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

data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Enrique Colacio'
'Hakima Aouryaghal'
'Joan Cano'
'Antonio J. Mota'
'A. Rodriguez-Dieguez'
'Reijo Sillanpaa'

_publ_contact_author_name        'Enrique Colacio'
_publ_contact_author_email       ECOLACIO@UGR.ES

_publ_section_title              
;
Anion Encapsulation Promoted by Anion****?
Interactions in Rationally Designed Hexanuclear Antiferromagnetic Wheels:
Synthesis, Structure and Magnetic Properties.
;
_publ_requested_category         ?

# Attachment 'Colacio.cif'

data_h176
_database_code_depnum_ccdc_archive 'CCDC 725440'

_audit_creation_date             2008-12-04T14:23:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C66 H114 N24 Ni6 O12, 6(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C66 H122 Cl6 N24 Ni6 O40'
_chemical_formula_weight         2456.84
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6363(7)
_cell_length_b                   13.8010(7)
_cell_length_c                   15.6910(8)
_cell_angle_alpha                70.683(3)
_cell_angle_beta                 82.958(3)
_cell_angle_gamma                89.263(3)
_cell_volume                     2561.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9052
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      28.283
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1276
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.904

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_number            23734
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_reflns_number_total             9640
_reflns_number_gt                6188
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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)+(0.0774P)²+3.7712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9640
_refine_ls_number_parameters     701
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1553
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.25
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.116

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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 0.23155(5) 0.32046(5) 0.87112(5) 0.01904(19) Uani 1 1 d . . .
Ni2 Ni 0.18183(6) 0.08010(5) 1.23481(5) 0.0217(2) Uani 1 1 d . . .
Ni3 Ni 0.53515(6) 0.22451(6) 0.62912(5) 0.0275(2) Uani 1 1 d . . .
O1 O 0.1226(3) 0.2287(3) 0.9752(2) 0.0203(8) Uani 1 1 d . . .
O2 O 0.1047(3) 0.1258(3) 1.1201(2) 0.0205(8) Uani 1 1 d . . .
O3 O 0.2843(3) 0.0296(3) 1.3326(2) 0.0280(9) Uani 1 1 d . . .
O4 O 0.4039(3) -0.0891(3) 1.3831(3) 0.0322(10) Uani 1 1 d . . .
O5 O 0.3569(3) 0.3841(3) 0.7700(2) 0.0240(9) Uani 1 1 d . . .
O6 O 0.4734(3) 0.3471(3) 0.6661(3) 0.0276(9) Uani 1 1 d . . .
Cl1 Cl 0.9832(2) 0.6166(3) 0.5052(2) 0.0366(8) Uani 0.5 1 d P . 1
Cl2 Cl 0.68127(13) 0.47737(12) -0.15119(14) 0.0465(5) Uani 1 1 d . A 1
Cl3 Cl 0.71612(12) 0.18907(12) 0.26601(11) 0.0346(4) Uani 1 1 d . B 1
Cl4 Cl 0.5 0 0 0.0326(5) Uani 1 2 d SD . 1
O1W O 0.9191(3) 0.0842(3) 0.0121(3) 0.0365(10) Uani 1 1 d D C 1
H1W H 0.896(4) 0.151(2) 0.006(4) 0.044 Uiso 1 1 d D D 1
H2W H 0.984(3) 0.081(4) 0.035(4) 0.044 Uiso 1 1 d D E 1
O2W O 0.8498(4) 0.2815(4) 0.0089(3) 0.0495(13) Uani 1 1 d D F 1
H3W H 0.800(4) 0.323(5) -0.023(4) 0.059 Uiso 1 1 d D G 1
H4W H 0.823(5) 0.251(5) 0.0695(18) 0.059 Uiso 1 1 d D H 1
O7 O 1.0252(7) 0.6326(7) 0.5793(6) 0.043(2) Uani 0.5 1 d P I 1
O8 O 0.9549(9) 0.5085(8) 0.5279(8) 0.071(3) Uani 0.5 1 d P . 1
O9 O 1.0618(7) 0.6448(7) 0.4265(6) 0.042(2) Uani 0.5 1 d P J 1
O10 O 0.8934(8) 0.6773(9) 0.4864(8) 0.072(4) Uani 0.5 1 d P K 1
O11 O 0.7856(5) 0.4811(4) -0.1927(5) 0.092(2) Uani 1 1 d . A 1
O12 O 0.6034(5) 0.4693(4) -0.2076(4) 0.0771(18) Uani 1 1 d . A 1
O13 O 0.6675(4) 0.3859(4) -0.0712(3) 0.0564(14) Uiso 1 1 d . A 1
O14 O 0.6620(4) 0.5670(4) -0.1247(4) 0.0624(15) Uani 1 1 d . A 1
O15 O 0.7167(5) 0.2728(4) 0.2993(4) 0.0655(16) Uani 1 1 d . B 1
O16 O 0.8094(4) 0.2010(4) 0.1996(3) 0.0528(13) Uani 1 1 d . B 1
O17 O 0.6244(4) 0.1896(4) 0.2221(4) 0.0699(17) Uani 1 1 d . B 1
O18 O 0.7221(4) 0.0935(4) 0.3364(3) 0.0527(13) Uani 1 1 d . B 1
O19A O 0.6006(7) -0.0402(7) -0.0111(7) 0.044(2) Uani 0.5 1 d P . 1
O19B O 0.4677(7) -0.0036(7) 0.0887(6) 0.042(2) Uani 0.5 1 d P . 1
O20A O 0.4841(7) 0.0925(6) -0.0667(6) 0.042(2) Uani 0.5 1 d P . 1
O20B O 0.4238(6) -0.0766(5) -0.0149(6) 0.033(2) Uani 0.5 1 d PD . 1
N1 N 0.3273(4) 0.2720(3) 0.9806(3) 0.0219(10) Uani 1 1 d . . .
N3 N 0.3038(4) 0.1736(3) 1.1376(3) 0.0217(10) Uani 1 1 d . . .
N4 N 0.1101(4) 0.3644(3) 0.7827(3) 0.0222(10) Uani 1 1 d . . .
N5 N 0.2034(4) 0.4633(3) 0.8927(3) 0.0281(11) Uani 1 1 d . . .
N6 N 0.2782(3) 0.1908(3) 0.8332(3) 0.0184(10) Uani 1 1 d . . .
N7 N 0.4115(3) 0.1492(3) 0.7308(3) 0.0214(10) Uani 1 1 d . . .
N8 N 0.6434(4) 0.3263(4) 0.5282(4) 0.0450(16) Uani 1 1 d . . .
N9 N 0.4419(4) 0.2363(5) 0.5215(3) 0.0434(15) Uani 1 1 d . . .
N10 N 0.2406(3) -0.0529(3) 1.2080(3) 0.0202(10) Uani 1 1 d . . .
N11 N 0.3585(4) -0.1871(3) 1.2703(3) 0.0234(11) Uani 1 1 d . . .
N12 N 0.1311(4) 0.1988(4) 1.2870(3) 0.0346(13) Uani 1 1 d . . .
N13 N 0.0402(4) -0.0029(4) 1.3171(3) 0.0293(12) Uani 1 1 d . . .
C2 C 0.2708(4) 0.2129(4) 1.0564(4) 0.0195(12) Uani 1 1 d . . .
C4 C 0.4057(4) 0.1964(4) 1.1435(4) 0.0279(14) Uani 1 1 d . . .
H4 H 0.4327 0.171 1.2005 0.034 Uiso 1 1 calc R . .
C5 C 0.4704(5) 0.2557(4) 1.0685(4) 0.0289(14) Uani 1 1 d . . .
H5 H 0.5425 0.2706 1.0724 0.035 Uiso 1 1 calc R . .
C6 C 0.4281(4) 0.2935(4) 0.9865(4) 0.0248(13) Uani 1 1 d . . .
H6 H 0.4718 0.3354 0.9337 0.03 Uiso 1 1 calc R . .
C7 C 0.1558(4) 0.1872(4) 1.0499(4) 0.0171(11) Uani 1 1 d . . .
C8 C 0.0566(5) 0.4497(5) 0.8069(5) 0.0412(17) Uani 1 1 d . . .
H8A H 0.0078 0.4219 0.8643 0.049 Uiso 1 1 calc R . .
H8B H 0.0142 0.4886 0.7583 0.049 Uiso 1 1 calc R . .
C9 C 0.1412(6) 0.5200(5) 0.8183(5) 0.0454(18) Uani 1 1 d . . .
H9A H 0.1897 0.5475 0.7607 0.054 Uiso 1 1 calc R . .
H9B H 0.1067 0.5786 0.8324 0.054 Uiso 1 1 calc R . .
C10 C 0.0287(5) 0.2832(5) 0.7970(4) 0.0359(15) Uani 1 1 d . . .
H10A H -0.0251 0.3097 0.7557 0.054 Uiso 1 1 calc R . .
H10B H -0.0055 0.2619 0.8601 0.054 Uiso 1 1 calc R . .
H10C H 0.0626 0.2242 0.7846 0.054 Uiso 1 1 calc R . .
C11 C 0.1528(5) 0.3994(6) 0.6858(4) 0.049(2) Uani 1 1 d . . .
H11A H 0.1863 0.3421 0.6701 0.074 Uiso 1 1 calc R . .
H11B H 0.2059 0.455 0.6736 0.074 Uiso 1 1 calc R . .
H11C H 0.0946 0.4246 0.649 0.074 Uiso 1 1 calc R . .
C12 C 0.1411(5) 0.4505(5) 0.9826(5) 0.0440(18) Uani 1 1 d . . .
H12A H 0.1827 0.4125 1.0311 0.066 Uiso 1 1 calc R . .
H12B H 0.0742 0.4124 0.9882 0.066 Uiso 1 1 calc R . .
H12C H 0.1252 0.5183 0.9876 0.066 Uiso 1 1 calc R . .
C13 C 0.3018(5) 0.5231(4) 0.8860(5) 0.0335(15) Uani 1 1 d . . .
H13A H 0.3489 0.5251 0.831 0.05 Uiso 1 1 calc R . .
H13B H 0.3382 0.4908 0.9397 0.05 Uiso 1 1 calc R . .
H13C H 0.2836 0.5933 0.8831 0.05 Uiso 1 1 calc R . .
C14 C 0.3602(4) 0.2141(4) 0.7691(3) 0.0205(12) Uani 1 1 d . . .
C15 C 0.3751(4) 0.0508(4) 0.7645(4) 0.0257(13) Uani 1 1 d . . .
H15 H 0.409 0.0015 0.7409 0.031 Uiso 1 1 calc R . .
C16 C 0.2898(4) 0.0197(4) 0.8322(4) 0.0230(12) Uani 1 1 d . . .
H16 H 0.2649 -0.0499 0.8556 0.028 Uiso 1 1 calc R . .
C17 C 0.2422(4) 0.0927(4) 0.8648(4) 0.0225(12) Uani 1 1 d . . .
H17 H 0.1825 0.0733 0.9106 0.027 Uiso 1 1 calc R . .
C18 C 0.4017(4) 0.3248(4) 0.7322(4) 0.0234(13) Uani 1 1 d . . .
C19 C 0.5770(7) 0.3717(7) 0.4519(5) 0.072(3) Uani 1 1 d . . .
H19A H 0.5288 0.4226 0.4666 0.087 Uiso 1 1 calc R . .
H19B H 0.6241 0.4075 0.3951 0.087 Uiso 1 1 calc R . .
C20 C 0.5124(6) 0.2893(8) 0.4380(5) 0.070(3) Uani 1 1 d . . .
H20A H 0.4693 0.32 0.3876 0.085 Uiso 1 1 calc R . .
H20B H 0.5605 0.2395 0.4213 0.085 Uiso 1 1 calc R . .
C21 C 0.6858(6) 0.4071(6) 0.5563(5) 0.062(3) Uani 1 1 d . . .
H21A H 0.7313 0.3769 0.6041 0.093 Uiso 1 1 calc R . .
H21B H 0.6266 0.4417 0.5798 0.093 Uiso 1 1 calc R . .
H21C H 0.7278 0.4571 0.504 0.093 Uiso 1 1 calc R . .
C22 C 0.7366(6) 0.2764(6) 0.4966(5) 0.060(2) Uani 1 1 d . . .
H22A H 0.7772 0.3261 0.4431 0.089 Uiso 1 1 calc R . .
H22B H 0.7126 0.2182 0.4806 0.089 Uiso 1 1 calc R . .
H22C H 0.7822 0.2518 0.5453 0.089 Uiso 1 1 calc R . .
C23 C 0.4074(7) 0.1352(7) 0.5159(6) 0.068(3) Uani 1 1 d . . .
H23A H 0.3699 0.1472 0.4624 0.102 Uiso 1 1 calc R . .
H23B H 0.3596 0.0982 0.571 0.102 Uiso 1 1 calc R . .
H23C H 0.4703 0.0942 0.5107 0.102 Uiso 1 1 calc R . .
C24 C 0.3447(5) 0.2969(6) 0.5267(5) 0.0459(18) Uani 1 1 d . . .
H24A H 0.3653 0.3654 0.5262 0.069 Uiso 1 1 calc R . .
H24B H 0.2981 0.2619 0.5831 0.069 Uiso 1 1 calc R . .
H24C H 0.3068 0.3035 0.4743 0.069 Uiso 1 1 calc R . .
C25 C 0.3104(4) -0.0995(4) 1.2656(3) 0.0206(12) Uani 1 1 d . . .
C26 C 0.3335(5) -0.2325(4) 1.2108(4) 0.0280(14) Uani 1 1 d . . .
H26 H 0.3648 -0.2959 1.2122 0.034 Uiso 1 1 calc R . .
C27 C 0.2644(4) -0.1898(4) 1.1485(4) 0.0268(13) Uani 1 1 d . . .
H27 H 0.2478 -0.2223 1.1068 0.032 Uiso 1 1 calc R . .
C28 C 0.2196(4) -0.0978(4) 1.1484(4) 0.0239(13) Uani 1 1 d . . .
H28 H 0.1727 -0.066 1.105 0.029 Uiso 1 1 calc R . .
C29 C 0.3349(4) -0.0476(5) 1.3331(4) 0.0259(13) Uani 1 1 d . . .
C30 C 0.0631(8) 0.1465(6) 1.3710(6) 0.076(3) Uani 1 1 d . . .
H30A H 0.0225 0.1977 1.3924 0.091 Uiso 1 1 calc R . .
H30B H 0.1077 0.109 1.4184 0.091 Uiso 1 1 calc R . .
C31 C -0.0111(5) 0.0743(7) 1.3572(5) 0.063(3) Uani 1 1 d . . .
H31A H -0.0619 0.1139 1.3165 0.076 Uiso 1 1 calc R . .
H31B H -0.0526 0.0366 1.4165 0.076 Uiso 1 1 calc R . .
C32 C 0.2200(8) 0.2443(7) 1.3188(7) 0.088(4) Uani 1 1 d . . .
H32A H 0.1903 0.2902 1.3511 0.132 Uiso 1 1 calc R . .
H32B H 0.2702 0.2832 1.2661 0.132 Uiso 1 1 calc R . .
H32C H 0.2574 0.189 1.3598 0.132 Uiso 1 1 calc R . .
C33 C 0.0842(5) 0.2860(5) 1.2239(4) 0.0366(16) Uani 1 1 d . . .
H33A H 0.0276 0.2615 1.198 0.055 Uiso 1 1 calc R . .
H33B H 0.1393 0.3237 1.1749 0.055 Uiso 1 1 calc R . .
H33C H 0.0541 0.3317 1.2564 0.055 Uiso 1 1 calc R . .
C34 C 0.0650(6) -0.0962(6) 1.3902(5) 0.072(3) Uani 1 1 d . . .
H34A H -0.0015 -0.1298 1.4262 0.108 Uiso 1 1 calc R . .
H34B H 0.1095 -0.0775 1.4296 0.108 Uiso 1 1 calc R . .
H34C H 0.1034 -0.1434 1.3633 0.108 Uiso 1 1 calc R . .
C35 C -0.0343(5) -0.0293(5) 1.2645(5) 0.0426(17) Uani 1 1 d . . .
H35A H 0.0004 -0.0733 1.2322 0.064 Uiso 1 1 calc R . .
H35B H -0.0572 0.0335 1.2204 0.064 Uiso 1 1 calc R . .
H35C H -0.0966 -0.0661 1.3054 0.064 Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.072(4) . ?
Ni1 O5 2.072(4) . ?
Ni1 N6 2.120(4) . ?
Ni1 N5 2.126(4) . ?
Ni1 N1 2.142(5) . ?
Ni1 N4 2.142(4) . ?
Ni2 O2 2.061(4) . ?
Ni2 O3 2.067(4) . ?
Ni2 N12 2.120(5) . ?
Ni2 N10 2.120(4) . ?
Ni2 N3 2.131(5) . ?
Ni2 N13 2.166(5) . ?
Ni3 O4 2.070(4) 2_657 ?
Ni3 O6 2.077(4) . ?
Ni3 N8 2.097(5) . ?
Ni3 N7 2.098(5) . ?
Ni3 N11 2.127(5) 2_657 ?
Ni3 N9 2.137(5) . ?
O1 C7 1.244(6) . ?
O2 C7 1.253(6) . ?
O3 C29 1.235(6) . ?
O4 C29 1.249(6) . ?
O4 Ni3 2.070(4) 2_657 ?
O5 C18 1.254(6) . ?
O6 C18 1.248(6) . ?
Cl1 O10 1.405(10) . ?
Cl1 O7 1.416(9) . ?
Cl1 O9 1.433(9) . ?
Cl1 O8 1.452(11) . ?
Cl1 O8 2.079(12) 2_766 ?
Cl2 O11 1.390(5) . ?
Cl2 O12 1.430(6) . ?
Cl2 O14 1.438(5) . ?
Cl2 O13 1.450(5) . ?
Cl3 O15 1.417(5) . ?
Cl3 O17 1.418(5) . ?
Cl3 O18 1.421(5) . ?
Cl3 O16 1.447(5) . ?
Cl4 O19B 1.387(8) 2_655 ?
Cl4 O19B 1.387(8) . ?
Cl4 O20A 1.388(8) 2_655 ?
Cl4 O20A 1.388(8) . ?
Cl4 O19A 1.395(8) 2_655 ?
Cl4 O19A 1.395(8) . ?
Cl4 O20B 1.530(6) . ?
Cl4 O20B 1.530(6) 2_655 ?
O1W H1W 0.94(2) . ?
O1W H2W 0.93(2) . ?
O2W H3W 0.93(2) . ?
O2W H4W 0.93(2) . ?
N1 C2 1.325(7) . ?
N1 C6 1.333(7) . ?
N3 C2 1.325(7) . ?
N3 C4 1.351(7) . ?
N4 C11 1.469(8) . ?
N4 C10 1.472(7) . ?
N4 C8 1.483(7) . ?
N5 C13 1.475(7) . ?
N5 C9 1.482(8) . ?
N5 C12 1.486(8) . ?
N6 C14 1.314(7) . ?
N6 C17 1.343(7) . ?
N7 C15 1.348(7) . ?
N7 C14 1.353(7) . ?
N8 C21 1.458(11) . ?
N8 C22 1.472(8) . ?
N8 C19 1.505(9) . ?
N9 C20 1.463(9) . ?
N9 C24 1.486(8) . ?
N9 C23 1.500(10) . ?
N10 C28 1.333(7) . ?
N10 C25 1.344(7) . ?
N11 C25 1.331(7) . ?
N11 C26 1.353(7) . ?
N11 Ni3 2.127(5) 2_657 ?
N12 C30 1.452(10) . ?
N12 C33 1.455(7) . ?
N12 C32 1.506(10) . ?
N13 C35 1.449(8) . ?
N13 C34 1.474(8) . ?
N13 C31 1.508(9) . ?
C2 C7 1.525(7) . ?
C4 C5 1.366(8) . ?
C4 H4 0.95 . ?
C5 C6 1.391(8) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C8 C9 1.518(9) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C18 1.518(8) . ?
C15 C16 1.380(8) . ?
C15 H15 0.95 . ?
C16 C17 1.373(7) . ?
C16 H16 0.95 . ?
C17 H17 0.95 . ?
C19 C20 1.496(13) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 C29 1.522(8) . ?
C26 C27 1.372(8) . ?
C26 H26 0.95 . ?
C27 C28 1.383(8) . ?
C27 H27 0.95 . ?
C28 H28 0.95 . ?
C30 C31 1.462(12) . ?
C30 H30A 0.99 . ?
C30 H30B 0.99 . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
C34 H34A 0.98 . ?
C34 H34B 0.98 . ?
C34 H34C 0.98 . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?

