# Electronic Supplementary Material (ESI) for Polymer Chemistry.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_Zr2
_database_code_depnum_ccdc_archive 'CCDC 1422872'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ' 	C38 H56 Br4 N2 O8 Zr2 '

_chemical_formula_sum            'C38 H56 Br4 N2 O8 Zr2'


_chemical_formula_weight         1170.93



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'
Br Br -0.2901 2.4595 '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   P2(1)/n

_symmetry_space_group_name_Hall  '-P 2yn'

loop_

_symmetry_equiv_pos_as_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                   10.3571(4)

_cell_length_b                   12.8862(6)

_cell_length_c                   35.6573(14)

_cell_angle_alpha                90.00

_cell_angle_beta                 96.839(2)

_cell_angle_gamma                90.00

_cell_volume                     4725.1(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    4302

_cell_measurement_theta_min      2.13

_cell_measurement_theta_max      21.38



_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.22

_exptl_crystal_size_min          0.15

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.646

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2328

_exptl_absorpt_coefficient_mu    3.870

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4446

_exptl_absorpt_correction_T_max  0.5945

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      173(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 APEXII 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            16563

_diffrn_reflns_av_R_equivalents  0.0401

_diffrn_reflns_av_sigmaI/netI    0.0626

_diffrn_reflns_limit_h_min       -11

_diffrn_reflns_limit_h_max       11

_diffrn_reflns_limit_k_min       -13

_diffrn_reflns_limit_k_max       12

_diffrn_reflns_limit_l_min       -38

_diffrn_reflns_limit_l_max       28

_diffrn_reflns_theta_min         1.68

_diffrn_reflns_theta_max         22.58

_reflns_number_total             5938

_reflns_number_gt                4484

_reflns_threshold_expression     >2sigma(I)




_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0215P)²+89.8252P] 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         5938

_refine_ls_number_parameters     499

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.1106

_refine_ls_R_factor_gt           0.0830

_refine_ls_wR_factor_ref         0.1752

_refine_ls_wR_factor_gt          0.1658

_refine_ls_goodness_of_fit_ref   1.169

_refine_ls_restrained_S_all      1.169

_refine_ls_shift/su_max          0.012

_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 0.48738(12) 0.43552(11) 0.12983(4) 0.0423(4) Uani 1 1 d . . .
Zr2 Zr 0.43490(13) 0.17451(11) 0.15004(4) 0.0392(4) Uani 1 1 d . . .
Br1 Br 0.18645(15) 0.72521(12) 0.13732(5) 0.0534(5) Uani 1 1 d . . .
Br3 Br -0.18842(14) -0.07911(15) 0.04538(5) 0.0635(5) Uani 1 1 d . . .
Br2 Br -0.01537(18) 0.70849(16) -0.01647(6) 0.0784(6) Uani 1 1 d . . .
Br4 Br 0.07314(17) -0.01319(16) 0.19038(5) 0.0712(6) Uani 1 1 d . . .
O1 O 0.3452(8) 0.5440(7) 0.1136(2) 0.040(2) Uani 1 1 d . . .
C4 C 0.0900(13) 0.6494(12) 0.0266(4) 0.045(4) Uani 1 1 d . . .
C1 C 0.2625(12) 0.5763(10) 0.0861(4) 0.034(3) Uani 1 1 d . . .
C6 C 0.2477(13) 0.5249(10) 0.0505(4) 0.035(3) Uani 1 1 d . . .
C2 C 0.1810(12) 0.6615(10) 0.0901(4) 0.032(3) Uani 1 1 d . . .
C5 C 0.1608(14) 0.5641(11) 0.0210(4) 0.046(4) Uani 1 1 d . . .
H5 H 0.1515 0.5308 -0.0030 0.055 Uiso 1 1 calc R . .
C3 C 0.0969(12) 0.6997(10) 0.0599(4) 0.040(4) Uani 1 1 d . . .
H3 H 0.0457 0.7598 0.0627 0.048 Uiso 1 1 calc R . .
C7 C 0.3205(16) 0.4332(11) 0.0426(4) 0.051(4) Uani 1 1 d . . .
H7 H 0.3031 0.4065 0.0177 0.061 Uiso 1 1 calc R . .
N1 N 0.4041(13) 0.3837(10) 0.0644(4) 0.059(4) Uani 1 1 d . . .
C15 C 0.1549(14) 0.0726(10) 0.0844(4) 0.043(4) Uani 1 1 d . . .
C18 C -0.0390(12) -0.0372(10) 0.1155(4) 0.041(4) Uani 1 1 d . . .
H18 H -0.1053 -0.0752 0.1257 0.049 Uiso 1 1 calc R . .
C17 C -0.0425(12) -0.0219(11) 0.0767(4) 0.039(4) Uani 1 1 d . . .
C16 C 0.0506(13) 0.0314(10) 0.0612(4) 0.039(4) Uani 1 1 d . . .
H16 H 0.0444 0.0404 0.0346 0.047 Uiso 1 1 calc R . .
C20 C 0.1657(13) 0.0593(11) 0.1247(4) 0.039(4) Uani 1 1 d . . .
O2 O 0.2592(8) 0.0999(8) 0.1470(3) 0.046(3) Uani 1 1 d . . .
C19 C 0.0620(12) 0.0040(10) 0.1381(4) 0.034(3) Uani 1 1 d . . .
N2 N 0.3619(13) 0.1663(10) 0.0815(3) 0.056(4) Uani 1 1 d . . .
C14 C 0.2567(16) 0.1236(11) 0.0658(4) 0.051(4) Uani 1 1 d . . .
H14 H 0.2435 0.1254 0.0390 0.061 Uiso 1 1 calc R . .
O8 O 0.3424(7) 0.3257(7) 0.1434(2) 0.036(2) Uani 1 1 d . . .
O5 O 0.5800(7) 0.2875(7) 0.1391(2) 0.038(2) Uani 1 1 d . . .
O4 O 0.4577(9) 0.1732(8) 0.2033(3) 0.049(3) Uani 1 1 d . . .
O3 O 0.5376(10) 0.0565(8) 0.1386(3) 0.066(3) Uani 1 1 d . . .
O6 O 0.5226(10) 0.4914(8) 0.1789(3) 0.063(3) Uani 1 1 d . . .
O7 O 0.6304(10) 0.4919(8) 0.1065(4) 0.086(4) Uani 1 1 d . . .
C37 C 0.1149(11) 0.3503(12) 0.1242(5) 0.052(4) Uani 1 1 d . . .
H37A H 0.1025 0.2780 0.1160 0.078 Uiso 1 1 calc R . .
H37B H 0.1394 0.3921 0.1032 0.078 Uiso 1 1 calc R . .
H37C H 0.0338 0.3772 0.1320 0.078 Uiso 1 1 calc R . .
C29 C 0.7802(13) 0.2192(13) 0.1200(5) 0.066(5) Uani 1 1 d . . .
H29A H 0.8748 0.2221 0.1263 0.099 Uiso 1 1 calc R . .
H29B H 0.7556 0.2537 0.0957 0.099 Uiso 1 1 calc R . .
H29C H 0.7521 0.1465 0.1182 0.099 Uiso 1 1 calc R . .
C27 C 0.7173(14) 0.2717(14) 0.1495(6) 0.074(6) Uani 1 1 d . . .
H27 H 0.7490 0.3440 0.1463 0.089 Uiso 1 1 calc R . .
C21 C 0.5854(16) -0.0442(13) 0.1323(6) 0.067(5) Uani 1 1 d . . .
H21 H 0.6481 -0.0406 0.1131 0.081 Uiso 1 1 calc R . .
C36 C 0.2205(13) 0.3559(18) 0.1567(4) 0.073(6) Uani 1 1 d . . .
H36 H 0.2343 0.4327 0.1564 0.088 Uiso 1 1 calc R . .
C22 C 0.4769(19) -0.1146(16) 0.1188(8) 0.135(11) Uani 1 1 d . . .
H22A H 0.4021 -0.0998 0.1323 0.203 Uiso 1 1 calc R . .
H22B H 0.5043 -0.1868 0.1233 0.203 Uiso 1 1 calc R . .
H22C H 0.4524 -0.1039 0.0916 0.203 Uiso 1 1 calc R . .
C23 C 0.655(2) -0.0831(18) 0.1694(7) 0.122(9) Uani 1 1 d . . .
H23A H 0.7214 -0.0326 0.1792 0.182 Uiso 1 1 calc R . .
H23B H 0.6965 -0.1498 0.1653 0.182 Uiso 1 1 calc R . .
H23C H 0.5922 -0.0919 0.1876 0.182 Uiso 1 1 calc R . .
C24 C 0.465(3) 0.1507(18) 0.2416(5) 0.109(9) Uani 1 1 d . . .
H24 H 0.3745 0.1755 0.2430 0.131 Uiso 1 1 calc R . .
C26 C 0.517(3) 0.2273(18) 0.2659(6) 0.141(11) Uani 1 1 d . . .
H26A H 0.4561 0.2434 0.2841 0.211 Uiso 1 1 calc R . .
H26B H 0.5329 0.2898 0.2515 0.211 Uiso 1 1 calc R . .
H26C H 0.5995 0.2030 0.2795 0.211 Uiso 1 1 calc R . .
C30 C 0.534(3) 0.549(2) 0.2134(7) 0.115(9) Uani 1 1 d . . .
H30 H 0.4793 0.5100 0.2297 0.138 Uiso 1 1 calc R . .
C28 C 0.7587(17) 0.258(3) 0.1866(6) 0.176(16) Uani 1 1 d . . .
H28A H 0.7362 0.3190 0.2009 0.264 Uiso 1 1 calc R . .
H28B H 0.8533 0.2483 0.1901 0.264 Uiso 1 1 calc R . .
H28C H 0.7167 0.1964 0.1959 0.264 Uiso 1 1 calc R . .
C33 C 0.721(3) 0.5428(16) 0.0873(9) 0.157(15) Uani 1 1 d D . .
H33 H 0.7499 0.5014 0.0661 0.189 Uiso 1 1 calc R . .
C38 C 0.197(2) 0.348(3) 0.1908(6) 0.187(17) Uani 1 1 d . . .
H38A H 0.2727 0.3165 0.2060 0.280 Uiso 1 1 calc R . .
H38B H 0.1208 0.3039 0.1920 0.280 Uiso 1 1 calc R . .
H38C H 0.1812 0.4168 0.2008 0.280 Uiso 1 1 calc R . .
C9 C 0.5515(14) 0.3308(11) 0.0171(4) 0.048(4) Uani 1 1 d . . .
H9A H 0.5033 0.3754 -0.0024 0.057 Uiso 1 1 calc R . .
H9B H 0.6206 0.3735 0.0311 0.057 Uiso 1 1 calc R . .
C12 C 0.5072(13) 0.1183(10) 0.0351(4) 0.044(4) Uani 1 1 d . . .
H12A H 0.4392 0.0715 0.0228 0.053 Uiso 1 1 calc R . .
H12B H 0.5591 0.0782 0.0553 0.053 Uiso 1 1 calc R . .
C11 C 0.597(2) 0.1511(14) 0.0056(6) 0.108(9) Uani 1 1 d . . .
H11A H 0.6843 0.1219 0.0138 0.129 Uiso 1 1 calc R . .
H11B H 0.5647 0.1162 -0.0184 0.129 Uiso 1 1 calc R . .
C13 C 0.444(2) 0.2029(14) 0.0525(6) 0.108(10) Uani 1 1 d . . .
C8 C 0.457(3) 0.2932(15) 0.0447(8) 0.159(15) Uani 1 1 d . . .
C10 C 0.613(3) 0.2439(13) -0.0018(8) 0.160(15) Uani 1 1 d . . .
H10A H 0.5855 0.2519 -0.0292 0.192 Uiso 1 1 calc R . .
H10B H 0.7077 0.2566 0.0021 0.192 Uiso 1 1 calc R . .
C25 C 0.437(3) 0.057(2) 0.2525(7) 0.198(17) Uani 1 1 d . . .
H25A H 0.4512 0.0071 0.2326 0.297 Uiso 1 1 calc R . .
H25B H 0.3464 0.0544 0.2574 0.297 Uiso 1 1 calc R . .
H25C H 0.4940 0.0392 0.2756 0.297 Uiso 1 1 calc R . .
C31 C 0.659(3) 0.535(4) 0.2305(9) 0.25(3) Uani 1 1 d . . .
H31A H 0.7181 0.5806 0.2188 0.378 Uiso 1 1 calc R . .
H31B H 0.6843 0.4625 0.2275 0.378 Uiso 1 1 calc R . .
H31C H 0.6625 0.5513 0.2575 0.378 Uiso 1 1 calc R . .
C35 C 0.685(3) 0.639(2) 0.0776(9) 0.209(18) Uani 1 1 d . . .
H35A H 0.7359 0.6879 0.0943 0.314 Uiso 1 1 calc R . .
H35B H 0.5926 0.6474 0.0797 0.314 Uiso 1 1 calc R . .
H35C H 0.7015 0.6513 0.0514 0.314 Uiso 1 1 calc R . .
C34 C 0.828(3) 0.571(4) 0.1167(11) 0.61(8) Uani 1 1 d D . .
H34A H 0.8415 0.5154 0.1354 0.911 Uiso 1 1 calc R . .
H34B H 0.8061 0.6355 0.1291 0.911 Uiso 1 1 calc R . .
H34C H 0.9082 0.5816 0.1050 0.911 Uiso 1 1 calc R . .
C32 C 0.479(5) 0.643(3) 0.2104(9) 0.33(4) Uani 1 1 d . . .
H32A H 0.4289 0.6503 0.1855 0.494 Uiso 1 1 calc R . .
H32B H 0.5470 0.6965 0.2136 0.494 Uiso 1 1 calc R . .
H32C H 0.4213 0.6513 0.2301 0.494 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 O6 1.887(11) . ?
Zr1 O7 1.926(10) . ?
Zr1 O1 2.062(9) . ?
Zr1 O5 2.143(9) . ?
Zr1 O8 2.160(8) . ?
Zr1 N1 2.479(15) . ?
Zr1 Zr2 3.496(2) . ?
Zr2 O4 1.885(10) . ?
Zr2 O3 1.927(10) . ?
Zr2 O2 2.050(8) . ?
Zr2 O5 2.161(8) . ?
Zr2 O8 2.172(9) . ?
Zr2 N2 2.472(13) . ?
Br1 C2 1.869(13) . ?
Br3 C17 1.917(13) . ?
Br2 C4 1.931(14) . ?
Br4 C19 1.868(14) . ?
O1 C1 1.292(14) . ?
C4 C3 1.346(19) . ?
C4 C5 1.350(19) . ?
C1 C2 1.402(17) . ?
C1 C6 1.426(18) . ?
C6 C5 1.394(19) . ?
C6 C7 1.447(19) . ?
C2 C3 1.392(18) . ?
C5 H5 0.9500 . ?
C3 H3 0.9500 . ?
C7 N1 1.267(18) . ?
C7 H7 0.9500 . ?
N1 C8 1.50(2) . ?
C15 C16 1.386(18) . ?
C15 C20 1.438(19) . ?
C15 C14 1.466(19) . ?
C18 C19 1.351(18) . ?
C18 C17 1.392(19) . ?
C18 H18 0.9500 . ?
C17 C16 1.354(18) . ?
C16 H16 0.9500 . ?
C20 O2 1.289(15) . ?
C20 C19 1.418(17) . ?
N2 C14 1.287(18) . ?
N2 C13 1.494(18) . ?
C14 H14 0.9500 . ?
O8 C36 1.452(16) . ?
O5 C27 1.441(16) . ?
O4 C24 1.389(19) . ?
O3 C21 1.417(18) . ?
O6 C30 1.43(3) . ?
O7 C33 1.39(2) . ?
C37 C36 1.498(19) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C29 C27 1.47(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C27 C28 1.35(2) . ?
C27 H27 1.0000 . ?
C21 C22 1.48(2) . ?
C21 C23 1.51(3) . ?
C21 H21 1.0000 . ?
C36 C38 1.27(2) . ?
C36 H36 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.31(3) . ?
C24 C26 1.38(3) . ?
C24 H24 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C30 C32 1.33(3) . ?
C30 C31 1.37(3) . ?
C30 H30 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C33 C35 1.32(3) . ?
C33 C34 1.480(2) . ?
C33 H33 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C9 C10 1.49(2) . ?
C9 C8 1.55(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C12 C13 1.45(2) . ?
C12 C11 1.548(19) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 C10 1.24(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C8 1.21(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?



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
















































































































































































































































O6 Zr1 O7 100.6(6) . . ?
O6 Zr1 O1 93.1(4) . . ?
O7 Zr1 O1 100.6(4) . . ?
O6 Zr1 O5 99.4(4) . . ?
O7 Zr1 O5 92.8(4) . . ?
O1 Zr1 O5 159.7(3) . . ?
O6 Zr1 O8 96.0(4) . . ?
O7 Zr1 O8 159.3(5) . . ?
O1 Zr1 O8 90.8(3) . . ?
O5 Zr1 O8 72.1(3) . . ?
O6 Zr1 N1 169.1(4) . . ?
O7 Zr1 N1 83.9(5) . . ?
O1 Zr1 N1 76.3(4) . . ?
O5 Zr1 N1 90.3(4) . . ?
O8 Zr1 N1 82.0(4) . . ?
O6 Zr1 Zr2 101.2(3) . . ?
O7 Zr1 Zr2 126.7(3) . . ?
O1 Zr1 Zr2 125.9(3) . . ?
O5 Zr1 Zr2 35.8(2) . . ?
O8 Zr1 Zr2 36.3(2) . . ?
N1 Zr1 Zr2 83.7(3) . . ?
O4 Zr2 O3 101.5(5) . . ?
O4 Zr2 O2 93.0(4) . . ?
O3 Zr2 O2 97.3(4) . . ?
O4 Zr2 O5 100.5(4) . . ?
O3 Zr2 O5 94.6(4) . . ?
O2 Zr2 O5 159.8(4) . . ?
O4 Zr2 O8 96.8(4) . . ?
O3 Zr2 O8 158.8(4) . . ?
O2 Zr2 O8 92.2(4) . . ?
O5 Zr2 O8 71.5(3) . . ?
O4 Zr2 N2 169.0(4) . . ?
O3 Zr2 N2 82.4(5) . . ?
O2 Zr2 N2 76.3(4) . . ?
O5 Zr2 N2 89.3(3) . . ?
O8 Zr2 N2 81.5(4) . . ?
O4 Zr2 Zr1 102.3(3) . . ?
O3 Zr2 Zr1 127.8(3) . . ?
O2 Zr2 Zr1 126.8(3) . . ?
O5 Zr2 Zr1 35.5(2) . . ?
O8 Zr2 Zr1 36.1(2) . . ?
N2 Zr2 Zr1 82.8(3) . . ?
C1 O1 Zr1 144.8(8) . . ?
C3 C4 C5 123.4(14) . . ?
C3 C4 Br2 118.4(11) . . ?
C5 C4 Br2 118.0(12) . . ?
O1 C1 C2 121.9(12) . . ?
O1 C1 C6 121.3(11) . . ?
C2 C1 C6 116.8(12) . . ?
C5 C6 C1 119.7(12) . . ?
C5 C6 C7 117.0(13) . . ?
C1 C6 C7 123.3(13) . . ?
C3 C2 C1 121.9(12) . . ?
C3 C2 Br1 119.4(10) . . ?
C1 C2 Br1 118.7(10) . . ?
C4 C5 C6 119.7(13) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C4 C3 C2 118.3(12) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
N1 C7 C6 128.8(15) . . ?
N1 C7 H7 115.6 . . ?
C6 C7 H7 115.6 . . ?
C7 N1 C8 111.4(17) . . ?
C7 N1 Zr1 125.4(10) . . ?
C8 N1 Zr1 123.0(15) . . ?
C16 C15 C20 120.9(13) . . ?
C16 C15 C14 117.0(13) . . ?
C20 C15 C14 122.0(12) . . ?
C19 C18 C17 117.6(13) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C16 C17 C18 122.8(13) . . ?
C16 C17 Br3 120.4(11) . . ?
C18 C17 Br3 116.7(10) . . ?
C17 C16 C15 119.5(14) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
O2 C20 C19 122.7(12) . . ?
O2 C20 C15 122.1(11) . . ?
C19 C20 C15 115.1(12) . . ?
C20 O2 Zr2 145.1(8) . . ?
C18 C19 C20 124.1(13) . . ?
C18 C19 Br4 120.0(10) . . ?
C20 C19 Br4 115.9(10) . . ?
C14 N2 C13 110.9(14) . . ?
C14 N2 Zr2 126.3(9) . . ?
C13 N2 Zr2 122.6(12) . . ?
N2 C14 C15 127.7(13) . . ?
N2 C14 H14 116.1 . . ?
C15 C14 H14 116.1 . . ?
C36 O8 Zr1 123.5(10) . . ?
C36 O8 Zr2 126.5(10) . . ?
Zr1 O8 Zr2 107.6(3) . . ?
C27 O5 Zr1 125.1(9) . . ?
C27 O5 Zr2 123.0(10) . . ?
Zr1 O5 Zr2 108.6(3) . . ?
C24 O4 Zr2 167.9(12) . . ?
C21 O3 Zr2 165.6(9) . . ?
C30 O6 Zr1 169.3(13) . . ?
C33 O7 Zr1 171.8(15) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C27 O5 117.3(17) . . ?
C28 C27 C29 121.7(17) . . ?
O5 C27 C29 112.9(14) . . ?
C28 C27 H27 99.6 . . ?
O5 C27 H27 99.6 . . ?
C29 C27 H27 99.6 . . ?
O3 C21 C22 110.3(15) . . ?
O3 C21 C23 107.7(16) . . ?
C22 C21 C23 110.3(18) . . ?
O3 C21 H21 109.5 . . ?
C22 C21 H21 109.5 . . ?
C23 C21 H21 109.5 . . ?
C38 C36 O8 123.9(16) . . ?
C38 C36 C37 122.3(17) . . ?
O8 C36 C37 108.6(12) . . ?
C38 C36 H36 97.6 . . ?
O8 C36 H36 97.6 . . ?
C37 C36 H36 97.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 124(2) . . ?
C25 C24 O4 120(2) . . ?
C26 C24 O4 116.2(18) . . ?
C25 C24 H24 92.2 . . ?
C26 C24 H24 92.2 . . ?
O4 C24 H24 92.2 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C30 C31 122(3) . . ?
C32 C30 O6 114(2) . . ?
C31 C30 O6 107(2) . . ?
C32 C30 H30 103.9 . . ?
C31 C30 H30 103.9 . . ?
O6 C30 H30 103.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C35 C33 O7 113(2) . . ?
C35 C33 C34 97(2) . . ?
O7 C33 C34 105(2) . . ?
C35 C33 H33 113.5 . . ?
O7 C33 H33 113.5 . . ?
C34 C33 H33 113.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C10 C9 C8 112.9(13) . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C13 C12 C11 115.1(13) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C10 C11 C12 120.9(16) . . ?
C10 C11 H11A 107.1 . . ?
C12 C11 H11A 107.1 . . ?
C10 C11 H11B 107.1 . . ?
C12 C11 H11B 107.1 . . ?
H11A C11 H11B 106.8 . . ?
C8 C13 C12 124.0(14) . . ?
C8 C13 N2 123.5(16) . . ?
C12 C13 N2 112.4(14) . . ?
C13 C8 N1 125.8(15) . . ?
C13 C8 C9 123.0(15) . . ?
N1 C8 C9 110.5(14) . . ?
C11 C10 C9 123.8(16) . . ?
C11 C10 H10A 106.4 . . ?
C9 C10 H10A 106.4 . . ?
C11 C10 H10B 106.4 . . ?
C9 C10 H10B 106.4 . . ?
H10A C10 H10B 106.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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

























































































































































































































