# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_b20122905a1526_0m
_database_code_depnum_ccdc_archive 'CCDC 2120873'
loop_
_audit_author_name
_audit_author_address
'Kelong ZHU'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2022-04-19 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_audit_creation_date             2022-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C2 H6 O S), C35 H22 N2 O4'
_chemical_formula_sum            'C39 H34 N2 O6 S2'
_chemical_formula_weight         690.80
_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 0.0148 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2924 0.4247 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9015(3)
_cell_length_b                   11.8523(4)
_cell_length_c                   14.5872(4)
_cell_angle_alpha                93.222(2)
_cell_angle_beta                 99.421(2)
_cell_angle_gamma                100.5780(10)
_cell_volume                     1653.52(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.267
_cell_measurement_theta_min      2.682
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.930
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8817.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26660
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.368
_diffrn_reflns_theta_min         2.682
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5454
_reflns_number_total             7157
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7157
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0667
_refine_ls_restrained_S_all      1.131
_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)+(0.0700P)²+2.1042P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1751
_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
 O002-H002
 1 with sigma of 0.02
 S1-C3 = S1A-C3A
 1.7 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.04
 O2-C3 \\sim O2A-C3A
 with sigma of 0.04
 O2-C4 \\sim O2A-C4A
 with sigma of 0.04
 S1-C3 \\sim S1A-C3A
 with sigma of 0.02
 S1-C4 \\sim S1A-C4A
 with sigma of 0.02
 S1-O2 \\sim S1A-O2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim S1 \\sim C3 \\sim C4: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
O2A \\sim S1A \\sim C3A \\sim C4A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O2A)=Sof(S1A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(S1)=Sof(O2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N006(H006), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00R(H00R), C00T(H00T), C00U(H00U), C00Z(H00Z),
 C010(H010), C012(H012), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C01A(H01A)
5.b Idealised Me refined as rotating group:
 C019(H01B,H01C,H01D), C01B(H01E,H01F,H01G), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC)
;
_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
S001 S 0.04548(8) 0.41377(6) 0.33748(6) 0.0330(2) Uani 1 1 d . . . . .
O002 O 1.3624(2) 0.1557(2) 0.94296(13) 0.0341(5) Uani 1 1 d D . . . .
O003 O 0.1148(2) 0.36745(19) 0.42255(16) 0.0380(5) Uani 1 1 d . . . . .
O004 O -0.4238(2) 0.1287(2) 0.06499(14) 0.0360(5) Uani 1 1 d . . . . .
O005 O 1.4926(2) 0.1408(2) 0.83277(14) 0.0381(5) Uani 1 1 d . . . . .
N006 N 0.3775(2) 0.30600(18) 0.48863(15) 0.0214(5) Uani 1 1 d . . . . .
H006 H 0.3018 0.3251 0.4582 0.026 Uiso 1 1 calc R . . . .
O007 O -0.2908(2) 0.1210(2) -0.04427(14) 0.0426(6) Uani 1 1 d . . . . .
N008 N 0.5614(2) 0.30852(18) 0.60216(15) 0.0220(5) Uani 1 1 d . . . . .
C009 C 0.5588(3) 0.2244(2) 0.53168(17) 0.0193(5) Uani 1 1 d . . . . .
C00A C 0.4435(3) 0.2210(2) 0.45972(17) 0.0205(5) Uani 1 1 d . . . . .
C00C C 0.7785(3) 0.1562(2) 0.59831(17) 0.0190(5) Uani 1 1 d . . . . .
C00D C 1.0262(3) 0.1549(2) 0.64510(17) 0.0190(5) Uani 1 1 d . . . . .
C00E C 0.4519(3) 0.3551(2) 0.57368(18) 0.0214(5) Uani 1 1 d . . . . .
C00F C -0.0882(3) 0.1284(2) 0.27620(17) 0.0208(5) Uani 1 1 d . . . . .
H00F H -0.0998 0.1301 0.3396 0.025 Uiso 1 1 calc R . . . .
C00G C 1.2733(3) 0.1556(2) 0.69078(18) 0.0228(5) Uani 1 1 d . . . . .
H00G H 1.3623 0.1552 0.6745 0.027 Uiso 1 1 calc R . . . .
C00H C 1.0120(3) 0.1631(2) 0.74082(17) 0.0205(5) Uani 1 1 d . . . . .
C00I C -0.2015(3) 0.1235(2) 0.20780(18) 0.0219(5) Uani 1 1 d . . . . .
H00I H -0.2913 0.1206 0.2238 0.026 Uiso 1 1 calc R . . . .
C00J C 0.9072(3) 0.1506(2) 0.57581(17) 0.0202(5) Uani 1 1 d . . . . .
H00J H 0.9161 0.1437 0.5120 0.024 Uiso 1 1 calc R . . . .
C00K C 1.1305(3) 0.1642(2) 0.81005(18) 0.0223(5) Uani 1 1 d . . . . .
H00K H 1.1222 0.1683 0.8741 0.027 Uiso 1 1 calc R . . . .
C00L C 0.6332(3) 0.0821(2) 0.44168(18) 0.0217(5) Uani 1 1 d . . . . .
H00L H 0.6973 0.0335 0.4333 0.026 Uiso 1 1 calc R . . . .
C00M C 0.5183(3) 0.0795(2) 0.37049(18) 0.0219(5) Uani 1 1 d . . . . .
H00M H 0.5077 0.0293 0.3156 0.026 Uiso 1 1 calc R . . . .
C00N C 0.4146(3) 0.4486(2) 0.62845(19) 0.0241(5) Uani 1 1 d . . . . .
C00O C 1.2579(3) 0.1592(2) 0.78544(18) 0.0213(5) Uani 1 1 d . . . . .
C00Q C 0.6562(3) 0.1532(2) 0.52383(18) 0.0203(5) Uani 1 1 d . . . . .
C00R C 0.8790(3) 0.1690(2) 0.76303(18) 0.0240(5) Uani 1 1 d . . . . .
H00R H 0.8680 0.1744 0.8265 0.029 Uiso 1 1 calc R . . . .
C00S C 0.4193(3) 0.1479(2) 0.37734(17) 0.0205(5) Uani 1 1 d . . . . .
C00T C 0.1656(3) 0.1381(2) 0.32409(17) 0.0208(5) Uani 1 1 d . . . . .
H00T H 0.1551 0.1411 0.3877 0.025 Uiso 1 1 calc R . . . .
C00U C 1.1598(3) 0.1527(2) 0.62255(18) 0.0227(5) Uani 1 1 d . . . . .
H00U H 1.1706 0.1492 0.5590 0.027 Uiso 1 1 calc R . . . .
C00V C 0.2967(3) 0.1410(2) 0.30251(17) 0.0209(5) Uani 1 1 d . . . . .
C00W C 0.0465(3) 0.1310(2) 0.25421(17) 0.0201(5) Uani 1 1 d . . . . .
C00X C 1.3798(3) 0.1521(2) 0.85723(18) 0.0239(5) Uani 1 1 d . . . . .
C00Y C 0.0625(3) 0.1269(2) 0.15885(18) 0.0232(5) Uani 1 1 d . . . . .
C00Z C 0.3108(3) 0.1346(2) 0.20734(19) 0.0266(6) Uani 1 1 d . . . . .
H00Z H 0.4002 0.1353 0.1915 0.032 Uiso 1 1 calc R . . . .
C010 C 0.7666(3) 0.1669(2) 0.69416(18) 0.0230(5) Uani 1 1 d . . . . .