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 O5 168.16(14) . . ?
O1 Ni1 N6 89.95(15) . . ?
O5 Ni1 N6 79.37(15) . . ?
O1 Ni1 N5 98.97(16) . . ?
O5 Ni1 N5 91.72(16) . . ?
N6 Ni1 N5 171.08(18) . . ?
O1 Ni1 N1 78.97(15) . . ?
O5 Ni1 N1 95.78(16) . . ?
N6 Ni1 N1 89.95(16) . . ?
N5 Ni1 N1 91.43(18) . . ?
O1 Ni1 N4 90.89(15) . . ?
O5 Ni1 N4 95.11(16) . . ?
N6 Ni1 N4 95.18(17) . . ?
N5 Ni1 N4 85.08(18) . . ?
N1 Ni1 N4 168.66(17) . . ?
O2 Ni2 O3 168.61(15) . . ?
O2 Ni2 N12 97.90(17) . . ?
O3 Ni2 N12 90.41(17) . . ?
O2 Ni2 N10 92.67(15) . . ?
O3 Ni2 N10 79.53(16) . . ?
N12 Ni2 N10 169.02(18) . . ?
O2 Ni2 N3 79.37(16) . . ?
O3 Ni2 N3 92.37(17) . . ?
N12 Ni2 N3 93.86(19) . . ?
N10 Ni2 N3 90.96(16) . . ?
O2 Ni2 N13 91.44(16) . . ?
O3 Ni2 N13 97.06(17) . . ?
N12 Ni2 N13 84.9(2) . . ?
N10 Ni2 N13 91.93(17) . . ?
N3 Ni2 N13 170.48(17) . . ?
O4 Ni3 O6 169.82(15) 2_657 . ?
O4 Ni3 N8 97.6(2) 2_657 . ?
O6 Ni3 N8 89.49(19) . . ?
O4 Ni3 N7 93.60(17) 2_657 . ?
O6 Ni3 N7 79.53(16) . . ?
N8 Ni3 N7 168.66(19) . . ?
O4 Ni3 N11 79.09(16) 2_657 2_657 ?
O6 Ni3 N11 93.15(16) . 2_657 ?
N8 Ni3 N11 94.7(2) . 2_657 ?
N7 Ni3 N11 88.81(17) . 2_657 ?
O4 Ni3 N9 89.43(18) 2_657 . ?
O6 Ni3 N9 98.39(18) . . ?
N8 Ni3 N9 85.5(2) . . ?
N7 Ni3 N9 93.2(2) . . ?
N11 Ni3 N9 168.45(19) 2_657 . ?
C7 O1 Ni1 116.5(3) . . ?
C7 O2 Ni2 116.2(3) . . ?
C29 O3 Ni2 116.6(4) . . ?
C29 O4 Ni3 116.8(4) . 2_657 ?
C18 O5 Ni1 116.0(3) . . ?
C18 O6 Ni3 115.8(3) . . ?
O10 Cl1 O7 108.7(6) . . ?
O10 Cl1 O9 109.6(7) . . ?
O7 Cl1 O9 110.1(5) . . ?
O10 Cl1 O8 110.8(7) . . ?
O7 Cl1 O8 109.6(6) . . ?
O9 Cl1 O8 108.1(6) . . ?
O11 Cl2 O12 113.3(5) . . ?
O11 Cl2 O14 109.9(3) . . ?
O12 Cl2 O14 109.3(3) . . ?
O11 Cl2 O13 108.0(4) . . ?
O12 Cl2 O13 106.6(3) . . ?
O14 Cl2 O13 109.7(3) . . ?
O15 Cl3 O17 110.8(4) . . ?
O15 Cl3 O18 111.7(3) . . ?
O17 Cl3 O18 110.3(3) . . ?
O15 Cl3 O16 107.7(3) . . ?
O17 Cl3 O16 108.2(3) . . ?
O18 Cl3 O16 108.0(3) . . ?
O19B Cl4 O20A 115.3(5) . . ?
O19B Cl4 O19A 113.1(5) . . ?
O20A Cl4 O19A 114.4(5) . . ?
O19B Cl4 O20B 103.9(5) . . ?
O20A Cl4 O20B 104.4(5) . . ?
O19A Cl4 O20B 104.1(5) . . ?
H1W O1W H2W 104(4) . . ?
H3W O2W H4W 110(4) . . ?
C2 N1 C6 116.5(5) . . ?
C2 N1 Ni1 111.1(3) . . ?
C6 N1 Ni1 132.4(4) . . ?
C2 N3 C4 116.5(5) . . ?
C2 N3 Ni2 111.3(4) . . ?
C4 N3 Ni2 132.2(4) . . ?
C11 N4 C10 107.4(5) . . ?
C11 N4 C8 110.1(5) . . ?
C10 N4 C8 107.7(5) . . ?
C11 N4 Ni1 113.2(4) . . ?
C10 N4 Ni1 114.2(3) . . ?
C8 N4 Ni1 104.1(4) . . ?
C13 N5 C9 109.2(5) . . ?
C13 N5 C12 107.7(5) . . ?
C9 N5 C12 110.2(5) . . ?
C13 N5 Ni1 113.7(3) . . ?
C9 N5 Ni1 103.7(4) . . ?
C12 N5 Ni1 112.3(4) . . ?
C14 N6 C17 117.0(4) . . ?
C14 N6 Ni1 111.0(3) . . ?
C17 N6 Ni1 131.9(4) . . ?
C15 N7 C14 115.5(5) . . ?
C15 N7 Ni3 132.7(4) . . ?
C14 N7 Ni3 111.8(4) . . ?
C21 N8 C22 106.1(6) . . ?
C21 N8 C19 110.3(6) . . ?
C22 N8 C19 110.1(6) . . ?
C21 N8 Ni3 113.5(4) . . ?
C22 N8 Ni3 114.0(4) . . ?
C19 N8 Ni3 102.8(4) . . ?
C20 N9 C24 109.6(5) . . ?
C20 N9 C23 107.8(6) . . ?
C24 N9 C23 107.6(6) . . ?
C20 N9 Ni3 104.8(5) . . ?
C24 N9 Ni3 112.4(4) . . ?
C23 N9 Ni3 114.5(4) . . ?
C28 N10 C25 116.6(4) . . ?
C28 N10 Ni2 132.7(4) . . ?
C25 N10 Ni2 110.6(3) . . ?
C25 N11 C26 115.8(5) . . ?
C25 N11 Ni3 111.1(4) . 2_657 ?
C26 N11 Ni3 133.1(4) . 2_657 ?
C30 N12 C33 115.3(6) . . ?
C30 N12 C32 103.1(7) . . ?
C33 N12 C32 105.1(5) . . ?
C30 N12 Ni2 104.4(4) . . ?
C33 N12 Ni2 115.5(4) . . ?
C32 N12 Ni2 113.0(4) . . ?
C35 N13 C34 109.3(6) . . ?
C35 N13 C31 108.1(5) . . ?
C34 N13 C31 110.3(6) . . ?
C35 N13 Ni2 113.4(4) . . ?
C34 N13 Ni2 112.7(4) . . ?
C31 N13 Ni2 102.6(4) . . ?
N1 C2 N3 126.9(5) . . ?
N1 C2 C7 116.7(5) . . ?
N3 C2 C7 116.4(5) . . ?
N3 C4 C5 120.8(5) . . ?
N3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 118.3(5) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
N1 C6 C5 121.1(5) . . ?
N1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
O1 C7 O2 126.8(5) . . ?
O1 C7 C2 116.6(5) . . ?
O2 C7 C2 116.6(4) . . ?
N4 C8 C9 108.7(5) . . ?
N4 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N4 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N5 C9 C8 110.5(5) . . ?
N5 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N5 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N4 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 N7 126.5(5) . . ?
N6 C14 C18 117.8(5) . . ?
N7 C14 C18 115.7(5) . . ?
N7 C15 C16 121.7(5) . . ?
N7 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C17 C16 C15 117.8(5) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
N6 C17 C16 121.4(5) . . ?
N6 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
O6 C18 O5 127.5(5) . . ?
O6 C18 C14 116.8(5) . . ?
O5 C18 C14 115.7(5) . . ?
C20 C19 N8 110.5(6) . . ?
C20 C19 H19A 109.6 . . ?
N8 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
N8 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
N9 C20 C19 109.9(7) . . ?
N9 C20 H20A 109.7 . . ?
C19 C20 H20A 109.7 . . ?
N9 C20 H20B 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
N8 C21 H21A 109.5 . . ?
N8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C22 H22A 109.5 . . ?
N8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N9 C23 H23A 109.5 . . ?
N9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N9 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N9 C24 H24A 109.5 . . ?
N9 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N9 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N11 C25 N10 126.3(5) . . ?
N11 C25 C29 117.1(5) . . ?
N10 C25 C29 116.6(5) . . ?
N11 C26 C27 122.0(5) . . ?
N11 C26 H26 119 . . ?
C27 C26 H26 119 . . ?
C26 C27 C28 117.7(5) . . ?
C26 C27 H27 121.1 . . ?
C28 C27 H27 121.1 . . ?
N10 C28 C27 121.5(5) . . ?
N10 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
O3 C29 O4 127.7(5) . . ?
O3 C29 C25 116.6(5) . . ?
O4 C29 C25 115.8(5) . . ?
N12 C30 C31 110.6(7) . . ?
N12 C30 H30A 109.5 . . ?
C31 C30 H30A 109.5 . . ?
N12 C30 H30B 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C30 C31 N13 115.0(6) . . ?
C30 C31 H31A 108.5 . . ?
N13 C31 H31A 108.5 . . ?
C30 C31 H31B 108.5 . . ?
N13 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
N12 C32 H32A 109.5 . . ?
N12 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N12 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N12 C33 H33A 109.5 . . ?
N12 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N12 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N13 C34 H34A 109.5 . . ?
N13 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N13 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N13 C35 H35A 109.5 . . ?
N13 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N13 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Ni1 O1 C7 63.8(8) . . . . ?
N6 Ni1 O1 C7 89.2(4) . . . . ?
N5 Ni1 O1 C7 -90.5(4) . . . . ?
N1 Ni1 O1 C7 -0.8(3) . . . . ?
N4 Ni1 O1 C7 -175.7(4) . . . . ?
O3 Ni2 O2 C7 -47.1(9) . . . . ?
N12 Ni2 O2 C7 89.4(4) . . . . ?
N10 Ni2 O2 C7 -93.5(3) . . . . ?
N3 Ni2 O2 C7 -3.0(3) . . . . ?
N13 Ni2 O2 C7 174.5(3) . . . . ?
O2 Ni2 O3 C29 -45.4(10) . . . . ?
N12 Ni2 O3 C29 177.6(4) . . . . ?
N10 Ni2 O3 C29 2.0(4) . . . . ?
N3 Ni2 O3 C29 -88.5(4) . . . . ?
N13 Ni2 O3 C29 92.7(4) . . . . ?
O1 Ni1 O5 C18 26.7(9) . . . . ?
N6 Ni1 O5 C18 0.9(4) . . . . ?
N5 Ni1 O5 C18 -178.7(4) . . . . ?
N1 Ni1 O5 C18 89.7(4) . . . . ?
N4 Ni1 O5 C18 -93.5(4) . . . . ?
O4 Ni3 O6 C18 -42.7(11) 2_657 . . . ?
N8 Ni3 O6 C18 -177.4(4) . . . . ?
N7 Ni3 O6 C18 5.4(4) . . . . ?
N11 Ni3 O6 C18 -82.8(4) 2_657 . . . ?
N9 Ni3 O6 C18 97.2(4) . . . . ?
O1 Ni1 N1 C2 -1.5(3) . . . . ?
O5 Ni1 N1 C2 -170.8(3) . . . . ?
N6 Ni1 N1 C2 -91.5(3) . . . . ?
N5 Ni1 N1 C2 97.4(3) . . . . ?
N4 Ni1 N1 C2 25.6(10) . . . . ?
O1 Ni1 N1 C6 -178.3(5) . . . . ?
O5 Ni1 N1 C6 12.4(5) . . . . ?
