# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Tong, Ming-Liang'
_publ_contact_author_email       tongml@mail.sysu.edu.cn

_publ_section_title              
;
Two new 1,2,4,5-cyclohexanetetracarboxylate-bridged
frameworks with metal hydroxide subunits. Synthesis, structures,
magnetism and adsorption
;
loop_
_publ_author_name
'Yong-Cong Ou'
'Jing Wang'
'Ji-Dong Leng'
'Zhuojia Lin'
'Ming-Liang Tong'

# Attachment '- CIF.cif'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 789365'
#TrackingRef '- CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H42 Mn1.1 Ni3.9 O30'
_chemical_formula_weight         1051.94

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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)/c

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

_cell_length_a                   10.1991(13)
_cell_length_b                   6.5786(8)
_cell_length_c                   24.405(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.011(4)
_cell_angle_gamma                90.00
_cell_volume                     1636.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1077
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7530
_exptl_absorpt_correction_T_max  0.8985
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10365
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3516
_reflns_number_gt                2994
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0321P)^2^+3.2739P] 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         3516
_refine_ls_number_parameters     250
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.002
_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 0.47755(4) 0.59819(6) 0.327399(16) 0.00726(11) Uani 0.78 1 d P . .
Ni2 Ni 1.0000 0.0000 0.5000 0.01129(14) Uani 0.78 2 d SP . .
Ni3 Ni 0.84770(4) -0.49849(6) 0.500263(16) 0.00819(11) Uani 0.78 1 d P . .
Mn1 Mn 0.47755(4) 0.59819(6) 0.327399(16) 0.00726(11) Uani 0.22 1 d P . .
Mn2 Mn 1.0000 0.0000 0.5000 0.01129(14) Uani 0.22 2 d SP . .
Mn3 Mn 0.84770(4) -0.49849(6) 0.500263(16) 0.00819(11) Uani 0.22 1 d P . .
O1 O 0.7818(2) 0.7067(4) 0.32919(11) 0.0185(5) Uani 1 1 d . . .
O2 O 0.6476(2) 0.4433(4) 0.31626(9) 0.0121(5) Uani 1 1 d . . .
O3 O 0.8348(2) 0.3929(4) 0.42228(9) 0.0133(5) Uani 1 1 d . . .
O4 O 0.8498(2) 0.0567(3) 0.43686(9) 0.0114(5) Uani 1 1 d . . .
O5 O 1.1463(2) 0.0428(3) 0.43974(9) 0.0121(5) Uani 1 1 d . . .
O6 O 1.1641(2) 0.3762(3) 0.42316(9) 0.0140(5) Uani 1 1 d . . .
O7 O 1.3605(2) 0.3435(3) 0.31808(9) 0.0111(5) Uani 1 1 d . . .
O8 O 1.2698(2) 0.6451(3) 0.32445(9) 0.0127(5) Uani 1 1 d . . .
O9 O 0.9980(2) -0.3070(3) 0.47669(9) 0.0106(5) Uani 1 1 d . . .
H9O H 0.9907 -0.3070 0.4419 0.013 Uiso 1 1 d R . .
O1W O 0.4894(2) 0.5462(3) 0.41160(9) 0.0125(5) Uani 1 1 d . . .
H1WA H 0.4882 0.4197 0.4186 0.015 Uiso 1 1 d R . .
H1WB H 0.5560 0.6010 0.4275 0.015 Uiso 1 1 d R . .
O2W O 0.5598(2) 0.8794(4) 0.34588(9) 0.0141(5) Uani 1 1 d . . .
H2WA H 0.5416 0.9530 0.3180 0.017 Uiso 1 1 d R . .
H2WB H 0.6411 0.8509 0.3462 0.017 Uiso 1 1 d R . .
O3W O 0.4716(2) 0.6515(3) 0.24289(9) 0.0121(5) Uani 1 1 d . . .
H3WA H 0.4104 0.7311 0.2320 0.014 Uiso 1 1 d R . .
H3WB H 0.5442 0.6975 0.2321 0.014 Uiso 1 1 d R . .
O4W O 0.7038(2) -0.7157(4) 0.52603(9) 0.0142(5) Uani 1 1 d . . .
H4WA H 0.7489 -0.8078 0.5422 0.017 Uiso 1 1 d R . .
H4WB H 0.6576 -0.6513 0.5486 0.017 Uiso 1 1 d R . .
O5W O 0.6981(2) -0.2766(4) 0.47138(9) 0.0147(5) Uani 1 1 d . . .
H5WA H 0.7352 -0.1825 0.4538 0.018 Uiso 1 1 d R . .
