# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_t2
_database_code_depnum_ccdc_archive 'CCDC 2092514'
loop_
_audit_author_name
_audit_author_address
'Yang Zou'
;nanjing tech univ
China
;
_audit_update_record             
;
2021-06-26 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_audit_creation_date             2020-07-02
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(F24 H16 O60 P12 Zr12), 10(H4 N)'
_chemical_formula_sum            'F12 H48 N10 O30 P6 Zr6'
_chemical_formula_weight         1629.62
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.502(2)
_cell_length_b                   7.5316(11)
_cell_length_c                   19.141(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.593(4)
_cell_angle_gamma                90
_cell_volume                     2181.0(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.69
_shelx_estimated_absorpt_T_max   0.817
_shelx_estimated_absorpt_T_min   0.710
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4009
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1195 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.5377.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21056
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.643
_diffrn_reflns_theta_min         1.536
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4666
_reflns_number_total             5031
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0098(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0639P)²+5.0405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1046
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups, H2W of O2W, H2 of O8, H1W of O1W
 At 1.5 times of:
  H3W of O3W
2.a Riding coordinates:
 O8(H2), O3W(H3W), O2W(H2W), O1W(H1W), N2(H2A,H2B,H2C,H2D), N1(H1A,H1B,H1C,
 H1D), N4(H4A,H4B,H4C,H4D), N5(H5A,H5B,H5C,H5D), N3(H3A,H3B,H3C,H3D)
;
_atom_sites_solution_hydrogens   difmap
_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 0.29898(2) 0.75748(4) 0.64897(2) 0.01320(11) Uani 1 1 d . . . . .
Zr2 Zr 0.59910(2) 0.54133(4) 0.62817(2) 0.01359(11) Uani 1 1 d . . . . .
Zr3 Zr 0.60092(2) 0.47816(4) 0.90432(2) 0.01385(12) Uani 1 1 d . . . . .
P1 P 0.07833(6) 0.75680(11) 0.54971(5) 0.01388(19) Uani 1 1 d . . . . .
P2 P 0.41503(6) 0.74466(11) 0.51204(5) 0.0148(2) Uani 1 1 d . . . . .
P3 P 0.51522(6) 0.75146(11) 0.75881(5) 0.0146(2) Uani 1 1 d . . . . .
F1 F 0.30724(16) 1.0246(3) 0.65441(13) 0.0264(5) Uani 1 1 d . . . . .
F2 F 0.25065(18) 0.7430(4) 0.73720(14) 0.0394(7) Uani 1 1 d . . . . .
F4 F 0.70123(16) 0.4142(3) 0.69052(12) 0.0290(5) Uani 1 1 d . . . . .
F5 F 0.70601(15) 0.6209(3) 0.90009(14) 0.0320(6) Uani 1 1 d . . . . .
F6 F 0.66987(16) 0.3297(3) 0.98419(12) 0.0302(5) Uani 1 1 d . . . . .
F3 F 0.51458(17) 0.3509(4) 0.64306(13) 0.0345(6) Uani 1 1 d . . . . .
O7 O 0.37360(17) 0.6046(4) 0.45728(14) 0.0222(6) Uani 1 1 d . . . . .
O10 O 0.42074(19) 0.7323(5) 0.71461(17) 0.0329(7) Uani 1 1 d . . . . .
O1 O 0.17073(19) 0.7949(5) 0.59254(17) 0.0338(7) Uani 1 1 d . . . . .
O6 O 0.50128(19) 0.6738(4) 0.55845(15) 0.0297(7) Uani 1 1 d . . . . .
O8 O 0.4352(2) 0.9115(4) 0.47224(16) 0.0312(7) Uani 1 1 d . . . . .
H2 H 0.404739 0.847768 0.439220 0.037 Uiso 1 1 d R . . . .
O12 O 0.5376(2) 0.9399(4) 0.77948(18) 0.0356(7) Uani 1 1 d . . . . .
O5 O 0.35144(19) 0.7907(4) 0.55886(15) 0.0289(6) Uani 1 1 d . . . . .
O9 O 0.57920(18) 0.6800(4) 0.71486(14) 0.0268(6) Uani 1 1 d . . . . .
O11 O 0.52161(18) 0.6336(4) 0.82535(14) 0.0268(6) Uani 1 1 d . . . . .
O4 O 0.06369(19) 0.8460(4) 0.47662(14) 0.0267(6) Uani 1 1 d . . . . .
