# Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Leigh Jones'
_publ_contact_author_email       LEIGH.JONES@NUIGALWAY.IE

_publ_section_title              
;
Planar [Ni7] Discs as Double-Bowl,
Pseudo Metallacalix[6]arene Host Cavities.
;
loop_
_publ_author_name
'Leigh Jones'
'Euan Brechin'
'Peter W. Dunne'
'Georgios Karotsis'
'Patrick McArdle'
'Sean Meally'
;
G.S.Papaefstathioi
;

# Attachment '[Ni7](1).cif'

data_lfj50a-1
_database_code_depnum_ccdc_archive 'CCDC 741051'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (Ni7(OH)6(L1)6)(NO3)2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H66 N8 Ni7 O24'
_chemical_formula_weight         1622.12
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3c1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
_cell_length_a                   13.806(2)
_cell_length_b                   13.806(2)
_cell_length_c                   23.270(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3841.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1668
_exptl_absorpt_coefficient_mu    1.749
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_exptl_absorpt_correction_T_min  0.57946
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            8234
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.6239
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      -0.0349664281
_diffrn_orient_matrix_UB_12      0.0096677209
_diffrn_orient_matrix_UB_13      0.0187042266
_diffrn_orient_matrix_UB_21      -0.0078340246
_diffrn_orient_matrix_UB_22      -0.0457483366
_diffrn_orient_matrix_UB_23      0.0173695959
_diffrn_orient_matrix_UB_31      0.0473800140
_diffrn_orient_matrix_UB_32      0.0366962609
_diffrn_orient_matrix_UB_33      0.0167299896
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega -33.00 79.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 19.5780 0.0000 -90.0000 112
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      150(2)
_reflns_number_total             2306
_reflns_number_gt                1376
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1573P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_number_reflns         2306
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2662
_refine_ls_wR_factor_gt          0.2446
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 0.0000 0.0000 0.0000 0.0270(7) Uani 1 6 d S . .
Ni2 Ni 0.10310(10) 0.25718(10) -0.00763(5) 0.0289(5) Uani 1 1 d . . .
O1 O 0.1252(5) 0.1349(5) -0.0442(3) 0.0255(14) Uani 1 1 d . . .
H1 H 0.1306 0.1314 -0.0869 0.031 Uiso 1 1 calc R . .
O2 O 0.2407(5) 0.2819(5) 0.0336(3) 0.0261(14) Uani 1 1 d . . .
O3 O 0.1427(6) 0.3972(5) 0.0564(3) 0.0381(17) Uani 1 1 d . . .
O4 O 0.6484(8) 0.4125(8) 0.2044(4) 0.072(3) Uani 1 1 d . . .
N1 N 0.3820(7) 0.2033(7) 0.0694(4) 0.038(2) Uani 1 1 d . . .
N2 N 0.6667 0.3333 0.2027(6) 0.045(4) Uani 1 3 d S . .
C1 C 0.4400(12) 0.1341(12) 0.0734(7) 0.077(5) Uani 1 1 d . . .
H1A H 0.4925 0.1608 0.1058 0.116 Uiso 1 1 calc R . .
H1B H 0.4808 0.1417 0.0377 0.116 Uiso 1 1 calc R . .
H1C H 0.3839 0.0552 0.0794 0.116 Uiso 1 1 calc R . .
C2 C 0.4066(9) 0.2756(9) 0.1097(5) 0.041(3) Uani 1 1 d . . .
H2 H 0.4634 0.2852 0.1359 0.049 Uiso 1 1 calc R . .
C3 C 0.3557(9) 0.3434(9) 0.1184(4) 0.036(2) Uiso 1 1 d . . .
C4 C 0.3873(9) 0.4115(9) 0.1688(5) 0.046(3) Uani 1 1 d . . .
H4 H 0.4420 0.4126 0.1940 0.056 Uiso 1 1 calc R . .
C5 C 0.3399(10) 0.4746(9) 0.1809(5) 0.047(3) Uani 1 1 d . . .
H5 H 0.3623 0.5205 0.2143 0.057 Uiso 1 1 calc R . .
C6 C 0.2589(10) 0.4723(9) 0.1449(4) 0.044(3) Uani 1 1 d . . .
H6 H 0.2243 0.5150 0.1541 0.053 Uiso 1 1 calc R . .
C7 C 0.2284(9) 0.4080(8) 0.0959(4) 0.035(2) Uani 1 1 d . . .
C8 C 0.1345(11) 0.4935(10) 0.0481(6) 0.063(4) Uani 1 1 d . . .
H8A H 0.0887 0.4989 0.0787 0.094 Uiso 1 1 calc R . .
H8B H 0.0996 0.4890 0.0108 0.094 Uiso 1 1 calc R . .
H8C H 0.2094 0.5597 0.0490 0.094 Uiso 1 1 calc R . .
C9 C 0.2740(8) 0.3411(8) 0.0806(4) 0.031(2) Uani 1 1 d . . .
_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 O1 2.072(6) 8 ?
Ni1 O1 2.072(6) 9 ?
Ni1 O1 2.072(6) 7 ?
Ni1 O1 2.072(6) . ?
Ni1 O1 2.072(6) 3 ?
Ni1 O1 2.072(6) 2 ?
Ni2 O2 1.983(6) 9 ?
Ni2 O2 1.999(6) . ?
Ni2 O1 2.045(6) . ?
Ni2 N1 2.080(8) 9 ?
Ni2 O1 2.088(6) 9 ?
Ni2 O3 2.280(7) . ?
