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        'M. Dolores Santana'
_publ_contact_author_address     
;
Quimica Inorganica
Universidad de Murcia
Facultad de Quimica
Campus de Espinardo
Murcia
30071
SPAIN
;

_publ_contact_author_email       DSL@UM.ES

_publ_section_title              
;
Structure and Magnetic Properties of Carbonate-Bridged
Five-coordinate Nickel(II) Complexes Controlled by Solvent Effect
;
loop_
_publ_author_name
'M. Dolores Santana'
'Gabriel Garcia'
'Luis Garcia'
'Luis Lezama'
'Gregorio Lopez'
'A. Abel Lozano'
;
J.Perez
;
'T. Rojo'
'Magali Saez'

# Attachment 'complex1a_1b.cif'

data_complex1a
_database_code_depnum_ccdc_archive 'CCDC 289012'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H54 N6 Ni2 O3, 2(F6 P)'
_chemical_formula_sum            'C27 H54 F12 N6 Ni2 O3 P2'

_chemical_formula_weight         918.12

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           Orthorhombic
_symmetry_space_group_name_H-M   Iba2
_symmetry_space_group_name_Hall  I2-2c

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

_cell_length_a                   15.977(3)
_cell_length_b                   16.6924(11)
_cell_length_c                   15.8375(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4223.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    100
_cell_measurement_theta_min      5.206
_cell_measurement_theta_max      12.084

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.5702
_exptl_absorpt_correction_T_max  0.8011
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Siemens P4'
_diffrn_measurement_method       /w-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 247
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        13.45
_diffrn_reflns_number            7598
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3641
_reflns_number_gt                3028
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens xscans'
_computing_cell_refinement       'Siemens xscans'
_computing_data_reduction        'Siemens xscans'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'

