# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_SUM-1-F
_database_code_depnum_ccdc_archive 'CCDC 2528071'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2026-02-03 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
_audit_creation_date             2025-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H8 F4 N4 O8 Zr, 2(Cl), 2(C2 H8 N)'
_chemical_formula_sum            'C20 H24 Cl2 F4 N6 O8 Zr'
_chemical_formula_weight         714.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        P-3c1
_space_group_name_Hall           '-P 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   23.2456(12)
_cell_length_b                   23.2456(12)
_cell_length_c                   16.2338(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7596.8(9)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    7250
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      74.81
_cell_measurement_theta_min      3.80
_shelx_estimated_absorpt_T_max   0.764
_shelx_estimated_absorpt_T_min   0.684
_exptl_absorpt_coefficient_mu    3.164
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0584 after correction.
The Ratio of minimum to maximum transmission is 0.7327.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.881
_diffrn_reflns_theta_min         3.803
_diffrn_ambient_temperature      200.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4246
_reflns_number_total             5196
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.41 (Bruker, 2024)'
_computing_data_collection       'APEX6 V2024.9-1 (Bruker, 2024)'
_computing_data_reduction        'SAINT V8.41 (Bruker, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.453
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5196
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0909P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1372
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C10 = N3-C9
 1.5 with sigma of 0.01
 C9-C10
 2.5 with sigma of 0.01
 N3A-C9A \\sim N3A-C10A \\sim N3-C10 \\sim N3-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C9 \\sim C10 \\sim N3A \\sim C9A \\sim C10A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(N3A)=Sof(H3AA)=Sof(H3AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N3A(H3AA,H3AB)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 1.000000 0.50407(2) 0.250000 0.01884(12) Uani 1 2 d S T P . .
F1 F 0.73029(11) 0.60192(13) 0.33897(14) 0.0579(6) Uani 1 1 d . . . . .
F2 F 0.78365(9) 0.43642(10) 0.16450(13) 0.0470(5) Uani 1 1 d . . . . .
O1 O 0.96213(8) 0.52725(10) 0.35975(11) 0.0274(4) Uani 1 1 d . . . . .
O2 O 0.91509(9) 0.51839(10) 0.21625(11) 0.0299(4) Uani 1 1 d . . . . .
O3 O 0.59622(9) 0.51453(11) 0.28525(11) 0.0313(4) Uani 1 1 d . . . . .
O4 O 0.55554(9) 0.51512(10) 0.13908(10) 0.0262(4) Uani 1 1 d . . . . .
N1 N 0.90390(10) 0.52740(12) 0.35084(14) 0.0288(5) Uani 1 1 d . . . . .
H1 H 0.882292 0.530541 0.393527 0.035 Uiso 1 1 calc R U . . .
N2 N 0.61472(11) 0.51671(12) 0.15043(14) 0.0284(5) Uani 1 1 d . . . . .
H2 H 0.639180 0.517767 0.108453 0.034 Uiso 1 1 calc R U . . .
C1 C 0.88176(13) 0.52262(13) 0.27564(16) 0.0282(5) Uani 1 1 d . . . . .
C2 C 0.81835(13) 0.52202(15) 0.26319(16) 0.0303(5) Uani 1 1 d . . . . .
C3 C 0.80325(15) 0.56383(17) 0.30792(17) 0.0368(6) Uani 1 1 d . . . . .
H3 H 0.834065 0.594110 0.346790 0.044 Uiso 1 1 calc R U . . .
C4 C 0.74348(15) 0.56096(16) 0.29543(18) 0.0364(6) Uani 1 1 d . . . . .
C5 C 0.69680(13) 0.51809(15) 0.23949(16) 0.0299(5) Uani 1 1 d . . . . .
C6 C 0.71204(13) 0.47604(14) 0.19440(17) 0.0309(5) Uani 1 1 d . . . . .
H6 H 0.681360 0.445845 0.155347 0.037 Uiso 1 1 calc R U . . .
C7 C 0.77154(14) 0.47895(15) 0.20723(17) 0.0323(6) Uani 1 1 d . . . . .
C8 C 0.63302(13) 0.51660(14) 0.22571(16) 0.0289(5) Uani 1 1 d . . . . .
Cl1 Cl 0.82547(8) 0.52212(11) 0.50203(6) 0.1052(6) Uani 1 1 d . . . . .
