#------------------------------------------------------------------------------
#$Date: 2020-09-06 12:34:29 +0300 (Sun, 06 Sep 2020) $
#$Revision: 256071 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/50/7705038.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7705038
loop_
_publ_author_name
'Do, Thomas H.'
'Brown, Seth N.'
_publ_section_title
;
 Synthesis, dynamics and redox properties of eight-coordinate zirconium
 catecholate complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11648
_journal_page_last               11656
_journal_paper_doi               10.1039/d0dt02487b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C90 H108 N4 O10 Zr, 3(C H Cl3), C6 H14'
_chemical_formula_sum            'C99 H125 Cl9 N4 O10 Zr'
_chemical_formula_weight         1941.37
_chemical_name_common            '(XbicH2)2Zr . 3 CHCl3 . C6H14'
_chemical_name_systematic
'Bis(9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butylcatecholatoaldiminium))zirconium(IV) tri-chloroform mono-hexane solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2020-07-12 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.9561(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.0034(17)
_cell_length_b                   15.2378(7)
_cell_length_c                   24.6829(12)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.216
_cell_measurement_theta_min      2.245
_cell_volume                     9477.3(8)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            99143
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.333
_diffrn_reflns_theta_min         1.562
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_recrystallization_method
'Crystals deposited from solvent layering of CHCl3 and hexanes.'
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.255
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.7096
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         12983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0519P)²+21.2066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11050
_reflns_number_total             12983
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02487b2.cif
_cod_data_source_block           zrxbic_sq
_cod_depositor_comments
'Adding full bibliography for 7705037--7705038.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7705038
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.918
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
ZR Zr 0.500000 0.09713(2) 0.250000 0.01031(6) Uani 1 2 d S T P . .
O1 O 0.46492(5) -0.00784(8) 0.16990(7) 0.0165(2) Uani 1 1 d . . . . .
H1 H 0.3901(10) 0.0634(17) 0.2450(14) 0.027(6) Uiso 1 1 d . . . . .
O2 O 0.42890(5) 0.04440(8) 0.22443(7) 0.0146(2) Uani 1 1 d . . . . .
H2 H 0.3917(10) 0.2577(17) 0.1871(14) 0.027(6) Uiso 1 1 d . . . . .
O3 O 0.49653(5) 0.15191(8) 0.16663(7) 0.0152(2) Uani 1 1 d . . . . .
O4 O 0.43750(5) 0.20121(8) 0.18605(7) 0.0148(2) Uani 1 1 d . . . . .
O5 O 0.34516(5) 0.20760(8) 0.22944(7) 0.0166(2) Uani 1 1 d . . . . .
N1 N 0.36744(6) 0.03540(10) 0.24413(8) 0.0161(3) Uani 1 1 d . . . . .
N2 N 0.36903(6) 0.30033(10) 0.16220(8) 0.0166(3) Uani 1 1 d . . . . .
C11 C 0.43405(6) -0.06479(11) 0.16480(9) 0.0150(3) Uani 1 1 d . . . . .
C12 C 0.41332(6) -0.03312(11) 0.19457(9) 0.0136(3) Uani 1 1 d . . . . .
C13 C 0.37668(6) -0.08343(11) 0.18977(9) 0.0157(3) Uani 1 1 d . . . . .
C14 C 0.36344(7) -0.17106(12) 0.15865(9) 0.0182(3) Uani 1 1 d . . . . .
C15 C 0.38533(7) -0.19785(12) 0.13248(10) 0.0200(3) Uani 1 1 d . . . . .
H15 H 0.376871 -0.255388 0.112117 0.024 Uiso 1 1 calc R U . . .
C16 C 0.41975(7) -0.14724(12) 0.13296(9) 0.0172(3) Uani 1 1 d . . . . .
C17 C 0.44032(8) -0.18363(13) 0.09935(10) 0.0227(4) Uani 1 1 d . . . . .
C171 C 0.42039(12) -0.27695(16) 0.06848(16) 0.0424(6) Uani 1 1 d . . . . .
H17A H 0.431782 -0.316007 0.109011 0.064 Uiso 1 1 calc R U . . .
