# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 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_f:\keyan\new\x-rayc~1\cotb1\01

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H32 Co N4 O5'
_chemical_formula_weight         563.51

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.192(4)
_cell_length_b                   12.0704(19)
_cell_length_c                   12.0780(15)
_cell_angle_alpha                91.254(12)
_cell_angle_beta                 98.01(3)
_cell_angle_gamma                106.54(3)
_cell_volume                     1407.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8283
_exptl_absorpt_correction_T_max  0.8486
_exptl_absorpt_process_details   ?

_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  ?
_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            13760
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5599
_reflns_number_gt                4714
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0567P)²+0.8480P] 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_extinction_coef       ?
_refine_ls_number_reflns         5599
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1231
_refine_ls_wR_factor_gt          0.1135
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.40010(3) 0.11822(3) 0.05392(3) 0.02359(12) Uani 1 1 d . . .
O1 O 0.36249(17) 0.27101(16) 0.15393(16) 0.0338(4) Uani 1 1 d . . .
O3 O -0.32254(18) 0.03161(16) 0.05258(17) 0.0373(5) Uani 1 1 d . . .
O2 O 0.19425(18) 0.10269(16) 0.07186(17) 0.0374(5) Uani 1 1 d . . .
O4 O -0.38165(17) 0.19028(15) 0.07065(17) 0.0354(4) Uani 1 1 d . . .
N1 N 0.4598(2) 0.0508(2) 0.21431(19) 0.0327(5) Uani 1 1 d . . .
N4 N 0.4567(3) 0.4870(2) -0.39481(19) 0.0370(5) Uani 1 1 d . . .
N2 N 0.3827(2) 0.22655(18) -0.08160(18) 0.0296(5) Uani 1 1 d . . .
C3 C -0.0279(2) 0.1745(2) 0.1056(2) 0.0263(5) Uani 1 1 d . . .
H009 H -0.0446 0.0984 0.0779 0.032 Uiso 1 1 calc R . .
C2 C 0.1161(2) 0.2496(2) 0.1397(2) 0.0255(5) Uani 1 1 d . . .
N3 N 0.8471(2) -0.0312(2) 0.4851(2) 0.0412(6) Uani 1 1 d . . .
C4 C -0.1349(2) 0.2180(2) 0.1154(2) 0.0264(5) Uani 1 1 d . . .
C1 C 0.2319(2) 0.2054(2) 0.1220(2) 0.0262(5) Uani 1 1 d . . .
C6 C -0.0967(3) 0.3352(2) 0.1578(2) 0.0315(6) Uani 1 1 d . . .
H014 H -0.1686 0.3666 0.1654 0.038 Uiso 1 1 calc R . .
C5 C -0.2915(2) 0.1402(2) 0.0765(2) 0.0248(5) Uani 1 1 d . . .
C14 C 0.5404(3) -0.0835(3) 0.3258(3) 0.0421(7) Uani 1 1 d . . .
H016 H 0.5399 -0.1600 0.3343 0.050 Uiso 1 1 calc R . .
C17 C 0.6231(3) 0.0043(3) 0.4127(2) 0.0415(7) Uani 1 1 d . . .
C7 C 0.0461(3) 0.4129(2) 0.1913(2) 0.0303(6) Uani 1 1 d . . .
C22 C 0.2611(3) 0.2744(3) -0.2547(3) 0.0422(7) Uani 1 1 d . . .
H019 H 0.1905 0.2543 -0.3158 0.051 Uiso 1 1 calc R . .
C20 C 1.0647(3) 0.0615(3) 0.4166(3) 0.0490(8) Uani 1 1 d . . .
H02A H 1.1171 0.1323 0.3879 0.059 Uiso 1 1 calc R . .
H02B H 1.0423 0.0003 0.3576 0.059 Uiso 1 1 calc R . .
C24 C 0.4708(3) 0.4206(2) -0.1420(2) 0.0384(7) Uani 1 1 d . . .
H021 H 0.5336 0.4943 -0.1320 0.046 Uiso 1 1 calc R . .
C8 C 0.1515(2) 0.3665(2) 0.1824(2) 0.0288(6) Uani 1 1 d . . .
H022 H 0.2434 0.4099 0.2035 0.035 Uiso 1 1 calc R . .
C28 C 0.5014(3) 0.3987(2) -0.5598(3) 0.0430(7) Uani 1 1 d . . .
H02C H 0.4653 0.3399 -0.6211 0.052 Uiso 1 1 calc R . .
H02D H 0.5818 0.3836 -0.5172 0.052 Uiso 1 1 calc R . .
C15 C 0.5376(3) 0.1356(3) 0.3002(3) 0.0446(7) Uani 1 1 d . . .
H024 H 0.5354 0.2113 0.2907 0.054 Uiso 1 1 calc R . .
C25 C 0.3605(3) 0.3888(2) -0.2392(2) 0.0361(6) Uani 1 1 d . . .
C23 C 0.4788(3) 0.3389(2) -0.0663(2) 0.0356(6) Uani 1 1 d . . .
H026 H 0.5480 0.3573 -0.0043 0.043 Uiso 1 1 calc R . .
C26 C 0.3558(4) 0.4788(3) -0.3229(3) 0.0478(8) Uani 1 1 d . . .
H02E H 0.2645 0.4589 -0.3674 0.057 Uiso 1 1 calc R . .
H02F H 0.3721 0.5534 -0.2833 0.057 Uiso 1 1 calc R . .
C21 C 0.2754(3) 0.1965(2) -0.1748(2) 0.0368(6) Uani 1 1 d . . .
H028 H 0.2132 0.1226 -0.1825 0.044 Uiso 1 1 calc R . .
C18 C 0.7216(3) -0.0176(3) 0.5149(3) 0.0517(8) Uani 1 1 d . . .
H02G H 0.7438 0.0469 0.5704 0.062 Uiso 1 1 calc R . .
H02H H 0.6740 -0.0869 0.5488 0.062 Uiso 1 1 calc R . .
C19 C 0.9362(3) 0.0771(3) 0.4459(3) 0.0488(8) Uani 1 1 d . . .
H03A H 0.8855 0.1003 0.3809 0.059 Uiso 1 1 calc R . .
H03B H 0.9585 0.1386 0.5045 0.059 Uiso 1 1 calc R . .
C16 C 0.6184(3) 0.1162(3) 0.3994(3) 0.0485(8) Uani 1 1 d . . .