H010 H 0.6790 0.1728 0.7106 0.028 Uiso 1 1 calc R . . . .
C011 C -0.3087(3) 0.1235(2) 0.04092(19) 0.0266(6) Uani 1 1 d . . . . .
C012 C -0.0566(3) 0.1228(2) 0.08913(19) 0.0267(6) Uani 1 1 d . . . . .
H012 H -0.0474 0.1201 0.0253 0.032 Uiso 1 1 calc R . . . .
C013 C -0.1856(3) 0.1227(2) 0.11301(18) 0.0240(5) Uani 1 1 d . . . . .
C014 C 0.3434(3) 0.5287(2) 0.5878(2) 0.0303(6) Uani 1 1 d . . . . .
H014 H 0.3139 0.5224 0.5221 0.036 Uiso 1 1 calc R . . . .
C015 C 0.1976(3) 0.1276(3) 0.13762(19) 0.0285(6) Uani 1 1 d . . . . .
H015 H 0.2097 0.1231 0.0743 0.034 Uiso 1 1 calc R . . . .
C016 C 0.3151(3) 0.6181(2) 0.6425(3) 0.0378(7) Uani 1 1 d . . . . .
H016 H 0.2664 0.6727 0.6141 0.045 Uiso 1 1 calc R . . . .
C017 C 0.4569(3) 0.4585(3) 0.7249(2) 0.0355(7) Uani 1 1 d . . . . .
H017 H 0.5050 0.4037 0.7535 0.043 Uiso 1 1 calc R . . . .
C018 C 0.3577(4) 0.6276(3) 0.7382(3) 0.0441(8) Uani 1 1 d . . . . .
H018 H 0.3379 0.6886 0.7757 0.053 Uiso 1 1 calc R . . . .
C019 C 0.0336(4) 0.5578(3) 0.3738(3) 0.0492(9) Uani 1 1 d . . . . .
H01B H -0.0290 0.5558 0.4194 0.074 Uiso 1 1 calc GR . . . .
H01C H -0.0032 0.5952 0.3196 0.074 Uiso 1 1 calc GR . . . .
H01D H 0.1266 0.6011 0.4023 0.074 Uiso 1 1 calc GR . . . .
C01A C 0.4288(4) 0.5485(3) 0.7792(3) 0.0473(9) Uani 1 1 d . . . . .
H01A H 0.4588 0.5555 0.8449 0.057 Uiso 1 1 calc R . . . .
C01B C 0.1765(4) 0.4491(3) 0.2684(3) 0.0560(10) Uani 1 1 d . . . . .
H01E H 0.2566 0.5028 0.3053 0.084 Uiso 1 1 calc GR . . . .
H01F H 0.1389 0.4851 0.2135 0.084 Uiso 1 1 calc GR . . . .
H01G H 0.2064 0.3787 0.2482 0.084 Uiso 1 1 calc GR . . . .
S1 S 0.7175(4) 0.4581(3) 0.9664(2) 0.0481(12) Uani 0.341(6) 1 d D U P A 1
O2 O 0.7958(6) 0.4263(4) 1.0445(4) 0.0169(12) Uani 0.341(6) 1 d D U P A 1
C3 C 0.5580(10) 0.4303(11) 0.9802(9) 0.0480(16) Uani 0.341(6) 1 d D U P A 1
H3A H 0.5479 0.3765 1.0283 0.072 Uiso 0.341(6) 1 calc GR . P A 1
H3B H 0.4986 0.3957 0.9213 0.072 Uiso 0.341(6) 1 calc GR . P A 1
H3C H 0.5299 0.5019 0.9995 0.072 Uiso 0.341(6) 1 calc GR . P A 1
C4 C 0.7554(13) 0.6080(9) 0.9701(8) 0.0498(16) Uani 0.341(6) 1 d D U P A 1
H4A H 0.7238 0.6410 1.0240 0.075 Uiso 0.341(6) 1 calc GR . P A 1
H4B H 0.7074 0.6327 0.9127 0.075 Uiso 0.341(6) 1 calc GR . P A 1
H4C H 0.8564 0.6346 0.9756 0.075 Uiso 0.341(6) 1 calc GR . P A 1
O2A O 0.9233(12) 0.4270(13) 1.0047(12) 0.268(6) Uani 0.659(6) 1 d D U P A 2
S1A S 0.7971(11) 0.4436(8) 1.0349(8) 0.292(4) Uani 0.659(6) 1 d D U P A 2
C3A C 0.7990(18) 0.5801(11) 1.0562(16) 0.249(8) Uani 0.659(6) 1 d D U P A 2
H3AA H 0.8093 0.5987 1.1237 0.374 Uiso 0.659(6) 1 calc GR . P A 2
H3AB H 0.7113 0.5983 1.0248 0.374 Uiso 0.659(6) 1 calc GR . P A 2
H3AC H 0.8775 0.6256 1.0331 0.374 Uiso 0.659(6) 1 calc GR . P A 2
C4A C 0.6321(17) 0.4170(15) 0.9600(13) 0.228(8) Uani 0.659(6) 1 d D U P A 2
H4AA H 0.6455 0.4130 0.8949 0.343 Uiso 0.659(6) 1 calc GR . P A 2
H4AB H 0.5828 0.4795 0.9715 0.343 Uiso 0.659(6) 1 calc GR . P A 2
H4AC H 0.5769 0.3437 0.9723 0.343 Uiso 0.659(6) 1 calc GR . P A 2
H007 H -0.374(6) 0.127(5) -0.077(4) 0.099(18) Uiso 1 1 d . . . . .
H002 H 1.447(4) 0.143(5) 0.987(3) 0.12(2) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S001 O003 1.499(2) . ?
S001 C019 1.789(3) . ?
S001 C01B 1.775(4) . ?
O002 C00X 1.289(3) . ?
O002 H002 1.01(2) . ?
O004 C011 1.257(3) . ?
O005 C00X 1.254(3) . ?
N006 H006 0.8800 . ?
N006 C00A 1.380(3) . ?
N006 C00E 1.372(3) . ?
O007 C011 1.283(3) . ?
O007 H007 0.90(5) . ?
N008 C009 1.385(3) . ?
N008 C00E 1.323(3) . ?
C009 C00A 1.412(3) . ?
C009 C00Q 1.408(3) . ?
C00A C00S 1.402(4) . ?
C00C C00J 1.378(3) . ?
C00C C00Q 1.483(3) . ?
C00C C010 1.423(4) . ?
C00D C00H 1.426(3) . ?
C00D C00J 1.413(3) . ?
C00D C00U 1.418(3) . ?
C00E C00N 1.466(4) . ?
C00F H00F 0.9500 . ?
C00F C00I 1.364(3) . ?
C00F C00W 1.417(3) . ?
C00G H00G 0.9500 . ?
C00G C00O 1.413(4) . ?
C00G C00U 1.368(3) . ?
C00H C00K 1.415(3) . ?
C00H C00R 1.419(3) . ?
C00I H00I 0.9500 . ?
C00I C013 1.417(4) . ?
C00J H00J 0.9500 . ?
C00K H00K 0.9500 . ?
C00K C00O 1.377(4) . ?
C00L H00L 0.9500 . ?
C00L C00M 1.403(3) . ?
C00L C00Q 1.387(4) . ?
C00M H00M 0.9500 . ?
C00M C00S 1.394(4) . ?
C00N C014 1.386(4) . ?
C00N C017 1.392(4) . ?
C00O C00X 1.481(3) . ?
C00R H00R 0.9500 . ?
