#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114022.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4114022
loop_
_publ_author_name
'Xiang Lin'
'Dan M. J. Doble'
'Alexander J. Blake'
'Andrew Harrison'
'Claire Wilson'
'Martin Schröder'
_publ_section_title
;
 Cationic Assembly of Metal Complex Aggregates: Structural Diversity,
 Solution Stability, and Magnetic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9476
_journal_page_last               9483
_journal_paper_doi               10.1021/ja0341438
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C84 H124 Cl3 N18 Na4 Ni9 O53.5'
_chemical_formula_weight         2968.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens
'CH3 found in delta-F, CH2 placed geometrically, solvent Hs not found'
_atom_sites_solution_primary     'Heavy atom methods'
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   17.008(2)
_cell_length_b                   17.008(2)
_cell_length_c                   25.054(5)
_cell_measurement_reflns_used    220
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      0
_cell_volume                     6276.5(16)
_computing_cell_refinement       'IPDS (1995)'
_computing_data_collection       'IPDS (1995)'
_computing_data_reduction        'IPDS (1995)'
_computing_molecular_graphics    'SHELXTL/PC (Version 5.03, Sheldrick, 1994)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997); PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe Imaging plate diffractometer system'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_av_sigmaI/netI    0.093
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24548
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(HABITUS; Herrendorf, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_F_000             3058
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.22
_refine_diff_density_rms         0.14
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    'riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.138P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.179
_refine_ls_wR_factor_ref         0.199
_reflns_number_gt                7728
_reflns_number_total             10027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_11.cif
_cod_data_source_block           NIXCLU_Compound_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.138P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.138P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6276.8(18)
_cod_original_formula_sum        'C84 H124 Cl3 N18 Na4 Ni9 O53.50'
_cod_database_code               4114022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.46307(5) 0.23067(5) 0.09161(3) 0.02755(19) Uani 1 d . . .
Ni2 Ni 0.76029(6) 0.22324(6) 0.40155(3) 0.02873(19) Uani 1 d . . .
Ni3 Ni 0.51231(6) 0.03709(4) 0.24646(3) 0.02913(18) Uani 1 d . . .
Na1 Na 0.6667 0.3333 0.15373(19) 0.0542(14) Uani 1 d S . .
Na2 Na 0.7615(3) 0.2307(3) 0.24674(15) 0.0367(7) Uani 0.67 d P . .
Na3 Na 0.6667 0.3333 0.3397(2) 0.0563(15) Uani 1 d S . .
C11 C 0.3119(6) 0.1336(6) -0.0010(3) 0.0440(17) Uani 1 d . . .
H11A H 0.3509 0.1081 -0.0074 0.053 Uiso 1 calc R . .
H11B H 0.2630 0.1066 -0.0269 0.053 Uiso 1 calc R . .
C2A C 0.2704(4) 0.1035(5) 0.0542(3) 0.0384(15) Uani 1 d . . .
H2A1 H 0.2426 0.1387 0.0653 0.046 Uiso 1 calc R . .
H2A2 H 0.2236 0.0400 0.0533 0.046 Uiso 1 calc R . .
N3A N 0.3409(3) 0.1165(4) 0.0921(2) 0.0294(10) Uani 1 d . . .
C4A C 0.3322(5) 0.0591(4) 0.1282(2) 0.0325(13) Uani 1 d . . .
C5A C 0.4168(5) 0.0897(4) 0.1633(2) 0.0297(12) Uani 1 d . . .
O6A O 0.4779(3) 0.1721(3) 0.16066(17) 0.0359(10) Uani 1 d . . .
O7A O 0.4180(4) 0.0290(3) 0.19130(18) 0.0379(10) Uani 1 d . . .
C8A C 0.2494(5) -0.0298(6) 0.1422(3) 0.0507(19) Uani 1 d . . .
H8A1 H 0.2041 -0.0457 0.1150 0.076 Uiso 1 calc R . .
H8A2 H 0.2256 -0.0240 0.1758 0.076 Uiso 1 calc R . .
H8A3 H 0.2655 -0.0763 0.1448 0.076 Uiso 1 calc R . .
C2B C 0.3663(5) 0.2338(5) -0.0126(3) 0.0444(17) Uani 1 d . . .
H2B1 H 0.3872 0.2423 -0.0493 0.053 Uiso 1 calc R . .
H2B2 H 0.3269 0.2596 -0.0091 0.053 Uiso 1 calc R . .
N3B N 0.4451(4) 0.2837(4) 0.0225(2) 0.0305(11) Uani 1 d . . .
C4B C 0.5090(5) 0.3643(4) 0.0114(2) 0.0298(12) Uani 1 d . . .
C5B C 0.5860(4) 0.4049(4) 0.0522(2) 0.0273(11) Uani 1 d . . .
O6B O 0.5801(3) 0.3529(3) 0.09059(16) 0.0297(9) Uani 1 d . . .
O7B O 0.6481(3) 0.4839(3) 0.04608(17) 0.0329(9) Uani 1 d . . .
C8B C 0.5121(5) 0.4178(5) -0.0369(3) 0.0432(16) Uani 1 d . . .
