# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_hsy10076-Ti-1
_database_code_depnum_ccdc_archive 'CCDC 2161198'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C10 H20 B2 Cl4 O4 Ti'
_chemical_formula_moiety         'C10 H20 B2 Cl4 O4 Ti'
_chemical_formula_weight         415.60
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   13.1002(15)
_cell_length_b                   14.9056(16)
_cell_length_c                   18.441(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.310(4)
_cell_angle_gamma                90.0000
_cell_volume                     3594.9(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5132
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.40
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696.00
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  0.979

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            114751
_diffrn_reflns_av_R_equivalents  0.1318
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         3.097
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8272
_reflns_number_gt                6572
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1548
_refine_ls_wR_factor_gt          0.1427
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         8272
_refine_ls_number_parameters     387
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0724P)²+9.9325P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         2.14
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
TI1 Ti 0.74681(5) 0.14524(4) 0.36994(3) 0.01739(15) Uani 1 1 d . . . . .
TI2 Ti 0.75970(5) 0.82072(4) 0.62174(3) 0.01845(15) Uani 1 1 d . . . . .
CL1 Cl 0.88496(7) 0.19959(6) 0.31117(5) 0.0245(2) Uani 1 1 d . . . . .
CL2 Cl 0.80406(7) 0.00444(6) 0.37220(5) 0.0253(2) Uani 1 1 d . . . . .
CL3 Cl 0.62178(7) 0.12157(6) 0.44765(5) 0.0262(2) Uani 1 1 d . . . . .
CL4 Cl 0.64232(8) 0.14126(6) 0.27097(5) 0.0286(2) Uani 1 1 d . . . . .
CL5 Cl 0.83815(7) 0.83098(6) 0.73103(5) 0.0256(2) Uani 1 1 d . . . . .
CL6 Cl 0.62672(7) 0.73446(7) 0.65505(5) 0.0303(2) Uani 1 1 d . . . . .
CL7 Cl 0.89473(7) 0.87389(6) 0.56061(5) 0.0262(2) Uani 1 1 d . . . . .
CL8 Cl 0.67644(8) 0.95040(7) 0.62092(5) 0.0301(2) Uani 1 1 d . . . . .
O1 O 0.8390(2) 0.17607(16) 0.46959(13) 0.0204(5) Uani 1 1 d . . . . .
O2 O 0.9370(2) 0.29292(18) 0.53038(15) 0.0311(6) Uani 1 1 d . . . . .
O3 O 0.7200(2) 0.29011(16) 0.38415(13) 0.0213(5) Uani 1 1 d . . . . .
O4 O 0.8278(2) 0.41974(18) 0.40331(16) 0.0328(7) Uani 1 1 d . . . . .
O5 O 0.8304(2) 0.68866(16) 0.60178(13) 0.0216(5) Uani 1 1 d . . . . .
O6 O 0.8622(2) 0.57984(17) 0.50939(13) 0.0229(5) Uani 1 1 d . . . . .
O7 O 0.6973(2) 0.79174(17) 0.50931(13) 0.0229(5) Uani 1 1 d . . . . .
O8 O 0.7378(2) 0.71163(19) 0.40104(13) 0.0275(6) Uani 1 1 d . . . . .
C1 C 0.8657(3) 0.1122(2) 0.52867(18) 0.0197(7) Uani 1 1 d . . . . .
H1A H 0.927854 0.078390 0.517400 0.024 Uiso 1 1 calc R U . . .
H1B H 0.809196 0.068676 0.532942 0.024 Uiso 1 1 calc R U . . .
C2 C 0.8846(3) 0.1623(2) 0.60050(19) 0.0208(7) Uani 1 1 d . . . . .
C3 C 0.9683(3) 0.2315(3) 0.5890(2) 0.0273(8) Uani 1 1 d . . . . .
H3A H 0.982604 0.265827 0.634452 0.033 Uiso 1 1 calc R U . . .
H3B H 1.031914 0.200313 0.577094 0.033 Uiso 1 1 calc R U . . .
C4 C 0.7864(3) 0.2063(3) 0.6235(2) 0.0289(8) Uani 1 1 d . . . . .
H4A H 0.761631 0.248989 0.586121 0.035 Uiso 1 1 calc R U . . .
H4B H 0.800218 0.238136 0.669589 0.035 Uiso 1 1 calc R U . . .
H4C H 0.734443 0.160136 0.629741 0.035 Uiso 1 1 calc R U . . .
C5 C 0.9252(3) 0.0956(3) 0.6586(2) 0.0284(8) Uani 1 1 d . . . . .
H5A H 0.873143 0.049881 0.666102 0.034 Uiso 1 1 calc R U . . .
H5B H 0.941215 0.127613 0.704289 0.034 Uiso 1 1 calc R U . . .
H5C H 0.987238 0.066783 0.642552 0.034 Uiso 1 1 calc R U . . .
C6 C 0.6461(3) 0.3430(2) 0.3391(2) 0.0210(7) Uani 1 1 d . . . . .
H6A H 0.576749 0.317440 0.342637 0.025 Uiso 1 1 calc R U . . .
H6B H 0.663664 0.339777 0.287664 0.025 Uiso 1 1 calc R U . . .
C7 C 0.6464(3) 0.4405(2) 0.36364(19) 0.0241(8) Uani 1 1 d . . . . .
C8 C 0.7556(3) 0.4748(3) 0.3600(2) 0.0313(9) Uani 1 1 d . . . . .
H8A H 0.774626 0.474612 0.308798 0.038 Uiso 1 1 calc R U . . .
H8B H 0.759353 0.537391 0.377804 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5767(4) 0.4938(3) 0.3106(2) 0.0335(9) Uani 1 1 d . . . . .
H9A H 0.577478 0.557171 0.324872 0.040 Uiso 1 1 calc R U . . .
H9B H 0.506755 0.470571 0.311215 0.040 Uiso 1 1 calc R U . . .
H9C H 0.600924 0.488106 0.261505 0.040 Uiso 1 1 calc R U . . .
C10 C 0.6108(4) 0.4484(3) 0.4406(2) 0.0416(12) Uani 1 1 d . . . . .
H10A H 0.656114 0.413117 0.473763 0.050 Uiso 1 1 calc R U . . .
H10B H 0.540762 0.425743 0.441932 0.050 Uiso 1 1 calc R U . . .
H10C H 0.612835 0.511483 0.455633 0.050 Uiso 1 1 calc R U . . .
C11 C 0.8814(3) 0.6332(2) 0.65845(18) 0.0227(8) Uani 1 1 d . . . . .
H11A H 0.848423 0.642319 0.704859 0.027 Uiso 1 1 calc R U . . .
H11B H 0.953952 0.651333 0.665560 0.027 Uiso 1 1 calc R U . . .
C12 C 0.8751(3) 0.5344(2) 0.63721(18) 0.0224(7) Uani 1 1 d . . . . .
C13 C 0.9162(3) 0.5240(3) 0.56241(19) 0.0240(8) Uani 1 1 d . . . . .
H13A H 0.989629 0.540021 0.564812 0.029 Uiso 1 1 calc R U . . .
H13B H 0.909897 0.460499 0.547077 0.029 Uiso 1 1 calc R U . . .
C14 C 0.7654(3) 0.5001(3) 0.6388(2) 0.0346(9) Uani 1 1 d . . . . .
H14A H 0.763086 0.436690 0.624832 0.042 Uiso 1 1 calc R U . . .
H14B H 0.721160 0.534908 0.604553 0.042 Uiso 1 1 calc R U . . .
H14C H 0.741617 0.506807 0.687882 0.042 Uiso 1 1 calc R U . . .
C15 C 0.9459(4) 0.4816(3) 0.6907(2) 0.0333(10) Uani 1 1 d . . . . .
H15A H 1.015396 0.505742 0.690225 0.040 Uiso 1 1 calc R U . . .
H15B H 0.946191 0.418255 0.676360 0.040 Uiso 1 1 calc R U . . .
H15C H 0.921306 0.486871 0.739709 0.040 Uiso 1 1 calc R U . . .
C16 C 0.6256(3) 0.8511(2) 0.46770(18) 0.0192(7) Uani 1 1 d . . . . .
H16A H 0.661591 0.906408 0.453859 0.023 Uiso 1 1 calc R U . . .
H16B H 0.569097 0.868480 0.498205 0.023 Uiso 1 1 calc R U . . .
C17 C 0.5824(3) 0.8033(3) 0.39958(19) 0.0233(8) Uani 1 1 d . . . . .
C18 C 0.6704(3) 0.7687(3) 0.35741(19) 0.0264(8) Uani 1 1 d . . . . .
H18A H 0.642726 0.734753 0.314526 0.032 Uiso 1 1 calc R U . . .
H18B H 0.709677 0.820254 0.339765 0.032 Uiso 1 1 calc R U . . .
C19 C 0.5127(3) 0.7258(3) 0.4204(2) 0.0308(9) Uani 1 1 d . . . . .
H19A H 0.552561 0.682054 0.449833 0.037 Uiso 1 1 calc R U . . .
H19B H 0.483756 0.696641 0.376223 0.037 Uiso 1 1 calc R U . . .
H19C H 0.457216 0.749280 0.448391 0.037 Uiso 1 1 calc R U . . .
C20 C 0.5219(4) 0.8725(3) 0.3534(2) 0.0365(10) Uani 1 1 d . . . . .
H20A H 0.488121 0.842713 0.311131 0.044 Uiso 1 1 calc R U . . .
H20B H 0.568453 0.918723 0.337023 0.044 Uiso 1 1 calc R U . . .
H20C H 0.470179 0.900321 0.382512 0.044 Uiso 1 1 calc R U . . .
B1 B 0.8723(3) 0.2655(3) 0.4762(2) 0.0239(9) Uani 1 1 d . . . . .
B2 B 0.8069(3) 0.3332(3) 0.4155(2) 0.0240(9) Uani 1 1 d . . . . .
B3 B 0.8223(3) 0.6573(3) 0.5300(2) 0.0203(8) Uani 1 1 d . . . . .
B4 B 0.7497(3) 0.7246(3) 0.4735(2) 0.0235(8) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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
TI1 O1 2.189(3) . ?
TI1 O3 2.206(2) . ?
TI1 CL4 2.2180(11) . ?
TI1 CL2 2.2283(11) . ?
TI1 CL3 2.2652(11) . ?
TI1 CL1 2.3093(11) . ?
TI2 CL5 2.2141(11) . ?
TI2 O5 2.215(3) . ?
TI2 CL8 2.2190(11) . ?
TI2 O7 2.227(2) . ?
TI2 CL6 2.2779(11) . ?
TI2 CL7 2.2930(11) . ?
O1 B1 1.405(5) . ?
O1 C1 1.474(4) . ?
O2 B1 1.336(5) . ?
O2 C3 1.458(5) . ?
O3 B2 1.402(5) . ?
O3 C6 1.468(4) . ?
O4 B2 1.341(5) . ?
O4 C8 1.456(5) . ?
O5 B3 1.402(4) . ?
O5 C11 1.464(4) . ?
O6 B3 1.332(5) . ?
O6 C13 1.439(4) . ?
O7 B4 1.400(5) . ?
O7 C16 1.473(4) . ?
O8 B4 1.351(5) . ?
O8 C18 1.438(4) . ?
C1 C2 1.529(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C4 1.526(5) . ?
C2 C3 1.528(5) . ?
C2 C5 1.534(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.522(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C9 1.523(5) . ?
C7 C10 1.524(5) . ?
C7 C8 1.524(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.517(5) . ?
C12 C14 1.527(6) . ?
C12 C15 1.532(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
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 1.524(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.517(5) . ?
C17 C20 1.530(5) . ?
C17 C19 1.535(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
B1 B2 1.702(6) . ?
B3 B4 1.697(6) . ?