C00R C010 1.368(4) . ?
C00S C00V 1.481(3) . ?
C00T H00T 0.9500 . ?
C00T C00V 1.380(3) . ?
C00T C00W 1.413(3) . ?
C00U H00U 0.9500 . ?
C00V C00Z 1.417(4) . ?
C00W C00Y 1.425(4) . ?
C00Y C012 1.417(3) . ?
C00Y C015 1.420(4) . ?
C00Z H00Z 0.9500 . ?
C00Z C015 1.371(4) . ?
C010 H010 0.9500 . ?
C011 C013 1.475(3) . ?
C012 H012 0.9500 . ?
C012 C013 1.378(4) . ?
C014 H014 0.9500 . ?
C014 C016 1.387(4) . ?
C015 H015 0.9500 . ?
C016 H016 0.9500 . ?
C016 C018 1.384(5) . ?
C017 H017 0.9500 . ?
C017 C01A 1.389(4) . ?
C018 H018 0.9500 . ?
C018 C01A 1.379(5) . ?
C019 H01B 0.9800 . ?
C019 H01C 0.9800 . ?
C019 H01D 0.9800 . ?
C01A H01A 0.9500 . ?
C01B H01E 0.9800 . ?
C01B H01F 0.9800 . ?
C01B H01G 0.9800 . ?
S1 O2 1.381(7) . ?
S1 C3 1.601(9) . ?
S1 C4 1.743(11) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
O2A S1A 1.434(10) . ?
S1A C3A 1.626(11) . ?
S1A C4A 1.775(14) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 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
O003 S001 C019 105.69(16) . . ?
O003 S001 C01B 105.76(17) . . ?
C01B S001 C019 97.56(18) . . ?
C00X O002 H002 113(3) . . ?
C00A N006 H006 126.4 . . ?
C00E N006 H006 126.4 . . ?
C00E N006 C00A 107.2(2) . . ?
C011 O007 H007 105(3) . . ?
C00E N008 C009 104.7(2) . . ?
N008 C009 C00A 110.4(2) . . ?
N008 C009 C00Q 128.5(2) . . ?
C00Q C009 C00A 121.0(2) . . ?
N006 C00A C009 104.7(2) . . ?
N006 C00A C00S 132.5(2) . . ?
C00S C00A C009 122.6(2) . . ?
C00J C00C C00Q 120.4(2) . . ?
C00J C00C C010 118.6(2) . . ?
C010 C00C C00Q 121.0(2) . . ?
C00J C00D C00H 118.9(2) . . ?
C00J C00D C00U 122.1(2) . . ?
C00U C00D C00H 119.0(2) . . ?
N006 C00E C00N 124.1(2) . . ?
N008 C00E N006 112.9(2) . . ?
N008 C00E C00N 123.0(2) . . ?
C00I C00F H00F 119.5 . . ?
C00I C00F C00W 121.1(2) . . ?
C00W C00F H00F 119.5 . . ?
C00O C00G H00G 120.1 . . ?
C00U C00G H00G 120.1 . . ?
C00U C00G C00O 119.9(2) . . ?
C00K C00H C00D 118.8(2) . . ?
C00K C00H C00R 122.5(2) . . ?
C00R C00H C00D 118.7(2) . . ?
C00F C00I H00I 119.9 . . ?
C00F C00I C013 120.2(2) . . ?
C013 C00I H00I 119.9 . . ?
C00C C00J C00D 121.8(2) . . ?
C00C C00J H00J 119.1 . . ?
C00D C00J H00J 119.1 . . ?
C00H C00K H00K 119.7 . . ?
C00O C00K C00H 120.6(2) . . ?
C00O C00K H00K 119.7 . . ?
C00M C00L H00L 118.9 . . ?
C00Q C00L H00L 118.9 . . ?
C00Q C00L C00M 122.3(2) . . ?
C00L C00M H00M 118.8 . . ?
C00S C00M C00L 122.4(2) . . ?
C00S C00M H00M 118.8 . . ?
C014 C00N C00E 122.7(3) . . ?
C014 C00N C017 119.3(3) . . ?
C017 C00N C00E 118.0(2) . . ?
C00G C00O C00X 118.7(2) . . ?
C00K C00O C00G 120.6(2) . . ?
C00K C00O C00X 120.7(2) . . ?
C009 C00Q C00C 121.8(2) . . ?
C00L C00Q C009 116.3(2) . . ?
C00L C00Q C00C 121.9(2) . . ?
C00H C00R H00R 119.6 . . ?
C010 C00R C00H 120.8(2) . . ?
C010 C00R H00R 119.6 . . ?
C00A C00S C00V 123.2(2) . . ?
C00M C00S C00A 115.4(2) . . ?
C00M C00S C00V 121.4(2) . . ?
C00V C00T H00T 119.1 . . ?
C00V C00T C00W 121.9(2) . . ?
C00W C00T H00T 119.1 . . ?
C00D C00U H00U 119.5 . . ?
C00G C00U C00D 121.1(2) . . ?
C00G C00U H00U 119.5 . . ?
C00T C00V C00S 120.6(2) . . ?
C00T C00V C00Z 118.6(2) . . ?
C00Z C00V C00S 120.9(2) . . ?
C00F C00W C00Y 119.1(2) . . ?
C00T C00W C00F 122.0(2) . . ?
C00T C00W C00Y 119.0(2) . . ?
O002 C00X C00O 117.2(2) . . ?
O005 C00X O002 123.2(2) . . ?
O005 C00X C00O 119.6(2) . . ?
C012 C00Y C00W 118.8(2) . . ?
C012 C00Y C015 122.7(2) . . ?
C015 C00Y C00W 118.5(2) . . ?
C00V C00Z H00Z 119.4 . . ?
C015 C00Z C00V 121.2(2) . . ?
C015 C00Z H00Z 119.4 . . ?
C00C C010 H010 119.4 . . ?
C00R C010 C00C 121.1(2) . . ?
C00R C010 H010 119.4 . . ?
O004 C011 O007 123.3(2) . . ?
O004 C011 C013 119.5(2) . . ?
O007 C011 C013 117.2(2) . . ?
C00Y C012 H012 119.7 . . ?
C013 C012 C00Y 120.7(2) . . ?
C013 C012 H012 119.7 . . ?
C00I C013 C011 119.0(2) . . ?
C012 C013 C00I 120.2(2) . . ?
C012 C013 C011 120.8(2) . . ?
C00N C014 H014 119.8 . . ?
C00N C014 C016 120.4(3) . . ?
C016 C014 H014 119.8 . . ?
C00Y C015 H015 119.6 . . ?
C00Z C015 C00Y 120.8(2) . . ?
C00Z C015 H015 119.6 . . ?
C014 C016 H016 120.0 . . ?
C018 C016 C014 120.0(3) . . ?
C018 C016 H016 120.0 . . ?
C00N C017 H017 120.0 . . ?
C01A C017 C00N 120.0(3) . . ?
C01A C017 H017 120.0 . . ?
C016 C018 H018 120.0 . . ?
C01A C018 C016 119.9(3) . . ?
C01A C018 H018 120.0 . . ?
S001 C019 H01B 109.5 . . ?
S001 C019 H01C 109.5 . . ?
S001 C019 H01D 109.5 . . ?
H01B C019 H01C 109.5 . . ?
H01B C019 H01D 109.5 . . ?
H01C C019 H01D 109.5 . . ?
C017 C01A H01A 119.8 . . ?
C018 C01A C017 120.3(3) . . ?
C018 C01A H01A 119.8 . . ?
