# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_fg110b
_database_code_depnum_ccdc_archive 'CCDC 1508469'
_audit_update_record             
;
2016-10-05 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'tetrakis(1-Hydroxy-6-(methylamino)carbonyl-1H-pyridin-2-onate)-zirconium tetrahydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H28 N8 O12 Zr, 4(H2 O)'
_chemical_formula_sum            'C28 H36 N8 O16 Zr'
_chemical_formula_weight         831.87

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'
Zr Zr -2.9673 0.5597 '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                   15.6724(9)
_cell_length_b                   9.7264(5)
_cell_length_c                   21.0842(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.6940(10)
_cell_angle_gamma                90.00
_cell_volume                     3210.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5185
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9297
_exptl_absorpt_correction_T_max  0.9416
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13270
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3652
_reflns_number_gt                3061
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0453P)²+7.0786P] 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         3652
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Zr1 Zr 1.0000 0.00110(3) 0.2500 0.01473(10) Uani 1 2 d S . .
O1 O 0.86759(10) 0.05961(17) 0.22126(7) 0.0176(3) Uani 1 1 d . . .
O2 O 0.91616(10) -0.17579(17) 0.25463(8) 0.0190(3) Uani 1 1 d . . .
O3 O 0.65684(11) 0.11385(19) 0.09622(8) 0.0279(4) Uani 1 1 d . . .
O4 O 0.98816(10) -0.05994(17) 0.14878(7) 0.0181(3) Uani 1 1 d . . .
O5 O 1.02349(10) 0.17606(17) 0.18980(7) 0.0192(3) Uani 1 1 d . . .
O6 O 0.85929(12) -0.11289(18) -0.02706(8) 0.0272(4) Uani 1 1 d . . .
O1W O 0.00461(12) 0.60936(18) 0.16524(9) 0.0339(4) Uani 1 1 d G . .
H1AW H 0.0190 0.6586 0.1973 0.051 Uiso 1 1 d G . .
H1BW H 0.0465 0.6026 0.1412 0.051 Uiso 1 1 d G . .
O2W O 0.10697(14) 0.4029(2) 0.27190(9) 0.0454(5) Uani 1 1 d G . .
H2AW H 0.0850 0.3508 0.2432 0.068 Uiso 1 1 d G . .
H2BW H 0.0709 0.4638 0.2815 0.068 Uiso 1 1 d G . .
N1 N 0.81917(12) -0.0476(2) 0.19912(9) 0.0168(4) Uani 1 1 d . . .
N2 N 0.76535(13) 0.2213(2) 0.14988(10) 0.0230(4) Uani 1 1 d . . .
H2N H 0.8100 0.2130 0.1749 0.028 Uiso 1 1 calc R . .
N3 N 0.96710(12) 0.0467(2) 0.10956(9) 0.0169(4) Uani 1 1 d . . .
N4 N 0.90373(13) -0.2208(2) 0.06325(9) 0.0219(4) Uani 1 1 d . . .
H4N H 0.9293 -0.2139 0.1001 0.026 Uiso 1 1 calc R . .
C1 C 0.84612(14) -0.1742(2) 0.21968(10) 0.0175(5) Uani 1 1 d . . .
C2 C 0.79769(15) -0.2896(2) 0.20120(11) 0.0202(5) Uani 1 1 d . . .
H2 H 0.8129 -0.3764 0.2164 0.024 Uiso 1 1 calc R . .
C3 C 0.72746(15) -0.2737(3) 0.16040(11) 0.0219(5) Uani 1 1 d . . .
H3 H 0.6952 -0.3499 0.1476 0.026 Uiso 1 1 calc R . .
C4 C 0.70451(15) -0.1433(3) 0.13817(11) 0.0209(5) Uani 1 1 d . . .
H4 H 0.6579 -0.1337 0.1095 0.025 Uiso 1 1 calc R . .
C5 C 0.74962(14) -0.0286(2) 0.15788(11) 0.0186(5) Uani 1 1 d . . .
C6 C 0.72098(15) 0.1102(3) 0.13240(11) 0.0208(5) Uani 1 1 d . . .
C7 C 0.73940(18) 0.3565(3) 0.12725(14) 0.0305(6) Uani 1 1 d . . .
H7A H 0.7492 0.3638 0.0828 0.046 Uiso 1 1 calc R . .