H17B H 0.381556 -0.276735 0.028158 0.064 Uiso 1 1 calc R U . . .
H17C H 0.435110 -0.297759 0.048527 0.064 Uiso 1 1 calc R U . . .
C172 C 0.42216(10) -0.12427(16) 0.03543(13) 0.0355(5) Uani 1 1 d . . . . .
H17D H 0.383294 -0.122054 -0.003489 0.053 Uiso 1 1 calc R U . . .
H17E H 0.436275 -0.065027 0.054900 0.053 Uiso 1 1 calc R U . . .
H17F H 0.435216 -0.147534 0.013755 0.053 Uiso 1 1 calc R U . . .
C173 C 0.50075(9) -0.18729(18) 0.16004(12) 0.0371(5) Uani 1 1 d . . . . .
H17G H 0.512305 -0.225527 0.201083 0.056 Uiso 1 1 calc R U . . .
H17H H 0.513867 -0.210603 0.138463 0.056 Uiso 1 1 calc R U . . .
H17I H 0.514927 -0.128096 0.179607 0.056 Uiso 1 1 calc R U . . .
C18 C 0.32806(8) -0.23348(13) 0.15670(11) 0.0233(4) Uani 1 1 d . . . . .
C181 C 0.35321(8) -0.25299(13) 0.23717(11) 0.0248(4) Uani 1 1 d . . . . .
H18A H 0.357626 -0.198022 0.261630 0.037 Uiso 1 1 calc R U . . .
H18B H 0.330034 -0.292615 0.234820 0.037 Uiso 1 1 calc R U . . .
H18C H 0.387924 -0.280737 0.266164 0.037 Uiso 1 1 calc R U . . .
C182 C 0.27138(8) -0.19722(17) 0.10729(12) 0.0355(5) Uani 1 1 d . . . . .
H18D H 0.272743 -0.140008 0.126719 0.053 Uiso 1 1 calc R U . . .
H18E H 0.255096 -0.190544 0.055444 0.053 Uiso 1 1 calc R U . . .
H18F H 0.250216 -0.238019 0.108258 0.053 Uiso 1 1 calc R U . . .
C183 C 0.32267(10) -0.32242(15) 0.12299(13) 0.0372(5) Uani 1 1 d . . . . .
H18G H 0.299965 -0.361059 0.122330 0.056 Uiso 1 1 calc R U . . .
H18H H 0.306752 -0.313969 0.071473 0.056 Uiso 1 1 calc R U . . .
H18I H 0.357827 -0.349128 0.153589 0.056 Uiso 1 1 calc R U . . .
C19 C 0.35593(7) -0.04440(12) 0.21587(10) 0.0170(3) Uani 1 1 d . . . . .
H19 H 0.3306(9) -0.0724(16) 0.2123(13) 0.022(6) Uiso 1 1 d . . . . .
C21 C 0.45903(6) 0.20792(11) 0.11667(9) 0.0142(3) Uani 1 1 d . . . . .
C22 C 0.42689(6) 0.23717(11) 0.12917(9) 0.0137(3) Uani 1 1 d . . . . .
C23 C 0.38602(7) 0.30082(11) 0.08248(9) 0.0156(3) Uani 1 1 d . . . . .
C24 C 0.37516(7) 0.33401(12) 0.01779(9) 0.0170(3) Uani 1 1 d . . . . .
C25 C 0.40558(7) 0.30080(12) 0.00667(10) 0.0193(3) Uani 1 1 d . . . . .
H25 H 0.398632 0.321844 -0.035699 0.023 Uiso 1 1 calc R U . . .
C26 C 0.44678(7) 0.23741(12) 0.05302(10) 0.0183(3) Uani 1 1 d . . . . .
C27 C 0.47633(8) 0.20102(16) 0.03296(11) 0.0287(4) Uani 1 1 d . . . . .
C271 C 0.53506(9) 0.2246(2) 0.09514(14) 0.0430(6) Uani 1 1 d . . . . .
H27A H 0.554096 0.201290 0.082385 0.064 Uiso 1 1 calc R U . . .