N6 Ni1 N1 C6 91.7(5) . . . . ?
N5 Ni1 N1 C6 -79.5(5) . . . . ?
N4 Ni1 N1 C6 -151.3(8) . . . . ?
O2 Ni2 N3 C2 0.4(3) . . . . ?
O3 Ni2 N3 C2 172.5(3) . . . . ?
N12 Ni2 N3 C2 -96.9(4) . . . . ?
N10 Ni2 N3 C2 93.0(3) . . . . ?
N13 Ni2 N3 C2 -14.7(12) . . . . ?
O2 Ni2 N3 C4 -177.5(5) . . . . ?
O3 Ni2 N3 C4 -5.4(5) . . . . ?
N12 Ni2 N3 C4 85.1(5) . . . . ?
N10 Ni2 N3 C4 -85.0(5) . . . . ?
N13 Ni2 N3 C4 167.3(9) . . . . ?
O1 Ni1 N4 C11 -157.0(4) . . . . ?
O5 Ni1 N4 C11 12.8(4) . . . . ?
N6 Ni1 N4 C11 -67.0(4) . . . . ?
N5 Ni1 N4 C11 104.1(4) . . . . ?
N1 Ni1 N4 C11 176.5(8) . . . . ?
O1 Ni1 N4 C10 -33.7(4) . . . . ?
O5 Ni1 N4 C10 136.0(4) . . . . ?
N6 Ni1 N4 C10 56.3(4) . . . . ?
N5 Ni1 N4 C10 -132.7(4) . . . . ?
N1 Ni1 N4 C10 -60.3(10) . . . . ?
O1 Ni1 N4 C8 83.5(4) . . . . ?
O5 Ni1 N4 C8 -106.8(4) . . . . ?
N6 Ni1 N4 C8 173.5(4) . . . . ?
N5 Ni1 N4 C8 -15.5(4) . . . . ?
N1 Ni1 N4 C8 56.9(10) . . . . ?
O1 Ni1 N5 C13 136.8(4) . . . . ?
O5 Ni1 N5 C13 -38.1(4) . . . . ?
N6 Ni1 N5 C13 -41.1(14) . . . . ?
N1 Ni1 N5 C13 57.7(4) . . . . ?
N4 Ni1 N5 C13 -133.1(4) . . . . ?
O1 Ni1 N5 C9 -104.8(4) . . . . ?
O5 Ni1 N5 C9 80.3(4) . . . . ?
N6 Ni1 N5 C9 77.4(12) . . . . ?
N1 Ni1 N5 C9 176.2(4) . . . . ?
N4 Ni1 N5 C9 -14.6(4) . . . . ?
O1 Ni1 N5 C12 14.2(4) . . . . ?
O5 Ni1 N5 C12 -160.6(4) . . . . ?
N6 Ni1 N5 C12 -163.6(10) . . . . ?
N1 Ni1 N5 C12 -64.8(4) . . . . ?
N4 Ni1 N5 C12 104.4(4) . . . . ?
O1 Ni1 N6 C14 -173.8(3) . . . . ?
O5 Ni1 N6 C14 1.1(3) . . . . ?
N5 Ni1 N6 C14 4.1(13) . . . . ?
N1 Ni1 N6 C14 -94.8(4) . . . . ?
N4 Ni1 N6 C14 95.3(4) . . . . ?
O1 Ni1 N6 C17 3.4(5) . . . . ?
O5 Ni1 N6 C17 178.2(5) . . . . ?
N5 Ni1 N6 C17 -178.8(10) . . . . ?
N1 Ni1 N6 C17 82.3(5) . . . . ?
N4 Ni1 N6 C17 -87.5(5) . . . . ?
O4 Ni3 N7 C15 -9.5(5) 2_657 . . . ?
O6 Ni3 N7 C15 178.0(5) . . . . ?
N8 Ni3 N7 C15 163.4(10) . . . . ?
N11 Ni3 N7 C15 -88.5(5) 2_657 . . . ?
N9 Ni3 N7 C15 80.1(5) . . . . ?
O4 Ni3 N7 C14 170.1(3) 2_657 . . . ?
O6 Ni3 N7 C14 -2.3(3) . . . . ?
N8 Ni3 N7 C14 -17.0(12) . . . . ?
N11 Ni3 N7 C14 91.1(4) 2_657 . . . ?
N9 Ni3 N7 C14 -100.3(4) . . . . ?
O4 Ni3 N8 C21 -134.3(4) 2_657 . . . ?
O6 Ni3 N8 C21 38.5(4) . . . . ?
N7 Ni3 N8 C21 52.9(13) . . . . ?
N11 Ni3 N8 C21 -54.7(4) 2_657 . . . ?
N9 Ni3 N8 C21 136.9(5) . . . . ?
O4 Ni3 N8 C22 -12.6(5) 2_657 . . . ?
O6 Ni3 N8 C22 160.2(5) . . . . ?
N7 Ni3 N8 C22 174.6(9) . . . . ?
N11 Ni3 N8 C22 67.0(5) 2_657 . . . ?
N9 Ni3 N8 C22 -101.4(5) . . . . ?
O4 Ni3 N8 C19 106.6(5) 2_657 . . . ?
O6 Ni3 N8 C19 -80.7(5) . . . . ?
N7 Ni3 N8 C19 -66.3(13) . . . . ?
N11 Ni3 N8 C19 -173.8(5) 2_657 . . . ?
N9 Ni3 N8 C19 17.8(5) . . . . ?
O4 Ni3 N9 C20 -86.7(5) 2_657 . . . ?
O6 Ni3 N9 C20 99.8(5) . . . . ?
N8 Ni3 N9 C20 11.0(5) . . . . ?
N7 Ni3 N9 C20 179.7(5) . . . . ?
N11 Ni3 N9 C20 -80.4(12) 2_657 . . . ?
O4 Ni3 N9 C24 154.4(5) 2_657 . . . ?
O6 Ni3 N9 C24 -19.1(5) . . . . ?
N8 Ni3 N9 C24 -107.9(5) . . . . ?
N7 Ni3 N9 C24 60.8(5) . . . . ?
N11 Ni3 N9 C24 160.6(9) 2_657 . . . ?
O4 Ni3 N9 C23 31.2(5) 2_657 . . . ?
O6 Ni3 N9 C23 -142.3(5) . . . . ?
N8 Ni3 N9 C23 128.9(5) . . . . ?
N7 Ni3 N9 C23 -62.4(5) . . . . ?
N11 Ni3 N9 C23 37.4(13) 2_657 . . . ?
O2 Ni2 N10 C28 -10.1(5) . . . . ?
O3 Ni2 N10 C28 178.3(5) . . . . ?
N12 Ni2 N10 C28 154.4(9) . . . . ?
N3 Ni2 N10 C28 -89.5(5) . . . . ?
N13 Ni2 N10 C28 81.5(5) . . . . ?
O2 Ni2 N10 C25 171.9(3) . . . . ?
O3 Ni2 N10 C25 0.2(3) . . . . ?
N12 Ni2 N10 C25 -23.7(12) . . . . ?
N3 Ni2 N10 C25 92.5(4) . . . . ?
N13 Ni2 N10 C25 -96.6(4) . . . . ?
O2 Ni2 N12 C30 113.6(5) . . . . ?
O3 Ni2 N12 C30 -74.2(5) . . . . ?
N10 Ni2 N12 C30 -50.7(12) . . . . ?
N3 Ni2 N12 C30 -166.6(5) . . . . ?
N13 Ni2 N12 C30 22.9(5) . . . . ?
O2 Ni2 N12 C33 -14.0(5) . . . . ?
O3 Ni2 N12 C33 158.2(5) . . . . ?
N10 Ni2 N12 C33 -178.4(9) . . . . ?
N3 Ni2 N12 C33 65.8(5) . . . . ?
N13 Ni2 N12 C33 -104.8(5) . . . . ?
O2 Ni2 N12 C32 -135.1(5) . . . . ?
O3 Ni2 N12 C32 37.1(5) . . . . ?
N10 Ni2 N12 C32 60.5(12) . . . . ?
N3 Ni2 N12 C32 -55.3(5) . . . . ?
N13 Ni2 N12 C32 134.1(6) . . . . ?
O2 Ni2 N13 C35 21.4(4) . . . . ?
O3 Ni2 N13 C35 -151.0(4) . . . . ?
N12 Ni2 N13 C35 119.2(4) . . . . ?
N10 Ni2 N13 C35 -71.3(4) . . . . ?
N3 Ni2 N13 C35 36.3(13) . . . . ?
O2 Ni2 N13 C34 146.4(5) . . . . ?
O3 Ni2 N13 C34 -26.0(5) . . . . ?
N12 Ni2 N13 C34 -115.8(5) . . . . ?
N10 Ni2 N13 C34 53.6(5) . . . . ?
N3 Ni2 N13 C34 161.3(10) . . . . ?
O2 Ni2 N13 C31 -95.0(4) . . . . ?
O3 Ni2 N13 C31 92.6(4) . . . . ?
N12 Ni2 N13 C31 2.8(4) . . . . ?
N10 Ni2 N13 C31 172.3(4) . . . . ?
N3 Ni2 N13 C31 -80.1(11) . . . . ?
C6 N1 C2 N3 0.5(8) . . . . ?
Ni1 N1 C2 N3 -176.9(4) . . . . ?
C6 N1 C2 C7 -179.4(4) . . . . ?
Ni1 N1 C2 C7 3.2(5) . . . . ?
C4 N3 C2 N1 0.2(8) . . . . ?
Ni2 N3 C2 N1 -178.1(4) . . . . ?
C4 N3 C2 C7 -179.9(4) . . . . ?
Ni2 N3 C2 C7 1.7(5) . . . . ?
C2 N3 C4 C5 -1.1(8) . . . . ?
Ni2 N3 C4 C5 176.8(4) . . . . ?
N3 C4 C5 C6 1.3(8) . . . . ?
C2 N1 C6 C5 -0.3(7) . . . . ?
Ni1 N1 C6 C5 176.4(4) . . . . ?
C4 C5 C6 N1 -0.6(8) . . . . ?
Ni1 O1 C7 O2 -176.8(4) . . . . ?
Ni1 O1 C7 C2 2.7(5) . . . . ?
Ni2 O2 C7 O1 -175.7(4) . . . . ?
Ni2 O2 C7 C2 4.8(5) . . . . ?
N1 C2 C7 O1 -4.1(7) . . . . ?
N3 C2 C7 O1 176.0(4) . . . . ?
N1 C2 C7 O2 175.4(4) . . . . ?
N3 C2 C7 O2 -4.5(7) . . . . ?
C11 N4 C8 C9 -78.8(7) . . . . ?
C10 N4 C8 C9 164.5(5) . . . . ?
Ni1 N4 C8 C9 42.8(6) . . . . ?
C13 N5 C9 C8 164.6(5) . . . . ?
C12 N5 C9 C8 -77.3(7) . . . . ?
Ni1 N5 C9 C8 43.1(6) . . . . ?
N4 C8 C9 N5 -61.2(7) . . . . ?
C17 N6 C14 N7 0.8(8) . . . . ?
Ni1 N6 C14 N7 178.4(4) . . . . ?
C17 N6 C14 C18 179.7(5) . . . . ?
Ni1 N6 C14 C18 -2.7(6) . . . . ?
C15 N7 C14 N6 -1.7(8) . . . . ?
Ni3 N7 C14 N6 178.6(4) . . . . ?
C15 N7 C14 C18 179.3(4) . . . . ?
Ni3 N7 C14 C18 -0.4(5) . . . . ?
C14 N7 C15 C16 1.1(7) . . . . ?
Ni3 N7 C15 C16 -179.2(4) . . . . ?
N7 C15 C16 C17 0.2(8) . . . . ?
C14 N6 C17 C16 0.8(7) . . . . ?
Ni1 N6 C17 C16 -176.2(4) . . . . ?
C15 C16 C17 N6 -1.2(8) . . . . ?
Ni3 O6 C18 O5 175.6(5) . . . . ?
Ni3 O6 C18 C14 -7.2(6) . . . . ?
Ni1 O5 C18 O6 174.8(4) . . . . ?
Ni1 O5 C18 C14 -2.4(6) . . . . ?
N6 C14 C18 O6 -174.0(5) . . . . ?
N7 C14 C18 O6 5.1(7) . . . . ?
N6 C14 C18 O5 3.6(7) . . . . ?
N7 C14 C18 O5 -177.3(5) . . . . ?
C21 N8 C19 C20 -166.3(6) . . . . ?
C22 N8 C19 C20 76.9(8) . . . . ?
Ni3 N8 C19 C20 -44.9(7) . . . . ?
C24 N9 C20 C19 81.9(7) . . . . ?
C23 N9 C20 C19 -161.3(6) . . . . ?
Ni3 N9 C20 C19 -38.9(7) . . . . ?
N8 C19 C20 N9 59.6(8) . . . . ?
C26 N11 C25 N10 -0.1(8) . . . . ?
Ni3 N11 C25 N10 178.3(4) 2_657 . . . ?
C26 N11 C25 C29 178.7(5) . . . . ?
Ni3 N11 C25 C29 -2.9(6) 2_657 . . . ?
C28 N10 C25 N11 -1.6(8) . . . . ?
Ni2 N10 C25 N11 176.8(4) . . . . ?
C28 N10 C25 C29 179.6(5) . . . . ?
Ni2 N10 C25 C29 -2.0(6) . . . . ?
C25 N11 C26 C27 1.1(8) . . . . ?
Ni3 N11 C26 C27 -176.9(4) 2_657 . . . ?
N11 C26 C27 C28 -0.4(8) . . . . ?
C25 N10 C28 C27 2.4(8) . . . . ?
Ni2 N10 C28 C27 -175.6(4) . . . . ?
C26 C27 C28 N10 -1.5(8) . . . . ?
Ni2 O3 C29 O4 176.9(5) . . . . ?
Ni2 O3 C29 C25 -3.7(6) . . . . ?
Ni3 O4 C29 O3 175.8(5) 2_657 . . . ?
Ni3 O4 C29 C25 -3.7(6) 2_657 . . . ?
N11 C25 C29 O3 -175.0(5) . . . . ?
N10 C25 C29 O3 3.9(7) . . . . ?
N11 C25 C29 O4 4.5(7) . . . . ?
N10 C25 C29 O4 -176.5(5) . . . . ?
C33 N12 C30 C31 81.9(8) . . . . ?
C32 N12 C30 C31 -164.2(7) . . . . ?
Ni2 N12 C30 C31 -45.9(8) . . . . ?
N12 C30 C31 N13 54.4(10) . . . . ?
C35 N13 C31 C30 -150.1(7) . . . . ?
C34 N13 C31 C30 90.4(9) . . . . ?
Ni2 N13 C31 C30 -30.0(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O2W 0.94(2) 1.90(2) 2.835(6) 173(6) .
O1W H2W O2 0.93(2) 2.36(3) 3.218(5) 153(5) 1_654
O1W H2W O1 0.93(2) 2.56(5) 3.150(5) 122(4) 1_654
O2W H3W O13 0.93(2) 1.99(3) 2.897(7) 166(6) .
O2W H4W O16 0.93(2) 1.91(3) 2.809(7) 162(6) .