O3 O 0.01176(19) 0.8264(4) 0.59084(15) 0.0298(7) Uani 1 1 d . . . . .
O2 O 0.0687(2) 0.5554(4) 0.53872(17) 0.0316(7) Uani 1 1 d . . . . .
O3W O 0.62193(17) 0.3111(3) 0.83149(13) 0.0183(5) Uani 1 1 d . . . . .
H3W H 0.646643 0.365412 0.802174 0.027 Uiso 1 1 d R . . . .
O2W O 0.68537(16) 0.7202(3) 0.60645(13) 0.0141(5) Uani 1 1 d . . . . .
H2W H 0.718599 0.722872 0.648107 0.017 Uiso 1 1 d R . . . .
O1W O 0.2892(2) 0.4976(4) 0.62859(18) 0.0309(7) Uani 1 1 d . . . . .
H1W H 0.340728 0.455704 0.631254 0.037 Uiso 1 1 d R . . . .
N2 N 0.4300(2) 1.2395(5) 0.75263(19) 0.0278(8) Uani 1 1 d . . . . .
H2A H 0.471573 1.155701 0.766782 0.033 Uiso 1 1 d R . . . .
H2B H 0.385373 1.190031 0.720492 0.033 Uiso 1 1 d R . . . .
H2C H 0.453263 1.329391 0.731782 0.033 Uiso 1 1 d R . . . .
H2D H 0.409753 1.277341 0.790652 0.033 Uiso 1 1 d R . . . .
N1 N 0.3574(3) 1.2216(5) 0.5453(2) 0.0327(8) Uani 1 1 d . . . . .
H1A H 0.339491 1.167737 0.581637 0.039 Uiso 1 1 d R . . . .
H1B H 0.380951 1.138687 0.521137 0.039 Uiso 1 1 d R . . . .
H1C H 0.396181 1.299527 0.561777 0.039 Uiso 1 1 d R . . . .
H1D H 0.310921 1.273197 0.515917 0.039 Uiso 1 1 d R . . . .
N4 N 0.6654(2) 0.9837(5) 0.9074(2) 0.0289(8) Uani 1 1 d . . . . .
H4A H 0.685226 0.871144 0.912207 0.035 Uiso 1 1 d R . . . .
H4B H 0.622706 0.990184 0.867197 0.035 Uiso 1 1 d R . . . .
H4C H 0.707576 1.052724 0.903717 0.035 Uiso 1 1 d R . . . .
H4D H 0.642706 1.012894 0.945317 0.035 Uiso 1 1 d R . . . .
N5 N 0.6688(3) 0.0471(5) 0.6887(2) 0.0386(9) Uani 1 1 d . . . . .
H5A H 0.686066 0.150877 0.672869 0.046 Uiso 1 1 d R . . . .
H5B H 0.650596 0.069357 0.729349 0.046 Uiso 1 1 d R . . . .
H5C H 0.715776 -0.026083 0.698879 0.046 Uiso 1 1 d R . . . .
H5D H 0.625226 0.007677 0.657629 0.046 Uiso 1 1 d R . . . .
N3 N 0.3586(2) 0.7429(5) 0.87661(19) 0.0301(8) Uani 1 1 d . . . . .
H3A H 0.318485 0.746902 0.834822 0.036 Uiso 1 1 d R . . . .
H3B H 0.410905 0.710942 0.867291 0.036 Uiso 1 1 d R . . . .
H3C H 0.341855 0.662112 0.905641 0.036 Uiso 1 1 d R . . . .
H3D H 0.363445 0.850952 0.897201 0.036 Uiso 1 1 d R . . . .


_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 F1 2.017(2) . ?
Zr1 F2 1.994(2) . ?
Zr1 O10 2.035(3) . ?
Zr1 O1 2.065(3) . ?
Zr1 O5 2.076(3) . ?
Zr1 O1W 1.995(3) . ?
Zr2 F4 2.006(2) . ?
Zr2 F3 2.004(2) . ?
Zr2 O7 2.089(3) 3_666 ?
Zr2 O6 2.048(3) . ?
Zr2 O9 2.040(3) . ?
Zr2 O2W 2.005(2) . ?
Zr3 F5 1.968(2) . ?
Zr3 F6 2.004(2) . ?
Zr3 O11 2.087(3) . ?
Zr3 O4 2.086(3) 4_676 ?
Zr3 O3 2.106(3) 2_546 ?
Zr3 O3W 1.957(2) . ?
P1 O1 1.515(3) . ?
P1 O4 1.524(3) . ?