H5WB H 0.6604 -0.2255 0.4987 0.018 Uiso 1 1 d R . .
O6W O 0.5063(3) 0.1513(4) 0.44394(10) 0.0220(6) Uani 1 1 d . . .
H6WA H 0.5817 0.1544 0.4599 0.026 Uiso 1 1 d R . .
H6WB H 0.5050 0.0672 0.4175 0.026 Uiso 1 1 d R . .
C1 C 0.8780(3) 0.3809(5) 0.31136(12) 0.0086(6) Uani 1 1 d . . .
H1 H 0.8727 0.3413 0.2718 0.010 Uiso 1 1 calc R . .
C2 C 0.8694(3) 0.1811(5) 0.34460(12) 0.0083(6) Uani 1 1 d . . .
H2 H 0.7909 0.1054 0.3298 0.010 Uiso 1 1 calc R . .
C3 C 0.9894(3) 0.0458(5) 0.33555(12) 0.0089(6) Uani 1 1 d . . .
H3A H 0.9856 -0.0042 0.2973 0.011 Uiso 1 1 calc R . .
H3B H 0.9853 -0.0739 0.3600 0.011 Uiso 1 1 calc R . .
C4 C 1.1219(3) 0.1556(5) 0.34648(12) 0.0083(6) Uani 1 1 d . . .
H4 H 1.1930 0.0633 0.3342 0.010 Uiso 1 1 calc R . .
C5 C 1.1262(3) 0.3497(5) 0.31155(12) 0.0081(6) Uani 1 1 d . . .
H5 H 1.1192 0.3054 0.2724 0.010 Uiso 1 1 calc R . .
C6 C 1.0096(3) 0.4907(5) 0.32066(12) 0.0089(6) Uani 1 1 d . . .
H6A H 1.0137 0.6076 0.2952 0.011 Uiso 1 1 calc R . .
H6B H 1.0155 0.5441 0.3586 0.011 Uiso 1 1 calc R . .
C7 C 0.7623(3) 0.5232(5) 0.32032(12) 0.0099(6) Uani 1 1 d . . .
C8 C 0.8494(3) 0.2151(5) 0.40592(12) 0.0090(6) Uani 1 1 d U . .
C9 C 1.1468(3) 0.1966(5) 0.40768(12) 0.0087(6) Uani 1 1 d . . .
C10 C 1.2568(3) 0.4556(5) 0.31916(12) 0.0090(6) Uani 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 0.0052(2) 0.0076(2) 0.0091(2) 0.00010(15) 0.00065(14) -0.00070(15)
Ni2 0.0129(3) 0.0096(3) 0.0115(3) 0.0006(2) 0.0010(2) -0.0002(2)
Ni3 0.0088(2) 0.0083(2) 0.0074(2) -0.00099(15) 0.00033(15) 0.00003(16)
Mn1 0.0052(2) 0.0076(2) 0.0091(2) 0.00010(15) 0.00065(14) -0.00070(15)
Mn2 0.0129(3) 0.0096(3) 0.0115(3) 0.0006(2) 0.0010(2) -0.0002(2)
Mn3 0.0088(2) 0.0083(2) 0.0074(2) -0.00099(15) 0.00033(15) 0.00003(16)
O1 0.0118(12) 0.0093(12) 0.0345(15) -0.0004(10) 0.0030(10) -0.0007(9)
O2 0.0057(11) 0.0139(12) 0.0165(11) -0.0020(9) -0.0002(9) -0.0005(9)
O3 0.0184(12) 0.0121(12) 0.0096(10) -0.0021(9) 0.0033(9) 0.0020(10)
O4 0.0127(11) 0.0108(11) 0.0108(11) 0.0018(8) 0.0018(9) -0.0029(9)
O5 0.0138(11) 0.0119(12) 0.0105(11) 0.0035(8) 0.0012(9) 0.0017(9)
O6 0.0212(13) 0.0102(11) 0.0104(11) 0.0003(9) -0.0019(9) -0.0043(10)
O7 0.0075(11) 0.0120(11) 0.0140(11) -0.0010(9) 0.0014(9) 0.0015(9)
O8 0.0083(11) 0.0109(11) 0.0189(12) 0.0011(9) 0.0020(9) -0.0012(9)
O9 0.0123(11) 0.0118(11) 0.0077(10) 0.0007(8) 0.0010(9) -0.0007(9)
O1W 0.0116(11) 0.0106(11) 0.0152(11) -0.0008(9) -0.0008(9) -0.0025(9)
O2W 0.0102(11) 0.0144(12) 0.0174(12) 0.0011(9) -0.0006(9) -0.0016(9)
O3W 0.0087(11) 0.0131(12) 0.0144(11) 0.0036(9) 0.0007(9) 0.0003(9)
O4W 0.0126(11) 0.0136(12) 0.0166(12) -0.0016(9) 0.0014(9) 0.0034(9)
O5W 0.0150(12) 0.0165(12) 0.0128(11) 0.0001(9) 0.0020(9) -0.0014(10)
O6W 0.0241(14) 0.0171(13) 0.0242(13) 0.0011(10) -0.0056(11) -0.0009(11)
C1 0.0079(15) 0.0089(15) 0.0088(14) -0.0008(11) 0.0004(11) 0.0005(12)
C2 0.0064(14) 0.0086(15) 0.0099(15) -0.0012(11) -0.0008(11) -0.0040(12)
C3 0.0103(15) 0.0072(14) 0.0093(14) -0.0012(11) -0.0003(12) -0.0006(12)
C4 0.0090(15) 0.0075(15) 0.0085(14) 0.0017(11) 0.0003(11) 0.0002(12)
C5 0.0058(14) 0.0104(15) 0.0082(14) -0.0017(11) 0.0005(11) -0.0024(12)
C6 0.0092(14) 0.0083(15) 0.0094(14) -0.0002(11) 0.0020(11) -0.0011(12)
C7 0.0084(15) 0.0119(16) 0.0093(14) 0.0018(11) 0.0000(11) 0.0009(12)
C8 0.0043(14) 0.0129(16) 0.0098(15) 0.0009(12) 0.0000(11) -0.0010(12)
C9 0.0038(14) 0.0132(16) 0.0091(14) 0.0001(12) -0.0006(11) -0.0005(12)
C10 0.0083(15) 0.0128(16) 0.0060(14) 0.0024(11) 0.0025(11) 0.0004(12)

