# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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_1-Gd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Cl Cu2 Gd N6 O14'
_chemical_formula_weight         736.02

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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   P2/a

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

_cell_length_a                   11.6361(4)
_cell_length_b                   6.8244(2)
_cell_length_c                   12.1675(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.755(4)
_cell_angle_gamma                90.00
_cell_volume                     938.50(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2614
_cell_measurement_theta_min      2.9789
_cell_measurement_theta_max      29.0398

_exptl_crystal_description       Block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             706
_exptl_absorpt_coefficient_mu    5.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CRYSALISPRO

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3292
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1656
_reflns_number_gt                1565
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSALISPRO
_computing_cell_refinement       CRYSALISPRO
_computing_data_reduction        CRYSALISPRO
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0135P)^2^+4.3015P] where P=(Fo^2^+2Fc^2^)/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         1656
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0606
_refine_ls_wR_factor_gt          0.0598
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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
Gd1 Gd 0.2500 0.51351(5) 0.5000 0.01339(11) Uani 1 2 d S . .
Cu1 Cu 0.61156(5) 0.90134(11) 0.91142(5) 0.02509(18) Uani 1 1 d . . .
Cl1 Cl 0.7500 0.6269(3) 1.0000 0.0313(4) Uani 1 2 d S . .
O2 O 0.5718(3) 0.7628(6) 0.7659(3) 0.0227(8) Uani 1 1 d . . .
O1 O 0.4238(3) 0.6582(5) 0.6285(3) 0.0207(8) Uani 1 1 d . . .
C1 C 0.4624(4) 0.7420(7) 0.7200(4) 0.0147(10) Uani 1 1 d . . .
C2 C 0.3822(4) 0.8257(7) 0.7875(4) 0.0143(10) Uani 1 1 d . . .
N1 N 0.4384(3) 0.9005(6) 0.8876(3) 0.0168(9) Uani 1 1 d . . .
C4 C 0.1529(4) 0.7994(8) 0.6906(4) 0.0222(12) Uani 1 1 d . . .
C3 C 0.2617(4) 0.8539(7) 0.7789(4) 0.0156(10) Uani 1 1 d . . .
N2 N 0.3589(3) 0.9742(6) 0.9387(3) 0.0163(9) Uani 1 1 d . . .
N3 N 0.2519(3) 0.9479(6) 0.8727(3) 0.0174(9) Uani 1 1 d . . .
O4 O 0.0564(3) 0.8175(6) 0.7150(3) 0.0342(10) Uani 1 1 d . . .
O3 O 0.1679(3) 0.7361(7) 0.5979(3) 0.0364(11) Uani 1 1 d . . .
O5 O 0.4048(3) 0.2809(6) 0.5095(3) 0.0287(9) Uani 1 1 d . . .
H5A H 0.4545 0.3246 0.4730 0.043 Uiso 1 1 d R . .
H5B H 0.4415 0.2615 0.5790 0.043 Uiso 1 1 d R . .
O6 O 0.2732(4) 0.3542(7) 0.6869(3) 0.0391(11) Uani 1 1 d . . .
H6A H 0.3157 0.4260 0.7383 0.059 Uiso 1 1 d R . .
H6B H 0.2053 0.3383 0.7007 0.059 Uiso 1 1 d R . .
O7 O 0.5267(6) 0.6064(11) 0.1259(5) 0.0804(19) Uani 1 1 d G . .
H7A H 0.4626 0.5898 0.0760 0.121 Uiso 1 1 d G . .
H7B H 0.5793 0.6522 0.0949 0.121 Uiso 1 1 d G . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.00819(18) 0.0224(2) 0.00946(17) 0.000 0.00180(12) 0.000
Cu1 0.0080(3) 0.0483(4) 0.0195(3) -0.0184(3) 0.0043(2) -0.0048(3)
Cl1 0.0267(10) 0.0264(10) 0.0368(11) 0.000 0.0000(8) 0.000
O2 0.0079(17) 0.040(2) 0.0206(18) -0.0146(18) 0.0043(14) -0.0014(16)
O1 0.0146(17) 0.032(2) 0.0157(18) -0.0068(17) 0.0036(14) -0.0020(16)
C1 0.010(2) 0.021(2) 0.014(2) -0.003(2) 0.0028(19) -0.002(2)
C2 0.011(2) 0.019(2) 0.012(2) -0.001(2) 0.0017(18) -0.002(2)
N1 0.011(2) 0.025(2) 0.016(2) -0.0062(19) 0.0060(17) 0.0010(18)
C4 0.013(2) 0.030(3) 0.020(3) -0.011(2) -0.002(2) 0.000(2)
C3 0.011(2) 0.023(2) 0.013(2) -0.003(2) 0.0040(19) 0.003(2)
N2 0.0067(19) 0.029(2) 0.013(2) -0.0071(19) 0.0019(16) 0.0007(18)
N3 0.0054(19) 0.030(2) 0.016(2) -0.0044(19) 0.0011(16) -0.0001(18)
O4 0.0098(18) 0.057(3) 0.034(2) -0.019(2) 0.0030(16) -0.0030(19)
O3 0.019(2) 0.062(3) 0.023(2) -0.021(2) -0.0033(16) 0.011(2)
O5 0.0180(19) 0.042(2) 0.024(2) -0.0014(19) 0.0004(16) 0.0075(18)
O6 0.031(2) 0.059(3) 0.026(2) 0.008(2) 0.0056(18) -0.019(2)
O7 0.095(5) 0.078(4) 0.073(4) 0.005(4) 0.030(4) -0.030(4)