O6 Zr1 Zr2 O4 0.3(4) . . . . ?
O7 Zr1 Zr2 O4 112.7(6) . . . . ?
O1 Zr1 Zr2 O4 -101.9(4) . . . . ?
O5 Zr1 Zr2 O4 90.9(5) . . . . ?
O8 Zr1 Zr2 O4 -84.6(5) . . . . ?
N1 Zr1 Zr2 O4 -169.8(4) . . . . ?
O6 Zr1 Zr2 O3 -115.0(6) . . . . ?
O7 Zr1 Zr2 O3 -2.6(7) . . . . ?
O1 Zr1 Zr2 O3 142.8(5) . . . . ?
O5 Zr1 Zr2 O3 -24.4(6) . . . . ?
O8 Zr1 Zr2 O3 160.1(6) . . . . ?
N1 Zr1 Zr2 O3 74.9(5) . . . . ?
O6 Zr1 Zr2 O2 103.6(5) . . . . ?
O7 Zr1 Zr2 O2 -144.0(6) . . . . ?
O1 Zr1 Zr2 O2 1.4(5) . . . . ?
O5 Zr1 Zr2 O2 -165.8(5) . . . . ?
O8 Zr1 Zr2 O2 18.7(5) . . . . ?
N1 Zr1 Zr2 O2 -66.5(4) . . . . ?
O6 Zr1 Zr2 O5 -90.6(5) . . . . ?
O7 Zr1 Zr2 O5 21.8(7) . . . . ?
O1 Zr1 Zr2 O5 167.3(5) . . . . ?
O8 Zr1 Zr2 O5 -175.5(5) . . . . ?
N1 Zr1 Zr2 O5 99.3(5) . . . . ?
O6 Zr1 Zr2 O8 84.9(5) . . . . ?
O7 Zr1 Zr2 O8 -162.7(7) . . . . ?
O1 Zr1 Zr2 O8 -17.2(5) . . . . ?
O5 Zr1 Zr2 O8 175.5(5) . . . . ?
N1 Zr1 Zr2 O8 -85.2(5) . . . . ?
O6 Zr1 Zr2 N2 170.4(4) . . . . ?
O7 Zr1 Zr2 N2 -77.2(6) . . . . ?
O1 Zr1 Zr2 N2 68.2(4) . . . . ?
O5 Zr1 Zr2 N2 -99.0(5) . . . . ?
O8 Zr1 Zr2 N2 85.5(5) . . . . ?
N1 Zr1 Zr2 N2 0.3(4) . . . . ?
O6 Zr1 O1 C1 178.6(15) . . . . ?
O7 Zr1 O1 C1 77.3(15) . . . . ?
O5 Zr1 O1 C1 -53(2) . . . . ?
O8 Zr1 O1 C1 -85.3(15) . . . . ?
N1 Zr1 O1 C1 -3.7(14) . . . . ?
Zr2 Zr1 O1 C1 -75.2(15) . . . . ?
Zr1 O1 C1 C2 -179.8(10) . . . . ?
Zr1 O1 C1 C6 2(2) . . . . ?
O1 C1 C6 C5 -177.7(12) . . . . ?
C2 C1 C6 C5 3.7(19) . . . . ?
O1 C1 C6 C7 1(2) . . . . ?
C2 C1 C6 C7 -177.2(13) . . . . ?
O1 C1 C2 C3 176.5(12) . . . . ?
C6 C1 C2 C3 -4.9(19) . . . . ?
O1 C1 C2 Br1 -3.5(17) . . . . ?
C6 C1 C2 Br1 175.1(10) . . . . ?
C3 C4 C5 C6 -1(2) . . . . ?
Br2 C4 C5 C6 173.8(11) . . . . ?
C1 C6 C5 C4 -1(2) . . . . ?
C7 C6 C5 C4 179.9(13) . . . . ?
C5 C4 C3 C2 0(2) . . . . ?
Br2 C4 C3 C2 -174.9(10) . . . . ?
C1 C2 C3 C4 3(2) . . . . ?
Br1 C2 C3 C4 -176.7(10) . . . . ?
C5 C6 C7 N1 180.0(15) . . . . ?
C1 C6 C7 N1 1(2) . . . . ?
C6 C7 N1 C8 -179.5(15) . . . . ?
C6 C7 N1 Zr1 -5(2) . . . . ?
O6 Zr1 N1 C7 17(3) . . . . ?
O7 Zr1 N1 C7 -97.8(13) . . . . ?
O1 Zr1 N1 C7 4.6(12) . . . . ?
O5 Zr1 N1 C7 169.4(12) . . . . ?
O8 Zr1 N1 C7 97.5(13) . . . . ?
Zr2 Zr1 N1 C7 134.0(12) . . . . ?
O6 Zr1 N1 C8 -169(2) . . . . ?
O7 Zr1 N1 C8 76.4(12) . . . . ?
O1 Zr1 N1 C8 178.9(13) . . . . ?
O5 Zr1 N1 C8 -16.4(12) . . . . ?
O8 Zr1 N1 C8 -88.3(12) . . . . ?
Zr2 Zr1 N1 C8 -51.7(12) . . . . ?
C19 C18 C17 C16 0(2) . . . . ?
C19 C18 C17 Br3 -179.0(10) . . . . ?
C18 C17 C16 C15 0(2) . . . . ?
Br3 C17 C16 C15 179.6(10) . . . . ?
C20 C15 C16 C17 0(2) . . . . ?
C14 C15 C16 C17 176.1(13) . . . . ?
C16 C15 C20 O2 -177.6(13) . . . . ?
C14 C15 C20 O2 7(2) . . . . ?
C16 C15 C20 C19 -1(2) . . . . ?
C14 C15 C20 C19 -177.0(13) . . . . ?
C19 C20 O2 Zr2 173.5(11) . . . . ?
C15 C20 O2 Zr2 -10(3) . . . . ?
O4 Zr2 O2 C20 -175.5(17) . . . . ?
O3 Zr2 O2 C20 -73.4(17) . . . . ?
O5 Zr2 O2 C20 52(2) . . . . ?
O8 Zr2 O2 C20 87.7(17) . . . . ?
N2 Zr2 O2 C20 6.9(17) . . . . ?
Zr1 Zr2 O2 C20 76.8(17) . . . . ?
C17 C18 C19 C20 -2(2) . . . . ?
C17 C18 C19 Br4 179.9(10) . . . . ?
O2 C20 C19 C18 178.3(13) . . . . ?
C15 C20 C19 C18 2(2) . . . . ?
O2 C20 C19 Br4 -3.1(19) . . . . ?
C15 C20 C19 Br4 -179.4(10) . . . . ?
O4 Zr2 N2 C14 -14(3) . . . . ?
O3 Zr2 N2 C14 97.8(14) . . . . ?
O2 Zr2 N2 C14 -1.7(13) . . . . ?
O5 Zr2 N2 C14 -167.5(14) . . . . ?
O8 Zr2 N2 C14 -96.0(14) . . . . ?
Zr1 Zr2 N2 C14 -132.5(14) . . . . ?
O4 Zr2 N2 C13 172(2) . . . . ?
O3 Zr2 N2 C13 -76.0(13) . . . . ?
O2 Zr2 N2 C13 -175.5(13) . . . . ?
O5 Zr2 N2 C13 18.7(13) . . . . ?
O8 Zr2 N2 C13 90.1(13) . . . . ?
Zr1 Zr2 N2 C13 53.7(12) . . . . ?
C13 N2 C14 C15 176.0(16) . . . . ?
Zr2 N2 C14 C15 2(2) . . . . ?
C16 C15 C14 N2 -179.4(15) . . . . ?
C20 C15 C14 N2 -3(3) . . . . ?
O6 Zr1 O8 C36 62.6(10) . . . . ?
O7 Zr1 O8 C36 -154.4(13) . . . . ?
O1 Zr1 O8 C36 -30.6(9) . . . . ?
O5 Zr1 O8 C36 160.6(10) . . . . ?
N1 Zr1 O8 C36 -106.6(9) . . . . ?
Zr2 Zr1 O8 C36 163.3(11) . . . . ?
O6 Zr1 O8 Zr2 -100.7(4) . . . . ?
O7 Zr1 O8 Zr2 42.2(13) . . . . ?
O1 Zr1 O8 Zr2 166.1(4) . . . . ?
O5 Zr1 O8 Zr2 -2.8(3) . . . . ?
N1 Zr1 O8 Zr2 90.1(4) . . . . ?
O4 Zr2 O8 C36 -61.1(10) . . . . ?
O3 Zr2 O8 C36 149.0(12) . . . . ?
O2 Zr2 O8 C36 32.2(10) . . . . ?
O5 Zr2 O8 C36 -159.9(10) . . . . ?
N2 Zr2 O8 C36 107.9(10) . . . . ?
Zr1 Zr2 O8 C36 -162.7(11) . . . . ?
O4 Zr2 O8 Zr1 101.6(4) . . . . ?
O3 Zr2 O8 Zr1 -48.3(11) . . . . ?
O2 Zr2 O8 Zr1 -165.1(4) . . . . ?
O5 Zr2 O8 Zr1 2.8(3) . . . . ?
N2 Zr2 O8 Zr1 -89.4(4) . . . . ?
O6 Zr1 O5 C27 -63.9(12) . . . . ?
O7 Zr1 O5 C27 37.3(13) . . . . ?
O1 Zr1 O5 C27 168.9(13) . . . . ?
O8 Zr1 O5 C27 -157.2(12) . . . . ?
N1 Zr1 O5 C27 121.2(12) . . . . ?
Zr2 Zr1 O5 C27 -160.0(14) . . . . ?
O6 Zr1 O5 Zr2 96.1(5) . . . . ?
O7 Zr1 O5 Zr2 -162.7(5) . . . . ?
O1 Zr1 O5 Zr2 -31.0(12) . . . . ?
O8 Zr1 O5 Zr2 2.8(3) . . . . ?
N1 Zr1 O5 Zr2 -78.8(4) . . . . ?
O4 Zr2 O5 C27 64.1(12) . . . . ?
O3 Zr2 O5 C27 -38.6(12) . . . . ?
O2 Zr2 O5 C27 -164.8(12) . . . . ?
O8 Zr2 O5 C27 157.8(12) . . . . ?
N2 Zr2 O5 C27 -121.0(12) . . . . ?
Zr1 Zr2 O5 C27 160.6(13) . . . . ?
O4 Zr2 O5 Zr1 -96.5(4) . . . . ?
O3 Zr2 O5 Zr1 160.9(5) . . . . ?
O2 Zr2 O5 Zr1 34.6(13) . . . . ?
O8 Zr2 O5 Zr1 -2.8(3) . . . . ?
N2 Zr2 O5 Zr1 78.5(5) . . . . ?
O3 Zr2 O4 C24 -54(7) . . . . ?
O2 Zr2 O4 C24 44(7) . . . . ?
O5 Zr2 O4 C24 -151(6) . . . . ?
O8 Zr2 O4 C24 136(7) . . . . ?
N2 Zr2 O4 C24 56(7) . . . . ?
Zr1 Zr2 O4 C24 173(6) . . . . ?
O4 Zr2 O3 C21 79(5) . . . . ?
O2 Zr2 O3 C21 -16(5) . . . . ?
O5 Zr2 O3 C21 -179(100) . . . . ?
O8 Zr2 O3 C21 -132(5) . . . . ?
N2 Zr2 O3 C21 -91(5) . . . . ?
Zr1 Zr2 O3 C21 -166(5) . . . . ?
O7 Zr1 O6 C30 92(7) . . . . ?
O1 Zr1 O6 C30 -10(7) . . . . ?
O5 Zr1 O6 C30 -174(7) . . . . ?
O8 Zr1 O6 C30 -101(7) . . . . ?
N1 Zr1 O6 C30 -22(8) . . . . ?
Zr2 Zr1 O6 C30 -137(7) . . . . ?
O6 Zr1 O7 C33 -101(11) . . . . ?
O1 Zr1 O7 C33 -6(11) . . . . ?
O5 Zr1 O7 C33 159(11) . . . . ?
O8 Zr1 O7 C33 117(11) . . . . ?
N1 Zr1 O7 C33 69(11) . . . . ?
Zr2 Zr1 O7 C33 146(11) . . . . ?
Zr1 O5 C27 C28 97(2) . . . . ?
Zr2 O5 C27 C28 -60(2) . . . . ?
Zr1 O5 C27 C29 -113.8(13) . . . . ?
Zr2 O5 C27 C29 88.8(17) . . . . ?
Zr2 O3 C21 C22 31(6) . . . . ?
Zr2 O3 C21 C23 -90(5) . . . . ?
Zr1 O8 C36 C38 -105(3) . . . . ?
Zr2 O8 C36 C38 55(3) . . . . ?
Zr1 O8 C36 C37 100.6(14) . . . . ?
Zr2 O8 C36 C37 -99.3(14) . . . . ?
Zr2 O4 C24 C25 3(9) . . . . ?
Zr2 O4 C24 C26 175(5) . . . . ?
Zr1 O6 C30 C32 -7(9) . . . . ?
Zr1 O6 C30 C31 -144(6) . . . . ?
Zr1 O7 C33 C35 21(13) . . . . ?
Zr1 O7 C33 C34 125(12) . . . . ?
C13 C12 C11 C10 1(4) . . . . ?
C11 C12 C13 C8 1(4) . . . . ?
C11 C12 C13 N2 -178.3(18) . . . . ?
C14 N2 C13 C8 107(3) . . . . ?
Zr2 N2 C13 C8 -78(4) . . . . ?
C14 N2 C13 C12 -74(2) . . . . ?
Zr2 N2 C13 C12 101.0(16) . . . . ?
C12 C13 C8 N1 -174(2) . . . . ?
N2 C13 C8 N1 6(5) . . . . ?
C12 C13 C8 C9 -5(5) . . . . ?
N2 C13 C8 C9 175(2) . . . . ?
C7 N1 C8 C13 -116(4) . . . . ?
Zr1 N1 C8 C13 69(4) . . . . ?
C7 N1 C8 C9 74(3) . . . . ?
Zr1 N1 C8 C9 -100.9(18) . . . . ?
C10 C9 C8 C13 6(4) . . . . ?
C10 C9 C8 N1 177(2) . . . . ?
C12 C11 C10 C9 2(5) . . . . ?
C8 C9 C10 C11 -5(4) . . . . ?



_diffrn_measured_fraction_theta_max 0.953

_diffrn_reflns_theta_full        22.58

_diffrn_measured_fraction_theta_full 0.953

_refine_diff_density_max         1.082

_refine_diff_density_min         -0.731

_refine_diff_density_rms         0.135

_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:  Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.

;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.58 Degree
RESPONSE: Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.
 
;
_vrf_PLAT213_I                   
;
PROBLEM: Atom C8              has ADP max/min Ratio .....        7.2 prolat
RESPONSE:  : This alarm is due to the elongated ADPs of carbon 
atoms which suggest that these are probably disordered between two 
orientations. 

;
_vrf_PLAT222_I                   
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       10.0 Ratio 
RESPONSE: This alarm is due to the elongated ADPs of carbon 
atoms which suggest that these are probably disordered between two 
orientations.  
;
_vrf_PLAT234_I                   
;
PROBLEM: Large Hirshfeld Difference C33    --  C34     ..       0.53 Ang.  
RESPONSE: This alarm is due to the elongated ADPs of carbon 
atoms which suggest that these are probably disordered between two 
orientations.  
;
_vrf_PLAT412_I                   
;
PROBLEM: Short Intra XH3 .. XHn     H24    ..  H25B    ..       1.68 Ang.  
RESPONSE:  This alarm is due to the elongated ADPs of carbon 
atoms which suggest that these are probably disordered between two 
orientations. 
;
# end Validation Reply Form
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_Hf2
_database_code_depnum_ccdc_archive 'CCDC 1815603'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C40 H32 Cl8 Hf N4 O4 '

_chemical_formula_sum            'C40 H32 Cl8 Hf N4 O4'


_chemical_formula_weight         1094.79



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source












C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Tetragonal

_symmetry_space_group_name_H-M   P-42(1)c

_symmetry_space_group_name_Hall  'P -4 2n '

loop_

_symmetry_equiv_pos_as_xyz








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



_cell_length_a                   11.3471(2)

_cell_length_b                   11.3471(2)

_cell_length_c                   16.1552(5)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     2080.09(8)

_cell_formula_units_Z            2

_cell_measurement_temperature    298(2)

_cell_measurement_reflns_used    4626

_cell_measurement_theta_min      2.54

_cell_measurement_theta_max      28.34



_exptl_crystal_description       Rectangular
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.748

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1080

_exptl_absorpt_coefficient_mu    3.068

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.4131

_exptl_absorpt_correction_T_max  0.7489

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      298(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 APEXII 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            6745

_diffrn_reflns_av_R_equivalents  0.0211

_diffrn_reflns_av_sigmaI/netI    0.0374

_diffrn_reflns_limit_h_min       -10

_diffrn_reflns_limit_h_max       15

_diffrn_reflns_limit_k_min       -13

_diffrn_reflns_limit_k_max       13

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       20

_diffrn_reflns_theta_min         2.19

_diffrn_reflns_theta_max         28.39

_reflns_number_total             2335

_reflns_number_gt                1985

_reflns_threshold_expression     >2sigma(I)




_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'


_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)+(0.1000P)²+1.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -0.02(2)

_refine_ls_number_reflns         2335

_refine_ls_number_parameters     129

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0301

_refine_ls_R_factor_gt           0.0218

_refine_ls_wR_factor_ref         0.0835

_refine_ls_wR_factor_gt          0.0713

_refine_ls_goodness_of_fit_ref   0.650

_refine_ls_restrained_S_all      0.650

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group























C1 C 0.0668(3) 0.7269(3) -0.0227(2) 0.0268(7) Uani 1 1 d . . .
C2 C 0.0907(3) 0.6985(3) 0.0603(2) 0.0303(8) Uani 1 1 d . . .
C3 C 0.1384(4) 0.5889(3) 0.0817(3) 0.0399(9) Uani 1 1 d . . .
H3 H 0.1523 0.5708 0.1370 0.048 Uiso 1 1 calc R . .
C4 C 0.1645(4) 0.5087(4) 0.0220(3) 0.0364(8) Uani 1 1 d . . .
C5 C 0.1414(3) 0.5318(3) -0.0600(3) 0.0355(9) Uani 1 1 d . . .
H5 H 0.1584 0.4761 -0.1006 0.043 Uiso 1 1 calc R . .
C6 C 0.0928(3) 0.6384(3) -0.0808(2) 0.0341(8) Uani 1 1 d . . .
C7 C 0.0568(3) 0.7754(3) 0.1272(2) 0.0343(8) Uani 1 1 d . . .
H7 H 0.0666 0.7454 0.1803 0.041 Uiso 1 1 calc R . .
C8 C -0.0245(4) 0.9373(4) 0.2009(3) 0.0285(9) Uani 1 1 d . . .
H8 H -0.1106 0.9431 0.1991 0.034 Uiso 1 1 calc R . .
C9 C 0.0086(5) 0.8706(3) 0.2807(2) 0.0397(9) Uani 1 1 d . . .
H9A H -0.0301 0.7944 0.2811 0.048 Uiso 1 1 calc R . .
H9B H 0.0930 0.8576 0.2820 0.048 Uiso 1 1 calc R . .
C10 C -0.0288(6) 0.9410(5) 0.3575(3) 0.0437(15) Uani 1 1 d . . .
H10A H -0.1138 0.9507 0.3576 0.052 Uiso 1 1 calc R . .
H10B H -0.0067 0.8983 0.4071 0.052 Uiso 1 1 calc R . .
Cl1 Cl 0.22299(10) 0.37126(9) 0.04896(9) 0.0553(3) Uani 1 1 d . . .
Cl2 Cl 0.05540(15) 0.66166(10) -0.18385(7) 0.0652(4) Uani 1 1 d . . .
Hf1 Hf 0.0000 1.0000 0.0000 0.01948(10) Uani 1 4 d S . .
N1 N 0.0146(3) 0.8803(2) 0.12240(17) 0.0257(6) Uani 1 1 d . . .
O1 O 0.0186(2) 0.8271(2) -0.04367(14) 0.0301(5) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag
































C1 O1 1.307(4) . ?
C1 C2 1.404(5) . ?
C1 C6 1.407(5) . ?
C2 C3 1.400(5) . ?
C2 C7 1.441(5) . ?
C3 C4 1.358(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(6) . ?
C4 Cl1 1.750(4) . ?
C5 C6 1.372(6) . ?
C5 H5 0.9300 . ?
C6 Cl2 1.738(4) . ?
C7 N1 1.285(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.491(5) . ?
C8 C8 1.527(9) 2_575 ?
C8 C9 1.541(6) . ?
C8 H8 0.9800 . ?
C9 C10 1.535(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C10 1.489(12) 2_575 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
Hf1 O1 2.096(2) 7_665 ?
Hf1 O1 2.096(2) . ?
Hf1 O1 2.096(2) 2_575 ?
Hf1 O1 2.096(2) 8_465 ?
Hf1 N1 2.405(3) 2_575 ?
Hf1 N1 2.405(3) 8_465 ?
Hf1 N1 2.405(3) . ?
Hf1 N1 2.405(3) 7_665 ?



