# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1234
data_global

#-------------------------------------------------------------------------
      #1    Data block identification for start of deposition

#-------------------------------------------------------------------------
      #2    Person making the deposition

_publ_contact_author
;
     J.M. Moreno
     Departamento de Qu\'imica Inorg\'anica.
     Facultad de Ciencias.
     Universidad de Granada
     18071-Granada
     SPAIN
;
_publ_contact_author_phone        34-58-243236
_publ_contact_author_fax          34-58-243322
_publ_contact_author_email        jmoreno@goliat.ugr.es



#-------------------------------------------------------------------------
      #3    Publication details

_publ_section_title
;
A novel two-dimensional honey-comb-like bimetallic Fe(III)-Ni(II)
cyanide-bridged magnetic material [Ni(cyclam)]3[Fe(CN)6]2.nH2O (cyclam=
1,4,8,11-tetraazacyclodecane).
;
loop_
     _publ_author_name
     _publ_author_address

    'Colacio, Enrique'
;
    Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias,
    Universidad de Granada, 18071 Granada, Spain
;
    'Dominguez-Vera, Jose M.'
;
    Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias,
    Universidad de Granada, 18071 Granada, Spain
;

    'Ghazi, Mustapha'
;
    Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias,
    Universidad de Granada, 18071 Granada, Spain
;
    'Kiveks, Raikko'
;
    Department of Chemistry, Laboratory of Inorganic Chemistry,
    University of Helsinki, F00014 Helsinki, Finland
;
    'Lloret, Francesc'
;
    Departament de Qu\'imica Inorg\'anica, Facultat de Qu\'imica,
    Universitat de Valencia, 46100 Burjassot, Spain
;
     'Moreno, Jose M.'
;
    Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias,
    Universidad de Granada, 18071 Granada, Spain
;

     'Stoeckli-Evans, Helen'
;
     Institut de Chimie, Universit/'e de Neuch/^atel, Avenue de Bellevaux
51,
     CH-2000 Neuchatel, Switzerland
;
_journal_name_full                
'Journal of the Chemical Society,Chemical Communications'
_journal_volume                    '?'
_journal_page_first                '?'
_journal_page_last                 '?'
_journal_year                      '?'
_ccdc_journal_depnumber            '?'
_publ_section_references
;
;

#-------------------------------------------------------------------------
      #4    Chemical and physical data for [Ni(cyclam)]3[Fe(CN)6]2.22.5H2O

data_1

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C42 H117 Fe2 N24 Ni3 O22.50'
_chemical_formula_weight          1606.43

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'
 'Fe'  'Fe'   0.3463   0.8444
 '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    'A 2/n'

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

_cell_length_a                    17.9384(12)
_cell_length_b                    16.7894(12)
_cell_length_c                    25.764(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.176(9)
_cell_angle_gamma                 90.00
_cell_volume                      7757.7(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     223(2)
_cell_measurement_reflns_used     5000
_cell_measurement_theta_min       2.43
_cell_measurement_theta_max       25.82

_exptl_crystal_description        block
_exptl_crystal_colour             'dark brown'
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.50
_exptl_crystal_size_min           0.40
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     1.375
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3396
_exptl_absorpt_coefficient_mu     1.157
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       223(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   'STOE Image Plate Diffraction System'
_diffrn_measurement_method        'phi oscillation scans'
_diffrn_detector_area_resol_mean  0.81
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             29143
_diffrn_reflns_av_R_equivalents   0.0497
_diffrn_reflns_av_sigmaI/netI     0.0482
_diffrn_reflns_limit_h_min        -21
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          2.43
_diffrn_reflns_theta_max          25.82
_reflns_number_total              7366
_reflns_number_gt                 4326
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'EXPOSE (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_cell_refinement        'CELL (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_reduction         'INTEGRATE (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^] 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     'riding atoms'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7366
_refine_ls_number_parameters      474
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0785
_refine_ls_R_factor_obs           0.0457
_refine_ls_wR_factor_all          0.1466
_refine_ls_wR_factor_obs          0.1326
_refine_ls_goodness_of_fit_all    0.958
_refine_ls_restrained_S_all       0.958
_refine_ls_shift/su_max           0.008
_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_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Fe1 Fe -0.12911(2) 0.24852(3) 0.074515(16) 0.01688(14) Uani 1 d . . .
Ni1 Ni 0.0000 0.0000 0.0000 0.0330(2) Uani 1 d S . .
Ni2 Ni 0.0000 0.2500 0.2500 0.02244(16) Uani 1 d S . .
Ni3 Ni 0.0000 0.5000 0.0000 0.02281(18) Uani 1 d S . .
N1 N 0.1010(2) 0.0583(2) -0.00142(15) 0.0452(9) Uani 1 d . . .
H1 H 0.0906 0.1113 -0.0002 0.054 Uiso 1 calc R . .
N2 N 0.0243(2) -0.0156(2) 0.07816(14) 0.0460(10) Uani 1 d . . .
H2 H 0.0434 -0.0655 0.0816 0.055 Uiso 1 calc R . .
N3 N 0.0522(2) -0.11109(19) -0.01667(14) 0.0375(8) Uani 1 d . . .
N4 N 0.0791(2) 0.3288(2) 0.22358(13) 0.0400(9) Uani 1 d . . .
H4 H 0.0727 0.3311 0.1885 0.048 Uiso 1 calc R . .
N5 N 0.0865(2) 0.1685(2) 0.25061(12) 0.0404(9) Uani 1 d . . .
H5 H 0.1038 0.1644 0.2839 0.049 Uiso 1 calc R . .
N6 N 0.02811(19) 0.27452(19) 0.32882(11) 0.0320(8) Uani 1 d . . .
N7 N 0.1070(2) 0.4708(2) 0.02482(14) 0.0459(9) Uani 1 d . . .
H7 H 0.1052 0.4196 0.0363 0.055 Uiso 1 calc R . .
N8 N -0.0107(2) 0.5519(2) 0.07198(14) 0.0479(10) Uani 1 d . . .
H8 H -0.0045 0.6052 0.0676 0.058 Uiso 1 calc R . .
N9 N 0.03943(18) 0.61215(18) -0.02830(11) 0.0284(7) Uani 1 d . . .
N10 N -0.2261(2) 0.1201(2) 0.12606(14) 0.0434(9) Uani 1 d . . .
N11 N -0.2025(2) 0.3771(2) 0.14232(14) 0.0444(9) Uani 1 d . . .
N12 N -0.2424(2) 0.2678(2) -0.01611(16) 0.0549(11) Uani 1 d . . .
C1 C 0.1402(3) 0.0387(3) 0.0472(2) 0.0572(14) Uani 1 d . . .
H1A H 0.1796 0.0772 0.0540 0.069 Uiso 1 calc R . .
H1B H 0.1627 -0.0137 0.0447 0.069 Uiso 1 calc R . .
C2 C 0.0856(3) 0.0401(3) 0.09054(19) 0.0564(14) Uani 1 d . . .
H2A H 0.1103 0.0244 0.1228 0.068 Uiso 1 calc R . .
H2B H 0.0661 0.0935 0.0948 0.068 Uiso 1 calc R . .
C3 C -0.0394(3) -0.0111(3) 0.11315(19) 0.0538(13) Uani 1 d . . .
H3A H -0.0583 0.0431 0.1132 0.065 Uiso 1 calc R . .
H3B H -0.0223 -0.0236 0.1482 0.065 Uiso 1 calc R . .
C4 C -0.1008(3) -0.0656(3) 0.0986(2) 0.0608(14) Uani 1 d . . .
H4A H -0.1354 -0.0674 0.1270 0.073 Uiso 1 calc R . .
H4B H -0.0802 -0.1187 0.0948 0.073 Uiso 1 calc R . .
C5 C -0.1451(3) -0.0455(3) 0.0486(2) 0.0556(14) Uani 1 d . . .
H5A H -0.1896 -0.0784 0.0467 0.067 Uiso 1 calc R . .
H5B H -0.1609 0.0098 0.0499 0.067 Uiso 1 calc R . .
C6 C 0.1521(3) 0.2912(4) 0.23327(18) 0.0564(13) Uani 1 d . . .
H6A H 0.1666 0.2970 0.2696 0.068 Uiso 1 calc R . .
H6B H 0.1896 0.3169 0.2124 0.068 Uiso 1 calc R . .
C7 C 0.1468(3) 0.2060(4) 0.21967(17) 0.0568(14) Uani 1 d . . .
H7A H 0.1940 0.1798 0.2272 0.068 Uiso 1 calc R . .
H7B H 0.1355 0.2002 0.1829 0.068 Uiso 1 calc R . .
C8 C 0.0652(3) 0.0886(3) 0.23335(17) 0.0583(15) Uani 1 d . . .
H8A H 0.1086 0.0542 0.2349 0.070 Uiso 1 calc R . .
H8B H 0.0477 0.0910 0.1975 0.070 Uiso 1 calc R . .
C9 C 0.0722(3) 0.4114(3) 0.24250(19) 0.0642(17) Uani 1 d . . .
H9A H 0.1084 0.4444 0.2251 0.077 Uiso 1 calc R . .
H9B H 0.0842 0.4125 0.2794 0.077 Uiso 1 calc R . .
C10 C -0.0046(4) 0.4466(3) 0.2336(2) 0.0635(16) Uani 1 d . . .
C11 C 0.1224(3) 0.5194(3) 0.06967(19) 0.0614(15) Uani 1 d . . .
H11A H 0.1363 0.5726 0.0589 0.074 Uiso 1 calc R . .
H11B H 0.1637 0.4970 0.0897 0.074 Uiso 1 calc R . .
C12 C 0.0537(3) 0.5233(3) 0.10274(17) 0.0545(13) Uani 1 d . . .
H12A H 0.0430 0.4708 0.1164 0.065 Uiso 1 calc R . .
H12B H 0.0628 0.5589 0.1318 0.065 Uiso 1 calc R . .
C13 C -0.0810(3) 0.5409(3) 0.09738(18) 0.0583(15) Uani 1 d . . .
H13A H -0.0804 0.5698 0.1300 0.070 Uiso 1 calc R . .
H13B H -0.0881 0.4848 0.1050 0.070 Uiso 1 calc R . .
C14 C -0.1462(3) 0.5709(3) 0.0628(2) 0.0635(15) Uani 1 d . . .
H14A H -0.1903 0.5724 0.0839 0.076 Uiso 1 calc R . .
H14B H -0.1352 0.6254 0.0530 0.076 Uiso 1 calc R . .
C15 C -0.1657(3) 0.5265(3) 0.0143(2) 0.0580(14) Uani 1 d . . .
H15A H -0.1754 0.4713 0.0231 0.070 Uiso 1 calc R . .
H15B H -0.2113 0.5485 -0.0006 0.070 Uiso 1 calc R . .
C16 C -0.1914(2) 0.1678(2) 0.10606(13) 0.0263(8) Uani 1 d . . .
C17 C -0.1776(2) 0.3293(2) 0.11607(14) 0.0268(8) Uani 1 d . . .
C18 C -0.0612(2) 0.23362(19) 0.13315(13) 0.0257(8) Uani 1 d . . .
C19 C -0.0795(2) 0.1647(2) 0.03621(13) 0.0230(8) Uani 1 d . . .
C20 C -0.2003(2) 0.2613(2) 0.01774(15) 0.0299(8) Uani 1 d . . .
C21 C -0.0692(2) 0.3338(2) 0.04489(13) 0.0223(8) Uani 1 d . . .
O1 O -0.2333(2) 0.51621(18) 0.19767(12) 0.0669(11) Uani 1 d . . .
O2 O -0.2417(3) -0.0083(2) 0.19736(15) 0.0798(13) Uani 1 d . . .
O3 O -0.3993(2) 0.2613(2) 0.01231(18) 0.0729(12) Uani 1 d . . .
O4 O -0.38553(19) 0.1727(2) 0.10645(13) 0.0615(10) Uani 1 d . . .
O5 O -0.0063(3) 0.7351(2) 0.0774(2) 0.1007(17) Uani 1 d . . .
O6 O -0.1191(4) 0.6274(3) 0.2315(3) 0.097(2) Uani 0.75 d P . .
O7 O 0.1757(4) 0.6453(3) 0.1857(3) 0.107(2) Uani 0.75 d P . .
O8 O 0.1515(5) -0.1171(3) 0.1609(2) 0.160(3) Uani 1 d . . .
O9 O -0.1436(5) 0.2474(4) -0.1040(3) 0.073(2) Uani 0.50 d P . .
O10 O -0.1139(8) 0.7508(5) 0.1644(4) 0.112(4) Uani 0.50 d P . .
O11 O 0.2500 0.7488(7) 0.2500 0.137(8) Uani 0.50 d SP . .
O12 O -0.2390(9) 0.2561(6) -0.1240(4) 0.129(5) Uani 0.50 d P . .
O13 O -0.1153(6) -0.1214(5) 0.2286(4) 0.104(3) Uani 0.50 d P . .
O14 O -0.0373(6) -0.1699(6) 0.2635(6) 0.128(4) Uani 0.50 d P . .
O15 O -0.0338(10) 0.6641(8) 0.2660(8) 0.188(7) Uani 0.50 d P . .
O16 O -0.1645(11) 0.6547(8) 0.1976(7) 0.077(5) Uani 0.25 d P . .
O17 O -0.1631(14) 0.7564(11) 0.1173(9) 0.108(7) Uani 0.25 d P . .