_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
Gd1 O3 2.276(4) . ?
Gd1 O3 2.276(4) 2_556 ?
Gd1 O5 2.383(4) 2_556 ?
Gd1 O5 2.383(3) . ?
Gd1 O1 2.451(3) 2_556 ?
Gd1 O1 2.451(3) . ?
Gd1 O6 2.477(4) . ?
Gd1 O6 2.477(4) 2_556 ?
Cu1 O2 1.963(3) . ?
Cu1 N1 1.966(4) . ?
Cu1 N2 1.967(4) 3_677 ?
Cu1 N3 2.076(4) 4_675 ?
Cu1 Cl1 2.5377(16) . ?
Cl1 Cu1 2.5378(16) 2_657 ?
O2 C1 1.271(6) . ?
O1 C1 1.237(6) . ?
C1 C2 1.495(6) . ?
C2 N1 1.339(6) . ?
C2 C3 1.394(6) . ?
N1 N2 1.330(5) . ?
C4 O4 1.235(6) . ?
C4 O3 1.259(6) . ?
C4 C3 1.499(7) . ?
C3 N3 1.338(6) . ?
N2 N3 1.323(5) . ?
N2 Cu1 1.967(4) 3_677 ?
N3 Cu1 2.076(4) 4_575 ?
O5 H5A 0.8621 . ?
O5 H5B 0.8627 . ?
O6 H6A 0.8533 . ?
O6 H6B 0.8531 . ?
O7 H7A 0.8499 . ?
O7 H7B 0.8503 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Gd1 O3 96.3(2) . 2_556 ?
O3 Gd1 O5 93.64(14) . 2_556 ?
O3 Gd1 O5 145.65(13) 2_556 2_556 ?
O3 Gd1 O5 145.65(13) . . ?
O3 Gd1 O5 93.64(14) 2_556 . ?
O5 Gd1 O5 96.47(19) 2_556 . ?
O3 Gd1 O1 71.31(12) . 2_556 ?
O3 Gd1 O1 77.45(12) 2_556 2_556 ?
O5 Gd1 O1 74.80(12) 2_556 2_556 ?
O5 Gd1 O1 143.04(12) . 2_556 ?
O3 Gd1 O1 77.45(12) . . ?
O3 Gd1 O1 71.31(12) 2_556 . ?
O5 Gd1 O1 143.04(12) 2_556 . ?
O5 Gd1 O1 74.79(12) . . ?
O1 Gd1 O1 132.48(17) 2_556 . ?
O3 Gd1 O6 77.29(15) . . ?
O3 Gd1 O6 143.70(13) 2_556 . ?
O5 Gd1 O6 70.62(13) 2_556 . ?
O5 Gd1 O6 75.35(14) . . ?
O1 Gd1 O6 130.97(12) 2_556 . ?
O1 Gd1 O6 72.42(12) . . ?
O3 Gd1 O6 143.70(13) . 2_556 ?
O3 Gd1 O6 77.29(15) 2_556 2_556 ?
O5 Gd1 O6 75.35(14) 2_556 2_556 ?
O5 Gd1 O6 70.62(13) . 2_556 ?
O1 Gd1 O6 72.42(12) 2_556 2_556 ?
O1 Gd1 O6 130.97(12) . 2_556 ?
O6 Gd1 O6 127.9(2) . 2_556 ?
O2 Cu1 N1 81.51(15) . . ?
O2 Cu1 N2 175.03(16) . 3_677 ?
N1 Cu1 N2 94.88(16) . 3_677 ?
O2 Cu1 N3 93.63(15) . 4_675 ?
N1 Cu1 N3 143.27(17) . 4_675 ?
N2 Cu1 N3 91.30(16) 3_677 4_675 ?
O2 Cu1 Cl1 90.98(11) . . ?
N1 Cu1 Cl1 125.83(13) . . ?
N2 Cu1 Cl1 88.37(12) 3_677 . ?
N3 Cu1 Cl1 90.45(12) 4_675 . ?
Cu1 Cl1 Cu1 84.85(7) . 2_657 ?
C1 O2 Cu1 116.5(3) . . ?
C1 O1 Gd1 145.9(3) . . ?
O1 C1 O2 123.9(4) . . ?
O1 C1 C2 122.1(4) . . ?
O2 C1 C2 114.0(4) . . ?
N1 C2 C3 106.3(4) . . ?
N1 C2 C1 114.3(4) . . ?
C3 C2 C1 139.4(4) . . ?
N2 N1 C2 109.0(4) . . ?
N2 N1 Cu1 137.1(3) . . ?
C2 N1 Cu1 113.4(3) . . ?
O4 C4 O3 125.3(5) . . ?
O4 C4 C3 117.7(4) . . ?
O3 C4 C3 117.0(4) . . ?
N3 C3 C2 106.9(4) . . ?
N3 C3 C4 120.1(4) . . ?
C2 C3 C4 133.0(4) . . ?
N3 N2 N1 108.9(4) . . ?
N3 N2 Cu1 123.5(3) . 3_677 ?
N1 N2 Cu1 127.5(3) . 3_677 ?
N2 N3 C3 108.9(4) . . ?
N2 N3 Cu1 118.2(3) . 4_575 ?
C3 N3 Cu1 131.5(3) . 4_575 ?
C4 O3 Gd1 149.7(4) . . ?
Gd1 O5 H5A 109.7 . . ?
Gd1 O5 H5B 110.0 . . ?
H5A O5 H5B 108.8 . . ?
Gd1 O6 H6A 109.8 . . ?
Gd1 O6 H6B 109.5 . . ?
H6A O6 H6B 109.4 . . ?
H7A O7 H7B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 940147'
#######################################################################
#
#                 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_2-Tb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Cl Cu2 N6 O14 Tb'
_chemical_formula_weight         737.65

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/a

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

_cell_length_a                   11.6342(4)
_cell_length_b                   6.8158(3)
_cell_length_c                   12.1505(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.834(4)
_cell_angle_gamma                90.00
_cell_volume                     935.54(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1740
_cell_measurement_theta_min      2.9827
_cell_measurement_theta_max      29.1076

_exptl_crystal_description       Block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    6.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3166
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1641
_reflns_number_gt                1436
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1491P)^2^+69.5422P] where P=(Fo^2^+2Fc^2^)/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         1641
_refine_ls_number_parameters     157
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0936
_refine_ls_wR_factor_ref         0.2699
_refine_ls_wR_factor_gt          0.2570
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.097
_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
Tb1 Tb 0.2500 0.01189(17) 0.0000 0.0135(5) Uani 1 2 d S . .
Cu2 Cu 0.6086(2) 0.4021(5) 0.4111(2) 0.0345(8) Uani 1 1 d . . .
Cl1 Cl 0.7500 0.1262(13) 0.5000 0.053(2) Uani 1 2 d S . .
N3 N 0.4368(15) 0.408(3) 0.3860(14) 0.030(4) Uani 1 1 d . . .
O4 O 0.5682(12) 0.265(2) 0.2638(13) 0.033(4) Uani 1 1 d . . .
O1 O 0.0553(13) 0.315(3) 0.2163(14) 0.041(4) Uani 1 1 d U . .
O3 O 0.4209(13) 0.159(3) 0.1271(13) 0.041(4) Uani 1 1 d . . .
C1 C 0.153(2) 0.294(4) 0.194(2) 0.039(5) Uani 1 1 d U . .
C2 C 0.2610(17) 0.350(3) 0.2785(16) 0.023(4) Uani 1 1 d . . .
C4 C 0.459(2) 0.242(3) 0.2179(18) 0.033(5) Uani 1 1 d . . .
C3 C 0.3816(16) 0.329(3) 0.2840(17) 0.023(4) Uani 1 1 d . . .
N2 N 0.3593(13) 0.477(2) 0.4361(13) 0.014(3) Uani 1 1 d U . .
N1 N 0.2527(14) 0.443(3) 0.3746(14) 0.023(3) Uani 1 1 d U . .
O5 O 0.4058(13) -0.214(2) 0.0082(14) 0.039(4) Uani 1 1 d . . .
H5A H 0.4032 -0.2674 -0.0594 0.058 Uiso 1 1 d R . .
H5B H 0.4018 -0.3120 0.0557 0.058 Uiso 1 1 d R . .
O2 O 0.1646(16) 0.231(3) 0.0990(16) 0.054(5) Uani 1 1 d U . .
O6 O 0.276(2) -0.143(3) 0.1869(15) 0.061(6) Uani 1 1 d . . .
H6A H 0.3260 -0.2574 0.1989 0.092 Uiso 1 1 d R . .
H6B H 0.2035 -0.1870 0.2013 0.092 Uiso 1 1 d R . .
O7 O 0.531(3) 0.104(5) 0.625(3) 0.037(7) Uani 0.50 1 d PU . .
O8 O 0.501(2) 0.124(4) 0.502(2) 0.025(6) Uani 0.50 1 d PU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tb1 0.0058(7) 0.0269(8) 0.0076(7) 0.000 0.0013(4) 0.000
Cu2 0.0210(13) 0.0572(19) 0.0256(13) -0.0205(13) 0.0061(10) -0.0059(12)
Cl1 0.053(5) 0.040(5) 0.060(6) 0.000 0.003(4) 0.000
N3 0.017(8) 0.049(11) 0.023(8) -0.011(8) 0.004(7) -0.009(8)
O4 0.018(7) 0.047(9) 0.038(8) -0.025(7) 0.016(6) -0.005(6)
O1 0.021(6) 0.049(7) 0.050(8) -0.018(6) 0.003(6) 0.002(6)
O3 0.028(8) 0.063(11) 0.031(8) -0.012(8) 0.008(7) -0.015(8)
C1 0.038(7) 0.042(7) 0.037(7) -0.007(5) 0.011(5) 0.002(5)
C2 0.027(10) 0.024(9) 0.022(9) -0.010(8) 0.013(8) -0.005(8)
C4 0.032(12) 0.037(11) 0.033(12) -0.010(10) 0.014(9) -0.009(10)
C3 0.017(9) 0.025(9) 0.029(10) 0.000(8) 0.008(8) -0.003(8)
N2 0.008(5) 0.023(5) 0.013(5) -0.003(4) 0.004(4) 0.000(4)
N1 0.018(5) 0.029(5) 0.024(5) -0.004(4) 0.010(4) 0.001(4)
O5 0.031(8) 0.040(9) 0.045(9) -0.006(7) 0.007(7) 0.012(7)
O2 0.050(6) 0.056(6) 0.053(6) -0.009(5) 0.008(4) 0.010(4)
O6 0.073(14) 0.070(13) 0.037(10) 0.020(9) 0.004(9) -0.019(11)
O7 0.044(11) 0.034(10) 0.038(10) 0.003(8) 0.019(8) -0.006(8)
O8 0.025(7) 0.025(8) 0.024(7) 0.000(5) 0.007(5) -0.001(5)