H8B1 H 0.5177 0.3888 -0.0684 0.065 Uiso 1 calc R . .
H8B2 H 0.5633 0.4781 -0.0344 0.065 Uiso 1 calc R . .
H8B3 H 0.4573 0.4208 -0.0389 0.065 Uiso 1 calc R . .
C12 C 0.8044(6) 0.1201(5) 0.4957(3) 0.0470(18) Uani 1 d . . .
H12A H 0.8232 0.0907 0.5218 0.056 Uiso 1 calc R . .
H12B H 0.7407 0.0992 0.5020 0.056 Uiso 1 calc R . .
C2C C 0.8131(5) 0.0879(5) 0.4408(3) 0.0419(16) Uani 1 d . . .
H2C1 H 0.8762 0.1203 0.4298 0.050 Uiso 1 calc R . .
H2C2 H 0.7934 0.0237 0.4422 0.050 Uiso 1 calc R . .
N3C N 0.7581(4) 0.1032(4) 0.4017(2) 0.0316(11) Uani 1 d . . .
C4C C 0.7069(5) 0.0472(4) 0.3661(2) 0.0341(13) Uani 1 d . . .
C5C C 0.6582(5) 0.0817(4) 0.3305(2) 0.0326(13) Uani 1 d . . .
O6C O 0.6863(4) 0.1676(3) 0.33250(16) 0.0349(10) Uani 1 d . . .
O7C O 0.5960(4) 0.0253(4) 0.30200(19) 0.0409(11) Uani 1 d . . .
C8C C 0.6910(7) -0.0467(6) 0.3553(3) 0.055(2) Uani 1 d . . .
H8C1 H 0.7112 -0.0491 0.3199 0.083 Uiso 1 calc R . .
H8C2 H 0.6274 -0.0899 0.3584 0.083 Uiso 1 calc R . .
H8C3 H 0.7242 -0.0610 0.3807 0.083 Uiso 1 calc R . .
C2D C 0.8579(6) 0.2223(6) 0.5060(3) 0.0491(18) Uani 1 d . . .
H2D1 H 0.8492 0.2338 0.5428 0.059 Uiso 1 calc R . .
H2D2 H 0.9220 0.2440 0.5008 0.059 Uiso 1 calc R . .
N3D N 0.8301(4) 0.2729(4) 0.4708(2) 0.0328(11) Uani 1 d . . .
C4D C 0.8492(5) 0.3543(5) 0.4818(2) 0.0329(13) Uani 1 d . . .
C5D C 0.8176(4) 0.3972(4) 0.4399(3) 0.0303(12) Uani 1 d . . .
O6D O 0.7715(3) 0.3477(3) 0.40213(16) 0.0313(9) Uani 1 d . . .
O7D O 0.8370(3) 0.4784(3) 0.44779(17) 0.0339(10) Uani 1 d . . .
C8D C 0.8993(5) 0.4064(5) 0.5312(3) 0.0439(16) Uani 1 d . . .
H8D1 H 0.8710 0.3702 0.5623 0.066 Uiso 1 calc R . .
H8D2 H 0.8974 0.4618 0.5332 0.066 Uiso 1 calc R . .
H8D3 H 0.9613 0.4203 0.5294 0.066 Uiso 1 calc R . .
C13 C 0.4272(15) -0.1798(16) 0.2679(8) 0.033(6) Uiso 0.30(2) d P A 1
H13A H 0.3971 -0.2454 0.2706 0.040 Uiso 0.30(2) calc PR A 1
H13B H 0.4757 -0.1556 0.2941 0.040 Uiso 0.30(2) calc PR A 1
C13' C 0.3777(7) -0.1812(7) 0.2289(5) 0.045(3) Uani 0.70(2) d P A 2
H13C H 0.3406 -0.2467 0.2258 0.054 Uiso 0.70(2) calc PR A 2
H13D H 0.3548 -0.1548 0.2032 0.054 Uiso 0.70(2) calc PR A 2
C2E C 0.4716(6) -0.1549(5) 0.2136(3) 0.0489(19) Uani 1 d . . .
H2EA H 0.5098 -0.1818 0.2095 0.059 Uiso 0.30(2) calc PR A 1
H2EB H 0.4247 -0.1809 0.1865 0.059 Uiso 0.30(2) calc PR A 1
H2EA H 0.4705 -0.1870 0.1814 0.059 Uiso 0.70(2) calc PR A 2
H2EB H 0.4990 -0.1724 0.2417 0.059 Uiso 0.70(2) calc PR A 2
N3E N 0.5266(4) -0.0570(4) 0.2045(2) 0.0347(12) Uani 1 d . . .
C4E C 0.5915(5) -0.0270(5) 0.1703(3) 0.0368(14) Uani 1 d . . .
C5E C 0.6462(4) 0.0791(4) 0.1677(2) 0.0303(12) Uani 1 d . . .
O6E O 0.6261(3) 0.1219(3) 0.20042(17) 0.0331(9) Uani 1 d . . .
O7E O 0.7061(4) 0.1098(3) 0.1319(2) 0.0404(11) Uani 1 d . . .
C8E C 0.6200(7) -0.0801(6) 0.1364(4) 0.063(3) Uani 1 d . . .