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 C1 C2 121.9(3) . . ?
O1 C1 C6 122.3(3) . . ?
C2 C1 C6 115.7(3) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 C7 117.1(4) . . ?
C1 C2 C7 121.7(3) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 Cl1 120.1(3) . . ?
C5 C4 Cl1 118.8(3) . . ?
C6 C5 C4 118.7(4) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 123.4(4) . . ?
C5 C6 Cl2 117.8(3) . . ?
C1 C6 Cl2 118.7(3) . . ?
N1 C7 C2 128.0(4) . . ?
N1 C7 H7 116.0 . . ?
C2 C7 H7 116.0 . . ?
N1 C8 C8 107.2(3) . 2_575 ?
N1 C8 C9 115.2(3) . . ?
C8 C8 C9 111.6(3) 2_575 . ?
N1 C8 H8 107.5 . . ?
C8 C8 H8 107.5 2_575 . ?
C9 C8 H8 107.5 . . ?
C10 C9 C8 110.7(4) . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C10 C10 C9 110.2(4) 2_575 . ?
C10 C10 H10A 109.6 2_575 . ?
C9 C10 H10A 109.6 . . ?
C10 C10 H10B 109.6 2_575 . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O1 Hf1 O1 96.51(4) 7_665 . ?
O1 Hf1 O1 96.51(4) 7_665 2_575 ?
O1 Hf1 O1 140.66(13) . 2_575 ?
O1 Hf1 O1 140.66(13) 7_665 8_465 ?
O1 Hf1 O1 96.51(4) . 8_465 ?
O1 Hf1 O1 96.51(4) 2_575 8_465 ?
O1 Hf1 N1 74.40(10) 7_665 2_575 ?
O1 Hf1 N1 144.36(9) . 2_575 ?
O1 Hf1 N1 74.98(9) 2_575 2_575 ?
O1 Hf1 N1 73.46(10) 8_465 2_575 ?
O1 Hf1 N1 144.36(9) 7_665 8_465 ?
O1 Hf1 N1 73.46(10) . 8_465 ?
O1 Hf1 N1 74.40(10) 2_575 8_465 ?
O1 Hf1 N1 74.98(9) 8_465 8_465 ?
N1 Hf1 N1 132.53(8) 2_575 8_465 ?
O1 Hf1 N1 73.46(10) 7_665 . ?
O1 Hf1 N1 74.98(9) . . ?
O1 Hf1 N1 144.36(9) 2_575 . ?
O1 Hf1 N1 74.40(10) 8_465 . ?
N1 Hf1 N1 69.39(13) 2_575 . ?
N1 Hf1 N1 132.53(8) 8_465 . ?
O1 Hf1 N1 74.98(9) 7_665 7_665 ?
O1 Hf1 N1 74.40(10) . 7_665 ?
O1 Hf1 N1 73.46(10) 2_575 7_665 ?
O1 Hf1 N1 144.36(9) 8_465 7_665 ?
N1 Hf1 N1 132.53(8) 2_575 7_665 ?
N1 Hf1 N1 69.39(13) 8_465 7_665 ?
N1 Hf1 N1 132.53(8) . 7_665 ?
C7 N1 C8 117.5(3) . . ?
C7 N1 Hf1 126.7(2) . . ?
C8 N1 Hf1 115.7(2) . . ?
C1 O1 Hf1 140.3(2) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag


















































O1 C1 C2 C3 177.6(3) . . . . ?
C6 C1 C2 C3 0.6(5) . . . . ?
O1 C1 C2 C7 3.8(5) . . . . ?
C6 C1 C2 C7 -173.2(3) . . . . ?
C1 C2 C3 C4 1.3(6) . . . . ?
C7 C2 C3 C4 175.3(4) . . . . ?
C2 C3 C4 C5 -2.1(6) . . . . ?
C2 C3 C4 Cl1 -179.5(3) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
Cl1 C4 C5 C6 178.4(3) . . . . ?
C4 C5 C6 C1 1.0(6) . . . . ?
C4 C5 C6 Cl2 -175.8(3) . . . . ?
O1 C1 C6 C5 -178.7(3) . . . . ?
C2 C1 C6 C5 -1.7(5) . . . . ?
O1 C1 C6 Cl2 -1.9(5) . . . . ?
C2 C1 C6 Cl2 175.1(3) . . . . ?
C3 C2 C7 N1 177.9(4) . . . . ?
C1 C2 C7 N1 -8.1(6) . . . . ?
N1 C8 C9 C10 176.3(4) . . . . ?
C8 C8 C9 C10 53.7(6) 2_575 . . . ?
C8 C9 C10 C10 -58.7(7) . . . 2_575 ?
C2 C7 N1 C8 174.2(4) . . . . ?
C2 C7 N1 Hf1 -8.9(6) . . . . ?
C8 C8 N1 C7 134.2(4) 2_575 . . . ?
C9 C8 N1 C7 9.3(5) . . . . ?
C8 C8 N1 Hf1 -43.0(4) 2_575 . . . ?
C9 C8 N1 Hf1 -168.0(3) . . . . ?
O1 Hf1 N1 C7 -82.1(3) 7_665 . . . ?
O1 Hf1 N1 C7 19.5(3) . . . . ?
O1 Hf1 N1 C7 -159.9(3) 2_575 . . . ?
O1 Hf1 N1 C7 120.9(3) 8_465 . . . ?
N1 Hf1 N1 C7 -161.3(4) 2_575 . . . ?
N1 Hf1 N1 C7 69.3(4) 8_465 . . . ?
N1 Hf1 N1 C7 -31.9(4) 7_665 . . . ?
O1 Hf1 N1 C8 94.8(2) 7_665 . . . ?
O1 Hf1 N1 C8 -163.6(3) . . . . ?
O1 Hf1 N1 C8 17.0(3) 2_575 . . . ?
O1 Hf1 N1 C8 -62.2(2) 8_465 . . . ?
N1 Hf1 N1 C8 15.62(19) 2_575 . . . ?
N1 Hf1 N1 C8 -113.80(19) 8_465 . . . ?
N1 Hf1 N1 C8 145.1(2) 7_665 . . . ?
C2 C1 O1 Hf1 24.6(5) . . . . ?
C6 C1 O1 Hf1 -158.6(3) . . . . ?
O1 Hf1 O1 C1 40.9(3) 7_665 . . . ?
O1 Hf1 O1 C1 149.5(4) 2_575 . . . ?
O1 Hf1 O1 C1 -101.8(4) 8_465 . . . ?
N1 Hf1 O1 C1 -31.3(4) 2_575 . . . ?
N1 Hf1 O1 C1 -174.0(4) 8_465 . . . ?
N1 Hf1 O1 C1 -30.0(3) . . . . ?
N1 Hf1 O1 C1 113.3(4) 7_665 . . . ?



_diffrn_measured_fraction_theta_max 0.957

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.984

_refine_diff_density_max         1.142

_refine_diff_density_min         -0.696

_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_Zr3
_database_code_depnum_ccdc_archive 'CCDC 1815597'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C32 H20 Cl8 N4 O4 Zr'

_chemical_formula_sum            'C32 H20 Cl8 N4 O4 Zr'

_chemical_formula_weight         899.34



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'
Cl Cl 0.1484 0.1585 '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   P2(1)/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                   20.4732(6)

_cell_length_b                   12.5483(4)

_cell_length_c                   13.5794(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 105.4610(10)

_cell_angle_gamma                90.00

_cell_volume                     3362.35(18)

_cell_formula_units_Z            4

_cell_measurement_temperature    298(2)

_cell_measurement_reflns_used    7302

_cell_measurement_theta_min      2.25

_cell_measurement_theta_max      28.48



_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.15

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.777

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1792

_exptl_absorpt_coefficient_mu    1.009

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.834

_exptl_absorpt_correction_T_max  0.934

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      298(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 APEXII 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            24858

_diffrn_reflns_av_R_equivalents  0.0171

_diffrn_reflns_av_sigmaI/netI    0.0220

_diffrn_reflns_limit_h_min       -27

_diffrn_reflns_limit_h_max       27

_diffrn_reflns_limit_k_min       -16

_diffrn_reflns_limit_k_max       16

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       17

_diffrn_reflns_theta_min         1.03

_diffrn_reflns_theta_max         28.53

_reflns_number_total             8358

_reflns_number_gt                7061

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0198P)²+3.2436P] 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         8358

_refine_ls_number_parameters     442

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0356

_refine_ls_R_factor_gt           0.0255

_refine_ls_wR_factor_ref         0.0608

_refine_ls_wR_factor_gt          0.0558

_refine_ls_goodness_of_fit_ref   1.049

_refine_ls_restrained_S_all      1.049

_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





































































C1 C 0.32242(9) 1.04411(14) -0.00925(13) 0.0173(3) Uani 1 1 d . . .
C2 C 0.31103(9) 1.15152(14) -0.04031(13) 0.0186(3) Uani 1 1 d . . .
C3 C 0.36229(9) 1.22547(14) -0.02587(14) 0.0202(4) Uani 1 1 d . . .
H3 H 0.3526 1.2963 -0.0441 0.024 Uiso 1 1 calc R . .
C4 C 0.42873(9) 1.19275(15) 0.01640(14) 0.0212(4) Uani 1 1 d . . .
C5 C 0.44324(9) 1.08885(15) 0.04508(14) 0.0210(4) Uani 1 1 d . . .
H5 H 0.4880 1.0677 0.0719 0.025 Uiso 1 1 calc R . .
C6 C 0.39076(9) 1.01454(14) 0.03402(14) 0.0190(4) Uani 1 1 d . . .
C7 C 0.40834(9) 0.90977(15) 0.07900(15) 0.0215(4) Uani 1 1 d . . .
H7 H 0.4537 0.8899 0.0944 0.026 Uiso 1 1 calc R . .
C8 C 0.39637(9) 0.74875(15) 0.15847(17) 0.0282(5) Uani 1 1 d . . .
H8A H 0.4453 0.7552 0.1812 0.034 Uiso 1 1 calc R . .
H8B H 0.3852 0.6850 0.1170 0.034 Uiso 1 1 calc R . .
C9 C 0.36710(9) 0.74224(15) 0.24941(16) 0.0257(4) Uani 1 1 d . . .
H9A H 0.3839 0.6794 0.2899 0.031 Uiso 1 1 calc R . .
H9B H 0.3796 0.8047 0.2923 0.031 Uiso 1 1 calc R . .
C10 C 0.26433(9) 0.65437(14) 0.23254(14) 0.0194(4) Uani 1 1 d . . .
H10 H 0.2909 0.6074 0.2795 0.023 Uiso 1 1 calc R . .
C11 C 0.19307(9) 0.62847(14) 0.19267(14) 0.0182(3) Uani 1 1 d . . .
C12 C 0.17296(9) 0.52410(15) 0.20509(14) 0.0213(4) Uani 1 1 d . . .
H12 H 0.2046 0.4741 0.2387 0.026 Uiso 1 1 calc R . .
C13 C 0.10616(10) 0.49568(15) 0.16739(15) 0.0231(4) Uani 1 1 d . . .
C14 C 0.05777(9) 0.57001(15) 0.12082(15) 0.0230(4) Uani 1 1 d . . .
H14 H 0.0125 0.5504 0.0962 0.028 Uiso 1 1 calc R . .
C15 C 0.07775(9) 0.67371(15) 0.11148(14) 0.0201(4) Uani 1 1 d . . .
C16 C 0.14626(9) 0.70670(14) 0.14326(13) 0.0173(3) Uani 1 1 d . . .
C17 C 0.31463(9) 1.06059(14) 0.21743(13) 0.0177(3) Uani 1 1 d . . .
C18 C 0.38072(9) 1.09649(15) 0.26632(14) 0.0208(4) Uani 1 1 d . . .
C19 C 0.39784(10) 1.20282(15) 0.27158(14) 0.0229(4) Uani 1 1 d . . .
H19 H 0.4422 1.2237 0.3020 0.027 Uiso 1 1 calc R . .
C20 C 0.34879(10) 1.27868(15) 0.23144(14) 0.0219(4) Uani 1 1 d . . .
C21 C 0.28298(10) 1.24886(15) 0.18690(14) 0.0208(4) Uani 1 1 d . . .
H21 H 0.2500 1.3003 0.1622 0.025 Uiso 1 1 calc R . .
C22 C 0.26585(9) 1.14039(14) 0.17891(13) 0.0180(3) Uani 1 1 d . . .
C23 C 0.19699(9) 1.11224(14) 0.12452(13) 0.0183(3) Uani 1 1 d . . .
H23 H 0.1646 1.1660 0.1137 0.022 Uiso 1 1 calc R . .
C24 C 0.10668(9) 1.01017(15) 0.02922(14) 0.0208(4) Uani 1 1 d . . .
H24A H 0.0842 1.0788 0.0242 0.025 Uiso 1 1 calc R . .
H24B H 0.0823 0.9598 0.0605 0.025 Uiso 1 1 calc R . .
C25 C 0.10857(9) 0.97158(14) -0.07568(14) 0.0211(4) Uani 1 1 d . . .
H25A H 0.0629 0.9601 -0.1181 0.025 Uiso 1 1 calc R . .
H25B H 0.1302 1.0244 -0.1085 0.025 Uiso 1 1 calc R . .
C26 C 0.11851(9) 0.79305(14) -0.11778(14) 0.0184(3) Uani 1 1 d . . .
H26 H 0.0761 0.8056 -0.1623 0.022 Uiso 1 1 calc R . .
C27 C 0.14583(9) 0.68632(14) -0.11752(14) 0.0184(3) Uani 1 1 d . . .
C28 C 0.10358(9) 0.60760(15) -0.17485(14) 0.0211(4) Uani 1 1 d . . .
H28 H 0.0593 0.6241 -0.2106 0.025 Uiso 1 1 calc R . .
C29 C 0.12790(10) 0.50648(15) -0.17780(14) 0.0226(4) Uani 1 1 d . . .
C30 C 0.19497(10) 0.48151(15) -0.12978(15) 0.0250(4) Uani 1 1 d . . .
H30 H 0.2115 0.4132 -0.1346 0.030 Uiso 1 1 calc R . .
C31 C 0.23649(10) 0.55916(15) -0.07517(15) 0.0231(4) Uani 1 1 d . . .
C32 C 0.21338(9) 0.66313(14) -0.06326(13) 0.0177(3) Uani 1 1 d . . .
Cl1 Cl 0.22825(2) 1.19202(3) -0.09445(4) 0.02349(10) Uani 1 1 d . . .
Cl2 Cl 0.49348(3) 1.28651(4) 0.03497(4) 0.03165(11) Uani 1 1 d . . .
Cl3 Cl 0.08198(3) 0.36433(4) 0.18081(5) 0.03545(12) Uani 1 1 d . . .
Cl4 Cl 0.01621(2) 0.76743(4) 0.05781(4) 0.03226(12) Uani 1 1 d . . .
Cl5 Cl 0.44394(2) 1.00462(4) 0.31747(4) 0.03023(11) Uani 1 1 d . . .
Cl6 Cl 0.37257(3) 1.41218(4) 0.23944(4) 0.03382(12) Uani 1 1 d . . .
Cl7 Cl 0.07504(3) 0.40542(4) -0.24324(4) 0.03133(11) Uani 1 1 d . . .
Cl8 Cl 0.32055(3) 0.52835(4) -0.01734(5) 0.04264(15) Uani 1 1 d . . .
N1 N 0.36692(7) 0.84278(12) 0.09906(12) 0.0207(3) Uani 1 1 d . . .
N2 N 0.29332(7) 0.73640(12) 0.20827(12) 0.0182(3) Uani 1 1 d . . .
N3 N 0.17719(7) 1.01934(12) 0.09021(11) 0.0170(3) Uani 1 1 d . . .
N4 N 0.14696(7) 0.87130(11) -0.06303(11) 0.0164(3) Uani 1 1 d . . .
O1 O 0.27203(6) 0.97730(10) -0.01904(10) 0.0184(3) Uani 1 1 d . . .
O2 O 0.16473(6) 0.80428(10) 0.12997(9) 0.0187(3) Uani 1 1 d . . .
O3 O 0.29966(6) 0.95887(10) 0.20709(10) 0.0200(3) Uani 1 1 d . . .
O4 O 0.25304(6) 0.73335(10) -0.00566(10) 0.0198(3) Uani 1 1 d . . .
Zr1 Zr 0.246205(8) 0.867378(13) 0.081105(13) 0.01373(4) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag














































































C1 O1 1.308(2) . ?
C1 C2 1.413(2) . ?
C1 C6 1.415(2) . ?
C2 C3 1.375(3) . ?
C2 Cl1 1.7339(18) . ?
C3 C4 1.390(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(3) . ?
C4 Cl2 1.7399(18) . ?
C5 C6 1.400(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.454(3) . ?
C7 N1 1.274(2) . ?
C7 H7 0.9300 . ?
C8 N1 1.465(2) . ?
C8 C9 1.512(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.466(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.275(2) . ?
C10 C11 1.451(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.397(2) . ?
C11 C16 1.410(2) . ?
C12 C13 1.373(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(3) . ?
C13 Cl3 1.7444(19) . ?
C14 C15 1.380(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.415(2) . ?
C15 Cl4 1.7355(18) . ?
C16 O2 1.308(2) . ?
C17 O3 1.311(2) . ?
C17 C18 1.413(2) . ?
C17 C22 1.412(2) . ?
C18 C19 1.377(3) . ?
C18 Cl5 1.7341(18) . ?
C19 C20 1.386(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.373(3) . ?
C20 Cl6 1.7398(19) . ?
C21 C22 1.403(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.450(2) . ?
C23 N3 1.280(2) . ?
C23 H23 0.9300 . ?
C24 N3 1.465(2) . ?
C24 C25 1.515(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N4 1.469(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.275(2) . ?
C26 C27 1.451(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.404(3) . ?
C27 C32 1.413(2) . ?
C28 C29 1.368(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.390(3) . ?
C29 Cl7 1.7481(19) . ?
C30 C31 1.373(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.412(2) . ?
C31 Cl8 1.7342(19) . ?
C32 O4 1.307(2) . ?
N1 Zr1 2.4374(15) . ?
N2 Zr1 2.3928(14) . ?
N3 Zr1 2.3960(14) . ?
N4 Zr1 2.4170(14) . ?
O1 Zr1 2.1011(12) . ?
O2 Zr1 2.1071(12) . ?
O3 Zr1 2.1082(12) . ?
O4 Zr1 2.0795(12) . ?



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 C1 C2 121.19(16) . . ?
O1 C1 C6 122.67(16) . . ?
C2 C1 C6 116.13(16) . . ?
C3 C2 C1 122.82(17) . . ?
C3 C2 Cl1 119.03(14) . . ?
C1 C2 Cl1 118.10(14) . . ?
C2 C3 C4 119.03(17) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 120.83(17) . . ?
C5 C4 Cl2 120.20(15) . . ?
C3 C4 Cl2 118.96(14) . . ?
C4 C5 C6 120.08(17) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 121.02(17) . . ?
C5 C6 C7 117.41(16) . . ?
C1 C6 C7 121.21(16) . . ?
N1 C7 C6 125.60(16) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
N1 C8 C9 107.39(15) . . ?
N1 C8 H8A 110.2 . . ?
C9 C8 H8A 110.2 . . ?
N1 C8 H8B 110.2 . . ?
C9 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N2 C9 C8 106.50(15) . . ?
N2 C9 H9A 110.4 . . ?
C8 C9 H9A 110.4 . . ?
N2 C9 H9B 110.4 . . ?
C8 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
N2 C10 C11 125.13(16) . . ?
N2 C10 H10 117.4 . . ?
C11 C10 H10 117.4 . . ?
C12 C11 C16 121.70(16) . . ?
C12 C11 C10 117.66(16) . . ?
C16 C11 C10 120.64(16) . . ?
C13 C12 C11 119.65(17) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.03(17) . . ?
C12 C13 Cl3 119.24(15) . . ?
C14 C13 Cl3 119.71(14) . . ?
C15 C14 C13 118.92(17) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 122.81(17) . . ?
C14 C15 Cl4 118.54(14) . . ?
C16 C15 Cl4 118.65(14) . . ?
O2 C16 C11 122.17(15) . . ?
O2 C16 C15 122.09(16) . . ?
C11 C16 C15 115.72(16) . . ?
O3 C17 C18 121.85(16) . . ?
O3 C17 C22 121.90(16) . . ?
C18 C17 C22 116.24(16) . . ?
C19 C18 C17 122.15(17) . . ?
C19 C18 Cl5 118.10(14) . . ?
C17 C18 Cl5 119.70(14) . . ?
C18 C19 C20 119.85(17) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 120.60(17) . . ?
C21 C20 Cl6 121.01(15) . . ?
C19 C20 Cl6 118.39(15) . . ?
C20 C21 C22 119.61(17) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C17 121.46(16) . . ?
C21 C22 C23 117.70(16) . . ?
C17 C22 C23 120.76(16) . . ?
N3 C23 C22 125.27(16) . . ?
N3 C23 H23 117.4 . . ?
C22 C23 H23 117.4 . . ?
N3 C24 C25 106.76(14) . . ?
N3 C24 H24A 110.4 . . ?
C25 C24 H24A 110.4 . . ?
N3 C24 H24B 110.4 . . ?
C25 C24 H24B 110.4 . . ?
H24A C24 H24B 108.6 . . ?
N4 C25 C24 108.11(14) . . ?
N4 C25 H25A 110.1 . . ?
C24 C25 H25A 110.1 . . ?
N4 C25 H25B 110.1 . . ?
C24 C25 H25B 110.1 . . ?
H25A C25 H25B 108.4 . . ?
N4 C26 C27 126.42(16) . . ?
N4 C26 H26 116.8 . . ?
C27 C26 H26 116.8 . . ?
C28 C27 C32 121.12(16) . . ?
C28 C27 C26 117.90(16) . . ?
C32 C27 C26 120.96(16) . . ?
C29 C28 C27 119.59(17) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 121.15(17) . . ?
C28 C29 Cl7 120.47(15) . . ?
C30 C29 Cl7 118.38(14) . . ?
C31 C30 C29 119.04(17) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C30 C31 C32 122.65(17) . . ?
C30 C31 Cl8 118.88(14) . . ?
C32 C31 Cl8 118.47(14) . . ?
O4 C32 C31 121.18(16) . . ?
O4 C32 C27 122.59(16) . . ?
C31 C32 C27 116.23(16) . . ?
C7 N1 C8 116.70(15) . . ?
C7 N1 Zr1 127.59(12) . . ?
C8 N1 Zr1 114.48(11) . . ?
C10 N2 C9 116.45(15) . . ?
C10 N2 Zr1 127.98(12) . . ?
C9 N2 Zr1 114.63(11) . . ?
C23 N3 C24 116.48(14) . . ?
C23 N3 Zr1 127.56(12) . . ?
C24 N3 Zr1 114.46(11) . . ?
C26 N4 C25 116.39(14) . . ?
C26 N4 Zr1 127.68(12) . . ?
C25 N4 Zr1 114.84(10) . . ?
C1 O1 Zr1 133.05(11) . . ?
C16 O2 Zr1 132.63(11) . . ?
C17 O3 Zr1 132.29(11) . . ?
C32 O4 Zr1 139.40(11) . . ?
O4 Zr1 O1 95.61(5) . . ?
O4 Zr1 O2 93.04(5) . . ?
O1 Zr1 O2 143.84(5) . . ?
O4 Zr1 O3 143.27(5) . . ?
O1 Zr1 O3 90.11(5) . . ?
O2 Zr1 O3 103.44(5) . . ?
O4 Zr1 N2 77.19(5) . . ?
O1 Zr1 N2 142.70(5) . . ?
O2 Zr1 N2 73.46(5) . . ?
O3 Zr1 N2 76.48(5) . . ?
O4 Zr1 N3 143.38(5) . . ?
O1 Zr1 N3 76.38(5) . . ?
O2 Zr1 N3 75.85(5) . . ?
O3 Zr1 N3 73.17(5) . . ?
N2 Zr1 N3 129.73(5) . . ?
O4 Zr1 N4 74.13(5) . . ?
O1 Zr1 N4 76.40(5) . . ?
O2 Zr1 N4 72.39(5) . . ?
O3 Zr1 N4 142.06(5) . . ?
N2 Zr1 N4 133.51(5) . . ?
N3 Zr1 N4 69.24(5) . . ?
O4 Zr1 N1 74.61(5) . . ?
O1 Zr1 N1 74.01(5) . . ?
O2 Zr1 N1 141.96(5) . . ?
O3 Zr1 N1 72.22(5) . . ?
N2 Zr1 N1 68.77(5) . . ?
N3 Zr1 N1 133.77(5) . . ?
N4 Zr1 N1 134.00(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






















































































































































