_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
Tb1 O2 2.289(18) 2 ?
Tb1 O2 2.289(18) . ?
Tb1 O5 2.363(14) 2 ?
Tb1 O5 2.363(14) . ?
Tb1 O3 2.424(15) . ?
Tb1 O3 2.424(15) 2 ?
Tb1 O6 2.456(17) 2 ?
Tb1 O6 2.456(17) . ?
Cu2 N3 1.950(17) . ?
Cu2 O4 1.973(14) . ?
Cu2 N2 1.984(15) 3_666 ?
Cu2 N1 2.114(16) 4_665 ?
Cu2 Cl1 2.561(7) . ?
Cl1 Cu2 2.561(7) 2_656 ?
N3 N2 1.29(2) . ?
N3 C3 1.36(3) . ?
O4 C4 1.27(3) . ?
O1 C1 1.24(3) . ?
O3 C4 1.22(3) . ?
C1 O2 1.27(3) . ?
C1 C2 1.47(3) . ?
C2 N1 1.35(2) . ?
C2 C3 1.40(3) . ?
C4 C3 1.47(3) . ?
N2 N1 1.31(2) . ?
N2 Cu2 1.984(15) 3_666 ?
N1 Cu2 2.114(16) 4_565 ?
O5 H5A 0.8918 . ?
O5 H5B 0.8903 . ?
O6 H6A 0.9637 . ?
O6 H6B 0.9527 . ?
O7 O8 1.46(4) . ?
O8 O8 1.69(6) 3_656 ?

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 Tb1 O2 98.5(10) 2 . ?
O2 Tb1 O5 146.0(6) 2 2 ?
O2 Tb1 O5 91.3(6) . 2 ?
O2 Tb1 O5 91.3(6) 2 . ?
O2 Tb1 O5 146.0(6) . . ?
O5 Tb1 O5 98.6(8) 2 . ?
O2 Tb1 O3 70.8(6) 2 . ?
O2 Tb1 O3 77.8(6) . . ?
O5 Tb1 O3 143.2(6) 2 . ?
O5 Tb1 O3 74.9(6) . . ?
O2 Tb1 O3 77.8(6) 2 2 ?
O2 Tb1 O3 70.8(6) . 2 ?
O5 Tb1 O3 74.9(6) 2 2 ?
O5 Tb1 O3 143.2(6) . 2 ?
O3 Tb1 O3 131.1(9) . 2 ?
O2 Tb1 O6 76.6(7) 2 2 ?
O2 Tb1 O6 142.4(7) . 2 ?
O5 Tb1 O6 75.9(7) 2 2 ?
O5 Tb1 O6 71.6(6) . 2 ?
O3 Tb1 O6 131.9(6) . 2 ?
O3 Tb1 O6 71.7(6) 2 2 ?
O2 Tb1 O6 142.4(7) 2 . ?
O2 Tb1 O6 76.6(7) . . ?
O5 Tb1 O6 71.6(6) 2 . ?
O5 Tb1 O6 75.9(7) . . ?
O3 Tb1 O6 71.8(6) . . ?
O3 Tb1 O6 131.9(6) 2 . ?
O6 Tb1 O6 129.2(10) 2 . ?
N3 Cu2 O4 81.7(6) . . ?
N3 Cu2 N2 95.4(7) . 3_666 ?
O4 Cu2 N2 175.1(6) . 3_666 ?
N3 Cu2 N1 142.3(8) . 4_665 ?
O4 Cu2 N1 94.3(6) . 4_665 ?
N2 Cu2 N1 90.4(6) 3_666 4_665 ?
N3 Cu2 Cl1 127.8(6) . . ?
O4 Cu2 Cl1 91.4(5) . . ?
N2 Cu2 Cl1 87.3(4) 3_666 . ?
N1 Cu2 Cl1 89.6(5) 4_665 . ?
Cu2 Cl1 Cu2 85.5(3) 2_656 . ?
N2 N3 C3 110.0(16) . . ?
N2 N3 Cu2 137.8(13) . . ?
C3 N3 Cu2 112.1(13) . . ?
C4 O4 Cu2 117.0(12) . . ?
C4 O3 Tb1 145.9(14) . . ?
O1 C1 O2 123(2) . . ?
O1 C1 C2 120(2) . . ?
O2 C1 C2 117(2) . . ?
N1 C2 C3 106.5(17) . . ?
N1 C2 C1 119.8(18) . . ?
C3 C2 C1 133.7(18) . . ?
O3 C4 O4 124(2) . . ?
O3 C4 C3 123(2) . . ?
O4 C4 C3 112.9(18) . . ?
N3 C3 C2 104.6(17) . . ?
N3 C3 C4 116.2(17) . . ?
C2 C3 C4 139.1(19) . . ?
N3 N2 N1 110.0(15) . . ?
N3 N2 Cu2 126.6(12) . 3_666 ?
N1 N2 Cu2 123.3(12) . 3_666 ?
N2 N1 C2 108.8(15) . . ?
N2 N1 Cu2 119.0(12) . 4_565 ?
C2 N1 Cu2 129.7(14) . 4_565 ?
Tb1 O5 H5A 111.7 . . ?
Tb1 O5 H5B 110.9 . . ?
H5A O5 H5B 107.3 . . ?
C1 O2 Tb1 148.6(17) . . ?
Tb1 O6 H6A 115.2 . . ?
Tb1 O6 H6B 112.7 . . ?
H6A O6 H6B 104.0 . . ?
O7 O8 O8 86(2) . 3_656 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         10.090
_refine_diff_density_min         -2.142
_refine_diff_density_rms         0.502
_database_code_depnum_ccdc_archive 'CCDC 940148'
#######################################################################
#
#                 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_3-Dy