H27B H 0.538971 0.288543 0.100114 0.064 Uiso 1 1 calc R U . . .
H27C H 0.549814 0.199032 0.142843 0.064 Uiso 1 1 calc R U . . .
C272 C 0.45481(11) 0.2367(2) -0.04192(14) 0.0528(8) Uani 1 1 d . . . . .
H27D H 0.417087 0.221991 -0.082327 0.079 Uiso 1 1 calc R U . . .
H27E H 0.459127 0.300619 -0.038581 0.079 Uiso 1 1 calc R U . . .
H27F H 0.474449 0.210385 -0.052755 0.079 Uiso 1 1 calc R U . . .
C273 C 0.47008(12) 0.10087(18) 0.02575(15) 0.0435(6) Uani 1 1 d . . . . .
H27G H 0.432370 0.085826 -0.014172 0.065 Uiso 1 1 calc R U . . .
H27H H 0.489175 0.076938 0.013271 0.065 Uiso 1 1 calc R U . . .
H27I H 0.484715 0.075893 0.073554 0.065 Uiso 1 1 calc R U . . .
C28 C 0.33101(7) 0.40057(13) -0.03754(11) 0.0225(4) Uani 1 1 d . . . . .
C281 C 0.27675(8) 0.36230(16) -0.07439(12) 0.0303(4) Uani 1 1 d . . . . .
H28A H 0.248798 0.405224 -0.109627 0.045 Uiso 1 1 calc R U . . .
H28B H 0.270002 0.308441 -0.101613 0.045 Uiso 1 1 calc R U . . .
H28C H 0.276967 0.348888 -0.035346 0.045 Uiso 1 1 calc R U . . .
C282 C 0.34158(10) 0.48958(14) 0.00038(13) 0.0345(5) Uani 1 1 d . . . . .
H28D H 0.312612 0.530226 -0.036633 0.052 Uiso 1 1 calc R U . . .
H28E H 0.343679 0.481339 0.041769 0.052 Uiso 1 1 calc R U . . .
H28F H 0.375166 0.513808 0.020145 0.052 Uiso 1 1 calc R U . . .
C283 C 0.32632(9) 0.42049(16) -0.10319(12) 0.0310(5) Uani 1 1 d . . . . .
H28G H 0.297795 0.463129 -0.137220 0.046 Uiso 1 1 calc R U . . .
H28H H 0.359924 0.444786 -0.083322 0.046 Uiso 1 1 calc R U . . .
H28I H 0.318258 0.366211 -0.130768 0.046 Uiso 1 1 calc R U . . .
C29 C 0.36023(7) 0.33008(11) 0.10395(10) 0.0171(3) Uani 1 1 d . . . . .
H29 H 0.3356(9) 0.3775(15) 0.0791(13) 0.022(6) Uiso 1 1 d . . . . .
C31 C 0.34732(7) 0.06934(12) 0.27319(9) 0.0170(3) Uani 1 1 d . . . . .
C32 C 0.33546(6) 0.15858(12) 0.26575(9) 0.0164(3) Uani 1 1 d . . . . .
C33 C 0.31464(7) 0.19318(13) 0.29263(10) 0.0196(3) Uani 1 1 d . . . . .
C34 C 0.30473(8) 0.13569(14) 0.32566(11) 0.0243(4) Uani 1 1 d . . . . .
H34 H 0.289179 0.157858 0.342639 0.029 Uiso 1 1 calc R U . . .
C35 C 0.31682(8) 0.04776(14) 0.33436(11) 0.0259(4) Uani 1 1 d . . . . .
H35 H 0.310075 0.010096 0.357605 0.031 Uiso 1 1 calc R U . . .
C36 C 0.33888(8) 0.01464(13) 0.30898(10) 0.0223(4) Uani 1 1 d . . . . .
H36 H 0.348253 -0.045642 0.316074 0.027 Uiso 1 1 calc R U . . .
C41 C 0.34989(7) 0.34405(12) 0.18984(10) 0.0180(3) Uani 1 1 d . . . . .
C42 C 0.34440(9) 0.43450(13) 0.18451(12) 0.0259(4) Uani 1 1 d . . . . .
