# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2113958'
loop_
_audit_author_name
_audit_author_address
'Charalampos Moiras'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-12-17 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H19.60 N6 O6 Zr, C H4 O, 2(Cl), H2 O '
_chemical_formula_sum            'C11 H25.60 Cl2 N6 O8 Zr'
_chemical_formula_weight         532.09

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.9010(6)
_cell_length_b                   14.1221(5)
_cell_length_c                   17.6833(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3970.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    174(2)
_cell_measurement_reflns_used    5016
_cell_measurement_theta_min      2.6330
_cell_measurement_theta_max      30.5160

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_F_000             2173
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.876
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      174(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            17472
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.562
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_full        24.499
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3310
_reflns_number_gt                2573
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0376P)²+2.9682P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3310
_refine_ls_number_parameters     296
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0733
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.120
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2053(2) 0.5632(2) 0.2614(2) 0.0187(8) Uani 1 1 d . . . A 1
C5 C 0.3831(2) 0.2182(2) 0.4160(2) 0.0226(8) Uani 1 1 d . . . A 1
C6 C 0.3903(3) 0.1348(3) 0.4673(2) 0.0344(10) Uani 1 1 d . . . A 1
H6A H 0.450408 0.120958 0.476881 0.041 Uiso 1 1 calc R U . A 1
H6B H 0.364984 0.078660 0.442659 0.041 Uiso 1 1 calc R U . A 1
C7 C 0.3467(3) 0.1533(4) 0.5408(3) 0.0375(13) Uani 0.8 1 d . . P A 1
H7A H 0.341804 0.093017 0.569080 0.045 Uiso 0.8 1 calc R U P A 1
H7B H 0.381377 0.197106 0.571371 0.045 Uiso 0.8 1 calc R U P A 1
C8 C 0.2612(3) 0.1948(3) 0.5311(3) 0.0422(11) Uani 1 1 d . . . A 1
H8A H 0.239761 0.216651 0.580701 0.051 Uiso 1 1 calc R U . A 1
H8B H 0.222278 0.145797 0.511656 0.051 Uiso 1 1 calc R U . A 1
C9 C 0.2639(2) 0.2762(3) 0.4773(2) 0.0308(9) Uani 1 1 d . . . A 1
C15 C 0.1455(2) 0.6085(3) 0.2071(2) 0.0301(9) Uani 1 1 d . . . A 1
H15A H 0.167192 0.671310 0.191642 0.036 Uiso 1 1 calc R U . A 1
H15B H 0.090174 0.617837 0.231800 0.036 Uiso 1 1 calc R U . A 1
C16 C 0.1355(3) 0.5453(3) 0.1379(2) 0.0358(10) Uani 1 1 d . . . A 1
H16A H 0.189233 0.542155 0.109807 0.043 Uiso 1 1 calc R U . A 1
H16B H 0.092011 0.571749 0.103887 0.043 Uiso 1 1 calc R U . A 1
C17 C 0.1096(2) 0.4457(3) 0.1638(2) 0.0283(9) Uani 1 1 d . . . A 1
H17A H 0.052875 0.447754 0.186766 0.034 Uiso 1 1 calc R U . A 1
H17B H 0.107831 0.402402 0.119818 0.034 Uiso 1 1 calc R U . A 1
C18 C 0.1714(2) 0.4109(3) 0.2199(2) 0.0208(8) Uani 1 1 d . . . A 1
Cl1 Cl 0.61854(5) 0.13712(6) 0.35665(5) 0.0228(2) Uani 1 1 d . . . B 1
Cl2 Cl 0.53704(6) 0.34259(7) 0.51142(6) 0.0309(2) Uani 1 1 d . . . C 1
N1 N 0.2130(2) 0.3474(2) 0.4807(2) 0.0387(9) Uani 1 1 d . . . A 1
H1 H 0.171055 0.348254 0.513177 0.046 Uiso 1 1 calc R U . A 1
N2 N 0.43475(18) 0.2364(2) 0.36209(17) 0.0225(7) Uani 1 1 d . . . A 1
H2 H 0.477347 0.198247 0.353150 0.027 Uiso 1 1 calc R U . A 1
N3 N 0.32069(18) 0.2833(2) 0.42156(17) 0.0236(7) Uani 1 1 d . . . A 1
N4 N 0.25275(18) 0.61010(19) 0.30675(16) 0.0201(7) Uani 1 1 d . . . A 1
H4 H 0.250741 0.672366 0.307470 0.024 Uiso 1 1 calc R U . A 1
N5 N 0.21535(18) 0.4682(2) 0.26659(17) 0.0208(7) Uani 1 1 d . . . A 1
N6 N 0.19051(18) 0.3224(2) 0.22808(17) 0.0241(7) Uani 1 1 d . . . A 1
H6 H 0.166454 0.278590 0.200108 0.029 Uiso 1 1 calc R U . A 1
O29 O 0.5439(2) 0.1904(2) 0.18409(19) 0.0495(8) Uani 1 1 d D . . D 1
O2 O 0.2261(3) 0.4214(3) 0.4324(2) 0.0294(10) Uani 0.8 1 d . . P A 1
O11 O 0.42320(15) 0.31515(17) 0.31879(14) 0.0229(6) Uani 1 1 d . . . A 1
O21 O 0.30591(15) 0.56312(17) 0.35347(14) 0.0251(6) Uani 1 1 d . . . A 1
O23 O 0.24922(16) 0.29900(16) 0.28151(15) 0.0272(6) Uani 1 1 d . . . A 1
O24 O 0.41111(18) 0.46298(18) 0.42479(16) 0.0337(7) Uani 1 1 d D . . A 1
O25 O 0.39004(18) 0.45651(19) 0.24276(16) 0.0328(7) Uani 1 1 d D . . A 1
Zr1 Zr 0.31688(2) 0.40896(2) 0.34318(2) 0.01840(11) Uani 1 1 d D . . A 1
O2B O 0.2016(10) 0.4044(13) 0.4135(10) 0.019(5) Uiso 0.2 1 d . . P E 2
C7B C 0.3117(12) 0.1156(13) 0.5092(11) 0.020(4) Uiso 0.2 1 d . . P F 2
O28B O 0.5139(5) 0.3752(5) 0.1799(3) 0.0675(17) Uani 0.7 1 d D . P G 2
H28B H 0.524971 0.317067 0.182079 0.101 Uiso 0.7 1 calc R U P G 2
C28B C 0.5345(5) 0.4090(6) 0.1102(5) 0.054(2) Uani 0.7 1 d D . P G 2
H28A H 0.494962 0.458991 0.095824 0.081 Uiso 0.7 1 calc R U P G 2
H28C H 0.531789 0.357398 0.073219 0.081 Uiso 0.7 1 calc R U P G 2
H28D H 0.591728 0.434793 0.111494 0.081 Uiso 0.7 1 calc R U P G 2
C28 C 0.5485(11) 0.3899(18) 0.1402(16) 0.054(7) Uiso 0.3 1 d D . P H 3
H28E H 0.546166 0.458858 0.146082 0.081 Uiso 0.3 1 calc R U P H 3
H28F H 0.566449 0.374303 0.088656 0.081 Uiso 0.3 1 calc R U P H 3
H28G H 0.588637 0.363444 0.176502 0.081 Uiso 0.3 1 calc R U P H 3
O28 O 0.4680(7) 0.3512(9) 0.1536(7) 0.044(3) Uani 0.3 1 d D . P H 3
H28 H 0.472333 0.292670 0.161148 0.065 Uiso 0.3 1 calc R U P H 3
H24A H 0.445(2) 0.431(2) 0.452(2) 0.065 Uiso 1 1 d D U . I 1
H24B H 0.418(3) 0.5214(16) 0.439(2) 0.065 Uiso 1 1 d D U . J 1
H25A H 0.427(3) 0.425(2) 0.218(2) 0.065 Uiso 1 1 d D U . K 1
H25B H 0.384(3) 0.508(2) 0.218(2) 0.065 Uiso 1 1 d D U . L 1
H29B H 0.581(2) 0.158(3) 0.211(2) 0.065 Uiso 1 1 d D U . . .
H29A H 0.546(3) 0.168(3) 0.1369(14) 0.065 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N4 1.285(4) . ?
C1 N5 1.353(4) . ?
C1 C15 1.496(5) . ?
C5 N2 1.285(5) . ?