H8E1 H 0.6586 -0.0951 0.1568 0.095 Uiso 1 calc R . .
H8E2 H 0.6525 -0.0447 0.1059 0.095 Uiso 1 calc R . .
H8E3 H 0.5674 -0.1350 0.1248 0.095 Uiso 1 calc R . .
C2F C 0.3645(6) -0.1543(5) 0.2840(3) 0.0493(19) Uani 1 d . . .
H2FA H 0.3375 -0.1840 0.3176 0.059 Uiso 0.30(2) calc PR A 1
H2FB H 0.3163 -0.1753 0.2577 0.059 Uiso 0.30(2) calc PR A 1
H2FA H 0.3000 -0.1834 0.2915 0.059 Uiso 0.70(2) calc PR A 2
H2FB H 0.3913 -0.1765 0.3099 0.059 Uiso 0.70(2) calc PR A 2
N3F N 0.4055(4) -0.0543(4) 0.2908(2) 0.0347(12) Uani 1 d . . .
C4F C 0.3782(5) -0.0206(4) 0.3269(3) 0.0372(15) Uani 1 d . . .
C5F C 0.4263(5) 0.0832(5) 0.3269(2) 0.0340(13) Uani 1 d . . .
O6F O 0.4877(3) 0.1243(3) 0.29232(17) 0.0341(10) Uani 1 d . . .
O7F O 0.3987(3) 0.1167(3) 0.3603(2) 0.0397(11) Uani 1 d . . .
C8F C 0.3074(8) -0.0727(7) 0.3680(4) 0.080(4) Uani 1 d . . .
H8F1 H 0.2517 -0.0753 0.3581 0.120 Uiso 1 calc R . .
H8F2 H 0.3273 -0.0432 0.4020 0.120 Uiso 1 calc R . .
H8F3 H 0.2979 -0.1332 0.3704 0.120 Uiso 1 calc R . .
Cl1 Cl 0.6667 0.3333 -0.08778(11) 0.0398(6) Uani 1 d SD . .
O11 O 0.6667 0.3333 -0.0305(2) 0.050(2) Uani 1 d SD . .
O12 O 0.5748(4) 0.2917(5) -0.1070(3) 0.073(2) Uani 1 d D . .
Cl2 Cl 0.6667 0.3333 0.59074(13) 0.0491(7) Uani 1 d SD . .
O21 O 0.6667 0.3333 0.5332(3) 0.068(3) Uani 1 d SD . .
O22 O 0.7190(5) 0.2931(5) 0.6099(3) 0.086(3) Uani 1 d D . .
O O 0.6912(11) 0.3068(11) 0.2459(5) 0.051(4) Uani 0.33 d P . .
Cl3 Cl 1.0000 0.0000 0.5000 0.167(6) Uani 1 d SD . .
O3 O 0.966(3) 0.036(4) 0.5405(12) 0.150 Uiso 0.33 d PD . 1
O3' O 0.936(3) 0.025(4) 0.5212(16) 0.150 Uiso 0.33 d PD . 2
Cl4 Cl 0.0000 0.0000 0.0000 0.160(6) Uani 1 d SD . .
O4 O 0.086(3) 0.003(6) -0.003(4) 0.09(4) Uiso 0.11(4) d PD . 1
O4' O 0.0797(14) 0.028(2) -0.0334(13) 0.157(13) Uiso 0.56(4) d PD . 2
O1M O 0.8420(11) 0.1519(10) 0.2468(5) 0.084(3) Uani 0.67 d PD . .
C1M C 0.8342(12) 0.0703(11) 0.2219(7) 0.055(4) Uiso 0.50 d PD B 1
C1M' C 0.922(3) 0.149(5) 0.266(3) 0.073(16) Uiso 0.17 d PD B 2
O1W O 0.8638(13) 0.1050(13) 0.2445(8) 0.059(4) Uiso 0.33 d P C 3
C2M C 1.025(2) 0.2061(19) 0.2867(10) 0.065(7) Uiso 0.33 d PD D 3
O2M O 1.0059(15) 0.1450(14) 0.3319(8) 0.068(5) Uiso 0.33 d PD D 3
O2W O 0.025(10) -0.087(10) 0.178(5) 0.13(4) Uiso 0.08 d P E 4
O2W' O 0.122(5) -0.039(5) 0.296(3) 0.050(14) Uiso 0.08 d P F 4
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N3A Ni1 O6B 174.5(2) . . y
N3A Ni1 N3B 96.9(2) . . y
O6B Ni1 N3B 79.9(2) . . y
N3A Ni1 O7E 87.8(2) . 3_665 y
O6B Ni1 O7E 87.59(19) . 3_665 y
N3B Ni1 O7E 87.9(2) . 3_665 y
N3A Ni1 O6A 81.2(2) . . y
O6B Ni1 O6A 102.07(18) . . y
N3B Ni1 O6A 177.9(2) . . y
O7E Ni1 O6A 92.9(2) 3_665 . y
N3A Ni1 O7B 89.89(19) . 2_655 y
O6B Ni1 O7B 94.53(18) . 2_655 y
N3B Ni1 O7B 88.69(19) . 2_655 y
O7E Ni1 O7B 175.63(18) 3_665 2_655 y
O6A Ni1 O7B 90.36(19) . 2_655 y
N3A Ni1 Na1 142.44(16) . . ?
