# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_nd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Nd Zn (H2 O) (C6 H3 N2 O4) (C6 H4 N2 O4), 2H2 O'
_chemical_formula_sum            'C12 H13 N4 Nd O11 Zn'
_chemical_formula_weight         598.87

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   12.9828(10)
_cell_length_b                   11.5064(9)
_cell_length_c                   13.0127(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.424(1)
_cell_angle_gamma                90.00
_cell_volume                     1755.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3368
_cell_measurement_theta_min      2.4772
_cell_measurement_theta_max      28.2849

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1164
_exptl_absorpt_coefficient_mu    4.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36659
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6144
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2926
_reflns_number_gt                2619
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0820P)²+15.1644P] 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         2926
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1412
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

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
Nd1 Nd 0.37129(4) 0.29557(4) 0.16382(4) 0.0190(2) Uani 1 1 d . . .
Zn1 Zn 0.05526(10) 0.54572(9) 0.33276(10) 0.0291(3) Uani 1 1 d . . .
O1 O 0.2166(6) 0.1832(6) 0.1169(7) 0.0372(18) Uani 1 1 d . . .
O2 O 0.0870(6) 0.0588(6) 0.1170(6) 0.0330(16) Uani 1 1 d . . .
O3 O 0.2521(7) 0.4267(6) 0.1757(7) 0.0419(19) Uani 1 1 d . . .
O4 O 0.1784(6) 0.5425(5) 0.2626(6) 0.0314(16) Uani 1 1 d . . .
O5 O 0.4554(7) 0.1147(7) 0.2327(6) 0.0438(19) Uani 1 1 d . . .
O6 O 0.4821(7) -0.0763(7) 0.2713(7) 0.0448(19) Uani 1 1 d . . .
O7 O 0.4144(8) 0.2962(6) 0.3547(7) 0.048(2) Uani 1 1 d . . .
O8 O 0.3953(8) 0.2944(6) 0.5159(7) 0.045(2) Uani 1 1 d . . .
O1w O 0.1719(7) 0.5704(6) 0.4918(6) 0.0402(18) Uani 1 1 d . . .
H11 H 0.1488 0.5413 0.5373 0.060 Uiso 1 1 d R . .
H12 H 0.2333 0.5382 0.5007 0.060 Uiso 1 1 d R . .
O2w O 0.3873(7) 0.5425(7) 0.5156(7) 0.051(2) Uani 1 1 d . . .
H21 H 0.4330 0.5538 0.5838 0.076 Uiso 1 1 d R . .
H22 H 0.3954 0.4746 0.4966 0.076 Uiso 1 1 d R . .
O3w O 0.3569(9) -0.2983(8) 0.3283(9) 0.067(3) Uani 1 1 d . . .
H31 H 0.2971 -0.3377 0.3096 0.100 Uiso 1 1 d R . .
H32 H 0.4109 -0.3288 0.3842 0.100 Uiso 1 1 d R . .
N1 N 0.0476(7) 0.3790(7) 0.2890(7) 0.0312(19) Uani 1 1 d . . .
N2 N 0.0161(8) 0.1957(7) 0.2381(8) 0.037(2) Uani 1 1 d . . .
N3 N 0.3252(8) 0.0724(7) 0.4905(7) 0.033(2) Uani 1 1 d . . .
N4 N 0.3507(8) -0.0681(8) 0.3894(7) 0.038(2) Uani 1 1 d . . .
H4 H 0.3518 -0.1385 0.3636 0.045 Uiso 1 1 calc R . .
C1 C 0.1362(8) 0.1570(8) 0.1413(8) 0.027(2) Uani 1 1 d . . .
C2 C 0.0932(9) 0.2383(8) 0.2020(8) 0.028(2) Uani 1 1 d . . .
C3 C 0.1117(8) 0.3526(8) 0.2320(8) 0.028(2) Uani 1 1 d . . .
C4 C 0.1879(9) 0.4452(8) 0.2234(8) 0.029(2) Uani 1 1 d . . .
C5 C -0.0085(10) 0.2846(8) 0.2894(10) 0.036(3) Uani 1 1 d . . .
C6 C -0.0811(13) 0.2772(11) 0.3523(13) 0.059(4) Uani 1 1 d . . .
H6A H -0.0645 0.3416 0.4039 0.088 Uiso 1 1 calc R . .
H6B H -0.0655 0.2058 0.3945 0.088 Uiso 1 1 calc R . .
H6C H -0.1601 0.2794 0.2991 0.088 Uiso 1 1 calc R . .
C7 C 0.4433(9) 0.0247(9) 0.2789(9) 0.034(2) Uani 1 1 d . . .
C8 C 0.3855(9) 0.0304(9) 0.3565(9) 0.032(2) Uani 1 1 d . . .
C9 C 0.3694(8) 0.1170(8) 0.4193(8) 0.025(2) Uani 1 1 d . . .
C10 C 0.3936(10) 0.2425(9) 0.4271(8) 0.036(3) Uani 1 1 d . . .
C11 C 0.3142(10) -0.0393(9) 0.4681(10) 0.040(3) Uani 1 1 d . . .
C12 C 0.2642(13) -0.1295(11) 0.5191(12) 0.059(4) Uani 1 1 d . . .
H12A H 0.3220 -0.1554 0.5908 0.088 Uiso 1 1 calc R . .
H12B H 0.2367 -0.1945 0.4682 0.088 Uiso 1 1 calc R . .
H12C H 0.2023 -0.0957 0.5304 0.088 Uiso 1 1 calc R . .


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
Nd1 O1 2.241(7) . ?
Nd1 O3 2.213(7) . ?
Nd1 O5 2.342(8) . ?
Nd1 O6 2.264(8) 2_655 ?
Nd1 O7 2.300(7) . ?
Nd1 O8 2.322(7) 4_565 ?
Nd1 N3 2.568(8) 4_565 ?
Zn1 O2 2.213(6) 2 ?
Zn1 O4 2.156(6) . ?
Zn1 O1w 1.992(8) . ?
Zn1 N1 1.992(8) . ?
Zn1 N2 1.988(8) 2 ?
O1 C1 1.251(11) . ?
O2 C1 1.270(11) . ?
O2 Zn1 2.213(6) 2_545 ?
O3 C4 1.254(11) . ?
O4 C4 1.258(11) . ?
O5 C7 1.241(13) . ?
O6 C7 1.288(12) . ?
O6 Nd1 2.264(8) 2_645 ?
O7 C10 1.250(11) . ?
O8 C10 1.292(12) . ?
O8 Nd1 2.322(7) 4_566 ?
O1w H11 0.8399 . ?
O1w H12 0.8400 . ?
O2w H21 0.8400 . ?
O2w H22 0.8400 . ?
O3w H31 0.8400 . ?
O3w H32 0.8400 . ?
N1 C5 1.309(12) . ?
N1 C3 1.365(11) . ?
N2 C5 1.333(12) . ?
N2 C2 1.366(12) . ?
N2 Zn1 1.988(8) 2_545 ?
N3 C11 1.312(13) . ?
N3 C9 1.380(11) . ?
N3 Nd1 2.568(8) 4_566 ?
N4 C11 1.342(13) . ?
N4 C8 1.355(13) . ?
N4 H4 0.8800 . ?
C1 C2 1.480(12) . ?
C2 C3 1.364(14) . ?
C3 C4 1.490(13) . ?
C5 C6 1.494(14) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.497(13) . ?
C8 C9 1.361(13) . ?
C9 C10 1.472(14) . ?
C11 C12 1.519(15) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 Nd1 O1 80.9(3) . . ?
O3 Nd1 O6 91.8(3) . 2_655 ?
O1 Nd1 O6 171.2(3) . 2_655 ?
O3 Nd1 O7 77.1(3) . . ?
O1 Nd1 O7 94.0(3) . . ?
O6 Nd1 O7 79.6(3) 2_655 . ?
O3 Nd1 O8 135.1(3) . 4_565 ?
O1 Nd1 O8 86.6(3) . 4_565 ?
O6 Nd1 O8 102.1(3) 2_655 4_565 ?
O7 Nd1 O8 147.1(3) . 4_565 ?
O3 Nd1 O5 143.5(2) . . ?
O1 Nd1 O5 78.9(3) . . ?
O6 Nd1 O5 104.9(3) 2_655 . ?
O7 Nd1 O5 74.5(3) . . ?
O8 Nd1 O5 73.4(2) 4_565 . ?
O3 Nd1 N3 75.6(3) . 4_565 ?
O1 Nd1 N3 105.0(3) . 4_565 ?
O6 Nd1 N3 77.5(3) 2_655 4_565 ?
O7 Nd1 N3 143.5(3) . 4_565 ?
O8 Nd1 N3 66.4(2) 4_565 4_565 ?
O5 Nd1 N3 139.1(2) . 4_565 ?
N2 Zn1 N1 138.4(4) 2 . ?
N2 Zn1 O1w 110.7(4) 2 . ?
N1 Zn1 O1w 110.9(3) . . ?
N2 Zn1 O4 95.8(3) 2 . ?
N1 Zn1 O4 79.5(3) . . ?
O1w Zn1 O4 94.1(3) . . ?
N2 Zn1 O2 78.2(3) 2 2 ?
N1 Zn1 O2 101.8(3) . 2 ?
O1w Zn1 O2 92.4(3) . 2 ?
O4 Zn1 O2 172.4(3) . 2 ?
C1 O1 Nd1 144.8(6) . . ?
C1 O2 Zn1 112.4(5) . 2_545 ?
C4 O3 Nd1 141.6(7) . . ?
C4 O4 Zn1 114.0(6) . . ?
C7 O5 Nd1 142.4(7) . . ?
C7 O6 Nd1 148.5(8) . 2_645 ?
C10 O7 Nd1 141.4(7) . . ?
C10 O8 Nd1 125.3(6) . 4_566 ?
Zn1 O1w H11 109.4 . . ?
Zn1 O1w H12 109.4 . . ?
H11 O1w H12 109.5 . . ?
H21 O2w H22 109.5 . . ?
H31 O3w H32 110.5 . . ?
C5 N1 C3 106.7(8) . . ?
C5 N1 Zn1 139.3(7) . . ?
C3 N1 Zn1 113.7(6) . . ?
C5 N2 C2 105.4(8) . . ?
C5 N2 Zn1 137.3(7) . 2_545 ?
C2 N2 Zn1 114.6(6) . 2_545 ?
C11 N3 C9 104.6(8) . . ?
C11 N3 Nd1 137.4(7) . 4_566 ?
C9 N3 Nd1 111.3(6) . 4_566 ?
C11 N4 C8 108.0(9) . . ?
C11 N4 H4 126.0 . . ?
C8 N4 H4 126.0 . . ?
O1 C1 O2 122.5(8) . . ?
O1 C1 C2 122.0(8) . . ?
O2 C1 C2 115.5(8) . . ?
C3 C2 N2 108.2(8) . . ?
C3 C2 C1 134.6(8) . . ?
N2 C2 C1 117.2(8) . . ?
C2 C3 N1 107.2(8) . . ?
C2 C3 C4 135.1(8) . . ?
N1 C3 C4 117.5(8) . . ?
O3 C4 O4 123.6(9) . . ?
O3 C4 C3 121.4(8) . . ?
O4 C4 C3 115.0(8) . . ?
N1 C5 N2 112.4(8) . . ?
N1 C5 C6 122.2(9) . . ?
N2 C5 C6 125.0(9) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O5 C7 O6 125.6(9) . . ?
O5 C7 C8 119.7(9) . . ?
O6 C7 C8 114.6(9) . . ?
N4 C8 C9 105.3(8) . . ?
N4 C8 C7 120.5(9) . . ?
C9 C8 C7 133.5(10) . . ?
C8 C9 N3 110.3(8) . . ?
C8 C9 C10 132.5(8) . . ?
N3 C9 C10 117.1(7) . . ?
O7 C10 O8 121.3(9) . . ?
O7 C10 C9 122.8(8) . . ?
O8 C10 C9 115.8(7) . . ?
N3 C11 N4 111.8(9) . . ?
N3 C11 C12 126.8(9) . . ?
N4 C11 C12 121.4(10) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O3 Nd1 O1 C1 -44.2(12) . . . . ?
O7 Nd1 O1 C1 32.0(12) . . . . ?
O8 Nd1 O1 C1 179.0(12) 4_565 . . . ?
O5 Nd1 O1 C1 105.3(12) . . . . ?
N3 Nd1 O1 C1 -116.6(12) 4_565 . . . ?
O1 Nd1 O3 C4 55.0(11) . . . . ?
O6 Nd1 O3 C4 -120.2(11) 2_655 . . . ?
O7 Nd1 O3 C4 -41.3(11) . . . . ?
O8 Nd1 O3 C4 130.7(11) 4_565 . . . ?
O5 Nd1 O3 C4 -1.9(14) . . . . ?
N3 Nd1 O3 C4 163.1(12) 4_565 . . . ?
N2 Zn1 O4 C4 -135.7(7) 2 . . . ?
N1 Zn1 O4 C4 2.5(7) . . . . ?
O1w Zn1 O4 C4 113.0(7) . . . . ?
O3 Nd1 O5 C7 21.0(14) . . . . ?
O1 Nd1 O5 C7 -36.5(12) . . . . ?
O6 Nd1 O5 C7 135.4(12) 2_655 . . . ?
O7 Nd1 O5 C7 60.9(12) . . . . ?
O8 Nd1 O5 C7 -126.2(12) 4_565 . . . ?
N3 Nd1 O5 C7 -136.6(11) 4_565 . . . ?
O3 Nd1 O7 C10 97.2(13) . . . . ?
O1 Nd1 O7 C10 17.5(13) . . . . ?
O6 Nd1 O7 C10 -168.6(13) 2_655 . . . ?
O8 Nd1 O7 C10 -72.4(15) 4_565 . . . ?
O5 Nd1 O7 C10 -59.8(13) . . . . ?
N3 Nd1 O7 C10 139.6(12) 4_565 . . . ?
N2 Zn1 N1 C5 -90.9(13) 2 . . . ?
O1w Zn1 N1 C5 91.9(13) . . . . ?
O4 Zn1 N1 C5 -177.7(13) . . . . ?
O2 Zn1 N1 C5 -5.3(13) 2 . . . ?
N2 Zn1 N1 C3 81.7(8) 2 . . . ?
O1w Zn1 N1 C3 -95.6(7) . . . . ?
O4 Zn1 N1 C3 -5.2(7) . . . . ?
O2 Zn1 N1 C3 167.2(7) 2 . . . ?
Nd1 O1 C1 O2 -154.5(8) . . . . ?
Nd1 O1 C1 C2 24.6(18) . . . . ?
Zn1 O2 C1 O1 -177.9(8) 2_545 . . . ?
Zn1 O2 C1 C2 2.9(11) 2_545 . . . ?
C5 N2 C2 C3 -0.6(13) . . . . ?
Zn1 N2 C2 C3 163.8(7) 2_545 . . . ?
C5 N2 C2 C1 179.9(10) . . . . ?
Zn1 N2 C2 C1 -15.6(12) 2_545 . . . ?
O1 C1 C2 C3 9.4(19) . . . . ?
O2 C1 C2 C3 -171.4(12) . . . . ?
O1 C1 C2 N2 -171.3(10) . . . . ?
O2 C1 C2 N2 7.9(14) . . . . ?
N2 C2 C3 N1 1.4(12) . . . . ?
C1 C2 C3 N1 -179.3(11) . . . . ?
N2 C2 C3 C4 176.4(11) . . . . ?
C1 C2 C3 C4 -4(2) . . . . ?
C5 N1 C3 C2 -1.7(12) . . . . ?
Zn1 N1 C3 C2 -176.6(7) . . . . ?
C5 N1 C3 C4 -177.7(10) . . . . ?
Zn1 N1 C3 C4 7.4(11) . . . . ?
Nd1 O3 C4 O4 139.6(9) . . . . ?
Nd1 O3 C4 C3 -43.6(17) . . . . ?
Zn1 O4 C4 O3 177.6(8) . . . . ?
Zn1 O4 C4 C3 0.7(11) . . . . ?
C2 C3 C4 O3 3.1(19) . . . . ?
N1 C3 C4 O3 177.7(9) . . . . ?
C2 C3 C4 O4 -179.9(11) . . . . ?
N1 C3 C4 O4 -5.3(14) . . . . ?
C3 N1 C5 N2 1.4(13) . . . . ?
Zn1 N1 C5 N2 174.2(8) . . . . ?
C3 N1 C5 C6 175.1(12) . . . . ?
Zn1 N1 C5 C6 -12(2) . . . . ?
C2 N2 C5 N1 -0.5(14) . . . . ?
Zn1 N2 C5 N1 -159.4(9) 2_545 . . . ?
C2 N2 C5 C6 -174.0(12) . . . . ?
Zn1 N2 C5 C6 27(2) 2_545 . . . ?
Nd1 O5 C7 O6 153.8(9) . . . . ?
Nd1 O5 C7 C8 -30.1(18) . . . . ?
Nd1 O6 C7 O5 85.5(16) 2_645 . . . ?
Nd1 O6 C7 C8 -90.8(15) 2_645 . . . ?
C11 N4 C8 C9 0.7(12) . . . . ?
C11 N4 C8 C7 173.0(10) . . . . ?
O5 C7 C8 N4 166.5(10) . . . . ?
O6 C7 C8 N4 -17.0(15) . . . . ?
O5 C7 C8 C9 -23.7(19) . . . . ?
O6 C7 C8 C9 152.7(12) . . . . ?
N4 C8 C9 N3 0.1(12) . . . . ?
C7 C8 C9 N3 -170.8(11) . . . . ?
N4 C8 C9 C10 177.6(11) . . . . ?
C7 C8 C9 C10 7(2) . . . . ?
C11 N3 C9 C8 -0.8(12) . . . . ?
Nd1 N3 C9 C8 155.8(7) 4_566 . . . ?
C11 N3 C9 C10 -178.7(10) . . . . ?
Nd1 N3 C9 C10 -22.2(11) 4_566 . . . ?
Nd1 O7 C10 O8 -150.5(10) . . . . ?
Nd1 O7 C10 C9 32(2) . . . . ?
Nd1 O8 C10 O7 -175.4(9) 4_566 . . . ?
Nd1 O8 C10 C9 2.7(15) 4_566 . . . ?
C8 C9 C10 O7 15(2) . . . . ?
N3 C9 C10 O7 -167.1(11) . . . . ?
C8 C9 C10 O8 -162.6(11) . . . . ?
N3 C9 C10 O8 14.8(15) . . . . ?
C9 N3 C11 N4 1.2(13) . . . . ?
Nd1 N3 C11 N4 -145.6(8) 4_566 . . . ?
C9 N3 C11 C12 -177.1(12) . . . . ?
Nd1 N3 C11 C12 36(2) 4_566 . . . ?
C8 N4 C11 N3 -1.2(14) . . . . ?
C8 N4 C11 C12 177.2(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O2 0.84 1.94 2.76(1) 166 4_566
O1w H12 O2w 0.84 1.92 2.70(1) 152 .
O2w H21 O6 0.84 2.26 3.04(1) 155 4_566
O2w H22 O8 0.84 2.09 2.86(1) 152 .
O3w H31 O4 0.84 1.96 2.78(1) 167 1_545
O3w H32 O8 0.84 2.32 2.98(2) 136 3_656
N4 H4 O3w 0.88 1.90 2.78(2) 172 .

