# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_cp1a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  -P2yn
_chemical_formula_moiety         'C26 H26 Cu N4 O10'
_chemical_formula_sum            'C26 H26 Cu N4 O10'
_chemical_formula_weight         618.05

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'
Cu Cu 0.3201 1.2651 '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/n

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

_cell_length_a                   7.943(3)
_cell_length_b                   12.822(5)
_cell_length_c                   13.509(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.626(12)
_cell_angle_gamma                90.00
_cell_volume                     1375.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             638
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7952
_exptl_absorpt_correction_T_max  0.9584
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_reflns_number            20886
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         32.31
_reflns_number_total             4556
_reflns_number_gt                2825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0660P)²+0.2050P] 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         4556
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1069
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1949(4) 0.51656(18) 0.3711(2) 0.0375(6) Uani 1 1 d . . .
H1 H 0.2051 0.4444 0.3677 0.045 Uiso 1 1 calc R . .
C2 C 0.0737(4) 0.5650(2) 0.3145(2) 0.0508(8) Uani 1 1 d . . .
H2 H 0.0019 0.5258 0.2744 0.061 Uiso 1 1 calc R . .
C3 C 0.0585(3) 0.6724(2) 0.3170(2) 0.0411(6) Uani 1 1 d . . .
H3 H -0.0192 0.7065 0.2765 0.049 Uiso 1 1 calc R . .
C4 C 0.1616(3) 0.72813(17) 0.38128(16) 0.0267(5) Uani 1 1 d . . .
C5 C 0.2789(3) 0.67358(17) 0.43726(16) 0.0253(5) Uani 1 1 d . . .
H5 H 0.3470 0.7107 0.4812 0.030 Uiso 1 1 calc R . .
C6 C 0.1570(3) 0.84480(18) 0.38296(18) 0.0299(5) Uani 1 1 d . . .
C7 C 0.2247(3) 0.99495(17) 0.49211(18) 0.0289(5) Uani 1 1 d . . .
C8 C 0.2092(4) 1.0746(2) 0.4237(2) 0.0471(7) Uani 1 1 d . . .
H8 H 0.1728 1.0604 0.3595 0.057 Uiso 1 1 calc R . .
C9 C 0.2479(4) 1.1755(2) 0.4513(2) 0.0469(7) Uani 1 1 d . . .
H9 H 0.2415 1.2281 0.4040 0.056 Uiso 1 1 calc R . .
C10 C 0.2960(3) 1.20078(17) 0.54666(17) 0.0287(5) Uani 1 1 d . . .
C11 C 0.3053(4) 1.1210(2) 0.6146(2) 0.0474(7) Uani 1 1 d . . .
H11 H 0.3354 1.1358 0.6798 0.057 Uiso 1 1 calc R . .
C12 C 0.2707(5) 1.01973(19) 0.5877(2) 0.0462(7) Uani 1 1 d . . .
H12 H 0.2784 0.9671 0.6349 0.055 Uiso 1 1 calc R . .
C13 C 0.3397(3) 1.31083(18) 0.57474(18) 0.0289(5) Uani 1 1 d . . .
N1 N 0.2997(2) 0.57017(14) 0.43151(14) 0.0260(4) Uani 1 1 d . . .
N2 N 0.1960(3) 0.88896(16) 0.47031(17) 0.0313(5) Uani 1 1 d . . .
H6 H 0.196(4) 0.856(2) 0.514(2) 0.037(9) Uiso 1 1 d . . .
O1 O 0.1251(3) 0.89336(15) 0.30674(14) 0.0472(5) Uani 1 1 d . . .
O2 O 0.3699(2) 1.37129(12) 0.50199(12) 0.0318(4) Uani 1 1 d . . .
O3 O 0.3493(3) 1.33725(14) 0.66350(13) 0.0427(5) Uani 1 1 d . . .
O4 O 0.2015(5) 0.7554(2) 0.64650(19) 0.0702(9) Uani 1 1 d . . .
H4A H 0.176(5) 0.770(3) 0.697(3) 0.067(12) Uiso 1 1 d . . .
H4B H 0.232(6) 0.706(4) 0.647(3) 0.085(16) Uiso 1 1 d . . .
O5 O 0.3805(2) 0.55401(14) 0.66334(13) 0.0413(4) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.5000 0.02429(13) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.348(3) . ?
C1 C2 1.372(4) . ?
C2 C3 1.383(4) . ?
C3 C4 1.385(3) . ?
C4 C5 1.383(3) . ?
C4 C6 1.496(3) . ?
C5 N1 1.339(3) . ?
C6 O1 1.227(3) . ?
C6 N2 1.342(3) . ?
C7 C12 1.375(4) . ?
C7 C8 1.382(3) . ?
C7 N2 1.409(3) . ?
C8 C9 1.379(4) . ?
C9 C10 1.378(4) . ?
C10 C11 1.376(3) . ?
C10 C13 1.501(3) . ?
C11 C12 1.375(4) . ?
C13 O3 1.248(3) . ?
C13 O2 1.277(3) . ?
N1 Cu1 2.0407(19) . ?
O2 Cu1 1.9474(16) 1_565 ?
Cu1 O2 1.9474(16) 3_676 ?
Cu1 O2 1.9474(16) 1_545 ?
Cu1 N1 2.0407(19) 3_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
N1 C1 C2 122.1(2) . . ?
C1 C2 C3 119.9(2) . . ?
C2 C3 C4 118.6(2) . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 C6 120.9(2) . . ?
C3 C4 C6 120.7(2) . . ?
N1 C5 C4 123.5(2) . . ?
O1 C6 N2 124.5(2) . . ?
O1 C6 C4 120.0(2) . . ?
N2 C6 C4 115.4(2) . . ?
C12 C7 C8 118.5(2) . . ?
C12 C7 N2 117.4(2) . . ?
C8 C7 N2 124.1(2) . . ?
C9 C8 C7 119.6(3) . . ?
C8 C9 C10 122.1(2) . . ?
C11 C10 C9 117.4(2) . . ?
C11 C10 C13 121.3(2) . . ?
C9 C10 C13 121.2(2) . . ?
C12 C11 C10 121.1(2) . . ?
C11 C12 C7 121.1(2) . . ?
O3 C13 O2 124.4(2) . . ?
O3 C13 C10 120.7(2) . . ?
O2 C13 C10 114.9(2) . . ?
C5 N1 C1 117.67(19) . . ?
C5 N1 Cu1 120.43(15) . . ?
C1 N1 Cu1 121.54(16) . . ?
C6 N2 C7 128.8(2) . . ?
C13 O2 Cu1 129.02(15) . 1_565 ?
O2 Cu1 O2 180.0 3_676 1_545 ?
O2 Cu1 N1 91.79(7) 3_676 . ?
O2 Cu1 N1 88.21(7) 1_545 . ?
O2 Cu1 N1 88.21(7) 3_676 3_666 ?
O2 Cu1 N1 91.79(7) 1_545 3_666 ?
N1 Cu1 N1 180.0 . 3_666 ?

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
O4 H4B O5 0.68(4) 2.29(5) 2.956(4) 168(5) 1
O4 H4A O3 0.74(4) 2.08(4) 2.806(3) 166(4) 2_546
N2 H6 O4 0.73(3) 2.21(3) 2.932(3) 179(3) 1

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.099
#
_vrf_PLAT043_cp1a                
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.02 Check           
RESPONSE: We are unable to locate the hydrogen atoms associated with coordinated solvent molecule (O5) from difference fourier map.
;
_vrf_PLAT232_cp1a                
;
PROBLEM: Hirshfeld Test Diff (M-X)  Cu1    --  O5      ..        5.2 su           
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989153'
#######################################################################
#
#                 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_cp1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  -P2yn
_chemical_formula_moiety         'C26 H26 Co N4 O10'
_chemical_formula_sum            'C26 H26 Co N4 O10'
_chemical_formula_weight         613.44

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           MONOCLINIC
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   7.7617(2)
_cell_length_b                   12.4624(3)
_cell_length_c                   13.3308(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2430(10)
_cell_angle_gamma                90.00
_cell_volume                     1264.73(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             634
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8068
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23878
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         32.29
_reflns_number_total             4051
_reflns_number_gt                3495
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.1000P)²+0.4398P] 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         4051
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.1170
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_restrained_S_all      0.878
_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
C1 C 0.35607(18) 0.89899(10) 1.00278(10) 0.0131(2) Uani 1 1 d . . .
H1 H 0.3590 0.9001 1.0729 0.016 Uiso 1 1 calc R . .
C2 C 0.47635(18) 0.83546(11) 0.96633(11) 0.0159(3) Uani 1 1 d . . .
H2 H 0.5602 0.7966 1.0112 0.019 Uiso 1 1 calc R . .
C3 C 0.46988(18) 0.83067(11) 0.86166(11) 0.0151(3) Uani 1 1 d . . .
H3 H 0.5429 0.7843 0.8346 0.018 Uiso 1 1 calc R . .
C4 C 0.35138(17) 0.89702(10) 0.79784(10) 0.0120(2) Uani 1 1 d . . .
C5 C 0.23881(17) 0.96104(10) 0.84179(10) 0.0120(2) Uani 1 1 d . . .
H5 H 0.1627 1.0072 0.7997 0.014 Uiso 1 1 calc R . .
C6 C 0.32967(17) 0.88927(10) 0.68428(10) 0.0122(2) Uani 1 1 d . . .
C7 C 0.2819(2) 1.00287(9) 0.52784(11) 0.0121(3) Uani 1 1 d . . .
C8 C 0.2482(2) 0.92250(10) 0.45351(10) 0.0170(3) Uani 1 1 d . . .
H8 H 0.2504 0.8507 0.4727 0.020 Uiso 1 1 calc R . .
C9 C 0.2112(2) 0.95079(11) 0.35068(10) 0.0163(3) Uani 1 1 d . . .
H9 H 0.1900 0.8972 0.3013 0.020 Uiso 1 1 calc R . .
C10 C 0.20527(18) 1.05794(10) 0.32021(9) 0.0114(2) Uani 1 1 d . . .
C11 C 0.24141(19) 1.13719(10) 0.39502(10) 0.0148(3) Uani 1 1 d . . .
H11 H 0.2393 1.2090 0.3758 0.018 Uiso 1 1 calc R . .
C12 C 0.28035(19) 1.11014(11) 0.49762(10) 0.0154(3) Uani 1 1 d . . .
H12 H 0.3057 1.1638 0.5468 0.018 Uiso 1 1 calc R . .
C13 C 0.15734(17) 1.08665(10) 0.20893(10) 0.0111(2) Uani 1 1 d . . .
N1 N 0.23514(15) 0.95916(9) 0.94196(8) 0.0114(2) Uani 1 1 d . . .
N2 N 0.31909(17) 0.98347(9) 0.63442(9) 0.0130(2) Uani 1 1 d . . .
H2A H 0.3375 1.0396 0.6725 0.016 Uiso 1 1 calc R . .
O1 O 0.31728(14) 0.79879(8) 0.64363(7) 0.0167(2) Uani 1 1 d . . .
O2 O 0.14311(15) 1.00921(7) 0.14614(8) 0.0123(2) Uani 1 1 d . . .
O3 O 0.13082(14) 1.18416(8) 0.18433(7) 0.0153(2) Uani 1 1 d . . .
O4 O 0.02230(14) 1.16630(8) 0.98332(8) 0.01407(19) Uani 1 1 d . . .
H4A H 0.0558 1.1937 1.0397 0.021 Uiso 1 1 calc R . .
H4B H 0.068(3) 1.2018(19) 0.9454(18) 0.032(6) Uiso 1 1 d . . .
O5 O 0.91362(16) 0.33169(9) 0.25787(8) 0.0189(2) Uani 1 1 d . . .
H5A H 0.988(4) 0.285(2) 0.2374(19) 0.044(7) Uiso 1 1 d . . .
H5B H 0.843(3) 0.299(2) 0.2805(19) 0.036(7) Uiso 1 1 d . . .
Co1 Co 0.0000 1.0000 1.0000 0.00878(9) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3431(16) . ?
C1 C2 1.3825(19) . ?
C2 C3 1.3877(19) . ?
C3 C4 1.3959(18) . ?
C4 C5 1.3939(19) . ?
C4 C6 1.4934(18) . ?
C5 N1 1.3414(16) . ?
C6 O1 1.2466(16) . ?
C6 N2 1.3436(17) . ?
C7 C12 1.3956(17) . ?
C7 C8 1.3973(18) . ?
C7 N2 1.4144(18) . ?
C8 C9 1.3902(18) . ?
C9 C10 1.3939(19) . ?
C10 C11 1.3928(17) . ?
C10 C13 1.5006(18) . ?
C11 C12 1.3836(18) . ?
C13 O3 1.2650(16) . ?
C13 O2 1.2681(15) . ?
N1 Co1 2.1770(11) . ?
O2 Co1 2.0490(10) 1_554 ?
O4 Co1 2.0951(10) . ?
Co1 O2 2.0490(10) 1_556 ?
Co1 O2 2.0490(10) 3_576 ?
Co1 O4 2.0952(10) 3_577 ?
Co1 N1 2.1770(11) 3_577 ?

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 123.22(12) . . ?
C1 C2 C3 118.91(12) . . ?
C2 C3 C4 118.54(13) . . ?
C5 C4 C3 118.39(12) . . ?
C5 C4 C6 120.47(11) . . ?
C3 C4 C6 120.68(12) . . ?
N1 C5 C4 123.03(12) . . ?
O1 C6 N2 125.67(12) . . ?
O1 C6 C4 118.88(11) . . ?
N2 C6 C4 115.40(11) . . ?
C12 C7 C8 119.47(12) . . ?
C12 C7 N2 116.25(11) . . ?
C8 C7 N2 124.27(11) . . ?
C9 C8 C7 119.44(12) . . ?
C8 C9 C10 121.27(12) . . ?
C11 C10 C9 118.69(12) . . ?
C11 C10 C13 121.02(11) . . ?
C9 C10 C13 120.28(11) . . ?
C12 C11 C10 120.65(12) . . ?
C11 C12 C7 120.45(12) . . ?
O3 C13 O2 124.83(12) . . ?
O3 C13 C10 118.80(11) . . ?
O2 C13 C10 116.36(11) . . ?
C5 N1 C1 117.56(12) . . ?
C5 N1 Co1 122.12(9) . . ?
C1 N1 Co1 116.85(9) . . ?
C6 N2 C7 128.84(11) . . ?
C13 O2 Co1 129.16(9) . 1_554 ?
O2 Co1 O2 180.00 1_556 3_576 ?
O2 Co1 O4 90.28(4) 1_556 . ?
O2 Co1 O4 89.73(4) 3_576 . ?
O2 Co1 O4 89.73(4) 1_556 3_577 ?
O2 Co1 O4 90.27(4) 3_576 3_577 ?
O4 Co1 O4 179.999 . 3_577 ?
O2 Co1 N1 89.18(4) 1_556 3_577 ?
O2 Co1 N1 90.82(4) 3_576 3_577 ?
O4 Co1 N1 84.19(4) . 3_577 ?
O4 Co1 N1 95.81(4) 3_577 3_577 ?
O2 Co1 N1 90.82(4) 1_556 . ?
O2 Co1 N1 89.17(4) 3_576 . ?
O4 Co1 N1 95.81(4) . . ?
O4 Co1 N1 84.19(4) 3_577 . ?
N1 Co1 N1 180.00 3_577 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O1 0.79(3) 2.13(3) 2.9151(16) 172(2) 3_666
O5 H5A O3 0.90(3) 1.90(3) 2.7979(15) 175(2) 1_645
O4 H4B O1 0.80(2) 2.02(2) 2.8218(15) 176(2) 2_556
O4 H4A O3 0.82 1.91 2.6569(14) 151.7 1_556
N2 H2A O5 0.86 1.99 2.8429(16) 172.2 4_576

_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 989154'
#######################################################################
#
#                 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_cp1c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  -P1
_chemical_formula_moiety         'C26 H26 N4 O10 Zn'
_chemical_formula_sum            'C26 H26 N4 O10 Zn'
_chemical_formula_weight         619.88

