# 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_[Cu2(L)(H2O)2].1.4DMF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14.70 H17.30 Cu0.50 N3.40 O3.90'
_chemical_formula_weight         335.79

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'
Cu Cu 0.3201 1.2651 '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   Pnnm

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

_cell_length_a                   11.9272(15)
_cell_length_b                   13.954(3)
_cell_length_c                   20.185(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3359.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1718
_cell_measurement_theta_min      2.4680
_cell_measurement_theta_max      29.4108

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_min  0.94393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -16.00   18.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.7838  -99.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega  -86.00   33.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.7838    0.0000  -30.0000 119

#__ type_ start__ end____ width___ exp.time_
  3 omega  -51.00   51.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.7838   77.0000   30.0000 102

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15847
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_sigmaI/netI    0.1445
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         29.34
_reflns_number_total             4172
_reflns_number_gt                1670
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4172
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2069
_refine_ls_R_factor_gt           0.1268
_refine_ls_wR_factor_ref         0.3829
_refine_ls_wR_factor_gt          0.3509
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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
Cu1 Cu 0.26257(10) 0.07272(10) 0.0000 0.0587(6) Uani 1 2 d S . .
O1 O 0.3216(5) 0.1533(5) 0.0721(2) 0.0770(17) Uani 1 1 d . . .
O2 O 0.1508(5) 0.2086(4) 0.0744(2) 0.0823(18) Uani 1 1 d . . .
O3 O 0.4116(9) -0.0332(11) 0.0000 0.206(8) Uani 1 2 d S . .
N1 N 0.3130(5) 0.4916(5) 0.4325(3) 0.0694(19) Uani 1 1 d . . .
N2 N 0.4067(5) 0.4361(4) 0.4416(2) 0.0521(14) Uani 1 1 d . . .
C1 C 0.2452(7) 0.2001(7) 0.0960(4) 0.063(2) Uani 1 1 d . . .
C2 C 0.2765(7) 0.2538(7) 0.1610(3) 0.063(2) Uani 1 1 d . . .
C3 C 0.2024(9) 0.3138(8) 0.1840(5) 0.102(3) Uani 1 1 d . . .
H3 H 0.1355 0.3259 0.1599 0.122 Uiso 1 1 calc R . .
C4 C 0.2222(9) 0.3617(8) 0.2460(5) 0.096(3) Uani 1 1 d . . .
H4 H 0.1673 0.4019 0.2657 0.116 Uiso 1 1 calc R . .
C5 C 0.3225(8) 0.3467(7) 0.2745(5) 0.091(3) Uani 1 1 d . . .
C6 C 0.3996(7) 0.2885(9) 0.2511(4) 0.108(4) Uani 1 1 d . . .
H6 H 0.4690 0.2788 0.2732 0.129 Uiso 1 1 calc R . .
C7 C 0.3732(8) 0.2413(8) 0.1912(4) 0.097(3) Uani 1 1 d . . .
H7 H 0.4268 0.1992 0.1721 0.117 Uiso 1 1 calc R . .
C8 C 0.3393(7) 0.3964(6) 0.3439(4) 0.078(2) Uani 1 1 d . . .
C9 C 0.2743(8) 0.4644(6) 0.3741(4) 0.077(3) Uani 1 1 d . . .
H9 H 0.2078 0.4896 0.3549 0.092 Uiso 1 1 calc R . .
C10 C 0.4256(6) 0.3790(5) 0.3903(3) 0.0595(18) Uani 1 1 d . . .
H10 H 0.4857 0.3348 0.3857 0.071 Uiso 1 1 calc R . .
C11 C 0.4747(7) 0.4492(6) 0.5000 0.042(2) Uani 1 2 d S . .
H11 H 0.5366 0.4010 0.5000 0.050 Uiso 1 2 calc SR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.970(5) . ?
Cu1 O1 1.970(5) 6 ?
Cu1 N1 1.987(6) 7_655 ?
Cu1 N1 1.987(6) 4_545 ?
Cu1 O3 2.312(12) . ?
O1 C1 1.221(10) . ?
O2 C1 1.213(9) . ?
N1 C9 1.322(8) . ?
N1 N2 1.373(8) . ?
N1 Cu1 1.987(6) 7_666 ?
N2 C10 1.325(8) . ?
N2 C11 1.443(7) . ?
C1 C2 1.556(11) . ?
C2 C3 1.303(13) . ?
C2 C7 1.316(11) . ?
C3 C4 1.438(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.344(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.315(13) . ?
C5 C8 1.574(12) . ?
C6 C7 1.413(12) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.369(11) . ?
C8 C10 1.414(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 N2 1.443(7) 6_556 ?
C11 C11 1.540(17) 5_666 ?
C11 H11 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 95.3(3) . 6 ?
O1 Cu1 N1 173.7(2) . 7_655 ?
O1 Cu1 N1 88.9(2) 6 7_655 ?
O1 Cu1 N1 88.9(2) . 4_545 ?
O1 Cu1 N1 173.7(2) 6 4_545 ?
N1 Cu1 N1 86.6(3) 7_655 4_545 ?
O1 Cu1 O3 95.2(3) . . ?
O1 Cu1 O3 95.2(3) 6 . ?
N1 Cu1 O3 89.1(3) 7_655 . ?
N1 Cu1 O3 89.1(3) 4_545 . ?
C1 O1 Cu1 109.3(5) . . ?
C9 N1 N2 103.9(6) . . ?
C9 N1 Cu1 128.1(5) . 7_666 ?
N2 N1 Cu1 126.8(4) . 7_666 ?
C10 N2 N1 112.0(5) . . ?
C10 N2 C11 128.2(6) . . ?
N1 N2 C11 119.6(6) . . ?
O2 C1 O1 127.0(8) . . ?
O2 C1 C2 118.7(8) . . ?
O1 C1 C2 114.3(7) . . ?
C3 C2 C7 121.0(8) . . ?
C3 C2 C1 116.5(8) . . ?
C7 C2 C1 122.5(9) . . ?
C2 C3 C4 119.8(9) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 116.5(11) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
C6 C5 C4 124.4(10) . . ?
C6 C5 C8 120.2(8) . . ?
C4 C5 C8 115.2(10) . . ?
C5 C6 C7 116.1(9) . . ?
C5 C6 H6 121.9 . . ?
C7 C6 H6 121.9 . . ?
C2 C7 C6 122.0(9) . . ?
C2 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C9 C8 C10 103.7(7) . . ?
C9 C8 C5 129.0(7) . . ?
C10 C8 C5 127.4(8) . . ?
N1 C9 C8 113.5(7) . . ?
N1 C9 H9 123.2 . . ?
C8 C9 H9 123.2 . . ?
N2 C10 C8 106.9(7) . . ?
N2 C10 H10 126.6 . . ?
C8 C10 H10 126.6 . . ?
N2 C11 N2 109.6(7) . 6_556 ?
N2 C11 C11 109.7(6) . 5_666 ?
N2 C11 C11 109.7(6) 6_556 5_666 ?
N2 C11 H11 109.2 . . ?
N2 C11 H11 109.2 6_556 . ?
C11 C11 H11 109.2 5_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu1 O1 C1 103.7(5) 6 . . . ?
N1 Cu1 O1 C1 -28(3) 7_655 . . . ?
N1 Cu1 O1 C1 -71.6(5) 4_545 . . . ?
O3 Cu1 O1 C1 -160.6(6) . . . . ?
C9 N1 N2 C10 1.3(9) . . . . ?
Cu1 N1 N2 C10 169.9(5) 7_666 . . . ?
C9 N1 N2 C11 177.4(7) . . . . ?
Cu1 N1 N2 C11 -14.1(9) 7_666 . . . ?
Cu1 O1 C1 O2 -10.1(10) . . . . ?
Cu1 O1 C1 C2 170.2(5) . . . . ?
O2 C1 C2 C3 -7.7(12) . . . . ?
O1 C1 C2 C3 171.9(8) . . . . ?
O2 C1 C2 C7 173.3(9) . . . . ?
O1 C1 C2 C7 -7.0(12) . . . . ?
C7 C2 C3 C4 -4.9(16) . . . . ?
C1 C2 C3 C4 176.1(8) . . . . ?
C2 C3 C4 C5 5.0(16) . . . . ?
C3 C4 C5 C6 -3.2(17) . . . . ?
C3 C4 C5 C8 -177.3(9) . . . . ?
C4 C5 C6 C7 1.2(17) . . . . ?
C8 C5 C6 C7 175.0(9) . . . . ?
C3 C2 C7 C6 2.8(16) . . . . ?
C1 C2 C7 C6 -178.3(9) . . . . ?
C5 C6 C7 C2 -0.8(16) . . . . ?
C6 C5 C8 C9 174.1(10) . . . . ?
C4 C5 C8 C9 -11.6(15) . . . . ?
C6 C5 C8 C10 -7.2(15) . . . . ?
C4 C5 C8 C10 167.1(9) . . . . ?
N2 N1 C9 C8 -1.8(11) . . . . ?
Cu1 N1 C9 C8 -170.1(6) 7_666 . . . ?
C10 C8 C9 N1 1.6(11) . . . . ?
C5 C8 C9 N1 -179.5(9) . . . . ?
N1 N2 C10 C8 -0.4(8) . . . . ?
C11 N2 C10 C8 -176.0(7) . . . . ?
C9 C8 C10 N2 -0.7(9) . . . . ?
C5 C8 C10 N2 -179.6(8) . . . . ?
C10 N2 C11 N2 -127.4(7) . . . 6_556 ?
N1 N2 C11 N2 57.3(10) . . . 6_556 ?
C10 N2 C11 C11 112.0(10) . . . 5_666 ?
N1 N2 C11 C11 -63.3(9) . . . 5_666 ?

