#------------------------------------------------------------------------------
#$Date: 2023-08-23 01:58:00 +0300 (Wed, 23 Aug 2023) $
#$Revision: 285840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/37/7713768.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_7713768
loop_
_publ_author_name
'Hosoya, Hiromu'
'Akiyama, Takuya'
'Mashima, Kazushi'
'Tsurugi, Hayato'
_publ_section_title
;
 Bis(neopentylglycolato)diboron (B2nep2) as a Bidentate Ligand and a
 Reducing Agent for Early Transition Metal Chlorides Giving MCl4(B2nep2)
 Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01828H
_journal_year                    2023
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C12 H24 B2 Cl4 O4 Zr'
_chemical_formula_sum            'C12 H24 B2 Cl4 O4 Zr'
_chemical_formula_weight         486.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-06-10 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.990(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.112(3)
_cell_length_b                   10.1415(18)
_cell_length_c                   15.181(3)
_cell_measurement_reflns_used    3434
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     2041.8(7)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39364
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         3.072
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.33
_refine_diff_density_min         -1.03
_refine_ls_abs_structure_details
;
 Flack x determined using 2798 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     431
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0599P)²+4.7744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                7367
_reflns_number_total             9287
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d3dt01828h1.cif
_cod_data_source_block           hsy11008-Zr-1
_cod_database_code               7713768
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-Z
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
ZR1 Zr 0.64727(6) 0.33169(8) 0.21311(5) 0.01784(19) Uani 1 1 d . . . . .
ZR2 Zr 0.12632(6) 0.32644(8) 0.21469(5) 0.01868(19) Uani 1 1 d . . . . .
CL1 Cl 0.76743(19) 0.2456(2) 0.14912(16) 0.0284(5) Uani 1 1 d . . . . .
CL2 Cl 0.58655(19) 0.1239(2) 0.24327(17) 0.0283(5) Uani 1 1 d . . . . .
CL3 Cl 0.51738(19) 0.3711(2) 0.06932(15) 0.0309(6) Uani 1 1 d . . . . .
CL4 Cl 0.56869(18) 0.4592(2) 0.30745(15) 0.0238(5) Uani 1 1 d . . . . .
CL5 Cl 0.2126(2) 0.1990(3) 0.13248(18) 0.0364(6) Uani 1 1 d . . . . .
CL6 Cl 0.0526(2) 0.1416(2) 0.26155(17) 0.0300(5) Uani 1 1 d . . . . .
CL7 Cl -0.0154(2) 0.3869(2) 0.08546(16) 0.0324(6) Uani 1 1 d . . . . .
CL8 Cl 0.08446(18) 0.4818(2) 0.32047(16) 0.0246(5) Uani 1 1 d . . . . .
O1 O 0.7837(4) 0.3338(7) 0.3530(3) 0.0181(11) Uani 1 1 d . . . . .
O2 O 0.8987(5) 0.4623(6) 0.4626(4) 0.0199(13) Uani 1 1 d . . . . .
O3 O 0.7225(5) 0.5343(5) 0.2054(4) 0.0190(13) Uani 1 1 d . . . . .
O4 O 0.8297(5) 0.6964(6) 0.2866(4) 0.0225(13) Uani 1 1 d . . . . .
O5 O 0.2759(4) 0.3188(7) 0.3427(4) 0.0196(12) Uani 1 1 d . . . . .
O6 O 0.3915(5) 0.4471(6) 0.4534(4) 0.0238(14) Uani 1 1 d . . . . .
O7 O 0.2175(5) 0.5060(6) 0.1935(4) 0.0186(13) Uani 1 1 d . . . . .
O8 O 0.3141(5) 0.6808(6) 0.2697(4) 0.0249(14) Uani 1 1 d . . . . .
C1 C 0.8223(7) 0.2481(8) 0.4395(6) 0.0187(18) Uani 1 1 d . . . . .
C2 C 0.7395(8) 0.2416(9) 0.4817(7) 0.027(2) Uani 1 1 d . . . . .
H2A H 0.679970 0.198673 0.437438 0.033 Uiso 1 1 calc R U . . .
H2B H 0.721784 0.331106 0.494901 0.033 Uiso 1 1 calc R U . . .
H2C H 0.763056 0.190821 0.540111 0.033 Uiso 1 1 calc R U . . .
C3 C 0.8454(7) 0.1112(8) 0.4103(6) 0.0220(19) Uani 1 1 d . . . . .