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 TI1 O3 77.21(9) . . ?
O1 TI1 CL4 168.78(7) . . ?
O3 TI1 CL4 91.66(7) . . ?
O1 TI1 CL2 90.75(7) . . ?
O3 TI1 CL2 167.30(8) . . ?
CL4 TI1 CL2 100.45(4) . . ?
O1 TI1 CL3 83.44(7) . . ?
O3 TI1 CL3 87.21(8) . . ?
CL4 TI1 CL3 94.70(4) . . ?
CL2 TI1 CL3 95.53(4) . . ?
O1 TI1 CL1 84.88(7) . . ?
O3 TI1 CL1 81.19(8) . . ?
CL4 TI1 CL1 94.95(4) . . ?
CL2 TI1 CL1 93.85(4) . . ?
CL3 TI1 CL1 165.10(4) . . ?
CL5 TI2 O5 92.07(7) . . ?
CL5 TI2 CL8 98.52(4) . . ?
O5 TI2 CL8 169.39(7) . . ?
CL5 TI2 O7 170.81(8) . . ?
O5 TI2 O7 78.89(9) . . ?
CL8 TI2 O7 90.50(7) . . ?
CL5 TI2 CL6 96.63(4) . . ?
O5 TI2 CL6 82.91(8) . . ?
CL8 TI2 CL6 96.33(5) . . ?
O7 TI2 CL6 84.04(8) . . ?
CL5 TI2 CL7 95.34(4) . . ?
O5 TI2 CL7 83.33(7) . . ?
CL8 TI2 CL7 95.07(4) . . ?
O7 TI2 CL7 82.04(8) . . ?
CL6 TI2 CL7 162.05(4) . . ?
B1 O1 C1 119.3(3) . . ?
B1 O1 TI1 115.2(2) . . ?
C1 O1 TI1 125.5(2) . . ?
B1 O2 C3 120.1(3) . . ?
B2 O3 C6 118.8(3) . . ?
B2 O3 TI1 111.5(2) . . ?
C6 O3 TI1 124.2(2) . . ?
B2 O4 C8 120.1(3) . . ?
B3 O5 C11 119.5(3) . . ?
B3 O5 TI2 116.3(2) . . ?
C11 O5 TI2 124.2(2) . . ?
B3 O6 C13 119.5(3) . . ?
B4 O7 C16 119.9(3) . . ?
B4 O7 TI2 114.4(2) . . ?
C16 O7 TI2 123.86(19) . . ?
B4 O8 C18 120.1(3) . . ?
O1 C1 C2 110.1(3) . . ?
O1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
O1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
C4 C2 C3 111.8(3) . . ?
C4 C2 C1 110.7(3) . . ?
C3 C2 C1 107.0(3) . . ?
C4 C2 C5 110.4(3) . . ?
C3 C2 C5 108.1(3) . . ?
C1 C2 C5 108.7(3) . . ?
O2 C3 C2 110.6(3) . . ?
O2 C3 H3A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
O2 C3 H3B 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 C7 110.7(3) . . ?
O3 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
O3 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C9 108.4(3) . . ?
C6 C7 C10 110.8(3) . . ?
C9 C7 C10 110.7(3) . . ?
C6 C7 C8 107.0(3) . . ?
C9 C7 C8 109.0(3) . . ?
C10 C7 C8 110.7(4) . . ?
O4 C8 C7 111.6(3) . . ?
O4 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
O4 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
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 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 C12 110.3(3) . . ?
O5 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
O5 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C13 C12 C11 108.4(3) . . ?
C13 C12 C14 111.5(3) . . ?
C11 C12 C14 110.8(3) . . ?
C13 C12 C15 107.4(3) . . ?
C11 C12 C15 108.0(3) . . ?
C14 C12 C15 110.5(3) . . ?
O6 C13 C12 111.9(3) . . ?
O6 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
O6 C13 H13B 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 C17 110.1(3) . . ?
O7 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
O7 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.2 . . ?
C18 C17 C16 108.9(3) . . ?
C18 C17 C20 109.2(3) . . ?
C16 C17 C20 107.4(3) . . ?
C18 C17 C19 110.7(3) . . ?
C16 C17 C19 110.1(3) . . ?
C20 C17 C19 110.4(3) . . ?
O8 C18 C17 112.0(3) . . ?
O8 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
O8 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
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 . . ?
O2 B1 O1 122.4(3) . . ?
O2 B1 B2 125.7(3) . . ?
O1 B1 B2 111.3(3) . . ?
O4 B2 O3 122.7(4) . . ?
O4 B2 B1 125.5(4) . . ?
O3 B2 B1 111.5(3) . . ?
O6 B3 O5 123.3(3) . . ?
O6 B3 B4 123.5(3) . . ?
O5 B3 B4 113.1(3) . . ?
O8 B4 O7 122.5(4) . . ?
O8 B4 B3 123.5(3) . . ?
O7 B4 B3 113.9(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
B1 O1 C1 C2 25.1(4) . . . . ?
TI1 O1 C1 C2 -153.6(2) . . . . ?
O1 C1 C2 C4 65.7(4) . . . . ?
O1 C1 C2 C3 -56.4(4) . . . . ?
O1 C1 C2 C5 -172.9(3) . . . . ?
B1 O2 C3 C2 -28.9(5) . . . . ?
C4 C2 C3 O2 -62.6(4) . . . . ?
C1 C2 C3 O2 58.8(4) . . . . ?
C5 C2 C3 O2 175.7(3) . . . . ?
B2 O3 C6 C7 -28.9(4) . . . . ?
TI1 O3 C6 C7 179.7(2) . . . . ?
O3 C6 C7 C9 174.3(3) . . . . ?
O3 C6 C7 C10 -63.9(4) . . . . ?
O3 C6 C7 C8 56.9(4) . . . . ?
B2 O4 C8 C7 27.0(5) . . . . ?
C6 C7 C8 O4 -56.4(4) . . . . ?
C9 C7 C8 O4 -173.5(3) . . . . ?
C10 C7 C8 O4 64.5(4) . . . . ?
B3 O5 C11 C12 -25.8(5) . . . . ?
TI2 O5 C11 C12 152.6(2) . . . . ?
O5 C11 C12 C13 53.5(4) . . . . ?
O5 C11 C12 C14 -69.2(4) . . . . ?
O5 C11 C12 C15 169.6(3) . . . . ?
B3 O6 C13 C12 30.3(5) . . . . ?
C11 C12 C13 O6 -56.6(4) . . . . ?
C14 C12 C13 O6 65.6(4) . . . . ?
C15 C12 C13 O6 -173.1(3) . . . . ?
B4 O7 C16 C17 27.0(4) . . . . ?
TI2 O7 C16 C17 -169.0(2) . . . . ?
O7 C16 C17 C18 -53.5(4) . . . . ?
O7 C16 C17 C20 -171.7(3) . . . . ?
O7 C16 C17 C19 68.0(4) . . . . ?
B4 O8 C18 C17 -29.9(5) . . . . ?
C16 C17 C18 O8 55.8(4) . . . . ?
C20 C17 C18 O8 172.9(3) . . . . ?
C19 C17 C18 O8 -65.3(4) . . . . ?
C3 O2 B1 O1 -5.6(6) . . . . ?
C3 O2 B1 B2 164.6(4) . . . . ?
C1 O1 B1 O2 7.6(6) . . . . ?
TI1 O1 B1 O2 -173.6(3) . . . . ?
C1 O1 B1 B2 -163.9(3) . . . . ?
TI1 O1 B1 B2 14.9(4) . . . . ?
C8 O4 B2 O3 4.3(6) . . . . ?
C8 O4 B2 B1 -168.8(4) . . . . ?
C6 O3 B2 O4 -3.3(6) . . . . ?
TI1 O3 B2 O4 151.6(3) . . . . ?
C6 O3 B2 B1 170.7(3) . . . . ?
TI1 O3 B2 B1 -34.4(4) . . . . ?
O2 B1 B2 O4 16.0(7) . . . . ?
O1 B1 B2 O4 -172.8(4) . . . . ?
O2 B1 B2 O3 -157.8(4) . . . . ?
O1 B1 B2 O3 13.4(5) . . . . ?
C13 O6 B3 O5 0.3(5) . . . . ?
C13 O6 B3 B4 -175.2(3) . . . . ?
C11 O5 B3 O6 -2.4(5) . . . . ?
TI2 O5 B3 O6 179.0(3) . . . . ?
C11 O5 B3 B4 173.5(3) . . . . ?
TI2 O5 B3 B4 -5.1(4) . . . . ?
C18 O8 B4 O7 0.9(6) . . . . ?
C18 O8 B4 B3 176.6(3) . . . . ?
C16 O7 B4 O8 0.4(6) . . . . ?
TI2 O7 B4 O8 -165.1(3) . . . . ?
C16 O7 B4 B3 -175.7(3) . . . . ?
TI2 O7 B4 B3 18.8(4) . . . . ?
O6 B3 B4 O8 -9.5(6) . . . . ?
O5 B3 B4 O8 174.6(4) . . . . ?
O6 B3 B4 O7 166.6(3) . . . . ?
O5 B3 B4 O7 -9.3(5) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy15030-Mo-2
_database_code_depnum_ccdc_archive 'CCDC 2162823'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C10 H20 B2 Cl4 Mo O4'
_chemical_formula_moiety         'C10 H20 B2 Cl4 Mo O4'
_chemical_formula_weight         463.64
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   6.553(2)
_cell_length_b                   14.886(5)
_cell_length_c                   18.470(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.581(10)
_cell_angle_gamma                90.0000
_cell_volume                     1798.2(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2318
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.10
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928.00
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  0.974