S001 C01B H01E 109.5 . . ?
S001 C01B H01F 109.5 . . ?
S001 C01B H01G 109.5 . . ?
H01E C01B H01F 109.5 . . ?
H01E C01B H01G 109.5 . . ?
H01F C01B H01G 109.5 . . ?
O2 S1 C3 106.8(5) . . ?
O2 S1 C4 107.8(5) . . ?
C3 S1 C4 103.4(6) . . ?
S1 C3 H3A 109.5 . . ?
S1 C3 H3B 109.5 . . ?
S1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S1 C4 H4A 109.5 . . ?
S1 C4 H4B 109.5 . . ?
S1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2A S1A C3A 110.6(10) . . ?
O2A S1A C4A 123.3(13) . . ?
C3A S1A C4A 94.0(10) . . ?
S1A C3A H3AA 109.5 . . ?
S1A C3A H3AB 109.5 . . ?
S1A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
S1A C4A H4AA 109.5 . . ?
S1A C4A H4AB 109.5 . . ?
S1A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 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
O004 C011 C013 C00I 2.3(4) . . . . ?
O004 C011 C013 C012 -176.7(3) . . . . ?
N006 C00A C00S C00M 174.1(3) . . . . ?
N006 C00A C00S C00V -6.8(4) . . . . ?
N006 C00E C00N C014 -28.7(4) . . . . ?
N006 C00E C00N C017 153.5(3) . . . . ?
O007 C011 C013 C00I -179.0(3) . . . . ?
O007 C011 C013 C012 1.9(4) . . . . ?
N008 C009 C00A N006 0.4(3) . . . . ?
N008 C009 C00A C00S 176.6(2) . . . . ?
N008 C009 C00Q C00C 3.4(4) . . . . ?
N008 C009 C00Q C00L -175.1(2) . . . . ?
N008 C00E C00N C014 151.9(3) . . . . ?
N008 C00E C00N C017 -25.9(4) . . . . ?
C009 N008 C00E N006 0.2(3) . . . . ?
C009 N008 C00E C00N 179.6(2) . . . . ?
C009 C00A C00S C00M -0.9(4) . . . . ?
C009 C00A C00S C00V 178.2(2) . . . . ?
C00A N006 C00E N008 0.1(3) . . . . ?
C00A N006 C00E C00N -179.4(2) . . . . ?
C00A C009 C00Q C00C 179.5(2) . . . . ?
C00A C009 C00Q C00L 1.0(4) . . . . ?
C00A C00S C00V C00T -43.3(4) . . . . ?
C00A C00S C00V C00Z 138.1(3) . . . . ?
C00D C00H C00K C00O 1.0(4) . . . . ?
C00D C00H C00R C010 0.0(4) . . . . ?
C00E N006 C00A C009 -0.3(3) . . . . ?
C00E N006 C00A C00S -176.0(3) . . . . ?
C00E N008 C009 C00A -0.4(3) . . . . ?
C00E N008 C009 C00Q 176.1(3) . . . . ?
C00E C00N C014 C016 -177.6(3) . . . . ?
C00E C00N C017 C01A 177.4(3) . . . . ?
C00F C00I C013 C011 -176.8(2) . . . . ?
C00F C00I C013 C012 2.3(4) . . . . ?
C00F C00W C00Y C012 1.3(4) . . . . ?
C00F C00W C00Y C015 -178.9(2) . . . . ?
C00G C00O C00X O002 179.9(2) . . . . ?
C00G C00O C00X O005 -1.4(4) . . . . ?
C00H C00D C00J C00C 1.1(4) . . . . ?
C00H C00D C00U C00G 1.6(4) . . . . ?
C00H C00K C00O C00G 1.5(4) . . . . ?
C00H C00K C00O C00X -175.7(2) . . . . ?
C00H C00R C010 C00C 1.5(4) . . . . ?
C00I C00F C00W C00T 178.9(2) . . . . ?
C00I C00F C00W C00Y -0.8(4) . . . . ?
C00J C00C C00Q C009 -139.0(3) . . . . ?
C00J C00C C00Q C00L 39.4(4) . . . . ?
C00J C00C C010 C00R -1.6(4) . . . . ?
C00J C00D C00H C00K 178.3(2) . . . . ?
C00J C00D C00H C00R -1.2(4) . . . . ?
C00J C00D C00U C00G -179.2(2) . . . . ?
C00K C00H C00R C010 -179.5(2) . . . . ?
C00K C00O C00X O002 -2.8(4) . . . . ?
C00K C00O C00X O005 175.8(3) . . . . ?
C00L C00M C00S C00A 1.0(4) . . . . ?
C00L C00M C00S C00V -178.1(2) . . . . ?
C00M C00L C00Q C009 -0.9(4) . . . . ?
C00M C00L C00Q C00C -179.4(2) . . . . ?
C00M C00S C00V C00T 135.7(3) . . . . ?
C00M C00S C00V C00Z -42.9(4) . . . . ?
C00N C014 C016 C018 -0.1(5) . . . . ?
C00N C017 C01A C018 0.7(5) . . . . ?
C00O C00G C00U C00D 0.9(4) . . . . ?
C00Q C009 C00A N006 -176.3(2) . . . . ?
C00Q C009 C00A C00S -0.1(4) . . . . ?
C00Q C00C C00J C00D 179.1(2) . . . . ?
C00Q C00C C010 C00R 179.6(2) . . . . ?
C00Q C00L C00M C00S -0.1(4) . . . . ?
C00R C00H C00K C00O -179.5(2) . . . . ?
C00S C00V C00Z C015 179.7(3) . . . . ?
C00T C00V C00Z C015 1.0(4) . . . . ?
C00T C00W C00Y C012 -178.4(2) . . . . ?
C00T C00W C00Y C015 1.4(4) . . . . ?
C00U C00D C00H C00K -2.5(4) . . . . ?
C00U C00D C00H C00R 178.0(2) . . . . ?
C00U C00D C00J C00C -178.1(2) . . . . ?
C00U C00G C00O C00K -2.5(4) . . . . ?
C00U C00G C00O C00X 174.8(2) . . . . ?
C00V C00T C00W C00F -179.8(2) . . . . ?
C00V C00T C00W C00Y -0.2(4) . . . . ?
C00V C00Z C015 C00Y 0.3(4) . . . . ?
C00W C00F C00I C013 -1.0(4) . . . . ?
C00W C00T C00V C00S -179.7(2) . . . . ?
C00W C00T C00V C00Z -1.0(4) . . . . ?
C00W C00Y C012 C013 0.0(4) . . . . ?
C00W C00Y C015 C00Z -1.5(4) . . . . ?
C00Y C012 C013 C00I -1.7(4) . . . . ?
C00Y C012 C013 C011 177.3(3) . . . . ?
C010 C00C C00J C00D 0.2(4) . . . . ?
C010 C00C C00Q C009 39.8(3) . . . . ?
C010 C00C C00Q C00L -141.7(3) . . . . ?
C012 C00Y C015 C00Z 178.3(3) . . . . ?
C014 C00N C017 C01A -0.5(5) . . . . ?
C014 C016 C018 C01A 0.3(5) . . . . ?
C015 C00Y C012 C013 -179.8(3) . . . . ?
C016 C018 C01A C017 -0.6(6) . . . . ?
