# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_DG1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H58 Co2 N12 O17'
_chemical_formula_weight         1264.98

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'

loop_
_space_group_symop_operation_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                   19.652(5)
_cell_length_b                   11.540(5)
_cell_length_c                   27.611(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 107.031(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5987(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      1.543
_cell_measurement_theta_max      27.489

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_process_details   
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL 
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47915
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6852
_reflns_number_gt                6057
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_cell_refinement       'SMART APEX II'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2008)'

_refine_special_details          
;
  Refined as a 2-component inversion twin.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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0842P)²+7.3698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6852
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.04231(11) 0.02127(19) 0.69602(8) 0.0347(4) Uani 1 1 d . . . . .
H1 H 1.0624 0.0944 0.7041 0.042 Uiso 1 1 calc R U . . .
C1S C 1.4660(3) -0.8878(4) 0.95441(17) 0.0952(14) Uani 1 1 d . . . . .
H1SA H 1.4647 -0.9664 0.9428 0.143 Uiso 1 1 calc R U . . .
H1SB H 1.4207 -0.8676 0.9587 0.143 Uiso 1 1 calc R U . . .
H1SC H 1.5023 -0.8800 0.9862 0.143 Uiso 1 1 calc R U . . .
C2 C 1.07952(12) -0.0730(2) 0.72004(8) 0.0383(5) Uani 1 1 d . . . . .
H2 H 1.1233 -0.0635 0.7443 0.046 Uiso 1 1 calc R U . . .
C3 C 1.05121(12) -0.18294(19) 0.70777(8) 0.0357(5) Uani 1 1 d . . . . .
C4 C 0.98487(13) -0.1922(2) 0.67157(9) 0.0379(5) Uani 1 1 d . . . . .
H4 H 0.9641 -0.2644 0.6622 0.046 Uiso 1 1 calc R U . . .
C5 C 0.95066(12) -0.09269(19) 0.64992(8) 0.0354(4) Uani 1 1 d . . . . .
H5 H 0.9062 -0.0995 0.6262 0.042 Uiso 1 1 calc R U . . .
C6 C 1.08888(14) -0.2874(2) 0.73131(9) 0.0426(5) Uani 1 1 d . . . . .
C7 C 1.23319(15) -0.3794(2) 0.81986(10) 0.0479(6) Uani 1 1 d . . . . .
C8 C 1.27458(13) -0.4822(2) 0.84159(9) 0.0419(5) Uani 1 1 d . . . . .
C9 C 1.33544(14) -0.4683(2) 0.88230(11) 0.0495(6) Uani 1 1 d . . . . .
H9 H 1.3479 -0.3956 0.8967 0.059 Uiso 1 1 calc R U . . .
C10 C 1.37714(15) -0.5637(3) 0.90104(11) 0.0550(7) Uani 1 1 d . . . . .
H10 H 1.4179 -0.5531 0.9281 0.066 Uiso 1 1 calc R U . . .
C11 C 1.30285(15) -0.6830(2) 0.84374(12) 0.0512(6) Uani 1 1 d . . . . .
H11 H 1.2913 -0.7570 0.8306 0.061 Uiso 1 1 calc R U . . .
C12 C 1.25797(13) -0.5929(2) 0.82245(10) 0.0461(6) Uani 1 1 d . . . . .
H12 H 1.2172 -0.6063 0.7957 0.055 Uiso 1 1 calc R U . . .
C13 C 0.79652(12) 0.31189(19) 0.56381(9) 0.0364(5) Uani 1 1 d . . . . .
H13 H 0.7745 0.2400 0.5618 0.044 Uiso 1 1 calc R U . . .
C14 C 0.75678(12) 0.4042(2) 0.53852(9) 0.0378(5) Uani 1 1 d . . . . .
H14 H 0.7095 0.3936 0.5197 0.045 Uiso 1 1 calc R U . . .
C15 C 0.78786(12) 0.51217(19) 0.54150(8) 0.0349(4) Uani 1 1 d . . . . .
C16 C 0.85881(13) 0.5227(2) 0.56946(10) 0.0452(6) Uani 1 1 d . . . . .
H16 H 0.8817 0.5939 0.5722 0.054 Uiso 1 1 calc R U . . .
