# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_ni1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H54 N18 Na3 Ni4 O18, C6 H16 N'
_chemical_formula_sum            'C60 H70 N19 Na3 Ni4 O18'
_chemical_formula_weight         1649.08

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'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n  '
_symmetry_space_group_name_Hall  ' -P 2yn '

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                   13.2004(4)
_cell_length_b                   26.6638(12)
_cell_length_c                   22.1197(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.526(3)
_cell_angle_gamma                90.00
_cell_volume                     7735.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    10738
_cell_measurement_theta_min      3.169
_cell_measurement_theta_max      28.168

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3408
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            34163
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.10
_reflns_number_total             13773
_reflns_number_gt                8437
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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  'Bruker SHELXTL'

_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)+(0.0729P)²+3.5981P] 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         13738
_refine_ls_number_parameters     946
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1797
_refine_ls_wR_factor_gt          0.1511
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.500 1.000 246.4 5.6
2 0.199 0.101 0.968 23.8 0.9
3 0.301 0.601 0.532 23.8 0.5
4 0.500 1.000 0.500 246.3 5.6
5 0.699 0.399 0.468 23.8 0.6
6 0.801 0.899 0.032 23.8 0.2
_platon_squeeze_details          
;
;


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
C1 C 0.8888(4) 0.5356(2) 0.3664(2) 0.0485(13) Uani 1 1 d . . .
C2 C 0.9175(5) 0.5017(2) 0.3229(3) 0.0621(16) Uani 1 1 d . . .
C3 C 1.0145(5) 0.4793(3) 0.3295(3) 0.088(2) Uani 1 1 d . . .
H3 H 1.0309 0.4565 0.3003 0.105 Uiso 1 1 calc R . .
C4 C 1.0841(6) 0.4901(3) 0.3768(4) 0.101(3) Uani 1 1 d . . .
H4 H 1.1487 0.4757 0.3797 0.121 Uiso 1 1 calc R . .
C5 C 1.0581(5) 0.5233(3) 0.4217(3) 0.082(2) Uani 1 1 d . . .
H5 H 1.1050 0.5298 0.4554 0.098 Uiso 1 1 calc R . .
C6 C 0.9643(4) 0.5462(2) 0.4165(2) 0.0567(15) Uani 1 1 d . . .
C7 C 1.0099(5) 0.5973(3) 0.5052(3) 0.0755(19) Uani 1 1 d . . .
H7A H 1.0661 0.6126 0.4873 0.091 Uiso 1 1 calc R . .
H7B H 1.0362 0.5695 0.5306 0.091 Uiso 1 1 calc R . .
C8 C 0.9610(6) 0.6345(3) 0.5420(3) 0.099(3) Uani 1 1 d . . .
H8A H 0.9453 0.6642 0.5183 0.149 Uiso 1 1 calc R . .
H8B H 1.0066 0.6428 0.5776 0.149 Uiso 1 1 calc R . .
H8C H 0.8992 0.6207 0.5542 0.149 Uiso 1 1 calc R . .
C9 C 0.8490(5) 0.4885(2) 0.2700(3) 0.078(2) Uani 1 1 d . . .
H9 H 0.8747 0.4655 0.2441 0.093 Uiso 1 1 calc R . .
C10 C 0.4794(4) 0.5312(2) 0.2311(2) 0.0489(13) Uani 1 1 d . . .
C11 C 0.4521(4) 0.5023(2) 0.2804(3) 0.0605(15) Uani 1 1 d . . .
C12 C 0.3525(6) 0.4817(3) 0.2774(4) 0.093(2) Uani 1 1 d . . .
H12 H 0.3345 0.4636 0.3105 0.112 Uiso 1 1 calc R . .
C13 C 0.2847(6) 0.4873(3) 0.2294(4) 0.111(3) Uani 1 1 d . . .
H13 H 0.2204 0.4729 0.2281 0.134 Uiso 1 1 calc R . .
C14 C 0.3123(5) 0.5158(3) 0.1801(3) 0.092(2) Uani 1 1 d . . .
H14 H 0.2648 0.5202 0.1461 0.111 Uiso 1 1 calc R . .
C15 C 0.4072(4) 0.5373(2) 0.1806(3) 0.0606(15) Uani 1 1 d . . .
C16 C 0.3631(6) 0.5801(3) 0.0847(3) 0.111(3) Uani 1 1 d . . .
H16A H 0.3358 0.5503 0.0637 0.134 Uiso 1 1 calc R . .
H16B H 0.3072 0.5979 0.1001 0.134 Uiso 1 1 calc R . .
C17 C 0.4100(7) 0.6117(4) 0.0434(3) 0.138(4) Uani 1 1 d . . .
H17A H 0.3616 0.6193 0.0088 0.207 Uiso 1 1 calc R . .
H17B H 0.4676 0.5947 0.0300 0.207 Uiso 1 1 calc R . .
H17C H 0.4323 0.6423 0.0636 0.207 Uiso 1 1 calc R . .
C18 C 0.5203(5) 0.4937(2) 0.3338(3) 0.0666(17) Uani 1 1 d . . .
H18 H 0.4931 0.4756 0.3641 0.080 Uiso 1 1 calc R . .
C19 C 0.7214(4) 0.6694(2) 0.07012(19) 0.0450(13) Uani 1 1 d . . .
C20 C 0.7616(4) 0.7115(3) 0.0430(2) 0.0533(15) Uani 1 1 d . . .
C21 C 0.8245(4) 0.7053(3) -0.0046(3) 0.078(2) Uani 1 1 d . . .
H21 H 0.8513 0.7334 -0.0220 0.093 Uiso 1 1 calc R . .
C22 C 0.8452(5) 0.6605(4) -0.0244(3) 0.093(3) Uani 1 1 d . . .
H22 H 0.8862 0.6572 -0.0557 0.112 Uiso 1 1 calc R . .
C23 C 0.8065(5) 0.6182(3) 0.0009(3) 0.077(2) Uani 1 1 d . . .
H23 H 0.8217 0.5867 -0.0136 0.092 Uiso 1 1 calc R . .
C24 C 0.7459(4) 0.6222(2) 0.0471(2) 0.0549(15) Uani 1 1 d . . .
C25 C 0.7156(6) 0.5315(3) 0.0554(3) 0.100(3) Uani 1 1 d . . .
H25A H 0.7875 0.5231 0.0607 0.120 Uiso 1 1 calc R . .
H25B H 0.6914 0.5287 0.0125 0.120 Uiso 1 1 calc R . .
C26 C 0.6596(7) 0.4958(3) 0.0901(4) 0.109(3) Uani 1 1 d . . .
H26A H 0.6705 0.4623 0.0763 0.163 Uiso 1 1 calc R . .
H26B H 0.5881 0.5035 0.0840 0.163 Uiso 1 1 calc R . .
H26C H 0.6837 0.4984 0.1326 0.163 Uiso 1 1 calc R . .
C27 C 0.7419(5) 0.7622(3) 0.0614(2) 0.0672(18) Uani 1 1 d . . .
H27 H 0.7734 0.7872 0.0411 0.081 Uiso 1 1 calc R . .
C28 C 0.4751(4) 0.8086(2) 0.2001(2) 0.0469(13) Uani 1 1 d . . .
C29 C 0.3926(4) 0.7914(2) 0.1578(2) 0.0521(14) Uani 1 1 d . . .
C30 C 0.2944(4) 0.8130(3) 0.1590(3) 0.0700(18) Uani 1 1 d . . .
H30 H 0.2414 0.8033 0.1300 0.084 Uiso 1 1 calc R . .
C31 C 0.2766(5) 0.8476(3) 0.2017(3) 0.086(2) Uani 1 1 d . . .
H31 H 0.2114 0.8605 0.2028 0.103 Uiso 1 1 calc R . .
C32 C 0.3569(5) 0.8636(2) 0.2441(3) 0.0733(18) Uani 1 1 d . . .
H32A H 0.3448 0.8874 0.2732 0.088 Uiso 1 1 calc R . .
C33 C 0.4519(4) 0.8450(2) 0.2433(2) 0.0524(14) Uani 1 1 d . . .
C34 C 0.5159(5) 0.8889(2) 0.3339(2) 0.0710(18) Uani 1 1 d . . .
H34A H 0.4700 0.8712 0.3578 0.085 Uiso 1 1 calc R . .
H34B H 0.4843 0.9203 0.3202 0.085 Uiso 1 1 calc R . .
C35 C 0.6167(6) 0.8986(3) 0.3719(3) 0.100(3) Uani 1 1 d . . .
H35A H 0.6625 0.9147 0.3473 0.149 Uiso 1 1 calc R . .
H35B H 0.6456 0.8674 0.3869 0.149 Uiso 1 1 calc R . .
H35C H 0.6058 0.9200 0.4055 0.149 Uiso 1 1 calc R . .
C36 C 0.4050(5) 0.7550(2) 0.1122(2) 0.0594(16) Uani 1 1 d . . .
H36 H 0.3472 0.7482 0.0853 0.071 Uiso 1 1 calc R . .
C37 C 0.8888(4) 0.8244(2) 0.3664(2) 0.0492(13) Uani 1 1 d . . .
C38 C 0.9662(4) 0.8173(2) 0.4166(2) 0.0549(15) Uani 1 1 d . . .
C39 C 1.0530(5) 0.8487(3) 0.4221(3) 0.085(2) Uani 1 1 d . . .
H39 H 1.1028 0.8446 0.4550 0.102 Uiso 1 1 calc R . .
C40 C 1.0649(5) 0.8844(3) 0.3804(3) 0.092(2) Uani 1 1 d . . .
H40 H 1.1220 0.9051 0.3857 0.111 Uiso 1 1 calc R . .
C41 C 0.9942(5) 0.8910(2) 0.3302(3) 0.0732(18) Uani 1 1 d . . .
H41 H 1.0041 0.9156 0.3016 0.088 Uiso 1 1 calc R . .
C42 C 0.9093(4) 0.8610(2) 0.3225(2) 0.0531(14) Uani 1 1 d . . .
C43 C 0.8560(5) 0.8937(2) 0.2231(2) 0.0693(18) Uani 1 1 d . . .
H43A H 0.9209 0.8842 0.2098 0.083 Uiso 1 1 calc R . .
H43B H 0.8592 0.9288 0.2346 0.083 Uiso 1 1 calc R . .
C44 C 0.7707(6) 0.8851(2) 0.1727(3) 0.092(2) Uani 1 1 d . . .
H44A H 0.7786 0.9074 0.1395 0.138 Uiso 1 1 calc R . .
H44B H 0.7064 0.8914 0.1877 0.138 Uiso 1 1 calc R . .
H44C H 0.7728 0.8510 0.1589 0.138 Uiso 1 1 calc R . .
C45 C 0.9598(4) 0.7800(2) 0.4614(2) 0.0593(16) Uani 1 1 d . . .
H45 H 1.0156 0.7775 0.4910 0.071 Uiso 1 1 calc R . .
C46 C 0.6450(3) 0.6940(2) 0.50371(19) 0.0424(12) Uani 1 1 d . . .
C47 C 0.6065(4) 0.7393(2) 0.5253(2) 0.0503(14) Uani 1 1 d . . .
C48 C 0.5412(4) 0.7384(3) 0.5720(3) 0.0670(18) Uani 1 1 d . . .
H48 H 0.5171 0.7684 0.5863 0.080 Uiso 1 1 calc R . .
C49 C 0.5137(5) 0.6944(3) 0.5960(3) 0.078(2) Uani 1 1 d . . .
H49 H 0.4708 0.6944 0.6266 0.093 Uiso 1 1 calc R . .
C50 C 0.5488(4) 0.6496(3) 0.5755(2) 0.0675(17) Uani 1 1 d . . .
H50 H 0.5290 0.6196 0.5922 0.081 Uiso 1 1 calc R . .
C51 C 0.6133(4) 0.6486(2) 0.5302(2) 0.0500(13) Uani 1 1 d . . .
C52 C 0.6259(5) 0.5587(2) 0.5303(3) 0.0779(19) Uani 1 1 d . . .
H52A H 0.5528 0.5542 0.5218 0.094 Uiso 1 1 calc R . .
H52B H 0.6438 0.5574 0.5740 0.094 Uiso 1 1 calc R . .
C53 C 0.6789(6) 0.5182(2) 0.5011(3) 0.089(2) Uani 1 1 d . . .
H53A H 0.6543 0.5168 0.4586 0.134 Uiso 1 1 calc R . .
H53B H 0.6660 0.4868 0.5200 0.134 Uiso 1 1 calc R . .
H53C H 0.7509 0.5247 0.5058 0.134 Uiso 1 1 calc R . .
C54 C 0.6313(4) 0.7869(2) 0.5010(2) 0.0610(16) Uani 1 1 d . . .
H54 H 0.6026 0.8145 0.5182 0.073 Uiso 1 1 calc R . .
C55 C 0.1649(9) 0.7699(5) 0.3173(6) 0.200(5) Uani 1 1 d U . .
H55A H 0.1652 0.8021 0.2978 0.299 Uiso 1 1 calc R . .
H55B H 0.2176 0.7690 0.3510 0.299 Uiso 1 1 calc R . .
H55C H 0.0999 0.7645 0.3318 0.299 Uiso 1 1 calc R . .
C56 C 0.1828(10) 0.7315(6) 0.2747(6) 0.206(6) Uani 1 1 d U . .
H56A H 0.2513 0.7355 0.2636 0.248 Uiso 1 1 calc R . .
H56B H 0.1357 0.7363 0.2382 0.248 Uiso 1 1 calc R . .
C57 C 0.1421(10) 0.6486(5) 0.2403(5) 0.217(5) Uani 1 1 d DU . .
H57A H 0.1915 0.6518 0.2112 0.261 Uiso 1 1 calc R . .
H57B H 0.0751 0.6576 0.2208 0.261 Uiso 1 1 calc R . .
C58 C 0.1424(16) 0.5834(5) 0.2731(8) 0.407(11) Uani 1 1 d DU . .
H58A H 0.1808 0.5832 0.3126 0.610 Uiso 1 1 calc R . .
H58B H 0.1729 0.5606 0.2468 0.610 Uiso 1 1 calc R . .
H58C H 0.0736 0.5731 0.2765 0.610 Uiso 1 1 calc R . .
C59 C 0.2542(9) 0.6702(4) 0.3427(5) 0.196(5) Uani 1 1 d DU . .
H59A H 0.2946 0.7006 0.3472 0.235 Uiso 1 1 calc R . .
H59B H 0.2963 0.6452 0.3259 0.235 Uiso 1 1 calc R . .
C60 C 0.2421(10) 0.6536(5) 0.4042(5) 0.231(6) Uani 1 1 d DU . .
H60A H 0.1958 0.6756 0.4217 0.347 Uiso 1 1 calc R . .
H60B H 0.3071 0.6542 0.4285 0.347 Uiso 1 1 calc R . .
H60C H 0.2154 0.6201 0.4028 0.347 Uiso 1 1 calc R . .
N1 N 0.7470(3) 0.61462(15) 0.24822(16) 0.0392(9) Uani 1 1 d . . .
N2 N 0.8229(4) 0.61038(19) 0.2252(2) 0.0619(13) Uani 1 1 d . . .
N3 N 0.8942(5) 0.6047(3) 0.2019(4) 0.140(3) Uani 1 1 d . . .
N4 N 0.8116(3) 0.68668(15) 0.35677(15) 0.0366(9) Uani 1 1 d . . .
N5 N 0.8991(3) 0.67967(18) 0.35465(18) 0.0542(12) Uani 1 1 d . . .
N6 N 0.9841(4) 0.6710(3) 0.3550(3) 0.113(3) Uani 1 1 d . . .
N7 N 0.7424(3) 0.72980(15) 0.22697(16) 0.0364(9) Uani 1 1 d . . .
N8 N 0.8279(3) 0.7335(2) 0.21763(19) 0.0600(14) Uani 1 1 d . . .
N9 N 0.9110(4) 0.7377(3) 0.2085(3) 0.125(3) Uani 1 1 d . . .
N10 N 0.6238(3) 0.61909(15) 0.33847(16) 0.0360(9) Uani 1 1 d . . .
N11 N 0.5464(3) 0.61684(17) 0.36115(18) 0.0486(11) Uani 1 1 d . . .
N12 N 0.4747(4) 0.6129(2) 0.3839(3) 0.100(2) Uani 1 1 d . . .
N13 N 0.5614(3) 0.68097(15) 0.21961(15) 0.0375(9) Uani 1 1 d . . .
N14 N 0.4733(3) 0.67318(18) 0.22333(18) 0.0523(12) Uani 1 1 d . . .
N15 N 0.3880(4) 0.6642(3) 0.2241(3) 0.102(2) Uani 1 1 d . . .
N16 N 0.6295(3) 0.73674(14) 0.34190(16) 0.0355(9) Uani 1 1 d . . .
N17 N 0.5443(3) 0.74363(16) 0.35272(18) 0.0461(10) Uani 1 1 d . . .
N18 N 0.4638(4) 0.7520(2) 0.3641(3) 0.0920(19) Uani 1 1 d . . .