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         3.936
_refine_diff_density_min         -2.292
_refine_diff_density_rms         0.211
#===============================================================================
_database_code_depnum_ccdc_archive 'CCDC 973545'
#######################################################################
#
#                 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_ho

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Ho Zn (H2 O)2 (C6 H3 N2 O4) (C6 H4 N2 O4), 2.5H2 O'
_chemical_formula_sum            'C12 H16 Ho N4 O12.50 Zn'
_chemical_formula_weight         646.59

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   24.1912(11)
_cell_length_b                   9.1774(4)
_cell_length_c                   19.0096(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.911(1)
_cell_angle_gamma                90.00
_cell_volume                     3858.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6983
_cell_measurement_theta_min      2.3210
_cell_measurement_theta_max      28.3774

_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2504
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.223760
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11077
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4388
_reflns_number_gt                4001
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0619P)²+26.4941P] 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         4388
_refine_ls_number_parameters     280
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1094
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

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
Ho1 Ho 0.541601(9) 0.69446(2) 0.494865(12) 0.01323(10) Uani 1 1 d . . .
Zn1 Zn 0.71217(3) 0.48835(6) 0.33532(3) 0.01668(15) Uani 1 1 d . . .
O1 O 0.6145(2) 0.6490(5) 0.4555(3) 0.0332(10) Uani 1 1 d . . .
O2 O 0.6643(2) 0.6340(4) 0.3811(3) 0.0284(9) Uani 1 1 d . . .
O3 O 0.54703(15) 0.4333(4) 0.4953(2) 0.0175(8) Uani 1 1 d . . .
O4 O 0.54174(18) 0.1979(4) 0.4826(3) 0.0251(9) Uani 1 1 d . . .
O5 O 0.60861(17) 0.8760(4) 0.5539(2) 0.0266(9) Uani 1 1 d . . .
O6 O 0.69579(18) 0.9830(4) 0.5740(2) 0.0234(8) Uani 1 1 d . . .
O7 O 0.57757(17) 0.6319(5) 0.6217(2) 0.0251(9) Uani 1 1 d . . .
O8 O 0.62098(17) 0.5437(5) 0.7385(2) 0.0261(9) Uani 1 1 d . . .
O1w O 0.51910(19) 0.9116(4) 0.4186(2) 0.0298(9) Uani 1 1 d . . .
H11 H 0.5435 0.9776 0.4427 0.045 Uiso 1 1 d R . .
H12 H 0.4837 0.9385 0.4094 0.045 Uiso 1 1 d R . .
O2w O 0.48040(18) 0.6316(4) 0.3692(2) 0.0353(11) Uani 1 1 d . . .
H21 H 0.4600 0.5575 0.3691 0.053 Uiso 1 1 d R . .
H22 H 0.5020 0.6134 0.3451 0.053 Uiso 1 1 d R . .
O3w O 0.43476(18) 1.0548(4) 0.2980(2) 0.109(3) Uani 1 1 d RU . .
H31 H 0.4245 1.0038 0.2580 0.163 Uiso 1 1 d R . .
H32 H 0.4493 1.1345 0.2916 0.163 Uiso 1 1 d R . .
O4w O 0.3988(4) 0.8910(10) 0.1629(5) 0.097(3) Uani 1 1 d U . .
H41 H 0.3746 0.8214 0.1453 0.146 Uiso 1 1 d R . .
H42 H 0.4021 0.9365 0.1264 0.146 Uiso 1 1 d R . .
O5w O 0.5000 0.7335(18) 0.2500 0.045(3) Uani 0.50 2 d SPU . .
H51 H 0.4703 0.7893 0.2286 0.068 Uiso 0.50 1 d PR . .
O6w O 0.5000 1.312(3) 0.2500 0.093(7) Uani 0.50 2 d SPU . .
H61 H 0.5230 1.3629 0.2869 0.139 Uiso 0.50 1 d PR . .
N1 N 0.6848(2) 0.3501(5) 0.4042(3) 0.0181(9) Uani 1 1 d . . .
N2 N 0.6440(2) 0.1837(5) 0.4506(3) 0.0251(11) Uani 1 1 d . . .
H2 H 0.6358 0.0978 0.4646 0.030 Uiso 1 1 calc R . .
N3 N 0.75685(19) 0.8347(5) 0.7039(3) 0.0186(9) Uani 1 1 d . . .
N4 N 0.7284(2) 0.6659(5) 0.7667(3) 0.0186(9) Uani 1 1 d . . .
C1 C 0.6400(2) 0.5785(6) 0.4207(3) 0.0200(10) Uani 1 1 d . . .
C2 C 0.6447(2) 0.4171(6) 0.4290(3) 0.0163(10) Uani 1 1 d . . .
C3 C 0.6181(3) 0.3144(6) 0.4572(3) 0.0195(11) Uani 1 1 d . . .
C4 C 0.5669(2) 0.3168(5) 0.4801(3) 0.0151(10) Uani 1 1 d . . .
C5 C 0.6839(3) 0.2096(6) 0.4192(3) 0.0226(11) Uani 1 1 d . . .
C6 C 0.7198(3) 0.0934(7) 0.4033(4) 0.0365(15) Uani 1 1 d . . .
H6A H 0.7584 0.1317 0.4094 0.055 Uiso 1 1 calc R . .
H6B H 0.6987 0.0588 0.3516 0.055 Uiso 1 1 calc R . .
H6C H 0.7256 0.0142 0.4386 0.055 Uiso 1 1 calc R . .
C7 C 0.6652(2) 0.8914(5) 0.5920(3) 0.0170(10) Uani 1 1 d . . .
C8 C 0.6968(2) 0.8046(5) 0.6615(3) 0.0158(10) Uani 1 1 d . . .
C9 C 0.6791(2) 0.7006(5) 0.7002(3) 0.0159(10) Uani 1 1 d . . .
C10 C 0.6224(2) 0.6219(5) 0.6858(3) 0.0163(9) Uani 1 1 d . . .
C11 C 0.7738(2) 0.7482(6) 0.7654(3) 0.0191(10) Uani 1 1 d . . .
C12 C 0.8363(3) 0.7464(9) 0.8269(4) 0.0435(18) Uani 1 1 d . . .
H12A H 0.8634 0.7923 0.8082 0.065 Uiso 1 1 calc R . .
H12B H 0.8488 0.6475 0.8410 0.065 Uiso 1 1 calc R . .
H12C H 0.8370 0.7983 0.8711 0.065 Uiso 1 1 calc R . .


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
Ho1 O1 2.218(4) . ?
Ho1 O5 2.278(4) . ?
Ho1 O7 2.281(4) . ?
Ho1 O2w 2.316(4) . ?
Ho1 O1w 2.393(4) . ?
Ho1 O3 2.400(4) . ?
Ho1 O4 2.434(4) 5_666 ?
Ho1 O3 2.517(3) 5_666 ?
Zn1 N3 2.052(5) 7_666 ?
Zn1 N4 2.067(5) 6_565 ?
Zn1 N1 2.113(5) . ?
Zn1 O2 2.168(4) . ?
Zn1 O6 2.210(4) 7_666 ?
Zn1 O8 2.247(4) 6_565 ?
O1 C1 1.252(7) . ?
O2 C1 1.237(7) . ?
O3 C4 1.252(6) . ?
O3 Ho1 2.517(3) 5_666 ?
O4 C4 1.260(6) . ?
O4 Ho1 2.434(4) 5_666 ?
O5 C7 1.270(6) . ?
O6 C7 1.256(6) . ?
O6 Zn1 2.210(4) 7_666 ?
O7 C10 1.264(6) . ?
O8 C10 1.244(6) . ?
O8 Zn1 2.247(4) 6_566 ?
O1w H11 0.8400 . ?
O1w H12 0.8399 . ?
O2w H21 0.8400 . ?
O2w H22 0.8400 . ?
O3w H31 0.8405 . ?
O3w H32 0.8414 . ?
O4w H41 0.8401 . ?
O4w H42 0.8398 . ?
O5w H51 0.8400 . ?
O6w H61 0.8400 . ?
N1 C5 1.323(7) . ?
N1 C2 1.382(6) . ?
N2 C5 1.347(7) . ?
N2 C3 1.382(7) . ?
N2 H2 0.8800 . ?
N3 C11 1.333(7) . ?
N3 C8 1.373(6) . ?
N3 Zn1 2.052(5) 7_666 ?
N4 C11 1.342(7) . ?
N4 C9 1.378(7) . ?
N4 Zn1 2.067(5) 6_566 ?
C1 C2 1.489(7) . ?
C2 C3 1.368(7) . ?
C3 C4 1.472(7) . ?
C5 C6 1.482(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.466(7) . ?
C8 C9 1.376(7) . ?
C9 C10 1.473(7) . ?
C11 C12 1.490(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 Ho1 O5 78.43(17) . . ?
O1 Ho1 O7 107.17(17) . . ?
O5 Ho1 O7 76.86(14) . . ?
O1 Ho1 O2w 82.44(17) . . ?
O5 Ho1 O2w 136.09(15) . . ?
O7 Ho1 O2w 146.95(14) . . ?
O1 Ho1 O1w 88.21(17) . . ?
O5 Ho1 O1w 68.35(14) . . ?
O7 Ho1 O1w 138.20(15) . . ?
O2w Ho1 O1w 71.92(14) . . ?
O1 Ho1 O3 76.31(14) . . ?
O5 Ho1 O3 134.56(13) . . ?
O7 Ho1 O3 75.42(14) . . ?
O2w Ho1 O3 76.46(13) . . ?
O1w Ho1 O3 146.32(13) . . ?
O1 Ho1 O4 164.74(16) . 5_666 ?
O5 Ho1 O4 95.22(14) . 5_666 ?
O7 Ho1 O4 84.50(15) . 5_666 ?
O2w Ho1 O4 93.08(15) . 5_666 ?
O1w Ho1 O4 76.54(15) . 5_666 ?
O3 Ho1 O4 116.94(12) . 5_666 ?
O1 Ho1 O3 139.11(14) . 5_666 ?
O5 Ho1 O3 139.61(14) . 5_666 ?
O7 Ho1 O3 77.01(12) . 5_666 ?
O2w Ho1 O3 75.69(13) . 5_666 ?
O1w Ho1 O3 116.20(13) . 5_666 ?
O3 Ho1 O3 65.27(13) . 5_666 ?
O4 Ho1 O3 52.02(13) 5_666 5_666 ?
N3 Zn1 N4 97.00(19) 7_666 6_565 ?
N3 Zn1 N1 162.39(18) 7_666 . ?
N4 Zn1 N1 99.60(18) 6_565 . ?
N3 Zn1 O2 89.49(17) 7_666 . ?
N4 Zn1 O2 160.73(17) 6_565 . ?
N1 Zn1 O2 76.67(16) . . ?
N3 Zn1 O6 77.79(16) 7_666 7_666 ?
N4 Zn1 O6 100.65(16) 6_565 7_666 ?
N1 Zn1 O6 93.33(15) . 7_666 ?
O2 Zn1 O6 98.46(16) . 7_666 ?
N3 Zn1 O8 100.82(17) 7_666 6_565 ?
N4 Zn1 O8 76.58(16) 6_565 6_565 ?
N1 Zn1 O8 88.76(17) . 6_565 ?
O2 Zn1 O8 84.40(16) . 6_565 ?
O6 Zn1 O8 176.78(15) 7_666 6_565 ?
C1 O1 Ho1 154.9(4) . . ?
C1 O2 Zn1 116.9(4) . . ?
C4 O3 Ho1 151.3(3) . . ?
C4 O3 Ho1 92.1(3) . 5_666 ?
Ho1 O3 Ho1 114.73(13) . 5_666 ?
C4 O4 Ho1 95.8(3) . 5_666 ?
C7 O5 Ho1 138.5(3) . . ?
C7 O6 Zn1 112.7(3) . 7_666 ?
C10 O7 Ho1 147.9(3) . . ?
C10 O8 Zn1 113.3(3) . 6_566 ?
Ho1 O1w H11 109.5 . . ?
Ho1 O1w H12 109.5 . . ?
H11 O1w H12 109.5 . . ?
Ho1 O2w H21 109.5 . . ?
Ho1 O2w H22 109.5 . . ?
H21 O2w H22 109.5 . . ?
H31 O3w H32 109.9 . . ?
H41 O4w H42 109.4 . . ?
C5 N1 C2 106.6(4) . . ?
C5 N1 Zn1 139.1(4) . . ?
C2 N1 Zn1 112.5(3) . . ?
C5 N2 C3 108.6(5) . . ?
C5 N2 H2 125.7 . . ?
C3 N2 H2 125.7 . . ?
C11 N3 C8 105.7(4) . . ?
C11 N3 Zn1 139.7(4) . 7_666 ?
C8 N3 Zn1 113.6(3) . 7_666 ?
C11 N4 C9 105.3(4) . . ?
C11 N4 Zn1 139.7(4) . 6_566 ?
C9 N4 Zn1 114.9(3) . 6_566 ?
O2 C1 O1 124.5(5) . . ?
O2 C1 C2 116.1(5) . . ?
O1 C1 C2 119.4(5) . . ?
C3 C2 N1 109.5(5) . . ?
C3 C2 C1 134.4(5) . . ?
N1 C2 C1 116.2(4) . . ?
C2 C3 N2 105.1(5) . . ?
C2 C3 C4 133.8(5) . . ?
N2 C3 C4 120.5(5) . . ?
O3 C4 O4 119.7(5) . . ?
O3 C4 C3 121.9(4) . . ?
O4 C4 C3 118.4(4) . . ?
N1 C5 N2 110.2(5) . . ?
N1 C5 C6 126.6(5) . . ?
N2 C5 C6 123.2(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 O5 122.5(5) . . ?
O6 C7 C8 117.3(4) . . ?
O5 C7 C8 120.1(5) . . ?
N3 C8 C9 108.1(4) . . ?
N3 C8 C7 117.5(4) . . ?
C9 C8 C7 134.2(5) . . ?
C8 C9 N4 108.0(4) . . ?
C8 C9 C10 135.1(5) . . ?
N4 C9 C10 116.9(4) . . ?
O8 C10 O7 121.6(5) . . ?
O8 C10 C9 117.4(5) . . ?
O7 C10 C9 121.0(5) . . ?
N3 C11 N4 112.8(4) . . ?
N3 C11 C12 123.2(5) . . ?
N4 C11 C12 123.9(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O5 Ho1 O1 C1 176.9(10) . . . . ?
O7 Ho1 O1 C1 104.7(10) . . . . ?
O2w Ho1 O1 C1 -42.9(10) . . . . ?
O1w Ho1 O1 C1 -114.9(10) . . . . ?
O3 Ho1 O1 C1 34.9(10) . . . . ?
O4 Ho1 O1 C1 -116.6(10) 5_666 . . . ?
O3 Ho1 O1 C1 14.8(12) 5_666 . . . ?
N3 Zn1 O2 C1 -173.1(4) 7_666 . . . ?
N4 Zn1 O2 C1 76.8(7) 6_565 . . . ?
N1 Zn1 O2 C1 -4.1(4) . . . . ?
O6 Zn1 O2 C1 -95.5(4) 7_666 . . . ?
O8 Zn1 O2 C1 86.0(4) 6_565 . . . ?
O1 Ho1 O3 C4 -7.7(7) . . . . ?
O5 Ho1 O3 C4 -65.8(7) . . . . ?
O7 Ho1 O3 C4 -119.9(7) . . . . ?
O2w Ho1 O3 C4 77.6(7) . . . . ?
O1w Ho1 O3 C4 57.2(8) . . . . ?
O4 Ho1 O3 C4 164.2(7) 5_666 . . . ?
O3 Ho1 O3 C4 157.9(8) 5_666 . . . ?
O1 Ho1 O3 Ho1 -165.6(2) . . . 5_666 ?
O5 Ho1 O3 Ho1 136.33(18) . . . 5_666 ?
O7 Ho1 O3 Ho1 82.19(16) . . . 5_666 ?
O2w Ho1 O3 Ho1 -80.27(17) . . . 5_666 ?
O1w Ho1 O3 Ho1 -100.7(2) . . . 5_666 ?
O4 Ho1 O3 Ho1 6.3(2) 5_666 . . 5_666 ?
O3 Ho1 O3 Ho1 0.0 5_666 . . 5_666 ?
O1 Ho1 O5 C7 -45.2(6) . . . . ?
O7 Ho1 O5 C7 65.8(6) . . . . ?
O2w Ho1 O5 C7 -111.2(5) . . . . ?
O1w Ho1 O5 C7 -137.9(6) . . . . ?
O3 Ho1 O5 C7 12.1(7) . . . . ?
O4 Ho1 O5 C7 148.9(6) 5_666 . . . ?
O3 Ho1 O5 C7 116.7(5) 5_666 . . . ?
O1 Ho1 O7 C10 32.4(7) . . . . ?
O5 Ho1 O7 C10 -40.9(7) . . . . ?
O2w Ho1 O7 C10 135.3(6) . . . . ?
O1w Ho1 O7 C10 -74.8(8) . . . . ?
O3 Ho1 O7 C10 102.8(7) . . . . ?
O4 Ho1 O7 C10 -137.6(7) 5_666 . . . ?
O3 Ho1 O7 C10 170.2(7) 5_666 . . . ?
N3 Zn1 N1 C5 -149.1(6) 7_666 . . . ?
N4 Zn1 N1 C5 11.2(6) 6_565 . . . ?
O2 Zn1 N1 C5 171.9(6) . . . . ?
O6 Zn1 N1 C5 -90.2(6) 7_666 . . . ?
O8 Zn1 N1 C5 87.3(6) 6_565 . . . ?
N3 Zn1 N1 C2 49.0(7) 7_666 . . . ?
N4 Zn1 N1 C2 -150.8(3) 6_565 . . . ?
O2 Zn1 N1 C2 9.9(3) . . . . ?
O6 Zn1 N1 C2 107.8(4) 7_666 . . . ?
O8 Zn1 N1 C2 -74.6(4) 6_565 . . . ?
Zn1 O2 C1 O1 174.7(5) . . . . ?
Zn1 O2 C1 C2 -2.5(6) . . . . ?
Ho1 O1 C1 O2 136.7(8) . . . . ?
Ho1 O1 C1 C2 -46.2(13) . . . . ?
C5 N1 C2 C3 -1.8(6) . . . . ?
Zn1 N1 C2 C3 165.9(4) . . . . ?
C5 N1 C2 C1 177.6(5) . . . . ?
Zn1 N1 C2 C1 -14.6(6) . . . . ?
O2 C1 C2 C3 -169.1(6) . . . . ?
O1 C1 C2 C3 13.6(10) . . . . ?
O2 C1 C2 N1 11.7(7) . . . . ?
O1 C1 C2 N1 -165.7(5) . . . . ?
N1 C2 C3 N2 1.3(6) . . . . ?
C1 C2 C3 N2 -178.0(6) . . . . ?
N1 C2 C3 C4 -169.3(6) . . . . ?
C1 C2 C3 C4 11.4(11) . . . . ?
C5 N2 C3 C2 -0.4(7) . . . . ?
C5 N2 C3 C4 171.8(5) . . . . ?
Ho1 O3 C4 O4 -165.8(5) . . . . ?
Ho1 O3 C4 O4 -5.8(5) 5_666 . . . ?
Ho1 O3 C4 C3 12.4(10) . . . . ?
Ho1 O3 C4 C3 172.5(5) 5_666 . . . ?
Ho1 O4 C4 O3 6.0(5) 5_666 . . . ?
Ho1 O4 C4 C3 -172.3(4) 5_666 . . . ?
C2 C3 C4 O3 -19.0(10) . . . . ?
N2 C3 C4 O3 171.6(5) . . . . ?
C2 C3 C4 O4 159.3(6) . . . . ?
N2 C3 C4 O4 -10.2(8) . . . . ?
C2 N1 C5 N2 1.6(6) . . . . ?
Zn1 N1 C5 N2 -161.0(4) . . . . ?
C2 N1 C5 C6 -179.6(6) . . . . ?
Zn1 N1 C5 C6 17.8(10) . . . . ?
C3 N2 C5 N1 -0.8(7) . . . . ?
C3 N2 C5 C6 -179.6(6) . . . . ?
Zn1 O6 C7 O5 168.3(4) 7_666 . . . ?
Zn1 O6 C7 C8 -9.1(6) 7_666 . . . ?
Ho1 O5 C7 O6 126.6(5) . . . . ?
Ho1 O5 C7 C8 -56.0(8) . . . . ?
C11 N3 C8 C9 0.8(6) . . . . ?
Zn1 N3 C8 C9 -170.3(3) 7_666 . . . ?
C11 N3 C8 C7 176.6(5) . . . . ?
Zn1 N3 C8 C7 5.4(6) 7_666 . . . ?
O6 C7 C8 N3 3.0(7) . . . . ?
O5 C7 C8 N3 -174.5(5) . . . . ?
O6 C7 C8 C9 177.3(6) . . . . ?
O5 C7 C8 C9 -0.2(9) . . . . ?
N3 C8 C9 N4 -0.1(6) . . . . ?
C7 C8 C9 N4 -174.8(5) . . . . ?
N3 C8 C9 C10 -179.0(6) . . . . ?
C7 C8 C9 C10 6.3(11) . . . . ?
C11 N4 C9 C8 -0.6(6) . . . . ?
Zn1 N4 C9 C8 179.4(3) 6_566 . . . ?
C11 N4 C9 C10 178.5(5) . . . . ?
Zn1 N4 C9 C10 -1.4(6) 6_566 . . . ?
Zn1 O8 C10 O7 168.2(4) 6_566 . . . ?
Zn1 O8 C10 C9 -10.5(6) 6_566 . . . ?
Ho1 O7 C10 O8 -161.7(5) . . . . ?
Ho1 O7 C10 C9 17.0(10) . . . . ?
C8 C9 C10 O8 -172.6(6) . . . . ?
N4 C9 C10 O8 8.5(7) . . . . ?
C8 C9 C10 O7 8.6(9) . . . . ?
N4 C9 C10 O7 -170.2(5) . . . . ?
C8 N3 C11 N4 -1.3(7) . . . . ?
Zn1 N3 C11 N4 166.2(4) 7_666 . . . ?
C8 N3 C11 C12 -180.0(6) . . . . ?
Zn1 N3 C11 C12 -12.5(10) 7_666 . . . ?
C9 N4 C11 N3 1.2(6) . . . . ?
Zn1 N4 C11 N3 -178.9(4) 6_566 . . . ?
C9 N4 C11 C12 179.9(6) . . . . ?
Zn1 N4 C11 C12 -0.2(10) 6_566 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O4 0.84 2.16 2.853(6) 139.0 1_565
O1w H12 O3w 0.84 2.23 2.712(6) 116.2 .
O2w H21 O7 0.84 2.00 2.835(6) 171.9 5_666
O2w H22 O5w 0.84 2.10 2.666(7) 124.3 .
O3w H31 O4w 0.84 1.95 2.793(9) 177.9 .
O3w H32 O6w 0.84 2.36 3.169(18) 162.3 .
O4w H41 O2 0.84 1.93 2.750(10) 166.3 2_655
O4w H42 O1w 0.84 2.40 2.979(10) 127.0 2_655
O5w H51 O4w 0.84 1.92 2.745(13) 168.7 .
N2 H2 O6 0.88 2.26 2.843(6) 123.8 1_545