C17 C 0.89500(12) 0.4257(2) 0.59312(10) 0.0433(5) Uani 1 1 d . . . . .
H17 H 0.9427 0.4336 0.6115 0.052 Uiso 1 1 calc R U . . .
C18 C 0.74592(13) 0.6112(2) 0.51499(9) 0.0393(5) Uani 1 1 d . . . . .
C19 C 0.79927(10) 0.06671(17) 0.65832(8) 0.0295(4) Uani 1 1 d . . . . .
C20 C 0.73533(10) -0.01271(18) 0.64469(8) 0.0306(4) Uani 1 1 d . . . . .
C21 C 0.71531(12) -0.0686(2) 0.59811(9) 0.0415(5) Uani 1 1 d . . . . .
H21 H 0.7418 -0.0576 0.5755 0.050 Uiso 1 1 calc R U . . .
C22 C 0.65645(13) -0.1406(2) 0.58488(9) 0.0404(5) Uani 1 1 d . . . . .
H22 H 0.6438 -0.1779 0.5537 0.048 Uiso 1 1 calc R U . . .
C23 C 0.61621(10) -0.15739(18) 0.61804(8) 0.0304(4) Uani 1 1 d . . . . .
C24 C 0.63642(12) -0.1023(2) 0.66467(9) 0.0397(5) Uani 1 1 d . . . . .
H24 H 0.6101 -0.1137 0.6873 0.048 Uiso 1 1 calc R U . . .
C25 C 0.69553(12) -0.0303(2) 0.67787(9) 0.0395(5) Uani 1 1 d . . . . .
H25 H 0.7085 0.0063 0.7092 0.047 Uiso 1 1 calc R U . . .
C26 C 0.55121(10) -0.23450(18) 0.60284(8) 0.0310(4) Uani 1 1 d . . . . .
N1 N 0.97809(9) 0.01327(15) 0.66133(7) 0.0319(4) Uani 1 1 d . . . . .
N2 N 1.14422(12) -0.27940(19) 0.76864(8) 0.0478(5) Uani 1 1 d . . . . .
N3 N 1.17362(12) -0.38803(19) 0.78592(8) 0.0460(5) Uani 1 1 d . . . . .
N4 N 1.36223(13) -0.6695(2) 0.88246(10) 0.0544(6) Uani 1 1 d . . . . .
N5 N 0.86475(10) 0.32059(15) 0.59089(7) 0.0325(4) Uani 1 1 d . . . . .
N6 N 0.77450(11) 0.70912(18) 0.51429(8) 0.0443(5) Uani 1 1 d . . . . .
O1 O 0.82844(7) 0.08459(13) 0.62368(6) 0.0337(3) Uani 1 1 d . . . . .
O1S O 1.48091(13) -0.8145(2) 0.91909(10) 0.0748(7) Uani 1 1 d . . . . .
H1S H 1.4446 -0.7798 0.9037 0.112 Uiso 1 1 calc R U . . .
O2 O 0.81840(9) 0.10900(16) 0.70162(6) 0.0418(4) Uani 1 1 d . . . . .
O1W O 0.91602(8) 0.10374(15) 0.55280(6) 0.0366(3) Uani 1 1 d . . . . .
H1WA H 0.8725 0.1073 0.5331 0.055 Uiso 1 1 d R U . . .
H1WB H 0.9300 0.0320 0.5543 0.055 Uiso 0.5 1 d R U P . .
O3 O 0.53540(9) -0.28110(18) 0.56033(7) 0.0497(5) Uani 1 1 d . . . . .
O2W O 0.93229(8) 0.22905(14) 0.70310(6) 0.0382(3) Uani 1 1 d . . . . .
H2WA H 0.8983 0.2012 0.7141 0.057 Uiso 1 1 d R U . . .
H2WB H 0.9297 0.3045 0.7035 0.057 Uiso 1 1 d R U . . .
O4 O 0.51704(7) -0.24620(13) 0.63467(6) 0.0334(3) Uani 1 1 d . . . . .
O3W O 0.55999(11) -0.37576(17) 0.47283(8) 0.0620(5) Uani 1 1 d G . . . .
H3WA H 0.5403 -0.3190 0.4544 0.093 Uiso 1 1 d G U . . .