O1 Ni2 2.088(6) 8 ?
O1 H1 1.0000 . ?
O2 C9 1.304(11) . ?
O2 Ni2 1.983(6) 8 ?
O3 C8 1.403(12) . ?
O3 C7 1.446(12) . ?
O4 N2 1.238(9) . ?
N1 C2 1.286(13) . ?
N1 C1 1.526(14) . ?
N1 Ni2 2.080(8) 8 ?
N2 O4 1.238(9) 3_665 ?
N2 O4 1.238(9) 2_655 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.439(14) . ?
C2 H2 0.9500 . ?
C3 C9 1.419(14) . ?
C3 C4 1.427(14) . ?
C4 C5 1.355(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(14) . ?
C6 H6 0.9500 . ?
C7 C9 1.398(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 97.5(2) 8 9 ?
O1 Ni1 O1 97.5(2) 8 7 ?
O1 Ni1 O1 97.5(2) 9 7 ?
O1 Ni1 O1 82.5(2) 8 . ?
O1 Ni1 O1 82.5(2) 9 . ?
O1 Ni1 O1 180.0(6) 7 . ?
O1 Ni1 O1 82.5(2) 8 3 ?
O1 Ni1 O1 180.0(4) 9 3 ?
O1 Ni1 O1 82.5(2) 7 3 ?
O1 Ni1 O1 97.5(2) . 3 ?
O1 Ni1 O1 180.0(4) 8 2 ?
O1 Ni1 O1 82.5(2) 9 2 ?
O1 Ni1 O1 82.5(2) 7 2 ?
O1 Ni1 O1 97.5(2) . 2 ?
O1 Ni1 O1 97.5(2) 3 2 ?
O2 Ni2 O2 168.54(15) 9 . ?
O2 Ni2 O1 109.6(2) 9 . ?
O2 Ni2 O1 79.6(2) . . ?
O2 Ni2 N1 86.8(3) 9 9 ?
O2 Ni2 N1 98.6(3) . 9 ?
O1 Ni2 N1 100.1(3) . 9 ?
O2 Ni2 O1 78.9(2) 9 9 ?
O2 Ni2 O1 95.9(2) . 9 ?
O1 Ni2 O1 82.8(3) . 9 ?
N1 Ni2 O1 165.5(3) 9 9 ?
O2 Ni2 O3 95.6(3) 9 . ?
O2 Ni2 O3 74.8(2) . . ?
O1 Ni2 O3 154.2(2) . . ?
N1 Ni2 O3 86.6(3) 9 . ?
O1 Ni2 O3 96.9(2) 9 . ?
Ni2 O1 Ni1 97.7(2) . . ?
Ni2 O1 Ni2 97.8(2) . 8 ?
Ni1 O1 Ni2 96.3(2) . 8 ?
Ni2 O1 H1 119.9 . . ?
Ni1 O1 H1 119.9 . . ?
Ni2 O1 H1 119.9 8 . ?
C9 O2 Ni2 130.7(6) . 8 ?
C9 O2 Ni2 121.1(6) . . ?
Ni2 O2 Ni2 102.9(3) 8 . ?
C8 O3 C7 116.1(8) . . ?
C8 O3 Ni2 127.9(7) . . ?
C7 O3 Ni2 109.9(5) . . ?
C2 N1 C1 115.1(9) . . ?
C2 N1 Ni2 127.7(7) . 8 ?
C1 N1 Ni2 116.6(7) . 8 ?
O4 N2 O4 119.89(10) 3_665 2_655 ?
O4 N2 O4 119.89(11) 3_665 . ?
O4 N2 O4 119.89(10) 2_655 . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 125.7(10) . . ?
N1 C2 H2 117.2 . . ?
C3 C2 H2 117.2 . . ?
C9 C3 C4 120.1(9) . . ?
C9 C3 C2 122.6(9) . . ?
C4 C3 C2 117.2(9) . . ?
C5 C4 C3 120.5(10) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.2(10) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 120.0(10) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C9 123.0(10) . . ?
C6 C7 O3 124.3(9) . . ?
C9 C7 O3 112.6(8) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C7 119.6(9) . . ?
O2 C9 C3 124.2(9) . . ?
C7 C9 C3 116.2(9) . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.961
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.210

# Attachment '[Ni7](2)cif.cif'

data_lfj54d-1
_database_code_depnum_ccdc_archive 'CCDC 741052'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (Ni7(OH)6(L1)6)(NO3)2.3MeNO2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H75 N11 Ni7 O24'
_chemical_formula_weight         1709.25
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           Trigonal
_symmetry_space_group_name_H-M   P-3c1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
_cell_length_a                   13.933(2)
_cell_length_b                   13.933(2)
_cell_length_c                   22.742(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3823.4(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    1.762
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_exptl_absorpt_correction_T_min  0.97599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            9773
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.0529
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      -0.0466997139
_diffrn_orient_matrix_UB_12      -0.0455575681
_diffrn_orient_matrix_UB_13      0.0131894495
_diffrn_orient_matrix_UB_21      0.0157415404
_diffrn_orient_matrix_UB_22      0.0269490050
_diffrn_orient_matrix_UB_23      0.0276872274
_diffrn_orient_matrix_UB_31      -0.0320891875
_diffrn_orient_matrix_UB_32      0.0256188138
_diffrn_orient_matrix_UB_33      -0.0056400845
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega -41.00 13.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- -17.2341 -77.0000 90.0000 54
#__ type_ start__ end____ width___ exp.time_
2 omega 7.00 81.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- 19.5778 37.0000 90.0000 74
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      150(2)
_reflns_number_total             2333
_reflns_number_gt                1835
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1104P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_number_reflns         2333
_refine_ls_number_parameters     157
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1725
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_restrained_S_all      1.191
_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 0.0000 0.0000 0.5000 0.0157(4) Uani 1 6 d S . .