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         3.699
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.227
#===============================================================================
_database_code_depnum_ccdc_archive 'CCDC 973546'
#######################################################################
#
#                 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_er

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Er Zn (H2 O)2 (C6 H3 N2 O4) (C6 H4 N2 O4), 2.5H2 O'
_chemical_formula_sum            'C12 H16 Er N4 O12.50 Zn'
_chemical_formula_weight         648.92

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   24.2346(14)
_cell_length_b                   9.1735(5)
_cell_length_c                   19.0739(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.153(1)
_cell_angle_gamma                90.00
_cell_volume                     3869.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8254
_cell_measurement_theta_min      2.4037
_cell_measurement_theta_max      28.1917

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2512
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.518840
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13649
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4361
_reflns_number_gt                4013
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0560P)²+15.0410P] 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         4361
_refine_ls_number_parameters     280
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0846
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

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 0.541852(8) 0.694238(18) 0.494915(10) 0.01694(8) Uani 1 1 d . . .
Zn1 Zn 0.71220(2) 0.48920(5) 0.33596(3) 0.02032(12) Uani 1 1 d . . .
O1 O 0.61502(17) 0.6492(4) 0.4571(2) 0.0359(8) Uani 1 1 d . . .
O2 O 0.66433(17) 0.6349(4) 0.3819(2) 0.0338(8) Uani 1 1 d . . .
O3 O 0.54712(13) 0.4332(3) 0.49581(16) 0.0220(6) Uani 1 1 d . . .
O4 O 0.54105(15) 0.1964(3) 0.4821(2) 0.0286(8) Uani 1 1 d . . .
O5 O 0.60784(14) 0.8765(3) 0.55409(19) 0.0303(7) Uani 1 1 d . . .
O6 O 0.69542(15) 0.9819(3) 0.57354(18) 0.0279(7) Uani 1 1 d . . .
O7 O 0.57664(15) 0.6323(4) 0.62112(18) 0.0296(7) Uani 1 1 d . . .
O8 O 0.62062(15) 0.5433(4) 0.73918(19) 0.0302(7) Uani 1 1 d . . .
O1w O 0.51820(17) 0.9106(4) 0.4181(2) 0.0359(8) Uani 1 1 d . . .
H11 H 0.5426 0.9766 0.4422 0.054 Uiso 1 1 d R . .
H12 H 0.4827 0.9375 0.4089 0.054 Uiso 1 1 d R . .
O2w O 0.48147(16) 0.6314(4) 0.36850(19) 0.0415(9) Uani 1 1 d . . .
H21 H 0.4610 0.5574 0.3684 0.062 Uiso 1 1 d R . .
H22 H 0.5031 0.6132 0.3444 0.062 Uiso 1 1 d R . .
O3w O 0.43583(16) 1.0547(4) 0.29726(19) 0.137(3) Uani 1 1 d RU . .
H31 H 0.4256 1.0037 0.2573 0.206 Uiso 1 1 d R . .
H32 H 0.4504 1.1344 0.2909 0.206 Uiso 1 1 d R . .
O4w O 0.4006(5) 0.8859(12) 0.1651(6) 0.155(4) Uani 1 1 d U . .
H41 H 0.3762 0.8167 0.1469 0.232 Uiso 1 1 d R . .
H42 H 0.4040 0.9322 0.1290 0.232 Uiso 1 1 d R . .
O5w O 0.5000 0.734(2) 0.2500 0.094(5) Uani 0.50 2 d SPU . .
H51 H 0.4703 0.7893 0.2286 0.140 Uiso 0.50 1 d PR . .
O6w O 0.5000 1.314(2) 0.2500 0.097(6) Uani 0.50 2 d SPU . .
H61 H 0.5230 1.3650 0.2869 0.146 Uiso 0.50 1 d PR . .
N1 N 0.68474(17) 0.3488(4) 0.4046(2) 0.0232(7) Uani 1 1 d . . .
N2 N 0.6432(2) 0.1827(4) 0.4502(3) 0.0298(9) Uani 1 1 d . . .
H2 H 0.6347 0.0970 0.4639 0.036 Uiso 1 1 calc R . .
N3 N 0.75692(17) 0.8328(4) 0.7039(2) 0.0212(7) Uani 1 1 d . . .
N4 N 0.72836(17) 0.6649(4) 0.7669(2) 0.0229(7) Uani 1 1 d . . .
C1 C 0.6406(2) 0.5776(5) 0.4217(3) 0.0240(9) Uani 1 1 d . . .
C2 C 0.64509(19) 0.4168(5) 0.4294(2) 0.0203(8) Uani 1 1 d . . .
C3 C 0.6182(2) 0.3131(4) 0.4576(3) 0.0218(9) Uani 1 1 d . . .
C4 C 0.5662(2) 0.3153(4) 0.4795(2) 0.0194(8) Uani 1 1 d . . .
C5 C 0.6831(2) 0.2073(5) 0.4184(3) 0.0272(10) Uani 1 1 d . . .
C6 C 0.7187(3) 0.0908(6) 0.4019(3) 0.0421(13) Uani 1 1 d . . .
H6A H 0.7574 0.1287 0.4083 0.063 Uiso 1 1 calc R . .
H6B H 0.6973 0.0575 0.3500 0.063 Uiso 1 1 calc R . .
H6C H 0.7243 0.0108 0.4366 0.063 Uiso 1 1 calc R . .
C7 C 0.6645(2) 0.8914(4) 0.5914(2) 0.0218(8) Uani 1 1 d . . .
C8 C 0.6969(2) 0.8038(4) 0.6616(2) 0.0190(8) Uani 1 1 d . . .
C9 C 0.6791(2) 0.6989(4) 0.7007(2) 0.0191(8) Uani 1 1 d . . .
C10 C 0.62214(19) 0.6210(4) 0.6863(2) 0.0206(8) Uani 1 1 d . . .
C11 C 0.77405(19) 0.7463(5) 0.7661(2) 0.0231(8) Uani 1 1 d . . .
C12 C 0.8365(2) 0.7445(8) 0.8273(3) 0.0475(15) Uani 1 1 d . . .
H12A H 0.8645 0.7208 0.8053 0.071 Uiso 1 1 calc R . .
H12B H 0.8391 0.6728 0.8652 0.071 Uiso 1 1 calc R . .
H12C H 0.8461 0.8388 0.8511 0.071 Uiso 1 1 calc R . .