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'
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'
Zn Zn 0.2839 1.4301 '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                   9.3173(6)
_cell_length_b                   10.4833(6)
_cell_length_c                   14.0375(8)
_cell_angle_alpha                97.468(2)
_cell_angle_beta                 96.161(2)
_cell_angle_gamma                91.980(2)
_cell_volume                     1350.01(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_T_max  0.8597
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21168
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         32.33
_reflns_number_total             7990
_reflns_number_gt                6404
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.1250P)²+0.8239P] 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         7990
_refine_ls_number_parameters     370
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1759
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
C1 C 0.8599(3) 0.7294(2) 0.75673(18) 0.0336(5) Uani 1 1 d . . .
C2 C 0.8043(3) 0.6433(2) 0.82232(17) 0.0323(5) Uani 1 1 d . . .
C3 C 0.8810(3) 0.6308(3) 0.9111(2) 0.0403(6) Uani 1 1 d . . .
H3 H 0.9680 0.6777 0.9310 0.048 Uiso 1 1 calc R . .
C4 C 0.8275(3) 0.5483(3) 0.9700(2) 0.0423(6) Uani 1 1 d . . .
H4A H 0.8783 0.5410 1.0296 0.051 Uiso 1 1 calc R . .
C5 C 0.6985(3) 0.4763(3) 0.94060(18) 0.0355(5) Uani 1 1 d . . .
C6 C 0.6186(3) 0.4927(3) 0.85374(19) 0.0395(5) Uani 1 1 d . . .
H6 H 0.5300 0.4480 0.8348 0.047 Uiso 1 1 calc R . .
C7 C 0.6719(3) 0.5762(3) 0.79571(18) 0.0375(5) Uani 1 1 d . . .
H7 H 0.6181 0.5875 0.7379 0.045 Uiso 1 1 calc R . .
C8 C 0.5555(3) 0.2907(3) 0.9806(2) 0.0449(6) Uani 1 1 d . . .
C9 C 0.5413(3) 0.2073(3) 1.0585(2) 0.0439(6) Uani 1 1 d . . .
C10 C 0.6538(4) 0.1878(3) 1.1277(3) 0.0538(7) Uani 1 1 d . . .
H10 H 0.7426 0.2307 1.1271 0.065 Uiso 1 1 calc R . .
C11 C 0.6406(4) 0.1098(3) 1.1956(3) 0.0535(8) Uani 1 1 d . . .
H11 H 0.7187 0.0974 1.2400 0.064 Uiso 1 1 calc R . .
C12 C 0.5136(5) 0.0518(4) 1.1972(3) 0.0653(10) Uani 1 1 d U . .
H12 H 0.5034 -0.0006 1.2449 0.078 Uiso 1 1 calc R . .
C13 C 0.4101(4) 0.1419(3) 1.0600(3) 0.0527(7) Uani 1 1 d . . .
H13 H 0.3331 0.1498 1.0136 0.063 Uiso 1 1 calc R . .
C14 C 0.9898(3) 0.7368(3) 0.4510(2) 0.0403(6) Uani 1 1 d . . .
H14 H 0.9202 0.7908 0.4291 0.048 Uiso 1 1 calc R . .
C15 C 1.0452(3) 0.6488(3) 0.3847(2) 0.0425(6) Uani 1 1 d . . .
H15 H 1.0133 0.6436 0.3191 0.051 Uiso 1 1 calc R . .
C16 C 1.1494(3) 0.5676(3) 0.41707(19) 0.0359(5) Uani 1 1 d . . .
H16 H 1.1889 0.5082 0.3733 0.043 Uiso 1 1 calc R . .
C17 C 1.1934(2) 0.5763(2) 0.51498(17) 0.0278(4) Uani 1 1 d . . .
C18 C 1.1329(3) 0.6686(2) 0.57704(19) 0.0339(5) Uani 1 1 d . . .
H18 H 1.1634 0.6759 0.6429 0.041 Uiso 1 1 calc R . .
C19 C 1.3057(2) 0.4974(2) 0.56076(17) 0.0290(4) Uani 1 1 d . . .
C20 C 1.4467(2) 0.3032(2) 0.53437(17) 0.0282(4) Uani 1 1 d . . .
C21 C 1.4995(3) 0.2215(2) 0.4606(2) 0.0351(5) Uani 1 1 d . . .
H21 H 1.4655 0.2249 0.3963 0.042 Uiso 1 1 calc R . .
C22 C 1.6030(3) 0.1354(2) 0.4842(2) 0.0404(6) Uani 1 1 d . . .
H22 H 1.6381 0.0809 0.4352 0.048 Uiso 1 1 calc R . .
C23 C 1.6550(3) 0.1293(2) 0.5798(2) 0.0389(6) Uani 1 1 d . . .
C24 C 1.5989(3) 0.2080(3) 0.6521(2) 0.0434(6) Uani 1 1 d . . .
H24 H 1.6320 0.2035 0.7164 0.052 Uiso 1 1 calc R . .
C25 C 1.4939(3) 0.2938(3) 0.6300(2) 0.0400(6) Uani 1 1 d . . .
H25 H 1.4554 0.3448 0.6794 0.048 Uiso 1 1 calc R . .
C26 C 1.7700(3) 0.0399(3) 0.6054(3) 0.0556(9) Uani 1 1 d . . .
N1 N 0.6552(3) 0.3903(2) 1.00252(17) 0.0415(5) Uani 1 1 d . . .
H1 H 0.6967 0.4025 1.0609 0.050 Uiso 1 1 calc R . .
N2 N 0.3945(4) 0.0641(4) 1.1319(3) 0.0757(10) Uani 1 1 d U . .
N3 N 1.0332(2) 0.7472(2) 0.54658(17) 0.0364(5) Uani 1 1 d . . .
N4 N 1.3426(2) 0.3906(2) 0.50594(14) 0.0307(4) Uani 1 1 d . . .
H4 H 1.2987 0.3739 0.4483 0.037 Uiso 1 1 calc R . .
O1 O 0.4809(3) 0.2666(3) 0.9026(2) 0.0668(7) Uani 1 1 d . . .
O2 O 0.7918(2) 0.7329(2) 0.67481(14) 0.0416(4) Uani 1 1 d . . .
O3 O 0.9740(2) 0.7992(2) 0.78212(15) 0.0460(5) Uani 1 1 d . . .
O4 O 1.3590(2) 0.5324(2) 0.64457(14) 0.0428(5) Uani 1 1 d . . .
O5 O 1.8143(3) 0.0351(3) 0.6927(3) 0.0754(9) Uani 1 1 d . . .
O6 O 1.8217(3) -0.0302(2) 0.5380(3) 0.0728(9) Uani 1 1 d . . .
O7 O 1.1438(3) 0.9859(2) 0.6840(2) 0.0585(6) Uani 1 1 d . . .
O8 O 0.2124(3) 0.5139(3) 0.80587(18) 0.0664(7) Uani 1 1 d . . .
O9 O 0.2018(4) 0.2383(4) 0.7986(3) 0.0893(10) Uani 1 1 d . . .
O10 O 0.9346(7) 0.1956(7) 0.8680(5) 0.176(3) Uani 1 1 d . . .
Zn1 Zn 0.95199(3) 0.88117(3) 0.64842(2) 0.03939(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.258(3) . ?
C1 O3 1.260(3) . ?
C1 C2 1.489(3) . ?
C2 C7 1.389(4) . ?
C2 C3 1.393(3) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.393(4) . ?
C5 N1 1.409(3) . ?
C6 C7 1.385(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O1 1.224(4) . ?
C8 N1 1.355(4) . ?
C8 C9 1.499(4) . ?
C9 C13 1.384(4) . ?
C9 C10 1.390(5) . ?
C10 C11 1.346(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.315(5) . ?
C11 H11 0.9300 . ?
C12 N2 1.382(6) . ?
C12 H12 0.9300 . ?
C13 N2 1.393(5) . ?
C13 H13 0.9300 . ?
C14 N3 1.349(4) . ?
C14 C15 1.377(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.392(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.392(3) . ?
C17 C19 1.498(3) . ?
C18 N3 1.336(3) . ?
C18 H18 0.9300 . ?
C19 O4 1.231(3) . ?
C19 N4 1.351(3) . ?
C20 C25 1.384(3) . ?
C20 C21 1.398(3) . ?
C20 N4 1.419(3) . ?
C21 C22 1.387(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.387(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.382(4) . ?
C23 C26 1.493(3) . ?
C24 C25 1.389(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O5 1.259(5) . ?
C26 O6 1.269(5) . ?
C26 Zn1 2.500(3) 1_645 ?
N1 H1 0.8600 . ?
N3 Zn1 2.091(2) . ?
N4 H4 0.8600 . ?
O2 Zn1 2.211(2) . ?
O3 Zn1 2.157(2) . ?
O5 Zn1 2.165(3) 1_645 ?
O6 Zn1 2.188(3) 1_645 ?
O7 Zn1 2.044(3) . ?
Zn1 O5 2.165(3) 1_465 ?
Zn1 O6 2.188(3) 1_465 ?
Zn1 C26 2.500(3) 1_465 ?

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
O2 C1 O3 119.5(2) . . ?
O2 C1 C2 119.5(2) . . ?
O3 C1 C2 121.0(2) . . ?
C7 C2 C3 119.1(2) . . ?
C7 C2 C1 119.6(2) . . ?
C3 C2 C1 121.3(2) . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.6(2) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 N1 117.0(2) . . ?
C6 C5 N1 123.4(2) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C2 121.1(2) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
O1 C8 N1 123.7(3) . . ?
O1 C8 C9 120.4(3) . . ?
N1 C8 C9 115.9(3) . . ?
C13 C9 C10 117.6(3) . . ?
C13 C9 C8 118.5(3) . . ?
C10 C9 C8 123.9(3) . . ?
C11 C10 C9 123.3(3) . . ?
C11 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C12 C11 C10 117.9(4) . . ?
C12 C11 H11 121.1 . . ?
C10 C11 H11 121.1 . . ?
C11 C12 N2 123.7(3) . . ?
C11 C12 H12 118.1 . . ?
N2 C12 H12 118.1 . . ?
C9 C13 N2 119.4(4) . . ?
C9 C13 H13 120.3 . . ?
N2 C13 H13 120.3 . . ?
N3 C14 C15 122.2(2) . . ?
N3 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 119.1(2) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 119.2(2) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 118.0(2) . . ?
C16 C17 C19 125.5(2) . . ?
C18 C17 C19 116.4(2) . . ?
N3 C18 C17 123.2(2) . . ?
N3 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
O4 C19 N4 123.8(2) . . ?
O4 C19 C17 119.3(2) . . ?
N4 C19 C17 116.9(2) . . ?
C25 C20 C21 119.8(2) . . ?
C25 C20 N4 123.2(2) . . ?
C21 C20 N4 117.0(2) . . ?
C22 C21 C20 119.4(2) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 121.0(2) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 119.0(2) . . ?
C24 C23 C26 119.8(3) . . ?
C22 C23 C26 121.2(3) . . ?
C23 C24 C25 120.9(3) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C20 C25 C24 119.8(2) . . ?
C20 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
O5 C26 O6 121.0(3) . . ?
O5 C26 C23 120.1(3) . . ?
O6 C26 C23 119.0(4) . . ?
O5 C26 Zn1 60.02(17) . 1_645 ?
O6 C26 Zn1 61.06(17) . 1_645 ?
C23 C26 Zn1 176.9(2) . 1_645 ?
C8 N1 C5 127.5(2) . . ?
C8 N1 H1 116.3 . . ?
C5 N1 H1 116.3 . . ?
C12 N2 C13 118.1(3) . . ?
C18 N3 C14 118.2(2) . . ?
C18 N3 Zn1 118.87(18) . . ?
C14 N3 Zn1 122.89(16) . . ?
C19 N4 C20 126.2(2) . . ?
C19 N4 H4 116.9 . . ?
C20 N4 H4 116.9 . . ?
C1 O2 Zn1 89.19(17) . . ?
C1 O3 Zn1 91.61(16) . . ?
C26 O5 Zn1 89.7(2) . 1_645 ?
C26 O6 Zn1 88.4(2) . 1_645 ?
O7 Zn1 N3 94.22(10) . . ?
O7 Zn1 O3 92.32(10) . . ?
N3 Zn1 O3 105.79(9) . . ?
O7 Zn1 O5 96.56(11) . 1_465 ?
N3 Zn1 O5 153.84(11) . 1_465 ?
O3 Zn1 O5 97.52(11) . 1_465 ?
O7 Zn1 O6 108.39(10) . 1_465 ?
N3 Zn1 O6 93.26(10) . 1_465 ?
O3 Zn1 O6 150.82(10) . 1_465 ?
O5 Zn1 O6 60.72(12) 1_465 1_465 ?
O7 Zn1 O2 151.69(10) . . ?
N3 Zn1 O2 89.87(8) . . ?
O3 Zn1 O2 59.71(7) . . ?
O5 Zn1 O2 91.80(10) 1_465 . ?
O6 Zn1 O2 99.30(9) 1_465 . ?
O7 Zn1 C26 105.43(10) . 1_465 ?
N3 Zn1 C26 123.64(12) . 1_465 ?
O3 Zn1 C26 125.00(12) . 1_465 ?
O5 Zn1 C26 30.25(13) 1_465 1_465 ?
O6 Zn1 C26 30.50(13) 1_465 1_465 ?
O2 Zn1 C26 95.36(9) . 1_465 ?

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
N1 H1 O8 0.86 2.04 2.875(4) 163.3 2_667
N4 H4 O2 0.86 2.02 2.834(3) 158.3 2_766

_diffrn_measured_fraction_theta_max 0.831
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.780
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.140
#
_vrf_PLAT043_cp1c                
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by ..       8.05 Check   
RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing Ox(x=8,9,10) in the difference fourier map.
;
_vrf_PLAT306_cp1c                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O8  
RESPONSE: We are unable to locate the H-atoms associated with the solvent water molecule containing Ox(x=8,9,10) in the difference fourier map.
;
_vrf_PLAT230_cp1c                
;
PROBLEM: Hirshfeld Test Diff for    N2     --  C12     ..        9.3 su          
RESPONSE: We are chemically sure about the identity of the elements
of the structure.Therefore this alart is definitely not due to the
wrong assignment of the atoms.However such alart could be due to the
inadequate absorption correction applied by SADABS of the
Bruker APEX-II software.
;
_vrf_PLAT232_cp1c                
;
PROBLEM: Hirshfeld Test Diff (M-X) Zn1 -- O5_a .. 17.0 su          
RESPONSE: We are chemically sure about the identity of the elements
of the structure.Therefore this alart is definitely not due to the
wrong assignment of the atoms.However such alart could be due to the
inadequate absorption correction applied by SADABS of the
Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989155'
#######################################################################
#
#                 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_cp1d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  -P1
_chemical_formula_moiety         'C26 H22 Cd N4 O9'
_chemical_formula_sum            'C26 H22 Cd N4 O9'
_chemical_formula_weight         646.88