C5 N3 1.356(4) . ?
C5 C6 1.492(5) . ?
C6 C7 1.496(7) . ?
C7 C8 1.490(7) . ?
C8 C9 1.493(5) . ?
C9 N1 1.293(5) . ?
C9 N3 1.341(5) . ?
C15 C16 1.523(6) . ?
C16 C17 1.535(5) . ?
C17 C18 1.480(5) . ?
C18 N6 1.293(4) . ?
C18 N5 1.352(4) . ?
N1 O2 1.365(5) . ?
N2 O11 1.362(4) . ?
N3 Zr1 2.252(3) . ?
N4 O21 1.355(4) . ?
N5 Zr1 2.267(3) . ?
N6 O23 1.369(4) . ?
O2 Zr1 2.146(4) . ?
O11 Zr1 2.191(2) . ?
O21 Zr1 2.192(2) . ?
O23 Zr1 2.181(2) . ?
O24 Zr1 2.216(3) . ?
O25 Zr1 2.227(3) . ?
O28B C28B 1.361(9) . ?
C28 O28 1.412(17) . ?

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
N4 C1 N5 113.6(3) . . ?
N4 C1 C15 123.6(3) . . ?
N5 C1 C15 122.9(3) . . ?
N2 C5 N3 112.7(3) . . ?
N2 C5 C6 124.1(3) . . ?
N3 C5 C6 123.2(3) . . ?
C5 C6 C7 110.8(4) . . ?
C8 C7 C6 113.1(4) . . ?
C7 C8 C9 110.5(4) . . ?
N1 C9 N3 113.4(3) . . ?
N1 C9 C8 123.5(4) . . ?
N3 C9 C8 123.1(3) . . ?
C1 C15 C16 109.3(3) . . ?
C15 C16 C17 109.0(3) . . ?
C18 C17 C16 109.1(3) . . ?
N6 C18 N5 112.9(3) . . ?
N6 C18 C17 123.5(3) . . ?
N5 C18 C17 123.6(3) . . ?
C9 N1 O2 118.1(4) . . ?
C5 N2 O11 119.6(3) . . ?
C9 N3 C5 119.7(3) . . ?
C9 N3 Zr1 119.6(2) . . ?
C5 N3 Zr1 120.6(2) . . ?
C1 N4 O21 119.6(3) . . ?
C18 N5 C1 119.4(3) . . ?
C18 N5 Zr1 120.8(2) . . ?
C1 N5 Zr1 119.3(2) . . ?
C18 N6 O23 118.1(3) . . ?
N1 O2 Zr1 120.0(3) . . ?
N2 O11 Zr1 119.14(19) . . ?
N4 O21 Zr1 119.03(19) . . ?
N6 O23 Zr1 120.62(18) . . ?
O2 Zr1 O23 95.38(15) . . ?
O2 Zr1 O11 135.52(12) . . ?
O23 Zr1 O11 81.47(9) . . ?
O2 Zr1 O21 78.71(13) . . ?
O23 Zr1 O21 135.19(9) . . ?
O11 Zr1 O21 132.72(9) . . ?
O2 Zr1 O24 87.03(15) . . ?
O23 Zr1 O24 154.72(9) . . ?
O11 Zr1 O24 79.32(10) . . ?
O21 Zr1 O24 69.98(9) . . ?
O2 Zr1 O25 155.96(12) . . ?
O23 Zr1 O25 94.23(11) . . ?
O11 Zr1 O25 67.80(9) . . ?
O21 Zr1 O25 78.94(10) . . ?
O24 Zr1 O25 93.57(11) . . ?
O2 Zr1 N3 68.29(13) . . ?
O23 Zr1 N3 76.12(10) . . ?
O11 Zr1 N3 67.92(10) . . ?
O21 Zr1 N3 137.19(10) . . ?
O24 Zr1 N3 81.50(10) . . ?
O25 Zr1 N3 135.59(10) . . ?
O2 Zr1 N5 85.97(14) . . ?
O23 Zr1 N5 67.23(9) . . ?
O11 Zr1 N5 130.93(10) . . ?
O21 Zr1 N5 68.05(10) . . ?
O24 Zr1 N5 138.02(10) . . ?
O25 Zr1 N5 77.54(10) . . ?
N3 Zr1 N5 132.65(11) . . ?

_refine_diff_density_max         0.524
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.081


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol'
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2113960'
loop_
_audit_author_name
_audit_author_address
'Charalampos Moiras'
;University of Glasgow
United Kingdom
;
_audit_update_record             
;
2021-12-20 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_shelx               
;
PROBLEM: Atom C32             has ADP max/min Ratio .....        4.2 prolat
RESPONSE: The relevant atom is disordered, and it is observed as the unordinary displacement parameters
;
_vrf_PLAT220_shelx               
;
PROBLEM: NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        6.2 Ratio
RESPONSE: These alerts are generated because there is a large amount of disorder in the solvent area and does not allow better thermal parameters to be obtained. The identity of the atom has been verified by other analytical techniques.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O26 Check
RESPONSE: The severely disordered solvent atoms does not allow reasonable assignment of hydrogen atoms.
;
_vrf_PLAT306_shelx_2             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O31 Check
RESPONSE: The severely disordered solvent atoms does not allow reasonable assignment of hydrogen atoms.
;
_vrf_PLAT306_shelx_3             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O35 Check
RESPONSE: The severely disordered solvent atoms does not allow reasonable assignment of hydrogen atoms.
;
_vrf_PLAT306_shelx_4             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O37 Check
RESPONSE: The severely disordered solvent atoms does not allow reasonable assignment of hydrogen atoms.
;
_vrf_PLAT306_shelx_5             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O38 Check
RESPONSE: The severely disordered solvent atoms does not allow reasonable assignment of hydrogen atoms.
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor  O40      --H40      .     Please Check
RESPONSE: no available acceptors could be found at an acceptable distance from the water hydrogens
;
# Added during the CSD deposition process: Monday 20 December 2021 04:01 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C42.93 H56 Cl1.20 K3.20 N24 O28.97 Zr5), 9(Cl0.10), 8(O0.50),'
_chemical_formula_sum            'C85.85 H112 Cl9.60 K8.60 N48 O69.94 Zr10'
_chemical_formula_weight         4524.33

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'
K K 0.2009 0.2494 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.456(4)
_cell_length_b                   40.268(10)
_cell_length_c                   14.682(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.042(4)
_cell_angle_gamma                90
_cell_volume                     8545(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5303
_cell_measurement_theta_min      2.205
_cell_measurement_theta_max      26.266