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
Fe1 0.0188(3) 0.0150(2) 0.0168(2) -0.00029(18) 0.00176(17) 0.0000(2)
Ni1 0.0270(5) 0.0261(4) 0.0458(4) -0.0159(3) -0.0029(3) 0.0081(3)
Ni2 0.0212(3) 0.0300(3) 0.0160(3) 0.0009(3) -0.0011(2) -0.0009(3)
Ni3 0.0237(4) 0.0210(3) 0.0238(3) 0.0055(2) 0.0032(3) -0.0031(3)
N1 0.034(2) 0.038(2) 0.064(2) -0.0223(17) 0.0026(18) 0.0044(16)
N2 0.047(3) 0.042(2) 0.049(2) -0.0090(17) 0.0035(18) 0.0179(18)
N3 0.034(2) 0.0296(18) 0.049(2) -0.0136(15) -0.0019(16) 0.0078(15)
N4 0.036(2) 0.055(2) 0.0286(17) 0.0039(15) 0.0008(15) -0.0164(18)
N5 0.044(2) 0.054(2) 0.0230(16) -0.0008(15) -0.0017(15) 0.0148(18)
N6 0.037(2) 0.0394(18) 0.0199(15) -0.0005(12) -0.0050(14) -0.0018(15)
N7 0.039(2) 0.043(2) 0.056(2) 0.0196(18) -0.0037(18) -0.0041(17)
N8 0.067(3) 0.0324(19) 0.045(2) 0.0014(16) 0.0152(19) -0.0101(18)
N9 0.0286(19) 0.0252(16) 0.0317(16) 0.0067(13) 0.0048(14) -0.0019(14)
N10 0.047(2) 0.039(2) 0.045(2) 0.0031(16) 0.0106(17) -0.0167(18)
N11 0.055(3) 0.0357(19) 0.043(2) -0.0099(16) 0.0196(18) 0.0026(17)
N12 0.048(3) 0.067(3) 0.049(2) 0.0022(19) -0.021(2) 0.007(2)
C1 0.034(3) 0.064(3) 0.073(3) -0.030(3) -0.007(2) 0.005(2)
C2 0.041(3) 0.072(3) 0.055(3) -0.026(3) -0.017(2) 0.014(3)
C3 0.064(4) 0.048(3) 0.050(3) -0.006(2) 0.004(2) 0.016(3)
C4 0.070(4) 0.048(3) 0.065(3) -0.004(2) 0.026(3) 0.013(3)
C5 0.039(3) 0.042(3) 0.086(4) -0.025(2) 0.024(3) -0.005(2)
C6 0.033(3) 0.099(4) 0.038(2) 0.004(3) 0.003(2) -0.018(3)
C7 0.035(3) 0.101(4) 0.034(2) 0.001(3) 0.001(2) 0.019(3)
C8 0.090(4) 0.053(3) 0.032(2) -0.004(2) -0.005(2) 0.027(3)
C9 0.093(5) 0.055(3) 0.045(3) -0.001(2) 0.001(3) -0.040(3)
C10 0.097(5) 0.041(3) 0.052(3) 0.007(2) -0.004(3) 0.001(3)
C11 0.067(4) 0.064(3) 0.052(3) 0.020(2) -0.024(3) -0.013(3)
C12 0.058(4) 0.072(3) 0.032(2) 0.008(2) -0.009(2) -0.015(3)
C13 0.086(4) 0.042(3) 0.048(3) -0.003(2) 0.033(3) -0.008(3)
C14 0.057(4) 0.058(3) 0.077(4) 0.018(3) 0.036(3) 0.006(3)
C15 0.031(3) 0.053(3) 0.091(4) 0.004(3) 0.021(3) -0.006(2)
C16 0.025(2) 0.0276(19) 0.0260(18) -0.0029(15) 0.0027(16) -0.0027(16)
C17 0.030(2) 0.0231(18) 0.0274(18) -0.0005(15) 0.0066(16) -0.0018(16)
C18 0.029(2) 0.026(2) 0.0218(17) 0.0010(13) 0.0003(15) -0.0029(14)
C19 0.023(2) 0.0200(17) 0.0262(18) -0.0006(14) 0.0011(15) 0.0003(15)
C20 0.026(2) 0.028(2) 0.035(2) -0.0036(15) 0.0023(16) 0.0046(16)
C21 0.023(2) 0.0241(18) 0.0199(16) -0.0003(14) 0.0034(14) 0.0023(15)
O1 0.120(4) 0.0319(16) 0.0496(19) -0.0063(14) 0.029(2) 0.0016(19)
O2 0.125(4) 0.052(2) 0.063(2) 0.0045(17) 0.029(2) -0.009(2)
O3 0.051(2) 0.052(2) 0.116(3) 0.017(2) 0.010(2) 0.0048(17)
O4 0.046(2) 0.079(2) 0.060(2) -0.0224(18) 0.0012(16) 0.0056(18)
O5 0.150(5) 0.053(3) 0.098(3) -0.008(2) -0.004(3) 0.012(3)
O6 0.126(6) 0.071(4) 0.095(5) -0.003(3) 0.040(4) -0.016(4)
O7 0.162(7) 0.051(3) 0.107(5) -0.020(3) -0.033(4) 0.025(4)
O8 0.249(9) 0.097(4) 0.135(5) -0.030(3) 0.057(5) -0.079(5)
O9 0.085(6) 0.077(5) 0.056(4) -0.015(4) -0.004(4) -0.012(5)
O10 0.203(13) 0.064(5) 0.071(6) 0.005(4) 0.020(7) -0.020(6)
O11 0.191(19) 0.056(7) 0.158(15) 0.000 -0.110(14) 0.000
O12 0.215(16) 0.096(8) 0.077(7) -0.006(5) 0.040(8) -0.001(8)
O13 0.102(8) 0.060(5) 0.150(9) 0.009(5) 0.041(7) 0.018(5)
O14 0.066(7) 0.098(8) 0.222(14) -0.032(8) 0.025(8) -0.008(6)
O15 0.177(16) 0.084(8) 0.30(2) -0.007(11) -0.007(15) 0.048(9)
O16 0.121(16) 0.030(7) 0.079(11) -0.003(7) -0.013(10) -0.002(8)
O17 0.113(18) 0.115(16) 0.096(15) 0.015(11) -0.012(13) -0.020(13)