O6B Ni1 Na1 41.59(13) . . ?
N3B Ni1 Na1 120.19(17) . . ?
O7E Ni1 Na1 98.49(14) 3_665 . ?
O6A Ni1 Na1 61.61(14) . . ?
O7B Ni1 Na1 85.60(13) 2_655 . ?
O6D Ni2 N3C 176.2(2) . . y
O6D Ni2 N3D 80.2(2) . . y
N3C Ni2 N3D 97.4(2) . . y
O6D Ni2 O6C 101.65(17) . . y
N3C Ni2 O6C 80.8(2) . . y
N3D Ni2 O6C 177.7(2) . . y
O6D Ni2 O7F 87.4(2) . 2_655 y
N3C Ni2 O7F 89.6(2) . 2_655 y
N3D Ni2 O7F 89.2(2) . 2_655 y
O6C Ni2 O7F 92.3(2) . 2_655 y
O6D Ni2 O7D 94.05(18) . 3_665 y
N3C Ni2 O7D 88.81(19) . 3_665 y
N3D Ni2 O7D 87.2(2) . 3_665 y
O6C Ni2 O7D 91.22(19) . 3_665 y
O7F Ni2 O7D 175.86(19) 2_655 3_665 y
O6D Ni2 Na3 41.38(13) . . ?
N3C Ni2 Na3 141.65(17) . . ?
N3D Ni2 Na3 119.99(17) . . ?
O6C Ni2 Na3 61.52(14) . . ?
O7F Ni2 Na3 98.34(14) 2_655 . ?
O7D Ni2 Na3 85.28(13) 3_665 . ?
N3E Ni3 N3F 95.42(18) . . y
N3E Ni3 O7A 89.8(2) . . y
N3F Ni3 O7A 87.0(2) . . y
N3E Ni3 O7C 85.0(2) . . y
N3F Ni3 O7C 87.3(2) . . y
O7A Ni3 O7C 171.88(16) . . y
N3E Ni3 O6E 79.81(19) . . y
N3F Ni3 O6E 174.6(2) . . y
O7A Ni3 O6E 95.55(19) . . y
O7C Ni3 O6E 89.6(2) . . y
N3E Ni3 O6F 175.1(2) . . y
N3F Ni3 O6F 79.7(2) . . y
O7A Ni3 O6F 89.45(19) . . y
O7C Ni3 O6F 95.24(19) . . y
O6E Ni3 O6F 105.11(15) . . y
O6B Na1 O6B 77.7(2) 2_655 3_665 ?
O6B Na1 O6B 77.7(2) 2_655 . ?
O6B Na1 O6B 77.7(2) 3_665 . ?
O6B Na1 O 118.7(4) 2_655 . ?
O6B Na1 O 128.4(4) 3_665 . ?
O6B Na1 O 149.8(4) . . ?
O6B Na1 O 149.8(4) 2_655 2_655 ?
O6B Na1 O 118.7(4) 3_665 2_655 ?
O6B Na1 O 128.4(4) . 2_655 ?
O Na1 O 31.2(7) . 2_655 ?
O6B Na1 O 128.4(4) 2_655 3_665 ?
O6B Na1 O 149.8(4) 3_665 3_665 ?
O6B Na1 O 118.7(4) . 3_665 ?
O Na1 O 31.2(7) . 3_665 ?
O Na1 O 31.2(7) 2_655 3_665 ?
O6B Na1 O6A 72.70(14) 2_655 2_655 ?
O6B Na1 O6A 69.76(14) 3_665 2_655 ?
O6B Na1 O6A 139.7(2) . 2_655 ?
O Na1 O6A 70.2(4) . 2_655 ?
O Na1 O6A 88.9(4) 2_655 2_655 ?
O Na1 O6A 101.2(4) 3_665 2_655 ?
O6B Na1 O6A 69.76(14) 2_655 . ?
O6B Na1 O6A 139.7(2) 3_665 . ?
O6B Na1 O6A 72.70(14) . . ?
O Na1 O6A 88.9(4) . . ?
O Na1 O6A 101.2(4) 2_655 . ?
O Na1 O6A 70.2(4) 3_665 . ?
O6A Na1 O6A 119.67(2) 2_655 . ?
O6B Na1 O6A 139.7(2) 2_655 3_665 ?
O6B Na1 O6A 72.70(14) 3_665 3_665 ?
O6B Na1 O6A 69.76(14) . 3_665 ?
O Na1 O6A 101.2(4) . 3_665 ?
O Na1 O6A 70.2(4) 2_655 3_665 ?
O Na1 O6A 88.9(4) 3_665 3_665 ?
O6A Na1 O6A 119.67(2) 2_655 3_665 ?
O6A Na1 O6A 119.67(2) . 3_665 ?
O6B Na1 Ni1 36.07(11) 2_655 2_655 ?
O6B Na1 Ni1 64.41(13) 3_665 2_655 ?
O6B Na1 Ni1 106.74(19) . 2_655 ?