Ni2 Ni 0.10544(5) 0.25516(5) 0.50881(3) 0.0188(3) Uani 1 1 d . . .
O1 O 0.1258(3) 0.1325(3) 0.54483(14) 0.0186(7) Uani 1 1 d . . .
O2 O 0.2396(3) 0.2769(3) 0.46571(15) 0.0199(7) Uani 1 1 d . . .
O3 O 0.1491(3) 0.3966(3) 0.44262(17) 0.0263(9) Uani 1 1 d . . .
O4 O 0.4181(5) 0.6561(5) 0.2054(3) 0.0704(16) Uani 1 1 d . . .
O5 O 0.156(2) 0.075(2) 0.1729(13) 0.209(11) Uiso 0.50 1 d PD . .
O6 O 0.066(2) 0.178(2) 0.1837(12) 0.197(11) Uiso 0.50 1 d PD . .
N1 N 0.3770(4) 0.1955(4) 0.4284(2) 0.0259(10) Uani 1 1 d . . .
N2 N 0.3333 0.6667 0.2029(4) 0.039(2) Uani 1 3 d S . .
N3 N 0.1255(17) 0.1389(18) 0.1949(8) 0.144(9) Uiso 0.50 1 d PD . .
C1 C 0.4355(6) 0.1312(6) 0.4268(3) 0.0427(16) Uani 1 1 d . . .
H1A H 0.4914 0.1601 0.3955 0.064 Uiso 1 1 calc R . .
H1B H 0.3820 0.0530 0.4190 0.064 Uiso 1 1 calc R . .
H1C H 0.4717 0.1378 0.4647 0.064 Uiso 1 1 calc R . .
C2 C 0.4055(5) 0.2703(4) 0.3898(2) 0.0278(12) Uani 1 1 d . . .
H2 H 0.4634 0.2810 0.3639 0.033 Uiso 1 1 calc R . .
C3 C 0.3580(4) 0.3417(4) 0.3814(2) 0.0243(11) Uani 1 1 d . . .
C4 C 0.3970(5) 0.4162(5) 0.3323(2) 0.0313(13) Uani 1 1 d . . .
H4 H 0.4539 0.4198 0.3078 0.038 Uiso 1 1 calc R . .
C5 C 0.3523(5) 0.4824(5) 0.3208(3) 0.0338(14) Uani 1 1 d . . .
H5 H 0.3786 0.5315 0.2881 0.041 Uiso 1 1 calc R . .
C6 C 0.2683(5) 0.4785(5) 0.3564(2) 0.0309(13) Uani 1 1 d . . .
H6 H 0.2366 0.5234 0.3478 0.037 Uiso 1 1 calc R . .
C7 C 0.2325(4) 0.4080(4) 0.4045(2) 0.0231(11) Uani 1 1 d . . .
C8 C 0.1433(5) 0.4950(4) 0.4542(3) 0.0350(14) Uani 1 1 d . . .
H8A H 0.2166 0.5552 0.4657 0.052 Uiso 1 1 calc R . .
H8B H 0.0904 0.4804 0.4861 0.052 Uiso 1 1 calc R . .
H8C H 0.1188 0.5164 0.4186 0.052 Uiso 1 1 calc R . .
C9 C 0.2764(4) 0.3394(4) 0.4180(2) 0.0196(11) Uani 1 1 d . . .
C10 C 0.1878(14) 0.1878(14) 0.2500 0.122(6) Uiso 1 2 d SD . .
_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 O1 2.070(3) . ?
Ni1 O1 2.070(3) 7_556 ?
Ni1 O1 2.070(3) 2 ?
Ni1 O1 2.070(3) 8_556 ?
Ni1 O1 2.070(3) 3 ?
Ni1 O1 2.070(3) 9_556 ?
Ni2 O2 1.976(3) 9_556 ?
Ni2 O2 1.996(3) . ?
Ni2 O1 2.038(3) . ?
Ni2 N1 2.060(4) 9_556 ?
Ni2 O1 2.089(3) 9_556 ?
Ni2 O3 2.307(4) . ?
O1 Ni2 2.089(3) 8_556 ?
O2 C9 1.323(6) . ?
O2 Ni2 1.976(3) 8_556 ?
O3 C7 1.394(6) . ?
O3 C8 1.437(6) . ?
O4 N2 1.262(6) . ?
O5 N3 1.258(17) . ?
O5 O6 1.77(3) 3 ?
O6 N3 1.224(17) . ?
O6 O5 1.77(3) 2 ?
N1 C2 1.265(7) . ?
N1 C1 1.483(7) . ?
N1 Ni2 2.060(4) 8_556 ?
N2 O4 1.262(6) 2_665 ?
N2 O4 1.262(6) 3_565 ?
N3 C10 1.483(17) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.456(7) . ?
C2 H2 0.9500 . ?
C3 C9 1.397(7) . ?
C3 C4 1.434(8) . ?
C4 C5 1.371(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(7) . ?
C6 H6 0.9500 . ?
C7 C9 1.404(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 N3 1.483(17) 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
O1 Ni1 O1 180.0 . 7_556 ?