_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
Fe1 C20 1.934(4) . ?
Fe1 C18 1.937(4) . ?
Fe1 C17 1.945(4) . ?
Fe1 C19 1.945(4) . ?
Fe1 C16 1.946(4) . ?
Fe1 C21 1.954(4) . ?
Ni1 N1 2.059(4) 5 ?
Ni1 N1 2.059(4) . ?
Ni1 N2 2.068(4) . ?
Ni1 N2 2.068(4) 5 ?
Ni1 N3 2.134(3) . ?
Ni1 N3 2.134(3) 5 ?
Ni2 N4 2.066(3) 7 ?
Ni2 N4 2.066(3) . ?
Ni2 N5 2.069(3) 7 ?
Ni2 N5 2.069(3) . ?
Ni2 N6 2.123(3) . ?
Ni2 N6 2.123(3) 7 ?
Ni3 N8 2.061(4) 5_565 ?
Ni3 N8 2.061(4) . ?
Ni3 N7 2.070(4) . ?
Ni3 N7 2.070(4) 5_565 ?
Ni3 N9 2.144(3) 5_565 ?
Ni3 N9 2.144(3) . ?
N1 C1 1.462(6) . ?
N1 C5 1.481(6) 5 ?
N2 C3 1.472(6) . ?
N2 C2 1.473(6) . ?
N3 C19 1.146(5) 5 ?
N4 C6 1.471(6) . ?
N4 C9 1.475(6) . ?
N5 C8 1.462(6) . ?
N5 C7 1.495(6) . ?
N6 C18 1.144(4) 7 ?
N7 C11 1.437(6) . ?
N7 C15 1.474(6) 5_565 ?
N8 C13 1.445(6) . ?
N8 C12 1.468(6) . ?
N9 C21 1.141(4) 5_565 ?
N10 C16 1.142(5) . ?
N11 C17 1.145(5) . ?
N12 C20 1.148(5) . ?
C1 C2 1.500(7) . ?
C3 C4 1.475(7) . ?
C4 C5 1.537(7) . ?
C5 N1 1.481(6) 5 ?
C6 C7 1.477(8) . ?
C8 C10 1.514(8) 7 ?
C9 C10 1.514(8) . ?
C10 C8 1.514(8) 7 ?
C11 C12 1.514(8) . ?
C13 C14 1.540(8) . ?
C14 C15 1.489(7) . ?
C15 N7 1.474(6) 5_565 ?
C18 N6 1.144(4) 7 ?
C19 N3 1.146(5) 5 ?
C21 N9 1.141(4) 5_565 ?
O6 O16 1.267(16) . ?
O9 O12 1.782(18) . ?
O10 O17 1.49(2) . ?
O12 O17 1.77(3) 4_444 ?
O14 O15 1.50(2) 7 ?
O15 O14 1.50(2) 7 ?
O17 O12 1.77(3) 4_454 ?