H7B H 0.7720 0.4254 0.1502 0.046 Uiso 1 1 calc R . .
H7C H 0.6798 0.3696 0.1338 0.046 Uiso 1 1 calc R . .
C8 C 0.99000(14) 0.1737(2) 0.13277(11) 0.0176(5) Uani 1 1 d . . .
C9 C 0.97367(15) 0.2893(2) 0.09425(11) 0.0208(5) Uani 1 1 d . . .
H9 H 0.9896 0.3765 0.1085 0.025 Uiso 1 1 calc R . .
C10 C 0.93395(15) 0.2727(3) 0.03537(11) 0.0220(5) Uani 1 1 d . . .
H10 H 0.9231 0.3487 0.0095 0.026 Uiso 1 1 calc R . .
C11 C 0.90996(15) 0.1420(3) 0.01436(11) 0.0207(5) Uani 1 1 d . . .
H11 H 0.8826 0.1319 -0.0255 0.025 Uiso 1 1 calc R . .
C12 C 0.92595(14) 0.0275(2) 0.05138(11) 0.0180(5) Uani 1 1 d . . .
C13 C 0.89432(15) -0.1100(2) 0.02613(11) 0.0203(5) Uani 1 1 d . . .
C14 C 0.87066(17) -0.3532(3) 0.04135(12) 0.0257(5) Uani 1 1 d . . .
H14A H 0.8111 -0.3444 0.0292 0.039 Uiso 1 1 calc R . .
H14B H 0.8777 -0.4195 0.0749 0.039 Uiso 1 1 calc R . .
H14C H 0.9013 -0.3830 0.0055 0.039 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
Zr1 O5 2.1648(16) 2_755 ?
Zr1 O5 2.1648(16) . ?
Zr1 O2 2.1698(16) . ?
Zr1 O2 2.1699(16) 2_755 ?
Zr1 O1 2.2089(15) 2_755 ?
Zr1 O1 2.2089(15) . ?
Zr1 O4 2.2145(15) . ?
Zr1 O4 2.2145(15) 2_755 ?
O1 N1 1.359(2) . ?
O2 C1 1.293(3) . ?
O3 C6 1.234(3) . ?
O4 N3 1.358(2) . ?
O5 C8 1.289(3) . ?
O6 C13 1.226(3) . ?
O1W H1AW 0.8502 . ?
O1W H1BW 0.8501 . ?
O2W H2AW 0.8501 . ?
O2W H2BW 0.8500 . ?
N1 C1 1.366(3) . ?
N1 C5 1.374(3) . ?
N2 C6 1.328(3) . ?
N2 C7 1.450(3) . ?
N2 H2N 0.8600 . ?
N3 C8 1.370(3) . ?
N3 C12 1.372(3) . ?
N4 C13 1.336(3) . ?
N4 C14 1.455(3) . ?
N4 H4N 0.8600 . ?
C1 C2 1.400(3) . ?
C2 C3 1.374(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.513(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.404(3) . ?
C9 C10 1.372(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.392(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.376(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.514(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 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
O5 Zr1 O5 76.35(9) 2_755 . ?
O5 Zr1 O2 118.48(6) 2_755 . ?
O5 Zr1 O2 140.33(6) . . ?
O5 Zr1 O2 140.33(6) 2_755 2_755 ?
O5 Zr1 O2 118.48(6) . 2_755 ?
O2 Zr1 O2 75.08(9) . 2_755 ?
O5 Zr1 O1 79.63(6) 2_755 2_755 ?
O5 Zr1 O1 76.99(6) . 2_755 ?
O2 Zr1 O1 139.03(6) . 2_755 ?
O2 Zr1 O1 69.73(6) 2_755 2_755 ?
O5 Zr1 O1 76.99(6) 2_755 . ?
O5 Zr1 O1 79.63(6) . . ?
O2 Zr1 O1 69.73(6) . . ?
O2 Zr1 O1 139.03(6) 2_755 . ?
O1 Zr1 O1 150.14(8) 2_755 . ?
O5 Zr1 O4 140.07(6) 2_755 . ?
O5 Zr1 O4 69.79(6) . . ?
O2 Zr1 O4 78.89(6) . . ?
O2 Zr1 O4 76.56(6) 2_755 . ?
O1 Zr1 O4 111.63(6) 2_755 . ?
O1 Zr1 O4 76.68(6) . . ?