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            21766
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         3.115
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4125
_reflns_number_gt                2641
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1800
_refine_ls_R_factor_gt           0.1232
_refine_ls_wR_factor_ref         0.3458
_refine_ls_wR_factor_gt          0.3020
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4125
_refine_ls_number_parameters     194
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1444P)²+46.1236P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         4.03
_refine_diff_density_min         -3.21
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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)
;
Mo Mo -1.6832 0.6857
;
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)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
MO1 Mo 0.50167(18) 0.83877(9) 0.62733(6) 0.0428(4) Uani 1 1 d . . . . .
CL1 Cl 0.7687(5) 0.8714(2) 0.55563(16) 0.0402(7) Uani 1 1 d . . . . .
CL2 Cl 0.3831(7) 0.9768(4) 0.6283(2) 0.0721(14) Uani 1 1 d . . . . .
CL3 Cl 0.2096(7) 0.7809(5) 0.6767(3) 0.131(3) Uani 1 1 d . . . . .
CL4 Cl 0.6849(5) 0.8481(2) 0.73411(16) 0.0426(8) Uani 1 1 d . . . . .
O1 O 0.585(3) 0.6951(7) 0.6139(6) 0.087(5) Uani 1 1 d . . . . .
O2 O 0.360(3) 0.5674(11) 0.5849(11) 0.145(9) Uani 1 1 d . . . . .
O3 O 0.3423(19) 0.8081(7) 0.5217(6) 0.066(4) Uani 1 1 d . . . . .
O4 O 0.131(2) 0.6952(10) 0.4637(8) 0.090(4) Uani 1 1 d . . . . .
C1 C 0.716(2) 0.6424(8) 0.6633(6) 0.041(3) Uani 1 1 d . . . . .
H1A H 0.662417 0.643403 0.712256 0.049 Uiso 1 1 calc R U . . .
H1B H 0.855450 0.668407 0.666904 0.049 Uiso 1 1 calc R U . . .
C2 C 0.725(2) 0.5462(9) 0.6363(7) 0.045(3) Uani 1 1 d . . . . .
C3 C 0.510(3) 0.5106(10) 0.6338(9) 0.062(5) Uani 1 1 d . . . . .
H3A H 0.462297 0.509489 0.683626 0.075 Uiso 1 1 calc R U . . .
H3B H 0.509178 0.448060 0.615547 0.075 Uiso 1 1 calc R U . . .
C4 C 0.812(3) 0.5440(15) 0.5617(9) 0.085(6) Uani 1 1 d . . . . .
H4A H 0.724677 0.579304 0.527505 0.102 Uiso 1 1 calc R U . . .
H4B H 0.817712 0.481679 0.544776 0.102 Uiso 1 1 calc R U . . .
H4C H 0.950353 0.569426 0.565035 0.102 Uiso 1 1 calc R U . . .
C5 C 0.868(3) 0.4915(9) 0.6896(7) 0.051(4) Uani 1 1 d . . . . .
H5A H 0.869837 0.428652 0.673836 0.061 Uiso 1 1 calc R U . . .
H5B H 0.817185 0.494812 0.738369 0.061 Uiso 1 1 calc R U . . .
H5C H 1.006191 0.516339 0.690336 0.061 Uiso 1 1 calc R U . . .
C6 C 0.2572(18) 0.8729(9) 0.4697(6) 0.036(3) Uani 1 1 d . . . . .
H6A H 0.358606 0.920734 0.462196 0.043 Uiso 1 1 calc R U . . .
H6B H 0.134176 0.901018 0.488489 0.043 Uiso 1 1 calc R U . . .
C7 C 0.201(2) 0.8261(10) 0.3987(6) 0.044(3) Uani 1 1 d . . . . .
C8 C 0.052(2) 0.7527(11) 0.4107(7) 0.054(4) Uani 1 1 d . . . . .
H8A H -0.078118 0.778801 0.425757 0.065 Uiso 1 1 calc R U . . .
H8B H 0.022121 0.719166 0.364963 0.065 Uiso 1 1 calc R U . . .
C9 C 0.399(3) 0.7885(11) 0.3673(8) 0.058(4) Uani 1 1 d . . . . .
H9A H 0.367005 0.765946 0.318038 0.070 Uiso 1 1 calc R U . . .
H9B H 0.453595 0.739448 0.398131 0.070 Uiso 1 1 calc R U . . .
H9C H 0.501095 0.836508 0.365939 0.070 Uiso 1 1 calc R U . . .
C10 C 0.101(3) 0.8952(11) 0.3458(8) 0.067(5) Uani 1 1 d . . . . .
H10A H -0.015985 0.923113 0.367779 0.080 Uiso 1 1 calc R U . . .
H10B H 0.053415 0.865061 0.300656 0.080 Uiso 1 1 calc R U . . .
H10C H 0.200739 0.941609 0.335221 0.080 Uiso 1 1 calc R U . . .
B1 B 0.391(4) 0.6560(16) 0.5769(13) 0.076(6) Uani 1 1 d . . . . .
B2 B 0.264(4) 0.7244(16) 0.5186(12) 0.073(6) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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
MO1 CL2 2.198(5) . ?
MO1 O3 2.203(9) . ?
MO1 O1 2.225(11) . ?
MO1 CL4 2.248(3) . ?
MO1 CL1 2.311(3) . ?
MO1 CL3 2.336(4) . ?
O1 C1 1.446(17) . ?
O1 B1 1.52(3) . ?
O2 B1 1.34(3) . ?
O2 C3 1.54(2) . ?
O3 B2 1.35(3) . ?
O3 C6 1.447(15) . ?
O4 B2 1.36(2) . ?
O4 C8 1.380(19) . ?
C1 C2 1.518(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.50(2) . ?
C2 C4 1.52(2) . ?
C2 C5 1.55(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.511(18) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.49(2) . ?
C7 C10 1.538(17) . ?
C7 C9 1.559(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
B1 B2 1.67(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
CL2 MO1 O3 93.1(3) . . ?
CL2 MO1 O1 171.6(3) . . ?
O3 MO1 O1 78.9(4) . . ?
CL2 MO1 CL4 95.99(16) . . ?
O3 MO1 CL4 170.9(3) . . ?
O1 MO1 CL4 92.1(3) . . ?
CL2 MO1 CL1 95.11(15) . . ?
O3 MO1 CL1 82.5(3) . . ?
O1 MO1 CL1 86.4(5) . . ?
CL4 MO1 CL1 96.18(13) . . ?
CL2 MO1 CL3 92.4(3) . . ?
O3 MO1 CL3 85.1(4) . . ?
O1 MO1 CL3 84.4(5) . . ?
CL4 MO1 CL3 94.93(16) . . ?
CL1 MO1 CL3 165.8(2) . . ?
C1 O1 B1 121.5(12) . . ?
C1 O1 MO1 126.3(7) . . ?
B1 O1 MO1 102.3(12) . . ?
B1 O2 C3 120.4(17) . . ?
B2 O3 C6 117.3(12) . . ?
B2 O3 MO1 112.8(10) . . ?
C6 O3 MO1 126.2(8) . . ?
B2 O4 C8 121.6(16) . . ?
O1 C1 C2 109.7(10) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C3 C2 C1 106.8(13) . . ?
C3 C2 C4 111.7(13) . . ?
C1 C2 C4 110.0(13) . . ?
C3 C2 C5 111.2(12) . . ?
C1 C2 C5 108.7(10) . . ?
C4 C2 C5 108.5(14) . . ?
C2 C3 O2 112.7(12) . . ?
C2 C3 H3A 109.1 . . ?
O2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
O2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 C7 109.3(11) . . ?
O3 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 C6 109.6(11) . . ?
C8 C7 C10 109.0(13) . . ?
C6 C7 C10 108.3(11) . . ?
C8 C7 C9 111.2(12) . . ?
C6 C7 C9 109.0(12) . . ?
C10 C7 C9 109.7(12) . . ?
O4 C8 C7 109.7(12) . . ?
O4 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
O4 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
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 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 B1 O1 117(2) . . ?
O2 B1 B2 127(2) . . ?
O1 B1 B2 115.2(16) . . ?
O3 B2 O4 123.3(18) . . ?
O3 B2 B1 111.3(17) . . ?
O4 B2 B1 124(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
B1 O1 C1 C2 38(2) . . . . ?
MO1 O1 C1 C2 176.9(11) . . . . ?
O1 C1 C2 C3 -60.6(15) . . . . ?
O1 C1 C2 C4 60.7(18) . . . . ?
O1 C1 C2 C5 179.3(13) . . . . ?
C1 C2 C3 O2 57.8(18) . . . . ?
C4 C2 C3 O2 -62(2) . . . . ?
C5 C2 C3 O2 176.2(15) . . . . ?
B1 O2 C3 C2 -30(3) . . . . ?
B2 O3 C6 C7 -35(2) . . . . ?
MO1 O3 C6 C7 168.4(10) . . . . ?
O3 C6 C7 C8 58.2(13) . . . . ?
O3 C6 C7 C10 177.1(13) . . . . ?
O3 C6 C7 C9 -63.7(14) . . . . ?
B2 O4 C8 C7 30(2) . . . . ?
C6 C7 C8 O4 -55.3(15) . . . . ?
C10 C7 C8 O4 -173.7(13) . . . . ?
C9 C7 C8 O4 65.2(16) . . . . ?
C3 O2 B1 O1 4(4) . . . . ?
C3 O2 B1 B2 171(2) . . . . ?
C1 O1 B1 O2 -8(3) . . . . ?
MO1 O1 B1 O2 -156(2) . . . . ?
C1 O1 B1 B2 -177.2(17) . . . . ?
MO1 O1 B1 B2 35(2) . . . . ?
C6 O3 B2 O4 9(3) . . . . ?
MO1 O3 B2 O4 169.0(18) . . . . ?
C6 O3 B2 B1 175.2(16) . . . . ?
MO1 O3 B2 B1 -25(2) . . . . ?
C8 O4 B2 O3 -7(3) . . . . ?
C8 O4 B2 B1 -170.7(19) . . . . ?
O2 B1 B2 O3 -176(3) . . . . ?
O1 B1 B2 O3 -8(3) . . . . ?
O2 B1 B2 O4 -10(4) . . . . ?
O1 B1 B2 O4 157(2) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy13091-Nb-1
_database_code_depnum_ccdc_archive 'CCDC 2161222'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C10 H20 B2 Cl4 Nb O4'
_chemical_formula_moiety         'C10 H20 B2 Cl4 Nb O4'
_chemical_formula_weight         460.59
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   15.394(6)
_cell_length_b                   6.4687(19)
_cell_length_c                   19.388(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.043(7)
_cell_angle_gamma                90.0000
_cell_volume                     1801.9(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1490
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      26.00
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892.00
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_T_max  0.975

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            39446
_diffrn_reflns_av_R_equivalents  0.2374
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         3.159
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4164
_reflns_number_gt                2350
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1315
_refine_ls_wR_factor_gt          0.1065
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4164
_refine_ls_number_parameters     194
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0517P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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)
;
Nb Nb -2.0727 0.6215
;
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)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
NB1 Nb 0.29562(4) 0.20954(9) 0.52236(3) 0.01801(17) Uani 1 1 d . . . . .
CL1 Cl 0.34600(11) -0.0690(3) 0.60626(8) 0.0244(4) Uani 1 1 d . . . . .
CL2 Cl 0.25885(11) 0.5375(3) 0.47261(8) 0.0248(4) Uani 1 1 d . . . . .
CL3 Cl 0.15760(11) 0.0504(3) 0.44626(9) 0.0278(4) Uani 1 1 d . . . . .
CL4 Cl 0.38007(11) 0.1129(3) 0.44804(9) 0.0273(4) Uani 1 1 d . . . . .
O1 O 0.2264(3) 0.3198(7) 0.6004(2) 0.0200(10) Uani 1 1 d . . . . .
O2 O 0.2591(3) 0.4719(7) 0.7205(2) 0.0223(10) Uani 1 1 d . . . . .
O3 O 0.4188(3) 0.3673(7) 0.6090(2) 0.0187(10) Uani 1 1 d . . . . .
O4 O 0.4652(3) 0.5251(7) 0.7294(2) 0.0232(11) Uani 1 1 d . . . . .
C1 C 0.1262(4) 0.3023(11) 0.5885(3) 0.0242(15) Uani 1 1 d . . . . .
H9A H 0.113459 0.163753 0.604416 0.029 Uiso 1 1 calc R U . . .
H9B H 0.089150 0.317460 0.535218 0.029 Uiso 1 1 calc R U . . .
C2 C 0.0975(4) 0.4669(10) 0.6317(3) 0.0182(14) Uani 1 1 d . . . . .
C3 C 0.1617(4) 0.4486(11) 0.7125(3) 0.0213(15) Uani 1 1 d . . . . .
H7A H 0.145207 0.556419 0.741951 0.026 Uiso 1 1 calc R U . . .
H7B H 0.152590 0.312014 0.731941 0.026 Uiso 1 1 calc R U . . .
C4 C 0.1031(4) 0.6833(10) 0.6030(4) 0.0245(15) Uani 1 1 d . . . . .
H15A H 0.059745 0.694891 0.551822 0.029 Uiso 1 1 calc R U . . .
H15B H 0.166630 0.709747 0.604988 0.029 Uiso 1 1 calc R U . . .
H15C H 0.086530 0.784895 0.633738 0.029 Uiso 1 1 calc R U . . .
C5 C -0.0018(4) 0.4178(12) 0.6267(4) 0.0269(16) Uani 1 1 d . . . . .
H12A H -0.003257 0.281083 0.648006 0.032 Uiso 1 1 calc R U . . .
H12B H -0.043397 0.418639 0.574738 0.032 Uiso 1 1 calc R U . . .
H12C H -0.022504 0.522306 0.654025 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5157(4) 0.3804(11) 0.6094(3) 0.0222(15) Uani 1 1 d . . . . .
H5A H 0.523944 0.511575 0.586182 0.027 Uiso 1 1 calc R U . . .
H5B H 0.527305 0.264573 0.580479 0.027 Uiso 1 1 calc R U . . .
C7 C 0.5852(4) 0.3706(10) 0.6890(3) 0.0210(15) Uani 1 1 d . . . . .
C8 C 0.5605(4) 0.5432(11) 0.7325(3) 0.0272(16) Uani 1 1 d . . . . .
H14A H 0.603238 0.537457 0.784696 0.033 Uiso 1 1 calc R U . . .
H14B H 0.568930 0.678762 0.712028 0.033 Uiso 1 1 calc R U . . .
C9 C 0.6829(4) 0.4114(12) 0.6887(4) 0.0269(16) Uani 1 1 d . . . . .
H10A H 0.727848 0.408353 0.739483 0.032 Uiso 1 1 calc R U . . .
H10B H 0.684477 0.547354 0.666873 0.032 Uiso 1 1 calc R U . . .
H10C H 0.698961 0.304514 0.659451 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5819(4) 0.1580(10) 0.7232(4) 0.0241(16) Uani 1 1 d . . . . .
H11A H 0.602280 0.051518 0.696335 0.029 Uiso 1 1 calc R U . . .
H11B H 0.518100 0.128562 0.719886 0.029 Uiso 1 1 calc R U . . .
H11C H 0.623291 0.158107 0.775168 0.029 Uiso 1 1 calc R U . . .
B13 B 0.3998(5) 0.4422(12) 0.6697(4) 0.0203(17) Uani 1 1 d . . . . .
B17 B 0.2870(5) 0.4131(12) 0.6654(4) 0.0193(16) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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
NB1 O1 2.257(4) . ?
NB1 O3 2.273(4) . ?
NB1 CL2 2.3148(18) . ?
NB1 CL3 2.3452(17) . ?
NB1 CL4 2.3457(17) . ?
NB1 CL1 2.3641(18) . ?
O1 B17 1.406(8) . ?
O1 C1 1.480(7) . ?
O2 B17 1.342(8) . ?
O2 C3 1.459(7) . ?
O3 B13 1.398(8) . ?
O3 C6 1.492(7) . ?
O4 B13 1.344(8) . ?
O4 C8 1.451(7) . ?
C1 C2 1.516(9) . ?
C1 H9A 0.9900 . ?
C1 H9B 0.9900 . ?
C2 C4 1.521(9) . ?
C2 C3 1.527(8) . ?
C2 C5 1.530(8) . ?
C3 H7A 0.9900 . ?
C3 H7B 0.9900 . ?
C4 H15A 0.9800 . ?
C4 H15B 0.9800 . ?
C4 H15C 0.9800 . ?
C5 H12A 0.9800 . ?
C5 H12B 0.9800 . ?
C5 H12C 0.9800 . ?
C6 C7 1.530(8) . ?
C6 H5A 0.9900 . ?
C6 H5B 0.9900 . ?
C7 C8 1.528(9) . ?
C7 C9 1.529(8) . ?
C7 C10 1.536(9) . ?
C8 H14A 0.9900 . ?
C8 H14B 0.9900 . ?
C9 H10A 0.9800 . ?
C9 H10B 0.9800 . ?
C9 H10C 0.9800 . ?
C10 H11A 0.9800 . ?
C10 H11B 0.9800 . ?
C10 H11C 0.9800 . ?
B13 B17 1.718(11) . ?