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
C20 Fe1 C18 177.47(16) . . ?
C20 Fe1 C17 92.46(15) . . ?
C18 Fe1 C17 86.67(15) . . ?
C20 Fe1 C19 89.92(15) . . ?
C18 Fe1 C19 90.88(15) . . ?
C17 Fe1 C19 177.07(14) . . ?
C20 Fe1 C16 90.96(16) . . ?
C18 Fe1 C16 86.65(15) . . ?
C17 Fe1 C16 89.36(15) . . ?
C19 Fe1 C16 88.89(15) . . ?
C20 Fe1 C21 89.04(15) . . ?
C18 Fe1 C21 93.30(14) . . ?
C17 Fe1 C21 87.68(15) . . ?
C19 Fe1 C21 94.07(14) . . ?
C16 Fe1 C21 177.04(15) . . ?
N1 Ni1 N1 180.0 5 . ?
N1 Ni1 N2 95.19(16) 5 . ?
N1 Ni1 N2 84.81(16) . . ?
N1 Ni1 N2 84.81(16) 5 5 ?
N1 Ni1 N2 95.19(16) . 5 ?
N2 Ni1 N2 180.0 . 5 ?
N1 Ni1 N3 88.73(14) 5 . ?
N1 Ni1 N3 91.27(14) . . ?
N2 Ni1 N3 90.07(14) . . ?
N2 Ni1 N3 89.93(14) 5 . ?
N1 Ni1 N3 91.27(14) 5 5 ?
N1 Ni1 N3 88.73(14) . 5 ?
N2 Ni1 N3 89.93(14) . 5 ?
N2 Ni1 N3 90.07(14) 5 5 ?
N3 Ni1 N3 180.0 . 5 ?
N4 Ni2 N4 180.0 7 . ?
N4 Ni2 N5 84.61(15) 7 7 ?
N4 Ni2 N5 95.39(15) . 7 ?
N4 Ni2 N5 95.39(15) 7 . ?
N4 Ni2 N5 84.61(15) . . ?
N5 Ni2 N5 180.0 7 . ?
N4 Ni2 N6 87.72(13) 7 . ?
N4 Ni2 N6 92.28(13) . . ?
N5 Ni2 N6 92.43(13) 7 . ?
N5 Ni2 N6 87.57(13) . . ?
N4 Ni2 N6 92.28(13) 7 7 ?
N4 Ni2 N6 87.72(13) . 7 ?
N5 Ni2 N6 87.57(13) 7 7 ?
N5 Ni2 N6 92.43(13) . 7 ?
N6 Ni2 N6 180.0 . 7 ?
N8 Ni3 N8 180.0 5_565 . ?
N8 Ni3 N7 94.28(16) 5_565 . ?
N8 Ni3 N7 85.72(16) . . ?
N8 Ni3 N7 85.71(16) 5_565 5_565 ?
N8 Ni3 N7 94.28(16) . 5_565 ?
N7 Ni3 N7 180.0 . 5_565 ?
N8 Ni3 N9 88.43(13) 5_565 5_565 ?
N8 Ni3 N9 91.57(13) . 5_565 ?
N7 Ni3 N9 89.84(13) . 5_565 ?
N7 Ni3 N9 90.16(13) 5_565 5_565 ?
N8 Ni3 N9 91.57(13) 5_565 . ?
N8 Ni3 N9 88.43(13) . . ?
N7 Ni3 N9 90.16(13) . . ?
N7 Ni3 N9 89.84(13) 5_565 . ?
N9 Ni3 N9 180.0 5_565 . ?
C1 N1 C5 114.5(4) . 5 ?
C1 N1 Ni1 106.7(3) . . ?
C5 N1 Ni1 115.6(3) 5 . ?
C3 N2 C2 114.9(4) . . ?
C3 N2 Ni1 116.1(3) . . ?
C2 N2 Ni1 105.8(3) . . ?
C19 N3 Ni1 165.4(3) 5 . ?
C6 N4 C9 115.3(4) . . ?
C6 N4 Ni2 106.5(3) . . ?
C9 N4 Ni2 115.5(3) . . ?
C8 N5 C7 114.3(4) . . ?
C8 N5 Ni2 114.4(3) . . ?
C7 N5 Ni2 105.6(3) . . ?
C18 N6 Ni2 154.9(3) 7 . ?
C11 N7 C15 113.9(4) . 5_565 ?
C11 N7 Ni3 106.0(3) . . ?
C15 N7 Ni3 116.9(3) 5_565 . ?
C13 N8 C12 113.5(4) . . ?
C13 N8 Ni3 116.9(3) . . ?
C12 N8 Ni3 105.1(3) . . ?
C21 N9 Ni3 170.5(3) 5_565 . ?
N1 C1 C2 108.9(4) . . ?
N2 C2 C1 109.0(4) . . ?
N2 C3 C4 113.4(4) . . ?
C3 C4 C5 116.6(4) . . ?
N1 C5 C4 112.3(4) 5 . ?
N4 C6 C7 108.8(4) . . ?
C6 C7 N5 109.0(4) . . ?
N5 C8 C10 111.9(4) . 7 ?
N4 C9 C10 113.5(4) . . ?
C9 C10 C8 115.1(4) . 7 ?
N7 C11 C12 109.4(4) . . ?
N8 C12 C11 110.6(4) . . ?
N8 C13 C14 110.8(4) . . ?
C15 C14 C13 119.0(4) . . ?
N7 C15 C14 113.5(4) 5_565 . ?
N10 C16 Fe1 177.4(3) . . ?
N11 C17 Fe1 176.0(4) . . ?
N6 C18 Fe1 172.3(3) 7 . ?
N3 C19 Fe1 174.4(3) 5 . ?
N12 C20 Fe1 179.1(3) . . ?
N9 C21 Fe1 174.0(3) 5_565 . ?
O17 O12 O9 157.1(10) 4_444 . ?
O10 O17 O12 119.6(17) . 4_454 ?