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'
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           TRICLINIC
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.7935(9)
_cell_length_b                   12.2071(13)
_cell_length_c                   12.6146(13)
_cell_angle_alpha                96.023(4)
_cell_angle_beta                 103.536(4)
_cell_angle_gamma                96.686(4)
_cell_volume                     1295.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8837
_exptl_absorpt_correction_T_max  0.9477
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23897
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         30.14
_reflns_number_total             7034
_reflns_number_gt                6318
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0569P)²+0.5650P] 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     SHELXL
_refine_ls_extinction_coef       0.0071(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7034
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.187
_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 0.9640(3) 0.6940(2) 0.6075(2) 0.0287(5) Uani 1 1 d . . .
H1A H 0.9793 0.7300 0.6787 0.034 Uiso 1 1 calc R . .
C2 C 1.0694(3) 0.7266(2) 0.5466(2) 0.0272(5) Uani 1 1 d . . .
C3 C 1.0514(3) 0.6677(2) 0.4423(2) 0.0297(5) Uani 1 1 d . . .
H3A H 1.1231 0.6849 0.4007 0.036 Uiso 1 1 calc R . .
C4 C 0.9255(3) 0.5837(2) 0.4024(2) 0.0306(5) Uani 1 1 d . . .
H4 H 0.9106 0.5436 0.3330 0.037 Uiso 1 1 calc R . .
C5 C 0.8213(3) 0.5596(2) 0.4665(2) 0.0294(5) Uani 1 1 d . . .
H5 H 0.7346 0.5045 0.4380 0.035 Uiso 1 1 calc R . .
C6 C 1.1918(3) 0.8266(2) 0.5933(2) 0.0305(5) Uani 1 1 d . . .
C7 C 1.3006(4) 0.9997(2) 0.5300(2) 0.0407(7) Uani 1 1 d . . .
C8 C 1.4023(4) 1.0538(3) 0.6285(2) 0.0502(9) Uani 1 1 d . . .
H8 H 1.4183 1.0186 0.6913 0.060 Uiso 1 1 calc R . .
C9 C 1.4790(4) 1.1600(2) 0.6319(2) 0.0420(7) Uani 1 1 d . . .
H9 H 1.5454 1.1964 0.6978 0.050 Uiso 1 1 calc R . .
C10 C 1.4588(3) 1.2134(2) 0.5387(2) 0.0301(5) Uani 1 1 d . . .
C11 C 1.3601(4) 1.1571(2) 0.4401(2) 0.0369(6) Uani 1 1 d . . .
H11 H 1.3473 1.1910 0.3765 0.044 Uiso 1 1 calc R . .
C12 C 1.2820(4) 1.0523(2) 0.4361(2) 0.0424(7) Uani 1 1 d . . .
H12 H 1.2159 1.0159 0.3700 0.051 Uiso 1 1 calc R . .
C13 C 1.5378(3) 1.3299(2) 0.5417(2) 0.0267(5) Uani 1 1 d . . .
C14 C 0.5676(3) 1.5564(2) 1.1927(2) 0.0314(5) Uani 1 1 d . . .
H14 H 0.5366 1.6193 1.2252 0.038 Uiso 1 1 calc R . .
C15 C 0.6592(3) 1.5698(2) 1.1181(2) 0.0340(6) Uani 1 1 d . . .
H15 H 0.6928 1.6405 1.1036 0.041 Uiso 1 1 calc R . .
C16 C 0.6996(3) 1.4776(2) 1.0661(2) 0.0316(5) Uani 1 1 d . . .
H16 H 0.7571 1.4844 1.0134 0.038 Uiso 1 1 calc R . .
C17 C 0.6537(3) 1.3738(2) 1.0930(2) 0.0270(5) Uani 1 1 d . . .
C18 C 0.5677(3) 1.3677(2) 1.1726(2) 0.0290(5) Uani 1 1 d . . .
H18 H 0.5413 1.2987 1.1936 0.035 Uiso 1 1 calc R . .
C19 C 0.6816(3) 1.2717(2) 1.0267(2) 0.0309(5) Uani 1 1 d . . .
C20 C 0.7311(3) 1.0788(2) 1.0281(2) 0.0311(5) Uani 1 1 d . . .
C21 C 0.6533(4) 1.0361(3) 0.9206(2) 0.0437(7) Uani 1 1 d . . .
H21 H 0.5843 1.0762 0.8783 0.052 Uiso 1 1 calc R . .
C22 C 0.6787(4) 0.9330(2) 0.8760(2) 0.0396(6) Uani 1 1 d . . .
H22 H 0.6261 0.9049 0.8037 0.048 Uiso 1 1 calc R . .
C23 C 0.7798(3) 0.8712(2) 0.9363(2) 0.0302(5) Uani 1 1 d . . .
C24 C 0.8567(5) 0.9147(3) 1.0445(2) 0.0502(9) Uani 1 1 d . . .
H24 H 0.9248 0.8741 1.0869 0.060 Uiso 1 1 calc R . .
C25 C 0.8330(5) 1.0175(3) 1.0896(2) 0.0490(8) Uani 1 1 d . . .
H25 H 0.8860 1.0457 1.1619 0.059 Uiso 1 1 calc R . .
C26 C 0.8062(3) 0.7602(2) 0.8865(2) 0.0294(5) Uani 1 1 d . . .
N1 N 0.8412(3) 0.61282(18) 0.56804(18) 0.0286(4) Uani 1 1 d . . .
N2 N 1.2119(4) 0.8926(2) 0.5170(2) 0.0448(7) Uani 1 1 d . . .
H2 H 1.145(5) 0.871(3) 0.447(3) 0.060(11) Uiso 1 1 d . . .
N3 N 0.5215(3) 1.45729(18) 1.22016(18) 0.0286(4) Uani 1 1 d . . .
N4 N 0.7081(3) 1.18277(19) 1.07838(18) 0.0338(5) Uani 1 1 d . . .
H4A H 0.7115 1.1893 1.1475 0.041 Uiso 1 1 calc R . .
O1 O 1.2602(3) 0.84625(17) 0.69117(15) 0.0417(5) Uani 1 1 d . . .
O2 O 1.5215(2) 1.37248(16) 0.45385(18) 0.0368(4) Uani 1 1 d . . .
O3 O 1.6180(2) 1.37867(15) 0.63406(16) 0.0344(4) Uani 1 1 d . . .
O4 O 0.6757(3) 1.27434(19) 0.92875(16) 0.0450(5) Uani 1 1 d . . .
O5 O 0.7509(2) 0.73472(15) 0.78418(14) 0.0324(4) Uani 1 1 d . . .
O6 O 0.8777(3) 0.69782(19) 0.94751(17) 0.0552(7) Uani 1 1 d . . .
O7 O 0.8975(3) 0.52607(18) 0.80074(17) 0.0438(5) Uani 1 1 d . . .
O8 O 0.0575(3) 0.6895(2) 0.15014(19) 0.0492(5) Uani 1 1 d . . .
O9 O 0.9598(9) 0.8598(5) 0.3070(5) 0.0235(13) Uiso 0.26 1 d P . 1
O9A O 0.8763(10) 0.8536(6) 0.3085(6) 0.0285(14) Uiso 0.24 1 d P . 2
O9B O 1.0236(5) 0.8485(3) 0.2976(3) 0.0331(8) Uiso 0.50 1 d P . 3
Cd1 Cd 0.670439(19) 0.564070(13) 0.675719(13) 0.02367(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
C1 N1 1.339(3) . ?
C1 C2 1.385(3) . ?
C2 C3 1.396(4) . ?
C2 C6 1.497(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.383(4) . ?
C5 N1 1.337(3) . ?
C6 O1 1.225(3) . ?
C6 N2 1.347(3) . ?
C7 C12 1.391(4) . ?
C7 C8 1.396(4) . ?
C7 N2 1.415(3) . ?
C8 C9 1.382(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.396(4) . ?
C10 C13 1.501(3) . ?
C11 C12 1.371(4) . ?
C13 O3 1.258(3) . ?
C13 O2 1.258(3) . ?
C14 N3 1.337(3) . ?
C14 C15 1.385(4) . ?
C15 C16 1.368(4) . ?
C16 C17 1.385(4) . ?
C17 C18 1.393(3) . ?
C17 C19 1.504(3) . ?
C18 N3 1.342(3) . ?
C19 O4 1.229(3) . ?
C19 N4 1.339(3) . ?
C20 C21 1.384(4) . ?
C20 C25 1.385(4) . ?
C20 N4 1.416(3) . ?
C21 C22 1.387(4) . ?
C22 C23 1.377(4) . ?
C23 C24 1.390(4) . ?
C23 C26 1.499(3) . ?
C24 C25 1.381(4) . ?
C26 O6 1.255(3) . ?
C26 O5 1.260(3) . ?
N1 Cd1 2.317(2) . ?
N3 Cd1 2.377(2) 2_677 ?
O2 Cd1 2.323(2) 2_776 ?
O3 Cd1 2.2371(18) 1_665 ?
O5 Cd1 2.3060(18) . ?
O7 Cd1 2.363(2) . ?
O9 O9 0.00(2) 1 ?
O9A O9A 0.00(2) 1 ?
O9B O9B 0.000(9) 1 ?
Cd1 O3 2.2371(18) 1_445 ?
Cd1 O2 2.323(2) 2_776 ?
Cd1 N3 2.377(2) 2_677 ?

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 122.7(2) . . ?
C1 C2 C3 118.3(2) . . ?
C1 C2 C6 118.5(2) . . ?
C3 C2 C6 123.1(2) . . ?
C4 C3 C2 118.7(2) . . ?
C3 C4 C5 119.4(2) . . ?
N1 C5 C4 122.2(2) . . ?
O1 C6 N2 124.9(2) . . ?
O1 C6 C2 122.4(2) . . ?
N2 C6 C2 112.6(2) . . ?
C12 C7 C8 119.5(2) . . ?
C12 C7 N2 115.9(2) . . ?
C8 C7 N2 124.7(2) . . ?
C9 C8 C7 119.4(3) . . ?
C8 C9 C10 121.2(3) . . ?
C9 C10 C11 118.7(2) . . ?
C9 C10 C13 121.9(2) . . ?
C11 C10 C13 119.5(2) . . ?
C12 C11 C10 120.6(2) . . ?
C11 C12 C7 120.6(3) . . ?
O3 C13 O2 124.2(2) . . ?
O3 C13 C10 116.6(2) . . ?
O2 C13 C10 119.3(2) . . ?
N3 C14 C15 123.0(2) . . ?
C16 C15 C14 119.1(2) . . ?
C15 C16 C17 119.1(2) . . ?
C16 C17 C18 118.3(2) . . ?
C16 C17 C19 118.9(2) . . ?
C18 C17 C19 122.3(2) . . ?
N3 C18 C17 122.8(2) . . ?
O4 C19 N4 124.3(3) . . ?
O4 C19 C17 118.3(2) . . ?
N4 C19 C17 117.5(2) . . ?
C21 C20 C25 119.2(2) . . ?
C21 C20 N4 122.2(2) . . ?
C25 C20 N4 118.6(2) . . ?
C20 C21 C22 119.7(3) . . ?
C23 C22 C21 121.7(2) . . ?
C22 C23 C24 118.2(2) . . ?
C22 C23 C26 120.9(2) . . ?
C24 C23 C26 121.0(2) . . ?
C25 C24 C23 120.7(3) . . ?
C24 C25 C20 120.6(3) . . ?
O6 C26 O5 123.9(2) . . ?
O6 C26 C23 119.4(2) . . ?
O5 C26 C23 116.6(2) . . ?
C5 N1 C1 118.6(2) . . ?
C5 N1 Cd1 121.08(17) . . ?
C1 N1 Cd1 120.32(17) . . ?
C6 N2 C7 129.9(2) . . ?
C14 N3 C18 117.6(2) . . ?
C14 N3 Cd1 121.10(17) . 2_677 ?
C18 N3 Cd1 120.51(16) . 2_677 ?
C19 N4 C20 125.1(2) . . ?
C13 O2 Cd1 140.55(17) . 2_776 ?
C13 O3 Cd1 123.29(17) . 1_665 ?
C26 O5 Cd1 131.35(17) . . ?
O3 Cd1 O5 158.11(7) 1_445 . ?
O3 Cd1 N1 102.81(7) 1_445 . ?
O5 Cd1 N1 90.14(7) . . ?
O3 Cd1 O2 103.90(7) 1_445 2_776 ?
O5 Cd1 O2 94.44(7) . 2_776 ?
N1 Cd1 O2 85.96(8) . 2_776 ?
O3 Cd1 O7 83.84(8) 1_445 . ?
O5 Cd1 O7 79.64(7) . . ?
N1 Cd1 O7 85.42(8) . . ?
O2 Cd1 O7 169.52(7) 2_776 . ?
O3 Cd1 N3 85.14(7) 1_445 2_677 ?
O5 Cd1 N3 84.11(7) . 2_677 ?
N1 Cd1 N3 170.26(7) . 2_677 ?
O2 Cd1 N3 86.65(8) 2_776 2_677 ?
O7 Cd1 N3 101.20(8) . 2_677 ?

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
N2 H2 O9B 0.93(4) 1.91(4) 2.834(5) 170(4) 1
N2 H2 O9 0.93(4) 2.09(4) 2.986(7) 163(4) 1
N2 H2 O9A 0.93(4) 2.56(4) 3.411(8) 152(3) 1
N4 H4A O1 0.86 2.09 2.918(3) 161.4 2_777

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.164
#
_vrf_PLAT306_cp1d                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O8 Check
RESPONSE: We could not locate hydrogen atoms associated with occluded water molecule (o8).
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989156'
#######################################################################
#
#                 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_cp1e

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 2yn'
_chemical_formula_moiety         'C26 H26 Cd N4 O10'
_chemical_formula_sum            'C26 H26 Cd N4 O10'
_chemical_formula_weight         666.91

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   'P 21/n'

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

_cell_length_a                   7.90160(10)
_cell_length_b                   12.7481(2)
_cell_length_c                   13.5560(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9350(10)
_cell_angle_gamma                90.00
_cell_volume                     1335.98(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_reflns_number            28656
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         32.99
_reflns_number_total             4653
_reflns_number_gt                3893
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0434P)²+0.3241P] 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         4653
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0777
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_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
C1 C 0.86788(19) 0.89705(12) 0.99990(10) 0.0307(3) Uani 1 1 d . . .
H1 H 0.8713 0.8965 1.0689 0.037 Uiso 1 1 calc R . .
C2 C 0.9847(2) 0.83597(14) 0.96265(12) 0.0357(3) Uani 1 1 d . . .
H2 H 1.0672 0.7966 1.0061 0.043 Uiso 1 1 calc R . .
C3 C 0.9771(2) 0.83411(13) 0.85991(12) 0.0338(3) Uani 1 1 d . . .
H3 H 1.0499 0.7903 0.8327 0.041 Uiso 1 1 calc R . .
C4 C 0.85909(17) 0.89872(11) 0.79788(10) 0.0250(2) Uani 1 1 d . . .
C5 C 0.74977(17) 0.95985(11) 0.84200(10) 0.0253(2) Uani 1 1 d . . .
H5 H 0.6729 1.0048 0.8012 0.030 Uiso 1 1 calc R . .
C6 C 0.83585(18) 0.89320(11) 0.68570(10) 0.0271(3) Uani 1 1 d . . .
C7 C 0.7787(2) 1.00538(10) 0.53297(12) 0.0260(3) Uani 1 1 d . . .
C8 C 0.7448(3) 0.92764(13) 0.45985(12) 0.0447(4) Uani 1 1 d . . .
H8 H 0.7467 0.8575 0.4788 0.054 Uiso 1 1 calc R . .
C9 C 0.7082(3) 0.95442(13) 0.35892(12) 0.0430(4) Uani 1 1 d . . .
H9 H 0.6882 0.9016 0.3106 0.052 Uiso 1 1 calc R . .
C10 C 0.70076(19) 1.05813(11) 0.32828(10) 0.0264(3) Uani 1 1 d . . .
C11 C 0.7348(3) 1.13522(12) 0.40150(12) 0.0385(4) Uani 1 1 d . . .
H11 H 0.7313 1.2054 0.3825 0.046 Uiso 1 1 calc R . .
C12 C 0.7742(3) 1.10910(12) 0.50265(11) 0.0391(4) Uani 1 1 d . . .
H12 H 0.7978 1.1619 0.5509 0.047 Uiso 1 1 calc R . .
C13 C 0.65699(18) 1.08519(12) 0.21812(10) 0.0274(3) Uani 1 1 d . . .
N1 N 0.75017(16) 0.95693(10) 0.94065(8) 0.0273(2) Uani 1 1 d . . .
N2 N 0.8184(2) 0.98585(9) 0.63785(10) 0.0285(3) Uani 1 1 d . . .
H2A H 0.8333 1.0405 0.6759 0.034 Uiso 1 1 calc R . .
O1 O 0.5273(2) 1.17954(10) 0.98916(10) 0.0417(3) Uani 1 1 d . . .
H14 H 0.572(3) 1.194(2) 1.045(2) 0.055(7) Uiso 1 1 d . . .
H15 H 0.569(3) 1.218(2) 0.950(2) 0.061(7) Uiso 1 1 d . . .
O2 O 0.6525(2) 1.00898(8) 0.15787(10) 0.0354(3) Uani 1 1 d . . .
O3 O 0.62584(17) 1.17890(9) 0.19240(8) 0.0385(3) Uani 1 1 d . . .
O4 O 0.82823(19) 0.80626(9) 0.64471(9) 0.0424(3) Uani 1 1 d . . .
O5 O 0.4045(2) 0.32706(11) 0.25909(11) 0.0479(3) Uani 1 1 d . . .
H16 H 0.470(4) 0.287(2) 0.242(2) 0.078(9) Uiso 1 1 d . . .
H17 H 0.331(3) 0.290(2) 0.287(2) 0.065(8) Uiso 1 1 d . . .
Cd1 Cd 0.5000 1.0000 1.0000 0.02455(5) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3356(19) . ?
C1 C2 1.380(2) . ?
C2 C3 1.382(2) . ?
C3 C4 1.390(2) . ?
C4 C5 1.3875(18) . ?
C4 C6 1.4952(18) . ?
C5 N1 1.3372(16) . ?
C6 O4 1.2356(17) . ?
C6 N2 1.3408(18) . ?
C7 C12 1.383(2) . ?
C7 C8 1.388(2) . ?
C7 N2 1.413(2) . ?
C8 C9 1.381(2) . ?
C9 C10 1.383(2) . ?
C10 C11 1.383(2) . ?
C10 C13 1.5016(19) . ?
C11 C12 1.382(2) . ?
C13 O3 1.2546(18) . ?
C13 O2 1.2650(17) . ?
N1 Cd1 2.3482(11) . ?
O1 Cd1 2.3065(13) . ?
O2 Cd1 2.2311(13) 1_554 ?
Cd1 O2 2.2311(13) 3_676 ?
Cd1 O2 2.2311(13) 1_556 ?
Cd1 O1 2.3065(13) 3_677 ?
Cd1 N1 2.3482(12) 3_677 ?