C017 C00N C014 C016 0.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_fm-3_sq
_database_code_depnum_ccdc_archive 'CCDC 2120874'
loop_
_audit_author_name
_audit_author_address
'Kelong ZHU'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2022-04-19 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_audit_creation_date             2022-04-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C210 H128 N12 O32 Zr6, 35[H2O], 13[C3H7NO]'
_chemical_formula_sum            'C249 H289 N25 O80 Zr6'
_chemical_formula_weight         5459.35
_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'
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      cubic
_space_group_IT_number           202
_space_group_name_H-M_alt        'F m -3'
_space_group_name_Hall           '-F 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x, y+1/2, z+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x, -y+1/2, -z+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'x, y+1/2, -z+1/2'
'-x, y+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, -y+1/2, -z'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   38.4865(7)
_cell_length_b                   38.4865(7)
_cell_length_c                   38.4865(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     57007(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3597
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      43.6230
_cell_measurement_theta_min      4.9840
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.909
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             11352
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9487
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        43.845
_diffrn_reflns_theta_max         43.845
_diffrn_reflns_theta_min         3.809
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.5826
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1442
_reflns_number_total             1886
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.1352
_refine_ls_restrained_S_all      1.713
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3408
_refine_ls_wR_factor_ref         0.3661
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.528(14)
 0.472(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C3-C1 = C12-C10 = C19-C18 = C26-C15 = C35-C33
 1.5 with sigma of 0.02
 C1-O2 = C1-O3 = C35-O4 = C35-O5
 1.25 with sigma of 0.02
 N1-C17 = N1-C18 = N2-C18 = N2-C16
 1.35 with sigma of 0.02
 C16-C18 = C18-C17 = C17-N2 = N2-N1 = N1-C16
 2.35 with sigma of 0.02
 C1-C2 \\sim C1-C4 \\sim C10-C17 \\sim C10-C13 \\sim C12-C9 \\sim C12-C11 \\sim
C18-C20 \\sim C18-C24 ~
 C15-C25 \\sim C15-C27 \\sim C26-C14 \\sim C26-C16 \\sim C35-C32 \\sim C35-C34
 with sigma of 0.02
 O2-C3 \\sim O3-C3 \\sim O4-C33 \\sim O5-C33
 with sigma of 0.01
 N1-C19 \\sim N2-C19
 with sigma of 0.01
4. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma of 0.1
 C15, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35
 with sigma of 0.1
 O2, O3, C1, C3
 with sigma of 0.01
 O4, O5, C33, C35
 with sigma of 0.01
 N1, N2, C10, C12, C13, C14, C15, C16, C17, C18, C19, C26
 with sigma of 0.1
 C18, C19, C20, C21, C22, C23, C24
 with sigma of 0.1
5. Rigid bond restraints
 Zr1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O4 \\sim O5 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C24 \\sim
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C25 \\sim C26 \\sim C27 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
7. Others
 Fixed Sof: H1A(0.33333) O2(0.25) O3(0.25) O4(0.25) O5(0.25) N1(0.25)
 H1(0.125) N2(0.25) H2(0.125) C1(0.25) C2(0.25) H2A(0.25) C3(0.25) C4(0.25)
 H4(0.25) C5(0.25) H5(0.25) C6(0.25) C7(0.25) C8(0.25) H8(0.25) C9(0.25)
 H9(0.25) C10(0.25) C11(0.25) H11(0.25) C12(0.25) C13(0.25) H13(0.25) C14(0.25)
 H14(0.25) C15(0.25) C16(0.25) C17(0.25) C18(0.25) C24(0.25) H24(0.25)
 C19(0.25) C20(0.25) H20(0.25) C21(0.25) H21(0.25) C22(0.25) H22(0.25)
 C23(0.25) H23(0.25) C25(0.25) H25(0.25) C26(0.25) C27(0.25) H27(0.25)
 C28(0.25) H28(0.25) C29(0.25) C30(0.25) C31(0.25) H31(0.25) C32(0.25)
 H32(0.25) C33(0.25) C34(0.25) H34(0.25) C35(0.25)
8.a Riding coordinates:
 O1(H1A)
8.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C13(H13),
 C14(H14), C24(H24), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27),
  C28(H28), C31(H31), C32(H32), C34(H34)
8.c Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C24(C19,C20,C21,C22,C23)
8.d Naphthalene refined as free rotating group:
 C2(C3,C4,C5,C6,C7,C8,C9,C10,C11), C25(C26,C27,C28,C29,C30,C31,C32,C33,C34)
;
_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 0.43611(4) 0.000000 1.000000 0.1837(15) Uani 1 4 d S TU P . .
O1 O 0.46906(15) 0.03094(15) 0.96906(15) 0.184(4) Uani 1 3 d S T P . .
H1A H 0.464762 0.026250 0.947280 0.276 Uiso 0.3333 1 d R U P . .
O2 O 0.4112(12) 0.0507(6) 0.9923(19) 0.25(2) Uani 0.25 1 d D U P A -1
O3 O 0.4544(6) 0.0907(5) 0.9908(14) 0.18(2) Uani 0.25 1 d D U P A -1
O4 O 0.0691(8) 0.4176(15) 0.996(3) 0.44(4) Uani 0.25 1 d D U P A -1
O5 O 0.1000(8) 0.4611(8) 0.998(2) 0.31(3) Uani 0.25 1 d D U P A -1
N1 N 0.2958(5) 0.2444(5) 0.9088(6) 0.44(2) Uani 0.25 1 d D U P A -1
H1 H 0.311332 0.228725 0.902833 0.523 Uiso 0.125 1 calc R U P A -1
N2 N 0.2512(6) 0.2849(6) 0.9068(6) 0.46(2) Uani 0.25 1 d D U P A -1
H2 H 0.234463 0.298583 0.899209 0.548 Uiso 0.125 1 calc R U P A -1