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Cl Cu2 Dy N6 O14'
_chemical_formula_weight         741.27

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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   P2/a

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

_cell_length_a                   11.550(2)
_cell_length_b                   6.7557(15)
_cell_length_c                   12.137(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.35(3)
_cell_angle_gamma                90.00
_cell_volume                     921.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    128(2)
_cell_measurement_reflns_used    1651
_cell_measurement_theta_min      3.0092
_cell_measurement_theta_max      28.9365

_exptl_crystal_description       Block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             710
_exptl_absorpt_coefficient_mu    6.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CRYSALISPRO

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      128(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3215
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1619
_reflns_number_gt                1379
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSALISPRO
_computing_cell_refinement       CRYSALISPRO
_computing_data_reduction        CRYSALISPRO
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0374P)^2^+49.2739P] where P=(Fo^2^+2Fc^2^)/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         1619
_refine_ls_number_parameters     164
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.7500 0.51314(6) 1.0000 0.01747(11) Uani 1 2 d SU . .
Cu1 Cu 0.88773(6) 1.10052(13) 0.58924(7) 0.0233(2) Uani 1 1 d U . .
Cl1 Cl 0.7500 1.3724(3) 0.5000 0.0344(8) Uani 1 2 d S . .
O4 O 0.4272(4) 0.7632(7) 0.7370(4) 0.0248(6) Uani 1 1 d U . .
O1 O 0.8331(4) 0.7337(8) 0.9036(4) 0.0391(15) Uani 1 1 d . . .
O2 O 0.9452(4) 0.8169(7) 0.7861(4) 0.0308(10) Uani 1 1 d U . .
O6 O 0.7276(4) 0.3514(8) 0.8177(4) 0.0368(15) Uani 1 1 d . . .
H6A H 0.6917 0.4290 0.7658 0.055 Uiso 1 1 d R . .
H6B H 0.7960 0.3237 0.8071 0.055 Uiso 1 1 d R . .
N1 N 0.7484(5) 0.9516(8) 0.6288(5) 0.0197(7) Uani 1 1 d U . .
O3 O 0.5759(4) 0.6570(7) 0.8743(4) 0.0226(12) Uani 1 1 d . . .
N2 N 0.6413(4) 0.9742(8) 0.5640(4) 0.0188(11) Uani 1 1 d U . .
N3 N 0.5615(4) 0.8983(8) 0.6143(5) 0.0200(11) Uani 1 1 d U . .
C4 C 0.5391(5) 0.7407(9) 0.7840(5) 0.0197(7) Uani 1 1 d U . .
C3 C 0.6186(5) 0.8249(9) 0.7163(5) 0.0184(12) Uani 1 1 d U . .
C1 C 0.8489(6) 0.7987(11) 0.8129(6) 0.0306(14) Uani 1 1 d U . .
C2 C 0.7401(5) 0.8579(10) 0.7242(6) 0.0249(19) Uani 1 1 d . . .
O5 O 0.5946(4) 0.2840(6) 0.9890(4) 0.0245(13) Uani 1 1 d . . .
H5A H 0.6218 0.1611 1.0069 0.037 Uiso 1 1 d R . .
H5B H 0.5488 0.3158 1.0367 0.037 Uiso 1 1 d R . .
O7 O 0.5072(12) 0.3479(17) 0.6299(14) 0.066(5) Uani 0.454(10) 1 d PG A 2
H7A H 0.5702 0.2841 0.6280 0.100 Uiso 0.454(10) 1 d PG A 2
H7B H 0.4561 0.3320 0.5677 0.100 Uiso 0.454(10) 1 d PG A 2
O8 O 0.5458(8) 0.4312(14) 0.6302(8) 0.035(2) Uani 0.546(10) 1 d PGU A 1
H8A H 0.5942 0.3498 0.6697 0.053 Uiso 0.546(10) 1 d PG A 1
H8B H 0.5694 0.4615 0.5710 0.053 Uiso 0.546(10) 1 d PG A 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.00231(15) 0.01993(19) 0.0294(2) 0.000 0.00210(15) 0.000
Cu1 0.0036(3) 0.0331(4) 0.0328(4) -0.0093(3) 0.0031(3) -0.0021(3)
Cl1 0.0142(10) 0.0173(10) 0.0662(17) 0.000 -0.0021(11) 0.000
O4 0.0217(10) 0.0260(10) 0.0259(10) 0.0016(8) 0.0037(8) 0.0000(8)
O1 0.009(2) 0.066(3) 0.036(3) 0.033(2) -0.007(2) -0.010(2)
O2 0.0207(16) 0.0374(17) 0.0344(17) 0.0073(14) 0.0064(13) -0.0022(14)
O6 0.014(2) 0.065(3) 0.031(3) 0.013(3) 0.0066(19) 0.020(2)
N1 0.0179(10) 0.0204(10) 0.0204(11) 0.0006(8) 0.0033(8) 0.0005(8)
O3 0.0135(19) 0.024(2) 0.032(2) 0.009(2) 0.0093(18) 0.0014(18)
N2 0.0109(18) 0.0244(19) 0.0201(19) 0.0028(16) 0.0012(15) -0.0010(16)
N3 0.0118(18) 0.0233(19) 0.0250(19) 0.0035(16) 0.0046(15) -0.0013(16)
C4 0.0185(10) 0.0198(11) 0.0211(11) 0.0001(9) 0.0052(8) -0.0003(9)
C3 0.0128(19) 0.020(2) 0.020(2) 0.0066(17) 0.0003(16) -0.0003(17)
C1 0.026(2) 0.032(2) 0.032(2) 0.0039(19) 0.0034(18) -0.0026(18)
C2 0.007(3) 0.032(3) 0.037(4) 0.007(3) 0.008(3) 0.004(3)
O5 0.0086(19) 0.017(2) 0.046(3) 0.004(2) 0.0029(19) 0.0007(17)
O7 0.043(7) 0.023(6) 0.126(12) 0.036(7) 0.005(8) 0.005(6)
O8 0.033(4) 0.029(4) 0.042(4) -0.014(3) 0.007(3) 0.000(3)