N19 N 0.1718(5) 0.6804(3) 0.2964(3) 0.124(3) Uani 1 1 d D . .
H19A H 0.1140 0.6762 0.3146 0.149 Uiso 1 1 d R . .
Na1 Na 0.76405(14) 0.61793(7) 0.42864(8) 0.0456(5) Uani 1 1 d . . .
Na2 Na 0.68841(13) 0.80812(8) 0.27772(8) 0.0457(5) Uani 1 1 d . . .
Na3 Na 0.60774(15) 0.60451(8) 0.15840(8) 0.0522(5) Uani 1 1 d . . .
Ni1 Ni 0.68488(4) 0.67826(2) 0.28882(2) 0.03294(17) Uani 1 1 d . . .
Ni2 Ni 0.68590(5) 0.55675(3) 0.29706(3) 0.04389(19) Uani 1 1 d . . .
Ni3 Ni 0.75504(5) 0.74499(2) 0.40991(2) 0.03928(18) Uani 1 1 d . . .
Ni4 Ni 0.61702(5) 0.73200(3) 0.15852(2) 0.03995(19) Uani 1 1 d . . .
O1 O 0.8015(3) 0.55748(13) 0.36419(14) 0.0507(9) Uani 1 1 d . . .
O2 O 0.7620(3) 0.50293(14) 0.25386(16) 0.0628(11) Uani 1 1 d . . .
O3 O 0.9329(3) 0.57970(15) 0.45791(15) 0.0594(10) Uani 1 1 d . . .
O4 O 0.5685(3) 0.55127(13) 0.23033(14) 0.0513(9) Uani 1 1 d . . .
O5 O 0.6091(3) 0.50633(14) 0.34588(16) 0.0614(10) Uani 1 1 d . . .
O6 O 0.4390(3) 0.56600(16) 0.13522(17) 0.0677(11) Uani 1 1 d . . .
O7 O 0.6634(3) 0.67226(13) 0.11280(13) 0.0490(9) Uani 1 1 d . . .
O8 O 0.6888(3) 0.77693(15) 0.10056(15) 0.0597(10) Uani 1 1 d . . .
O9 O 0.7024(3) 0.58271(16) 0.07512(16) 0.0661(11) Uani 1 1 d . . .
O10 O 0.5673(2) 0.79233(13) 0.19992(13) 0.0468(9) Uani 1 1 d . . .
O11 O 0.4821(3) 0.73120(15) 0.10357(14) 0.0552(10) Uani 1 1 d . . .
O12 O 0.5354(3) 0.85930(14) 0.28302(15) 0.0575(10) Uani 1 1 d . . .
O13 O 0.8049(2) 0.79909(13) 0.35867(13) 0.0466(9) Uani 1 1 d . . .
O14 O 0.8889(3) 0.75035(14) 0.46616(14) 0.0555(10) Uani 1 1 d . . .
O15 O 0.8343(3) 0.86308(14) 0.27377(15) 0.0571(10) Uani 1 1 d . . .
O16 O 0.7058(2) 0.69086(12) 0.46259(12) 0.0422(8) Uani 1 1 d . . .
O17 O 0.6853(3) 0.79652(14) 0.46055(15) 0.0555(10) Uani 1 1 d . . .
O18 O 0.6543(3) 0.60603(14) 0.50762(14) 0.0546(9) 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
C1 O1 1.287(6) . ?
C1 C2 1.405(7) . ?
C1 C6 1.431(7) . ?
C2 C3 1.405(8) . ?
C2 C9 1.438(8) . ?
C3 C4 1.343(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(7) . ?
C5 H5 0.9300 . ?
C6 O3 1.376(6) . ?
C7 O3 1.451(6) . ?
C7 C8 1.478(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 O2 1.225(7) . ?
C9 H9 0.9300 . ?
C10 O4 1.295(6) . ?
C10 C15 1.393(7) . ?
C10 C11 1.413(7) . ?
C11 C18 1.420(8) . ?
C11 C12 1.419(8) . ?
C12 C13 1.317(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(8) . ?
C14 H14 0.9300 . ?
C15 O6 1.367(6) . ?
C16 C17 1.435(10) . ?
C16 O6 1.463(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O5 1.220(6) . ?
C18 H18 0.9300 . ?
C19 O7 1.284(5) . ?
C19 C20 1.405(7) . ?
C19 C24 1.410(7) . ?
C19 Na3 3.119(5) . ?
C20 C21 1.423(7) . ?
C20 C27 1.442(8) . ?
C21 C22 1.311(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.383(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.372(7) . ?
C23 H23 0.9300 . ?
C24 O9 1.379(7) . ?
C25 O9 1.450(7) . ?
C25 C26 1.473(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 O8 1.238(7) . ?
C27 H27 0.9300 . ?
C28 O10 1.292(6) . ?
C28 C33 1.418(7) . ?
C28 C29 1.428(7) . ?
C28 Na2 3.127(5) . ?
C29 C30 1.420(7) . ?
C29 C36 1.424(8) . ?
C30 C31 1.361(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.400(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.351(7) . ?
C32 H32A 0.9300 . ?
C33 O12 1.384(6) . ?
C34 O12 1.421(6) . ?
C34 C35 1.513(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 O11 1.232(6) . ?
C36 H36 0.9300 . ?
C37 O13 1.293(6) . ?
C37 C42 1.423(7) . ?
C37 C38 1.434(7) . ?
C38 C45 1.413(7) . ?
C38 C39 1.413(7) . ?
C39 C40 1.348(8) . ?
C39 H39 0.9300 . ?
C40 C41 1.379(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.371(7) . ?
C41 H41 0.9300 . ?
C42 O15 1.380(6) . ?
C43 O15 1.443(6) . ?
C43 C44 1.509(8) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 O14 1.239(6) . ?
C45 H45 0.9300 . ?
C46 O16 1.282(5) . ?
C46 C47 1.415(7) . ?
C46 C51 1.428(7) . ?
C47 C48 1.418(7) . ?
C47 C54 1.430(8) . ?
C48 C49 1.355(8) . ?
C48 H48 0.9300 . ?
C49 C50 1.376(8) . ?
C49 H49 0.9300 . ?
C50 C51 1.388(7) . ?
C50 H50 0.9300 . ?
C51 O18 1.375(6) . ?
C52 O18 1.424(6) . ?
C52 C53 1.473(8) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 O17 1.233(6) . ?
C54 H54 0.9300 . ?
C55 C56 1.430(15) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 N19 1.456(14) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 N19 1.516(8) . ?
C57 C58 1.884(18) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 N19 1.433(11) . ?
C59 C60 1.456(13) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N1 N2 1.180(5) . ?
N1 Ni2 2.096(4) . ?
N1 Ni1 2.127(4) . ?
N1 Na3 2.563(4) . ?
N2 N3 1.133(7) . ?
N2 Na3 3.053(5) . ?
N4 N5 1.176(5) . ?
N4 Ni1 2.129(3) . ?
N4 Ni3 2.134(4) . ?
N4 Na1 2.551(4) . ?
N5 N6 1.146(6) . ?
N5 Na1 3.038(5) . ?
N7 N8 1.175(5) . ?
N7 Ni4 2.113(3) . ?
N7 Ni1 2.138(4) . ?
N7 Na2 2.512(4) . ?
N8 N9 1.143(6) . ?
N10 N11 1.190(5) . ?
N10 Ni2 2.108(4) . ?
N10 Ni1 2.132(4) . ?
N10 Na1 2.563(4) . ?
N11 N12 1.126(6) . ?
N13 N14 1.192(5) . ?
N13 Ni1 2.107(3) . ?
N13 Ni4 2.108(4) . ?
N13 Na3 2.560(4) . ?
N14 N15 1.154(6) . ?
N14 Na3 3.024(5) . ?
N16 N17 1.191(5) . ?
N16 Ni3 2.119(3) . ?
N16 Ni1 2.130(4) . ?
N16 Na2 2.548(4) . ?
N17 N18 1.142(6) . ?
N19 H19A 0.9104 . ?
Na1 O1 2.244(4) . ?
Na1 O16 2.251(4) . ?
Na1 O18 2.414(4) . ?
Na1 O3 2.470(4) . ?
Na1 Ni2 3.3931(19) . ?
Na1 Ni3 3.414(2) . ?
Na1 Ni1 3.5370(19) . ?
Na2 O13 2.237(3) . ?
Na2 O10 2.252(3) . ?
Na2 O15 2.429(4) . ?
Na2 O12 2.451(4) . ?
Na2 Ni4 3.3756(19) . ?
Na2 Ni3 3.4018(18) . ?
Na2 Ni1 3.472(2) . ?
Na3 O7 2.233(4) . ?
Na3 O4 2.237(4) . ?
Na3 O9 2.412(4) . ?
Na3 O6 2.453(4) . ?
Na3 Ni2 3.3727(19) . ?
Na3 Ni4 3.401(2) . ?
Na3 Ni1 3.544(2) . ?
Ni2 O1 2.005(3) . ?
Ni2 O4 2.020(3) . ?
Ni2 O2 2.050(4) . ?
Ni2 O5 2.061(4) . ?
Ni3 O13 1.992(3) . ?
Ni3 O16 2.009(3) . ?
Ni3 O14 2.047(3) . ?
Ni3 O17 2.055(4) . ?
Ni4 O10 1.999(3) . ?
Ni4 O7 2.019(3) . ?
Ni4 O11 2.039(3) . ?
Ni4 O8 2.062(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 C1 C2 125.1(5) . . ?
O1 C1 C6 118.8(5) . . ?
C2 C1 C6 116.1(5) . . ?
C1 C2 C3 121.0(6) . . ?
C1 C2 C9 121.5(5) . . ?
C3 C2 C9 117.5(6) . . ?
C4 C3 C2 121.7(6) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.0(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.9(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 O3 124.8(5) . . ?
C5 C6 C1 121.2(6) . . ?
O3 C6 C1 114.0(5) . . ?
O3 C7 C8 107.5(5) . . ?
O3 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
O3 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C2 130.0(6) . . ?
O2 C9 H9 115.0 . . ?
C2 C9 H9 115.0 . . ?
O4 C10 C15 118.7(5) . . ?
O4 C10 C11 123.2(5) . . ?
C15 C10 C11 118.1(5) . . ?
C10 C11 C18 122.4(5) . . ?
C10 C11 C12 119.4(6) . . ?
C18 C11 C12 118.2(6) . . ?
C13 C12 C11 122.3(7) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C12 C13 C14 118.2(7) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C15 C14 C13 122.2(7) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
O6 C15 C14 125.6(6) . . ?
O6 C15 C10 114.6(5) . . ?
C14 C15 C10 119.8(6) . . ?
C17 C16 O6 109.3(6) . . ?
C17 C16 H16A 109.8 . . ?
O6 C16 H16A 109.8 . . ?
C17 C16 H16B 109.8 . . ?
O6 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C18 C11 129.8(6) . . ?
O5 C18 H18 115.1 . . ?
C11 C18 H18 115.1 . . ?
O7 C19 C20 123.5(5) . . ?
O7 C19 C24 119.9(5) . . ?
C20 C19 C24 116.5(5) . . ?
O7 C19 Na3 37.1(2) . . ?
C20 C19 Na3 160.5(4) . . ?
C24 C19 Na3 82.9(3) . . ?
C19 C20 C21 120.2(6) . . ?
C19 C20 C27 122.6(5) . . ?
C21 C20 C27 117.2(6) . . ?
C22 C21 C20 121.0(7) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120.5(6) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 120.8(7) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 O9 125.7(6) . . ?
C23 C24 C19 121.0(6) . . ?
O9 C24 C19 113.3(4) . . ?
O9 C25 C26 111.6(6) . . ?
O9 C25 H25A 109.3 . . ?
C26 C25 H25A 109.3 . . ?
O9 C25 H25B 109.3 . . ?
C26 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O8 C27 C20 129.0(6) . . ?
O8 C27 H27 115.5 . . ?
C20 C27 H27 115.5 . . ?
O10 C28 C33 120.4(5) . . ?
O10 C28 C29 122.6(5) . . ?
C33 C28 C29 117.0(5) . . ?
O10 C28 Na2 37.9(2) . . ?
C33 C28 Na2 83.3(3) . . ?
C29 C28 Na2 158.5(4) . . ?
C30 C29 C36 117.9(5) . . ?
C30 C29 C28 119.2(5) . . ?
C36 C29 C28 122.8(5) . . ?
C31 C30 C29 121.1(6) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C30 C31 C32 119.7(6) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C33 C32 C31 120.8(6) . . ?
C33 C32 H32A 119.6 . . ?
C31 C32 H32A 119.6 . . ?
C32 C33 O12 124.3(5) . . ?
C32 C33 C28 122.2(5) . . ?
O12 C33 C28 113.5(5) . . ?
O12 C34 C35 107.9(5) . . ?
O12 C34 H34A 110.1 . . ?
C35 C34 H34A 110.1 . . ?
O12 C34 H34B 110.1 . . ?
C35 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O11 C36 C29 128.7(5) . . ?
O11 C36 H36 115.7 . . ?
C29 C36 H36 115.7 . . ?
O13 C37 C42 119.6(4) . . ?
O13 C37 C38 123.9(5) . . ?
C42 C37 C38 116.5(5) . . ?
C45 C38 C39 118.0(5) . . ?
C45 C38 C37 122.9(5) . . ?
C39 C38 C37 119.1(5) . . ?
C40 C39 C38 121.1(6) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C39 C40 C41 121.3(6) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 H40 119.3 . . ?
C42 C41 C40 119.6(6) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
C41 C42 O15 125.2(5) . . ?
C41 C42 C37 122.1(5) . . ?
O15 C42 C37 112.6(4) . . ?
O15 C43 C44 106.8(5) . . ?
O15 C43 H43A 110.4 . . ?
C44 C43 H43A 110.4 . . ?
O15 C43 H43B 110.4 . . ?
C44 C43 H43B 110.4 . . ?
H43A C43 H43B 108.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O14 C45 C38 127.9(5) . . ?
O14 C45 H45 116.0 . . ?
C38 C45 H45 116.0 . . ?
O16 C46 C47 124.9(5) . . ?
O16 C46 C51 118.2(5) . . ?
C47 C46 C51 116.9(5) . . ?
C46 C47 C48 120.2(6) . . ?
C46 C47 C54 121.6(5) . . ?
C48 C47 C54 118.2(5) . . ?
C49 C48 C47 120.8(6) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C48 C49 C50 120.5(6) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 120.8(6) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
O18 C51 C50 125.3(5) . . ?
O18 C51 C46 113.9(4) . . ?
C50 C51 C46 120.8(6) . . ?
O18 C52 C53 109.8(5) . . ?
O18 C52 H52A 109.7 . . ?
C53 C52 H52A 109.7 . . ?
O18 C52 H52B 109.7 . . ?
C53 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O17 C54 C47 129.3(5) . . ?
O17 C54 H54 115.3 . . ?
C47 C54 H54 115.3 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C55 C56 N19 115.1(12) . . ?
C55 C56 H56A 108.5 . . ?
N19 C56 H56A 108.5 . . ?
C55 C56 H56B 108.5 . . ?
N19 C56 H56B 108.5 . . ?
H56A C56 H56B 107.5 . . ?
N19 C57 C58 102.4(8) . . ?
N19 C57 H57A 111.3 . . ?
C58 C57 H57A 111.3 . . ?
N19 C57 H57B 111.3 . . ?
C58 C57 H57B 111.3 . . ?