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
N1 Ni1 N1 C1 -166(40) 5 . . . ?
N2 Ni1 N1 C1 14.2(3) . . . . ?
N2 Ni1 N1 C1 -165.8(3) 5 . . . ?
N3 Ni1 N1 C1 -75.8(3) . . . . ?
N3 Ni1 N1 C1 104.2(3) 5 . . . ?
N1 Ni1 N1 C5 -37(40) 5 . . 5 ?
N2 Ni1 N1 C5 142.7(3) . . . 5 ?
N2 Ni1 N1 C5 -37.3(3) 5 . . 5 ?
N3 Ni1 N1 C5 52.8(3) . . . 5 ?
N3 Ni1 N1 C5 -127.2(3) 5 . . 5 ?
N1 Ni1 N2 C3 -36.4(3) 5 . . . ?
N1 Ni1 N2 C3 143.6(3) . . . . ?
N2 Ni1 N2 C3 4(69) 5 . . . ?
N3 Ni1 N2 C3 -125.1(3) . . . . ?
N3 Ni1 N2 C3 54.9(3) 5 . . . ?
N1 Ni1 N2 C2 -165.1(3) 5 . . . ?
N1 Ni1 N2 C2 14.9(3) . . . . ?
N2 Ni1 N2 C2 -125(69) 5 . . . ?
N3 Ni1 N2 C2 106.2(3) . . . . ?
N3 Ni1 N2 C2 -73.8(3) 5 . . . ?
N1 Ni1 N3 C19 99.2(13) 5 . . 5 ?
N1 Ni1 N3 C19 -80.8(13) . . . 5 ?
N2 Ni1 N3 C19 -165.6(13) . . . 5 ?
N2 Ni1 N3 C19 14.4(13) 5 . . 5 ?
N3 Ni1 N3 C19 18(100) 5 . . 5 ?
N4 Ni2 N4 C6 -121(68) 7 . . . ?
N5 Ni2 N4 C6 165.4(3) 7 . . . ?
N5 Ni2 N4 C6 -14.6(3) . . . . ?
N6 Ni2 N4 C6 72.8(3) . . . . ?
N6 Ni2 N4 C6 -107.2(3) 7 . . . ?
N4 Ni2 N4 C9 110(68) 7 . . . ?
N5 Ni2 N4 C9 36.0(3) 7 . . . ?
N5 Ni2 N4 C9 -144.0(3) . . . . ?
N6 Ni2 N4 C9 -56.7(3) . . . . ?
N6 Ni2 N4 C9 123.3(3) 7 . . . ?
N4 Ni2 N5 C8 39.1(3) 7 . . . ?
N4 Ni2 N5 C8 -140.9(3) . . . . ?
N5 Ni2 N5 C8 -93(57) 7 . . . ?
N6 Ni2 N5 C8 126.6(3) . . . . ?
N6 Ni2 N5 C8 -53.4(3) 7 . . . ?
N4 Ni2 N5 C7 165.6(3) 7 . . . ?
N4 Ni2 N5 C7 -14.4(3) . . . . ?
N5 Ni2 N5 C7 33(57) 7 . . . ?
N6 Ni2 N5 C7 -106.9(3) . . . . ?
N6 Ni2 N5 C7 73.1(3) 7 . . . ?
N4 Ni2 N6 C18 93.4(7) 7 . . 7 ?
N4 Ni2 N6 C18 -86.6(7) . . . 7 ?
N5 Ni2 N6 C18 177.9(7) 7 . . 7 ?
N5 Ni2 N6 C18 -2.1(7) . . . 7 ?
N6 Ni2 N6 C18 -130(82) 7 . . 7 ?
N8 Ni3 N7 C11 164.3(3) 5_565 . . . ?
N8 Ni3 N7 C11 -15.7(3) . . . . ?
N7 Ni3 N7 C11 100(100) 5_565 . . . ?
N9 Ni3 N7 C11 -107.3(3) 5_565 . . . ?
N9 Ni3 N7 C11 72.7(3) . . . . ?
N8 Ni3 N7 C15 36.2(3) 5_565 . . 5_565 ?
N8 Ni3 N7 C15 -143.8(3) . . . 5_565 ?
N7 Ni3 N7 C15 -29(100) 5_565 . . 5_565 ?
N9 Ni3 N7 C15 124.6(3) 5_565 . . 5_565 ?
N9 Ni3 N7 C15 -55.4(3) . . . 5_565 ?
N8 Ni3 N8 C13 86.7(9) 5_565 . . . ?
N7 Ni3 N8 C13 -139.5(3) . . . . ?
N7 Ni3 N8 C13 40.5(3) 5_565 . . . ?
N9 Ni3 N8 C13 -49.8(3) 5_565 . . . ?
N9 Ni3 N8 C13 130.2(3) . . . . ?
N8 Ni3 N8 C12 -146.5(9) 5_565 . . . ?
N7 Ni3 N8 C12 -12.7(3) . . . . ?
N7 Ni3 N8 C12 167.3(3) 5_565 . . . ?
N9 Ni3 N8 C12 77.0(3) 5_565 . . . ?
N9 Ni3 N8 C12 -103.0(3) . . . . ?
N8 Ni3 N9 C21 -60.5(17) 5_565 . . 5_565 ?
N8 Ni3 N9 C21 119.5(17) . . . 5_565 ?
N7 Ni3 N9 C21 33.8(17) . . . 5_565 ?
N7 Ni3 N9 C21 -146.2(17) 5_565 . . 5_565 ?
N9 Ni3 N9 C21 -121(79) 5_565 . . 5_565 ?
C5 N1 C1 C2 -169.9(4) 5 . . . ?
Ni1 N1 C1 C2 -40.7(4) . . . . ?
C3 N2 C2 C1 -170.7(4) . . . . ?
Ni1 N2 C2 C1 -41.3(4) . . . . ?
N1 C1 C2 N2 56.5(5) . . . . ?
C2 N2 C3 C4 178.1(4) . . . . ?
Ni1 N2 C3 C4 53.9(5) . . . . ?
N2 C3 C4 C5 -69.7(5) . . . . ?
C3 C4 C5 N1 70.2(5) . . . 5 ?
C9 N4 C6 C7 171.4(4) . . . . ?
Ni2 N4 C6 C7 41.8(4) . . . . ?
N4 C6 C7 N5 -57.2(4) . . . . ?
C8 N5 C7 C6 168.1(4) . . . . ?
Ni2 N5 C7 C6 41.5(4) . . . . ?
C7 N5 C8 C10 179.4(4) . . . 7 ?
Ni2 N5 C8 C10 -58.7(4) . . . 7 ?
C6 N4 C9 C10 -177.7(4) . . . . ?
Ni2 N4 C9 C10 -52.7(5) . . . . ?
N4 C9 C10 C8 69.9(6) . . . 7 ?
C15 N7 C11 C12 170.5(4) 5_565 . . . ?
Ni3 N7 C11 C12 40.6(4) . . . . ?
C13 N8 C12 C11 167.4(4) . . . . ?
Ni3 N8 C12 C11 38.5(5) . . . . ?
N7 C11 C12 N8 -55.5(5) . . . . ?
C12 N8 C13 C14 -179.2(4) . . . . ?
Ni3 N8 C13 C14 -56.5(5) . . . . ?
N8 C13 C14 C15 68.9(6) . . . . ?
C13 C14 C15 N7 -65.7(6) . . . 5_565 ?
C20 Fe1 C16 N10 -180(100) . . . . ?
C18 Fe1 C16 N10 0(8) . . . . ?
C17 Fe1 C16 N10 -87(8) . . . . ?
C19 Fe1 C16 N10 90(8) . . . . ?
C21 Fe1 C16 N10 -90(9) . . . . ?
C20 Fe1 C17 N11 -164(5) . . . . ?
C18 Fe1 C17 N11 18(5) . . . . ?
C19 Fe1 C17 N11 52(7) . . . . ?
C16 Fe1 C17 N11 105(5) . . . . ?
C21 Fe1 C17 N11 -75(5) . . . . ?
C20 Fe1 C18 N6 -28(5) . . . 7 ?
C17 Fe1 C18 N6 42(2) . . . 7 ?
C19 Fe1 C18 N6 -137(2) . . . 7 ?
C16 Fe1 C18 N6 -48(2) . . . 7 ?
C21 Fe1 C18 N6 129(2) . . . 7 ?
C20 Fe1 C19 N3 -113(3) . . . 5 ?
C18 Fe1 C19 N3 65(3) . . . 5 ?
C17 Fe1 C19 N3 31(6) . . . 5 ?
C16 Fe1 C19 N3 -22(3) . . . 5 ?
C21 Fe1 C19 N3 158(3) . . . 5 ?
C18 Fe1 C20 N12 -80(26) . . . . ?
C17 Fe1 C20 N12 -150(25) . . . . ?
C19 Fe1 C20 N12 28(25) . . . . ?
C16 Fe1 C20 N12 -61(25) . . . . ?
C21 Fe1 C20 N12 122(25) . . . . ?
C20 Fe1 C21 N9 63(3) . . . 5_565 ?
C18 Fe1 C21 N9 -116(3) . . . 5_565 ?
C17 Fe1 C21 N9 -30(3) . . . 5_565 ?
C19 Fe1 C21 N9 153(3) . . . 5_565 ?
C16 Fe1 C21 N9 -27(5) . . . 5_565 ?

_diffrn_measured_fraction_theta_max    0.475
_diffrn_reflns_theta_full              25.82
_diffrn_measured_fraction_theta_full   0.475
_refine_diff_density_max    1.013
_refine_diff_density_min   -0.381
_refine_diff_density_rms    0.088
#===END

#-------------------------------------------------------------------------
      #5    Chemical and physical data for [Ni(cyclam)]3[Fe(CN)6]2.12H2O

data_2

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C42 H96 Fe2 N24 Ni3 O12'
_chemical_formula_weight          1417.26

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'
 'Fe'  'Fe'   0.3463   0.8444
 '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/m'

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

_cell_length_a                    27.384(3)
_cell_length_b                    14.3128(11)
_cell_length_c                    8.4772(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.176(13)
_cell_angle_gamma                 90.00
_cell_volume                      3322.6(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     193(2)
_cell_measurement_reflns_used     5000
_cell_measurement_theta_min       2.40
_cell_measurement_theta_max       25.97