H3A H 0.889289 0.119296 0.372570 0.026 Uiso 1 1 calc R U . . .
H3B H 0.782355 0.067723 0.373220 0.026 Uiso 1 1 calc R U . . .
H3C H 0.879463 0.058545 0.466359 0.026 Uiso 1 1 calc R U . . .
C4 C 0.9181(6) 0.3259(9) 0.5006(5) 0.0178(15) Uani 1 1 d . . . . .
C5 C 0.9315(7) 0.3355(10) 0.6043(5) 0.0242(18) Uani 1 1 d . . . . .
H5A H 0.872307 0.378339 0.611498 0.029 Uiso 1 1 calc R U . . .
H5B H 0.991889 0.387565 0.636771 0.029 Uiso 1 1 calc R U . . .
H5C H 0.938961 0.246807 0.631482 0.029 Uiso 1 1 calc R U . . .
C6 C 1.0149(7) 0.2812(9) 0.4874(7) 0.025(2) Uani 1 1 d . . . . .
H6A H 1.070042 0.340486 0.521706 0.030 Uiso 1 1 calc R U . . .
H6B H 1.006386 0.283135 0.420530 0.030 Uiso 1 1 calc R U . . .
H6C H 1.030986 0.191209 0.511291 0.030 Uiso 1 1 calc R U . . .
C7 C 0.6962(7) 0.6570(8) 0.1429(6) 0.0212(19) Uani 1 1 d . . . . .
C8 C 0.6033(8) 0.7154(9) 0.1566(7) 0.029(2) Uani 1 1 d . . . . .
H8A H 0.548080 0.651268 0.136791 0.035 Uiso 1 1 calc R U . . .
H8B H 0.583423 0.795714 0.118901 0.035 Uiso 1 1 calc R U . . .
H8C H 0.618447 0.736830 0.222925 0.035 Uiso 1 1 calc R U . . .
C9 C 0.6777(8) 0.6163(10) 0.0428(6) 0.027(2) Uani 1 1 d . . . . .
H9A H 0.674693 0.694950 0.004459 0.032 Uiso 1 1 calc R U . . .
H9B H 0.613665 0.568410 0.018600 0.032 Uiso 1 1 calc R U . . .
H9C H 0.732722 0.559098 0.040409 0.032 Uiso 1 1 calc R U . . .
C10 C 0.7933(8) 0.7387(9) 0.1876(6) 0.021(2) Uani 1 1 d . . . . .
C11 C 0.8782(7) 0.7087(10) 0.1503(6) 0.027(2) Uani 1 1 d . . . . .
H11A H 0.894553 0.614569 0.158125 0.033 Uiso 1 1 calc R U . . .
H11B H 0.937876 0.760504 0.185158 0.033 Uiso 1 1 calc R U . . .
H11C H 0.856851 0.731745 0.083690 0.033 Uiso 1 1 calc R U . . .
C12 C 0.7751(9) 0.8873(10) 0.1862(7) 0.030(2) Uani 1 1 d . . . . .
H12A H 0.839687 0.933111 0.213459 0.036 Uiso 1 1 calc R U . . .
H12B H 0.731710 0.907493 0.222990 0.036 Uiso 1 1 calc R U . . .
H12C H 0.742073 0.916721 0.121437 0.036 Uiso 1 1 calc R U . . .
C13 C 0.3434(8) 0.2238(9) 0.4140(7) 0.025(2) Uani 1 1 d . . . . .
C14 C 0.4200(8) 0.1746(10) 0.3720(7) 0.031(2) Uani 1 1 d . . . . .
H14A H 0.384919 0.132151 0.311640 0.038 Uiso 1 1 calc R U . . .
H14B H 0.464908 0.110743 0.414683 0.038 Uiso 1 1 calc R U . . .
H14C H 0.459686 0.249138 0.362583 0.038 Uiso 1 1 calc R U . . .
C15 C 0.2834(9) 0.1112(10) 0.4325(7) 0.036(3) Uani 1 1 d . . . . .
H15A H 0.261562 0.052895 0.377790 0.043 Uiso 1 1 calc R U . . .
H15B H 0.224192 0.145811 0.444617 0.043 Uiso 1 1 calc R U . . .
H15C H 0.325485 0.061504 0.487330 0.043 Uiso 1 1 calc R U . . .
C16 C 0.3887(7) 0.3181(10) 0.4982(6) 0.0225(18) Uani 1 1 d . . . . .