H57A C57 H57B 109.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N19 C59 C60 124.8(10) . . ?
N19 C59 H59A 106.1 . . ?
C60 C59 H59A 106.1 . . ?
N19 C59 H59B 106.1 . . ?
C60 C59 H59B 106.1 . . ?
H59A C59 H59B 106.3 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N2 N1 Ni2 123.2(4) . . ?
N2 N1 Ni1 130.2(4) . . ?
Ni2 N1 Ni1 100.39(15) . . ?
N2 N1 Na3 103.0(3) . . ?
Ni2 N1 Na3 92.20(15) . . ?
Ni1 N1 Na3 97.73(15) . . ?
N3 N2 N1 177.3(7) . . ?
N3 N2 Na3 123.2(6) . . ?
N1 N2 Na3 54.9(3) . . ?
N5 N4 Ni1 130.6(3) . . ?
N5 N4 Ni3 123.0(3) . . ?
Ni1 N4 Ni3 99.78(15) . . ?
N5 N4 Na1 102.9(3) . . ?
Ni1 N4 Na1 97.76(15) . . ?
Ni3 N4 Na1 93.11(13) . . ?
N6 N5 N4 176.4(6) . . ?
N6 N5 Na1 121.5(5) . . ?
N4 N5 Na1 55.0(3) . . ?
N8 N7 Ni4 124.2(3) . . ?
N8 N7 Ni1 125.7(3) . . ?
Ni4 N7 Ni1 99.81(15) . . ?
N8 N7 Na2 109.6(4) . . ?
Ni4 N7 Na2 93.35(14) . . ?
Ni1 N7 Na2 96.26(14) . . ?
N9 N8 N7 179.1(7) . . ?
N11 N10 Ni2 122.6(4) . . ?
N11 N10 Ni1 130.4(3) . . ?
Ni2 N10 Ni1 99.85(15) . . ?
N11 N10 Na1 104.5(3) . . ?
Ni2 N10 Na1 92.66(14) . . ?
Ni1 N10 Na1 97.33(14) . . ?
N12 N11 N10 177.0(6) . . ?
N14 N13 Ni1 128.6(3) . . ?
N14 N13 Ni4 124.8(3) . . ?
Ni1 N13 Ni4 100.98(16) . . ?
N14 N13 Na3 101.0(3) . . ?
Ni1 N13 Na3 98.35(15) . . ?
Ni4 N13 Na3 93.05(13) . . ?
N15 N14 N13 176.4(6) . . ?
N15 N14 Na3 120.5(5) . . ?
N13 N14 Na3 56.2(3) . . ?
N17 N16 Ni3 121.4(3) . . ?
N17 N16 Ni1 127.9(3) . . ?
Ni3 N16 Ni1 100.23(15) . . ?
N17 N16 Na2 110.6(3) . . ?
Ni3 N16 Na2 93.12(14) . . ?
Ni1 N16 Na2 95.40(14) . . ?
N18 N17 N16 177.3(6) . . ?
C59 N19 C56 108.5(9) . . ?
C59 N19 C57 125.6(9) . . ?
C56 N19 C57 106.4(9) . . ?
C59 N19 H19A 105.4 . . ?
C56 N19 H19A 112.5 . . ?
C57 N19 H19A 98.1 . . ?
O1 Na1 O16 160.17(14) . . ?
O1 Na1 O18 124.00(15) . . ?
O16 Na1 O18 67.43(13) . . ?
O1 Na1 O3 67.20(13) . . ?
O16 Na1 O3 126.98(14) . . ?
O18 Na1 O3 110.73(14) . . ?
O1 Na1 N4 91.87(14) . . ?
O16 Na1 N4 72.82(13) . . ?
O18 Na1 N4 139.09(15) . . ?
O3 Na1 N4 100.46(14) . . ?
O1 Na1 N10 72.92(13) . . ?
O16 Na1 N10 90.29(13) . . ?
O18 Na1 N10 97.18(13) . . ?
O3 Na1 N10 139.44(14) . . ?
N4 Na1 N10 73.35(12) . . ?
O1 Na1 N5 82.05(14) . . ?
O16 Na1 N5 87.44(13) . . ?
O18 Na1 N5 153.93(15) . . ?
O3 Na1 N5 78.33(13) . . ?
N4 Na1 N5 22.18(11) . . ?
N10 Na1 N5 89.45(12) . . ?
O1 Na1 Ni2 34.64(9) . . ?
O16 Na1 Ni2 128.26(10) . . ?
O18 Na1 Ni2 114.12(11) . . ?
O3 Na1 Ni2 101.76(10) . . ?
N4 Na1 Ni2 83.30(9) . . ?
N10 Na1 Ni2 38.36(9) . . ?
N5 Na1 Ni2 86.46(9) . . ?
O1 Na1 Ni3 130.01(11) . . ?
O16 Na1 Ni3 34.38(8) . . ?
O18 Na1 Ni3 101.70(11) . . ?
O3 Na1 Ni3 117.35(11) . . ?
N4 Na1 Ni3 38.63(9) . . ?
N10 Na1 Ni3 83.19(10) . . ?
N5 Na1 Ni3 53.93(10) . . ?
Ni2 Na1 Ni3 111.72(5) . . ?
O1 Na1 Ni1 80.55(9) . . ?
O16 Na1 Ni1 79.66(9) . . ?
O18 Na1 Ni1 123.41(11) . . ?
O3 Na1 Ni1 125.82(10) . . ?
N4 Na1 Ni1 36.62(8) . . ?
N10 Na1 Ni1 36.72(9) . . ?
N5 Na1 Ni1 54.24(8) . . ?
Ni2 Na1 Ni1 55.79(3) . . ?
Ni3 Na1 Ni1 55.92(3) . . ?
O13 Na2 O10 162.87(16) . . ?
O13 Na2 O15 67.56(12) . . ?
O10 Na2 O15 125.60(14) . . ?
O13 Na2 O12 121.11(14) . . ?
O10 Na2 O12 67.87(12) . . ?
O15 Na2 O12 109.05(15) . . ?
O13 Na2 N7 93.69(14) . . ?
O10 Na2 N7 73.50(13) . . ?
O15 Na2 N7 102.67(14) . . ?
O12 Na2 N7 139.57(13) . . ?
O13 Na2 N16 72.49(12) . . ?
O10 Na2 N16 92.93(13) . . ?
O15 Na2 N16 139.81(13) . . ?
O12 Na2 N16 94.82(14) . . ?
N7 Na2 N16 75.40(13) . . ?
O13 Na2 C28 159.12(14) . . ?
O10 Na2 C28 20.63(13) . . ?
O15 Na2 C28 130.19(14) . . ?
O12 Na2 C28 47.82(13) . . ?
N7 Na2 C28 92.38(14) . . ?
N16 Na2 C28 89.81(13) . . ?
O13 Na2 Ni4 131.77(12) . . ?
O10 Na2 Ni4 34.88(9) . . ?
O15 Na2 Ni4 119.13(11) . . ?
O12 Na2 Ni4 102.34(9) . . ?
N7 Na2 Ni4 38.67(8) . . ?
N16 Na2 Ni4 84.86(10) . . ?
C28 Na2 Ni4 54.52(10) . . ?
O13 Na2 Ni3 34.06(9) . . ?
O10 Na2 Ni3 131.01(12) . . ?
O15 Na2 Ni3 101.59(9) . . ?
O12 Na2 Ni3 111.61(10) . . ?
N7 Na2 Ni3 85.07(9) . . ?
N16 Na2 Ni3 38.46(8) . . ?
C28 Na2 Ni3 127.09(11) . . ?
Ni4 Na2 Ni3 113.32(6) . . ?
O13 Na2 Ni1 81.35(10) . . ?
O10 Na2 Ni1 81.58(11) . . ?
O15 Na2 Ni1 128.42(11) . . ?
O12 Na2 Ni1 122.29(11) . . ?
N7 Na2 Ni1 37.75(9) . . ?
N16 Na2 Ni1 37.66(9) . . ?
C28 Na2 Ni1 91.42(11) . . ?
Ni4 Na2 Ni1 56.69(3) . . ?
Ni3 Na2 Ni1 56.63(3) . . ?
O7 Na3 O4 161.66(15) . . ?
O7 Na3 O9 67.95(14) . . ?
O4 Na3 O9 124.91(17) . . ?
O7 Na3 O6 125.55(15) . . ?
O4 Na3 O6 66.74(14) . . ?
O9 Na3 O6 106.05(15) . . ?
O7 Na3 N13 72.86(13) . . ?
O4 Na3 N13 92.33(14) . . ?
O9 Na3 N13 140.52(16) . . ?
O6 Na3 N13 100.24(14) . . ?
O7 Na3 N1 91.23(14) . . ?
O4 Na3 N1 73.66(13) . . ?
O9 Na3 N1 103.26(14) . . ?
O6 Na3 N1 139.47(15) . . ?
N13 Na3 N1 72.53(13) . . ?
O7 Na3 N14 88.02(14) . . ?
O4 Na3 N14 81.41(14) . . ?
O9 Na3 N14 153.09(15) . . ?
O6 Na3 N14 77.58(14) . . ?
N13 Na3 N14 22.77(11) . . ?
N1 Na3 N14 88.61(13) . . ?
O7 Na3 N2 80.88(14) . . ?
O4 Na3 N2 88.05(14) . . ?
O9 Na3 N2 81.24(14) . . ?
O6 Na3 N2 153.53(16) . . ?
N13 Na3 N2 88.19(13) . . ?
N1 Na3 N2 22.13(11) . . ?
N14 Na3 N2 107.63(13) . . ?
O7 Na3 C19 20.29(13) . . ?
O4 Na3 C19 164.67(15) . . ?
O9 Na3 C19 47.74(14) . . ?
O6 Na3 C19 126.26(14) . . ?
N13 Na3 C19 92.88(14) . . ?
N1 Na3 C19 94.21(13) . . ?
N14 Na3 C19 108.14(15) . . ?
N2 Na3 C19 77.72(13) . . ?
O7 Na3 Ni2 129.33(11) . . ?
O4 Na3 Ni2 35.41(9) . . ?
O9 Na3 Ni2 118.17(12) . . ?
O6 Na3 Ni2 102.04(11) . . ?
N13 Na3 Ni2 83.48(9) . . ?
N1 Na3 Ni2 38.40(9) . . ?
N14 Na3 Ni2 86.10(9) . . ?
N2 Na3 Ni2 53.67(10) . . ?
C19 Na3 Ni2 131.28(10) . . ?
O7 Na3 Ni4 34.75(9) . . ?
O4 Na3 Ni4 130.16(12) . . ?
O9 Na3 Ni4 102.69(12) . . ?
O6 Na3 Ni4 116.76(12) . . ?
N13 Na3 Ni4 38.23(9) . . ?
N1 Na3 Ni4 82.63(10) . . ?
N14 Na3 Ni4 54.37(10) . . ?
N2 Na3 Ni4 85.23(11) . . ?
C19 Na3 Ni4 54.97(11) . . ?
Ni2 Na3 Ni4 111.68(5) . . ?
O7 Na3 Ni1 80.79(9) . . ?
O4 Na3 Ni1 80.87(10) . . ?
O9 Na3 Ni1 129.02(12) . . ?
O6 Na3 Ni1 124.92(11) . . ?
N13 Na3 Ni1 36.04(8) . . ?
N1 Na3 Ni1 36.50(9) . . ?
N14 Na3 Ni1 53.64(9) . . ?
N2 Na3 Ni1 53.99(10) . . ?
C19 Na3 Ni1 95.02(10) . . ?
Ni2 Na3 Ni1 55.89(3) . . ?
Ni4 Na3 Ni1 55.79(3) . . ?
N13 Ni1 N1 91.37(15) . . ?
N13 Ni1 N4 171.86(16) . . ?
N1 Ni1 N4 94.18(15) . . ?
N13 Ni1 N16 95.15(14) . . ?
N1 Ni1 N16 171.59(14) . . ?
N4 Ni1 N16 79.92(14) . . ?
N13 Ni1 N10 95.32(14) . . ?
N1 Ni1 N10 79.25(15) . . ?
N4 Ni1 N10 91.56(14) . . ?
N16 Ni1 N10 94.83(14) . . ?
N13 Ni1 N7 79.32(14) . . ?
N1 Ni1 N7 93.49(15) . . ?
N4 Ni1 N7 94.39(14) . . ?
N16 Ni1 N7 92.93(15) . . ?
N10 Ni1 N7 170.94(14) . . ?
N13 Ni1 Na2 85.98(11) . . ?
N1 Ni1 Na2 139.18(11) . . ?
N4 Ni1 Na2 85.93(11) . . ?
N16 Ni1 Na2 46.95(10) . . ?
N10 Ni1 Na2 141.56(11) . . ?
N7 Ni1 Na2 45.99(11) . . ?
N13 Ni1 Na1 141.09(11) . . ?
N1 Ni1 Na1 85.22(10) . . ?
N4 Ni1 Na1 45.62(11) . . ?
N16 Ni1 Na1 86.38(10) . . ?
N10 Ni1 Na1 45.94(10) . . ?
N7 Ni1 Na1 139.53(10) . . ?
Na2 Ni1 Na1 120.69(4) . . ?
N13 Ni1 Na3 45.61(11) . . ?
N1 Ni1 Na3 45.77(10) . . ?
N4 Ni1 Na3 139.73(11) . . ?
N16 Ni1 Na3 140.34(10) . . ?
N10 Ni1 Na3 85.30(10) . . ?
N7 Ni1 Na3 85.74(10) . . ?
Na2 Ni1 Na3 120.05(4) . . ?
Na1 Ni1 Na3 119.24(5) . . ?
O1 Ni2 O4 176.35(15) . . ?
O1 Ni2 O2 88.83(14) . . ?
O4 Ni2 O2 89.12(15) . . ?
O1 Ni2 O5 89.81(15) . . ?
O4 Ni2 O5 87.34(15) . . ?
O2 Ni2 O5 94.81(16) . . ?
O1 Ni2 N1 93.99(15) . . ?
O4 Ni2 N1 89.11(14) . . ?
O2 Ni2 N1 92.15(16) . . ?
O5 Ni2 N1 172.13(16) . . ?
O1 Ni2 N10 88.37(13) . . ?
O4 Ni2 N10 94.05(14) . . ?
O2 Ni2 N10 171.93(15) . . ?
O5 Ni2 N10 92.75(15) . . ?
N1 Ni2 N10 80.50(14) . . ?
O1 Ni2 Na3 142.97(11) . . ?
O4 Ni2 Na3 39.90(10) . . ?
O2 Ni2 Na3 87.47(11) . . ?
O5 Ni2 Na3 127.21(12) . . ?
N1 Ni2 Na3 49.40(11) . . ?
N10 Ni2 Na3 90.20(10) . . ?
O1 Ni2 Na1 39.51(10) . . ?
O4 Ni2 Na1 142.63(11) . . ?
O2 Ni2 Na1 128.25(11) . . ?
O5 Ni2 Na1 89.08(11) . . ?
N1 Ni2 Na1 89.49(11) . . ?
N10 Ni2 Na1 48.98(10) . . ?
Na3 Ni2 Na1 129.07(5) . . ?
O13 Ni3 O16 179.23(13) . . ?
O13 Ni3 O14 88.69(13) . . ?
O16 Ni3 O14 90.67(13) . . ?
O13 Ni3 O17 91.34(15) . . ?
O16 Ni3 O17 88.26(14) . . ?
O14 Ni3 O17 91.79(15) . . ?
O13 Ni3 N16 87.33(13) . . ?
O16 Ni3 N16 93.36(14) . . ?
O14 Ni3 N16 171.88(15) . . ?
O17 Ni3 N16 95.38(14) . . ?
O13 Ni3 N4 93.18(15) . . ?
O16 Ni3 N4 87.28(13) . . ?
O14 Ni3 N4 93.10(14) . . ?
O17 Ni3 N4 173.42(15) . . ?
N16 Ni3 N4 80.07(14) . . ?
O13 Ni3 Na2 38.96(9) . . ?
O16 Ni3 Na2 141.71(9) . . ?
O14 Ni3 Na2 127.50(11) . . ?
O17 Ni3 Na2 92.85(10) . . ?
N16 Ni3 Na2 48.41(11) . . ?
N4 Ni3 Na2 87.68(10) . . ?
O13 Ni3 Na1 141.13(11) . . ?
O16 Ni3 Na1 39.26(9) . . ?
O14 Ni3 Na1 88.84(11) . . ?
O17 Ni3 Na1 127.51(11) . . ?
N16 Ni3 Na1 89.81(11) . . ?
N4 Ni3 Na1 48.27(10) . . ?
Na2 Ni3 Na1 126.69(5) . . ?
O10 Ni4 O7 177.15(12) . . ?
O10 Ni4 O11 88.36(14) . . ?
O7 Ni4 O11 89.26(14) . . ?
O10 Ni4 O8 90.88(15) . . ?
O7 Ni4 O8 87.72(14) . . ?
O11 Ni4 O8 93.86(15) . . ?
O10 Ni4 N13 93.97(15) . . ?
O7 Ni4 N13 87.67(14) . . ?
O11 Ni4 N13 91.78(15) . . ?
O8 Ni4 N13 172.67(15) . . ?
O10 Ni4 N7 88.00(14) . . ?
O7 Ni4 N7 94.58(14) . . ?
O11 Ni4 N7 170.65(14) . . ?
O8 Ni4 N7 94.81(14) . . ?
N13 Ni4 N7 79.88(14) . . ?
O10 Ni4 Na2 40.11(9) . . ?
O7 Ni4 Na2 142.39(10) . . ?
O11 Ni4 Na2 128.27(11) . . ?
O8 Ni4 Na2 91.67(11) . . ?
N13 Ni4 Na2 88.52(11) . . ?
N7 Ni4 Na2 47.97(11) . . ?
O10 Ni4 Na3 142.29(11) . . ?
O7 Ni4 Na3 39.10(9) . . ?
O11 Ni4 Na3 87.72(11) . . ?
O8 Ni4 Na3 126.81(12) . . ?
N13 Ni4 Na3 48.72(11) . . ?
N7 Ni4 Na3 89.89(11) . . ?
Na2 Ni4 Na3 127.47(5) . . ?
C1 O1 Ni2 128.9(3) . . ?
C1 O1 Na1 124.2(3) . . ?
Ni2 O1 Na1 105.85(15) . . ?
C9 O2 Ni2 125.2(4) . . ?
C6 O3 C7 116.8(4) . . ?
C6 O3 Na1 115.1(3) . . ?
C7 O3 Na1 126.3(3) . . ?
C10 O4 Ni2 130.0(3) . . ?
C10 O4 Na3 123.8(3) . . ?
Ni2 O4 Na3 104.70(15) . . ?
C18 O5 Ni2 125.6(4) . . ?
C15 O6 C16 117.7(5) . . ?
C15 O6 Na3 115.4(3) . . ?
C16 O6 Na3 125.4(4) . . ?
C19 O7 Ni4 130.9(4) . . ?
C19 O7 Na3 122.6(4) . . ?
Ni4 O7 Na3 106.15(14) . . ?
C27 O8 Ni4 125.9(4) . . ?
C24 O9 C25 120.9(5) . . ?
C24 O9 Na3 116.0(3) . . ?
C25 O9 Na3 123.2(4) . . ?
C28 O10 Ni4 129.1(3) . . ?
C28 O10 Na2 121.5(3) . . ?
Ni4 O10 Na2 105.01(14) . . ?
C36 O11 Ni4 125.7(3) . . ?
C33 O12 C34 116.9(4) . . ?
C33 O12 Na2 114.6(3) . . ?
C34 O12 Na2 124.8(3) . . ?
C37 O13 Ni3 129.6(3) . . ?
C37 O13 Na2 123.4(3) . . ?
Ni3 O13 Na2 106.98(14) . . ?
C45 O14 Ni3 127.0(3) . . ?
C42 O15 C43 116.2(4) . . ?
C42 O15 Na2 116.7(3) . . ?
C43 O15 Na2 126.8(3) . . ?
C46 O16 Ni3 129.4(3) . . ?
C46 O16 Na1 123.9(3) . . ?
Ni3 O16 Na1 106.36(13) . . ?
C54 O17 Ni3 126.0(4) . . ?
C51 O18 C52 118.3(4) . . ?
C51 O18 Na1 116.6(3) . . ?
C52 O18 Na1 125.1(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
N19 H19A N6 0.91 2.02 2.934(9) 176.8 1_455