O5 Zr1 O4 69.79(6) 2_755 2_755 ?
O5 Zr1 O4 140.08(6) . 2_755 ?
O2 Zr1 O4 76.56(6) . 2_755 ?
O2 Zr1 O4 78.89(6) 2_755 2_755 ?
O1 Zr1 O4 76.68(6) 2_755 2_755 ?
O1 Zr1 O4 111.63(6) . 2_755 ?
O4 Zr1 O4 148.90(8) . 2_755 ?
N1 O1 Zr1 113.50(13) . . ?
C1 O2 Zr1 117.67(14) . . ?
N3 O4 Zr1 112.90(12) . . ?
C8 O5 Zr1 117.38(14) . . ?
H1AW O1W H1BW 109.5 . . ?
H2AW O2W H2BW 109.5 . . ?
O1 N1 C1 115.04(17) . . ?
O1 N1 C5 121.84(19) . . ?
C1 N1 C5 123.1(2) . . ?
C6 N2 C7 120.8(2) . . ?
C6 N2 H2N 119.6 . . ?
C7 N2 H2N 119.6 . . ?
O4 N3 C8 114.78(18) . . ?
O4 N3 C12 122.10(19) . . ?
C8 N3 C12 123.1(2) . . ?
C13 N4 C14 120.0(2) . . ?
C13 N4 H4N 120.0 . . ?
C14 N4 H4N 120.0 . . ?
O2 C1 N1 115.7(2) . . ?
O2 C1 C2 125.7(2) . . ?
N1 C1 C2 118.6(2) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 N1 117.6(2) . . ?
C4 C5 C6 118.5(2) . . ?
N1 C5 C6 123.9(2) . . ?
O3 C6 N2 123.3(2) . . ?
O3 C6 C5 117.7(2) . . ?
N2 C6 C5 119.0(2) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O5 C8 N3 115.9(2) . . ?
O5 C8 C9 125.5(2) . . ?
N3 C8 C9 118.6(2) . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.0(2) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 121.3(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
N3 C12 C11 117.5(2) . . ?
N3 C12 C13 124.5(2) . . ?
C11 C12 C13 117.9(2) . . ?
O6 C13 N4 123.4(2) . . ?
O6 C13 C12 117.8(2) . . ?
N4 C13 C12 118.8(2) . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H2BW O1W 0.85 2.19 3.011(3) 162.7 2
O1W H1BW O3 0.85 2.01 2.853(3) 168.7 3_455
O1W H1AW O2 0.85 2.13 2.927(2) 154.9 2_665

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.087
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_fg111b
_database_code_depnum_ccdc_archive 'CCDC 1508470'
_audit_update_record             
;
2016-10-05 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'tetrakis(3-Hydroxy-1-[3-(methylamino)-3-oxopropyl]-1H-pyridin-2-onate)-zirconium pentahydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H44 N8 O12 Zr, 5(H2 O)'
_chemical_formula_sum            'C36 H54 N8 O17 Zr'
_chemical_formula_weight         962.09

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.7979(11)
_cell_length_b                   14.9292(18)
_cell_length_c                   17.7180(19)
_cell_angle_alpha                106.292(6)
_cell_angle_beta                 93.813(6)
_cell_angle_gamma                103.366(6)
_cell_volume                     2151.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.22

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1004
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9755
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38302
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         26.30
_reflns_number_total             8678
_reflns_number_gt                6508
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0379P)²+2.1322P] 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         8678
_refine_ls_number_parameters     593
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.005
_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
Zr1 Zr 0.88973(4) 0.52772(2) 0.715920(16) 0.01669(9) Uani 1 1 d . . .
O1 O 0.9769(2) 0.68873(14) 0.73321(11) 0.0195(5) Uani 1 1 d . . .
O2 O 0.9781(2) 0.54604(14) 0.61086(11) 0.0209(5) Uani 1 1 d . . .
O3 O 0.8469(3) 1.04943(17) 0.78804(14) 0.0409(6) Uani 1 1 d . . .
O4 O 1.0113(2) 0.40953(14) 0.67554(11) 0.0193(4) Uani 1 1 d . . .
O5 O 1.1192(2) 0.57278(14) 0.78870(11) 0.0204(5) Uani 1 1 d . . .
O6 O 1.0702(3) 0.03880(16) 0.62873(15) 0.0397(6) Uani 1 1 d . . .