O1 Ni1 O1 97.82(12) . 2 ?
O1 Ni1 O1 82.18(12) 7_556 2 ?
O1 Ni1 O1 82.18(12) . 8_556 ?
O1 Ni1 O1 97.82(12) 7_556 8_556 ?
O1 Ni1 O1 180.00(16) 2 8_556 ?
O1 Ni1 O1 97.82(12) . 3 ?
O1 Ni1 O1 82.18(12) 7_556 3 ?
O1 Ni1 O1 97.82(12) 2 3 ?
O1 Ni1 O1 82.18(12) 8_556 3 ?
O1 Ni1 O1 82.18(12) . 9_556 ?
O1 Ni1 O1 97.82(12) 7_556 9_556 ?
O1 Ni1 O1 82.18(12) 2 9_556 ?
O1 Ni1 O1 97.82(12) 8_556 9_556 ?
O1 Ni1 O1 180.00(16) 3 9_556 ?
O2 Ni2 O2 167.34(8) 9_556 . ?
O2 Ni2 O1 110.14(14) 9_556 . ?
O2 Ni2 O1 79.17(13) . . ?
O2 Ni2 N1 87.82(15) 9_556 9_556 ?
O2 Ni2 N1 99.11(16) . 9_556 ?
O1 Ni2 N1 100.51(15) . 9_556 ?
O2 Ni2 O1 78.40(13) 9_556 9_556 ?
O2 Ni2 O1 94.83(14) . 9_556 ?
O1 Ni2 O1 82.48(17) . 9_556 ?
N1 Ni2 O1 166.05(15) 9_556 9_556 ?
O2 Ni2 O3 96.09(14) 9_556 . ?
O2 Ni2 O3 73.93(13) . . ?
O1 Ni2 O3 152.95(13) . . ?
N1 Ni2 O3 86.60(16) 9_556 . ?
O1 Ni2 O3 96.90(13) 9_556 . ?
Ni2 O1 Ni1 98.02(14) . . ?
Ni2 O1 Ni2 98.22(13) . 8_556 ?
Ni1 O1 Ni2 96.41(13) . 8_556 ?
C9 O2 Ni2 130.6(3) . 8_556 ?
C9 O2 Ni2 121.8(3) . . ?
Ni2 O2 Ni2 103.55(15) 8_556 . ?
C7 O3 C8 116.5(4) . . ?
C7 O3 Ni2 110.6(3) . . ?
C8 O3 Ni2 125.3(4) . . ?
N3 O5 O6 133(2) . 3 ?
N3 O6 O5 115(2) . 2 ?
C2 N1 C1 116.1(5) . . ?
C2 N1 Ni2 127.3(4) . 8_556 ?
C1 N1 Ni2 116.6(4) . 8_556 ?
O4 N2 O4 119.79(9) 2_665 3_565 ?
O4 N2 O4 119.79(9) 2_665 . ?
O4 N2 O4 119.79(9) 3_565 . ?
O6 N3 O5 140(3) . . ?
O6 N3 C10 110(2) . . ?
O5 N3 C10 110(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 126.3(5) . . ?
N1 C2 H2 116.8 . . ?
C3 C2 H2 116.8 . . ?
C9 C3 C4 119.3(5) . . ?
C9 C3 C2 123.2(5) . . ?
C4 C3 C2 117.4(5) . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.9(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 118.8(5) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
C6 C7 O3 123.8(5) . . ?
C6 C7 C9 122.1(5) . . ?
O3 C7 C9 114.1(4) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C3 123.2(5) . . ?
O2 C9 C7 118.1(5) . . ?
C3 C9 C7 118.7(5) . . ?
N3 C10 N3 117.0(18) . 4 ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.881
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.159

# Attachment '[Ni7](3)cif.cif'

data_lfj41c-4
_database_code_depnum_ccdc_archive 'CCDC 741053'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (Ni7(OH)6(L2)6)(NO3)2.2MeCN
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H66 Br6 N10 Ni7 O24'
_chemical_formula_weight         2177.64
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'
Br Br -0.2901 2.4595 '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/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   28.8575(14)
_cell_length_b                   11.1352(3)
_cell_length_c                   27.4079(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.603(6)
_cell_angle_gamma                90.00
_cell_volume                     8296.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4328
_exptl_absorpt_coefficient_mu    4.516
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_exptl_absorpt_correction_T_min  0.79476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan 8 2009,16:24:04)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            18887
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.1312
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.6741
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      0.0205093959
_diffrn_orient_matrix_UB_12      0.0134896450
_diffrn_orient_matrix_UB_13      -0.0077844625
_diffrn_orient_matrix_UB_21      0.0160299555
_diffrn_orient_matrix_UB_22      -0.0113405526
_diffrn_orient_matrix_UB_23      0.0255346062
_diffrn_orient_matrix_UB_31      0.0015659969
_diffrn_orient_matrix_UB_32      -0.0612051726
_diffrn_orient_matrix_UB_33      -0.0064358310
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega 51.00 90.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 19.5778 77.0000 -120.0000 39
#__ type_ start__ end____ width___ exp.time_
2 omega -10.00 87.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 19.5778 77.0000 -150.0000 97
#__ type_ start__ end____ width___ exp.time_
3 omega -21.00 80.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 19.5778 21.0000 -136.0000 101
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      373(2)
_reflns_number_total             7348
_reflns_number_gt                3779
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0677P)²+0.0000P] where P=(Fo²+2Fc²)/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         7348
_refine_ls_number_parameters     467
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1217
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_restrained_S_all      0.852
_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 0.30834(4) 0.32502(8) 0.61337(4) 0.0209(3) Uani 1 1 d . . .