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 122.51(13) . . ?
C1 C2 C3 119.06(14) . . ?
C2 C3 C4 118.90(14) . . ?
C5 C4 C3 118.15(12) . . ?
C5 C4 C6 120.56(12) . . ?
C3 C4 C6 120.89(12) . . ?
N1 C5 C4 122.86(13) . . ?
O4 C6 N2 125.59(13) . . ?
O4 C6 C4 118.94(13) . . ?
N2 C6 C4 115.42(12) . . ?
C12 C7 C8 118.75(14) . . ?
C12 C7 N2 117.02(12) . . ?
C8 C7 N2 124.23(12) . . ?
C9 C8 C7 120.05(15) . . ?
C8 C9 C10 121.39(15) . . ?
C11 C10 C9 118.27(13) . . ?
C11 C10 C13 121.41(13) . . ?
C9 C10 C13 120.32(13) . . ?
C12 C11 C10 120.74(14) . . ?
C11 C12 C7 120.78(14) . . ?
O3 C13 O2 125.04(13) . . ?
O3 C13 C10 119.12(12) . . ?
O2 C13 C10 115.83(13) . . ?
C1 N1 C5 118.33(12) . . ?
C1 N1 Cd1 117.29(9) . . ?
C5 N1 Cd1 120.54(9) . . ?
C6 N2 C7 128.40(12) . . ?
C13 O2 Cd1 126.61(10) . 1_554 ?
O2 Cd1 O2 180.000 3_676 1_556 ?
O2 Cd1 O1 91.65(5) 3_676 . ?
O2 Cd1 O1 88.35(5) 1_556 . ?
O2 Cd1 O1 88.35(5) 3_676 3_677 ?
O2 Cd1 O1 91.65(5) 1_556 3_677 ?
O1 Cd1 O1 180.00 . 3_677 ?
O2 Cd1 N1 89.15(5) 3_676 . ?
O2 Cd1 N1 90.85(5) 1_556 . ?
O1 Cd1 N1 96.54(5) . . ?
O1 Cd1 N1 83.46(5) 3_677 . ?
O2 Cd1 N1 90.85(5) 3_676 3_677 ?
O2 Cd1 N1 89.15(5) 1_556 3_677 ?
O1 Cd1 N1 83.46(5) . 3_677 ?
O1 Cd1 N1 96.54(5) 3_677 3_677 ?
N1 Cd1 N1 180.0 . 3_677 ?

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
N2 H2A O5 0.86 2.04 2.8966(18) 171.0 4_676
O1 H14 O3 0.79(3) 1.96(3) 2.7037(17) 156(3) 1_556
O1 H15 O4 0.84(3) 2.00(3) 2.8396(18) 179(3) 2_656
O5 H16 O3 0.80(3) 2.05(3) 2.845(2) 176(3) 1_545
O5 H17 O4 0.89(3) 2.11(3) 2.994(2) 176(2) 3_666

_diffrn_measured_fraction_theta_max 0.925
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.139
_database_code_depnum_ccdc_archive 'CCDC 989157'
#######################################################################
#
#                 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_cp1f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 2yn'
_chemical_formula_moiety         'C26 H26 Fe N4 O10'
_chemical_formula_sum            'C26 H26 Fe N4 O10'
_chemical_formula_weight         610.36

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   7.7788(3)
_cell_length_b                   12.5459(4)
_cell_length_c                   13.3501(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4830(10)
_cell_angle_gamma                90.00
_cell_volume                     1276.79(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19371
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         32.18
_reflns_number_total             4090
_reflns_number_gt                3540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0622P)²+0.4240P] 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         4090
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2495(2) 0.57616(10) -0.04657(10) 0.0170(3) Uani 1 1 d . . .
H1 H 0.2535 0.6476 -0.0277 0.020 Uiso 1 1 calc R . .
C2 C 0.21242(19) 0.54775(10) -0.14930(10) 0.0162(3) Uani 1 1 d . . .
H2 H 0.1924 0.6008 -0.1989 0.019 Uiso 1 1 calc R . .
C3 C 0.20464(17) 0.44133(10) -0.17931(9) 0.0115(2) Uani 1 1 d . . .
C4 C 0.23791(19) 0.36247(10) -0.10420(10) 0.0158(3) Uani 1 1 d . . .
H4 H 0.2340 0.2910 -0.1230 0.019 Uiso 1 1 calc R . .
C5 C 0.27664(19) 0.39007(10) -0.00185(10) 0.0160(3) Uani 1 1 d . . .
H5 H 0.3002 0.3369 0.0476 0.019 Uiso 1 1 calc R . .
C6 C 0.28068(19) 0.49666(9) 0.02803(10) 0.0117(2) Uani 1 1 d . . .
C7 C 0.32882(17) 0.61001(10) 0.18375(9) 0.0113(2) Uani 1 1 d . . .
C8 C 0.35193(17) 0.60275(10) 0.29750(9) 0.0110(2) Uani 1 1 d . . .
C9 C 0.46985(18) 0.66952(10) 0.36051(10) 0.0148(2) Uani 1 1 d . . .
H9 H 0.5414 0.7159 0.3330 0.018 Uiso 1 1 calc R . .
C10 C 0.47820(18) 0.66526(11) 0.46518(10) 0.0153(2) Uani 1 1 d . . .
H10 H 0.5614 0.7050 0.5095 0.018 Uiso 1 1 calc R . .
C11 C 0.36070(18) 0.60093(10) 0.50273(9) 0.0135(2) Uani 1 1 d . . .
H11 H 0.3652 0.5998 0.5729 0.016 Uiso 1 1 calc R . .
C12 C 0.24209(17) 0.53840(10) 0.34197(9) 0.0116(2) Uani 1 1 d . . .
H12 H 0.1663 0.4921 0.3003 0.014 Uiso 1 1 calc R . .
C13 C 0.15767(17) 0.41223(10) -0.29032(9) 0.0116(2) Uani 1 1 d . . .
N1 N 0.24061(15) 0.54015(9) 0.44232(8) 0.0123(2) Uani 1 1 d . . .
N2 N 0.31797(16) 0.51616(8) 0.13443(8) 0.0123(2) Uani 1 1 d . . .
H2A H 0.3361 0.4605 0.1727 0.015 Uiso 1 1 calc R . .
O1 O 0.12948(14) 0.31598(7) -0.31494(7) 0.0162(2) Uani 1 1 d . . .
O2 O 0.14627(14) 0.48911(7) -0.35347(7) 0.01357(19) Uani 1 1 d . . .
O3 O 0.02027(14) 0.33084(8) 0.48238(7) 0.0159(2) Uani 1 1 d . . .
H3 H 0.0551 0.3034 0.5385 0.024 Uiso 1 1 calc R . .
H3A H 0.070(3) 0.2951(18) 0.4436(17) 0.033(5) Uiso 1 1 d . . .
O4 O 0.31597(14) 0.69959(7) 0.14292(7) 0.0170(2) Uani 1 1 d . . .
O5 O 0.08917(16) 0.83131(8) 0.24258(8) 0.0194(2) Uani 1 1 d . . .
H14 H 0.163(3) 0.7956(18) 0.2206(17) 0.036(6) Uiso 1 1 d . . .
H13 H 0.022(3) 0.7913(18) 0.2583(16) 0.031(6) Uiso 1 1 d . . .
Fe1 Fe 0.0000 0.5000 0.5000 0.01018(9) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3906(17) . ?
C1 C6 1.3961(17) . ?
C2 C3 1.3917(18) . ?
C3 C4 1.3957(17) . ?
C3 C13 1.4991(17) . ?
C4 C5 1.3833(17) . ?
C5 C6 1.3940(16) . ?
C6 N2 1.4134(16) . ?
C7 O4 1.2444(15) 1 ?
C7 O4 1.2444(15) . ?
C7 N2 1.3435(15) . ?
C7 C8 1.4961(16) . ?
C8 C12 1.3915(17) . ?
C8 C9 1.3941(18) . ?
C9 C10 1.3870(18) . ?
C10 C11 1.3858(18) . ?
C11 N1 1.3434(17) . ?
C12 N1 1.3422(15) . ?
C13 O1 1.2592(15) . ?
C13 O2 1.2724(15) . ?
N1 Fe1 2.2189(11) . ?
O2 Fe1 2.0625(10) 1_554 ?
O3 Fe1 2.1445(10) . ?
Fe1 O2 2.0625(10) 1_556 ?
Fe1 O2 2.0625(10) 3_565 ?
Fe1 O3 2.1445(10) 3_566 ?
Fe1 N1 2.2189(11) 3_566 ?

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
C2 C1 C6 119.53(12) . . ?
C1 C2 C3 121.22(12) . . ?
C2 C3 C4 118.82(11) . . ?
C2 C3 C13 120.41(11) . . ?
C4 C3 C13 120.76(11) . . ?
C5 C4 C3 120.33(11) . . ?
C4 C5 C6 120.72(12) . . ?
C5 C6 C1 119.36(11) . . ?
C5 C6 N2 116.23(11) . . ?
C1 C6 N2 124.40(11) . . ?
O4 C7 N2 125.82(11) 1 . ?
O4 C7 N2 125.82(11) . . ?
O4 C7 C8 118.85(11) 1 . ?
O4 C7 C8 118.85(11) . . ?
N2 C7 C8 115.29(10) . . ?
C12 C8 C9 118.52(11) . . ?
C12 C8 C7 120.56(11) . . ?
C9 C8 C7 120.50(11) . . ?
C10 C9 C8 118.55(12) . . ?
C11 C10 C9 119.01(12) . . ?
N1 C11 C10 122.91(11) . . ?
N1 C12 C8 122.98(12) . . ?
O1 C13 O2 124.64(11) . . ?
O1 C13 C3 119.15(11) . . ?
O2 C13 C3 116.20(11) . . ?
C11 N1 C12 117.73(11) . . ?
C11 N1 Fe1 117.02(8) . . ?
C12 N1 Fe1 121.21(9) . . ?
C7 N2 C6 128.64(10) . . ?
C13 O2 Fe1 129.14(8) . 1_554 ?
O2 Fe1 O2 180.00 1_556 3_565 ?
O2 Fe1 O3 90.02(4) 1_556 3_566 ?
O2 Fe1 O3 89.99(4) 3_565 3_566 ?
O2 Fe1 O3 89.99(4) 1_556 . ?
O2 Fe1 O3 90.01(4) 3_565 . ?
O3 Fe1 O3 180.0 3_566 . ?
O2 Fe1 N1 90.00(4) 1_556 3_566 ?
O2 Fe1 N1 90.00(4) 3_565 3_566 ?
O3 Fe1 N1 95.80(4) 3_566 3_566 ?
O3 Fe1 N1 84.20(4) . 3_566 ?
O2 Fe1 N1 90.00(4) 1_556 . ?
O2 Fe1 N1 90.00(4) 3_565 . ?
O3 Fe1 N1 84.20(4) 3_566 . ?
O3 Fe1 N1 95.80(4) . . ?
N1 Fe1 N1 180.0 3_566 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H13 O1 0.78(2) 2.03(2) 2.8098(15) 173(2) 3_565
O5 H14 O4 0.83(2) 2.10(2) 2.9237(15) 170(2) 1
O3 H3A O4 0.83(2) 1.99(2) 2.8250(14) 175(2) 2_545
O3 H3 O1 0.82 1.93 2.6763(13) 150.3 1_556
N2 H2A O5 0.86 2.00 2.8502(15) 172.3 2_545

_diffrn_measured_fraction_theta_max 0.908
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.106
_database_code_depnum_ccdc_archive 'CCDC 989158'
#######################################################################
#
#                 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_cp2a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 2ybc'
_chemical_formula_moiety         'C26 H30 Cu N4 O12'
_chemical_formula_sum            'C26 H30 Cu N4 O12'
_chemical_formula_weight         654.08

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

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/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                   8.8359(6)
_cell_length_b                   19.4935(13)
_cell_length_c                   8.0415(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.394(2)
_cell_angle_gamma                90.00
_cell_volume                     1376.47(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24406
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         32.25
_reflns_number_total             4462
_reflns_number_gt                3541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0718P)²+0.6916P] 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         4462
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1165(2) 0.36442(9) 0.5942(2) 0.0114(3) Uani 1 1 d . . .
C2 C 0.2500(2) 0.32001(9) 0.6567(2) 0.0109(3) Uani 1 1 d . . .
C3 C 0.2396(2) 0.24883(10) 0.6395(3) 0.0149(4) Uani 1 1 d . . .
H3 H 0.1502 0.2289 0.5896 0.018 Uiso 1 1 calc R . .
C4 C 0.3633(2) 0.20785(10) 0.6971(3) 0.0174(4) Uani 1 1 d . . .
H4 H 0.3573 0.1605 0.6835 0.021 Uiso 1 1 calc R . .
C5 C 0.4961(2) 0.23736(10) 0.7749(3) 0.0155(4) Uani 1 1 d . . .
H5 H 0.5780 0.2098 0.8152 0.019 Uiso 1 1 calc R . .
C6 C 0.5058(2) 0.30831(9) 0.7923(2) 0.0115(3) Uani 1 1 d . . .
C7 C 0.3837(2) 0.34998(9) 0.7321(2) 0.0109(3) Uani 1 1 d . . .
H7 H 0.3914 0.3974 0.7420 0.013 Uiso 1 1 calc R . .
C8 C 0.6588(2) 0.38973(9) 0.9756(2) 0.0111(3) Uani 1 1 d . . .
C9 C 0.8188(2) 0.40810(9) 1.0420(2) 0.0105(3) Uani 1 1 d . . .
C10 C 0.9456(2) 0.39546(9) 0.9583(2) 0.0125(3) Uani 1 1 d . . .
H10 H 0.9346 0.3752 0.8530 0.015 Uiso 1 1 calc R . .
C13 C 0.8410(2) 0.44075(9) 1.1965(2) 0.0117(3) Uani 1 1 d . . .
H13 H 0.7561 0.4523 1.2495 0.014 Uiso 1 1 calc R . .
C12 C 1.1024(2) 0.44239(9) 1.1929(2) 0.0131(4) Uani 1 1 d . . .
H12 H 1.1988 0.4525 1.2459 0.016 Uiso 1 1 calc R . .
C11 C 1.0895(2) 0.41359(9) 1.0348(2) 0.0132(4) Uani 1 1 d . . .
H11 H 1.1755 0.4064 0.9802 0.016 Uiso 1 1 calc R . .
N1 N 0.64575(18) 0.33606(8) 0.8679(2) 0.0126(3) Uani 1 1 d . . .
H1 H 0.7285 0.3173 0.8432 0.015 Uiso 1 1 calc R . .
N2 N 0.97973(18) 0.45630(8) 1.27244(19) 0.0115(3) Uani 1 1 d . . .
O1 O 0.14204(16) 0.42860(7) 0.58939(17) 0.0140(3) Uani 1 1 d . . .
O2 O -0.01130(15) 0.33673(7) 0.55444(18) 0.0146(3) Uani 1 1 d . . .
O3 O 0.54953(17) 0.42149(7) 1.01961(18) 0.0168(3) Uani 1 1 d . . .
O4 O 0.86829(18) 0.25785(8) 0.2781(2) 0.0184(3) Uani 1 1 d . . .
H17 H 0.918(4) 0.2394(17) 0.213(4) 0.036(9) Uiso 1 1 d . . .
H16 H 0.915(4) 0.2817(17) 0.347(4) 0.037(9) Uiso 1 1 d . . .
O6 O 0.4629(2) 0.48783(9) 0.3021(2) 0.0285(4) Uani 1 1 d . . .
O5 O 0.2475(2) 0.56390(9) 0.4552(2) 0.0269(4) Uani 1 1 d . . .
H14 H 0.298(4) 0.5544(18) 0.376(4) 0.045(10) Uiso 1 1 d . . .
H15 H 0.203(4) 0.602(2) 0.427(4) 0.054(11) Uiso 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.01187(11) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.260(2) . ?
C1 O1 1.273(2) . ?
C1 C2 1.504(3) . ?
C2 C7 1.395(3) . ?
C2 C3 1.396(2) . ?
C3 C4 1.391(3) . ?
C4 C5 1.391(3) . ?
C5 C6 1.392(3) . ?
C6 C7 1.393(3) . ?
C6 N1 1.422(2) . ?
C8 O3 1.231(2) . ?
C8 N1 1.355(2) . ?
C8 C9 1.498(3) . ?
C9 C10 1.391(3) . ?
C9 C13 1.391(2) . ?
C10 C11 1.394(3) . ?
C13 N2 1.342(2) . ?
C12 N2 1.346(2) . ?
C12 C11 1.383(3) . ?
N2 Cu1 2.0083(15) 1_656 ?
O1 Cu1 1.9565(13) . ?
Cu1 O1 1.9565(13) 3_566 ?
Cu1 N2 2.0083(15) 1_454 ?
Cu1 N2 2.0083(15) 3_667 ?