data_ar190
_database_code_depnum_ccdc_archive 'CCDC 725441'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H114 B F6 N24 Ni6 O12'
_chemical_formula_weight         1912.88

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   23.206(5)
_cell_length_b                   20.746(5)
_cell_length_c                   16.193(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 130.773(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5904(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6028
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      22.61

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2002
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34133
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.1160
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         28.18
_reflns_number_total             7074
_reflns_number_gt                4736
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL)'
_computing_publication_material  'publCIF (Westrip, 2007)'

_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)+(0.0480P)²+2.3724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    contr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7074
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1810
_refine_ls_wR_factor_gt          0.1664
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.23396(3) 0.0000 0.05398(19) Uani 1 2 d S . .
Ni2 Ni 0.26223(2) 0.366935(18) 0.32525(4) 0.05773(17) Uani 1 1 d . . .
N1A N 0.07054(15) 0.30722(12) 0.0136(2) 0.0541(6) Uani 1 1 d . . .
C2A C 0.0653(2) 0.33972(18) -0.0616(3) 0.0692(9) Uani 1 1 d . . .
H2A H 0.0250 0.3316 -0.1351 0.083 Uiso 1 1 calc R . .
C3A C 0.1200(2) 0.3862(2) -0.0314(3) 0.0769(10) Uani 1 1 d . . .
H3A H 0.1168 0.4091 -0.0836 0.092 Uiso 1 1 calc R . .
C4A C 0.1782(2) 0.39662(18) 0.0777(3) 0.0688(9) Uani 1 1 d . . .
H4A H 0.2156 0.4268 0.0999 0.083 Uiso 1 1 calc R . .
N5A N 0.18244(15) 0.36413(12) 0.1531(2) 0.0558(7) Uani 1 1 d . . .
C6A C 0.12710(17) 0.32114(14) 0.1161(3) 0.0518(7) Uani 1 1 d . . .
C7A C 0.13321(17) 0.28345(14) 0.2016(3) 0.0530(7) Uani 1 1 d . . .
O8A O 0.08252(12) 0.24362(10) 0.16673(18) 0.0584(6) Uani 1 1 d . . .
O9A O 0.18830(13) 0.29665(10) 0.29800(18) 0.0619(6) Uani 1 1 d . . .
N1B N 0.19942(15) 0.44243(12) 0.3211(2) 0.0554(6) Uani 1 1 d . . .
C2B C 0.1396(2) 0.44332(18) 0.3178(3) 0.0665(9) Uani 1 1 d . . .
H2B H 0.1195 0.4047 0.3181 0.080 Uiso 1 1 calc R . .
C3B C 0.1087(3) 0.5000 0.3139(5) 0.0731(14) Uani 1 2 d S . .
H3B H 0.0663 0.5000 0.3086 0.088 Uiso 1 2 calc SR . .
C4B C 0.2252(2) 0.5000 0.3221(4) 0.0527(10) Uani 1 2 d S . .
C5B C 0.2936(2) 0.5000 0.3281(4) 0.0537(11) Uani 1 2 d S . .
O6B O 0.31739(12) 0.44652(10) 0.3288(2) 0.0625(6) Uani 1 1 d . . .
C1C C 0.3069(3) 0.2390(2) 0.2923(6) 0.148(3) Uani 1 1 d . . .
H1C1 H 0.2709 0.2415 0.2142 0.222 Uiso 1 1 calc R . .
H1C2 H 0.2818 0.2239 0.3178 0.222 Uiso 1 1 calc R . .
H1C3 H 0.3470 0.2097 0.3153 0.222 Uiso 1 1 calc R . .
C2C C 0.3693(3) 0.3276(3) 0.2836(6) 0.1197(19) Uani 1 1 d . . .
H2C1 H 0.4144 0.3041 0.3111 0.179 Uiso 1 1 calc R . .
H2C2 H 0.3812 0.3726 0.2994 0.179 Uiso 1 1 calc R . .
H2C3 H 0.3313 0.3216 0.2061 0.179 Uiso 1 1 calc R . .
N3C N 0.33900(18) 0.30284(16) 0.3377(4) 0.0914(12) Uani 1 1 d . . .
C4C C 0.4043(3) 0.2988(4) 0.4599(6) 0.144(3) Uani 1 1 d . . .
H4C1 H 0.4346 0.2609 0.4763 0.173 Uiso 1 1 calc R . .
H4C2 H 0.4366 0.3364 0.4838 0.173 Uiso 1 1 calc R . .
C5C C 0.3784(4) 0.2956(3) 0.5182(5) 0.137(2) Uani 1 1 d . . .
H5C1 H 0.4216 0.2922 0.5956 0.165 Uiso 1 1 calc R . .
H5C2 H 0.3471 0.2574 0.4961 0.165 Uiso 1 1 calc R . .
N6C N 0.3331(2) 0.35410(15) 0.4969(3) 0.0816(10) Uani 1 1 d . . .
C7C C 0.2913(3) 0.3420(3) 0.5349(4) 0.116(2) Uani 1 1 d . . .
H7C1 H 0.2441 0.3209 0.4783 0.175 Uiso 1 1 calc R . .
H7C2 H 0.2813 0.3822 0.5527 0.175 Uiso 1 1 calc R . .
H7C3 H 0.3213 0.3150 0.5984 0.175 Uiso 1 1 calc R . .
C8C C 0.3820(3) 0.4104(2) 0.5615(4) 0.125(2) Uani 1 1 d . . .
H8C1 H 0.4168 0.3995 0.6375 0.188 Uiso 1 1 calc R . .
H8C2 H 0.3508 0.4460 0.5494 0.188 Uiso 1 1 calc R . .
H8C3 H 0.4101 0.4223 0.5393 0.188 Uiso 1 1 calc R . .
C1D C -0.0458(4) 0.1655(3) 0.1150(5) 0.122(2) Uani 1 1 d . . .
H1D1 H -0.0812 0.1975 0.1007 0.183 Uiso 1 1 calc R . .
H1D2 H 0.0050 0.1786 0.1762 0.183 Uiso 1 1 calc R . .
H1D3 H -0.0568 0.1251 0.1311 0.183 Uiso 1 1 calc R . .
C2D C -0.1349(3) 0.1489(2) -0.0798(4) 0.1101(18) Uani 1 1 d . . .
H2D1 H -0.1511 0.1068 -0.0778 0.165 Uiso 1 1 calc R . .
H2D2 H -0.1413 0.1531 -0.1444 0.165 Uiso 1 1 calc R . .
H2D3 H -0.1650 0.1810 -0.0803 0.165 Uiso 1 1 calc R . .
N3D N -0.05272(18) 0.15809(15) 0.0189(3) 0.0769(9) Uani 1 1 d . . .
C4D C -0.0071(4) 0.1009(2) 0.0359(7) 0.142(3) Uani 1 1 d . . .
H4D1 H 0.0410 0.1009 0.1103 0.170 Uiso 1 1 calc R . .
H4D2 H -0.0343 0.0619 0.0252 0.170 Uiso 1 1 calc R . .
B1E B 0.0000 0.5000 0.0000 0.092(3) Uani 1 4 d S . .
F2E F 0.0286(8) 0.5000 -0.0593(11) 0.280(5) Uani 1 2 d S . .
F3E F 0.0440(6) 0.4588(5) 0.0654(6) 0.447(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
Ni1 O8A 2.060(2) . ?
Ni1 O8A 2.060(2) 2 ?
Ni1 N3D 2.134(3) . ?
Ni1 N3D 2.134(3) 2 ?
Ni1 N1A 2.137(3) . ?
Ni1 N1A 2.137(3) 2 ?
Ni2 O6B 2.067(2) . ?
Ni2 O9A 2.068(2) . ?
Ni2 N1B 2.111(3) . ?
Ni2 N5A 2.112(3) . ?
Ni2 N3C 2.125(3) . ?
Ni2 N6C 2.129(4) . ?
N1A C6A 1.310(4) . ?
N1A C2A 1.327(5) . ?
C2A C3A 1.403(6) . ?
C3A C4A 1.369(6) . ?
C4A N5A 1.341(5) . ?
N5A C6A 1.341(4) . ?
C6A C7A 1.514(5) . ?
C7A O8A 1.232(4) . ?
C7A O9A 1.240(4) . ?
N1B C4B 1.332(3) . ?
N1B C2B 1.353(4) . ?
C2B C3B 1.357(5) . ?
C3B C2B 1.357(5) 6_565 ?
C4B N1B 1.332(3) 6_565 ?
C4B C5B 1.525(6) . ?
C5B O6B 1.236(3) . ?
C5B O6B 1.236(3) 6_565 ?
C1C N3C 1.460(6) . ?
C2C N3C 1.526(7) . ?
N3C C4C 1.518(8) . ?
C4C C5C 1.413(8) . ?
C5C N6C 1.492(7) . ?
N6C C7C 1.469(7) . ?
N6C C8C 1.482(5) . ?
C1D N3D 1.466(6) . ?
C2D N3D 1.499(5) . ?
N3D C4D 1.492(6) . ?
C4D C4D 1.398(12) 2 ?
B1E F3E 1.217(7) 6_565 ?
B1E F3E 1.217(7) 2 ?
B1E F3E 1.217(7) 5_565 ?
B1E F3E 1.217(7) . ?
B1E F2E 1.481(11) 5_565 ?
B1E F2E 1.481(11) . ?
F3E F3E 1.71(2) 6_565 ?
F3E F3E 1.734(17) 2 ?

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
O8A Ni1 O8A 168.83(12) . 2 ?
O8A Ni1 N3D 90.77(11) . . ?
O8A Ni1 N3D 97.48(11) 2 . ?
O8A Ni1 N3D 97.48(11) . 2 ?
O8A Ni1 N3D 90.77(11) 2 2 ?
N3D Ni1 N3D 85.0(2) . 2 ?
O8A Ni1 N1A 78.57(9) . . ?
O8A Ni1 N1A 93.43(10) 2 . ?
N3D Ni1 N1A 169.04(11) . . ?
N3D Ni1 N1A 93.86(12) 2 . ?
O8A Ni1 N1A 93.43(10) . 2 ?
O8A Ni1 N1A 78.57(9) 2 2 ?
N3D Ni1 N1A 93.86(12) . 2 ?
N3D Ni1 N1A 169.04(11) 2 2 ?
N1A Ni1 N1A 89.33(14) . 2 ?
O6B Ni2 O9A 169.04(9) . . ?
O6B Ni2 N1B 79.07(10) . . ?
O9A Ni2 N1B 93.27(10) . . ?
O6B Ni2 N5A 92.97(10) . . ?
O9A Ni2 N5A 78.98(10) . . ?
N1B Ni2 N5A 89.24(11) . . ?
O6B Ni2 N3C 91.81(11) . . ?
O9A Ni2 N3C 96.11(12) . . ?
N1B Ni2 N3C 170.54(12) . . ?
N5A Ni2 N3C 93.78(14) . . ?
O6B Ni2 N6C 97.32(12) . . ?
O9A Ni2 N6C 90.93(12) . . ?
N1B Ni2 N6C 93.59(13) . . ?
N5A Ni2 N6C 169.67(12) . . ?
N3C Ni2 N6C 85.02(16) . . ?
C6A N1A C2A 117.8(3) . . ?
C6A N1A Ni1 110.7(2) . . ?
C2A N1A Ni1 131.5(2) . . ?
N1A C2A C3A 120.7(4) . . ?
C4A C3A C2A 117.6(4) . . ?
N5A C4A C3A 121.3(3) . . ?
C6A N5A C4A 116.7(3) . . ?
C6A N5A Ni2 111.5(2) . . ?
C4A N5A Ni2 131.9(2) . . ?
N1A C6A N5A 126.0(3) . . ?
N1A C6A C7A 117.6(3) . . ?
N5A C6A C7A 116.4(3) . . ?
O8A C7A O9A 128.0(3) . . ?
O8A C7A C6A 115.8(3) . . ?
O9A C7A C6A 116.1(3) . . ?
C7A O8A Ni1 117.3(2) . . ?
C7A O9A Ni2 117.0(2) . . ?
C4B N1B C2B 115.5(3) . . ?
C4B N1B Ni2 111.7(2) . . ?
C2B N1B Ni2 132.9(2) . . ?
N1B C2B C3B 120.7(3) . . ?
C2B C3B C2B 120.1(5) 6_565 . ?
N1B C4B N1B 127.5(4) 6_565 . ?
N1B C4B C5B 116.2(2) 6_565 . ?
N1B C4B C5B 116.2(2) . . ?
O6B C5B O6B 127.7(4) . 6_565 ?
O6B C5B C4B 116.1(2) . . ?
O6B C5B C4B 116.1(2) 6_565 . ?
C5B O6B Ni2 116.9(2) . . ?
C1C N3C C4C 110.7(5) . . ?
C1C N3C C2C 106.9(5) . . ?
C4C N3C C2C 109.0(4) . . ?
C1C N3C Ni2 113.5(3) . . ?
C4C N3C Ni2 102.7(4) . . ?
C2C N3C Ni2 114.0(3) . . ?
C5C C4C N3C 112.1(4) . . ?
C4C C5C N6C 110.5(5) . . ?
C7C N6C C8C 104.5(4) . . ?
C7C N6C C5C 108.8(4) . . ?
C8C N6C C5C 112.3(4) . . ?
C7C N6C Ni2 114.2(3) . . ?
C8C N6C Ni2 113.9(3) . . ?
C5C N6C Ni2 103.3(3) . . ?
C1D N3D C4D 108.4(4) . . ?
C1D N3D C2D 109.0(4) . . ?
C4D N3D C2D 110.6(4) . . ?
C1D N3D Ni1 113.6(3) . . ?
C4D N3D Ni1 102.1(3) . . ?
C2D N3D Ni1 113.0(3) . . ?
C4D C4D N3D 111.7(5) 2 . ?
F3E B1E F3E 180.0(7) 6_565 2 ?
F3E B1E F3E 90.9(11) 6_565 5_565 ?
F3E B1E F3E 89.1(11) 2 5_565 ?
F3E B1E F3E 89.1(11) 6_565 . ?
F3E B1E F3E 90.9(11) 2 . ?
F3E B1E F3E 180.0(7) 5_565 . ?
F3E B1E F2E 84.9(5) 6_565 5_565 ?
F3E B1E F2E 95.1(5) 2 5_565 ?
F3E B1E F2E 95.1(5) 5_565 5_565 ?
F3E B1E F2E 84.9(5) . 5_565 ?
F3E B1E F2E 95.1(5) 6_565 . ?
F3E B1E F2E 84.9(5) 2 . ?
F3E B1E F2E 84.9(5) 5_565 . ?
F3E B1E F2E 95.1(5) . . ?
F2E B1E F2E 180.0(7) 5_565 . ?
B1E F3E F3E 45.4(5) . 6_565 ?
B1E F3E F3E 44.6(5) . 2 ?
F3E F3E F3E 90.000(9) 6_565 2 ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        28.18
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.072