O7 O 0.8490(2) 0.42611(14) 0.79363(11) 0.0218(5) Uani 1 1 d . . .
O8 O 0.8143(2) 0.59941(14) 0.82435(12) 0.0231(5) Uani 1 1 d . . .
O9 O 0.5876(3) 0.25039(19) 0.97626(14) 0.0440(7) Uani 1 1 d . . .
O10 O 0.6894(2) 0.57991(14) 0.67457(12) 0.0218(5) Uani 1 1 d . . .
O11 O 0.7098(2) 0.40428(14) 0.64222(11) 0.0206(5) Uani 1 1 d . . .
O12 O 0.4966(3) 0.83360(17) 0.68482(15) 0.0426(6) Uani 1 1 d . . .
O1W O 0.3796(3) 0.12799(18) 0.69168(15) 0.0394(6) Uani 1 1 d D . .
O2W O 0.2060(3) 0.75236(18) 0.90265(15) 0.0426(7) Uani 1 1 d D . .
O3W O 0.9079(3) 0.79674(17) 0.90107(15) 0.0424(6) Uani 1 1 d GD . .
H3AW H 1.0056 0.7956 0.9107 0.064 Uiso 1 1 d GD . .
H3BW H 0.8559 0.7429 0.8658 0.064 Uiso 1 1 d GD . .
O4W O 0.3391(3) 0.79221(19) 0.37436(17) 0.0439(7) Uani 1 1 d D . .
O5W O 0.4335(4) 0.9863(2) 0.32152(19) 0.0560(8) Uani 1 1 d GD . .
H5AW H 0.3436 0.9609 0.2905 0.084 Uiso 1 1 d GD . .
H5BW H 0.4747 1.0435 0.3179 0.084 Uiso 1 1 d GD . .
N1 N 1.0554(3) 0.80198(17) 0.66877(14) 0.0204(6) Uani 1 1 d . . .
N2 N 0.8597(4) 0.9659(2) 0.87552(16) 0.0367(7) Uani 1 1 d . . .
H2 H 0.8657 0.9108 0.8828 0.044 Uiso 1 1 calc R . .
N3 N 1.2155(3) 0.34993(17) 0.70724(14) 0.0208(6) Uani 1 1 d . . .
N4 N 0.8356(4) 0.0622(2) 0.58971(16) 0.0352(7) Uani 1 1 d . . .
H4' H 0.7792 0.1044 0.5931 0.042 Uiso 1 1 calc R . .
N5 N 0.8203(3) 0.41963(18) 0.92016(14) 0.0252(6) Uani 1 1 d . . .
N6 N 0.4179(4) 0.1884(2) 0.86258(17) 0.0367(7) Uani 1 1 d . . .
H6 H 0.4062 0.1772 0.8108 0.044 Uiso 1 1 calc R . .
N7 N 0.4455(3) 0.53780(18) 0.60092(14) 0.0216(6) Uani 1 1 d . . .
N8 N 0.3941(4) 0.8305(2) 0.79749(17) 0.0385(7) Uani 1 1 d . . .
H8 H 0.3455 0.7939 0.8244 0.046 Uiso 1 1 calc R . .
C1 C 1.0167(3) 0.7095(2) 0.67143(17) 0.0179(6) Uani 1 1 d . . .
C2 C 1.0224(3) 0.6330(2) 0.60181(16) 0.0185(6) Uani 1 1 d . . .
C3 C 1.0728(4) 0.6545(2) 0.53575(17) 0.0209(7) Uani 1 1 d . . .
H3 H 1.0786 0.6045 0.4899 0.025 Uiso 1 1 calc R . .
C4 C 1.1157(4) 0.7519(2) 0.53710(18) 0.0236(7) Uani 1 1 d . . .
H4 H 1.1528 0.7677 0.4921 0.028 Uiso 1 1 calc R . .
C5 C 1.1047(4) 0.8232(2) 0.60151(18) 0.0254(7) Uani 1 1 d . . .
H5 H 1.1309 0.8883 0.6007 0.030 Uiso 1 1 calc R . .
C6 C 1.0385(4) 0.8802(2) 0.73761(18) 0.0240(7) Uani 1 1 d . . .
H6A H 1.1058 0.9427 0.7363 0.029 Uiso 1 1 calc R . .
H6B H 1.0748 0.8687 0.7873 0.029 Uiso 1 1 calc R . .