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 NB1 O3 80.33(15) . . ?
O1 NB1 CL2 83.46(12) . . ?
O3 NB1 CL2 84.87(12) . . ?
O1 NB1 CL3 91.24(12) . . ?
O3 NB1 CL3 171.32(11) . . ?
CL2 NB1 CL3 96.28(6) . . ?
O1 NB1 CL4 174.53(12) . . ?
O3 NB1 CL4 94.25(11) . . ?
CL2 NB1 CL4 95.43(6) . . ?
CL3 NB1 CL4 94.20(7) . . ?
O1 NB1 CL1 84.07(12) . . ?
O3 NB1 CL1 81.58(12) . . ?
CL2 NB1 CL1 162.93(6) . . ?
CL3 NB1 CL1 95.60(7) . . ?
CL4 NB1 CL1 95.87(7) . . ?
B17 O1 C1 119.5(5) . . ?
B17 O1 NB1 114.6(4) . . ?
C1 O1 NB1 126.0(3) . . ?
B17 O2 C3 119.8(5) . . ?
B13 O3 C6 119.1(5) . . ?
B13 O3 NB1 114.0(4) . . ?
C6 O3 NB1 126.7(3) . . ?
B13 O4 C8 120.2(5) . . ?
O1 C1 C2 110.8(5) . . ?
O1 C1 H9A 109.5 . . ?
C2 C1 H9A 109.5 . . ?
O1 C1 H9B 109.5 . . ?
C2 C1 H9B 109.5 . . ?
H9A C1 H9B 108.1 . . ?
C1 C2 C4 112.2(5) . . ?
C1 C2 C3 107.6(5) . . ?
C4 C2 C3 110.2(5) . . ?
C1 C2 C5 107.6(5) . . ?
C4 C2 C5 110.8(5) . . ?
C3 C2 C5 108.3(5) . . ?
O2 C3 C2 111.3(5) . . ?
O2 C3 H7A 109.4 . . ?
C2 C3 H7A 109.4 . . ?
O2 C3 H7B 109.4 . . ?
C2 C3 H7B 109.4 . . ?
H7A C3 H7B 108.0 . . ?
C2 C4 H15A 109.5 . . ?
C2 C4 H15B 109.5 . . ?
H15A C4 H15B 109.5 . . ?
C2 C4 H15C 109.5 . . ?
H15A C4 H15C 109.5 . . ?
H15B C4 H15C 109.5 . . ?
C2 C5 H12A 109.5 . . ?
C2 C5 H12B 109.5 . . ?
H12A C5 H12B 109.5 . . ?
C2 C5 H12C 109.5 . . ?
H12A C5 H12C 109.5 . . ?
H12B C5 H12C 109.5 . . ?
O3 C6 C7 109.9(5) . . ?
O3 C6 H5A 109.7 . . ?
C7 C6 H5A 109.7 . . ?
O3 C6 H5B 109.7 . . ?
C7 C6 H5B 109.7 . . ?
H5A C6 H5B 108.2 . . ?
C8 C7 C9 108.4(5) . . ?
C8 C7 C6 107.7(5) . . ?
C9 C7 C6 108.8(5) . . ?
C8 C7 C10 111.3(5) . . ?
C9 C7 C10 109.9(5) . . ?
C6 C7 C10 110.7(5) . . ?
O4 C8 C7 111.5(5) . . ?
O4 C8 H14A 109.3 . . ?
C7 C8 H14A 109.3 . . ?
O4 C8 H14B 109.3 . . ?
C7 C8 H14B 109.3 . . ?
H14A C8 H14B 108.0 . . ?
C7 C9 H10A 109.5 . . ?
C7 C9 H10B 109.5 . . ?
H10A C9 H10B 109.5 . . ?
C7 C9 H10C 109.5 . . ?
H10A C9 H10C 109.5 . . ?
H10B C9 H10C 109.5 . . ?
C7 C10 H11A 109.5 . . ?
C7 C10 H11B 109.5 . . ?
H11A C10 H11B 109.5 . . ?
C7 C10 H11C 109.5 . . ?
H11A C10 H11C 109.5 . . ?
H11B C10 H11C 109.5 . . ?
O4 B13 O3 123.0(6) . . ?
O4 B13 B17 121.1(6) . . ?
O3 B13 B17 115.8(6) . . ?
O2 B17 O1 122.4(6) . . ?
O2 B17 B13 122.5(6) . . ?
O1 B17 B13 115.1(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
B17 O1 C1 C2 24.7(8) . . . . ?
NB1 O1 C1 C2 -155.1(4) . . . . ?
O1 C1 C2 C4 66.8(7) . . . . ?
O1 C1 C2 C3 -54.6(7) . . . . ?
O1 C1 C2 C5 -171.1(5) . . . . ?
B17 O2 C3 C2 -30.0(8) . . . . ?
C1 C2 C3 O2 57.9(7) . . . . ?
C4 C2 C3 O2 -64.7(7) . . . . ?
C5 C2 C3 O2 174.0(5) . . . . ?
B13 O3 C6 C7 29.1(8) . . . . ?
NB1 O3 C6 C7 -145.1(4) . . . . ?
O3 C6 C7 C8 -55.7(7) . . . . ?
O3 C6 C7 C9 -173.0(5) . . . . ?
O3 C6 C7 C10 66.1(7) . . . . ?
B13 O4 C8 C7 -30.5(8) . . . . ?
C9 C7 C8 O4 174.7(5) . . . . ?
C6 C7 C8 O4 57.2(7) . . . . ?
C10 C7 C8 O4 -64.3(7) . . . . ?
C8 O4 B13 O3 0.9(10) . . . . ?
C8 O4 B13 B17 178.4(6) . . . . ?
C6 O3 B13 O4 -0.4(9) . . . . ?
NB1 O3 B13 O4 174.5(5) . . . . ?
C6 O3 B13 B17 -178.0(5) . . . . ?
NB1 O3 B13 B17 -3.1(7) . . . . ?
C3 O2 B17 O1 -2.9(9) . . . . ?
C3 O2 B17 B13 178.2(6) . . . . ?
C1 O1 B17 O2 5.8(9) . . . . ?
NB1 O1 B17 O2 -174.4(5) . . . . ?
C1 O1 B17 B13 -175.3(5) . . . . ?
NB1 O1 B17 B13 4.6(7) . . . . ?
O4 B13 B17 O2 0.4(10) . . . . ?
O3 B13 B17 O2 178.0(6) . . . . ?
O4 B13 B17 O1 -178.6(6) . . . . ?
O3 B13 B17 O1 -1.0(9) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy15029-Ti2-1
_database_code_depnum_ccdc_archive 'CCDC 2162485'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C32 H52 B4 Cl6 O8 Ti2'
_chemical_formula_moiety         'C20 H40 B4 Cl6 O8 Ti2, 2(C6 H6)'
_chemical_formula_weight         916.52
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   11.301(2)
_cell_length_b                   11.476(2)
_cell_length_c                   16.502(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.560(6)
_cell_angle_gamma                90.0000
_cell_volume                     2130.1(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7981
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948.00
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_T_max  0.820

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            20161
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         3.050
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4868
_reflns_number_gt                4289
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0944
_refine_ls_wR_factor_gt          0.0934
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4868
_refine_ls_number_parameters     235
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0561P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
TI1 Ti 0.51880(2) 0.38830(2) 0.56853(2) 0.01265(9) Uani 1 1 d . . . . .
CL2 Cl 0.35585(3) 0.45009(3) 0.46985(2) 0.01541(10) Uani 1 1 d . . . . .
CL3 Cl 0.44722(3) 0.49438(3) 0.67230(2) 0.01886(10) Uani 1 1 d . . . . .
CL4 Cl 0.59073(3) 0.26239(3) 0.47448(2) 0.01871(10) Uani 1 1 d . . . . .
O1 O 0.66246(9) 0.31671(9) 0.65069(6) 0.0156(2) Uani 1 1 d . . . . .
O2 O 0.42116(9) 0.24206(8) 0.61148(6) 0.0148(2) Uani 1 1 d . . . . .
O3 O 0.45704(10) 0.05063(9) 0.66707(7) 0.0200(2) Uani 1 1 d . . . . .
O4 O 0.73150(10) 0.12092(9) 0.67838(7) 0.0217(2) Uani 1 1 d . . . . .
C5 C 0.27067(13) 0.09018(13) 0.57964(9) 0.0167(3) Uani 1 1 d . . . . .
C6 C 0.78512(13) 0.36015(14) 0.65208(9) 0.0179(3) Uani 1 1 d . . . . .
H6A H 0.788832 0.441042 0.673028 0.021 Uiso 1 1 calc R U . . .
H6B H 0.808960 0.361264 0.595917 0.021 Uiso 1 1 calc R U . . .
C7 C 0.87140(13) 0.28438(13) 0.70536(9) 0.0170(3) Uani 1 1 d . . . . .
C8 C 0.29326(13) 0.21878(13) 0.59950(9) 0.0168(3) Uani 1 1 d . . . . .
H8A H 0.256503 0.267530 0.554370 0.020 Uiso 1 1 calc R U . . .
H8B H 0.256208 0.239484 0.649518 0.020 Uiso 1 1 calc R U . . .
C9 C 0.33320(14) 0.01844(13) 0.64902(9) 0.0192(3) Uani 1 1 d . . . . .
H9A H 0.291367 0.029340 0.698486 0.023 Uiso 1 1 calc R U . . .
H9B H 0.328333 -0.065146 0.634231 0.023 Uiso 1 1 calc R U . . .
C10 C 0.51160(16) 0.28226(15) 0.83794(10) 0.0245(3) Uani 1 1 d . . . . .
H10 H 0.555683 0.344188 0.817263 0.029 Uiso 1 1 calc R U . . .
C11 C 0.38953(15) 0.27696(15) 0.81950(9) 0.0244(3) Uani 1 1 d . . . . .
H11 H 0.350089 0.334929 0.785798 0.029 Uiso 1 1 calc R U . . .
C12 C 0.85386(14) 0.15847(14) 0.67699(10) 0.0227(3) Uani 1 1 d . . . . .
H12A H 0.877173 0.151073 0.620914 0.027 Uiso 1 1 calc R U . . .
H12B H 0.906288 0.107011 0.712740 0.027 Uiso 1 1 calc R U . . .
C13 C 0.31707(16) 0.05889(14) 0.49829(9) 0.0236(3) Uani 1 1 d . . . . .
H13A H 0.275695 0.105960 0.454800 0.028 Uiso 1 1 calc R U . . .
H13B H 0.402614 0.074617 0.501245 0.028 Uiso 1 1 calc R U . . .
H13C H 0.302610 -0.023928 0.486734 0.028 Uiso 1 1 calc R U . . .
C14 C 0.32477(16) 0.18730(16) 0.85011(10) 0.0279(4) Uani 1 1 d . . . . .
H14 H 0.240987 0.183994 0.837621 0.034 Uiso 1 1 calc R U . . .
C15 C 0.99835(14) 0.32187(15) 0.69255(10) 0.0234(3) Uani 1 1 d . . . . .
H15A H 1.055144 0.273816 0.726508 0.028 Uiso 1 1 calc R U . . .
H15B H 1.011614 0.311828 0.635158 0.028 Uiso 1 1 calc R U . . .
H15C H 1.009490 0.403954 0.707804 0.028 Uiso 1 1 calc R U . . .
C16 C 0.13710(14) 0.06722(14) 0.57592(10) 0.0243(3) Uani 1 1 d . . . . .
H16A H 0.095946 0.112841 0.531556 0.029 Uiso 1 1 calc R U . . .
H16B H 0.121709 -0.015892 0.566155 0.029 Uiso 1 1 calc R U . . .
H16C H 0.107945 0.089970 0.627667 0.029 Uiso 1 1 calc R U . . .
C17 C 0.85105(15) 0.29719(16) 0.79490(9) 0.0247(4) Uani 1 1 d . . . . .
H17A H 0.907496 0.247701 0.828004 0.030 Uiso 1 1 calc R U . . .
H17B H 0.862912 0.378683 0.811479 0.030 Uiso 1 1 calc R U . . .
H17C H 0.769665 0.273419 0.802768 0.030 Uiso 1 1 calc R U . . .
C18 C 0.56949(16) 0.19724(16) 0.88654(10) 0.0289(4) Uani 1 1 d . . . . .
H18 H 0.653229 0.200695 0.899216 0.035 Uiso 1 1 calc R U . . .
C20 C 0.38217(18) 0.10292(17) 0.89871(12) 0.0347(4) Uani 1 1 d . . . . .
H20 H 0.337829 0.041705 0.920037 0.042 Uiso 1 1 calc R U . . .
C22 C 0.50476(18) 0.10731(17) 0.91653(11) 0.0341(4) Uani 1 1 d . . . . .
H22 H 0.544256 0.048450 0.949371 0.041 Uiso 1 1 calc R U . . .
B21 B 0.64248(16) 0.19655(15) 0.66206(10) 0.0173(3) Uani 1 1 d . . . . .
B23 B 0.49680(15) 0.15631(15) 0.64868(10) 0.0171(3) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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
TI1 O2 2.1652(10) . ?
TI1 O1 2.1730(10) . ?
TI1 CL3 2.3103(4) . ?
TI1 CL4 2.3241(4) . ?
TI1 CL2 2.4423(4) . ?
TI1 CL2 2.4539(4) 3_666 ?
CL2 TI1 2.4539(4) 3_666 ?
O1 B21 1.413(2) . ?
O1 C6 1.4712(17) . ?
O2 B23 1.4050(19) . ?
O2 C8 1.4643(17) . ?
O3 B23 1.338(2) . ?
O3 C9 1.4502(18) . ?
O4 B21 1.336(2) . ?
O4 C12 1.4508(19) . ?
C5 C9 1.527(2) . ?
C5 C16 1.528(2) . ?
C5 C8 1.528(2) . ?
C5 C13 1.530(2) . ?
C6 C7 1.521(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C17 1.524(2) . ?
C7 C12 1.526(2) . ?
C7 C15 1.532(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.385(2) . ?
C10 C18 1.386(2) . ?
C10 H10 0.9500 . ?
C11 C14 1.386(2) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C20 1.379(3) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C22 1.384(3) . ?
C18 H18 0.9500 . ?
C20 C22 1.389(3) . ?
C20 H20 0.9500 . ?
C22 H22 0.9500 . ?
B21 B23 1.703(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
O2 TI1 O1 82.90(4) . . ?
O2 TI1 CL3 86.54(3) . . ?
O1 TI1 CL3 91.77(3) . . ?
O2 TI1 CL4 87.65(3) . . ?
O1 TI1 CL4 83.87(3) . . ?
CL3 TI1 CL4 173.125(17) . . ?
O2 TI1 CL2 93.90(3) . . ?
O1 TI1 CL2 174.41(3) . . ?
CL3 TI1 CL2 92.617(15) . . ?
CL4 TI1 CL2 91.442(15) . . ?
O2 TI1 CL2 174.61(3) . 3_666 ?
O1 TI1 CL2 91.82(3) . 3_666 ?
CL3 TI1 CL2 92.600(15) . 3_666 ?
CL4 TI1 CL2 92.842(15) . 3_666 ?
CL2 TI1 CL2 91.451(14) . 3_666 ?
TI1 CL2 TI1 88.549(14) . 3_666 ?
B21 O1 C6 119.42(12) . . ?
B21 O1 TI1 109.42(9) . . ?
C6 O1 TI1 121.84(8) . . ?
B23 O2 C8 118.82(11) . . ?
B23 O2 TI1 112.21(9) . . ?
C8 O2 TI1 128.67(8) . . ?
B23 O3 C9 121.52(12) . . ?
B21 O4 C12 120.27(12) . . ?
C9 C5 C16 108.71(12) . . ?
C9 C5 C8 107.72(12) . . ?
C16 C5 C8 108.61(13) . . ?
C9 C5 C13 111.00(13) . . ?
C16 C5 C13 110.21(13) . . ?
C8 C5 C13 110.51(13) . . ?
O1 C6 C7 111.44(12) . . ?
O1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
O1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C17 110.90(13) . . ?
C6 C7 C12 107.88(12) . . ?
C17 C7 C12 111.19(13) . . ?
C6 C7 C15 108.43(12) . . ?
C17 C7 C15 109.75(12) . . ?
C12 C7 C15 108.61(13) . . ?
O2 C8 C5 110.33(12) . . ?
O2 C8 H8A 109.6 . . ?
C5 C8 H8A 109.6 . . ?
O2 C8 H8B 109.6 . . ?
C5 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
O3 C9 C5 112.58(12) . . ?
O3 C9 H9A 109.1 . . ?
C5 C9 H9A 109.1 . . ?
O3 C9 H9B 109.1 . . ?
C5 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C18 120.03(16) . . ?
C11 C10 H10 120.0 . . ?
C18 C10 H10 120.0 . . ?
C10 C11 C14 120.16(16) . . ?
C10 C11 H11 119.9 . . ?
C14 C11 H11 119.9 . . ?
O4 C12 C7 111.85(12) . . ?
O4 C12 H12A 109.2 . . ?
C7 C12 H12A 109.2 . . ?
O4 C12 H12B 109.2 . . ?
C7 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C5 C13 H13A 109.5 . . ?
C5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C20 C14 C11 119.87(17) . . ?
C20 C14 H14 120.1 . . ?
C11 C14 H14 120.1 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 C16 H16A 109.5 . . ?
C5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C7 C17 H17A 109.5 . . ?
C7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C18 C10 119.71(17) . . ?
C22 C18 H18 120.1 . . ?
C10 C18 H18 120.1 . . ?
C14 C20 C22 120.06(17) . . ?
C14 C20 H20 120.0 . . ?
C22 C20 H20 120.0 . . ?
C18 C22 C20 120.16(17) . . ?
C18 C22 H22 119.9 . . ?
C20 C22 H22 119.9 . . ?
O4 B21 O1 122.27(14) . . ?
O4 B21 B23 123.32(14) . . ?
O1 B21 B23 114.35(13) . . ?
O3 B23 O2 122.02(14) . . ?
O3 B23 B21 123.90(14) . . ?
O2 B23 B21 113.97(13) . . ?