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_F_000             4499
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.042
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6850
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63187
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.477
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16786
_reflns_number_gt                10689
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  WinGX'
_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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0486P)²+47.5533P] 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         16786
_refine_ls_number_parameters     1150
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1508
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4293(4) 0.42252(17) 0.5396(4) 0.0162(15) Uani 1 1 d . . . A 1
C2 C 0.4732(5) 0.45477(19) 0.5114(5) 0.0261(17) Uani 1 1 d . . . A 1
H2A H 0.526428 0.459841 0.552353 0.031 Uiso 1 1 calc R U . A 1
H2B H 0.427719 0.473044 0.516248 0.031 Uiso 1 1 calc R U . A 1
C3 C 0.5059(5) 0.4521(2) 0.4130(5) 0.034(2) Uani 1 1 d . . . A 1
H3A H 0.451700 0.450414 0.371104 0.041 Uiso 1 1 calc R U . A 1
H3B H 0.541029 0.472314 0.396931 0.041 Uiso 1 1 calc R U . A 1
C4 C 0.5668(5) 0.4218(2) 0.4026(5) 0.037(2) Uani 1 1 d . . . A 1
H4A H 0.580800 0.418492 0.337480 0.044 Uiso 1 1 calc R U . A 1
H4B H 0.625916 0.425209 0.436355 0.044 Uiso 1 1 calc R U . A 1
C5 C 0.5188(5) 0.3918(2) 0.4386(5) 0.0268(18) Uani 1 1 d . . . A 1
C6 C 0.2648(5) 0.30744(19) 0.4051(5) 0.0232(17) Uani 1 1 d . . . A 1
C7 C 0.2244(7) 0.2804(2) 0.3459(7) 0.052(3) Uani 1 1 d . . . A 1
H7A H 0.162172 0.287157 0.323347 0.063 Uiso 1 1 calc R U . A 1
H7B H 0.264119 0.276868 0.292592 0.063 Uiso 1 1 calc R U . A 1
C8 C 0.2177(9) 0.2507(3) 0.3964(8) 0.036(3) Uani 0.7 1 d . . P A 1
H8A H 0.199832 0.232482 0.354184 0.043 Uiso 0.7 1 calc R U P A 1
H8B H 0.167589 0.253122 0.440930 0.043 Uiso 0.7 1 calc R U P A 1
C9 C 0.3085(5) 0.24037(19) 0.4488(6) 0.0299(19) Uani 1 1 d . . . A 1
H9A H 0.294463 0.223239 0.494857 0.036 Uiso 1 1 calc R U . A 1
H9B H 0.353290 0.230911 0.405639 0.036 Uiso 1 1 calc R U . A 1
C10 C 0.3494(5) 0.27033(18) 0.4945(5) 0.0201(16) Uani 1 1 d . . . A 1
C11 C -0.0747(5) 0.38006(18) 0.4265(4) 0.0196(15) Uani 1 1 d . . . A 1
C12 C -0.1182(6) 0.35286(19) 0.3717(6) 0.033(2) Uani 1 1 d . . . A 1
H12A H -0.084816 0.350067 0.313966 0.040 Uiso 1 1 calc R U . A 1
H12B H -0.183307 0.358646 0.356677 0.040 Uiso 1 1 calc R U . A 1
C13 C -0.1150(6) 0.3208(2) 0.4254(6) 0.035(2) Uani 1 1 d . . . A 1
H13A H -0.135861 0.302218 0.385736 0.043 Uiso 1 1 calc R U . A 1
H13B H -0.157798 0.322277 0.477060 0.043 Uiso 1 1 calc R U . A 1
C14 C -0.0176(5) 0.31362(18) 0.4614(5) 0.0281(18) Uani 1 1 d . . . A 1
H14A H -0.018685 0.294367 0.503347 0.034 Uiso 1 1 calc R U . A 1
H14B H 0.023257 0.308078 0.410183 0.034 Uiso 1 1 calc R U . A 1
C15 C 0.0190(5) 0.34344(17) 0.5107(4) 0.0180(15) Uani 1 1 d . . . A 1
C16 C -0.0832(5) 0.45409(17) 0.7041(4) 0.0160(15) Uani 1 1 d . . . A 1
C17 C -0.1344(4) 0.48075(17) 0.7526(4) 0.0178(15) Uani 1 1 d . . . A 1
H17A H -0.159669 0.471993 0.810083 0.021 Uiso 1 1 calc R U . A 1
H17B H -0.186575 0.488880 0.714082 0.021 Uiso 1 1 calc R U . A 1
C18 C -0.0670(5) 0.50888(18) 0.7728(5) 0.0229(16) Uani 1 1 d . . . A 1
H18A H -0.017310 0.500952 0.814718 0.027 Uiso 1 1 calc R U . A 1
H18B H -0.099752 0.527337 0.802982 0.027 Uiso 1 1 calc R U . A 1
C19 C -0.0248(5) 0.52126(17) 0.6843(4) 0.0181(15) Uani 1 1 d . . . A 1
H19A H -0.072675 0.532669 0.646761 0.022 Uiso 1 1 calc R U . A 1
H19B H 0.025268 0.537349 0.698284 0.022 Uiso 1 1 calc R U . A 1
C20 C 0.0135(5) 0.49226(16) 0.6324(4) 0.0155(15) Uani 1 1 d . . . A 1
C21 C 0.4396(5) 0.48616(18) 0.8757(5) 0.0203(16) Uani 1 1 d . . . A 1
C22 C 0.4788(5) 0.51829(18) 0.8439(5) 0.0268(17) Uani 1 1 d . . . A 1
H22A H 0.477581 0.534753 0.893949 0.032 Uiso 1 1 calc R U . A 1
H22B H 0.440831 0.526986 0.792452 0.032 Uiso 1 1 calc R U . A 1
C23 C 0.5773(5) 0.51324(19) 0.8138(5) 0.0278(18) Uani 1 1 d . . . A 1
H23A H 0.617586 0.508866 0.867729 0.033 Uiso 1 1 calc R U . A 1
H23B H 0.599619 0.533710 0.783993 0.033 Uiso 1 1 calc R U . A 1
C24 C 0.5833(5) 0.48417(18) 0.7475(5) 0.0233(17) Uani 1 1 d . . . A 1
H24A H 0.556392 0.490869 0.687834 0.028 Uiso 1 1 calc R U . A 1
H24B H 0.649155 0.478485 0.738466 0.028 Uiso 1 1 calc R U . A 1
C25 C 0.5336(4) 0.45437(18) 0.7813(4) 0.0179(15) Uani 1 1 d . . . A 1
C26 C 0.4310(4) 0.33051(18) 0.9064(5) 0.0189(15) Uani 1 1 d . . . A 1
C27 C 0.4697(5) 0.29781(19) 0.9378(5) 0.0266(18) Uani 1 1 d . . . A 1
H27A H 0.471408 0.282088 0.886047 0.032 Uiso 1 1 calc R U . A 1
H27B H 0.429869 0.288224 0.985266 0.032 Uiso 1 1 calc R U . A 1
C28 C 0.5681(7) 0.3033(3) 0.9767(7) 0.028(3) Uani 0.7 1 d . . P A 1
H28A H 0.589869 0.282544 1.006387 0.034 Uiso 0.7 1 calc R U P A 1
H28B H 0.610216 0.308248 0.926070 0.034 Uiso 0.7 1 calc R U P A 1
C29 C 0.5725(6) 0.3301(2) 1.0423(6) 0.053(3) Uani 1 1 d . . . A 1
H29A H 0.638099 0.335132 1.057181 0.063 Uiso 1 1 calc R U . A 1