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
O2 C1 O1 124.77(17) . . ?
O2 C1 C2 119.06(16) . . ?
O1 C1 C2 116.15(16) . . ?
C7 C2 C3 120.19(17) . . ?
C7 C2 C1 119.95(16) . . ?
C3 C2 C1 119.86(17) . . ?
C4 C3 C2 119.79(18) . . ?
C5 C4 C3 120.29(18) . . ?
C4 C5 C6 119.72(18) . . ?
C5 C6 C7 120.49(17) . . ?
C5 C6 N1 117.51(17) . . ?
C7 C6 N1 121.96(16) . . ?
C6 C7 C2 119.50(17) . . ?
O3 C8 N1 123.95(18) . . ?
O3 C8 C9 121.11(16) . . ?
N1 C8 C9 114.94(16) . . ?
C10 C9 C13 118.18(17) . . ?
C10 C9 C8 124.37(16) . . ?
C13 C9 C8 117.45(16) . . ?
C9 C10 C11 119.04(17) . . ?
N2 C13 C9 122.72(18) . . ?
N2 C12 C11 122.04(17) . . ?
C12 C11 C10 119.08(18) . . ?
C8 N1 C6 125.06(16) . . ?
C13 N2 C12 118.78(16) . . ?
C13 N2 Cu1 119.64(13) . 1_656 ?
C12 N2 Cu1 121.58(12) . 1_656 ?
C1 O1 Cu1 127.00(13) . . ?
O1 Cu1 O1 180.00 3_566 . ?
O1 Cu1 N2 88.77(6) 3_566 1_454 ?
O1 Cu1 N2 91.23(6) . 1_454 ?
O1 Cu1 N2 91.23(6) 3_566 3_667 ?
O1 Cu1 N2 88.77(6) . 3_667 ?
N2 Cu1 N2 180.0 1_454 3_667 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H15 O2 0.85(4) 2.10(4) 2.842(2) 146(3) 3_566
O5 H14 O6 0.84(4) 2.08(4) 2.803(3) 143(3) 1
O4 H16 O2 0.80(3) 2.03(4) 2.812(2) 165(3) 1_655
O4 H17 O2 0.80(4) 2.10(4) 2.862(2) 159(3) 4_665
N1 H1 O4 0.86 2.02 2.838(2) 157.9 4_566

_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.302
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.229
#
_vrf_PLAT306_cp2a                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O6 Check
RESPONSE: Despite our best effort we could not locate hydrogen atoms associated with solvent water molecule (O6).
;
_vrf_PLAT232_cp2a                
;
PROBLEM: Hirshfeld Test Diff (M-X) Cu1 -- O5 .. 11.1 su           
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form 
_database_code_depnum_ccdc_archive 'CCDC 989159'
#######################################################################
#
#                 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_cp2b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 2yn'
_chemical_formula_moiety         'C26 H26 Cu N4 O10'
_chemical_formula_sum            'C26 H26 Cu N4 O10'
_chemical_formula_weight         618.05

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   9.0273(8)
_cell_length_b                   9.6688(8)
_cell_length_c                   15.3406(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.176(3)
_cell_angle_gamma                90.00
_cell_volume                     1321.84(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             638
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8011
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16730
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         30.03
_reflns_number_total             3543
_reflns_number_gt                2501
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0731P)²+3.6079P] 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         3543
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1359
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8647(4) 0.7230(4) 0.9790(2) 0.0180(7) Uani 1 1 d . . .
H1 H 0.8318 0.7598 0.9233 0.022 Uiso 1 1 calc R . .
C2 C 0.8124(4) 0.5934(4) 0.9984(2) 0.0175(7) Uani 1 1 d . . .
C3 C 0.8659(5) 0.5364(4) 1.0806(3) 0.0197(8) Uani 1 1 d . . .
H3 H 0.8342 0.4493 1.0958 0.024 Uiso 1 1 calc R . .
C4 C 0.9672(5) 0.6114(4) 1.1396(3) 0.0212(8) Uani 1 1 d . . .
H4 H 1.0059 0.5748 1.1946 0.025 Uiso 1 1 calc R . .
C5 C 1.0104(4) 0.7424(4) 1.1154(3) 0.0202(8) Uani 1 1 d . . .
H5 H 1.0766 0.7934 1.1557 0.024 Uiso 1 1 calc R . .
C6 C 0.6965(4) 0.5314(3) 0.9286(3) 0.0188(8) Uani 1 1 d . . .
C7 C 0.5384(4) 0.3321(4) 0.8796(2) 0.0176(7) Uani 1 1 d . . .
C8 C 0.4530(4) 0.2301(4) 0.9123(3) 0.0179(7) Uani 1 1 d . . .
H8 H 0.4716 0.2068 0.9719 0.021 Uiso 1 1 calc R . .
C9 C 0.3401(4) 0.1632(4) 0.8557(3) 0.0202(8) Uani 1 1 d . . .
H9 H 0.2844 0.0940 0.8774 0.024 Uiso 1 1 calc R . .
C10 C 0.3096(4) 0.1988(4) 0.7668(3) 0.0178(7) Uani 1 1 d . . .
H10 H 0.2318 0.1557 0.7296 0.021 Uiso 1 1 calc R . .
C11 C 0.3964(4) 0.2995(3) 0.7337(2) 0.0157(7) Uani 1 1 d . . .
C12 C 0.5126(4) 0.3630(4) 0.7900(2) 0.0173(7) Uani 1 1 d . . .
H12 H 0.5736 0.4269 0.7675 0.021 Uiso 1 1 calc R . .
C13 C 0.3682(4) 0.3443(3) 0.6385(2) 0.0161(7) Uani 1 1 d . . .
N1 N 0.9597(4) 0.7977(3) 1.0360(2) 0.0185(7) Uani 1 1 d . . .
N2 N 0.6522(4) 0.4002(3) 0.9387(2) 0.0192(7) Uani 1 1 d . . .
H2 H 0.688(5) 0.366(5) 0.982(3) 0.022(12) Uiso 1 1 d . . .
O1 O 0.6446(4) 0.6023(3) 0.8645(2) 0.0340(8) Uani 1 1 d . . .
O2 O 0.4598(3) 0.4315(3) 0.61672(16) 0.0182(5) Uani 1 1 d . . .
O3 O 0.2557(3) 0.2964(3) 0.58782(17) 0.0195(6) Uani 1 1 d . . .
O4 O 1.2456(3) 0.9649(3) 1.0612(2) 0.0257(6) Uani 1 1 d . . .
O5 O 0.0308(4) 0.6363(3) 0.3590(2) 0.0329(7) Uani 1 1 d . . .
Cu1 Cu 1.0000 1.0000 1.0000 0.01294(18) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.335(5) . ?
C1 C2 1.388(5) . ?
C2 C3 1.391(5) . ?
C2 C6 1.498(5) . ?
C3 C4 1.384(5) . ?
C4 C5 1.394(5) . ?
C5 N1 1.342(5) . ?
C6 O1 1.229(4) . ?
C6 N2 1.346(5) . ?
C7 C12 1.388(5) . ?
C7 C8 1.394(5) . ?
C7 N2 1.419(5) . ?
C8 C9 1.389(5) . ?
C9 C10 1.391(5) . ?
C10 C11 1.395(5) . ?
C11 C12 1.391(5) . ?
C11 C13 1.505(5) . ?
C13 O3 1.264(4) . ?
C13 O2 1.263(4) . ?
N1 Cu1 2.080(3) . ?
O2 Cu1 1.996(2) 2_646 ?
O4 Cu1 2.291(3) . ?
Cu1 O2 1.996(2) 2_656 ?
Cu1 O2 1.996(2) 4_676 ?
Cu1 N1 2.080(3) 3_777 ?
Cu1 O4 2.291(3) 3_777 ?

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 123.6(3) . . ?
C1 C2 C3 118.1(3) . . ?
C1 C2 C6 115.5(3) . . ?
C3 C2 C6 126.3(3) . . ?
C4 C3 C2 118.9(3) . . ?
C3 C4 C5 119.1(4) . . ?
N1 C5 C4 122.3(3) . . ?
O1 C6 N2 122.4(3) . . ?
O1 C6 C2 118.9(3) . . ?
N2 C6 C2 118.8(3) . . ?
C12 C7 C8 119.6(3) . . ?
C12 C7 N2 121.5(3) . . ?
C8 C7 N2 118.9(3) . . ?
C9 C8 C7 119.8(3) . . ?
C8 C9 C10 120.6(3) . . ?
C9 C10 C11 119.6(3) . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 C13 118.0(3) . . ?
C10 C11 C13 122.4(3) . . ?
C11 C12 C7 120.7(3) . . ?
O3 C13 O2 125.2(3) . . ?
O3 C13 C11 119.1(3) . . ?
O2 C13 C11 115.6(3) . . ?
C1 N1 C5 118.0(3) . . ?
C1 N1 Cu1 117.1(2) . . ?
C5 N1 Cu1 124.5(2) . . ?
C6 N2 C7 124.1(3) . . ?
C13 O2 Cu1 132.8(2) . 2_646 ?
O2 Cu1 O2 179.999 2_656 4_676 ?
O2 Cu1 N1 89.48(11) 2_656 . ?
O2 Cu1 N1 90.52(11) 4_676 . ?
O2 Cu1 N1 90.52(11) 2_656 3_777 ?
O2 Cu1 N1 89.48(11) 4_676 3_777 ?
N1 Cu1 N1 179.999 . 3_777 ?
O2 Cu1 O4 90.92(11) 2_656 . ?
O2 Cu1 O4 89.08(11) 4_676 . ?
N1 Cu1 O4 87.15(11) . . ?
N1 Cu1 O4 92.85(11) 3_777 . ?
O2 Cu1 O4 89.08(11) 2_656 3_777 ?
O2 Cu1 O4 90.92(11) 4_676 3_777 ?
N1 Cu1 O4 92.85(11) . 3_777 ?
N1 Cu1 O4 87.15(11) 3_777 3_777 ?
O4 Cu1 O4 180.000 . 3_777 ?

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
N2 H2 O3 0.76(5) 2.27(5) 3.006(4) 161(5) 4_666

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.998
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.150
#
_vrf_PLAT043_cp2b                
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by ..       8.06 Check
RESPONSE: We could not locate hydrogen atoms associated with both coordinated and occluded solvent water molecules(O4 and O6).
;
_vrf_PLAT306_cp2b                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check 
RESPONSE: We could not locate hydrogen atoms associated with solvate water molecule (O5).
;
_vrf_PLAT232_cp2b                
;
PROBLEM: Hirshfeld Test Diff (M-X) Cu1 -- N1 .. 6.9 su           
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989160'
#######################################################################
#
#                 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_cp2c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 2yn'
_chemical_formula_moiety         'C26 H26 Co N4 O10'
_chemical_formula_sum            'C26 H26 Co N4 O10'
_chemical_formula_weight         613.44

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           MONOCLINIC
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   8.7930(10)
_cell_length_b                   9.8082(11)
_cell_length_c                   15.5768(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.664(3)
_cell_angle_gamma                90.00
_cell_volume                     1320.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             634
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19416
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         32.11
_reflns_number_total             4287
_reflns_number_gt                4036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0401P)²+0.5538P] 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         4287
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.13222(10) 0.15903(9) 0.13767(5) 0.00874(14) Uani 1 1 d . . .
C2 C -0.10491(10) 0.20558(9) 0.23138(5) 0.00897(15) Uani 1 1 d . . .
C3 C -0.19672(10) 0.30515(9) 0.26088(6) 0.01032(15) Uani 1 1 d . . .
H3 H -0.2766 0.3467 0.2222 0.012 Uiso 1 1 calc R . .
C4 C -0.16721(10) 0.34148(9) 0.34882(6) 0.01128(16) Uani 1 1 d . . .
H4 H -0.2249 0.4104 0.3684 0.014 Uiso 1 1 calc R . .
C5 C -0.05227(10) 0.27558(9) 0.40772(6) 0.01070(15) Uani 1 1 d . . .
H5 H -0.0351 0.2990 0.4666 0.013 Uiso 1 1 calc R . .
C6 C 0.03733(10) 0.17418(9) 0.37823(6) 0.00982(15) Uani 1 1 d . . .
C7 C 0.01373(10) 0.14236(9) 0.28964(6) 0.01034(15) Uani 1 1 d . . .
H7 H 0.0772 0.0789 0.2693 0.012 Uiso 1 1 calc R . .
C8 C 0.19046(11) -0.02662(10) 0.43087(6) 0.01272(16) Uani 1 1 d . . .
C9 C 0.30951(10) -0.08902(9) 0.50113(6) 0.01057(15) Uani 1 1 d . . .
C10 C 0.36372(11) -0.03442(10) 0.58369(6) 0.01257(16) Uani 1 1 d . . .
H10 H 0.3307 0.0509 0.5988 0.015 Uiso 1 1 calc R . .
C11 C 0.46839(11) -0.11028(10) 0.64308(6) 0.01409(17) Uani 1 1 d . . .
H11 H 0.5077 -0.0757 0.6983 0.017 Uiso 1 1 calc R . .
C12 C 0.51333(10) -0.23846(10) 0.61870(6) 0.01276(16) Uani 1 1 d . . .
H12 H 0.5814 -0.2893 0.6591 0.015 Uiso 1 1 calc R . .
C13 C 0.36450(10) -0.21675(9) 0.48179(6) 0.01062(15) Uani 1 1 d . . .
H13 H 0.3313 -0.2517 0.4260 0.013 Uiso 1 1 calc R . .
N1 N 0.15136(9) 0.10529(8) 0.43973(5) 0.01112(14) Uani 1 1 d . . .
H1 H 0.1976 0.1496 0.4847 0.013 Uiso 1 1 calc R . .
N2 N 0.46228(9) -0.29183(8) 0.53895(5) 0.01022(14) Uani 1 1 d . . .
O1 O -0.03408(7) 0.07670(7) 0.11757(4) 0.01090(12) Uani 1 1 d . . .
O2 O -0.25154(8) 0.20141(7) 0.08591(4) 0.01181(13) Uani 1 1 d . . .
O3 O 0.13148(10) -0.09683(8) 0.36780(5) 0.02370(18) Uani 1 1 d . . .
O4 O 0.23367(8) -0.03207(8) 0.05272(5) 0.01392(13) Uani 1 1 d . . .
H14 H 0.2710 -0.0846 0.0213 0.021 Uiso 1 1 calc R . .
H15 H 0.305(2) 0.0222(18) 0.0764(12) 0.029(4) Uiso 1 1 d . . .
O5 O 0.45805(8) 0.13604(8) 0.13676(5) 0.01707(14) Uani 1 1 d . . .
H16 H 0.425(2) 0.222(2) 0.1355(13) 0.048(6) Uiso 1 1 d . . .
H17 H 0.558(2) 0.142(2) 0.1252(12) 0.041(5) Uiso 1 1 d . . .
Co1 Co 0.0000 0.0000 0.0000 0.00736(5) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.2629(11) . ?
C1 O2 1.2690(10) . ?
C1 C2 1.5057(12) . ?
C2 C7 1.3950(12) . ?
C2 C3 1.3978(12) . ?
C3 C4 1.3925(12) . ?
C4 C5 1.3921(12) . ?
C5 C6 1.3981(12) . ?
C6 C7 1.3925(12) . ?
C6 N1 1.4227(11) . ?
C8 O3 1.2328(12) . ?
C8 N1 1.3523(12) . ?
C8 C9 1.4980(12) . ?
C9 C10 1.3932(12) . ?
C9 C13 1.3957(12) . ?
C10 C11 1.3934(13) . ?
C11 C12 1.3915(13) . ?
C12 N2 1.3462(12) . ?
C13 N2 1.3383(11) . ?
N2 Co1 2.1729(8) 2_545 ?
O1 Co1 2.0525(7) . ?
O4 Co1 2.0906(7) . ?
O5 O5 0.000 1 ?
Co1 O1 2.0525(7) 3 ?
Co1 O4 2.0906(7) 3 ?
Co1 N2 2.1729(8) 4 ?
Co1 N2 2.1729(8) 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
O1 C1 O2 125.06(8) . . ?
O1 C1 C2 116.14(7) . . ?
O2 C1 C2 118.78(8) . . ?
C7 C2 C3 120.31(8) . . ?
C7 C2 C1 117.50(8) . . ?
C3 C2 C1 122.16(8) . . ?
C4 C3 C2 119.23(8) . . ?
C5 C4 C3 120.66(8) . . ?
C4 C5 C6 119.89(8) . . ?
C7 C6 C5 119.69(8) . . ?
C7 C6 N1 121.20(8) . . ?
C5 C6 N1 119.10(8) . . ?
C6 C7 C2 120.09(8) . . ?
O3 C8 N1 122.57(9) . . ?
O3 C8 C9 119.21(9) . . ?
N1 C8 C9 118.22(8) . . ?
C10 C9 C13 118.12(8) . . ?
C10 C9 C8 126.21(8) . . ?
C13 C9 C8 115.61(8) . . ?
C9 C10 C11 118.60(9) . . ?
C12 C11 C10 119.16(8) . . ?
N2 C12 C11 122.69(8) . . ?
N2 C13 C9 123.77(8) . . ?
C8 N1 C6 123.12(8) . . ?
C13 N2 C12 117.61(8) . . ?
C13 N2 Co1 116.34(6) . 2_545 ?
C12 N2 Co1 125.52(6) . 2_545 ?
C1 O1 Co1 132.44(6) . . ?
O1 Co1 O1 179.999 3 . ?
O1 Co1 O4 89.99(3) 3 3 ?
O1 Co1 O4 90.01(3) . 3 ?
O1 Co1 O4 90.01(3) 3 . ?
O1 Co1 O4 89.99(3) . . ?
O4 Co1 O4 180.0 3 . ?
O1 Co1 N2 87.69(3) 3 4 ?
O1 Co1 N2 92.31(3) . 4 ?
O4 Co1 N2 93.52(3) 3 4 ?
O4 Co1 N2 86.48(3) . 4 ?
O1 Co1 N2 92.31(3) 3 2 ?
O1 Co1 N2 87.69(3) . 2 ?
O4 Co1 N2 86.48(3) 3 2 ?
O4 Co1 N2 93.52(3) . 2 ?
N2 Co1 N2 180.0 4 2 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H17 O2 0.93(2) 1.97(2) 2.8823(10) 164.8(18) 1_655
O5 H16 O3 0.89(2) 1.84(2) 2.7329(12) 176(2) 2
O4 H15 O5 0.854(18) 1.863(18) 2.7146(10) 175.4(18) 1
O4 H14 O2 0.82 2.01 2.7518(10) 150.9 3
N1 H1 O2 0.86 2.14 2.9645(10) 161.8 4_666