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
B21 O1 C6 C7 -28.49(17) . . . . ?
TI1 O1 C6 C7 -171.57(9) . . . . ?
O1 C6 C7 C17 -68.91(16) . . . . ?
O1 C6 C7 C12 53.08(16) . . . . ?
O1 C6 C7 C15 170.53(12) . . . . ?
B23 O2 C8 C5 -35.56(16) . . . . ?
TI1 O2 C8 C5 137.67(10) . . . . ?
C9 C5 C8 O2 56.91(15) . . . . ?
C16 C5 C8 O2 174.48(11) . . . . ?
C13 C5 C8 O2 -64.50(15) . . . . ?
B23 O3 C9 C5 24.15(19) . . . . ?
C16 C5 C9 O3 -169.23(12) . . . . ?
C8 C5 C9 O3 -51.72(16) . . . . ?
C13 C5 C9 O3 69.38(16) . . . . ?
C18 C10 C11 C14 0.5(2) . . . . ?
B21 O4 C12 C7 33.57(19) . . . . ?
C6 C7 C12 O4 -56.01(16) . . . . ?
C17 C7 C12 O4 65.80(16) . . . . ?
C15 C7 C12 O4 -173.34(12) . . . . ?
C10 C11 C14 C20 -0.3(2) . . . . ?
C11 C10 C18 C22 -0.1(3) . . . . ?
C11 C14 C20 C22 -0.4(3) . . . . ?
C10 C18 C22 C20 -0.7(3) . . . . ?
C14 C20 C22 C18 0.9(3) . . . . ?
C12 O4 B21 O1 -6.2(2) . . . . ?
C12 O4 B21 B23 170.74(13) . . . . ?
C6 O1 B21 O4 3.6(2) . . . . ?
TI1 O1 B21 O4 150.81(12) . . . . ?
C6 O1 B21 B23 -173.62(11) . . . . ?
TI1 O1 B21 B23 -26.39(14) . . . . ?
C9 O3 B23 O2 0.4(2) . . . . ?
C9 O3 B23 B21 -175.53(13) . . . . ?
C8 O2 B23 O3 5.8(2) . . . . ?
TI1 O2 B23 O3 -168.47(11) . . . . ?
C8 O2 B23 B21 -177.85(11) . . . . ?
TI1 O2 B23 B21 7.85(15) . . . . ?
O4 B21 B23 O3 12.2(2) . . . . ?
O1 B21 B23 O3 -170.64(13) . . . . ?
O4 B21 B23 O2 -164.04(14) . . . . ?
O1 B21 B23 O2 13.12(18) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy11008-Zr-1
_database_code_depnum_ccdc_archive 'CCDC 2162478'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C12 H24 B2 Cl4 O4 Zr'
_chemical_formula_moiety         'C12 H24 B2 Cl4 O4 Zr'
_chemical_formula_weight         486.97
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
_space_group_IT_number           4
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   14.112(3)
_cell_length_b                   10.1415(18)
_cell_length_c                   15.181(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.990(4)
_cell_angle_gamma                90.0000
_cell_volume                     2041.8(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3434
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984.00
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.979

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            39364
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         3.072
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             9287
_reflns_number_gt                7367
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_max     0.979
_reflns_Friedel_fraction_full    0.991

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1372
_refine_ls_wR_factor_gt          0.1233
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9287
_refine_ls_number_parameters     431
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0599P)²+4.7744P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.33
_refine_diff_density_min         -1.03
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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)

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)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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 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_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_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) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy11007-Ti-1
_database_code_depnum_ccdc_archive 'CCDC 2269213'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C12 H24 B2 Cl4 O4 Ti'
_chemical_formula_moiety         'C12 H24 B2 Cl4 O4 Ti'
_chemical_formula_weight         443.65
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
_space_group_IT_number           4
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   13.978(2)
_cell_length_b                   10.0266(13)
_cell_length_c                   14.979(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.049(3)
_cell_angle_gamma                90.0000
_cell_volume                     1972.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6129
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912.00
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.990

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            43249
_diffrn_reflns_av_R_equivalents  0.2855
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         3.103
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8978
_reflns_number_gt                8189
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_max     0.981
_reflns_Friedel_fraction_full    0.995

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0966
_refine_ls_wR_factor_ref         0.2156
_refine_ls_wR_factor_gt          0.2115
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         8978
_refine_ls_number_parameters     431
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1452P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.69
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 2686 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(6)