H031 H 0.6659 0.1760 0.4527 0.058 Uiso 1 1 calc R . .
C9 C 0.0805(3) 0.5415(2) 0.2364(3) 0.0440(8) Uani 1 1 d . . .
C13 C 0.4608(3) -0.0580(2) 0.2289(2) 0.0378(6) Uani 1 1 d . . .
H033 H 0.4095 -0.1170 0.1760 0.045 Uiso 1 1 calc R . .
C27 C 0.3961(3) 0.3910(2) -0.4876(2) 0.0419(7) Uani 1 1 d . . .
H03C H 0.3730 0.3159 -0.4559 0.050 Uiso 1 1 calc R . .
H03D H 0.3126 0.4010 -0.5300 0.050 Uiso 1 1 calc R . .
C11 C -0.0184(4) 0.5934(3) 0.1603(4) 0.0751(13) Uani 1 1 d . . .
H03E H -0.0030 0.5872 0.0841 0.113 Uiso 1 1 calc R . .
H03F H -0.0013 0.6734 0.1836 0.113 Uiso 1 1 calc R . .
H03G H -0.1125 0.5518 0.1658 0.113 Uiso 1 1 calc R . .
C12 C 0.2362(3) 0.6198(3) 0.2430(4) 0.0715(13) Uani 1 1 d . . .
H03H H 0.2596 0.6284 0.1687 0.107 Uiso 1 1 calc R . .
H03I H 0.2969 0.5836 0.2864 0.107 Uiso 1 1 calc R . .
H03J H 0.2463 0.6946 0.2777 0.107 Uiso 1 1 calc R . .
C10 C 0.0545(4) 0.5430(4) 0.3573(4) 0.0759(13) Uani 1 1 d . . .
H03K H 0.0697 0.6215 0.3850 0.114 Uiso 1 1 calc R . .
H03L H 0.1168 0.5094 0.4022 0.114 Uiso 1 1 calc R . .
H03M H -0.0393 0.4991 0.3610 0.114 Uiso 1 1 calc R . .
O1W O 0.0784(6) -0.1032(5) 0.1752(5) 0.187(2) Uiso 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
Co1 O3 2.0858(19) 2 ?
Co1 O2 2.0949(19) . ?
Co1 O4 2.1239(19) 1_655 ?
Co1 N2 2.137(2) . ?
Co1 N1 2.193(2) . ?
Co1 O1 2.3327(18) . ?
Co1 C1 2.470(2) . ?
O1 C1 1.338(3) . ?
O3 C5 1.274(3) . ?
O3 Co1 2.0858(19) 2 ?
O2 C1 1.297(3) . ?
O4 C5 1.231(3) . ?
O4 Co1 2.1239(19) 1_455 ?
N1 C13 1.332(3) . ?
N1 C15 1.419(4) . ?
N4 C26 1.420(4) . ?
N4 C28 1.466(3) 2_664 ?
N4 C27 1.524(4) . ?
N2 C21 1.417(4) . ?
N2 C23 1.420(3) . ?
C3 C4 1.356(3) . ?
C3 C2 1.485(3) . ?
C2 C8 1.419(3) . ?
C2 C1 1.466(3) . ?
N3 C18 1.427(4) . ?
N3 C19 1.493(4) . ?
N3 C20 1.503(4) 2_756 ?
C4 C6 1.419(3) . ?
C4 C5 1.602(3) . ?
C6 C7 1.485(4) . ?
C14 C13 1.420(4) . ?
C14 C17 1.459(4) . ?
C17 C16 1.376(4) . ?
C17 C18 1.557(4) . ?
C7 C8 1.360(3) . ?
C7 C9 1.559(4) . ?
C22 C21 1.384(4) . ?
C22 C25 1.451(4) . ?
C20 C19 1.464(4) . ?
C20 N3 1.503(4) 2_756 ?
C24 C23 1.371(4) . ?
C24 C25 1.469(4) . ?
C28 C27 1.459(4) . ?
C28 N4 1.466(3) 2_664 ?
C15 C16 1.419(4) . ?
C25 C26 1.506(4) . ?
C9 C10 1.520(5) . ?
C9 C11 1.543(5) . ?
C9 C12 1.589(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O2 86.75(8) 2 . ?
O3 Co1 O4 113.93(8) 2 1_655 ?
O2 Co1 O4 159.21(7) . 1_655 ?
O3 Co1 N2 92.01(8) 2 . ?
O2 Co1 N2 89.26(8) . . ?
O4 Co1 N2 87.91(8) 1_655 . ?
O3 Co1 N1 102.57(9) 2 . ?
O2 Co1 N1 97.49(8) . . ?
O4 Co1 N1 80.71(8) 1_655 . ?
N2 Co1 N1 164.21(9) . . ?
O3 Co1 O1 149.77(7) 2 . ?
O2 Co1 O1 63.73(7) . . ?
O4 Co1 O1 95.47(7) 1_655 . ?
N2 Co1 O1 81.78(7) . . ?
N1 Co1 O1 88.40(8) . . ?
O3 Co1 C1 117.83(8) 2 . ?
O2 Co1 C1 31.66(8) . . ?
O4 Co1 C1 127.59(8) 1_655 . ?
N2 Co1 C1 82.73(8) . . ?
N1 Co1 C1 95.52(8) . . ?
O1 Co1 C1 32.19(7) . . ?
C1 O1 Co1 79.58(13) . . ?
C5 O3 Co1 154.42(19) . 2 ?
C1 O2 Co1 90.35(14) . . ?
C5 O4 Co1 128.92(17) . 1_455 ?
C13 N1 C15 116.9(2) . . ?
C13 N1 Co1 125.30(19) . . ?
C15 N1 Co1 115.52(18) . . ?
C26 N4 C28 112.4(2) . 2_664 ?
C26 N4 C27 107.4(2) . . ?
C28 N4 C27 111.7(2) 2_664 . ?
C21 N2 C23 120.8(2) . . ?
C21 N2 Co1 124.00(17) . . ?
C23 N2 Co1 114.82(17) . . ?
C4 C3 C2 119.2(2) . . ?
C8 C2 C1 116.3(2) . . ?
C8 C2 C3 124.3(2) . . ?
C1 C2 C3 119.3(2) . . ?
C18 N3 C19 112.7(3) . . ?
C18 N3 C20 111.7(2) . 2_756 ?