_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^)+(0.1180P)^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    'NH free, rigid methyls, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_number_reflns         3641
_refine_ls_number_parameters     244
_refine_ls_number_restraints     307
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1722
_refine_ls_wR_factor_gt          0.1653
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.08162(4) 0.90534(4) 0.60931(6) 0.0258(2) Uani 1 1 d . . .
N1 N 0.1026(4) 0.9039(3) 0.7344(4) 0.0353(13) Uani 1 1 d . . .
N2 N 0.1993(3) 0.8726(4) 0.5807(4) 0.0288(12) Uani 1 1 d . . .
N3 N 0.0177(3) 0.7989(3) 0.6086(5) 0.0379(11) Uani 1 1 d . . .
C1 C 0.1737(5) 0.9084(4) 0.7696(4) 0.0341(15) Uani 1 1 d . . .
C2 C 0.2510(5) 0.9160(4) 0.7222(4) 0.0345(15) Uani 1 1 d . . .
H2A H 0.2836 0.8666 0.7333 0.041 Uiso 1 1 calc R . .
H2B H 0.2826 0.9606 0.7482 0.041 Uiso 1 1 calc R . .
C3 C 0.2537(4) 0.9299(4) 0.6249(4) 0.0346(15) Uani 1 1 d . . .
C4 C 0.2214(4) 0.7859(4) 0.5894(4) 0.0381(17) Uani 1 1 d . . .
H4A H 0.2332 0.7738 0.6495 0.046 Uiso 1 1 calc R . .
H4B H 0.2728 0.7746 0.5566 0.046 Uiso 1 1 calc R . .
C5 C 0.1515(4) 0.7322(4) 0.5586(5) 0.0390(16) Uani 1 1 d . . .
H5A H 0.1332 0.7514 0.5024 0.047 Uiso 1 1 calc R . .
H5B H 0.1740 0.6774 0.5513 0.047 Uiso 1 1 calc R . .
C6 C 0.0763(4) 0.7281(4) 0.6153(7) 0.0453(16) Uani 1 1 d . . .
H6A H 0.0958 0.7237 0.6745 0.054 Uiso 1 1 calc R . .
H6B H 0.0446 0.6787 0.6019 0.054 Uiso 1 1 calc R . .
C7 C -0.0451(6) 0.7963(6) 0.6794(5) 0.049(2) Uani 1 1 d . . .
H7A H -0.0728 0.7432 0.6784 0.059 Uiso 1 1 calc R . .
H7B H -0.0887 0.8370 0.6680 0.059 Uiso 1 1 calc R . .
C8 C -0.0114(5) 0.8104(5) 0.7681(4) 0.0442(18) Uani 1 1 d . . .
H8A H 0.0326 0.7702 0.7800 0.053 Uiso 1 1 calc R . .
H8B H -0.0573 0.8020 0.8092 0.053 Uiso 1 1 calc R . .
C9 C 0.0252(5) 0.8939(4) 0.7814(5) 0.0382(17) Uani 1 1 d . . .
H9A H -0.0159 0.9347 0.7628 0.046 Uiso 1 1 calc R . .
H9B H 0.0361 0.9024 0.8423 0.046 Uiso 1 1 calc R . .
C10 C 0.1843(5) 0.9023(5) 0.8648(5) 0.0428(17) Uani 1 1 d . . .
H10A H 0.1571 0.9481 0.8920 0.064 Uiso 1 1 calc R . .
H10B H 0.2441 0.9023 0.8788 0.064 Uiso 1 1 calc R . .
H10C H 0.1587 0.8524 0.8849 0.064 Uiso 1 1 calc R . .
C11 C 0.2228(4) 1.0138(4) 0.6052(5) 0.0364(14) Uani 1 1 d . . .
H11A H 0.2150 1.0195 0.5441 0.055 Uiso 1 1 calc R . .
H11B H 0.2640 1.0531 0.6248 0.055 Uiso 1 1 calc R . .
H11C H 0.1693 1.0230 0.6339 0.055 Uiso 1 1 calc R . .
C12 C 0.3462(4) 0.9221(5) 0.5950(5) 0.048(2) Uani 1 1 d . . .
H12A H 0.3688 0.8704 0.6135 0.072 Uiso 1 1 calc R . .
H12B H 0.3795 0.9656 0.6194 0.072 Uiso 1 1 calc R . .
H12C H 0.3484 0.9253 0.5333 0.072 Uiso 1 1 calc R . .
C13 C -0.0311(6) 0.7916(5) 0.5288(5) 0.046(2) Uani 1 1 d . . .
H13A H -0.0525 0.7368 0.5234 0.069 Uiso 1 1 calc R . .
H13B H 0.0053 0.8038 0.4807 0.069 Uiso 1 1 calc R . .
H13C H -0.0781 0.8293 0.5299 0.069 Uiso 1 1 calc R . .
C27 C 0.0000 1.0000 0.5253(6) 0.033(2) Uani 1 2 d S . .
O1 O 0.0000 1.0000 0.6100(5) 0.0327(12) Uani 1 2 d S . .
O2 O 0.0478(3) 0.9496(3) 0.4911(3) 0.0314(10) Uani 1 1 d . . .
P1 P 0.27420(13) 0.85295(13) 0.33431(13) 0.0456(5) Uani 1 1 d . . .
F1 F 0.2043(5) 0.8291(5) 0.3983(4) 0.097(2) Uani 1 1 d U . .
F2 F 0.3395(5) 0.8897(4) 0.2707(5) 0.0872(19) Uani 1 1 d U . .
F3 F 0.2619(8) 0.7783(5) 0.2799(5) 0.128(3) Uani 1 1 d U . .
F4 F 0.2860(5) 0.9329(4) 0.3882(5) 0.089(2) Uani 1 1 d U . .
F5 F 0.3460(5) 0.8136(4) 0.3873(5) 0.103(2) Uani 1 1 d U . .
F6 F 0.2044(4) 0.9007(4) 0.2809(4) 0.0816(19) Uani 1 1 d U . .
H2 H 0.203(4) 0.885(4) 0.527(5) 0.013(15) 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 0.0283(4) 0.0304(4) 0.0187(4) 0.0007(4) 0.0002(4) 0.0050(3)
N1 0.050(4) 0.028(3) 0.028(3) 0.001(2) 0.001(3) -0.002(2)
N2 0.029(3) 0.036(3) 0.022(3) 0.000(2) 0.001(2) 0.006(2)
N3 0.034(3) 0.046(3) 0.033(3) 0.004(4) -0.002(3) -0.002(2)
C1 0.044(4) 0.032(3) 0.026(4) -0.001(3) -0.009(3) 0.001(3)
C2 0.040(4) 0.038(4) 0.026(3) 0.001(3) -0.004(3) -0.006(3)
C3 0.038(3) 0.037(3) 0.029(4) -0.001(3) -0.001(3) -0.002(3)
C4 0.045(4) 0.035(3) 0.035(5) 0.003(3) -0.003(3) 0.008(3)
C5 0.048(4) 0.028(3) 0.042(4) -0.002(3) -0.003(3) 0.001(3)
C6 0.051(4) 0.036(3) 0.049(4) 0.007(5) -0.008(4) 0.001(3)
C7 0.044(5) 0.064(5) 0.038(4) 0.002(4) 0.008(4) -0.005(4)
C8 0.049(4) 0.053(4) 0.031(4) 0.010(3) 0.009(3) -0.008(4)
C9 0.041(4) 0.048(4) 0.025(4) 0.003(3) 0.006(3) 0.001(3)
C10 0.055(5) 0.048(4) 0.025(4) 0.006(3) -0.010(3) -0.004(4)
C11 0.043(3) 0.034(3) 0.031(3) 0.002(4) 0.000(4) -0.005(2)
C12 0.033(3) 0.067(5) 0.044(6) 0.003(4) 0.001(3) -0.006(3)
C13 0.054(5) 0.049(5) 0.035(4) -0.002(4) -0.012(3) -0.015(4)
C27 0.029(5) 0.037(5) 0.033(5) 0.000 0.000 0.007(4)
O1 0.040(3) 0.040(3) 0.018(3) 0.000 0.000 0.013(2)
O2 0.042(3) 0.035(2) 0.017(2) 0.0008(18) 0.0021(19) 0.011(2)
P1 0.0577(11) 0.0533(12) 0.0257(9) -0.0045(8) 0.0032(8) 0.0089(9)
F1 0.098(4) 0.142(5) 0.050(3) 0.010(4) 0.021(3) -0.018(4)
F2 0.079(4) 0.092(4) 0.090(4) 0.015(3) 0.024(3) 0.004(3)
F3 0.215(7) 0.084(5) 0.086(5) -0.037(4) 0.013(5) -0.027(5)
F4 0.113(5) 0.069(3) 0.086(4) -0.013(3) -0.025(4) 0.006(3)
F5 0.104(5) 0.091(4) 0.115(5) 0.028(4) -0.025(4) 0.031(4)
F6 0.074(4) 0.095(4) 0.076(4) 0.029(3) -0.014(3) -0.001(3)

_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 N2 2.009(5) . ?
Ni1 N1 2.010(6) . ?
Ni1 O1 2.0488(7) . ?
Ni1 N3 2.049(5) . ?
Ni1 O2 2.084(5) . ?
Ni1 C27 2.443(5) . ?
Ni1 Ni1 4.0976(13) 2_575 ?
N1 C1 1.267(10) . ?
N1 C9 1.454(10) . ?
N2 C3 1.471(9) . ?
N2 C4 1.497(9) . ?
N3 C13 1.490(10) . ?
N3 C7 1.505(10) . ?
N3 C6 1.512(8) . ?
C1 C2 1.451(11) . ?
C1 C10 1.521(10) . ?
C2 C3 1.560(9) . ?
C3 C11 1.517(9) . ?
C3 C12 1.557(9) . ?
C4 C5 1.512(10) . ?
C5 C6 1.502(11) . ?
C7 C8 1.523(11) . ?
C8 C9 1.526(11) . ?
C27 O2 1.258(6) 2_575 ?
C27 O2 1.258(6) . ?
C27 O1 1.341(12) . ?
C27 Ni1 2.443(5) 2_575 ?
O1 Ni1 2.0488(7) 2_575 ?
P1 F3 1.527(7) . ?
P1 F1 1.560(7) . ?
P1 F5 1.566(7) . ?
P1 F2 1.574(7) . ?
P1 F4 1.596(7) . ?
P1 F6 1.611(6) . ?