N3 N 1.0443(3) 0.5835(3) 0.5021(3) 0.0602(19) Uani 0.550(9) 1 d D U P A 1
H3A H 1.023351 0.559038 0.547475 0.072 Uiso 0.550(9) 1 calc R U P A 1
H3B H 1.027242 0.556589 0.457351 0.072 Uiso 0.550(9) 1 calc R U P A 1
C9 C 1.1161(5) 0.6056(7) 0.5082(11) 0.072(3) Uani 0.550(9) 1 d D U P A 1
H9A H 1.139533 0.633084 0.460378 0.108 Uiso 0.550(9) 1 calc R U P A 1
H9B H 1.121933 0.566610 0.509587 0.108 Uiso 0.550(9) 1 calc R U P A 1
H9C H 1.134317 0.631509 0.558735 0.108 Uiso 0.550(9) 1 calc R U P A 1
C10 C 1.0295(9) 0.6387(8) 0.4948(10) 0.083(4) Uani 0.550(9) 1 d D U P A 1
H10A H 1.052875 0.666223 0.446922 0.125 Uiso 0.550(9) 1 calc R U P A 1
H10B H 1.044433 0.666026 0.544776 0.125 Uiso 0.550(9) 1 calc R U P A 1
H10C H 0.981597 0.620261 0.487993 0.125 Uiso 0.550(9) 1 calc R U P A 1
N3A N 1.0636(5) 0.6398(4) 0.4526(5) 0.068(2) Uani 0.450(9) 1 d D U P A 2
H3AA H 1.038205 0.608917 0.414201 0.081 Uiso 0.450(9) 1 calc R U P A 2
H3AB H 1.089104 0.679245 0.426627 0.081 Uiso 0.450(9) 1 calc R U P A 2
C9A C 1.1061(8) 0.6191(10) 0.4952(12) 0.073(4) Uani 0.450(9) 1 d D U P A 2
H9AA H 1.133814 0.612848 0.454876 0.110 Uiso 0.450(9) 1 calc R U P A 2
H9AB H 1.078193 0.577254 0.524420 0.110 Uiso 0.450(9) 1 calc R U P A 2
H9AC H 1.134526 0.653445 0.534857 0.110 Uiso 0.450(9) 1 calc R U P A 2
C10A C 1.0208(11) 0.6464(13) 0.5144(11) 0.082(5) Uani 0.450(9) 1 d D U P A 2
H10D H 0.999790 0.669851 0.489913 0.123 Uiso 0.450(9) 1 calc R U P A 2
H10E H 1.047791 0.671611 0.561751 0.123 Uiso 0.450(9) 1 calc R U P A 2
H10F H 0.986465 0.602188 0.532521 0.123 Uiso 0.450(9) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.1711(17) . ?
Zr1 O1 2.1711(17) 6_765 ?
Zr1 O2 2.2279(17) 6_765 ?
Zr1 O2 2.2279(17) . ?
Zr1 O3 2.2231(18) 3_665 ?
Zr1 O3 2.2231(18) 5_665 ?
Zr1 O4 2.1781(17) 5_665 ?
Zr1 O4 2.1780(17) 3_665 ?
F1 C4 1.339(3) . ?
F2 C7 1.348(3) . ?
O1 N1 1.363(3) . ?
O2 C1 1.271(3) . ?
O3 C8 1.276(3) . ?
O4 N2 1.370(3) . ?
N1 H1 0.8800 . ?
N1 C1 1.308(3) . ?
N2 H2 0.8800 . ?
N2 C8 1.294(3) . ?
C1 C2 1.481(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.386(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(4) . ?
C4 C5 1.383(4) . ?
C5 C6 1.401(4) . ?
C5 C8 1.483(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.366(4) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C9 1.484(8) . ?
N3 C10 1.490(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N3A H3AA 0.9100 . ?
N3A H3AB 0.9100 . ?
N3A C9A 1.469(13) . ?
N3A C10A 1.474(13) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O1 126.39(10) . 6_765 ?
O1 Zr1 O2 70.45(6) . . ?
O1 Zr1 O2 78.49(7) 6_765 . ?
O1 Zr1 O2 70.45(6) 6_765 6_765 ?
O1 Zr1 O2 78.50(7) . 6_765 ?
O1 Zr1 O3 79.01(7) 6_765 5_665 ?
O1 Zr1 O3 79.00(7) . 3_665 ?
O1 Zr1 O3 138.70(6) 6_765 3_665 ?
O1 Zr1 O3 138.70(6) . 5_665 ?
O1 Zr1 O4 137.47(6) 6_765 5_665 ?
O1 Zr1 O4 69.05(7) . 5_665 ?
O1 Zr1 O4 69.05(7) 6_765 3_665 ?
O1 Zr1 O4 137.46(6) . 3_665 ?
O2 Zr1 O2 107.36(11) . 6_765 ?
O3 Zr1 O2 150.75(7) 3_665 6_765 ?
O3 Zr1 O2 82.18(8) 5_665 6_765 ?
O3 Zr1 O2 82.18(8) 3_665 . ?
O3 Zr1 O2 150.75(7) 5_665 . ?
O3 Zr1 O3 103.13(11) 3_665 5_665 ?
O4 Zr1 O2 76.06(7) 3_665 . ?
O4 Zr1 O2 76.06(7) 5_665 6_765 ?
O4 Zr1 O2 137.65(6) 3_665 6_765 ?
O4 Zr1 O2 137.65(6) 5_665 . ?
O4 Zr1 O3 71.03(6) 3_665 3_665 ?
O4 Zr1 O3 71.03(6) 5_665 5_665 ?
O4 Zr1 O3 78.59(7) 5_665 3_665 ?
O4 Zr1 O3 78.59(7) 3_665 5_665 ?
O4 Zr1 O4 130.26(10) 3_665 5_665 ?
N1 O1 Zr1 116.10(14) . . ?
C1 O2 Zr1 116.41(16) . . ?
C8 O3 Zr1 115.50(16) . 2_655 ?