_diffrn_measured_fraction_theta_max 0.925
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.059
#
_vrf_PLAT232_cp2c                
;
PROBLEM: Hirshfeld Test Diff (M-X) Co1 -- O4 .. 6.0 su           
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989161'
#######################################################################
#
#                 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_cp2d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-P 1'
_chemical_formula_moiety         'C27 H26 N4 O9 Zn'
_chemical_formula_sum            'C27 H26 N4 O9 Zn'
_chemical_formula_weight         615.89

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'
Zn Zn 0.2839 1.4301 '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                   10.6479(4)
_cell_length_b                   11.0165(5)
_cell_length_c                   12.9533(5)
_cell_angle_alpha                106.997(2)
_cell_angle_beta                 96.481(2)
_cell_angle_gamma                106.063(2)
_cell_volume                     1364.96(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4467
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48913
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         33.98
_reflns_number_total             8582
_reflns_number_gt                7322
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0611P)²+0.4927P] 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         8582
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
C1 C 0.63001(15) 0.59399(16) -0.39422(11) 0.0315(3) Uani 1 1 d . . .
H1 H 0.6363 0.5870 -0.4666 0.038 Uiso 1 1 calc R . .
C2 C 0.63390(17) 0.48765(16) -0.36002(12) 0.0348(3) Uani 1 1 d . . .
H2 H 0.6402 0.4099 -0.4090 0.042 Uiso 1 1 calc R . .
C3 C 0.62821(16) 0.49830(15) -0.25128(12) 0.0311(3) Uani 1 1 d . . .
H3 H 0.6312 0.4280 -0.2261 0.037 Uiso 1 1 calc R . .
C4 C 0.61804(13) 0.61567(14) -0.18074(10) 0.0253(2) Uani 1 1 d . . .
C5 C 0.61099(16) 0.71561(15) -0.22336(11) 0.0304(3) Uani 1 1 d . . .
H5 H 0.6012 0.7930 -0.1768 0.036 Uiso 1 1 calc R . .
C6 C 0.61650(14) 0.64568(14) -0.06023(11) 0.0270(2) Uani 1 1 d . . .
C7 C 0.68753(14) 0.58657(14) 0.10255(11) 0.0270(2) Uani 1 1 d . . .
C8 C 0.65127(14) 0.67791(14) 0.18255(11) 0.0274(3) Uani 1 1 d . . .
H8 H 0.6052 0.7307 0.1623 0.033 Uiso 1 1 calc R . .
C9 C 0.68416(15) 0.69027(14) 0.29354(11) 0.0279(3) Uani 1 1 d . A .
C10 C 0.75090(19) 0.61102(19) 0.32402(13) 0.0396(4) Uani 1 1 d . . .
H10 H 0.7742 0.6207 0.3981 0.048 Uiso 1 1 calc R . .
C11 C 0.7830(2) 0.5167(2) 0.24337(15) 0.0501(5) Uani 1 1 d . . .
H11 H 0.8254 0.4612 0.2634 0.060 Uiso 1 1 calc R . .
C12 C 0.7523(2) 0.50499(19) 0.13379(13) 0.0422(4) Uani 1 1 d . . .
H12 H 0.7749 0.4422 0.0804 0.051 Uiso 1 1 calc R . .
C14 C 0.92491(17) 0.98609(18) -0.33238(14) 0.0386(3) Uani 1 1 d . . .
H14 H 0.9123 0.9497 -0.4087 0.046 Uiso 1 1 calc R . .
C15 C 1.05336(17) 1.04557(19) -0.27036(15) 0.0443(4) Uani 1 1 d . . .
H15 H 1.1261 1.0484 -0.3042 0.053 Uiso 1 1 calc R . .
C16 C 1.07246(15) 1.10087(17) -0.15726(14) 0.0372(3) Uani 1 1 d . . .
H16 H 1.1584 1.1409 -0.1137 0.045 Uiso 1 1 calc R . .
C17 C 0.96211(14) 1.09616(14) -0.10908(12) 0.0287(3) Uani 1 1 d . . .
C18 C 0.83661(14) 1.03241(16) -0.17734(12) 0.0311(3) Uani 1 1 d . . .
H18 H 0.7622 1.0268 -0.1454 0.037 Uiso 1 1 calc R . .
C19 C 0.98686(14) 1.15367(16) 0.01434(12) 0.0322(3) Uani 1 1 d . . .
C20 C 0.87520(14) 1.19916(16) 0.17198(12) 0.0311(3) Uani 1 1 d . . .
C21 C 0.98721(16) 1.27736(18) 0.25592(14) 0.0396(3) Uani 1 1 d . . .
H20 H 1.0704 1.3077 0.2392 0.047 Uiso 1 1 calc R . .
C22 C 0.97309(18) 1.3095(2) 0.36494(15) 0.0474(4) Uani 1 1 d . . .
H21 H 1.0478 1.3613 0.4213 0.057 Uiso 1 1 calc R . .
C23 C 0.85034(18) 1.2661(2) 0.39139(13) 0.0429(4) Uani 1 1 d . . .
H22 H 0.8427 1.2886 0.4649 0.052 Uiso 1 1 calc R . .
C24 C 0.73803(15) 1.18844(16) 0.30749(12) 0.0321(3) Uani 1 1 d . . .
C25 C 0.75084(14) 1.15513(16) 0.19820(12) 0.0313(3) Uani 1 1 d . . .
H23 H 0.6760 1.1031 0.1421 0.038 Uiso 1 1 calc R . .
C26 C 0.60242(16) 1.14642(16) 0.33352(13) 0.0324(3) Uani 1 1 d . . .
C13 C 0.64391(17) 0.78922(16) 0.37900(12) 0.0336(3) Uani 1 1 d . . .
C27 C 0.8804(4) 0.3672(4) 0.8202(4) 0.1108(14) Uani 1 1 d . . .
H27A H 0.9260 0.4587 0.8278 0.166 Uiso 1 1 calc R . .
H27B H 0.8404 0.3165 0.7439 0.166 Uiso 1 1 calc R . .
H27C H 0.9432 0.3294 0.8465 0.166 Uiso 1 1 calc R . .
N1 N 0.61749(13) 0.70726(13) -0.32793(10) 0.0309(2) Uani 1 1 d . . .
N2 N 0.66520(14) 0.57105(13) -0.01101(9) 0.0294(2) Uani 1 1 d . . .
N3 N 0.81705(12) 0.97860(13) -0.28685(10) 0.0309(2) Uani 1 1 d . . .
N4 N 0.87872(12) 1.16203(15) 0.05863(10) 0.0351(3) Uani 1 1 d . . .
H4 H 0.8049 1.1428 0.0131 0.042 Uiso 1 1 calc R . .
O1 O 0.57653(14) 0.73603(14) -0.01152(9) 0.0423(3) Uani 1 1 d . . .
O4 O 1.09856(12) 1.18648(18) 0.06909(11) 0.0551(4) Uani 1 1 d . . .
O5 O 0.59079(13) 1.18987(13) 0.43258(10) 0.0399(3) Uani 1 1 d . . .
O6 O 0.50235(11) 1.07438(12) 0.25807(9) 0.0349(2) Uani 1 1 d . . .
O2 O 0.67648(14) 0.79387(13) 0.47760(9) 0.0412(3) Uani 1 1 d . . .
O3A O 0.6090(3) 0.8760(2) 0.3556(2) 0.0377(5) Uiso 0.53 1 d P A 1
O3B O 0.5546(3) 0.8356(3) 0.3435(2) 0.0370(5) Uiso 0.47 1 d P A 2
O7 O 0.63046(15) 1.07117(15) -0.39961(13) 0.0479(3) Uani 1 1 d . . .
H7A H 0.5629 1.0878 -0.3847 0.072 Uiso 1 1 calc R . .
H7B H 0.629(4) 1.073(4) -0.458(3) 0.098(12) Uiso 1 1 d . . .
O8 O 0.61175(16) 0.1432(2) 0.93236(15) 0.0662(5) Uani 1 1 d . . .
H8A H 0.559(4) 0.171(4) 0.970(3) 0.098(11) Uiso 1 1 d . . .
H8B H 0.562(3) 0.075(3) 0.877(3) 0.075(9) Uiso 1 1 d . . .
O9 O 0.7816(3) 0.3631(2) 0.88184(17) 0.0775(6) Uani 1 1 d . . .
Zn1 Zn 0.623201(17) 0.880574(17) -0.385992(12) 0.03008(6) Uani 1 1 d . . .
H9 H 0.725(4) 0.271(4) 0.866(3) 0.124(15) Uiso 1 1 d . . .
H2A H 0.691(2) 0.516(2) -0.0489(18) 0.041(5) 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
C1 N1 1.343(2) . ?
C1 C2 1.377(2) . ?
C2 C3 1.3884(19) . ?
C3 C4 1.3883(19) . ?
C4 C5 1.3835(19) . ?
C4 C6 1.5011(17) . ?
C5 N1 1.3417(17) . ?
C6 O1 1.2238(17) . ?
C6 N2 1.3488(19) . ?
C7 C8 1.3896(18) . ?
C7 C12 1.392(2) . ?
C7 N2 1.4147(16) . ?
C8 C9 1.3977(18) . ?
C9 C10 1.380(2) . ?
C9 C13 1.503(2) . ?
C10 C11 1.389(2) . ?
C11 C12 1.380(2) . ?
C14 N3 1.3426(19) . ?
C14 C15 1.376(2) . ?
C15 C16 1.379(2) . ?
C16 C17 1.3868(19) . ?
C17 C18 1.383(2) . ?
C17 C19 1.499(2) . ?
C18 N3 1.3344(18) . ?
C19 O4 1.2125(19) . ?
C19 N4 1.3566(19) . ?
C20 C21 1.392(2) . ?
C20 C25 1.3952(19) . ?
C20 N4 1.4121(18) . ?
C21 C22 1.388(2) . ?
C22 C23 1.380(3) . ?
C23 C24 1.393(2) . ?
C24 C25 1.3874(19) . ?
C24 C26 1.498(2) . ?
C26 O6 1.251(2) . ?
C26 O5 1.2652(18) . ?
C26 Zn1 2.5324(15) 2_675 ?
C13 O3A 1.219(3) . ?
C13 O2 1.2673(17) . ?
C13 O3B 1.297(3) . ?
C27 O9 1.390(4) . ?
N1 Zn1 2.2361(13) . ?
N3 Zn1 2.1055(13) . ?
O5 Zn1 2.1437(13) 2_675 ?
O6 Zn1 2.2728(11) 2_675 ?
O2 Zn1 1.9737(11) 1_556 ?
O7 Zn1 2.1390(14) . ?
Zn1 O2 1.9738(11) 1_554 ?
Zn1 O5 2.1438(13) 2_675 ?
Zn1 O6 2.2728(11) 2_675 ?
Zn1 C26 2.5324(15) 2_675 ?

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 123.08(13) . . ?
C1 C2 C3 118.99(14) . . ?
C2 C3 C4 118.85(14) . . ?
C5 C4 C3 118.03(12) . . ?
C5 C4 C6 116.34(12) . . ?
C3 C4 C6 125.62(13) . . ?
N1 C5 C4 123.79(13) . . ?
O1 C6 N2 123.73(12) . . ?
O1 C6 C4 120.25(13) . . ?
N2 C6 C4 115.98(12) . . ?
C8 C7 C12 119.36(13) . . ?
C8 C7 N2 124.32(13) . . ?
C12 C7 N2 116.31(12) . . ?
C7 C8 C9 119.83(13) . . ?
C10 C9 C8 120.39(13) . . ?
C10 C9 C13 120.42(12) . . ?
C8 C9 C13 119.18(13) . . ?
C9 C10 C11 119.57(14) . . ?
C12 C11 C10 120.35(16) . . ?
C11 C12 C7 120.44(15) . . ?
N3 C14 C15 122.48(15) . . ?
C14 C15 C16 118.96(14) . . ?
C15 C16 C17 119.30(15) . . ?
C18 C17 C16 117.95(14) . . ?
C18 C17 C19 124.22(12) . . ?
C16 C17 C19 117.72(13) . . ?
N3 C18 C17 123.19(13) . . ?
O4 C19 N4 123.55(15) . . ?
O4 C19 C17 119.88(14) . . ?
N4 C19 C17 116.54(12) . . ?
C21 C20 C25 119.85(14) . . ?
C21 C20 N4 123.51(13) . . ?
C25 C20 N4 116.63(13) . . ?
C22 C21 C20 119.11(15) . . ?
C23 C22 C21 121.30(16) . . ?
C22 C23 C24 119.67(15) . . ?
C25 C24 C23 119.63(14) . . ?
C25 C24 C26 119.54(14) . . ?
C23 C24 C26 120.76(14) . . ?
C24 C25 C20 120.44(13) . . ?
O6 C26 O5 120.92(14) . . ?
O6 C26 C24 120.48(13) . . ?
O5 C26 C24 118.54(15) . . ?
O6 C26 Zn1 63.65(8) . 2_675 ?
O5 C26 Zn1 57.76(8) . 2_675 ?
C24 C26 Zn1 169.71(11) . 2_675 ?
O3A C13 O2 122.96(17) . . ?
O3A C13 O3B 27.14(13) . . ?
O2 C13 O3B 125.49(17) . . ?
O3A C13 C9 119.83(16) . . ?
O2 C13 C9 115.42(14) . . ?
O3B C13 C9 116.85(17) . . ?
C5 N1 C1 117.22(13) . . ?
C5 N1 Zn1 121.41(10) . . ?
C1 N1 Zn1 121.21(9) . . ?
C6 N2 C7 127.77(12) . . ?
C18 N3 C14 118.10(13) . . ?
C18 N3 Zn1 121.31(10) . . ?
C14 N3 Zn1 120.58(11) . . ?
C19 N4 C20 126.50(13) . . ?
C26 O5 Zn1 92.29(10) . 2_675 ?
C26 O6 Zn1 86.81(9) . 2_675 ?
C13 O2 Zn1 131.42(11) . 1_556 ?
O2 Zn1 N3 97.02(5) 1_554 . ?
O2 Zn1 O7 102.27(6) 1_554 . ?
N3 Zn1 O7 86.49(5) . . ?
O2 Zn1 O5 102.99(5) 1_554 2_675 ?
N3 Zn1 O5 159.93(5) . 2_675 ?
O7 Zn1 O5 90.85(5) . 2_675 ?
O2 Zn1 N1 91.20(5) 1_554 . ?
N3 Zn1 N1 87.56(5) . . ?
O7 Zn1 N1 165.84(6) . . ?
O5 Zn1 N1 90.33(5) 2_675 . ?
O2 Zn1 O6 161.15(5) 1_554 2_675 ?
N3 Zn1 O6 100.61(4) . 2_675 ?
O7 Zn1 O6 85.52(5) . 2_675 ?
O5 Zn1 O6 59.33(4) 2_675 2_675 ?
N1 Zn1 O6 82.96(4) . 2_675 ?
O2 Zn1 C26 132.16(5) 1_554 2_675 ?
N3 Zn1 C26 130.07(5) . 2_675 ?
O7 Zn1 C26 90.15(5) . 2_675 ?
O5 Zn1 C26 29.94(5) 2_675 2_675 ?
N1 Zn1 C26 83.88(5) . 2_675 ?
O6 Zn1 C26 29.54(5) 2_675 2_675 ?