H3WB H 0.5626 -0.3616 0.5035 0.093 Uiso 1 1 d G U . . .
O4W O 0.94164(15) 0.4653(2) 0.71045(13) 0.0470(9) Uani 0.5 1 d G . P . .
Co1 Co 0.92241(2) 0.16702(2) 0.62711(2) 0.02573(10) Uani 1 1 d . . . . .
H1WC H 0.952(2) 0.137(3) 0.5500(12) -0.001(7) Uiso 0.5 1 d . . P . .
H6 H 1.0692(16) -0.361(3) 0.7176(11) 0.049(8) Uiso 1 1 d . . . . .
H7 H 1.2557(19) -0.307(3) 0.8276(13) 0.070(10) Uiso 1 1 d . . . . .
H18 H 0.6926(18) 0.593(3) 0.4956(12) 0.064(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.346(3) . ?
C1 C2 1.369(3) . ?
C1S O1S 1.385(5) . ?
C2 C3 1.387(3) . ?
C3 C4 1.395(3) . ?
C3 C6 1.463(3) . ?
C4 C5 1.376(3) . ?
C5 N1 1.336(3) . ?
C6 N2 1.264(3) . ?
C7 N3 1.271(3) . ?
C7 C8 1.464(3) . ?
C8 C12 1.385(4) . ?
C8 C9 1.390(3) . ?
C9 C10 1.380(4) . ?
C10 N4 1.323(4) . ?
C11 N4 1.341(4) . ?
C11 C12 1.378(4) . ?
C13 N5 1.334(3) . ?
C13 C14 1.383(3) . ?
C14 C15 1.379(3) . ?
C15 C16 1.387(3) . ?
C15 C18 1.472(3) . ?
C16 C17 1.383(3) . ?
C17 N5 1.344(3) . ?
C18 N6 1.265(3) . ?
C19 O2 1.243(3) . ?
C19 O1 1.268(2) . ?
C19 C20 1.511(3) . ?
C20 C25 1.383(3) . ?
C20 C21 1.389(3) . ?
C21 C22 1.383(3) . ?
C22 C23 1.387(3) . ?
C23 C24 1.386(3) . ?
C23 C26 1.512(3) . ?
C24 C25 1.387(3) . ?
C26 O3 1.245(3) . ?
C26 O4 1.260(2) . ?
N1 Co1 2.1523(19) . ?
N2 N3 1.404(3) . ?
N5 Co1 2.1819(18) . ?
N6 N6 1.413(4) 7_666 ?
O1 Co1 2.0546(14) . ?
O1W Co1 2.1468(16) . ?
O2W Co1 2.1709(16) . ?
O4 Co1 2.0682(14) 3_445 ?
Co1 O4 2.0682(14) 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
N1 C1 C2 123.1(2) . . ?
C1 C2 C3 119.3(2) . . ?
C2 C3 C4 118.0(2) . . ?
C2 C3 C6 122.0(2) . . ?
C4 C3 C6 120.0(2) . . ?
C5 C4 C3 118.9(2) . . ?
N1 C5 C4 123.3(2) . . ?
N2 C6 C3 120.3(2) . . ?
N3 C7 C8 121.3(3) . . ?
C12 C8 C9 117.8(2) . . ?
C12 C8 C7 123.4(2) . . ?
C9 C8 C7 118.8(2) . . ?
C10 C9 C8 119.1(3) . . ?
N4 C10 C9 123.5(3) . . ?
N4 C11 C12 123.5(3) . . ?
C11 C12 C8 118.9(2) . . ?
N5 C13 C14 123.4(2) . . ?
C15 C14 C13 119.4(2) . . ?
C14 C15 C16 117.9(2) . . ?
C14 C15 C18 119.8(2) . . ?
C16 C15 C18 122.3(2) . . ?
C17 C16 C15 119.1(2) . . ?
N5 C17 C16 123.3(2) . . ?
N6 C18 C15 121.0(2) . . ?
O2 C19 O1 125.84(18) . . ?
O2 C19 C20 118.22(18) . . ?
O1 C19 C20 115.94(18) . . ?
C25 C20 C21 118.91(19) . . ?
C25 C20 C19 120.98(19) . . ?
C21 C20 C19 120.11(18) . . ?
C22 C21 C20 120.8(2) . . ?