H29B H 0.542326 0.323039 1.099041 0.063 Uiso 1 1 calc R U . A 1
C30 C 0.5268(5) 0.3605(2) 1.0075(5) 0.0314(19) Uani 1 1 d . . . A 1
C31 C 0.1000(5) 0.2599(2) 0.9163(6) 0.033(2) Uani 1 1 d . . . A 1
C32 C 0.1403(6) 0.2284(2) 0.9589(8) 0.056(3) Uani 1 1 d D U . A 1
H32A H 0.150982 0.211631 0.911002 0.068 Uiso 1 1 calc R U . A 1
H32B H 0.096319 0.219071 1.002969 0.068 Uiso 1 1 calc R U . A 1
C34 C 0.2317(6) 0.2654(3) 1.0646(8) 0.060(3) Uani 1 1 d D . . A 1
H34A H 0.295805 0.270844 1.084149 0.072 Uiso 1 1 calc R U . A 1
H34B H 0.195185 0.260855 1.119678 0.072 Uiso 1 1 calc R U . A 1
C35 C 0.1901(5) 0.2939(2) 1.0126(6) 0.040(2) Uani 1 1 d . . . A 1
C37 C -0.1103(5) 0.40388(19) 1.0654(5) 0.0239(17) Uani 1 1 d . . . A 1
H37A H -0.121269 0.396808 1.128852 0.029 Uiso 1 1 calc R U . A 1
H37B H -0.170859 0.409295 1.036418 0.029 Uiso 1 1 calc R U . A 1
C38 C -0.0478(5) 0.43462(18) 1.0652(5) 0.0241(17) Uani 1 1 d . . . A 1
H38A H -0.081416 0.453817 1.090672 0.029 Uiso 1 1 calc R U . A 1
H38B H 0.007760 0.430510 1.103959 0.029 Uiso 1 1 calc R U . A 1
C39 C -0.0191(5) 0.44236(18) 0.9693(5) 0.0241(17) Uani 1 1 d . . . A 1
H39A H -0.073682 0.449672 0.932900 0.029 Uiso 1 1 calc R U . A 1
H39B H 0.026571 0.460683 0.970306 0.029 Uiso 1 1 calc R U . A 1
C40 C 0.0224(4) 0.41244(17) 0.9263(4) 0.0160(15) Uani 1 1 d . . . A 1
Cl5 Cl 0.73323(14) 0.47634(5) 0.53300(14) 0.0343(5) Uani 1 1 d . U . B 1
Cl1 Cl 0.16230(12) 0.27203(4) 0.63852(12) 0.0226(4) Uani 1 1 d . U . C 1
K3 K 0.2877(2) 0.54300(8) 1.04107(17) 0.0515(7) Uani 0.85 1 d . . P A 1
K4 K -0.19491(19) 0.30442(8) 0.7006(2) 0.0492(9) Uani 0.7 1 d . . P D 1
Cl4 Cl 0.8245(2) 0.51905(9) 1.1874(3) 0.0603(10) Uani 0.75 1 d . U P E 1
K10 K 0.7908(2) 0.45267(10) 1.2641(2) 0.0220(8) Uani 0.5 1 d . . P E 1
Cl2 Cl 0.6629(2) 0.32960(8) 1.27059(19) 0.0354(7) Uani 0.65 1 d . U P F 2
K7 K -0.00162(16) 0.27073(6) 1.22796(16) 0.0609(7) Uani 1 1 d . . . G 1
Cl3 Cl 0.3473(7) 0.3409(3) 1.1684(7) 0.100(4) Uani 0.4 1 d . U P H 1
K9 K 0.2236(3) 0.42869(10) 1.1700(3) 0.0576(10) Uani 0.6 1 d . . P A 1
N2 N -0.0081(4) 0.37449(13) 0.4926(3) 0.0148(12) Uani 1 1 d . . . A 1
N3 N -0.0974(4) 0.41119(15) 0.4168(4) 0.0212(13) Uani 1 1 d . . . A 1
N4 N 0.0776(4) 0.49521(14) 0.5716(4) 0.0168(12) Uani 1 1 d . . . A 1
N5 N -0.0146(4) 0.46056(14) 0.6453(3) 0.0151(12) Uani 1 1 d . . . A 1
N6 N -0.1013(4) 0.42282(14) 0.7148(4) 0.0188(13) Uani 1 1 d . . . A 1
N7 N 0.3255(4) 0.30184(14) 0.4738(4) 0.0157(12) Uani 1 1 d . . . A 1
N8 N 0.4106(4) 0.26841(15) 0.5604(4) 0.0227(14) Uani 1 1 d . . . A 1
N9 N 0.2422(4) 0.33861(16) 0.3943(4) 0.0254(15) Uani 1 1 d . . . A 1
N10 N 0.5365(4) 0.36260(18) 0.4100(4) 0.0337(17) Uani 1 1 d . . . A 1
N11 N 0.4532(4) 0.39318(14) 0.5041(4) 0.0187(13) Uani 1 1 d . . . A 1
N12 N 0.3653(4) 0.42156(14) 0.6010(3) 0.0155(12) Uani 1 1 d . . . A 1
N13 N 0.5525(4) 0.42464(15) 0.7532(4) 0.0205(13) Uani 1 1 d . . . A 1
N14 N 0.4654(4) 0.45604(14) 0.8424(4) 0.0181(13) Uani 1 1 d . . . A 1
N15 N 0.3769(4) 0.48409(15) 0.9374(4) 0.0220(14) Uani 1 1 d . . . A 1
N16 N 0.5456(4) 0.38987(18) 1.0368(4) 0.0331(17) Uani 1 1 d . . . A 1
N17 N 0.4602(4) 0.35976(15) 0.9407(4) 0.0199(13) Uani 1 1 d . . . A 1
N18 N 0.3654(4) 0.33193(14) 0.8448(4) 0.0172(13) Uani 1 1 d . . . A 1
N19 N 0.2116(4) 0.32369(18) 1.0335(5) 0.0369(18) Uani 1 1 d . . . A 1
N20 N 0.1274(4) 0.29020(15) 0.9440(4) 0.0247(15) Uani 1 1 d . . . A 1
N21 N 0.0378(4) 0.26047(14) 0.8519(4) 0.0262(15) Uani 1 1 d . . . A 1
N22 N 0.0817(4) 0.34057(13) 0.5747(4) 0.0171(13) Uani 1 1 d . . . A 1
N24 N -0.0024(4) 0.38121(14) 0.9489(3) 0.0168(13) Uani 1 1 d . . . A 1
N25 N 0.0855(4) 0.41453(14) 0.8639(4) 0.0181(13) Uani 1 1 d . . . A 1
O1 O 0.3310(3) 0.39064(11) 0.6219(3) 0.0132(10) Uani 1 1 d . . . A 1
O2 O 0.4905(4) 0.33595(14) 0.4479(4) 0.0336(13) Uani 1 1 d . . . A 1
O3 O 0.4420(3) 0.29741(12) 0.5981(3) 0.0211(11) Uani 1 1 d . . . A 1
O4 O 0.2840(3) 0.36135(12) 0.4517(3) 0.0210(11) Uani 1 1 d . . . A 1
O5 O 0.4995(3) 0.39923(12) 0.7886(3) 0.0209(11) Uani 1 1 d . . . A 1
O6 O 0.3434(3) 0.45323(12) 0.9586(3) 0.0225(11) Uani 1 1 d . . . A 1
O7 O 0.1069(3) 0.46673(11) 0.5298(3) 0.0179(10) Uani 1 1 d . . . A 1
O8 O -0.0493(3) 0.40055(11) 0.6654(3) 0.0161(10) Uani 1 1 d . . . A 1
O9 O -0.0521(3) 0.43427(11) 0.4693(3) 0.0200(11) Uani 1 1 d . . . A 1
O10 O 0.1127(3) 0.36954(10) 0.6160(3) 0.0136(10) Uani 1 1 d . . . A 1
O11 O 0.1181(3) 0.38486(11) 0.8291(3) 0.0143(10) Uani 1 1 d . . . A 1
O12 O -0.0409(3) 0.32175(12) 0.9794(3) 0.0242(11) Uani 1 1 d . . . A 1
O13 O 0.1671(3) 0.34834(13) 0.9844(3) 0.0287(13) Uani 1 1 d . . . A 1
O14 O 0.0082(3) 0.29067(12) 0.8193(3) 0.0217(11) Uani 1 1 d . . . A 1
O16 O 0.4961(3) 0.41609(13) 1.0033(3) 0.0310(13) Uani 1 1 d . . . A 1
O17 O 0.1585(3) 0.42206(11) 0.6719(3) 0.0141(10) Uani 1 1 d . . . A 1
O18 O 0.1627(3) 0.41122(11) 0.4690(3) 0.0198(11) Uani 1 1 d . . . A 1
O19 O 0.2894(3) 0.41848(11) 0.7959(3) 0.0163(10) Uani 1 1 d . . . A 1
O20 O 0.2908(3) 0.39481(13) 0.9932(3) 0.0253(12) Uani 1 1 d . . . A 1
O21 O 0.3347(3) 0.36359(11) 0.8226(3) 0.0143(10) Uani 1 1 d . . . A 1
O22 O -0.0426(3) 0.34845(11) 0.7745(3) 0.0179(10) Uani 1 1 d . U . . .