C7 C 0.8684(4) 0.8856(2) 0.73709(19) 0.0295(8) Uani 1 1 d . . .
H7A H 0.8030 0.8266 0.7455 0.035 Uiso 1 1 calc R . .
H7B H 0.8275 0.8890 0.6848 0.035 Uiso 1 1 calc R . .
C8 C 0.8566(4) 0.9743(2) 0.8022(2) 0.0314(8) Uani 1 1 d . . .
C9 C 0.8533(5) 1.0462(3) 0.9436(2) 0.0437(10) Uani 1 1 d . . .
H9A H 0.9409 1.1023 0.9477 0.066 Uiso 1 1 calc R . .
H9B H 0.8617 1.0274 0.9921 0.066 Uiso 1 1 calc R . .
H9C H 0.7529 1.0629 0.9367 0.066 Uiso 1 1 calc R . .
C10 C 1.1388(4) 0.4211(2) 0.71870(16) 0.0188(6) Uani 1 1 d . . .
C11 C 1.2056(3) 0.5098(2) 0.78188(17) 0.0189(6) Uani 1 1 d . . .
C12 C 1.3472(4) 0.5228(2) 0.82519(18) 0.0254(7) Uani 1 1 d . . .
H12 H 1.3950 0.5824 0.8652 0.031 Uiso 1 1 calc R . .
C13 C 1.4221(4) 0.4470(2) 0.80997(19) 0.0274(7) Uani 1 1 d . . .
H13 H 1.5203 0.4553 0.8404 0.033 Uiso 1 1 calc R . .
C14 C 1.3559(4) 0.3628(2) 0.75275(18) 0.0256(7) Uani 1 1 d . . .
H14 H 1.4068 0.3119 0.7438 0.031 Uiso 1 1 calc R . .
C15 C 1.1399(4) 0.2554(2) 0.64945(18) 0.0238(7) Uani 1 1 d . . .
H15A H 1.2216 0.2221 0.6304 0.029 Uiso 1 1 calc R . .
H15B H 1.0828 0.2643 0.6032 0.029 Uiso 1 1 calc R . .
C16 C 1.0248(4) 0.1936(2) 0.68698(19) 0.0272(7) Uani 1 1 d . . .
H16A H 1.0754 0.1963 0.7395 0.033 Uiso 1 1 calc R . .
H16B H 0.9305 0.2188 0.6949 0.033 Uiso 1 1 calc R . .
C17 C 0.9763(4) 0.0903(2) 0.6334(2) 0.0318(8) Uani 1 1 d . . .
C18 C 0.7699(5) -0.0361(3) 0.5360(2) 0.0493(11) Uani 1 1 d . . .
H18A H 0.8559 -0.0656 0.5201 0.074 Uiso 1 1 calc R . .
H18B H 0.7083 -0.0338 0.4887 0.074 Uiso 1 1 calc R . .
H18C H 0.7014 -0.0747 0.5632 0.074 Uiso 1 1 calc R . .
C19 C 0.8277(3) 0.4662(2) 0.86393(17) 0.0206(7) Uani 1 1 d . . .
C20 C 0.8077(4) 0.5623(2) 0.88411(18) 0.0237(7) Uani 1 1 d . . .
C21 C 0.7791(4) 0.6045(2) 0.95918(19) 0.0347(9) Uani 1 1 d . . .
H21 H 0.7637 0.6677 0.9733 0.042 Uiso 1 1 calc R . .
C22 C 0.7727(5) 0.5536(3) 1.0151(2) 0.0396(9) Uani 1 1 d . . .
H22 H 0.7537 0.5830 1.0673 0.048 Uiso 1 1 calc R . .
C23 C 0.7930(4) 0.4638(2) 0.99572(18) 0.0332(8) Uani 1 1 d . . .
H23 H 0.7885 0.4305 1.0343 0.040 Uiso 1 1 calc R . .
C24 C 0.8417(4) 0.3209(2) 0.89898(19) 0.0290(8) Uani 1 1 d . . .
H24A H 0.8734 0.3068 0.9482 0.035 Uiso 1 1 calc R . .
H24B H 0.9283 0.3177 0.8662 0.035 Uiso 1 1 calc R . .
C25 C 0.6938(4) 0.2440(2) 0.85355(19) 0.0308(8) Uani 1 1 d . . .