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.159 -0.032 -0.045 2214 745 ' '
_platon_squeeze_details          
;
;

data_h127s
_database_code_depnum_ccdc_archive 'CCDC 725442'

_audit_creation_date             2008-12-02T13:40:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C39 H75 Cl Cu4 N14 O7, 4(Cl O4), 4.5(H2 O)'
_chemical_formula_sum            'C39 H84 Cl5 Cu4 N14 O27.50'
_chemical_formula_weight         1620.61
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   43.2705(9)
_cell_length_b                   7.95110(10)
_cell_length_c                   20.8778(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.6400(10)
_cell_angle_gamma                90
_cell_volume                     6528.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    15718
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      28.283
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       bar
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3348
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_T_max  0.753

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.053
_diffrn_reflns_number            23679
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             6377
_reflns_number_gt                5016
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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)+(0.0542P)²+23.8481P] 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_number_reflns         6377
_refine_ls_number_parameters     472
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.047
_refine_ls_wR_factor_ref         0.1218
_refine_ls_wR_factor_gt          0.1133
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.093

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Cu1 Cu 0.830769(11) 0.18863(5) 0.68578(2) 0.02218(13) Uani 1 1 d U E .
Cu2 Cu 0.935662(11) -0.09498(5) 0.63323(2) 0.01937(13) Uani 1 1 d . . .
Cl1 Cl 0.7949(2) -0.0315(12) 0.6044(6) 0.0386(13) Uani 0.5 1 d P . .
O1 O 0.85537(7) 0.2215(4) 0.62641(15) 0.0340(7) Uani 1 1 d . . .
O2 O 0.89883(6) 0.1280(3) 0.60459(13) 0.0253(6) Uani 1 1 d . . .
O3 O 0.7956(7) -0.009(3) 0.6184(14) 0.035(4) Uani 0.5 1 d PU . .
O4 O 0.97532(6) -0.2819(3) 0.70165(13) 0.0245(6) Uani 1 1 d . . .
O13A O 0.7232(2) -0.1643(14) 0.5897(6) 0.044(3) Uani 0.503(5) 1 d P . .
O14A O 0.7907(2) -0.0780(11) 0.4527(4) 0.047(2) Uani 0.497(5) 1 d P . .
Cl2 Cl 0.93825(3) 0.33546(13) 0.82949(6) 0.0363(3) Uani 1 1 d . A 2
Cl3 Cl 0.83399(3) 0.29364(12) 0.40535(5) 0.0393(3) Uani 1 1 d D B 2
O5 O 0.92184(10) 0.3626(5) 0.75536(18) 0.0580(10) Uani 1 1 d . A 2
O6 O 0.91586(13) 0.3672(6) 0.8612(3) 0.0963(18) Uani 1 1 d . A 2
O7 O 0.95059(9) 0.1669(4) 0.84290(19) 0.0562(9) Uani 1 1 d . A 2
O8 O 0.96612(12) 0.4489(5) 0.8562(2) 0.0824(13) Uani 1 1 d . A 2
O9 O 0.84014(11) 0.1217(4) 0.4262(2) 0.0635(11) Uani 1 1 d D B 2
O10A O 0.8247(3) 0.3825(11) 0.4534(4) 0.056(3) Uiso 0.492(11) 1 d PD B 2
O10B O 0.8363(3) 0.4161(11) 0.4569(4) 0.064(3) Uiso 0.508(11) 1 d PD B 2
O11A O 0.8182(2) 0.3159(11) 0.3338(4) 0.071(3) Uiso 0.492(11) 1 d PD B 2
O11B O 0.7993(2) 0.3099(9) 0.3462(4) 0.061(3) Uiso 0.508(11) 1 d PD B 2
O12A O 0.8690(2) 0.3540(12) 0.4178(6) 0.080(3) Uiso 0.492(11) 1 d PD B 2
O12B O 0.8540(3) 0.3460(12) 0.3722(6) 0.078(3) Uiso 0.508(11) 1 d P B 2
O16 O 1.0206(4) 0.460(2) 0.9923(11) 0.088(6) Uani 0.25 1 d P C 2
O13B O 0.7339(3) -0.1134(15) 0.6045(7) 0.048(3) Uani 0.503(5) 1 d P D 1
O14B O 0.7949(2) -0.0363(11) 0.4869(4) 0.045(2) Uani 0.497(5) 1 d P D 1
N1 N 0.87020(8) 0.0136(4) 0.73445(16) 0.0235(7) Uani 1 1 d . . .
N3 N 0.91331(7) -0.1086(4) 0.70708(16) 0.0216(7) Uani 1 1 d . . .
N4 N 0.80669(10) 0.4080(5) 0.6462(2) 0.0395(9) Uani 1 1 d . . .
N5 N 0.80949(9) 0.2043(4) 0.75598(18) 0.0334(8) Uani 1 1 d . . .
N6 N 0.97301(7) 0.0564(3) 0.70192(16) 0.0200(6) Uani 1 1 d . . .
N7 N 0.94993(8) -0.0447(4) 0.55126(17) 0.0294(7) Uani 1 1 d . . .
N8 N 0.90362(8) -0.2741(4) 0.56855(16) 0.0247(7) Uani 1 1 d . . .
C2 C 0.88879(9) 0.0035(4) 0.69752(19) 0.0213(7) Uani 1 1 d . . .
C4 C 0.92057(9) -0.2181(5) 0.7605(2) 0.0246(8) Uani 1 1 d . . .
H4 H 0.938 -0.2994 0.7693 0.03 Uiso 1 1 calc R . .
C5 C 0.90311(10) -0.2142(5) 0.8025(2) 0.0291(9) Uani 1 1 d . . .
H5 H 0.9084 -0.2903 0.8407 0.035 Uiso 1 1 calc R . .
C6 C 0.87774(10) -0.0967(5) 0.7874(2) 0.0291(9) Uani 1 1 d . . .
H6 H 0.8652 -0.0935 0.8154 0.035 Uiso 1 1 calc R . .
C7 C 0.88054(9) 0.1282(5) 0.63701(19) 0.0232(8) Uani 1 1 d . . .
C11 C 0.78680(16) 0.3984(8) 0.5703(3) 0.0749(19) Uani 1 1 d . E .
H111 H 0.7764 0.5081 0.5527 0.112 Uiso 1 1 calc R . .
H112 H 0.7689 0.3136 0.5598 0.112 Uiso 1 1 calc R . .
H113 H 0.8017 0.3672 0.5474 0.112 Uiso 1 1 calc R . .
C12 C 0.79146(12) 0.0502(7) 0.7608(2) 0.0446(12) Uani 1 1 d . E .
H12A H 0.8069 -0.0463 0.7709 0.067 Uiso 1 1 calc R . .
H12B H 0.7717 0.0319 0.716 0.067 Uiso 1 1 calc R . .
H12C H 0.7839 0.0629 0.7987 0.067 Uiso 1 1 calc R . .
C13 C 0.83555(13) 0.2466(7) 0.8280(3) 0.0497(12) Uani 1 1 d . E .
H13A H 0.8242 0.2741 0.8586 0.075 Uiso 1 1 calc R . .
H13B H 0.8489 0.3435 0.8252 0.075 Uiso 1 1 calc R . .
H14C H 0.8506 0.15 0.8475 0.075 Uiso 1 1 calc R . .
C14 C 1 -0.0211(6) 0.75 0.0182(10) Uani 1 2 d S . .
C15 C 1 0.3157(6) 0.75 0.0276(12) Uani 1 2 d S . .
H15 H 1 0.4352 0.75 0.033 Uiso 1 2 calc SR . .
C16 C 0.97287(10) 0.2263(4) 0.7032(2) 0.0258(8) Uani 1 1 d . . .
H16 H 0.9536 0.2852 0.6709 0.031 Uiso 1 1 calc R . .
C17 C 1 -0.2144(6) 0.75 0.0188(10) Uani 1 2 d S . .
C18 C 0.92159(12) -0.1172(6) 0.4886(2) 0.0400(11) Uani 1 1 d . . .
H18A H 0.9284 -0.1267 0.449 0.048 Uiso 1 1 calc R . .
H18B H 0.9014 -0.0428 0.4737 0.048 Uiso 1 1 calc R . .
C19 C 0.91288(12) -0.2896(5) 0.5074(2) 0.0374(10) Uani 1 1 d . . .
H19A H 0.8936 -0.338 0.4665 0.045 Uiso 1 1 calc R . .
H19B H 0.9326 -0.3657 0.5197 0.045 Uiso 1 1 calc R . .
C20 C 0.98290(11) -0.1257(6) 0.5647(3) 0.0424(11) Uani 1 1 d . . .
H20A H 0.9821 -0.2444 0.5765 0.064 Uiso 1 1 calc R . .
H20B H 1.0011 -0.069 0.6041 0.064 Uiso 1 1 calc R . .
H20C H 0.9873 -0.1173 0.5224 0.064 Uiso 1 1 calc R . .
C21 C 0.95212(12) 0.1360(5) 0.5358(2) 0.0395(10) Uani 1 1 d . . .
H21A H 0.9714 0.1876 0.5749 0.059 Uiso 1 1 calc R . .
H21B H 0.931 0.193 0.5301 0.059 Uiso 1 1 calc R . .
H21C H 0.9554 0.1469 0.4923 0.059 Uiso 1 1 calc R . .
C22 C 0.86744(9) -0.2237(5) 0.5423(2) 0.0305(9) Uani 1 1 d . . .
H22A H 0.8531 -0.3106 0.5104 0.046 Uiso 1 1 calc R . .
H22B H 0.864 -0.1168 0.5169 0.046 Uiso 1 1 calc R . .
H22C H 0.8613 -0.2105 0.5822 0.046 Uiso 1 1 calc R . .
C23 C 0.90805(11) -0.4409(5) 0.6034(2) 0.0353(10) Uani 1 1 d . . .
H23A H 0.902 -0.4326 0.6436 0.053 Uiso 1 1 calc R . .
H23B H 0.9318 -0.4767 0.6199 0.053 Uiso 1 1 calc R . .
H23C H 0.8933 -0.5234 0.5697 0.053 Uiso 1 1 calc R . .
C8A C 0.7923(3) 0.4750(8) 0.6945(6) 0.046(3) Uani 0.549(19) 1 d PR E 1
H8A1 H 0.8098 0.5353 0.7347 0.055 Uiso 0.549(19) 1 calc PR E 1
H8A2 H 0.7731 0.5526 0.6693 0.055 Uiso 0.549(19) 1 calc PR E 1
C9A C 0.7805(5) 0.323(3) 0.7186(9) 0.052(5) Uani 0.549(19) 1 d PU E 1
H9A1 H 0.7629 0.2655 0.6776 0.062 Uiso 0.549(19) 1 calc PR E 1
H9A2 H 0.7701 0.3564 0.7509 0.062 Uiso 0.549(19) 1 calc PR E 1
C10A C 0.8352(5) 0.541(2) 0.6518(14) 0.084(6) Uani 0.549(19) 1 d P E 1
H101 H 0.8248 0.6529 0.6382 0.125 Uiso 0.549(19) 1 calc PR E 1
H102 H 0.8457 0.5084 0.6202 0.125 Uiso 0.549(19) 1 calc PR E 1
H103 H 0.8526 0.5453 0.7004 0.125 Uiso 0.549(19) 1 calc PR E 1
C8B C 0.7759(3) 0.400(2) 0.6665(7) 0.039(4) Uani 0.451(19) 1 d P E 2
H8B1 H 0.7636 0.5091 0.6555 0.047 Uiso 0.451(19) 1 calc PR E 2
H8B2 H 0.7599 0.3113 0.6389 0.047 Uiso 0.451(19) 1 calc PR E 2
C9B C 0.7882(6) 0.364(3) 0.7430(10) 0.044(5) Uani 0.451(19) 1 d P E 2
H9B1 H 0.7688 0.3466 0.7557 0.053 Uiso 0.451(19) 1 calc PR E 2
H9B2 H 0.8021 0.4585 0.7713 0.053 Uiso 0.451(19) 1 calc PR E 2
C10B C 0.8262(6) 0.547(3) 0.6698(13) 0.063(5) Uani 0.451(19) 1 d P E 2
H104 H 0.8449 0.543 0.655 0.094 Uiso 0.451(19) 1 calc PR E 2
H105 H 0.8355 0.5506 0.7214 0.094 Uiso 0.451(19) 1 calc PR E 2
H106 H 0.8124 0.6472 0.6502 0.094 Uiso 0.451(19) 1 calc PR E 2


#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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

Cu1 O1 1.959(3) . ?
Cu1 N4 2.023(3) . ?
Cu1 N5 2.034(3) . ?
Cu1 N1 2.106(3) . ?
Cu1 O3 2.233(18) . ?
Cu1 Cl1 2.482(6) . ?
Cu2 N6 2.046(3) . ?
Cu2 N8 2.052(3) . ?
Cu2 N7 2.086(3) . ?
Cu2 N3 2.137(3) . ?
Cu2 O4 2.270(2) . ?
Cu2 O2 2.290(2) . ?
O1 C7 1.259(4) . ?
O2 C7 1.238(4) . ?
O4 C17 1.245(3) . ?
Cl2 O6 1.405(4) . ?
Cl2 O8 1.421(4) . ?
Cl2 O5 1.425(3) . ?
Cl2 O7 1.427(3) . ?
Cl3 O11A 1.370(8) . ?
Cl3 O12B 1.379(9) . ?
Cl3 O10A 1.414(8) . ?
Cl3 O10B 1.424(8) . ?
Cl3 O9 1.425(3) . ?
Cl3 O11B 1.499(7) . ?
Cl3 O12A 1.505(9) . ?
N1 C2 1.328(5) . ?
N1 C6 1.341(5) . ?
N3 C2 1.335(5) . ?
N3 C4 1.344(5) . ?
N4 C10B 1.35(2) . ?
N4 C11 1.456(7) . ?
N4 C8A 1.488(6) . ?
N4 C8B 1.560(11) . ?
N4 C10A 1.593(17) . ?
N5 C12 1.478(6) . ?
N5 C13 1.494(6) . ?
N5 C9A 1.50(2) . ?
N5 C9B 1.527(19) . ?
N6 C14 1.332(4) . ?
N6 C16 1.352(4) . ?
N7 C20 1.482(5) . ?
N7 C21 1.484(5) . ?
N7 C18 1.487(6) . ?
N8 C22 1.482(5) . ?
N8 C23 1.487(5) . ?
N8 C19 1.494(5) . ?
C2 C7 1.527(5) . ?
C4 C5 1.377(5) . ?
C4 H4 0.95 . ?
C5 C6 1.374(5) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C11 H111 0.98 . ?
C11 H112 0.98 . ?
C11 H113 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H14C 0.98 . ?
C14 N6 1.332(4) 2_756 ?
C14 C17 1.537(6) . ?
C15 C16 1.372(5) . ?
C15 C16 1.372(5) 2_756 ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C17 O4 1.245(3) 2_756 ?
C18 C19 1.516(6) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C8A C9A 1.48(2) . ?
C8A H8A1 0.99 . ?
C8A H8A2 0.99 . ?
C9A H9A1 0.99 . ?
C9A H9A2 0.99 . ?
C10A H101 0.98 . ?
C10A H102 0.98 . ?
C10A H103 0.98 . ?
C8B C9B 1.48(2) . ?
C8B H8B1 0.99 . ?
C8B H8B2 0.99 . ?
C9B H9B1 0.99 . ?
C9B H9B2 0.99 . ?
C10B H104 0.98 . ?
C10B H105 0.98 . ?
C10B H106 0.98 . ?
Cl1 O13A 3.171(13) . ?
Cl1 O14A 3.118(14) . ?
O3 O13B 2.69(3) . ?
O3 O14B 2.74(3) . ?