C17 C 0.4946(8) 0.2848(10) 0.5596(7) 0.032(2) Uani 1 1 d . . . . .
H17A H 0.516011 0.345140 0.613199 0.039 Uiso 1 1 calc R U . . .
H17B H 0.539939 0.293619 0.523381 0.039 Uiso 1 1 calc R U . . .
H17C H 0.496760 0.193904 0.582133 0.039 Uiso 1 1 calc R U . . .
C18 C 0.3204(8) 0.3393(12) 0.5560(6) 0.035(2) Uani 1 1 d . . . . .
H18A H 0.251722 0.358568 0.514103 0.041 Uiso 1 1 calc R U . . .
H18B H 0.345665 0.413578 0.598977 0.041 Uiso 1 1 calc R U . . .
H18C H 0.319835 0.259450 0.592210 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2291(7) 0.5968(9) 0.1185(6) 0.0212(19) Uani 1 1 d . . . . .
C20 C 0.3154(8) 0.5394(9) 0.0924(7) 0.027(2) Uani 1 1 d . . . . .
H20A H 0.296580 0.451462 0.065245 0.032 Uiso 1 1 calc R U . . .
H20B H 0.375619 0.532687 0.148681 0.032 Uiso 1 1 calc R U . . .
H20C H 0.329516 0.596858 0.046549 0.032 Uiso 1 1 calc R U . . .
C21 C 0.1335(8) 0.6004(10) 0.0346(7) 0.029(2) Uani 1 1 d . . . . .
H21A H 0.077416 0.629404 0.054129 0.035 Uiso 1 1 calc R U . . .
H21B H 0.119124 0.512040 0.007066 0.035 Uiso 1 1 calc R U . . .
H21C H 0.141634 0.662014 -0.012014 0.035 Uiso 1 1 calc R U . . .
C22 C 0.2559(7) 0.7266(8) 0.1742(6) 0.023(2) Uani 1 1 d . . . . .
C23 C 0.3231(8) 0.8179(11) 0.1423(7) 0.037(2) Uani 1 1 d . . . . .
H23A H 0.387184 0.773602 0.150025 0.044 Uiso 1 1 calc R U . . .
H23B H 0.336102 0.898517 0.180246 0.044 Uiso 1 1 calc R U . . .
H23C H 0.289541 0.840649 0.076209 0.044 Uiso 1 1 calc R U . . .
C24 C 0.1645(8) 0.7994(9) 0.1814(7) 0.030(2) Uani 1 1 d . . . . .
H24A H 0.187003 0.870250 0.227829 0.036 Uiso 1 1 calc R U . . .
H24B H 0.121902 0.737724 0.200777 0.036 Uiso 1 1 calc R U . . .
H24C H 0.125786 0.837207 0.120252 0.036 Uiso 1 1 calc R U . . .
B1 B 0.8302(8) 0.4564(9) 0.3759(7) 0.0169(19) Uani 1 1 d . . . . .
B2 B 0.7962(8) 0.5718(9) 0.2901(7) 0.017(2) Uani 1 1 d . . . . .
B3 B 0.3216(8) 0.4428(10) 0.3669(8) 0.022(2) Uani 1 1 d . . . . .
B4 B 0.2851(9) 0.5547(10) 0.2783(7) 0.023(2) 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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
B B 0.0013 0.0007
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Zr Zr -2.9673 0.5597
;
International Tables for Crystallography
(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
O1 ZR1 O3 77.8(2) . . ?
O1 ZR1 CL3 169.23(18) . . ?
O3 ZR1 CL3 91.54(16) . . ?
O1 ZR1 CL2 94.17(18) . . ?
O3 ZR1 CL2 171.89(16) . . ?
CL3 ZR1 CL2 96.41(9) . . ?
O1 ZR1 CL1 83.89(15) . . ?
O3 ZR1 CL1 84.43(16) . . ?
CL3 ZR1 CL1 96.94(9) . . ?
CL2 ZR1 CL1 96.15(9) . . ?
O1 ZR1 CL4 82.00(15) . . ?
O3 ZR1 CL4 82.51(16) . . ?
CL3 ZR1 CL4 95.02(9) . . ?
CL2 ZR1 CL4 95.16(8) . . ?
CL1 ZR1 CL4 162.49(9) . . ?
O7 ZR2 O5 75.7(2) . . ?
O7 ZR2 CL7 91.91(16) . . ?