C21 C22 C23 120.3(2) . . ?
C24 C23 C22 119.04(19) . . ?
C24 C23 C26 121.12(18) . . ?
C22 C23 C26 119.8(2) . . ?
C23 C24 C25 120.59(19) . . ?
C20 C25 C24 120.4(2) . . ?
O3 C26 O4 125.07(19) . . ?
O3 C26 C23 118.25(18) . . ?
O4 C26 C23 116.68(19) . . ?
C5 N1 C1 117.39(18) . . ?
C5 N1 Co1 122.19(14) . . ?
C1 N1 Co1 120.41(14) . . ?
C6 N2 N3 112.5(2) . . ?
C7 N3 N2 112.3(2) . . ?
C10 N4 C11 117.3(2) . . ?
C13 N5 C17 116.87(19) . . ?
C13 N5 Co1 119.84(14) . . ?
C17 N5 Co1 123.27(15) . . ?
C18 N6 N6 111.9(3) . 7_666 ?
C19 O1 Co1 129.74(13) . . ?
C26 O4 Co1 128.96(14) . 3_445 ?
O1 Co1 O4 176.65(6) . 3 ?
O1 Co1 O1W 89.89(6) . . ?
O4 Co1 O1W 93.45(6) 3 . ?
O1 Co1 N1 88.46(7) . . ?
O4 Co1 N1 91.62(7) 3 . ?
O1W Co1 N1 91.09(7) . . ?
O1 Co1 O2W 91.27(6) . . ?
O4 Co1 O2W 85.39(6) 3 . ?
O1W Co1 O2W 178.20(6) . . ?
N1 Co1 O2W 87.57(7) . . ?
O1 Co1 N5 90.91(7) . . ?
O4 Co1 N5 89.07(7) 3 . ?
O1W Co1 N5 87.76(7) . . ?
N1 Co1 N5 178.69(7) . . ?
O2W Co1 N5 93.59(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.074
_vrf_PLAT415_DG1                 
;
PROBLEM: Short Inter D-H..H-X H1WA .. H14 .. 1.83 Ang.
RESPONSE:...
This is due to the disordered hydrogen atom of coordinated water (O1W).
This short contacts involve partial hydrogen atoms. Due to the
complexity of the disorder model, these checkcif alerts may also
be ignored. We believe that the hydrogen model used is the best model
for the available intensity data. 
;
# end Validation Reply Form
_vrf_PLAT420_DG1                 
;
PROBLEM: D-H Without Acceptor O1W - H1WA
RESPONSE:...
This is probably due to the presence of a half occupancy lattice
water (O4W) where the hydrogen atom has not fixed.
;
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 981262'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_DG2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H58 N12 Ni2 O17'
_chemical_formula_weight         1264.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   19.6754(3)
_cell_length_b                   11.3812(3)
_cell_length_c                   27.5363(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.3420(10)
_cell_angle_gamma                90.00
_cell_volume                     5885.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      27.60

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2632
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8972
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_process_details   
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL 
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47291
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6795
_reflns_number_gt                5990
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_cell_refinement       'SMART APEX II'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2008)'

_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 > 2σ(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)+(0.0616P)²+9.0089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6795
_refine_ls_number_parameters     395
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1280
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.95037(13) -0.0939(2) 0.64944(9) 0.0368(5) Uani 1 1 d . . .
H1 H 0.9057 -0.1010 0.6257 0.044 Uiso 1 1 calc R . .
C1S C 1.4694(4) -0.8917(6) 0.9556(3) 0.148(3) Uani 1 1 d . . .
H1SA H 1.4195 -0.9098 0.9460 0.222 Uiso 1 1 calc R . .
H1SB H 1.4829 -0.8512 0.9876 0.222 Uiso 1 1 calc R . .
H1SC H 1.4962 -0.9632 0.9586 0.222 Uiso 1 1 calc R . .
C2 C 0.98490(14) -0.1945(2) 0.67110(10) 0.0409(5) Uani 1 1 d . . .
H2 H 0.9642 -0.2677 0.6616 0.049 Uiso 1 1 calc R . .
C3 C 1.05127(14) -0.1856(2) 0.70736(10) 0.0392(5) Uani 1 1 d . . .