O Na1 Ni1 99.4(4) . 2_655 ?
O Na1 Ni1 124.7(4) 2_655 2_655 ?
O Na1 Ni1 125.6(4) 3_665 2_655 ?
O6A Na1 Ni1 37.33(9) 2_655 2_655 ?
O6A Na1 Ni1 98.65(11) . 2_655 ?
O6A Na1 Ni1 136.43(13) 3_665 2_655 ?
O6B Na1 Ni1 64.41(13) 2_655 . ?
O6B Na1 Ni1 106.74(19) 3_665 . ?
O6B Na1 Ni1 36.07(11) . . ?
O Na1 Ni1 124.7(4) . . ?
O Na1 Ni1 125.6(4) 2_655 . ?
O Na1 Ni1 99.4(4) 3_665 . ?
O6A Na1 Ni1 136.43(13) 2_655 . ?
O6A Na1 Ni1 37.33(9) . . ?
O6A Na1 Ni1 98.65(11) 3_665 . ?
Ni1 Na1 Ni1 100.47(9) 2_655 . ?
O6B Na1 Ni1 106.74(19) 2_655 3_665 ?
O6B Na1 Ni1 36.07(11) 3_665 3_665 ?
O6B Na1 Ni1 64.41(13) . 3_665 ?
O Na1 Ni1 125.6(4) . 3_665 ?
O Na1 Ni1 99.4(4) 2_655 3_665 ?
O Na1 Ni1 124.7(4) 3_665 3_665 ?
O6A Na1 Ni1 98.65(11) 2_655 3_665 ?
O6A Na1 Ni1 136.43(13) . 3_665 ?
O6A Na1 Ni1 37.33(9) 3_665 3_665 ?
Ni1 Na1 Ni1 100.47(9) 2_655 3_665 ?
Ni1 Na1 Ni1 100.47(9) . 3_665 ?
O1M Na2 O6F 96.2(4) . 2_655 ?
O1M Na2 O6E 99.7(4) . . ?
O6F Na2 O6E 164.1(2) 2_655 . ?
O1M Na2 O6A 92.8(4) . 2_655 ?
O6F Na2 O6A 89.1(2) 2_655 2_655 ?
O6E Na2 O6A 89.49(19) . 2_655 ?
O1M Na2 O6C 94.3(4) . . ?
O6F Na2 O6C 89.7(2) 2_655 . ?
O6E Na2 O6C 89.8(2) . . ?
O6A Na2 O6C 172.9(2) 2_655 . ?
O1M Na2 C5A 75.1(4) . 2_655 ?
O6F Na2 C5A 76.0(2) 2_655 2_655 ?
O6E Na2 C5A 107.4(2) . 2_655 ?
O6A Na2 C5A 23.54(16) 2_655 2_655 ?
O6C Na2 C5A 160.9(2) . 2_655 ?
O1M Na2 C5E 80.2(4) . . ?
O6F Na2 C5E 167.1(2) 2_655 . ?
O6E Na2 C5E 22.76(17) . . ?
O6A Na2 C5E 78.78(19) 2_655 . ?
O6C Na2 C5E 102.9(2) . . ?
C5A Na2 C5E 91.08(19) 2_655 . ?
O1M Na2 C5C 77.6(4) . . ?
O6F Na2 C5C 108.0(2) 2_655 . ?
O6E Na2 C5C 76.3(2) . . ?
O6A Na2 C5C 161.1(2) 2_655 . ?
O6C Na2 C5C 23.78(16) . . ?
C5A Na2 C5C 152.7(2) 2_655 . ?
C5E Na2 C5C 83.4(2) . . ?
O1M Na2 C5F 78.0(4) . 2_655 ?
O6F Na2 C5F 22.29(18) 2_655 2_655 ?
O6E Na2 C5F 167.7(2) . 2_655 ?
O6A Na2 C5F 102.6(2) 2_655 2_655 ?
O6C Na2 C5F 78.45(19) . 2_655 ?
C5A Na2 C5F 83.72(19) 2_655 2_655 ?
C5E Na2 C5F 158.2(2) . 2_655 ?
C5C Na2 C5F 91.5(2) . 2_655 ?
O1M Na2 Na1 141.3(3) . . ?
O6F Na2 Na1 101.14(17) 2_655 . ?
O6E Na2 Na1 65.65(14) . . ?
O6A Na2 Na1 53.54(14) 2_655 . ?
O6C Na2 Na1 119.93(17) . . ?
C5A Na2 Na1 75.93(15) 2_655 . ?
C5E Na2 Na1 75.23(15) . . ?
C5C Na2 Na1 127.56(18) . . ?
C5F Na2 Na1 123.42(18) 2_655 . ?
O1M Na2 Na3 141.2(3) . . ?
O6F Na2 Na3 66.39(14) 2_655 . ?
O6E Na2 Na3 100.92(16) . . ?
O6A Na2 Na3 119.73(18) 2_655 . ?
O6C Na2 Na3 53.49(14) . . ?
C5A Na2 Na3 127.84(18) 2_655 . ?
C5E Na2 Na3 123.67(17) . . ?
C5C Na2 Na3 75.92(15) . . ?
C5F Na2 Na3 74.99(15) 2_655 . ?