_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 O2 2.038(2) . ?
Ni1 O7 2.065(2) 1_455 ?
Ni1 O2W 2.074(2) . ?
Ni1 O1W 2.083(2) . ?
Ni1 O3W 2.091(2) . ?
Ni1 O8 2.140(2) 1_455 ?
Ni1 C10 2.441(3) 1_455 ?
Ni2 O9 2.098(2) . ?
Ni2 O9 2.098(2) 3_756 ?
Ni2 O5 2.150(2) . ?
Ni2 O5 2.150(2) 3_756 ?
Ni2 O4 2.167(2) 3_756 ?
Ni2 O4 2.167(2) . ?
Ni3 O3 2.033(2) 1_545 ?
Ni3 O6 2.042(2) 3_756 ?
Ni3 O9 2.081(2) . ?
Ni3 O9 2.090(2) 3_746 ?
Ni3 O4W 2.158(2) . ?
Ni3 O5W 2.209(2) . ?
Ni3 Mn3 3.1073(9) 3_746 ?
O1 C7 1.242(4) . ?
O2 C7 1.283(4) . ?
O3 C8 1.247(4) . ?
O3 Mn3 2.033(2) 1_565 ?
O3 Ni3 2.033(2) 1_565 ?
O4 C8 1.286(4) . ?
O5 C9 1.279(4) . ?
O6 C9 1.251(4) . ?
O6 Mn3 2.042(2) 3_756 ?
O6 Ni3 2.042(2) 3_756 ?
O7 C10 1.290(4) . ?
O7 Mn1 2.065(2) 1_655 ?
O7 Ni1 2.065(2) 1_655 ?
O8 C10 1.260(4) . ?
O8 Mn1 2.140(2) 1_655 ?
O8 Ni1 2.140(2) 1_655 ?
O9 Mn3 2.090(2) 3_746 ?
O9 Ni3 2.090(2) 3_746 ?
O9 H9O 0.8502 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8501 . ?
O5W H5WA 0.8500 . ?
O5W H5WB 0.8500 . ?
O6W H6WA 0.8502 . ?
O6W H6WB 0.8496 . ?
C1 C7 1.527(4) . ?
C1 C6 1.534(4) . ?
C1 C2 1.549(4) . ?
C1 H1 1.0000 . ?
C2 C8 1.534(4) . ?
C2 C3 1.535(4) . ?
C2 H2 1.0000 . ?
C3 C4 1.546(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.530(4) . ?
C4 C5 1.537(4) . ?
C4 H4 1.0000 . ?
C5 C10 1.508(4) . ?
C5 C6 1.530(4) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C10 Mn1 2.441(3) 1_655 ?
C10 Ni1 2.441(3) 1_655 ?