C4 C 1.07984(13) -0.0740(2) 0.71973(9) 0.0401(5) Uani 1 1 d . . .
H4 H 1.1239 -0.0644 0.7440 0.048 Uiso 1 1 calc R . .
C5 C 1.04239(12) 0.0218(2) 0.69576(9) 0.0365(5) Uani 1 1 d . . .
H5 H 1.0624 0.0960 0.7040 0.044 Uiso 1 1 calc R . .
C6 C 1.08956(15) -0.2908(3) 0.73133(11) 0.0475(6) Uani 1 1 d . . .
H6 H 1.0730 -0.3646 0.7187 0.057 Uiso 1 1 calc R . .
C7 C 1.23352(16) -0.3826(3) 0.82071(12) 0.0526(7) Uani 1 1 d . . .
H7 H 1.2503 -0.3081 0.8322 0.063 Uiso 1 1 calc R . .
C8 C 1.27596(14) -0.4858(3) 0.84284(11) 0.0463(6) Uani 1 1 d . . .
C9 C 1.33694(15) -0.4709(3) 0.88365(12) 0.0536(7) Uani 1 1 d . . .
H9 H 1.3491 -0.3968 0.8979 0.064 Uiso 1 1 calc R . .
C10 C 1.37917(16) -0.5662(3) 0.90289(13) 0.0597(8) Uani 1 1 d . . .
H10 H 1.4198 -0.5544 0.9302 0.072 Uiso 1 1 calc R . .
C11 C 1.30526(17) -0.6887(3) 0.84548(13) 0.0560(7) Uani 1 1 d . . .
H11 H 1.2939 -0.7640 0.8324 0.067 Uiso 1 1 calc R . .
C12 C 1.26024(16) -0.5984(3) 0.82393(12) 0.0509(7) Uani 1 1 d . . .
H12 H 1.2196 -0.6127 0.7969 0.061 Uiso 1 1 calc R . .
C13 C 0.79736(13) 0.3069(2) 0.56507(9) 0.0373(5) Uani 1 1 d . . .
H13 H 0.7757 0.2336 0.5627 0.045 Uiso 1 1 calc R . .
C14 C 0.75754(13) 0.3999(2) 0.53948(10) 0.0398(5) Uani 1 1 d . . .
H14 H 0.7104 0.3888 0.5203 0.048 Uiso 1 1 calc R . .
C15 C 0.78837(13) 0.5097(2) 0.54267(9) 0.0372(5) Uani 1 1 d . . .
C16 C 0.85892(14) 0.5210(2) 0.57153(12) 0.0483(7) Uani 1 1 d . . .
H16 H 0.8816 0.5936 0.5747 0.058 Uiso 1 1 calc R . .
C17 C 0.89509(14) 0.4230(2) 0.59554(11) 0.0465(6) Uani 1 1 d . . .
H17 H 0.9426 0.4316 0.6145 0.056 Uiso 1 1 calc R . .
C18 C 0.74646(14) 0.6096(2) 0.51560(10) 0.0420(6) Uani 1 1 d . . .
H18 H 0.6983 0.5993 0.4988 0.050 Uiso 1 1 calc R . .
C19 C 0.80017(11) 0.06434(19) 0.65814(9) 0.0305(4) Uani 1 1 d . . .
C20 C 0.73537(11) -0.0144(2) 0.64438(9) 0.0317(5) Uani 1 1 d . . .
C21 C 0.69737(13) -0.0344(2) 0.67841(10) 0.0408(6) Uani 1 1 d . . .
H21 H 0.7120 0.0002 0.7104 0.049 Uiso 1 1 calc R . .
C22 C 0.63745(13) -0.1058(2) 0.66520(10) 0.0410(6) Uani 1 1 d . . .
H22 H 0.6124 -0.1188 0.6885 0.049 Uiso 1 1 calc R . .
C23 C 0.61483(12) -0.1577(2) 0.61781(9) 0.0333(5) Uani 1 1 d . . .
C24 C 0.65362(15) -0.1389(3) 0.58388(10) 0.0477(7) Uani 1 1 d . . .
H24 H 0.6396 -0.1745 0.5520 0.057 Uiso 1 1 calc R . .
C25 C 0.71300(14) -0.0674(3) 0.59730(10) 0.0482(7) Uani 1 1 d . . .