C19 N3 C20 105.3(2) . 2_756 ?
C3 C4 C6 115.3(2) . . ?
C3 C4 C5 120.4(2) . . ?
C6 C4 C5 124.2(2) . . ?
O2 C1 O1 125.9(2) . . ?
O2 C1 C2 114.0(2) . . ?
O1 C1 C2 120.2(2) . . ?
O2 C1 Co1 57.99(12) . . ?
O1 C1 Co1 68.23(12) . . ?
C2 C1 Co1 168.37(19) . . ?
C4 C6 C7 126.8(2) . . ?
O4 C5 O3 121.0(2) . . ?
O4 C5 C4 116.8(2) . . ?
O3 C5 C4 122.2(2) . . ?
C13 C14 C17 123.3(3) . . ?
C16 C17 C14 117.0(3) . . ?
C16 C17 C18 117.8(3) . . ?
C14 C17 C18 125.1(3) . . ?
C8 C7 C6 116.7(2) . . ?
C8 C7 C9 119.3(2) . . ?
C6 C7 C9 124.0(2) . . ?
C21 C22 C25 117.3(3) . . ?
C19 C20 N3 112.5(3) . 2_756 ?
C23 C24 C25 118.3(3) . . ?
C7 C8 C2 117.7(2) . . ?
C27 C28 N4 111.8(2) . 2_664 ?
C16 C15 N1 126.4(3) . . ?
C22 C25 C24 121.2(2) . . ?
C22 C25 C26 121.4(3) . . ?
C24 C25 C26 117.4(3) . . ?
C24 C23 N2 120.8(3) . . ?
N4 C26 C25 111.4(2) . . ?
C22 C21 N2 121.6(3) . . ?
N3 C18 C17 112.7(2) . . ?
C20 C19 N3 111.8(3) . . ?
C17 C16 C15 116.7(3) . . ?
C10 C9 C11 111.5(3) . . ?
C10 C9 C7 108.3(3) . . ?
C11 C9 C7 105.6(3) . . ?
C10 C9 C12 103.8(3) . . ?
C11 C9 C12 110.6(3) . . ?
C7 C9 C12 117.2(2) . . ?
N1 C13 C14 119.7(3) . . ?
C28 C27 N4 107.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 993066'
#######################################################################
#
#                 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_f:\keyan\struct~1\nitbip\01

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 N6 Ni O6'
_chemical_formula_weight         713.47

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   P21/c

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

_cell_length_a                   11.0054(3)
_cell_length_b                   17.5194(5)
_cell_length_c                   19.5049(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.175(3)
_cell_angle_gamma                90.00
_cell_volume                     3629.57(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8437
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            36444
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         26.37
_reflns_number_total             7399
_reflns_number_gt                6313
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0577P)²+3.3442P] 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_extinction_coef       ?
_refine_ls_number_reflns         7399
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.1129
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.81208(2) 0.220384(16) 0.113449(14) 0.02188(10) Uani 1 1 d . . .
O2 O 1.10993(16) 0.28231(11) 0.18897(9) 0.0418(5) Uani 1 1 d . . .
O1W O 0.87263(15) 0.30550(10) 0.19098(8) 0.0330(4) Uani 1 1 d . . .
O3 O 1.63132(14) 0.21026(10) 0.12146(9) 0.0321(4) Uani 1 1 d . . .
N1 N 0.77631(17) 0.13014(11) 0.03625(9) 0.0263(4) Uani 1 1 d . . .
O1 O 0.98312(14) 0.23162(9) 0.09125(8) 0.0292(4) Uani 1 1 d . . .
N2 N 0.6455(2) -0.01950(12) -0.19039(11) 0.0341(5) Uani 1 1 d . . .
O4 O 1.57627(18) 0.27204(14) 0.20826(11) 0.0606(7) Uani 1 1 d . . .
N6 N 0.9643(2) -0.00807(11) 0.42409(11) 0.0362(5) Uani 1 1 d . . .
N3 N 0.4531(2) -0.02670(12) -0.32196(11) 0.0366(5) Uani 1 1 d . . .
C4 C 1.41831(19) 0.24362(12) 0.10327(12) 0.0249(4) Uani 1 1 d . . .
N5 N 0.87452(17) 0.13734(11) 0.19216(10) 0.0279(4) Uani 1 1 d . . .
C6 C 1.3927(2) 0.22862(13) 0.03063(12) 0.0288(5) Uani 1 1 d . . .
H013 H 1.4594 0.2212 0.0103 0.035 Uiso 1 1 calc R . .
C8 C 1.2695(2) 0.22441(13) -0.01220(12) 0.0294(5) Uani 1 1 d . . .
C25 C 0.3237(2) -0.14350(15) -0.41880(13) 0.0367(6) Uani 1 1 d . . .
H015 H 0.3331 -0.1516 -0.3706 0.044 Uiso 1 1 calc R . .
C3 C 1.32004(19) 0.25551(12) 0.13434(12) 0.0235(4) Uani 1 1 d . . .
H016 H 1.3368 0.2681 0.1822 0.028 Uiso 1 1 calc R . .
C7 C 1.1730(2) 0.23342(13) 0.02115(12) 0.0278(5) Uani 1 1 d . . .
H017 H 1.0900 0.2293 -0.0059 0.033 Uiso 1 1 calc R . .
C35 C 0.9754(3) -0.07403(14) 0.47143(14) 0.0410(6) Uani 1 1 d . . .
H01A H 1.0595 -0.0952 0.4805 0.049 Uiso 1 1 calc R . .
H01B H 0.9160 -0.1131 0.4487 0.049 Uiso 1 1 calc R . .
N4 N 0.26496(17) -0.19419(11) -0.53703(10) 0.0286(4) Uani 1 1 d . . .
C2 C 1.19615(19) 0.24844(12) 0.09344(11) 0.0236(4) Uani 1 1 d . . .
C24 C 0.3556(2) -0.07353(15) -0.44230(13) 0.0337(5) Uani 1 1 d . . .
C17 C 0.7295(2) 0.01133(13) -0.06338(12) 0.0320(5) Uani 1 1 d . . .
C14 C 0.8358(2) 0.05556(16) -0.05251(14) 0.0400(6) Uani 1 1 d . . .
H023 H 0.8941 0.0465 -0.0785 0.048 Uiso 1 1 calc R . .