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
O2 Ni1 O7 94.08(9) . 1_455 ?
O2 Ni1 O2W 97.77(9) . . ?
O7 Ni1 O2W 167.23(9) 1_455 . ?
O2 Ni1 O1W 91.69(9) . . ?
O7 Ni1 O1W 89.36(9) 1_455 . ?
O2W Ni1 O1W 85.57(9) . . ?
O2 Ni1 O3W 86.99(9) . . ?
O7 Ni1 O3W 91.76(9) 1_455 . ?
O2W Ni1 O3W 93.58(9) . . ?
O1W Ni1 O3W 178.33(9) . . ?
O2 Ni1 O8 156.05(9) . 1_455 ?
O7 Ni1 O8 62.96(9) 1_455 1_455 ?
O2W Ni1 O8 105.74(9) . 1_455 ?
O1W Ni1 O8 94.58(9) . 1_455 ?
O3W Ni1 O8 87.04(9) . 1_455 ?
O2 Ni1 C10 125.71(10) . 1_455 ?
O7 Ni1 C10 31.90(10) 1_455 1_455 ?
O2W Ni1 C10 136.52(10) . 1_455 ?
O1W Ni1 C10 92.27(9) . 1_455 ?
O3W Ni1 C10 89.34(9) . 1_455 ?
O8 Ni1 C10 31.05(10) 1_455 1_455 ?
O9 Ni2 O9 180.00(11) . 3_756 ?
O9 Ni2 O5 86.61(8) . . ?
O9 Ni2 O5 93.39(8) 3_756 . ?
O9 Ni2 O5 93.39(8) . 3_756 ?
O9 Ni2 O5 86.61(8) 3_756 3_756 ?
O5 Ni2 O5 180.000(1) . 3_756 ?
O9 Ni2 O4 91.54(8) . 3_756 ?
O9 Ni2 O4 88.46(8) 3_756 3_756 ?
O5 Ni2 O4 91.08(8) . 3_756 ?
O5 Ni2 O4 88.92(8) 3_756 3_756 ?
O9 Ni2 O4 88.46(8) . . ?
O9 Ni2 O4 91.54(8) 3_756 . ?
O5 Ni2 O4 88.92(8) . . ?
O5 Ni2 O4 91.08(8) 3_756 . ?
O4 Ni2 O4 180.000(1) 3_756 . ?
O3 Ni3 O6 172.46(10) 1_545 3_756 ?
O3 Ni3 O9 88.74(9) 1_545 . ?
O6 Ni3 O9 94.71(9) 3_756 . ?
O3 Ni3 O9 93.45(9) 1_545 3_746 ?
O6 Ni3 O9 93.60(9) 3_756 3_746 ?
O9 Ni3 O9 83.68(9) . 3_746 ?
O3 Ni3 O4W 91.02(9) 1_545 . ?
O6 Ni3 O4W 86.08(9) 3_756 . ?
O9 Ni3 O4W 175.35(9) . . ?
O9 Ni3 O4W 91.70(9) 3_746 . ?
O3 Ni3 O5W 84.96(9) 1_545 . ?
O6 Ni3 O5W 88.26(9) 3_756 . ?
O9 Ni3 O5W 91.09(9) . . ?
O9 Ni3 O5W 174.57(9) 3_746 . ?
O4W Ni3 O5W 93.52(9) . . ?
O3 Ni3 Mn3 91.48(7) 1_545 3_746 ?
O6 Ni3 Mn3 95.58(7) 3_756 3_746 ?
O9 Ni3 Mn3 41.95(6) . 3_746 ?
O9 Ni3 Mn3 41.73(6) 3_746 3_746 ?
O4W Ni3 Mn3 133.42(7) . 3_746 ?
O5W Ni3 Mn3 133.03(7) . 3_746 ?
C7 O2 Ni1 124.2(2) . . ?
C8 O3 Mn3 128.7(2) . 1_565 ?
C8 O3 Ni3 128.7(2) . 1_565 ?
Mn3 O3 Ni3 0.000(8) 1_565 1_565 ?
C8 O4 Ni2 123.0(2) . . ?
C9 O5 Ni2 122.7(2) . . ?
C9 O6 Mn3 129.5(2) . 3_756 ?
C9 O6 Ni3 129.5(2) . 3_756 ?
Mn3 O6 Ni3 0.00(2) 3_756 3_756 ?
C10 O7 Mn1 90.32(19) . 1_655 ?
C10 O7 Ni1 90.32(19) . 1_655 ?
Mn1 O7 Ni1 0.00(3) 1_655 1_655 ?
C10 O8 Mn1 87.78(18) . 1_655 ?
C10 O8 Ni1 87.78(18) . 1_655 ?
Mn1 O8 Ni1 0.00(2) 1_655 1_655 ?
Ni3 O9 Mn3 96.32(9) . 3_746 ?
Ni3 O9 Ni3 96.32(9) . 3_746 ?
Mn3 O9 Ni3 0.00(3) 3_746 3_746 ?
Ni3 O9 Ni2 120.53(10) . . ?
Mn3 O9 Ni2 121.08(11) 3_746 . ?
Ni3 O9 Ni2 121.08(11) 3_746 . ?
Ni3 O9 H9O 103.7 . . ?
Mn3 O9 H9O 107.9 3_746 . ?
Ni3 O9 H9O 107.9 3_746 . ?
Ni2 O9 H9O 105.7 . . ?
Ni1 O1W H1WA 111.0 . . ?
Ni1 O1W H1WB 113.5 . . ?
H1WA O1W H1WB 109.9 . . ?
Ni1 O2W H2WA 105.0 . . ?
Ni1 O2W H2WB 101.1 . . ?
H2WA O2W H2WB 108.6 . . ?
Ni1 O3W H3WA 114.0 . . ?
Ni1 O3W H3WB 111.7 . . ?
H3WA O3W H3WB 108.8 . . ?
Ni3 O4W H4WA 104.2 . . ?
Ni3 O4W H4WB 104.9 . . ?
H4WA O4W H4WB 111.0 . . ?
Ni3 O5W H5WA 109.1 . . ?
Ni3 O5W H5WB 109.7 . . ?
H5WA O5W H5WB 109.3 . . ?
H6WA O6W H6WB 110.7 . . ?
C7 C1 C6 111.5(3) . . ?
C7 C1 C2 112.8(2) . . ?
C6 C1 C2 112.8(3) . . ?
C7 C1 H1 106.4 . . ?
C6 C1 H1 106.4 . . ?
C2 C1 H1 106.4 . . ?
C8 C2 C3 111.0(3) . . ?
C8 C2 C1 113.5(2) . . ?
C3 C2 C1 110.9(2) . . ?
C8 C2 H2 107.0 . . ?
C3 C2 H2 107.0 . . ?
C1 C2 H2 107.0 . . ?
C2 C3 C4 113.6(2) . . ?
C2 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C9 C4 C5 112.8(3) . . ?
C9 C4 C3 111.4(2) . . ?
C5 C4 C3 109.5(2) . . ?
C9 C4 H4 107.6 . . ?
C5 C4 H4 107.6 . . ?
C3 C4 H4 107.6 . . ?
C10 C5 C6 112.9(3) . . ?
C10 C5 C4 111.0(3) . . ?
C6 C5 C4 112.7(2) . . ?
C10 C5 H5 106.6 . . ?
C6 C5 H5 106.6 . . ?
C4 C5 H5 106.6 . . ?
C5 C6 C1 112.0(3) . . ?
C5 C6 H6A 109.2 . . ?
C1 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O1 C7 O2 123.5(3) . . ?
O1 C7 C1 120.1(3) . . ?
O2 C7 C1 116.4(3) . . ?
O3 C8 O4 124.7(3) . . ?
O3 C8 C2 118.1(3) . . ?
O4 C8 C2 117.2(3) . . ?
O6 C9 O5 124.5(3) . . ?
O6 C9 C4 118.5(3) . . ?
O5 C9 C4 117.0(3) . . ?
O8 C10 O7 118.9(3) . . ?
O8 C10 C5 124.0(3) . . ?
O7 C10 C5 117.0(3) . . ?
O8 C10 Mn1 61.17(16) . 1_655 ?
O7 C10 Mn1 57.77(16) . 1_655 ?
C5 C10 Mn1 174.5(2) . 1_655 ?
O8 C10 Ni1 61.17(16) . 1_655 ?
O7 C10 Ni1 57.77(16) . 1_655 ?
C5 C10 Ni1 174.5(2) . 1_655 ?
Mn1 C10 Ni1 0.00(2) 1_655 1_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O6W 0.85 1.88 2.719(3) 170.1 .
O1W H1WB O5W 0.85 1.95 2.793(3) 173.6 1_565
O2W H2WA O3W 0.85 1.98 2.820(3) 169.7 2_655
O2W H2WB O1 0.85 1.78 2.578(3) 155.3 .
O3W H3WA O2 0.85 1.91 2.669(3) 148.4 2_655
O3W H3WB O7 0.85 1.86 2.631(3) 150.5 2_755
O4W H4WA O5 0.85 1.92 2.752(3) 165.4 3_746
O4W H4WB O1W 0.85 1.94 2.766(3) 163.1 3_656
O5W H5WA O4 0.85 2.01 2.829(3) 161.0 .
O5W H5WB O6W 0.85 2.29 3.098(4) 158.1 3_656
O6W H6WA O4W 0.85 2.18 2.925(3) 146.5 1_565
O6W H6WB O2W 0.85 2.23 3.053(3) 163.6 1_545