N2 O4 Zr1 114.95(13) . 2_655 ?
O1 N1 H1 121.7 . . ?
C1 N1 O1 116.6(2) . . ?
C1 N1 H1 121.7 . . ?
O4 N2 H2 121.5 . . ?
C8 N2 O4 117.0(2) . . ?
C8 N2 H2 121.5 . . ?
O2 C1 N1 119.0(2) . . ?
O2 C1 C2 122.5(2) . . ?
N1 C1 C2 118.4(2) . . ?
C3 C2 C1 121.3(2) . . ?
C7 C2 C1 121.0(2) . . ?
C7 C2 C3 117.7(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
F1 C4 C3 118.3(3) . . ?
F1 C4 C5 118.9(2) . . ?
C3 C4 C5 122.8(3) . . ?
C4 C5 C6 117.7(2) . . ?
C4 C5 C8 122.1(2) . . ?
C6 C5 C8 120.2(2) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 H6 120.4 . . ?
F2 C7 C2 119.4(2) . . ?
F2 C7 C6 117.6(2) . . ?
C6 C7 C2 123.0(3) . . ?
O3 C8 N2 120.0(2) . . ?
O3 C8 C5 122.0(2) . . ?
N2 C8 C5 117.9(2) . . ?
H3A N3 H3B 107.6 . . ?
C9 N3 H3A 108.7 . . ?
C9 N3 H3B 108.7 . . ?
C9 N3 C10 114.3(8) . . ?
C10 N3 H3A 108.7 . . ?
C10 N3 H3B 108.7 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H3AA N3A H3AB 108.4 . . ?
C9A N3A H3AA 110.1 . . ?
C9A N3A H3AB 110.1 . . ?
C9A N3A C10A 108.2(13) . . ?
C10A N3A H3AA 110.1 . . ?
C10A N3A H3AB 110.1 . . ?
N3A C9A H9AA 109.5 . . ?
N3A C9A H9AB 109.5 . . ?
N3A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
N3A C10A H10D 109.5 . . ?
N3A C10A H10E 109.5 . . ?
N3A C10A H10F 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 N1 C1 -9.0(3) . . . . ?
Zr1 O2 C1 N1 9.1(3) . . . . ?
Zr1 O2 C1 C2 -170.6(2) . . . . ?
Zr1 O3 C8 N2 8.9(3) 2_655 . . . ?
Zr1 O3 C8 C5 -170.3(2) 2_655 . . . ?
Zr1 O4 N2 C8 -9.9(3) 2_655 . . . ?
F1 C4 C5 C6 179.6(3) . . . . ?
F1 C4 C5 C8 0.6(5) . . . . ?
O1 N1 C1 O2 -0.2(4) . . . . ?
O1 N1 C1 C2 179.5(2) . . . . ?
O2 C1 C2 C3 -139.4(3) . . . . ?
O2 C1 C2 C7 41.6(4) . . . . ?
O4 N2 C8 O3 0.6(4) . . . . ?
O4 N2 C8 C5 179.8(2) . . . . ?
N1 C1 C2 C3 40.9(4) . . . . ?
N1 C1 C2 C7 -138.1(3) . . . . ?
C1 C2 C3 C4 -179.0(3) . . . . ?
C1 C2 C7 F2 0.9(4) . . . . ?
C1 C2 C7 C6 179.2(3) . . . . ?
C2 C3 C4 F1 -179.7(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C3 C2 C7 F2 -178.1(3) . . . . ?
C3 C2 C7 C6 0.1(4) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C3 C4 C5 C8 -178.8(3) . . . . ?
C4 C5 C6 C7 0.0(4) . . . . ?
C4 C5 C8 O3 -47.9(4) . . . . ?
C4 C5 C8 N2 132.9(3) . . . . ?
C5 C6 C7 F2 178.1(3) . . . . ?
C5 C6 C7 C2 -0.1(4) . . . . ?
C6 C5 C8 O3 133.2(3) . . . . ?
C6 C5 C8 N2 -46.1(4) . . . . ?
C7 C2 C3 C4 0.1(4) . . . . ?
C8 C5 C6 C7 179.0(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.963 3328.4 327.5 ?
2 0.333 0.667 -0.928 319.6 148.3 ?
3 0.667 0.333 -0.056 319.6 140.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU
####################################################################### 
# 
# 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_SUM-1-Br
_database_code_depnum_ccdc_archive 'CCDC 2528073'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2026-02-03 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
_audit_creation_date             2025-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H16 Br8 N8 O16 Zr2'
_chemical_formula_sum            'C32 H16 Br8 N8 O16 Zr2'
_chemical_formula_weight         1590.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'y, x, -z+1/2'
'-x, y, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'-y, -x, z-1/2'
'x, -y, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   16.505(4)
_cell_length_b                   16.505(4)
_cell_length_c                   15.103(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4114(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7707
_cell_measurement_temperature    237.00
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.705
_shelx_estimated_absorpt_T_min   0.613
_exptl_absorpt_coefficient_mu    4.180
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.8621.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23820
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         2.468
_diffrn_ambient_temperature      237.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON II'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Turbo X-Ray Source (TXS)'
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                995
_reflns_number_total             1155
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.41 (Bruker, 2024)'
_computing_data_collection       'APEX6 V2024.9-1 (Bruker, 2024)'
_computing_data_reduction        'SAINT V8.41 (Bruker, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1155
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0834
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1310P)²+42.8324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2467
_refine_ls_wR_factor_ref         0.2536
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C3-C2
 1.39 with sigma of 0.01
 Br1-C3 \\sim Br2-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Br2: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C3 \\sim Br1 \\sim Br2 \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Sof(Br1)=0.5*(1-FVAR(2))
 Sof(Br2)=0.5*FVAR(2)
 Fixed Sof: H3(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.000000 -0.500000 -0.250000 0.0237(5) Uani 1 8 d S T P . .