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 982504'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_co7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H54 Co4 N18 Na3 O18, C6 H16 N'
_chemical_formula_sum            'C60 H70 Co4 N19 Na3 O18'
_chemical_formula_weight         1650.04

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'

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                   13.2448(5)
_cell_length_b                   26.5297(9)
_cell_length_c                   22.1593(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.648(3)
_cell_angle_gamma                90.00
_cell_volume                     7734.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    16772
_cell_measurement_theta_min      3.380
_cell_measurement_theta_max      28.875

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3392
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            58550
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.01
_reflns_number_total             13561
_reflns_number_gt                9059
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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  'Bruker SHELXTL'

_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)+(0.0969P)²+14.5981P] 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         13561
_refine_ls_number_parameters     946
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2229
_refine_ls_wR_factor_gt          0.1863
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.500 1.000 234.5 5.4
2 0.213 0.106 0.971 22.7 0.6
3 0.287 0.606 0.529 22.7 0.5
4 0.500 1.000 0.500 234.5 5.1
5 0.713 0.394 0.471 22.7 0.2
6 0.787 0.894 0.029 22.7 -0.1
_platon_squeeze_details          
;
;

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
C1 C 0.8890(5) 0.5351(2) 0.3668(3) 0.0546(15) Uani 1 1 d . . .
C2 C 0.9204(6) 0.5025(3) 0.3222(3) 0.0720(19) Uani 1 1 d . . .
C3 C 1.0187(7) 0.4825(4) 0.3282(4) 0.101(3) Uani 1 1 d . . .
H3 H 1.0376 0.4612 0.2981 0.121 Uiso 1 1 calc R . .
C4 C 1.0866(8) 0.4933(4) 0.3765(5) 0.115(3) Uani 1 1 d . . .
H4 H 1.1514 0.4793 0.3800 0.138 Uiso 1 1 calc R . .
C5 C 1.0584(6) 0.5258(3) 0.4212(4) 0.090(2) Uani 1 1 d . . .
H5 H 1.1051 0.5337 0.4545 0.108 Uiso 1 1 calc R . .
C6 C 0.9630(5) 0.5460(3) 0.4166(3) 0.0618(17) Uani 1 1 d . . .
C7 C 1.0031(7) 0.5977(3) 0.5057(3) 0.088(2) Uani 1 1 d . . .
H7A H 1.0582 0.6141 0.4879 0.106 Uiso 1 1 calc R . .
H7B H 1.0313 0.5700 0.5307 0.106 Uiso 1 1 calc R . .
C8 C 0.9537(8) 0.6337(4) 0.5429(4) 0.109(3) Uani 1 1 d . . .
H8A H 0.9325 0.6628 0.5189 0.163 Uiso 1 1 calc R . .
H8B H 1.0007 0.6438 0.5770 0.163 Uiso 1 1 calc R . .
H8C H 0.8954 0.6182 0.5572 0.163 Uiso 1 1 calc R . .
C9 C 0.8542(7) 0.4889(3) 0.2690(4) 0.083(2) Uani 1 1 d . . .
H9 H 0.8824 0.4667 0.2431 0.100 Uiso 1 1 calc R . .
C10 C 0.4760(5) 0.5311(2) 0.2284(3) 0.0555(15) Uani 1 1 d . . .
C11 C 0.4458(6) 0.5032(3) 0.2773(3) 0.0697(19) Uani 1 1 d . . .
C12 C 0.3436(8) 0.4847(4) 0.2733(5) 0.105(3) Uani 1 1 d . . .
H12 H 0.3231 0.4666 0.3057 0.126 Uiso 1 1 calc R . .
C13 C 0.2775(8) 0.4927(4) 0.2245(6) 0.126(4) Uani 1 1 d . . .
H13 H 0.2119 0.4799 0.2226 0.151 Uiso 1 1 calc R . .
C14 C 0.3068(7) 0.5205(4) 0.1762(5) 0.102(3) Uani 1 1 d . . .
H14 H 0.2598 0.5263 0.1424 0.123 Uiso 1 1 calc R . .
C15 C 0.4036(6) 0.5396(3) 0.1771(4) 0.0700(19) Uani 1 1 d . . .
C16 C 0.3625(9) 0.5817(5) 0.0829(5) 0.138(4) Uani 1 1 d . . .
H16A H 0.3361 0.5516 0.0617 0.165 Uiso 1 1 calc R . .
H16B H 0.3063 0.5986 0.0988 0.165 Uiso 1 1 calc R . .
C17 C 0.4029(12) 0.6128(5) 0.0432(5) 0.192(7) Uani 1 1 d . . .
H17A H 0.3526 0.6200 0.0095 0.287 Uiso 1 1 calc R . .
H17B H 0.4603 0.5966 0.0286 0.287 Uiso 1 1 calc R . .
H17C H 0.4244 0.6436 0.0633 0.287 Uiso 1 1 calc R . .
C18 C 0.5134(7) 0.4929(3) 0.3312(4) 0.077(2) Uani 1 1 d . . .
H18 H 0.4849 0.4749 0.3609 0.093 Uiso 1 1 calc R . .
C19 C 0.7191(4) 0.6707(2) 0.0690(2) 0.0516(15) Uani 1 1 d . . .
C20 C 0.7617(5) 0.7127(3) 0.0420(3) 0.0609(17) Uani 1 1 d . . .
C21 C 0.8263(6) 0.7058(4) -0.0038(3) 0.084(2) Uani 1 1 d . . .
H21 H 0.8545 0.7337 -0.0209 0.101 Uiso 1 1 calc R . .
C22 C 0.8475(7) 0.6593(4) -0.0230(4) 0.100(3) Uani 1 1 d . . .
H22 H 0.8886 0.6553 -0.0540 0.120 Uiso 1 1 calc R . .
C23 C 0.8084(6) 0.6178(4) 0.0032(4) 0.092(3) Uani 1 1 d . . .
H23 H 0.8255 0.5859 -0.0096 0.110 Uiso 1 1 calc R . .
C24 C 0.7442(5) 0.6220(3) 0.0482(3) 0.0622(17) Uani 1 1 d . . .
C25 C 0.7163(8) 0.5324(3) 0.0569(4) 0.102(3) Uani 1 1 d . . .
H25A H 0.7882 0.5246 0.0645 0.122 Uiso 1 1 calc R . .
H25B H 0.6955 0.5290 0.0137 0.122 Uiso 1 1 calc R . .
C26 C 0.6588(8) 0.4976(3) 0.0902(4) 0.110(3) Uani 1 1 d . . .
H26A H 0.6758 0.4636 0.0805 0.165 Uiso 1 1 calc R . .
H26B H 0.5874 0.5031 0.0792 0.165 Uiso 1 1 calc R . .
H26C H 0.6752 0.5032 0.1331 0.165 Uiso 1 1 calc R . .
C27 C 0.7422(6) 0.7626(3) 0.0590(3) 0.074(2) Uani 1 1 d . . .
H27 H 0.7741 0.7874 0.0385 0.089 Uiso 1 1 calc R . .
C28 C 0.4722(5) 0.8112(2) 0.2012(2) 0.0482(14) Uani 1 1 d . . .
C29 C 0.3895(5) 0.7949(3) 0.1592(3) 0.0606(16) Uani 1 1 d . . .
C30 C 0.2910(6) 0.8153(3) 0.1623(4) 0.083(2) Uani 1 1 d . . .
H30 H 0.2368 0.8048 0.1347 0.100 Uiso 1 1 calc R . .
C31 C 0.2756(7) 0.8504(3) 0.2061(4) 0.094(3) Uani 1 1 d . . .
H31 H 0.2113 0.8642 0.2074 0.113 Uiso 1 1 calc R . .
C32 C 0.3554(6) 0.8652(3) 0.2480(4) 0.076(2) Uani 1 1 d . . .
H32A H 0.3436 0.8878 0.2785 0.092 Uiso 1 1 calc R . .
C33 C 0.4498(5) 0.8473(2) 0.2455(3) 0.0560(15) Uani 1 1 d . . .
C34 C 0.5177(7) 0.8906(3) 0.3365(3) 0.079(2) Uani 1 1 d . . .
H34A H 0.4720 0.8732 0.3607 0.095 Uiso 1 1 calc R . .
H34B H 0.4870 0.9225 0.3233 0.095 Uiso 1 1 calc R . .
C35 C 0.6184(8) 0.8995(3) 0.3738(3) 0.106(3) Uani 1 1 d . . .
H35A H 0.6664 0.9120 0.3481 0.159 Uiso 1 1 calc R . .
H35B H 0.6430 0.8685 0.3923 0.159 Uiso 1 1 calc R . .
H35C H 0.6102 0.9239 0.4049 0.159 Uiso 1 1 calc R . .
C36 C 0.3989(6) 0.7584(3) 0.1131(3) 0.0698(19) Uani 1 1 d . . .
H36 H 0.3402 0.7516 0.0872 0.084 Uiso 1 1 calc R . .
C37 C 0.8888(5) 0.8258(2) 0.3682(3) 0.0521(15) Uani 1 1 d . . .
C38 C 0.9655(5) 0.8192(3) 0.4169(3) 0.0632(18) Uani 1 1 d . . .
C39 C 1.0527(7) 0.8504(3) 0.4217(4) 0.096(3) Uani 1 1 d . . .
H39 H 1.1029 0.8462 0.4543 0.115 Uiso 1 1 calc R . .
C40 C 1.0642(7) 0.8862(4) 0.3797(4) 0.111(3) Uani 1 1 d . . .
H40 H 1.1210 0.9071 0.3844 0.133 Uiso 1 1 calc R . .
C41 C 0.9926(6) 0.8921(3) 0.3298(4) 0.083(2) Uani 1 1 d . . .
H41 H 1.0025 0.9162 0.3006 0.100 Uiso 1 1 calc R . .
C42 C 0.9069(5) 0.8627(2) 0.3230(3) 0.0584(16) Uani 1 1 d . . .
C43 C 0.8531(6) 0.8937(3) 0.2240(3) 0.072(2) Uani 1 1 d . . .
H43A H 0.9174 0.8834 0.2109 0.086 Uiso 1 1 calc R . .
H43B H 0.8576 0.9291 0.2350 0.086 Uiso 1 1 calc R . .
C44 C 0.7684(7) 0.8854(3) 0.1740(3) 0.094(3) Uani 1 1 d . . .
H44A H 0.7765 0.9079 0.1409 0.140 Uiso 1 1 calc R . .
H44B H 0.7045 0.8918 0.1889 0.140 Uiso 1 1 calc R . .
H44C H 0.7701 0.8512 0.1600 0.140 Uiso 1 1 calc R . .
C45 C 0.9592(6) 0.7823(3) 0.4624(3) 0.0697(19) Uani 1 1 d . . .
H45 H 1.0147 0.7806 0.4923 0.084 Uiso 1 1 calc R . .
C46 C 0.6436(4) 0.6920(2) 0.5057(2) 0.0468(13) Uani 1 1 d . . .
C47 C 0.6035(5) 0.7367(2) 0.5280(3) 0.0549(15) Uani 1 1 d . . .
C48 C 0.5377(6) 0.7343(3) 0.5747(3) 0.075(2) Uani 1 1 d . . .
H48 H 0.5129 0.7639 0.5899 0.090 Uiso 1 1 calc R . .
C49 C 0.5114(6) 0.6893(3) 0.5969(3) 0.082(2) Uani 1 1 d . . .
H49 H 0.4681 0.6881 0.6270 0.099 Uiso 1 1 calc R . .
C50 C 0.5480(6) 0.6453(3) 0.5753(3) 0.074(2) Uani 1 1 d . . .
H50 H 0.5290 0.6147 0.5910 0.089 Uiso 1 1 calc R . .
C51 C 0.6130(5) 0.6456(2) 0.5304(3) 0.0553(15) Uani 1 1 d . . .
C52 C 0.6257(7) 0.5556(3) 0.5285(4) 0.082(2) Uani 1 1 d . . .
H52A H 0.5528 0.5509 0.5202 0.098 Uiso 1 1 calc R . .
H52B H 0.6443 0.5536 0.5721 0.098 Uiso 1 1 calc R . .
C53 C 0.6792(7) 0.5156(3) 0.4976(4) 0.094(3) Uani 1 1 d . . .
H53A H 0.6583 0.5169 0.4547 0.142 Uiso 1 1 calc R . .
H53B H 0.6627 0.4832 0.5131 0.142 Uiso 1 1 calc R . .
H53C H 0.7513 0.5209 0.5050 0.142 Uiso 1 1 calc R . .
C54 C 0.6266(6) 0.7854(3) 0.5062(3) 0.0663(18) Uani 1 1 d . . .
H54 H 0.5977 0.8124 0.5246 0.080 Uiso 1 1 calc R . .
C55 C 0.1599(13) 0.7703(6) 0.3178(8) 0.212(6) Uani 1 1 d U . .
H55A H 0.0965 0.7856 0.3022 0.317 Uiso 1 1 calc R . .
H55B H 0.2124 0.7955 0.3219 0.317 Uiso 1 1 calc R . .
H55C H 0.1537 0.7557 0.3568 0.317 Uiso 1 1 calc R . .
C56 C 0.1852(13) 0.7322(7) 0.2771(8) 0.204(5) Uani 1 1 d U . .
H56A H 0.2562 0.7359 0.2709 0.244 Uiso 1 1 calc R . .
H56B H 0.1449 0.7372 0.2382 0.244 Uiso 1 1 calc R . .
C57 C 0.1403(15) 0.6502(6) 0.2421(6) 0.231(6) Uani 1 1 d DU . .
H57A H 0.1911 0.6559 0.2147 0.277 Uiso 1 1 calc R . .
H57B H 0.0767 0.6635 0.2223 0.277 Uiso 1 1 calc R . .
C58 C 0.1267(19) 0.5919(6) 0.2471(9) 0.349(10) Uani 1 1 d DU . .
H58A H 0.1547 0.5808 0.2868 0.524 Uiso 1 1 calc R . .
H58B H 0.1614 0.5754 0.2170 0.524 Uiso 1 1 calc R . .
H58C H 0.0557 0.5836 0.2407 0.524 Uiso 1 1 calc R . .
C59 C 0.2493(13) 0.6665(6) 0.3412(7) 0.207(5) Uani 1 1 d DU . .
H59A H 0.2810 0.6378 0.3238 0.249 Uiso 1 1 calc R . .
H59B H 0.2989 0.6935 0.3436 0.249 Uiso 1 1 calc R . .
C60 C 0.2393(14) 0.6534(7) 0.4002(8) 0.228(7) Uani 1 1 d U . .
H60A H 0.1945 0.6768 0.4168 0.342 Uiso 1 1 calc R . .
H60B H 0.3047 0.6543 0.4239 0.342 Uiso 1 1 calc R . .
H60C H 0.2117 0.6200 0.4012 0.342 Uiso 1 1 calc R . .
N1 N 0.7462(3) 0.61470(17) 0.2461(2) 0.0435(10) Uani 1 1 d . . .
N2 N 0.8208(4) 0.6106(2) 0.2223(3) 0.0646(14) Uani 1 1 d . . .
N3 N 0.8901(7) 0.6054(4) 0.1966(4) 0.133(3) Uani 1 1 d . . .
N4 N 0.8116(3) 0.68534(16) 0.35805(17) 0.0358(9) Uani 1 1 d . . .
N5 N 0.8984(4) 0.6789(2) 0.3555(2) 0.0573(13) Uani 1 1 d . . .
N6 N 0.9831(5) 0.6708(4) 0.3556(4) 0.123(3) Uani 1 1 d . . .
N7 N 0.7425(3) 0.73189(15) 0.22740(18) 0.0360(9) Uani 1 1 d . . .
N8 N 0.8283(4) 0.7368(2) 0.2187(2) 0.0609(14) Uani 1 1 d . . .
N9 N 0.9108(5) 0.7421(4) 0.2105(4) 0.130(3) Uani 1 1 d . . .
N10 N 0.6206(3) 0.61815(16) 0.3390(2) 0.0414(10) Uani 1 1 d . . .
N11 N 0.5435(4) 0.61540(18) 0.3618(2) 0.0548(12) Uani 1 1 d . . .
N12 N 0.4711(5) 0.6116(3) 0.3849(4) 0.109(3) Uani 1 1 d . . .
N13 N 0.5564(3) 0.68043(16) 0.21918(18) 0.0383(10) Uani 1 1 d . . .
N14 N 0.4690(4) 0.6737(2) 0.2226(2) 0.0544(13) Uani 1 1 d . . .
N15 N 0.3847(5) 0.6650(3) 0.2234(4) 0.108(3) Uani 1 1 d . . .
N16 N 0.6257(3) 0.73859(15) 0.34282(18) 0.0360(9) Uani 1 1 d . . .