Na1 Na2 Na3 77.38(10) . . ?
O6D Na3 O6D 78.6(2) . 3_665 ?
O6D Na3 O6D 78.6(2) . 2_655 ?
O6D Na3 O6D 78.6(2) 3_665 2_655 ?
O6D Na3 O 118.4(4) . . ?
O6D Na3 O 128.1(4) 3_665 . ?
O6D Na3 O 149.0(4) 2_655 . ?
O6D Na3 O 128.1(4) . 2_655 ?
O6D Na3 O 149.0(4) 3_665 2_655 ?
O6D Na3 O 118.4(4) 2_655 2_655 ?
O Na3 O 30.6(6) . 2_655 ?
O6D Na3 O 149.0(4) . 3_665 ?
O6D Na3 O 118.4(4) 3_665 3_665 ?
O6D Na3 O 128.1(4) 2_655 3_665 ?
O Na3 O 30.6(6) . 3_665 ?
O Na3 O 30.6(6) 2_655 3_665 ?
O6D Na3 O6C 72.26(14) . . ?
O6D Na3 O6C 69.97(15) 3_665 . ?
O6D Na3 O6C 140.4(2) 2_655 . ?
O Na3 O6C 70.3(4) . . ?
O Na3 O6C 100.7(4) 2_655 . ?
O Na3 O6C 88.8(4) 3_665 . ?
O6D Na3 O6C 69.97(15) . 2_655 ?
O6D Na3 O6C 140.4(2) 3_665 2_655 ?
O6D Na3 O6C 72.26(14) 2_655 2_655 ?
O Na3 O6C 88.8(4) . 2_655 ?
O Na3 O6C 70.3(4) 2_655 2_655 ?
O Na3 O6C 100.7(4) 3_665 2_655 ?
O6C Na3 O6C 119.64(3) . 2_655 ?
O6D Na3 O6C 140.4(2) . 3_665 ?
O6D Na3 O6C 72.26(14) 3_665 3_665 ?
O6D Na3 O6C 69.97(15) 2_655 3_665 ?
O Na3 O6C 100.7(4) . 3_665 ?
O Na3 O6C 88.8(4) 2_655 3_665 ?
O Na3 O6C 70.3(4) 3_665 3_665 ?
O6C Na3 O6C 119.64(3) . 3_665 ?
O6C Na3 O6C 119.64(3) 2_655 3_665 ?
O6D Na3 Ni2 35.81(12) . . ?
O6D Na3 Ni2 64.88(13) 3_665 . ?
O6D Na3 Ni2 107.3(2) 2_655 . ?
O Na3 Ni2 99.5(4) . . ?
O Na3 Ni2 125.3(4) 2_655 . ?
O Na3 Ni2 124.5(4) 3_665 . ?
O6C Na3 Ni2 37.23(9) . . ?
O6C Na3 Ni2 98.88(11) 2_655 . ?
O6C Na3 Ni2 136.45(13) 3_665 . ?
O6D Na3 Ni2 64.88(13) . 2_655 ?
O6D Na3 Ni2 107.3(2) 3_665 2_655 ?
O6D Na3 Ni2 35.81(12) 2_655 2_655 ?
O Na3 Ni2 124.5(4) . 2_655 ?
O Na3 Ni2 99.5(4) 2_655 2_655 ?
O Na3 Ni2 125.3(4) 3_665 2_655 ?
O6C Na3 Ni2 136.45(13) . 2_655 ?
O6C Na3 Ni2 37.23(9) 2_655 2_655 ?
O6C Na3 Ni2 98.88(11) 3_665 2_655 ?
Ni2 Na3 Ni2 100.67(10) . 2_655 ?
O6D Na3 Ni2 107.3(2) . 3_665 ?
O6D Na3 Ni2 35.81(11) 3_665 3_665 ?
O6D Na3 Ni2 64.88(13) 2_655 3_665 ?
O Na3 Ni2 125.3(4) . 3_665 ?
O Na3 Ni2 124.5(4) 2_655 3_665 ?
O Na3 Ni2 99.5(4) 3_665 3_665 ?
O6C Na3 Ni2 98.88(11) . 3_665 ?
O6C Na3 Ni2 136.45(13) 2_655 3_665 ?
O6C Na3 Ni2 37.23(9) 3_665 3_665 ?
Ni2 Na3 Ni2 100.67(10) . 3_665 ?
Ni2 Na3 Ni2 100.67(10) 2_655 3_665 ?
C2B C11 C2A 118.4(6) . . ?
N3A C2A C11 109.5(6) . . ?
C4A N3A C2A 124.7(6) . . ?
C4A N3A Ni1 114.1(4) . . ?
C2A N3A Ni1 121.2(4) . . ?
N3A C4A C8A 128.5(6) . . ?
N3A C4A C5A 114.4(6) . . ?
C8A C4A C5A 117.0(6) . . ?
O7A C5A O6A 126.7(6) . . ?
O7A C5A C4A 116.0(6) . . ?
O6A C5A C4A 117.2(6) . . ?
O7A C5A Na2 100.4(4) . 3_665 ?
O6A C5A Na2 51.5(3) . 3_665 ?