O1 C1 C2 C3 176.16(17) . . . . ?
C6 C1 C2 C3 -2.8(3) . . . . ?
O1 C1 C2 Cl1 -1.3(2) . . . . ?
C6 C1 C2 Cl1 179.68(13) . . . . ?
C1 C2 C3 C4 3.3(3) . . . . ?
Cl1 C2 C3 C4 -179.23(14) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C2 C3 C4 Cl2 -179.80(14) . . . . ?
C3 C4 C5 C6 -1.4(3) . . . . ?
Cl2 C4 C5 C6 177.31(14) . . . . ?
C4 C5 C6 C1 1.8(3) . . . . ?
C4 C5 C6 C7 -171.41(17) . . . . ?
O1 C1 C6 C5 -178.72(17) . . . . ?
C2 C1 C6 C5 0.3(3) . . . . ?
O1 C1 C6 C7 -5.8(3) . . . . ?
C2 C1 C6 C7 173.19(17) . . . . ?
C5 C6 C7 N1 161.37(19) . . . . ?
C1 C6 C7 N1 -11.8(3) . . . . ?
N1 C8 C9 N2 57.97(19) . . . . ?
N2 C10 C11 C12 163.35(19) . . . . ?
N2 C10 C11 C16 -16.7(3) . . . . ?
C16 C11 C12 C13 0.8(3) . . . . ?
C10 C11 C12 C13 -179.17(18) . . . . ?
C11 C12 C13 C14 -2.7(3) . . . . ?
C11 C12 C13 Cl3 178.56(15) . . . . ?
C12 C13 C14 C15 0.8(3) . . . . ?
Cl3 C13 C14 C15 179.57(15) . . . . ?
C13 C14 C15 C16 3.0(3) . . . . ?
C13 C14 C15 Cl4 -177.35(15) . . . . ?
C12 C11 C16 O2 -179.02(17) . . . . ?
C10 C11 C16 O2 1.0(3) . . . . ?
C12 C11 C16 C15 2.7(3) . . . . ?
C10 C11 C16 C15 -177.33(17) . . . . ?
C14 C15 C16 O2 177.05(17) . . . . ?
Cl4 C15 C16 O2 -2.6(2) . . . . ?
C14 C15 C16 C11 -4.6(3) . . . . ?
Cl4 C15 C16 C11 175.73(14) . . . . ?
O3 C17 C18 C19 175.67(18) . . . . ?
C22 C17 C18 C19 -3.4(3) . . . . ?
O3 C17 C18 Cl5 -1.7(3) . . . . ?
C22 C17 C18 Cl5 179.25(14) . . . . ?
C17 C18 C19 C20 2.5(3) . . . . ?
Cl5 C18 C19 C20 179.91(15) . . . . ?
C18 C19 C20 C21 0.4(3) . . . . ?
C18 C19 C20 Cl6 -179.88(15) . . . . ?
C19 C20 C21 C22 -2.2(3) . . . . ?
Cl6 C20 C21 C22 178.10(14) . . . . ?
C20 C21 C22 C17 1.2(3) . . . . ?
C20 C21 C22 C23 -175.45(17) . . . . ?
O3 C17 C22 C21 -177.52(17) . . . . ?
C18 C17 C22 C21 1.5(3) . . . . ?
O3 C17 C22 C23 -1.0(3) . . . . ?
C18 C17 C22 C23 178.04(16) . . . . ?
C21 C22 C23 N3 163.10(18) . . . . ?
C17 C22 C23 N3 -13.6(3) . . . . ?
N3 C24 C25 N4 56.35(18) . . . . ?
N4 C26 C27 C28 172.86(18) . . . . ?
N4 C26 C27 C32 -8.7(3) . . . . ?
C32 C27 C28 C29 0.5(3) . . . . ?
C26 C27 C28 C29 178.95(17) . . . . ?
C27 C28 C29 C30 -3.7(3) . . . . ?
C27 C28 C29 Cl7 176.72(14) . . . . ?
C28 C29 C30 C31 2.6(3) . . . . ?
Cl7 C29 C30 C31 -177.81(16) . . . . ?
C29 C30 C31 C32 1.8(3) . . . . ?
C29 C30 C31 Cl8 -178.83(15) . . . . ?
C30 C31 C32 O4 175.76(18) . . . . ?
Cl8 C31 C32 O4 -3.6(2) . . . . ?
C30 C31 C32 C27 -4.8(3) . . . . ?
Cl8 C31 C32 C27 175.84(14) . . . . ?
C28 C27 C32 O4 -176.95(17) . . . . ?
C26 C27 C32 O4 4.6(3) . . . . ?
C28 C27 C32 C31 3.6(3) . . . . ?
C26 C27 C32 C31 -174.82(17) . . . . ?
C6 C7 N1 C8 -170.91(18) . . . . ?
C6 C7 N1 Zr1 -4.3(3) . . . . ?
C9 C8 N1 C7 126.53(18) . . . . ?
C9 C8 N1 Zr1 -41.80(18) . . . . ?
C11 C10 N2 C9 -174.05(18) . . . . ?
C11 C10 N2 Zr1 -5.8(3) . . . . ?
C8 C9 N2 C10 120.97(18) . . . . ?
C8 C9 N2 Zr1 -48.83(17) . . . . ?
C22 C23 N3 C24 -174.55(17) . . . . ?
C22 C23 N3 Zr1 -9.4(3) . . . . ?
C25 C24 N3 C23 119.31(17) . . . . ?
C25 C24 N3 Zr1 -47.78(16) . . . . ?
C27 C26 N4 C25 -178.97(17) . . . . ?
C27 C26 N4 Zr1 -11.6(3) . . . . ?
C24 C25 N4 C26 128.86(17) . . . . ?
C24 C25 N4 Zr1 -40.19(17) . . . . ?
C2 C1 O1 Zr1 -131.70(15) . . . . ?
C6 C1 O1 Zr1 47.2(2) . . . . ?
C11 C16 O2 Zr1 44.5(2) . . . . ?
C15 C16 O2 Zr1 -137.25(15) . . . . ?
C18 C17 O3 Zr1 -132.55(15) . . . . ?
C22 C17 O3 Zr1 46.4(2) . . . . ?
C31 C32 O4 Zr1 -152.64(15) . . . . ?
C27 C32 O4 Zr1 27.9(3) . . . . ?
C32 O4 Zr1 O1 -108.40(18) . . . . ?
C32 O4 Zr1 O2 36.45(18) . . . . ?
C32 O4 Zr1 O3 153.85(16) . . . . ?
C32 O4 Zr1 N2 108.72(18) . . . . ?
C32 O4 Zr1 N3 -33.7(2) . . . . ?
C32 O4 Zr1 N4 -34.28(17) . . . . ?
C32 O4 Zr1 N1 179.91(19) . . . . ?
C1 O1 Zr1 O4 -117.76(15) . . . . ?
C1 O1 Zr1 O2 139.26(14) . . . . ?
C1 O1 Zr1 O3 25.90(15) . . . . ?
C1 O1 Zr1 N2 -41.57(19) . . . . ?
C1 O1 Zr1 N3 98.54(15) . . . . ?
C1 O1 Zr1 N4 170.08(16) . . . . ?
C1 O1 Zr1 N1 -45.54(15) . . . . ?
C16 O2 Zr1 O4 27.90(15) . . . . ?
C16 O2 Zr1 O1 131.70(14) . . . . ?
C16 O2 Zr1 O3 -119.01(15) . . . . ?
C16 O2 Zr1 N2 -47.77(15) . . . . ?
C16 O2 Zr1 N3 172.54(16) . . . . ?
C16 O2 Zr1 N4 100.20(15) . . . . ?
C16 O2 Zr1 N1 -40.79(19) . . . . ?
C17 O3 Zr1 O4 125.91(15) . . . . ?
C17 O3 Zr1 O1 26.36(16) . . . . ?
C17 O3 Zr1 O2 -119.80(15) . . . . ?
C17 O3 Zr1 N2 171.21(16) . . . . ?
C17 O3 Zr1 N3 -49.36(15) . . . . ?
C17 O3 Zr1 N4 -41.30(19) . . . . ?
C17 O3 Zr1 N1 99.51(16) . . . . ?
C10 N2 Zr1 O4 -69.92(16) . . . . ?
C9 N2 Zr1 O4 98.48(13) . . . . ?
C10 N2 Zr1 O1 -152.27(14) . . . . ?
C9 N2 Zr1 O1 16.12(17) . . . . ?
C10 N2 Zr1 O2 27.21(16) . . . . ?
C9 N2 Zr1 O2 -164.39(14) . . . . ?
C10 N2 Zr1 O3 135.92(17) . . . . ?
C9 N2 Zr1 O3 -55.68(13) . . . . ?
C10 N2 Zr1 N3 81.88(17) . . . . ?
C9 N2 Zr1 N3 -109.73(13) . . . . ?
C10 N2 Zr1 N4 -16.97(19) . . . . ?
C9 N2 Zr1 N4 151.43(12) . . . . ?
C10 N2 Zr1 N1 -148.17(17) . . . . ?
C9 N2 Zr1 N1 20.22(13) . . . . ?
C23 N3 Zr1 O4 -145.70(14) . . . . ?
C24 N3 Zr1 O4 19.70(17) . . . . ?
C23 N3 Zr1 O1 -64.76(15) . . . . ?
C24 N3 Zr1 O1 100.64(12) . . . . ?
C23 N3 Zr1 O2 138.63(16) . . . . ?
C24 N3 Zr1 O2 -55.97(12) . . . . ?
C23 N3 Zr1 O3 29.56(15) . . . . ?
C24 N3 Zr1 O3 -165.04(13) . . . . ?
C23 N3 Zr1 N2 84.88(16) . . . . ?
C24 N3 Zr1 N2 -109.72(12) . . . . ?
C23 N3 Zr1 N4 -145.14(16) . . . . ?
C24 N3 Zr1 N4 20.25(12) . . . . ?
C23 N3 Zr1 N1 -13.41(19) . . . . ?
C24 N3 Zr1 N1 151.98(11) . . . . ?
C26 N4 Zr1 O4 23.71(15) . . . . ?
C25 N4 Zr1 O4 -168.70(13) . . . . ?
C26 N4 Zr1 O1 123.69(16) . . . . ?
C25 N4 Zr1 O1 -68.72(12) . . . . ?
C26 N4 Zr1 O2 -74.80(15) . . . . ?
C25 N4 Zr1 O2 92.78(12) . . . . ?
C26 N4 Zr1 O3 -164.20(14) . . . . ?
C25 N4 Zr1 O3 3.39(16) . . . . ?
C26 N4 Zr1 N2 -30.30(18) . . . . ?
C25 N4 Zr1 N2 137.29(12) . . . . ?
C26 N4 Zr1 N3 -155.95(17) . . . . ?
C25 N4 Zr1 N3 11.64(11) . . . . ?
C26 N4 Zr1 N1 72.57(17) . . . . ?
C25 N4 Zr1 N1 -119.84(12) . . . . ?
C7 N1 Zr1 O4 123.81(17) . . . . ?
C8 N1 Zr1 O4 -69.37(14) . . . . ?
C7 N1 Zr1 O1 23.19(16) . . . . ?
C8 N1 Zr1 O1 -169.98(14) . . . . ?
C7 N1 Zr1 O2 -161.41(15) . . . . ?
C8 N1 Zr1 O2 5.41(18) . . . . ?
C7 N1 Zr1 O3 -72.20(17) . . . . ?
C8 N1 Zr1 O3 94.62(14) . . . . ?
C7 N1 Zr1 N2 -154.22(18) . . . . ?
C8 N1 Zr1 N2 12.60(13) . . . . ?
C7 N1 Zr1 N3 -28.9(2) . . . . ?
C8 N1 Zr1 N3 137.87(13) . . . . ?
C7 N1 Zr1 N4 75.11(18) . . . . ?
C8 N1 Zr1 N4 -118.07(14) . . . . ?



_diffrn_measured_fraction_theta_max 0.977

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.969

_refine_diff_density_min         -0.822

_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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_Zr1
_database_code_depnum_ccdc_archive 'CCDC 1815596'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C57 H96 N2 O8 Zr2'

_chemical_formula_sum            'C57 H96 N2 O8 Zr2'


_chemical_formula_weight         1119.80



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   P2(1)/n

_symmetry_space_group_name_Hall  '-P 2yn'

loop_

_symmetry_equiv_pos_as_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                   10.4865(3)

_cell_length_b                   30.3069(8)

_cell_length_c                   19.5427(5)

_cell_angle_alpha                90.00

_cell_angle_beta                 101.0420(10)

_cell_angle_gamma                90.00

_cell_volume                     6095.9(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    9729

_cell_measurement_theta_min      2.06

_cell_measurement_theta_max      28.30



_exptl_crystal_description       Block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.22

_exptl_crystal_size_min          0.05

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.220

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2384

_exptl_absorpt_coefficient_mu    0.391

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.8754

_exptl_absorpt_correction_T_max  0.9807

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'




_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      173(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 APEXII 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            41638

_diffrn_reflns_av_R_equivalents  0.0277

_diffrn_reflns_av_sigmaI/netI    0.0334

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       12

_diffrn_reflns_limit_k_min       -40

_diffrn_reflns_limit_k_max       35

_diffrn_reflns_limit_l_min       -23

_diffrn_reflns_limit_l_max       19

_diffrn_reflns_theta_min         1.26

_diffrn_reflns_theta_max         28.38

_reflns_number_total             12814

_reflns_number_gt                10638

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'