N17 N 0.5404(4) 0.74472(18) 0.3538(2) 0.0499(12) Uani 1 1 d . . .
N18 N 0.4607(5) 0.7531(3) 0.3649(4) 0.101(2) Uani 1 1 d . . .
N19 N 0.1693(8) 0.6818(4) 0.2972(5) 0.152(3) Uani 1 1 d DU . .
H19A H 0.1115 0.6775 0.3155 0.182 Uiso 1 1 d R . .
Na1 Na 0.76040(17) 0.61695(8) 0.42763(9) 0.0475(5) Uani 1 1 d . . .
Na2 Na 0.68653(16) 0.80891(8) 0.27922(9) 0.0453(5) Uani 1 1 d . . .
Na3 Na 0.60620(19) 0.60556(9) 0.15773(10) 0.0540(6) Uani 1 1 d . . .
Co1 Co 0.68281(5) 0.67856(3) 0.28884(3) 0.0361(2) Uani 1 1 d . . .
Co2 Co 0.68409(6) 0.55518(3) 0.29577(3) 0.0490(2) Uani 1 1 d . . .
Co3 Co 0.75330(6) 0.74544(3) 0.41205(3) 0.0433(2) Uani 1 1 d . . .
Co4 Co 0.61452(6) 0.73412(3) 0.15763(3) 0.0444(2) Uani 1 1 d . . .
O1 O 0.7996(3) 0.55420(14) 0.36422(17) 0.0535(10) Uani 1 1 d . . .
O2 O 0.7667(4) 0.50156(17) 0.2522(2) 0.0711(13) Uani 1 1 d . . .
O3 O 0.9286(4) 0.57901(17) 0.45822(19) 0.0668(12) Uani 1 1 d . . .
O4 O 0.5667(3) 0.54881(15) 0.22779(17) 0.0554(10) Uani 1 1 d . . .
O5 O 0.6017(4) 0.50414(16) 0.3439(2) 0.0680(13) Uani 1 1 d . . .
O6 O 0.4374(4) 0.56734(19) 0.1329(2) 0.0789(14) Uani 1 1 d . . .
O7 O 0.6590(3) 0.67381(14) 0.11021(16) 0.0516(10) Uani 1 1 d . . .
O8 O 0.6882(4) 0.77855(17) 0.09767(19) 0.0680(13) Uani 1 1 d . . .
O9 O 0.6993(4) 0.58305(18) 0.0756(2) 0.0703(13) Uani 1 1 d . . .
O10 O 0.5643(3) 0.79550(14) 0.19994(16) 0.0494(9) Uani 1 1 d . . .
O11 O 0.4754(3) 0.73468(17) 0.10343(18) 0.0602(11) Uani 1 1 d . . .
O12 O 0.5346(3) 0.86077(15) 0.28509(18) 0.0597(11) Uani 1 1 d . . .
O13 O 0.8040(3) 0.80113(15) 0.36112(16) 0.0510(10) Uani 1 1 d . . .
O14 O 0.8899(3) 0.75180(16) 0.46799(17) 0.0606(11) Uani 1 1 d . . .
O15 O 0.8314(3) 0.86418(15) 0.27461(18) 0.0613(11) Uani 1 1 d . . .
O16 O 0.7049(3) 0.69019(14) 0.46494(15) 0.0476(9) Uani 1 1 d . . .
O17 O 0.6798(4) 0.79632(15) 0.46600(19) 0.0636(12) Uani 1 1 d . . .
O18 O 0.6535(3) 0.60375(15) 0.50674(18) 0.0592(11) 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
C1 O1 1.284(7) . ?
C1 C2 1.411(9) . ?
C1 C6 1.419(9) . ?
C2 C3 1.398(10) . ?
C2 C9 1.431(10) . ?
C3 C4 1.348(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.366(9) . ?
C5 H5 0.9300 . ?
C6 O3 1.386(7) . ?
C7 O3 1.445(8) . ?
C7 C8 1.466(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 O2 1.223(9) . ?
C9 H9 0.9300 . ?
C10 O4 1.291(7) . ?
C10 C11 1.407(9) . ?
C10 C15 1.418(9) . ?
C11 C18 1.434(11) . ?
C11 C12 1.433(11) . ?
C12 C13 1.327(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(10) . ?
C14 H14 0.9300 . ?
C15 O6 1.343(8) . ?
C16 C17 1.361(14) . ?
C16 O6 1.450(11) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O5 1.208(9) . ?
C18 H18 0.9300 . ?
C19 O7 1.283(7) . ?
C19 C20 1.413(9) . ?
C19 C24 1.423(9) . ?
C19 Na3 3.126(6) . ?
C20 C27 1.409(10) . ?
C20 C21 1.414(9) . ?
C21 C22 1.345(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.389(9) . ?
C23 H23 0.9300 . ?
C24 O9 1.368(8) . ?
C25 O9 1.430(9) . ?
C25 C26 1.453(12) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 O8 1.250(8) . ?
C27 H27 0.9300 . ?
C28 O10 1.293(7) . ?
C28 C29 1.420(9) . ?
C28 C33 1.426(8) . ?
C29 C30 1.421(9) . ?
C29 C36 1.424(9) . ?
C30 C31 1.377(11) . ?
C30 H30 0.9300 . ?
C31 C32 1.381(11) . ?
C31 H31 0.9300 . ?
C32 C33 1.345(9) . ?
C32 H32A 0.9300 . ?
C33 O12 1.390(7) . ?
C34 O12 1.427(7) . ?
C34 C35 1.504(11) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 O11 1.232(8) . ?
C36 H36 0.9300 . ?
C37 O13 1.292(7) . ?
C37 C38 1.406(8) . ?
C37 C42 1.439(8) . ?
C38 C45 1.415(9) . ?
C38 C39 1.414(9) . ?
C39 C40 1.351(11) . ?
C39 H39 0.9300 . ?
C40 C41 1.379(10) . ?
C40 H40 0.9300 . ?
C41 C42 1.371(9) . ?
C41 H41 0.9300 . ?
C42 O15 1.380(7) . ?
C43 O15 1.424(7) . ?
C43 C44 1.499(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 O14 1.240(8) . ?
C45 H45 0.9300 . ?
C46 O16 1.284(6) . ?
C46 C47 1.411(8) . ?
C46 C51 1.425(8) . ?
C47 C54 1.425(9) . ?
C47 C48 1.429(9) . ?
C48 C49 1.353(10) . ?
C48 H48 0.9300 . ?
C49 C50 1.371(10) . ?
C49 H49 0.9300 . ?
C50 C51 1.388(8) . ?
C50 H50 0.9300 . ?
C51 O18 1.363(7) . ?
C52 O18 1.429(7) . ?
C52 C53 1.487(10) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 O17 1.232(8) . ?
C54 H54 0.9300 . ?
C55 C56 1.422(19) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 N19 1.433(16) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 N19 1.494(9) . ?
C57 C58 1.563(9) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 C60 1.375(18) . ?
C59 N19 1.413(16) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N1 N2 1.178(7) . ?
N1 Co2 2.143(4) . ?
N1 Co1 2.158(4) . ?
N1 Na3 2.548(5) . ?
N2 N3 1.142(8) . ?
N2 Na3 3.034(6) . ?
N4 N5 1.170(6) . ?
N4 Co1 2.165(4) . ?
N4 Co3 2.187(4) . ?
N4 Na1 2.524(5) . ?
N5 N6 1.143(8) . ?
N5 Na1 3.045(5) . ?
N7 N8 1.182(6) . ?
N7 Co4 2.158(4) . ?
N7 Co1 2.174(4) . ?
N7 Na2 2.498(5) . ?
N8 N9 1.136(8) . ?
N10 N11 1.193(6) . ?
N10 Co2 2.145(4) . ?
N10 Co1 2.167(4) . ?
N10 Na1 2.539(5) . ?
N11 N12 1.142(7) . ?
N13 N14 1.181(6) . ?
N13 Co1 2.143(4) . ?
N13 Co4 2.174(4) . ?
N13 Na3 2.538(5) . ?
N14 N15 1.143(7) . ?
N14 Na3 3.039(5) . ?
N16 N17 1.194(6) . ?
N16 Co3 2.155(4) . ?
N16 Co1 2.179(4) . ?
N16 Na2 2.526(4) . ?
N17 N18 1.133(7) . ?
N19 H19A 0.9137 . ?
Na1 O16 2.267(4) . ?
Na1 O1 2.277(4) . ?
Na1 O18 2.403(4) . ?
Na1 O3 2.467(5) . ?
Na1 Co2 3.400(2) . ?
Na1 Co3 3.426(2) . ?
Na1 Co1 3.529(2) . ?
Na2 O13 2.259(4) . ?
Na2 O10 2.275(4) . ?
Na2 O15 2.427(5) . ?
Na2 O12 2.453(5) . ?
Na2 Co4 3.393(2) . ?
Na2 Co3 3.417(2) . ?
Na2 Co1 3.465(2) . ?
Na3 O7 2.246(4) . ?
Na3 O4 2.267(4) . ?
Na3 O9 2.390(5) . ?
Na3 O6 2.458(6) . ?
Na3 Co2 3.388(2) . ?
Na3 Co4 3.412(2) . ?
Na3 Co1 3.541(2) . ?
Co2 O1 2.026(4) . ?
Co2 O4 2.043(4) . ?
Co2 O2 2.098(4) . ?
Co2 O5 2.105(5) . ?
Co3 O13 2.021(4) . ?
Co3 O16 2.026(4) . ?
Co3 O14 2.078(4) . ?
Co3 O17 2.114(4) . ?
Co4 O10 2.029(4) . ?
Co4 O7 2.038(4) . ?
Co4 O11 2.080(4) . ?
Co4 O8 2.100(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 C1 C2 123.8(6) . . ?
O1 C1 C6 120.3(5) . . ?
C2 C1 C6 115.9(6) . . ?
C3 C2 C1 120.8(7) . . ?
C3 C2 C9 117.2(7) . . ?
C1 C2 C9 121.9(7) . . ?
C4 C3 C2 121.5(8) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.2(8) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 120.7(8) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 O3 124.8(7) . . ?
C5 C6 C1 121.8(7) . . ?
O3 C6 C1 113.4(6) . . ?
O3 C7 C8 108.7(7) . . ?
O3 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C2 130.6(7) . . ?
O2 C9 H9 114.7 . . ?
C2 C9 H9 114.7 . . ?
O4 C10 C11 123.2(6) . . ?
O4 C10 C15 118.5(6) . . ?
C11 C10 C15 118.3(6) . . ?
C10 C11 C18 122.3(7) . . ?
C10 C11 C12 118.9(8) . . ?
C18 C11 C12 118.7(8) . . ?
C13 C12 C11 121.6(9) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 119.7(9) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 121.8(9) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
O6 C15 C14 125.4(8) . . ?
O6 C15 C10 114.9(6) . . ?
C14 C15 C10 119.7(8) . . ?
C17 C16 O6 111.5(10) . . ?
C17 C16 H16A 109.3 . . ?
O6 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
O6 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C18 C11 130.0(7) . . ?
O5 C18 H18 115.0 . . ?
C11 C18 H18 115.0 . . ?
O7 C19 C20 124.1(6) . . ?
O7 C19 C24 118.4(6) . . ?
C20 C19 C24 117.5(6) . . ?
O7 C19 Na3 37.4(3) . . ?
C20 C19 Na3 161.0(4) . . ?
C24 C19 Na3 81.2(4) . . ?
C27 C20 C19 122.3(6) . . ?
C27 C20 C21 117.4(7) . . ?
C19 C20 C21 120.3(7) . . ?
C22 C21 C20 120.8(8) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 119.9(7) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 122.1(8) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
O9 C24 C23 126.3(7) . . ?
O9 C24 C19 114.4(5) . . ?
C23 C24 C19 119.3(7) . . ?
O9 C25 C26 109.9(7) . . ?
O9 C25 H25A 109.7 . . ?
C26 C25 H25A 109.7 . . ?
O9 C25 H25B 109.7 . . ?
C26 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O8 C27 C20 129.6(6) . . ?
O8 C27 H27 115.2 . . ?
C20 C27 H27 115.2 . . ?
O10 C28 C29 123.1(5) . . ?
O10 C28 C33 120.2(5) . . ?
C29 C28 C33 116.7(6) . . ?
C30 C29 C28 119.7(6) . . ?
C30 C29 C36 116.7(7) . . ?
C28 C29 C36 123.5(6) . . ?
C31 C30 C29 120.2(8) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 120.1(8) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 120.9(7) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C32 C33 O12 124.8(6) . . ?
C32 C33 C28 122.3(7) . . ?
O12 C33 C28 112.9(5) . . ?
O12 C34 C35 108.3(7) . . ?
O12 C34 H34A 110.0 . . ?
C35 C34 H34A 110.0 . . ?
O12 C34 H34B 110.0 . . ?
C35 C34 H34B 110.0 . . ?
H34A C34 H34B 108.4 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O11 C36 C29 127.9(7) . . ?
O11 C36 H36 116.0 . . ?
C29 C36 H36 116.0 . . ?
O13 C37 C38 124.8(5) . . ?
O13 C37 C42 118.2(5) . . ?
C38 C37 C42 117.0(6) . . ?
C37 C38 C45 122.5(6) . . ?
C37 C38 C39 119.7(6) . . ?
C45 C38 C39 117.8(6) . . ?
C40 C39 C38 121.1(7) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C39 C40 C41 120.6(8) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C42 C41 C40 120.5(7) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 O15 125.7(6) . . ?
C41 C42 C37 120.9(6) . . ?
O15 C42 C37 113.4(5) . . ?
O15 C43 C44 107.5(6) . . ?
O15 C43 H43A 110.2 . . ?
C44 C43 H43A 110.2 . . ?
O15 C43 H43B 110.2 . . ?
C44 C43 H43B 110.2 . . ?
H43A C43 H43B 108.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O14 C45 C38 128.8(6) . . ?
O14 C45 H45 115.6 . . ?
C38 C45 H45 115.6 . . ?
O16 C46 C47 124.8(5) . . ?
O16 C46 C51 118.0(5) . . ?
C47 C46 C51 117.2(5) . . ?
C46 C47 C54 122.6(6) . . ?
C46 C47 C48 120.1(6) . . ?
C54 C47 C48 117.3(6) . . ?
C49 C48 C47 120.4(7) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C48 C49 C50 120.5(6) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 121.3(7) . . ?
C49 C50 H50 119.3 . . ?
C51 C50 H50 119.3 . . ?
O18 C51 C50 125.2(6) . . ?
O18 C51 C46 114.4(5) . . ?
C50 C51 C46 120.5(6) . . ?
O18 C52 C53 109.1(6) . . ?
O18 C52 H52A 109.9 . . ?
C53 C52 H52A 109.9 . . ?
O18 C52 H52B 109.9 . . ?
C53 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O17 C54 C47 128.5(6) . . ?
O17 C54 H54 115.8 . . ?
C47 C54 H54 115.8 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C55 C56 N19 114.4(15) . . ?
C55 C56 H56A 108.6 . . ?
N19 C56 H56A 108.7 . . ?
C55 C56 H56B 108.7 . . ?
N19 C56 H56B 108.6 . . ?
H56A C56 H56B 107.6 . . ?
N19 C57 C58 121.2(10) . . ?
N19 C57 H57A 107.0 . . ?
C58 C57 H57A 107.0 . . ?
N19 C57 H57B 107.0 . . ?