C18 C 0.7017(3) -0.05042(15) -0.11899(13) 0.0401(6) Uani 1 1 d . . .
H02A H 0.7792 -0.0769 -0.1189 0.048 Uiso 1 1 calc R . .
H02B H 0.6444 -0.0872 -0.1073 0.048 Uiso 1 1 calc R . .
C20 C 0.5816(3) -0.05129(17) -0.31662(14) 0.0429(6) Uani 1 1 d . . .
H02C H 0.6302 -0.0088 -0.3272 0.051 Uiso 1 1 calc R . .
H02D H 0.5812 -0.0913 -0.3510 0.051 Uiso 1 1 calc R . .
C5 C 1.5531(2) 0.24327(14) 0.14847(13) 0.0288(5) Uani 1 1 d . . .
C23 C 0.3880(3) -0.00520(16) -0.39418(14) 0.0413(6) Uani 1 1 d . . .
H02E H 0.4409 0.0291 -0.4127 0.050 Uiso 1 1 calc R . .
H02F H 0.3113 0.0219 -0.3938 0.050 Uiso 1 1 calc R . .
C36 C 1.0504(3) 0.05127(14) 0.45944(14) 0.0401(6) Uani 1 1 d . . .
H02G H 1.0416 0.0955 0.4287 0.048 Uiso 1 1 calc R . .
H02H H 1.1363 0.0330 0.4683 0.048 Uiso 1 1 calc R . .
C26 C 0.2782(2) -0.20094(15) -0.46680(13) 0.0347(5) Uani 1 1 d . . .
H029 H 0.2553 -0.2469 -0.4497 0.042 Uiso 1 1 calc R . .
C19 C 0.6413(3) -0.08052(16) -0.24277(14) 0.0413(6) Uani 1 1 d . . .
H03A H 0.5931 -0.1233 -0.2324 0.050 Uiso 1 1 calc R . .
H03B H 0.7260 -0.0982 -0.2399 0.050 Uiso 1 1 calc R . .
C33 C 0.9512(2) 0.02837(14) 0.29986(12) 0.0351(5) Uani 1 1 d . . .
C9 C 1.2404(3) 0.21055(17) -0.09263(13) 0.0401(6) Uani 1 1 d . . .
C30 C 0.8545(3) 0.07882(17) 0.29871(15) 0.0481(7) Uani 1 1 d . . .
H033 H 0.8129 0.0771 0.3345 0.058 Uiso 1 1 calc R . .
C28 C 0.3037(2) -0.12829(15) -0.55900(13) 0.0342(5) Uani 1 1 d . . .
H034 H 0.3007 -0.1232 -0.6069 0.041 Uiso 1 1 calc R . .
C27 C 0.3478(2) -0.06773(15) -0.51440(13) 0.0368(6) Uani 1 1 d . . .
H035 H 0.3724 -0.0229 -0.5325 0.044 Uiso 1 1 calc R . .
C13 C 0.8558(2) 0.11327(16) -0.00298(14) 0.0392(6) Uani 1 1 d . . .
H036 H 0.9288 0.1422 0.0036 0.047 Uiso 1 1 calc R . .
C29 C 0.8190(3) 0.13166(16) 0.24493(13) 0.0412(6) Uani 1 1 d . . .
H037 H 0.7533 0.1649 0.2455 0.049 Uiso 1 1 calc R . .
C1 C 1.08905(19) 0.25504(13) 0.12832(11) 0.0249(4) Uani 1 1 d . . .
C31 C 0.9680(2) 0.08841(16) 0.19287(14) 0.0421(6) Uani 1 1 d . . .
H039 H 1.0077 0.0911 0.1563 0.051 Uiso 1 1 calc R . .
O2W O 1.7594(2) 0.3507(3) 0.29632(17) 0.1243(16) Uani 1 1 d . . .
C32 C 1.0084(3) 0.03426(16) 0.24479(14) 0.0450(7) Uani 1 1 d . . .
H041 H 1.0741 0.0016 0.2429 0.054 Uiso 1 1 calc R . .
C22 C 0.4556(3) 0.03516(17) -0.27130(15) 0.0466(7) Uani 1 1 d . . .
H04A H 0.3703 0.0520 -0.2744 0.056 Uiso 1 1 calc R . .
H04B H 0.5023 0.0781 -0.2827 0.056 Uiso 1 1 calc R . .
C16 C 0.6500(3) 0.02717(18) -0.02164(17) 0.0536(8) Uani 1 1 d . . .
H043 H 0.5779 -0.0022 -0.0261 0.064 Uiso 1 1 calc R . .
C21 C 0.5167(3) 0.00784(17) -0.19703(15) 0.0451(7) Uani 1 1 d . . .
H04C H 0.5188 0.0493 -0.1638 0.054 Uiso 1 1 calc R . .
H04D H 0.4669 -0.0332 -0.1849 0.054 Uiso 1 1 calc R . .
C34 C 0.9895(3) -0.03111(16) 0.35700(14) 0.0481(7) Uani 1 1 d . . .
H04E H 0.9443 -0.0780 0.3408 0.058 Uiso 1 1 calc R . .
H04F H 1.0787 -0.0414 0.3651 0.058 Uiso 1 1 calc R . .
C15 C 0.6753(3) 0.08611(17) 0.02696(15) 0.0446(7) Uani 1 1 d . . .
H046 H 0.6192 0.0953 0.0543 0.054 Uiso 1 1 calc R . .
C10 C 1.1447(8) 0.1503(5) -0.1156(3) 0.194(5) Uani 1 1 d . . .
H04G H 1.0642 0.1692 -0.1128 0.233 Uiso 1 1 calc R . .
H04H H 1.1673 0.1066 -0.0853 0.233 Uiso 1 1 calc R . .
H04I H 1.1403 0.1361 -0.1637 0.233 Uiso 1 1 calc R . .
C11 C 1.3535(6) 0.1882(6) -0.1161(2) 0.208(5) Uani 1 1 d . . .
H04J H 1.3308 0.1819 -0.1667 0.250 Uiso 1 1 calc R . .
H04K H 1.3862 0.1409 -0.0938 0.250 Uiso 1 1 calc R . .
H04L H 1.4165 0.2272 -0.1028 0.250 Uiso 1 1 calc R . .
C12 C 1.1912(10) 0.2803(3) -0.1309(2) 0.184(4) Uani 1 1 d . . .