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.121

#=================================================END

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 789366'
#TrackingRef '- CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H56 N4 Ni4 O32'
_chemical_formula_weight         1279.68

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   C2/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                   22.1211(12)
_cell_length_b                   17.5536(10)
_cell_length_c                   7.0480(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.060(2)
_cell_angle_gamma                90.00
_cell_volume                     2716.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1324
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Rigaku R-AXIS SPIDER IP'
_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            7147
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.00
_reflns_number_total             2938
_reflns_number_gt                2548
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_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.
;

_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^)+(0.0857P)^2^+12.1037P] 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         2938
_refine_ls_number_parameters     189
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1637
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.259
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.24423(3) 0.0000 0.46905(10) 0.0168(2) Uani 1 2 d S . .
Ni1 Ni 0.11447(3) 0.0000 0.70499(11) 0.0205(2) Uani 1 2 d S . .
O1W O 0.0792(3) 0.0000 0.9667(8) 0.0485(14) Uani 1 2 d S A .
H1W H 0.0973 -0.0334 1.0403 0.058 Uiso 1 1 d RD . .
O1 O 0.14990(18) 0.0000 0.4517(6) 0.0194(8) Uani 1 2 d S A .
H1O H 0.1360 -0.0381 0.3857 0.023 Uiso 0.50 1 d PR . .
O2 O 0.16783(15) -0.0873(2) 0.8081(5) 0.0357(8) Uani 1 1 d . A .
O3 O 0.25393(15) -0.08285(18) 0.6725(5) 0.0330(8) Uani 1 1 d . A .
O4 O 0.24003(14) -0.08344(17) 1.2586(5) 0.0278(7) Uani 1 1 d . . .
O5 O 0.14284(15) -0.11886(18) 1.2431(5) 0.0325(8) Uani 1 1 d . . .
H5O H 0.1226 -0.1600 1.2282 0.039 Uiso 1 1 d R . .
C1 C 0.2487(2) -0.1720(2) 0.9207(6) 0.0220(8) Uani 1 1 d . . .
H1 H 0.2887 -0.1536 0.9861 0.026 Uiso 1 1 calc R . .
C2 C 0.20876(18) -0.1940(2) 1.0742(6) 0.0206(8) Uani 1 1 d . . .
H2 H 0.1689 -0.2132 1.0098 0.025 Uiso 1 1 calc R . .
C3 C 0.2393(2) -0.2577(2) 1.2010(6) 0.0237(8) Uani 1 1 d . . .
H3A H 0.2126 -0.2724 1.2979 0.028 Uiso 1 1 calc R . .
H3B H 0.2783 -0.2390 1.2689 0.028 Uiso 1 1 calc R . .
C4 C 0.22078(19) -0.1085(2) 0.7896(6) 0.0208(8) Uani 1 1 d . . .
C5 C 0.1966(2) -0.1265(2) 1.2011(6) 0.0230(8) Uani 1 1 d . . .
O6 O 0.04692(14) 0.07676(17) 0.5904(5) 0.0259(7) Uani 0.50 1 d P A 1
N1 N 0.04692(14) 0.07676(17) 0.5904(5) 0.0259(7) Uani 0.50 1 d PD . 2
C6 C 0.0000 0.0433(3) 0.5000 0.0216(11) Uani 1 2 d SD . 2
C7 C 0.0474(4) 0.1539(5) 0.5898(18) 0.047(3) Uani 0.50 1 d PD . 2
H7 H 0.0816 0.1801 0.6535 0.057 Uiso 0.50 1 calc PR . 2
C8 C 0.0000 0.1944(7) 0.5000 0.063(6) Uani 0.50 2 d SPD . 2
H8 H 0.0000 0.2485 0.5000 0.075 Uiso 0.50 2 calc SPR . 2
N2 N 0.3382(2) 0.0000 0.4756(8) 0.0262(11) Uani 1 2 d S . .
C9 C 0.3693(2) 0.0645(3) 0.4806(11) 0.0506(16) Uani 1 1 d . . .
H9 H 0.3475 0.1112 0.4767 0.061 Uiso 1 1 calc R . .
C10 C 0.4328(3) 0.0670(3) 0.4914(14) 0.061(2) Uani 1 1 d . . .
H10 H 0.4532 0.1148 0.4953 0.073 Uiso 1 1 calc R . .
C11 C 0.4663(3) 0.0000 0.4966(12) 0.0357(15) Uani 1 2 d S . .
O2W O 0.3422(5) 0.0000 1.0017(14) 0.101(3) Uani 1 2 d S . .
O3W O 0.4121(6) 0.1369(8) 1.015(2) 0.094(4) Uiso 0.50 1 d P . .
O4W O 0.0818(7) -0.2577(8) 1.296(2) 0.102(4) Uiso 0.50 1 d P . .
O4W' O 0.0441(15) -0.2138(19) 1.160(5) 0.115(10) Uiso 0.25 1 d P . .
O5W O 0.0882(12) -0.2433(13) 1.686(5) 0.176(9) Uiso 0.50 1 d P . .
O6W O 0.478(4) 0.0000 0.984(16) 0.35(4) Uiso 0.50 2 d SP . .