O5 ZR2 CL7 166.55(18) . . ?
O7 ZR2 CL6 170.62(16) . . ?
O5 ZR2 CL6 95.12(17) . . ?
CL7 ZR2 CL6 96.96(9) . . ?
O7 ZR2 CL5 86.91(16) . . ?
O5 ZR2 CL5 86.55(16) . . ?
CL7 ZR2 CL5 98.30(10) . . ?
CL6 ZR2 CL5 94.77(10) . . ?
O7 ZR2 CL8 81.73(15) . . ?
O5 ZR2 CL8 80.11(16) . . ?
CL7 ZR2 CL8 92.99(9) . . ?
CL6 ZR2 CL8 94.74(8) . . ?
CL5 ZR2 CL8 164.24(10) . . ?
B1 O1 C1 107.3(6) . . ?
B1 O1 ZR1 114.1(5) . . ?
C1 O1 ZR1 136.6(5) . . ?
B1 O2 C4 108.3(6) . . ?
B2 O3 C7 107.2(6) . . ?
B2 O3 ZR1 113.6(5) . . ?
C7 O3 ZR1 136.7(5) . . ?
B2 O4 C10 107.9(7) . . ?
B3 O5 C13 105.2(7) . . ?
B3 O5 ZR2 113.1(6) . . ?
C13 O5 ZR2 141.6(5) . . ?
B3 O6 C16 107.1(7) . . ?
B4 O7 C19 105.1(7) . . ?
B4 O7 ZR2 112.6(5) . . ?
C19 O7 ZR2 142.2(5) . . ?
B4 O8 C22 107.7(7) . . ?
O1 C1 C2 107.0(7) . . ?
O1 C1 C3 108.7(7) . . ?
C2 C1 C3 110.8(7) . . ?
O1 C1 C4 101.9(6) . . ?
C2 C1 C4 113.9(7) . . ?
C3 C1 C4 113.8(8) . . ?
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 . . ?
O2 C4 C6 106.3(6) . . ?
O2 C4 C5 106.4(7) . . ?
C6 C4 C5 110.9(7) . . ?
O2 C4 C1 103.4(6) . . ?
C6 C4 C1 113.9(7) . . ?
C5 C4 C1 115.0(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C7 C8 112.7(8) . . ?
C9 C7 O3 108.9(7) . . ?
C8 C7 O3 105.7(7) . . ?
C9 C7 C10 114.3(7) . . ?
C8 C7 C10 114.1(8) . . ?
O3 C7 C10 99.9(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 C11 106.0(7) . . ?
O4 C10 C12 107.4(8) . . ?
C11 C10 C12 110.1(9) . . ?
O4 C10 C7 103.8(7) . . ?
C11 C10 C7 115.0(8) . . ?
C12 C10 C7 113.8(8) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C14 110.9(8) . . ?
C15 C13 O5 111.1(8) . . ?
C14 C13 O5 105.9(7) . . ?
C15 C13 C16 114.4(8) . . ?
C14 C13 C16 113.5(8) . . ?
O5 C13 C16 100.3(7) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O6 C16 C17 107.8(7) . . ?
O6 C16 C18 105.1(8) . . ?
C17 C16 C18 111.4(7) . . ?
O6 C16 C13 103.5(6) . . ?
C17 C16 C13 114.5(8) . . ?
C18 C16 C13 113.5(8) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 O7 110.7(7) . . ?
C21 C19 C20 110.8(8) . . ?
O7 C19 C20 105.3(7) . . ?
C21 C19 C22 115.1(8) . . ?
O7 C19 C22 100.2(6) . . ?
C20 C19 C22 113.7(8) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O8 C22 C23 107.8(8) . . ?
O8 C22 C24 106.4(7) . . ?
C23 C22 C24 111.3(8) . . ?
O8 C22 C19 102.7(6) . . ?
C23 C22 C19 114.2(8) . . ?
C24 C22 C19 113.5(8) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 B1 O1 113.9(7) . . ?
O2 B1 B2 130.0(8) . . ?
O1 B1 B2 116.0(7) . . ?
O4 B2 O3 112.0(8) . . ?
O4 B2 B1 131.5(8) . . ?
O3 B2 B1 116.4(7) . . ?
O6 B3 O5 113.7(8) . . ?
O6 B3 B4 132.3(9) . . ?
O5 B3 B4 113.7(8) . . ?
O8 B4 O7 112.0(8) . . ?