_diffrn_measured_fraction_theta_max 0.879
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.121

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.028 0.000 0.500 876 231 ' '
2 -0.036 0.500 0.000 876 231 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 980812'
#######################################################################
#
#                 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_[Zn2(L)].DMF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H20 N5 O5 Zn'
_chemical_formula_weight         523.82

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           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   23.269(5)
_cell_length_b                   10.602(2)
_cell_length_c                   24.340(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.28(3)
_cell_angle_gamma                90.00
_cell_volume                     5595.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    462
_cell_measurement_theta_min      2.138
_cell_measurement_theta_max      25.999

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2152
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8380
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38075
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5463
_reflns_number_gt                4853
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0995P)²+24.9191P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5463
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1961
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Zn1 Zn 0.24100(2) 0.42591(5) 0.51009(2) 0.0413(2) Uani 1 1 d . . .
O3 O 0.23090(16) 0.6401(3) 0.08343(14) 0.0513(8) Uani 1 1 d . . .
O1 O -0.17304(14) 0.6733(3) 0.54720(14) 0.0489(7) Uani 1 1 d . . .
N2 N 0.17080(16) 0.6991(3) 0.49040(15) 0.0414(8) Uani 1 1 d . . .
O4 O 0.29853(17) 0.4832(3) 0.11224(14) 0.0532(8) Uani 1 1 d . . .
N1 N 0.17673(18) 0.5831(3) 0.51648(16) 0.0447(8) Uani 1 1 d . . .
C21 C 0.2644(2) 0.5648(4) 0.1227(2) 0.0491(11) Uani 1 1 d . . .
N4 N 0.25075(18) 0.5439(4) 0.44354(15) 0.0439(8) Uani 1 1 d . . .
C1 C -0.1485(2) 0.7670(4) 0.5316(2) 0.0469(10) Uani 1 1 d . . .
C18 C 0.2610(3) 0.5735(4) 0.1828(2) 0.0508(11) Uani 1 1 d . . .
C10 C 0.1280(2) 0.5738(4) 0.5325(2) 0.0495(11) Uani 1 1 d . . .
H10 H 0.1191 0.5024 0.5516 0.059 Uiso 1 1 calc R . .
C13 C 0.2484(2) 0.5946(4) 0.35281(19) 0.0477(10) Uani 1 1 d . . .
C14 C 0.2613(2) 0.5006(4) 0.39720(19) 0.0489(11) Uani 1 1 d . . .
H14 H 0.2757 0.4181 0.3940 0.059 Uiso 1 1 calc R . .
C15 C 0.2533(3) 0.5854(4) 0.2941(2) 0.0501(11) Uani 1 1 d . . .
C16 C 0.2135(3) 0.6567(5) 0.2472(2) 0.0574(12) Uani 1 1 d . . .
H16 H 0.1835 0.7098 0.2535 0.069 Uiso 1 1 calc R . .
C9 C 0.1210(2) 0.7601(5) 0.4912(2) 0.0470(10) Uani 1 1 d . . .
H9 H 0.1085 0.8424 0.4762 0.056 Uiso 1 1 calc R . .
C19 C 0.3003(3) 0.5020(5) 0.2291(2) 0.0545(12) Uani 1 1 d . . .
H19 H 0.3300 0.4484 0.2226 0.065 Uiso 1 1 calc R . .
C8 C 0.0911(2) 0.6838(5) 0.5173(2) 0.0509(11) Uani 1 1 d . . .
C3 C -0.0613(3) 0.8345(6) 0.5020(3) 0.0731(17) Uani 1 1 d . . .
H3 H -0.0844 0.9074 0.4845 0.088 Uiso 1 1 calc R . .
C6 C 0.0085(3) 0.6253(5) 0.5547(2) 0.0582(12) Uani 1 1 d . . .
H6 H 0.0322 0.5542 0.5737 0.070 Uiso 1 1 calc R . .
C20 C 0.2965(2) 0.5083(5) 0.2845(2) 0.0541(11) Uani 1 1 d . . .
H20 H 0.3236 0.4595 0.3160 0.065 Uiso 1 1 calc R . .
C7 C -0.0492(2) 0.6457(5) 0.5579(2) 0.0561(12) Uani 1 1 d . . .
H7 H -0.0649 0.5872 0.5785 0.067 Uiso 1 1 calc R . .
C2 C -0.0840(2) 0.7496(5) 0.5316(2) 0.0516(11) Uani 1 1 d . . .
C5 C 0.0312(2) 0.7082(5) 0.5241(2) 0.0548(12) Uani 1 1 d . . .
C17 C 0.2173(3) 0.6504(5) 0.1923(2) 0.0571(12) Uani 1 1 d . . .
H17 H 0.1900 0.6988 0.1608 0.069 Uiso 1 1 calc R . .
C4 C -0.0041(3) 0.8129(6) 0.4977(3) 0.0743(17) Uani 1 1 d . . .
H4 H 0.0112 0.8707 0.4765 0.089 Uiso 1 1 calc R . .
O2 O -0.17448(15) 0.8712(3) 0.51484(15) 0.0530(8) Uani 1 1 d . . .
N3 N 0.22998(17) 0.6638(3) 0.42950(15) 0.0408(8) Uani 1 1 d . . .
C11 C 0.21968(19) 0.7441(4) 0.47313(17) 0.0390(9) Uani 1 1 d . . .
H11 H 0.2081 0.8299 0.4555 0.047 Uiso 1 1 calc R . .
C12 C 0.2286(2) 0.6980(4) 0.37576(18) 0.0455(10) Uani 1 1 d . . .
H12 H 0.2165 0.7776 0.3572 0.055 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.988(3) 5_566 ?
Zn1 O3 2.009(3) 6_566 ?
Zn1 O2 2.013(3) 3_545 ?
Zn1 N4 2.123(3) . ?
Zn1 N1 2.281(4) . ?
Zn1 C21 2.594(5) 6_566 ?
O3 C21 1.271(6) . ?
O3 Zn1 2.009(3) 6_565 ?
O1 C1 1.270(5) . ?
O1 Zn1 1.988(3) 5_566 ?
N2 C9 1.332(5) . ?
N2 N1 1.368(5) . ?
N2 C11 1.430(5) . ?
O4 C21 1.262(6) . ?
N1 C10 1.328(6) . ?
C21 C18 1.498(6) . ?
C21 Zn1 2.594(5) 6_565 ?
N4 C14 1.321(5) . ?
N4 N3 1.358(5) . ?
C1 O2 1.254(6) . ?
C1 C2 1.512(6) . ?
C18 C17 1.385(7) . ?
C18 C19 1.390(7) . ?
C10 C8 1.416(7) . ?
C10 H10 0.9500 . ?
C13 C12 1.383(6) . ?
C13 C14 1.419(6) . ?
C13 C15 1.479(6) . ?
C14 H14 0.9500 . ?
C15 C20 1.378(7) . ?
C15 C16 1.402(7) . ?
C16 C17 1.372(6) . ?
C16 H16 0.9500 . ?
C9 C8 1.365(6) . ?
C9 H9 0.9500 . ?
C19 C20 1.386(6) . ?
C19 H19 0.9500 . ?
C8 C5 1.486(6) . ?
C3 C2 1.375(7) . ?
C3 C4 1.390(8) . ?
C3 H3 0.9500 . ?
C6 C5 1.375(7) . ?
C6 C7 1.389(7) . ?
C6 H6 0.9500 . ?
C20 H20 0.9500 . ?
C7 C2 1.379(7) . ?
C7 H7 0.9500 . ?
C5 C4 1.391(8) . ?
C17 H17 0.9500 . ?
C4 H4 0.9500 . ?
O2 Zn1 2.013(3) 3_455 ?
N3 C12 1.347(5) . ?
N3 C11 1.448(5) . ?
C11 C11 1.542(8) 7_566 ?
C11 H11 1.0000 . ?
C12 H12 0.9500 . ?