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
Ni2 0.0221(4) 0.0141(4) 0.0146(4) 0.000 0.0031(3) 0.000
Ni1 0.0223(4) 0.0232(4) 0.0157(4) 0.000 0.0010(3) 0.000
O1W 0.047(3) 0.069(4) 0.031(3) 0.000 0.009(2) 0.000
O1 0.029(2) 0.0144(17) 0.014(2) 0.000 0.0012(15) 0.000
O2 0.0317(17) 0.047(2) 0.0296(19) 0.0220(15) 0.0077(13) 0.0121(14)
O3 0.0335(17) 0.0314(16) 0.036(2) 0.0162(14) 0.0100(14) 0.0084(13)
O4 0.0306(16) 0.0263(15) 0.0271(17) -0.0098(13) 0.0059(12) 0.0011(12)
O5 0.0332(17) 0.0269(16) 0.040(2) -0.0140(14) 0.0131(14) -0.0078(13)
C1 0.037(2) 0.0147(17) 0.0146(19) 0.0025(14) 0.0037(16) 0.0057(15)
C2 0.029(2) 0.0168(17) 0.016(2) -0.0005(15) 0.0033(15) -0.0001(15)
C3 0.041(2) 0.0174(18) 0.0130(19) 0.0018(15) 0.0052(16) 0.0055(16)
C4 0.030(2) 0.0146(17) 0.017(2) 0.0007(14) 0.0006(15) 0.0007(15)
C5 0.036(2) 0.0156(17) 0.017(2) 0.0003(15) 0.0018(16) 0.0006(15)
O6 0.0260(16) 0.0193(15) 0.032(2) -0.0031(13) 0.0012(14) -0.0009(12)
N1 0.0260(16) 0.0193(15) 0.032(2) -0.0031(13) 0.0012(14) -0.0009(12)
C6 0.022(3) 0.020(3) 0.024(3) 0.000 0.008(2) 0.000
C7 0.046(6) 0.033(5) 0.061(8) -0.006(5) 0.001(5) -0.001(4)
C8 0.047(10) 0.029(8) 0.113(19) 0.000 0.014(10) 0.000
N2 0.028(3) 0.025(2) 0.026(3) 0.000 0.004(2) 0.000
C9 0.031(3) 0.030(3) 0.092(5) -0.004(3) 0.010(3) 0.002(2)
C10 0.034(3) 0.028(3) 0.120(7) -0.007(3) 0.010(3) -0.004(2)
C11 0.030(4) 0.031(3) 0.045(5) 0.000 0.003(3) 0.000
O2W 0.146(9) 0.091(6) 0.059(6) 0.000 -0.017(5) 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
Ni2 O3 2.035(3) 6 ?
Ni2 O3 2.035(3) . ?
Ni2 N2 2.074(5) . ?
Ni2 O1 2.075(4) . ?
Ni2 O4 2.078(3) 1_554 ?
Ni2 O4 2.078(3) 6_554 ?
Ni1 O2 2.014(3) 6 ?
Ni1 O2 2.014(3) . ?
Ni1 O1 2.036(4) . ?
Ni1 O1W 2.089(6) . ?
Ni1 N1 2.099(3) 6 ?
Ni1 O6 2.099(3) 6 ?
Ni1 O6 2.099(3) . ?
O1W H1W 0.8500 . ?
O1 H1O 0.8501 . ?
O2 C4 1.251(5) . ?
O3 C4 1.253(5) . ?
O4 C5 1.250(5) . ?
O4 Ni2 2.078(3) 1_556 ?
O5 C5 1.268(5) . ?
O5 H5O 0.8500 . ?
C1 C2 1.527(5) . ?
C1 C4 1.529(5) . ?
C1 C3 1.543(5) 7_547 ?
C1 H1 1.0000 . ?
C2 C5 1.527(5) . ?
C2 C3 1.536(5) . ?
C2 H2 1.0000 . ?
C3 C1 1.543(5) 7_547 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 N1 1.291(4) 2_556 ?
C6 C6 1.519(10) 5_556 ?
C7 C8 1.358(10) . ?
C7 O5W 1.89(3) 6_554 ?
C7 H7 0.9500 . ?
C8 C7 1.358(10) 2_556 ?
C8 H8 0.9500 . ?
N2 C9 1.323(6) . ?
N2 C9 1.323(6) 6 ?
C9 C10 1.399(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(7) . ?
C10 H10 0.9500 . ?
C11 C10 1.388(7) 6 ?
C11 C11 1.486(14) 5_656 ?
O4W O4W' 1.42(4) . ?
O5W C7 1.89(3) 6_556 ?
O6W O6W 0.99(15) 5_657 ?