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
N2 Ni1 N1 93.6(3) . . ?
N2 Ni1 O1 143.73(19) . . ?
N1 Ni1 O1 96.3(3) . . ?
N2 Ni1 N3 103.3(2) . . ?
N1 Ni1 N3 94.5(3) . . ?
O1 Ni1 N3 110.55(15) . . ?
N2 Ni1 O2 97.8(2) . . ?
N1 Ni1 O2 158.9(2) . . ?
O1 Ni1 O2 64.3(2) . . ?
N3 Ni1 O2 100.0(2) . . ?
N2 Ni1 C27 123.5(2) . . ?
N1 Ni1 C27 129.3(3) . . ?
O1 Ni1 C27 33.3(3) . . ?
N3 Ni1 C27 106.95(17) . . ?
O2 Ni1 C27 31.0(2) . . ?
N2 Ni1 Ni1 143.62(18) . 2_575 ?
N1 Ni1 Ni1 96.62(17) . 2_575 ?
O1 Ni1 Ni1 0.3(2) . 2_575 ?
N3 Ni1 Ni1 110.55(14) . 2_575 ?
O2 Ni1 Ni1 63.98(12) . 2_575 ?
C27 Ni1 Ni1 33.00(19) . 2_575 ?
C1 N1 C9 123.0(6) . . ?
C1 N1 Ni1 125.6(5) . . ?
C9 N1 Ni1 111.3(5) . . ?
C3 N2 C4 116.5(5) . . ?
C3 N2 Ni1 105.6(4) . . ?
C4 N2 Ni1 117.6(4) . . ?
C13 N3 C7 106.3(5) . . ?
C13 N3 C6 108.6(7) . . ?
C7 N3 C6 109.8(6) . . ?
C13 N3 Ni1 109.7(5) . . ?
C7 N3 Ni1 110.7(5) . . ?
C6 N3 Ni1 111.6(4) . . ?
N1 C1 C2 122.7(7) . . ?
N1 C1 C10 122.2(7) . . ?
C2 C1 C10 115.0(7) . . ?
C1 C2 C3 123.2(6) . . ?
N2 C3 C11 108.0(5) . . ?
N2 C3 C12 111.2(6) . . ?
C11 C3 C12 108.9(6) . . ?
N2 C3 C2 110.9(6) . . ?
C11 C3 C2 109.4(6) . . ?
C12 C3 C2 108.3(6) . . ?
N2 C4 C5 111.6(6) . . ?
C6 C5 C4 115.1(7) . . ?
C5 C6 N3 114.7(7) . . ?
N3 C7 C8 116.5(7) . . ?
C7 C8 C9 113.9(7) . . ?
N1 C9 C8 111.1(6) . . ?
O2 C27 O2 129.0(9) 2_575 . ?
O2 C27 O1 115.5(5) 2_575 . ?
O2 C27 O1 115.5(5) . . ?
O2 C27 Ni1 58.6(3) 2_575 2_575 ?
O2 C27 Ni1 172.1(6) . 2_575 ?
O1 C27 Ni1 57.00(19) . 2_575 ?
O2 C27 Ni1 172.1(6) 2_575 . ?
O2 C27 Ni1 58.6(3) . . ?
O1 C27 Ni1 57.00(19) . . ?
Ni1 C27 Ni1 114.0(4) 2_575 . ?
C27 O1 Ni1 89.7(2) . 2_575 ?
C27 O1 Ni1 89.7(2) . . ?
Ni1 O1 Ni1 179.4(4) 2_575 . ?
C27 O2 Ni1 90.4(5) . . ?
F3 P1 F1 93.8(5) . . ?
F3 P1 F5 93.1(6) . . ?
F1 P1 F5 94.0(4) . . ?
F3 P1 F2 92.4(5) . . ?
F1 P1 F2 171.7(4) . . ?
F5 P1 F2 91.2(4) . . ?
F3 P1 F4 177.9(5) . . ?
F1 P1 F4 87.2(4) . . ?
F5 P1 F4 88.7(4) . . ?
F2 P1 F4 86.4(4) . . ?
F3 P1 F6 91.1(6) . . ?
F1 P1 F6 88.4(4) . . ?
F5 P1 F6 175.0(4) . . ?
F2 P1 F6 86.0(4) . . ?
F4 P1 F6 87.0(4) . . ?

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
N2 H2 F1 0.87(7) 2.25(7) 2.979(9) 142(5) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.139

#===END

data_complex1b
_database_code_depnum_ccdc_archive 'CCDC 289013'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H57 N7 Ni2 O3, C2 H3 N, 2(F6 P)'
_chemical_formula_sum            'C31 H60 F12 N8 Ni2 O3 P2'
_chemical_formula_weight         1000.23

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  -P2yn

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

_cell_length_a                   11.0176(7)
_cell_length_b                   30.997(2)
_cell_length_c                   12.4487(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.409(1)
_cell_angle_gamma                90.00
_cell_volume                     4243.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4162
_cell_measurement_theta_min      4.536
_cell_measurement_theta_max      44.252

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8243
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       \w-scan
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26579
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         28.20
_reflns_number_total             9484
_reflns_number_gt                7542
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'