H25 H 0.7383 -0.0548 0.5742 0.058 Uiso 1 1 calc R . .
C26 C 0.54921(11) -0.2350(2) 0.60260(9) 0.0335(5) Uani 1 1 d . . .
N1 N 0.97789(10) 0.01348(17) 0.66082(7) 0.0325(4) Uani 1 1 d . . .
N2 N 1.14452(13) -0.2826(2) 0.76880(9) 0.0529(6) Uani 1 1 d . . .
N3 N 1.17455(13) -0.3923(2) 0.78628(9) 0.0504(6) Uani 1 1 d . . .
N4 N 1.36507(14) -0.6740(2) 0.88461(12) 0.0601(7) Uani 1 1 d . . .
N5 N 0.86556(10) 0.31646(17) 0.59310(8) 0.0336(4) Uani 1 1 d . . .
N6 N 0.77450(12) 0.7091(2) 0.51469(9) 0.0477(5) Uani 1 1 d . . .
O1 O 0.82953(8) 0.07996(14) 0.62361(6) 0.0343(4) Uani 1 1 d . . .
O1S O 1.48289(18) -0.8229(3) 0.91976(14) 0.1004(10) Uani 1 1 d . . .
H1S H 1.4467 -0.7870 0.9045 0.151 Uiso 1 1 calc R . .
O2 O 0.81923(9) 0.10886(17) 0.70133(7) 0.0430(4) Uani 1 1 d . . .
O1W O 0.91401(9) 0.10362(15) 0.55414(6) 0.0373(4) Uani 1 1 d . . .
H1WA H 0.9183 0.0310 0.5460 0.056 Uiso 1 1 d R . .
H1WB H 0.9055 0.1469 0.5271 0.056 Uiso 1 1 d R . .
O3 O 0.53132(11) -0.2794(2) 0.55924(8) 0.0585(6) Uani 1 1 d . . .
O2W O 0.93271(9) 0.22750(16) 0.70221(6) 0.0391(4) Uani 1 1 d . . .
H2WA H 0.9000 0.1976 0.7134 0.059 Uiso 1 1 d R . .
H2WB H 0.9286 0.3029 0.7018 0.059 Uiso 1 1 d R . .
O4 O 0.51663(8) -0.24829(15) 0.63511(6) 0.0342(4) Uani 1 1 d . . .
O3W O 0.56120(15) -0.3727(2) 0.47303(10) 0.0684(6) Uani 1 1 d G . .
H3WA H 0.5630 -0.3537 0.5032 0.103 Uiso 1 1 d G . .
H3WB H 0.5462 -0.3147 0.4533 0.103 Uiso 1 1 d G . .
Ni1 Ni 0.922684(13) 0.16503(2) 0.627856(10) 0.02724(10) Uani 1 1 d . . .
O4W O 0.9418(2) 0.4648(4) 0.71153(18) 0.0628(12) Uani 0.50 1 d P . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.336(3) . ?
C1 C2 1.373(3) . ?
C1S O1S 1.346(7) . ?
C2 C3 1.391(4) . ?
C3 C4 1.389(4) . ?
C3 C6 1.463(4) . ?
C4 C5 1.370(3) . ?
C5 N1 1.348(3) . ?
C6 N2 1.256(4) . ?
C7 N3 1.266(4) . ?
C7 C8 1.465(4) . ?
C8 C12 1.383(4) . ?
C8 C9 1.388(4) . ?
C9 C10 1.373(4) . ?
C10 N4 1.324(4) . ?
C11 N4 1.348(4) . ?
C11 C12 1.371(4) . ?
C13 N5 1.338(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.380(4) . ?
C15 C16 1.385(4) . ?
C15 C18 1.470(3) . ?
C16 C17 1.381(4) . ?
C17 N5 1.338(3) . ?
C18 N6 1.264(4) . ?
C19 O2 1.244(3) . ?
C19 O1 1.263(3) . ?
C19 C20 1.511(3) . ?
C20 C25 1.378(4) . ?
C20 C21 1.381(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.380(3) . ?
C23 C24 1.388(3) . ?
C23 C26 1.515(3) . ?
C24 C25 1.381(3) . ?
C26 O3 1.247(3) . ?