H25A H 0.6550 0.2624 0.8078 0.037 Uiso 1 1 calc R . .
H25B H 0.7216 0.1820 0.8323 0.037 Uiso 1 1 calc R . .
C26 C 0.5623(4) 0.2290(2) 0.9029(2) 0.0317(8) Uani 1 1 d . . .
C27 C 0.2787(5) 0.1616(3) 0.8992(2) 0.0483(10) Uani 1 1 d . . .
H27A H 0.3109 0.1638 0.9539 0.072 Uiso 1 1 calc R . .
H27B H 0.2174 0.0960 0.8689 0.072 Uiso 1 1 calc R . .
H27C H 0.2139 0.2070 0.8996 0.072 Uiso 1 1 calc R . .
C28 C 0.5736(3) 0.5149(2) 0.62971(16) 0.0189(6) Uani 1 1 d . . .
C29 C 0.5796(4) 0.4161(2) 0.60833(16) 0.0194(6) Uani 1 1 d . . .
C30 C 0.4579(4) 0.3467(2) 0.55799(17) 0.0225(7) Uani 1 1 d . . .
H30 H 0.4612 0.2809 0.5422 0.027 Uiso 1 1 calc R . .
C31 C 0.3269(4) 0.3736(2) 0.52969(17) 0.0243(7) Uani 1 1 d . . .
H31 H 0.2414 0.3255 0.4949 0.029 Uiso 1 1 calc R . .
C32 C 0.3216(4) 0.4670(2) 0.55145(18) 0.0254(7) Uani 1 1 d . . .
H32 H 0.2319 0.4838 0.5325 0.030 Uiso 1 1 calc R . .
C33 C 0.4470(4) 0.6409(2) 0.62164(18) 0.0244(7) Uani 1 1 d . . .
H33A H 0.3679 0.6493 0.5836 0.029 Uiso 1 1 calc R . .
H33B H 0.5521 0.6789 0.6167 0.029 Uiso 1 1 calc R . .
C34 C 0.4107(4) 0.6797(2) 0.70571(18) 0.0284(8) Uani 1 1 d . . .
H34A H 0.2999 0.6488 0.7089 0.034 Uiso 1 1 calc R . .
H34B H 0.4802 0.6638 0.7434 0.034 Uiso 1 1 calc R . .
C35 C 0.4360(4) 0.7879(2) 0.7281(2) 0.0304(8) Uani 1 1 d . . .
C36 C 0.4251(5) 0.9346(3) 0.8303(2) 0.0502(11) Uani 1 1 d . . .
H36A H 0.5392 0.9638 0.8390 0.075 Uiso 1 1 calc R . .
H36B H 0.3834 0.9504 0.8809 0.075 Uiso 1 1 calc R . .
H36C H 0.3737 0.9599 0.7931 0.075 Uiso 1 1 calc R . .
H1AW H 0.432(3) 0.0850(18) 0.684(2) 0.040(11) Uiso 1 1 d D . .
H2AW H 0.273(4) 0.752(3) 0.9396(18) 0.069(16) Uiso 1 1 d D . .
H4AW H 0.423(3) 0.805(3) 0.354(2) 0.051(13) Uiso 1 1 d D . .
H1BW H 0.2832(16) 0.096(2) 0.675(2) 0.055(14) Uiso 1 1 d D . .
H2BW H 0.178(6) 0.6966(17) 0.868(2) 0.10(2) Uiso 1 1 d D . .
H4BW H 0.311(5) 0.7312(10) 0.366(3) 0.10(2) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O2 2.127(2) . ?
Zr1 O8 2.149(2) . ?
Zr1 O11 2.153(2) . ?
Zr1 O5 2.175(2) . ?
Zr1 O10 2.243(2) . ?
Zr1 O4 2.244(2) . ?
Zr1 O1 2.2723(19) . ?
Zr1 O7 2.305(2) . ?
O1 C1 1.268(3) . ?
O2 C2 1.325(3) . ?
O3 C8 1.236(4) . ?
O4 C10 1.263(3) . ?
O5 C11 1.325(3) . ?
O6 C17 1.244(4) . ?
O7 C19 1.269(3) . ?
O8 C20 1.324(4) . ?
O9 C26 1.239(4) . ?
O10 C28 1.270(3) . ?
O11 C29 1.329(4) . ?
O12 C35 1.231(4) . ?