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 Zn1 O3 96.85(14) 5_566 6_566 ?
O1 Zn1 O2 113.56(14) 5_566 3_545 ?
O3 Zn1 O2 105.99(14) 6_566 3_545 ?
O1 Zn1 N4 93.14(14) 5_566 . ?
O3 Zn1 N4 164.27(14) 6_566 . ?
O2 Zn1 N4 80.85(14) 3_545 . ?
O1 Zn1 N1 93.44(14) 5_566 . ?
O3 Zn1 N1 84.43(13) 6_566 . ?
O2 Zn1 N1 149.03(15) 3_545 . ?
N4 Zn1 N1 82.86(13) . . ?
O1 Zn1 C21 124.70(14) 5_566 6_566 ?
O3 Zn1 C21 28.59(15) 6_566 6_566 ?
O2 Zn1 C21 97.15(15) 3_545 6_566 ?
N4 Zn1 C21 138.08(15) . 6_566 ?
N1 Zn1 C21 77.98(14) . 6_566 ?
C21 O3 Zn1 102.2(3) . 6_565 ?
C1 O1 Zn1 122.3(3) . 5_566 ?
C9 N2 N1 111.8(3) . . ?
C9 N2 C11 129.1(4) . . ?
N1 N2 C11 118.6(3) . . ?
C10 N1 N2 104.4(4) . . ?
C10 N1 Zn1 128.0(3) . . ?
N2 N1 Zn1 125.7(2) . . ?
O4 C21 O3 122.6(4) . . ?
O4 C21 C18 120.0(5) . . ?
O3 C21 C18 117.4(4) . . ?
O4 C21 Zn1 73.7(2) . 6_565 ?
O3 C21 Zn1 49.2(2) . 6_565 ?
C18 C21 Zn1 164.8(4) . 6_565 ?
C14 N4 N3 105.6(3) . . ?
C14 N4 Zn1 123.5(3) . . ?
N3 N4 Zn1 128.1(2) . . ?
O2 C1 O1 124.8(4) . . ?
O2 C1 C2 118.0(4) . . ?
O1 C1 C2 117.2(4) . . ?
C17 C18 C19 119.5(4) . . ?
C17 C18 C21 120.1(5) . . ?
C19 C18 C21 120.3(4) . . ?
N1 C10 C8 111.3(4) . . ?
N1 C10 H10 124.3 . . ?
C8 C10 H10 124.3 . . ?
C12 C13 C14 105.0(4) . . ?
C12 C13 C15 126.6(4) . . ?
C14 C13 C15 128.4(4) . . ?
N4 C14 C13 110.6(4) . . ?
N4 C14 H14 124.7 . . ?
C13 C14 H14 124.7 . . ?
C20 C15 C16 119.4(4) . . ?
C20 C15 C13 121.3(5) . . ?
C16 C15 C13 119.4(4) . . ?
C17 C16 C15 120.5(5) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
N2 C9 C8 108.2(4) . . ?
N2 C9 H9 125.9 . . ?
C8 C9 H9 125.9 . . ?
C20 C19 C18 120.4(5) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C9 C8 C10 104.2(4) . . ?
C9 C8 C5 127.4(4) . . ?
C10 C8 C5 128.3(4) . . ?
C2 C3 C4 119.4(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C6 C7 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C15 C20 C19 120.1(5) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C2 C7 C6 121.0(5) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C3 C2 C7 119.6(4) . . ?
C3 C2 C1 119.4(5) . . ?
C7 C2 C1 120.9(4) . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 C8 120.6(5) . . ?
C4 C5 C8 120.5(5) . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C3 C4 C5 121.2(5) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C1 O2 Zn1 128.1(3) . 3_455 ?
C12 N3 N4 112.2(3) . . ?
C12 N3 C11 127.1(4) . . ?
N4 N3 C11 120.3(3) . . ?
N2 C11 N3 112.4(3) . . ?
N2 C11 C11 111.0(4) . 7_566 ?
N3 C11 C11 109.0(4) . 7_566 ?
N2 C11 H11 108.1 . . ?
N3 C11 H11 108.1 . . ?
C11 C11 H11 108.1 7_566 . ?
N3 C12 C13 106.5(4) . . ?
N3 C12 H12 126.7 . . ?
C13 C12 H12 126.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N2 N1 C10 1.1(5) . . . . ?
C11 N2 N1 C10 174.0(4) . . . . ?
C9 N2 N1 Zn1 166.5(3) . . . . ?
C11 N2 N1 Zn1 -20.7(5) . . . . ?
O1 Zn1 N1 C10 58.0(4) 5_566 . . . ?
O3 Zn1 N1 C10 -38.5(4) 6_566 . . . ?
O2 Zn1 N1 C10 -150.6(4) 3_545 . . . ?
N4 Zn1 N1 C10 150.7(4) . . . . ?
C21 Zn1 N1 C10 -66.8(4) 6_566 . . . ?
O1 Zn1 N1 N2 -103.9(4) 5_566 . . . ?
O3 Zn1 N1 N2 159.5(4) 6_566 . . . ?
O2 Zn1 N1 N2 47.5(5) 3_545 . . . ?
N4 Zn1 N1 N2 -11.2(3) . . . . ?
C21 Zn1 N1 N2 131.3(4) 6_566 . . . ?
Zn1 O3 C21 O4 7.2(5) 6_565 . . . ?
Zn1 O3 C21 C18 -171.3(3) 6_565 . . . ?
O1 Zn1 N4 C14 -56.0(4) 5_566 . . . ?
O3 Zn1 N4 C14 174.5(5) 6_566 . . . ?
O2 Zn1 N4 C14 57.3(4) 3_545 . . . ?
N1 Zn1 N4 C14 -149.1(4) . . . . ?
C21 Zn1 N4 C14 147.9(4) 6_566 . . . ?
O1 Zn1 N4 N3 102.1(4) 5_566 . . . ?
O3 Zn1 N4 N3 -27.3(8) 6_566 . . . ?
O2 Zn1 N4 N3 -144.5(4) 3_545 . . . ?
N1 Zn1 N4 N3 9.0(4) . . . . ?
C21 Zn1 N4 N3 -54.0(5) 6_566 . . . ?
Zn1 O1 C1 O2 70.3(5) 5_566 . . . ?
Zn1 O1 C1 C2 -107.7(4) 5_566 . . . ?
O4 C21 C18 C17 -170.9(5) . . . . ?
O3 C21 C18 C17 7.6(7) . . . . ?
Zn1 C21 C18 C17 -18.4(15) 6_565 . . . ?
O4 C21 C18 C19 7.2(7) . . . . ?
O3 C21 C18 C19 -174.2(4) . . . . ?
Zn1 C21 C18 C19 159.8(10) 6_565 . . . ?
N2 N1 C10 C8 -0.6(5) . . . . ?
Zn1 N1 C10 C8 -165.5(3) . . . . ?
N3 N4 C14 C13 1.1(5) . . . . ?
Zn1 N4 C14 C13 163.4(3) . . . . ?
C12 C13 C14 N4 -0.4(6) . . . . ?
C15 C13 C14 N4 -179.4(5) . . . . ?
C12 C13 C15 C20 150.7(5) . . . . ?
C14 C13 C15 C20 -30.6(8) . . . . ?
C12 C13 C15 C16 -29.2(8) . . . . ?
C14 C13 C15 C16 149.5(6) . . . . ?
C20 C15 C16 C17 -0.2(8) . . . . ?
C13 C15 C16 C17 179.7(5) . . . . ?
N1 N2 C9 C8 -1.2(5) . . . . ?
C11 N2 C9 C8 -173.1(4) . . . . ?
C17 C18 C19 C20 -0.7(8) . . . . ?
C21 C18 C19 C20 -178.9(5) . . . . ?
N2 C9 C8 C10 0.8(6) . . . . ?
N2 C9 C8 C5 -175.3(5) . . . . ?
N1 C10 C8 C9 -0.1(6) . . . . ?
N1 C10 C8 C5 175.9(5) . . . . ?
C16 C15 C20 C19 0.2(8) . . . . ?
C13 C15 C20 C19 -179.7(5) . . . . ?
C18 C19 C20 C15 0.3(8) . . . . ?
C5 C6 C7 C2 -1.2(8) . . . . ?
C4 C3 C2 C7 1.4(10) . . . . ?
C4 C3 C2 C1 -174.6(6) . . . . ?
C6 C7 C2 C3 -0.2(8) . . . . ?
C6 C7 C2 C1 175.8(5) . . . . ?
O2 C1 C2 C3 -14.1(7) . . . . ?
O1 C1 C2 C3 164.0(5) . . . . ?
O2 C1 C2 C7 169.9(5) . . . . ?
O1 C1 C2 C7 -12.0(7) . . . . ?
C7 C6 C5 C4 1.3(9) . . . . ?
C7 C6 C5 C8 -176.4(5) . . . . ?
C9 C8 C5 C6 -176.0(5) . . . . ?
C10 C8 C5 C6 8.8(9) . . . . ?
C9 C8 C5 C4 6.3(9) . . . . ?
C10 C8 C5 C4 -168.9(6) . . . . ?
C15 C16 C17 C18 -0.2(8) . . . . ?
C19 C18 C17 C16 0.7(8) . . . . ?
C21 C18 C17 C16 178.9(5) . . . . ?
C2 C3 C4 C5 -1.4(11) . . . . ?
C6 C5 C4 C3 0.0(10) . . . . ?
C8 C5 C4 C3 177.7(6) . . . . ?
O1 C1 O2 Zn1 2.6(7) . . . 3_455 ?
C2 C1 O2 Zn1 -179.4(3) . . . 3_455 ?
C14 N4 N3 C12 -1.5(5) . . . . ?
Zn1 N4 N3 C12 -162.6(3) . . . . ?
C14 N4 N3 C11 -173.8(4) . . . . ?
Zn1 N4 N3 C11 25.1(6) . . . . ?
C9 N2 C11 N3 -127.0(5) . . . . ?
N1 N2 C11 N3 61.5(5) . . . . ?
C9 N2 C11 C11 110.6(6) . . . 7_566 ?
N1 N2 C11 C11 -60.8(6) . . . 7_566 ?
C12 N3 C11 N2 123.3(5) . . . . ?
N4 N3 C11 N2 -65.6(5) . . . . ?
C12 N3 C11 C11 -113.2(5) . . . 7_566 ?
N4 N3 C11 C11 57.9(6) . . . 7_566 ?
N4 N3 C12 C13 1.2(5) . . . . ?
C11 N3 C12 C13 172.9(4) . . . . ?
C14 C13 C12 N3 -0.5(6) . . . . ?
C15 C13 C12 N3 178.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.081
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.091