H42 H 0.353361 0.467351 0.161924 0.031 Uiso 1 1 calc R U . . .
C43 C 0.32590(9) 0.47700(14) 0.21200(13) 0.0302(4) Uani 1 1 d . . . . .
H43 H 0.321862 0.538983 0.207848 0.036 Uiso 1 1 calc R U . . .
C44 C 0.31334(8) 0.42991(14) 0.24531(12) 0.0268(4) Uani 1 1 d . . . . .
H44 H 0.300717 0.459969 0.264046 0.032 Uiso 1 1 calc R U . . .
C45 C 0.31873(7) 0.33912(12) 0.25217(10) 0.0197(3) Uani 1 1 d . . . . .
C46 C 0.33754(7) 0.29686(11) 0.22484(9) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.30355(8) 0.28991(13) 0.28827(11) 0.0229(4) Uani 1 1 d . . . . .
C2 C 0.33686(11) 0.32448(16) 0.36884(13) 0.0358(5) Uani 1 1 d . . . . .
H2A H 0.329991 0.387268 0.367047 0.054 Uiso 1 1 calc R U . . .
H2B H 0.374624 0.315396 0.398376 0.054 Uiso 1 1 calc R U . . .
H2C H 0.327142 0.292755 0.392365 0.054 Uiso 1 1 calc R U . . .
C3 C 0.24424(9) 0.30438(17) 0.24153(14) 0.0361(5) Uani 1 1 d . . . . .
H3A H 0.223215 0.283032 0.190140 0.054 Uiso 1 1 calc R U . . .
H3B H 0.237494 0.367135 0.240187 0.054 Uiso 1 1 calc R U . . .
H3C H 0.234205 0.272193 0.264464 0.054 Uiso 1 1 calc R U . . .
C4 C 0.16971(8) 0.44352(13) -0.01661(11) 0.0245(4) Uani 1 1 d . . . . .
H4 H 0.130783 0.455108 -0.058202 0.029 Uiso 1 1 calc R U . . .
CL1 Cl 0.18065(2) 0.37831(4) 0.05136(3) 0.03401(12) Uani 1 1 d . . . . .
CL2 Cl 0.20297(2) 0.54441(4) 0.02228(3) 0.04053(14) Uani 1 1 d . . . . .
CL3 Cl 0.19113(2) 0.38894(4) -0.05386(3) 0.04063(14) Uani 1 1 d . . . . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 ZR O3 134.19(7) . 2_655 ?
O3 ZR O1 142.12(4) . 2_655 ?
O3 ZR O1 77.93(5) 2_655 2_655 ?
O3 ZR O1 77.93(5) . . ?
O3 ZR O1 142.12(4) 2_655 . ?
O1 ZR O1 83.62(7) 2_655 . ?
O3 ZR O4 77.14(4) . 2_655 ?
O3 ZR O4 70.76(4) 2_655 2_655 ?
O1 ZR O4 102.97(5) 2_655 2_655 ?
O1 ZR O4 146.40(4) . 2_655 ?
O3 ZR O4 70.77(4) . . ?
O3 ZR O4 77.13(4) 2_655 . ?
O1 ZR O4 146.39(4) 2_655 . ?
O1 ZR O4 102.97(5) . . ?
O4 ZR O4 89.64(6) 2_655 . ?
O3 ZR O2 123.72(4) . . ?
O3 ZR O2 73.91(4) 2_655 . ?
O1 ZR O2 78.83(4) 2_655 . ?
O1 ZR O2 70.19(4) . . ?
O4 ZR O2 143.28(4) 2_655 . ?
O4 ZR O2 72.86(4) . . ?
O3 ZR O2 73.91(4) . 2_655 ?
O3 ZR O2 123.72(4) 2_655 2_655 ?
O1 ZR O2 70.19(4) 2_655 2_655 ?
O1 ZR O2 78.83(4) . 2_655 ?
O4 ZR O2 72.86(4) 2_655 2_655 ?
O4 ZR O2 143.28(4) . 2_655 ?
O2 ZR O2 138.13(6) . 2_655 ?