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 Cu1 N4 87.13(13) . . ?
O1 Cu1 N5 167.53(14) . . ?
N4 Cu1 N5 86.02(14) . . ?
O1 Cu1 N1 81.30(11) . . ?
N4 Cu1 N1 160.48(14) . . ?
N5 Cu1 N1 102.23(12) . . ?
O1 Cu1 O3 95.9(7) . . ?
N4 Cu1 O3 104.5(8) . . ?
N5 Cu1 O3 95.9(7) . . ?
N1 Cu1 O3 92.4(8) . . ?
O1 Cu1 Cl1 90.6(3) . . ?
N4 Cu1 Cl1 105.1(3) . . ?
N5 Cu1 Cl1 101.2(3) . . ?
N1 Cu1 Cl1 90.8(3) . . ?
O3 Cu1 Cl1 5.4(9) . . ?
N6 Cu2 N8 171.50(12) . . ?
N6 Cu2 N7 92.57(12) . . ?
N8 Cu2 N7 86.74(13) . . ?
N6 Cu2 N3 89.25(11) . . ?
N8 Cu2 N3 93.14(12) . . ?
N7 Cu2 N3 168.33(12) . . ?
N6 Cu2 O4 77.00(10) . . ?
N8 Cu2 O4 94.92(11) . . ?
N7 Cu2 O4 103.72(11) . . ?
N3 Cu2 O4 87.92(10) . . ?
N6 Cu2 O2 89.31(10) . . ?
N8 Cu2 O2 99.19(11) . . ?
N7 Cu2 O2 92.82(11) . . ?
N3 Cu2 O2 75.67(10) . . ?
O4 Cu2 O2 158.82(9) . . ?
C7 O1 Cu1 118.0(2) . . ?
C7 O2 Cu2 113.1(2) . . ?
C17 O4 Cu2 113.3(2) . . ?
O6 Cl2 O8 109.9(3) . . ?
O6 Cl2 O5 110.8(3) . . ?
O8 Cl2 O5 106.7(3) . . ?
O6 Cl2 O7 110.6(2) . . ?
O8 Cl2 O7 109.4(3) . . ?
O5 Cl2 O7 109.4(2) . . ?
O11A Cl3 O10A 123.3(5) . . ?
O12B Cl3 O10B 108.2(6) . . ?
O11A Cl3 O9 113.7(4) . . ?
O12B Cl3 O9 111.5(4) . . ?
O10A Cl3 O9 109.6(4) . . ?
O10B Cl3 O9 118.7(4) . . ?
O12B Cl3 O11B 100.5(5) . . ?
O10B Cl3 O11B 107.1(5) . . ?
O9 Cl3 O11B 109.2(3) . . ?
O11A Cl3 O12A 98.9(6) . . ?
O10A Cl3 O12A 106.3(6) . . ?
O9 Cl3 O12A 101.9(4) . . ?
C2 N1 C6 116.2(3) . . ?
C2 N1 Cu1 108.9(2) . . ?
C6 N1 Cu1 134.4(3) . . ?
C2 N3 C4 116.9(3) . . ?
C2 N3 Cu2 115.4(2) . . ?
C4 N3 Cu2 127.7(2) . . ?
C10B N4 C11 115.8(11) . . ?
C11 N4 C8A 122.1(6) . . ?
C10B N4 C8B 114.0(9) . . ?
C11 N4 C8B 96.3(7) . . ?
C11 N4 C10A 101.7(10) . . ?
C8A N4 C10A 104.0(8) . . ?
C10B N4 Cu1 114.7(9) . . ?
C11 N4 Cu1 111.7(3) . . ?
C8A N4 Cu1 108.8(3) . . ?
C8B N4 Cu1 102.0(5) . . ?
C10A N4 Cu1 107.1(7) . . ?
C12 N5 C13 108.4(3) . . ?
C12 N5 C9A 101.8(9) . . ?
C13 N5 C9A 119.8(8) . . ?
C12 N5 C9B 113.9(11) . . ?
C13 N5 C9B 97.9(9) . . ?
C12 N5 Cu1 114.1(3) . . ?
C13 N5 Cu1 111.2(3) . . ?
C9A N5 Cu1 101.3(7) . . ?
C9B N5 Cu1 110.1(8) . . ?
C14 N6 C16 117.2(3) . . ?
C14 N6 Cu2 116.4(2) . . ?
C16 N6 Cu2 126.4(3) . . ?
C20 N7 C21 108.6(3) . . ?
C20 N7 C18 112.0(3) . . ?
C21 N7 C18 106.7(3) . . ?
C20 N7 Cu2 110.6(3) . . ?
C21 N7 Cu2 115.6(2) . . ?
C18 N7 Cu2 103.3(2) . . ?
C22 N8 C23 108.8(3) . . ?
C22 N8 C19 109.0(3) . . ?
C23 N8 C19 108.6(3) . . ?
C22 N8 Cu2 112.1(2) . . ?
C23 N8 Cu2 112.5(2) . . ?
C19 N8 Cu2 105.7(2) . . ?
N1 C2 N3 126.1(3) . . ?
N1 C2 C7 116.9(3) . . ?
N3 C2 C7 117.0(3) . . ?
N3 C4 C5 120.9(3) . . ?
N3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 117.9(3) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
N1 C6 C5 122.0(4) . . ?
N1 C6 H6 119 . . ?
C5 C6 H6 119 . . ?
O2 C7 O1 127.5(3) . . ?
O2 C7 C2 118.0(3) . . ?
O1 C7 C2 114.5(3) . . ?
N4 C11 H111 109.5 . . ?
N4 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
N4 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N5 C13 H14C 109.5 . . ?
H13A C13 H14C 109.5 . . ?
H13B C13 H14C 109.5 . . ?
N6 C14 N6 124.9(4) 2_756 . ?
N6 C14 C17 117.6(2) 2_756 . ?
N6 C14 C17 117.6(2) . . ?
C16 C15 C16 117.6(5) . 2_756 ?
C16 C15 H15 121.2 . . ?
C16 C15 H15 121.2 2_756 . ?
N6 C16 C15 121.5(4) . . ?
N6 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
O4 C17 O4 128.9(4) 2_756 . ?
O4 C17 C14 115.6(2) 2_756 . ?
O4 C17 C14 115.6(2) . . ?
N7 C18 C19 109.0(4) . . ?
N7 C18 H18A 109.9 . . ?
C19 C18 H18A 109.9 . . ?
N7 C18 H18B 109.9 . . ?
C19 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
N8 C19 C18 109.3(3) . . ?
N8 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
N8 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
N7 C20 H20A 109.5 . . ?
N7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N7 C21 H21A 109.5 . . ?
N7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C22 H22A 109.5 . . ?
N8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N8 C23 H23A 109.5 . . ?
N8 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N8 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C9A C8A N4 103.9(9) . . ?
C9A C8A H8A1 111 . . ?
N4 C8A H8A1 111 . . ?
C9A C8A H8A2 111 . . ?
N4 C8A H8A2 111 . . ?
H8A1 C8A H8A2 109 . . ?
C8A C9A N5 110.9(14) . . ?
C8A C9A H9A1 109.5 . . ?
N5 C9A H9A1 109.5 . . ?
C8A C9A H9A2 109.5 . . ?
N5 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 108 . . ?
N4 C10A H101 109.5 . . ?
N4 C10A H102 109.5 . . ?
N4 C10A H103 109.5 . . ?
C9B C8B N4 109.6(13) . . ?
C9B C8B H8B1 109.7 . . ?
N4 C8B H8B1 109.7 . . ?
C9B C8B H8B2 109.7 . . ?
N4 C8B H8B2 109.7 . . ?
H8B1 C8B H8B2 108.2 . . ?
C8B C9B N5 105.8(13) . . ?
C8B C9B H9B1 110.6 . . ?
N5 C9B H9B1 110.6 . . ?
C8B C9B H9B2 110.6 . . ?
N5 C9B H9B2 110.6 . . ?
H9B1 C9B H9B2 108.7 . . ?
N4 C10B H104 109.5 . . ?
N4 C10B H105 109.5 . . ?
H104 C10B H105 109.5 . . ?
N4 C10B H106 109.5 . . ?
H104 C10B H106 109.5 . . ?
H105 C10B H106 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Cu1 O1 C7 168.3(3) . . . . ?
N5 Cu1 O1 C7 111.6(6) . . . . ?
N1 Cu1 O1 C7 4.1(3) . . . . ?
O3 Cu1 O1 C7 -87.4(9) . . . . ?
Cl1 Cu1 O1 C7 -86.6(4) . . . . ?
N6 Cu2 O2 C7 -97.5(3) . . . . ?
N8 Cu2 O2 C7 82.9(3) . . . . ?
N7 Cu2 O2 C7 170.0(3) . . . . ?
N3 Cu2 O2 C7 -8.1(3) . . . . ?
O4 Cu2 O2 C7 -48.3(4) . . . . ?
N6 Cu2 O4 C17 3.18(17) . . . . ?
N8 Cu2 O4 C17 -179.50(18) . . . . ?
N7 Cu2 O4 C17 92.66(19) . . . . ?
N3 Cu2 O4 C17 -86.52(18) . . . . ?
O2 Cu2 O4 C17 -47.7(4) . . . . ?
O1 Cu1 N1 C2 -5.8(2) . . . . ?
N4 Cu1 N1 C2 -60.1(5) . . . . ?
N5 Cu1 N1 C2 -173.6(2) . . . . ?
O3 Cu1 N1 C2 89.8(8) . . . . ?
Cl1 Cu1 N1 C2 84.7(4) . . . . ?
O1 Cu1 N1 C6 -177.4(4) . . . . ?
N4 Cu1 N1 C6 128.3(5) . . . . ?
N5 Cu1 N1 C6 14.8(4) . . . . ?
O3 Cu1 N1 C6 -81.8(8) . . . . ?
Cl1 Cu1 N1 C6 -86.9(5) . . . . ?
N6 Cu2 N3 C2 94.1(3) . . . . ?
N8 Cu2 N3 C2 -94.1(3) . . . . ?
N7 Cu2 N3 C2 -5.0(7) . . . . ?
O4 Cu2 N3 C2 171.1(3) . . . . ?
O2 Cu2 N3 C2 4.6(2) . . . . ?
N6 Cu2 N3 C4 -87.5(3) . . . . ?
N8 Cu2 N3 C4 84.4(3) . . . . ?
N7 Cu2 N3 C4 173.5(5) . . . . ?
O4 Cu2 N3 C4 -10.4(3) . . . . ?
O2 Cu2 N3 C4 -176.9(3) . . . . ?
O1 Cu1 N4 C10B -72.1(11) . . . . ?
N5 Cu1 N4 C10B 97.5(11) . . . . ?
N1 Cu1 N4 C10B -18.6(12) . . . . ?
O3 Cu1 N4 C10B -167.5(13) . . . . ?
Cl1 Cu1 N4 C10B -162.0(11) . . . . ?
O1 Cu1 N4 C11 62.2(4) . . . . ?
N5 Cu1 N4 C11 -128.2(4) . . . . ?
N1 Cu1 N4 C11 115.8(5) . . . . ?
O3 Cu1 N4 C11 -33.1(8) . . . . ?
Cl1 Cu1 N4 C11 -27.6(5) . . . . ?
O1 Cu1 N4 C8A -160.1(6) . . . . ?
N5 Cu1 N4 C8A 9.5(6) . . . . ?
N1 Cu1 N4 C8A -106.6(7) . . . . ?
O3 Cu1 N4 C8A 104.5(10) . . . . ?
Cl1 Cu1 N4 C8A 110.1(7) . . . . ?
O1 Cu1 N4 C8B 164.1(7) . . . . ?
N5 Cu1 N4 C8B -26.3(7) . . . . ?
N1 Cu1 N4 C8B -142.4(8) . . . . ?
O3 Cu1 N4 C8B 68.7(10) . . . . ?
Cl1 Cu1 N4 C8B 74.2(8) . . . . ?
O1 Cu1 N4 C10A -48.3(10) . . . . ?
N5 Cu1 N4 C10A 121.3(10) . . . . ?
N1 Cu1 N4 C10A 5.2(11) . . . . ?
O3 Cu1 N4 C10A -143.6(12) . . . . ?
Cl1 Cu1 N4 C10A -138.1(10) . . . . ?
O1 Cu1 N5 C12 -174.1(5) . . . . ?
N4 Cu1 N5 C12 129.1(3) . . . . ?
N1 Cu1 N5 C12 -68.8(3) . . . . ?
O3 Cu1 N5 C12 24.9(9) . . . . ?
Cl1 Cu1 N5 C12 24.5(4) . . . . ?
O1 Cu1 N5 C13 -51.1(7) . . . . ?
N4 Cu1 N5 C13 -107.9(3) . . . . ?
N1 Cu1 N5 C13 54.2(3) . . . . ?
O3 Cu1 N5 C13 147.9(9) . . . . ?
Cl1 Cu1 N5 C13 147.5(4) . . . . ?
O1 Cu1 N5 C9A 77.3(10) . . . . ?
N4 Cu1 N5 C9A 20.5(9) . . . . ?
N1 Cu1 N5 C9A -177.4(9) . . . . ?
O3 Cu1 N5 C9A -83.7(12) . . . . ?
Cl1 Cu1 N5 C9A -84.1(9) . . . . ?
O1 Cu1 N5 C9B 56.4(12) . . . . ?
N4 Cu1 N5 C9B -0.5(10) . . . . ?
N1 Cu1 N5 C9B 161.6(10) . . . . ?
O3 Cu1 N5 C9B -104.6(13) . . . . ?
Cl1 Cu1 N5 C9B -105.1(11) . . . . ?
N8 Cu2 N6 C14 -19.2(9) . . . . ?
N7 Cu2 N6 C14 -104.3(2) . . . . ?
N3 Cu2 N6 C14 87.25(19) . . . . ?
O4 Cu2 N6 C14 -0.79(17) . . . . ?
O2 Cu2 N6 C14 162.93(19) . . . . ?
N8 Cu2 N6 C16 160.9(7) . . . . ?
N7 Cu2 N6 C16 75.8(3) . . . . ?
N3 Cu2 N6 C16 -92.7(3) . . . . ?
O4 Cu2 N6 C16 179.3(3) . . . . ?
O2 Cu2 N6 C16 -17.0(3) . . . . ?
N6 Cu2 N7 C20 70.7(3) . . . . ?
N8 Cu2 N7 C20 -100.9(3) . . . . ?
N3 Cu2 N7 C20 169.4(5) . . . . ?
O4 Cu2 N7 C20 -6.6(3) . . . . ?
O2 Cu2 N7 C20 160.1(3) . . . . ?
N6 Cu2 N7 C21 -53.2(3) . . . . ?
N8 Cu2 N7 C21 135.3(3) . . . . ?
N3 Cu2 N7 C21 45.5(8) . . . . ?
O4 Cu2 N7 C21 -130.4(3) . . . . ?
O2 Cu2 N7 C21 36.2(3) . . . . ?
N6 Cu2 N7 C18 -169.4(3) . . . . ?
N8 Cu2 N7 C18 19.1(3) . . . . ?
N3 Cu2 N7 C18 -70.6(7) . . . . ?
O4 Cu2 N7 C18 113.4(3) . . . . ?
O2 Cu2 N7 C18 -79.9(3) . . . . ?
N6 Cu2 N8 C22 165.9(7) . . . . ?
N7 Cu2 N8 C22 -108.6(3) . . . . ?
N3 Cu2 N8 C22 59.7(3) . . . . ?
O4 Cu2 N8 C22 147.9(2) . . . . ?
O2 Cu2 N8 C22 -16.2(3) . . . . ?
N6 Cu2 N8 C23 42.9(9) . . . . ?
N7 Cu2 N8 C23 128.4(3) . . . . ?
N3 Cu2 N8 C23 -63.3(3) . . . . ?
O4 Cu2 N8 C23 24.9(3) . . . . ?
O2 Cu2 N8 C23 -139.3(2) . . . . ?
N6 Cu2 N8 C19 -75.5(9) . . . . ?
N7 Cu2 N8 C19 10.0(2) . . . . ?
N3 Cu2 N8 C19 178.3(2) . . . . ?
O4 Cu2 N8 C19 -93.5(2) . . . . ?
O2 Cu2 N8 C19 102.3(2) . . . . ?
C6 N1 C2 N3 2.1(5) . . . . ?
Cu1 N1 C2 N3 -171.2(3) . . . . ?
C6 N1 C2 C7 -180.0(3) . . . . ?
Cu1 N1 C2 C7 6.7(4) . . . . ?
C4 N3 C2 N1 -2.2(5) . . . . ?
Cu2 N3 C2 N1 176.5(3) . . . . ?
C4 N3 C2 C7 179.9(3) . . . . ?
Cu2 N3 C2 C7 -1.4(4) . . . . ?
C2 N3 C4 C5 0.5(5) . . . . ?
Cu2 N3 C4 C5 -178.0(3) . . . . ?
N3 C4 C5 C6 1.0(6) . . . . ?
C2 N1 C6 C5 -0.3(6) . . . . ?
Cu1 N1 C6 C5 170.8(3) . . . . ?
C4 C5 C6 N1 -1.1(6) . . . . ?
Cu2 O2 C7 O1 -170.6(3) . . . . ?
Cu2 O2 C7 C2 9.8(4) . . . . ?
Cu1 O1 C7 O2 178.9(3) . . . . ?
Cu1 O1 C7 C2 -1.6(4) . . . . ?
N1 C2 C7 O2 175.7(3) . . . . ?
N3 C2 C7 O2 -6.2(5) . . . . ?
N1 C2 C7 O1 -3.9(5) . . . . ?
N3 C2 C7 O1 174.2(3) . . . . ?
C16 N6 C14 N6 -1.3(2) . . . 2_756 ?
Cu2 N6 C14 N6 178.7(2) . . . 2_756 ?
C16 N6 C14 C17 178.7(2) . . . . ?
Cu2 N6 C14 C17 -1.3(2) . . . . ?
C14 N6 C16 C15 2.7(5) . . . . ?
Cu2 N6 C16 C15 -177.4(2) . . . . ?
C16 C15 C16 N6 -1.4(2) 2_756 . . . ?
Cu2 O4 C17 O4 175.39(18) . . . 2_756 ?
Cu2 O4 C17 C14 -4.61(18) . . . . ?
N6 C14 C17 O4 4.20(19) 2_756 . . 2_756 ?
N6 C14 C17 O4 -175.80(19) . . . 2_756 ?
N6 C14 C17 O4 -175.80(19) 2_756 . . . ?
N6 C14 C17 O4 4.20(19) . . . . ?
C20 N7 C18 C19 74.1(4) . . . . ?
C21 N7 C18 C19 -167.2(3) . . . . ?
Cu2 N7 C18 C19 -44.9(4) . . . . ?
C22 N8 C19 C18 83.0(4) . . . . ?
C23 N8 C19 C18 -158.6(4) . . . . ?
Cu2 N8 C19 C18 -37.7(4) . . . . ?
N7 C18 C19 N8 57.8(5) . . . . ?
C10B N4 C8A C9A -150.6(16) . . . . ?
C11 N4 C8A C9A 94.8(11) . . . . ?
C8B N4 C8A C9A 46.6(11) . . . . ?
C10A N4 C8A C9A -151.5(14) . . . . ?
Cu1 N4 C8A C9A -37.6(13) . . . . ?
N4 C8A C9A N5 59.9(16) . . . . ?
C12 N5 C9A C8A -167.8(11) . . . . ?
C13 N5 C9A C8A 72.7(13) . . . . ?
Cu1 N5 C9A C8A -49.9(13) . . . . ?
C10B N4 C8B C9B -72.4(18) . . . . ?
C11 N4 C8B C9B 165.6(14) . . . . ?
C8A N4 C8B C9B -53.8(12) . . . . ?
Cu1 N4 C8B C9B 51.8(15) . . . . ?
N4 C8B C9B N5 -54(2) . . . . ?
C12 N5 C9B C8B -100.6(16) . . . . ?
C13 N5 C9B C8B 145.2(16) . . . . ?
Cu1 N5 C9B C8B 29(2) . . . . ?