C4A C5A Na2 120.5(4) . 3_665 ?
C5A O6A Ni1 110.3(4) . . ?
C5A O6A Na2 104.9(4) . 3_665 ?
Ni1 O6A Na2 117.3(2) . 3_665 ?
C5A O6A Na1 157.9(4) . . ?
Ni1 O6A Na1 81.07(16) . . ?
Na2 O6A Na1 85.09(18) 3_665 . ?
C5A O7A Ni3 130.5(4) . . ?
N3B C2B C11 113.9(6) . . ?
C4B N3B C2B 121.9(6) . . ?
C4B N3B Ni1 114.9(4) . . ?
C2B N3B Ni1 123.2(5) . . ?
N3B C4B C8B 125.2(6) . . ?
N3B C4B C5B 114.5(5) . . ?
C8B C4B C5B 120.3(6) . . ?
O7B C5B O6B 125.1(6) . . ?
O7B C5B C4B 118.8(5) . . ?
O6B C5B C4B 116.0(5) . . ?
C5B O6B Ni1 114.5(4) . . ?
C5B O6B Na1 141.8(4) . . ?
Ni1 O6B Na1 102.35(18) . . ?
C5B O7B Ni1 121.1(4) . 3_665 ?
C2C C12 C2D 117.1(7) . . ?
N3C C2C C12 110.9(6) . . ?
C4C N3C C2C 126.4(6) . . ?
C4C N3C Ni2 114.3(4) . . ?
C2C N3C Ni2 119.3(5) . . ?
N3C C4C C8C 127.6(7) . . ?
N3C C4C C5C 115.0(6) . . ?
C8C C4C C5C 117.4(6) . . ?
O7C C5C O6C 126.0(6) . . ?
O7C C5C C4C 117.3(6) . . ?
O6C C5C C4C 116.6(6) . . ?
O7C C5C Na2 99.2(4) . . ?
O6C C5C Na2 50.1(3) . . ?
C4C C5C Na2 121.4(4) . . ?
C5C O6C Ni2 110.3(4) . . ?
C5C O6C Na2 106.2(4) . . ?
Ni2 O6C Na2 117.8(2) . . ?
C5C O6C Na3 155.7(5) . . ?
Ni2 O6C Na3 81.25(16) . . ?
Na2 O6C Na3 85.45(18) . . ?
C5C O7C Ni3 132.4(5) . . ?
N3D C2D C12 112.5(6) . . ?
C4D N3D C2D 121.4(6) . . ?
C4D N3D Ni2 114.3(4) . . ?
C2D N3D Ni2 124.2(5) . . ?
N3D C4D C8D 124.9(6) . . ?
N3D C4D C5D 114.1(6) . . ?
C8D C4D C5D 120.9(6) . . ?
O7D C5D O6D 126.1(6) . . ?
O7D C5D C4D 117.0(5) . . ?
O6D C5D C4D 116.9(5) . . ?
C5D O6D Ni2 114.2(4) . . ?
C5D O6D Na3 141.4(4) . . ?
Ni2 O6D Na3 102.81(19) . . ?
C5D O7D Ni2 120.6(4) . 2_655 ?
C2F C13 C2E 121.7(16) . . ?
C2E C13' C2F 116.6(9) . . ?
C13' C2E N3E 111.4(7) . . ?
C13' C2E C13 50.8(10) . . ?
N3E C2E C13 114.0(10) . . ?
C4E N3E C2E 119.3(6) . . ?
C4E N3E Ni3 116.8(5) . . ?
C2E N3E Ni3 123.7(4) . . ?
N3E C4E C8E 128.0(7) . . ?
N3E C4E C5E 112.6(6) . . ?
C8E C4E C5E 119.4(6) . . ?
O7E C5E O6E 128.7(6) . . ?
O7E C5E C4E 113.6(5) . . ?
O6E C5E C4E 117.7(5) . . ?
O7E C5E Na2 93.8(4) . . ?
O6E C5E Na2 48.1(3) . . ?
C4E C5E Na2 134.9(4) . . ?
C5E O6E Ni3 112.9(4) . . ?
C5E O6E Na2 109.1(4) . . ?
Ni3 O6E Na2 117.6(2) . . ?
C5E O7E Ni1 132.1(4) . 2_655 ?
C13 C2F N3F 113.2(11) . . ?
N3F C2F C13' 113.3(7) . . ?
C4F N3F C2F 121.7(6) . . ?
C4F N3F Ni3 115.5(4) . . ?
C2F N3F Ni3 122.7(5) . . ?
N3F C4F C8F 126.1(7) . . ?
N3F C4F C5F 114.4(6) . . ?
C8F C4F C5F 119.5(7) . . ?
O7F C5F O6F 127.6(6) . . ?
O7F C5F C4F 115.3(6) . . ?
O6F C5F C4F 117.1(6) . . ?
O7F C5F Na2 91.5(4) . 3_665 ?
O6F C5F Na2 46.2(3) . 3_665 ?
C4F C5F Na2 138.1(4) . 3_665 ?
C5F O6F Ni3 112.9(4) . . ?
C5F O6F Na2 111.5(4) . 3_665 ?