Ni2 Ni 0.36004(4) 0.32193(8) 0.53002(4) 0.0239(3) Uani 1 1 d . . .
Ni3 Ni 0.30592(4) 0.19807(8) 0.42406(4) 0.0203(3) Uani 1 1 d . . .
Ni4 Ni 0.2500 0.2500 0.5000 0.0192(3) Uani 1 2 d S . .
Br1 Br 0.37781(5) 0.94535(8) 0.63389(5) 0.0596(4) Uani 1 1 d . . .
Br2 Br 0.51546(4) -0.19234(9) 0.57124(4) 0.0530(3) Uani 1 1 d . . .
Br3 Br 0.25576(4) 0.72170(7) 0.27376(4) 0.0372(3) Uani 1 1 d . . .
O1 O 0.31542(19) 0.2110(4) 0.55773(19) 0.0213(13) Uani 1 1 d . . .
H1 H 0.3248 0.1272 0.5665 0.026 Uiso 1 1 calc R . .
O2 O 0.29627(19) 0.3396(4) 0.4694(2) 0.0225(13) Uani 1 1 d . . .
H2 H 0.2867 0.4188 0.4536 0.027 Uiso 1 1 calc R . .
O3 O 0.25382(19) 0.1187(4) 0.44759(19) 0.0224(13) Uani 1 1 d . . .
H3A H 0.2573 0.0341 0.4581 0.027 Uiso 1 1 calc R . .
O4 O 0.2452(2) 0.2345(4) 0.36281(19) 0.0201(12) Uani 1 1 d . . .
O5 O 0.3318(2) 0.3317(4) 0.3763(2) 0.0270(14) Uani 1 1 d . . .
O6 O 0.3694(2) 0.1985(4) 0.4815(2) 0.0245(13) Uani 1 1 d . . .
O7 O 0.4323(2) 0.2281(5) 0.5743(2) 0.0373(15) Uani 1 1 d . . .
O8 O 0.3567(2) 0.4177(4) 0.5890(2) 0.0258(14) Uani 1 1 d . . .
O9 O 0.3215(2) 0.5037(4) 0.6582(2) 0.0306(15) Uani 1 1 d . . .
O10 O 0.6073(3) 0.2984(6) 0.6121(3) 0.062(2) Uani 1 1 d . . .
O11 O 0.5910(3) 0.1768(7) 0.6656(3) 0.071(2) Uani 1 1 d . . .
O12 O 0.5991(3) 0.3640(7) 0.6814(4) 0.094(3) Uani 1 1 d . . .
N1 N 0.3991(3) 0.4605(6) 0.5128(3) 0.0304(17) Uiso 1 1 d . . .
N2 N 0.3303(3) 0.0541(5) 0.3945(3) 0.0223(15) Uiso 1 1 d . . .
N3 N 0.1433(2) 0.2563(5) 0.3234(2) 0.0235(15) Uiso 1 1 d . . .
N4 N 0.5995(3) 0.2794(9) 0.6532(4) 0.053(2) Uani 1 1 d . . .
N5 N 0.2518(5) 0.5951(9) 0.4774(5) 0.107(4) Uani 1 1 d . . .
C1 C 0.3307(4) 0.5163(7) 0.7127(3) 0.038(2) Uani 1 1 d . . .
H1A H 0.3651 0.5316 0.7300 0.057 Uiso 1 1 calc R . .
H1B H 0.3215 0.4436 0.7259 0.057 Uiso 1 1 calc R . .
H1C H 0.3118 0.5821 0.7186 0.057 Uiso 1 1 calc R . .
C2 C 0.3444(3) 0.5845(6) 0.6355(3) 0.028(2) Uani 1 1 d . . .
C3 C 0.3479(4) 0.7060(7) 0.6459(4) 0.041(3) Uani 1 1 d . . .
H3 H 0.3354 0.7391 0.6701 0.049 Uiso 1 1 calc R . .
C4 C 0.3705(4) 0.7770(7) 0.6189(4) 0.041(3) Uani 1 1 d . . .
C5 C 0.3865(4) 0.7338(7) 0.5816(4) 0.039(3) Uani 1 1 d . . .
H5 H 0.4002 0.7854 0.5634 0.047 Uiso 1 1 calc R . .
C6 C 0.3608(3) 0.5343(6) 0.5969(3) 0.027(2) Uani 1 1 d . . .
C7 C 0.3824(3) 0.6089(7) 0.5699(3) 0.029(2) Uani 1 1 d . . .
C8 C 0.4022(3) 0.5666(7) 0.5311(3) 0.033(2) Uani 1 1 d . . .
H8 H 0.4190 0.6225 0.5181 0.040 Uiso 1 1 calc R . .
C9 C 0.4246(4) 0.4410(9) 0.4748(4) 0.072(4) Uani 1 1 d . . .
H9A H 0.4375 0.5161 0.4676 0.108 Uiso 1 1 calc R . .
H9B H 0.4019 0.4092 0.4433 0.108 Uiso 1 1 calc R . .
H9C H 0.4512 0.3853 0.4887 0.108 Uiso 1 1 calc R . .
C10 C 0.4774(4) 0.2832(10) 0.6058(4) 0.061(3) Uani 1 1 d . . .
H10A H 0.4920 0.2357 0.6364 0.092 Uiso 1 1 calc R . .