_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         12814

_refine_ls_number_parameters     647

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0457

_refine_ls_R_factor_gt           0.0344

_refine_ls_wR_factor_ref         0.1255

_refine_ls_wR_factor_gt          0.1127

_refine_ls_goodness_of_fit_ref   0.954

_refine_ls_restrained_S_all      0.954

_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





































































































































































C1 C 1.01135(19) 0.18884(6) 0.69686(11) 0.0150(4) Uani 1 1 d . . .
C2 C 1.0433(2) 0.19135(6) 0.77061(11) 0.0163(4) Uani 1 1 d . . .
C3 C 1.1341(2) 0.22249(6) 0.80280(11) 0.0172(5) Uani 1 1 d . . .
H3 H 1.1535 0.2240 0.8523 0.021 Uiso 1 1 calc R . .
C4 C 1.19615(19) 0.25099(6) 0.76506(11) 0.0159(4) Uani 1 1 d . . .
C5 C 1.1606(2) 0.24828(6) 0.69231(11) 0.0168(4) Uani 1 1 d . . .
H5 H 1.2014 0.2679 0.6653 0.020 Uiso 1 1 calc R . .
C6 C 1.06945(19) 0.21866(6) 0.65683(11) 0.0158(4) Uani 1 1 d . . .
C7 C 0.9873(2) 0.16246(7) 0.81540(12) 0.0178(5) Uani 1 1 d . . .
H7 H 1.0103 0.1682 0.8640 0.021 Uiso 1 1 calc R . .
C8 C 0.8787(2) 0.10426(7) 0.85602(12) 0.0233(5) Uani 1 1 d . . .
H8A H 0.7886 0.0930 0.8435 0.028 Uiso 1 1 calc R . .
H8B H 0.8839 0.1238 0.8970 0.028 Uiso 1 1 calc R . .
C9 C 0.9730(2) 0.06506(7) 0.87516(12) 0.0217(5) Uani 1 1 d . . .
H9A H 1.0480 0.0688 0.8517 0.026 Uiso 1 1 calc R . .
H9B H 1.0062 0.0651 0.9261 0.026 Uiso 1 1 calc R . .
C10 C 0.8592(2) 0.00374(7) 0.90227(12) 0.0195(5) Uani 1 1 d . . .
H10 H 0.8730 0.0183 0.9461 0.023 Uiso 1 1 calc R . .
C11 C 0.7844(2) -0.03641(7) 0.89802(12) 0.0190(5) Uani 1 1 d . . .
C12 C 0.7605(2) -0.06255(7) 0.83663(11) 0.0172(5) Uani 1 1 d . . .
C13 C 0.6905(2) -0.10287(7) 0.83763(12) 0.0172(5) Uani 1 1 d . . .
C14 C 0.6430(2) -0.11258(7) 0.89754(12) 0.0201(5) Uani 1 1 d . . .
H14 H 0.5946 -0.1390 0.8979 0.024 Uiso 1 1 calc R . .
C15 C 0.6612(2) -0.08610(7) 0.95768(12) 0.0206(5) Uani 1 1 d . . .
C16 C 0.7342(2) -0.04839(7) 0.95649(11) 0.0198(5) Uani 1 1 d . . .
H16 H 0.7508 -0.0300 0.9966 0.024 Uiso 1 1 calc R . .
C17 C 1.2993(2) 0.28360(7) 0.80165(12) 0.0199(5) Uani 1 1 d . . .
C18 C 1.4132(2) 0.25731(8) 0.84474(13) 0.0296(6) Uani 1 1 d . . .
H18A H 1.3809 0.2390 0.8791 0.044 Uiso 1 1 calc R . .
H18B H 1.4789 0.2779 0.8688 0.044 Uiso 1 1 calc R . .
H18C H 1.4520 0.2384 0.8136 0.044 Uiso 1 1 calc R . .
C19 C 1.2407(2) 0.31358(8) 0.85084(13) 0.0280(6) Uani 1 1 d . . .
H19A H 1.2034 0.2954 0.8835 0.042 Uiso 1 1 calc R . .
H19B H 1.1725 0.3320 0.8235 0.042 Uiso 1 1 calc R . .
H19C H 1.3089 0.3325 0.8769 0.042 Uiso 1 1 calc R . .
C20 C 1.3530(3) 0.31274(8) 0.74985(14) 0.0332(6) Uani 1 1 d . . .
H20A H 1.4167 0.3334 0.7754 0.050 Uiso 1 1 calc R . .
H20B H 1.2817 0.3293 0.7214 0.050 Uiso 1 1 calc R . .
H20C H 1.3949 0.2942 0.7195 0.050 Uiso 1 1 calc R . .
C21 C 1.0332(2) 0.21861(7) 0.57740(12) 0.0216(5) Uani 1 1 d . . .
C22 C 1.1061(3) 0.25444(9) 0.54506(13) 0.0403(7) Uani 1 1 d . . .
H22A H 1.0830 0.2835 0.5610 0.060 Uiso 1 1 calc R . .
H22B H 1.0819 0.2529 0.4941 0.060 Uiso 1 1 calc R . .
H22C H 1.1999 0.2498 0.5594 0.060 Uiso 1 1 calc R . .
C23 C 0.8875(2) 0.22702(8) 0.55426(13) 0.0306(6) Uani 1 1 d . . .
H23A H 0.8388 0.2041 0.5735 0.046 Uiso 1 1 calc R . .
H23B H 0.8647 0.2264 0.5032 0.046 Uiso 1 1 calc R . .
H23C H 0.8657 0.2560 0.5712 0.046 Uiso 1 1 calc R . .
C24 C 1.0686(3) 0.17419(8) 0.54823(14) 0.0337(6) Uani 1 1 d . . .
H24A H 1.1601 0.1675 0.5668 0.051 Uiso 1 1 calc R . .
H24B H 1.0544 0.1758 0.4972 0.051 Uiso 1 1 calc R . .
H24C H 1.0138 0.1509 0.5621 0.051 Uiso 1 1 calc R . .
C25 C 0.6679(2) -0.13357(7) 0.77402(12) 0.0205(5) Uani 1 1 d . . .
C26 C 0.5883(2) -0.10974(8) 0.71083(13) 0.0265(5) Uani 1 1 d . . .
H26A H 0.5046 -0.1006 0.7215 0.040 Uiso 1 1 calc R . .
H26B H 0.5734 -0.1297 0.6706 0.040 Uiso 1 1 calc R . .
H26C H 0.6359 -0.0836 0.7000 0.040 Uiso 1 1 calc R . .
C27 C 0.7986(2) -0.14813(8) 0.75759(14) 0.0294(6) Uani 1 1 d . . .
H27A H 0.8468 -0.1222 0.7468 0.044 Uiso 1 1 calc R . .
H27B H 0.7836 -0.1681 0.7174 0.044 Uiso 1 1 calc R . .
H27C H 0.8490 -0.1635 0.7980 0.044 Uiso 1 1 calc R . .
C28 C 0.5939(3) -0.17525(8) 0.78718(13) 0.0303(6) Uani 1 1 d . . .
H28A H 0.6443 -0.1916 0.8265 0.045 Uiso 1 1 calc R . .
H28B H 0.5803 -0.1939 0.7454 0.045 Uiso 1 1 calc R . .
H28C H 0.5096 -0.1670 0.7980 0.045 Uiso 1 1 calc R . .
C29 C 0.6016(2) -0.09917(8) 1.02033(13) 0.0286(6) Uani 1 1 d . . .
C30 C 0.6674(3) -0.14290(10) 1.05221(17) 0.0527(8) Uani 1 1 d . . .
H30A H 0.6324 -0.1510 1.0935 0.079 Uiso 1 1 calc R . .
H30B H 0.7615 -0.1384 1.0655 0.079 Uiso 1 1 calc R . .
H30C H 0.6496 -0.1666 1.0176 0.079 Uiso 1 1 calc R . .
C31 C 0.4584(3) -0.10673(13) 0.99884(17) 0.0564(10) Uani 1 1 d . . .
H31A H 0.4153 -0.0788 0.9834 0.085 Uiso 1 1 calc R . .
H31B H 0.4241 -0.1182 1.0385 0.085 Uiso 1 1 calc R . .
H31C H 0.4422 -0.1281 0.9605 0.085 Uiso 1 1 calc R . .
C32 C 0.6269(3) -0.06503(11) 1.07820(15) 0.0453(8) Uani 1 1 d . . .
H32A H 0.5820 -0.0375 1.0619 0.068 Uiso 1 1 calc R . .
H32B H 0.7205 -0.0595 1.0911 0.068 Uiso 1 1 calc R . .
H32C H 0.5947 -0.0760 1.1189 0.068 Uiso 1 1 calc R . .
C33 C 0.5873(2) 0.17507(8) 0.71460(16) 0.0337(6) Uani 1 1 d . . .
H33 H 0.5743 0.1702 0.7634 0.040 Uiso 1 1 calc R . .
C34 C 0.4569(3) 0.17568(12) 0.6673(2) 0.0686(11) Uani 1 1 d . . .
H34A H 0.4682 0.1780 0.6188 0.103 Uiso 1 1 calc R . .
H34B H 0.4070 0.2011 0.6787 0.103 Uiso 1 1 calc R . .
H34C H 0.4102 0.1484 0.6733 0.103 Uiso 1 1 calc R . .
C35 C 0.6590(3) 0.21800(9) 0.7122(2) 0.0605(10) Uani 1 1 d . . .
H35A H 0.7412 0.2171 0.7460 0.091 Uiso 1 1 calc R . .
H35B H 0.6056 0.2424 0.7239 0.091 Uiso 1 1 calc R . .
H35C H 0.6769 0.2225 0.6653 0.091 Uiso 1 1 calc R . .
C36 C 0.7281(3) 0.10140(8) 0.50958(13) 0.0323(6) Uani 1 1 d . . .
H36 H 0.7966 0.1186 0.4921 0.039 Uiso 1 1 calc R . .
C37 C 0.6046(3) 0.12799(11) 0.49651(15) 0.0454(8) Uani 1 1 d . . .
H37A H 0.5368 0.1120 0.5145 0.068 Uiso 1 1 calc R . .
H37B H 0.5765 0.1328 0.4463 0.068 Uiso 1 1 calc R . .
H37C H 0.6200 0.1565 0.5203 0.068 Uiso 1 1 calc R . .
C38 C 0.7129(4) 0.05740(11) 0.47263(16) 0.0611(10) Uani 1 1 d . . .
H38A H 0.7956 0.0414 0.4827 0.092 Uiso 1 1 calc R . .
H38B H 0.6876 0.0622 0.4223 0.092 Uiso 1 1 calc R . .
H38C H 0.6457 0.0401 0.4890 0.092 Uiso 1 1 calc R . .
C39 C 1.0895(2) 0.06936(8) 0.67839(13) 0.0260(5) Uani 1 1 d . . .
H39 H 1.0724 0.0978 0.6524 0.031 Uiso 1 1 calc R . .
C40 C 1.2021(2) 0.07760(9) 0.73683(15) 0.0350(6) Uani 1 1 d . . .
H40A H 1.1794 0.1009 0.7672 0.053 Uiso 1 1 calc R . .
H40B H 1.2777 0.0869 0.7177 0.053 Uiso 1 1 calc R . .
H40C H 1.2231 0.0504 0.7639 0.053 Uiso 1 1 calc R . .
C41 C 1.1142(3) 0.03566(10) 0.62656(16) 0.0410(7) Uani 1 1 d . . .
H41A H 1.1318 0.0070 0.6497 0.062 Uiso 1 1 calc R . .
H41B H 1.1895 0.0446 0.6069 0.062 Uiso 1 1 calc R . .
H41C H 1.0377 0.0332 0.5891 0.062 Uiso 1 1 calc R . .
C42 C 0.6122(2) 0.02912(8) 0.71614(13) 0.0260(5) Uani 1 1 d . . .
H42 H 0.6184 -0.0036 0.7218 0.031 Uiso 1 1 calc R . .
C43 C 0.5569(2) 0.04650(10) 0.77592(15) 0.0378(7) Uani 1 1 d . . .
H43A H 0.6100 0.0363 0.8199 0.057 Uiso 1 1 calc R . .
H43B H 0.4677 0.0358 0.7723 0.057 Uiso 1 1 calc R . .
H43C H 0.5569 0.0788 0.7748 0.057 Uiso 1 1 calc R . .
C44 C 0.5292(2) 0.03785(9) 0.64564(15) 0.0375(7) Uani 1 1 d . . .
H44A H 0.5213 0.0698 0.6378 0.056 Uiso 1 1 calc R . .
H44B H 0.4427 0.0251 0.6438 0.056 Uiso 1 1 calc R . .
H44C H 0.5696 0.0244 0.6095 0.056 Uiso 1 1 calc R . .
C45 C 1.1842(2) -0.04058(10) 0.81935(15) 0.0394(7) Uani 1 1 d . . .
H45 H 1.2230 -0.0156 0.8498 0.047 Uiso 1 1 calc R . .
C46 C 1.2854(3) -0.05777(12) 0.7821(2) 0.0602(10) Uani 1 1 d . . .
H46A H 1.2503 -0.0828 0.7527 0.090 Uiso 1 1 calc R . .
H46B H 1.3614 -0.0674 0.8162 0.090 Uiso 1 1 calc R . .
H46C H 1.3112 -0.0344 0.7528 0.090 Uiso 1 1 calc R . .
C47 C 1.1374(3) -0.07516(12) 0.86537(18) 0.0594(10) Uani 1 1 d . . .
H47A H 1.0784 -0.0614 0.8924 0.089 Uiso 1 1 calc R . .
H47B H 1.2122 -0.0877 0.8973 0.089 Uiso 1 1 calc R . .
H47C H 1.0915 -0.0987 0.8361 0.089 Uiso 1 1 calc R . .
C48 C 0.8718(3) -0.05308(8) 0.58321(13) 0.0306(6) Uani 1 1 d . . .
H48 H 0.9001 -0.0318 0.5500 0.037 Uiso 1 1 calc R . .
C49 C 0.9738(3) -0.08864(11) 0.59987(19) 0.0602(10) Uani 1 1 d . . .
H49A H 1.0562 -0.0754 0.6230 0.090 Uiso 1 1 calc R . .
H49B H 0.9857 -0.1030 0.5566 0.090 Uiso 1 1 calc R . .
H49C H 0.9459 -0.1105 0.6308 0.090 Uiso 1 1 calc R . .
C50 C 0.7404(3) -0.07110(11) 0.54989(16) 0.0511(8) Uani 1 1 d . . .
H50A H 0.7099 -0.0915 0.5822 0.077 Uiso 1 1 calc R . .
H50B H 0.7474 -0.0868 0.5069 0.077 Uiso 1 1 calc R . .
H50C H 0.6785 -0.0467 0.5389 0.077 Uiso 1 1 calc R . .
C51 C 0.9145(3) 0.23490(11) 0.95753(17) 0.0507(8) Uani 1 1 d . . .
C52 C 1.0383(4) 0.23412(11) 0.99272(17) 0.0522(8) Uani 1 1 d . . .
H52 H 1.0954 0.2576 0.9871 0.063 Uiso 1 1 calc R . .
C53 C 1.0844(4) 0.19861(12) 1.03793(19) 0.0660(11) Uani 1 1 d . . .
H53 H 1.1718 0.1985 1.0626 0.079 Uiso 1 1 calc R . .
C54 C 1.0043(3) 0.16512(12) 1.04594(18) 0.0580(9) Uani 1 1 d . . .
H54 H 1.0353 0.1411 1.0758 0.070 Uiso 1 1 calc R . .
C55 C 0.8772(3) 0.16577(11) 1.01069(17) 0.0495(8) Uani 1 1 d . . .
H55 H 0.8202 0.1425 1.0173 0.059 Uiso 1 1 calc R . .
C56 C 0.8332(3) 0.19891(9) 0.96726(16) 0.0390(7) Uani 1 1 d . . .
H56 H 0.7459 0.1983 0.9425 0.047 Uiso 1 1 calc R . .
C57 C 0.8667(5) 0.27203(13) 0.9104(2) 0.0772(12) Uani 1 1 d . . .
H57A H 0.8475 0.2973 0.9379 0.116 Uiso 1 1 calc R . .
H57B H 0.7875 0.2630 0.8781 0.116 Uiso 1 1 calc R . .
H57C H 0.9334 0.2803 0.8838 0.116 Uiso 1 1 calc R . .
N1 N 0.90963(17) 0.12970(6) 0.79745(10) 0.0183(4) Uani 1 1 d . . .
N2 N 0.90978(17) 0.02258(6) 0.85459(9) 0.0186(4) Uani 1 1 d . . .
O1 O 0.92859(14) 0.15838(5) 0.66716(7) 0.0181(3) Uani 1 1 d . . .
O2 O 0.66194(15) 0.13996(5) 0.69622(9) 0.0266(4) Uani 1 1 d . . .
O3 O 0.76940(15) 0.09484(5) 0.58207(8) 0.0222(3) Uani 1 1 d . . .
O4 O 0.97352(13) 0.05937(5) 0.70487(8) 0.0161(3) Uani 1 1 d . . .
O5 O 0.74311(13) 0.04526(4) 0.71917(8) 0.0162(3) Uani 1 1 d . . .
O6 O 0.86360(15) -0.03028(5) 0.64504(8) 0.0219(3) Uani 1 1 d . . .
O7 O 0.80257(15) -0.04954(5) 0.78066(8) 0.0191(3) Uani 1 1 d . . .
O8 O 1.07672(14) -0.02438(5) 0.77248(8) 0.0252(4) Uani 1 1 d . . .
Zr1 Zr 0.810863(18) 0.106224(6) 0.680907(10) 0.01461(8) Uani 1 1 d . . .
Zr2 Zr 0.902720(18) -0.002928(6) 0.735570(11) 0.01429(8) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag











































































































































































C1 O1 1.323(2) . ?
C1 C6 1.408(3) . ?
C1 C2 1.418(3) . ?
C2 C3 1.402(3) . ?
C2 C7 1.440(3) . ?
C3 C4 1.377(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(3) . ?
C4 C17 1.537(3) . ?
C5 C6 1.395(3) . ?
C5 H5 0.9500 . ?
C6 C21 1.526(3) . ?
C7 N1 1.289(3) . ?
C7 H7 0.9500 . ?
C8 N1 1.467(3) . ?
C8 C9 1.545(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.469(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.290(3) . ?
C10 C11 1.441(3) . ?
C10 H10 0.9500 . ?
C11 C16 1.395(3) . ?
C11 C12 1.419(3) . ?
C12 O7 1.316(3) . ?
C12 C13 1.427(3) . ?
C13 C14 1.389(3) . ?
C13 C25 1.534(3) . ?
C14 C15 1.405(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(3) . ?
C15 C29 1.530(3) . ?
C16 H16 0.9500 . ?
C17 C20 1.530(3) . ?
C17 C19 1.534(3) . ?
C17 C18 1.544(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.529(3) . ?
C21 C22 1.532(3) . ?
C21 C24 1.535(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C28 1.530(3) . ?
C25 C27 1.531(3) . ?
C25 C26 1.533(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.497(4) . ?
C29 C32 1.518(4) . ?
C29 C30 1.567(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 O2 1.408(3) . ?
C33 C34 1.497(4) . ?
C33 C35 1.508(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 O3 1.414(3) . ?
C36 C37 1.505(4) . ?
C36 C38 1.510(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 O4 1.442(3) . ?
C39 C41 1.496(4) . ?
C39 C40 1.498(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O5 1.448(2) . ?
C42 C43 1.496(4) . ?
C42 C44 1.505(3) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O8 1.398(3) . ?
C45 C46 1.492(4) . ?
C45 C47 1.522(4) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O6 1.409(3) . ?
C48 C50 1.509(4) . ?
C48 C49 1.510(4) . ?
C48 H48 1.0000 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.348(5) . ?
C51 C56 1.420(4) . ?
C51 C57 1.480(5) . ?
C52 C53 1.417(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.346(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.339(4) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
N1 Zr1 2.4212(18) . ?
N2 Zr2 2.4386(19) . ?
O1 Zr1 2.0547(14) . ?
O2 Zr1 1.9372(15) . ?
O3 Zr1 1.9281(15) . ?
O4 Zr2 2.1556(14) . ?
O4 Zr1 2.1998(14) . ?
O5 Zr1 2.1635(14) . ?
O5 Zr2 2.1981(14) . ?
O6 Zr2 1.9255(15) . ?
O7 Zr2 2.0565(15) . ?
O8 Zr2 1.9411(14) . ?
Zr1 Zr2 3.5522(3) . ?



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 C1 C6 121.43(19) . . ?
O1 C1 C2 119.39(19) . . ?
C6 C1 C2 119.17(18) . . ?
C3 C2 C1 120.0(2) . . ?
C3 C2 C7 117.23(19) . . ?
C1 C2 C7 122.75(18) . . ?
C4 C3 C2 122.1(2) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 116.45(18) . . ?
C3 C4 C17 121.10(19) . . ?
C5 C4 C17 122.45(19) . . ?
C6 C5 C4 124.4(2) . . ?
C6 C5 H5 117.8 . . ?
C4 C5 H5 117.8 . . ?
C5 C6 C1 117.71(19) . . ?
C5 C6 C21 121.31(19) . . ?
C1 C6 C21 120.98(18) . . ?
N1 C7 C2 127.8(2) . . ?
N1 C7 H7 116.1 . . ?
C2 C7 H7 116.1 . . ?
N1 C8 C9 111.5(2) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C8 111.95(17) . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C11 128.8(2) . . ?
N2 C10 H10 115.6 . . ?
C11 C10 H10 115.6 . . ?
C16 C11 C12 120.90(19) . . ?
C16 C11 C10 117.3(2) . . ?
C12 C11 C10 121.8(2) . . ?
O7 C12 C11 120.13(19) . . ?
O7 C12 C13 121.53(19) . . ?
C11 C12 C13 118.3(2) . . ?
C14 C13 C12 117.5(2) . . ?
C14 C13 C25 122.00(19) . . ?
C12 C13 C25 120.5(2) . . ?
C13 C14 C15 124.8(2) . . ?
C13 C14 H14 117.6 . . ?
C15 C14 H14 117.6 . . ?
C16 C15 C14 116.5(2) . . ?
C16 C15 C29 122.8(2) . . ?
C14 C15 C29 120.68(19) . . ?
C15 C16 C11 121.9(2) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C20 C17 C19 108.4(2) . . ?
C20 C17 C4 112.26(18) . . ?
C19 C17 C4 110.01(18) . . ?
C20 C17 C18 108.3(2) . . ?
C19 C17 C18 108.93(19) . . ?
C4 C17 C18 108.90(17) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C6 C21 C23 109.9(2) . . ?
C6 C21 C22 111.87(18) . . ?
C23 C21 C22 108.0(2) . . ?
C6 C21 C24 110.35(18) . . ?
C23 C21 C24 109.56(19) . . ?
C22 C21 C24 107.1(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C25 C27 107.51(19) . . ?
C28 C25 C26 107.99(18) . . ?
C27 C25 C26 109.8(2) . . ?
C28 C25 C13 111.6(2) . . ?
C27 C25 C13 109.82(18) . . ?
C26 C25 C13 110.04(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 C29 C32 109.7(2) . . ?
C31 C29 C15 110.9(2) . . ?
C32 C29 C15 112.3(2) . . ?
C31 C29 C30 108.9(3) . . ?
C32 C29 C30 106.2(2) . . ?
C15 C29 C30 108.7(2) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O2 C33 C34 109.8(2) . . ?
O2 C33 C35 109.8(2) . . ?
C34 C33 C35 111.9(3) . . ?
O2 C33 H33 108.4 . . ?
C34 C33 H33 108.4 . . ?
C35 C33 H33 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O3 C36 C37 109.5(2) . . ?
O3 C36 C38 109.8(2) . . ?
C37 C36 C38 112.5(2) . . ?
O3 C36 H36 108.3 . . ?
C37 C36 H36 108.3 . . ?
C38 C36 H36 108.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O4 C39 C41 111.54(19) . . ?
O4 C39 C40 110.9(2) . . ?
C41 C39 C40 114.6(2) . . ?
O4 C39 H39 106.4 . . ?
C41 C39 H39 106.4 . . ?
C40 C39 H39 106.4 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O5 C42 C43 110.80(19) . . ?
O5 C42 C44 110.8(2) . . ?
C43 C42 C44 114.2(2) . . ?
O5 C42 H42 106.9 . . ?
C43 C42 H42 106.9 . . ?
C44 C42 H42 106.9 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O8 C45 C46 111.3(2) . . ?
O8 C45 C47 108.6(2) . . ?
C46 C45 C47 112.8(3) . . ?
O8 C45 H45 108.0 . . ?
C46 C45 H45 108.0 . . ?
C47 C45 H45 108.0 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O6 C48 C50 110.3(2) . . ?
O6 C48 C49 108.8(2) . . ?
C50 C48 C49 112.7(3) . . ?
O6 C48 H48 108.3 . . ?
C50 C48 H48 108.3 . . ?
C49 C48 H48 108.3 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C56 117.6(3) . . ?
C52 C51 C57 120.6(4) . . ?
C56 C51 C57 121.8(3) . . ?
C51 C52 C53 120.8(3) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
C54 C53 C52 120.0(3) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 119.8(3) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C56 C55 C54 120.7(3) . . ?
C56 C55 H55 119.7 . . ?
C54 C55 H55 119.7 . . ?
C55 C56 C51 121.2(3) . . ?
C55 C56 H56 119.4 . . ?
C51 C56 H56 119.4 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C7 N1 C8 114.51(18) . . ?
C7 N1 Zr1 128.05(15) . . ?
C8 N1 Zr1 117.44(13) . . ?
C10 N2 C9 114.61(19) . . ?
C10 N2 Zr2 127.37(14) . . ?
C9 N2 Zr2 117.95(14) . . ?
C1 O1 Zr1 147.11(14) . . ?
C33 O2 Zr1 160.47(15) . . ?
C36 O3 Zr1 161.03(15) . . ?
C39 O4 Zr2 130.00(13) . . ?
C39 O4 Zr1 117.45(13) . . ?
Zr2 O4 Zr1 109.29(6) . . ?
C42 O5 Zr1 130.24(13) . . ?
C42 O5 Zr2 118.10(12) . . ?
Zr1 O5 Zr2 109.06(6) . . ?
C48 O6 Zr2 164.17(15) . . ?
C12 O7 Zr2 147.36(13) . . ?
C45 O8 Zr2 160.64(18) . . ?
O3 Zr1 O2 102.44(7) . . ?
O3 Zr1 O1 91.86(6) . . ?
O2 Zr1 O1 97.84(6) . . ?
O3 Zr1 O5 99.64(6) . . ?
O2 Zr1 O5 93.99(6) . . ?
O1 Zr1 O5 161.34(5) . . ?
O3 Zr1 O4 96.58(6) . . ?
O2 Zr1 O4 157.37(7) . . ?
O1 Zr1 O4 93.65(6) . . ?
O5 Zr1 O4 70.60(5) . . ?
O3 Zr1 N1 165.63(7) . . ?
O2 Zr1 N1 84.94(7) . . ?
O1 Zr1 N1 74.78(6) . . ?
O5 Zr1 N1 92.03(6) . . ?
O4 Zr1 N1 79.33(6) . . ?
O3 Zr1 Zr2 97.51(5) . . ?
O2 Zr1 Zr2 128.70(5) . . ?
O1 Zr1 Zr2 128.36(4) . . ?
O5 Zr1 Zr2 35.80(4) . . ?
O4 Zr1 Zr2 34.94(4) . . ?
N1 Zr1 Zr2 87.04(4) . . ?
O6 Zr2 O8 102.53(7) . . ?
O6 Zr2 O7 93.53(6) . . ?
O8 Zr2 O7 97.56(6) . . ?
O6 Zr2 O4 98.37(6) . . ?
O8 Zr2 O4 92.72(6) . . ?
O7 Zr2 O4 162.23(6) . . ?
O6 Zr2 O5 97.46(6) . . ?
O8 Zr2 O5 155.78(6) . . ?
O7 Zr2 O5 94.69(6) . . ?
O4 Zr2 O5 70.77(5) . . ?
O6 Zr2 N2 167.17(6) . . ?
O8 Zr2 N2 84.09(7) . . ?
O7 Zr2 N2 74.56(6) . . ?
O4 Zr2 N2 92.22(6) . . ?
O5 Zr2 N2 79.14(6) . . ?
O6 Zr2 Zr1 97.29(5) . . ?
O8 Zr2 Zr1 127.23(5) . . ?
O7 Zr2 Zr1 129.58(4) . . ?
O4 Zr2 Zr1 35.77(4) . . ?
O5 Zr2 Zr1 35.15(4) . . ?
N2 Zr2 Zr1 87.05(4) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag











































































































































































































