N1 C1 1.358(4) . ?
N1 C5 1.387(4) . ?
N1 C6 1.476(4) . ?
N2 C8 1.338(4) . ?
N2 C9 1.457(4) . ?
N3 C10 1.362(4) . ?
N3 C14 1.373(4) . ?
N3 C15 1.465(4) . ?
N4 C17 1.326(4) . ?
N4 C18 1.464(4) . ?
N5 C19 1.363(4) . ?
N5 C23 1.380(4) . ?
N5 C24 1.475(4) . ?
N6 C26 1.332(4) . ?
N6 C27 1.451(5) . ?
N7 C28 1.359(4) . ?
N7 C32 1.377(4) . ?
N7 C33 1.475(4) . ?
N8 C35 1.336(4) . ?
N8 C36 1.450(5) . ?
C1 C2 1.440(4) . ?
C2 C3 1.372(4) . ?
C3 C4 1.408(4) . ?
C4 C5 1.351(4) . ?
C6 C7 1.517(4) . ?
C7 C8 1.521(4) . ?
C10 C11 1.439(4) . ?
C11 C12 1.363(4) . ?
C12 C13 1.409(4) . ?
C13 C14 1.347(4) . ?
C15 C16 1.524(4) . ?
C16 C17 1.510(4) . ?
C19 C20 1.433(4) . ?
C20 C21 1.370(4) . ?
C21 C22 1.404(5) . ?
C22 C23 1.345(5) . ?
C24 C25 1.521(5) . ?
C25 C26 1.509(5) . ?
C28 C29 1.430(4) . ?
C29 C30 1.363(4) . ?
C30 C31 1.411(4) . ?
C31 C32 1.351(4) . ?
C33 C34 1.524(4) . ?
C34 C35 1.509(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zr1 O8 144.44(8) . . ?
O2 Zr1 O11 88.29(8) . . ?
O8 Zr1 O11 112.79(8) . . ?
O2 Zr1 O5 95.70(8) . . ?
O8 Zr1 O5 83.72(8) . . ?
O11 Zr1 O5 144.04(8) . . ?
O2 Zr1 O10 84.46(8) . . ?
O8 Zr1 O10 76.28(8) . . ?
O11 Zr1 O10 71.63(7) . . ?
O5 Zr1 O10 144.29(7) . . ?
O2 Zr1 O4 75.03(7) . . ?
O8 Zr1 O4 136.69(7) . . ?
O11 Zr1 O4 74.33(7) . . ?
O5 Zr1 O4 72.30(7) . . ?
O10 Zr1 O4 140.50(7) . . ?
O2 Zr1 O1 71.75(7) . . ?
O8 Zr1 O1 73.84(7) . . ?
O11 Zr1 O1 139.15(7) . . ?
O5 Zr1 O1 74.92(7) . . ?
O10 Zr1 O1 71.26(7) . . ?
O4 Zr1 O1 129.94(7) . . ?
O2 Zr1 O7 144.18(7) . . ?
O8 Zr1 O7 70.83(7) . . ?
O11 Zr1 O7 76.87(7) . . ?
O5 Zr1 O7 79.31(7) . . ?
O10 Zr1 O7 119.95(8) . . ?
O4 Zr1 O7 69.64(7) . . ?
O1 Zr1 O7 138.01(7) . . ?
C1 O1 Zr1 114.39(17) . . ?
C2 O2 Zr1 120.87(17) . . ?
C10 O4 Zr1 114.48(17) . . ?
C11 O5 Zr1 118.62(17) . . ?
C19 O7 Zr1 114.31(18) . . ?
C20 O8 Zr1 120.47(18) . . ?
C28 O10 Zr1 115.81(18) . . ?
C29 O11 Zr1 120.23(17) . . ?
C1 N1 C5 121.0(3) . . ?
C1 N1 C6 119.1(2) . . ?
C5 N1 C6 119.8(2) . . ?
C8 N2 C9 121.4(3) . . ?
C10 N3 C14 121.3(3) . . ?
C10 N3 C15 119.0(3) . . ?
C14 N3 C15 119.5(3) . . ?
C17 N4 C18 122.9(3) . . ?
C19 N5 C23 120.7(3) . . ?
C19 N5 C24 118.9(2) . . ?
C23 N5 C24 120.4(3) . . ?
C26 N6 C27 123.7(3) . . ?