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 Ni2 O3 91.2(2) 6 . ?
O3 Ni2 N2 88.04(14) 6 . ?
O3 Ni2 N2 88.04(14) . . ?
O3 Ni2 O1 93.42(12) 6 . ?
O3 Ni2 O1 93.42(12) . . ?
N2 Ni2 O1 177.91(19) . . ?
O3 Ni2 O4 176.38(12) 6 1_554 ?
O3 Ni2 O4 89.47(15) . 1_554 ?
N2 Ni2 O4 88.43(14) . 1_554 ?
O1 Ni2 O4 90.09(12) . 1_554 ?
O3 Ni2 O4 89.47(15) 6 6_554 ?
O3 Ni2 O4 176.38(12) . 6_554 ?
N2 Ni2 O4 88.43(14) . 6_554 ?
O1 Ni2 O4 90.09(12) . 6_554 ?
O4 Ni2 O4 89.62(19) 1_554 6_554 ?
O2 Ni1 O2 99.0(2) 6 . ?
O2 Ni1 O1 92.55(12) 6 . ?
O2 Ni1 O1 92.55(12) . . ?
O2 Ni1 O1W 86.97(15) 6 . ?
O2 Ni1 O1W 86.97(15) . . ?
O1 Ni1 O1W 179.3(2) . . ?
O2 Ni1 N1 170.10(14) 6 6 ?
O2 Ni1 N1 90.49(14) . 6 ?
O1 Ni1 N1 89.72(14) . 6 ?
O1W Ni1 N1 90.83(16) . 6 ?
O2 Ni1 O6 170.10(14) 6 6 ?
O2 Ni1 O6 90.49(14) . 6 ?
O1 Ni1 O6 89.72(14) . 6 ?
O1W Ni1 O6 90.83(16) . 6 ?
N1 Ni1 O6 0.00(18) 6 6 ?
O2 Ni1 O6 90.49(14) 6 . ?
O2 Ni1 O6 170.10(14) . . ?
O1 Ni1 O6 89.72(14) . . ?
O1W Ni1 O6 90.83(16) . . ?
N1 Ni1 O6 79.89(17) 6 . ?
O6 Ni1 O6 79.89(17) 6 . ?
Ni1 O1W H1W 109.9 . . ?
Ni1 O1 Ni2 116.18(19) . . ?
Ni1 O1 H1O 109.1 . . ?
Ni2 O1 H1O 109.1 . . ?
C4 O2 Ni1 134.7(3) . . ?
C4 O3 Ni2 134.5(3) . . ?
C5 O4 Ni2 128.5(3) . 1_556 ?
C5 O5 H5O 112.1 . . ?
C2 C1 C4 112.7(3) . . ?
C2 C1 C3 110.3(3) . 7_547 ?
C4 C1 C3 109.4(3) . 7_547 ?
C2 C1 H1 108.1 . . ?
C4 C1 H1 108.1 . . ?
C3 C1 H1 108.1 7_547 . ?
C1 C2 C5 112.2(3) . . ?
C1 C2 C3 110.2(3) . . ?
C5 C2 C3 108.7(3) . . ?
C1 C2 H2 108.6 . . ?
C5 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C2 C3 C1 110.6(3) . 7_547 ?
C2 C3 H3A 109.5 . . ?
C1 C3 H3A 109.5 7_547 . ?
C2 C3 H3B 109.5 . . ?
C1 C3 H3B 109.5 7_547 . ?
H3A C3 H3B 108.1 . . ?
O2 C4 O3 126.4(4) . . ?
O2 C4 C1 117.9(4) . . ?
O3 C4 C1 115.7(4) . . ?
O4 C5 O5 124.4(4) . . ?
O4 C5 C2 118.4(4) . . ?
O5 C5 C2 117.1(4) . . ?
N1 C6 C6 117.1(2) 2_556 5_556 ?
C8 C7 O5W 92.3(10) . 6_554 ?
C8 C7 H7 119.4 . . ?
O5W C7 H7 27.4 6_554 . ?
C7 C8 C7 116.8(10) 2_556 . ?
C7 C8 H8 121.6 2_556 . ?
C7 C8 H8 121.6 . . ?
C9 N2 C9 117.7(6) . 6 ?
C9 N2 Ni2 121.1(3) . . ?
C9 N2 Ni2 121.1(3) 6 . ?
N2 C9 C10 123.0(5) . . ?
N2 C9 H9 118.5 . . ?
C10 C9 H9 118.5 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C10 115.9(7) 6 . ?
C10 C11 C11 122.0(3) 6 5_656 ?
C10 C11 C11 122.0(3) . 5_656 ?