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 O1 2.210(3) . ?
Er1 O3 2.397(3) . ?
Er1 O3 2.522(3) 5_666 ?
Er1 O4 2.441(3) 5_666 ?
Er1 O5 2.269(3) . ?
Er1 O7 2.273(3) . ?
Er1 O1w 2.393(3) . ?
Er1 O2w 2.324(3) . ?
Zn1 O2 2.175(3) . ?
Zn1 O6 2.214(3) 7_666 ?
Zn1 O8 2.252(3) 6_565 ?
Zn1 N1 2.129(4) . ?
Zn1 N3 2.066(4) 7_666 ?
Zn1 N4 2.076(4) 6_565 ?
O1 C1 1.269(5) . ?
O2 C1 1.242(5) . ?
O3 C4 1.265(5) . ?
O3 Er1 2.522(3) 5_666 ?
O4 C4 1.261(5) . ?
O4 Er1 2.441(3) 5_666 ?
O5 C7 1.270(5) . ?
O6 C7 1.255(5) . ?
O6 Zn1 2.214(3) 7_666 ?
O7 C10 1.285(5) . ?
O8 C10 1.248(5) . ?
O8 Zn1 2.252(3) 6_566 ?
O1w H11 0.8395 . ?
O1w H12 0.8405 . ?
O2w H21 0.8403 . ?
O2w H22 0.8432 . ?
O3w H31 0.8416 . ?
O3w H32 0.8418 . ?
O4w H41 0.8400 . ?
O4w H42 0.8401 . ?
O5w H51 0.8396 . ?
O6w H61 0.8397 . ?
N1 C5 1.327(6) . ?
N1 C2 1.381(5) . ?
N2 C5 1.353(6) . ?
N2 C3 1.375(5) . ?
N2 H2 0.8800 . ?
N3 C11 1.343(5) . ?
N3 C8 1.370(6) . ?
N3 Zn1 2.066(4) 7_666 ?
N4 C11 1.341(6) . ?
N4 C9 1.372(6) . ?
N4 Zn1 2.076(4) 6_566 ?
C1 C2 1.482(6) . ?
C2 C3 1.381(6) . ?
C3 C4 1.480(6) . ?
C5 C6 1.486(6) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.481(6) . ?
C8 C9 1.389(6) . ?
C9 C10 1.478(6) . ?
C11 C12 1.486(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 Er1 O5 78.69(13) . . ?
O1 Er1 O7 107.44(14) . . ?
O5 Er1 O7 77.12(11) . . ?
O1 Er1 O2w 82.15(14) . . ?
O5 Er1 O2w 135.66(12) . . ?
O7 Er1 O2w 147.14(12) . . ?
O1 Er1 O1w 88.75(14) . . ?
O5 Er1 O1w 68.72(12) . . ?
O7 Er1 O1w 138.41(12) . . ?
O2w Er1 O1w 71.27(12) . . ?
O1 Er1 O3 76.59(11) . . ?
O5 Er1 O3 135.04(11) . . ?
O7 Er1 O3 75.35(11) . . ?
O2w Er1 O3 76.64(11) . . ?
O1w Er1 O3 146.23(11) . . ?
O1 Er1 O4 164.82(12) . 5_666 ?
O5 Er1 O4 94.13(12) . 5_666 ?
O7 Er1 O4 83.59(12) . 5_666 ?
O2w Er1 O4 94.20(13) . 5_666 ?
O1w Er1 O4 76.15(12) . 5_666 ?
O3 Er1 O4 117.05(9) . 5_666 ?
O1 Er1 O3 139.43(11) . 5_666 ?
O5 Er1 O3 139.07(11) . 5_666 ?
O7 Er1 O3 76.53(10) . 5_666 ?
O2w Er1 O3 76.37(11) . 5_666 ?
O1w Er1 O3 115.47(11) . 5_666 ?
O3 Er1 O3 65.23(11) . 5_666 ?
O4 Er1 O3 52.25(11) 5_666 5_666 ?
N3 Zn1 N4 96.55(15) 7_666 6_565 ?
N3 Zn1 N1 162.96(14) 7_666 . ?
N4 Zn1 N1 99.54(15) 6_565 . ?
N3 Zn1 O2 89.78(13) 7_666 . ?
N4 Zn1 O2 160.77(15) 6_565 . ?
N1 Zn1 O2 76.78(13) . . ?
N3 Zn1 O6 77.84(13) 7_666 7_666 ?
N4 Zn1 O6 100.55(14) 6_565 7_666 ?
N1 Zn1 O6 93.66(13) . 7_666 ?
O2 Zn1 O6 98.52(14) . 7_666 ?
N3 Zn1 O8 100.77(14) 7_666 6_565 ?
N4 Zn1 O8 76.60(13) 6_565 6_565 ?
N1 Zn1 O8 88.44(14) . 6_565 ?
O2 Zn1 O8 84.39(13) . 6_565 ?
O6 Zn1 O8 176.73(12) 7_666 6_565 ?
C1 O1 Er1 154.3(3) . . ?
C1 O2 Zn1 116.3(3) . . ?
C4 O3 Er1 151.2(3) . . ?
C4 O3 Er1 91.7(2) . 5_666 ?
Er1 O3 Er1 114.77(11) . 5_666 ?
C4 O4 Er1 95.7(2) . 5_666 ?
C7 O5 Er1 137.6(3) . . ?
C7 O6 Zn1 113.1(3) . 7_666 ?
C10 O7 Er1 147.6(3) . . ?
C10 O8 Zn1 113.1(3) . 6_566 ?
Er1 O1w H11 108.9 . . ?
Er1 O1w H12 109.9 . . ?
H11 O1w H12 109.4 . . ?
Er1 O2w H21 108.9 . . ?
Er1 O2w H22 110.3 . . ?
H21 O2w H22 109.6 . . ?
H31 O3w H32 109.7 . . ?
H41 O4w H42 109.5 . . ?
C5 N1 C2 107.0(4) . . ?
C5 N1 Zn1 139.1(3) . . ?
C2 N1 Zn1 111.9(3) . . ?
C5 N2 C3 109.1(4) . . ?
C5 N2 H2 125.4 . . ?
C3 N2 H2 125.4 . . ?
C11 N3 C8 106.0(3) . . ?
C11 N3 Zn1 139.8(3) . 7_666 ?
C8 N3 Zn1 113.2(3) . 7_666 ?
C11 N4 C9 105.9(3) . . ?
C11 N4 Zn1 139.3(3) . 6_566 ?
C9 N4 Zn1 114.8(3) . 6_566 ?
O2 C1 O1 123.7(4) . . ?
O2 C1 C2 116.6(4) . . ?
O1 C1 C2 119.7(4) . . ?
C3 C2 N1 109.1(4) . . ?
C3 C2 C1 134.2(4) . . ?
N1 C2 C1 116.7(4) . . ?
N2 C3 C2 105.1(4) . . ?
N2 C3 C4 120.2(4) . . ?
C2 C3 C4 133.8(4) . . ?
O4 C4 O3 119.9(4) . . ?
O4 C4 C3 118.7(4) . . ?
O3 C4 C3 121.4(4) . . ?
N1 C5 N2 109.6(4) . . ?
N1 C5 C6 126.5(4) . . ?
N2 C5 C6 123.9(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 O5 123.2(4) . . ?
O6 C7 C8 116.8(4) . . ?
O5 C7 C8 120.0(4) . . ?
N3 C8 C9 107.8(4) . . ?
N3 C8 C7 117.9(4) . . ?
C9 C8 C7 134.1(4) . . ?
N4 C9 C8 107.9(4) . . ?
N4 C9 C10 117.1(4) . . ?
C8 C9 C10 134.9(4) . . ?
O8 C10 O7 122.1(4) . . ?
O8 C10 C9 117.4(4) . . ?
O7 C10 C9 120.5(4) . . ?
N4 C11 N3 112.4(4) . . ?
N4 C11 C12 124.3(4) . . ?
N3 C11 C12 123.3(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O5 Er1 O1 C1 178.3(8) . . . . ?
O7 Er1 O1 C1 105.9(8) . . . . ?
O2w Er1 O1 C1 -41.9(8) . . . . ?
O1w Er1 O1 C1 -113.1(8) . . . . ?
O3 Er1 O1 C1 36.2(8) . . . . ?
O4 Er1 O1 C1 -118.8(8) 5_666 . . . ?
O3 Er1 O1 C1 16.4(9) 5_666 . . . ?
N3 Zn1 O2 C1 -173.0(4) 7_666 . . . ?
N4 Zn1 O2 C1 77.4(6) 6_565 . . . ?
N1 Zn1 O2 C1 -3.5(3) . . . . ?
O6 Zn1 O2 C1 -95.3(3) 7_666 . . . ?
O8 Zn1 O2 C1 86.2(4) 6_565 . . . ?
O1 Er1 O3 C4 -10.6(6) . . . . ?
O5 Er1 O3 C4 -69.0(6) . . . . ?
O7 Er1 O3 C4 -123.0(6) . . . . ?
O2w Er1 O3 C4 74.3(6) . . . . ?
O1w Er1 O3 C4 56.0(7) . . . . ?
O4 Er1 O3 C4 162.2(6) 5_666 . . . ?
O3 Er1 O3 C4 155.3(7) 5_666 . . . ?
O1 Er1 O3 Er1 -165.93(16) . . . 5_666 ?
O5 Er1 O3 Er1 135.68(15) . . . 5_666 ?
O7 Er1 O3 Er1 81.69(13) . . . 5_666 ?
O2w Er1 O3 Er1 -80.96(14) . . . 5_666 ?
O1w Er1 O3 Er1 -99.3(2) . . . 5_666 ?
O4 Er1 O3 Er1 6.93(17) 5_666 . . 5_666 ?
O3 Er1 O3 Er1 0.0 5_666 . . 5_666 ?
O1 Er1 O5 C7 -43.4(4) . . . . ?
O7 Er1 O5 C7 67.7(4) . . . . ?
O2w Er1 O5 C7 -109.6(4) . . . . ?
O1w Er1 O5 C7 -136.5(5) . . . . ?
O3 Er1 O5 C7 14.3(5) . . . . ?
O4 Er1 O5 C7 150.1(4) 5_666 . . . ?
O3 Er1 O5 C7 118.7(4) 5_666 . . . ?
O1 Er1 O7 C10 31.1(6) . . . . ?
O5 Er1 O7 C10 -42.5(5) . . . . ?
O2w Er1 O7 C10 134.0(5) . . . . ?
O1w Er1 O7 C10 -77.5(6) . . . . ?
O3 Er1 O7 C10 101.6(6) . . . . ?
O4 Er1 O7 C10 -138.2(6) 5_666 . . . ?
O3 Er1 O7 C10 169.1(6) 5_666 . . . ?
N3 Zn1 N1 C5 -150.7(5) 7_666 . . . ?
N4 Zn1 N1 C5 9.9(5) 6_565 . . . ?
O2 Zn1 N1 C5 170.6(5) . . . . ?
O6 Zn1 N1 C5 -91.5(5) 7_666 . . . ?
O8 Zn1 N1 C5 86.0(5) 6_565 . . . ?
N3 Zn1 N1 C2 48.3(6) 7_666 . . . ?
N4 Zn1 N1 C2 -151.2(3) 6_565 . . . ?
O2 Zn1 N1 C2 9.6(3) . . . . ?
O6 Zn1 N1 C2 107.5(3) 7_666 . . . ?
O8 Zn1 N1 C2 -75.0(3) 6_565 . . . ?
Zn1 O2 C1 O1 174.6(4) . . . . ?
Zn1 O2 C1 C2 -3.1(5) . . . . ?
Er1 O1 C1 O2 135.1(6) . . . . ?
Er1 O1 C1 C2 -47.3(10) . . . . ?
C5 N1 C2 C3 -1.1(5) . . . . ?
Zn1 N1 C2 C3 166.0(3) . . . . ?
C5 N1 C2 C1 178.3(4) . . . . ?
Zn1 N1 C2 C1 -14.5(5) . . . . ?
O2 C1 C2 C3 -168.6(5) . . . . ?
O1 C1 C2 C3 13.6(8) . . . . ?
O2 C1 C2 N1 12.1(6) . . . . ?
O1 C1 C2 N1 -165.6(4) . . . . ?
C5 N2 C3 C2 -0.5(6) . . . . ?
C5 N2 C3 C4 170.5(4) . . . . ?
N1 C2 C3 N2 1.0(5) . . . . ?
C1 C2 C3 N2 -178.4(5) . . . . ?
N1 C2 C3 C4 -168.2(5) . . . . ?
C1 C2 C3 C4 12.5(9) . . . . ?
Er1 O4 C4 O3 7.0(5) 5_666 . . . ?
Er1 O4 C4 C3 -173.4(4) 5_666 . . . ?
Er1 O3 C4 O4 -164.4(4) . . . . ?
Er1 O3 C4 O4 -6.7(4) 5_666 . . . ?
Er1 O3 C4 C3 15.9(9) . . . . ?
Er1 O3 C4 C3 173.6(4) 5_666 . . . ?
N2 C3 C4 O4 -8.5(7) . . . . ?
C2 C3 C4 O4 159.4(5) . . . . ?
N2 C3 C4 O3 171.2(4) . . . . ?
C2 C3 C4 O3 -21.0(8) . . . . ?
C2 N1 C5 N2 0.8(5) . . . . ?
Zn1 N1 C5 N2 -160.8(4) . . . . ?
C2 N1 C5 C6 -179.6(5) . . . . ?
Zn1 N1 C5 C6 18.8(9) . . . . ?
C3 N2 C5 N1 -0.2(6) . . . . ?
C3 N2 C5 C6 -179.8(5) . . . . ?
Zn1 O6 C7 O5 167.8(3) 7_666 . . . ?
Zn1 O6 C7 C8 -9.7(5) 7_666 . . . ?
Er1 O5 C7 O6 125.2(4) . . . . ?
Er1 O5 C7 C8 -57.4(6) . . . . ?
C11 N3 C8 C9 0.4(5) . . . . ?
Zn1 N3 C8 C9 -170.4(3) 7_666 . . . ?
C11 N3 C8 C7 176.1(4) . . . . ?
Zn1 N3 C8 C7 5.4(5) 7_666 . . . ?
O6 C7 C8 N3 3.3(6) . . . . ?
O5 C7 C8 N3 -174.2(4) . . . . ?
O6 C7 C8 C9 177.7(4) . . . . ?
O5 C7 C8 C9 0.2(7) . . . . ?
C11 N4 C9 C8 -0.9(5) . . . . ?
Zn1 N4 C9 C8 179.3(3) 6_566 . . . ?
C11 N4 C9 C10 178.7(4) . . . . ?
Zn1 N4 C9 C10 -1.1(5) 6_566 . . . ?
N3 C8 C9 N4 0.3(5) . . . . ?
C7 C8 C9 N4 -174.5(4) . . . . ?
N3 C8 C9 C10 -179.2(4) . . . . ?
C7 C8 C9 C10 6.1(8) . . . . ?
Zn1 O8 C10 O7 168.3(3) 6_566 . . . ?
Zn1 O8 C10 C9 -10.6(5) 6_566 . . . ?
Er1 O7 C10 O8 -161.2(4) . . . . ?
Er1 O7 C10 C9 17.7(8) . . . . ?
N4 C9 C10 O8 8.4(6) . . . . ?
C8 C9 C10 O8 -172.2(4) . . . . ?
N4 C9 C10 O7 -170.5(4) . . . . ?
C8 C9 C10 O7 8.9(7) . . . . ?
C9 N4 C11 N3 1.2(5) . . . . ?
Zn1 N4 C11 N3 -179.1(3) 6_566 . . . ?
C9 N4 C11 C12 179.9(5) . . . . ?
Zn1 N4 C11 C12 -0.3(8) 6_566 . . . ?
C8 N3 C11 N4 -1.0(5) . . . . ?
Zn1 N3 C11 N4 165.8(3) 7_666 . . . ?
C8 N3 C11 C12 -179.8(5) . . . . ?
Zn1 N3 C11 C12 -13.0(8) 7_666 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O4 0.84 2.16 2.849(5) 139.1 1_565
O1w H12 O3w 0.84 2.24 2.698(5) 114.7 .
O2w H21 O7 0.84 2.01 2.847(5) 171.8 5_666
O2w H22 O5w 0.84 2.09 2.649(8) 123.7 .
O3w H31 O4w 0.84 1.94 2.779(10) 178.9 .
O3w H32 O6w 0.84 2.35 3.167(15) 163.2 .
O4w H41 O2 0.84 1.90 2.725(11) 167.6 2_655
O4w H42 O1w 0.84 2.41 2.999(10) 128.1 2_655
O5w H51 O4w 0.84 1.85 2.681(15) 168.4 .
N2 H2 O6 0.88 2.27 2.845(5) 123.3 1_545

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.532
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.160
#===============================================================================
_database_code_depnum_ccdc_archive 'CCDC 973547'
#######################################################################
#
#                 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_yb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Er Zn (H2 O)2 (C6 H3 N2 O4) (C6 H4 N2 O4), 2.5H2 O'
_chemical_formula_sum            'C12 H16 N4 O12.50 Yb Zn'
_chemical_formula_weight         654.70

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'
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   24.1744(13)
_cell_length_b                   9.1789(5)
_cell_length_c                   18.9734(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.0500(10)
_cell_angle_gamma                90.00
_cell_volume                     3844.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9226
_cell_measurement_theta_min      2.3229
_cell_measurement_theta_max      28.2398

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    6.158
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.724373
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15582
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4399
_reflns_number_gt                4075
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0461P)²+13.5489P] 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         4399
_refine_ls_number_parameters     280
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