C26 O4 1.256(3) . ?
N1 Ni1 2.0954(19) . ?
N2 N3 1.404(3) . ?
N5 Ni1 2.1234(19) . ?
N6 N6 1.408(4) 7_666 ?
O1 Ni1 2.0452(14) . ?
O1W Ni1 2.1051(17) . ?
O2W Ni1 2.1202(17) . ?
O4 Ni1 2.0518(14) 3_445 ?
Ni1 O4 2.0518(15) 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
N1 C1 C2 123.2(2) . . ?
C1 C2 C3 119.2(2) . . ?
C4 C3 C2 117.9(2) . . ?
C4 C3 C6 121.4(2) . . ?
C2 C3 C6 120.7(2) . . ?
C5 C4 C3 119.3(2) . . ?
N1 C5 C4 123.0(2) . . ?
N2 C6 C3 120.7(3) . . ?
N3 C7 C8 121.5(3) . . ?
C12 C8 C9 117.4(3) . . ?
C12 C8 C7 123.4(3) . . ?
C9 C8 C7 119.1(3) . . ?
C10 C9 C8 119.5(3) . . ?
N4 C10 C9 123.5(3) . . ?
N4 C11 C12 123.4(3) . . ?
C11 C12 C8 119.2(3) . . ?
N5 C13 C14 123.5(2) . . ?
C13 C14 C15 119.4(2) . . ?
C14 C15 C16 117.9(2) . . ?
C14 C15 C18 119.9(2) . . ?
C16 C15 C18 122.3(2) . . ?
C17 C16 C15 119.0(2) . . ?
N5 C17 C16 123.6(2) . . ?
N6 C18 C15 121.4(2) . . ?
O2 C19 O1 126.0(2) . . ?
O2 C19 C20 118.2(2) . . ?
O1 C19 C20 115.8(2) . . ?
C25 C20 C21 118.7(2) . . ?
C25 C20 C19 120.3(2) . . ?
C21 C20 C19 121.0(2) . . ?
C20 C21 C22 120.6(2) . . ?
C23 C22 C21 120.5(2) . . ?
C22 C23 C24 118.9(2) . . ?
C22 C23 C26 121.2(2) . . ?
C24 C23 C26 119.9(2) . . ?
C25 C24 C23 120.1(2) . . ?
C20 C25 C24 121.2(2) . . ?
O3 C26 O4 125.1(2) . . ?
O3 C26 C23 118.3(2) . . ?
O4 C26 C23 116.6(2) . . ?
C1 N1 C5 117.5(2) . . ?
C1 N1 Ni1 122.02(15) . . ?
C5 N1 Ni1 120.49(16) . . ?
C6 N2 N3 112.8(3) . . ?
C7 N3 N2 112.2(3) . . ?
C10 N4 C11 116.9(3) . . ?
C17 N5 C13 116.7(2) . . ?
C17 N5 Ni1 123.33(16) . . ?
C13 N5 Ni1 119.93(16) . . ?
C18 N6 N6 112.0(3) . 7_666 ?
C19 O1 Ni1 128.79(15) . . ?
C26 O4 Ni1 128.69(15) . 3_445 ?
O1 Ni1 O4 177.72(6) . 3 ?
O1 Ni1 N1 88.57(7) . . ?
O4 Ni1 N1 91.03(7) 3 . ?
O1 Ni1 O1W 88.51(6) . . ?
O4 Ni1 O1W 93.74(6) 3 . ?
N1 Ni1 O1W 91.54(7) . . ?
O1 Ni1 O2W 92.17(6) . . ?
O4 Ni1 O2W 85.58(6) 3 . ?
N1 Ni1 O2W 88.32(7) . . ?
O1W Ni1 O2W 179.30(6) . . ?
O1 Ni1 N5 90.78(7) . . ?
O4 Ni1 N5 89.66(7) 3 . ?
N1 Ni1 N5 178.79(8) . . ?
O1W Ni1 N5 87.42(7) . . ?
O2W Ni1 N5 92.72(7) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.069
_vrf_PLAT420_DG2                 
;
PROBLEM: D-H Without Acceptor O1W - H1WB
RESPONSE:...
This is probably due to the presence of a half occupancy lattice
water (O4W) where the hydrogen atom has not fixed.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981263'