C58 C57 H57B 107.0 . . ?
H57A C57 H57B 106.8 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 N19 125.5(16) . . ?
C60 C59 H59A 105.9 . . ?
N19 C59 H59A 105.9 . . ?
C60 C59 H59B 105.9 . . ?
N19 C59 H59B 105.9 . . ?
H59A C59 H59B 106.3 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N2 N1 Co2 123.6(4) . . ?
N2 N1 Co1 131.2(4) . . ?
Co2 N1 Co1 99.25(18) . . ?
N2 N1 Na3 102.7(4) . . ?
Co2 N1 Na3 92.06(17) . . ?
Co1 N1 Na3 97.25(17) . . ?
N3 N2 N1 176.3(8) . . ?
N3 N2 Na3 121.5(6) . . ?
N1 N2 Na3 55.0(3) . . ?
N5 N4 Co1 130.7(4) . . ?
N5 N4 Co3 122.9(4) . . ?
Co1 N4 Co3 98.58(16) . . ?
N5 N4 Na1 105.1(4) . . ?
Co1 N4 Na1 97.34(16) . . ?
Co3 N4 Na1 93.05(14) . . ?
N6 N5 N4 176.2(7) . . ?
N6 N5 Na1 123.1(6) . . ?
N4 N5 Na1 53.2(3) . . ?
N8 N7 Co4 124.7(4) . . ?
N8 N7 Co1 126.9(4) . . ?
Co4 N7 Co1 98.88(17) . . ?
N8 N7 Na2 109.1(4) . . ?
Co4 N7 Na2 93.26(16) . . ?
Co1 N7 Na2 95.50(15) . . ?
N9 N8 N7 179.2(9) . . ?
N11 N10 Co2 122.7(4) . . ?
N11 N10 Co1 131.1(4) . . ?
Co2 N10 Co1 98.89(17) . . ?
N11 N10 Na1 104.8(4) . . ?
Co2 N10 Na1 92.69(16) . . ?
Co1 N10 Na1 96.85(17) . . ?
N12 N11 N10 177.8(7) . . ?
N14 N13 Co1 129.8(4) . . ?
N14 N13 Co4 124.0(4) . . ?
Co1 N13 Co4 99.38(17) . . ?
N14 N13 Na3 103.5(4) . . ?
Co1 N13 Na3 97.94(17) . . ?
Co4 N13 Na3 92.46(15) . . ?
N15 N14 N13 176.0(7) . . ?
N15 N14 Na3 121.8(5) . . ?
N13 N14 Na3 54.3(3) . . ?
N17 N16 Co3 121.7(4) . . ?
N17 N16 Co1 127.5(4) . . ?
Co3 N16 Co1 99.13(17) . . ?
N17 N16 Na2 112.6(3) . . ?
Co3 N16 Na2 93.45(16) . . ?
Co1 N16 Na2 94.59(15) . . ?
N18 N17 N16 176.5(7) . . ?
C59 N19 C56 110.8(12) . . ?
C59 N19 C57 120.3(11) . . ?
C56 N19 C57 107.6(12) . . ?
C59 N19 H19A 105.0 . . ?
C56 N19 H19A 114.4 . . ?
C57 N19 H19A 98.2 . . ?
O16 Na1 O1 163.41(16) . . ?
O16 Na1 O18 67.39(14) . . ?
O1 Na1 O18 122.63(17) . . ?
O16 Na1 O3 124.75(17) . . ?
O1 Na1 O3 66.94(16) . . ?
O18 Na1 O3 109.25(17) . . ?
O16 Na1 N4 74.21(14) . . ?
O1 Na1 N4 92.99(15) . . ?
O18 Na1 N4 140.61(16) . . ?
O3 Na1 N4 99.40(16) . . ?
O16 Na1 N10 91.90(15) . . ?
O1 Na1 N10 74.31(15) . . ?
O18 Na1 N10 97.32(16) . . ?
O3 Na1 N10 140.57(16) . . ?
N4 Na1 N10 75.04(14) . . ?
O16 Na1 N5 88.17(15) . . ?
O1 Na1 N5 82.97(16) . . ?
O18 Na1 N5 154.36(17) . . ?
O3 Na1 N5 77.69(16) . . ?
N4 Na1 N5 21.78(13) . . ?
N10 Na1 N5 90.90(15) . . ?
O16 Na1 Co2 130.53(13) . . ?
O1 Na1 Co2 35.26(11) . . ?
O18 Na1 Co2 114.52(13) . . ?
O3 Na1 Co2 102.04(12) . . ?
N4 Na1 Co2 84.01(11) . . ?
N10 Na1 Co2 39.07(10) . . ?
N5 Na1 Co2 86.90(11) . . ?
O16 Na1 Co3 34.70(9) . . ?
O1 Na1 Co3 132.13(12) . . ?
O18 Na1 Co3 101.94(12) . . ?
O3 Na1 Co3 116.55(14) . . ?
N4 Na1 Co3 39.60(9) . . ?
N10 Na1 Co3 84.29(11) . . ?
N5 Na1 Co3 54.62(11) . . ?
Co2 Na1 Co3 113.01(6) . . ?
O16 Na1 Co1 81.19(10) . . ?
O1 Na1 Co1 82.24(11) . . ?
O18 Na1 Co1 124.50(13) . . ?
O3 Na1 Co1 126.23(13) . . ?
N4 Na1 Co1 37.48(10) . . ?
N10 Na1 Co1 37.57(10) . . ?
N5 Na1 Co1 54.87(10) . . ?
Co2 Na1 Co1 56.41(4) . . ?
Co3 Na1 Co1 56.60(4) . . ?
O13 Na2 O10 165.59(17) . . ?
O13 Na2 O15 67.31(14) . . ?
O10 Na2 O15 123.88(16) . . ?
O13 Na2 O12 120.10(16) . . ?
O10 Na2 O12 67.29(14) . . ?
O15 Na2 O12 108.71(17) . . ?
O13 Na2 N7 94.66(16) . . ?
O10 Na2 N7 74.90(15) . . ?
O15 Na2 N7 101.36(16) . . ?
O12 Na2 N7 140.52(16) . . ?
O13 Na2 N16 73.69(15) . . ?
O10 Na2 N16 94.07(15) . . ?
O15 Na2 N16 140.79(16) . . ?
O12 Na2 N16 93.90(15) . . ?
N7 Na2 N16 77.47(14) . . ?
O13 Na2 Co4 133.53(13) . . ?
O10 Na2 Co4 35.49(10) . . ?
O15 Na2 Co4 118.09(12) . . ?
O12 Na2 Co4 102.31(12) . . ?
N7 Na2 Co4 39.43(10) . . ?
N16 Na2 Co4 86.14(11) . . ?
O13 Na2 Co3 34.68(10) . . ?
O10 Na2 Co3 132.70(13) . . ?
O15 Na2 Co3 101.94(11) . . ?
O12 Na2 Co3 111.27(12) . . ?
N7 Na2 Co3 86.09(11) . . ?
N16 Na2 Co3 39.01(10) . . ?
Co4 Na2 Co3 114.63(6) . . ?
O13 Na2 Co1 82.70(11) . . ?
O10 Na2 Co1 82.97(11) . . ?
O15 Na2 Co1 128.50(13) . . ?
O12 Na2 Co1 122.60(12) . . ?
N7 Na2 Co1 38.65(10) . . ?
N16 Na2 Co1 38.82(10) . . ?
Co4 Na2 Co1 57.36(4) . . ?
Co3 Na2 Co1 57.28(4) . . ?
O7 Na3 O4 164.88(17) . . ?
O7 Na3 O9 68.17(16) . . ?
O4 Na3 O9 122.42(18) . . ?
O7 Na3 O6 123.51(18) . . ?
O4 Na3 O6 66.62(17) . . ?
O9 Na3 O6 105.22(19) . . ?
O7 Na3 N13 74.65(14) . . ?
O4 Na3 N13 93.29(15) . . ?
O9 Na3 N13 142.50(18) . . ?
O6 Na3 N13 99.01(18) . . ?
O7 Na3 N1 92.58(16) . . ?
O4 Na3 N1 75.06(16) . . ?
O9 Na3 N1 102.43(18) . . ?
O6 Na3 N1 140.66(17) . . ?
N13 Na3 N1 74.02(15) . . ?
O7 Na3 N2 81.94(16) . . ?
O4 Na3 N2 89.11(17) . . ?
O9 Na3 N2 80.33(17) . . ?
O6 Na3 N2 154.40(18) . . ?
N13 Na3 N2 90.02(16) . . ?
N1 Na3 N2 22.25(14) . . ?
O7 Na3 N14 88.73(15) . . ?
O4 Na3 N14 82.72(16) . . ?
O9 Na3 N14 153.92(18) . . ?
O6 Na3 N14 76.90(17) . . ?
N13 Na3 N14 22.21(13) . . ?
N1 Na3 N14 90.11(15) . . ?
N2 Na3 N14 109.26(16) . . ?
O7 Na3 C19 20.29(15) . . ?
O4 Na3 C19 164.40(19) . . ?
O9 Na3 C19 48.09(17) . . ?
O6 Na3 C19 125.18(17) . . ?
N13 Na3 C19 94.49(16) . . ?
N1 Na3 C19 94.14(16) . . ?
N2 Na3 C19 77.40(16) . . ?
N14 Na3 C19 108.94(16) . . ?
O7 Na3 Co2 131.48(13) . . ?
O4 Na3 Co2 35.91(11) . . ?
O9 Na3 Co2 117.33(14) . . ?
O6 Na3 Co2 102.32(13) . . ?
N13 Na3 Co2 83.99(11) . . ?
N1 Na3 Co2 39.21(10) . . ?
N2 Na3 Co2 54.61(11) . . ?
N14 Na3 Co2 86.80(11) . . ?
C19 Na3 Co2 131.93(13) . . ?
O7 Na3 Co4 35.15(10) . . ?
O4 Na3 Co4 132.40(13) . . ?
O9 Na3 Co4 103.28(14) . . ?
O6 Na3 Co4 116.15(15) . . ?
N13 Na3 Co4 39.53(10) . . ?
N1 Na3 Co4 83.38(12) . . ?
N2 Na3 Co4 85.86(12) . . ?
N14 Na3 Co4 55.04(10) . . ?
C19 Na3 Co4 55.22(12) . . ?
Co2 Na3 Co4 112.86(7) . . ?
O7 Na3 Co1 82.45(11) . . ?
O4 Na3 Co1 82.43(11) . . ?
O9 Na3 Co1 129.61(15) . . ?
O6 Na3 Co1 125.17(14) . . ?
N13 Na3 Co1 36.82(10) . . ?
N1 Na3 Co1 37.20(10) . . ?
N2 Na3 Co1 54.92(11) . . ?
N14 Na3 Co1 54.34(10) . . ?
C19 Na3 Co1 95.83(12) . . ?
Co2 Na3 Co1 56.40(4) . . ?
Co4 Na3 Co1 56.48(4) . . ?
N13 Co1 N1 90.77(17) . . ?
N13 Co1 N4 173.85(16) . . ?
N1 Co1 N4 93.52(16) . . ?
N13 Co1 N10 94.28(16) . . ?
N1 Co1 N10 80.51(17) . . ?
N4 Co1 N10 90.76(16) . . ?
N13 Co1 N7 81.04(16) . . ?
N1 Co1 N7 92.74(16) . . ?
N4 Co1 N7 94.36(16) . . ?
N10 Co1 N7 171.78(16) . . ?
N13 Co1 N16 94.95(16) . . ?
N1 Co1 N16 172.81(16) . . ?
N4 Co1 N16 81.12(15) . . ?
N10 Co1 N16 94.71(16) . . ?
N7 Co1 N16 92.44(16) . . ?
N13 Co1 Na2 87.02(12) . . ?
N1 Co1 Na2 138.36(12) . . ?
N4 Co1 Na2 86.85(12) . . ?
N10 Co1 Na2 141.13(12) . . ?
N7 Co1 Na2 45.85(11) . . ?
N16 Co1 Na2 46.59(11) . . ?
N13 Co1 Na1 139.73(12) . . ?
N1 Co1 Na1 85.99(12) . . ?
N4 Co1 Na1 45.18(11) . . ?
N10 Co1 Na1 45.58(13) . . ?
N7 Co1 Na1 139.17(12) . . ?
N16 Co1 Na1 86.84(11) . . ?
Na2 Co1 Na1 120.73(5) . . ?
N13 Co1 Na3 45.23(12) . . ?
N1 Co1 Na3 45.54(13) . . ?
N4 Co1 Na3 138.94(11) . . ?
N10 Co1 Na3 85.78(12) . . ?
N7 Co1 Na3 86.13(11) . . ?
N16 Co1 Na3 139.93(12) . . ?
Na2 Co1 Na3 120.00(5) . . ?
Na1 Co1 Na3 119.25(5) . . ?
O1 Co2 O4 174.46(16) . . ?
O1 Co2 O2 86.98(18) . . ?
O4 Co2 O2 89.86(18) . . ?
O1 Co2 O5 90.16(19) . . ?
O4 Co2 O5 85.72(18) . . ?
O2 Co2 O5 97.22(19) . . ?
O1 Co2 N1 95.31(17) . . ?
O4 Co2 N1 89.27(16) . . ?
O2 Co2 N1 90.65(18) . . ?
O5 Co2 N1 170.65(19) . . ?
O1 Co2 N10 88.66(16) . . ?
O4 Co2 N10 95.12(17) . . ?
O2 Co2 N10 170.50(19) . . ?
O5 Co2 N10 91.23(17) . . ?
N1 Co2 N10 81.35(17) . . ?
O1 Co2 Na3 143.69(12) . . ?
O4 Co2 Na3 40.60(11) . . ?
O2 Co2 Na3 88.41(14) . . ?
O5 Co2 Na3 126.15(15) . . ?
N1 Co2 Na3 48.73(13) . . ?
N10 Co2 Na3 90.11(12) . . ?
O1 Co2 Na1 40.46(11) . . ?
O4 Co2 Na1 143.00(12) . . ?
O2 Co2 Na1 127.13(15) . . ?
O5 Co2 Na1 89.68(13) . . ?
N1 Co2 Na1 89.58(13) . . ?
N10 Co2 Na1 48.23(13) . . ?
Na3 Co2 Na1 127.95(6) . . ?
O13 Co3 O16 178.54(16) . . ?
O13 Co3 O14 87.19(15) . . ?
O16 Co3 O14 91.46(16) . . ?
O13 Co3 O17 93.07(17) . . ?
O16 Co3 O17 86.42(16) . . ?
O14 Co3 O17 92.11(18) . . ?
O13 Co3 N16 87.04(15) . . ?
O16 Co3 N16 94.37(16) . . ?
O14 Co3 N16 171.30(16) . . ?
O17 Co3 N16 94.69(17) . . ?
O13 Co3 N4 93.80(16) . . ?
O16 Co3 N4 86.81(15) . . ?
O14 Co3 N4 92.73(17) . . ?
O17 Co3 N4 171.77(17) . . ?
N16 Co3 N4 81.17(15) . . ?
O13 Co3 Na2 39.50(11) . . ?
O16 Co3 Na2 141.90(12) . . ?
O14 Co3 Na2 126.47(12) . . ?
O17 Co3 Na2 94.72(12) . . ?
N16 Co3 Na2 47.54(11) . . ?
N4 Co3 Na2 87.74(11) . . ?
O13 Co3 Na1 140.95(12) . . ?
O16 Co3 Na1 39.55(10) . . ?
O14 Co3 Na1 90.51(13) . . ?
O17 Co3 Na1 125.97(13) . . ?
N16 Co3 Na1 89.88(11) . . ?
N4 Co3 Na1 47.36(11) . . ?
Na2 Co3 Na1 125.34(5) . . ?
O10 Co4 O7 176.30(15) . . ?
O10 Co4 O11 86.85(16) . . ?
O7 Co4 O11 89.88(17) . . ?
O10 Co4 O8 92.47(17) . . ?
O7 Co4 O8 86.05(16) . . ?
O11 Co4 O8 94.38(18) . . ?
O10 Co4 N7 87.89(15) . . ?
O7 Co4 N7 95.62(16) . . ?
O11 Co4 N7 169.55(17) . . ?
O8 Co4 N7 94.86(17) . . ?
O10 Co4 N13 94.41(16) . . ?
O7 Co4 N13 87.35(15) . . ?
O11 Co4 N13 90.71(17) . . ?
O8 Co4 N13 171.65(18) . . ?
N7 Co4 N13 80.70(15) . . ?
O10 Co4 Na2 40.61(11) . . ?
O7 Co4 Na2 142.84(12) . . ?
O11 Co4 Na2 127.09(13) . . ?
O8 Co4 Na2 93.76(13) . . ?
N7 Co4 Na2 47.31(12) . . ?
N13 Co4 Na2 88.41(12) . . ?
O10 Co4 Na3 142.13(12) . . ?
O7 Co4 Na3 39.38(11) . . ?
O11 Co4 Na3 88.92(13) . . ?
O8 Co4 Na3 125.38(14) . . ?
N7 Co4 Na3 89.71(12) . . ?
N13 Co4 Na3 48.01(12) . . ?
Na2 Co4 Na3 126.16(5) . . ?
C1 O1 Co2 130.6(4) . . ?
C1 O1 Na1 122.5(4) . . ?
Co2 O1 Na1 104.28(17) . . ?
C9 O2 Co2 124.9(5) . . ?
C6 O3 C7 116.8(6) . . ?
C6 O3 Na1 115.5(4) . . ?
C7 O3 Na1 125.4(4) . . ?
C10 O4 Co2 130.7(4) . . ?
C10 O4 Na3 122.5(4) . . ?
Co2 O4 Na3 103.50(18) . . ?
C18 O5 Co2 125.7(5) . . ?
C15 O6 C16 116.4(7) . . ?
C15 O6 Na3 115.7(4) . . ?
C16 O6 Na3 126.0(5) . . ?
C19 O7 Co4 131.2(4) . . ?
C19 O7 Na3 122.3(4) . . ?
Co4 O7 Na3 105.47(16) . . ?
C27 O8 Co4 126.0(5) . . ?
C24 O9 C25 119.3(6) . . ?
C24 O9 Na3 116.0(4) . . ?
C25 O9 Na3 124.6(5) . . ?
C28 O10 Co4 129.0(4) . . ?
C28 O10 Na2 121.5(3) . . ?
Co4 O10 Na2 103.90(17) . . ?
C36 O11 Co4 126.5(4) . . ?
C33 O12 C34 117.2(5) . . ?
C33 O12 Na2 115.5(3) . . ?
C34 O12 Na2 124.0(4) . . ?
C37 O13 Co3 130.0(4) . . ?
C37 O13 Na2 124.0(3) . . ?
Co3 O13 Na2 105.82(17) . . ?
C45 O14 Co3 126.7(4) . . ?
C42 O15 C43 115.8(5) . . ?
C42 O15 Na2 117.0(3) . . ?
C43 O15 Na2 126.7(4) . . ?
C46 O16 Co3 130.5(4) . . ?
C46 O16 Na1 123.1(4) . . ?
Co3 O16 Na1 105.75(15) . . ?
C54 O17 Co3 126.7(4) . . ?
C51 O18 C52 118.0(5) . . ?
C51 O18 Na1 117.0(3) . . ?
C52 O18 Na1 125.0(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
N19 H19A N6 0.91 2.02 2.929(12) 178.0 1_455