_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^)+(0.0651P)^2^+3.0280P] 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    'NH free, rigid methyls, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9484
_refine_ls_number_parameters     564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1231
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.62498(3) 0.076125(11) 0.47112(3) 0.02108(10) Uani 1 1 d . . .
Ni2 Ni 0.46618(3) 0.147020(11) 0.71988(3) 0.02131(10) Uani 1 1 d . . .
O1 O 0.56543(16) 0.11222(6) 0.59795(14) 0.0232(4) Uani 1 1 d . . .
O2 O 0.53288(17) 0.04227(6) 0.58088(15) 0.0251(4) Uani 1 1 d . . .
O3 O 0.45000(17) 0.08007(6) 0.71397(15) 0.0259(4) Uani 1 1 d . . .
N1 N 0.6651(2) 0.12413(7) 0.37210(19) 0.0257(5) Uani 1 1 d . . .
N2 N 0.5923(2) 0.03447(8) 0.34861(19) 0.0252(5) Uani 1 1 d . . .
H2 H 0.554(3) 0.0147(11) 0.377(2) 0.027(8) Uiso 1 1 d . . .
N3 N 0.8031(2) 0.06332(7) 0.51941(19) 0.0262(5) Uani 1 1 d . . .
N4 N 0.3188(2) 0.15255(7) 0.61098(18) 0.0239(5) Uani 1 1 d . . .
N5 N 0.5171(2) 0.21109(8) 0.69015(19) 0.0262(5) Uani 1 1 d . . .
H5 H 0.591(3) 0.2059(11) 0.679(3) 0.033(9) Uiso 1 1 d . . .
N6 N 0.3690(2) 0.15443(8) 0.85818(19) 0.0295(5) Uani 1 1 d . . .
N7 N 0.6312(2) 0.14149(8) 0.81386(19) 0.0292(5) Uani 1 1 d . . .
C1 C 0.6336(3) 0.12677(9) 0.2716(2) 0.0314(6) Uani 1 1 d . . .
C2 C 0.5528(3) 0.09369(10) 0.2144(2) 0.0373(7) Uani 1 1 d . . .
H2A H 0.6001 0.0808 0.1573 0.045 Uiso 1 1 calc R . .
H2B H 0.4843 0.1096 0.1777 0.045 Uiso 1 1 calc R . .
C3 C 0.4977(3) 0.05626(10) 0.2757(2) 0.0319(7) Uani 1 1 d . . .
C4 C 0.6984(3) 0.01630(9) 0.2970(2) 0.0302(6) Uani 1 1 d . . .
H4A H 0.7322 0.0382 0.2493 0.036 Uiso 1 1 calc R . .
H4B H 0.6724 -0.0089 0.2523 0.036 Uiso 1 1 calc R . .
C5 C 0.7960(3) 0.00239(9) 0.3816(3) 0.0328(7) Uani 1 1 d . . .
H5A H 0.8539 -0.0170 0.3475 0.039 Uiso 1 1 calc R . .
H5B H 0.7572 -0.0143 0.4381 0.039 Uiso 1 1 calc R . .
C6 C 0.8668(3) 0.04009(10) 0.4346(3) 0.0319(7) Uani 1 1 d . . .
H6A H 0.9450 0.0290 0.4669 0.038 Uiso 1 1 calc R . .
H6B H 0.8859 0.0610 0.3780 0.038 Uiso 1 1 calc R . .
C7 C 0.8688(3) 0.10427(10) 0.5474(3) 0.0326(7) Uani 1 1 d . . .
H7A H 0.9541 0.0971 0.5700 0.039 Uiso 1 1 calc R . .
H7B H 0.8316 0.1173 0.6101 0.039 Uiso 1 1 calc R . .
C8 C 0.8698(3) 0.13819(10) 0.4581(3) 0.0324(7) Uani 1 1 d . . .
H8A H 0.9245 0.1620 0.4825 0.039 Uiso 1 1 calc R . .
H8B H 0.9040 0.1250 0.3940 0.039 Uiso 1 1 calc R . .
C9 C 0.7450(3) 0.15692(9) 0.4250(2) 0.0294(6) Uani 1 1 d . . .
H9A H 0.7070 0.1680 0.4896 0.035 Uiso 1 1 calc R . .
H9B H 0.7547 0.1814 0.3751 0.035 Uiso 1 1 calc R . .
C10 C 0.6760(3) 0.16146(11) 0.1981(3) 0.0438(8) Uani 1 1 d . . .
H10A H 0.6448 0.1895 0.2205 0.066 Uiso 1 1 calc R . .
H10B H 0.6457 0.1553 0.1240 0.066 Uiso 1 1 calc R . .
H10C H 0.7651 0.1622 0.2019 0.066 Uiso 1 1 calc R . .
C11 C 0.3994(3) 0.07250(11) 0.3471(3) 0.0384(7) Uani 1 1 d . . .
H11A H 0.3658 0.0481 0.3857 0.058 Uiso 1 1 calc R . .
H11B H 0.3344 0.0864 0.3023 0.058 Uiso 1 1 calc R . .
H11C H 0.4348 0.0934 0.3990 0.058 Uiso 1 1 calc R . .
C12 C 0.4405(3) 0.02423(11) 0.1919(3) 0.0441(9) Uani 1 1 d . . .
H12A H 0.5033 0.0137 0.1459 0.066 Uiso 1 1 calc R . .
H12B H 0.3766 0.0389 0.1475 0.066 Uiso 1 1 calc R . .
H12C H 0.4052 -0.0002 0.2291 0.066 Uiso 1 1 calc R . .
C13 C 0.8079(3) 0.03679(10) 0.6193(3) 0.0363(7) Uani 1 1 d . . .
H13A H 0.7658 0.0094 0.6049 0.054 Uiso 1 1 calc R . .
H13B H 0.7681 0.0524 0.6760 0.054 Uiso 1 1 calc R . .
H13C H 0.8929 0.0311 0.6428 0.054 Uiso 1 1 calc R . .
C14 C 0.3264(3) 0.17299(9) 0.5227(2) 0.0278(6) Uani 1 1 d . . .
C15 C 0.4422(2) 0.19712(9) 0.5031(2) 0.0257(6) Uani 1 1 d . . .
H15A H 0.4343 0.2105 0.4308 0.031 Uiso 1 1 calc R . .
H15B H 0.5104 0.1763 0.5036 0.031 Uiso 1 1 calc R . .
C16 C 0.4727(3) 0.23240(9) 0.5870(2) 0.0298(6) Uani 1 1 d . . .
C17 C 0.5228(3) 0.23903(10) 0.7870(2) 0.0358(7) Uani 1 1 d . . .
H17A H 0.5314 0.2694 0.7641 0.043 Uiso 1 1 calc R . .