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.001 0.250 610 67 ' '
2 0.000 -0.031 0.750 610 67 ' '
3 0.500 -0.038 0.250 610 67 ' '
4 0.500 -0.009 0.750 610 67 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 980813'
#######################################################################
#
#                 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_[Cd2(L)].1.75DMF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26.25 H25.25 Cd N5.75 O5.75'
_chemical_formula_weight         625.67

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   C2/c

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

_cell_length_a                   23.324(3)
_cell_length_b                   10.2514(6)
_cell_length_c                   25.426(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.190(15)
_cell_angle_gamma                90.00
_cell_volume                     5455.3(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3857
_cell_measurement_theta_min      2.4686
_cell_measurement_theta_max      29.0981

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2536
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_min  0.95018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00   39.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -57.0000  -90.0000 86

#__ type_ start__ end____ width___ exp.time_
  2 omega  -54.00   46.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -37.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega  -48.00  -20.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -57.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega  -16.00   14.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276 -102.0000 -161.0000 30

#__ type_ start__ end____ width___ exp.time_
  5 omega   -9.00   92.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   37.0000   60.0000 101

#__ type_ start__ end____ width___ exp.time_
  6 omega   32.00   98.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463 -179.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
  7 omega   -3.00   22.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   57.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
  8 omega  -25.00   24.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -99.0000 -120.0000 49