H10B H 0.4707 0.3624 0.6155 0.092 Uiso 1 1 calc R . .
H10C H 0.4997 0.2882 0.5866 0.092 Uiso 1 1 calc R . .
C11 C 0.4362(3) 0.1205(8) 0.5490(3) 0.029(2) Uani 1 1 d . . .
C12 C 0.4704(3) 0.0351(8) 0.5703(4) 0.037(2) Uani 1 1 d . . .
H12 H 0.4935 0.0446 0.6032 0.044 Uiso 1 1 calc R . .
C13 C 0.4698(3) -0.0668(7) 0.5411(4) 0.034(2) Uani 1 1 d . . .
C14 C 0.4363(3) -0.0845(7) 0.4927(4) 0.034(2) Uani 1 1 d . . .
H14 H 0.4369 -0.1547 0.4745 0.041 Uiso 1 1 calc R . .
C15 C 0.4008(3) 0.1113(7) 0.5005(3) 0.0227(19) Uani 1 1 d . . .
C16 C 0.4006(3) 0.0056(7) 0.4705(3) 0.025(2) Uani 1 1 d . . .
C17 C 0.3674(3) -0.0124(6) 0.4188(3) 0.022(2) Uani 1 1 d . . .
H17 H 0.3732 -0.0787 0.4010 0.026 Uiso 1 1 calc R . .
C18 C 0.3034(4) 0.0167(8) 0.3423(4) 0.051(3) Uani 1 1 d . . .
H18A H 0.3228 -0.0400 0.3310 0.077 Uiso 1 1 calc R . .
H18B H 0.2966 0.0853 0.3198 0.077 Uiso 1 1 calc R . .
H18C H 0.2731 -0.0202 0.3413 0.077 Uiso 1 1 calc R . .
C19 C 0.0904(3) 0.2185(8) 0.3047(4) 0.042(2) Uani 1 1 d . . .
H19A H 0.0730 0.2612 0.3235 0.063 Uiso 1 1 calc R . .
H19B H 0.0883 0.1337 0.3101 0.063 Uiso 1 1 calc R . .
H19C H 0.0761 0.2362 0.2684 0.063 Uiso 1 1 calc R . .
C20 C 0.1534(3) 0.3457(6) 0.2981(3) 0.0238(19) Uani 1 1 d . . .
H20 H 0.1280 0.3771 0.2704 0.029 Uiso 1 1 calc R . .
C21 C 0.2022(3) 0.3997(6) 0.3105(3) 0.0169(18) Uani 1 1 d . . .
C22 C 0.2451(3) 0.3406(6) 0.3410(3) 0.022(2) Uani 1 1 d . . .
C23 C 0.2910(3) 0.3978(6) 0.3482(3) 0.0197(19) Uani 1 1 d . . .
C24 C 0.2940(3) 0.5097(6) 0.3287(3) 0.023(2) Uani 1 1 d . . .
H24 H 0.3242 0.5474 0.3348 0.027 Uiso 1 1 calc R . .
C25 C 0.2507(4) 0.5642(6) 0.2995(3) 0.027(2) Uani 1 1 d . . .
C26 C 0.2062(3) 0.5129(6) 0.2903(3) 0.0210(19) Uani 1 1 d . . .
H26 H 0.1780 0.5533 0.2704 0.025 Uiso 1 1 calc R . .
C27 C 0.3671(3) 0.3124(9) 0.3507(4) 0.053(3) Uani 1 1 d . . .
H27A H 0.3511 0.2768 0.3174 0.080 Uiso 1 1 calc R . .
H27B H 0.3925 0.2597 0.3712 0.080 Uiso 1 1 calc R . .
H27C H 0.3814 0.3879 0.3463 0.080 Uiso 1 1 calc R . .
C29 C 0.2682(5) 0.6622(11) 0.4576(5) 0.080(4) Uani 1 1 d . . .
C30 C 0.2884(5) 0.7528(11) 0.4333(6) 0.095(5) Uani 1 1 d . . .
H30A H 0.2922 0.7207 0.4024 0.143 Uiso 1 1 calc R . .
H30B H 0.3198 0.7778 0.4567 0.143 Uiso 1 1 calc R . .
H30C H 0.2665 0.8205 0.4245 0.143 Uiso 1 1 calc R . .
_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 O4 1.984(5) 7_556 ?
Ni1 O8 2.020(5) . ?
Ni1 N3 2.036(7) 7_556 ?
Ni1 O1 2.046(5) . ?
Ni1 O3 2.096(5) 7_556 ?
Ni1 O9 2.302(5) . ?
Ni2 O8 1.966(5) . ?
Ni2 O6 1.993(5) . ?
Ni2 O2 2.034(6) . ?
Ni2 N1 2.056(6) . ?
Ni2 O1 2.101(5) . ?
Ni2 O7 2.283(6) . ?
Ni3 O6 1.975(6) . ?
Ni3 O4 2.019(6) . ?
Ni3 N2 2.027(6) . ?
Ni3 O3 2.027(5) . ?
Ni3 O2 2.083(5) . ?
Ni3 O5 2.266(5) . ?
Ni4 O2 2.058(4) 7_556 ?
Ni4 O2 2.058(4) . ?
Ni4 O1 2.062(5) . ?
Ni4 O1 2.062(5) 7_556 ?
Ni4 O3 2.079(4) 7_556 ?
Ni4 O3 2.079(4) . ?
Br1 C4 1.915(8) . ?
Br2 C13 1.909(8) . ?
Br3 C25 1.915(7) . ?