_exptl_crystal_description        block
_exptl_crystal_colour             'dark brown-red'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     1.417
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1496
_exptl_absorpt_coefficient_mu     1.330
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       193(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   'STOE Image Plate Diffraction System'
_diffrn_measurement_method        'phi oscillation scans'
_diffrn_detector_area_resol_mean  0.81
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             13131
_diffrn_reflns_av_R_equivalents   0.1973
_diffrn_reflns_av_sigmaI/netI     0.1665
_diffrn_reflns_limit_h_min        -33
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.40
_diffrn_reflns_theta_max          25.97
_reflns_number_total              3357
_reflns_number_gt                 1571
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'EXPOSE (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_cell_refinement        'CELL (Stoe & Cie GmbH, Darmstadt, 1997)'
_computing_data_reduction         'INTEGRATE (Stoe & Cie GmbH, Darmstadt,1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+0.0000P] 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_extinction_coef        0.0051(7)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3357
_refine_ls_number_parameters      227
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1363
_refine_ls_R_factor_gt            0.0764
_refine_ls_wR_factor_ref          0.2071
_refine_ls_wR_factor_gt           0.1840
_refine_ls_goodness_of_fit_ref    0.831
_refine_ls_restrained_S_all       0.831
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Fe1 Fe 0.15515(5) 0.0000 0.30113(14) 0.0524(5) Uani 1 d S . .
C1 C 0.1192(2) 0.1038(6) 0.3933(8) 0.0568(19) Uani 1 d . . .
C2 C 0.2024(4) 0.0000 0.4742(12) 0.063(3) Uani 1 d S . .
C3 C 0.1922(3) 0.0885(6) 0.1817(8) 0.0584(19) Uani 1 d . . .
C4 C 0.1056(3) 0.0000 0.1432(11) 0.073(4) Uani 1 d S . .
N1 N 0.0983(3) 0.1697(6) 0.4304(8) 0.079(2) Uani 1 d . . .
N2 N 0.2295(4) 0.0000 0.5779(12) 0.079(3) Uani 1 d S . .
N3 N 0.2147(2) 0.1415(5) 0.1042(7) 0.0616(16) Uani 1 d . . .
N4 N 0.0737(3) 0.0000 0.0560(10) 0.086(3) Uani 1 d S . .
Ni1 Ni 0.2500 0.2500 0.0000 0.0597(5) Uani 1 d S . .
N11 N 0.3161(2) 0.1983(5) 0.0837(8) 0.074(2) Uani 1 d . . .
H11 H 0.3102 0.1390 0.1246 0.089 Uiso 1 calc R . .
N12 N 0.2532(3) 0.1787(5) -0.2130(7) 0.0728(19) Uani 1 d . . .
H12 H 0.2427 0.1179 -0.1941 0.087 Uiso 1 calc R . .
C11 C 0.3549(3) 0.1892(9) -0.0373(14) 0.102(4) Uani 1 d . . .
H11A H 0.3842 0.1603 0.0112 0.123 Uiso 1 calc R . .
H11B H 0.3642 0.2521 -0.0754 0.123 Uiso 1 calc R . .
C12 C 0.3382(4) 0.1298(8) -0.1767(14) 0.103(4) Uani 1 d . . .
H12A H 0.3674 0.1127 -0.2390 0.124 Uiso 1 calc R . .
H12B H 0.3242 0.0711 -0.1347 0.124 Uiso 1 calc R . .
C13 C 0.3017(4) 0.1724(8) -0.2861(11) 0.093(3) Uani 1 d . . .
H13A H 0.3127 0.2358 -0.3164 0.112 Uiso 1 calc R . .
H13B H 0.2994 0.1342 -0.3832 0.112 Uiso 1 calc R . .
C14 C 0.2148(4) 0.2255(8) -0.3129(10) 0.089(3) Uani 1 d . . .
H14A H 0.2271 0.2861 -0.3522 0.107 Uiso 1 calc R . .
H14B H 0.2068 0.1857 -0.4050 0.107 Uiso 1 calc R . .
C15 C 0.1703(4) 0.2406(8) -0.2160(11) 0.091(3) Uani 1 d . . .
H15A H 0.1443 0.2703 -0.2804 0.110 Uiso 1 calc R . .
H15B H 0.1578 0.1802 -0.1760 0.110 Uiso 1 calc R . .
Ni2 Ni 0.0000 0.0000 0.0000 0.0488(5) Uani 1 d S . .
N21A N 0.0306(5) 0.1573(14) -0.216(3) 0.086(8) Uani 0.48(3) d P . 1
C21A C 0.0100(6) 0.0696(16) -0.226(4) 0.057(8) Uani 0.67(7) d P . 1
N21B N 0.0202(4) 0.1196(11) -0.1167(16) 0.058(6) Uani 0.52(3) d P . 2
C21B C 0.0165(10) 0.101(3) -0.300(5) 0.049(9) Uani 0.33(7) d P . 2
C22 C 0.0377(4) 0.0000 -0.3095(12) 0.064(3) Uani 1 d S . .
H22A H 0.0708 0.0000 -0.3497 0.077 Uiso 1 d S . .
H22B H 0.0153 0.0000 -0.3981 0.077 Uiso 1 d S . .
C23 C -0.0015(3) 0.2162(7) -0.0913(10) 0.084(3) Uani 1 d . . .
H23A H -0.0354 0.2124 -0.1236 0.101 Uiso 1 d . . .
H23B H 0.0124 0.2730 -0.1313 0.101 Uiso 1 d . . .
O1 O 0.3098(3) 0.0000 0.2587(10) 0.086(2) Uani 1 d S . .
O2 O 0.4608(3) 0.0000 -0.2321(10) 0.086(2) Uani 1 d S . .
O3 O 0.5526(4) 0.0000 -0.0971(13) 0.135(4) Uani 1 d S . .
O4 O 0.05017(18) 0.3502(4) 0.4561(6) 0.0702(14) Uani 1 d . . .
O5 O 0.0955(3) 0.5000 0.6148(10) 0.089(3) Uani 1 d S . .

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
Fe1 0.0434(7) 0.0801(11) 0.0337(7) 0.000 0.0029(5) 0.000
C1 0.046(4) 0.081(6) 0.044(4) 0.010(4) 0.006(3) 0.005(4)
C2 0.063(6) 0.077(8) 0.049(6) 0.000 0.007(5) 0.000
C3 0.054(4) 0.080(6) 0.041(3) 0.000(4) 0.006(3) 0.015(4)
C4 0.033(5) 0.144(12) 0.041(5) 0.000 0.009(4) 0.000
N1 0.074(4) 0.101(6) 0.064(4) 0.017(4) 0.019(3) 0.023(4)
N2 0.078(6) 0.087(8) 0.070(6) 0.000 -0.029(5) 0.000
N3 0.057(3) 0.080(5) 0.048(3) 0.009(3) 0.010(3) 0.012(3)
N4 0.051(5) 0.160(11) 0.048(5) 0.000 -0.009(4) 0.000
Ni1 0.0547(8) 0.0798(11) 0.0445(7) 0.0118(7) 0.0101(5) 0.0071(7)
N11 0.064(4) 0.080(5) 0.079(5) 0.028(4) 0.000(3) 0.009(4)
N12 0.077(4) 0.082(5) 0.060(4) 0.007(4) 0.023(3) -0.002(4)
C11 0.057(5) 0.118(9) 0.131(9) 0.055(8) 0.024(5) 0.027(5)
C12 0.099(8) 0.091(8) 0.120(9) 0.008(7) 0.060(7) 0.030(6)
C13 0.106(7) 0.090(7) 0.084(6) -0.016(6) 0.045(5) -0.016(6)
C14 0.095(7) 0.118(8) 0.055(5) 0.013(5) 0.004(4) -0.018(6)
C15 0.084(6) 0.106(8) 0.084(6) 0.020(6) -0.014(5) -0.007(6)
Ni2 0.0417(9) 0.0701(13) 0.0346(8) 0.000 0.0023(6) 0.000
N21A 0.049(8) 0.103(15) 0.104(17) 0.042(14) 0.012(9) 0.007(9)
C21A 0.062(8) 0.053(11) 0.056(16) -0.009(11) -0.006(7) 0.012(6)
N21B 0.054(7) 0.071(11) 0.049(9) 0.015(7) 0.011(5) 0.003(6)
C21B 0.082(16) 0.05(2) 0.013(14) 0.008(12) 0.010(9) -0.007(13)
C22 0.054(6) 0.087(9) 0.052(6) 0.000 0.009(4) 0.000
C23 0.068(5) 0.107(7) 0.078(5) -0.004(5) -0.006(4) 0.022(5)
O1 0.067(5) 0.101(7) 0.088(6) 0.000 -0.007(4) 0.000
O2 0.072(5) 0.106(7) 0.078(5) 0.000 -0.004(4) 0.000
O3 0.082(7) 0.219(14) 0.104(8) 0.000 0.003(6) 0.000
O4 0.059(3) 0.076(4) 0.076(3) -0.001(3) 0.010(2) -0.002(3)
O5 0.079(5) 0.101(7) 0.085(6) 0.000 -0.011(4) 0.000

_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
Fe1 C4 1.903(10) . ?
Fe1 C3 1.915(8) . ?
Fe1 C3 1.915(8) 6 ?
Fe1 C1 1.947(9) 6 ?
Fe1 C1 1.947(9) . ?
Fe1 C2 1.953(11) . ?
C1 N1 1.148(10) . ?
C2 N2 1.150(13) . ?
C3 N3 1.177(9) . ?
C4 N4 1.142(13) . ?
N3 Ni1 2.033(7) . ?
N4 Ni2 2.072(9) . ?
Ni1 N3 2.033(7) 7 ?
Ni1 N12 2.076(6) 7 ?
Ni1 N12 2.076(6) . ?
Ni1 N11 2.078(6) 7 ?
Ni1 N11 2.078(6) . ?
N11 C15 1.469(12) 7 ?
N11 C11 1.486(11) . ?
N12 C13 1.468(11) . ?
N12 C14 1.507(12) . ?
C11 C12 1.525(15) . ?
C12 C13 1.493(15) . ?
C14 C15 1.488(14) . ?
C15 N11 1.469(12) 7 ?
Ni2 N21B 2.054(16) 2 ?
Ni2 N21B 2.054(16) . ?
Ni2 N21B 2.054(16) 5 ?
Ni2 N21B 2.054(16) 6 ?
Ni2 N4 2.072(9) 5 ?
Ni2 C21A 2.18(4) 2 ?
Ni2 C21A 2.18(4) 5 ?
Ni2 C21A 2.18(4) . ?
Ni2 C21A 2.18(4) 6 ?
N21A C21A 1.38(3) . ?
N21A C23 1.61(2) . ?
C21A C22 1.440(16) . ?
C21A C21A 1.99(4) 6 ?
N21B C23 1.520(16) . ?
N21B C21B 1.58(4) . ?
C21B C22 1.56(4) . ?
C22 C21A 1.440(16) 6 ?
C22 C21B 1.56(4) 6 ?
C23 C23 1.550(17) 2 ?