O23 O 0.1629(3) 0.33237(11) 0.7780(3) 0.0139(10) Uani 1 1 d . . . A 1
O24 O 0.2833(3) 0.33637(11) 0.6482(3) 0.0144(10) Uani 1 1 d . . . A 1
O25 O 0.4922(3) 0.35227(12) 0.6624(3) 0.0187(11) Uani 1 1 d . . . A 1
O26 O 0.3173(4) 0.26787(13) 0.7911(3) 0.0327(13) Uani 1 1 d . . . I 1
O27 O -0.0522(5) 0.2539(2) 0.6303(4) 0.066(2) Uani 1 1 d . . . D 1
O31 O -0.1752(5) 0.31145(17) 1.1566(4) 0.060(2) Uani 1 1 d . . . G 1
Cl2A Cl 0.6733(8) 0.3982(3) 1.1700(6) 0.058(3) Uani 0.25 1 d . U P J 2
O35 O -0.0364(5) 0.20343(19) 0.7708(6) 0.087(3) Uani 1 1 d . . . K 1
O36 O 0.3211(8) 0.4846(3) 0.6512(9) 0.027(3) Uiso 0.5 1 d . . P L 1
O37 O 0.2700(4) 0.45257(14) 0.3835(4) 0.0419(15) Uani 1 1 d . . . M 1
O38 O 0.5908(4) 0.30485(14) 0.7415(3) 0.0351(14) Uani 1 1 d . . . N 1
O39 O 0.1927(9) 0.4621(5) 1.0612(10) 0.083(6) Uani 0.5 1 d . U P O 2
Zr1 Zr 0.22404(4) 0.37718(2) 0.72311(4) 0.01018(14) Uani 1 1 d . . . A 1
Zr2 Zr 0.05153(4) 0.41913(2) 0.56886(4) 0.01247(15) Uani 1 1 d . . . A 1
Zr3 Zr 0.38906(4) 0.34456(2) 0.55095(4) 0.01360(15) Uani 1 1 d . . . A 1
Zr4 Zr 0.39881(4) 0.40924(2) 0.89346(4) 0.01611(16) Uani 1 1 d . . . A 1
Zr5 Zr 0.06073(4) 0.33562(2) 0.88225(4) 0.01350(15) Uani 1 1 d . . . A 1
O40B O 0.0900(16) 0.3446(6) 0.2769(16) 0.049(5) Uiso 0.273(15) 1 d D U . P 1
C43B C 0.163(3) 0.3644(11) 0.244(3) 0.053(5) Uiso 0.23(2) 1 d D U . P 1
O39B O 0.1598(6) 0.4873(2) 1.0149(6) 0.017(2) Uani 0.5 1 d . . P A 1
C33A C 0.2316(10) 0.2370(3) 1.0074(8) 0.052(4) Uani 0.7 1 d D . P A 1
H33A H 0.250902 0.217641 1.044606 0.062 Uiso 0.7 1 calc R U P A 1
H33B H 0.279133 0.240336 0.960544 0.062 Uiso 0.7 1 calc R U P A 1
N23 N -0.0845(4) 0.34554(15) 1.0304(4) 0.0221(14) Uani 1 1 d . . . A 1
C36A C -0.0656(4) 0.37660(19) 1.0147(4) 0.0201(16) Uani 1 1 d . . . A 1
Cl2C Cl 0.6655(4) 0.3788(3) 1.2275(5) 0.101(3) Uani 0.45 1 d . U P E 1
O36B O 0.2793(8) 0.4819(3) 0.6462(7) 0.021(2) Uani 0.5 1 d . . P Q 2
C33B C 0.1627(19) 0.2295(7) 1.0417(18) 0.028(6) Uiso 0.3 1 d . . P R 2
Cl3A Cl 0.418(3) 0.3975(11) 1.203(3) 0.107(12) Uiso 0.1 1 d . . P S 4
K9A K 0.2504(14) 0.4277(5) 1.2363(15) 0.115(6) Uiso 0.2 1 d . . P O 2
K9B K 0.378(3) 0.3843(10) 1.269(3) 0.112(12) Uiso 0.1 1 d . . P T 3
Cl3B Cl 0.3458(10) 0.3589(2) 1.1777(9) 0.016(2) Uani 0.2 1 d . U P O 2
C43 C 0.0792(9) 0.3609(4) 0.2012(8) 0.055(3) Uani 0.7 1 d D U P U 2
H43A H 0.017832 0.371149 0.196132 0.082 Uiso 0.7 1 calc R U P U 2
H43B H 0.072609 0.336694 0.203646 0.082 Uiso 0.7 1 calc R U P U 2
H43C H 0.115736 0.367032 0.148250 0.082 Uiso 0.7 1 calc R U P U 2
O40 O 0.1223(8) 0.3716(3) 0.2777(6) 0.053(2) Uani 0.7 1 d D U P U 2
H40 H 0.144741 0.390560 0.268608 0.080 Uiso 0.7 1 calc R U P U 2
C41 C 0.7178(8) 0.3816(3) 0.5929(7) 0.070(3) Uani 1 1 d . . . V 2
H41A H 0.712280 0.378371 0.526843 0.105 Uiso 1 1 calc R U . V 2
H41B H 0.691184 0.362459 0.624166 0.105 Uiso 1 1 calc R U . V 2
H41C H 0.783257 0.383807 0.610433 0.105 Uiso 1 1 calc R U . V 2
O28 O -0.2226(4) 0.40219(14) 0.8409(4) 0.0438(16) Uani 1 1 d . . . W 1
C42 C -0.2691(7) 0.3716(2) 0.8595(7) 0.055(3) Uani 1 1 d . U . W 1
H42A H -0.261198 0.366073 0.924123 0.083 Uiso 1 1 calc R U . W 1
H42B H -0.242809 0.353857 0.822320 0.083 Uiso 1 1 calc R U . W 1
H42C H -0.335151 0.373969 0.844622 0.083 Uiso 1 1 calc R U . W 1
O30 O 0.6687(4) 0.41140(15) 0.6182(4) 0.0447(16) Uani 1 1 d . . . V 2
H30 H 0.696939 0.428110 0.598692 0.067 Uiso 1 1 calc R U . V 2
C8B C 0.2765(18) 0.2468(7) 0.3588(17) 0.026(6) Uani 0.3 1 d . . P X 2
C28B C 0.522(2) 0.3000(8) 1.028(2) 0.043(8) Uiso 0.3 1 d . . P Y 2
K3B K 0.2474(19) 0.5284(7) 1.0335(19) 0.059(8) Uiso 0.1 1 d . . P O 2
K10B K 0.7989(15) 0.4368(5) 1.2755(15) 0.071(7) Uiso 0.15 1 d . . P J 2
K4B K -0.216(3) 0.3244(10) 0.679(3) 0.102(12) Uiso 0.1 1 d . . P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N12 1.304(8) . ?
C1 N11 1.339(9) . ?
C1 C2 1.507(10) . ?
C2 C3 1.531(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.513(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.494(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N10 1.276(10) . ?
C5 N11 1.365(9) . ?
C6 N9 1.305(9) . ?
C6 N7 1.345(8) . ?
C6 C7 1.503(10) . ?
C7 C8 1.414(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.565(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.497(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N8 1.302(9) . ?
C10 N7 1.348(9) . ?
C11 N3 1.303(9) . ?
C11 N2 1.374(8) . ?
C11 C12 1.491(9) . ?
C12 C13 1.514(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.523(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.494(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N22 1.299(8) . ?
C15 N2 1.335(8) . ?
C16 N6 1.296(8) . ?
C16 N5 1.352(8) . ?
C16 C17 1.492(9) . ?
C17 C18 1.520(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.530(9) . ?
C18 K9 3.495(8) 3_567 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.505(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 N4 1.304(8) . ?
C20 N5 1.354(8) . ?
C21 N15 1.297(9) . ?
C21 N14 1.362(8) . ?
C21 C22 1.491(10) . ?
C22 C23 1.512(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.526(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.488(10) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 N13 1.297(9) . ?
C25 N14 1.347(8) . ?
C26 N18 1.300(8) . ?
C26 N17 1.346(9) . ?
C26 C27 1.500(10) . ?
C27 C28 1.539(11) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.449(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.475(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 N16 1.286(10) . ?
C30 N17 1.363(8) . ?
C31 N21 1.293(10) . ?
C31 N20 1.344(10) . ?
C31 C32 1.524(11) . ?
C32 C33A 1.529(13) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C34 C33A 1.417(13) . ?
C34 C35 1.500(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N19 1.275(11) . ?
C35 N20 1.350(10) . ?
C37 C36A 1.481(10) . ?
C37 C38 1.533(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.508(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.491(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 N25 1.306(8) . ?
C40 N24 1.351(8) . ?
K3 O39B 2.926(10) . ?
K3 O28 2.969(6) 3_567 ?
K3 N15 3.111(6) . ?
K3 K10 4.605(4) 3_667 ?
K4 O22 3.013(5) . ?
K4 O27 3.088(8) . ?
K4 O38 3.166(6) 1_455 ?
K4 C33A 3.443(12) 4_565 ?
K4 H41B 3.06(4) 1_455 ?
Cl4 K10 2.945(6) . ?
K10 N3 3.208(7) 1_656 ?
K10 O36 3.259(14) 3_667 ?
K10 Cl2C 3.519(10) . ?
K7 O31 3.160(8) . ?
K7 N8 3.168(6) 4_566 ?
K7 O26 3.197(6) 4_566 ?
K7 O38 3.328(6) 4_566 ?
K7 O40B 3.33(3) 1_556 ?
K9 C43B 2.94(3) 1_556 ?
K9 O20 3.103(6) . ?
K9 O37 3.336(8) 1_556 ?
K9 O39B 3.395(10) . ?
K9 H40 2.41(5) 1_556 ?
N2 Zr2 2.278(5) . ?
N3 O9 1.368(7) . ?