O1 H1 0.9800 . ?
O2 H2 0.9800 . ?
O3 Ni1 2.096(5) 7_556 ?
O3 H3A 0.9800 . ?
O4 C22 1.324(8) . ?
O4 Ni1 1.984(5) 7_556 ?
O5 C23 1.383(9) . ?
O5 C27 1.437(9) . ?
O6 C15 1.312(9) . ?
O7 C11 1.408(9) . ?
O7 C10 1.436(11) . ?
O8 C6 1.316(8) . ?
O9 C2 1.382(8) . ?
O9 C1 1.433(9) . ?
O10 N4 1.237(10) . ?
O11 N4 1.239(10) . ?
O12 N4 1.222(9) . ?
N1 C8 1.275(9) . ?
N1 C9 1.481(10) . ?
N2 C17 1.287(10) . ?
N2 C18 1.441(11) . ?
N3 C20 1.302(9) . ?
N3 C19 1.497(10) . ?
N3 Ni1 2.036(7) 7_556 ?
N5 C29 1.117(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.379(10) . ?
C2 C6 1.411(10) . ?
C3 C4 1.387(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.344(11) . ?
C5 C7 1.423(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(10) . ?
C7 C8 1.446(10) . ?
C8 H8 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.354(11) . ?
C11 C15 1.380(11) . ?
C12 C13 1.384(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(13) . ?
C14 C16 1.421(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.434(11) . ?
C16 C17 1.435(11) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.461(10) . ?
C20 H20 0.9300 . ?
C21 C26 1.397(10) . ?
C21 C22 1.405(11) . ?
C22 C23 1.420(10) . ?
C23 C24 1.371(10) . ?
C24 C25 1.378(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.350(11) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 C30 1.436(16) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
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
O4 Ni1 O8 168.66(19) 7_556 . ?
O4 Ni1 N3 87.7(2) 7_556 7_556 ?
O8 Ni1 N3 98.9(2) . 7_556 ?
O4 Ni1 O1 108.77(19) 7_556 . ?
O8 Ni1 O1 79.51(19) . . ?
N3 Ni1 O1 98.4(2) 7_556 . ?
O4 Ni1 O3 79.0(2) 7_556 7_556 ?
O8 Ni1 O3 94.9(2) . 7_556 ?
N3 Ni1 O3 166.0(2) 7_556 7_556 ?
O1 Ni1 O3 82.2(2) . 7_556 ?
O4 Ni1 O9 96.92(18) 7_556 . ?
O8 Ni1 O9 74.12(18) . . ?
N3 Ni1 O9 89.3(2) 7_556 . ?
O1 Ni1 O9 153.38(18) . . ?
O3 Ni1 O9 96.4(2) 7_556 . ?
O8 Ni2 O6 167.9(2) . . ?
O8 Ni2 O2 109.8(2) . . ?
O6 Ni2 O2 79.0(2) . . ?
O8 Ni2 N1 87.9(2) . . ?
O6 Ni2 N1 99.0(2) . . ?
O2 Ni2 N1 98.9(2) . . ?
O8 Ni2 O1 79.40(19) . . ?
O6 Ni2 O1 94.18(19) . . ?
O2 Ni2 O1 81.71(19) . . ?
N1 Ni2 O1 166.7(2) . . ?
O8 Ni2 O7 95.7(2) . . ?
O6 Ni2 O7 74.6(2) . . ?
O2 Ni2 O7 153.28(19) . . ?
N1 Ni2 O7 89.6(3) . . ?
O1 Ni2 O7 95.8(2) . . ?
O6 Ni3 O4 167.46(19) . . ?
O6 Ni3 N2 88.1(2) . . ?
O4 Ni3 N2 98.5(2) . . ?
O6 Ni3 O3 109.7(2) . . ?
O4 Ni3 O3 79.8(2) . . ?
N2 Ni3 O3 100.2(2) . . ?
O6 Ni3 O2 78.3(2) . . ?
O4 Ni3 O2 95.3(2) . . ?
N2 Ni3 O2 166.3(3) . . ?
O3 Ni3 O2 83.01(18) . . ?
O6 Ni3 O5 93.5(2) . . ?
O4 Ni3 O5 75.5(2) . . ?
N2 Ni3 O5 93.6(2) . . ?
O3 Ni3 O5 153.2(2) . . ?
O2 Ni3 O5 89.03(18) . . ?
O2 Ni4 O2 180.00(19) 7_556 . ?
O2 Ni4 O1 97.90(19) 7_556 . ?
O2 Ni4 O1 82.10(19) . . ?
O2 Ni4 O1 82.10(19) 7_556 7_556 ?
O2 Ni4 O1 97.90(19) . 7_556 ?
O1 Ni4 O1 180.000(1) . 7_556 ?
O2 Ni4 O3 82.37(18) 7_556 7_556 ?
O2 Ni4 O3 97.63(18) . 7_556 ?
O1 Ni4 O3 82.24(19) . 7_556 ?
O1 Ni4 O3 97.76(19) 7_556 7_556 ?
O2 Ni4 O3 97.63(18) 7_556 . ?
O2 Ni4 O3 82.37(18) . . ?
O1 Ni4 O3 97.76(19) . . ?
O1 Ni4 O3 82.24(19) 7_556 . ?
O3 Ni4 O3 180.000(1) 7_556 . ?
Ni1 O1 Ni4 98.4(2) . . ?
Ni1 O1 Ni2 97.55(19) . . ?
Ni4 O1 Ni2 96.5(2) . . ?