H04M H 1.2519 0.3206 -0.1171 0.221 Uiso 1 1 calc R . .
H04N H 1.1144 0.2947 -0.1196 0.221 Uiso 1 1 calc R . .
H04O H 1.1748 0.2716 -0.1811 0.221 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 2.0436(15) 1_455 ?
Ni1 O1 2.0485(15) . ?
Ni1 N5 2.0961(19) . ?
Ni1 O1W 2.1040(17) . ?
Ni1 N4 2.1258(19) 2_654 ?
Ni1 N1 2.1474(18) . ?
O2 C1 1.240(3) . ?
O3 C5 1.261(3) . ?
O3 Ni1 2.0436(15) 1_655 ?
N1 C15 1.326(3) . ?
N1 C13 1.337(3) . ?
O1 C1 1.268(3) . ?
N2 C21 1.470(3) . ?
N2 C19 1.471(3) . ?
N2 C18 1.471(3) . ?
O4 C5 1.234(3) . ?
N6 C36 1.453(3) . ?
N6 C34 1.463(3) . ?
N6 C35 1.464(3) . ?
N3 C23 1.453(3) . ?
N3 C20 1.455(3) . ?
N3 C22 1.462(3) . ?
C4 C3 1.387(3) . ?
C4 C6 1.395(3) . ?
C4 C5 1.515(3) . ?
N5 C29 1.331(3) . ?
N5 C31 1.336(3) . ?
C6 C8 1.397(3) . ?
C8 C7 1.392(3) . ?
C8 C9 1.536(3) . ?
C25 C26 1.376(3) . ?
C25 C24 1.386(4) . ?
C3 C2 1.393(3) . ?
C7 C2 1.391(3) . ?
C35 C36 1.502(4) 3_756 ?
N4 C28 1.339(3) . ?
N4 C26 1.345(3) . ?
N4 Ni1 2.1258(19) 2_644 ?
C2 C1 1.512(3) . ?
C24 C27 1.390(3) . ?
C24 C23 1.505(3) . ?
C17 C16 1.371(4) . ?
C17 C14 1.372(4) . ?
C17 C18 1.506(3) . ?
C14 C13 1.376(3) . ?
C20 C19 1.508(4) . ?
C36 C35 1.502(4) 3_756 ?
C33 C30 1.380(4) . ?
C33 C32 1.383(4) . ?
C33 C34 1.503(3) . ?
C9 C12 1.461(6) . ?
C9 C10 1.475(6) . ?
C9 C11 1.486(5) . ?
C30 C29 1.377(4) . ?
C28 C27 1.377(3) . ?
C31 C32 1.374(4) . ?
C22 C21 1.507(4) . ?
C16 C15 1.380(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 O1 172.43(6) 1_455 . ?
O3 Ni1 N5 91.30(7) 1_455 . ?
O1 Ni1 N5 94.49(7) . . ?
O3 Ni1 O1W 97.94(6) 1_455 . ?
O1 Ni1 O1W 87.03(6) . . ?
N5 Ni1 O1W 89.09(7) . . ?
O3 Ni1 N4 84.10(7) 1_455 2_654 ?
O1 Ni1 N4 90.23(7) . 2_654 ?
N5 Ni1 N4 175.11(7) . 2_654 ?
O1W Ni1 N4 89.89(7) . 2_654 ?
O3 Ni1 N1 89.21(7) 1_455 . ?
O1 Ni1 N1 86.13(6) . . ?
N5 Ni1 N1 88.13(7) . . ?
O1W Ni1 N1 172.39(7) . . ?
N4 Ni1 N1 93.47(7) 2_654 . ?
C5 O3 Ni1 140.95(16) . 1_655 ?
C15 N1 C13 116.3(2) . . ?
C15 N1 Ni1 121.16(16) . . ?
C13 N1 Ni1 122.45(15) . . ?
C1 O1 Ni1 131.98(14) . . ?
C21 N2 C19 108.7(2) . . ?
C21 N2 C18 111.1(2) . . ?
C19 N2 C18 108.6(2) . . ?
C36 N6 C34 111.7(2) . . ?
C36 N6 C35 109.2(2) . . ?
C34 N6 C35 110.0(2) . . ?
C23 N3 C20 111.7(2) . . ?
C23 N3 C22 112.3(2) . . ?
C20 N3 C22 109.0(2) . . ?
C3 C4 C6 119.9(2) . . ?
C3 C4 C5 120.2(2) . . ?
C6 C4 C5 119.79(19) . . ?
C29 N5 C31 116.9(2) . . ?
C29 N5 Ni1 119.29(16) . . ?
C31 N5 Ni1 123.83(16) . . ?
C4 C6 C8 121.6(2) . . ?
C7 C8 C6 117.1(2) . . ?
C7 C8 C9 121.0(2) . . ?
C6 C8 C9 121.9(2) . . ?
C26 C25 C24 120.0(2) . . ?
C4 C3 C2 119.6(2) . . ?
C2 C7 C8 122.4(2) . . ?
N6 C35 C36 110.6(2) . 3_756 ?
C28 N4 C26 116.3(2) . . ?
C28 N4 Ni1 118.98(15) . 2_644 ?
C26 N4 Ni1 124.70(17) . 2_644 ?
C7 C2 C3 119.32(19) . . ?
C7 C2 C1 120.87(19) . . ?
C3 C2 C1 119.80(19) . . ?
C25 C24 C27 116.5(2) . . ?
C25 C24 C23 122.4(2) . . ?
C27 C24 C23 121.0(2) . . ?
C16 C17 C14 116.4(2) . . ?
C16 C17 C18 122.2(2) . . ?
C14 C17 C18 121.4(2) . . ?
C17 C14 C13 119.8(2) . . ?
N2 C18 C17 111.9(2) . . ?
N3 C20 C19 110.0(2) . . ?
O4 C5 O3 126.0(2) . . ?
O4 C5 C4 118.5(2) . . ?
O3 C5 C4 115.5(2) . . ?
N3 C23 C24 112.0(2) . . ?
N6 C36 C35 111.3(2) . 3_756 ?
N4 C26 C25 123.5(2) . . ?
N2 C19 C20 110.1(2) . . ?
C30 C33 C32 116.5(2) . . ?
C30 C33 C34 121.4(2) . . ?
C32 C33 C34 122.1(2) . . ?
C12 C9 C10 107.6(6) . . ?
C12 C9 C11 107.0(5) . . ?