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23055
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5356
_reflns_number_gt                3843
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0634P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5356
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1366
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Cd1 Cd 0.24596(2) 1.08663(4) 0.527390(17) 0.02689(16) Uani 1 1 d . . .
C11 C 0.2164(3) 0.7571(5) 0.4731(2) 0.0223(12) Uani 1 1 d . . .
H11 H 0.2034 0.6688 0.4551 0.027 Uiso 1 1 calc R . .
N1 N 0.1761(2) 0.9174(4) 0.5204(2) 0.0264(11) Uani 1 1 d . . .
O3 O 0.2924(2) 0.9902(4) 0.12940(16) 0.0365(10) Uani 1 1 d . . .
C21 C 0.2549(3) 0.9137(6) 0.1371(3) 0.0324(14) Uani 1 1 d . . .
C18 C 0.2509(3) 0.9151(6) 0.1945(3) 0.0343(15) Uani 1 1 d . . .
O7 O -0.17951(19) 0.7606(4) 0.53669(16) 0.0305(9) Uani 1 1 d . . .
N2 N 0.1693(2) 0.7987(4) 0.49242(19) 0.0230(11) Uani 1 1 d . . .
C9 C 0.1274(3) 0.9206(6) 0.5341(3) 0.0351(15) Uani 1 1 d . . .
H9 H 0.1194 0.9912 0.5542 0.042 Uiso 1 1 calc R . .
O6 O -0.1477(2) 0.5572(4) 0.5414(2) 0.0456(12) Uani 1 1 d . . .
N3 N 0.2378(2) 0.9692(4) 0.4426(2) 0.0285(12) Uani 1 1 d . . .
O4 O 0.2200(2) 0.8339(4) 0.09840(17) 0.0331(10) Uani 1 1 d . . .
C1 C -0.1400(3) 0.6782(6) 0.5372(2) 0.0352(15) Uani 1 1 d . . .
C2 C -0.0795(3) 0.7181(6) 0.5325(3) 0.0473(19) Uani 1 1 d . . .
C4 C 0.0062(3) 0.8623(6) 0.5490(3) 0.0427(17) Uani 1 1 d . . .
H1 H 0.0278 0.9416 0.5652 0.051 Uiso 1 1 calc R . .
C10 C 0.1192(3) 0.7339(6) 0.4901(3) 0.0383(16) Uani 1 1 d . . .
H10 H 0.1057 0.6498 0.4735 0.046 Uiso 1 1 calc R . .
C3 C -0.0489(3) 0.8323(6) 0.5543(3) 0.0430(17) Uani 1 1 d . . .
H3 H -0.0652 0.8915 0.5731 0.052 Uiso 1 1 calc R . .
C8 C 0.0898(3) 0.8106(6) 0.5161(3) 0.0430(17) Uani 1 1 d . . .
C5 C 0.0300(3) 0.7812(6) 0.5214(3) 0.049(2) Uani 1 1 d . . .
C7 C -0.0605(5) 0.6416(11) 0.4979(6) 0.133(5) Uani 1 1 d . . .
H7 H -0.0835 0.5647 0.4799 0.159 Uiso 1 1 calc R . .
C6 C -0.0087(5) 0.6780(9) 0.4903(5) 0.119(5) Uani 1 1 d . . .
H6 H 0.0014 0.6317 0.4630 0.143 Uiso 1 1 calc R . .
C13 C 0.2365(3) 0.9117(6) 0.3559(3) 0.0349(15) Uani 1 1 d . . .
C15 C 0.2418(4) 0.9155(6) 0.3004(3) 0.0385(16) Uani 1 1 d . . .
C14 C 0.2199(3) 0.8049(6) 0.3787(2) 0.0283(14) Uani 1 1 d . . .
H14 H 0.2103 0.7204 0.3617 0.034 Uiso 1 1 calc R . .
C12 C 0.2470(3) 1.0106(6) 0.3972(2) 0.0339(16) Uani 1 1 d . . .
H12 H 0.2593 1.0970 0.3933 0.041 Uiso 1 1 calc R . .
C19 C 0.2048(4) 0.8423(6) 0.2012(3) 0.050(2) Uani 1 1 d . . .
H19 H 0.1761 0.7910 0.1694 0.060 Uiso 1 1 calc R . .
C20 C 0.1997(4) 0.8425(7) 0.2526(3) 0.055(2) Uani 1 1 d . . .
H20 H 0.1672 0.7924 0.2559 0.066 Uiso 1 1 calc R . .
C16 C 0.2867(4) 0.9891(7) 0.2933(3) 0.057(2) Uani 1 1 d . . .
H16 H 0.3157 1.0406 0.3249 0.069 Uiso 1 1 calc R . .
C17 C 0.2903(4) 0.9893(7) 0.2401(3) 0.0480(19) Uani 1 1 d . . .
H17 H 0.3211 1.0429 0.2357 0.058 Uiso 1 1 calc R . .
N4 N 0.2198(2) 0.8417(5) 0.42947(19) 0.0306(12) 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
Cd1 O4 2.292(3) 6_576 ?
Cd1 O7 2.298(4) 5_576 ?
Cd1 N1 2.333(4) . ?
Cd1 O6 2.363(4) 3 ?
Cd1 N3 2.401(4) . ?
Cd1 O7 2.428(4) 3 ?
Cd1 O3 2.458(4) 6_576 ?
Cd1 C21 2.703(6) 6_576 ?
Cd1 C1 2.728(6) 3 ?
C11 N4 1.439(6) . ?
C11 N2 1.450(6) . ?
C11 C11 1.568(11) 7_566 ?
C11 H11 1.0000 . ?
N1 C9 1.327(7) . ?
N1 N2 1.383(6) . ?
O3 C21 1.252(7) . ?
O3 Cd1 2.458(4) 6_575 ?
C21 O4 1.262(7) . ?
C21 C18 1.503(7) . ?
C21 Cd1 2.703(6) 6_575 ?
C18 C17 1.352(9) . ?
C18 C19 1.379(8) . ?
O7 C1 1.247(7) . ?
O7 Cd1 2.298(4) 5_576 ?
O7 Cd1 2.428(4) 3_445 ?
N2 C10 1.323(7) . ?
C9 C8 1.378(8) . ?
C9 H9 0.9500 . ?
O6 C1 1.265(7) . ?
O6 Cd1 2.363(4) 3_445 ?
N3 C12 1.334(6) . ?
N3 N4 1.368(6) . ?
O4 Cd1 2.292(3) 6_575 ?
C1 C2 1.523(8) . ?
C1 Cd1 2.727(6) 3_445 ?
C2 C3 1.355(8) . ?
C2 C7 1.387(10) . ?
C4 C5 1.356(8) . ?
C4 C3 1.383(8) . ?
C4 H1 0.9500 . ?
C10 C8 1.390(8) . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
C8 C5 1.488(8) . ?
C5 C6 1.389(10) . ?
C7 C6 1.360(11) . ?
C7 H7 0.9500 . ?
C6 H6 0.9500 . ?
C13 C14 1.371(7) . ?
C13 C12 1.401(8) . ?
C13 C15 1.471(7) . ?
C15 C16 1.365(9) . ?
C15 C20 1.396(9) . ?
C14 N4 1.347(6) . ?
C14 H14 0.9500 . ?
C12 H12 0.9500 . ?
C19 C20 1.364(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C16 C17 1.392(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?