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)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
TI1 Ti 0.12708(10) 0.67261(13) 0.21570(9) 0.0149(3) Uani 1 1 d . . . . .
TI2 Ti 0.65003(10) 0.66483(13) 0.21315(9) 0.0147(3) Uani 1 1 d . . . . .
CL1 Cl 0.20760(18) 0.7935(2) 0.13583(15) 0.0262(5) Uani 1 1 d . . . . .
CL2 Cl 0.05844(16) 0.84658(19) 0.26221(15) 0.0231(4) Uani 1 1 d . . . . .
CL3 Cl -0.00832(16) 0.6180(2) 0.09368(14) 0.0247(4) Uani 1 1 d . . . . .
CL4 Cl 0.08768(14) 0.52250(18) 0.31687(13) 0.0182(4) Uani 1 1 d . . . . .
CL5 Cl 0.52767(15) 0.6295(2) 0.07579(13) 0.0239(4) Uani 1 1 d . . . . .
CL6 Cl 0.57338(14) 0.54400(18) 0.30214(13) 0.0184(4) Uani 1 1 d . . . . .
CL7 Cl 0.76670(15) 0.7438(2) 0.15332(14) 0.0215(4) Uani 1 1 d . . . . .
CL8 Cl 0.59324(15) 0.86212(19) 0.24021(15) 0.0223(4) Uani 1 1 d . . . . .
O1 O 0.2746(4) 0.6819(5) 0.3403(4) 0.0154(10) Uani 1 1 d . . . . .
O2 O 0.3919(4) 0.5539(5) 0.4530(4) 0.0175(11) Uani 1 1 d . . . . .
O3 O 0.2145(4) 0.4970(5) 0.1915(4) 0.0155(11) Uani 1 1 d . . . . .
O4 O 0.3096(5) 0.3176(6) 0.2660(4) 0.0197(12) Uani 1 1 d . . . . .
O5 O 0.7827(4) 0.6649(6) 0.3511(4) 0.0145(10) Uani 1 1 d . . . . .
O6 O 0.8985(4) 0.5365(5) 0.4632(4) 0.0163(11) Uani 1 1 d . . . . .
O7 O 0.7222(4) 0.4649(5) 0.2033(4) 0.0149(10) Uani 1 1 d . . . . .
O8 O 0.8285(4) 0.2993(6) 0.2856(4) 0.0176(11) Uani 1 1 d . . . . .
C1 C 0.3439(6) 0.7782(8) 0.4111(5) 0.0163(15) Uani 1 1 d . . . . .
C2 C 0.2844(7) 0.8952(9) 0.4301(7) 0.0281(19) Uani 1 1 d . . . . .
H2A H 0.257549 0.949575 0.372461 0.034 Uiso 1 1 calc R U . . .
H2B H 0.329419 0.949714 0.481738 0.034 Uiso 1 1 calc R U . . .
H2C H 0.227736 0.861737 0.448214 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4197(7) 0.8252(9) 0.3669(7) 0.0263(18) Uani 1 1 d . . . . .
H3A H 0.384021 0.872574 0.307624 0.032 Uiso 1 1 calc R U . . .
H3B H 0.455790 0.748187 0.353471 0.032 Uiso 1 1 calc R U . . .
H3C H 0.468840 0.885412 0.410996 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3894(6) 0.6844(8) 0.4977(6) 0.0184(15) Uani 1 1 d . . . . .
C5 C 0.3218(7) 0.6669(10) 0.5565(6) 0.0286(18) Uani 1 1 d . . . . .
H5A H 0.345188 0.590108 0.598848 0.034 Uiso 1 1 calc R U . . .
H5B H 0.251546 0.651718 0.514346 0.034 Uiso 1 1 calc R U . . .
H5C H 0.324634 0.747399 0.594363 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4975(7) 0.7205(9) 0.5606(6) 0.0250(18) Uani 1 1 d . . . . .
H6A H 0.541880 0.721949 0.522231 0.030 Uiso 1 1 calc R U . . .
H6B H 0.522610 0.654061 0.611272 0.030 Uiso 1 1 calc R U . . .
H6C H 0.497421 0.808725 0.588764 0.030 Uiso 1 1 calc R U . . .
C7 C 0.2258(6) 0.4082(8) 0.1141(5) 0.0159(15) Uani 1 1 d . . . . .
C8 C 0.3146(6) 0.4667(8) 0.0902(6) 0.0200(16) Uani 1 1 d . . . . .
H8A H 0.298389 0.558499 0.067554 0.024 Uiso 1 1 calc R U . . .
H8B H 0.326686 0.412936 0.040479 0.024 Uiso 1 1 calc R U . . .
H8C H 0.375846 0.466445 0.147170 0.024 Uiso 1 1 calc R U . . .
C9 C 0.1297(6) 0.4073(9) 0.0280(6) 0.0224(16) Uani 1 1 d . . . . .
H9A H 0.118208 0.496402 -0.000709 0.027 Uiso 1 1 calc R U . . .
H9B H 0.071749 0.382416 0.047152 0.027 Uiso 1 1 calc R U . . .
H9C H 0.136714 0.342656 -0.018453 0.027 Uiso 1 1 calc R U . . .
C10 C 0.2510(6) 0.2740(8) 0.1688(6) 0.0188(16) Uani 1 1 d . . . . .
C11 C 0.1587(7) 0.2007(8) 0.1745(6) 0.0254(18) Uani 1 1 d . . . . .
H11A H 0.119578 0.260101 0.201047 0.031 Uiso 1 1 calc R U . . .
H11B H 0.180813 0.122317 0.215474 0.031 Uiso 1 1 calc R U . . .
H11C H 0.115930 0.172332 0.110702 0.031 Uiso 1 1 calc R U . . .
C12 C 0.3185(7) 0.1817(9) 0.1353(7) 0.0279(18) Uani 1 1 d . . . . .
H12A H 0.327547 0.097097 0.169995 0.033 Uiso 1 1 calc R U . . .
H12B H 0.384972 0.223801 0.147291 0.033 Uiso 1 1 calc R U . . .
H12C H 0.286246 0.164821 0.067069 0.033 Uiso 1 1 calc R U . . .
C13 C 0.8205(6) 0.7525(7) 0.4385(5) 0.0154(14) Uani 1 1 d . . . . .
C14 C 0.8450(7) 0.8901(8) 0.4081(6) 0.0209(16) Uani 1 1 d . . . . .
H14A H 0.781611 0.935341 0.371386 0.025 Uiso 1 1 calc R U . . .
H14B H 0.888082 0.880136 0.368874 0.025 Uiso 1 1 calc R U . . .
H14C H 0.881145 0.942997 0.464670 0.025 Uiso 1 1 calc R U . . .
C15 C 0.7365(6) 0.7596(8) 0.4805(6) 0.0194(15) Uani 1 1 d . . . . .
H15A H 0.721177 0.669597 0.497304 0.023 Uiso 1 1 calc R U . . .
H15B H 0.675331 0.798206 0.433768 0.023 Uiso 1 1 calc R U . . .
H15C H 0.758532 0.815507 0.537591 0.023 Uiso 1 1 calc R U . . .
C16 C 0.9171(6) 0.6740(7) 0.5012(5) 0.0135(13) Uani 1 1 d . . . . .
C17 C 1.0151(6) 0.7191(8) 0.4882(6) 0.0185(15) Uani 1 1 d . . . . .
H17A H 1.029913 0.811372 0.510233 0.022 Uiso 1 1 calc R U . . .
H17B H 1.007603 0.713835 0.420819 0.022 Uiso 1 1 calc R U . . .
H17C H 1.071193 0.661222 0.525226 0.022 Uiso 1 1 calc R U . . .
C18 C 0.9303(6) 0.6666(8) 0.6062(5) 0.0200(15) Uani 1 1 d . . . . .
H18A H 0.988273 0.608773 0.638962 0.024 Uiso 1 1 calc R U . . .
H18B H 0.868378 0.630047 0.613451 0.024 Uiso 1 1 calc R U . . .
H18C H 0.942906 0.756234 0.633916 0.024 Uiso 1 1 calc R U . . .
C19 C 0.6939(6) 0.3425(8) 0.1404(5) 0.0161(15) Uani 1 1 d . . . . .
C20 C 0.5989(6) 0.2833(9) 0.1532(6) 0.0232(17) Uani 1 1 d . . . . .
H20A H 0.582826 0.197731 0.119692 0.028 Uiso 1 1 calc R U . . .
H20B H 0.541541 0.344741 0.127006 0.028 Uiso 1 1 calc R U . . .
H20C H 0.611263 0.269358 0.220954 0.028 Uiso 1 1 calc R U . . .
C21 C 0.6760(6) 0.3805(9) 0.0380(5) 0.0204(16) Uani 1 1 d . . . . .
H21A H 0.672788 0.299593 0.000368 0.024 Uiso 1 1 calc R U . . .
H21B H 0.732064 0.437048 0.035103 0.024 Uiso 1 1 calc R U . . .
H21C H 0.611667 0.429388 0.012359 0.024 Uiso 1 1 calc R U . . .
C22 C 0.7925(6) 0.2572(8) 0.1853(5) 0.0148(14) Uani 1 1 d . . . . .
C23 C 0.8769(7) 0.2892(9) 0.1466(6) 0.0235(17) Uani 1 1 d . . . . .
H23A H 0.939698 0.244345 0.185272 0.028 Uiso 1 1 calc R U . . .
H23B H 0.888075 0.385788 0.148694 0.028 Uiso 1 1 calc R U . . .
H23C H 0.857362 0.258094 0.080700 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7728(7) 0.1067(8) 0.1818(6) 0.0245(17) Uani 1 1 d . . . . .
H24A H 0.723671 0.086527 0.213425 0.029 Uiso 1 1 calc R U . . .
H24B H 0.836814 0.059730 0.214191 0.029 Uiso 1 1 calc R U . . .
H24C H 0.745281 0.077425 0.115369 0.029 Uiso 1 1 calc R U . . .
B1 B 0.3199(7) 0.5571(9) 0.3657(6) 0.0154(16) Uani 1 1 d . . . . .
B2 B 0.2824(7) 0.4439(9) 0.2757(6) 0.0172(16) Uani 1 1 d . . . . .
B3 B 0.8296(6) 0.5408(9) 0.3748(6) 0.0148(16) Uani 1 1 d . . . . .
B4 B 0.7947(7) 0.4249(9) 0.2886(6) 0.0160(16) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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
TI1 CL3 2.202(2) . ?
TI1 CL2 2.215(2) . ?
TI1 O3 2.242(5) . ?
TI1 CL1 2.256(2) . ?
TI1 O1 2.260(5) . ?
TI1 CL4 2.332(2) . ?
TI2 CL5 2.207(2) . ?
TI2 CL8 2.220(2) . ?
TI2 O5 2.254(5) . ?
TI2 CL7 2.257(2) . ?
TI2 O7 2.271(5) . ?
TI2 CL6 2.318(2) . ?
O1 B1 1.395(10) . ?
O1 C1 1.514(9) . ?
O2 B1 1.350(10) . ?
O2 C4 1.476(9) . ?
O3 B2 1.398(10) . ?
O3 C7 1.513(8) . ?
O4 B2 1.345(11) . ?
O4 C10 1.471(9) . ?
O5 B3 1.394(10) . ?
O5 C13 1.514(9) . ?
O6 B3 1.344(10) . ?
O6 C16 1.480(9) . ?
O7 B4 1.391(10) . ?
O7 C19 1.515(9) . ?
O8 B4 1.351(11) . ?
O8 C22 1.473(8) . ?
C1 C3 1.505(11) . ?
C1 C2 1.520(11) . ?
C1 C4 1.551(11) . ?
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 C5 1.507(11) . ?
C4 C6 1.524(11) . ?
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 1.511(11) . ?
C7 C8 1.522(10) . ?
C7 C10 1.551(11) . ?
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 1.512(11) . ?
C10 C12 1.524(11) . ?
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 1.512(10) . ?
C13 C14 1.527(10) . ?
C13 C16 1.566(10) . ?
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 1.518(10) . ?
C16 C18 1.521(10) . ?
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 1.516(10) . ?
C19 C20 1.526(10) . ?
C19 C22 1.564(11) . ?
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 1.517(11) . ?
C22 C24 1.531(11) . ?
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 1.701(12) . ?
B3 B4 1.681(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
CL3 TI1 CL2 96.60(9) . . ?
CL3 TI1 O3 91.82(16) . . ?
CL2 TI1 O3 171.09(16) . . ?
CL3 TI1 CL1 97.84(10) . . ?
CL2 TI1 CL1 95.30(9) . . ?
O3 TI1 CL1 86.40(15) . . ?
CL3 TI1 O1 167.69(16) . . ?
CL2 TI1 O1 94.52(15) . . ?
O3 TI1 O1 76.8(2) . . ?
CL1 TI1 O1 86.34(15) . . ?
CL3 TI1 CL4 92.97(9) . . ?
CL2 TI1 CL4 94.57(8) . . ?
O3 TI1 CL4 82.06(14) . . ?
CL1 TI1 CL4 164.42(10) . . ?
O1 TI1 CL4 80.88(15) . . ?
CL5 TI2 CL8 95.84(9) . . ?
CL5 TI2 O5 170.29(16) . . ?
CL8 TI2 O5 93.77(16) . . ?
CL5 TI2 CL7 96.93(9) . . ?
CL8 TI2 CL7 96.44(9) . . ?
O5 TI2 CL7 83.36(14) . . ?
CL5 TI2 O7 90.99(15) . . ?
CL8 TI2 O7 173.12(16) . . ?
O5 TI2 O7 79.4(2) . . ?
CL7 TI2 O7 83.49(15) . . ?
CL5 TI2 CL6 95.11(9) . . ?
CL8 TI2 CL6 95.51(8) . . ?
O5 TI2 CL6 82.55(14) . . ?
CL7 TI2 CL6 162.06(9) . . ?
O7 TI2 CL6 83.05(15) . . ?
B1 O1 C1 105.1(6) . . ?
B1 O1 TI1 112.9(5) . . ?
C1 O1 TI1 142.0(4) . . ?
B1 O2 C4 107.1(6) . . ?
B2 O3 C7 104.5(6) . . ?
B2 O3 TI1 113.1(5) . . ?
C7 O3 TI1 142.4(4) . . ?
B2 O4 C10 107.7(6) . . ?
B3 O5 C13 107.6(5) . . ?
B3 O5 TI2 113.6(4) . . ?
C13 O5 TI2 136.6(4) . . ?
B3 O6 C16 108.7(6) . . ?
B4 O7 C19 106.9(6) . . ?
B4 O7 TI2 113.3(5) . . ?
C19 O7 TI2 136.8(5) . . ?
B4 O8 C22 107.5(6) . . ?
C3 C1 O1 105.7(6) . . ?
C3 C1 C2 110.7(7) . . ?
O1 C1 C2 111.3(6) . . ?
C3 C1 C4 114.1(7) . . ?
O1 C1 C4 100.4(6) . . ?
C2 C1 C4 113.9(7) . . ?
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 C5 106.2(7) . . ?
O2 C4 C6 108.6(6) . . ?
C5 C4 C6 110.7(7) . . ?
O2 C4 C1 103.0(6) . . ?
C5 C4 C1 113.5(7) . . ?
C6 C4 C1 114.1(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 O3 111.2(6) . . ?
C9 C7 C8 111.1(6) . . ?
O3 C7 C8 105.1(6) . . ?
C9 C7 C10 114.9(7) . . ?
O3 C7 C10 99.8(5) . . ?
C8 C7 C10 113.8(7) . . ?
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 106.6(6) . . ?
O4 C10 C12 108.0(7) . . ?
C11 C10 C12 111.1(7) . . ?
O4 C10 C7 102.4(6) . . ?
C11 C10 C7 114.1(7) . . ?
C12 C10 C7 114.0(7) . . ?
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 O5 107.2(6) . . ?
C15 C13 C14 111.5(6) . . ?
O5 C13 C14 108.3(6) . . ?
C15 C13 C16 114.0(6) . . ?
O5 C13 C16 101.6(5) . . ?
C14 C13 C16 113.4(6) . . ?
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 105.9(6) . . ?
O6 C16 C18 107.2(6) . . ?
C17 C16 C18 110.6(6) . . ?
O6 C16 C13 103.7(6) . . ?
C17 C16 C13 113.8(6) . . ?
C18 C16 C13 114.8(6) . . ?
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 . . ?
O7 C19 C21 110.1(6) . . ?
O7 C19 C20 106.8(6) . . ?
C21 C19 C20 112.1(7) . . ?
O7 C19 C22 99.9(6) . . ?
C21 C19 C22 112.8(6) . . ?
C20 C19 C22 114.2(6) . . ?
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 106.9(6) . . ?
O8 C22 C24 108.2(6) . . ?
C23 C22 C24 110.4(7) . . ?
O8 C22 C19 103.0(6) . . ?
C23 C22 C19 113.9(6) . . ?
C24 C22 C19 113.8(6) . . ?
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 113.8(7) . . ?
O2 B1 B2 132.6(7) . . ?
O1 B1 B2 113.3(6) . . ?
O4 B2 O3 113.0(7) . . ?
O4 B2 B1 133.7(7) . . ?
O3 B2 B1 113.0(7) . . ?
O6 B3 O5 113.3(6) . . ?
O6 B3 B4 131.0(7) . . ?
O5 B3 B4 115.7(6) . . ?
O8 B4 O7 113.0(7) . . ?
O8 B4 B3 131.1(7) . . ?
O7 B4 B3 115.8(7) . . ?