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 982505'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ni2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H72 Ni7 O24, 2(Cl O4) '
_chemical_formula_sum            'C60 H72 Cl2 Ni7 O32'
_chemical_formula_weight         1786.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_space_group_name_Hall  '-P 3'

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'

_cell_length_a                   14.6487(7)
_cell_length_b                   14.6487(7)
_cell_length_c                   9.6629(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1795.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1423
_cell_measurement_theta_min      3.833
_cell_measurement_theta_max      26.478

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             918
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3860
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         25.08
_reflns_number_total             2128
_reflns_number_gt                1602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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  'Bruker SHELXTL'

_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)+(0.1080P)²+3.0726P] 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         2124
_refine_ls_number_parameters     153
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1865
_refine_ls_wR_factor_gt          0.1596
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.017
_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 0.08596(5) 0.24133(5) 1.01184(7) 0.0455(3) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.2535(4) 0.0749(8) Uani 1 3 d S . .
O1 O 0.2154(3) 0.2663(3) 0.9109(4) 0.0510(9) Uani 1 1 d . . .
C1 C 0.2494(4) 0.3216(4) 0.7958(6) 0.0490(13) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.0000 1.0000 0.0498(5) Uani 1 6 d S . .
C2 C 0.2026(5) 0.3803(5) 0.7534(6) 0.0603(15) Uani 1 1 d . . .
O2 O 0.3621(4) 0.2044(4) 0.8515(5) 0.0805(14) Uani 1 1 d . . .
O3 O 0.1195(4) 0.3663(3) 0.8384(5) 0.0677(12) Uani 1 1 d . . .
C3 C 0.2386(7) 0.4441(6) 0.6366(8) 0.085(2) Uani 1 1 d . . .
H3A H 0.2081 0.4840 0.6106 0.103 Uiso 1 1 calc R . .
O4 O -0.0190(3) 0.1128(3) 0.8942(5) 0.0488(10) Uani 1 1 d U . .
C4 C 0.3203(8) 0.4481(8) 0.5589(8) 0.100(3) Uani 1 1 d . . .
H4A H 0.3435 0.4897 0.4797 0.120 Uiso 1 1 calc R . .
C5 C 0.3660(6) 0.3920(7) 0.5979(7) 0.082(2) Uani 1 1 d . . .
H5A H 0.4215 0.3965 0.5457 0.098 Uiso 1 1 calc R . .
O5 O 0.3333 0.6667 0.3996(12) 0.150(5) Uani 1 3 d S . .
O6 O 0.3528(4) 0.5856(4) 0.2138(8) 0.112(2) Uani 1 1 d . . .
C6 C 0.3315(5) 0.3262(5) 0.7167(6) 0.0603(15) Uani 1 1 d . . .
C7 C 0.3859(5) 0.2710(5) 0.7510(7) 0.0637(16) Uani 1 1 d . . .
H7A H 0.4434 0.2840 0.6963 0.076 Uiso 1 1 calc R . .
C8 C 0.0730(8) 0.4324(7) 0.8254(10) 0.104(3) Uani 1 1 d . . .
H8A H 0.0630 0.4406 0.7279 0.124 Uiso 1 1 calc R . .
H8B H 0.0041 0.3971 0.8687 0.124 Uiso 1 1 calc R . .
C9 C 0.1326(16) 0.5321(11) 0.8843(14) 0.208(9) Uani 1 1 d . . .
H9A H 0.0971 0.5716 0.8711 0.312 Uiso 1 1 calc R . .
H9B H 0.2006 0.5684 0.8409 0.312 Uiso 1 1 calc R . .
H9C H 0.1410 0.5250 0.9816 0.312 Uiso 1 1 calc R . .
C10 C -0.0165(7) 0.1217(7) 0.7388(11) 0.108(3) Uani 1 1 d U . .
H10A H -0.0271 0.1790 0.7124 0.162 Uiso 1 1 calc R . .
H10B H -0.0714 0.0572 0.6998 0.162 Uiso 1 1 calc R . .
H10C H 0.0506 0.1348 0.7051 0.162 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 O1 1.990(4) 6_557 ?
Ni1 O1 1.997(4) . ?
Ni1 O2 2.029(5) 6_557 ?
Ni1 O4 2.045(4) 5_557 ?
Ni1 O4 2.076(4) . ?
Ni1 O3 2.345(4) . ?
Cl1 O6 1.406(5) 3_565 ?
Cl1 O6 1.406(6) 2_665 ?
Cl1 O6 1.406(5) . ?
Cl1 O5 1.412(12) . ?
O1 C1 1.318(6) . ?
O1 Ni1 1.990(4) 5_557 ?
C1 C6 1.398(8) . ?
C1 C2 1.404(8) . ?
Ni2 O4 2.077(4) 5_557 ?
Ni2 O4 2.077(4) 2 ?
Ni2 O4 2.077(4) 6_557 ?
Ni2 O4 2.077(4) . ?
Ni2 O4 2.077(4) 4_557 ?
Ni2 O4 2.077(4) 3 ?
C2 C3 1.390(9) . ?
C2 O3 1.395(7) . ?
O2 C7 1.295(8) . ?
O2 Ni1 2.029(5) 5_557 ?
O3 C8 1.441(8) . ?
C3 C4 1.390(11) . ?
C3 H3A 0.9300 . ?
O4 C10 1.506(11) . ?
O4 Ni1 2.045(4) 6_557 ?
C4 C5 1.348(11) . ?
C4 H4A 0.9300 . ?
C5 C6 1.419(9) . ?
C5 H5A 0.9300 . ?
C6 C7 1.429(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.395(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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
O1 Ni1 O1 172.78(9) 6_557 . ?
O1 Ni1 O2 87.44(18) 6_557 6_557 ?
O1 Ni1 O2 97.35(18) . 6_557 ?
O1 Ni1 O4 104.70(16) 6_557 5_557 ?
O1 Ni1 O4 79.85(15) . 5_557 ?
O2 Ni1 O4 100.13(19) 6_557 5_557 ?
O1 Ni1 O4 79.26(15) 6_557 . ?
O1 Ni1 O4 95.94(16) . . ?
O2 Ni1 O4 166.69(18) 6_557 . ?
O4 Ni1 O4 83.0(2) 5_557 . ?
O1 Ni1 O3 102.43(15) 6_557 . ?
O1 Ni1 O3 72.44(15) . . ?
O2 Ni1 O3 88.27(18) 6_557 . ?
O4 Ni1 O3 151.87(15) 5_557 . ?
O4 Ni1 O3 95.03(16) . . ?
O6 Cl1 O6 112.9(3) 3_565 2_665 ?
O6 Cl1 O6 112.9(3) 3_565 . ?
O6 Cl1 O6 112.9(3) 2_665 . ?
O6 Cl1 O5 105.8(4) 3_565 . ?
O6 Cl1 O5 105.8(4) 2_665 . ?
O6 Cl1 O5 105.8(4) . . ?
C1 O1 Ni1 130.6(3) . 5_557 ?
C1 O1 Ni1 123.9(3) . . ?
Ni1 O1 Ni1 102.61(16) 5_557 . ?
O1 C1 C6 122.9(5) . . ?
O1 C1 C2 118.2(5) . . ?
C6 C1 C2 118.9(5) . . ?
O4 Ni2 O4 180.00(17) 5_557 2 ?
O4 Ni2 O4 97.83(15) 5_557 6_557 ?
O4 Ni2 O4 82.17(15) 2 6_557 ?
O4 Ni2 O4 82.17(15) 5_557 . ?
O4 Ni2 O4 97.83(15) 2 . ?
O4 Ni2 O4 82.17(15) 6_557 . ?
O4 Ni2 O4 97.83(15) 5_557 4_557 ?
O4 Ni2 O4 82.17(15) 2 4_557 ?
O4 Ni2 O4 97.83(15) 6_557 4_557 ?
O4 Ni2 O4 180.000(1) . 4_557 ?
O4 Ni2 O4 82.17(15) 5_557 3 ?
O4 Ni2 O4 97.83(15) 2 3 ?
O4 Ni2 O4 180.00(10) 6_557 3 ?
O4 Ni2 O4 97.83(15) . 3 ?
O4 Ni2 O4 82.17(15) 4_557 3 ?
C3 C2 O3 125.9(6) . . ?
C3 C2 C1 120.8(6) . . ?
O3 C2 C1 113.3(5) . . ?
C7 O2 Ni1 127.9(4) . 5_557 ?
C2 O3 C8 121.3(6) . . ?
C2 O3 Ni1 111.3(3) . . ?
C8 O3 Ni1 127.0(5) . . ?
C2 C3 C4 119.7(7) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C10 O4 Ni1 116.0(4) . 6_557 ?
C10 O4 Ni1 119.5(4) . . ?
Ni1 O4 Ni1 98.07(16) 6_557 . ?
C10 O4 Ni2 123.6(4) . . ?
Ni1 O4 Ni2 97.77(16) 6_557 . ?
Ni1 O4 Ni2 96.81(17) . . ?
C5 C4 C3 120.2(7) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C4 C5 C6 121.6(7) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C1 C6 C5 118.7(6) . . ?
C1 C6 C7 123.7(6) . . ?
C5 C6 C7 117.5(6) . . ?
O2 C7 C6 125.7(6) . . ?
O2 C7 H7A 117.1 . . ?
C6 C7 H7A 117.1 . . ?
C9 C8 O3 114.2(9) . . ?
C9 C8 H8A 108.7 . . ?
O3 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
O3 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.100
_database_code_depnum_ccdc_archive 'CCDC 982508'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_co5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H72 Co7 O24, 2(Cl O4)'
_chemical_formula_sum            'C60 H72 Cl2 Co7 O32'
_chemical_formula_weight         1788.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_space_group_name_Hall  '-P 3'

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'

_cell_length_a                   14.8180(11)
_cell_length_b                   14.8180(11)
_cell_length_c                   9.3912(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1785.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1397
_cell_measurement_theta_min      3.496
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             911
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3653
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.05
_reflns_number_total             2108
_reflns_number_gt                1602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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  'Bruker SHELXTL'