H17B H 0.5963 0.2314 0.8327 0.043 Uiso 1 1 calc R . .
C18 C 0.4121(3) 0.23541(10) 0.8541(3) 0.0395(8) Uani 1 1 d . . .
H18A H 0.4121 0.2604 0.9037 0.047 Uiso 1 1 calc R . .
H18B H 0.3382 0.2376 0.8052 0.047 Uiso 1 1 calc R . .
C19 C 0.4035(3) 0.19450(11) 0.9201(2) 0.0393(8) Uani 1 1 d . . .
H19A H 0.4831 0.1895 0.9593 0.047 Uiso 1 1 calc R . .
H19B H 0.3430 0.1992 0.9746 0.047 Uiso 1 1 calc R . .
C20 C 0.2350(3) 0.15511(11) 0.8285(2) 0.0352(7) Uani 1 1 d . . .
H20A H 0.2132 0.1834 0.7958 0.042 Uiso 1 1 calc R . .
H20B H 0.1902 0.1521 0.8947 0.042 Uiso 1 1 calc R . .
C21 C 0.1949(3) 0.11945(11) 0.7500(2) 0.0338(7) Uani 1 1 d . . .
H21A H 0.2472 0.0939 0.7643 0.041 Uiso 1 1 calc R . .
H21B H 0.1104 0.1111 0.7632 0.041 Uiso 1 1 calc R . .
C22 C 0.2010(3) 0.13224(10) 0.6326(2) 0.0320(6) Uani 1 1 d . . .
H22A H 0.1890 0.1063 0.5869 0.038 Uiso 1 1 calc R . .
H22B H 0.1343 0.1527 0.6131 0.038 Uiso 1 1 calc R . .
C23 C 0.2257(3) 0.17552(10) 0.4359(2) 0.0345(7) Uani 1 1 d . . .
H23A H 0.1891 0.1469 0.4249 0.052 Uiso 1 1 calc R . .
H23B H 0.2587 0.1854 0.3688 0.052 Uiso 1 1 calc R . .
H23C H 0.1636 0.1959 0.4575 0.052 Uiso 1 1 calc R . .
C24 C 0.5693(3) 0.26245(10) 0.5457(3) 0.0372(7) Uani 1 1 d . . .
H24A H 0.5882 0.2851 0.5990 0.056 Uiso 1 1 calc R . .
H24B H 0.5387 0.2757 0.4778 0.056 Uiso 1 1 calc R . .
H24C H 0.6431 0.2459 0.5336 0.056 Uiso 1 1 calc R . .
C25 C 0.3568(3) 0.25939(10) 0.6011(3) 0.0374(7) Uani 1 1 d . . .
H25A H 0.2931 0.2408 0.6277 0.056 Uiso 1 1 calc R . .
H25B H 0.3286 0.2718 0.5316 0.056 Uiso 1 1 calc R . .
H25C H 0.3751 0.2826 0.6529 0.056 Uiso 1 1 calc R . .
C26 C 0.3944(3) 0.11713(11) 0.9319(2) 0.0372(7) Uani 1 1 d . . .
H26A H 0.4817 0.1159 0.9521 0.056 Uiso 1 1 calc R . .
H26B H 0.3690 0.0903 0.8954 0.056 Uiso 1 1 calc R . .
H26C H 0.3492 0.1207 0.9968 0.056 Uiso 1 1 calc R . .
C27 C 0.5137(2) 0.07706(9) 0.6340(2) 0.0237(6) Uani 1 1 d . . .
C28 C 0.7240(3) 0.13659(10) 0.8559(2) 0.0306(6) Uani 1 1 d . . .
C29 C 0.8427(3) 0.13015(12) 0.9116(3) 0.0444(8) Uani 1 1 d . . .
H29A H 0.8333 0.1279 0.9891 0.067 Uiso 1 1 calc R . .
H29B H 0.8955 0.1547 0.8973 0.067 Uiso 1 1 calc R . .
H29C H 0.8793 0.1036 0.8856 0.067 Uiso 1 1 calc R . .
P1 P 0.05779(9) 0.09587(4) 0.17788(8) 0.0493(3) Uani 1 1 d . . .
F1 F 0.0371(3) 0.09624(18) 0.0532(2) 0.158(2) Uani 1 1 d . . .
F2 F 0.1043(5) 0.04797(12) 0.1754(3) 0.159(2) Uani 1 1 d . . .
F3 F 0.1928(2) 0.11324(16) 0.1690(3) 0.1371(19) Uani 1 1 d . . .
F4 F 0.08363(19) 0.09361(8) 0.30371(17) 0.0567(6) Uani 1 1 d . . .
F5 F 0.0116(3) 0.14349(10) 0.1879(4) 0.1216(14) Uani 1 1 d . . .
F6 F -0.0779(2) 0.08195(10) 0.1873(2) 0.0812(9) Uani 1 1 d . . .
P2 P 0.92801(8) 0.23050(3) 0.70573(7) 0.0364(2) Uani 1 1 d . . .
F7 F 0.85097(19) 0.22817(7) 0.81004(17) 0.0527(5) Uani 1 1 d . . .
F8 F 1.0071(2) 0.23178(8) 0.60253(17) 0.0623(6) Uani 1 1 d . . .
F9 F 0.8936(2) 0.27963(8) 0.69087(19) 0.0667(7) Uani 1 1 d . . .
F10 F 0.96544(18) 0.18056(7) 0.72341(17) 0.0508(5) Uani 1 1 d . . .
F11 F 0.8135(2) 0.21523(10) 0.6334(2) 0.0833(9) Uani 1 1 d . . .
F12 F 1.04638(18) 0.24395(7) 0.77956(16) 0.0498(5) Uani 1 1 d . . .
N8A N 0.6753(11) 0.0533(3) -0.0073(7) 0.054(3) Uani 0.57(3) 1 d P A 1
C30A C 0.744(2) 0.0258(8) 0.0150(15) 0.052(7) Uani 0.57(3) 1 d P A 1
C31A C 0.8239(18) -0.0079(6) 0.0505(14) 0.074(6) Uani 0.57(3) 1 d P A 1
H31A H 0.8985 0.0046 0.0842 0.110 Uiso 0.57(3) 1 calc PR A 1
H31B H 0.8441 -0.0256 -0.0113 0.110 Uiso 0.57(3) 1 calc PR A 1
H31C H 0.7845 -0.0259 0.1029 0.110 Uiso 0.57(3) 1 calc PR A 1
N8B N 0.734(5) 0.0332(15) 0.000(2) 0.110(14) Uani 0.43(3) 1 d P A 2
C30B C 0.815(4) 0.0072(16) 0.0281(18) 0.15(2) Uani 0.43(3) 1 d P A 2
C31B C 0.888(3) -0.0182(6) 0.085(2) 0.095(9) Uani 0.43(3) 1 d P A 2
H31D H 0.8422 -0.0423 0.1133 0.142 Uiso 0.43(3) 1 calc PR A 2
H31E H 0.9270 -0.0019 0.1456 0.142 Uiso 0.43(3) 1 calc PR A 2
H31F H 0.9511 -0.0293 0.0401 0.142 Uiso 0.43(3) 1 calc PR A 2