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
Yb1 Yb 0.542120(6) 0.693092(16) 0.495871(9) 0.01795(7) Uani 1 1 d . . .
Zn1 Zn 0.712595(19) 0.49132(5) 0.33675(2) 0.02123(10) Uani 1 1 d . . .
O1 O 0.61579(15) 0.6496(3) 0.4596(2) 0.0360(7) Uani 1 1 d . . .
O2 O 0.66533(15) 0.6360(3) 0.38426(19) 0.0349(7) Uani 1 1 d . . .
O3 O 0.54675(11) 0.4330(3) 0.49615(15) 0.0237(6) Uani 1 1 d . . .
O4 O 0.53977(14) 0.1968(3) 0.4806(2) 0.0303(7) Uani 1 1 d . . .
O5 O 0.60706(13) 0.8756(3) 0.55526(17) 0.0314(6) Uani 1 1 d . . .
O6 O 0.69424(13) 0.9804(3) 0.57288(16) 0.0278(6) Uani 1 1 d . . .
O7 O 0.57670(12) 0.6293(3) 0.62139(16) 0.0292(6) Uani 1 1 d . . .
O8 O 0.62069(13) 0.5411(3) 0.73975(17) 0.0309(6) Uani 1 1 d . . .
O1w O 0.51907(15) 0.9074(3) 0.41891(18) 0.0362(7) Uani 1 1 d . . .
H11 H 0.5435 0.9734 0.4430 0.054 Uiso 1 1 d R . .
H12 H 0.4836 0.9343 0.4097 0.054 Uiso 1 1 d R . .
O2w O 0.48243(14) 0.6311(3) 0.37021(17) 0.0414(8) Uani 1 1 d . . .
H21 H 0.4620 0.5570 0.3701 0.062 Uiso 1 1 d R . .
H22 H 0.5040 0.6129 0.3461 0.062 Uiso 1 1 d R . .
O3w O 0.43679(14) 1.0543(3) 0.29896(17) 0.132(3) Uani 1 1 d RU . .
H31 H 0.4266 1.0033 0.2590 0.198 Uiso 1 1 d R . .
H32 H 0.4514 1.1340 0.2926 0.198 Uiso 1 1 d R . .
O4w O 0.4003(4) 0.8875(9) 0.1634(5) 0.135(3) Uani 1 1 d U . .
H41 H 0.3758 0.8184 0.1453 0.202 Uiso 1 1 d R . .
H42 H 0.4036 0.9339 0.1274 0.202 Uiso 1 1 d R . .
O5w O 0.5000 0.7285(16) 0.2500 0.074(4) Uani 0.50 2 d SPU . .
H51 H 0.4703 0.7843 0.2286 0.112 Uiso 0.50 1 d PR . .
O6w O 0.5000 1.3153(17) 0.2500 0.086(5) Uani 0.50 2 d SPU . .
H61 H 0.5230 1.3666 0.2869 0.129 Uiso 0.50 1 d PR . .
N1 N 0.68517(15) 0.3504(4) 0.40524(19) 0.0247(7) Uani 1 1 d . . .
N2 N 0.64286(18) 0.1830(4) 0.4495(2) 0.0312(8) Uani 1 1 d . . .
H2 H 0.6340 0.0968 0.4625 0.037 Uiso 1 1 calc R . .
N3 N 0.75706(15) 0.8301(4) 0.70335(19) 0.0226(6) Uani 1 1 d . . .
N4 N 0.72864(15) 0.6618(4) 0.76654(19) 0.0237(7) Uani 1 1 d . . .
C1 C 0.64129(17) 0.5787(4) 0.4240(2) 0.0247(8) Uani 1 1 d . . .
C2 C 0.64540(16) 0.4172(4) 0.4304(2) 0.0223(7) Uani 1 1 d . . .
C3 C 0.61803(19) 0.3130(4) 0.4578(2) 0.0243(8) Uani 1 1 d . . .
C4 C 0.56592(18) 0.3155(4) 0.4793(2) 0.0218(8) Uani 1 1 d . . .
C5 C 0.6831(2) 0.2088(4) 0.4183(3) 0.0279(9) Uani 1 1 d . . .
C6 C 0.7187(2) 0.0932(6) 0.4006(3) 0.0427(11) Uani 1 1 d . . .
H6A H 0.7573 0.1317 0.4069 0.064 Uiso 1 1 calc R . .
H6B H 0.6971 0.0608 0.3484 0.064 Uiso 1 1 calc R . .
H6C H 0.7245 0.0127 0.4352 0.064 Uiso 1 1 calc R . .
C7 C 0.66376(17) 0.8894(4) 0.5913(2) 0.0213(7) Uani 1 1 d . . .
C8 C 0.69667(17) 0.8012(4) 0.6613(2) 0.0205(7) Uani 1 1 d . . .
C9 C 0.67933(17) 0.6960(4) 0.7009(2) 0.0206(7) Uani 1 1 d . . .
C10 C 0.62204(17) 0.6186(4) 0.6866(2) 0.0212(7) Uani 1 1 d . . .
C11 C 0.77447(17) 0.7429(4) 0.7654(2) 0.0237(7) Uani 1 1 d . . .
C12 C 0.8370(2) 0.7411(7) 0.8265(3) 0.0480(13) Uani 1 1 d . . .
H12A H 0.8654 0.7313 0.8032 0.072 Uiso 1 1 calc R . .
H12B H 0.8414 0.6604 0.8606 0.072 Uiso 1 1 calc R . .
H12C H 0.8446 0.8304 0.8553 0.072 Uiso 1 1 calc R . .


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
Yb1 O1 2.192(3) . ?
Yb1 O3 2.390(3) . ?
Yb1 O3 2.499(3) 5_666 ?
Yb1 O4 2.420(3) 5_666 ?
Yb1 O5 2.258(3) . ?
Yb1 O7 2.256(3) . ?
Yb1 O1w 2.376(3) . ?
Yb1 O2w 2.299(3) . ?
Zn1 O2 2.173(3) . ?
Zn1 O6 2.221(3) 7_666 ?
Zn1 O8 2.254(3) 6_565 ?
Zn1 N1 2.122(3) . ?
Zn1 N3 2.064(3) 7_666 ?
Zn1 N4 2.079(3) 6_565 ?
O1 C1 1.263(5) . ?
O2 C1 1.242(5) . ?
O3 C4 1.265(5) . ?
O3 Yb1 2.499(3) 5_666 ?
O4 C4 1.266(5) . ?
O4 Yb1 2.420(3) 5_666 ?
O5 C7 1.264(5) . ?
O6 C7 1.255(5) . ?
O6 Zn1 2.221(3) 7_666 ?
O7 C10 1.279(5) . ?
O8 C10 1.245(5) . ?
O8 Zn1 2.254(3) 6_566 ?
O1w H11 0.8389 . ?
O1w H12 0.8390 . ?
O2w H21 0.8399 . ?
O2w H22 0.8397 . ?
O3w H31 0.8390 . ?
O3w H32 0.8415 . ?
O4w H41 0.8397 . ?
O4w H42 0.8370 . ?
O5w H51 0.8389 . ?
O6w H61 0.8381 . ?
N1 C5 1.328(5) . ?
N1 C2 1.379(5) . ?
N2 C5 1.350(5) . ?
N2 C3 1.373(5) . ?
N2 H2 0.8800 . ?
N3 C11 1.342(5) . ?
N3 C8 1.374(5) . ?
N3 Zn1 2.064(3) 7_666 ?
N4 C11 1.342(5) . ?
N4 C9 1.364(5) . ?
N4 Zn1 2.079(3) 6_566 ?
C1 C2 1.488(6) . ?
C2 C3 1.379(5) . ?
C3 C4 1.474(5) . ?
C5 C6 1.487(6) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.479(5) . ?
C8 C9 1.389(5) . ?
C9 C10 1.480(5) . ?
C11 C12 1.483(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 Yb1 O7 106.58(12) . . ?
O1 Yb1 O5 78.66(12) . . ?
O7 Yb1 O5 77.45(10) . . ?
O1 Yb1 O2w 82.87(13) . . ?
O7 Yb1 O2w 146.74(11) . . ?
O5 Yb1 O2w 135.73(11) . . ?
O1 Yb1 O1w 88.56(12) . . ?
O7 Yb1 O1w 139.17(11) . . ?
O5 Yb1 O1w 68.53(10) . . ?
O2w Yb1 O1w 71.15(11) . . ?
O1 Yb1 O3 77.02(10) . . ?
O7 Yb1 O3 75.01(10) . . ?
O5 Yb1 O3 135.85(10) . . ?
O2w Yb1 O3 76.35(10) . . ?
O1w Yb1 O3 145.80(10) . . ?
O1 Yb1 O4 164.60(11) . 5_666 ?
O7 Yb1 O4 83.86(11) . 5_666 ?
O5 Yb1 O4 93.02(11) . 5_666 ?
O2w Yb1 O4 94.57(12) . 5_666 ?
O1w Yb1 O4 76.29(11) . 5_666 ?
O3 Yb1 O4 117.25(9) . 5_666 ?
O1 Yb1 O3 139.75(10) . 5_666 ?
O7 Yb1 O3 76.91(9) . 5_666 ?
O5 Yb1 O3 138.90(10) . 5_666 ?
O2w Yb1 O3 75.90(10) . 5_666 ?
O1w Yb1 O3 115.38(10) . 5_666 ?
O3 Yb1 O3 65.02(10) . 5_666 ?
O4 Yb1 O3 52.73(10) 5_666 5_666 ?
N3 Zn1 N4 96.54(14) 7_666 6_565 ?
N3 Zn1 N1 163.05(13) 7_666 . ?
N4 Zn1 N1 99.59(14) 6_565 . ?
N3 Zn1 O2 89.62(12) 7_666 . ?
N4 Zn1 O2 161.10(13) 6_565 . ?
N1 Zn1 O2 76.72(12) . . ?
N3 Zn1 O6 77.92(12) 7_666 7_666 ?
N4 Zn1 O6 100.28(12) 6_565 7_666 ?
N1 Zn1 O6 94.02(11) . 7_666 ?
O2 Zn1 O6 98.48(12) . 7_666 ?
N3 Zn1 O8 100.61(12) 7_666 6_565 ?
N4 Zn1 O8 76.51(11) 6_565 6_565 ?
N1 Zn1 O8 88.25(12) . 6_565 ?
O2 Zn1 O8 84.81(12) . 6_565 ?
O6 Zn1 O8 176.36(11) 7_666 6_565 ?
C1 O1 Yb1 153.8(3) . . ?
C1 O2 Zn1 116.7(3) . . ?
C4 O3 Yb1 150.7(2) . . ?
C4 O3 Yb1 91.9(2) . 5_666 ?
Yb1 O3 Yb1 114.98(10) . 5_666 ?
C4 O4 Yb1 95.6(2) . 5_666 ?
C7 O5 Yb1 136.4(3) . . ?
C7 O6 Zn1 112.9(2) . 7_666 ?
C10 O7 Yb1 147.5(2) . . ?
C10 O8 Zn1 113.2(2) . 6_566 ?
Yb1 O1w H11 109.0 . . ?
Yb1 O1w H12 109.6 . . ?
H11 O1w H12 109.4 . . ?
Yb1 O2w H21 108.8 . . ?
Yb1 O2w H22 110.3 . . ?
H21 O2w H22 109.5 . . ?
H31 O3w H32 110.0 . . ?
H41 O4w H42 109.6 . . ?
C5 N1 C2 106.6(3) . . ?
C5 N1 Zn1 139.1(3) . . ?
C2 N1 Zn1 112.2(3) . . ?
C5 N2 C3 108.9(3) . . ?
C5 N2 H2 125.5 . . ?
C3 N2 H2 125.5 . . ?
C11 N3 C8 105.9(3) . . ?
C11 N3 Zn1 140.0(3) . 7_666 ?
C8 N3 Zn1 113.1(2) . 7_666 ?
C11 N4 C9 106.1(3) . . ?
C11 N4 Zn1 139.1(3) . 6_566 ?
C9 N4 Zn1 114.8(2) . 6_566 ?
O2 C1 O1 123.9(4) . . ?
O2 C1 C2 116.1(3) . . ?
O1 C1 C2 120.0(3) . . ?
C3 C2 N1 109.3(3) . . ?
C3 C2 C1 134.1(3) . . ?
N1 C2 C1 116.6(3) . . ?
C2 C3 N2 105.1(3) . . ?
C2 C3 C4 133.5(3) . . ?
N2 C3 C4 120.5(3) . . ?
O3 C4 O4 119.4(4) . . ?
O3 C4 C3 121.7(3) . . ?
O4 C4 C3 118.8(3) . . ?
N1 C5 N2 110.0(3) . . ?
N1 C5 C6 125.9(4) . . ?
N2 C5 C6 124.1(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 O5 123.1(4) . . ?
O6 C7 C8 116.9(3) . . ?
O5 C7 C8 119.9(3) . . ?
N3 C8 C9 107.7(3) . . ?
N3 C8 C7 118.1(3) . . ?
C9 C8 C7 134.0(4) . . ?
N4 C9 C8 108.0(3) . . ?
N4 C9 C10 117.5(3) . . ?
C8 C9 C10 134.5(4) . . ?
O8 C10 O7 122.1(3) . . ?
O8 C10 C9 117.2(3) . . ?
O7 C10 C9 120.6(3) . . ?
N4 C11 N3 112.3(3) . . ?
N4 C11 C12 124.5(4) . . ?
N3 C11 C12 123.2(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O7 Yb1 O1 C1 106.8(7) . . . . ?
O5 Yb1 O1 C1 179.9(7) . . . . ?
O2w Yb1 O1 C1 -40.6(7) . . . . ?
O1w Yb1 O1 C1 -111.7(7) . . . . ?
O3 Yb1 O1 C1 37.0(7) . . . . ?
O4 Yb1 O1 C1 -121.8(7) 5_666 . . . ?
O3 Yb1 O1 C1 17.6(8) 5_666 . . . ?
N3 Zn1 O2 C1 -173.7(3) 7_666 . . . ?
N4 Zn1 O2 C1 76.9(5) 6_565 . . . ?
N1 Zn1 O2 C1 -3.9(3) . . . . ?
O6 Zn1 O2 C1 -96.0(3) 7_666 . . . ?
O8 Zn1 O2 C1 85.6(3) 6_565 . . . ?
O1 Yb1 O3 C4 -11.3(5) . . . . ?
O7 Yb1 O3 C4 -122.7(5) . . . . ?
O5 Yb1 O3 C4 -69.5(6) . . . . ?
O2w Yb1 O3 C4 74.4(5) . . . . ?
O1w Yb1 O3 C4 56.1(6) . . . . ?
O4 Yb1 O3 C4 162.5(5) 5_666 . . . ?
O3 Yb1 O3 C4 155.0(6) 5_666 . . . ?
O1 Yb1 O3 Yb1 -166.29(15) . . . 5_666 ?
O7 Yb1 O3 Yb1 82.31(12) . . . 5_666 ?
O5 Yb1 O3 Yb1 135.53(13) . . . 5_666 ?
O2w Yb1 O3 Yb1 -80.59(13) . . . 5_666 ?
O1w Yb1 O3 Yb1 -98.95(19) . . . 5_666 ?
O4 Yb1 O3 Yb1 7.52(16) 5_666 . . 5_666 ?
O3 Yb1 O3 Yb1 0.0 5_666 . . 5_666 ?
O1 Yb1 O5 C7 -41.1(4) . . . . ?
O7 Yb1 O5 C7 68.9(4) . . . . ?
O2w Yb1 O5 C7 -108.3(4) . . . . ?
O1w Yb1 O5 C7 -134.0(4) . . . . ?
O3 Yb1 O5 C7 16.5(5) . . . . ?
O4 Yb1 O5 C7 152.0(4) 5_666 . . . ?
O3 Yb1 O5 C7 121.5(4) 5_666 . . . ?
O1 Yb1 O7 C10 32.0(5) . . . . ?
O5 Yb1 O7 C10 -41.9(5) . . . . ?
O2w Yb1 O7 C10 134.6(5) . . . . ?
O1w Yb1 O7 C10 -75.7(5) . . . . ?
O3 Yb1 O7 C10 103.2(5) . . . . ?
O4 Yb1 O7 C10 -136.4(5) 5_666 . . . ?
O3 Yb1 O7 C10 170.5(5) 5_666 . . . ?
N3 Zn1 N1 C5 -152.6(5) 7_666 . . . ?
N4 Zn1 N1 C5 9.3(5) 6_565 . . . ?
O2 Zn1 N1 C5 170.4(5) . . . . ?
O6 Zn1 N1 C5 -91.8(4) 7_666 . . . ?
O8 Zn1 N1 C5 85.3(4) 6_565 . . . ?
N3 Zn1 N1 C2 47.2(6) 7_666 . . . ?
N4 Zn1 N1 C2 -150.9(3) 6_565 . . . ?
O2 Zn1 N1 C2 10.2(3) . . . . ?
O6 Zn1 N1 C2 108.0(3) 7_666 . . . ?
O8 Zn1 N1 C2 -74.9(3) 6_565 . . . ?
Zn1 O2 C1 O1 175.1(3) . . . . ?
Zn1 O2 C1 C2 -3.1(5) . . . . ?
Yb1 O1 C1 O2 134.0(6) . . . . ?
Yb1 O1 C1 C2 -47.8(9) . . . . ?
C5 N1 C2 C3 -1.2(5) . . . . ?
Zn1 N1 C2 C3 165.4(3) . . . . ?
C5 N1 C2 C1 178.1(4) . . . . ?
Zn1 N1 C2 C1 -15.3(4) . . . . ?
O2 C1 C2 C3 -168.4(4) . . . . ?
O1 C1 C2 C3 13.4(7) . . . . ?
O2 C1 C2 N1 12.6(5) . . . . ?
O1 C1 C2 N1 -165.7(4) . . . . ?
N1 C2 C3 N2 0.9(5) . . . . ?
C1 C2 C3 N2 -178.2(4) . . . . ?
N1 C2 C3 C4 -168.2(4) . . . . ?
C1 C2 C3 C4 12.8(8) . . . . ?
C5 N2 C3 C2 -0.2(5) . . . . ?
C5 N2 C3 C4 170.5(4) . . . . ?
Yb1 O3 C4 O4 -163.6(3) . . . . ?
Yb1 O3 C4 O4 -6.1(4) 5_666 . . . ?
Yb1 O3 C4 C3 16.2(8) . . . . ?
Yb1 O3 C4 C3 173.7(3) 5_666 . . . ?
Yb1 O4 C4 O3 6.4(4) 5_666 . . . ?
Yb1 O4 C4 C3 -173.4(3) 5_666 . . . ?
C2 C3 C4 O3 -20.8(7) . . . . ?
N2 C3 C4 O3 171.5(4) . . . . ?
C2 C3 C4 O4 159.0(5) . . . . ?
N2 C3 C4 O4 -8.7(6) . . . . ?
C2 N1 C5 N2 1.0(5) . . . . ?
Zn1 N1 C5 N2 -159.9(3) . . . . ?
C2 N1 C5 C6 -179.8(5) . . . . ?
Zn1 N1 C5 C6 19.3(8) . . . . ?
C3 N2 C5 N1 -0.5(5) . . . . ?
C3 N2 C5 C6 -179.7(4) . . . . ?
Zn1 O6 C7 O5 167.0(3) 7_666 . . . ?
Zn1 O6 C7 C8 -9.8(4) 7_666 . . . ?
Yb1 O5 C7 O6 124.5(4) . . . . ?
Yb1 O5 C7 C8 -58.9(5) . . . . ?
C11 N3 C8 C9 0.5(4) . . . . ?
Zn1 N3 C8 C9 -170.2(2) 7_666 . . . ?
C11 N3 C8 C7 176.0(3) . . . . ?
Zn1 N3 C8 C7 5.3(4) 7_666 . . . ?
O6 C7 C8 N3 3.5(5) . . . . ?
O5 C7 C8 N3 -173.4(4) . . . . ?
O6 C7 C8 C9 177.5(4) . . . . ?
O5 C7 C8 C9 0.7(6) . . . . ?
C11 N4 C9 C8 -1.0(4) . . . . ?
Zn1 N4 C9 C8 178.6(2) 6_566 . . . ?
C11 N4 C9 C10 178.7(3) . . . . ?
Zn1 N4 C9 C10 -1.7(4) 6_566 . . . ?
N3 C8 C9 N4 0.3(4) . . . . ?
C7 C8 C9 N4 -174.2(4) . . . . ?
N3 C8 C9 C10 -179.3(4) . . . . ?
C7 C8 C9 C10 6.2(7) . . . . ?
Zn1 O8 C10 O7 168.0(3) 6_566 . . . ?
Zn1 O8 C10 C9 -10.4(4) 6_566 . . . ?
Yb1 O7 C10 O8 -162.5(4) . . . . ?
Yb1 O7 C10 C9 15.9(7) . . . . ?
N4 C9 C10 O8 8.7(5) . . . . ?
C8 C9 C10 O8 -171.7(4) . . . . ?
N4 C9 C10 O7 -169.8(4) . . . . ?
C8 C9 C10 O7 9.8(7) . . . . ?
C9 N4 C11 N3 1.4(5) . . . . ?
Zn1 N4 C11 N3 -178.1(3) 6_566 . . . ?
C9 N4 C11 C12 179.6(5) . . . . ?
Zn1 N4 C11 C12 0.1(8) 6_566 . . . ?
C8 N3 C11 N4 -1.2(5) . . . . ?
Zn1 N3 C11 N4 165.4(3) 7_666 . . . ?
C8 N3 C11 C12 -179.4(4) . . . . ?
Zn1 N3 C11 C12 -12.8(7) 7_666 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O4 0.84 2.19 2.864(4) 138.0 1_565
O1w H12 O3w 0.84 2.23 2.696(4) 115.2 .
O2w H21 O7 0.84 1.99 2.822(4) 172.9 5_666
O2w H22 O5w 0.84 2.08 2.641(6) 124.0 .
O3w H31 O4w 0.84 1.97 2.808(8) 178.1 .
O3w H32 O6w 0.84 2.36 3.177(12) 163.2 .
O4w H41 O2 0.84 1.91 2.737(9) 167.9 2_655
O4w H42 O1w 0.84 2.38 2.960(8) 127.0 2_655
O5w H51 O4w 0.84 1.89 2.723(12) 169.0 .
N2 H2 O6 0.88 2.27 2.848(5) 122.9 1_545