# Attachment 'suppmat.cif'

data_h165
_database_code_depnum_ccdc_archive 'CCDC 732637'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H114 Cl Co6 N24 O18'
_chemical_formula_weight         1920.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   18.109(5)
_cell_length_b                   27.020(5)
_cell_length_c                   22.118(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.740(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     10666(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2188
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      22.51

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4004
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13288
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         17.78
_reflns_number_total             3536
_reflns_number_gt                2702
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL)'
_computing_publication_material  'publCIF (Westrip, 2007)'

_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)+(0.0817P)²+145.8813P] 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         3536
_refine_ls_number_parameters     526
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1846
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.537
_refine_ls_shift/su_mean         0.014

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
C1D C 0.1861(7) 0.6806(6) 0.4877(9) 0.130(6) Uani 1 1 d . . .
H1D1 H 0.1407 0.6982 0.4902 0.195 Uiso 1 1 calc R . .
H1D2 H 0.2284 0.7006 0.5048 0.195 Uiso 1 1 calc R . .
H1D3 H 0.1871 0.6502 0.5103 0.195 Uiso 1 1 calc R . .
C1E C 0.6400(8) 0.7507(6) 0.4302(7) 0.128(6) Uani 1 1 d . . .
H1E1 H 0.6426 0.7801 0.4063 0.192 Uiso 1 1 calc R . .
H1E2 H 0.6191 0.7241 0.4039 0.192 Uiso 1 1 calc R . .
H1E3 H 0.6894 0.7418 0.4503 0.192 Uiso 1 1 calc R . .
C1F C 0.9062(4) 0.5558(8) 0.5294(5) 0.179(10) Uani 1 1 d . . .
H1F1 H 0.8952 0.5902 0.5217 0.268 Uiso 1 1 calc R . .
H1F2 H 0.8721 0.5360 0.5015 0.268 Uiso 1 1 calc R . .
H1F3 H 0.9566 0.5490 0.5238 0.268 Uiso 1 1 calc R . .
N1A N 0.2926(4) 0.5793(3) 0.4620(5) 0.081(4) Uani 1 1 d R . .
C2A C 0.3116(4) 0.5781(3) 0.5256(5) 0.093(5) Uani 1 1 d R . .
H2A H 0.3266 0.6065 0.5481 0.111 Uiso 1 1 calc R . .
C3A C 0.3070(7) 0.5331(6) 0.5535(7) 0.091(4) Uani 1 1 d . . .
H3A H 0.3216 0.5293 0.5956 0.109 Uiso 1 1 calc R . .
C4A C 0.2799(8) 0.4935(5) 0.5167(10) 0.089(4) Uani 1 1 d . . .
H4A H 0.2756 0.4630 0.5355 0.106 Uiso 1 1 calc R . .
N5A N 0.2592(6) 0.4964(5) 0.4547(7) 0.073(4) Uani 1 1 d . . .
C6A C 0.2665(7) 0.5378(7) 0.4326(9) 0.085(6) Uani 1 1 d . . .
N1B N 0.5297(8) 0.6529(4) 0.4546(5) 0.073(3) Uani 1 1 d . . .
C2B C 0.5621(9) 0.6272(7) 0.4169(8) 0.101(5) Uani 1 1 d . . .
H2B H 0.6141 0.6264 0.4208 0.122 Uiso 1 1 calc R . .
C3B C 0.5160(15) 0.6003(7) 0.3695(9) 0.134(6) Uani 1 1 d . . .
H3B H 0.5378 0.5808 0.3427 0.161 Uiso 1 1 calc R . .
C4B C 0.4379(10) 0.6032(6) 0.3631(7) 0.090(4) Uani 1 1 d . . .
H4B H 0.4077 0.5857 0.3321 0.108 Uiso 1 1 calc R . .
N5B N 0.4078(6) 0.6305(4) 0.4007(6) 0.069(3) Uani 1 1 d . . .
C6B C 0.4529(9) 0.6544(6) 0.4455(8) 0.076(4) Uani 1 1 d . . .
N1C N 0.6737(6) 0.5712(5) 0.6269(6) 0.072(3) Uani 1 1 d . . .
C2C C 0.6236(12) 0.5522(5) 0.6604(6) 0.082(4) Uani 1 1 d . . .
H2C H 0.6365 0.5252 0.6861 0.098 Uiso 1 1 calc R . .
C3C C 0.5555(10) 0.5729(7) 0.6559(6) 0.080(4) Uani 1 1 d . . .
H3C H 0.5205 0.5588 0.6770 0.096 Uiso 1 1 calc R . .
C4C C 0.5364(8) 0.6144(6) 0.6210(7) 0.071(4) Uani 1 1 d . . .
H4C H 0.4897 0.6289 0.6202 0.086 Uiso 1 1 calc R . .
N5C N 0.5841(8) 0.6338(4) 0.5885(5) 0.068(3) Uani 1 1 d . . .
C6C C 0.6497(10) 0.6118(6) 0.5931(6) 0.067(4) Uani 1 1 d . . .
C2D C 0.1266(8) 0.6361(6) 0.4044(9) 0.155(8) Uani 1 1 d . . .
H2D1 H 0.0813 0.6517 0.4118 0.232 Uiso 1 1 calc R . .
H2D2 H 0.1346 0.6061 0.4278 0.232 Uiso 1 1 calc R . .
H2D3 H 0.1223 0.6287 0.3615 0.232 Uiso 1 1 calc R . .
C2E C 0.5173(7) 0.7790(5) 0.4440(7) 0.118(5) Uani 1 1 d . . .
H2E1 H 0.5236 0.8120 0.4294 0.177 Uiso 1 1 calc R . .
H2E2 H 0.4813 0.7795 0.4713 0.177 Uiso 1 1 calc R . .
H2E3 H 0.4997 0.7577 0.4099 0.177 Uiso 1 1 calc R . .
C2F C 0.9287(10) 0.4918(6) 0.6042(13) 0.219(13) Uani 1 1 d . . .
H2F1 H 0.9751 0.4898 0.5888 0.328 Uiso 1 1 calc R . .
H2F2 H 0.8935 0.4687 0.5826 0.328 Uiso 1 1 calc R . .
H2F3 H 0.9373 0.4841 0.6472 0.328 Uiso 1 1 calc R . .
C4D C 0.1758(9) 0.7177(6) 0.3871(11) 0.135(7) Uani 1 1 d . . .
H4D1 H 0.1227 0.7251 0.3791 0.162 Uiso 1 1 calc R . .
H4D2 H 0.2017 0.7447 0.4106 0.162 Uiso 1 1 calc R . .
C4E C 0.6278(10) 0.7961(6) 0.5238(10) 0.133(7) Uani 1 1 d . . .
H4E1 H 0.6805 0.7880 0.5351 0.159 Uiso 1 1 calc R . .
H4E2 H 0.6240 0.8292 0.5065 0.159 Uiso 1 1 calc R . .
C4F C 0.9392(11) 0.5761(11) 0.6429(13) 0.205(12) Uani 1 1 d . . .
H4F1 H 0.9897 0.5630 0.6525 0.246 Uiso 1 1 calc R . .
H4F2 H 0.9432 0.6081 0.6238 0.246 Uiso 1 1 calc R . .
C5D C 0.2047(12) 0.7117(7) 0.3272(10) 0.146(7) Uani 1 1 d . . .
H5D1 H 0.1770 0.6855 0.3033 0.175 Uiso 1 1 calc R . .
H5D2 H 0.1966 0.7421 0.3038 0.175 Uiso 1 1 calc R . .
C5E C 0.5919(9) 0.7946(6) 0.5779(8) 0.113(5) Uani 1 1 d . . .
H5E1 H 0.5389 0.8017 0.5663 0.135 Uiso 1 1 calc R . .
H5E2 H 0.6138 0.8196 0.6069 0.135 Uiso 1 1 calc R . .
C5F C 0.9163(13) 0.5852(10) 0.6981(13) 0.211(14) Uani 1 1 d . . .
H5F1 H 0.9402 0.6154 0.7151 0.253 Uiso 1 1 calc R . .
H5F2 H 0.9345 0.5585 0.7260 0.253 Uiso 1 1 calc R . .
C7A C 0.2465(7) 0.5497(7) 0.3651(7) 0.074(4) Uani 1 1 d . . .
C7B C 0.4204(10) 0.6865(5) 0.4887(7) 0.062(3) Uani 1 1 d . . .
C7C C 0.7009(8) 0.6340(6) 0.5564(7) 0.077(5) Uani 1 1 d . . .
C7D C 0.3014(9) 0.6810(6) 0.2806(8) 0.131(6) Uani 1 1 d . . .
H7D1 H 0.3547 0.6788 0.2834 0.197 Uiso 1 1 calc R . .
H7D2 H 0.2815 0.7031 0.2479 0.197 Uiso 1 1 calc R . .
H7D3 H 0.2795 0.6488 0.2725 0.197 Uiso 1 1 calc R . .
C7E C 0.5500(7) 0.7411(5) 0.6518(6) 0.094(4) Uani 1 1 d . . .
H7E1 H 0.5553 0.7697 0.6779 0.140 Uiso 1 1 calc R . .
H7E2 H 0.5617 0.7118 0.6762 0.140 Uiso 1 1 calc R . .
H7E3 H 0.4994 0.7391 0.6303 0.140 Uiso 1 1 calc R . .
C7F C 0.8170(8) 0.6420(5) 0.6969(7) 0.113(5) Uani 1 1 d . . .
H7F1 H 0.8331 0.6587 0.6631 0.169 Uiso 1 1 calc R . .
H7F2 H 0.8403 0.6570 0.7347 0.169 Uiso 1 1 calc R . .
H7F3 H 0.7635 0.6446 0.6932 0.169 Uiso 1 1 calc R . .
C8D C 0.3288(8) 0.7452(6) 0.3575(7) 0.127(6) Uani 1 1 d . . .
H8D1 H 0.3269 0.7670 0.3230 0.190 Uiso 1 1 calc R . .
H8D2 H 0.3799 0.7360 0.3723 0.190 Uiso 1 1 calc R . .
H8D3 H 0.3086 0.7617 0.3895 0.190 Uiso 1 1 calc R . .
C8E C 0.6791(7) 0.7415(5) 0.6423(6) 0.109(5) Uani 1 1 d . . .
H8E1 H 0.6840 0.7635 0.6768 0.163 Uiso 1 1 calc R . .
H8E2 H 0.7145 0.7506 0.6165 0.163 Uiso 1 1 calc R . .
H8E3 H 0.6885 0.7082 0.6564 0.163 Uiso 1 1 calc R . .
C8F C 0.8186(11) 0.5662(6) 0.7556(8) 0.156(8) Uani 1 1 d . . .
H8F1 H 0.8464 0.5824 0.7910 0.234 Uiso 1 1 calc R . .
H8F2 H 0.8313 0.5317 0.7566 0.234 Uiso 1 1 calc R . .
H8F3 H 0.7659 0.5699 0.7559 0.234 Uiso 1 1 calc R . .
N3D N 0.1897(6) 0.6695(4) 0.4228(7) 0.095(4) Uani 1 1 d . . .
N3E N 0.5911(6) 0.7602(5) 0.4776(6) 0.096(4) Uani 1 1 d . . .
N3F N 0.8977(6) 0.5434(4) 0.5948(8) 0.122(5) Uani 1 1 d . . .
N6D N 0.2837(7) 0.6997(4) 0.3382(6) 0.096(4) Uani 1 1 d . . .
N6E N 0.6020(6) 0.7451(4) 0.6068(5) 0.081(3) Uani 1 1 d . . .
N6F N 0.8384(7) 0.5899(5) 0.6967(7) 0.117(5) Uani 1 1 d . . .
O2G O 0.4633(17) 0.5381(12) 0.4872(18) 0.45(3) Uani 1 1 d . . .
O3G O 0.5583(14) 0.5321(12) 0.5091(14) 0.37(2) Uani 1 1 d . . .
O5G O 0.5350(15) 0.4996(12) 0.4340(13) 0.362(16) Uani 1 1 d . . .
O8A O 0.2569(5) 0.5924(4) 0.3450(4) 0.096(3) Uani 1 1 d . . .
O8B O 0.4636(5) 0.7067(3) 0.5304(4) 0.068(2) Uani 1 1 d . . .
O8C O 0.7656(6) 0.6138(3) 0.5596(4) 0.085(3) Uani 1 1 d . . .
O9A O 0.2202(5) 0.5134(3) 0.3369(5) 0.091(3) Uani 1 1 d . . .
O9B O 0.3498(5) 0.6876(3) 0.4782(4) 0.072(2) Uani 1 1 d . . .
O9C O 0.6845(4) 0.6720(3) 0.5255(4) 0.071(2) Uani 1 1 d . . .
Cl1G Cl 0.5000 0.5000 0.5000 0.130(3) Uani 1 2 d S . .
Co1 Co 0.29550(9) 0.64516(6) 0.40755(8) 0.0736(7) Uani 1 1 d . . .
Co2 Co 0.57659(8) 0.69562(6) 0.53095(7) 0.0629(6) Uani 1 1 d . . .
Co3 Co 0.78516(9) 0.55128(6) 0.61540(8) 0.0756(7) 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
C1D N3D 1.479(18) . ?
C1E N3E 1.504(16) . ?
C1F N3F 1.517(17) . ?
N1A C6A 1.342(14) . ?
N1A C2A 1.3899 . ?
N1A Co1 2.154(9) . ?
C2A C3A 1.374(16) . ?
C3A C4A 1.382(18) . ?
C4A N5A 1.363(17) . ?
N5A C6A 1.238(18) . ?
N5A Co3 2.069(13) 5_666 ?
C6A C7A 1.51(2) . ?
N1B C2B 1.298(16) . ?
N1B C6B 1.371(14) . ?
N1B Co2 2.103(11) . ?
C2B C3B 1.43(2) . ?
C3B C4B 1.40(2) . ?
C4B N5B 1.298(16) . ?
N5B C6B 1.339(16) . ?
N5B Co1 2.102(11) . ?
C6B C7B 1.484(18) . ?
N1C C6C 1.358(15) . ?
N1C C2C 1.363(15) . ?
N1C Co3 2.145(12) . ?
C2C C3C 1.342(17) . ?
C3C C4C 1.372(16) . ?
C4C N5C 1.321(14) . ?
N5C C6C 1.316(16) . ?
N5C Co2 2.091(12) . ?
C6C C7C 1.461(19) . ?
C2D N3D 1.459(16) . ?
C2E N3E 1.505(15) . ?
C2F N3F 1.502(18) . ?
C4D C5D 1.51(2) . ?
C4D N3D 1.522(18) . ?
C4E C5E 1.45(2) . ?
C4E N3E 1.482(18) . ?
C4F C5F 1.38(3) . ?
C4F N3F 1.49(2) . ?
C5D N6D 1.45(2) . ?
C5E N6E 1.481(17) . ?
C5F N6F 1.41(2) . ?
C7A O9A 1.216(15) . ?
C7A O8A 1.263(16) . ?
C7B O8B 1.230(14) . ?
C7B O9B 1.261(15) . ?
C7C O9C 1.242(16) . ?
C7C O8C 1.284(14) . ?
C7D N6D 1.457(17) . ?
C7E N6E 1.484(14) . ?
C7F N6F 1.461(16) . ?
C8D N6D 1.496(16) . ?
C8E N6E 1.485(14) . ?
C8F N6F 1.55(2) . ?
N3D Co1 2.107(11) . ?
N3E Co2 2.147(10) . ?
N3F Co3 2.173(11) . ?
N6D Co1 2.112(11) . ?
N6E Co2 2.134(10) . ?
N6F Co3 2.159(11) . ?
O2G Cl1G 1.233(19) . ?
O2G O3G 1.72(3) . ?
O3G Cl1G 1.36(3) . ?
O5G Cl1G 1.69(3) . ?
O8A Co1 2.028(9) . ?
O8B Co2 2.066(8) . ?
O8C Co3 2.086(9) . ?
O9A Co3 2.052(9) 5_666 ?
O9B Co1 2.051(8) . ?
O9C Co2 2.078(9) . ?
Cl1G O2G 1.233(19) 5_666 ?
Cl1G O3G 1.36(3) 5_666 ?
Cl1G O5G 1.69(3) 5_666 ?
Co3 O9A 2.052(9) 5_666 ?
Co3 N5A 2.069(13) 5_666 ?