Ni1 O1 H1 119.8 . . ?
Ni4 O1 H1 119.8 . . ?
Ni2 O1 H1 119.8 . . ?
Ni2 O2 Ni4 98.8(2) . . ?
Ni2 O2 Ni3 98.6(2) . . ?
Ni4 O2 Ni3 96.39(19) . . ?
Ni2 O2 H2 119.4 . . ?
Ni4 O2 H2 119.4 . . ?
Ni3 O2 H2 119.4 . . ?
Ni3 O3 Ni4 97.5(2) . . ?
Ni3 O3 Ni1 98.3(2) . 7_556 ?
Ni4 O3 Ni1 96.36(19) . 7_556 ?
Ni3 O3 H3A 119.9 . . ?
Ni4 O3 H3A 119.9 . . ?
Ni1 O3 H3A 119.9 7_556 . ?
C22 O4 Ni1 124.3(5) . 7_556 ?
C22 O4 Ni3 115.2(5) . . ?
Ni1 O4 Ni3 102.3(2) 7_556 . ?
C23 O5 C27 114.8(6) . . ?
C23 O5 Ni3 106.7(4) . . ?
C27 O5 Ni3 127.6(5) . . ?
C15 O6 Ni3 130.4(5) . . ?
C15 O6 Ni2 118.4(5) . . ?
Ni3 O6 Ni2 103.7(2) . . ?
C11 O7 C10 116.9(7) . . ?
C11 O7 Ni2 109.7(5) . . ?
C10 O7 Ni2 127.3(6) . . ?
C6 O8 Ni2 130.1(5) . . ?
C6 O8 Ni1 119.0(4) . . ?
Ni2 O8 Ni1 103.0(2) . . ?
C2 O9 C1 117.1(6) . . ?
C2 O9 Ni1 109.9(4) . . ?
C1 O9 Ni1 125.5(4) . . ?
C8 N1 C9 115.2(7) . . ?
C8 N1 Ni2 125.3(5) . . ?
C9 N1 Ni2 119.5(5) . . ?
C17 N2 C18 115.1(7) . . ?
C17 N2 Ni3 126.0(6) . . ?
C18 N2 Ni3 118.8(6) . . ?
C20 N3 C19 114.7(7) . . ?
C20 N3 Ni1 125.4(6) . 7_556 ?
C19 N3 Ni1 119.7(5) . 7_556 ?
O12 N4 O10 119.2(10) . . ?
O12 N4 O11 119.5(10) . . ?
O10 N4 O11 121.3(8) . . ?
O9 C1 H1A 109.5 . . ?
O9 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O9 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O9 123.9(6) . . ?
C3 C2 C6 121.6(7) . . ?
O9 C2 C6 114.3(6) . . ?
C2 C3 C4 117.6(7) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C5 C4 C3 123.0(7) . . ?
C5 C4 Br1 118.2(6) . . ?
C3 C4 Br1 118.7(6) . . ?
C4 C5 C7 119.8(7) . . ?
C4 C5 H5 120.1 . . ?
C7 C5 H5 120.1 . . ?
O8 C6 C7 122.3(6) . . ?
O8 C6 C2 118.6(6) . . ?
C7 C6 C2 119.0(6) . . ?
C6 C7 C5 118.9(7) . . ?
C6 C7 C8 123.7(7) . . ?
C5 C7 C8 117.4(7) . . ?
N1 C8 C7 126.7(7) . . ?
N1 C8 H8 116.6 . . ?
C7 C8 H8 116.6 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O7 C10 H10A 109.5 . . ?
O7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C15 124.0(8) . . ?
C12 C11 O7 123.5(9) . . ?
C15 C11 O7 112.4(7) . . ?
C11 C12 C13 117.4(9) . . ?
C11 C12 H12 121.3 . . ?
C13 C12 H12 121.3 . . ?
C14 C13 C12 123.1(8) . . ?
C14 C13 Br2 118.3(7) . . ?
C12 C13 Br2 118.5(8) . . ?
C13 C14 C16 119.2(8) . . ?
C13 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
O6 C15 C11 121.2(7) . . ?
O6 C15 C16 120.6(8) . . ?
C11 C15 C16 118.2(8) . . ?
C14 C16 C15 118.1(8) . . ?
C14 C16 C17 118.1(7) . . ?
C15 C16 C17 123.7(7) . . ?
N2 C17 C16 126.4(7) . . ?
N2 C17 H17 116.8 . . ?
C16 C17 H17 116.8 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 C21 124.3(8) . . ?
N3 C20 H20 117.9 . . ?
C21 C20 H20 117.9 . . ?
C26 C21 C22 119.0(7) . . ?
C26 C21 C20 118.8(8) . . ?
C22 C21 C20 122.2(7) . . ?
O4 C22 C21 123.7(7) . . ?
O4 C22 C23 118.4(8) . . ?
C21 C22 C23 117.9(7) . . ?
C24 C23 O5 123.2(7) . . ?
C24 C23 C22 122.1(8) . . ?
O5 C23 C22 114.7(6) . . ?
C23 C24 C25 117.5(8) . . ?
C23 C24 H24 121.2 . . ?
C25 C24 H24 121.2 . . ?
C26 C25 C24 122.9(7) . . ?
C26 C25 Br3 120.3(7) . . ?
C24 C25 Br3 116.8(6) . . ?
C25 C26 C21 120.5(8) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
O5 C27 H27A 109.5 . . ?
O5 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O5 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N5 C29 C30 177.4(15) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         1.892
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.142