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
O4 Cd1 O7 89.23(14) 6_576 5_576 ?
O4 Cd1 N1 84.62(14) 6_576 . ?
O7 Cd1 N1 102.87(15) 5_576 . ?
O4 Cd1 O6 123.40(16) 6_576 3 ?
O7 Cd1 O6 121.88(14) 5_576 3 ?
N1 Cd1 O6 124.61(15) . 3 ?
O4 Cd1 N3 160.22(16) 6_576 . ?
O7 Cd1 N3 86.77(15) 5_576 . ?
N1 Cd1 N3 77.43(15) . . ?
O6 Cd1 N3 74.58(16) 3 . ?
O4 Cd1 O7 95.08(13) 6_576 3 ?
O7 Cd1 O7 78.37(15) 5_576 3 ?
N1 Cd1 O7 178.72(15) . 3 ?
O6 Cd1 O7 54.59(13) 3 3 ?
N3 Cd1 O7 103.04(14) . 3 ?
O4 Cd1 O3 55.21(14) 6_576 6_576 ?
O7 Cd1 O3 144.29(13) 5_576 6_576 ?
N1 Cd1 O3 79.06(15) . 6_576 ?
O6 Cd1 O3 81.68(15) 3 6_576 ?
N3 Cd1 O3 127.57(15) . 6_576 ?
O7 Cd1 O3 99.74(13) 3 6_576 ?
O4 Cd1 C21 27.73(16) 6_576 6_576 ?
O7 Cd1 C21 116.96(17) 5_576 6_576 ?
N1 Cd1 C21 79.12(16) . 6_576 ?
O6 Cd1 C21 104.24(18) 3 6_576 ?
N3 Cd1 C21 149.83(16) . 6_576 ?
O7 Cd1 C21 100.04(15) 3 6_576 ?
O3 Cd1 C21 27.57(16) 6_576 6_576 ?
O4 Cd1 C1 113.06(16) 6_576 3 ?
O7 Cd1 C1 98.95(18) 5_576 3 ?
N1 Cd1 C1 152.09(18) . 3 ?
O6 Cd1 C1 27.60(16) 3 3 ?
N3 Cd1 C1 86.70(17) . 3 ?
O7 Cd1 C1 27.20(15) 3 3 ?
O3 Cd1 C1 93.21(16) 6_576 3 ?
C21 Cd1 C1 106.15(18) 6_576 3 ?
N4 C11 N2 113.1(4) . . ?
N4 C11 C11 110.7(5) . 7_566 ?
N2 C11 C11 110.4(5) . 7_566 ?
N4 C11 H11 107.5 . . ?
N2 C11 H11 107.5 . . ?
C11 C11 H11 107.5 7_566 . ?
C9 N1 N2 103.9(4) . . ?
C9 N1 Cd1 127.7(4) . . ?
N2 N1 Cd1 127.7(3) . . ?
C21 O3 Cd1 87.2(4) . 6_575 ?
O3 C21 O4 122.6(5) . . ?
O3 C21 C18 119.5(6) . . ?
O4 C21 C18 117.8(5) . . ?
O3 C21 Cd1 65.3(3) . 6_575 ?
O4 C21 Cd1 57.7(3) . 6_575 ?
C18 C21 Cd1 172.8(5) . 6_575 ?
C17 C18 C19 118.0(5) . . ?
C17 C18 C21 121.9(6) . . ?
C19 C18 C21 120.1(6) . . ?
C1 O7 Cd1 137.2(4) . 5_576 ?
C1 O7 Cd1 89.9(3) . 3_445 ?
Cd1 O7 Cd1 101.63(15) 5_576 3_445 ?
C10 N2 N1 111.3(4) . . ?
C10 N2 C11 128.5(5) . . ?
N1 N2 C11 120.0(4) . . ?
N1 C9 C8 112.8(5) . . ?
N1 C9 H9 123.6 . . ?
C8 C9 H9 123.6 . . ?
C1 O6 Cd1 92.4(4) . 3_445 ?
C12 N3 N4 103.9(4) . . ?
C12 N3 Cd1 129.7(4) . . ?
N4 N3 Cd1 126.4(3) . . ?
C21 O4 Cd1 94.6(3) . 6_575 ?
O7 C1 O6 122.1(6) . . ?
O7 C1 C2 121.6(6) . . ?
O6 C1 C2 116.3(6) . . ?
O7 C1 Cd1 62.9(3) . 3_445 ?
O6 C1 Cd1 60.0(3) . 3_445 ?
C2 C1 Cd1 170.1(4) . 3_445 ?
C3 C2 C7 119.3(6) . . ?
C3 C2 C1 122.6(6) . . ?
C7 C2 C1 117.6(6) . . ?
C5 C4 C3 121.6(6) . . ?
C5 C4 H1 119.2 . . ?
C3 C4 H1 119.2 . . ?
N2 C10 C8 107.8(5) . . ?
N2 C10 H10 126.1 . . ?
C8 C10 H10 126.1 . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C9 C8 C10 104.2(5) . . ?
C9 C8 C5 128.4(6) . . ?
C10 C8 C5 127.4(6) . . ?
C4 C5 C6 116.7(7) . . ?
C4 C5 C8 122.5(6) . . ?
C6 C5 C8 120.1(6) . . ?
C6 C7 C2 119.2(8) . . ?
C6 C7 H7 120.4 . . ?
C2 C7 H7 120.4 . . ?
C7 C6 C5 121.5(8) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C14 C13 C12 104.5(5) . . ?
C14 C13 C15 125.8(5) . . ?
C12 C13 C15 129.7(5) . . ?
C16 C15 C20 117.8(6) . . ?
C16 C15 C13 122.4(6) . . ?
C20 C15 C13 119.8(6) . . ?
N4 C14 C13 107.5(5) . . ?
N4 C14 H14 126.3 . . ?
C13 C14 H14 126.3 . . ?
N3 C12 C13 112.2(5) . . ?
N3 C12 H12 123.9 . . ?
C13 C12 H12 123.9 . . ?
C20 C19 C18 121.4(6) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C15 120.7(6) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C15 C16 C17 120.6(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 121.6(6) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C14 N4 N3 111.9(4) . . ?
C14 N4 C11 126.5(5) . . ?
N3 N4 C11 120.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Cd1 N1 C9 25.3(5) 6_576 . . . ?
O7 Cd1 N1 C9 -62.7(5) 5_576 . . . ?
O6 Cd1 N1 C9 152.6(5) 3 . . . ?
N3 Cd1 N1 C9 -146.4(5) . . . . ?
O7 Cd1 N1 C9 102(6) 3 . . . ?
O3 Cd1 N1 C9 80.8(5) 6_576 . . . ?
C21 Cd1 N1 C9 52.8(5) 6_576 . . . ?
C1 Cd1 N1 C9 156.8(5) 3 . . . ?
O4 Cd1 N1 N2 -166.2(4) 6_576 . . . ?
O7 Cd1 N1 N2 105.9(4) 5_576 . . . ?
O6 Cd1 N1 N2 -38.8(5) 3 . . . ?
N3 Cd1 N1 N2 22.2(4) . . . . ?
O7 Cd1 N1 N2 -90(6) 3 . . . ?
O3 Cd1 N1 N2 -110.6(4) 6_576 . . . ?
C21 Cd1 N1 N2 -138.7(5) 6_576 . . . ?
C1 Cd1 N1 N2 -34.7(6) 3 . . . ?
Cd1 O3 C21 O4 6.4(6) 6_575 . . . ?
Cd1 O3 C21 C18 -173.9(5) 6_575 . . . ?
O3 C21 C18 C17 -5.3(9) . . . . ?
O4 C21 C18 C17 174.3(6) . . . . ?
Cd1 C21 C18 C17 -135(3) 6_575 . . . ?
O3 C21 C18 C19 172.6(6) . . . . ?
O4 C21 C18 C19 -7.7(9) . . . . ?
Cd1 C21 C18 C19 43(4) 6_575 . . . ?
C9 N1 N2 C10 -0.5(6) . . . . ?
Cd1 N1 N2 C10 -171.2(4) . . . . ?
C9 N1 N2 C11 -177.1(5) . . . . ?
Cd1 N1 N2 C11 12.2(7) . . . . ?
N4 C11 N2 C10 121.2(6) . . . . ?
C11 C11 N2 C10 -114.2(7) 7_566 . . . ?
N4 C11 N2 N1 -62.9(6) . . . . ?
C11 C11 N2 N1 61.8(7) 7_566 . . . ?
N2 N1 C9 C8 -0.3(7) . . . . ?
Cd1 N1 C9 C8 170.4(4) . . . . ?
O4 Cd1 N3 C12 130.2(6) 6_576 . . . ?
O7 Cd1 N3 C12 51.5(6) 5_576 . . . ?
N1 Cd1 N3 C12 155.5(6) . . . . ?
O6 Cd1 N3 C12 -72.8(6) 3 . . . ?
O7 Cd1 N3 C12 -25.8(6) 3 . . . ?
O3 Cd1 N3 C12 -139.2(5) 6_576 . . . ?
C21 Cd1 N3 C12 -164.7(5) 6_576 . . . ?
C1 Cd1 N3 C12 -47.7(6) 3 . . . ?
O4 Cd1 N3 N4 -47.4(7) 6_576 . . . ?
O7 Cd1 N3 N4 -126.1(5) 5_576 . . . ?
N1 Cd1 N3 N4 -22.1(4) . . . . ?
O6 Cd1 N3 N4 109.6(5) 3 . . . ?
O7 Cd1 N3 N4 156.7(4) 3 . . . ?
O3 Cd1 N3 N4 43.3(5) 6_576 . . . ?
C21 Cd1 N3 N4 17.7(7) 6_576 . . . ?
C1 Cd1 N3 N4 134.8(5) 3 . . . ?
O3 C21 O4 Cd1 -6.9(6) . . . 6_575 ?
C18 C21 O4 Cd1 173.4(5) . . . 6_575 ?
Cd1 O7 C1 O6 -117.0(6) 5_576 . . . ?
Cd1 O7 C1 O6 -9.9(6) 3_445 . . . ?
Cd1 O7 C1 C2 62.8(8) 5_576 . . . ?
Cd1 O7 C1 C2 169.9(5) 3_445 . . . ?
Cd1 O7 C1 Cd1 -107.1(5) 5_576 . . 3_445 ?
Cd1 O6 C1 O7 10.1(6) 3_445 . . . ?
Cd1 O6 C1 C2 -169.6(5) 3_445 . . . ?
O7 C1 C2 C3 31.9(10) . . . . ?
O6 C1 C2 C3 -148.3(7) . . . . ?
Cd1 C1 C2 C3 147(3) 3_445 . . . ?
O7 C1 C2 C7 -139.7(9) . . . . ?
O6 C1 C2 C7 40.1(11) . . . . ?
Cd1 C1 C2 C7 -25(3) 3_445 . . . ?
N1 N2 C10 C8 1.0(7) . . . . ?
C11 N2 C10 C8 177.3(5) . . . . ?
C7 C2 C3 C4 -9.1(13) . . . . ?
C1 C2 C3 C4 179.4(6) . . . . ?
C5 C4 C3 C2 1.4(11) . . . . ?
N1 C9 C8 C10 0.9(8) . . . . ?
N1 C9 C8 C5 -177.3(7) . . . . ?
N2 C10 C8 C9 -1.2(8) . . . . ?
N2 C10 C8 C5 177.1(7) . . . . ?
C3 C4 C5 C6 10.4(12) . . . . ?
C3 C4 C5 C8 -179.0(7) . . . . ?
C9 C8 C5 C4 -3.7(13) . . . . ?
C10 C8 C5 C4 178.5(7) . . . . ?
C9 C8 C5 C6 166.7(9) . . . . ?
C10 C8 C5 C6 -11.1(13) . . . . ?
C3 C2 C7 C6 4.8(18) . . . . ?
C1 C2 C7 C6 176.7(11) . . . . ?
C2 C7 C6 C5 7(2) . . . . ?
C4 C5 C6 C7 -14.8(17) . . . . ?
C8 C5 C6 C7 174.3(11) . . . . ?
C14 C13 C15 C16 -144.8(7) . . . . ?
C12 C13 C15 C16 34.8(12) . . . . ?
C14 C13 C15 C20 35.6(10) . . . . ?
C12 C13 C15 C20 -144.9(8) . . . . ?
C12 C13 C14 N4 1.1(7) . . . . ?
C15 C13 C14 N4 -179.3(6) . . . . ?
N4 N3 C12 C13 -1.1(7) . . . . ?
Cd1 N3 C12 C13 -179.1(4) . . . . ?
C14 C13 C12 N3 0.1(8) . . . . ?
C15 C13 C12 N3 -179.5(7) . . . . ?
C17 C18 C19 C20 -1.4(11) . . . . ?
C21 C18 C19 C20 -179.5(7) . . . . ?
C18 C19 C20 C15 -0.8(12) . . . . ?
C16 C15 C20 C19 1.9(11) . . . . ?
C13 C15 C20 C19 -178.4(7) . . . . ?
C20 C15 C16 C17 -0.7(11) . . . . ?
C13 C15 C16 C17 179.6(7) . . . . ?
C19 C18 C17 C16 2.6(11) . . . . ?
C21 C18 C17 C16 -179.4(7) . . . . ?
C15 C16 C17 C18 -1.6(12) . . . . ?
C13 C14 N4 N3 -1.9(7) . . . . ?
C13 C14 N4 C11 -168.2(6) . . . . ?
C12 N3 N4 C14 1.8(7) . . . . ?
Cd1 N3 N4 C14 179.9(4) . . . . ?
C12 N3 N4 C11 169.1(5) . . . . ?
Cd1 N3 N4 C11 -12.8(7) . . . . ?
N2 C11 N4 C14 -132.1(6) . . . . ?
C11 C11 N4 C14 103.4(7) 7_566 . . . ?
N2 C11 N4 N3 62.7(7) . . . . ?
C11 C11 N4 N3 -61.8(7) 7_566 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.116