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
N2 H2A O9 0.79(2) 2.19(2) 2.968(2) 167(2) 1_554
O9 H9 O8 0.98(4) 2.04(4) 2.887(3) 144(3) 1
O8 H8B O6 0.86(3) 1.91(3) 2.750(2) 164(3) 2_666
O8 H8A O1 0.84(4) 2.03(4) 2.8253(19) 158(3) 2_666
O7 H7B O3A 0.76(4) 2.67(4) 3.210(3) 130(3) 1_554
O7 H7B O5 0.76(4) 2.25(4) 2.8937(18) 143(4) 1_554
O7 H7A O3A 0.82 2.03 2.849(3) 177.2 2_675
O7 H7A O3B 0.82 1.74 2.544(3) 165.7 2_675
N4 H4 O8 0.86 2.20 3.037(2) 163.8 1_564

_diffrn_measured_fraction_theta_max 0.771
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.079
#
_vrf_PLAT201_cp2d                
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Why ?  
RESPONSE: This is due to disordered carbonyl oxygen atom O3 over two positions.
;
_vrf_PLAT230_cp2d                
;
PROBLEM: Hirshfeld Test Diff for    O6     --  C26     ..        5.6 su  
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
_vrf_PLAT232_cp2d                
;
PROBLEM: Hirshfeld Test Diff (M-X) Zn1 -- N1 .. 9.3 su  
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989162'
#######################################################################
#
#                 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_cp2e

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-C 2yc'
_chemical_formula_moiety         'C28 H31 Cd N4 O11'
_chemical_formula_sum            'C28 H31 Cd N4 O11'
_chemical_formula_weight         711.97

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'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'C 2/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                   20.3394(16)
_cell_length_b                   10.1426(7)
_cell_length_c                   14.9680(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.500(5)
_cell_angle_gamma                90.00
_cell_volume                     2989.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5028
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_reflns_number            33276
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         34.06
_reflns_number_total             5412
_reflns_number_gt                4925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0365P)²+1.9860P] 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         5412
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.02447(6) 0.24002(13) -0.04706(9) 0.0236(2) Uani 1 1 d . . .
H1 H 0.0589 0.2790 -0.0687 0.028 Uiso 1 1 calc R . .
C2 C 0.01686(6) 0.27769(13) 0.03911(9) 0.0238(2) Uani 1 1 d . . .
C3 C -0.03476(7) 0.21954(16) 0.07153(10) 0.0299(3) Uani 1 1 d . . .
H3 H -0.0417 0.2432 0.1285 0.036 Uiso 1 1 calc R . .
C4 C -0.07540(8) 0.12588(15) 0.01708(11) 0.0316(3) Uani 1 1 d . . .
H4 H -0.1100 0.0849 0.0373 0.038 Uiso 1 1 calc R . .
C5 C -0.06424(7) 0.09355(14) -0.06784(10) 0.0265(3) Uani 1 1 d . . .
H5 H -0.0917 0.0300 -0.1037 0.032 Uiso 1 1 calc R . .
C6 C 0.05951(7) 0.38502(14) 0.09251(10) 0.0268(3) Uani 1 1 d . . .
C7 C 0.17581(6) 0.47690(14) 0.12660(9) 0.0252(2) Uani 1 1 d . . .
C8 C 0.24312(6) 0.43465(14) 0.14651(10) 0.0256(2) Uani 1 1 d . . .
H8 H 0.2527 0.3466 0.1379 0.031 Uiso 1 1 calc R . .
C9 C 0.29607(6) 0.52256(14) 0.17904(9) 0.0254(2) Uani 1 1 d . . .
C10 C 0.28167(7) 0.65416(17) 0.19222(12) 0.0356(3) Uani 1 1 d . . .
H10 H 0.3167 0.7135 0.2149 0.043 Uiso 1 1 calc R . .
C11 C 0.21487(8) 0.69598(16) 0.17128(14) 0.0410(4) Uani 1 1 d . . .
H11 H 0.2054 0.7843 0.1792 0.049 Uiso 1 1 calc R . .
C12 C 0.16160(8) 0.60905(15) 0.13866(13) 0.0343(3) Uani 1 1 d . . .
H12 H 0.1169 0.6387 0.1250 0.041 Uiso 1 1 calc R . .
C13 C 0.36810(6) 0.47447(15) 0.19977(9) 0.0267(3) Uani 1 1 d . . .
C14 C 0.34313(17) -0.0147(3) 0.1235(2) 0.0747(7) Uani 1 1 d . . .
N1 N -0.01521(5) 0.15065(12) -0.10029(8) 0.0234(2) Uani 1 1 d . . .
N2 N 0.12534(6) 0.38188(12) 0.09054(10) 0.0294(3) Uani 1 1 d . . .
H2 H 0.1421 0.3070 0.0705 0.035 Uiso 1 1 d R . .
O1 O 0.03397(6) 0.46869(14) 0.13210(10) 0.0478(3) Uani 1 1 d . . .
O2 O 0.41539(5) 0.55142(12) 0.23609(8) 0.0337(2) Uani 1 1 d . . .
O3 O 0.37911(6) 0.35668(13) 0.17965(10) 0.0400(3) Uani 1 1 d . . .
O4 O 0.0000 0.35106(18) -0.2500 0.0513(5) Uani 1 2 d S . .
H13 H -0.0050 0.3780 -0.2005 0.077 Uiso 0.50 1 calc PR . .
O5 O 0.17795(8) 0.14016(15) 0.03210(12) 0.0518(3) Uani 1 1 d . . .
H14 H 0.2130 0.1263 0.0557 0.078 Uiso 1 1 d R . .
H15 H 0.1711 0.1287 -0.0302 0.078 Uiso 1 1 d R . .
O6 O 0.31826(10) 0.11458(16) 0.10321(15) 0.0662(5) Uani 1 1 d . . .
H16 H 0.3431 0.1661 0.1411 0.099 Uiso 1 1 d R . .
Cd1 Cd 0.0000 0.113387(13) -0.2500 0.02238(5) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3363(17) . ?
C1 C2 1.3905(18) . ?
C2 C3 1.3932(18) . ?
C2 C6 1.4931(19) . ?
C3 C4 1.383(2) . ?
C4 C5 1.385(2) . ?
C5 N1 1.3448(17) . ?
C6 O1 1.2228(17) . ?
C6 N2 1.3471(17) . ?
C7 C12 1.392(2) . ?
C7 C8 1.3936(17) . ?
C7 N2 1.4130(17) . ?
C8 C9 1.3890(19) . ?
C9 C10 1.391(2) . ?
C9 C13 1.5009(18) . ?
C10 C11 1.382(2) . ?
C11 C12 1.387(2) . ?
C13 O2 1.2522(17) . ?
C13 O3 1.2657(19) 1 ?
C13 O3 1.2657(19) . ?
C13 Cd1 2.7472(13) 7 ?
C14 O6 1.411(3) 1 ?
C14 O6 1.411(3) . ?
N1 Cd1 2.3679(11) . ?
O2 Cd1 2.3706(11) 7 ?
O3 Cd1 2.4393(11) 7 ?
O4 Cd1 2.4107(18) . ?
Cd1 N1 2.3679(11) 2_554 ?
Cd1 O2 2.3705(11) 8_455 ?
Cd1 O2 2.3705(11) 7 ?
Cd1 O3 2.4393(11) 8_455 ?
Cd1 O3 2.4393(11) 7 ?
Cd1 C13 2.7472(13) 8_455 ?
Cd1 C13 2.7472(13) 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
N1 C1 C2 123.27(12) . . ?
C1 C2 C3 118.39(12) . . ?
C1 C2 C6 120.81(12) . . ?
C3 C2 C6 120.65(12) . . ?
C4 C3 C2 118.48(13) . . ?
C3 C4 C5 119.49(13) . . ?
N1 C5 C4 122.43(13) . . ?
O1 C6 N2 124.90(13) . . ?
O1 C6 C2 120.34(12) . . ?
N2 C6 C2 114.74(11) . . ?
C12 C7 C8 119.54(13) . . ?
C12 C7 N2 123.47(12) . . ?
C8 C7 N2 116.92(12) . . ?
C9 C8 C7 120.76(13) . . ?
C8 C9 C10 119.56(12) . . ?
C8 C9 C13 119.66(13) . . ?
C10 C9 C13 120.78(12) . . ?
C11 C10 C9 119.48(14) . . ?
C10 C11 C12 121.43(15) . . ?
C11 C12 C7 119.22(13) . . ?
O2 C13 O3 121.95(13) . 1 ?
O2 C13 O3 121.95(13) . . ?
O2 C13 C9 119.41(13) . . ?
O3 C13 C9 118.64(12) 1 . ?
O3 C13 C9 118.64(12) . . ?
O2 C13 Cd1 59.47(7) . 7 ?
O3 C13 Cd1 62.61(7) 1 7 ?
O3 C13 Cd1 62.61(7) . 7 ?
C9 C13 Cd1 176.17(9) . 7 ?
C1 N1 C5 117.93(12) . . ?
C1 N1 Cd1 118.04(8) . . ?
C5 N1 Cd1 123.88(9) . . ?
C6 N2 C7 127.34(12) . . ?
C13 O2 Cd1 93.47(9) . 7 ?
C13 O3 Cd1 89.95(8) . 7 ?
N1 Cd1 N1 161.63(6) . 2_554 ?
N1 Cd1 O2 86.08(4) . 8_455 ?
N1 Cd1 O2 107.06(4) 2_554 8_455 ?
N1 Cd1 O2 107.06(4) . 7 ?
N1 Cd1 O2 86.08(4) 2_554 7 ?
O2 Cd1 O2 90.32(5) 8_455 7 ?
N1 Cd1 O4 80.82(3) . . ?
N1 Cd1 O4 80.82(3) 2_554 . ?
O2 Cd1 O4 134.84(3) 8_455 . ?
O2 Cd1 O4 134.84(3) 7 . ?
N1 Cd1 O3 91.85(4) . 8_455 ?
N1 Cd1 O3 85.87(4) 2_554 8_455 ?
O2 Cd1 O3 54.46(4) 8_455 8_455 ?
O2 Cd1 O3 139.19(4) 7 8_455 ?
O4 Cd1 O3 82.85(3) . 8_455 ?
N1 Cd1 O3 85.87(4) . 7 ?
N1 Cd1 O3 91.85(4) 2_554 7 ?
O2 Cd1 O3 139.18(4) 8_455 7 ?
O2 Cd1 O3 54.46(4) 7 7 ?
O4 Cd1 O3 82.85(3) . 7 ?
O3 Cd1 O3 165.70(6) 8_455 7 ?
N1 Cd1 C13 87.75(4) . 8_455 ?
N1 Cd1 C13 98.21(4) 2_554 8_455 ?
O2 Cd1 C13 27.07(4) 8_455 8_455 ?
O2 Cd1 C13 115.66(4) 7 8_455 ?
O4 Cd1 C13 108.93(3) . 8_455 ?
O3 Cd1 C13 27.43(4) 8_455 8_455 ?
O3 Cd1 C13 165.53(5) 7 8_455 ?
N1 Cd1 C13 98.21(4) . 7 ?
N1 Cd1 C13 87.75(4) 2_554 7 ?
O2 Cd1 C13 115.66(4) 8_455 7 ?
O2 Cd1 C13 27.07(4) 7 7 ?
O4 Cd1 C13 108.93(3) . 7 ?
O3 Cd1 C13 165.54(5) 8_455 7 ?
O3 Cd1 C13 27.43(4) 7 7 ?
C13 Cd1 C13 142.15(6) 8_455 7 ?

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
O6 H16 O3 0.84 2.10 2.857(2) 150.2 1
O5 H15 O3 0.92 2.22 3.091(2) 158.9 7
O5 H14 O6 0.73 2.08 2.797(2) 167.8 1
O4 H13 O1 0.82 2.03 2.7467(17) 146.0 5_565
N2 H2 O5 0.91 1.98 2.8964(18) 177.3 1

_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.106
#
_vrf_PLAT230_cp2e                
;
PROBLEM: Hirshfeld Test Diff for    O3     --  C13     ..        6.5 su           
RESPONSE: We are chemically sure about the identity of the elements of the structure. 
Therefore this alart is definitely not due to the wrong assignment of the atoms .
However such alart could be due to the inadequate absorption correction applied by SADABS
of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989163'
#######################################################################
#
#                 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_cp2f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  '-C 2yc'
_chemical_formula_moiety         'C26 H28 Cd2 Cl2 N4 O11'
_chemical_formula_sum            'C26 H28 Cd2 Cl2 N4 O11'
_chemical_formula_weight         868.22

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   'C 2/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                   16.5778(8)
_cell_length_b                   16.9789(8)
_cell_length_c                   21.8040(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.606(2)
_cell_angle_gamma                90.00
_cell_volume                     6117.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3440
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_T_max  0.7804
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45949
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         32.18
_reflns_number_total             9876
_reflns_number_gt                7674
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0644P)²+10.9187P] 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     SHELXL
_refine_ls_extinction_coef       0.00055(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9876
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1171
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.46295(18) 0.19837(18) 0.32517(13) 0.0411(6) Uani 1 1 d . . .
H1 H 0.4309 0.1818 0.2906 0.049 Uiso 1 1 calc R . .
C2 C 0.4721(2) 0.27749(18) 0.33532(14) 0.0489(7) Uani 1 1 d . . .
H2 H 0.4471 0.3138 0.3081 0.059 Uiso 1 1 calc R . .
C3 C 0.51923(19) 0.30222(16) 0.38663(13) 0.0434(6) Uani 1 1 d . . .
H3 H 0.5265 0.3557 0.3945 0.052 Uiso 1 1 calc R . .
C4 C 0.55561(15) 0.24690(14) 0.42646(11) 0.0312(5) Uani 1 1 d . . .
C5 C 0.54324(15) 0.16801(14) 0.41244(11) 0.0328(5) Uani 1 1 d . . .
H5 H 0.5676 0.1304 0.4388 0.039 Uiso 1 1 calc R . .
C6 C 0.60684(17) 0.27732(14) 0.48117(12) 0.0360(5) Uani 1 1 d . . .
C7 C 0.69533(15) 0.23954(14) 0.57307(11) 0.0307(5) Uani 1 1 d . . .
C8 C 0.71766(17) 0.31452(15) 0.59438(14) 0.0408(6) Uani 1 1 d . . .
H8 H 0.6978 0.3591 0.5736 0.049 Uiso 1 1 calc R . .
C9 C 0.77002(18) 0.32160(15) 0.64715(14) 0.0428(6) Uani 1 1 d . . .
H9 H 0.7853 0.3715 0.6613 0.051 Uiso 1 1 calc R . .
C10 C 0.79958(15) 0.25641(16) 0.67878(13) 0.0367(5) Uani 1 1 d . . .
H10 H 0.8344 0.2623 0.7141 0.044 Uiso 1 1 calc R . .
C11 C 0.77737(14) 0.18208(13) 0.65787(11) 0.0302(4) Uani 1 1 d . . .
C12 C 0.72547(15) 0.17371(13) 0.60546(11) 0.0316(5) Uani 1 1 d . . .
H12 H 0.7105 0.1236 0.5917 0.038 Uiso 1 1 calc R . .
C13 C 0.81065(15) 0.11059(15) 0.69098(12) 0.0335(5) Uani 1 1 d . . .
C14 C 0.89724(17) -0.19043(17) 0.77031(13) 0.0411(6) Uani 1 1 d . . .
H14 H 0.9324 -0.1741 0.8032 0.049 Uiso 1 1 calc R . .
C15 C 0.89093(17) -0.26933(16) 0.75816(13) 0.0417(6) Uani 1 1 d . . .
H15 H 0.9211 -0.3056 0.7823 0.050 Uiso 1 1 calc R . .
C16 C 0.83890(17) -0.29386(15) 0.70945(13) 0.0383(6) Uani 1 1 d . . .
H16 H 0.8338 -0.3472 0.7001 0.046 Uiso 1 1 calc R . .
C17 C 0.79394(15) -0.23831(13) 0.67435(11) 0.0300(5) Uani 1 1 d . . .
C18 C 0.80382(16) -0.15964(14) 0.69017(12) 0.0335(5) Uani 1 1 d . . .
H18 H 0.7736 -0.1221 0.6673 0.040 Uiso 1 1 calc R . .
C19 C 0.73774(16) -0.26821(14) 0.62257(12) 0.0332(5) Uani 1 1 d . . .
C20 C 0.65310(16) -0.22961(13) 0.52838(11) 0.0317(5) Uani 1 1 d . . .
C21 C 0.6287(2) -0.30449(15) 0.50896(14) 0.0438(6) Uani 1 1 d . . .
H21 H 0.6478 -0.3487 0.5308 0.053 Uiso 1 1 calc R . .
C22 C 0.5756(2) -0.31296(15) 0.45670(14) 0.0446(7) Uani 1 1 d . . .
H22 H 0.5595 -0.3631 0.4436 0.054 Uiso 1 1 calc R . .
C23 C 0.54667(17) -0.24811(15) 0.42418(12) 0.0375(5) Uani 1 1 d . . .
H23 H 0.5110 -0.2543 0.3894 0.045 Uiso 1 1 calc R . .
C24 C 0.57098(15) -0.17344(14) 0.44350(11) 0.0314(5) Uani 1 1 d . . .
C25 C 0.62370(16) -0.16414(14) 0.49528(11) 0.0320(5) Uani 1 1 d . . .
H25 H 0.6397 -0.1139 0.5081 0.038 Uiso 1 1 calc R . .
C26 C 0.53936(17) -0.10351(15) 0.40703(12) 0.0359(5) Uani 1 1 d . . .
N1 N 0.49783(13) 0.14371(13) 0.36260(10) 0.0333(4) Uani 1 1 d . . .
N2 N 0.64444(14) 0.22410(12) 0.51915(10) 0.0348(5) Uani 1 1 d . . .
H28 H 0.637(2) 0.172(2) 0.5123(16) 0.048(9) Uiso 1 1 d . . .
N3 N 0.85509(14) -0.13541(12) 0.73703(10) 0.0350(4) Uani 1 1 d . A .
N4 N 0.70735(16) -0.21500(13) 0.58083(11) 0.0390(5) Uani 1 1 d . . .
H4 H 0.719(3) -0.167(3) 0.584(2) 0.083(15) Uiso 1 1 d . . .
O1 O 0.61275(17) 0.34841(12) 0.48903(12) 0.0621(7) Uani 1 1 d . . .
O2 O 0.86400(14) 0.12053(12) 0.73442(10) 0.0491(5) Uani 1 1 d . A .
O3 O 0.78656(12) 0.04255(11) 0.67448(9) 0.0396(4) Uani 1 1 d . A .
O4 O 0.72126(16) -0.33831(11) 0.61942(11) 0.0566(6) Uani 1 1 d . . .
O5 O 0.49446(15) -0.11546(12) 0.35891(10) 0.0532(6) Uani 1 1 d . . .
O6 O 0.55697(15) -0.03492(11) 0.42455(10) 0.0501(5) Uani 1 1 d . . .
O7 O 0.35752(15) 0.02126(14) 0.37859(11) 0.0511(5) Uani 1 1 d . . .
O8 O 0.6548(2) 0.04495(13) 0.50502(12) 0.0548(6) Uani 1 1 d . . .
H26 H 0.695(2) 0.028(2) 0.5091(18) 0.039(10) Uiso 1 1 d . . .
H27 H 0.623(3) 0.019(3) 0.484(2) 0.073(14) Uiso 1 1 d . . .
O9 O 0.20326(19) 0.0312(2) 0.44635(16) 0.0850(10) Uani 1 1 d . . .
O11A O 0.8192(4) 0.0090(3) 0.8465(3) 0.0520(12) Uiso 0.48 1 d P A 1
O11B O 0.7900(3) 0.0139(3) 0.8263(2) 0.0472(10) Uiso 0.52 1 d P A 2
O10A O 0.5946(4) 0.4949(3) 0.5342(3) 0.0666(13) Uiso 0.61 1 d P B 1
O10B O 0.5604(7) 0.4957(5) 0.5190(5) 0.077(2) Uiso 0.39 1 d P C 2
Cd1 Cd 0.481619(13) 0.014423(11) 0.334047(9) 0.03769(7) Uani 1 1 d . . .
Cd2 Cd 0.887141(13) -0.007090(11) 0.755653(10) 0.04023(7) Uani 1 1 d . . .
Cl2 Cl 1.00793(5) -0.01681(5) 0.83341(3) 0.04965(18) Uani 1 1 d . . .
Cl1 Cl 0.60701(4) 0.01878(5) 0.26756(3) 0.04649(17) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.336(3) . ?
C1 C2 1.368(4) . ?
C2 C3 1.378(4) . ?
C3 C4 1.384(3) . ?
C4 C5 1.385(3) . ?
C4 C6 1.500(4) . ?
C5 N1 1.336(3) . ?
C6 O1 1.222(3) . ?
C6 N2 1.345(3) . ?
C7 C12 1.393(3) . ?
C7 C8 1.395(3) . ?
C7 N2 1.415(3) . ?
C8 C9 1.390(4) . ?
C9 C10 1.374(4) . ?
C10 C11 1.382(3) . ?
C11 C12 1.381(3) . ?
C11 C13 1.495(3) . ?
C13 O2 1.254(3) . ?
C13 O3 1.265(3) . ?
C14 N3 1.344(3) . ?
C14 C15 1.368(4) . ?
C15 C16 1.378(4) . ?
C16 C17 1.392(3) . ?
C17 C18 1.386(3) . ?
C17 C19 1.494(3) . ?
C18 N3 1.340(3) . ?
C19 O4 1.222(3) . ?
C19 N4 1.351(3) . ?
C20 C21 1.390(3) . ?
C20 C25 1.392(3) . ?
C20 N4 1.419(3) . ?
C21 C22 1.390(4) . ?
C22 C23 1.375(4) . ?
C23 C24 1.386(3) . ?
C24 C25 1.380(3) . ?
C24 C26 1.500(3) . ?
C26 O6 1.253(3) 1 ?
C26 O6 1.253(3) . ?
C26 O5 1.253(3) . ?
N1 Cd1 2.292(2) . ?
N3 Cd2 2.271(2) . ?
O2 Cd2 2.242(2) . ?
O3 Cd2 2.4797(18) . ?
O5 Cd1 2.277(2) . ?
O6 Cd1 2.4001(19) . ?
O7 Cd1 2.347(3) . ?
O11A Cd2 2.371(6) . ?
O11B Cd2 2.343(5) . ?
Cd1 O6 2.4001(19) 1 ?
Cd1 Cl1 2.5590(7) 2_655 ?
Cd1 Cl1 2.6291(8) . ?
Cd2 Cl2 2.5232(8) . ?
Cd2 Cl2 2.7142(9) 2_756 ?
Cl2 Cd2 2.7142(9) 2_756 ?
Cl1 Cd1 2.5591(7) 2_655 ?