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 0.02056(18) 0.01582(17) 0.02651(18) -0.00135(13) -0.00154(13) -0.00094(13)
Ni2 0.02061(18) 0.01910(18) 0.02373(18) -0.00196(13) -0.00292(13) 0.00215(13)
O1 0.0248(10) 0.0157(9) 0.0290(10) -0.0010(7) 0.0018(7) -0.0007(7)
O2 0.0286(10) 0.0156(9) 0.0311(10) -0.0020(7) 0.0009(8) -0.0014(8)
O3 0.0270(10) 0.0210(10) 0.0297(10) 0.0001(8) 0.0028(8) -0.0005(8)
N1 0.0253(12) 0.0181(11) 0.0339(13) 0.0003(9) 0.0023(10) -0.0017(9)
N2 0.0310(13) 0.0195(12) 0.0248(12) 0.0007(9) -0.0019(9) -0.0026(10)
N3 0.0207(12) 0.0213(12) 0.0359(13) -0.0028(10) -0.0030(9) 0.0003(9)
N4 0.0205(11) 0.0248(12) 0.0261(11) -0.0001(9) -0.0007(9) -0.0012(9)
N5 0.0250(13) 0.0196(12) 0.0332(13) -0.0042(10) -0.0056(10) 0.0026(10)
N6 0.0297(13) 0.0329(14) 0.0257(12) -0.0002(10) -0.0012(10) 0.0088(10)
N7 0.0276(13) 0.0264(13) 0.0329(13) -0.0018(10) -0.0044(10) 0.0020(10)
C1 0.0343(16) 0.0223(14) 0.0377(16) 0.0039(12) 0.0027(12) 0.0017(12)
C2 0.052(2) 0.0283(16) 0.0304(15) 0.0052(13) -0.0096(14) -0.0033(14)
C3 0.0382(17) 0.0266(15) 0.0293(14) 0.0030(12) -0.0106(12) -0.0053(13)
C4 0.0363(16) 0.0230(15) 0.0314(15) -0.0041(12) 0.0036(12) -0.0051(12)
C5 0.0319(16) 0.0212(15) 0.0454(17) -0.0054(13) 0.0026(13) 0.0039(12)
C6 0.0248(15) 0.0260(15) 0.0446(17) -0.0049(13) -0.0004(12) 0.0027(12)
C7 0.0214(14) 0.0283(16) 0.0471(18) -0.0084(13) -0.0054(12) -0.0008(12)
C8 0.0226(14) 0.0234(15) 0.0512(18) -0.0065(13) 0.0031(12) -0.0060(11)
C9 0.0255(15) 0.0212(14) 0.0415(16) -0.0030(12) 0.0033(12) -0.0035(11)
C10 0.055(2) 0.0306(17) 0.0459(19) 0.0118(15) 0.0059(16) -0.0047(15)
C11 0.0283(16) 0.0341(17) 0.0511(19) 0.0033(14) -0.0116(14) -0.0013(13)
C12 0.056(2) 0.0358(18) 0.0382(17) 0.0008(14) -0.0197(15) -0.0119(16)
C13 0.0291(16) 0.0363(17) 0.0419(17) 0.0039(14) -0.0108(13) 0.0016(13)
C14 0.0240(14) 0.0284(15) 0.0304(14) -0.0049(12) -0.0031(11) 0.0015(12)
C15 0.0239(14) 0.0232(14) 0.0297(14) 0.0002(11) -0.0025(11) 0.0029(11)
C16 0.0336(16) 0.0220(14) 0.0334(15) -0.0026(12) -0.0017(12) -0.0005(12)
C17 0.0395(18) 0.0253(15) 0.0406(17) -0.0093(13) -0.0137(14) 0.0028(13)
C18 0.051(2) 0.0315(17) 0.0346(16) -0.0133(13) -0.0076(14) 0.0118(15)
C19 0.0458(19) 0.044(2) 0.0278(15) -0.0083(14) -0.0027(13) 0.0134(15)
C20 0.0291(16) 0.046(2) 0.0309(15) 0.0025(13) 0.0054(12) 0.0115(14)
C21 0.0227(14) 0.0431(18) 0.0357(16) 0.0056(14) 0.0031(12) -0.0004(13)
C22 0.0230(14) 0.0360(17) 0.0367(16) -0.0011(13) -0.0018(12) -0.0028(12)
C23 0.0334(16) 0.0352(17) 0.0335(15) -0.0001(13) -0.0105(12) 0.0008(13)
C24 0.0349(17) 0.0265(16) 0.0494(19) 0.0046(14) -0.0036(14) -0.0041(13)
C25 0.0413(18) 0.0247(16) 0.0455(18) -0.0033(13) -0.0042(14) 0.0067(13)
C26 0.0396(18) 0.046(2) 0.0266(14) 0.0064(13) 0.0035(13) 0.0104(15)
C27 0.0218(13) 0.0190(13) 0.0294(14) 0.0012(11) -0.0052(11) -0.0001(10)
C28 0.0308(16) 0.0278(15) 0.0325(15) -0.0005(12) -0.0026(12) 0.0019(12)
C29 0.0322(17) 0.048(2) 0.051(2) 0.0045(16) -0.0131(15) 0.0030(15)
P1 0.0418(5) 0.0642(7) 0.0420(5) 0.0056(5) 0.0036(4) 0.0193(5)
F1 0.095(2) 0.336(6) 0.0437(15) 0.035(2) 0.0052(15) 0.119(3)
F2 0.237(5) 0.114(3) 0.112(3) -0.066(2) -0.095(3) 0.114(3)
F3 0.0426(15) 0.269(5) 0.101(2) 0.104(3) 0.0150(15) 0.018(2)
F4 0.0387(11) 0.0797(16) 0.0519(12) -0.0153(12) 0.0035(9) -0.0098(11)
F5 0.079(2) 0.0564(18) 0.227(4) 0.044(2) -0.010(2) 0.0103(16)
F6 0.0603(16) 0.109(2) 0.0718(17) -0.0038(15) -0.0136(13) -0.0307(15)
P2 0.0383(5) 0.0364(5) 0.0334(4) -0.0082(3) -0.0071(3) 0.0071(4)
F7 0.0491(12) 0.0484(13) 0.0613(13) -0.0148(10) 0.0089(10) -0.0017(10)
F8 0.0818(17) 0.0664(16) 0.0392(11) -0.0016(10) 0.0073(11) 0.0172(13)
F9 0.0873(18) 0.0511(14) 0.0609(14) 0.0029(11) -0.0024(12) 0.0303(13)
F10 0.0441(12) 0.0404(12) 0.0681(14) -0.0057(10) 0.0034(10) 0.0052(9)
F11 0.0516(14) 0.108(2) 0.0858(18) -0.0552(17) -0.0336(13) 0.0269(14)
F12 0.0474(12) 0.0527(13) 0.0481(12) -0.0037(10) -0.0062(9) -0.0061(10)
N8A 0.053(6) 0.066(5) 0.043(4) 0.003(3) -0.002(3) -0.003(4)
C30A 0.057(13) 0.074(10) 0.029(6) -0.031(6) 0.023(7) -0.040(10)
C31A 0.079(10) 0.091(11) 0.056(10) -0.019(9) 0.043(8) -0.001(8)
N8B 0.09(2) 0.15(3) 0.087(18) -0.028(15) -0.017(12) -0.04(2)
C30B 0.11(2) 0.26(4) 0.068(13) 0.040(15) -0.044(12) -0.14(3)
C31B 0.13(2) 0.050(9) 0.116(16) -0.045(10) 0.065(14) -0.032(11)