Br1 Br 0.2982(2) -0.56092(18) -0.2164(4) 0.1047(16) Uani 0.347(4) 1 d D U P A 2
O1 O 0.0515(2) -0.5515(2) -0.3713(3) 0.0358(12) Uani 1 2 d S T P . .
O2 O 0.0915(2) -0.5915(2) -0.2128(4) 0.0465(16) Uani 1 2 d S T P . .
N1 N 0.1090(3) -0.6090(3) -0.3592(5) 0.0407(16) Uani 1 2 d S T P . .
H1 H 0.132354 -0.632354 -0.404070 0.049 Uiso 1 2 calc R U P . .
C2 C 0.1910(4) -0.6910(4) -0.2623(8) 0.059(2) Uani 1 2 d DS TU P A .
C1 C 0.1280(4) -0.6280(4) -0.2781(5) 0.0406(19) Uani 1 2 d S T P . .
C3 C 0.2712(5) -0.6722(6) -0.2561(8) 0.093(2) Uani 1 1 d D U . . .
H3 H 0.287126 -0.617654 -0.260442 0.111 Uiso 0.5 1 calc R U P A 3
Br2 Br 0.3067(5) -0.5652(5) -0.3024(11) 0.120(3) Uani 0.153(4) 1 d D U P A 1


_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 2.191(5) 28_444 ?
Zr1 O1 2.191(5) 26_544 ?
Zr1 O1 2.191(5) 3_545 ?
Zr1 O1 2.191(5) . ?
Zr1 O2 2.208(6) . ?
Zr1 O2 2.208(6) 26_544 ?
Zr1 O2 2.208(6) 28_444 ?
Zr1 O2 2.208(6) 3_545 ?
Br1 Br1 2.252(8) 5_544 ?
Br1 C3 1.982(11) . ?
O1 N1 1.352(8) . ?
O2 C1 1.303(10) . ?
N1 H1 0.8700 . ?
N1 C1 1.304(11) . ?
C2 C1 1.490(12) . ?
C2 C3 1.363(7) . ?
C2 C3 1.363(7) 30_445 ?
C3 C3 1.334(18) 6_644 ?
C3 H3 0.9400 . ?
C3 Br2 1.988(12) . ?
Br2 Br2 2.67(3) 5_544 ?

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 O1 134.31(17) 28_444 3_545 ?
O1 Zr1 O1 134.31(17) 28_444 . ?
O1 Zr1 O1 66.6(3) 3_545 . ?
O1 Zr1 O1 134.31(17) 3_545 26_544 ?
O1 Zr1 O1 66.6(3) 28_444 26_544 ?
O1 Zr1 O1 134.31(17) 26_544 . ?
O1 Zr1 O2 77.74(14) 3_545 28_444 ?
O1 Zr1 O2 77.74(14) 28_444 . ?
O1 Zr1 O2 71.4(2) 28_444 28_444 ?
O1 Zr1 O2 138.0(2) . 3_545 ?
O1 Zr1 O2 77.74(14) 26_544 . ?
O1 Zr1 O2 77.74(14) 28_444 3_545 ?
O1 Zr1 O2 77.74(14) . 28_444 ?
O1 Zr1 O2 77.74(14) . 26_544 ?
O1 Zr1 O2 71.4(2) 3_545 3_545 ?
O1 Zr1 O2 77.74(14) 26_544 3_545 ?
O1 Zr1 O2 138.0(2) 28_444 26_544 ?
O1 Zr1 O2 71.4(2) . . ?
O1 Zr1 O2 77.74(14) 3_545 26_544 ?
O1 Zr1 O2 138.0(2) 3_545 . ?
O1 Zr1 O2 138.0(2) 26_544 28_444 ?
O1 Zr1 O2 71.4(2) 26_544 26_544 ?
O2 Zr1 O2 93.70(8) . 28_444 ?
O2 Zr1 O2 93.70(8) 28_444 3_545 ?
O2 Zr1 O2 150.6(3) 26_544 28_444 ?
O2 Zr1 O2 150.6(3) . 3_545 ?
O2 Zr1 O2 93.70(8) . 26_544 ?
O2 Zr1 O2 93.70(8) 26_544 3_545 ?
C3 Br1 Br1 133.7(5) . 5_544 ?
N1 O1 Zr1 115.6(4) . . ?
C1 O2 Zr1 116.1(5) . . ?
O1 N1 H1 121.2 . . ?
C1 N1 O1 117.7(7) . . ?