C10 C9 C11 107.8(5) . . ?
C12 C9 C8 109.9(3) . . ?
C10 C9 C8 111.4(3) . . ?
C11 C9 C8 112.9(3) . . ?
C33 C30 C29 120.5(2) . . ?
N4 C28 C27 123.4(2) . . ?
C28 C27 C24 120.1(2) . . ?
N1 C13 C14 123.7(2) . . ?
N5 C29 C30 122.9(2) . . ?
O2 C1 O1 125.5(2) . . ?
O2 C1 C2 119.16(19) . . ?
O1 C1 C2 115.30(19) . . ?
N5 C31 C32 123.4(2) . . ?
C31 C32 C33 119.9(2) . . ?
N3 C22 C21 109.8(2) . . ?
C17 C16 C15 120.9(2) . . ?
N2 C21 C22 111.5(2) . . ?
N6 C34 C33 113.0(2) . . ?
N1 C15 C16 122.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 981096'
#######################################################################
#
#                 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_f:\keyan\struct~1\713x-r~1\cdtbip\01

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 Cd N6 O7'
_chemical_formula_weight         783.16

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   17.0669(10)
_cell_length_b                   10.2827(7)
_cell_length_c                   21.854(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.664(5)
_cell_angle_gamma                90.00
_cell_volume                     3816.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  ?
_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            29564
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8670
_reflns_number_gt                6911
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0824P)²+2.1614P] 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_extinction_coef       ?
_refine_ls_number_reflns         8670
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1719
_refine_ls_wR_factor_gt          0.1592
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.003
_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
Cd1 Cd 0.772210(18) 0.01364(3) 0.130860(13) 0.03778(12) Uani 1 1 d . . .
O4 O 0.7205(2) -0.8356(3) 0.05809(15) 0.0591(9) Uani 1 1 d . . .
N4 N 1.6437(2) -0.0032(3) 0.16771(19) 0.0474(9) Uani 1 1 d . . .
N2 N 1.2034(2) -0.0016(3) 0.1122(2) 0.0512(9) Uani 1 1 d . . .
N5 N 0.8143(2) 0.0215(3) 0.23627(17) 0.0431(8) Uani 1 1 d . . .
O3 O 0.7745(2) -0.7371(3) 0.14045(15) 0.0621(9) Uani 1 1 d . . .
N6 N 0.9285(2) -0.0147(3) 0.45939(16) 0.0401(8) Uani 1 1 d . . .
O1 O 0.7286(2) -0.1416(3) 0.06261(16) 0.0612(9) Uani 1 1 d . . .
O2 O 0.7863(2) -0.2454(3) 0.14227(16) 0.0648(9) Uani 1 1 d . . .
N1 N 0.9037(2) 0.0221(3) 0.10607(19) 0.0468(8) Uani 1 1 d . . .
C35 C 0.9912(2) 0.0744(4) 0.44535(18) 0.0449(9) Uani 1 1 d . . .
H01A H 0.9808 0.1619 0.4616 0.054 Uiso 1 1 calc R . .
H01B H 0.9917 0.0816 0.4002 0.054 Uiso 1 1 calc R . .
C2 C 0.7176(2) -0.3706(3) 0.06165(18) 0.0390(8) Uani 1 1 d . . .
C34 C 0.8524(3) 0.0335(5) 0.4336(2) 0.0530(11) Uani 1 1 d . . .
H01C H 0.8455 0.1235 0.4482 0.064 Uiso 1 1 calc R . .
H01D H 0.8105 -0.0207 0.4489 0.064 Uiso 1 1 calc R . .
C7 C 0.6409(3) -0.4825(3) -0.0230(2) 0.0408(9) Uani 1 1 d . . .
C20 C 1.3415(3) -0.0677(5) 0.1310(2) 0.0546(11) Uani 1 1 d . . .
H01E H 1.3262 -0.1577 0.1406 0.065 Uiso 1 1 calc R . .
H01F H 1.3918 -0.0713 0.1121 0.065 Uiso 1 1 calc R . .
C4 C 0.7133(2) -0.6048(3) 0.06017(18) 0.0379(8) Uani 1 1 d . . .
N3 N 1.3521(2) 0.0087(3) 0.18782(19) 0.0497(9) Uani 1 1 d . . .
C30 C 0.8111(3) 0.1364(4) 0.3306(2) 0.0520(11) Uani 1 1 d . . .
H018 H 0.7984 0.2143 0.3509 0.062 Uiso 1 1 calc R . .
C21 C 1.2140(3) 0.0752(5) 0.1694(2) 0.0532(11) Uani 1 1 d . . .
H01G H 1.1636 0.0790 0.1882 0.064 Uiso 1 1 calc R . .
H01H H 1.2294 0.1652 0.1598 0.064 Uiso 1 1 calc R . .
C8 C 0.6696(2) -0.3683(3) 0.00667(18) 0.0389(8) Uani 1 1 d . . .
H020 H 0.6557 -0.2867 -0.0116 0.047 Uiso 1 1 calc R . .
C18 C 1.1451(3) 0.0594(6) 0.0678(2) 0.0631(13) Uani 1 1 d . . .
H02A H 1.1489 0.0197 0.0269 0.076 Uiso 1 1 calc R . .
H02B H 1.1579 0.1529 0.0646 0.076 Uiso 1 1 calc R . .
C15 C 0.9551(3) -0.0720(5) 0.1199(3) 0.0616(13) Uani 1 1 d . . .
H022 H 0.9368 -0.1494 0.1375 0.074 Uiso 1 1 calc R . .
C6 C 0.6659(2) -0.5996(4) 0.00489(19) 0.0397(8) Uani 1 1 d . . .
H023 H 0.6497 -0.6789 -0.0148 0.048 Uiso 1 1 calc R . .
C24 C 1.4943(3) -0.0351(5) 0.2075(2) 0.0528(11) Uani 1 1 d . . .
C22 C 1.2769(3) 0.0147(5) 0.2145(2) 0.0558(12) Uani 1 1 d . . .
H02C H 1.2831 0.0671 0.2527 0.067 Uiso 1 1 calc R . .
H02D H 1.2606 -0.0741 0.2252 0.067 Uiso 1 1 calc R . .
C9 C 0.5901(3) -0.4746(5) -0.0842(2) 0.0552(12) Uani 1 1 d . . .