_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 N1 1.998(2) . ?
Ni1 N2 2.014(2) . ?
Ni1 O2 2.0402(19) . ?
Ni1 N3 2.057(2) . ?
Ni1 O1 2.0732(18) . ?
Ni1 C27 2.431(3) . ?
Ni1 Ni2 4.2572(5) . ?
Ni2 N4 2.059(2) . ?
Ni2 O3 2.0839(19) . ?
Ni2 N6 2.093(2) . ?
Ni2 N5 2.103(2) . ?
Ni2 N7 2.110(2) . ?
Ni2 O1 2.2047(18) . ?
Ni2 C27 2.487(3) . ?
O1 C27 1.320(3) . ?
O2 C27 1.289(3) . ?
O3 C27 1.256(3) . ?
N1 C1 1.281(4) . ?
N1 C9 1.475(3) . ?
N2 C4 1.478(4) . ?
N2 C3 1.502(4) . ?
N3 C6 1.488(4) . ?
N3 C13 1.489(4) . ?
N3 C7 1.493(4) . ?
N4 C14 1.276(4) . ?
N4 C22 1.482(4) . ?
N5 C17 1.483(4) . ?
N5 C16 1.500(4) . ?
N6 C26 1.492(4) . ?
N6 C19 1.499(4) . ?
N6 C20 1.500(4) . ?
N7 C28 1.130(4) . ?
C1 C10 1.504(4) . ?
C1 C2 1.508(4) . ?
C2 C3 1.534(4) . ?
C3 C11 1.527(5) . ?
C3 C12 1.547(4) . ?
C4 C5 1.522(4) . ?
C5 C6 1.533(4) . ?
C7 C8 1.531(4) . ?
C8 C9 1.526(4) . ?
C14 C23 1.504(4) . ?
C14 C15 1.511(4) . ?
C15 C16 1.535(4) . ?
C16 C24 1.527(4) . ?
C16 C25 1.545(4) . ?
C17 C18 1.523(5) . ?
C18 C19 1.517(5) . ?
C20 C21 1.523(4) . ?
C21 C22 1.519(4) . ?
C28 C29 1.457(4) . ?
P1 F1 1.555(3) . ?
P1 F6 1.567(3) . ?
P1 F5 1.569(3) . ?
P1 F2 1.572(3) . ?
P1 F4 1.577(2) . ?
P1 F3 1.592(3) . ?
P2 F9 1.578(2) . ?
P2 F11 1.578(2) . ?
P2 F7 1.595(2) . ?
P2 F8 1.595(2) . ?
P2 F12 1.605(2) . ?
P2 F10 1.614(2) . ?
N8A C30A 1.16(4) . ?
C30A C31A 1.42(4) . ?
N8B C30B 1.24(6) . ?
C30B C31B 1.31(4) . ?