O1 C1 C2 C3 177.86(18) . . . . ?
C6 C1 C2 C3 -1.6(3) . . . . ?
O1 C1 C2 C7 -1.2(3) . . . . ?
C6 C1 C2 C7 179.32(19) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C7 C2 C3 C4 178.30(19) . . . . ?
C2 C3 C4 C5 2.0(3) . . . . ?
C2 C3 C4 C17 -177.60(19) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C17 C4 C5 C6 178.72(19) . . . . ?
C4 C5 C6 C1 -1.4(3) . . . . ?
C4 C5 C6 C21 178.3(2) . . . . ?
O1 C1 C6 C5 -176.81(18) . . . . ?
C2 C1 C6 C5 2.6(3) . . . . ?
O1 C1 C6 C21 3.5(3) . . . . ?
C2 C1 C6 C21 -177.08(19) . . . . ?
C3 C2 C7 N1 -174.7(2) . . . . ?
C1 C2 C7 N1 4.4(3) . . . . ?
N1 C8 C9 N2 -107.9(2) . . . . ?
N2 C10 C11 C16 -176.4(2) . . . . ?
N2 C10 C11 C12 2.5(4) . . . . ?
C16 C11 C12 O7 176.28(19) . . . . ?
C10 C11 C12 O7 -2.6(3) . . . . ?
C16 C11 C12 C13 -3.8(3) . . . . ?
C10 C11 C12 C13 177.27(19) . . . . ?
O7 C12 C13 C14 -176.10(19) . . . . ?
C11 C12 C13 C14 4.0(3) . . . . ?
O7 C12 C13 C25 3.0(3) . . . . ?
C11 C12 C13 C25 -176.87(18) . . . . ?
C12 C13 C14 C15 -1.5(3) . . . . ?
C25 C13 C14 C15 179.4(2) . . . . ?
C13 C14 C15 C16 -1.4(3) . . . . ?
C13 C14 C15 C29 178.3(2) . . . . ?
C14 C15 C16 C11 1.7(3) . . . . ?
C29 C15 C16 C11 -178.0(2) . . . . ?
C12 C11 C16 C15 0.9(3) . . . . ?
C10 C11 C16 C15 179.8(2) . . . . ?
C3 C4 C17 C20 -178.6(2) . . . . ?
C5 C4 C17 C20 1.8(3) . . . . ?
C3 C4 C17 C19 -57.9(3) . . . . ?
C5 C4 C17 C19 122.5(2) . . . . ?
C3 C4 C17 C18 61.4(3) . . . . ?
C5 C4 C17 C18 -118.2(2) . . . . ?
C5 C6 C21 C23 -121.0(2) . . . . ?
C1 C6 C21 C23 58.7(3) . . . . ?
C5 C6 C21 C22 -1.0(3) . . . . ?
C1 C6 C21 C22 178.7(2) . . . . ?
C5 C6 C21 C24 118.1(2) . . . . ?
C1 C6 C21 C24 -62.2(3) . . . . ?
C14 C13 C25 C28 -2.3(3) . . . . ?
C12 C13 C25 C28 178.62(19) . . . . ?
C14 C13 C25 C27 -121.4(2) . . . . ?
C12 C13 C25 C27 59.5(3) . . . . ?
C14 C13 C25 C26 117.6(2) . . . . ?
C12 C13 C25 C26 -61.5(3) . . . . ?
C16 C15 C29 C31 125.8(3) . . . . ?
C14 C15 C29 C31 -54.0(3) . . . . ?
C16 C15 C29 C32 2.7(3) . . . . ?
C14 C15 C29 C32 -177.1(2) . . . . ?
C16 C15 C29 C30 -114.5(3) . . . . ?
C14 C15 C29 C30 65.7(3) . . . . ?
C56 C51 C52 C53 -0.3(5) . . . . ?
C57 C51 C52 C53 -180.0(3) . . . . ?
C51 C52 C53 C54 0.2(6) . . . . ?
C52 C53 C54 C55 -0.8(6) . . . . ?
C53 C54 C55 C56 1.5(5) . . . . ?
C54 C55 C56 C51 -1.7(5) . . . . ?
C52 C51 C56 C55 1.1(5) . . . . ?
C57 C51 C56 C55 -179.2(3) . . . . ?
C2 C7 N1 C8 174.9(2) . . . . ?
C2 C7 N1 Zr1 -5.4(3) . . . . ?
C9 C8 N1 C7 -92.2(2) . . . . ?
C9 C8 N1 Zr1 88.02(19) . . . . ?
C11 C10 N2 C9 176.1(2) . . . . ?
C11 C10 N2 Zr2 -1.0(3) . . . . ?
C8 C9 N2 C10 -91.8(2) . . . . ?
C8 C9 N2 Zr2 85.5(2) . . . . ?
C6 C1 O1 Zr1 178.94(17) . . . . ?
C2 C1 O1 Zr1 -0.5(4) . . . . ?
C34 C33 O2 Zr1 145.8(4) . . . . ?
C35 C33 O2 Zr1 22.4(6) . . . . ?
C37 C36 O3 Zr1 -44.1(6) . . . . ?
C38 C36 O3 Zr1 -168.2(4) . . . . ?
C41 C39 O4 Zr2 41.7(3) . . . . ?
C40 C39 O4 Zr2 -87.4(2) . . . . ?
C41 C39 O4 Zr1 -115.5(2) . . . . ?
C40 C39 O4 Zr1 115.43(18) . . . . ?
C43 C42 O5 Zr1 -85.3(2) . . . . ?
C44 C42 O5 Zr1 42.6(3) . . . . ?
C43 C42 O5 Zr2 115.18(18) . . . . ?
C44 C42 O5 Zr2 -116.92(18) . . . . ?
C50 C48 O6 Zr2 156.4(5) . . . . ?
C49 C48 O6 Zr2 32.3(7) . . . . ?
C11 C12 O7 Zr2 1.6(4) . . . . ?
C13 C12 O7 Zr2 -178.29(17) . . . . ?
C46 C45 O8 Zr2 165.9(4) . . . . ?
C47 C45 O8 Zr2 41.2(6) . . . . ?
C36 O3 Zr1 O2 45.0(5) . . . . ?
C36 O3 Zr1 O1 -53.5(5) . . . . ?
C36 O3 Zr1 O5 141.3(5) . . . . ?
C36 O3 Zr1 O4 -147.4(5) . . . . ?
C36 O3 Zr1 N1 -74.8(6) . . . . ?
C36 O3 Zr1 Zr2 177.4(5) . . . . ?
C33 O2 Zr1 O3 -119.0(5) . . . . ?
C33 O2 Zr1 O1 -25.3(5) . . . . ?
C33 O2 Zr1 O5 140.2(5) . . . . ?
C33 O2 Zr1 O4 94.5(5) . . . . ?
C33 O2 Zr1 N1 48.5(5) . . . . ?
C33 O2 Zr1 Zr2 130.6(5) . . . . ?
C1 O1 Zr1 O3 -174.7(2) . . . . ?
C1 O1 Zr1 O2 82.5(2) . . . . ?
C1 O1 Zr1 O5 -46.3(4) . . . . ?
C1 O1 Zr1 O4 -77.9(2) . . . . ?
C1 O1 Zr1 N1 0.0(2) . . . . ?
C1 O1 Zr1 Zr2 -73.6(3) . . . . ?
C42 O5 Zr1 O3 -71.42(18) . . . . ?
Zr2 O5 Zr1 O3 89.49(7) . . . . ?
C42 O5 Zr1 O2 31.92(18) . . . . ?
Zr2 O5 Zr1 O2 -167.16(7) . . . . ?
C42 O5 Zr1 O1 161.27(19) . . . . ?
Zr2 O5 Zr1 O1 -37.8(2) . . . . ?
C42 O5 Zr1 O4 -165.06(19) . . . . ?
Zr2 O5 Zr1 O4 -4.14(5) . . . . ?
C42 O5 Zr1 N1 117.00(18) . . . . ?
Zr2 O5 Zr1 N1 -82.09(7) . . . . ?
C42 O5 Zr1 Zr2 -160.9(2) . . . . ?
C39 O4 Zr1 O3 67.95(14) . . . . ?
Zr2 O4 Zr1 O3 -93.71(7) . . . . ?
C39 O4 Zr1 O2 -144.90(17) . . . . ?
Zr2 O4 Zr1 O2 53.45(17) . . . . ?
C39 O4 Zr1 O1 -24.35(14) . . . . ?
Zr2 O4 Zr1 O1 173.99(7) . . . . ?
C39 O4 Zr1 O5 165.89(15) . . . . ?
Zr2 O4 Zr1 O5 4.23(6) . . . . ?
C39 O4 Zr1 N1 -98.11(14) . . . . ?
Zr2 O4 Zr1 N1 100.24(7) . . . . ?
C39 O4 Zr1 Zr2 161.66(17) . . . . ?
C7 N1 Zr1 O3 25.0(4) . . . . ?
C8 N1 Zr1 O3 -155.3(2) . . . . ?
C7 N1 Zr1 O2 -96.71(19) . . . . ?
C8 N1 Zr1 O2 83.01(15) . . . . ?
C7 N1 Zr1 O1 2.85(18) . . . . ?
C8 N1 Zr1 O1 -177.43(16) . . . . ?
C7 N1 Zr1 O5 169.47(18) . . . . ?
C8 N1 Zr1 O5 -10.81(15) . . . . ?
C7 N1 Zr1 O4 99.65(18) . . . . ?
C8 N1 Zr1 O4 -80.63(15) . . . . ?
C7 N1 Zr1 Zr2 134.01(18) . . . . ?
C8 N1 Zr1 Zr2 -46.27(15) . . . . ?
C48 O6 Zr2 O8 -11.1(6) . . . . ?
C48 O6 Zr2 O7 -109.6(6) . . . . ?
C48 O6 Zr2 O4 83.6(6) . . . . ?
C48 O6 Zr2 O5 155.2(6) . . . . ?
C48 O6 Zr2 N2 -131.1(5) . . . . ?
C48 O6 Zr2 Zr1 119.7(6) . . . . ?
C45 O8 Zr2 O6 -140.4(5) . . . . ?
C45 O8 Zr2 O7 -45.0(5) . . . . ?
C45 O8 Zr2 O4 120.4(5) . . . . ?
C45 O8 Zr2 O5 74.7(5) . . . . ?
C45 O8 Zr2 N2 28.5(5) . . . . ?
C45 O8 Zr2 Zr1 110.2(5) . . . . ?
C12 O7 Zr2 O6 -175.4(2) . . . . ?
C12 O7 Zr2 O8 81.5(3) . . . . ?
C12 O7 Zr2 O4 -43.3(3) . . . . ?
C12 O7 Zr2 O5 -77.6(3) . . . . ?
C12 O7 Zr2 N2 -0.2(2) . . . . ?
C12 O7 Zr2 Zr1 -72.9(3) . . . . ?
C39 O4 Zr2 O6 -67.74(17) . . . . ?
Zr1 O4 Zr2 O6 90.87(7) . . . . ?
C39 O4 Zr2 O8 35.34(17) . . . . ?
Zr1 O4 Zr2 O8 -166.04(7) . . . . ?
C39 O4 Zr2 O7 160.77(19) . . . . ?
Zr1 O4 Zr2 O7 -40.6(2) . . . . ?
C39 O4 Zr2 O5 -162.78(18) . . . . ?
Zr1 O4 Zr2 O5 -4.16(6) . . . . ?
C39 O4 Zr2 N2 119.53(17) . . . . ?
Zr1 O4 Zr2 N2 -81.85(7) . . . . ?
C39 O4 Zr2 Zr1 -158.6(2) . . . . ?
C42 O5 Zr2 O6 71.49(15) . . . . ?
Zr1 O5 Zr2 O6 -92.08(7) . . . . ?
C42 O5 Zr2 O8 -142.98(18) . . . . ?
Zr1 O5 Zr2 O8 53.45(18) . . . . ?
C42 O5 Zr2 O7 -22.70(15) . . . . ?
Zr1 O5 Zr2 O7 173.74(6) . . . . ?
C42 O5 Zr2 O4 167.79(16) . . . . ?
Zr1 O5 Zr2 O4 4.22(6) . . . . ?
C42 O5 Zr2 N2 -95.98(15) . . . . ?
Zr1 O5 Zr2 N2 100.46(7) . . . . ?
C42 O5 Zr2 Zr1 163.56(18) . . . . ?
C10 N2 Zr2 O6 22.1(4) . . . . ?
C9 N2 Zr2 O6 -154.9(2) . . . . ?
C10 N2 Zr2 O8 -99.71(19) . . . . ?
C9 N2 Zr2 O8 83.30(15) . . . . ?
C10 N2 Zr2 O7 -0.17(18) . . . . ?
C9 N2 Zr2 O7 -177.15(16) . . . . ?
C10 N2 Zr2 O4 167.78(18) . . . . ?
C9 N2 Zr2 O4 -9.20(15) . . . . ?
C10 N2 Zr2 O5 97.84(18) . . . . ?
C9 N2 Zr2 O5 -79.14(14) . . . . ?
C10 N2 Zr2 Zr1 132.37(18) . . . . ?
C9 N2 Zr2 Zr1 -44.61(14) . . . . ?
O3 Zr1 Zr2 O6 -3.46(7) . . . . ?
O2 Zr1 Zr2 O6 109.13(8) . . . . ?
O1 Zr1 Zr2 O6 -101.87(7) . . . . ?
O5 Zr1 Zr2 O6 92.62(8) . . . . ?
O4 Zr1 Zr2 O6 -94.21(8) . . . . ?
N1 Zr1 Zr2 O6 -169.76(6) . . . . ?
O3 Zr1 Zr2 O8 108.37(8) . . . . ?
O2 Zr1 Zr2 O8 -139.04(9) . . . . ?
O1 Zr1 Zr2 O8 9.96(8) . . . . ?
O5 Zr1 Zr2 O8 -155.55(9) . . . . ?
O4 Zr1 Zr2 O8 17.62(9) . . . . ?
N1 Zr1 Zr2 O8 -57.93(8) . . . . ?
O3 Zr1 Zr2 O7 -104.19(7) . . . . ?
O2 Zr1 Zr2 O7 8.40(8) . . . . ?
O1 Zr1 Zr2 O7 157.40(7) . . . . ?
O5 Zr1 Zr2 O7 -8.11(8) . . . . ?
O4 Zr1 Zr2 O7 165.06(8) . . . . ?
N1 Zr1 Zr2 O7 89.51(7) . . . . ?
O3 Zr1 Zr2 O4 90.75(8) . . . . ?
O2 Zr1 Zr2 O4 -156.66(9) . . . . ?
O1 Zr1 Zr2 O4 -7.65(8) . . . . ?
O5 Zr1 Zr2 O4 -173.17(9) . . . . ?
N1 Zr1 Zr2 O4 -75.55(8) . . . . ?
O3 Zr1 Zr2 O5 -96.08(8) . . . . ?
O2 Zr1 Zr2 O5 16.50(9) . . . . ?
O1 Zr1 Zr2 O5 165.51(8) . . . . ?
O4 Zr1 Zr2 O5 173.17(9) . . . . ?
N1 Zr1 Zr2 O5 97.61(8) . . . . ?
O3 Zr1 Zr2 N2 -171.33(6) . . . . ?
O2 Zr1 Zr2 N2 -58.75(8) . . . . ?
O1 Zr1 Zr2 N2 90.26(7) . . . . ?
O5 Zr1 Zr2 N2 -75.25(8) . . . . ?
O4 Zr1 Zr2 N2 97.91(8) . . . . ?
N1 Zr1 Zr2 N2 22.36(6) . . . . ?



_diffrn_measured_fraction_theta_max 0.841

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.920

_refine_diff_density_max         1.008

_refine_diff_density_min         -0.451

_refine_diff_density_rms         0.067

_vrf_PLAT029_new                 
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.920       
RESPONSE: Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals

;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_Hf1
_database_code_depnum_ccdc_archive 'CCDC 1815600'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C28 H32 Br4 Hf N2 O4'

_chemical_formula_weight         958.69



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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   P2(1)/c

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                   11.9424(4)

_cell_length_b                   25.8050(10)

_cell_length_c                   11.3456(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 111.2790(10)

_cell_angle_gamma                90.00

_cell_volume                     3258.04(19)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    5187

_cell_measurement_theta_min      2.42

_cell_measurement_theta_max      31.50



_exptl_crystal_description       Hexagonal

_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1832

_exptl_absorpt_coefficient_mu    8.141

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1628

_exptl_absorpt_correction_T_max  0.4965

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'


_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      173(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 APEXII 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            27332

_diffrn_reflns_av_R_equivalents  0.0391

_diffrn_reflns_av_sigmaI/netI    0.0607

_diffrn_reflns_limit_h_min       -16

_diffrn_reflns_limit_h_max       16

_diffrn_reflns_limit_k_min       -38

_diffrn_reflns_limit_k_max       38

_diffrn_reflns_limit_l_min       -10

_diffrn_reflns_limit_l_max       15

_diffrn_reflns_theta_min         1.58

_diffrn_reflns_theta_max         32.22

_reflns_number_total             10150

_reflns_number_gt                7314

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'


_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)+(0.0309P)²+0.4752P] 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         10150

_refine_ls_number_parameters     358

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0720

_refine_ls_R_factor_gt           0.0379

_refine_ls_wR_factor_ref         0.0747

_refine_ls_wR_factor_gt          0.0663

_refine_ls_goodness_of_fit_ref   1.013

_refine_ls_restrained_S_all      1.013

_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







































































Br1 Br 0.33718(4) 0.122074(17) 0.27890(4) 0.03677(10) Uani 1 1 d . . .
Br2 Br 0.20490(5) 0.312151(18) 0.01683(5) 0.05299(14) Uani 1 1 d . . .
Br3 Br 0.92441(4) -0.162382(17) 0.20935(4) 0.04578(12) Uani 1 1 d . . .
Br4 Br 0.82016(5) 0.001039(18) 0.48673(4) 0.04544(12) Uani 1 1 d . . .
C1 C 0.3506(3) 0.16972(14) 0.1583(3) 0.0253(8) Uani 1 1 d . . .
C2 C 0.2866(3) 0.21549(15) 0.1371(3) 0.0303(9) Uani 1 1 d . . .
H2 H 0.2369 0.2233 0.1839 0.036 Uiso 1 1 calc R . .
C3 C 0.2950(3) 0.24996(15) 0.0475(4) 0.0302(9) Uani 1 1 d . . .
C4 C 0.3631(3) 0.23808(15) -0.0236(3) 0.0302(9) Uani 1 1 d . . .
H4 H 0.3657 0.2613 -0.0875 0.036 Uiso 1 1 calc R . .
C5 C 0.4287(3) 0.19182(14) -0.0025(3) 0.0241(8) Uani 1 1 d . . .
C6 C 0.4248(3) 0.15604(14) 0.0916(3) 0.0232(8) Uani 1 1 d . . .
C7 C 0.4840(3) 0.17637(13) -0.0918(3) 0.0255(8) Uani 1 1 d . . .
H7 H 0.4567 0.1925 -0.1726 0.031 Uiso 1 1 calc R . .
C8 C 0.5990(3) 0.11846(13) -0.1711(3) 0.0237(8) Uani 1 1 d . . .
C9 C 0.5430(4) 0.14241(14) -0.3018(3) 0.0299(9) Uani 1 1 d . . .
H9A H 0.4543 0.1409 -0.3301 0.036 Uiso 1 1 calc R . .
H9B H 0.5672 0.1792 -0.2991 0.036 Uiso 1 1 calc R . .
C10 C 0.5851(4) 0.11268(15) -0.3934(4) 0.0369(10) Uani 1 1 d . . .
H10A H 0.5519 0.1288 -0.4783 0.044 Uiso 1 1 calc R . .
H10B H 0.6739 0.1139 -0.3645 0.044 Uiso 1 1 calc R . .
C11 C 0.5439(4) 0.05700(15) -0.4008(3) 0.0380(10) Uani 1 1 d . . .
H11A H 0.5723 0.0378 -0.4602 0.046 Uiso 1 1 calc R . .
H11B H 0.4549 0.0560 -0.4346 0.046 Uiso 1 1 calc R . .
C12 C 0.5907(4) 0.03033(15) -0.2720(3) 0.0323(9) Uani 1 1 d . . .
H12A H 0.6792 0.0268 -0.2436 0.039 Uiso 1 1 calc R . .
H12B H 0.5558 -0.0049 -0.2800 0.039 Uiso 1 1 calc R . .
C13 C 0.5588(3) 0.06080(13) -0.1731(3) 0.0246(8) Uani 1 1 d . . .
C14 C 0.6533(3) -0.00504(13) -0.0209(3) 0.0229(8) Uani 1 1 d . . .
H14 H 0.6374 -0.0267 -0.0928 0.028 Uiso 1 1 calc R . .
C15 C 0.7196(3) -0.02802(13) 0.1029(3) 0.0210(7) Uani 1 1 d . . .
C16 C 0.7770(3) -0.07541(14) 0.1027(3) 0.0264(8) Uani 1 1 d . . .
H16 H 0.7677 -0.0915 0.0244 0.032 Uiso 1 1 calc R . .
C17 C 0.8462(4) -0.09889(14) 0.2134(4) 0.0300(9) Uani 1 1 d . . .
C18 C 0.8606(3) -0.07628(15) 0.3290(3) 0.0293(9) Uani 1 1 d . . .
H18 H 0.9094 -0.0923 0.4059 0.035 Uiso 1 1 calc R . .
C19 C 0.8026(3) -0.03011(14) 0.3301(3) 0.0266(8) Uani 1 1 d . . .
C20 C 0.7323(3) -0.00426(13) 0.2190(3) 0.0223(7) Uani 1 1 d . . .
C21 C 0.9342(3) 0.09820(15) 0.1008(4) 0.0339(9) Uani 1 1 d . . .
C22 C 0.9847(4) 0.15244(18) 0.1036(5) 0.0472(12) Uani 1 1 d . . .
H22A H 0.9331 0.1719 0.0297 0.071 Uiso 1 1 calc R . .
H22B H 1.0660 0.1502 0.1018 0.071 Uiso 1 1 calc R . .
H22C H 0.9876 0.1702 0.1810 0.071 Uiso 1 1 calc R . .
C23 C 0.9300(4) 0.0699(2) -0.0194(5) 0.0628(15) Uani 1 1 d . . .
H23A H 0.8918 0.0359 -0.0236 0.094 Uiso 1 1 calc R . .
H23B H 1.0119 0.0651 -0.0179 0.094 Uiso 1 1 calc R . .
H23C H 0.8835 0.0904 -0.0938 0.094 Uiso 1 1 calc R . .
C24 C 1.0067(4) 0.0680(2) 0.2181(5) 0.0723(18) Uani 1 1 d . . .
H24A H 1.0044 0.0860 0.2932 0.108 Uiso 1 1 calc R . .
H24B H 1.0902 0.0653 0.2231 0.108 Uiso 1 1 calc R . .
H24C H 0.9726 0.0332 0.2139 0.108 Uiso 1 1 calc R . .
C25 C 0.7971(5) 0.24557(19) 0.2655(5) 0.0678(16) Uani 1 1 d . . .
H25A H 0.8558 0.2318 0.2317 0.102 Uiso 1 1 calc R . .
H25B H 0.8350 0.2726 0.3280 0.102 Uiso 1 1 calc R . .
H25C H 0.7289 0.2604 0.1964 0.102 Uiso 1 1 calc R . .
C26 C 0.7528(4) 0.20189(15) 0.3284(4) 0.0343(9) Uani 1 1 d . . .
C27 C 0.8545(5) 0.1776(2) 0.4356(5) 0.082(2) Uani 1 1 d . . .
H27A H 0.8251 0.1467 0.4655 0.122 Uiso 1 1 calc R . .
H27B H 0.8854 0.2025 0.5051 0.122 Uiso 1 1 calc R . .
H27C H 0.9190 0.1677 0.4059 0.122 Uiso 1 1 calc R . .
C28 C 0.6545(5) 0.22131(18) 0.3728(4) 0.0512(13) Uani 1 1 d . . .
H28A H 0.5855 0.2329 0.2997 0.077 Uiso 1 1 calc R . .
H28B H 0.6852 0.2503 0.4315 0.077 Uiso 1 1 calc R . .
H28C H 0.6295 0.1932 0.4158 0.077 Uiso 1 1 calc R . .
Hf1 Hf 0.664333(13) 0.105538(5) 0.122509(13) 0.01990(5) Uani 1 1 d . . .
N1 N 0.5674(2) 0.14232(11) -0.0682(3) 0.0202(6) Uani 1 1 d . . .
N2 N 0.6151(3) 0.04148(11) -0.0407(3) 0.0206(6) Uani 1 1 d . . .
O1 O 0.4841(2) 0.11224(9) 0.1130(2) 0.0234(5) Uani 1 1 d . . .
O2 O 0.8157(2) 0.10270(10) 0.0981(2) 0.0285(6) Uani 1 1 d . . .
O3 O 0.6792(2) 0.03997(9) 0.2248(2) 0.0273(6) Uani 1 1 d . . .
O4 O 0.7015(2) 0.16337(10) 0.2365(2) 0.0324(6) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag












































































Br1 C1 1.889(4) . ?
Br2 C3 1.893(4) . ?
Br3 C17 1.895(4) . ?
Br4 C19 1.892(3) . ?
C1 C2 1.380(5) . ?
C1 C6 1.404(5) . ?
C2 C3 1.382(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(5) . ?
C4 C5 1.400(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.425(5) . ?
C5 C7 1.451(5) . ?
C6 O1 1.309(4) . ?
C7 N1 1.281(4) . ?
C7 H7 0.9500 . ?
C8 N1 1.485(4) . ?
C8 C9 1.519(5) . ?
C8 C13 1.561(5) . ?
C9 C10 1.517(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.511(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.526(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.527(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N2 1.491(4) . ?
C14 N2 1.275(4) . ?
C14 C15 1.464(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.402(5) . ?
C15 C20 1.410(5) . ?
C16 C17 1.369(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(5) . ?
C18 C19 1.380(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.404(5) . ?
C20 O3 1.319(4) . ?
C21 O2 1.410(4) . ?
C21 C24 1.513(6) . ?
C21 C22 1.520(6) . ?
C21 C23 1.532(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.528(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O4 1.410(4) . ?
C26 C27 1.509(6) . ?
C26 C28 1.521(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
Hf1 O4 1.918(2) . ?
Hf1 O2 1.927(2) . ?
Hf1 O3 2.023(2) . ?
Hf1 O1 2.122(2) . ?
Hf1 N1 2.259(3) . ?
Hf1 N2 2.391(3) . ?