C29 C 0.7976(3) 0.1271(4) 0.2679(2) 0.0523(11) Uani 1 1 d . . .
H027 H 0.7751 0.1998 0.2458 0.063 Uiso 1 1 calc R . .
C36 C 1.0709(3) 0.0267(5) 0.47350(19) 0.0492(10) Uani 1 1 d . . .
H02E H 1.0825 -0.0588 0.4557 0.059 Uiso 1 1 calc R . .
H02F H 1.1123 0.0886 0.4637 0.059 Uiso 1 1 calc R . .
C31 C 0.8482(3) -0.0774(4) 0.2682(2) 0.0522(11) Uani 1 1 d . . .
H029 H 0.8622 -0.1527 0.2466 0.063 Uiso 1 1 calc R . .
C33 C 0.8430(3) 0.0323(5) 0.3643(2) 0.0457(9) Uani 1 1 d . . .
C13 C 0.9309(3) 0.1298(5) 0.0818(2) 0.0594(12) Uani 1 1 d . . .
H031 H 0.8950 0.1987 0.0713 0.071 Uiso 1 1 calc R . .
C19 C 1.2791(3) -0.0082(5) 0.0865(3) 0.0614(14) Uani 1 1 d . . .
H03A H 1.2956 0.0806 0.0758 0.074 Uiso 1 1 calc R . .
H03B H 1.2733 -0.0605 0.0483 0.074 Uiso 1 1 calc R . .
C27 C 1.5479(3) -0.1344(5) 0.2111(2) 0.0607(12) Uani 1 1 d . . .
H033 H 1.5344 -0.2166 0.2269 0.073 Uiso 1 1 calc R . .
C23 C 1.4141(3) -0.0473(6) 0.2307(3) 0.0669(14) Uani 1 1 d . . .
H03C H 1.4025 -0.1403 0.2372 0.080 Uiso 1 1 calc R . .
H03D H 1.4147 -0.0026 0.2709 0.080 Uiso 1 1 calc R . .
C17 C 1.0617(3) 0.0462(5) 0.0841(2) 0.0520(10) Uani 1 1 d . . .
C14 C 1.0089(3) 0.1467(5) 0.0711(2) 0.0613(13) Uani 1 1 d . . .
H036 H 1.0259 0.2266 0.0551 0.074 Uiso 1 1 calc R . .
C26 C 1.5909(3) 0.0909(5) 0.1632(3) 0.0602(12) Uani 1 1 d . . .
H037 H 1.6049 0.1708 0.1453 0.072 Uiso 1 1 calc R . .
C28 C 1.6210(3) -0.1150(5) 0.1920(2) 0.0615(13) Uani 1 1 d . . .
H038 H 1.6577 -0.1847 0.1961 0.074 Uiso 1 1 calc R . .
C32 C 0.8638(3) -0.0752(5) 0.3314(2) 0.0549(11) Uani 1 1 d . . .
H039 H 0.8887 -0.1474 0.3523 0.066 Uiso 1 1 calc R . .
C3 C 0.7375(3) -0.4901(3) 0.08922(19) 0.0375(8) Uani 1 1 d . . .
H040 H 0.7677 -0.4926 0.1281 0.045 Uiso 1 1 calc R . .
C5 C 0.7378(3) -0.7334(4) 0.0885(2) 0.0435(9) Uani 1 1 d . . .
C16 C 1.0332(3) -0.0650(5) 0.1104(3) 0.0669(14) Uani 1 1 d . . .
H042 H 1.0675 -0.1356 0.1217 0.080 Uiso 1 1 calc R . .
C1 C 0.7468(3) -0.2457(4) 0.0911(2) 0.0493(10) Uani 1 1 d . . .
C11 C 0.5234(4) -0.3804(7) -0.0815(4) 0.111(3) Uani 1 1 d . . .
H04A H 0.4951 -0.3714 -0.1225 0.167 Uiso 1 1 calc R . .
H04B H 0.5443 -0.2956 -0.0675 0.167 Uiso 1 1 calc R . .
H04C H 0.4873 -0.4127 -0.0528 0.167 Uiso 1 1 calc R . .
C25 C 1.5164(3) 0.0806(5) 0.1828(3) 0.0650(14) Uani 1 1 d . . .
H045 H 1.4812 0.1523 0.1793 0.078 Uiso 1 1 calc R . .
C10 C 0.5489(8) -0.6001(7) -0.1006(5) 0.240(10) Uani 1 1 d . . .
H05A H 0.5224 -0.6308 -0.0655 0.360 Uiso 1 1 calc R . .
H05B H 0.5875 -0.6651 -0.1109 0.360 Uiso 1 1 calc R . .
H05C H 0.5099 -0.5867 -0.1360 0.360 Uiso 1 1 calc R . .
C12 C 0.6376(6) -0.4311(18) -0.1325(4) 0.275(10) Uani 1 1 d . . .
H05D H 0.6596 -0.5069 -0.1519 0.412 Uiso 1 1 calc R . .
H05E H 0.6805 -0.3757 -0.1145 0.412 Uiso 1 1 calc R . .
H05F H 0.6044 -0.3816 -0.1634 0.412 Uiso 1 1 calc R . .
O1W O 0.9265(5) -0.3668(8) 0.2057(4) 0.190(3) Uiso 1 1 d . . .
O2W O 0.9221(6) -0.6433(9) 0.2091(4) 0.202(4) Uiso 1 1 d . . .
O4W O 1.4174(9) 0.0071(10) -0.0059(7) 0.265(6) Uiso 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
Cd1 O1 2.260(3) . ?
Cd1 O4 2.331(3) 1_565 ?
Cd1 N5 2.346(4) . ?
Cd1 N1 2.361(4) . ?
Cd1 N4 2.416(4) 1_455 ?
Cd1 O3 2.571(3) 1_565 ?
O4 C5 1.263(5) . ?
O4 Cd1 2.331(3) 1_545 ?
N4 C26 1.319(6) . ?
N4 C28 1.339(6) . ?
N4 Cd1 2.416(4) 1_655 ?
N2 C19 1.461(7) . ?
N2 C18 1.461(6) . ?
N2 C21 1.474(6) . ?
N5 C31 1.333(5) . ?
N5 C29 1.334(5) . ?
O3 C5 1.242(5) . ?
O3 Cd1 2.571(3) 1_545 ?
N6 C35 1.464(5) . ?
N6 C34 1.452(6) . ?