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
N1 Ni1 N2 92.65(10) . . ?
N1 Ni1 O2 158.92(9) . . ?
N2 Ni1 O2 95.96(9) . . ?
N1 Ni1 N3 94.70(9) . . ?
N2 Ni1 N3 102.82(10) . . ?
O2 Ni1 N3 102.06(9) . . ?
N1 Ni1 O1 99.18(8) . . ?
N2 Ni1 O1 150.71(9) . . ?
O2 Ni1 O1 64.85(7) . . ?
N3 Ni1 O1 102.78(8) . . ?
N1 Ni1 C27 130.28(9) . . ?
N2 Ni1 C27 124.25(10) . . ?
O2 Ni1 C27 32.01(8) . . ?
N3 Ni1 C27 106.16(9) . . ?
O1 Ni1 C27 32.89(8) . . ?
N1 Ni1 Ni2 100.36(7) . . ?
N2 Ni1 Ni2 144.99(7) . . ?
O2 Ni1 Ni2 62.36(5) . . ?
N3 Ni1 Ni2 108.26(7) . . ?
O1 Ni1 Ni2 5.81(5) . . ?
C27 Ni1 Ni2 30.43(6) . . ?
N4 Ni2 O3 89.85(8) . . ?
N4 Ni2 N6 96.35(9) . . ?
O3 Ni2 N6 95.24(9) . . ?
N4 Ni2 N5 90.78(9) . . ?
O3 Ni2 N5 163.26(9) . . ?
N6 Ni2 N5 101.31(10) . . ?
N4 Ni2 N7 172.50(9) . . ?
O3 Ni2 N7 90.45(8) . . ?
N6 Ni2 N7 91.09(9) . . ?
N5 Ni2 N7 86.79(9) . . ?
N4 Ni2 O1 89.51(8) . . ?
O3 Ni2 O1 62.18(7) . . ?
N6 Ni2 O1 156.74(8) . . ?
N5 Ni2 O1 101.10(9) . . ?
N7 Ni2 O1 84.00(8) . . ?
N4 Ni2 C27 88.13(9) . . ?
O3 Ni2 C27 30.27(8) . . ?
N6 Ni2 C27 125.47(10) . . ?
N5 Ni2 C27 133.04(10) . . ?
N7 Ni2 C27 88.34(9) . . ?
O1 Ni2 C27 31.97(8) . . ?
N4 Ni2 Ni1 84.62(6) . . ?
O3 Ni2 Ni1 59.88(5) . . ?
N6 Ni2 Ni1 155.13(7) . . ?
N5 Ni2 Ni1 103.53(7) . . ?
N7 Ni2 Ni1 89.05(7) . . ?
O1 Ni2 Ni1 5.46(5) . . ?
C27 Ni2 Ni1 29.67(6) . . ?
C27 O1 Ni1 88.60(15) . . ?
C27 O1 Ni2 85.89(15) . . ?
Ni1 O1 Ni2 168.73(10) . . ?
C27 O2 Ni1 90.93(16) . . ?
C27 O3 Ni2 92.94(16) . . ?
C1 N1 C9 120.8(2) . . ?
C1 N1 Ni1 126.4(2) . . ?
C9 N1 Ni1 112.70(18) . . ?
C4 N2 C3 116.6(2) . . ?
C4 N2 Ni1 117.60(18) . . ?
C3 N2 Ni1 104.82(17) . . ?
C6 N3 C13 109.3(2) . . ?
C6 N3 C7 109.5(2) . . ?
C13 N3 C7 106.4(2) . . ?
C6 N3 Ni1 111.62(17) . . ?
C13 N3 Ni1 109.66(18) . . ?
C7 N3 Ni1 110.20(17) . . ?
C14 N4 C22 118.1(2) . . ?
C14 N4 Ni2 121.26(19) . . ?
C22 N4 Ni2 120.64(18) . . ?
C17 N5 C16 115.8(2) . . ?
C17 N5 Ni2 114.04(19) . . ?
C16 N5 Ni2 119.31(17) . . ?
C26 N6 C19 107.0(2) . . ?
C26 N6 C20 108.0(2) . . ?
C19 N6 C20 109.3(2) . . ?
C26 N6 Ni2 109.56(18) . . ?
C19 N6 Ni2 112.8(2) . . ?
C20 N6 Ni2 110.03(17) . . ?
C28 N7 Ni2 173.4(2) . . ?
N1 C1 C10 124.3(3) . . ?
N1 C1 C2 122.4(3) . . ?
C10 C1 C2 113.3(3) . . ?
C1 C2 C3 121.3(2) . . ?
N2 C3 C11 106.7(2) . . ?
N2 C3 C2 111.1(2) . . ?
C11 C3 C2 110.8(3) . . ?
N2 C3 C12 111.1(3) . . ?
C11 C3 C12 109.2(3) . . ?
C2 C3 C12 107.9(2) . . ?
N2 C4 C5 110.6(2) . . ?
C4 C5 C6 113.7(2) . . ?
N3 C6 C5 115.1(2) . . ?
N3 C7 C8 116.0(2) . . ?
C9 C8 C7 114.3(2) . . ?
N1 C9 C8 111.3(2) . . ?
N4 C14 C23 124.1(3) . . ?
N4 C14 C15 119.0(2) . . ?
C23 C14 C15 116.9(3) . . ?
C14 C15 C16 113.3(2) . . ?
N5 C16 C24 111.0(2) . . ?
N5 C16 C15 108.4(2) . . ?
C24 C16 C15 109.5(2) . . ?
N5 C16 C25 111.8(2) . . ?
C24 C16 C25 107.8(3) . . ?
C15 C16 C25 108.3(2) . . ?
N5 C17 C18 114.0(3) . . ?
C19 C18 C17 115.9(3) . . ?
N6 C19 C18 115.9(2) . . ?
N6 C20 C21 113.0(2) . . ?
C22 C21 C20 113.5(3) . . ?
N4 C22 C21 112.0(2) . . ?
O3 C27 O2 125.8(3) . . ?
O3 C27 O1 118.7(2) . . ?
O2 C27 O1 115.4(2) . . ?
O3 C27 Ni1 174.8(2) . . ?
O2 C27 Ni1 57.06(14) . . ?
O1 C27 Ni1 58.50(13) . . ?
O3 C27 Ni2 56.79(14) . . ?
O2 C27 Ni2 174.34(19) . . ?
O1 C27 Ni2 62.14(13) . . ?
Ni1 C27 Ni2 119.90(11) . . ?
N7 C28 C29 179.2(4) . . ?
F1 P1 F6 89.60(19) . . ?
F1 P1 F5 92.5(2) . . ?
F6 P1 F5 86.42(18) . . ?
F1 P1 F2 90.9(2) . . ?
F6 P1 F2 93.2(2) . . ?
F5 P1 F2 176.6(2) . . ?
F1 P1 F4 177.10(18) . . ?
F6 P1 F4 91.73(13) . . ?
F5 P1 F4 90.2(2) . . ?
F2 P1 F4 86.42(16) . . ?
F1 P1 F3 90.6(2) . . ?
F6 P1 F3 176.2(2) . . ?
F5 P1 F3 89.8(2) . . ?
F2 P1 F3 90.6(3) . . ?
F4 P1 F3 88.28(15) . . ?
F9 P2 F11 92.55(15) . . ?
F9 P2 F7 90.20(13) . . ?
F11 P2 F7 90.28(14) . . ?
F9 P2 F8 91.18(14) . . ?
F11 P2 F8 90.25(15) . . ?
F7 P2 F8 178.51(14) . . ?
F9 P2 F12 89.87(13) . . ?
F11 P2 F12 177.56(14) . . ?
F7 P2 F12 89.96(11) . . ?
F8 P2 F12 89.46(13) . . ?
F9 P2 F10 178.59(13) . . ?
F11 P2 F10 88.80(14) . . ?
F7 P2 F10 89.40(12) . . ?
F8 P2 F10 89.22(12) . . ?
F12 P2 F10 88.78(12) . . ?
N8A C30A C31A 175.6(13) . . ?
N8B C30B C31B 163(4) . . ?

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
N2 H2 O2 0.83(3) 2.09(3) 2.911(3) 168(3) 3_656

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        28.20
_diffrn_measured_fraction_theta_full 0.906
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.084

#===END