P1 O3 1.521(3) . ?
P1 O2 1.534(3) . ?
P2 O7 1.527(3) . ?
P2 O6 1.531(3) . ?
P2 O8 1.537(3) . ?
P2 O5 1.510(3) . ?
P3 O10 1.530(3) . ?
P3 O12 1.494(3) . ?
P3 O9 1.531(3) . ?
P3 O11 1.538(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Zr1 O10 91.22(12) . . ?
F1 Zr1 O1 86.20(12) . . ?
F1 Zr1 O5 83.72(12) . . ?
F2 Zr1 F1 92.43(11) . . ?
F2 Zr1 O10 86.64(12) . . ?
F2 Zr1 O1 87.35(13) . . ?
F2 Zr1 O5 176.05(13) . . ?
F2 Zr1 O1W 94.89(13) . . ?
O10 Zr1 O1 173.35(13) . . ?
O10 Zr1 O5 92.61(12) . . ?
O1 Zr1 O5 93.20(13) . . ?
O1W Zr1 F1 171.82(12) . . ?
O1W Zr1 O10 92.86(14) . . ?
O1W Zr1 O1 90.47(14) . . ?
O1W Zr1 O5 89.02(13) . . ?
F4 Zr2 O7 86.93(10) . 3_666 ?
F4 Zr2 O6 175.24(11) . . ?
F4 Zr2 O9 90.01(11) . . ?
F3 Zr2 F4 91.70(11) . . ?
F3 Zr2 O7 89.15(11) . 3_666 ?
F3 Zr2 O6 91.55(12) . . ?
F3 Zr2 O9 91.79(11) . . ?
F3 Zr2 O2W 175.31(10) . . ?
O6 Zr2 O7 89.64(11) . 3_666 ?
O9 Zr2 O7 176.82(11) . 3_666 ?
O9 Zr2 O6 93.37(12) . . ?
O2W Zr2 F4 88.19(11) . . ?
O2W Zr2 O7 86.16(10) . 3_666 ?
O2W Zr2 O6 88.30(12) . . ?
O2W Zr2 O9 92.90(11) . . ?
F5 Zr3 F6 91.58(11) . . ?
F5 Zr3 O11 91.49(12) . . ?
F5 Zr3 O4 91.82(11) . 4_676 ?
F5 Zr3 O3 179.71(12) . 2_546 ?
F6 Zr3 O11 175.73(11) . . ?
F6 Zr3 O4 91.55(11) . 4_676 ?
F6 Zr3 O3 88.47(12) . 2_546 ?
O11 Zr3 O3 88.44(12) . 2_546 ?
O4 Zr3 O11 85.40(11) 4_676 . ?
O4 Zr3 O3 87.89(12) 4_676 2_546 ?
O3W Zr3 F5 93.10(11) . . ?
O3W Zr3 F6 92.33(10) . . ?
O3W Zr3 O11 90.45(11) . . ?
O3W Zr3 O4 173.65(11) . 4_676 ?
O3W Zr3 O3 87.19(12) . 2_546 ?
O1 P1 O4 110.33(18) . . ?
O1 P1 O3 108.82(18) . . ?
O1 P1 O2 108.31(18) . . ?
O4 P1 O2 108.63(17) . . ?
O3 P1 O4 109.95(16) . . ?
O3 P1 O2 110.79(19) . . ?
O7 P2 O6 109.92(16) . . ?
O7 P2 O8 108.98(16) . . ?
O6 P2 O8 109.08(18) . . ?
O5 P2 O7 109.57(17) . . ?
O5 P2 O6 109.66(17) . . ?
O5 P2 O8 109.62(19) . . ?
O10 P3 O9 108.64(17) . . ?
O10 P3 O11 106.53(17) . . ?
O12 P3 O10 112.06(19) . . ?
O12 P3 O9 109.75(19) . . ?
O12 P3 O11 111.09(18) . . ?
O9 P3 O11 108.65(17) . . ?
P2 O7 Zr2 140.75(17) . 3_666 ?
P3 O10 Zr1 168.4(2) . . ?
P1 O1 Zr1 161.2(2) . . ?
P2 O6 Zr2 167.7(2) . . ?
P2 O5 Zr1 152.9(2) . . ?
P3 O9 Zr2 149.04(18) . . ?
P3 O11 Zr3 147.66(18) . . ?
P1 O4 Zr3 151.85(19) . 4_575 ?
P1 O3 Zr3 150.75(18) . 2_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