_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
Dy1 O1 2.243(5) . ?
Dy1 O1 2.243(5) 2_657 ?
Dy1 O5 2.351(4) . ?
Dy1 O5 2.351(4) 2_657 ?
Dy1 O6 2.427(5) 2_657 ?
Dy1 O6 2.427(5) . ?
Dy1 O3 2.429(4) 2_657 ?
Dy1 O3 2.429(4) . ?
Cu1 N3 1.959(5) 4_675 ?
Cu1 O4 1.973(5) 4_675 ?
Cu1 N2 2.003(5) 2_656 ?
Cu1 N1 2.046(6) . ?
Cu1 Cl1 2.5063(19) . ?
Cl1 Cu1 2.5062(19) 2_656 ?
O4 C4 1.295(7) . ?
O4 Cu1 1.973(5) 4_575 ?
O1 C1 1.237(9) . ?
O2 C1 1.235(9) . ?
O6 H6A 0.8501 . ?
O6 H6B 0.8501 . ?
N1 N2 1.313(7) . ?
N1 C2 1.342(9) . ?
O3 C4 1.219(7) . ?
N2 N3 1.321(8) . ?
N2 Cu1 2.003(5) 2_656 ?
N3 C3 1.355(8) . ?
N3 Cu1 1.959(5) 4_575 ?
C4 C3 1.480(10) . ?
C3 C2 1.403(9) . ?
C1 C2 1.508(9) . ?
O5 H5A 0.8967 . ?
O5 H5B 0.8950 . ?
O7 H7A 0.8502 . ?
O7 H7B 0.8505 . ?
O7 H8A 1.0100 . ?
O7 H8B 1.3619 . ?
O8 H7A 1.0346 . ?
O8 H7B 1.3167 . ?
O8 H8A 0.8496 . ?
O8 H8B 0.8502 . ?

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 Dy1 O1 96.7(3) . 2_657 ?
O1 Dy1 O5 145.21(16) . . ?
O1 Dy1 O5 93.08(18) 2_657 . ?
O1 Dy1 O5 93.08(18) . 2_657 ?
O1 Dy1 O5 145.21(16) 2_657 2_657 ?
O5 Dy1 O5 97.6(2) . 2_657 ?
O1 Dy1 O6 143.74(16) . 2_657 ?
O1 Dy1 O6 77.98(19) 2_657 2_657 ?
O5 Dy1 O6 71.00(16) . 2_657 ?
O5 Dy1 O6 74.50(18) 2_657 2_657 ?
O1 Dy1 O6 77.98(19) . . ?
O1 Dy1 O6 143.74(16) 2_657 . ?
O5 Dy1 O6 74.50(18) . . ?
O5 Dy1 O6 71.00(16) 2_657 . ?
O6 Dy1 O6 126.5(3) 2_657 . ?
O1 Dy1 O3 70.73(16) . 2_657 ?
O1 Dy1 O3 78.36(16) 2_657 2_657 ?
O5 Dy1 O3 144.06(16) . 2_657 ?
O5 Dy1 O3 73.58(15) 2_657 2_657 ?
O6 Dy1 O3 73.08(16) 2_657 2_657 ?
O6 Dy1 O3 130.65(16) . 2_657 ?
O1 Dy1 O3 78.36(16) . . ?
O1 Dy1 O3 70.73(16) 2_657 . ?
O5 Dy1 O3 73.58(15) . . ?
O5 Dy1 O3 144.06(16) 2_657 . ?
O6 Dy1 O3 130.65(16) 2_657 . ?
O6 Dy1 O3 73.08(16) . . ?
O3 Dy1 O3 132.8(2) 2_657 . ?
N3 Cu1 O4 81.0(2) 4_675 4_675 ?
N3 Cu1 N2 95.3(2) 4_675 2_656 ?
O4 Cu1 N2 175.3(2) 4_675 2_656 ?
N3 Cu1 N1 143.0(2) 4_675 . ?
O4 Cu1 N1 92.6(2) 4_675 . ?
N2 Cu1 N1 92.1(2) 2_656 . ?
N3 Cu1 Cl1 126.11(17) 4_675 . ?
O4 Cu1 Cl1 92.36(14) 4_675 . ?
N2 Cu1 Cl1 87.56(15) 2_656 . ?
N1 Cu1 Cl1 90.39(14) . . ?
Cu1 Cl1 Cu1 85.75(8) 2_656 . ?
C4 O4 Cu1 116.9(4) . 4_575 ?
C1 O1 Dy1 150.3(5) . . ?
Dy1 O6 H6A 109.2 . . ?
Dy1 O6 H6B 109.3 . . ?
H6A O6 H6B 109.5 . . ?
N2 N1 C2 109.0(5) . . ?
N2 N1 Cu1 119.0(4) . . ?
C2 N1 Cu1 130.6(4) . . ?
C4 O3 Dy1 144.8(4) . . ?
N1 N2 N3 109.9(5) . . ?
N1 N2 Cu1 122.6(4) . 2_656 ?
N3 N2 Cu1 127.5(4) . 2_656 ?
N2 N3 C3 108.6(5) . . ?
N2 N3 Cu1 136.6(4) . 4_575 ?
C3 N3 Cu1 114.1(4) . 4_575 ?
O3 C4 O4 123.8(6) . . ?
O3 C4 C3 123.0(5) . . ?
O4 C4 C3 113.2(5) . . ?
N3 C3 C2 105.8(6) . . ?
N3 C3 C4 114.5(5) . . ?
C2 C3 C4 139.7(6) . . ?
O2 C1 O1 126.6(6) . . ?
O2 C1 C2 116.0(7) . . ?
O1 C1 C2 117.4(6) . . ?
N1 C2 C3 106.6(5) . . ?
N1 C2 C1 121.8(6) . . ?
C3 C2 C1 131.4(7) . . ?
Dy1 O5 H5A 112.0 . . ?
Dy1 O5 H5B 111.3 . . ?
H5A O5 H5B 107.0 . . ?
H7A O7 H7B 109.5 . . ?
H7A O7 H8A 41.9 . . ?
H7B O7 H8A 146.7 . . ?
H7A O7 H8B 73.3 . . ?
H7B O7 H8B 87.0 . . ?
H7A O8 H7B 71.3 . . ?
H7A O8 H8A 41.0 . . ?
H7B O8 H8A 108.9 . . ?
H7A O8 H8B 93.9 . . ?
H7B O8 H8B 90.0 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.455
_refine_diff_density_min         -2.797
_refine_diff_density_rms         0.339
_database_code_depnum_ccdc_archive 'CCDC 940149'
#######################################################################
#
#                 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_4-Ho

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Cl Cu2 Ho N6 O14'
_chemical_formula_weight         743.70

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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   P2/a

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

_cell_length_a                   11.5691(17)
_cell_length_b                   6.7563(9)
_cell_length_c                   12.088(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.437(15)
_cell_angle_gamma                90.00
_cell_volume                     919.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1895
_cell_measurement_theta_min      3.0089
_cell_measurement_theta_max      29.3531

_exptl_crystal_description       Block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    6.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.27523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CRYSALISPRO