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.001 0.250 548 138 ' '
2 0.000 -0.041 0.750 548 138 ' '
3 0.500 -0.048 0.250 548 138 ' '
4 0.500 0.008 0.750 548 138 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 980814'
#######################################################################
#
#                 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_[Co2(L)(H2O)6].DMF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13.50 H16.50 Co0.50 N3 O4.50'
_chemical_formula_weight         322.26

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'
Co Co 0.3494 0.9721 '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   Pnnm

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

_cell_length_a                   10.0477(3)
_cell_length_b                   15.2023(10)
_cell_length_c                   22.6589(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3461.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    109(2)
_cell_measurement_reflns_used    2903
_cell_measurement_theta_min      2.4249
_cell_measurement_theta_max      29.1994

_exptl_crystal_description       cube
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_min  0.93639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      109(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -75.00  -41.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276 -179.0000  -60.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega  -35.00   48.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276   57.0000  -90.0000 83

#__ type_ start__ end____ width___ exp.time_
  3 omega  -85.00  -44.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -19.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
  4 omega  -31.00   67.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   19.0000   30.0000 98

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13993
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3132
_reflns_number_gt                2418
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0973P)²+3.3688P] 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         3132
_refine_ls_number_parameters     166
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1791
_refine_ls_wR_factor_gt          0.1698
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.84292(6) 0.02263(5) 0.0000 0.0175(2) Uani 1 2 d S . .
O1 O 0.6992(3) 0.2996(2) 0.40102(12) 0.0488(9) Uani 1 1 d . . .
C1 C 0.6153(4) 0.3172(4) 0.3622(2) 0.0578(16) Uani 1 1 d . . .
O2 O 0.5378(4) 0.3831(3) 0.36322(17) 0.0897(16) Uani 1 1 d . . .
C2 C 0.6097(4) 0.2614(4) 0.3071(2) 0.0558(16) Uani 1 1 d . . .
C3 C 0.6886(5) 0.1920(4) 0.2994(2) 0.0568(14) Uani 1 1 d . . .
H3 H 0.7475 0.1751 0.3302 0.068 Uiso 1 1 calc R . .
N4 N 0.5736(2) 0.07867(19) 0.05333(11) 0.0179(6) Uani 1 1 d . . .
C4 C 0.6867(5) 0.1437(4) 0.2475(2) 0.0573(14) Uani 1 1 d . . .
H4 H 0.7430 0.0938 0.2437 0.069 Uiso 1 1 calc R . .
N5 N 0.6983(3) 0.0489(2) 0.06621(12) 0.0203(7) Uani 1 1 d . . .
C5 C 0.6059(4) 0.1663(3) 0.20190(19) 0.0435(12) Uani 1 1 d . . .
C6 C 0.5194(8) 0.2314(7) 0.2120(3) 0.158(5) Uani 1 1 d . . .
H6 H 0.4551 0.2452 0.1827 0.190 Uiso 1 1 calc R . .
C7 C 0.5210(8) 0.2794(7) 0.2642(3) 0.165(5) Uani 1 1 d . . .
H7 H 0.4586 0.3256 0.2698 0.198 Uiso 1 1 calc R . .
C8 C 0.6120(3) 0.1215(3) 0.14445(16) 0.0297(9) Uani 1 1 d . . .
C9 C 0.7207(3) 0.0756(3) 0.12087(14) 0.0249(8) Uani 1 1 d . . .
H9 H 0.8012 0.0649 0.1417 0.030 Uiso 1 1 calc R . .
C10 C 0.5195(3) 0.1215(3) 0.09954(16) 0.0286(9) Uani 1 1 d . . .
H10 H 0.4333 0.1470 0.1009 0.034 Uiso 1 1 calc R . .
C11 C 0.5072(4) 0.0511(3) 0.0000 0.0159(10) Uani 1 2 d S . .
H11 H 0.4159 0.0772 0.0000 0.019 Uiso 1 2 calc SR . .
O13 O 1.0000 0.0000 0.06095(14) 0.0203(8) Uani 1 2 d SD . .
H13A H 1.017(4) 0.0522(17) 0.0801(17) 0.031 Uiso 1 1 d D . .
O14 O 0.7933(3) -0.1090(2) 0.0000 0.0205(8) Uani 1 2 d SD . .
H14A H 0.810(4) -0.136(2) -0.0336(11) 0.031 Uiso 1 1 d D . .
O12 O 0.8953(4) 0.1548(3) 0.0000 0.0364(10) Uani 1 2 d SD . .
H12A H 0.875(4) 0.1977(19) -0.0309(4) 0.055 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O14 2.063(4) . ?
Co1 O12 2.077(4) . ?
Co1 O13 2.125(2) . ?
Co1 O13 2.125(2) 5_755 ?
Co1 N5 2.126(3) 6 ?
Co1 N5 2.126(3) . ?
O1 C1 1.247(6) . ?
C1 O2 1.270(6) . ?
C1 C2 1.512(6) . ?
C2 C3 1.332(7) . ?
C2 C7 1.345(7) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9500 . ?
N4 C10 1.347(4) . ?
N4 N5 1.364(4) . ?
N4 C11 1.443(3) . ?
C4 C5 1.357(6) . ?
C4 H4 0.9500 . ?
N5 C9 1.323(4) . ?
C5 C6 1.337(7) . ?
C5 C8 1.471(5) . ?
C6 C7 1.390(8) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C10 1.378(5) . ?
C8 C9 1.402(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 N4 1.443(3) 6 ?
C11 C11 1.561(10) 5_655 ?
C11 H11 1.0000 . ?
O13 Co1 2.125(2) 5_755 ?
O13 H13A 0.921(18) . ?
O14 H14A 0.878(18) . ?
O12 H12A 0.979(18) . ?