O8 B4 B3 133.0(9) . . ?
O7 B4 B3 114.7(8) . . ?
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 O1 2.328(5) . ?
ZR1 O3 2.335(6) . ?
ZR1 CL3 2.356(2) . ?
ZR1 CL2 2.378(2) . ?
ZR1 CL1 2.389(2) . ?
ZR1 CL4 2.457(2) . ?
ZR2 O7 2.315(6) . ?
ZR2 O5 2.331(5) . ?
ZR2 CL7 2.354(3) . ?
ZR2 CL6 2.368(2) . ?
ZR2 CL5 2.398(2) . ?
ZR2 CL8 2.461(2) . ?
O1 B1 1.393(11) . ?
O1 C1 1.512(10) . ?
O2 B1 1.342(11) . ?
O2 C4 1.488(10) . ?
O3 B2 1.402(12) . ?
O3 C7 1.531(10) . ?
O4 B2 1.357(11) . ?
O4 C10 1.476(10) . ?
O5 B3 1.404(12) . ?
O5 C13 1.517(11) . ?
O6 B3 1.346(13) . ?
O6 C16 1.482(11) . ?
O7 B4 1.404(13) . ?
O7 C19 1.515(9) . ?
O8 B4 1.362(12) . ?
O8 C22 1.476(11) . ?
C1 C2 1.515(12) . ?
C1 C3 1.527(12) . ?
C1 C4 1.566(12) . ?
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 C6 1.517(12) . ?
C4 C5 1.524(10) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C9 1.508(12) . ?
C7 C8 1.516(13) . ?
C7 C10 1.546(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.520(14) . ?
C10 C12 1.528(13) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.504(13) . ?
C13 C14 1.515(14) . ?
C13 C16 1.549(13) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.504(13) . ?
C16 C18 1.525(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.507(13) . ?
C19 C20 1.519(13) . ?
C19 C22 1.539(12) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.519(13) . ?
C22 C24 1.522(13) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
B1 B2 1.694(14) . ?
B3 B4 1.700(14) . ?
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
B1 O1 C1 C2 103.4(8) . . . . ?
ZR1 O1 C1 C2 -58.5(9) . . . . ?
B1 O1 C1 C3 -136.9(7) . . . . ?
ZR1 O1 C1 C3 61.2(9) . . . . ?
B1 O1 C1 C4 -16.4(8) . . . . ?
ZR1 O1 C1 C4 -178.4(5) . . . . ?
B1 O2 C4 C6 99.4(8) . . . . ?
B1 O2 C4 C5 -142.4(7) . . . . ?
B1 O2 C4 C1 -20.9(8) . . . . ?
O1 C1 C4 O2 22.0(7) . . . . ?
C2 C1 C4 O2 -92.9(8) . . . . ?
C3 C1 C4 O2 138.8(7) . . . . ?
O1 C1 C4 C6 -93.0(8) . . . . ?
C2 C1 C4 C6 152.2(7) . . . . ?
C3 C1 C4 C6 23.8(10) . . . . ?
O1 C1 C4 C5 137.5(7) . . . . ?
C2 C1 C4 C5 22.7(11) . . . . ?
C3 C1 C4 C5 -105.7(9) . . . . ?
B2 O3 C7 C9 142.9(8) . . . . ?
ZR1 O3 C7 C9 -57.2(10) . . . . ?
B2 O3 C7 C8 -95.8(8) . . . . ?
ZR1 O3 C7 C8 64.0(9) . . . . ?
B2 O3 C7 C10 22.9(8) . . . . ?
ZR1 O3 C7 C10 -177.3(5) . . . . ?
B2 O4 C10 C11 -94.6(9) . . . . ?
B2 O4 C10 C12 147.7(9) . . . . ?
B2 O4 C10 C7 26.9(9) . . . . ?
C9 C7 C10 O4 -145.3(7) . . . . ?
C8 C7 C10 O4 83.0(8) . . . . ?
O3 C7 C10 O4 -29.2(8) . . . . ?
C9 C7 C10 C11 -29.9(11) . . . . ?
C8 C7 C10 C11 -161.6(8) . . . . ?
O3 C7 C10 C11 86.1(8) . . . . ?
C9 C7 C10 C12 98.3(10) . . . . ?
C8 C7 C10 C12 -33.4(11) . . . . ?
O3 C7 C10 C12 -145.6(8) . . . . ?