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3224
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1617
_reflns_number_gt                1521
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSALISPRO
_computing_cell_refinement       CRYSALISPRO
_computing_data_reduction        CRYSALISPRO
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0267P)^2^+10.9587P] where P=(Fo^2^+2Fc^2^)/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         1617
_refine_ls_number_parameters     151
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_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 0.1516(7) 0.2050(15) 0.1883(9) 0.024(2) Uani 1 1 d . . .
C2 C 0.2615(7) 0.1457(13) 0.2764(7) 0.0110(17) Uani 1 1 d . . .
C3 C 0.3819(7) 0.1764(13) 0.2864(7) 0.0108(17) Uani 1 1 d . . .
C4 C 0.4623(7) 0.2624(13) 0.2183(7) 0.0113(18) Uani 1 1 d U . .
Cl1 Cl 0.2500 -0.3752(5) 0.5000 0.0207(7) Uani 1 2 d S . .
Cu1 Cu 0.11249(8) -0.10094(17) 0.41109(9) 0.0164(3) Uani 1 1 d . . .
Ho1 Ho 0.2500 0.48838(8) 0.0000 0.00938(18) Uani 1 2 d S . .
N1 N 0.2510(6) 0.0514(11) 0.3723(6) 0.0139(16) Uani 1 1 d . . .
N2 N 0.3590(6) 0.0266(11) 0.4374(6) 0.0121(15) Uani 1 1 d U . .
N3 N 0.4386(6) 0.1018(11) 0.3877(6) 0.0112(15) Uani 1 1 d . . .
O1 O 0.1677(5) 0.2682(11) 0.0958(5) 0.0269(17) Uani 1 1 d . . .
O2 O 0.0540(5) 0.1834(10) 0.2134(5) 0.0220(15) Uani 1 1 d . . .
O3 O 0.4236(4) 0.3454(9) 0.1261(5) 0.0136(13) Uani 1 1 d . . .
O4 O 0.5730(5) 0.2388(9) 0.2640(5) 0.0152(13) Uani 1 1 d U . .
O5 O 0.4049(5) 0.7143(9) 0.0095(5) 0.0149(13) Uani 1 1 d . . .
H5A H 0.4448 0.6819 -0.0387 0.022 Uiso 1 1 d R . .
H5B H 0.3762 0.8296 -0.0058 0.022 Uiso 1 1 d R . .
O6 O 0.2736(5) 0.6476(11) 0.1839(5) 0.0261(16) Uani 1 1 d . . .
H6A H 0.2052 0.6523 0.2059 0.039 Uiso 1 1 d R . .
H6B H 0.3256 0.5823 0.2373 0.039 Uiso 1 1 d R . .
O7 O -0.0293(10) 0.3947(18) 0.3717(8) 0.077(4) Uani 1 1 d G . .
H7A H -0.0035 0.3542 0.3154 0.116 Uiso 1 1 d G . .
H7B H 0.0104 0.3412 0.4324 0.116 Uiso 1 1 d G . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.008(5) 0.028(6) 0.032(6) 0.013(5) -0.002(4) -0.008(4)
C2 0.005(4) 0.017(4) 0.009(4) 0.001(4) -0.002(3) -0.002(3)
C3 0.008(4) 0.017(5) 0.006(4) 0.005(3) 0.000(3) 0.004(3)
C4 0.006(3) 0.016(4) 0.012(4) 0.001(3) 0.000(3) 0.000(3)
Cl1 0.0159(15) 0.0144(16) 0.0280(18) 0.000 -0.0027(12) 0.000
Cu1 0.0034(5) 0.0328(7) 0.0128(6) -0.0120(5) 0.0011(4) -0.0031(4)
Ho1 0.0041(3) 0.0150(3) 0.0086(3) 0.000 0.00056(19) 0.000
N1 0.008(4) 0.026(4) 0.006(4) 0.002(3) -0.002(3) 0.002(3)
N2 0.005(3) 0.017(3) 0.013(3) 0.003(3) -0.001(2) -0.001(2)
N3 0.010(3) 0.019(4) 0.005(3) 0.001(3) 0.003(3) -0.001(3)
O1 0.012(3) 0.047(5) 0.018(4) 0.021(3) -0.003(3) -0.009(3)
O2 0.004(3) 0.042(4) 0.019(4) 0.011(3) -0.001(2) 0.001(3)
O3 0.007(3) 0.024(3) 0.008(3) 0.007(3) -0.003(2) 0.002(2)
O4 0.006(3) 0.025(3) 0.014(3) 0.008(2) 0.001(2) 0.004(2)
O5 0.011(3) 0.015(3) 0.018(3) 0.002(3) -0.001(2) 0.001(2)
O6 0.015(3) 0.048(5) 0.015(3) -0.003(3) 0.002(2) 0.013(3)
O7 0.102(8) 0.099(9) 0.036(6) -0.010(6) 0.027(6) -0.063(7)

_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 1.244(10) . ?
C1 O1 1.250(11) . ?
C1 C2 1.511(11) . ?
C2 N1 1.352(11) . ?
C2 C3 1.385(11) . ?
C3 N3 1.346(10) . ?
C3 C4 1.496(11) . ?
C4 O3 1.235(10) . ?
C4 O4 1.281(9) . ?
Cl1 Cu1 2.515(3) . ?
Cl1 Cu1 2.515(3) 2_556 ?
Cu1 O4 1.965(6) 4 ?
Cu1 N3 1.966(6) 4 ?
Cu1 N2 1.981(7) 2_556 ?
Cu1 N1 2.049(7) . ?
Ho1 O1 2.230(6) 2 ?
Ho1 O1 2.230(6) . ?
Ho1 O5 2.337(6) . ?
Ho1 O5 2.337(5) 2 ?
Ho1 O3 2.423(5) . ?
Ho1 O3 2.423(5) 2 ?
Ho1 O6 2.428(6) 2 ?
Ho1 O6 2.428(6) . ?
N1 N2 1.323(9) . ?
N2 N3 1.313(9) . ?
N2 Cu1 1.981(7) 2_556 ?
N3 Cu1 1.966(6) 4_655 ?
O4 Cu1 1.965(6) 4_655 ?
O5 H5A 0.8504 . ?
O5 H5B 0.8503 . ?
O6 H6A 0.8919 . ?
O6 H6B 0.8906 . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8501 . ?

