N5 C17 Cr 173.9(7) . . ?
N6 C18 Cr 174.1(8) . . ?
C25 C19 N10 116(3) . . ?
C25 C19 C20 125(3) . . ?
N7 C19 C20 115.4(17) . . ?
N10 C19 C24 107.0(19) . . ?
C20 C19 C24 147.5(17) . . ?
C26 C20 N10 122(3) . . ?
C26 C20 C19 162(3) . . ?
C19 C20 N8 102.0(15) . . ?
N10 C20 C27 105.9(13) . . ?
C19 C20 C27 142.7(15) . . ?
C28 C21 C27 164(3) . . ?
C28 C21 N8 110(3) . . ?
C27 C21 N8 66.2(17) . . ?
C27 C21 C22 138(2) . . ?
N8 C21 C22 108.3(17) . . ?
C27 C21 N9 125.2(18) . 7 ?
N8 C21 N9 65.5(11) . 7 ?
C28 C21 C26 146(3) . . ?
N8 C21 C26 47.8(12) . . ?
C22 C21 C26 156.1(17) . . ?
N9 C21 C26 110.9(11) 7 . ?
C28 C22 N9 74(2) . 7 ?
C28 C22 C23 103(3) . 7 ?
N9 C22 C23 53.5(13) 7 7 ?
N9 C22 C21 78.7(17) 7 . ?
C23 C22 C21 118(2) 7 . ?
C24 C23 N9 112(3) . . ?
C24 C23 N7 47(2) . . ?
N9 C23 N7 65.5(13) . . ?
C24 C23 C22 158(3) . 7 ?
N9 C23 C22 57.0(14) . 7 ?
N7 C23 C22 119.8(19) . 7 ?
N9 C23 C25 95.0(13) . . ?
C22 C23 C25 143.9(17) 7 . ?
C24 C23 C28 156(3) . 7 ?
N7 C23 C28 110.9(15) . 7 ?
C25 C23 C28 140.8(12) . 7 ?
C23 C24 N7 105(3) . . ?
C23 C24 C25 154(3) . . ?
C25 C24 N9 108.1(14) . . ?
C23 C24 C19 151(3) . . ?
N9 C24 C19 109.0(13) . . ?
C19 C25 N7 107(3) . . ?
C19 C25 C24 120(3) . . ?
N7 C25 N10 77.0(17) . . ?
C24 C25 N10 110.9(15) . . ?
C19 C25 C23 122(3) . . ?
N10 C25 C23 107.1(12) . . ?
C20 C26 C27 147(4) . . ?
C20 C26 N8 95(3) . . ?
C27 C26 N10 116(2) . . ?
C20 C26 C21 146(4) . . ?
N10 C26 C21 108.0(15) . . ?
C21 C27 C26 109(2) . . ?
C21 C27 N8 75.1(18) . . ?
C26 C27 C28 113(2) . . ?
N8 C27 C28 73.8(14) . . ?
C21 C27 C20 112(2) . . ?
C28 C27 C20 115.4(15) . . ?
C21 C28 C22 134(3) . . ?
C21 C28 N9 115(2) . 7 ?
C22 C28 C27 126(2) . . ?
N9 C28 C27 110.1(14) 7 . ?
C22 C28 N8 118(2) . . ?
N9 C28 N8 66.6(10) 7 . ?
C21 C28 C23 156(3) . 7 ?
C27 C28 C23 151.0(14) . 7 ?
N8 C28 C23 106.4(12) . 7 ?