C28 N7 C32 120.7(3) . . ?
C28 N7 C33 117.9(2) . . ?
C32 N7 C33 121.4(3) . . ?
C35 N8 C36 122.7(3) . . ?
O1 C1 N1 122.2(3) . . ?
O1 C1 C2 119.2(3) . . ?
N1 C1 C2 118.6(3) . . ?
O2 C2 C3 126.9(3) . . ?
O2 C2 C1 113.1(2) . . ?
C3 C2 C1 120.0(3) . . ?
C2 C3 C4 118.9(3) . . ?
C5 C4 C3 120.9(3) . . ?
C4 C5 N1 120.5(3) . . ?
N1 C6 C7 111.2(2) . . ?
C6 C7 C8 110.4(3) . . ?
O3 C8 N2 122.4(3) . . ?
O3 C8 C7 121.8(3) . . ?
N2 C8 C7 115.8(3) . . ?
O4 C10 N3 121.0(3) . . ?
O4 C10 C11 120.6(3) . . ?
N3 C10 C11 118.4(3) . . ?
O5 C11 C12 127.1(3) . . ?
O5 C11 C10 113.2(3) . . ?
C12 C11 C10 119.7(3) . . ?
C11 C12 C13 119.2(3) . . ?
C14 C13 C12 120.7(3) . . ?
C13 C14 N3 120.6(3) . . ?
N3 C15 C16 110.5(2) . . ?
C17 C16 C15 109.5(3) . . ?
O6 C17 N4 123.7(3) . . ?
O6 C17 C16 120.0(3) . . ?
N4 C17 C16 116.1(3) . . ?
O7 C19 N5 121.7(3) . . ?
O7 C19 C20 119.0(3) . . ?
N5 C19 C20 119.3(3) . . ?
O8 C20 C21 127.0(3) . . ?
O8 C20 C19 113.8(3) . . ?
C21 C20 C19 119.1(3) . . ?
C20 C21 C22 119.5(3) . . ?
C23 C22 C21 120.8(3) . . ?
C22 C23 N5 120.5(3) . . ?
N5 C24 C25 113.1(3) . . ?
C26 C25 C24 113.9(3) . . ?
O9 C26 N6 122.0(3) . . ?
O9 C26 C25 122.2(3) . . ?
N6 C26 C25 115.8(3) . . ?
O10 C28 N7 121.1(3) . . ?
O10 C28 C29 119.3(3) . . ?
N7 C28 C29 119.6(3) . . ?
O11 C29 C30 127.7(3) . . ?
O11 C29 C28 113.0(3) . . ?
C30 C29 C28 119.3(3) . . ?
C29 C30 C31 119.2(3) . . ?
C32 C31 C30 120.9(3) . . ?
C31 C32 N7 120.3(3) . . ?
N7 C33 C34 112.2(2) . . ?
C35 C34 C33 110.1(3) . . ?
O12 C35 N8 122.6(3) . . ?
O12 C35 C34 120.8(3) . . ?
N8 C35 C34 116.6(3) . . ?

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 H1AW O5W 0.860(10) 1.755(11) 2.607(4) 170(3) 2_666
O1W H1BW O6 0.858(10) 1.891(12) 2.741(4) 171(4) 1_455
O5W H5BW O12 0.87 1.81 2.653(4) 163.3 2_676
O5W H5AW O3 0.87 2.05 2.883(4) 158.9 2_676
O4W H4AW O1W 0.850(10) 2.123(13) 2.953(4) 165(3) 2_666
O4W H4BW O11 0.854(10) 1.950(15) 2.792(3) 168(5) 2_666
O3W H3AW O2W 0.87 2.01 2.850(4) 160.9 1_655
O2W H2AW O9 0.853(10) 1.881(11) 2.733(4) 177(5) 2_667
O2W H2BW O5 0.851(10) 1.917(11) 2.767(3) 178(5) 1_455
N4 H4' O4W 0.88 2.03 2.897(4) 168.1 2_666
N6 H6 O1W 0.88 2.01 2.879(4) 170.1 .
O3W H3BW O8 0.87 2.00 2.773(3) 148.2 .
N2 H2 O3W 0.88 1.93 2.806(4) 172.6 .
N8 H8 O2W 0.88 2.04 2.883(4) 159.4 .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.30
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.080
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethyl Acetate/Methanol 50:50'