_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)+(0.0679P)²+5.3753P] 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         2108
_refine_ls_number_parameters     153
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1657
_refine_ls_wR_factor_gt          0.1464
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.030
_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
C1 C 0.0700(4) 0.3239(4) 0.2915(6) 0.0416(13) Uani 1 1 d . . .
C2 C 0.1753(5) 0.3851(5) 0.2505(6) 0.0504(14) Uani 1 1 d . . .
C3 C 0.2022(6) 0.4486(6) 0.1321(7) 0.070(2) Uani 1 1 d . . .
H3A H 0.2717 0.4881 0.1053 0.085 Uiso 1 1 calc R . .
C4 C 0.1266(7) 0.4538(7) 0.0536(8) 0.081(2) Uani 1 1 d . . .
H4A H 0.1455 0.4971 -0.0257 0.097 Uiso 1 1 calc R . .
C5 C 0.0246(6) 0.3965(6) 0.0908(7) 0.069(2) Uani 1 1 d . . .
H5A H -0.0254 0.4011 0.0367 0.083 Uiso 1 1 calc R . .
C6 C -0.0064(5) 0.3300(5) 0.2100(6) 0.0476(14) Uani 1 1 d . . .
C7 C -0.1156(5) 0.2741(5) 0.2436(6) 0.0520(15) Uani 1 1 d . . .
H7A H -0.1591 0.2878 0.1875 0.062 Uiso 1 1 calc R . .
C8 C 0.3546(6) 0.4325(7) 0.3239(10) 0.095(3) Uani 1 1 d DU . .
H8A H 0.3743 0.4398 0.2243 0.142 Uiso 1 1 calc R . .
H8B H 0.3870 0.3983 0.3728 0.142 Uiso 1 1 calc R . .
C9 C 0.3903(10) 0.5365(9) 0.3872(13) 0.162(5) Uani 1 1 d DU . .
H9B H 0.4643 0.5791 0.3753 0.243 Uiso 1 1 calc R . .
H9C H 0.3736 0.5290 0.4868 0.243 Uiso 1 1 calc R . .
H9D H 0.3561 0.5689 0.3405 0.243 Uiso 1 1 calc R . .
C10 C 0.1418(6) 0.1305(7) 0.2311(9) 0.084(2) Uani 1 1 d . . .
H10A H 0.2092 0.1881 0.2080 0.126 Uiso 1 1 calc R . .
H10B H 0.0888 0.1442 0.1971 0.126 Uiso 1 1 calc R . .
H10C H 0.1335 0.0684 0.1869 0.126 Uiso 1 1 calc R . .
Cl1 Cl 0.6667 0.3333 0.2506(4) 0.0647(8) Uani 1 3 d S . .
Co1 Co 0.15315(5) 0.24290(5) 0.51373(8) 0.0396(3) Uani 1 1 d . . .
Co2 Co 0.0000 0.0000 0.5000 0.0472(5) Uani 1 6 d S . .
O1 O 0.0482(3) 0.2659(3) 0.4065(4) 0.0445(9) Uani 1 1 d . . .
O2 O -0.1591(4) 0.2062(4) 0.3447(5) 0.0714(13) Uani 1 1 d . . .
O3 O 0.2420(3) 0.3707(3) 0.3373(5) 0.0586(12) Uani 1 1 d U . .
O4 O 0.1324(3) 0.1160(3) 0.3881(5) 0.0441(10) Uani 1 1 d . . .
O5 O 0.5868(4) 0.3516(4) 0.2950(7) 0.0935(19) Uani 1 1 d . . .
O6 O 0.6667 0.3333 0.0965(12) 0.129(5) Uani 1 3 d S . .


_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
C1 O1 1.315(6) . ?
C1 C6 1.407(8) . ?
C1 C2 1.411(8) . ?
C2 O3 1.378(7) . ?
C2 C3 1.381(9) . ?
C3 C4 1.374(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.358(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.408(8) . ?
C5 H5A 0.9300 . ?
C6 C7 1.436(8) . ?
C7 O2 1.297(7) . ?
C7 H7A 0.9300 . ?
C8 O3 1.452(8) . ?
C8 C9 1.481(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 H9D 0.9600 . ?
C10 O4 1.486(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Cl1 O5 1.402(5) 2_655 ?
Cl1 O5 1.402(5) 3_665 ?
Cl1 O5 1.402(5) . ?
Cl1 O6 1.447(11) . ?
Co1 O1 2.021(4) . ?
Co1 O1 2.029(4) 5_556 ?
Co1 O2 2.062(5) 5_556 ?
Co1 O4 2.078(4) 6_556 ?
Co1 O4 2.108(4) . ?
Co1 O3 2.360(4) . ?
Co2 O4 2.129(4) 5_556 ?
Co2 O4 2.129(4) 3 ?
Co2 O4 2.129(4) 6_556 ?
Co2 O4 2.129(4) . ?
Co2 O4 2.129(4) 4_556 ?
Co2 O4 2.129(4) 2 ?
O1 Co1 2.029(4) 6_556 ?
O2 Co1 2.062(5) 6_556 ?
O4 Co1 2.078(4) 5_556 ?

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 C1 C6 123.0(5) . . ?
O1 C1 C2 118.4(5) . . ?
C6 C1 C2 118.5(5) . . ?
O3 C2 C3 126.7(6) . . ?
O3 C2 C1 112.8(5) . . ?
C3 C2 C1 120.5(6) . . ?
C4 C3 C2 120.3(7) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C5 C4 C3 120.6(7) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 121.0(7) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
C1 C6 C5 119.1(6) . . ?
C1 C6 C7 123.6(5) . . ?
C5 C6 C7 117.3(6) . . ?
O2 C7 C6 126.1(5) . . ?
O2 C7 H7A 117.0 . . ?
C6 C7 H7A 117.0 . . ?
O3 C8 C9 108.8(8) . . ?
O3 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C9 H9D 109.5 . . ?
H9B C9 H9D 109.5 . . ?
H9C C9 H9D 109.5 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 Cl1 O5 111.6(3) 2_655 3_665 ?
O5 Cl1 O5 111.6(3) 2_655 . ?
O5 Cl1 O5 111.6(3) 3_665 . ?
O5 Cl1 O6 107.3(3) 2_655 . ?
O5 Cl1 O6 107.3(3) 3_665 . ?
O5 Cl1 O6 107.3(3) . . ?
O1 Co1 O1 171.78(9) . 5_556 ?
O1 Co1 O2 99.20(18) . 5_556 ?
O1 Co1 O2 86.37(17) 5_556 5_556 ?
O1 Co1 O4 79.90(15) . 6_556 ?
O1 Co1 O4 105.04(16) 5_556 6_556 ?
O2 Co1 O4 101.54(18) 5_556 6_556 ?
O1 Co1 O4 95.19(16) . . ?
O1 Co1 O4 79.00(14) 5_556 . ?
O2 Co1 O4 165.28(17) 5_556 . ?
O4 Co1 O4 84.0(2) 6_556 . ?
O1 Co1 O3 71.49(14) . . ?
O1 Co1 O3 103.06(15) 5_556 . ?
O2 Co1 O3 86.12(18) 5_556 . ?
O4 Co1 O3 151.24(15) 6_556 . ?
O4 Co1 O3 95.56(16) . . ?
O4 Co2 O4 82.26(14) 5_556 3 ?
O4 Co2 O4 97.74(14) 5_556 6_556 ?
O4 Co2 O4 180.00(17) 3 6_556 ?
O4 Co2 O4 82.26(14) 5_556 . ?
O4 Co2 O4 97.74(14) 3 . ?
O4 Co2 O4 82.26(14) 6_556 . ?
O4 Co2 O4 97.74(14) 5_556 4_556 ?
O4 Co2 O4 82.26(14) 3 4_556 ?
O4 Co2 O4 97.74(14) 6_556 4_556 ?
O4 Co2 O4 180.00(18) . 4_556 ?
O4 Co2 O4 180.00(11) 5_556 2 ?
O4 Co2 O4 97.74(14) 3 2 ?
O4 Co2 O4 82.26(14) 6_556 2 ?
O4 Co2 O4 97.74(14) . 2 ?
O4 Co2 O4 82.26(14) 4_556 2 ?
C1 O1 Co1 124.1(3) . . ?
C1 O1 Co1 131.2(3) . 6_556 ?
Co1 O1 Co1 102.72(16) . 6_556 ?
C7 O2 Co1 128.2(4) . 6_556 ?
C2 O3 C8 122.5(6) . . ?
C2 O3 Co1 112.6(3) . . ?
C8 O3 Co1 124.8(5) . . ?
C10 O4 Co1 116.2(4) . 5_556 ?
C10 O4 Co1 117.7(4) . . ?
Co1 O4 Co1 98.13(16) 5_556 . ?
C10 O4 Co2 126.0(4) . . ?
Co1 O4 Co2 97.14(16) 5_556 . ?
Co1 O4 Co2 96.23(16) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 982509'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_co

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 Co4 O20, 2(H2 O) '
_chemical_formula_sum            'C44 H68 Co4 O22'
_chemical_formula_weight         1184.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/n c c'
_symmetry_space_group_name_Hall  ' -P 4a 2ac '

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

_cell_length_a                   17.0166(4)
_cell_length_b                   17.0166(4)
_cell_length_c                   18.7995(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5443.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3915
_cell_measurement_theta_min      3.935
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12303
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2432
_reflns_number_gt                1872
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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  'Bruker SHELXTL'

_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)+(0.1260P)²+10.4802P] 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         2432
_refine_ls_number_parameters     159
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.2013
_refine_ls_wR_factor_gt          0.1788
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      1.009
_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
Co1 Co 0.71772(4) 1.16191(4) 0.55610(3) 0.0406(3) Uani 1 1 d U . .
O4 O 0.6747(2) 1.27509(18) 0.55375(16) 0.0398(8) Uani 1 1 d . . .
O2 O 0.7053(2) 1.1503(2) 0.6651(2) 0.0584(10) Uani 1 1 d . . .
O1 O 0.7740(2) 1.0564(2) 0.55574(16) 0.0475(8) Uani 1 1 d . . .
O3 O 0.8470(2) 0.9256(2) 0.5239(2) 0.0666(11) Uani 1 1 d . . .
O5 O 0.6003(2) 1.1160(3) 0.5449(2) 0.0628(10) Uani 1 1 d U . .
H5B H 0.5728 1.1388 0.5075 0.094 Uiso 1 1 calc R . .
C1 C 0.7854(3) 1.0083(3) 0.6072(3) 0.0451(11) Uani 1 1 d . . .
C6 C 0.7603(3) 1.0211(3) 0.6788(3) 0.0533(13) Uani 1 1 d . . .
C8 C 0.8791(5) 0.8515(4) 0.5039(4) 0.094(2) Uani 1 1 d . . .
H8A H 0.8442 0.8094 0.5186 0.112 Uiso 1 1 calc R . .
H8B H 0.9296 0.8437 0.5266 0.112 Uiso 1 1 calc R . .
C7 C 0.7221(3) 1.0919(3) 0.7013(3) 0.0573(14) Uani 1 1 d . . .
H7A H 0.7081 1.0943 0.7490 0.069 Uiso 1 1 calc R . .
C2 C 0.8255(3) 0.9353(3) 0.5933(3) 0.0510(12) Uani 1 1 d . . .
C5 C 0.7740(4) 0.9633(4) 0.7316(3) 0.0663(16) Uani 1 1 d . . .
H5A H 0.7564 0.9719 0.7778 0.080 Uiso 1 1 calc R . .
C10 C 0.6131(3) 1.2982(3) 0.6001(3) 0.0568(14) Uani 1 1 d . . .
H10A H 0.6004 1.3524 0.5918 0.085 Uiso 1 1 calc R . .
H10B H 0.6296 1.2914 0.6485 0.085 Uiso 1 1 calc R . .
H10C H 0.5676 1.2663 0.5912 0.085 Uiso 1 1 calc R . .
C3 C 0.8383(4) 0.8821(3) 0.6461(3) 0.0627(15) Uani 1 1 d . . .
H3A H 0.8651 0.8358 0.6357 0.075 Uiso 1 1 calc R . .
C4 C 0.8122(4) 0.8954(4) 0.7158(3) 0.0706(17) Uani 1 1 d . . .
H4A H 0.8210 0.8580 0.7509 0.085 Uiso 1 1 calc R . .
C9 C 0.8884(7) 0.8510(6) 0.4245(5) 0.126(4) Uani 1 1 d . . .
H9A H 0.9096 0.8014 0.4097 0.190 Uiso 1 1 calc R . .
H9B H 0.9235 0.8925 0.4106 0.190 Uiso 1 1 calc R . .
H9C H 0.8381 0.8589 0.4025 0.190 Uiso 1 1 calc R . .
O6 O 0.4904(16) 0.9904(16) 0.7500 0.466(19) Uani 1 2 d S . .
H6 H 0.5000 1.0180 0.7147 0.699 Uiso 0.50 1 d PR . .
H6A H 0.4563 0.9563 0.7500 0.699 Uiso 1 2 d SR . .
C11 C 0.5583(7) 1.0622(8) 0.5798(9) 0.172(5) Uani 1 1 d U . .
H11A H 0.5076 1.0570 0.5579 0.258 Uiso 1 1 calc R . .
H11B H 0.5520 1.0782 0.6284 0.258 Uiso 1 1 calc R . .
H11C H 0.5851 1.0126 0.5781 0.258 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
Co1 O1 2.034(3) . ?
Co1 O4 2.061(3) . ?
Co1 O2 2.069(4) . ?
Co1 O4 2.080(3) 15_766 ?
Co1 O4 2.122(3) 4_675 ?
Co1 O5 2.156(4) . ?
O4 C10 1.418(6) . ?
O4 Co1 2.080(3) 10_576 ?
O4 Co1 2.122(3) 4_675 ?
O2 C7 1.237(6) . ?
O1 C1 1.283(6) . ?
O3 C2 1.365(7) . ?
O3 C8 1.424(7) . ?
O5 C11 1.334(11) . ?
O5 H5B 0.9300 . ?
C1 C6 1.429(7) . ?
C1 C2 1.440(7) . ?
C6 C5 1.417(7) . ?
C6 C7 1.433(8) . ?
C8 C9 1.501(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 H7A 0.9300 . ?
C2 C3 1.362(8) . ?
C5 C4 1.360(8) . ?
C5 H5A 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C3 C4 1.401(9) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
O6 H6 0.8293 . ?
O6 H6A 0.8209 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 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
O1 Co1 O4 172.62(14) . . ?
O1 Co1 O2 88.11(13) . . ?
O4 Co1 O2 94.25(13) . . ?
O1 Co1 O4 93.50(13) . 15_766 ?
O4 Co1 O4 84.38(13) . 15_766 ?
O2 Co1 O4 177.48(15) . 15_766 ?
O1 Co1 O4 92.27(13) . 4_675 ?
O4 Co1 O4 80.45(15) . 4_675 ?
O2 Co1 O4 99.01(15) . 4_675 ?
O4 Co1 O4 82.87(13) 15_766 4_675 ?
O1 Co1 O5 96.67(16) . . ?
O4 Co1 O5 90.41(15) . . ?
O2 Co1 O5 88.15(16) . . ?
O4 Co1 O5 89.74(14) 15_766 . ?
O4 Co1 O5 168.73(14) 4_675 . ?
C10 O4 Co1 120.6(3) . . ?
C10 O4 Co1 121.1(3) . 10_576 ?
Co1 O4 Co1 96.51(13) . 10_576 ?
C10 O4 Co1 119.0(3) . 4_675 ?
Co1 O4 Co1 99.49(14) . 4_675 ?
Co1 O4 Co1 94.65(13) 10_576 4_675 ?
C7 O2 Co1 126.7(4) . . ?
C1 O1 Co1 129.2(3) . . ?
C2 O3 C8 117.5(5) . . ?
C11 O5 Co1 134.2(6) . . ?
C11 O5 H5B 112.9 . . ?
Co1 O5 H5B 112.9 . . ?
O1 C1 C6 124.5(4) . . ?
O1 C1 C2 119.0(4) . . ?
C6 C1 C2 116.4(4) . . ?
C5 C6 C1 120.3(5) . . ?
C5 C6 C7 116.9(5) . . ?
C1 C6 C7 122.8(5) . . ?
O3 C8 C9 107.9(6) . . ?
O3 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
O3 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O2 C7 C6 128.2(5) . . ?
O2 C7 H7A 115.9 . . ?
C6 C7 H7A 115.9 . . ?
C3 C2 O3 125.0(5) . . ?
C3 C2 C1 121.1(5) . . ?
O3 C2 C1 113.9(4) . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 C3 C4 121.6(5) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H6 O6 H6A 122.6 . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
O5 H5B O1 0.93 1.92 2.764(5) 149.7 10_576
O5 H5B O3 0.93 2.58 3.302(6) 134.3 10_576

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 982510'