C1 N1 H1 121.2 . . ?
C3 C2 C1 122.0(5) . . ?
C3 C2 C1 122.0(5) 30_445 . ?
C3 C2 C3 116.0(11) . 30_445 ?
O2 C1 N1 119.2(7) . . ?
O2 C1 C2 121.7(8) . . ?
N1 C1 C2 119.1(8) . . ?
C2 C3 Br1 116.8(7) . . ?
C2 C3 C3 122.0(5) . 6_644 ?
C2 C3 H3 119.0 . . ?
C2 C3 Br2 117.7(7) . . ?
C3 C3 Br1 116.8(6) 6_644 . ?
C3 C3 H3 119.0 6_644 . ?
C3 C3 Br2 117.6(5) 6_644 . ?
C3 Br2 Br2 120.5(9) . 5_544 ?

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
Zr1 O1 N1 C1 -0.001(2) . . . . ?
Zr1 O2 C1 N1 -0.001(2) . . . . ?
Zr1 O2 C1 C2 180.000(2) . . . . ?
O1 N1 C1 O2 0.001(3) . . . . ?
O1 N1 C1 C2 180.000(3) . . . . ?
C1 C2 C3 Br1 26.1(16) . . . . ?
C1 C2 C3 C3 -178.5(15) . . . 6_644 ?
C1 C2 C3 Br2 -17.4(16) . . . . ?
C3 C2 C1 O2 91.0(11) 30_445 . . . ?
C3 C2 C1 O2 -91.1(11) . . . . ?
C3 C2 C1 N1 88.9(11) . . . . ?
C3 C2 C1 N1 -88.9(11) 30_445 . . . ?
C3 C2 C3 Br1 -155.9(7) 30_445 . . . ?
C3 C2 C3 C3 0(3) 30_445 . . 6_644 ?
C3 C2 C3 Br2 160.6(8) 30_445 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.605 -0.664 -0.845 1822.2 116.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU
####################################################################### 
# 
# 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_SUM-1-Cl
_database_code_depnum_ccdc_archive 'CCDC 2528072'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2026-02-03 deposited with the CCDC.	2026-03-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_SUM-1-Cl            
;
PROBLEM: Unit-Cell Contains Solvent Accessible VOIDS .LE.        487 Ang**3
RESPONSE: The MOF structure is intrinsically porous with cavities.
;
_vrf_RINTA01_SUM-1-Cl            
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystal diffracted weakly, a large number of "invisible" diffraction points were used in the refinement process.
;
_vrf_PLAT020_SUM-1-Cl            
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.227 Report
RESPONSE: The crystal diffracted weakly, a large number of "invisible" diffraction points were used in the refinement process.
;
# Added during the CSD deposition process: Tuesday 03 February 2026 04:22 AM
# end Validation Reply Form

_audit_creation_date             2025-03-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C16 H8 Cl4 N4 O8 Zr, 2(Cl), C4 H10 O2, 2.5[CH3CH2OH]'
_chemical_formula_sum            'C22 H22 Cl6 N6 O10 Zr'
_chemical_formula_weight         834.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr Cl'
_chemical_oxdiff_usercomment     'C H O N Zr Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.3299(7)
_cell_length_b                   17.5645(7)
_cell_length_c                   14.9948(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4037.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13690
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5940
_cell_measurement_theta_min      3.8360
_cell_oxdiff_angle_alpha         101.359(3)
_cell_oxdiff_angle_beta          114.488(4)
_cell_oxdiff_angle_gamma         112.818(3)
_cell_oxdiff_length_a            13.8513(6)
_cell_oxdiff_length_b            13.8569(4)
_cell_oxdiff_length_c            13.8623(5)
_cell_oxdiff_measurement_reflns_used 13682
_cell_oxdiff_volume              2018.75(13)
_shelx_estimated_absorpt_T_max   0.571
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    6.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.140a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2266
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21903
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.058
_diffrn_reflns_theta_max         65.058
_diffrn_reflns_theta_min         5.902
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -34.00   0.50    1.00    --  -45.68 -11.00 -64.00  170
  2  ω    -21.00   5.00   0.50    1.00    --  -45.68  11.00 108.00   52
  3  ω     -4.00  23.00   0.50    1.00    --   45.68 -11.00 -64.00   54
  4  ω     66.00 120.00   0.50    1.00    --   45.68  11.00 108.00  108
  5  ω   -172.00 -92.00   0.50    3.00    -- -102.76 -11.00 -64.00  160
  6  ω     86.00 175.00   0.50    3.00    --  102.76  11.00 108.00  178
  7  ω    -83.00 -38.00   0.50    1.00    --  -45.68 -38.00  60.00   90
  8  ω    -40.00  23.00   0.50    1.00    --  -45.68  38.00  60.00  126
  9  ω    -24.00  66.00   0.50    1.00    --   45.68 -77.00 -60.00  180
 10  ω    -26.00  54.00   0.50    1.00    --   45.68 -57.00-180.00  160