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
C6A N1A C2A 118.5(11) . . ?
C6A N1A Co1 117.3(12) . . ?
C2A N1A Co1 124.1(3) . . ?
N1A C2A C3A 116.9(8) . . ?
C4A C3A C2A 117.6(13) . . ?
N5A C4A C3A 123.9(13) . . ?
C6A N5A C4A 114.8(14) . . ?
C6A N5A Co3 108.8(11) . 5_666 ?
C4A N5A Co3 136.4(12) . 5_666 ?
N5A C6A N1A 128.2(17) . . ?
N5A C6A C7A 123.9(14) . . ?
N1A C6A C7A 107.9(18) . . ?
C2B N1B C6B 118.6(13) . . ?
C2B N1B Co2 130.1(12) . . ?
C6B N1B Co2 111.3(13) . . ?
N1B C2B C3B 118.2(15) . . ?
C4B C3B C2B 120.1(15) . . ?
N5B C4B C3B 119.6(14) . . ?
C6B N5B C4B 118.6(12) . . ?
C6B N5B Co1 109.5(11) . . ?
C4B N5B Co1 132.0(12) . . ?
N5B C6B N1B 124.8(15) . . ?
N5B C6B C7B 119.9(14) . . ?
N1B C6B C7B 115.2(17) . . ?
C6C N1C C2C 114.9(12) . . ?
C6C N1C Co3 110.9(12) . . ?
C2C N1C Co3 134.1(13) . . ?
C3C C2C N1C 119.4(13) . . ?
C2C C3C C4C 121.5(13) . . ?
N5C C4C C3C 120.3(12) . . ?
C6C N5C C4C 116.3(12) . . ?
C6C N5C Co2 111.8(11) . . ?
C4C N5C Co2 131.9(11) . . ?
N5C C6C N1C 127.5(12) . . ?
N5C C6C C7C 114.9(16) . . ?
N1C C6C C7C 117.6(17) . . ?
C5D C4D N3D 108.2(14) . . ?
C5E C4E N3E 109.7(13) . . ?
C5F C4F N3F 123(2) . . ?
N6D C5D C4D 110.8(15) . . ?
C4E C5E N6E 110.0(14) . . ?
C4F C5F N6F 117(2) . . ?
O9A C7A O8A 128.6(14) . . ?
O9A C7A C6A 110.1(15) . . ?
O8A C7A C6A 121.3(15) . . ?
O8B C7B O9B 128.6(13) . . ?
O8B C7B C6B 118.1(14) . . ?
O9B C7B C6B 113.3(14) . . ?
O9C C7C O8C 120.9(17) . . ?
O9C C7C C6C 122.1(14) . . ?
O8C C7C C6C 117.0(16) . . ?
C2D N3D C1D 103.6(13) . . ?
C2D N3D C4D 109.4(11) . . ?
C1D N3D C4D 107.5(14) . . ?
C2D N3D Co1 116.9(9) . . ?
C1D N3D Co1 114.1(8) . . ?
C4D N3D Co1 105.0(10) . . ?
C4E N3E C2E 112.1(12) . . ?
C4E N3E C1E 110.1(13) . . ?
C2E N3E C1E 107.0(11) . . ?
C4E N3E Co2 103.6(9) . . ?
C2E N3E Co2 111.4(8) . . ?
C1E N3E Co2 112.7(9) . . ?
C4F N3F C2F 108.7(17) . . ?
C4F N3F C1F 115.5(16) . . ?
C2F N3F C1F 103.9(15) . . ?
C4F N3F Co3 99.8(12) . . ?
C2F N3F Co3 113.8(10) . . ?
C1F N3F Co3 115.3(7) . . ?
C7D N6D C8D 110.1(13) . . ?
C7D N6D C5D 106.7(14) . . ?
C8D N6D C5D 110.0(13) . . ?
C7D N6D Co1 112.5(9) . . ?
C8D N6D Co1 112.5(9) . . ?
C5D N6D Co1 104.7(10) . . ?
C5E N6E C7E 108.1(12) . . ?
C5E N6E C8E 108.8(11) . . ?
C7E N6E C8E 106.7(10) . . ?
C5E N6E Co2 103.4(8) . . ?
C7E N6E Co2 113.8(7) . . ?
C8E N6E Co2 115.6(8) . . ?
C7F N6F C5F 110.6(15) . . ?
C7F N6F C8F 107.2(13) . . ?
C5F N6F C8F 108.4(18) . . ?
C7F N6F Co3 112.8(9) . . ?
C5F N6F Co3 106.2(12) . . ?
C8F N6F Co3 111.5(9) . . ?
Cl1G O2G O3G 51.6(13) . . ?
Cl1G O3G O2G 45.5(12) . . ?
C7A O8A Co1 117.1(9) . . ?
C7B O8B Co2 116.3(9) . . ?
C7C O8C Co3 116.0(11) . . ?
C7A O9A Co3 118.1(10) . 5_666 ?
C7B O9B Co1 117.9(9) . . ?
C7C O9C Co2 111.2(9) . . ?
O2G Cl1G O2G 180.000(11) 5_666 . ?
O2G Cl1G O3G 82.9(16) 5_666 5_666 ?
O2G Cl1G O3G 97.1(16) . 5_666 ?
O2G Cl1G O3G 97.1(16) 5_666 . ?
O2G Cl1G O3G 82.9(16) . . ?
O3G Cl1G O3G 180(2) 5_666 . ?
O2G Cl1G O5G 94.2(14) 5_666 5_666 ?
O2G Cl1G O5G 85.8(14) . 5_666 ?
O3G Cl1G O5G 74.6(13) 5_666 5_666 ?
O3G Cl1G O5G 105.4(13) . 5_666 ?
O2G Cl1G O5G 85.8(14) 5_666 . ?
O2G Cl1G O5G 94.2(14) . . ?
O3G Cl1G O5G 105.4(13) 5_666 . ?
O3G Cl1G O5G 74.6(13) . . ?
O5G Cl1G O5G 180.000(5) 5_666 . ?
O8A Co1 O9B 168.3(4) . . ?
O8A Co1 N3D 96.4(4) . . ?
O9B Co1 N3D 92.0(4) . . ?
O8A Co1 N5B 92.6(5) . . ?
O9B Co1 N5B 79.3(5) . . ?
N3D Co1 N5B 170.9(5) . . ?
O8A Co1 N1A 76.3(4) . . ?
O9B Co1 N1A 95.1(4) . . ?
N3D Co1 N1A 93.4(4) . . ?
N5B Co1 N1A 90.1(3) . . ?
O8A Co1 N6D 90.8(5) . . ?
O9B Co1 N6D 98.0(4) . . ?
N3D Co1 N6D 85.1(5) . . ?
N5B Co1 N6D 93.4(5) . . ?
N1A Co1 N6D 166.8(5) . . ?
O8B Co2 O9C 169.8(3) . . ?
O8B Co2 N1B 79.0(5) . . ?
O9C Co2 N1B 92.3(5) . . ?
O8B Co2 N5C 94.7(5) . . ?
O9C Co2 N5C 80.0(5) . . ?
N1B Co2 N5C 91.5(4) . . ?
O8B Co2 N6E 89.8(4) . . ?
O9C Co2 N6E 99.1(4) . . ?
N1B Co2 N6E 168.4(5) . . ?
N5C Co2 N6E 92.2(4) . . ?
O8B Co2 N3E 95.3(4) . . ?
O9C Co2 N3E 90.8(4) . . ?
N1B Co2 N3E 94.3(5) . . ?
N5C Co2 N3E 169.3(5) . . ?
N6E Co2 N3E 83.8(5) . . ?
O9A Co3 O8C 167.3(4) 5_666 . ?
O9A Co3 N5A 79.0(5) 5_666 5_666 ?
O8C Co3 N5A 93.2(5) . 5_666 ?
O9A Co3 N1C 91.4(5) 5_666 . ?
O8C Co3 N1C 78.4(5) . . ?
N5A Co3 N1C 89.5(4) 5_666 . ?
O9A Co3 N3F 98.7(4) 5_666 . ?
O8C Co3 N3F 91.6(5) . . ?
N5A Co3 N3F 92.3(5) 5_666 . ?
N1C Co3 N3F 169.9(6) . . ?
O9A Co3 N6F 92.1(5) 5_666 . ?
O8C Co3 N6F 96.2(5) . . ?
N5A Co3 N6F 170.4(6) 5_666 . ?
N1C Co3 N6F 94.4(4) . . ?
N3F Co3 N6F 85.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        17.78
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.071

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.032 -0.045 0.250 834 249 ' '
2 -0.029 0.045 0.750 828 257 ' '
3 -0.001 0.456 0.250 830 250 ' '
4 -0.005 0.545 0.750 824 257 ' '
_platon_squeeze_details          
;
;