Ni3 O6F Na2 117.9(2) . 3_665 ?
C5F O7F Ni2 132.2(5) . 3_665 ?
O11 Cl1 O12 109.5(3) . . ?
O22 Cl2 O22 109.6(4) 3_665 2_655 ?
O O Na3 74.7(3) 3_665 . ?
O O Na1 74.4(3) 2_655 . ?
Na3 O Na1 144.2(7) . . ?
O3' Cl3 O3' 107.4(18) 3_765 . ?
O3 Cl3 O3 103(3) 6_546 . ?
C1M' O1M C1M 76(3) . . ?
C1M' O1M Na2 147(3) . . ?
C1M O1M Na2 137.6(11) . . ?
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 N3A 2.013(5) . y
Ni1 O6B 2.036(4) . y
Ni1 N3B 2.045(5) . y
Ni1 O7E 2.069(5) 3_665 y
Ni1 O6A 2.074(4) . y
Ni1 O7B 2.101(5) 2_655 y
Ni1 Na1 3.379(2) . ?
Ni2 O6D 2.028(4) . y
Ni2 N3C 2.024(6) . y
Ni2 N3D 2.032(5) . y
Ni2 O6C 2.069(4) . y
Ni2 O7F 2.086(5) 2_655 y
Ni2 O7D 2.099(5) 3_665 y
Ni2 Na3 3.380(2) . ?
Ni3 N3E 2.028(5) . y
Ni3 N3F 2.032(5) . y
Ni3 O7A 2.069(5) . y
Ni3 O7C 2.071(5) . y
Ni3 O6E 2.089(4) . y
Ni3 O6F 2.078(4) . y
Na1 O6B 2.296(5) . y
Na1 O 2.429(14) . y
Na1 O6A 3.009(5) . y
Na2 O1M 2.347(9) . y
Na2 O6F 2.406(6) 2_655 y
Na2 O6E 2.411(6) . y
Na2 O6A 2.473(6) 2_655 y
Na2 O6C 2.456(6) . y
Na2 C5A 3.052(7) 2_655 ?
Na2 C5E 3.060(7) . ?
Na2 C5C 3.077(8) . ?
Na2 C5F 3.102(8) 2_655 ?
Na2 Na3 3.728(5) . ?
Na3 O6D 2.291(5) . y
Na3 O 2.469(15) . y
Na3 O6C 3.006(4) . y
Na3 Ni2 3.380(2) 2_655 ?
C11 C2B 1.506(11) . ?
C11 C2A 1.522(11) . ?
C2A N3A 1.457(8) . ?
N3A C4A 1.284(8) . ?
C4A C8A 1.505(9) . ?
C4A C5A 1.538(9) . ?
C5A O7A 1.257(8) . ?
C5A O6A 1.262(8) . ?
C5A Na2 3.052(7) 3_665 ?
O6A Na2 2.473(6) 3_665 ?
C2B N3B 1.467(8) . ?
N3B C4B 1.284(8) . ?
C4B C8B 1.499(9) . ?
C4B C5B 1.527(9) . ?
C5B O7B 1.235(8) . ?
C5B O6B 1.276(7) . ?
O7B Ni1 2.101(5) 3_665 ?
C12 C2C 1.514(11) . ?
C12 C2D 1.528(11) . ?
C2C N3C 1.464(8) . ?
N3C C4C 1.277(9) . ?
C4C C8C 1.505(10) . ?
C4C C5C 1.520(9) . ?
C5C O7C 1.239(8) . ?
C5C O6C 1.291(8) . ?
C2D N3D 1.467(9) . ?
N3D C4D 1.283(9) . ?
C4D C8D 1.512(9) . ?
C4D C5D 1.523(9) . ?
C5D O7D 1.265(8) . ?
C5D O6D 1.248(8) . ?
O7D Ni2 2.099(5) 2_655 ?
C13 C2F 1.40(2) . ?
C13 C2E 1.51(2) . ?
C13' C2E 1.477(14) . ?
C13' C2F 1.507(13) . ?
C2E N3E 1.464(9) . ?
N3E C4E 1.284(9) . ?
C4E C8E 1.487(10) . ?
C4E C5E 1.563(9) . ?
C5E O7E 1.258(7) . ?
C5E O6E 1.253(8) . ?
O7E Ni1 2.069(5) 2_655 ?
C2F N3F 1.492(9) . ?
N3F C4F 1.275(9) . ?
C4F C8F 1.493(10) . ?
C4F C5F 1.529(9) . ?
C5F O7F 1.230(8) . ?
C5F O6F 1.265(8) . ?
C5F Na2 3.102(8) 3_665 ?
O6F Na2 2.406(6) 3_665 ?
O7F Ni2 2.086(5) 3_665 ?
Cl1 O11 1.434(6) . ?
Cl1 O12 1.438(5) . ?
Cl2 O21 1.443(7) . ?
Cl2 O22 1.449(5) . ?
Cl3 O3' 1.449(8) . ?
Cl3 O3 1.452(8) . ?
Cl4 O4' 1.455(8) . ?
O1M C1M' 1.460(19) . ?
O1M C1M 1.466(17) . ?
C2M O2M 1.460(18) . ?