 11  ω   -168.00 -90.00   0.50    3.00    -- -102.76 -45.00  30.00  156
 12  ω   -141.00 -81.00   0.50    3.00    -- -102.76 -77.00  90.00  120
 13  ω   -100.00 -31.00   0.50    3.00    -- -102.76  77.00-150.00  138
 14  ω    -69.00 -31.00   0.50    3.00    -- -102.76  61.00-180.00   76
 15  ω   -111.00 -64.00   0.50    3.00    -- -102.76 125.00 -90.00   94
 16  ω    -62.00 -36.00   0.50    3.00    -- -102.76 140.00 168.57   52
 17  ω    -72.00 -46.00   0.50    3.00    -- -102.76 125.00 150.00   52
 18  ω   -108.00 -75.00   0.50    3.00    -- -102.76 125.00 150.00   66
 19  ω    -97.00 -34.00   0.50    3.00    -- -102.76 125.00-150.00  126
 20  ω    -67.00 -36.00   0.50    3.00    -- -102.76  61.00 150.00   62
 21  ω   -123.00 -85.00   0.50    3.00    -- -102.76 140.00 168.57   76
 22  ω     68.00  98.00   0.50    3.00    --  102.76 -95.00   0.00   60
 23  ω     51.00 111.00   0.50    3.00    --  102.76-125.00  30.00  120
 24  ω    116.00 176.00   0.50    3.00    --  102.76  15.00  30.00  120
 25  ω     32.00 105.00   0.50    3.00    --  102.76 -95.00  30.00  146
 26  ω    145.00 174.00   0.50    3.00    --  102.76  15.00 -60.00   58
 27  ω     92.00 126.00   0.50    3.00    --  102.76  15.00 -60.00   68
 28  ω     42.00  73.00   0.50    3.00    --  102.76 -61.00-120.00   62
 29  ω     80.00 111.00   0.50    3.00    --  102.76-125.00 150.00   62
 30  ω     36.00  83.00   0.50    3.00    --  102.76 -95.00-120.00   94
 31  ω     38.00  84.00   0.50    3.00    --  102.76 -95.00  90.00   92
 32  ω     46.00  75.00   0.50    3.00    --  102.76-125.00 150.00   58
 33  ω     34.00  59.00   0.50    3.00    --  102.76 -61.00-180.00   50
 34  ω     43.00 112.00   0.50    3.00    --  102.76-125.00 -30.00  138
 35  ω     58.00 112.00   0.50    3.00    --  102.76-125.00-150.00  108
 36  ω     95.00 158.00   0.50    3.00    --  102.76  61.00 150.00  126
 37  ω     31.00  77.00   0.50    3.00    --  102.76 -95.00 -30.00   92
 38  ω     55.00  80.00   0.50    3.00    --  102.76 -77.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0570760000
_diffrn_orient_matrix_UB_12      0.0180628000
_diffrn_orient_matrix_UB_13      0.1287360000
_diffrn_orient_matrix_UB_21      -0.1086177000
_diffrn_orient_matrix_UB_22      0.0075248000
_diffrn_orient_matrix_UB_23      -0.0013836000
_diffrn_orient_matrix_UB_31      -0.0748238000
_diffrn_orient_matrix_UB_32      -0.1319046000
_diffrn_orient_matrix_UB_33      -0.0406606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1728
_reflns_number_total             1776
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1776
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.1355
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1229P)²+201.6341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3377
_refine_ls_wR_factor_ref         0.3380
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C10
 1.46 with sigma of 0.02
 N4-C1
 1.45 with sigma of 0.02
 C2-O1
 1.22 with sigma of 0.02
 C2-N4
 1.36 with sigma of 0.02
 C2-C10
 2.45 with sigma of 0.04
 C2-C1
 2.46 with sigma of 0.04
 N4-C1 \\sim N4-C10
 with sigma of 0.02
 Cl1-C3 \\sim Cl2-C7
 with sigma of 0.02
 C9-C6 \\sim C9-C5
 with sigma of 0.02
 C6-C3 \\sim C5-C7
 with sigma of 0.02
 C6-C8 \\sim C5-C4
 with sigma of 0.02
 Cl1-C6 \\sim Cl2-C5
 with sigma of 0.04
 C9-C3 \\sim C9-C7
 with sigma of 0.04
 C9-C8 \\sim C9-C4
 with sigma of 0.04
 C3-C8 \\sim C7-C4
 with sigma of 0.04
3. Restrained planarity
 C2, O1, N4, C1, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2 \\sim O1 \\sim N4 \\sim C1 \\sim C10: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C2, O1, N4, C1, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl2)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C7)=1-FVAR(1)
 Sof(Cl1)=Sof(C3)=Sof(C6)=Sof(C8)=Sof(H8)=FVAR(1)
 Fixed Sof: H1B(0.5) H1C(0.5) H1A(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
7.a Riding coordinates:
 C1(H1B,H1C,H1A), C10(H10A,H10B,H10C)
7.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C8(H8), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.500000 0.000000 0.250000 0.0202(6) Uani 1 4 d S T P . .
Cl1 Cl 0.1881(4) 0.0873(4) 0.3001(6) 0.056(3) Uani 0.502(12) 1 d D . P A 1
Cl2 Cl 0.4469(9) 0.2823(9) 0.2638(14) 0.142(6) Uani 0.498(12) 1 d D U P A 2
O2 O 0.4057(6) 0.0890(5) 0.2857(6) 0.040(2) Uani 1 1 d . . . . .