N4 O7 1.371(7) . ?
N5 Zr2 2.236(5) . ?
N6 O8 1.385(7) . ?
N7 Zr3 2.247(5) . ?
N8 O3 1.366(7) . ?
N9 O4 1.376(7) . ?
N10 O2 1.385(8) . ?
N11 Zr3 2.278(6) . ?
N12 O1 1.376(7) . ?
N13 O5 1.385(7) . ?
N14 Zr4 2.251(6) . ?
N15 O6 1.371(7) . ?
N16 O16 1.363(8) . ?
N17 Zr4 2.284(6) . ?
N18 O21 1.387(7) . ?
N19 O13 1.379(8) . ?
N20 Zr5 2.250(6) . ?
N21 O14 1.372(7) . ?
N22 O10 1.386(6) . ?
N24 C36A 1.355(8) . ?
N24 Zr5 2.279(6) . ?
N25 O11 1.386(7) . ?
O1 Zr1 2.231(4) . ?
O1 Zr3 2.294(4) . ?
O2 Zr3 2.154(5) . ?
O3 Zr3 2.156(5) . ?
O4 Zr3 2.192(4) . ?
O5 Zr4 2.175(4) . ?
O6 Zr4 2.173(5) . ?
O7 Zr2 2.159(5) . ?
O8 Zr2 2.184(4) . ?
O9 Zr2 2.161(4) . ?
O10 Zr1 2.251(4) . ?
O10 Zr2 2.286(4) . ?
O11 Zr1 2.225(4) . ?
O11 Zr5 2.292(4) . ?
O12 N23 1.376(7) . ?
O12 Zr5 2.140(5) . ?
O13 Zr5 2.188(5) . ?
O14 Zr5 2.163(5) . ?
O16 Zr4 2.138(5) . ?
O17 Zr2 2.147(4) . ?
O17 Zr1 2.169(4) . ?
O18 Zr2 2.217(5) . ?
O19 Zr4 2.148(4) . ?
O19 Zr1 2.182(4) . ?
O20 Zr4 2.237(5) . ?
O21 Zr1 2.215(4) . ?
O21 Zr4 2.299(4) . ?
O22 Zr5 2.218(4) . ?
O22 K4B 3.02(4) . ?
O23 Zr5 2.151(4) . ?
O23 Zr1 2.170(4) . ?
O24 Zr3 2.136(4) . ?
O24 Zr1 2.163(4) . ?
O25 Zr3 2.215(4) . ?
Cl2A K10B 2.83(2) . ?
O39 K3B 2.82(3) . ?
O39 K9A 3.02(3) . ?
O40B C43B 1.419(19) . ?
C33A H33A 0.9900 . ?
C33A H33B 0.9900 . ?
N23 C36A 1.302(9) . ?
C33B K4B 3.42(5) 4_666 ?
K9A O40 2.99(2) 1_556 ?
K9A Cl3B 3.22(2) . ?
K9A K3B 5.03(4) . ?
K9A H40 2.19(4) 1_556 ?
C43 O40 1.345(13) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O40 H40 0.8400 . ?
C41 O30 1.446(12) . ?
C41 K4B 2.79(4) 1_655 ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
O28 C42 1.432(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O30 H30 0.8400 . ?
K3B K10B 4.78(4) 3_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N12 C1 N11 115.8(6) . . ?
N12 C1 C2 121.5(6) . . ?
N11 C1 C2 122.7(6) . . ?
C1 C2 C3 109.7(6) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 110.0(6) . . ?
C4 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 C3 110.0(6) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N10 C5 N11 114.5(7) . . ?
N10 C5 C4 122.1(7) . . ?
N11 C5 C4 123.3(7) . . ?
N9 C6 N7 114.2(6) . . ?
N9 C6 C7 122.2(7) . . ?
N7 C6 C7 123.7(7) . . ?
C8 C7 C6 109.9(8) . . ?
C8 C7 H7A 109.7 . . ?
C6 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 C9 114.7(9) . . ?
C7 C8 H8A 108.6 . . ?
C9 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
C9 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C8 109.1(7) . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N8 C10 N7 113.0(6) . . ?
N8 C10 C9 122.9(7) . . ?
N7 C10 C9 124.1(6) . . ?
N3 C11 N2 114.0(6) . . ?
N3 C11 C12 123.0(6) . . ?
N2 C11 C12 123.0(6) . . ?
C11 C12 C13 109.8(6) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C12 C13 C14 111.2(7) . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C15 C14 C13 109.5(6) . . ?
C15 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
N22 C15 N2 115.2(6) . . ?
N22 C15 C14 121.0(6) . . ?
N2 C15 C14 123.8(6) . . ?
N6 C16 N5 114.6(6) . . ?
N6 C16 C17 122.6(6) . . ?
N5 C16 C17 122.8(6) . . ?
C16 C17 C18 107.9(6) . . ?
C16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C17 C18 C19 110.0(6) . . ?
C17 C18 K9 99.6(4) . 3_567 ?
C19 C18 K9 103.9(4) . 3_567 ?
C17 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
K9 C18 H18A 123.3 3_567 . ?
C17 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
K9 C18 H18B 15.3 3_567 . ?
H18A C18 H18B 108.2 . . ?
C20 C19 C18 109.5(6) . . ?
C20 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
N4 C20 N5 113.6(6) . . ?
N4 C20 C19 123.3(6) . . ?
N5 C20 C19 123.1(6) . . ?
N15 C21 N14 113.1(6) . . ?
N15 C21 C22 123.3(6) . . ?
N14 C21 C22 123.5(6) . . ?
C21 C22 C23 109.9(6) . . ?
C21 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C22 C23 C24 110.8(6) . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C25 C24 C23 111.9(6) . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
N13 C25 N14 114.7(6) . . ?
N13 C25 C24 122.2(6) . . ?
N14 C25 C24 123.1(6) . . ?
N18 C26 N17 116.2(6) . . ?
N18 C26 C27 121.1(6) . . ?
N17 C26 C27 122.7(6) . . ?
C26 C27 C28 109.0(7) . . ?
C26 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
C26 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C29 C28 C27 112.5(8) . . ?
C29 C28 H28A 109.1 . . ?
C27 C28 H28A 109.1 . . ?
C29 C28 H28B 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
C28 C29 C30 112.0(7) . . ?
C28 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
N16 C30 N17 113.7(7) . . ?
N16 C30 C29 123.8(7) . . ?
N17 C30 C29 122.5(8) . . ?
N21 C31 N20 113.7(7) . . ?
N21 C31 C32 124.8(8) . . ?
N20 C31 C32 121.5(8) . . ?
C31 C32 C33A 108.9(8) . . ?
C31 C32 H32A 109.9 . . ?
C33A C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C33A C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C33A C34 C35 108.6(9) . . ?
C33A C34 H34A 110.0 . . ?
C35 C34 H34A 110.0 . . ?
C33A C34 H34B 110.0 . . ?
C35 C34 H34B 110.0 . . ?
H34A C34 H34B 108.4 . . ?
N19 C35 N20 116.1(7) . . ?
N19 C35 C34 120.3(8) . . ?
N20 C35 C34 123.6(9) . . ?
C36A C37 C38 109.6(6) . . ?
C36A C37 H37A 109.8 . . ?
C38 C37 H37A 109.8 . . ?
C36A C37 H37B 109.8 . . ?
C38 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
C39 C38 C37 109.9(6) . . ?
C39 C38 H38A 109.7 . . ?
C37 C38 H38A 109.7 . . ?
C39 C38 H38B 109.7 . . ?
C37 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C40 C39 C38 110.4(6) . . ?
C40 C39 H39A 109.6 . . ?
C38 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
C38 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
N25 C40 N24 115.1(6) . . ?
N25 C40 C39 122.4(6) . . ?
N24 C40 C39 122.5(6) . . ?
O39B K3 O28 116.1(2) . 3_567 ?
O39B K3 N15 67.5(2) . . ?
O28 K3 N15 172.19(19) 3_567 . ?
O39B K3 K10 75.98(19) . 3_667 ?
O28 K3 K10 117.70(15) 3_567 3_667 ?
N15 K3 K10 69.51(12) . 3_667 ?
O22 K4 O27 91.13(17) . . ?
O22 K4 O38 129.78(16) . 1_455 ?
O27 K4 O38 136.78(19) . 1_455 ?