C11 O1 ZR 118.96(10) . . ?
C12 O2 ZR 115.61(10) . . ?
C21 O3 ZR 120.53(10) . . ?
C22 O4 ZR 117.91(10) . . ?
C46 O5 C32 117.93(13) . . ?
C19 N1 C31 122.11(15) . . ?
C19 N1 H1 113.4(16) . . ?
C31 N1 H1 124.4(16) . . ?
C29 N2 C41 122.18(15) . . ?
C29 N2 H2 115.8(16) . . ?
C41 N2 H2 121.3(16) . . ?
O1 C11 C16 127.01(15) . . ?
O1 C11 C12 113.75(15) . . ?
C16 C11 C12 119.22(15) . . ?
O2 C12 C13 122.43(15) . . ?
O2 C12 C11 115.93(14) . . ?
C13 C12 C11 121.62(15) . . ?
C19 C13 C12 117.32(15) . . ?
C19 C13 C14 124.13(15) . . ?
C12 C13 C14 118.55(15) . . ?
C15 C14 C13 116.73(15) . . ?
C15 C14 C18 120.40(16) . . ?
C13 C14 C18 122.84(16) . . ?
C14 C15 C16 125.78(16) . . ?
C14 C15 H15 117.1 . . ?
C16 C15 H15 117.1 . . ?
C11 C16 C15 117.96(15) . . ?
C11 C16 C17 121.18(15) . . ?
C15 C16 C17 120.86(16) . . ?
C172 C17 C173 109.67(18) . . ?
C172 C17 C16 109.34(16) . . ?
C173 C17 C16 109.55(15) . . ?
C172 C17 C171 108.49(18) . . ?
C173 C17 C171 107.26(19) . . ?
C16 C17 C171 112.49(16) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C183 C18 C14 110.96(16) . . ?
C183 C18 C182 106.38(18) . . ?
C14 C18 C182 111.74(16) . . ?
C183 C18 C181 105.90(17) . . ?
C14 C18 C181 110.61(15) . . ?
C182 C18 C181 111.03(17) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
N1 C19 C13 124.87(15) . . ?
N1 C19 H19 113.2(14) . . ?
C13 C19 H19 121.8(14) . . ?
O3 C21 C26 126.63(15) . . ?
O3 C21 C22 115.05(14) . . ?
C26 C21 C22 118.26(15) . . ?
O4 C22 C23 122.37(14) . . ?
O4 C22 C21 115.14(14) . . ?
C23 C22 C21 122.48(14) . . ?
C29 C23 C22 117.40(15) . . ?
C29 C23 C24 124.08(15) . . ?
C22 C23 C24 118.47(14) . . ?
C25 C24 C23 116.48(15) . . ?
C25 C24 C28 120.63(15) . . ?
C23 C24 C28 122.87(15) . . ?
C24 C25 C26 125.76(16) . . ?
C24 C25 H25 117.1 . . ?
C26 C25 H25 117.1 . . ?
C21 C26 C25 118.33(15) . . ?
C21 C26 C27 120.24(16) . . ?
C25 C26 C27 121.42(15) . . ?
C271 C27 C26 109.33(18) . . ?
C271 C27 C272 108.7(2) . . ?
C26 C27 C272 112.69(16) . . ?
C271 C27 C273 109.5(2) . . ?
C26 C27 C273 108.95(17) . . ?
C272 C27 C273 107.6(2) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C24 C28 C282 111.88(16) . . ?
C24 C28 C283 111.88(15) . . ?
C282 C28 C283 105.73(17) . . ?
C24 C28 C281 110.02(16) . . ?
C282 C28 C281 111.69(17) . . ?
C283 C28 C281 105.41(16) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
N2 C29 C23 125.25(16) . . ?
N2 C29 H29 112.6(14) . . ?
C23 C29 H29 122.0(14) . . ?
C36 C31 C32 119.57(16) . . ?
C36 C31 N1 120.47(17) . . ?
C32 C31 N1 119.96(15) . . ?
O5 C32 C33 123.65(16) . . ?
O5 C32 C31 115.36(14) . . ?