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
C4 Fe1 C3 90.4(3) . . ?
C4 Fe1 C3 90.4(3) . 6 ?
C3 Fe1 C3 82.8(4) . 6 ?
C4 Fe1 C1 85.5(3) . 6 ?
C3 Fe1 C1 170.5(3) . 6 ?
C3 Fe1 C1 88.7(3) 6 6 ?
C4 Fe1 C1 85.5(3) . . ?
C3 Fe1 C1 88.7(3) . . ?
C3 Fe1 C1 170.5(3) 6 . ?
C1 Fe1 C1 99.4(4) 6 . ?
C4 Fe1 C2 176.0(4) . . ?
C3 Fe1 C2 92.6(3) . . ?
C3 Fe1 C2 92.6(3) 6 . ?
C1 Fe1 C2 91.9(3) 6 . ?
C1 Fe1 C2 91.9(3) . . ?
N1 C1 Fe1 172.0(6) . . ?
N2 C2 Fe1 178.8(10) . . ?
N3 C3 Fe1 178.0(7) . . ?
N4 C4 Fe1 175.7(9) . . ?
C3 N3 Ni1 169.8(6) . . ?
C4 N4 Ni2 152.9(8) . . ?
N3 Ni1 N3 180.0 . 7 ?
N3 Ni1 N12 88.6(3) . 7 ?
N3 Ni1 N12 91.4(2) 7 7 ?
N3 Ni1 N12 91.4(3) . . ?
N3 Ni1 N12 88.6(2) 7 . ?
N12 Ni1 N12 180.0 7 . ?
N3 Ni1 N11 90.3(3) . 7 ?
N3 Ni1 N11 89.7(3) 7 7 ?
N12 Ni1 N11 94.7(3) 7 7 ?
N12 Ni1 N11 85.3(3) . 7 ?
N3 Ni1 N11 89.7(3) . . ?
N3 Ni1 N11 90.3(3) 7 . ?
N12 Ni1 N11 85.3(3) 7 . ?
N12 Ni1 N11 94.7(3) . . ?
N11 Ni1 N11 180.0 7 . ?
C15 N11 C11 113.5(8) 7 . ?
C15 N11 Ni1 105.5(6) 7 . ?
C11 N11 Ni1 114.9(5) . . ?
C13 N12 C14 114.8(7) . . ?
C13 N12 Ni1 116.0(6) . . ?
C14 N12 Ni1 103.8(5) . . ?
N11 C11 C12 111.7(8) . . ?
C13 C12 C11 117.0(8) . . ?
N12 C13 C12 111.5(7) . . ?
C15 C14 N12 109.0(7) . . ?
N11 C15 C14 107.6(8) 7 . ?
N21B Ni2 N21B 67.1(7) 2 . ?
N21B Ni2 N21B 112.9(7) 2 5 ?
N21B Ni2 N21B 180.000(1) . 5 ?
N21B Ni2 N21B 180.0 2 6 ?
N21B Ni2 N21B 112.9(7) . 6 ?
N21B Ni2 N21B 67.1(7) 5 6 ?
N21B Ni2 N4 81.2(3) 2 5 ?
N21B Ni2 N4 98.8(3) . 5 ?
N21B Ni2 N4 81.2(3) 5 5 ?
N21B Ni2 N4 98.8(3) 6 5 ?
N21B Ni2 N4 98.8(3) 2 . ?
N21B Ni2 N4 81.2(3) . . ?
N21B Ni2 N4 98.8(3) 5 . ?
N21B Ni2 N4 81.2(3) 6 . ?
N4 Ni2 N4 180.0 5 . ?
N21B Ni2 C21A 32.8(5) 2 2 ?
N21B Ni2 C21A 94.4(5) . 2 ?
N21B Ni2 C21A 85.6(5) 5 2 ?
N21B Ni2 C21A 147.2(5) 6 2 ?
N4 Ni2 C21A 94.4(4) 5 2 ?
N4 Ni2 C21A 85.6(4) . 2 ?
N21B Ni2 C21A 85.6(5) 2 5 ?
N21B Ni2 C21A 147.2(5) . 5 ?
N21B Ni2 C21A 32.8(5) 5 5 ?
N21B Ni2 C21A 94.4(5) 6 5 ?
N4 Ni2 C21A 94.4(4) 5 5 ?
N4 Ni2 C21A 85.6(4) . 5 ?
C21A Ni2 C21A 54.5(7) 2 5 ?
N21B Ni2 C21A 94.4(5) 2 . ?
N21B Ni2 C21A 32.8(5) . . ?
N21B Ni2 C21A 147.2(5) 5 . ?
N21B Ni2 C21A 85.6(5) 6 . ?
N4 Ni2 C21A 85.6(4) 5 . ?
N4 Ni2 C21A 94.4(4) . . ?
C21A Ni2 C21A 125.5(7) 2 . ?
C21A Ni2 C21A 180.000(1) 5 . ?
N21B Ni2 C21A 147.2(5) 2 6 ?
N21B Ni2 C21A 85.6(5) . 6 ?
N21B Ni2 C21A 94.4(5) 5 6 ?
N21B Ni2 C21A 32.8(5) 6 6 ?
N4 Ni2 C21A 85.6(4) 5 6 ?
N4 Ni2 C21A 94.4(4) . 6 ?
C21A Ni2 C21A 180.000(2) 2 6 ?
C21A Ni2 C21A 125.5(7) 5 6 ?
C21A Ni2 C21A 54.5(7) . 6 ?
C21A N21A C23 107.1(16) . . ?
N21A C21A C22 116(2) . . ?
N21A C21A C21A 155.6(8) . 6 ?
C22 C21A C21A 46.2(14) . 6 ?
N21A C21A Ni2 114.5(18) . . ?
C22 C21A Ni2 100.6(16) . . ?
C21A C21A Ni2 62.8(3) 6 . ?
C23 N21B C21B 105.7(18) . . ?
C23 N21B Ni2 125.7(8) . . ?
C21B N21B Ni2 108.4(19) . . ?
C22 C21B N21B 101(3) . . ?
C21A C22 C21A 88(3) 6 . ?
C21A C22 C21B 30.2(7) 6 6 ?
C21A C22 C21B 115(3) . 6 ?
C21A C22 C21B 115(3) 6 . ?
C21A C22 C21B 30.2(7) . . ?
C21B C22 C21B 136(3) 6 . ?
N21B C23 C23 97.0(7) . 2 ?
N21B C23 N21A 38.6(7) . . ?
C23 C23 N21A 128.8(10) 2 . ?