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

















































































































































C2 C1 C6 122.6(3) . . ?
C2 C1 Br1 119.8(3) . . ?
C6 C1 Br1 117.6(3) . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 Br2 120.0(3) . . ?
C2 C3 Br2 119.5(3) . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.8(3) . . ?
C4 C5 C7 118.9(3) . . ?
C6 C5 C7 119.4(3) . . ?
O1 C6 C1 121.5(3) . . ?
O1 C6 C5 122.4(3) . . ?
C1 C6 C5 116.1(3) . . ?
N1 C7 C5 124.0(3) . . ?
N1 C7 H7 118.0 . . ?
C5 C7 H7 118.0 . . ?
N1 C8 C9 116.8(3) . . ?
N1 C8 C13 104.0(3) . . ?
C9 C8 C13 110.4(3) . . ?
C10 C9 C8 109.0(3) . . ?
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 . . ?
C11 C10 C9 109.7(3) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 112.1(3) . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C13 111.6(3) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N2 C13 C12 115.2(3) . . ?
N2 C13 C8 106.2(3) . . ?
C12 C13 C8 110.1(3) . . ?
N2 C14 C15 125.8(3) . . ?
N2 C14 H14 117.1 . . ?
C15 C14 H14 117.1 . . ?
C16 C15 C20 119.6(3) . . ?
C16 C15 C14 116.5(3) . . ?
C20 C15 C14 123.9(3) . . ?
C17 C16 C15 121.1(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.5(3) . . ?
C16 C17 Br3 119.9(3) . . ?
C18 C17 Br3 119.6(3) . . ?
C19 C18 C17 118.8(3) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 122.7(3) . . ?
C18 C19 Br4 119.4(3) . . ?
C20 C19 Br4 117.9(3) . . ?
O3 C20 C19 120.5(3) . . ?
O3 C20 C15 122.2(3) . . ?
C19 C20 C15 117.3(3) . . ?
O2 C21 C24 108.1(3) . . ?
O2 C21 C22 108.2(3) . . ?
C24 C21 C22 111.1(4) . . ?
O2 C21 C23 108.1(3) . . ?
C24 C21 C23 111.1(4) . . ?
C22 C21 C23 110.1(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O4 C26 C27 108.0(4) . . ?
O4 C26 C28 107.3(3) . . ?
C27 C26 C28 111.2(4) . . ?
O4 C26 C25 107.8(3) . . ?
C27 C26 C25 111.7(4) . . ?
C28 C26 C25 110.6(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O4 Hf1 O2 97.29(11) . . ?
O4 Hf1 O3 108.27(10) . . ?
O2 Hf1 O3 99.15(10) . . ?
O4 Hf1 O1 87.32(10) . . ?
O2 Hf1 O1 169.28(9) . . ?
O3 Hf1 O1 88.49(9) . . ?
O4 Hf1 N1 103.38(10) . . ?
O2 Hf1 N1 93.43(10) . . ?
O3 Hf1 N1 143.96(10) . . ?
O1 Hf1 N1 76.06(9) . . ?
O4 Hf1 N2 172.57(10) . . ?
O2 Hf1 N2 80.91(10) . . ?
O3 Hf1 N2 79.15(9) . . ?
O1 Hf1 N2 93.28(9) . . ?
N1 Hf1 N2 69.65(9) . . ?
C7 N1 C8 121.3(3) . . ?
C7 N1 Hf1 125.3(2) . . ?
C8 N1 Hf1 113.0(2) . . ?
C14 N2 C13 119.6(3) . . ?
C14 N2 Hf1 122.9(2) . . ?
C13 N2 Hf1 116.3(2) . . ?
C6 O1 Hf1 123.4(2) . . ?
C21 O2 Hf1 170.8(2) . . ?
C20 O3 Hf1 129.7(2) . . ?
C26 O4 Hf1 168.3(3) . . ?



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













































































































C6 C1 C2 C3 -0.4(6) . . . . ?
Br1 C1 C2 C3 -179.0(3) . . . . ?
C1 C2 C3 C4 2.4(6) . . . . ?
C1 C2 C3 Br2 178.9(3) . . . . ?
C2 C3 C4 C5 -2.6(6) . . . . ?
Br2 C3 C4 C5 -179.1(3) . . . . ?
C3 C4 C5 C6 0.8(6) . . . . ?
C3 C4 C5 C7 170.2(3) . . . . ?
C2 C1 C6 O1 -179.6(3) . . . . ?
Br1 C1 C6 O1 -0.9(5) . . . . ?
C2 C1 C6 C5 -1.4(5) . . . . ?
Br1 C1 C6 C5 177.3(2) . . . . ?
C4 C5 C6 O1 179.4(3) . . . . ?
C7 C5 C6 O1 10.0(5) . . . . ?
C4 C5 C6 C1 1.1(5) . . . . ?
C7 C5 C6 C1 -168.2(3) . . . . ?
C4 C5 C7 N1 163.1(4) . . . . ?
C6 C5 C7 N1 -27.4(5) . . . . ?
N1 C8 C9 C10 -179.6(3) . . . . ?
C13 C8 C9 C10 -61.0(4) . . . . ?
C8 C9 C10 C11 61.7(4) . . . . ?
C9 C10 C11 C12 -58.4(5) . . . . ?
C10 C11 C12 C13 54.0(5) . . . . ?
C11 C12 C13 N2 -172.0(3) . . . . ?
C11 C12 C13 C8 -51.9(4) . . . . ?
N1 C8 C13 N2 -52.2(3) . . . . ?
C9 C8 C13 N2 -178.3(3) . . . . ?
N1 C8 C13 C12 -177.6(3) . . . . ?
C9 C8 C13 C12 56.2(4) . . . . ?
N2 C14 C15 C16 -165.8(3) . . . . ?
N2 C14 C15 C20 11.4(6) . . . . ?
C20 C15 C16 C17 -0.6(5) . . . . ?
C14 C15 C16 C17 176.7(3) . . . . ?
C15 C16 C17 C18 0.3(6) . . . . ?
C15 C16 C17 Br3 -179.0(3) . . . . ?
C16 C17 C18 C19 0.8(6) . . . . ?
Br3 C17 C18 C19 -179.8(3) . . . . ?
C17 C18 C19 C20 -1.9(6) . . . . ?
C17 C18 C19 Br4 179.5(3) . . . . ?
C18 C19 C20 O3 -179.5(3) . . . . ?
Br4 C19 C20 O3 -0.9(5) . . . . ?
C18 C19 C20 C15 1.6(5) . . . . ?
Br4 C19 C20 C15 -179.8(2) . . . . ?
C16 C15 C20 O3 -179.2(3) . . . . ?
C14 C15 C20 O3 3.7(5) . . . . ?
C16 C15 C20 C19 -0.4(5) . . . . ?
C14 C15 C20 C19 -177.5(3) . . . . ?
C5 C7 N1 C8 164.3(3) . . . . ?
C5 C7 N1 Hf1 -8.0(5) . . . . ?
C9 C8 N1 C7 9.8(5) . . . . ?
C13 C8 N1 C7 -112.2(3) . . . . ?
C9 C8 N1 Hf1 -177.0(2) . . . . ?
C13 C8 N1 Hf1 61.0(3) . . . . ?
O4 Hf1 N1 C7 -45.8(3) . . . . ?
O2 Hf1 N1 C7 -144.1(3) . . . . ?
O3 Hf1 N1 C7 105.2(3) . . . . ?
O1 Hf1 N1 C7 38.0(3) . . . . ?
N2 Hf1 N1 C7 136.9(3) . . . . ?
O4 Hf1 N1 C8 141.4(2) . . . . ?
O2 Hf1 N1 C8 43.0(2) . . . . ?
O3 Hf1 N1 C8 -67.7(3) . . . . ?
O1 Hf1 N1 C8 -134.9(2) . . . . ?
N2 Hf1 N1 C8 -36.0(2) . . . . ?
C15 C14 N2 C13 174.4(3) . . . . ?
C15 C14 N2 Hf1 7.4(5) . . . . ?
C12 C13 N2 C14 -20.9(5) . . . . ?
C8 C13 N2 C14 -143.2(3) . . . . ?
C12 C13 N2 Hf1 146.9(3) . . . . ?
C8 C13 N2 Hf1 24.6(3) . . . . ?
O4 Hf1 N2 C14 151.2(8) . . . . ?
O2 Hf1 N2 C14 74.7(3) . . . . ?
O3 Hf1 N2 C14 -26.5(3) . . . . ?
O1 Hf1 N2 C14 -114.4(3) . . . . ?
N1 Hf1 N2 C14 171.8(3) . . . . ?
O4 Hf1 N2 C13 -16.2(9) . . . . ?
O2 Hf1 N2 C13 -92.7(2) . . . . ?
O3 Hf1 N2 C13 166.1(2) . . . . ?
O1 Hf1 N2 C13 78.3(2) . . . . ?
N1 Hf1 N2 C13 4.4(2) . . . . ?
C1 C6 O1 Hf1 -138.4(3) . . . . ?
C5 C6 O1 Hf1 43.4(4) . . . . ?
O4 Hf1 O1 C6 49.3(3) . . . . ?
O2 Hf1 O1 C6 -66.5(6) . . . . ?
O3 Hf1 O1 C6 157.7(3) . . . . ?
N1 Hf1 O1 C6 -55.2(2) . . . . ?
N2 Hf1 O1 C6 -123.3(3) . . . . ?
C24 C21 O2 Hf1 15.4(17) . . . . ?
C22 C21 O2 Hf1 -105.0(14) . . . . ?
C23 C21 O2 Hf1 135.8(14) . . . . ?
O4 Hf1 O2 C21 67.5(15) . . . . ?
O3 Hf1 O2 C21 -42.4(15) . . . . ?
O1 Hf1 O2 C21 -177.5(13) . . . . ?
N1 Hf1 O2 C21 171.4(15) . . . . ?
N2 Hf1 O2 C21 -119.8(15) . . . . ?
C19 C20 O3 Hf1 137.4(3) . . . . ?
C15 C20 O3 Hf1 -43.9(5) . . . . ?
O4 Hf1 O3 C20 -134.2(3) . . . . ?
O2 Hf1 O3 C20 -33.3(3) . . . . ?
O1 Hf1 O3 C20 139.1(3) . . . . ?
N1 Hf1 O3 C20 75.6(3) . . . . ?
N2 Hf1 O3 C20 45.5(3) . . . . ?
C27 C26 O4 Hf1 -32.5(14) . . . . ?
C28 C26 O4 Hf1 -152.6(11) . . . . ?
C25 C26 O4 Hf1 88.3(13) . . . . ?
O2 Hf1 O4 C26 -32.2(13) . . . . ?
O3 Hf1 O4 C26 69.9(13) . . . . ?
O1 Hf1 O4 C26 157.5(13) . . . . ?
N1 Hf1 O4 C26 -127.5(12) . . . . ?
N2 Hf1 O4 C26 -107.7(13) . . . . ?



_diffrn_measured_fraction_theta_max 0.881

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         1.736

_refine_diff_density_min         -1.257

_refine_diff_density_rms         0.151
####################################################################### 
# 
# 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_Zr4
_database_code_depnum_ccdc_archive 'CCDC 1815598'
loop_
_audit_author_name
_audit_author_address
'Venkatachalam Ramkumar' 'Indian Institute of Technology Madras'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C40 H28 Cl8 N4 O4 Zr'

_chemical_formula_sum            'C40 H28 Cl8 N4 O4 Zr'


_chemical_formula_weight         1003.48



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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic

_symmetry_space_group_name_H-M   Fdd2

_symmetry_space_group_name_Hall  ' F 2 -2d'

loop_

_symmetry_equiv_pos_as_xyz
















'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'



_cell_length_a                   26.427(3)

_cell_length_b                   46.619(5)

_cell_length_c                   12.8792(11)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     15867(3)

_cell_formula_units_Z            16

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    8813

_cell_measurement_theta_min      0.00

_cell_measurement_theta_max      0.00



_exptl_crystal_description       Block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.35

_exptl_crystal_size_mid          0.25

_exptl_crystal_size_min          0.15

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.680

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             8064

_exptl_absorpt_coefficient_mu    0.865

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.7516

_exptl_absorpt_correction_T_max  0.8812

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'




_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      173(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 APEXII 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            57581

_diffrn_reflns_av_R_equivalents  0.0733

_diffrn_reflns_av_sigmaI/netI    0.0732

_diffrn_reflns_limit_h_min       -40

_diffrn_reflns_limit_h_max       39

_diffrn_reflns_limit_k_min       -71

_diffrn_reflns_limit_k_max       54

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       18

_diffrn_reflns_theta_min         1.75

_diffrn_reflns_theta_max         33.08

_reflns_number_total             13823

_reflns_number_gt                11034

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       APEXII,Bruker,2004

_computing_cell_refinement       APEXII,Bruker,2004

_computing_data_reduction        SAINT,Bruker,2004

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0585P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   -0.05(3)

_refine_ls_number_reflns         13823

_refine_ls_number_parameters     509

_refine_ls_number_restraints     1

_refine_ls_R_factor_all          0.0691

_refine_ls_R_factor_gt           0.0455

_refine_ls_wR_factor_ref         0.1134

_refine_ls_wR_factor_gt          0.1010

_refine_ls_goodness_of_fit_ref   1.024

_refine_ls_restrained_S_all      1.024

_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





















































































C1 C 0.08380(11) 0.14446(7) 1.0695(3) 0.0151(6) Uani 1 1 d . . .
C2 C 0.07698(12) 0.17315(7) 1.1031(3) 0.0179(6) Uani 1 1 d . . .
C3 C 0.07531(12) 0.18013(8) 1.2075(3) 0.0205(7) Uani 1 1 d . . .
H3 H 0.0719 0.1996 1.2286 0.025 Uiso 1 1 calc R . .
C4 C 0.07862(12) 0.15855(8) 1.2808(3) 0.0227(7) Uani 1 1 d . . .
C5 C 0.08308(12) 0.13054(8) 1.2521(3) 0.0206(7) Uani 1 1 d . . .
H5 H 0.0840 0.1159 1.3034 0.025 Uiso 1 1 calc R . .
C6 C 0.08636(11) 0.12334(7) 1.1463(3) 0.0169(6) Uani 1 1 d . . .
C7 C 0.09581(12) 0.09329(7) 1.1216(3) 0.0184(6) Uani 1 1 d . . .
H7 H 0.0884 0.0797 1.1746 0.022 Uiso 1 1 calc R . .
C8 C 0.12491(13) 0.05213(7) 1.0299(3) 0.0166(6) Uani 1 1 d . . .
C9 C 0.12071(13) 0.03583(7) 1.1337(3) 0.0211(6) Uani 1 1 d . . .
H9A H 0.1405 0.0461 1.1873 0.025 Uiso 1 1 calc R . .
H9B H 0.0849 0.0356 1.1562 0.025 Uiso 1 1 calc R . .
C10 C 0.13994(13) 0.00510(7) 1.1258(3) 0.0240(7) Uani 1 1 d . . .
H10A H 0.1383 -0.0042 1.1948 0.029 Uiso 1 1 calc R . .
H10B H 0.1181 -0.0059 1.0776 0.029 Uiso 1 1 calc R . .
C11 C 0.19428(13) 0.00466(7) 1.0865(3) 0.0219(7) Uani 1 1 d . . .
H11A H 0.2066 -0.0153 1.0824 0.026 Uiso 1 1 calc R . .
H11B H 0.2164 0.0154 1.1348 0.026 Uiso 1 1 calc R . .
C12 C 0.19571(13) 0.01848(7) 0.9792(3) 0.0202(7) Uani 1 1 d . . .
H12A H 0.1731 0.0078 0.9316 0.024 Uiso 1 1 calc R . .
H12B H 0.2305 0.0174 0.9512 0.024 Uiso 1 1 calc R . .
C13 C 0.17884(12) 0.04985(7) 0.9843(3) 0.0174(6) Uani 1 1 d . . .
C14 C 0.19140(13) 0.05285(7) 0.8005(3) 0.0179(6) Uiso 1 1 d . . .
H14 H 0.2004 0.0332 0.8063 0.021 Uiso 1 1 calc R . .
C15 C 0.19301(11) 0.06517(7) 0.6979(3) 0.0168(6) Uani 1 1 d . . .
C16 C 0.19562(12) 0.04681(7) 0.6121(3) 0.0186(6) Uani 1 1 d . . .
H16 H 0.1954 0.0266 0.6221 0.022 Uiso 1 1 calc R . .
C17 C 0.19847(13) 0.05778(7) 0.5138(3) 0.0196(6) Uani 1 1 d . . .
C18 C 0.20073(12) 0.08716(7) 0.4963(3) 0.0200(6) Uani 1 1 d . . .
H18 H 0.2033 0.0945 0.4278 0.024 Uiso 1 1 calc R . .
C19 C 0.19912(13) 0.10538(7) 0.5805(3) 0.0187(6) Uani 1 1 d . . .
C20 C 0.19313(11) 0.09540(7) 0.6832(3) 0.0161(6) Uani 1 1 d . . .
C21 C 0.07363(11) 0.07451(7) 0.7325(2) 0.0152(6) Uani 1 1 d . . .
C22 C 0.06573(12) 0.04572(7) 0.7025(3) 0.0174(6) Uani 1 1 d . . .
C23 C 0.05414(12) 0.03793(7) 0.6022(3) 0.0183(6) Uani 1 1 d . . .
H23 H 0.0503 0.0183 0.5842 0.022 Uiso 1 1 calc R . .
C24 C 0.04804(12) 0.05930(7) 0.5271(3) 0.0191(6) Uani 1 1 d . . .
C25 C 0.05164(12) 0.08782(7) 0.5540(3) 0.0181(6) Uani 1 1 d . . .
H25 H 0.0449 0.1023 0.5039 0.022 Uiso 1 1 calc R . .
C26 C 0.06523(11) 0.09541(7) 0.6550(3) 0.0164(6) Uani 1 1 d . . .
C27 C 0.06997(12) 0.12600(7) 0.6783(2) 0.0167(6) Uani 1 1 d . . .
H27 H 0.0544 0.1389 0.6311 0.020 Uiso 1 1 calc R . .
C28 C 0.09537(12) 0.16899(6) 0.7618(2) 0.0149(6) Uani 1 1 d . . .
C29 C 0.07462(13) 0.18440(7) 0.6671(3) 0.0190(6) Uani 1 1 d . . .
H29A H 0.0378 0.1806 0.6618 0.023 Uiso 1 1 calc R . .
H29B H 0.0910 0.1765 0.6041 0.023 Uiso 1 1 calc R . .
C30 C 0.08328(13) 0.21666(7) 0.6707(3) 0.0224(7) Uani 1 1 d . . .
H30A H 0.0651 0.2249 0.7308 0.027 Uiso 1 1 calc R . .
H30B H 0.0697 0.2256 0.6067 0.027 Uiso 1 1 calc R . .
C31 C 0.13981(13) 0.22315(7) 0.6800(3) 0.0207(7) Uani 1 1 d . . .
H31A H 0.1580 0.2154 0.6189 0.025 Uiso 1 1 calc R . .
H31B H 0.1452 0.2441 0.6824 0.025 Uiso 1 1 calc R . .
C32 C 0.16017(12) 0.20933(7) 0.7792(3) 0.0182(6) Uani 1 1 d . . .
H32A H 0.1428 0.2178 0.8400 0.022 Uiso 1 1 calc R . .
H32B H 0.1968 0.2135 0.7855 0.022 Uiso 1 1 calc R . .
C33 C 0.15215(12) 0.17677(6) 0.7792(2) 0.0145(6) Uani 1 1 d . . .
C34 C 0.18931(11) 0.17611(7) 0.9462(3) 0.0158(6) Uani 1 1 d . . .
H34 H 0.1968 0.1956 0.9308 0.019 Uiso 1 1 calc R . .
C35 C 0.20386(12) 0.16581(7) 1.0488(2) 0.0166(6) Uani 1 1 d . . .
C36 C 0.21370(11) 0.18635(7) 1.1255(3) 0.0187(6) Uani 1 1 d . . .
H36 H 0.2133 0.2062 1.1084 0.022 Uiso 1 1 calc R . .
C37 C 0.22382(12) 0.17788(7) 1.2247(3) 0.0188(6) Uani 1 1 d . . .
C38 C 0.22622(12) 0.14900(8) 1.2521(3) 0.0191(6) Uani 1 1 d . . .
H38 H 0.2335 0.1433 1.3212 0.023 Uiso 1 1 calc R . .
C39 C 0.21750(12) 0.12879(7) 1.1743(3) 0.0172(6) Uani 1 1 d . . .
C40 C 0.20569(11) 0.13611(7) 1.0716(3) 0.0161(6) Uani 1 1 d . . .
Cl1 Cl 0.07392(3) 0.201067(18) 1.01382(7) 0.02324(17) Uani 1 1 d . . .
Cl2 Cl 0.07709(4) 0.16798(2) 1.41145(7) 0.0321(2) Uani 1 1 d . . .
Cl3 Cl 0.20048(4) 0.035233(18) 0.40565(7) 0.02744(18) Uani 1 1 d . . .
Cl4 Cl 0.20428(4) 0.141988(18) 0.55730(7) 0.02761(19) Uani 1 1 d . . .
Cl5 Cl 0.07342(4) 0.018484(18) 0.79376(7) 0.02559(18) Uani 1 1 d . . .
Cl6 Cl 0.03497(3) 0.049246(19) 0.39934(7) 0.02633(18) Uani 1 1 d . . .
Cl7 Cl 0.23374(4) 0.20375(2) 1.32132(7) 0.0295(2) Uani 1 1 d . . .
Cl8 Cl 0.21904(3) 0.092795(18) 1.20873(7) 0.02313(17) Uani 1 1 d . . .
N1 N 0.11289(10) 0.08334(6) 1.0366(2) 0.0156(5) Uani 1 1 d . . .
N2 N 0.17898(9) 0.06578(5) 0.8850(2) 0.0159(5) Uani 1 1 d . . .
N3 N 0.09305(10) 0.13713(6) 0.7561(2) 0.0144(5) Uani 1 1 d . . .
N4 N 0.16773(9) 0.16174(5) 0.8753(2) 0.0143(5) Uani 1 1 d . . .
O1 O 0.08802(8) 0.13796(5) 0.97088(17) 0.0161(4) Uani 1 1 d . . .
O2 O 0.08754(8) 0.08178(5) 0.82674(17) 0.0153(4) Uani 1 1 d . . .
O3 O 0.18897(9) 0.11334(5) 0.76177(19) 0.0172(5) Uani 1 1 d . . .
O4 O 0.19591(9) 0.11662(5) 1.00077(18) 0.0173(5) Uani 1 1 d . . .
Zr1 Zr 0.138909(10) 0.112253(6) 0.88913(2) 0.01244(6) Uani 1 1 d . . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag
































































































C1 O1 1.310(4) . ?
C1 C6 1.398(5) . ?
C1 C2 1.417(5) . ?
C2 C3 1.384(5) . ?
C2 Cl1 1.739(3) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(5) . ?
C4 Cl2 1.740(3) . ?
C5 C6 1.406(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.458(5) . ?
C7 N1 1.272(4) . ?
C7 H7 0.9500 . ?
C8 N1 1.491(4) . ?
C8 C9 1.542(5) . ?
C8 C13 1.545(5) . ?
C9 C10 1.523(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.522(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.525(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.530(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N2 1.479(4) . ?
C14 N2 1.287(4) . ?
C14 C15 1.442(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(5) . ?
C15 C20 1.422(5) . ?
C16 C17 1.367(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.389(5) . ?
C17 Cl3 1.746(3) . ?
C18 C19 1.377(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(5) . ?
C19 Cl4 1.738(3) . ?
C20 O3 1.318(4) . ?
C21 O2 1.313(4) . ?
C21 C26 1.412(5) . ?
C21 C22 1.412(5) . ?
C22 C23 1.376(5) . ?
C22 Cl5 1.743(3) . ?
C23 C24 1.397(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(5) . ?
C24 Cl6 1.746(3) . ?
C25 C26 1.396(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.463(4) . ?
C27 N3 1.282(4) . ?
C27 H27 0.9500 . ?
C28 N3 1.488(4) . ?
C28 C29 1.518(4) . ?
C28 C33 1.560(4) . ?
C29 C30 1.522(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.529(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.528(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.533(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N4 1.481(4) . ?
C34 N4 1.268(4) . ?
C34 C35 1.458(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.400(5) . ?
C35 C40 1.416(4) . ?
C36 C37 1.364(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(5) . ?
C37 Cl7 1.753(3) . ?
C38 C39 1.394(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.402(5) . ?
C39 Cl8 1.736(3) . ?
C40 O4 1.313(4) . ?
N1 Zr1 2.428(3) . ?
N2 Zr1 2.412(3) . ?
N3 Zr1 2.398(3) . ?
N4 Zr1 2.436(3) . ?
O1 Zr1 2.087(2) . ?
O2 Zr1 2.123(2) . ?
O3 Zr1 2.108(2) . ?
O4 Zr1 2.092(2) . ?