O22 K4 C33A 142.6(3) . 4_565 ?
O27 K4 C33A 66.6(3) . 4_565 ?
O38 K4 C33A 82.6(3) 1_455 4_565 ?
O22 K4 H41B 93.9(4) . 1_455 ?
O27 K4 H41B 137.6(11) . 1_455 ?
O38 K4 H41B 62.8(7) 1_455 1_455 ?
C33A K4 H41B 85.0(9) 4_565 1_455 ?
Cl4 K10 N3 130.91(16) . 1_656 ?
Cl4 K10 O36 61.9(2) . 3_667 ?
N3 K10 O36 112.6(3) 1_656 3_667 ?
Cl4 K10 Cl2C 142.87(19) . . ?
N3 K10 Cl2C 85.3(2) 1_656 . ?
O36 K10 Cl2C 117.1(3) 3_667 . ?
Cl4 K10 K3 68.47(10) . 3_667 ?
N3 K10 K3 144.23(15) 1_656 3_667 ?
O36 K10 K3 103.1(2) 3_667 3_667 ?
Cl2C K10 K3 76.50(15) . 3_667 ?
O31 K7 N8 72.32(17) . 4_566 ?
O31 K7 O26 72.47(15) . 4_566 ?
N8 K7 O26 70.40(15) 4_566 4_566 ?
O31 K7 O38 144.07(17) . 4_566 ?
N8 K7 O38 75.29(14) 4_566 4_566 ?
O26 K7 O38 82.42(15) 4_566 4_566 ?
O31 K7 O40B 85.3(4) . 1_556 ?
N8 K7 O40B 139.8(4) 4_566 1_556 ?
O26 K7 O40B 134.2(4) 4_566 1_556 ?
O38 K7 O40B 130.3(4) 4_566 1_556 ?
C43B K9 O20 91.2(10) 1_556 . ?
C43B K9 O37 87.9(9) 1_556 1_556 ?
O20 K9 O37 148.42(19) . 1_556 ?
C43B K9 O39B 141.2(9) 1_556 . ?
O20 K9 O39B 80.2(2) . . ?
O37 K9 O39B 118.5(2) 1_556 . ?
C43B K9 C18 110.3(10) 1_556 3_567 ?
O20 K9 C18 137.0(2) . 3_567 ?
O37 K9 C18 71.76(16) 1_556 3_567 ?
O39B K9 C18 59.5(2) . 3_567 ?
C43B K9 H40 22(3) 1_556 1_556 ?
O20 K9 H40 112(3) . 1_556 ?
O37 K9 H40 73.0(9) 1_556 1_556 ?
O39B K9 H40 136(3) . 1_556 ?
C18 K9 H40 90(4) 3_567 1_556 ?
C15 N2 C11 119.5(6) . . ?
C15 N2 Zr2 122.3(4) . . ?
C11 N2 Zr2 118.2(4) . . ?
C11 N3 O9 118.3(5) . . ?
C11 N3 K10 134.4(4) . 1_454 ?
O9 N3 K10 105.7(4) . 1_454 ?
C20 N4 O7 117.3(5) . . ?
C16 N5 C20 119.8(6) . . ?
C16 N5 Zr2 120.1(4) . . ?
C20 N5 Zr2 120.1(4) . . ?
C16 N6 O8 116.9(6) . . ?
C6 N7 C10 119.2(6) . . ?
C6 N7 Zr3 120.4(5) . . ?
C10 N7 Zr3 120.4(4) . . ?
C10 N8 O3 117.8(6) . . ?
C10 N8 K7 149.8(5) . 4_665 ?
O3 N8 K7 89.2(3) . 4_665 ?
C6 N9 O4 117.4(5) . . ?
C5 N10 O2 118.8(6) . . ?
C1 N11 C5 119.8(6) . . ?
C1 N11 Zr3 122.1(4) . . ?
C5 N11 Zr3 118.1(5) . . ?
C1 N12 O1 116.3(5) . . ?
C25 N13 O5 116.2(6) . . ?
C25 N14 C21 119.5(6) . . ?
C25 N14 Zr4 120.2(5) . . ?
C21 N14 Zr4 120.3(4) . . ?
C21 N15 O6 118.1(6) . . ?
C21 N15 K3 126.5(5) . . ?
O6 N15 K3 115.4(4) . . ?
C30 N16 O16 119.1(6) . . ?
C26 N17 C30 120.1(7) . . ?
C26 N17 Zr4 122.1(4) . . ?
C30 N17 Zr4 117.8(5) . . ?
C26 N18 O21 115.5(6) . . ?
C35 N19 O13 116.2(6) . . ?
C31 N20 C35 121.1(7) . . ?
C31 N20 Zr5 119.6(5) . . ?
C35 N20 Zr5 119.2(6) . . ?
C31 N21 O14 118.6(6) . . ?
C15 N22 O10 117.2(5) . . ?
C40 N24 C36A 119.3(6) . . ?
C40 N24 Zr5 122.3(4) . . ?
C36A N24 Zr5 118.5(5) . . ?
C40 N25 O11 116.7(5) . . ?
N12 O1 Zr1 128.6(3) . . ?
N12 O1 Zr3 119.6(3) . . ?
Zr1 O1 Zr3 111.68(18) . . ?
N10 O2 Zr3 119.7(4) . . ?
N8 O3 Zr3 120.6(4) . . ?
N9 O4 Zr3 119.5(4) . . ?
N13 O5 Zr4 120.7(4) . . ?
N15 O6 Zr4 120.3(4) . . ?
N4 O7 Zr2 120.3(4) . . ?
N6 O8 Zr2 119.6(4) . . ?
N3 O9 Zr2 120.6(4) . . ?
N22 O10 Zr1 130.0(3) . . ?
N22 O10 Zr2 118.8(3) . . ?
Zr1 O10 Zr2 111.11(17) . . ?
N25 O11 Zr1 128.4(3) . . ?
N25 O11 Zr5 119.5(3) . . ?
Zr1 O11 Zr5 112.08(18) . . ?
N23 O12 Zr5 120.5(4) . . ?
N19 O13 Zr5 120.3(4) . . ?
N21 O14 Zr5 119.2(4) . . ?
N16 O16 Zr4 120.4(4) . . ?
Zr2 O17 Zr1 120.2(2) . . ?
Zr4 O19 Zr1 120.1(2) . . ?
Zr4 O20 K9 131.8(2) . . ?
N18 O21 Zr1 127.3(3) . . ?
N18 O21 Zr4 120.2(3) . . ?
Zr1 O21 Zr4 112.42(18) . . ?
Zr5 O22 K4 126.72(19) . . ?
Zr5 O23 Zr1 120.2(2) . . ?
Zr3 O24 Zr1 121.2(2) . . ?
K4 O38 K7 112.14(17) 1_655 4_665 ?
K3B O39 K9A 118.9(8) . . ?
O24 Zr1 O17 129.14(16) . . ?
O24 Zr1 O23 74.03(16) . . ?
O17 Zr1 O23 130.04(16) . . ?
O24 Zr1 O19 131.00(16) . . ?
O17 Zr1 O19 73.56(16) . . ?
O23 Zr1 O19 128.86(16) . . ?
O24 Zr1 O21 81.95(16) . . ?
O17 Zr1 O21 137.74(16) . . ?
O23 Zr1 O21 81.01(16) . . ?
O19 Zr1 O21 64.19(16) . . ?
O24 Zr1 O11 138.19(16) . . ?
O17 Zr1 O11 79.91(16) . . ?
O23 Zr1 O11 64.27(16) . . ?
O19 Zr1 O11 81.32(16) . . ?
O21 Zr1 O11 94.09(16) . . ?
O24 Zr1 O1 63.90(16) . . ?
O17 Zr1 O1 82.53(16) . . ?
O23 Zr1 O1 137.82(16) . . ?
O19 Zr1 O1 80.90(16) . . ?
O21 Zr1 O1 89.92(16) . . ?
O11 Zr1 O1 157.89(16) . . ?
O24 Zr1 O10 79.97(16) . . ?
O17 Zr1 O10 64.48(15) . . ?
O23 Zr1 O10 81.66(16) . . ?
O19 Zr1 O10 138.04(16) . . ?
O21 Zr1 O10 157.77(16) . . ?
O11 Zr1 O10 90.84(16) . . ?
O1 Zr1 O10 93.62(16) . . ?