B3 O5 C13 C15 149.3(8) . . . . ?
ZR2 O5 C13 C15 -28.6(12) . . . . ?
B3 O5 C13 C14 -90.2(9) . . . . ?
ZR2 O5 C13 C14 91.8(9) . . . . ?
B3 O5 C13 C16 27.9(8) . . . . ?
ZR2 O5 C13 C16 -150.0(6) . . . . ?
B3 O6 C16 C17 145.3(8) . . . . ?
B3 O6 C16 C18 -95.8(8) . . . . ?
B3 O6 C16 C13 23.6(9) . . . . ?
C15 C13 C16 O6 -149.8(8) . . . . ?
C14 C13 C16 O6 81.6(9) . . . . ?
O5 C13 C16 O6 -30.8(8) . . . . ?
C15 C13 C16 C17 93.1(10) . . . . ?
C14 C13 C16 C17 -35.5(11) . . . . ?
O5 C13 C16 C17 -147.9(7) . . . . ?
C15 C13 C16 C18 -36.4(12) . . . . ?
C14 C13 C16 C18 -165.0(8) . . . . ?
O5 C13 C16 C18 82.6(9) . . . . ?
B4 O7 C19 C21 -153.2(8) . . . . ?
ZR2 O7 C19 C21 24.0(12) . . . . ?
B4 O7 C19 C20 87.0(8) . . . . ?
ZR2 O7 C19 C20 -95.8(9) . . . . ?
B4 O7 C19 C22 -31.2(9) . . . . ?
ZR2 O7 C19 C22 146.0(7) . . . . ?
B4 O8 C22 C23 -145.9(8) . . . . ?
B4 O8 C22 C24 94.6(9) . . . . ?
B4 O8 C22 C19 -24.9(9) . . . . ?
C21 C19 C22 O8 152.2(7) . . . . ?
O7 C19 C22 O8 33.4(8) . . . . ?
C20 C19 C22 O8 -78.4(8) . . . . ?
C21 C19 C22 C23 -91.3(10) . . . . ?
O7 C19 C22 C23 149.9(7) . . . . ?
C20 C19 C22 C23 38.1(11) . . . . ?
C21 C19 C22 C24 37.8(10) . . . . ?
O7 C19 C22 C24 -81.0(8) . . . . ?
C20 C19 C22 C24 167.1(7) . . . . ?
C4 O2 B1 O1 11.2(10) . . . . ?
C4 O2 B1 B2 -165.8(8) . . . . ?
C1 O1 B1 O2 4.1(10) . . . . ?
ZR1 O1 B1 O2 170.6(6) . . . . ?
C1 O1 B1 B2 -178.4(7) . . . . ?
ZR1 O1 B1 B2 -11.9(9) . . . . ?
C10 O4 B2 O3 -12.5(10) . . . . ?
C10 O4 B2 B1 165.2(9) . . . . ?
C7 O3 B2 O4 -7.6(10) . . . . ?
ZR1 O3 B2 O4 -172.7(6) . . . . ?
C7 O3 B2 B1 174.3(7) . . . . ?
ZR1 O3 B2 B1 9.2(9) . . . . ?
O2 B1 B2 O4 1.1(17) . . . . ?
O1 B1 B2 O4 -175.9(9) . . . . ?
O2 B1 B2 O3 178.8(9) . . . . ?
O1 B1 B2 O3 1.8(12) . . . . ?
C16 O6 B3 O5 -5.7(10) . . . . ?
C16 O6 B3 B4 -179.7(9) . . . . ?
C13 O5 B3 O6 -15.3(10) . . . . ?
ZR2 O5 B3 O6 163.3(6) . . . . ?
C13 O5 B3 B4 159.9(8) . . . . ?
ZR2 O5 B3 B4 -21.5(9) . . . . ?
C22 O8 B4 O7 5.0(11) . . . . ?
C22 O8 B4 B3 178.9(10) . . . . ?
C19 O7 B4 O8 17.6(10) . . . . ?
ZR2 O7 B4 O8 -160.5(6) . . . . ?
C19 O7 B4 B3 -157.4(8) . . . . ?
ZR2 O7 B4 B3 24.4(10) . . . . ?
O6 B3 B4 O8 -1.6(19) . . . . ?
O5 B3 B4 O8 -175.7(10) . . . . ?
O6 B3 B4 O7 172.1(9) . . . . ?
O5 B3 B4 O7 -1.9(12) . . . . ?