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 C1 C6 121.3(3) . . ?
O1 C1 C2 121.7(3) . . ?
C6 C1 C2 117.0(3) . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 Cl1 117.7(3) . . ?
C1 C2 Cl1 120.7(3) . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 121.2(3) . . ?
C5 C4 Cl2 120.4(3) . . ?
C3 C4 Cl2 118.4(3) . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 C7 122.1(3) . . ?
C5 C6 C7 116.8(3) . . ?
N1 C7 C6 126.8(3) . . ?
N1 C7 H7 116.6 . . ?
C6 C7 H7 116.6 . . ?
N1 C8 C9 114.6(3) . . ?
N1 C8 C13 106.6(3) . . ?
C9 C8 C13 111.2(3) . . ?
C10 C9 C8 112.4(3) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 C9 110.5(3) . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 C12 108.6(3) . . ?
C10 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
C10 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 C13 110.9(3) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.0 . . ?
N2 C13 C12 116.2(3) . . ?
N2 C13 C8 107.2(2) . . ?
C12 C13 C8 110.5(3) . . ?
N2 C14 C15 126.6(3) . . ?
N2 C14 H14 116.7 . . ?
C15 C14 H14 116.7 . . ?
C16 C15 C20 120.1(3) . . ?
C16 C15 C14 118.8(3) . . ?
C20 C15 C14 121.1(3) . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 121.4(3) . . ?
C16 C17 Cl3 121.0(3) . . ?
C18 C17 Cl3 117.6(3) . . ?
C19 C18 C17 118.6(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C20 122.5(3) . . ?
C18 C19 Cl4 117.9(3) . . ?
C20 C19 Cl4 119.6(3) . . ?
O3 C20 C19 121.3(3) . . ?
O3 C20 C15 121.8(3) . . ?
C19 C20 C15 116.8(3) . . ?
O2 C21 C26 121.3(3) . . ?
O2 C21 C22 122.7(3) . . ?
C26 C21 C22 116.1(3) . . ?
C23 C22 C21 122.7(3) . . ?
C23 C22 Cl5 117.8(3) . . ?
C21 C22 Cl5 119.4(3) . . ?
C22 C23 C24 119.1(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C25 C24 C23 120.5(3) . . ?
C25 C24 Cl6 120.6(3) . . ?
C23 C24 Cl6 118.9(3) . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 121.6(3) . . ?
C25 C26 C27 117.4(3) . . ?
C21 C26 C27 121.0(3) . . ?
N3 C27 C26 126.5(3) . . ?
N3 C27 H27 116.7 . . ?
C26 C27 H27 116.7 . . ?
N3 C28 C29 114.7(3) . . ?
N3 C28 C33 106.2(2) . . ?
C29 C28 C33 110.6(3) . . ?
C28 C29 C30 112.9(3) . . ?
C28 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
C28 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 C31 110.2(3) . . ?
C29 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C32 C31 C30 109.0(3) . . ?
C32 C31 H31A 109.9 . . ?
C30 C31 H31A 109.9 . . ?
C32 C31 H31B 109.9 . . ?
C30 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
C31 C32 C33 111.7(3) . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
N4 C33 C32 115.5(3) . . ?
N4 C33 C28 106.1(2) . . ?
C32 C33 C28 111.3(2) . . ?
N4 C34 C35 126.6(3) . . ?
N4 C34 H34 116.7 . . ?
C35 C34 H34 116.7 . . ?
C36 C35 C40 121.1(3) . . ?
C36 C35 C34 117.6(3) . . ?
C40 C35 C34 121.3(3) . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 121.7(3) . . ?
C36 C37 Cl7 119.7(3) . . ?
C38 C37 Cl7 118.6(3) . . ?
C37 C38 C39 117.7(3) . . ?
C37 C38 H38 121.2 . . ?
C39 C38 H38 121.2 . . ?
C38 C39 C40 123.4(3) . . ?
C38 C39 Cl8 117.8(3) . . ?
C40 C39 Cl8 118.8(3) . . ?
O4 C40 C39 122.1(3) . . ?
O4 C40 C35 121.7(3) . . ?
C39 C40 C35 116.2(3) . . ?
C7 N1 C8 118.7(3) . . ?
C7 N1 Zr1 124.8(2) . . ?
C8 N1 Zr1 115.86(19) . . ?
C14 N2 C13 119.8(3) . . ?
C14 N2 Zr1 123.5(2) . . ?
C13 N2 Zr1 115.54(19) . . ?
C27 N3 C28 117.5(3) . . ?
C27 N3 Zr1 127.1(2) . . ?
C28 N3 Zr1 115.25(18) . . ?
C34 N4 C33 118.5(3) . . ?
C34 N4 Zr1 126.1(2) . . ?
C33 N4 Zr1 114.97(18) . . ?
C1 O1 Zr1 132.6(2) . . ?
C21 O2 Zr1 134.6(2) . . ?
C20 O3 Zr1 129.4(2) . . ?
C40 O4 Zr1 133.3(2) . . ?
O1 Zr1 O4 93.52(9) . . ?
O1 Zr1 O3 141.56(9) . . ?
O4 Zr1 O3 94.62(9) . . ?
O1 Zr1 O2 99.39(8) . . ?
O4 Zr1 O2 141.78(9) . . ?
O3 Zr1 O2 97.06(9) . . ?
O1 Zr1 N3 75.93(9) . . ?
O4 Zr1 N3 143.88(9) . . ?
O3 Zr1 N3 75.50(9) . . ?
O2 Zr1 N3 74.34(8) . . ?
O1 Zr1 N2 144.10(9) . . ?
O4 Zr1 N2 77.67(9) . . ?
O3 Zr1 N2 74.28(9) . . ?
O2 Zr1 N2 70.82(8) . . ?
N3 Zr1 N2 129.84(9) . . ?
O1 Zr1 N1 75.04(9) . . ?
O4 Zr1 N1 73.76(9) . . ?
O3 Zr1 N1 143.10(9) . . ?
O2 Zr1 N1 75.14(9) . . ?
N3 Zr1 N1 133.18(9) . . ?
N2 Zr1 N1 69.07(9) . . ?
O1 Zr1 N4 72.20(9) . . ?
O4 Zr1 N4 74.50(9) . . ?
O3 Zr1 N4 73.99(9) . . ?
O2 Zr1 N4 143.71(9) . . ?
N3 Zr1 N4 69.38(9) . . ?
N2 Zr1 N4 135.38(8) . . ?
N1 Zr1 N4 132.17(9) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag


















































































































































































































O1 C1 C2 C3 -176.4(3) . . . . ?
C6 C1 C2 C3 3.0(5) . . . . ?
O1 C1 C2 Cl1 0.0(4) . . . . ?
C6 C1 C2 Cl1 179.4(2) . . . . ?
C1 C2 C3 C4 -2.3(5) . . . . ?
Cl1 C2 C3 C4 -178.8(2) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C2 C3 C4 Cl2 179.3(3) . . . . ?
C3 C4 C5 C6 2.5(5) . . . . ?
Cl2 C4 C5 C6 -177.4(2) . . . . ?
O1 C1 C6 C5 178.4(3) . . . . ?
C2 C1 C6 C5 -1.0(4) . . . . ?
O1 C1 C6 C7 2.5(4) . . . . ?
C2 C1 C6 C7 -176.9(3) . . . . ?
C4 C5 C6 C1 -1.7(4) . . . . ?
C4 C5 C6 C7 174.4(3) . . . . ?
C1 C6 C7 N1 15.8(5) . . . . ?
C5 C6 C7 N1 -160.3(3) . . . . ?
N1 C8 C9 C10 -172.5(3) . . . . ?
C13 C8 C9 C10 -51.5(4) . . . . ?
C8 C9 C10 C11 56.2(4) . . . . ?
C9 C10 C11 C12 -60.4(4) . . . . ?
C10 C11 C12 C13 62.0(4) . . . . ?
C11 C12 C13 N2 179.5(3) . . . . ?
C11 C12 C13 C8 -58.0(4) . . . . ?
N1 C8 C13 N2 -55.1(3) . . . . ?
C9 C8 C13 N2 179.4(3) . . . . ?
N1 C8 C13 C12 177.3(3) . . . . ?
C9 C8 C13 C12 51.8(4) . . . . ?
N2 C14 C15 C16 -165.1(3) . . . . ?
N2 C14 C15 C20 16.3(5) . . . . ?
C20 C15 C16 C17 0.2(5) . . . . ?
C14 C15 C16 C17 -178.4(3) . . . . ?
C15 C16 C17 C18 2.4(5) . . . . ?
C15 C16 C17 Cl3 -178.7(3) . . . . ?
C16 C17 C18 C19 -1.2(5) . . . . ?
Cl3 C17 C18 C19 179.9(3) . . . . ?
C17 C18 C19 C20 -2.7(5) . . . . ?
C17 C18 C19 Cl4 177.7(3) . . . . ?
C18 C19 C20 O3 -176.3(3) . . . . ?
Cl4 C19 C20 O3 3.2(4) . . . . ?
C18 C19 C20 C15 5.1(5) . . . . ?
Cl4 C19 C20 C15 -175.3(2) . . . . ?
C16 C15 C20 O3 177.6(3) . . . . ?
C14 C15 C20 O3 -3.8(5) . . . . ?
C16 C15 C20 C19 -3.8(4) . . . . ?
C14 C15 C20 C19 174.8(3) . . . . ?
O2 C21 C22 C23 -176.0(3) . . . . ?
C26 C21 C22 C23 4.6(5) . . . . ?
O2 C21 C22 Cl5 1.2(4) . . . . ?
C26 C21 C22 Cl5 -178.2(2) . . . . ?
C21 C22 C23 C24 -2.4(5) . . . . ?
Cl5 C22 C23 C24 -179.6(2) . . . . ?
C22 C23 C24 C25 -2.5(5) . . . . ?
C22 C23 C24 Cl6 178.3(2) . . . . ?
C23 C24 C25 C26 4.8(5) . . . . ?
Cl6 C24 C25 C26 -176.0(2) . . . . ?
C24 C25 C26 C21 -2.4(5) . . . . ?
C24 C25 C26 C27 178.2(3) . . . . ?
O2 C21 C26 C25 178.4(3) . . . . ?
C22 C21 C26 C25 -2.2(4) . . . . ?
O2 C21 C26 C27 -2.2(4) . . . . ?
C22 C21 C26 C27 177.2(3) . . . . ?
C25 C26 C27 N3 -162.2(3) . . . . ?
C21 C26 C27 N3 18.4(5) . . . . ?
N3 C28 C29 C30 -173.3(3) . . . . ?
C33 C28 C29 C30 -53.2(4) . . . . ?
C28 C29 C30 C31 58.1(4) . . . . ?
C29 C30 C31 C32 -59.5(4) . . . . ?
C30 C31 C32 C33 59.1(4) . . . . ?
C31 C32 C33 N4 -176.2(3) . . . . ?
C31 C32 C33 C28 -55.2(4) . . . . ?
N3 C28 C33 N4 -57.4(3) . . . . ?
C29 C28 C33 N4 177.5(2) . . . . ?
N3 C28 C33 C32 176.2(2) . . . . ?
C29 C28 C33 C32 51.2(3) . . . . ?
N4 C34 C35 C36 -162.0(3) . . . . ?
N4 C34 C35 C40 15.1(5) . . . . ?
C40 C35 C36 C37 -1.9(5) . . . . ?
C34 C35 C36 C37 175.2(3) . . . . ?
C35 C36 C37 C38 2.0(5) . . . . ?
C35 C36 C37 Cl7 -177.6(2) . . . . ?
C36 C37 C38 C39 -0.5(5) . . . . ?
Cl7 C37 C38 C39 179.1(2) . . . . ?
C37 C38 C39 C40 -1.1(5) . . . . ?
C37 C38 C39 Cl8 -178.6(2) . . . . ?
C38 C39 C40 O4 -177.6(3) . . . . ?
Cl8 C39 C40 O4 -0.1(4) . . . . ?
C38 C39 C40 C35 1.2(5) . . . . ?
Cl8 C39 C40 C35 178.6(2) . . . . ?
C36 C35 C40 O4 179.1(3) . . . . ?
C34 C35 C40 O4 2.1(5) . . . . ?
C36 C35 C40 C39 0.4(4) . . . . ?
C34 C35 C40 C39 -176.6(3) . . . . ?
C6 C7 N1 C8 173.9(3) . . . . ?
C6 C7 N1 Zr1 2.8(5) . . . . ?
C9 C8 N1 C7 -6.8(4) . . . . ?
C13 C8 N1 C7 -130.2(3) . . . . ?
C9 C8 N1 Zr1 165.1(2) . . . . ?
C13 C8 N1 Zr1 41.6(3) . . . . ?
C15 C14 N2 C13 179.4(3) . . . . ?
C15 C14 N2 Zr1 12.6(5) . . . . ?
C12 C13 N2 C14 2.0(4) . . . . ?
C8 C13 N2 C14 -122.2(3) . . . . ?
C12 C13 N2 Zr1 169.8(2) . . . . ?
C8 C13 N2 Zr1 45.6(3) . . . . ?
C26 C27 N3 C28 177.0(3) . . . . ?
C26 C27 N3 Zr1 1.9(5) . . . . ?
C29 C28 N3 C27 -6.4(4) . . . . ?
C33 C28 N3 C27 -128.9(3) . . . . ?
C29 C28 N3 Zr1 169.3(2) . . . . ?
C33 C28 N3 Zr1 46.8(3) . . . . ?
C35 C34 N4 C33 175.0(3) . . . . ?
C35 C34 N4 Zr1 3.4(5) . . . . ?
C32 C33 N4 C34 -4.8(4) . . . . ?
C28 C33 N4 C34 -128.6(3) . . . . ?
C32 C33 N4 Zr1 167.7(2) . . . . ?
C28 C33 N4 Zr1 43.9(3) . . . . ?
C6 C1 O1 Zr1 -46.9(4) . . . . ?
C2 C1 O1 Zr1 132.4(3) . . . . ?
C26 C21 O2 Zr1 -41.2(4) . . . . ?
C22 C21 O2 Zr1 139.4(3) . . . . ?
C19 C20 O3 Zr1 136.4(3) . . . . ?
C15 C20 O3 Zr1 -45.1(4) . . . . ?
C39 C40 O4 Zr1 133.1(3) . . . . ?
C35 C40 O4 Zr1 -45.6(4) . . . . ?
C1 O1 Zr1 O4 -24.5(3) . . . . ?
C1 O1 Zr1 O3 -126.5(3) . . . . ?
C1 O1 Zr1 O2 119.4(3) . . . . ?
C1 O1 Zr1 N3 -169.5(3) . . . . ?
C1 O1 Zr1 N2 49.3(3) . . . . ?
C1 O1 Zr1 N1 47.7(3) . . . . ?
C1 O1 Zr1 N4 -97.0(3) . . . . ?
C40 O4 Zr1 O1 -24.0(3) . . . . ?
C40 O4 Zr1 O3 118.4(3) . . . . ?
C40 O4 Zr1 O2 -134.0(3) . . . . ?
C40 O4 Zr1 N3 46.8(4) . . . . ?
C40 O4 Zr1 N2 -168.8(3) . . . . ?
C40 O4 Zr1 N1 -97.3(3) . . . . ?
C40 O4 Zr1 N4 46.4(3) . . . . ?
C20 O3 Zr1 O1 -130.0(3) . . . . ?
C20 O3 Zr1 O4 128.4(3) . . . . ?
C20 O3 Zr1 O2 -15.1(3) . . . . ?
C20 O3 Zr1 N3 -86.9(3) . . . . ?
C20 O3 Zr1 N2 52.6(3) . . . . ?
C20 O3 Zr1 N1 59.5(3) . . . . ?
C20 O3 Zr1 N4 -159.2(3) . . . . ?
C21 O2 Zr1 O1 117.1(3) . . . . ?
C21 O2 Zr1 O4 -134.8(3) . . . . ?
C21 O2 Zr1 O3 -28.1(3) . . . . ?
C21 O2 Zr1 N3 44.7(3) . . . . ?
C21 O2 Zr1 N2 -98.7(3) . . . . ?
C21 O2 Zr1 N1 -171.3(3) . . . . ?
C21 O2 Zr1 N4 44.4(3) . . . . ?
C27 N3 Zr1 O1 -127.1(3) . . . . ?
C28 N3 Zr1 O1 57.8(2) . . . . ?
C27 N3 Zr1 O4 156.6(2) . . . . ?
C28 N3 Zr1 O4 -18.6(3) . . . . ?
C27 N3 Zr1 O3 78.9(3) . . . . ?
C28 N3 Zr1 O3 -96.3(2) . . . . ?
C27 N3 Zr1 O2 -22.9(3) . . . . ?
C28 N3 Zr1 O2 161.9(2) . . . . ?
C27 N3 Zr1 N2 24.4(3) . . . . ?
C28 N3 Zr1 N2 -150.77(18) . . . . ?
C27 N3 Zr1 N1 -74.0(3) . . . . ?
C28 N3 Zr1 N1 110.9(2) . . . . ?
C27 N3 Zr1 N4 157.0(3) . . . . ?
C28 N3 Zr1 N4 -18.20(19) . . . . ?
C14 N2 Zr1 O1 147.7(2) . . . . ?
C13 N2 Zr1 O1 -19.6(3) . . . . ?
C14 N2 Zr1 O4 -133.5(3) . . . . ?
C13 N2 Zr1 O4 59.2(2) . . . . ?
C14 N2 Zr1 O3 -35.0(2) . . . . ?
C13 N2 Zr1 O3 157.7(2) . . . . ?
C14 N2 Zr1 O2 68.4(2) . . . . ?
C13 N2 Zr1 O2 -98.9(2) . . . . ?
C14 N2 Zr1 N3 19.9(3) . . . . ?
C13 N2 Zr1 N3 -147.36(19) . . . . ?
C14 N2 Zr1 N1 149.4(3) . . . . ?
C13 N2 Zr1 N1 -17.94(19) . . . . ?
C14 N2 Zr1 N4 -81.2(3) . . . . ?
C13 N2 Zr1 N4 111.5(2) . . . . ?
C7 N1 Zr1 O1 -23.9(3) . . . . ?
C8 N1 Zr1 O1 164.9(2) . . . . ?
C7 N1 Zr1 O4 74.4(3) . . . . ?
C8 N1 Zr1 O4 -96.9(2) . . . . ?
C7 N1 Zr1 O3 150.0(2) . . . . ?
C8 N1 Zr1 O3 -21.2(3) . . . . ?
C7 N1 Zr1 O2 -128.1(3) . . . . ?
C8 N1 Zr1 O2 60.6(2) . . . . ?
C7 N1 Zr1 N3 -77.3(3) . . . . ?
C8 N1 Zr1 N3 111.4(2) . . . . ?
C7 N1 Zr1 N2 157.1(3) . . . . ?
C8 N1 Zr1 N2 -14.15(19) . . . . ?
C7 N1 Zr1 N4 24.1(3) . . . . ?
C8 N1 Zr1 N4 -147.13(19) . . . . ?
C34 N4 Zr1 O1 75.2(3) . . . . ?
C33 N4 Zr1 O1 -96.7(2) . . . . ?
C34 N4 Zr1 O4 -23.8(2) . . . . ?
C33 N4 Zr1 O4 164.4(2) . . . . ?
C34 N4 Zr1 O3 -123.4(3) . . . . ?
C33 N4 Zr1 O3 64.79(19) . . . . ?
C34 N4 Zr1 O2 156.7(2) . . . . ?
C33 N4 Zr1 O2 -15.1(3) . . . . ?
C34 N4 Zr1 N3 156.4(3) . . . . ?
C33 N4 Zr1 N3 -15.40(18) . . . . ?
C34 N4 Zr1 N2 -77.2(3) . . . . ?
C33 N4 Zr1 N2 111.0(2) . . . . ?
C34 N4 Zr1 N1 26.2(3) . . . . ?
C33 N4 Zr1 N1 -145.61(18) . . . . ?



_diffrn_measured_fraction_theta_max 0.967

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         1.432

_refine_diff_density_min         -1.485

_refine_diff_density_rms         0.163