C33 C32 C31 120.99(16) . . ?
C32 C33 C34 117.88(17) . . ?
C32 C33 C1 122.15(16) . . ?
C34 C33 C1 119.96(16) . . ?
C35 C34 C33 121.89(17) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 119.49(17) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 120.11(18) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C41 C46 119.12(16) . . ?
C42 C41 N2 120.31(16) . . ?
C46 C41 N2 120.54(16) . . ?
C43 C42 C41 120.07(18) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.21(19) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 121.32(17) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C46 C45 C44 118.24(17) . . ?
C46 C45 C1 122.38(17) . . ?
C44 C45 C1 119.38(16) . . ?
O5 C46 C45 123.35(15) . . ?
O5 C46 C41 115.63(14) . . ?
C45 C46 C41 121.02(16) . . ?
C33 C1 C45 110.34(14) . . ?
C33 C1 C3 109.88(17) . . ?
C45 C1 C3 109.25(16) . . ?
C33 C1 C2 108.37(16) . . ?
C45 C1 C2 109.27(17) . . ?
C3 C1 C2 109.72(17) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
CL3 C4 CL1 110.25(11) . . ?
CL3 C4 CL2 109.89(11) . . ?
CL1 C4 CL2 110.62(11) . . ?
CL3 C4 H4 108.7 . . ?
CL1 C4 H4 108.7 . . ?
CL2 C4 H4 108.7 . . ?
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
ZR O3 2.1446(11) . ?
ZR O3 2.1446(11) 2_655 ?
ZR O1 2.1459(12) 2_655 ?
ZR O1 2.1459(12) . ?
ZR O4 2.2358(12) 2_655 ?
ZR O4 2.2359(11) . ?
ZR O2 2.2489(11) . ?
ZR O2 2.2490(11) 2_655 ?
O1 C11 1.322(2) . ?
O2 C12 1.295(2) . ?
O3 C21 1.313(2) . ?
O4 C22 1.2983(19) . ?
O5 C46 1.375(2) . ?
O5 C32 1.3783(19) . ?
N1 C19 1.318(2) . ?
N1 C31 1.407(2) . ?
N1 H1 0.89(3) . ?
N2 C29 1.324(2) . ?
N2 C41 1.412(2) . ?
N2 H2 0.87(3) . ?
C11 C16 1.379(2) . ?
C11 C12 1.428(2) . ?
C12 C13 1.427(2) . ?
C13 C19 1.395(2) . ?
C13 C14 1.447(2) . ?
C14 C15 1.363(3) . ?
C14 C18 1.536(2) . ?
C15 C16 1.423(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.531(2) . ?
C17 C172 1.523(3) . ?
C17 C173 1.524(3) . ?
C17 C171 1.534(3) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C18 C183 1.532(3) . ?
C18 C182 1.540(3) . ?
C18 C181 1.543(3) . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C19 H19 0.93(2) . ?
C21 C26 1.385(2) . ?
C21 C22 1.429(2) . ?
C22 C23 1.424(2) . ?
C23 C29 1.400(2) . ?
C23 C24 1.451(2) . ?
C24 C25 1.368(2) . ?
C24 C28 1.534(2) . ?
C25 C26 1.425(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.527(2) . ?
C27 C271 1.527(3) . ?
C27 C272 1.532(3) . ?
C27 C273 1.534(4) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C28 C282 1.540(3) . ?
C28 C283 1.541(3) . ?
C28 C281 1.542(3) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C29 H29 0.95(2) . ?
C31 C36 1.387(2) . ?
C31 C32 1.396(3) . ?
C32 C33 1.386(2) . ?
C33 C34 1.395(3) . ?
C33 C1 1.509(3) . ?
C34 C35 1.376(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.385(3) . ?
C41 C46 1.403(2) . ?
C42 C43 1.382(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.373(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.386(2) . ?
C45 C1 1.515(3) . ?
C1 C3 1.538(3) . ?
C1 C2 1.540(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 CL3 1.748(2) . ?
C4 CL1 1.748(2) . ?
C4 CL2 1.757(2) . ?
C4 H4 1.0000 . ?