C1 C 0.4224(7) 0.0825(7) 0.9908(8) 0.27(2) Uani 0.25 1 d D U P A -1
C2 C 0.4040(5) 0.1436(6) 0.9787(7) 0.265(17) Uani 0.25 1 d DG U P A -1
H2A H 0.427257 0.148800 0.972436 0.318 Uiso 0.25 1 calc R U P A -1
C3 C 0.3953(6) 0.1109(5) 0.9890(7) 0.224(15) Uani 0.25 1 d DG U P A -1
C4 C 0.3620(7) 0.1034(5) 0.9980(11) 0.267(17) Uani 0.25 1 d DG U P A -1
H4 H 0.355949 0.080611 1.005190 0.321 Uiso 0.25 1 calc R U P A -1
C5 C 0.3372(6) 0.1286(6) 0.9966(12) 0.313(19) Uani 0.25 1 d G U P A -1
H5 H 0.313936 0.123411 1.002829 0.376 Uiso 0.25 1 calc R U P A -1
C6 C 0.3459(5) 0.1613(5) 0.9862(7) 0.302(17) Uani 0.25 1 d G U P A -1
C7 C 0.3792(5) 0.1688(5) 0.9773(5) 0.292(16) Uani 0.25 1 d G U P A -1
C8 C 0.3878(6) 0.2014(6) 0.9670(10) 0.306(18) Uani 0.25 1 d G U P A -1
H8 H 0.411147 0.206669 0.960708 0.368 Uiso 0.25 1 calc R U P A -1
C9 C 0.3631(7) 0.2266(6) 0.9656(9) 0.319(19) Uani 0.25 1 d DG U P A -1
H9 H 0.369135 0.249470 0.958346 0.382 Uiso 0.25 1 calc R U P A -1
C10 C 0.3298(6) 0.2192(6) 0.9745(7) 0.369(19) Uani 0.25 1 d DG U P A -1
C11 C 0.3211(5) 0.1865(6) 0.9849(9) 0.326(19) Uani 0.25 1 d DG U P A -1
H11 H 0.297825 0.181283 0.991100 0.392 Uiso 0.25 1 calc R U P A -1
C12 C 0.3013(6) 0.2457(6) 0.9741(5) 0.418(19) Uani 0.25 1 d DG U P A -1
C13 C 0.2890(7) 0.2594(6) 1.0042(5) 0.47(2) Uani 0.25 1 d DG U P A -1
H13 H 0.298685 0.252454 1.025824 0.566 Uiso 0.25 1 calc R U P A -1
C14 C 0.2627(8) 0.2830(7) 1.0035(5) 0.48(2) Uani 0.25 1 d DG U P A -1
H14 H 0.254085 0.292599 1.024542 0.571 Uiso 0.25 1 calc R U P A -1
C15 C 0.2488(7) 0.2930(7) 0.9726(6) 0.47(2) Uani 0.25 1 d DG U P A -1
C16 C 0.2611(6) 0.2793(6) 0.9424(5) 0.45(2) Uani 0.25 1 d DG U P A -1
C17 C 0.2874(5) 0.2557(5) 0.9432(5) 0.44(2) Uani 0.25 1 d DG U P A -1
C18 C 0.2739(7) 0.2640(7) 0.8860(5) 0.396(19) Uani 0.25 1 d D U P A -1
C24 C 0.2706(7) 0.2887(4) 0.8263(6) 0.270(18) Uani 0.25 1 d DG U P A -1
H24 H 0.271757 0.311463 0.835809 0.324 Uiso 0.25 1 calc R U P A -1
C19 C 0.2718(5) 0.2599(5) 0.8481(4) 0.285(15) Uani 0.25 1 d DG U P A -1
C20 C 0.2701(5) 0.2267(4) 0.8341(4) 0.105(6) Uani 0.25 1 d DG U P A -1
H20 H 0.270969 0.206988 0.849019 0.126 Uiso 0.25 1 calc R U P A -1
C21 C 0.2672(6) 0.2222(5) 0.7984(4) 0.196(13) Uani 0.25 1 d G U P A -1
H21 H 0.266089 0.199422 0.788889 0.235 Uiso 0.25 1 calc R U P A -1
C22 C 0.2660(6) 0.2509(7) 0.7766(4) 0.223(16) Uani 0.25 1 d G U P A -1
H22 H 0.264044 0.247876 0.752219 0.268 Uiso 0.25 1 calc R U P A -1
C23 C 0.2677(7) 0.2842(6) 0.7906(5) 0.212(16) Uani 0.25 1 d G U P A -1
H23 H 0.266878 0.303896 0.775678 0.254 Uiso 0.25 1 calc R U P A -1
C25 C 0.2112(7) 0.3376(8) 1.0004(8) 0.46(3) Uani 0.25 1 d DG U P A -1
H25 H 0.224423 0.334934 1.021080 0.547 Uiso 0.25 1 calc R U P A -1
C26 C 0.2191(7) 0.3184(7) 0.9718(7) 0.46(2) Uani 0.25 1 d DG U P A -1
C27 C 0.2002(12) 0.3222(13) 0.9422(8) 0.43(3) Uani 0.25 1 d DG U P A -1
H27 H 0.205745 0.308797 0.922209 0.518 Uiso 0.25 1 calc R U P A -1
C28 C 0.1734(14) 0.3451(14) 0.9412(9) 0.43(3) Uani 0.25 1 d G U P A -1
H28 H 0.160144 0.347787 0.920517 0.520 Uiso 0.25 1 calc R U P A -1
C29 C 0.1654(8) 0.3643(8) 0.9698(9) 0.42(2) Uani 0.25 1 d G U P A -1
C30 C 0.1844(7) 0.3605(7) 0.9994(8) 0.42(2) Uani 0.25 1 d G U P A -1
C31 C 0.1764(11) 0.3797(13) 1.0280(10) 0.41(3) Uani 0.25 1 d G U P A -1
H31 H 0.189652 0.377059 1.048690 0.488 Uiso 0.25 1 calc R U P A -1
C32 C 0.1496(11) 0.4027(12) 1.0270(12) 0.41(3) Uani 0.25 1 d DG U P A -1
H32 H 0.144051 0.416048 1.047000 0.496 Uiso 0.25 1 calc R U P A -1
C33 C 0.1307(8) 0.4064(8) 0.9974(12) 0.42(2) Uani 0.25 1 d DG U P A -1
C34 C 0.1386(10) 0.3873(10) 0.9688(11) 0.42(3) Uani 0.25 1 d DG U P A -1
H34 H 0.125371 0.389914 0.948129 0.505 Uiso 0.25 1 calc R U P A -1
C35 C 0.0994(9) 0.4296(8) 0.9972(14) 0.39(3) Uani 0.25 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 Zr1 3.4775(19) 86_656 ?
Zr1 Zr1 3.4775(19) 27_545 ?
Zr1 Zr1 3.4775(19) 38_446 ?
Zr1 Zr1 3.4775(19) 75_566 ?
Zr1 O1 2.108(3) 75_566 ?
Zr1 O1 2.108(3) 38_446 ?
Zr1 O1 2.108(3) 91_446 ?
Zr1 O1 2.108(3) . ?
Zr1 H1A 1.745(7) 41_456 ?
Zr1 H1A 1.745(6) 38_446 ?
Zr1 H1A 1.745(6) 91_446 ?
Zr1 H1A 1.745(7) 92_456 ?
Zr1 O2 2.19(2) . ?
O1 H1A 0.8733 . ?
O1 H1A 0.8733 28_565 ?
O1 H1A 0.8733 41_456 ?
O2 C1 1.30(2) . ?
O3 C1 1.273(19) . ?
O4 C35 1.26(2) . ?
O5 C35 1.21(2) . ?
N1 H1 0.8800 . ?
N1 C17 1.430(16) . ?
N1 C18 1.431(17) . ?
N2 H2 0.8800 . ?
N2 C16 1.440(16) . ?
N2 C18 1.433(17) . ?
C1 C3 1.510(12) . ?
C2 H2A 0.9500 . ?
C2 C3 1.3600 . ?
C2 C7 1.3600 . ?
C3 C4 1.3600 . ?
C4 H4 0.9500 . ?
C4 C5 1.3600 . ?
C5 H5 0.9500 . ?
C5 C6 1.3600 . ?
C6 C7 1.3600 . ?
C6 C11 1.3600 . ?
C7 C8 1.3600 . ?
C8 H8 0.9500 . ?
C8 C9 1.3600 . ?
C9 H9 0.9500 . ?
C9 C10 1.3600 . ?
C10 C11 1.3600 . ?
C10 C12 1.498(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.3600 . ?
C12 C17 1.3600 . ?
C13 H13 0.9500 . ?
C13 C14 1.3600 . ?
C14 H14 0.9500 . ?
C14 C15 1.3600 . ?
C15 C16 1.3600 . ?
C15 C26 1.503(11) . ?
C16 C17 1.3600 . ?
C18 C19 1.469(12) . ?
C24 H24 0.9500 . ?
C24 C19 1.3900 . ?
C24 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 H20 0.9500 . ?
C20 C21 1.3900 . ?
C21 H21 0.9500 . ?
C21 C22 1.3900 . ?
C22 H22 0.9500 . ?
C22 C23 1.3900 . ?
C23 H23 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.3600 . ?
C25 C30 1.3600 . ?
C26 C27 1.3600 . ?
C27 H27 0.9500 . ?