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 C3 90.5(7) . . . . ?
TI1 O1 C1 C3 -91.7(8) . . . . ?
B1 O1 C1 C2 -149.3(7) . . . . ?
TI1 O1 C1 C2 28.5(10) . . . . ?
B1 O1 C1 C4 -28.3(7) . . . . ?
TI1 O1 C1 C4 149.5(6) . . . . ?
B1 O2 C4 C5 94.9(7) . . . . ?
B1 O2 C4 C6 -146.0(7) . . . . ?
B1 O2 C4 C1 -24.7(8) . . . . ?
C3 C1 C4 O2 -80.8(8) . . . . ?
O1 C1 C4 O2 31.7(7) . . . . ?
C2 C1 C4 O2 150.8(6) . . . . ?
C3 C1 C4 C5 164.9(7) . . . . ?
O1 C1 C4 C5 -82.6(8) . . . . ?
C2 C1 C4 C5 36.5(10) . . . . ?
C3 C1 C4 C6 36.7(9) . . . . ?
O1 C1 C4 C6 149.2(6) . . . . ?
C2 C1 C4 C6 -91.7(8) . . . . ?
B2 O3 C7 C9 153.5(7) . . . . ?
TI1 O3 C7 C9 -24.2(11) . . . . ?
B2 O3 C7 C8 -86.2(7) . . . . ?
TI1 O3 C7 C8 96.1(8) . . . . ?
B2 O3 C7 C10 31.8(7) . . . . ?
TI1 O3 C7 C10 -145.8(6) . . . . ?
B2 O4 C10 C11 -95.4(8) . . . . ?
B2 O4 C10 C12 145.2(7) . . . . ?
B2 O4 C10 C7 24.6(8) . . . . ?
C9 C7 C10 O4 -152.7(6) . . . . ?
O3 C7 C10 O4 -33.7(7) . . . . ?
C8 C7 C10 O4 77.7(7) . . . . ?
C9 C7 C10 C11 -38.1(9) . . . . ?
O3 C7 C10 C11 81.0(7) . . . . ?
C8 C7 C10 C11 -167.6(7) . . . . ?
C9 C7 C10 C12 91.0(8) . . . . ?
O3 C7 C10 C12 -150.0(7) . . . . ?
C8 C7 C10 C12 -38.6(9) . . . . ?
B3 O5 C13 C15 -103.4(7) . . . . ?
TI2 O5 C13 C15 58.2(8) . . . . ?
B3 O5 C13 C14 136.1(6) . . . . ?
TI2 O5 C13 C14 -62.3(8) . . . . ?
B3 O5 C13 C16 16.5(7) . . . . ?
TI2 O5 C13 C16 178.0(4) . . . . ?
B3 O6 C16 C17 -99.5(7) . . . . ?
B3 O6 C16 C18 142.4(6) . . . . ?
B3 O6 C16 C13 20.6(7) . . . . ?
C15 C13 C16 O6 93.2(7) . . . . ?
O5 C13 C16 O6 -21.8(7) . . . . ?
C14 C13 C16 O6 -137.8(6) . . . . ?
C15 C13 C16 C17 -152.2(6) . . . . ?
O5 C13 C16 C17 92.8(7) . . . . ?
C14 C13 C16 C17 -23.2(9) . . . . ?
C15 C13 C16 C18 -23.4(9) . . . . ?
O5 C13 C16 C18 -138.3(6) . . . . ?
C14 C13 C16 C18 105.7(7) . . . . ?
B4 O7 C19 C21 -143.0(7) . . . . ?
TI2 O7 C19 C21 59.2(8) . . . . ?
B4 O7 C19 C20 95.1(7) . . . . ?
TI2 O7 C19 C20 -62.7(8) . . . . ?
B4 O7 C19 C22 -24.1(7) . . . . ?
TI2 O7 C19 C22 178.2(5) . . . . ?
B4 O8 C22 C23 93.4(7) . . . . ?
B4 O8 C22 C24 -147.6(7) . . . . ?
B4 O8 C22 C19 -26.9(7) . . . . ?
O7 C19 C22 O8 30.1(6) . . . . ?
C21 C19 C22 O8 147.0(6) . . . . ?
C20 C19 C22 O8 -83.6(7) . . . . ?
O7 C19 C22 C23 -85.3(7) . . . . ?
C21 C19 C22 C23 31.6(9) . . . . ?
C20 C19 C22 C23 161.1(6) . . . . ?
O7 C19 C22 C24 147.0(6) . . . . ?
C21 C19 C22 C24 -96.2(8) . . . . ?
C20 C19 C22 C24 33.3(9) . . . . ?
C4 O2 B1 O1 6.7(9) . . . . ?
C4 O2 B1 B2 178.9(8) . . . . ?
C1 O1 B1 O2 14.9(8) . . . . ?
TI1 O1 B1 O2 -163.6(5) . . . . ?
C1 O1 B1 B2 -158.8(6) . . . . ?
TI1 O1 B1 B2 22.7(7) . . . . ?
C10 O4 B2 O3 -4.2(9) . . . . ?
C10 O4 B2 B1 -178.3(9) . . . . ?
C7 O3 B2 O4 -18.8(9) . . . . ?
TI1 O3 B2 O4 159.6(5) . . . . ?
C7 O3 B2 B1 156.5(6) . . . . ?
TI1 O3 B2 B1 -25.0(8) . . . . ?
O2 B1 B2 O4 3.3(16) . . . . ?
O1 B1 B2 O4 175.5(8) . . . . ?
O2 B1 B2 O3 -170.8(8) . . . . ?
O1 B1 B2 O3 1.4(10) . . . . ?
C16 O6 B3 O5 -10.8(8) . . . . ?
C16 O6 B3 B4 166.7(7) . . . . ?
C13 O5 B3 O6 -4.5(8) . . . . ?
TI2 O5 B3 O6 -170.7(5) . . . . ?
C13 O5 B3 B4 177.7(6) . . . . ?
TI2 O5 B3 B4 11.4(8) . . . . ?
C22 O8 B4 O7 12.1(9) . . . . ?
C22 O8 B4 B3 -164.4(8) . . . . ?
C19 O7 B4 O8 8.9(8) . . . . ?
TI2 O7 B4 O8 172.5(5) . . . . ?
C19 O7 B4 B3 -174.0(6) . . . . ?
TI2 O7 B4 B3 -10.4(8) . . . . ?
O6 B3 B4 O8 -1.5(14) . . . . ?
O5 B3 B4 O8 175.8(8) . . . . ?
O6 B3 B4 O7 -178.0(8) . . . . ?
O5 B3 B4 O7 -0.6(10) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_hsy10075-Zr-1
_database_code_depnum_ccdc_archive 'CCDC 2161220'
loop_
_audit_author_name
_audit_author_address
'Hayato Tsurugi'
;Osaka University
Japan
;
_audit_update_record             
;
2023-06-10 deposited with the CCDC.	2023-09-01 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C10 H20 B2 Cl4 O4 Zr'
_chemical_formula_moiety         'C10 H20 B2 Cl4 O4 Zr'
_chemical_formula_weight         458.92
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   13.270(2)
_cell_length_b                   15.036(2)
_cell_length_c                   18.597(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.265(4)
_cell_angle_gamma                90.0000
_cell_volume                     3700.3(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5321
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    113
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840.00
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.977

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      113
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            135638
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         3.079
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8484
_reflns_number_gt                6400
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0691
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         8484
_refine_ls_number_parameters     387
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0432P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.76226(2) 0.81959(2) 0.62540(2) 0.01467(6) Uani 1 1 d . . . . .
ZR2 Zr 0.74193(2) 0.13972(2) 0.36635(2) 0.01452(6) Uani 1 1 d . . . . .
CL1 Cl 0.62373(5) 0.72710(5) 0.65833(3) 0.02738(15) Uani 1 1 d . . . . .
CL2 Cl 0.84394(5) 0.82715(4) 0.74232(3) 0.02375(14) Uani 1 1 d . . . . .
CL3 Cl 0.67353(5) 0.95606(4) 0.62317(4) 0.02769(15) Uani 1 1 d . . . . .
CL4 Cl 0.90321(5) 0.87586(4) 0.56283(3) 0.02320(14) Uani 1 1 d . . . . .
CL5 Cl 0.61481(5) 0.11115(5) 0.44891(3) 0.02555(15) Uani 1 1 d . . . . .
CL6 Cl 0.80425(5) -0.00822(4) 0.36639(3) 0.02394(14) Uani 1 1 d . . . . .
CL7 Cl 0.62785(5) 0.14141(4) 0.26264(4) 0.02744(15) Uani 1 1 d . . . . .
CL8 Cl 0.88378(5) 0.20077(4) 0.30583(3) 0.02228(14) Uani 1 1 d . . . . .
O1 O 0.83356(13) 0.68448(11) 0.60289(8) 0.0163(4) Uani 1 1 d . . . . .
O2 O 0.86206(13) 0.57780(11) 0.51031(8) 0.0186(4) Uani 1 1 d . . . . .
O3 O 0.69938(13) 0.78920(11) 0.50934(8) 0.0176(4) Uani 1 1 d . . . . .
O4 O 0.73124(14) 0.70334(11) 0.40433(9) 0.0212(4) Uani 1 1 d . . . . .
O5 O 0.83789(12) 0.17370(11) 0.46951(8) 0.0164(4) Uani 1 1 d . . . . .
O6 O 0.93540(14) 0.29057(12) 0.52904(10) 0.0250(4) Uani 1 1 d . . . . .
O7 O 0.71719(12) 0.28918(11) 0.38362(9) 0.0178(4) Uani 1 1 d . . . . .
O8 O 0.82652(13) 0.41589(12) 0.40399(9) 0.0239(4) Uani 1 1 d . . . . .
C1 C 0.8889(2) 0.62891(16) 0.65846(12) 0.0182(5) Uani 1 1 d . . . . .
H1A H 0.859780 0.637652 0.705426 0.022 Uiso 1 1 calc R U . . .
H1B H 0.960692 0.647415 0.663764 0.022 Uiso 1 1 calc R U . . .
C2 C 0.88219(19) 0.53118(16) 0.63751(13) 0.0171(5) Uani 1 1 d . . . . .
C3 C 0.9191(2) 0.52156(17) 0.56216(13) 0.0202(5) Uani 1 1 d . . . . .
H3A H 0.991501 0.537758 0.563508 0.024 Uiso 1 1 calc R U . . .
H3B H 0.912349 0.458736 0.546615 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7739(2) 0.49673(19) 0.64042(15) 0.0281(6) Uani 1 1 d . . . . .
H4A H 0.729066 0.528895 0.605114 0.034 Uiso 1 1 calc R U . . .
H4B H 0.751412 0.506214 0.688859 0.034 Uiso 1 1 calc R U . . .
H4C H 0.771854 0.433057 0.629156 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9548(2) 0.47943(17) 0.68961(14) 0.0245(6) Uani 1 1 d . . . . .
H5A H 1.023389 0.502744 0.687235 0.029 Uiso 1 1 calc R U . . .
H5B H 0.953456 0.416382 0.676224 0.029 Uiso 1 1 calc R U . . .
H5C H 0.933969 0.485962 0.738814 0.029 Uiso 1 1 calc R U . . .
C6 C 0.62699(19) 0.84734(16) 0.46680(13) 0.0174(5) Uani 1 1 d . . . . .
H6A H 0.662704 0.900331 0.449924 0.021 Uiso 1 1 calc R U . . .
H6B H 0.573720 0.867766 0.497496 0.021 Uiso 1 1 calc R U . . .
C7 C 0.57906(19) 0.79619(17) 0.40213(13) 0.0200(5) Uani 1 1 d . . . . .
C8 C 0.6629(2) 0.75923(18) 0.35953(13) 0.0224(6) Uani 1 1 d . . . . .
H8A H 0.632894 0.723982 0.318361 0.027 Uiso 1 1 calc R U . . .
H8B H 0.701258 0.809036 0.339977 0.027 Uiso 1 1 calc R U . . .
C9 C 0.5104(2) 0.72223(18) 0.42692(15) 0.0261(6) Uani 1 1 d . . . . .
H9A H 0.458016 0.748120 0.454912 0.031 Uiso 1 1 calc R U . . .
H9B H 0.550711 0.679852 0.457016 0.031 Uiso 1 1 calc R U . . .
H9C H 0.478657 0.691358 0.384710 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5177(2) 0.86311(19) 0.35432(15) 0.0297(7) Uani 1 1 d . . . . .
H10A H 0.467674 0.892206 0.382569 0.036 Uiso 1 1 calc R U . . .
H10B H 0.483093 0.831842 0.313367 0.036 Uiso 1 1 calc R U . . .
H10C H 0.563282 0.908006 0.336521 0.036 Uiso 1 1 calc R U . . .
C11 C 0.86528(19) 0.11064(16) 0.52922(12) 0.0179(5) Uani 1 1 d . . . . .
H11A H 0.926825 0.077190 0.518891 0.021 Uiso 1 1 calc R U . . .
H11B H 0.809747 0.067480 0.533686 0.021 Uiso 1 1 calc R U . . .
C12 C 0.8843(2) 0.16239(17) 0.59949(13) 0.0198(5) Uani 1 1 d . . . . .
C13 C 0.9670(2) 0.23059(18) 0.58790(14) 0.0248(6) Uani 1 1 d . . . . .
H13A H 0.981724 0.265284 0.632693 0.030 Uiso 1 1 calc R U . . .
H13B H 1.029569 0.199379 0.576678 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7873(2) 0.20637(19) 0.62079(14) 0.0273(6) Uani 1 1 d . . . . .
H14A H 0.736160 0.160619 0.627360 0.033 Uiso 1 1 calc R U . . .
H14B H 0.762250 0.247559 0.582707 0.033 Uiso 1 1 calc R U . . .
H14C H 0.801071 0.239176 0.665984 0.033 Uiso 1 1 calc R U . . .
C15 C 0.9247(2) 0.09804(18) 0.65874(13) 0.0254(6) Uani 1 1 d . . . . .
H15A H 0.986409 0.069521 0.644255 0.031 Uiso 1 1 calc R U . . .
H15B H 0.873633 0.052502 0.666125 0.031 Uiso 1 1 calc R U . . .
H15C H 0.939817 0.130970 0.703731 0.031 Uiso 1 1 calc R U . . .
C16 C 0.64474(19) 0.34388(16) 0.33871(14) 0.0189(5) Uani 1 1 d . . . . .
H16A H 0.575625 0.320023 0.341638 0.023 Uiso 1 1 calc R U . . .
H16B H 0.661417 0.340942 0.287759 0.023 Uiso 1 1 calc R U . . .
C17 C 0.6481(2) 0.43987(16) 0.36389(13) 0.0201(5) Uani 1 1 d . . . . .
C18 C 0.7559(2) 0.47253(18) 0.36087(14) 0.0248(6) Uani 1 1 d . . . . .
H18A H 0.774058 0.472699 0.310183 0.030 Uiso 1 1 calc R U . . .
H18B H 0.761117 0.534308 0.379183 0.030 Uiso 1 1 calc R U . . .
C19 C 0.6132(2) 0.4482(2) 0.44037(15) 0.0336(7) Uani 1 1 d . . . . .
H19A H 0.658103 0.413387 0.473794 0.040 Uiso 1 1 calc R U . . .
H19B H 0.543971 0.425820 0.441120 0.040 Uiso 1 1 calc R U . . .
H19C H 0.615316 0.510834 0.455070 0.040 Uiso 1 1 calc R U . . .
C20 C 0.5786(2) 0.49433(18) 0.31154(15) 0.0271(6) Uani 1 1 d . . . . .
H20A H 0.508932 0.473263 0.313164 0.033 Uiso 1 1 calc R U . . .
H20B H 0.599964 0.487450 0.262519 0.033 Uiso 1 1 calc R U . . .
H20C H 0.582357 0.557208 0.325359 0.033 Uiso 1 1 calc R U . . .
B1 B 0.8221(2) 0.65401(19) 0.53101(15) 0.0171(6) Uani 1 1 d . . . . .
B2 B 0.7472(2) 0.71957(19) 0.47532(15) 0.0181(6) Uani 1 1 d . . . . .
B3 B 0.8703(2) 0.2624(2) 0.47546(16) 0.0206(6) Uani 1 1 d . . . . .
B4 B 0.8046(2) 0.33099(19) 0.41558(16) 0.0197(6) Uani 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2016/4 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'