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 126.2(8) . . ?
O2 C1 C2 117.3(8) . . ?
O1 C1 C2 116.4(7) . . ?
N1 C2 C3 106.5(7) . . ?
N1 C2 C1 120.1(7) . . ?
C3 C2 C1 133.3(8) . . ?
N3 C3 C2 106.9(7) . . ?
N3 C3 C4 114.3(7) . . ?
C2 C3 C4 138.7(8) . . ?
O3 C4 O4 124.2(7) . . ?
O3 C4 C3 122.1(7) . . ?
O4 C4 C3 113.7(7) . . ?
Cu1 Cl1 Cu1 85.08(11) . 2_556 ?
O4 Cu1 N3 81.6(2) 4 4 ?
O4 Cu1 N2 175.3(3) 4 2_556 ?
N3 Cu1 N2 94.5(3) 4 2_556 ?
O4 Cu1 N1 93.5(3) 4 . ?
N3 Cu1 N1 142.9(3) 4 . ?
N2 Cu1 N1 91.2(3) 2_556 . ?
O4 Cu1 Cl1 91.63(19) 4 . ?
N3 Cu1 Cl1 125.7(2) 4 . ?
N2 Cu1 Cl1 88.4(2) 2_556 . ?
N1 Cu1 Cl1 91.0(2) . . ?
O1 Ho1 O1 96.3(4) 2 . ?
O1 Ho1 O5 92.6(2) 2 . ?
O1 Ho1 O5 145.6(2) . . ?
O1 Ho1 O5 145.6(2) 2 2 ?
O1 Ho1 O5 92.6(2) . 2 ?
O5 Ho1 O5 98.4(3) . 2 ?
O1 Ho1 O3 70.7(2) 2 . ?
O1 Ho1 O3 78.4(2) . . ?
O5 Ho1 O3 73.4(2) . . ?
O5 Ho1 O3 143.7(2) 2 . ?
O1 Ho1 O3 78.4(2) 2 2 ?
O1 Ho1 O3 70.7(2) . 2 ?
O5 Ho1 O3 143.7(2) . 2 ?
O5 Ho1 O3 73.4(2) 2 2 ?
O3 Ho1 O3 133.0(3) . 2 ?
O1 Ho1 O6 77.9(3) 2 2 ?
O1 Ho1 O6 143.2(2) . 2 ?
O5 Ho1 O6 71.2(2) . 2 ?
O5 Ho1 O6 75.2(2) 2 2 ?
O3 Ho1 O6 130.79(19) . 2 ?
O3 Ho1 O6 72.5(2) 2 2 ?
O1 Ho1 O6 143.2(2) 2 . ?
O1 Ho1 O6 77.9(3) . . ?
O5 Ho1 O6 75.2(2) . . ?
O5 Ho1 O6 71.2(2) 2 . ?
O3 Ho1 O6 72.5(2) . . ?
O3 Ho1 O6 130.79(19) 2 . ?
O6 Ho1 O6 127.4(3) 2 . ?
N2 N1 C2 108.0(6) . . ?
N2 N1 Cu1 118.7(5) . . ?
C2 N1 Cu1 131.6(5) . . ?
N3 N2 N1 110.1(7) . . ?
N3 N2 Cu1 127.4(5) . 2_556 ?
N1 N2 Cu1 122.5(5) . 2_556 ?
N2 N3 C3 108.4(6) . . ?
N2 N3 Cu1 137.4(6) . 4_655 ?
C3 N3 Cu1 113.5(5) . 4_655 ?
C1 O1 Ho1 149.6(7) . . ?
C4 O3 Ho1 145.4(5) . . ?
C4 O4 Cu1 116.6(5) . 4_655 ?
Ho1 O5 H5A 109.2 . . ?
Ho1 O5 H5B 109.3 . . ?
H5A O5 H5B 109.5 . . ?
Ho1 O6 H6A 111.7 . . ?
Ho1 O6 H6B 110.9 . . ?
H6A O6 H6B 107.3 . . ?
H7A O7 H7B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.465
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.224
_database_code_depnum_ccdc_archive 'CCDC 940150'
#######################################################################
#
#                 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_5-Er

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Cl Cu2 Er N6 O14'
_chemical_formula_weight         746.02

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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   P2/a

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

_cell_length_a                   11.5842(10)
_cell_length_b                   6.7720(6)
_cell_length_c                   12.0905(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.604(11)
_cell_angle_gamma                90.00
_cell_volume                     921.87(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    128.70(14)
_cell_measurement_reflns_used    3328
_cell_measurement_theta_min      3.0020
_cell_measurement_theta_max      29.1294

_exptl_crystal_description       Block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             706
_exptl_absorpt_coefficient_mu    7.031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CRYSALISPRO

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      128.70(14)
_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  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5548
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1620
_reflns_number_gt                1574
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSALISPRO
_computing_cell_refinement       CRYSALISPRO
_computing_data_reduction        CRYSALISPRO
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0008P)^2^+50.5032P] where P=(Fo^2^+2Fc^2^)/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         1620
_refine_ls_number_parameters     157
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.207
_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
Er1 Er 0.7500 0.98821(12) 1.0000 0.0096(3) Uani 1 2 d S . .
Cu1 Cu 0.38932(14) 0.6003(3) 0.58916(14) 0.0207(4) Uani 1 1 d . . .
Cl1 Cl 0.2500 0.8751(8) 0.5000 0.0300(12) Uani 1 2 d S . .
O3 O 0.8331(9) 0.7698(17) 0.9034(9) 0.033(3) Uani 1 1 d U . .
O5 O 0.7764(10) 1.1474(18) 1.1834(9) 0.035(3) Uani 1 1 d . . .
H5A H 0.7074 1.1630 1.2034 0.053 Uiso 1 1 d R . .
H5B H 0.8235 1.0761 1.2377 0.053 Uiso 1 1 d R . .
O1 O 0.4275(8) 0.7375(15) 0.7371(8) 0.021(2) Uani 1 1 d . . .
O6 O 0.9039(8) 1.2112(14) 1.0075(8) 0.019(2) Uani 1 1 d . . .
H6A H 0.9102 1.2399 0.9396 0.028 Uiso 1 1 d R . .
H6B H 0.8900 1.3183 1.0408 0.028 Uiso 1 1 d R . .
O2 O 0.5774(8) 0.8448(15) 0.8751(8) 0.022(2) Uani 1 1 d . . .
N2 N 0.6415(8) 0.5262(16) 0.5633(8) 0.010(2) Uani 1 1 d U . .
N3 N 0.7486(9) 0.5533(17) 0.6268(10) 0.018(2) Uani 1 1 d U . .
O4 O 0.9462(8) 0.6840(16) 0.7869(8) 0.025(2) Uani 1 1 d U . .
N1 N 0.5624(9) 0.5995(17) 0.6141(10) 0.018(2) Uani 1 1 d . . .
C1 C 0.5387(11) 0.760(2) 0.7825(12) 0.018(3) Uani 1 1 d . . .
C3 C 0.7383(11) 0.648(2) 0.7231(10) 0.016(3) Uani 1 1 d . . .
C4 C 0.8499(13) 0.707(2) 0.8117(14) 0.032(4) Uani 1 1 d . . .
C2 C 0.6194(11) 0.672(2) 0.7147(11) 0.017(3) Uani 1 1 d . . .
O7 O 0.4716(18) 0.896(3) 0.3718(14) 0.056(5) Uani 0.75 1 d P . .
O8 O 0.503(4) 0.886(7) 0.499(4) 0.035(10) Uani 0.25 1 d PU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Er1 0.0043(4) 0.0168(4) 0.0072(4) 0.000 0.0006(3) 0.000
Cu1 0.0100(8) 0.0364(11) 0.0150(8) -0.0124(8) 0.0013(6) -0.0031(7)
Cl1 0.025(3) 0.017(3) 0.043(3) 0.000 -0.001(2) 0.000
O3 0.026(4) 0.037(4) 0.030(4) -0.014(4) -0.002(3) 0.008(4)
O5 0.035(6) 0.045(7) 0.024(6) -0.006(5) 0.005(5) 0.014(6)
O1 0.007(4) 0.035(6) 0.022(5) -0.014(4) 0.004(4) -0.001(4)
O6 0.016(5) 0.020(5) 0.017(5) 0.000(4) -0.001(4) -0.001(4)
O2 0.023(5) 0.026(5) 0.018(5) -0.011(4) 0.004(4) -0.010(4)
N2 0.004(4) 0.018(4) 0.010(4) -0.002(3) 0.003(3) 0.001(3)
N3 0.013(4) 0.024(4) 0.017(4) -0.003(4) 0.003(3) -0.001(3)
O4 0.011(4) 0.035(5) 0.027(5) -0.016(4) 0.000(4) 0.000(4)
N1 0.009(5) 0.026(6) 0.019(6) -0.007(5) 0.005(5) -0.005(5)
C1 0.010(6) 0.022(7) 0.024(8) -0.007(6) 0.006(5) -0.003(5)
C3 0.015(6) 0.024(7) 0.008(6) -0.008(5) 0.001(5) 0.004(6)
C4 0.016(7) 0.034(9) 0.041(10) -0.024(8) -0.001(7) 0.010(7)
C2 0.011(6) 0.025(8) 0.015(7) -0.003(6) 0.008(5) -0.006(6)
O7 0.079(13) 0.066(13) 0.027(9) -0.009(9) 0.018(9) -0.048(11)
O8 0.036(11) 0.036(11) 0.034(11) 0.000(5) 0.009(5) 0.000(5)