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.185
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.137
#===============================================================================
_database_code_depnum_ccdc_archive 'CCDC 973548'
#######################################################################
#
#                 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_Tb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 Co N4 O12.50 Tb'
_chemical_formula_weight         634.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   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                   24.339(3)
_cell_length_b                   9.1443(12)
_cell_length_c                   19.064(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.6550(10)
_cell_angle_gamma                90.00
_cell_volume                     3856.0(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4402
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    4.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4770
_exptl_absorpt_correction_T_max  0.5878
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11780
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4402
_reflns_number_gt                3352
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0515P)²+12.9958P] 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         4402
_refine_ls_number_parameters     280
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.542350(13) 0.69517(3) 0.494230(18) 0.01893(11) Uani 1 1 d . . .
Co1 Co 0.71142(4) 0.48790(10) 0.33683(5) 0.0200(2) Uani 1 1 d . . .
O1 O 0.6152(2) 0.6456(6) 0.4548(3) 0.0403(14) Uani 1 1 d . . .
O2 O 0.6675(2) 0.6302(5) 0.3842(3) 0.0295(11) Uani 1 1 d . . .
O3 O 0.54759(19) 0.4316(5) 0.4953(3) 0.0243(10) Uani 1 1 d . . .
O4 O 0.5411(2) 0.1940(5) 0.4820(3) 0.0288(11) Uani 1 1 d . . .
O5 O 0.6104(2) 0.8773(5) 0.5537(3) 0.0308(11) Uani 1 1 d . . .
O6 O 0.6981(2) 0.9804(5) 0.5748(3) 0.0268(11) Uani 1 1 d . . .
O7 O 0.5784(2) 0.6336(6) 0.6225(3) 0.0296(11) Uani 1 1 d . . .
O8 O 0.62324(19) 0.5428(5) 0.7413(3) 0.0271(11) Uani 1 1 d . . .
O1W O 0.5182(2) 0.9141(5) 0.4161(3) 0.0365(12) Uani 1 1 d . . .
H11 H 0.5426 0.9802 0.4402 0.055 Uiso 1 1 d R . .
H12 H 0.4828 0.9411 0.4069 0.055 Uiso 1 1 d R . .
O2W O 0.4798(2) 0.6318(5) 0.3653(3) 0.0448(14) Uani 1 1 d . . .
H21 H 0.4594 0.5577 0.3652 0.067 Uiso 1 1 d R . .
H22 H 0.5014 0.6136 0.3411 0.067 Uiso 1 1 d R . .
O3W O 0.4342(2) 1.0551(5) 0.2940(3) 0.133(4) Uani 1 1 d RU . .
H31 H 0.4240 1.0041 0.2540 0.200 Uiso 1 1 d R . .
H32 H 0.4488 1.1347 0.2877 0.200 Uiso 1 1 d R . .
O4W O 0.4104(8) 0.849(2) 0.1868(11) 0.243(8) Uani 1 1 d U . .
H41 H 0.3862 0.7796 0.1692 0.364 Uiso 1 1 d R . .
H42 H 0.4137 0.8947 0.1502 0.364 Uiso 1 1 d R . .
O5W O 0.5000 0.737(5) 0.2500 0.182(15) Uani 0.50 2 d SPU . .
H51 H 0.4703 0.7929 0.2286 0.272 Uiso 0.50 1 d PR . .
O6W O 0.5000 1.292(3) 0.2500 0.099(8) Uani 0.50 2 d SPU . .
H61 H 0.5230 1.3431 0.2869 0.148 Uiso 0.50 1 d PR . .
N1 N 0.6836(2) 0.3433(6) 0.4038(3) 0.0243(13) Uani 1 1 d . . .
N2 N 0.6414(3) 0.1777(6) 0.4481(4) 0.0290(14) Uani 1 1 d . . .
H2 H 0.6318 0.0914 0.4601 0.035 Uiso 1 1 calc R . .
N3 N 0.7583(2) 0.8367(6) 0.7071(3) 0.0231(12) Uani 1 1 d . . .
N4 N 0.7299(2) 0.6683(6) 0.7702(3) 0.0240(13) Uani 1 1 d . . .
C1 C 0.6416(3) 0.5731(7) 0.4223(4) 0.0231(14) Uani 1 1 d . . .
C2 C 0.6445(3) 0.4120(7) 0.4291(4) 0.0200(13) Uani 1 1 d . . .
C3 C 0.6175(3) 0.3092(7) 0.4570(4) 0.0232(14) Uani 1 1 d . . .
C4 C 0.5668(3) 0.3139(8) 0.4796(4) 0.0238(14) Uani 1 1 d . . .
C5 C 0.6814(3) 0.2018(8) 0.4182(4) 0.0271(15) Uani 1 1 d . . .
C6 C 0.7162(4) 0.0843(9) 0.4020(5) 0.042(2) Uani 1 1 d . . .
H6A H 0.7564 0.1182 0.4139 0.062 Uiso 1 1 calc R . .
H6B H 0.6967 0.0579 0.3485 0.062 Uiso 1 1 calc R . .
H6C H 0.7180 0.0005 0.4333 0.062 Uiso 1 1 calc R . .
C7 C 0.6665(3) 0.8921(7) 0.5929(4) 0.0222(14) Uani 1 1 d . . .
C8 C 0.6986(3) 0.8064(7) 0.6642(4) 0.0209(13) Uani 1 1 d . . .
C9 C 0.6804(3) 0.7006(7) 0.7030(4) 0.0222(14) Uani 1 1 d . . .
C10 C 0.6245(3) 0.6225(7) 0.6879(4) 0.0221(14) Uani 1 1 d . . .
C11 C 0.7749(3) 0.7517(8) 0.7694(4) 0.0234(14) Uani 1 1 d . . .
C12 C 0.8367(4) 0.7505(11) 0.8331(5) 0.047(2) Uani 1 1 d . . .
H12A H 0.8510 0.8491 0.8455 0.070 Uiso 1 1 calc R . .
H12B H 0.8634 0.6970 0.8171 0.070 Uiso 1 1 calc R . .
H12C H 0.8356 0.7046 0.8778 0.070 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
Tb1 O1 2.241(5) . ?
Tb1 O5 2.288(5) . ?
Tb1 O7 2.298(5) . ?
Tb1 O2W 2.361(5) . ?
Tb1 O3 2.413(5) . ?
Tb1 O1W 2.418(5) . ?
Tb1 O4 2.474(4) 5_666 ?
Tb1 O3 2.557(4) 5_666 ?
Tb1 C4 2.902(6) 5_666 ?
Co1 N4 2.081(5) 6_565 ?
Co1 N3 2.081(5) 7_666 ?
Co1 O2 2.111(5) . ?
Co1 N1 2.135(6) . ?
Co1 O6 2.162(5) 7_666 ?
Co1 O8 2.178(5) 6_565 ?
O1 C1 1.253(7) . ?
O2 C1 1.257(7) . ?
O3 C4 1.259(8) . ?
O3 Tb1 2.557(4) 5_666 ?
O4 C4 1.273(8) . ?
O4 Tb1 2.474(4) 5_666 ?
O5 C7 1.261(8) . ?
O6 C7 1.260(7) . ?
O6 Co1 2.162(5) 7_666 ?
O7 C10 1.286(8) . ?
O8 C10 1.262(8) . ?
O8 Co1 2.178(5) 6_566 ?
O1W H11 0.8367 . ?
O1W H12 0.8423 . ?
O2W H21 0.8398 . ?
O2W H22 0.8470 . ?
O3W H31 0.8385 . ?
O3W H32 0.8409 . ?
O4W H41 0.8376 . ?
O4W H42 0.8418 . ?
O4W H51 1.4344 . ?
O5W H51 0.8378 . ?
O6W H61 0.8357 . ?
N1 C5 1.328(9) . ?
N1 C2 1.384(7) . ?
N2 C5 1.337(8) . ?
N2 C3 1.377(8) . ?
N2 H2 0.8800 . ?
N3 C11 1.334(9) . ?
N3 C8 1.366(8) . ?
N3 Co1 2.081(5) 7_666 ?
N4 C11 1.340(8) . ?
N4 C9 1.375(8) . ?
N4 Co1 2.081(5) 6_566 ?
C1 C2 1.478(9) . ?
C2 C3 1.374(9) . ?
C3 C4 1.466(8) . ?
C4 Tb1 2.902(6) 5_666 ?
C5 C6 1.478(9) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.478(9) . ?
C8 C9 1.398(9) . ?
C9 C10 1.456(9) . ?
C11 C12 1.488(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 Tb1 O5 78.68(19) . . ?
O1 Tb1 O7 107.6(2) . . ?
O5 Tb1 O7 76.96(17) . . ?
O1 Tb1 O2W 81.8(2) . . ?
O5 Tb1 O2W 135.52(17) . . ?
O7 Tb1 O2W 147.42(18) . . ?
O1 Tb1 O3 75.79(17) . . ?
O5 Tb1 O3 134.28(16) . . ?
O7 Tb1 O3 75.58(17) . . ?
O2W Tb1 O3 76.86(16) . . ?
O1 Tb1 O1W 89.05(19) . . ?
O5 Tb1 O1W 69.02(17) . . ?
O7 Tb1 O1W 138.22(18) . . ?
O2W Tb1 O1W 71.10(18) . . ?
O3 Tb1 O1W 146.19(16) . . ?
O1 Tb1 O4 165.54(18) . 5_666 ?
O5 Tb1 O4 95.19(17) . 5_666 ?
O7 Tb1 O4 83.34(17) . 5_666 ?
O2W Tb1 O4 93.97(17) . 5_666 ?
O3 Tb1 O4 116.87(14) . 5_666 ?
O1W Tb1 O4 76.51(17) . 5_666 ?
O1 Tb1 O3 139.20(17) . 5_666 ?
O5 Tb1 O3 139.21(16) . 5_666 ?
O7 Tb1 O3 76.43(15) . 5_666 ?
O2W Tb1 O3 76.66(16) . 5_666 ?
O3 Tb1 O3 65.83(16) . 5_666 ?
O1W Tb1 O3 115.33(16) . 5_666 ?
O4 Tb1 O3 51.45(15) 5_666 5_666 ?
O1 Tb1 C4 163.9(2) . 5_666 ?
O5 Tb1 C4 117.40(19) . 5_666 ?
O7 Tb1 C4 77.32(18) . 5_666 ?
O2W Tb1 C4 86.20(18) . 5_666 ?
O3 Tb1 C4 91.09(17) . 5_666 ?
O1W Tb1 C4 97.20(19) . 5_666 ?
O4 Tb1 C4 25.85(16) 5_666 5_666 ?
O3 Tb1 C4 25.68(16) 5_666 5_666 ?
N4 Co1 N3 94.6(2) 6_565 7_666 ?
N4 Co1 O2 163.9(2) 6_565 . ?
N3 Co1 O2 91.4(2) 7_666 . ?