N6 C36 1.471(5) 3_756 ?
O1 C1 1.261(5) . ?
O2 C1 1.248(6) . ?
N1 C15 1.321(6) . ?
N1 C13 1.331(6) . ?
C35 C36 1.517(6) . ?
C2 C8 1.386(6) . ?
C2 C3 1.395(5) . ?
C2 C1 1.500(5) . ?
C34 C33 1.508(6) . ?
C7 C6 1.398(5) . ?
C7 C8 1.406(5) . ?
C7 C9 1.523(7) . ?
C20 N3 1.466(6) . ?
C20 C19 1.499(7) . ?
C4 C6 1.388(6) . ?
C4 C3 1.383(5) . ?
C4 C5 1.501(5) . ?
N3 C23 1.461(6) . ?
N3 C22 1.463(6) . ?
C30 C29 1.371(6) . ?
C30 C33 1.381(6) . ?
C21 C22 1.517(7) . ?
C18 C17 1.508(6) . ?
C15 C16 1.371(7) . ?
C24 C27 1.367(7) . ?
C24 C25 1.375(7) . ?
C24 C23 1.510(7) . ?
C9 C12 1.463(10) . ?
C9 C11 1.500(8) . ?
C9 C10 1.495(9) . ?
C36 N6 1.471(5) 3_756 ?
C31 C32 1.381(6) . ?
C33 C32 1.383(6) . ?
C13 C14 1.384(6) . ?
C27 C28 1.369(7) . ?
C17 C14 1.382(7) . ?
C17 C16 1.390(7) . ?
C26 C25 1.385(7) . ?

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 Cd1 O4 86.65(13) . 1_565 ?
O1 Cd1 N5 136.17(12) . . ?
O4 Cd1 N5 134.90(11) 1_565 . ?
O1 Cd1 N1 97.67(14) . . ?
O4 Cd1 N1 97.08(13) 1_565 . ?
N5 Cd1 N1 91.03(14) . . ?
O1 Cd1 N4 85.31(13) . 1_455 ?
O4 Cd1 N4 88.87(13) 1_565 1_455 ?
N5 Cd1 N4 82.84(14) . 1_455 ?
N1 Cd1 N4 173.47(13) . 1_455 ?
O1 Cd1 O3 139.38(11) . 1_565 ?
O4 Cd1 O3 52.73(11) 1_565 1_565 ?
N5 Cd1 O3 83.40(11) . 1_565 ?
N1 Cd1 O3 88.56(12) . 1_565 ?
N4 Cd1 O3 92.94(11) 1_455 1_565 ?
C5 O4 Cd1 98.2(3) . 1_545 ?
C26 N4 C28 115.9(4) . . ?
C26 N4 Cd1 123.9(3) . 1_655 ?
C28 N4 Cd1 120.1(3) . 1_655 ?
C19 N2 C18 109.6(4) . . ?
C19 N2 C21 108.2(4) . . ?
C18 N2 C21 110.6(4) . . ?
C31 N5 C29 117.0(4) . . ?
C31 N5 Cd1 124.3(3) . . ?
C29 N5 Cd1 118.4(3) . . ?
C5 O3 Cd1 87.4(3) . 1_545 ?
C35 N6 C34 110.5(3) . . ?
C35 N6 C36 109.2(3) . 3_756 ?
C34 N6 C36 109.4(3) . 3_756 ?
C1 O1 Cd1 103.0(3) . . ?
C15 N1 C13 116.7(4) . . ?
C15 N1 Cd1 123.1(3) . . ?
C13 N1 Cd1 120.0(3) . . ?
N6 C35 C36 110.9(3) . . ?
C8 C2 C3 119.1(3) . . ?
C8 C2 C1 120.0(4) . . ?
C3 C2 C1 120.9(4) . . ?
N6 C34 C33 112.9(4) . . ?
C6 C7 C8 116.2(4) . . ?
C6 C7 C9 123.5(4) . . ?
C8 C7 C9 120.2(3) . . ?
N3 C20 C19 110.6(4) . . ?
C6 C4 C3 119.3(3) . . ?
C6 C4 C5 120.5(3) . . ?
C3 C4 C5 120.3(4) . . ?
C23 N3 C22 111.7(4) . . ?
C23 N3 C20 110.7(4) . . ?
C22 N3 C20 108.7(4) . . ?
C29 C30 C33 119.8(4) . . ?
N2 C21 C22 110.5(4) . . ?
C2 C8 C7 122.4(3) . . ?
N2 C18 C17 113.7(4) . . ?
N1 C15 C16 124.1(4) . . ?
C4 C6 C7 122.6(4) . . ?
C27 C24 C25 117.4(5) . . ?
C27 C24 C23 122.8(5) . . ?
C25 C24 C23 119.8(5) . . ?
N3 C22 C21 110.6(4) . . ?
C12 C9 C11 107.9(8) . . ?
C12 C9 C10 111.8(9) . . ?
C11 C9 C10 103.1(7) . . ?
C12 C9 C7 110.0(5) . . ?
C11 C9 C7 111.6(5) . . ?
C10 C9 C7 112.2(5) . . ?
N5 C29 C30 123.5(4) . . ?
N6 C36 C35 110.4(4) 3_756 . ?
N5 C31 C32 122.8(4) . . ?
C32 C33 C30 116.8(4) . . ?
C32 C33 C34 121.4(4) . . ?
C30 C33 C34 121.7(4) . . ?
N1 C13 C14 123.4(4) . . ?
N2 C19 C20 111.6(4) . . ?
C24 C27 C28 119.9(4) . . ?
N3 C23 C24 112.0(4) . . ?
C14 C17 C16 116.9(4) . . ?
C14 C17 C18 119.8(4) . . ?
C16 C17 C18 123.3(5) . . ?
C17 C14 C13 119.3(4) . . ?
N4 C26 C25 124.1(5) . . ?
N4 C28 C27 123.6(5) . . ?
C31 C32 C33 119.9(4) . . ?
C4 C3 C2 120.3(4) . . ?
O3 C5 O4 121.7(4) . . ?
O3 C5 C4 119.9(4) . . ?
O4 C5 C4 118.4(4) . . ?
C15 C16 C17 119.4(5) . . ?
O2 C1 O1 121.7(4) . . ?
O2 C1 C2 120.9(4) . . ?
O1 C1 C2 117.4(4) . . ?
C24 C25 C26 119.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 981097'