_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
Er1 O3 2.237(10) 2_657 ?
Er1 O3 2.237(10) . ?
Er1 O6 2.322(9) 2_657 ?
Er1 O6 2.322(9) . ?
Er1 O2 2.409(9) . ?
Er1 O2 2.409(9) 2_657 ?
Er1 O5 2.420(11) . ?
Er1 O5 2.420(10) 2_657 ?
Cu1 N1 1.956(11) . ?
Cu1 O1 1.971(9) . ?
Cu1 N2 1.988(10) 3_666 ?
Cu1 N3 2.073(11) 4_565 ?
Cu1 Cl1 2.532(4) . ?
Cl1 Cu1 2.532(4) 2_556 ?
O3 C4 1.246(18) . ?
O5 H5A 0.8936 . ?
O5 H5B 0.8911 . ?
O1 C1 1.285(15) . ?
O6 H6A 0.8631 . ?
O6 H6B 0.8627 . ?
O2 C1 1.242(16) . ?
N2 N3 1.309(14) . ?
N2 N1 1.314(14) . ?
N2 Cu1 1.988(10) 3_666 ?
N3 C3 1.358(16) . ?
N3 Cu1 2.073(11) 4_665 ?
O4 C4 1.232(17) . ?
N1 C2 1.334(17) . ?
C1 C2 1.504(18) . ?
C3 C2 1.368(18) . ?
C3 C4 1.525(19) . ?
O7 O8 1.49(5) . ?
O8 O8 1.55(9) 3_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Er1 O3 97.3(6) 2_657 . ?
O3 Er1 O6 91.7(4) 2_657 2_657 ?
O3 Er1 O6 146.1(4) . 2_657 ?
O3 Er1 O6 146.1(4) 2_657 . ?
O3 Er1 O6 91.7(4) . . ?
O6 Er1 O6 98.9(5) 2_657 . ?
O3 Er1 O2 70.4(4) 2_657 . ?
O3 Er1 O2 78.6(4) . . ?
O6 Er1 O2 73.8(3) 2_657 . ?
O6 Er1 O2 143.4(3) . . ?
O3 Er1 O2 78.6(4) 2_657 2_657 ?
O3 Er1 O2 70.4(4) . 2_657 ?
O6 Er1 O2 143.4(3) 2_657 2_657 ?
O6 Er1 O2 73.8(3) . 2_657 ?
O2 Er1 O2 132.4(5) . 2_657 ?
O3 Er1 O5 78.1(4) 2_657 . ?
O3 Er1 O5 142.7(4) . . ?
O6 Er1 O5 71.1(3) 2_657 . ?
O6 Er1 O5 75.2(4) . . ?
O2 Er1 O5 131.4(4) . . ?
O2 Er1 O5 72.4(4) 2_657 . ?
O3 Er1 O5 142.7(4) 2_657 2_657 ?
O3 Er1 O5 78.1(4) . 2_657 ?
O6 Er1 O5 75.2(4) 2_657 2_657 ?
O6 Er1 O5 71.1(3) . 2_657 ?
O2 Er1 O5 72.4(4) . 2_657 ?
O2 Er1 O5 131.4(4) 2_657 2_657 ?
O5 Er1 O5 127.1(6) . 2_657 ?
N1 Cu1 O1 81.9(4) . . ?
N1 Cu1 N2 95.5(4) . 3_666 ?
O1 Cu1 N2 176.2(4) . 3_666 ?
N1 Cu1 N3 142.7(5) . 4_565 ?
O1 Cu1 N3 93.3(4) . 4_565 ?
N2 Cu1 N3 90.5(4) 3_666 4_565 ?
N1 Cu1 Cl1 126.5(4) . . ?
O1 Cu1 Cl1 91.4(3) . . ?
N2 Cu1 Cl1 88.0(3) 3_666 . ?
N3 Cu1 Cl1 90.4(3) 4_565 . ?
Cu1 Cl1 Cu1 85.40(17) . 2_556 ?
C4 O3 Er1 150.2(11) . . ?
Er1 O5 H5A 111.8 . . ?
Er1 O5 H5B 110.9 . . ?
H5A O5 H5B 107.2 . . ?
C1 O1 Cu1 115.7(8) . . ?
Er1 O6 H6A 110.2 . . ?
Er1 O6 H6B 109.8 . . ?
H6A O6 H6B 108.8 . . ?
C1 O2 Er1 145.1(9) . . ?
N3 N2 N1 110.0(10) . . ?
N3 N2 Cu1 122.9(8) . 3_666 ?
N1 N2 Cu1 127.1(8) . 3_666 ?
N2 N3 C3 107.9(10) . . ?
N2 N3 Cu1 119.1(8) . 4_665 ?
C3 N3 Cu1 131.0(9) . 4_665 ?
N2 N1 C2 108.4(10) . . ?
N2 N1 Cu1 137.0(9) . . ?
C2 N1 Cu1 114.1(9) . . ?
O2 C1 O1 123.6(12) . . ?
O2 C1 C2 122.4(12) . . ?
O1 C1 C2 114.0(11) . . ?
N3 C3 C2 106.4(11) . . ?
N3 C3 C4 119.7(11) . . ?
C2 C3 C4 133.9(12) . . ?
O4 C4 O3 126.9(14) . . ?
O4 C4 C3 117.6(13) . . ?
O3 C4 C3 115.6(12) . . ?
N1 C2 C3 107.3(11) . . ?
N1 C2 C1 114.0(11) . . ?
C3 C2 C1 138.7(12) . . ?
O7 O8 O8 89(4) . 3_676 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.564
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.302

_database_code_depnum_ccdc_archive 'CCDC 940151'