C27 C28 1.3600 . ?
C28 H28 0.9500 . ?
C28 C29 1.3600 . ?
C29 C30 1.3600 . ?
C29 C34 1.3600 . ?
C30 C31 1.3600 . ?
C31 H31 0.9500 . ?
C31 C32 1.3600 . ?
C32 H32 0.9500 . ?
C32 C33 1.3600 . ?
C33 C34 1.3600 . ?
C33 C35 1.497(13) . ?
C34 H34 0.9500 . ?

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
Zr1 Zr1 Zr1 60.0 86_656 27_545 ?
Zr1 Zr1 Zr1 90.0 86_656 38_446 ?
Zr1 Zr1 Zr1 90.0 75_566 27_545 ?
Zr1 Zr1 Zr1 60.0 27_545 38_446 ?
Zr1 Zr1 Zr1 60.0 75_566 38_446 ?
Zr1 Zr1 Zr1 60.0 86_656 75_566 ?
Zr1 Zr1 H1A 112.0(2) 86_656 91_446 ?
Zr1 Zr1 H1A 54.29(15) 27_545 91_446 ?
Zr1 Zr1 H1A 112.0(2) 86_656 38_446 ?
Zr1 Zr1 H1A 43.6(2) 38_446 38_446 ?
Zr1 Zr1 H1A 103.6(2) 75_566 91_446 ?
Zr1 Zr1 H1A 103.6(2) 75_566 41_456 ?
Zr1 Zr1 H1A 43.6(2) 38_446 91_446 ?
Zr1 Zr1 H1A 103.6(2) 27_545 92_456 ?
Zr1 Zr1 H1A 43.6(2) 86_656 92_456 ?
Zr1 Zr1 H1A 103.6(2) 27_545 38_446 ?
Zr1 Zr1 H1A 112.0(2) 38_446 92_456 ?
Zr1 Zr1 H1A 54.29(15) 27_545 41_456 ?
Zr1 Zr1 H1A 54.29(15) 75_566 38_446 ?
Zr1 Zr1 H1A 54.29(15) 75_566 92_456 ?
Zr1 Zr1 H1A 43.6(2) 86_656 41_456 ?
Zr1 Zr1 H1A 112.0(2) 38_446 41_456 ?
O1 Zr1 Zr1 34.43(12) 38_446 38_446 ?
O1 Zr1 Zr1 88.5(2) . 75_566 ?
O1 Zr1 Zr1 88.5(2) 75_566 38_446 ?
O1 Zr1 Zr1 88.5(2) 38_446 27_545 ?
O1 Zr1 Zr1 34.43(12) 75_566 86_656 ?
O1 Zr1 Zr1 34.43(12) . 86_656 ?
O1 Zr1 Zr1 88.5(2) . 38_446 ?
O1 Zr1 Zr1 34.43(12) 75_566 75_566 ?
O1 Zr1 Zr1 88.5(2) 38_446 86_656 ?
O1 Zr1 Zr1 88.5(2) 91_446 86_656 ?
O1 Zr1 Zr1 88.5(2) 75_566 27_545 ?
O1 Zr1 Zr1 88.5(2) 91_446 75_566 ?
O1 Zr1 Zr1 34.43(12) 91_446 38_446 ?
O1 Zr1 Zr1 34.43(12) 91_446 27_545 ?
O1 Zr1 Zr1 34.43(12) . 27_545 ?
O1 Zr1 Zr1 34.43(12) 38_446 75_566 ?
O1 Zr1 O1 68.8(3) 91_446 38_446 ?
O1 Zr1 O1 68.8(3) 91_446 . ?
O1 Zr1 O1 68.8(3) 75_566 . ?
O1 Zr1 O1 106.0(5) 38_446 . ?
O1 Zr1 O1 68.8(3) 75_566 38_446 ?
O1 Zr1 O1 106.0(5) 75_566 91_446 ?
O1 Zr1 H1A 23.90(2) . 41_456 ?
O1 Zr1 H1A 23.90(2) 38_446 38_446 ?
O1 Zr1 H1A 128.1(5) 75_566 91_446 ?
O1 Zr1 H1A 87.9(2) 75_566 38_446 ?
O1 Zr1 H1A 87.9(2) . 91_446 ?
O1 Zr1 H1A 128.2(5) . 38_446 ?
O1 Zr1 H1A 87.9(2) 38_446 92_456 ?
O1 Zr1 H1A 23.90(2) 91_446 91_446 ?
O1 Zr1 H1A 87.9(2) 91_446 41_456 ?
O1 Zr1 H1A 128.1(5) 91_446 92_456 ?
O1 Zr1 H1A 74.9(2) 75_566 41_456 ?
O1 Zr1 H1A 128.1(5) 38_446 41_456 ?
O1 Zr1 H1A 74.9(2) 91_446 38_446 ?
O1 Zr1 H1A 74.9(2) 38_446 91_446 ?
O1 Zr1 H1A 74.9(2) . 92_456 ?
O1 Zr1 H1A 23.90(2) 75_566 92_456 ?
O1 Zr1 O2 147.3(17) 38_446 . ?
O1 Zr1 O2 133.6(19) 91_446 . ?
O1 Zr1 O2 80.6(14) 75_566 . ?
O1 Zr1 O2 71.6(16) . . ?
H1A Zr1 H1A 151.5 91_446 92_456 ?
H1A Zr1 H1A 70.8 38_446 91_446 ?
H1A Zr1 H1A 70.8 41_456 92_456 ?
H1A Zr1 H1A 102.0 41_456 91_446 ?
H1A Zr1 H1A 102.0 38_446 92_456 ?
H1A Zr1 H1A 151.5 38_446 41_456 ?
O2 Zr1 Zr1 159.7(14) . 38_446 ?
O2 Zr1 Zr1 113.8(15) . 75_566 ?
O2 Zr1 Zr1 71.3(12) . 86_656 ?
O2 Zr1 Zr1 102.3(17) . 27_545 ?
O2 Zr1 H1A 136.1(19) . 91_446 ?
O2 Zr1 H1A 48.6(16) . 41_456 ?
O2 Zr1 H1A 151.3(19) . 38_446 ?
O2 Zr1 H1A 59.6(16) . 92_456 ?
Zr1 O1 Zr1 111.1(2) 86_656 27_545 ?
Zr1 O1 Zr1 111.1(2) 86_656 . ?
Zr1 O1 Zr1 111.1(2) 27_545 . ?
Zr1 O1 H1A 54.1(2) 86_656 28_565 ?
Zr1 O1 H1A 140.7 86_656 . ?
Zr1 O1 H1A 108.1 . . ?
Zr1 O1 H1A 54.1(2) . 41_456 ?
Zr1 O1 H1A 54.0 27_545 . ?
Zr1 O1 H1A 140.67(13) . 28_565 ?
Zr1 O1 H1A 108.15(13) 86_656 41_456 ?
Zr1 O1 H1A 108.15(13) 27_545 28_565 ?
Zr1 O1 H1A 140.67(13) 27_545 41_456 ?
H1A O1 H1A 93.2 . 41_456 ?
H1A O1 H1A 93.2 28_565 41_456 ?
H1A O1 H1A 93.2 . 28_565 ?
C1 O2 Zr1 134(3) . . ?
C17 N1 H1 127.0 . . ?
C17 N1 C18 105.9(11) . . ?
C18 N1 H1 127.0 . . ?
C16 N2 H2 126.7 . . ?
C18 N2 H2 126.7 . . ?
C18 N2 C16 106.6(11) . . ?