O17 Zr2 O7 82.66(17) . . ?
O17 Zr2 O9 160.46(17) . . ?
O7 Zr2 O9 79.97(17) . . ?
O17 Zr2 O8 92.42(16) . . ?
O7 Zr2 O8 137.03(17) . . ?
O9 Zr2 O8 94.20(17) . . ?
O17 Zr2 O18 87.25(16) . . ?
O7 Zr2 O18 71.05(17) . . ?
O9 Zr2 O18 95.46(17) . . ?
O8 Zr2 O18 151.66(17) . . ?
O17 Zr2 N5 85.10(17) . . ?
O7 Zr2 N5 68.58(18) . . ?
O9 Zr2 N5 80.29(18) . . ?
O8 Zr2 N5 68.47(18) . . ?
O18 Zr2 N5 139.53(19) . . ?
O17 Zr2 N2 130.59(18) . . ?
O7 Zr2 N2 135.13(18) . . ?
O9 Zr2 N2 68.85(18) . . ?
O8 Zr2 N2 78.36(18) . . ?
O18 Zr2 N2 80.44(18) . . ?
N5 Zr2 N2 132.4(2) . . ?
O17 Zr2 O10 64.20(15) . . ?
O7 Zr2 O10 135.44(16) . . ?
O9 Zr2 O10 135.30(16) . . ?
O8 Zr2 O10 76.31(16) . . ?
O18 Zr2 O10 78.10(16) . . ?
N5 Zr2 O10 131.80(17) . . ?
N2 Zr2 O10 66.46(16) . . ?
O24 Zr3 O2 161.64(19) . . ?
O24 Zr3 O3 84.45(17) . . ?
O2 Zr3 O3 80.9(2) . . ?
O24 Zr3 O4 89.81(17) . . ?
O2 Zr3 O4 93.1(2) . . ?
O3 Zr3 O4 136.24(17) . . ?
O24 Zr3 O25 90.50(16) . . ?
O2 Zr3 O25 94.78(19) . . ?
O3 Zr3 O25 69.88(17) . . ?
O4 Zr3 O25 153.72(17) . . ?
O24 Zr3 N7 85.85(18) . . ?
O2 Zr3 N7 78.5(2) . . ?
O3 Zr3 N7 68.11(18) . . ?
O4 Zr3 N7 68.22(18) . . ?
O25 Zr3 N7 137.99(19) . . ?
O24 Zr3 N11 129.40(19) . . ?
O2 Zr3 N11 68.9(2) . . ?
O3 Zr3 N11 135.20(19) . . ?
O4 Zr3 N11 79.36(19) . . ?
O25 Zr3 N11 80.21(18) . . ?
N7 Zr3 N11 132.1(2) . . ?
O24 Zr3 O1 63.23(16) . . ?
O2 Zr3 O1 135.09(18) . . ?
O3 Zr3 O1 134.18(16) . . ?
O4 Zr3 O1 78.34(16) . . ?
O25 Zr3 O1 78.38(16) . . ?
N7 Zr3 O1 134.30(17) . . ?
N11 Zr3 O1 66.18(18) . . ?
O16 Zr4 O19 161.31(19) . . ?
O16 Zr4 O6 78.80(19) . . ?
O19 Zr4 O6 83.06(17) . . ?
O16 Zr4 O5 96.79(19) . . ?
O19 Zr4 O5 93.11(17) . . ?
O6 Zr4 O5 135.99(18) . . ?
O16 Zr4 O20 89.83(19) . . ?
O19 Zr4 O20 88.13(17) . . ?
O6 Zr4 O20 69.89(18) . . ?
O5 Zr4 O20 154.06(18) . . ?
O16 Zr4 N14 82.2(2) . . ?
O19 Zr4 N14 86.96(18) . . ?
O6 Zr4 N14 68.14(19) . . ?
O5 Zr4 N14 67.88(19) . . ?
O20 Zr4 N14 138.03(19) . . ?
O16 Zr4 N17 68.7(2) . . ?
O19 Zr4 N17 129.15(18) . . ?
O6 Zr4 N17 136.20(19) . . ?
O5 Zr4 N17 78.01(19) . . ?
O20 Zr4 N17 81.17(19) . . ?
N14 Zr4 N17 131.7(2) . . ?
O16 Zr4 O21 134.33(18) . . ?
O19 Zr4 O21 63.28(16) . . ?
O6 Zr4 O21 134.57(17) . . ?
O5 Zr4 O21 78.54(16) . . ?
O20 Zr4 O21 78.93(17) . . ?
N14 Zr4 O21 133.62(17) . . ?
N17 Zr4 O21 65.89(17) . . ?
O12 Zr5 O23 161.30(18) . . ?
O12 Zr5 O14 80.02(18) . . ?
O23 Zr5 O14 83.41(17) . . ?
O12 Zr5 O13 94.97(19) . . ?
O23 Zr5 O13 91.08(18) . . ?
O14 Zr5 O13 136.48(18) . . ?
O12 Zr5 O22 94.29(18) . . ?
O23 Zr5 O22 88.21(16) . . ?
O14 Zr5 O22 70.34(17) . . ?
O13 Zr5 O22 152.88(18) . . ?
O12 Zr5 N20 79.3(2) . . ?
O23 Zr5 N20 86.71(19) . . ?
O14 Zr5 N20 68.7(2) . . ?
O13 Zr5 N20 67.9(2) . . ?
O22 Zr5 N20 139.0(2) . . ?
O12 Zr5 N24 68.84(19) . . ?
O23 Zr5 N24 129.81(18) . . ?
O14 Zr5 N24 135.83(18) . . ?
O13 Zr5 N24 78.40(19) . . ?
O22 Zr5 N24 81.31(18) . . ?
N20 Zr5 N24 130.8(2) . . ?
O12 Zr5 O11 135.21(17) . . ?
O23 Zr5 O11 63.43(16) . . ?
O14 Zr5 O11 134.79(17) . . ?
O13 Zr5 O11 77.11(17) . . ?
O22 Zr5 O11 78.36(16) . . ?
N20 Zr5 O11 133.28(18) . . ?
N24 Zr5 O11 66.38(17) . . ?
C43B O40B K7 136(3) . 1_554 ?
O40B C43B K9 148(3) . 1_554 ?
K3 O39B K9 106.4(3) . . ?
C34 C33A C32 116.7(11) . . ?
C34 C33A K4 84.5(6) . 4_666 ?
C32 C33A K4 121.7(8) . 4_666 ?
C34 C33A H33A 108.1 . . ?
C32 C33A H33A 108.1 . . ?
K4 C33A H33A 23.6 4_666 . ?
C34 C33A H33B 108.1 . . ?
C32 C33A H33B 108.1 . . ?
K4 C33A H33B 115.5 4_666 . ?
H33A C33A H33B 107.3 . . ?
C36A N23 O12 118.2(6) . . ?
N23 C36A N24 113.8(6) . . ?
N23 C36A C37 121.9(6) . . ?
N24 C36A C37 124.2(7) . . ?
O40 K9A O39 110.9(7) 1_556 . ?
O40 K9A Cl3B 71.0(5) 1_556 . ?
O39 K9A Cl3B 106.3(7) . . ?
O40 K9A K3B 136.9(7) 1_556 . ?
O39 K9A K3B 29.3(5) . . ?
Cl3B K9A K3B 122.3(7) . . ?
O40 C43 H43A 109.5 . . ?
O40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C43 O40 H40 109.5 . . ?
K9A O40 H40 16.2 1_554 . ?
O30 C41 H41A 109.5 . . ?
K4B C41 H41A 111.1 1_655 . ?
O30 C41 H41B 109.5 . . ?
K4B C41 H41B 43.1 1_655 . ?
H41A C41 H41B 109.5 . . ?
O30 C41 H41C 109.5 . . ?
K4B C41 H41C 68.6 1_655 . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 O28 K3 111.9(5) . 3_567 ?
O28 C42 H42A 109.5 . . ?
O28 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O28 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 O30 H30 109.5 . . ?
O39 K3B K9A 31.7(5) . . ?
K10B K3B K9A 142.8(7) 3_667 . ?
C41 K4B O22 102.7(12) 1_455 . ?
O22 K4B C33B 152.9(15) . 4_565 ?
O22 K4B H41B 116.5(16) . 1_455 ?

_refine_diff_density_max         1.021
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.149