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
O2 Ni1 O1 Ni2 49.58(11) 6 . . . ?
O2 Ni1 O1 Ni2 -49.58(11) . . . . ?
O1W Ni1 O1 Ni2 0.000(19) . . . . ?
N1 Ni1 O1 Ni2 -140.06(8) 6 . . . ?
O6 Ni1 O1 Ni2 -140.06(8) 6 . . . ?
O6 Ni1 O1 Ni2 140.06(8) . . . . ?
O3 Ni2 O1 Ni1 -45.71(11) 6 . . . ?
O3 Ni2 O1 Ni1 45.71(11) . . . . ?
N2 Ni2 O1 Ni1 180.000(6) . . . . ?
O4 Ni2 O1 Ni1 135.19(9) 1_554 . . . ?
O4 Ni2 O1 Ni1 -135.19(9) 6_554 . . . ?
O2 Ni1 O2 C4 -59.0(5) 6 . . . ?
O1 Ni1 O2 C4 34.0(5) . . . . ?
O1W Ni1 O2 C4 -145.5(5) . . . . ?
N1 Ni1 O2 C4 123.7(5) 6 . . . ?
O6 Ni1 O2 C4 123.7(5) 6 . . . ?
O6 Ni1 O2 C4 137.1(8) . . . . ?
O3 Ni2 O3 C4 73.5(5) 6 . . . ?
N2 Ni2 O3 C4 161.4(5) . . . . ?
O1 Ni2 O3 C4 -20.0(5) . . . . ?
O4 Ni2 O3 C4 -110.1(5) 1_554 . . . ?
O4 Ni2 O3 C4 174(2) 6_554 . . . ?
C4 C1 C2 C5 -58.6(5) . . . . ?
C3 C1 C2 C5 178.8(3) 7_547 . . . ?
C4 C1 C2 C3 -179.9(3) . . . . ?
C3 C1 C2 C3 57.6(5) 7_547 . . . ?
C1 C2 C3 C1 -57.8(5) . . . 7_547 ?
C5 C2 C3 C1 178.9(3) . . . 7_547 ?
Ni1 O2 C4 O3 -10.2(8) . . . . ?
Ni1 O2 C4 C1 170.1(3) . . . . ?
Ni2 O3 C4 O2 1.3(7) . . . . ?
Ni2 O3 C4 C1 -179.0(3) . . . . ?
C2 C1 C4 O2 -6.9(5) . . . . ?
C3 C1 C4 O2 116.2(4) 7_547 . . . ?
C2 C1 C4 O3 173.4(4) . . . . ?
C3 C1 C4 O3 -63.6(5) 7_547 . . . ?
Ni2 O4 C5 O5 11.3(7) 1_556 . . . ?
Ni2 O4 C5 C2 -167.7(3) 1_556 . . . ?
C1 C2 C5 O4 -43.5(5) . . . . ?
C3 C2 C5 O4 78.5(5) . . . . ?
C1 C2 C5 O5 137.4(4) . . . . ?
C3 C2 C5 O5 -100.5(4) . . . . ?
O5W C7 C8 C7 -176.3(12) 6_554 . . 2_556 ?
O3 Ni2 N2 C9 -43.3(6) 6 . . . ?
O3 Ni2 N2 C9 -134.6(6) . . . . ?
O1 Ni2 N2 C9 91.0(6) . . . . ?
O4 Ni2 N2 C9 135.9(6) 1_554 . . . ?
O4 Ni2 N2 C9 46.2(6) 6_554 . . . ?
O3 Ni2 N2 C9 134.6(6) 6 . . 6 ?
O3 Ni2 N2 C9 43.3(6) . . . 6 ?
O1 Ni2 N2 C9 -91.0(6) . . . 6 ?
O4 Ni2 N2 C9 -46.2(6) 1_554 . . 6 ?
O4 Ni2 N2 C9 -135.9(6) 6_554 . . 6 ?
C9 N2 C9 C10 -0.2(13) 6 . . . ?
Ni2 N2 C9 C10 177.8(6) . . . . ?
N2 C9 C10 C11 0.3(13) . . . . ?
C9 C10 C11 C10 -0.3(15) . . . 6 ?
C9 C10 C11 C11 178.5(10) . . . 5_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O5 0.85 2.23 3.074(6) 177.6 .
O1 H1O O5 0.85 1.76 2.546(4) 153.8 1_554
O5 H5O O4W' 0.85 1.98 2.75(3) 150.1 .
O5 H5O O4W 0.85 2.02 2.832(15) 159.3 .

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.132

#_eof
#End of Crystallographic Information File