O3 O 0.4413(4) 0.0468(4) 0.1285(5) 0.0262(17) Uani 1 1 d . . . . .
N1 N 0.3852(6) 0.1049(6) 0.1404(6) 0.032(2) Uani 1 1 d . . . . .
H1 H 0.360522 0.128391 0.095089 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2260(15) 0.1770(16) 0.2740(19) 0.037(7) Uani 0.502(12) 1 d D . P A 1
C4 C 0.2181(19) 0.178(2) 0.233(3) 0.062(11) Uani 0.498(12) 1 d D U P A 2
H4 H 0.193299 0.129515 0.220846 0.074 Uiso 0.498(12) 1 calc R U P A 2
C5 C 0.2988(15) 0.1828(13) 0.239(2) 0.032(8) Uani 0.498(12) 1 d D U P A 2
C6 C 0.3141(16) 0.1953(12) 0.2349(19) 0.025(7) Uani 0.502(12) 1 d D U P A 1
C7 C 0.337(2) 0.2608(19) 0.257(4) 0.081(16) Uani 0.498(12) 1 d D U P A 2
C8 C 0.3317(17) 0.2624(12) 0.215(2) 0.036(6) Uani 0.502(12) 1 d D . P A 1
H8 H 0.387544 0.272808 0.189971 0.044 Uiso 0.502(12) 1 calc R U P A 1
C9 C 0.3687(7) 0.1256(6) 0.2273(7) 0.027(2) Uani 1 1 d D U . . .
Cl3 Cl 0.2889(10) 0.1917(10) 0.000000 0.184(7) Uani 1 2 d S T P . .
C2 C 0.4049(12) 0.0769(11) 0.500000 0.055(5) Uani 1 2 d DS TU P . .
H2 H 0.446312 0.036695 0.500000 0.066 Uiso 1 2 calc R U P . .
O1 O 0.3233(13) 0.0661(16) 0.500000 0.137(10) Uani 1 2 d DS TU P . .
N4 N 0.4280(18) 0.1537(12) 0.500000 0.104(7) Uani 1 2 d DS TU P . .
C1 C 0.522(2) 0.168(3) 0.500000 0.24(3) Uani 1 2 d DS TU P . .
H1B H 0.544599 0.162737 0.439202 0.367 Uiso 0.5 1 d R U P B -1
H1C H 0.550638 0.131055 0.539077 0.367 Uiso 0.5 1 d R U P B -1
H1A H 0.533735 0.219735 0.521721 0.367 Uiso 0.5 1 d R U P B -1
C10 C 0.356(3) 0.208(2) 0.500000 0.24(3) Uani 1 2 d DS TU P . .
H10A H 0.365396 0.245314 0.547848 0.366 Uiso 0.5 1 d R U P C -1
H10B H 0.300693 0.181661 0.509700 0.366 Uiso 0.5 1 d R U P C -1
H10C H 0.354490 0.234585 0.442452 0.366 Uiso 0.5 1 d R U P C -1


_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 O2 2.196(7) 2_655 ?
Zr1 O2 2.196(7) 4_655 ?
Zr1 O2 2.196(7) 3 ?
Zr1 O2 2.196(7) . ?
Zr1 O3 2.192(7) 2_655 ?
Zr1 O3 2.192(7) 4_655 ?
Zr1 O3 2.192(7) 3 ?
Zr1 O3 2.192(7) . ?
Cl1 C3 1.72(3) . ?
Cl2 Cl2 1.68(3) 4_655 ?
Cl2 C7 1.72(3) . ?
O2 C9 1.226(13) . ?
O3 N1 1.346(11) . ?
N1 H1 0.8800 . ?
N1 C9 1.377(15) . ?
C3 C6 1.51(3) . ?
C3 C8 1.39(3) 13 ?
C4 H4 0.9500 . ?
C4 C5 1.24(3) . ?
C4 C7 1.38(4) 13 ?
C5 C7 1.52(4) . ?
C5 C9 1.479(18) . ?
C6 C8 1.25(3) . ?
C6 C9 1.486(18) . ?
C8 H8 0.9500 . ?
C2 H2 0.9500 . ?
C2 O1 1.266(17) . ?
C2 N4 1.395(18) . ?
N4 C1 1.463(16) . ?
N4 C10 1.459(16) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1A 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zr1 O2 151.8(4) 3 4_655 ?
O2 Zr1 O2 97.7(5) 4_655 2_655 ?
O2 Zr1 O2 89.2(5) 3 2_655 ?
O2 Zr1 O2 97.7(5) 3 . ?
O2 Zr1 O2 151.8(4) 2_655 . ?
O2 Zr1 O2 89.2(5) 4_655 . ?
O3 Zr1 O2 137.7(3) 3 4_655 ?
O3 Zr1 O2 78.5(3) 4_655 . ?
O3 Zr1 O2 78.1(3) 2_655 4_655 ?
O3 Zr1 O2 78.5(3) . 4_655 ?
O3 Zr1 O2 78.1(3) 3 . ?
O3 Zr1 O2 137.7(3) 4_655 3 ?