N4 Co1 N1 98.2(2) 6_565 . ?
N3 Co1 N1 166.4(2) 7_666 . ?
O2 Co1 N1 77.42(19) . . ?
N4 Co1 O6 99.1(2) 6_565 7_666 ?
N3 Co1 O6 78.1(2) 7_666 7_666 ?
O2 Co1 O6 96.73(19) . 7_666 ?
N1 Co1 O6 95.2(2) . 7_666 ?
N4 Co1 O8 77.82(19) 6_565 6_565 ?
N3 Co1 O8 98.8(2) 7_666 6_565 ?
O2 Co1 O8 86.49(18) . 6_565 ?
N1 Co1 O8 88.4(2) . 6_565 ?
O6 Co1 O8 175.58(17) 7_666 6_565 ?
C1 O1 Tb1 156.0(5) . . ?
C1 O2 Co1 117.2(4) . . ?
C4 O3 Tb1 151.1(4) . . ?
C4 O3 Tb1 92.6(4) . 5_666 ?
Tb1 O3 Tb1 114.17(16) . 5_666 ?
C4 O4 Tb1 96.2(4) . 5_666 ?
C7 O5 Tb1 138.8(4) . . ?
C7 O6 Co1 114.4(4) . 7_666 ?
C10 O7 Tb1 147.4(4) . . ?
C10 O8 Co1 113.7(4) . 6_566 ?
Tb1 O1W H11 109.0 . . ?
Tb1 O1W H12 109.6 . . ?
H11 O1W H12 109.5 . . ?
Tb1 O2W H21 108.9 . . ?
Tb1 O2W H22 109.7 . . ?
H21 O2W H22 109.9 . . ?
H31 O3W H32 109.5 . . ?
H41 O4W H42 109.7 . . ?
H41 O4W H51 109.4 . . ?
H42 O4W H51 102.3 . . ?
C5 N1 C2 106.1(5) . . ?
C5 N1 Co1 140.9(5) . . ?
C2 N1 Co1 111.3(4) . . ?
C5 N2 C3 109.2(6) . . ?
C5 N2 H2 125.4 . . ?
C3 N2 H2 125.4 . . ?
C11 N3 C8 105.4(5) . . ?
C11 N3 Co1 141.5(5) . 7_666 ?
C8 N3 Co1 112.4(4) . 7_666 ?
C11 N4 C9 105.6(5) . . ?
C11 N4 Co1 141.5(5) . 6_566 ?
C9 N4 Co1 112.9(4) . 6_566 ?
O1 C1 O2 123.4(6) . . ?
O1 C1 C2 120.0(6) . . ?
O2 C1 C2 116.6(6) . . ?
C3 C2 N1 109.5(6) . . ?
C3 C2 C1 134.6(6) . . ?
N1 C2 C1 115.9(5) . . ?
C2 C3 N2 104.8(5) . . ?
C2 C3 C4 133.6(6) . . ?
N2 C3 C4 120.8(6) . . ?
O3 C4 O4 119.3(6) . . ?
O3 C4 C3 122.4(6) . . ?
O4 C4 C3 118.3(6) . . ?
O3 C4 Tb1 61.7(3) . 5_666 ?
O4 C4 Tb1 57.9(3) . 5_666 ?
C3 C4 Tb1 172.8(5) . 5_666 ?
N1 C5 N2 110.4(6) . . ?
N1 C5 C6 126.2(6) . . ?
N2 C5 C6 123.5(7) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 O5 122.8(6) . . ?
O6 C7 C8 116.2(6) . . ?
O5 C7 C8 121.0(6) . . ?
N3 C8 C9 108.4(6) . . ?
N3 C8 C7 117.8(6) . . ?
C9 C8 C7 133.7(6) . . ?
N4 C9 C8 107.2(5) . . ?
N4 C9 C10 117.5(6) . . ?
C8 C9 C10 135.4(6) . . ?
O8 C10 O7 121.5(6) . . ?
O8 C10 C9 117.3(6) . . ?
O7 C10 C9 121.2(6) . . ?
N3 C11 N4 113.4(6) . . ?
N3 C11 C12 123.9(6) . . ?
N4 C11 C12 122.7(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O5 Tb1 O1 C1 173.0(13) . . . . ?
O7 Tb1 O1 C1 100.8(13) . . . . ?
O2W Tb1 O1 C1 -47.2(13) . . . . ?
O3 Tb1 O1 C1 31.3(13) . . . . ?
O1W Tb1 O1 C1 -118.2(13) . . . . ?
O4 Tb1 O1 C1 -121.0(12) 5_666 . . . ?
O3 Tb1 O1 C1 11.3(14) 5_666 . . . ?
C4 Tb1 O1 C1 -4.9(18) 5_666 . . . ?
N4 Co1 O2 C1 70.4(9) 6_565 . . . ?
N3 Co1 O2 C1 -177.6(5) 7_666 . . . ?
N1 Co1 O2 C1 -5.5(5) . . . . ?
O6 Co1 O2 C1 -99.4(5) 7_666 . . . ?
O8 Co1 O2 C1 83.7(5) 6_565 . . . ?
O1 Tb1 O3 C4 -9.1(9) . . . . ?
O5 Tb1 O3 C4 -67.1(10) . . . . ?
O7 Tb1 O3 C4 -122.0(9) . . . . ?
O2W Tb1 O3 C4 75.6(9) . . . . ?
O1W Tb1 O3 C4 56.7(10) . . . . ?
O4 Tb1 O3 C4 163.4(9) 5_666 . . . ?
O3 Tb1 O3 C4 156.7(10) 5_666 . . . ?
C4 Tb1 O3 C4 161.4(8) 5_666 . . . ?
O1 Tb1 O3 Tb1 -165.8(2) . . . 5_666 ?
O5 Tb1 O3 Tb1 136.2(2) . . . 5_666 ?
O7 Tb1 O3 Tb1 81.4(2) . . . 5_666 ?
O2W Tb1 O3 Tb1 -81.1(2) . . . 5_666 ?
O1W Tb1 O3 Tb1 -99.9(3) . . . 5_666 ?
O4 Tb1 O3 Tb1 6.7(2) 5_666 . . 5_666 ?
O3 Tb1 O3 Tb1 0.0 5_666 . . 5_666 ?
C4 Tb1 O3 Tb1 4.8(2) 5_666 . . 5_666 ?
O1 Tb1 O5 C7 -46.5(7) . . . . ?
O7 Tb1 O5 C7 64.9(7) . . . . ?
O2W Tb1 O5 C7 -112.2(7) . . . . ?
O3 Tb1 O5 C7 10.5(8) . . . . ?
O1W Tb1 O5 C7 -139.8(7) . . . . ?
O4 Tb1 O5 C7 146.8(7) 5_666 . . . ?
O3 Tb1 O5 C7 115.3(7) 5_666 . . . ?
C4 Tb1 O5 C7 132.9(7) 5_666 . . . ?
O1 Tb1 O7 C10 31.5(9) . . . . ?
O5 Tb1 O7 C10 -41.9(8) . . . . ?
O2W Tb1 O7 C10 134.2(8) . . . . ?
O3 Tb1 O7 C10 101.2(8) . . . . ?
O1W Tb1 O7 C10 -77.7(9) . . . . ?
O4 Tb1 O7 C10 -138.8(8) 5_666 . . . ?
O3 Tb1 O7 C10 169.3(9) 5_666 . . . ?
C4 Tb1 O7 C10 -164.4(9) 5_666 . . . ?
N4 Co1 N1 C5 8.7(8) 6_565 . . . ?
N3 Co1 N1 C5 -151.4(9) 7_666 . . . ?
O2 Co1 N1 C5 172.9(8) . . . . ?
O6 Co1 N1 C5 -91.3(8) 7_666 . . . ?
O8 Co1 N1 C5 86.2(8) 6_565 . . . ?
N4 Co1 N1 C2 -153.7(4) 6_565 . . . ?
N3 Co1 N1 C2 46.2(11) 7_666 . . . ?
O2 Co1 N1 C2 10.5(4) . . . . ?
O6 Co1 N1 C2 106.2(4) 7_666 . . . ?
O8 Co1 N1 C2 -76.3(4) 6_565 . . . ?
Tb1 O1 C1 O2 141.1(10) . . . . ?
Tb1 O1 C1 C2 -40.0(16) . . . . ?
Co1 O2 C1 O1 178.3(5) . . . . ?
Co1 O2 C1 C2 -0.6(8) . . . . ?
C5 N1 C2 C3 -1.6(8) . . . . ?
Co1 N1 C2 C3 167.0(5) . . . . ?
C5 N1 C2 C1 177.2(6) . . . . ?
Co1 N1 C2 C1 -14.3(7) . . . . ?
O1 C1 C2 C3 9.7(12) . . . . ?
O2 C1 C2 C3 -171.3(7) . . . . ?
O1 C1 C2 N1 -168.6(6) . . . . ?
O2 C1 C2 N1 10.4(9) . . . . ?
N1 C2 C3 N2 0.1(8) . . . . ?
C1 C2 C3 N2 -178.3(7) . . . . ?
N1 C2 C3 C4 -168.9(7) . . . . ?
C1 C2 C3 C4 12.7(14) . . . . ?
C5 N2 C3 C2 1.4(8) . . . . ?
C5 N2 C3 C4 172.2(6) . . . . ?
Tb1 O3 C4 O4 -164.7(6) . . . . ?
Tb1 O3 C4 O4 -5.9(7) 5_666 . . . ?
Tb1 O3 C4 C3 14.3(13) . . . . ?
Tb1 O3 C4 C3 173.1(6) 5_666 . . . ?
Tb1 O3 C4 Tb1 -158.8(9) . . . 5_666 ?
Tb1 O4 C4 O3 6.1(7) 5_666 . . . ?
Tb1 O4 C4 C3 -172.9(5) 5_666 . . . ?
C2 C3 C4 O3 -19.2(12) . . . . ?
N2 C3 C4 O3 173.2(7) . . . . ?
C2 C3 C4 O4 159.8(8) . . . . ?
N2 C3 C4 O4 -7.8(10) . . . . ?
C2 C3 C4 Tb1 103(4) . . . 5_666 ?
N2 C3 C4 Tb1 -64(4) . . . 5_666 ?
C2 N1 C5 N2 2.5(8) . . . . ?
Co1 N1 C5 N2 -160.5(6) . . . . ?
C2 N1 C5 C6 -179.2(7) . . . . ?
Co1 N1 C5 C6 17.8(13) . . . . ?
C3 N2 C5 N1 -2.5(8) . . . . ?
C3 N2 C5 C6 179.1(7) . . . . ?
Co1 O6 C7 O5 168.9(5) 7_666 . . . ?
Co1 O6 C7 C8 -10.2(7) 7_666 . . . ?
Tb1 O5 C7 O6 125.6(6) . . . . ?
Tb1 O5 C7 C8 -55.4(10) . . . . ?
C11 N3 C8 C9 -0.1(7) . . . . ?
Co1 N3 C8 C9 -172.6(4) 7_666 . . . ?
C11 N3 C8 C7 176.3(6) . . . . ?
Co1 N3 C8 C7 3.8(7) 7_666 . . . ?
O6 C7 C8 N3 4.5(9) . . . . ?
O5 C7 C8 N3 -174.6(6) . . . . ?
O6 C7 C8 C9 179.8(7) . . . . ?
O5 C7 C8 C9 0.7(11) . . . . ?
C11 N4 C9 C8 -0.6(7) . . . . ?
Co1 N4 C9 C8 179.7(4) 6_566 . . . ?
C11 N4 C9 C10 178.9(6) . . . . ?
Co1 N4 C9 C10 -0.8(7) 6_566 . . . ?
N3 C8 C9 N4 0.4(7) . . . . ?
C7 C8 C9 N4 -175.2(7) . . . . ?
N3 C8 C9 C10 -178.9(7) . . . . ?
C7 C8 C9 C10 5.5(13) . . . . ?
Co1 O8 C10 O7 169.3(5) 6_566 . . . ?
Co1 O8 C10 C9 -10.1(7) 6_566 . . . ?
Tb1 O7 C10 O8 -160.3(6) . . . . ?
Tb1 O7 C10 C9 19.1(12) . . . . ?
N4 C9 C10 O8 7.7(9) . . . . ?
C8 C9 C10 O8 -173.0(7) . . . . ?
N4 C9 C10 O7 -171.7(6) . . . . ?
C8 C9 C10 O7 7.6(12) . . . . ?
C8 N3 C11 N4 -0.3(8) . . . . ?
Co1 N3 C11 N4 168.5(5) 7_666 . . . ?
C8 N3 C11 C12 -179.1(7) . . . . ?
Co1 N3 C11 C12 -10.3(12) 7_666 . . . ?
C9 N4 C11 N3 0.6(8) . . . . ?
Co1 N4 C11 N3 -179.8(5) 6_566 . . . ?
C9 N4 C11 C12 179.4(7) . . . . ?
Co1 N4 C11 C12 -1.0(13) 6_566 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11 O4 0.84 2.12 2.803(7) 138.8 1_565
O1W H12 O3W 0.84 2.23 2.699(7) 115.0 .
O2W H21 O7 0.84 2.04 2.869(7) 171.4 5_666
O2W H22 O5W 0.85 2.06 2.626(16) 123.7 .
O3W H31 O4W 0.84 1.84 2.659(17) 163.4 .
O3W H32 O6W 0.84 2.21 3.013(19) 160.0 .
O4W H41 O2 0.84 1.87 2.701(18) 171.5 2_655
O4W H42 O1W 0.84 2.48 3.170(17) 140.4 2_655
O5W H51 O4W 0.84 1.43 2.25(3) 163.5 .
N2 H2 O6 0.88 2.34 2.866(7) 118.5 1_545