O2 C1 C3 117.2(17) . . ?
O3 C1 O2 124(3) . . ?
O3 C1 C3 119.2(15) . . ?
C3 C2 H2A 120.0 . . ?
C3 C2 C7 120.0 . . ?
C7 C2 H2A 120.0 . . ?
C2 C3 C1 120.9(8) . . ?
C4 C3 C1 119.1(8) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C11 120.0 . . ?
C7 C6 C11 120.0 . . ?
C6 C7 C2 120.0 . . ?
C8 C7 C2 120.0 . . ?
C8 C7 C6 120.0 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 C12 122.9(7) . . ?
C11 C10 C12 117.1(7) . . ?
C6 C11 H11 120.0 . . ?
C10 C11 C6 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C10 120.6(8) . . ?
C13 C12 C17 120.0 . . ?
C17 C12 C10 119.4(8) . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 C26 120.0(7) . . ?
C16 C15 C26 120.0(7) . . ?
C15 C16 N2 131.5(9) . . ?
C17 C16 N2 108.5(9) . . ?
C17 C16 C15 120.0 . . ?
C12 C17 N1 129.4(9) . . ?
C16 C17 N1 110.6(9) . . ?
C16 C17 C12 120.0 . . ?
N1 C18 N2 108.3(12) . . ?
N1 C18 C19 125.8(12) . . ?
N2 C18 C19 125.5(12) . . ?
C19 C24 H24 120.0 . . ?
C19 C24 C23 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C19 C18 121.1(8) . . ?
C24 C19 C20 120.0 . . ?
C20 C19 C18 118.9(7) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 C30 120.0 . . ?
C30 C25 H25 120.0 . . ?
C25 C26 C15 120.5(7) . . ?
C27 C26 C15 119.5(7) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 C34 120.0 . . ?
C30 C29 C34 120.0 . . ?
C29 C30 C25 120.0 . . ?
C31 C30 C25 120.0 . . ?
C31 C30 C29 120.0 . . ?
C30 C31 H31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 C35 120.0(9) . . ?
C34 C33 C35 119.8(8) . . ?
C29 C34 H34 120.0 . . ?
C33 C34 C29 120.0 . . ?
C33 C34 H34 120.0 . . ?
O4 C35 C33 122(2) . . ?
O5 C35 O4 113(3) . . ?
O5 C35 C33 125(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
Zr1 O2 C1 O3 7(4) . . . . ?
Zr1 O2 C1 C3 -173(4) . . . . ?
O2 C1 C3 C2 -163(3) . . . . ?
O2 C1 C3 C4 17(3) . . . . ?
O3 C1 C3 C2 17(3) . . . . ?
O3 C1 C3 C4 -163(3) . . . . ?
N1 C18 C19 C24 -136.8(15) . . . . ?
N1 C18 C19 C20 44.9(17) . . . . ?
N2 C16 C17 N1 -0.5(8) . . . . ?
N2 C16 C17 C12 -179.6(10) . . . . ?
N2 C18 C19 C24 51.6(17) . . . . ?
N2 C18 C19 C20 -126.6(17) . . . . ?
C1 C3 C4 C5 179.9(4) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C2 C7 C8 C9 180.0 . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C3 C2 C7 C8 180.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C11 180.0 . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C5 C6 C7 C8 180.0 . . . . ?
C5 C6 C11 C10 180.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C2 C3 C1 -179.9(4) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C7 C6 C11 C10 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C12 179.1(13) . . . . ?
C9 C10 C11 C6 0.0 . . . . ?
C9 C10 C12 C13 -105.0(18) . . . . ?
C9 C10 C12 C17 76.1(19) . . . . ?
C10 C12 C13 C14 -178.9(10) . . . . ?
C10 C12 C17 N1 -0.1(12) . . . . ?
C10 C12 C17 C16 178.9(10) . . . . ?
C11 C6 C7 C2 180.0 . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C11 C10 C12 C13 74.2(15) . . . . ?
C11 C10 C12 C17 -104.7(15) . . . . ?
C12 C10 C11 C6 -179.2(12) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C12 C17 N1 -179.0(12) . . . . ?
C13 C12 C17 C16 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C26 178.4(12) . . . . ?
C14 C15 C16 N2 179.5(13) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C14 C15 C26 C25 15(2) . . . . ?
C14 C15 C26 C27 -165(2) . . . . ?
C15 C16 C17 N1 179.2(10) . . . . ?
C15 C16 C17 C12 0.0 . . . . ?
C15 C26 C27 C28 -179.9(5) . . . . ?
C16 N2 C18 N1 3.3(12) . . . . ?
C16 N2 C18 C19 176.1(13) . . . . ?
C16 C15 C26 C25 -166(2) . . . . ?
C16 C15 C26 C27 13(2) . . . . ?
C17 N1 C18 N2 -3.5(12) . . . . ?
C17 N1 C18 C19 -176.3(14) . . . . ?
C17 C12 C13 C14 0.0 . . . . ?
C18 N1 C17 C12 -178.4(10) . . . . ?
C18 N1 C17 C16 2.5(10) . . . . ?
C18 N2 C16 C15 178.7(11) . . . . ?
C18 N2 C16 C17 -1.7(10) . . . . ?
C18 C19 C20 C21 178.3(8) . . . . ?
C24 C19 C20 C21 0.0 . . . . ?
C19 C24 C23 C22 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C23 C24 C19 C18 -178.2(8) . . . . ?
C23 C24 C19 C20 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C30 C31 C32 180.0 . . . . ?
C26 C15 C16 N2 1.1(14) . . . . ?
C26 C15 C16 C17 -178.4(12) . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C26 C25 C30 C31 180.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C27 C28 C29 C34 180.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C28 C29 C30 C31 180.0 . . . . ?
C28 C29 C34 C33 180.0 . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C25 C26 C15 179.9(5) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C30 C29 C34 C33 0.0 . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C31 C32 C33 C35 175.2(17) . . . . ?
C32 C33 C34 C29 0.0 . . . . ?
C32 C33 C35 O4 -108(5) . . . . ?
C32 C33 C35 O5 72(5) . . . . ?
C34 C29 C30 C25 180.0 . . . . ?
C34 C29 C30 C31 0.0 . . . . ?
C34 C33 C35 O4 67(5) . . . . ?
C34 C33 C35 O5 -113(5) . . . . ?
C35 C33 C34 C29 -175.2(17) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  
;
A solvent mask was calculated and 3397 electrons were 
found in a volume of 31033Å³ in 1 void per unit cell. 
This is consistent with the presence of 
35[H2O], 13[C3H7NO] per Formula Unit 
which account for 3480 electrons 
per unit cell.

The solvent data was based on TG result.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.010 -0.006 31033 3397 '140 H2O,52 DMF'

_platon_squeeze_void_probe_radius 1.20
# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.528(14)
2 0.472(14)

_vrf_PLAT084_fm-3_sq             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: This alert is caused by significant disorder in the structure.
;
_vrf_PLAT088_fm-3_sq             
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.16 Note  
RESPONSE: This alert is caused by significant disorder in the structure.
;
_vrf_PLAT260_fm-3_sq             
;
PROBLEM: Large Average Ueq of Residue Including       Zr1      0.344 Check 
RESPONSE: This is due to the low quality of the crystals and disorder of ligands.
;
# start Validation Reply Form
_vrf_THETM01_fm-3_sq             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:  Due to the low quality of the crystals data and the
disorder of ligands, it was difficult to reach higher resolution using our
machine for the structure.
;