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(3) . . ?
C1 C2 C3 118.6(2) . . ?
C2 C3 C4 119.5(3) . . ?
C3 C4 C5 117.9(2) . . ?
C3 C4 C6 117.1(2) . . ?
C5 C4 C6 125.0(2) . . ?
N1 C5 C4 122.8(2) . . ?
O1 C6 N2 123.3(3) . . ?
O1 C6 C4 119.1(2) . . ?
N2 C6 C4 117.6(2) . . ?
C12 C7 C8 119.2(2) . . ?
C12 C7 N2 116.0(2) . . ?
C8 C7 N2 124.8(2) . . ?
C9 C8 C7 119.1(2) . . ?
C10 C9 C8 121.3(2) . . ?
C9 C10 C11 119.7(2) . . ?
C12 C11 C10 119.9(2) . . ?
C12 C11 C13 119.8(2) . . ?
C10 C11 C13 120.3(2) . . ?
C11 C12 C7 120.7(2) . . ?
O2 C13 O3 121.7(2) . . ?
O2 C13 C11 117.8(2) . . ?
O3 C13 C11 120.6(2) . . ?
N3 C14 C15 123.2(2) . . ?
C14 C15 C16 118.6(2) . . ?
C15 C16 C17 119.5(2) . . ?
C18 C17 C16 118.0(2) . . ?
C18 C17 C19 124.7(2) . . ?
C16 C17 C19 117.3(2) . . ?
N3 C18 C17 122.7(2) . . ?
O4 C19 N4 123.0(2) . . ?
O4 C19 C17 119.8(2) . . ?
N4 C19 C17 117.3(2) . . ?
C21 C20 C25 119.4(2) . . ?
C21 C20 N4 123.7(2) . . ?
C25 C20 N4 116.8(2) . . ?
C20 C21 C22 119.6(2) . . ?
C23 C22 C21 120.8(2) . . ?
C22 C23 C24 119.7(2) . . ?
C25 C24 C23 120.2(2) . . ?
C25 C24 C26 121.0(2) . . ?
C23 C24 C26 118.8(2) . . ?
C24 C25 C20 120.3(2) . . ?
O6 C26 O5 120.9(2) 1 . ?
O6 C26 O5 120.9(2) . . ?
O6 C26 C24 120.7(2) 1 . ?
O6 C26 C24 120.7(2) . . ?
O5 C26 C24 118.3(2) . . ?
C1 N1 C5 118.0(2) . . ?
C1 N1 Cd1 117.63(18) . . ?
C5 N1 Cd1 124.24(16) . . ?
C6 N2 C7 127.1(2) . . ?
C18 N3 C14 118.0(2) . . ?
C18 N3 Cd2 123.76(16) . . ?
C14 N3 Cd2 117.79(17) . . ?
C19 N4 C20 127.2(2) . . ?
C13 O2 Cd2 97.15(16) . . ?
C13 O3 Cd2 85.90(14) . . ?
C26 O5 Cd1 94.61(16) . . ?
C26 O6 Cd1 88.89(15) . . ?
O5 Cd1 N1 148.92(8) . . ?
O5 Cd1 O7 91.01(9) . . ?
N1 Cd1 O7 85.86(8) . . ?
O5 Cd1 O6 55.50(7) . 1 ?
N1 Cd1 O6 93.96(7) . 1 ?
O7 Cd1 O6 95.32(9) . 1 ?
O5 Cd1 O6 55.50(7) . . ?
N1 Cd1 O6 93.96(7) . . ?
O7 Cd1 O6 95.32(9) . . ?
O5 Cd1 Cl1 105.68(5) . 2_655 ?
N1 Cd1 Cl1 104.72(5) . 2_655 ?
O7 Cd1 Cl1 84.00(6) . 2_655 ?
O6 Cd1 Cl1 161.18(5) 1 2_655 ?
O6 Cd1 Cl1 161.18(5) . 2_655 ?
O5 Cd1 Cl1 95.49(7) . . ?
N1 Cd1 Cl1 92.42(6) . . ?
O7 Cd1 Cl1 169.99(6) . . ?
O6 Cd1 Cl1 94.64(7) 1 . ?
O6 Cd1 Cl1 94.64(7) . . ?
Cl1 Cd1 Cl1 86.92(2) 2_655 . ?
O2 Cd2 N3 148.90(8) . . ?
O2 Cd2 O11B 82.73(13) . . ?
N3 Cd2 O11B 95.76(13) . . ?
O2 Cd2 O11A 88.65(14) . . ?
N3 Cd2 O11A 98.02(14) . . ?
O11B Cd2 O11A 15.41(15) . . ?
O2 Cd2 O3 55.26(6) . . ?
N3 Cd2 O3 93.68(7) . . ?
O11B Cd2 O3 87.67(14) . . ?
O11A Cd2 O3 102.69(17) . . ?
O2 Cd2 Cl2 108.38(5) . . ?
N3 Cd2 Cl2 102.65(6) . . ?
O11B Cd2 Cl2 96.80(14) . . ?
O11A Cd2 Cl2 81.43(16) . . ?
O3 Cd2 Cl2 162.50(5) . . ?
O2 Cd2 Cl2 91.14(7) . 2_756 ?
N3 Cd2 Cl2 88.16(6) . 2_756 ?
O11B Cd2 Cl2 173.35(12) . 2_756 ?
O11A Cd2 Cl2 168.30(16) . 2_756 ?
O3 Cd2 Cl2 86.72(5) . 2_756 ?
Cl2 Cd2 Cl2 87.55(3) . 2_756 ?
Cd2 Cl2 Cd2 92.00(3) . 2_756 ?
Cd1 Cl1 Cd1 92.99(2) 2_655 . ?

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
N2 H28 O8 0.90(4) 2.19(4) 3.064(3) 164(3) 1
O8 H26 O9 0.72(4) 2.13(4) 2.817(4) 158(4) 5_656
O8 H27 O6 0.80(5) 1.87(5) 2.662(3) 172(5) 1

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.163
#
_vrf_PLAT201_cp2f                
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......    1 Why ?          
RESPONSE: This is coming due to disordered oxygen atoms of
solvent water molecules.
;
_vrf_PLAT306_cp2f                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......    O9 Check          
RESPONSE: We could not locate Hydrogen atoms associated with
solvate water molecule (O9).
;
_vrf_PLAT232_cp2f                
;
PROBLEM: Hirshfeld Test Diff (M-X)  Cd1    --  Cl1 ..10.0 su          
RESPONSE: We are chemically sure about the identity of the
elements of the structure.Therefore this alart is definitely
not due to the wrong assignment of the atoms.However such alart
could be due to the inadequate absorption correction applied by
SADABS of the Bruker APEX-II software.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 989164'
#######################################################################
#
#                 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_l1h

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_symmetry_space_group_name_Hall  -P2n2ab
_chemical_formula_moiety         'C13 H10 N2 O3'
_chemical_formula_sum            'C13 H10 N2 O3'
_chemical_formula_weight         242.23

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   9.4072(3)
_cell_length_b                   12.7350(3)
_cell_length_c                   17.8919(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2143.46(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9774
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38464
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         29.46
_reflns_number_total             2967
_reflns_number_gt                1907
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97

_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)+(0.0650P)²+1.4589P] 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         2967
_refine_ls_number_parameters     176
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1543
_refine_ls_wR_factor_gt          0.1295
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
C1 C 0.9059(4) 0.2399(2) 0.66290(16) 0.0675(9) Uani 1 1 d . . .
C2 C 0.8237(6) 0.3057(2) 0.7053(2) 0.119(2) Uani 1 1 d . . .
H2 H 0.813(5) 0.371(4) 0.694(2) 0.156(18) Uiso 1 1 d . . .
C3 C 0.7316(4) 0.26368(19) 0.75665(19) 0.0818(12) Uani 1 1 d . . .
C4 C 0.7265(2) 0.15688(15) 0.76593(11) 0.0336(4) Uani 1 1 d . . .
C5 C 0.8170(2) 0.09756(16) 0.72159(11) 0.0352(5) Uani 1 1 d . . .
H5 H 0.8167 0.0251 0.7280 0.042 Uiso 1 1 calc R . .
C6 C 0.6308(2) 0.09920(15) 0.81865(11) 0.0327(4) Uani 1 1 d . . .
C7 C 0.44806(19) 0.12475(14) 0.91752(11) 0.0293(4) Uani 1 1 d . . .
C8 C 0.3998(2) 0.02168(15) 0.92164(11) 0.0343(4) Uani 1 1 d . . .
H8 H 0.4384 -0.0295 0.8906 0.041 Uiso 1 1 calc R . .
C9 C 0.2939(2) -0.00441(15) 0.97218(11) 0.0343(4) Uani 1 1 d . . .
H9 H 0.2614 -0.0733 0.9742 0.041 Uiso 1 1 calc R . .
C10 C 0.23547(19) 0.06958(14) 1.01960(11) 0.0303(4) Uani 1 1 d . . .
C11 C 0.2860(2) 0.17212(15) 1.01596(12) 0.0384(5) Uani 1 1 d . . .
H11 H 0.2487 0.2228 1.0479 0.046 Uiso 1 1 calc R . .
C12 C 0.3906(2) 0.19966(15) 0.96575(12) 0.0388(5) Uani 1 1 d . . .
H12 H 0.4232 0.2686 0.9640 0.047 Uiso 1 1 calc R . .
C13 C 0.12282(19) 0.04149(14) 1.07447(11) 0.0303(4) Uani 1 1 d . . .
N1 N 0.90439(18) 0.13780(13) 0.67042(10) 0.0372(4) Uani 1 1 d . . .
N2 N 0.55187(17) 0.15922(12) 0.86623(9) 0.0329(4) Uani 1 1 d . . .
H2B H 0.5672 0.2258 0.8648 0.039 Uiso 1 1 calc R . .
O1 O 0.62605(18) 0.00356(12) 0.81742(10) 0.0526(5) Uani 1 1 d . . .
O2 O 0.09102(16) -0.05896(10) 1.07442(9) 0.0417(4) Uani 1 1 d . . .
H2A H 0.0298 -0.0705 1.1060 0.062 Uiso 1 1 calc R . .
O3 O 0.06521(15) 0.10526(11) 1.11539(8) 0.0386(4) Uani 1 1 d . . .
H1 H 0.967(4) 0.268(2) 0.6266(17) 0.086(10) Uiso 1 1 d . . .
H3 H 0.672(4) 0.308(2) 0.7829(17) 0.088(10) 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
C1 N1 1.307(3) . ?
C1 C2 1.370(4) . ?
C1 H1 0.94(3) . ?
C2 C3 1.371(4) . ?
C2 H2 0.86(5) . ?
C3 C4 1.371(3) . ?
C3 H3 0.93(3) . ?
C4 C5 1.388(3) . ?
C4 C6 1.497(3) . ?
C5 N1 1.333(3) . ?
C5 H5 0.9300 . ?
C6 O1 1.219(2) . ?
C6 N2 1.364(2) . ?
C7 C8 1.391(3) . ?
C7 C12 1.395(3) . ?
C7 N2 1.410(2) . ?
C8 C9 1.386(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(3) . ?
C10 C13 1.488(3) . ?
C11 C12 1.378(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 O3 1.220(2) . ?
C13 O2 1.314(2) . ?
N2 H2B 0.8600 . ?
O2 H2A 0.8200 . ?

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) . . ?
N1 C1 H1 117.3(19) . . ?
C2 C1 H1 119.7(19) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 117(3) . . ?
C1 C2 H2 122(3) . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 122(2) . . ?
C2 C3 H3 119(2) . . ?
C3 C4 C5 116.7(2) . . ?
C3 C4 C6 125.76(19) . . ?
C5 C4 C6 117.54(17) . . ?
N1 C5 C4 124.19(18) . . ?
N1 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
O1 C6 N2 123.45(18) . . ?
O1 C6 C4 120.07(18) . . ?
N2 C6 C4 116.48(17) . . ?
C8 C7 C12 119.08(17) . . ?
C8 C7 N2 123.67(17) . . ?
C12 C7 N2 117.25(16) . . ?
C9 C8 C7 119.71(18) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 121.53(18) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 118.39(18) . . ?
C9 C10 C13 121.62(16) . . ?
C11 C10 C13 119.99(17) . . ?
C12 C11 C10 120.90(19) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 120.38(18) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
O3 C13 O2 123.18(18) . . ?
O3 C13 C10 123.51(17) . . ?
O2 C13 C10 113.31(16) . . ?
C1 N1 C5 117.37(19) . . ?
C6 N2 C7 127.50(16) . . ?
C6 N2 H2B 116.2 . . ?
C7 N2 H2B 116.2 . . ?
C13 O2 H2A 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A N1 0.82 1.86 2.653(2) 162.8 7_456
N2 H2B O3 0.86 2.18 3.020(2) 165.0 4_557

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.46
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 989165'