O3 Zr1 O2 70.4(3) 4_655 4_655 ?
O3 Zr1 O2 78.5(3) 2_655 3 ?
O3 Zr1 O2 137.7(3) 2_655 . ?
O3 Zr1 O2 70.4(3) 3 3 ?
O3 Zr1 O2 70.4(3) . . ?
O3 Zr1 O2 137.7(3) . 2_655 ?
O3 Zr1 O2 78.1(3) . 3 ?
O3 Zr1 O2 78.1(3) 4_655 2_655 ?
O3 Zr1 O2 78.5(3) 3 2_655 ?
O3 Zr1 O2 70.4(3) 2_655 2_655 ?
O3 Zr1 O3 135.9(4) 4_655 . ?
O3 Zr1 O3 135.9(4) 2_655 3 ?
O3 Zr1 O3 131.5(4) 4_655 2_655 ?
O3 Zr1 O3 67.6(4) 2_655 . ?
O3 Zr1 O3 131.5(4) 3 . ?
O3 Zr1 O3 67.6(4) 4_655 3 ?
Cl2 Cl2 C7 158(2) 4_655 . ?
C9 O2 Zr1 120.3(7) . . ?
N1 O3 Zr1 115.9(6) . . ?
O3 N1 H1 121.9 . . ?
O3 N1 C9 116.3(9) . . ?
C9 N1 H1 121.9 . . ?
C6 C3 Cl1 125.8(17) . . ?
C8 C3 Cl1 117(2) 13 . ?
C8 C3 C6 117(3) 13 . ?
C5 C4 H4 118.2 . . ?
C7 C4 H4 118.2 13 . ?
C4 C5 C7 118(2) . . ?
C4 C5 C9 132(3) . . ?
C9 C5 C7 111(2) . . ?
C8 C6 C3 119.3(17) . . ?
C8 C6 C9 130(2) . . ?
C9 C6 C3 111.0(18) . . ?
C4 C7 Cl2 115(3) 13 . ?
C4 C7 C5 119(3) 13 . ?
C5 C7 Cl2 126(2) . . ?
C3 C8 H8 118.2 13 . ?
C6 C8 C3 124(3) . 13 ?
C6 C8 H8 118.2 . . ?
O2 C9 N1 116.9(9) . . ?
O2 C9 C5 127.3(16) . . ?
O2 C9 C6 129.6(15) . . ?
N1 C9 C5 115.2(15) . . ?
N1 C9 C6 113.1(13) . . ?
O1 C2 H2 123.3 . . ?
O1 C2 N4 113(2) . . ?
N4 C2 H2 123.3 . . ?
C2 N4 C1 115(3) . . ?
C2 N4 C10 116(2) . . ?
C10 N4 C1 129(4) . . ?
N4 C1 H1B 109.4 . . ?
N4 C1 H1C 109.1 . . ?
N4 C1 H1A 110.0 . . ?
H1B C1 H1C 109.5 . . ?
H1B C1 H1A 109.5 . . ?
H1C C1 H1A 109.5 . . ?
N4 C10 H10A 109.1 . . ?
N4 C10 H10B 110.1 . . ?
N4 C10 H10C 109.3 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O2 C9 N1 3.8(14) . . . . ?
Zr1 O2 C9 C5 174.7(14) . . . . ?
Zr1 O2 C9 C6 -169.4(15) . . . . ?
Zr1 O3 N1 C9 -2.8(12) . . . . ?
Cl1 C3 C6 C8 176(3) . . . . ?
Cl1 C3 C6 C9 -4(4) . . . . ?
Cl2 Cl2 C7 C4 -134(4) 4_655 . . 13 ?
Cl2 Cl2 C7 C5 44(9) 4_655 . . . ?
O3 N1 C9 O2 -0.6(15) . . . . ?
O3 N1 C9 C5 -172.6(13) . . . . ?
O3 N1 C9 C6 173.7(14) . . . . ?
C3 C6 C8 C3 0(6) . . . 13 ?
C3 C6 C9 O2 -74(3) . . . . ?
C3 C6 C9 N1 113(2) . . . . ?
C4 C5 C7 Cl2 -177(4) . . . . ?
C4 C5 C7 C4 1(7) . . . 13 ?
C4 C5 C9 O2 -97(5) . . . . ?
C4 C5 C9 N1 74(5) . . . . ?
C7 C4 C5 C7 -1(8) 13 . . . ?
C7 C4 C5 C9 -177(4) 13 . . . ?
C7 C5 C9 O2 86(3) . . . . ?
C7 C5 C9 N1 -103(3) . . . . ?
C8 C3 C6 C8 0(5) 13 . . . ?
C8 C3 C6 C9 179(2) 13 . . . ?
C8 C6 C9 O2 106(4) . . . . ?
C8 C6 C9 N1 -67(4) . . . . ?
C9 C5 C7 Cl2 0(5) . . . . ?
C9 C5 C7 C4 178(4) . . . 13 ?
C9 C6 C8 C3 -179(3) . . . 13 ?
O1 C2 N4 C1 180.0 . . . . ?
O1 C2 N4 C10 0.0 . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.536
_oxdiff_exptl_absorpt_empirical_full_min 0.551