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
O14 Co1 O12 179.30(14) . . ?
O14 Co1 O13 91.28(7) . . ?
O12 Co1 O13 88.19(8) . . ?
O14 Co1 O13 91.28(7) . 5_755 ?
O12 Co1 O13 88.19(8) . 5_755 ?
O13 Co1 O13 81.06(13) . 5_755 ?
O14 Co1 N5 90.98(10) . 6 ?
O12 Co1 N5 89.52(11) . 6 ?
O13 Co1 N5 175.11(9) . 6 ?
O13 Co1 N5 94.55(10) 5_755 6 ?
O14 Co1 N5 90.98(10) . . ?
O12 Co1 N5 89.52(11) . . ?
O13 Co1 N5 94.55(10) . . ?
O13 Co1 N5 175.11(9) 5_755 . ?
N5 Co1 N5 89.75(15) 6 . ?
O1 C1 O2 124.9(4) . . ?
O1 C1 C2 119.2(4) . . ?
O2 C1 C2 115.7(4) . . ?
C3 C2 C7 117.5(5) . . ?
C3 C2 C1 122.0(4) . . ?
C7 C2 C1 120.5(5) . . ?
C2 C3 C4 121.4(5) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C10 N4 N5 111.4(3) . . ?
C10 N4 C11 127.2(3) . . ?
N5 N4 C11 120.5(3) . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C9 N5 N4 104.8(3) . . ?
C9 N5 Co1 127.0(2) . . ?
N4 N5 Co1 122.6(2) . . ?
C6 C5 C4 116.5(4) . . ?
C6 C5 C8 121.5(4) . . ?
C4 C5 C8 122.1(4) . . ?
C5 C6 C7 121.8(5) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C2 C7 C6 121.0(6) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C10 C8 C9 104.1(3) . . ?
C10 C8 C5 128.7(3) . . ?
C9 C8 C5 126.9(3) . . ?
N5 C9 C8 112.1(3) . . ?
N5 C9 H9 123.9 . . ?
C8 C9 H9 123.9 . . ?
N4 C10 C8 107.6(3) . . ?
N4 C10 H10 126.2 . . ?
C8 C10 H10 126.2 . . ?
N4 C11 N4 113.8(4) . 6 ?
N4 C11 C11 109.4(3) . 5_655 ?
N4 C11 C11 109.4(3) 6 5_655 ?
N4 C11 H11 108.0 . . ?
N4 C11 H11 108.0 6 . ?
C11 C11 H11 108.0 5_655 . ?
Co1 O13 Co1 98.94(13) . 5_755 ?
Co1 O13 H13A 108(2) . . ?
Co1 O13 H13A 108(2) 5_755 . ?
Co1 O14 H14A 114(3) . . ?
Co1 O12 H12A 126(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 2.4(9) . . . . ?
O2 C1 C2 C3 177.8(6) . . . . ?
O1 C1 C2 C7 -179.3(8) . . . . ?
O2 C1 C2 C7 -3.9(10) . . . . ?
C7 C2 C3 C4 4.6(11) . . . . ?
C1 C2 C3 C4 -177.0(5) . . . . ?
C2 C3 C4 C5 1.2(9) . . . . ?
C10 N4 N5 C9 -1.1(4) . . . . ?
C11 N4 N5 C9 -171.0(3) . . . . ?
C10 N4 N5 Co1 -156.3(3) . . . . ?
C11 N4 N5 Co1 33.8(4) . . . . ?
O14 Co1 N5 C9 114.3(3) . . . . ?
O12 Co1 N5 C9 -65.2(3) . . . . ?
O13 Co1 N5 C9 23.0(3) . . . . ?
O13 Co1 N5 C9 -3.1(13) 5_755 . . . ?
N5 Co1 N5 C9 -154.7(3) 6 . . . ?
O14 Co1 N5 N4 -96.2(3) . . . . ?
O12 Co1 N5 N4 84.3(3) . . . . ?
O13 Co1 N5 N4 172.4(2) . . . . ?
O13 Co1 N5 N4 146.3(9) 5_755 . . . ?
N5 Co1 N5 N4 -5.2(3) 6 . . . ?
C3 C4 C5 C6 -6.7(10) . . . . ?
C3 C4 C5 C8 173.8(5) . . . . ?
C4 C5 C6 C7 6.4(15) . . . . ?
C8 C5 C6 C7 -174.1(9) . . . . ?
C3 C2 C7 C6 -5.0(15) . . . . ?
C1 C2 C7 C6 176.7(9) . . . . ?
C5 C6 C7 C2 -0.6(18) . . . . ?
C6 C5 C8 C10 -16.4(10) . . . . ?
C4 C5 C8 C10 163.1(5) . . . . ?
C6 C5 C8 C9 156.8(7) . . . . ?
C4 C5 C8 C9 -23.7(8) . . . . ?
N4 N5 C9 C8 0.8(4) . . . . ?
Co1 N5 C9 C8 154.6(3) . . . . ?
C10 C8 C9 N5 -0.3(5) . . . . ?
C5 C8 C9 N5 -174.8(4) . . . . ?
N5 N4 C10 C8 1.0(4) . . . . ?
C11 N4 C10 C8 170.1(4) . . . . ?
C9 C8 C10 N4 -0.4(5) . . . . ?
C5 C8 C10 N4 174.0(4) . . . . ?
C10 N4 C11 N4 128.5(4) . . . 6 ?
N5 N4 C11 N4 -63.3(5) . . . 6 ?
C10 N4 C11 C11 -108.8(5) . . . 5_655 ?
N5 N4 C11 C11 59.4(5) . . . 5_655 ?
O14 Co1 O13 Co1 91.09(6) . . . 5_755 ?
O12 Co1 O13 Co1 -88.45(7) . . . 5_755 ?
O13 Co1 O13 Co1 0.0 5_755 . . 5_755 ?
N5 Co1 O13 Co1 -26.4(11) 6 . . 5_755 ?
N5 Co1 O13 Co1 -177.82(9) . . . 5_755 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.084

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.023 0.000 0.500 840 132 ' '
2 -0.031 0.500 0.000 840 132 ' '
_platon_squeeze_details          
;
;


# start Validation Reply Form
_vrf_CHEMW03_Cu2LH2O2.1.4DMF     
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The electron density removed by the SQUEEZE routine 
was included in the formula (1.4 DMF per asymmetric unit).
;
_vrf_CHEMW03_Zn2L.DMF            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The electron density removed by the SQUEEZE routine 
was included in the formula (1 DMF per asymmetric unit).
;
_vrf_CHEMW03_Cd2L.1.75DMF        
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The electron density removed by the SQUEEZE routine 
was included in the formula (1.75 DMF per asymmetric unit).
;
_vrf_CHEMW03_Co2LH2O6.DMF        
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The electron density removed by the SQUEEZE routine 
was included in the formula (1 DMF per asymmetric unit).
;
_vrf_PLAT222_Co2LH2O6.DMF        
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       10.0 Ratio 
RESPONSE: These correspond to possible disorder of the phenyl ring. 
Splitting and refining these atoms over two sites led to the minor 
component becoming NPD. A satisfactory refinement could not be achieved.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 980815'