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.370
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.190
_database_code_depnum_ccdc_archive 'CCDC 995739'
#######################################################################
#
#                 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_dy

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H15 Co Dy N4 O12'
_chemical_formula_weight         628.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   24.3237(17)
_cell_length_b                   9.1523(6)
_cell_length_c                   19.0813(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.6250(10)
_cell_angle_gamma                90.00
_cell_volume                     3861.5(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6670
_cell_measurement_theta_min      2.3483
_cell_measurement_theta_max      28.1667

_exptl_crystal_description       prism
_exptl_crystal_colour            'light red'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2432
_exptl_absorpt_coefficient_mu    4.770
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4067
_exptl_absorpt_correction_T_max  0.5548
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16179
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4401
_reflns_number_gt                3823
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0702P)²+46.0802P] 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         4401
_refine_ls_number_parameters     267
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1286
_refine_ls_wR_factor_gt          0.1240
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.111
_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
Dy1 Dy 0.542466(12) 0.69471(3) 0.494620(16) 0.01902(12) Uani 1 1 d . . .
Co1 Co 0.71135(4) 0.48810(10) 0.33688(5) 0.0208(2) Uani 1 1 d . . .
O1 O 0.6155(3) 0.6465(6) 0.4559(4) 0.0416(14) Uani 1 1 d . . .
O2 O 0.6672(2) 0.6305(6) 0.3847(3) 0.0332(11) Uani 1 1 d . . .
O3 O 0.5471(2) 0.4319(5) 0.4951(3) 0.0246(10) Uani 1 1 d . . .
O4 O 0.5402(2) 0.1945(5) 0.4815(3) 0.0304(11) Uani 1 1 d . . .
O5 O 0.6103(2) 0.8767(6) 0.5539(3) 0.0343(12) Uani 1 1 d . . .
O6 O 0.6981(2) 0.9799(5) 0.5749(3) 0.0270(10) Uani 1 1 d . . .
O7 O 0.5784(2) 0.6328(6) 0.6224(3) 0.0312(11) Uani 1 1 d . . .
O8 O 0.6229(2) 0.5434(6) 0.7408(3) 0.0288(10) Uani 1 1 d . . .
O1W O 0.5175(3) 0.9121(6) 0.4164(3) 0.0407(13) Uani 1 1 d . . .
H11 H 0.5417 0.9792 0.4400 0.061 Uiso 1 1 d R . .
H12 H 0.4820 0.9381 0.4073 0.061 Uiso 1 1 d R . .
O2W O 0.4803(2) 0.6300(6) 0.3665(3) 0.0458(15) Uani 1 1 d . . .
H21 H 0.4598 0.5559 0.3661 0.069 Uiso 1 1 d R . .
H22 H 0.5020 0.6112 0.3430 0.069 Uiso 1 1 d R . .
O3W O 0.4347(2) 1.0532(6) 0.2953(3) 0.134(5) Uani 1 1 d RU . .
H31 H 0.4247 0.9952 0.2579 0.201 Uiso 1 1 d R . .
H32 H 0.4492 1.1298 0.2856 0.201 Uiso 1 1 d R . .
O4W O 0.4059(2) 0.8595(6) 0.1795(3) 0.219(8) Uani 1 1 d RU . .
H41 H 0.3799 0.7931 0.1696 0.329 Uiso 1 1 d R . .
H42 H 0.3976 0.9149 0.1413 0.329 Uiso 1 1 d R . .
N1 N 0.6833(3) 0.3430(7) 0.4039(3) 0.0257(12) Uani 1 1 d . . .
N2 N 0.6417(3) 0.1776(6) 0.4491(4) 0.0284(13) Uani 1 1 d . . .
H2 H 0.6329 0.0917 0.4625 0.034 Uiso 1 1 calc R . .
N3 N 0.7582(2) 0.8363(6) 0.7074(3) 0.0234(11) Uani 1 1 d . . .
N4 N 0.7300(3) 0.6670(6) 0.7694(3) 0.0239(11) Uani 1 1 d . . .
C1 C 0.6417(3) 0.5739(7) 0.4225(4) 0.0242(13) Uani 1 1 d . . .
C2 C 0.6446(3) 0.4117(7) 0.4289(4) 0.0214(12) Uani 1 1 d . . .
C3 C 0.6169(3) 0.3092(8) 0.4565(4) 0.0263(14) Uani 1 1 d . . .
C4 C 0.5658(3) 0.3127(7) 0.4794(4) 0.0209(12) Uani 1 1 d . . .
C5 C 0.6814(3) 0.2021(8) 0.4180(4) 0.0285(15) Uani 1 1 d . . .
C6 C 0.7161(4) 0.0856(10) 0.4013(6) 0.046(2) Uani 1 1 d . . .
H6A H 0.7574 0.1159 0.4180 0.070 Uiso 1 1 calc R . .
H6B H 0.6989 0.0668 0.3469 0.070 Uiso 1 1 calc R . .
H6C H 0.7145 -0.0018 0.4282 0.070 Uiso 1 1 calc R . .
C7 C 0.6669(3) 0.8908(7) 0.5928(4) 0.0234(13) Uani 1 1 d . . .
C8 C 0.6984(3) 0.8050(7) 0.6637(4) 0.0218(13) Uani 1 1 d . . .
C9 C 0.6809(3) 0.7003(7) 0.7032(4) 0.0216(13) Uani 1 1 d . . .
C10 C 0.6243(3) 0.6218(8) 0.6877(4) 0.0232(13) Uani 1 1 d . . .
C11 C 0.7746(3) 0.7518(9) 0.7696(4) 0.0265(14) Uani 1 1 d . . .
C12 C 0.8369(4) 0.7522(13) 0.8327(5) 0.051(2) Uani 1 1 d . . .
H12A H 0.8659 0.7578 0.8109 0.077 Uiso 1 1 calc R . .
H12B H 0.8432 0.6641 0.8623 0.077 Uiso 1 1 calc R . .
H12C H 0.8415 0.8351 0.8656 0.077 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
Dy1 O1 2.233(5) . ?
Dy1 O5 2.285(5) . ?
Dy1 O7 2.292(5) . ?
Dy1 O2W 2.352(5) . ?
Dy1 O3 2.408(5) . ?
Dy1 O1W 2.408(6) . ?
Dy1 O4 2.459(5) 5_666 ?
Dy1 O3 2.545(5) 5_666 ?
Dy1 C4 2.878(7) 5_666 ?
Co1 N4 2.089(6) 6_565 ?
Co1 N3 2.090(6) 7_666 ?
Co1 O2 2.121(5) . ?
Co1 N1 2.143(6) . ?
Co1 O6 2.163(5) 7_666 ?
Co1 O8 2.187(5) 6_565 ?
O1 C1 1.262(8) . ?
O2 C1 1.244(8) . ?
O3 C4 1.266(8) . ?
O3 Dy1 2.545(5) 5_666 ?
O4 C4 1.257(8) . ?
O4 Dy1 2.459(5) 5_666 ?
O5 C7 1.269(8) . ?
O6 C7 1.256(8) . ?
O6 Co1 2.163(5) 7_666 ?
O7 C10 1.285(8) . ?
O8 C10 1.254(8) . ?
O8 Co1 2.187(5) 6_566 ?
O1W H11 0.8401 . ?
O1W H12 0.8398 . ?
O2W H21 0.8398 . ?
O2W H22 0.8401 . ?
O3W H31 0.8401 . ?
O3W H32 0.8401 . ?
O4W H41 0.8399 . ?
O4W H42 0.8401 . ?
N1 C5 1.322(9) . ?
N1 C2 1.372(8) . ?
N2 C5 1.347(9) . ?
N2 C3 1.380(9) . ?
N2 H2 0.8800 . ?
N3 C11 1.331(9) . ?
N3 C8 1.372(8) . ?
N3 Co1 2.090(6) 7_666 ?
N4 C11 1.332(9) . ?
N4 C9 1.363(8) . ?
N4 Co1 2.089(6) 6_566 ?
C1 C2 1.489(9) . ?
C2 C3 1.381(9) . ?
C3 C4 1.478(9) . ?
C4 Dy1 2.878(7) 5_666 ?
C5 C6 1.474(10) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.473(9) . ?
C8 C9 1.390(9) . ?
C9 C10 1.470(9) . ?
C11 C12 1.492(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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 O5 78.3(2) . . ?
O1 Dy1 O7 107.4(2) . . ?
O5 Dy1 O7 77.10(18) . . ?
O1 Dy1 O2W 82.0(2) . . ?
O5 Dy1 O2W 135.81(19) . . ?
O7 Dy1 O2W 146.96(19) . . ?
O1 Dy1 O3 76.23(18) . . ?
O5 Dy1 O3 134.70(17) . . ?
O7 Dy1 O3 75.67(18) . . ?
O2W Dy1 O3 76.16(17) . . ?
O1 Dy1 O1W 89.3(2) . . ?
O5 Dy1 O1W 69.41(18) . . ?
O7 Dy1 O1W 138.5(2) . . ?
O2W Dy1 O1W 71.17(19) . . ?
O3 Dy1 O1W 145.79(17) . . ?
O1 Dy1 O4 165.4(2) . 5_666 ?
O5 Dy1 O4 94.91(19) . 5_666 ?
O7 Dy1 O4 83.31(19) . 5_666 ?
O2W Dy1 O4 94.3(2) . 5_666 ?
O3 Dy1 O4 116.83(15) . 5_666 ?
O1W Dy1 O4 76.10(19) . 5_666 ?
O1 Dy1 O3 139.42(18) . 5_666 ?
O5 Dy1 O3 139.29(18) . 5_666 ?
O7 Dy1 O3 76.38(16) . 5_666 ?
O2W Dy1 O3 76.45(17) . 5_666 ?
O3 Dy1 O3 65.48(17) . 5_666 ?
O1W Dy1 O3 114.89(18) . 5_666 ?
O4 Dy1 O3 51.76(16) 5_666 5_666 ?
O1 Dy1 C4 164.5(2) . 5_666 ?
O5 Dy1 C4 117.13(19) . 5_666 ?
O7 Dy1 C4 77.37(18) . 5_666 ?
O2W Dy1 C4 86.30(19) . 5_666 ?
O3 Dy1 C4 91.16(16) . 5_666 ?
O1W Dy1 C4 96.53(19) . 5_666 ?
O4 Dy1 C4 25.75(16) 5_666 5_666 ?
O3 Dy1 C4 26.08(16) 5_666 5_666 ?
N4 Co1 N3 93.9(2) 6_565 7_666 ?
N4 Co1 O2 164.0(2) 6_565 . ?
N3 Co1 O2 91.7(2) 7_666 . ?
N4 Co1 N1 98.7(2) 6_565 . ?
N3 Co1 N1 166.6(2) 7_666 . ?
O2 Co1 N1 77.3(2) . . ?
N4 Co1 O6 99.2(2) 6_565 7_666 ?
N3 Co1 O6 78.1(2) 7_666 7_666 ?
O2 Co1 O6 96.7(2) . 7_666 ?
N1 Co1 O6 95.4(2) . 7_666 ?
N4 Co1 O8 77.6(2) 6_565 6_565 ?
N3 Co1 O8 98.8(2) 7_666 6_565 ?
O2 Co1 O8 86.8(2) . 6_565 ?
N1 Co1 O8 88.4(2) . 6_565 ?
O6 Co1 O8 175.37(18) 7_666 6_565 ?
C1 O1 Dy1 155.4(5) . . ?
C1 O2 Co1 117.3(5) . . ?
C4 O3 Dy1 151.7(4) . . ?
C4 O3 Dy1 91.8(4) . 5_666 ?
Dy1 O3 Dy1 114.52(17) . 5_666 ?
C4 O4 Dy1 96.1(4) . 5_666 ?
C7 O5 Dy1 138.3(5) . . ?
C7 O6 Co1 114.3(4) . 7_666 ?
C10 O7 Dy1 147.5(4) . . ?
C10 O8 Co1 113.9(4) . 6_566 ?
Dy1 O1W H11 109.4 . . ?
Dy1 O1W H12 109.6 . . ?
H11 O1W H12 109.5 . . ?
Dy1 O2W H21 109.6 . . ?
Dy1 O2W H22 109.4 . . ?
H21 O2W H22 109.5 . . ?
H31 O3W H32 109.9 . . ?
H41 O4W H42 110.8 . . ?
C5 N1 C2 106.8(6) . . ?
C5 N1 Co1 140.6(5) . . ?
C2 N1 Co1 111.0(4) . . ?
C5 N2 C3 108.9(6) . . ?
C5 N2 H2 125.6 . . ?
C3 N2 H2 125.6 . . ?
C11 N3 C8 105.6(5) . . ?
C11 N3 Co1 141.5(5) . 7_666 ?
C8 N3 Co1 112.3(4) . 7_666 ?
C11 N4 C9 105.7(5) . . ?
C11 N4 Co1 141.3(5) . 6_566 ?
C9 N4 Co1 113.0(4) . 6_566 ?
O2 C1 O1 123.6(6) . . ?
O2 C1 C2 116.3(6) . . ?
O1 C1 C2 120.1(6) . . ?
N1 C2 C3 109.6(6) . . ?
N1 C2 C1 116.4(6) . . ?
C3 C2 C1 133.9(6) . . ?
N2 C3 C2 104.5(6) . . ?
N2 C3 C4 120.4(6) . . ?
C2 C3 C4 134.5(6) . . ?
O4 C4 O3 120.1(6) . . ?
O4 C4 C3 118.6(6) . . ?
O3 C4 C3 121.3(6) . . ?
O4 C4 Dy1 58.2(3) . 5_666 ?
O3 C4 Dy1 62.1(3) . 5_666 ?
C3 C4 Dy1 172.9(5) . 5_666 ?
N1 C5 N2 110.1(6) . . ?
N1 C5 C6 126.2(7) . . ?
N2 C5 C6 123.7(7) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C7 O5 122.6(6) . . ?
O6 C7 C8 117.0(6) . . ?
O5 C7 C8 120.3(6) . . ?
N3 C8 C9 107.5(6) . . ?
N3 C8 C7 117.4(6) . . ?
C9 C8 C7 134.9(6) . . ?
N4 C9 C8 108.0(6) . . ?
N4 C9 C10 117.6(6) . . ?
C8 C9 C10 134.4(6) . . ?
O8 C10 O7 121.6(6) . . ?
O8 C10 C9 117.1(6) . . ?
O7 C10 C9 121.3(6) . . ?
N3 C11 N4 113.3(6) . . ?
N3 C11 C12 123.0(7) . . ?
N4 C11 C12 123.7(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

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
O5 Dy1 O1 C1 174.8(14) . . . . ?
O7 Dy1 O1 C1 102.5(13) . . . . ?
O2W Dy1 O1 C1 -45.0(13) . . . . ?
O3 Dy1 O1 C1 32.6(13) . . . . ?
O1W Dy1 O1 C1 -116.1(14) . . . . ?
O4 Dy1 O1 C1 -121.6(13) 5_666 . . . ?
O3 Dy1 O1 C1 13.2(15) 5_666 . . . ?
C4 Dy1 O1 C1 -3.5(19) 5_666 . . . ?
N4 Co1 O2 C1 71.8(10) 6_565 . . . ?
N3 Co1 O2 C1 -177.5(5) 7_666 . . . ?
N1 Co1 O2 C1 -5.3(5) . . . . ?
O6 Co1 O2 C1 -99.4(5) 7_666 . . . ?
O8 Co1 O2 C1 83.7(5) 6_565 . . . ?
O1 Dy1 O3 C4 -9.4(9) . . . . ?
O5 Dy1 O3 C4 -67.0(9) . . . . ?
O7 Dy1 O3 C4 -121.8(9) . . . . ?
O2W Dy1 O3 C4 75.7(9) . . . . ?
O1W Dy1 O3 C4 58.2(10) . . . . ?
O4 Dy1 O3 C4 163.5(9) 5_666 . . . ?
O3 Dy1 O3 C4 156.9(10) 5_666 . . . ?
C4 Dy1 O3 C4 161.6(8) 5_666 . . . ?
O1 Dy1 O3 Dy1 -166.3(3) . . . 5_666 ?
O5 Dy1 O3 Dy1 136.1(2) . . . 5_666 ?
O7 Dy1 O3 Dy1 81.3(2) . . . 5_666 ?
O2W Dy1 O3 Dy1 -81.2(2) . . . 5_666 ?
O1W Dy1 O3 Dy1 -98.7(3) . . . 5_666 ?
O4 Dy1 O3 Dy1 6.7(3) 5_666 . . 5_666 ?
O3 Dy1 O3 Dy1 0.0 5_666 . . 5_666 ?
C4 Dy1 O3 Dy1 4.7(2) 5_666 . . 5_666 ?
O1 Dy1 O5 C7 -45.8(7) . . . . ?
O7 Dy1 O5 C7 65.4(7) . . . . ?
O2W Dy1 O5 C7 -111.3(7) . . . . ?
O3 Dy1 O5 C7 11.1(8) . . . . ?
O1W Dy1 O5 C7 -139.5(8) . . . . ?
O4 Dy1 O5 C7 147.3(7) 5_666 . . . ?
O3 Dy1 O5 C7 115.8(7) 5_666 . . . ?
C4 Dy1 O5 C7 133.7(7) 5_666 . . . ?
O1 Dy1 O7 C10 31.6(9) . . . . ?
O5 Dy1 O7 C10 -41.6(9) . . . . ?
O2W Dy1 O7 C10 134.1(8) . . . . ?
O3 Dy1 O7 C10 101.8(9) . . . . ?
O1W Dy1 O7 C10 -78.1(10) . . . . ?
O4 Dy1 O7 C10 -138.2(9) 5_666 . . . ?
O3 Dy1 O7 C10 169.6(9) 5_666 . . . ?
C4 Dy1 O7 C10 -163.7(9) 5_666 . . . ?
N4 Co1 N1 C5 9.1(8) 6_565 . . . ?
N3 Co1 N1 C5 -151.0(9) 7_666 . . . ?
O2 Co1 N1 C5 173.3(8) . . . . ?
O6 Co1 N1 C5 -91.0(8) 7_666 . . . ?
O8 Co1 N1 C5 86.3(8) 6_565 . . . ?
N4 Co1 N1 C2 -153.8(4) 6_565 . . . ?
N3 Co1 N1 C2 46.1(12) 7_666 . . . ?
O2 Co1 N1 C2 10.4(4) . . . . ?
O6 Co1 N1 C2 106.0(5) 7_666 . . . ?
O8 Co1 N1 C2 -76.7(5) 6_565 . . . ?
Co1 O2 C1 O1 177.7(6) . . . . ?
Co1 O2 C1 C2 -0.7(8) . . . . ?
Dy1 O1 C1 O2 139.8(11) . . . . ?
Dy1 O1 C1 C2 -41.8(17) . . . . ?
C5 N1 C2 C3 -2.1(8) . . . . ?
Co1 N1 C2 C3 166.6(5) . . . . ?
C5 N1 C2 C1 176.9(6) . . . . ?
Co1 N1 C2 C1 -14.3(7) . . . . ?
O2 C1 C2 N1 10.6(9) . . . . ?
O1 C1 C2 N1 -167.9(6) . . . . ?
O2 C1 C2 C3 -170.6(7) . . . . ?
O1 C1 C2 C3 10.9(12) . . . . ?
C5 N2 C3 C2 -0.6(8) . . . . ?
C5 N2 C3 C4 171.8(6) . . . . ?
N1 C2 C3 N2 1.7(8) . . . . ?
C1 C2 C3 N2 -177.2(7) . . . . ?
N1 C2 C3 C4 -169.1(7) . . . . ?
C1 C2 C3 C4 12.0(14) . . . . ?
Dy1 O4 C4 O3 5.8(7) 5_666 . . . ?
Dy1 O4 C4 C3 -172.7(5) 5_666 . . . ?
Dy1 O3 C4 O4 -164.7(6) . . . . ?
Dy1 O3 C4 O4 -5.6(6) 5_666 . . . ?
Dy1 O3 C4 C3 13.8(13) . . . . ?
Dy1 O3 C4 C3 172.9(6) 5_666 . . . ?
Dy1 O3 C4 Dy1 -159.1(9) . . . 5_666 ?
N2 C3 C4 O4 -9.7(10) . . . . ?
C2 C3 C4 O4 159.9(8) . . . . ?
N2 C3 C4 O3 171.7(6) . . . . ?
C2 C3 C4 O3 -18.6(12) . . . . ?
N2 C3 C4 Dy1 -71(4) . . . 5_666 ?
C2 C3 C4 Dy1 99(4) . . . 5_666 ?
C2 N1 C5 N2 1.7(8) . . . . ?
Co1 N1 C5 N2 -161.6(6) . . . . ?
C2 N1 C5 C6 -179.5(8) . . . . ?
Co1 N1 C5 C6 17.1(14) . . . . ?
C3 N2 C5 N1 -0.7(9) . . . . ?
C3 N2 C5 C6 -179.5(8) . . . . ?
Co1 O6 C7 O5 168.2(5) 7_666 . . . ?
Co1 O6 C7 C8 -9.5(7) 7_666 . . . ?
Dy1 O5 C7 O6 126.2(7) . . . . ?
Dy1 O5 C7 C8 -56.2(10) . . . . ?
C11 N3 C8 C9 0.4(8) . . . . ?
Co1 N3 C8 C9 -172.6(4) 7_666 . . . ?
C11 N3 C8 C7 176.1(6) . . . . ?
Co1 N3 C8 C7 3.2(7) 7_666 . . . ?
O6 C7 C8 N3 4.5(9) . . . . ?
O5 C7 C8 N3 -173.3(6) . . . . ?
O6 C7 C8 C9 178.8(7) . . . . ?
O5 C7 C8 C9 1.0(12) . . . . ?
C11 N4 C9 C8 1.3(8) . . . . ?
Co1 N4 C9 C8 179.3(4) 6_566 . . . ?
C11 N4 C9 C10 -180.0(6) . . . . ?
Co1 N4 C9 C10 -2.0(7) 6_566 . . . ?
N3 C8 C9 N4 -1.0(7) . . . . ?
C7 C8 C9 N4 -175.7(7) . . . . ?
N3 C8 C9 C10 -179.5(7) . . . . ?
C7 C8 C9 C10 5.8(14) . . . . ?
Co1 O8 C10 O7 169.2(5) 6_566 . . . ?
Co1 O8 C10 C9 -10.5(8) 6_566 . . . ?
Dy1 O7 C10 O8 -161.0(6) . . . . ?
Dy1 O7 C10 C9 18.6(13) . . . . ?
N4 C9 C10 O8 8.8(9) . . . . ?
C8 C9 C10 O8 -172.9(7) . . . . ?
N4 C9 C10 O7 -170.9(6) . . . . ?
C8 C9 C10 O7 7.4(12) . . . . ?
C8 N3 C11 N4 0.5(8) . . . . ?
Co1 N3 C11 N4 169.9(5) 7_666 . . . ?
C8 N3 C11 C12 -179.9(8) . . . . ?
Co1 N3 C11 C12 -10.4(14) 7_666 . . . ?
C9 N4 C11 N3 -1.1(8) . . . . ?
Co1 N4 C11 N3 -178.2(5) 6_566 . . . ?
C9 N4 C11 C12 179.2(8) . . . . ?
Co1 N4 C11 C12 2.2(14) 6_566 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11 O4 0.84 2.13 2.821(8) 139.4 1_565
O1W H12 O3W 0.84 2.22 2.681(8) 114.2 .
O2W H21 O7 0.84 2.02 2.850(8) 171.7 5_666
O3W H31 O4W 0.84 1.85 2.687 176.6 .
O4W H41 O2 0.84 1.90 2.691(7) 156.4 2_655
O4W H42 O1W 0.84 2.72 3.146(8) 113.5 2_655
N2 H2 O6 0.88 2.31 2.859(8) 120.7 1_545

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.836
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.240
_database_code_depnum_ccdc_archive 'CCDC 973549'