#==============================================================================
# MOLECULAR GEOMETRY

_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 O1 2.2928(16) . ?
ZR1 O3 2.3011(16) . ?
ZR1 CL2 2.3590(7) . ?
ZR1 CL3 2.3645(7) . ?
ZR1 CL1 2.4199(7) . ?
ZR1 CL4 2.4274(7) . ?
ZR2 O5 2.2804(16) . ?
ZR2 O7 2.2971(17) . ?
ZR2 CL7 2.3617(7) . ?
ZR2 CL6 2.3732(7) . ?
ZR2 CL5 2.4027(7) . ?
ZR2 CL8 2.4428(7) . ?
O1 B1 1.411(3) . ?
O1 C1 1.481(3) . ?
O2 B1 1.331(3) . ?
O2 C3 1.452(3) . ?
O3 B2 1.400(3) . ?
O3 C6 1.483(3) . ?
O4 B2 1.344(3) . ?
O4 C8 1.453(3) . ?
O5 B3 1.403(3) . ?
O5 C11 1.485(3) . ?
O6 B3 1.338(3) . ?
O6 C13 1.456(3) . ?
O7 B4 1.411(3) . ?
O7 C16 1.476(3) . ?
O8 B4 1.330(3) . ?
O8 C18 1.461(3) . ?
C1 C2 1.521(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.525(3) . ?
C2 C5 1.527(3) . ?
C2 C4 1.533(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.526(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.518(3) . ?
C7 C9 1.530(4) . ?
C7 C10 1.535(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.526(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.526(4) . ?
C12 C13 1.529(4) . ?
C12 C15 1.533(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
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 1.517(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.517(4) . ?
C17 C20 1.528(3) . ?
C17 C19 1.533(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
B1 B2 1.697(4) . ?
B3 B4 1.709(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 77.21(6) . . ?
O1 ZR1 CL2 92.49(4) . . ?
O3 ZR1 CL2 169.65(4) . . ?
O1 ZR1 CL3 167.81(4) . . ?
O3 ZR1 CL3 90.60(4) . . ?
CL2 ZR1 CL3 99.70(2) . . ?
O1 ZR1 CL1 82.45(5) . . ?
O3 ZR1 CL1 83.91(5) . . ?
CL2 ZR1 CL1 95.74(2) . . ?
CL3 ZR1 CL1 96.69(3) . . ?
O1 ZR1 CL4 83.00(4) . . ?
O3 ZR1 CL4 81.85(5) . . ?
CL2 ZR1 CL4 96.17(3) . . ?
CL3 ZR1 CL4 95.14(3) . . ?
CL1 ZR1 CL4 161.55(2) . . ?
O5 ZR2 O7 74.92(6) . . ?
O5 ZR2 CL7 165.60(5) . . ?
O7 ZR2 CL7 90.81(4) . . ?
O5 ZR2 CL6 92.12(5) . . ?
O7 ZR2 CL6 166.01(4) . . ?
CL7 ZR2 CL6 102.27(2) . . ?
O5 ZR2 CL5 82.94(5) . . ?
O7 ZR2 CL5 88.34(5) . . ?
CL7 ZR2 CL5 94.93(3) . . ?
CL6 ZR2 CL5 95.36(2) . . ?
O5 ZR2 CL8 84.39(4) . . ?
O7 ZR2 CL8 79.62(5) . . ?
CL7 ZR2 CL8 95.09(3) . . ?
CL6 ZR2 CL8 94.12(2) . . ?
CL5 ZR2 CL8 164.42(2) . . ?
B1 O1 C1 119.40(19) . . ?
B1 O1 ZR1 116.36(15) . . ?
C1 O1 ZR1 124.24(13) . . ?
B1 O2 C3 120.54(19) . . ?
B2 O3 C6 119.81(19) . . ?
B2 O3 ZR1 115.32(15) . . ?
C6 O3 ZR1 123.96(13) . . ?
B2 O4 C8 120.3(2) . . ?
B3 O5 C11 119.44(19) . . ?
B3 O5 ZR2 115.35(15) . . ?
C11 O5 ZR2 125.20(13) . . ?
B3 O6 C13 119.8(2) . . ?
B4 O7 C16 118.06(19) . . ?
B4 O7 ZR2 111.91(15) . . ?
C16 O7 ZR2 124.04(13) . . ?
B4 O8 C18 120.6(2) . . ?
O1 C1 C2 110.47(19) . . ?
O1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
O1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 108.1(2) . . ?
C1 C2 C5 107.9(2) . . ?
C3 C2 C5 107.7(2) . . ?
C1 C2 C4 110.8(2) . . ?
C3 C2 C4 111.5(2) . . ?
C5 C2 C4 110.7(2) . . ?
O2 C3 C2 111.6(2) . . ?
O2 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
O2 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 C7 109.81(19) . . ?
O3 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
O3 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C6 108.5(2) . . ?
C8 C7 C9 111.5(2) . . ?
C6 C7 C9 110.6(2) . . ?
C8 C7 C10 108.4(2) . . ?
C6 C7 C10 107.3(2) . . ?
C9 C7 C10 110.4(2) . . ?
O4 C8 C7 111.29(19) . . ?
O4 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
O4 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
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 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 C12 109.30(19) . . ?
O5 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
C14 C12 C11 110.8(2) . . ?
C14 C12 C13 112.0(2) . . ?
C11 C12 C13 107.2(2) . . ?
C14 C12 C15 110.1(2) . . ?
C11 C12 C15 108.7(2) . . ?
C13 C12 C15 108.0(2) . . ?
O6 C13 C12 110.6(2) . . ?
O6 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
O6 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 C17 110.63(19) . . ?
O7 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16 C17 C18 107.6(2) . . ?
C16 C17 C20 108.1(2) . . ?
C18 C17 C20 109.2(2) . . ?
C16 C17 C19 111.1(2) . . ?
C18 C17 C19 111.0(2) . . ?
C20 C17 C19 109.7(2) . . ?
O8 C18 C17 111.0(2) . . ?
O8 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
O8 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
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 . . ?
O2 B1 O1 122.4(2) . . ?
O2 B1 B2 123.5(2) . . ?
O1 B1 B2 114.0(2) . . ?
O4 B2 O3 122.4(2) . . ?
O4 B2 B1 122.5(2) . . ?
O3 B2 B1 115.0(2) . . ?
O6 B3 O5 122.5(2) . . ?
O6 B3 B4 124.3(2) . . ?
O5 B3 B4 112.6(2) . . ?
O8 B4 O7 122.8(2) . . ?
O8 B4 B3 125.3(2) . . ?
O7 B4 B3 111.7(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
B1 O1 C1 C2 -26.8(3) . . . . ?
ZR1 O1 C1 C2 152.79(15) . . . . ?
O1 C1 C2 C3 54.3(3) . . . . ?
O1 C1 C2 C5 170.53(19) . . . . ?
O1 C1 C2 C4 -68.1(3) . . . . ?
B1 O2 C3 C2 29.6(3) . . . . ?
C1 C2 C3 O2 -56.4(3) . . . . ?
C5 C2 C3 O2 -172.8(2) . . . . ?
C4 C2 C3 O2 65.5(3) . . . . ?
B2 O3 C6 C7 27.3(3) . . . . ?
ZR1 O3 C6 C7 -164.17(15) . . . . ?
O3 C6 C7 C8 -54.7(3) . . . . ?
O3 C6 C7 C9 67.9(3) . . . . ?
O3 C6 C7 C10 -171.6(2) . . . . ?
B2 O4 C8 C7 -30.4(3) . . . . ?
C6 C7 C8 O4 57.0(3) . . . . ?
C9 C7 C8 O4 -65.0(3) . . . . ?
C10 C7 C8 O4 173.2(2) . . . . ?
B3 O5 C11 C12 25.0(3) . . . . ?
ZR2 O5 C11 C12 -153.60(15) . . . . ?
O5 C11 C12 C14 65.6(3) . . . . ?
O5 C11 C12 C13 -56.8(2) . . . . ?
O5 C11 C12 C15 -173.3(2) . . . . ?
B3 O6 C13 C12 -28.6(3) . . . . ?
C14 C12 C13 O6 -62.1(3) . . . . ?
C11 C12 C13 O6 59.6(3) . . . . ?
C15 C12 C13 O6 176.5(2) . . . . ?
B4 O7 C16 C17 -28.7(3) . . . . ?
ZR2 O7 C16 C17 -179.24(15) . . . . ?
O7 C16 C17 C18 57.3(3) . . . . ?
O7 C16 C17 C20 175.2(2) . . . . ?
O7 C16 C17 C19 -64.4(3) . . . . ?
B4 O8 C18 C17 26.7(3) . . . . ?
C16 C17 C18 O8 -56.5(3) . . . . ?
C20 C17 C18 O8 -173.6(2) . . . . ?
C19 C17 C18 O8 65.3(3) . . . . ?
C3 O2 B1 O1 0.7(4) . . . . ?
C3 O2 B1 B2 -175.2(2) . . . . ?
C1 O1 B1 O2 -2.1(4) . . . . ?
ZR1 O1 B1 O2 178.23(19) . . . . ?
C1 O1 B1 B2 174.2(2) . . . . ?
ZR1 O1 B1 B2 -5.5(3) . . . . ?
C8 O4 B2 O3 0.5(4) . . . . ?
C8 O4 B2 B1 177.3(2) . . . . ?
C6 O3 B2 O4 0.9(4) . . . . ?
ZR1 O3 B2 O4 -168.6(2) . . . . ?
C6 O3 B2 B1 -176.1(2) . . . . ?
ZR1 O3 B2 B1 14.4(3) . . . . ?
O2 B1 B2 O4 -6.8(4) . . . . ?
O1 B1 B2 O4 176.9(2) . . . . ?
O2 B1 B2 O3 170.2(2) . . . . ?
O1 B1 B2 O3 -6.1(3) . . . . ?
C13 O6 B3 O5 -6.4(4) . . . . ?
C13 O6 B3 B4 163.8(2) . . . . ?
C11 O5 B3 O6 8.2(4) . . . . ?
ZR2 O5 B3 O6 -173.0(2) . . . . ?
C11 O5 B3 B4 -163.0(2) . . . . ?
ZR2 O5 B3 B4 15.8(3) . . . . ?
C18 O8 B4 O7 4.5(4) . . . . ?
C18 O8 B4 B3 -169.5(2) . . . . ?
C16 O7 B4 O8 -3.5(4) . . . . ?
ZR2 O7 B4 O8 150.5(2) . . . . ?
C16 O7 B4 B3 171.3(2) . . . . ?
ZR2 O7 B4 B3 -34.7(2) . . . . ?
O6 B3 B4 O8 16.7(4) . . . . ?
O5 B3 B4 O8 -172.3(2) . . . . ?
O6 B3 B4 O7 -158.0(2) . . . . ?
O5 B3 B4 O7 13.1(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