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
C4 Fe1 C1 N1 -53(5) . . . . ?
C3 Fe1 C1 N1 37(5) . . . . ?
C3 Fe1 C1 N1 11(6) 6 . . . ?
C1 Fe1 C1 N1 -138(5) 6 . . . ?
C2 Fe1 C1 N1 130(5) . . . . ?
C4 Fe1 C2 N2 0.00(5) . . . . ?
C3 Fe1 C2 N2 138.5(2) . . . . ?
C3 Fe1 C2 N2 -138.5(2) 6 . . . ?
C1 Fe1 C2 N2 -49.7(2) 6 . . . ?
C1 Fe1 C2 N2 49.7(2) . . . . ?
C4 Fe1 C3 N3 -40(17) . . . . ?
C3 Fe1 C3 N3 50(17) 6 . . . ?
C1 Fe1 C3 N3 23(18) 6 . . . ?
C1 Fe1 C3 N3 -126(17) . . . . ?
C2 Fe1 C3 N3 142(17) . . . . ?
C3 Fe1 C4 N4 -138.6(2) . . . . ?
C3 Fe1 C4 N4 138.6(2) 6 . . . ?
C1 Fe1 C4 N4 49.9(2) 6 . . . ?
C1 Fe1 C4 N4 -49.9(2) . . . . ?
C2 Fe1 C4 N4 0.000(6) . . . . ?
Fe1 C3 N3 Ni1 148(15) . . . . ?
Fe1 C4 N4 Ni2 0.000(5) . . . . ?
C3 N3 Ni1 N3 119(26) . . . 7 ?
C3 N3 Ni1 N12 18(3) . . . 7 ?
C3 N3 Ni1 N12 -162(3) . . . . ?
C3 N3 Ni1 N11 -77(3) . . . 7 ?
C3 N3 Ni1 N11 103(3) . . . . ?
N3 Ni1 N11 C15 -104.7(5) . . . 7 ?
N3 Ni1 N11 C15 75.3(5) 7 . . 7 ?
N12 Ni1 N11 C15 -16.0(6) 7 . . 7 ?
N12 Ni1 N11 C15 164.0(6) . . . 7 ?
N11 Ni1 N11 C15 110(100) 7 . . 7 ?
N3 Ni1 N11 C11 129.6(8) . . . . ?
N3 Ni1 N11 C11 -50.4(8) 7 . . . ?
N12 Ni1 N11 C11 -141.8(8) 7 . . . ?
N12 Ni1 N11 C11 38.2(8) . . . . ?
N11 Ni1 N11 C11 -16(100) 7 . . . ?
N3 Ni1 N12 C13 -128.4(7) . . . . ?
N3 Ni1 N12 C13 51.6(7) 7 . . . ?
N12 Ni1 N12 C13 -2(69) 7 . . . ?
N11 Ni1 N12 C13 141.4(7) 7 . . . ?
N11 Ni1 N12 C13 -38.6(7) . . . . ?
N3 Ni1 N12 C14 104.7(5) . . . . ?
N3 Ni1 N12 C14 -75.3(5) 7 . . . ?
N12 Ni1 N12 C14 -129(68) 7 . . . ?
N11 Ni1 N12 C14 14.5(5) 7 . . . ?
N11 Ni1 N12 C14 -165.5(5) . . . . ?
C15 N11 C11 C12 -176.7(8) 7 . . . ?
Ni1 N11 C11 C12 -55.2(10) . . . . ?
N11 C11 C12 C13 72.1(11) . . . . ?
C14 N12 C13 C12 177.0(9) . . . . ?
Ni1 N12 C13 C12 55.8(10) . . . . ?
C11 C12 C13 N12 -71.9(11) . . . . ?
C13 N12 C14 C15 -171.0(9) . . . . ?
Ni1 N12 C14 C15 -43.4(9) . . . . ?
N12 C14 C15 N11 60.9(11) . . . 7 ?
C4 N4 Ni2 N21B 57.5(4) . . . 2 ?
C4 N4 Ni2 N21B 122.5(4) . . . . ?
C4 N4 Ni2 N21B -57.5(4) . . . 5 ?
C4 N4 Ni2 N21B -122.5(4) . . . 6 ?
C4 N4 Ni2 N4 180.00(5) . . . 5 ?
C4 N4 Ni2 C21A 27.3(3) . . . 2 ?
C4 N4 Ni2 C21A -27.3(3) . . . 5 ?
C4 N4 Ni2 C21A 152.7(3) . . . . ?
C4 N4 Ni2 C21A -152.7(3) . . . 6 ?
C23 N21A C21A C22 -169.5(17) . . . . ?
C23 N21A C21A C21A -130(3) . . . 6 ?
C23 N21A C21A Ni2 -52.6(13) . . . . ?
N21B Ni2 C21A N21A 38.4(10) 2 . . . ?
N21B Ni2 C21A N21A 5.6(9) . . . . ?
N21B Ni2 C21A N21A -174.4(9) 5 . . . ?
N21B Ni2 C21A N21A -141.6(10) 6 . . . ?
N4 Ni2 C21A N21A 119.2(10) 5 . . . ?
N4 Ni2 C21A N21A -60.8(10) . . . . ?
C21A Ni2 C21A N21A 27.0(9) 2 . . . ?
C21A Ni2 C21A N21A -67(17) 5 . . . ?
C21A Ni2 C21A N21A -153.0(9) 6 . . . ?
N21B Ni2 C21A C22 164.2(8) 2 . . . ?
N21B Ni2 C21A C22 131.3(12) . . . . ?
N21B Ni2 C21A C22 -48.7(12) 5 . . . ?
N21B Ni2 C21A C22 -15.8(8) 6 . . . ?
N4 Ni2 C21A C22 -115.0(8) 5 . . . ?
N4 Ni2 C21A C22 65.0(8) . . . . ?
C21A Ni2 C21A C22 152.7(9) 2 . . . ?
C21A Ni2 C21A C22 59(6) 5 . . . ?
C21A Ni2 C21A C22 -27.3(9) 6 . . . ?
N21B Ni2 C21A C21A -168.6(4) 2 . . 6 ?
N21B Ni2 C21A C21A 158.6(7) . . . 6 ?
N21B Ni2 C21A C21A -21.4(7) 5 . . 6 ?
N21B Ni2 C21A C21A 11.4(4) 6 . . 6 ?
N4 Ni2 C21A C21A -87.8(2) 5 . . 6 ?
N4 Ni2 C21A C21A 92.2(2) . . . 6 ?
C21A Ni2 C21A C21A 180.000(2) 2 . . 6 ?
C21A Ni2 C21A C21A 86(24) 5 . . 6 ?
N21B Ni2 N21B C23 -19.5(6) 2 . . . ?
N21B Ni2 N21B C23 136.4(11) 5 . . . ?
N21B Ni2 N21B C23 160.5(6) 6 . . . ?
N4 Ni2 N21B C23 57.0(10) 5 . . . ?
N4 Ni2 N21B C23 -123.0(10) . . . . ?
C21A Ni2 N21B C23 -38.2(10) 2 . . . ?
C21A Ni2 N21B C23 -55.5(14) 5 . . . ?
C21A Ni2 N21B C23 124.5(14) . . . . ?
C21A Ni2 N21B C23 141.8(10) 6 . . . ?
N21B Ni2 N21B C21B -145.7(14) 2 . . . ?
N21B Ni2 N21B C21B 10.2(12) 5 . . . ?
N21B Ni2 N21B C21B 34.3(14) 6 . . . ?
N4 Ni2 N21B C21B -69.2(12) 5 . . . ?
N4 Ni2 N21B C21B 110.8(12) . . . . ?
C21A Ni2 N21B C21B -164.3(13) 2 . . . ?
C21A Ni2 N21B C21B 178.3(13) 5 . . . ?
C21A Ni2 N21B C21B -1.7(13) . . . . ?
C21A Ni2 N21B C21B 15.7(13) 6 . . . ?
C23 N21B C21B C22 -178.0(14) . . . . ?
Ni2 N21B C21B C22 -40.9(18) . . . . ?
N21A C21A C22 C21A 158.8(16) . . . 6 ?
Ni2 C21A C22 C21A 34.4(10) . . . 6 ?
N21A C21A C22 C21B 172.5(18) . . . 6 ?
C21A C21A C22 C21B 13.7(13) 6 . . 6 ?
Ni2 C21A C22 C21B 48.1(17) . . . 6 ?
N21A C21A C22 C21B -47(3) . . . . ?
C21A C21A C22 C21B 155(2) 6 . . . ?
Ni2 C21A C22 C21B -171(3) . . . . ?
N21B C21B C22 C21A 62.4(18) . . . 6 ?
N21B C21B C22 C21A 34.4(18) . . . . ?
N21B C21B C22 C21B 89(3) . . . 6 ?
C21B N21B C23 C23 175.3(16) . . . 2 ?
Ni2 N21B C23 C23 48.0(11) . . . 2 ?
C21B N21B C23 N21A -35.7(16) . . . . ?
Ni2 N21B C23 N21A -162.9(18) . . . . ?
C21A N21A C23 N21B 41.3(15) . . . . ?
C21A N21A C23 C23 82.2(19) . . . 2 ?

_diffrn_measured_fraction_theta_max    0.493
_diffrn_reflns_theta_full              25.97
_diffrn_measured_fraction_theta_full   0.493
_refine_diff_density_max    0.580
_refine_diff_density_min   -0.754
_refine_diff_density_rms    0.118

#===END