# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
# 
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data_LIFM-94
_database_code_depnum_ccdc_archive 'CCDC 1544325'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            LIFM-94
_chemical_melting_point          ?
_chemical_formula_moiety         'C104 H76 N12 O34 Zr6'
_chemical_formula_sum            'C104 H76 N12 O34 Zr6'
_chemical_formula_weight         2585.08

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+1/2'
'-x, -y, z'
'y, -x, z+1/2'
'x, -y, -z'
'-x, y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y, -x, -z-1/2'
'x, y, -z'
'-y, x, -z-1/2'
'-x, y, z'
'x, -y, z'
'-y, -x, z-1/2'
'y, x, z-1/2'

_cell_length_a                   23.0742(4)
_cell_length_b                   23.0742(4)
_cell_length_c                   18.6187(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9912.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6601
_cell_measurement_theta_min      4.2700
_cell_measurement_theta_max      64.9040

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.866
_exptl_crystal_F_000             2592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.897
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.58534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_reflns_number            19426
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.831
_diffrn_reflns_theta_max         65.298
_diffrn_reflns_theta_full        65.298
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             4560
_reflns_number_gt                3299
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1465P)²+90.1019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4560
_refine_ls_number_parameters     302
_refine_ls_number_restraints     475
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0926
_refine_ls_wR_factor_ref         0.2878
_refine_ls_wR_factor_gt          0.2422
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.5000 0.10726(4) 0.0000 0.0237(3) Uani 1 4 d S T P A .
Zr2 Zr 0.42413(5) 0.0000 0.09336(7) 0.0577(5) Uani 1 2 d S T P . .
O1 O 0.4416(2) 0.1563(2) 0.0725(3) 0.0507(15) Uani 1 1 d . U . . .
O2 O 0.3932(4) 0.0864(3) 0.1311(5) 0.103(3) Uani 1 1 d . U . . .
O3 O 0.4106(12) 0.0000 0.199(2) 0.137(8) Uani 0.5 2 d DS TU P A 1
O4 O 0.3056(11) 0.0000 0.2068(18) 0.147(9) Uani 0.5 2 d DS TU P . .
O5 O 0.3338(13) 0.0000 0.0892(12) 0.105(6) Uani 0.5 2 d DS TU P A .
O6 O 0.3238(13) 0.0000 -0.0430(12) 0.114(6) Uani 0.5 2 d DS TU P A .
O7 O 0.4242(5) 0.0529(4) 0.0000 0.082(3) Uani 1 2 d S T P A .
O8 O 0.5000 0.0518(4) 0.0948(6) 0.077(3) Uani 1 2 d S T P A .
O9 O 0.4478(13) 0.0000 0.2205(10) 0.074(6) Uani 0.5 2 d S T P A 2
N1 N 0.0693(2) 0.1621(8) 0.1243(15) 0.270(9) Uani 0.5 1 d D U P . .
N2 N 0.0733(17) 0.1619(14) 0.1894(15) 0.285(10) Uani 0.5 1 d D U P . .
N3 N 0.094(2) 0.1562(19) 0.2452(15) 0.312(13) Uani 0.5 1 d D U P . .
C1 C 0.3020(4) 0.2622(3) 0.2303(5) 0.107(3) Uani 1 1 d D U . . .
C2 C 0.3020(4) 0.2046(4) 0.2512(5) 0.120(3) Uani 1 1 d D U . . .
H2 H 0.2785 0.1923 0.2903 0.144 Uiso 0.697(18) 1 calc R U P B 2
C3 C 0.3365(4) 0.1647(3) 0.2152(5) 0.114(3) Uani 1 1 d D U . . .
H3 H 0.3365 0.1252 0.2295 0.136 Uiso 1 1 calc R U . . .
C4 C 0.3710(4) 0.1826(3) 0.1580(5) 0.091(3) Uani 1 1 d D U . . .
C5 C 0.3710(4) 0.2401(3) 0.1371(5) 0.093(3) Uani 1 1 d D U . . .
H5 H 0.3947 0.2523 0.0982 0.112 Uiso 1 1 calc R U . . .
C6 C 0.3363(4) 0.2803(3) 0.1733(5) 0.103(3) Uani 1 1 d D U . . .
H6 H 0.3362 0.3198 0.1589 0.124 Uiso 0.303(18) 1 calc R U P B 1
C7 C 0.4048(5) 0.1384(4) 0.1162(7) 0.079(2) Uani 1 1 d . U . . .
C8 C 0.2661(8) 0.1816(12) 0.3124(8) 0.136(9) Uani 0.303(18) 1 d D U P B 1
H8A H 0.2404 0.2123 0.3302 0.204 Uiso 0.303(18) 1 calc R U P B 1
H8B H 0.2917 0.1687 0.3513 0.204 Uiso 0.303(18) 1 calc R U P B 1
H8C H 0.2427 0.1488 0.2956 0.204 Uiso 0.303(18) 1 calc R U P B 1
C9 C 0.3592(10) 0.0000 0.2294(7) 0.149(7) Uani 0.5 2 d DS TU P A 1
C10 C 0.3597(8) 0.0000 0.3099(4) 0.161(7) Uani 0.5 2 d DS TU P . .
C11 C 0.4120(8) 0.0000 0.3469(4) 0.165(8) Uani 0.5 2 d DS TU P A .
H11 H 0.4476 0.0000 0.3213 0.198 Uiso 0.5 2 calc R U P . .
C12 C 0.4121(8) 0.0000 0.4218(3) 0.172(8) Uani 0.5 2 d DS TU P . .
H12 H 0.4478 0.0000 0.4471 0.206 Uiso 0.25 2 calc R U P A 2
C13 C 0.3600(8) 0.0000 0.4595(2) 0.174(8) Uani 0.5 2 d DS TU P A .
C14 C 0.3078(8) 0.0000 0.4219(4) 0.173(8) Uani 0.5 2 d DS TU P . .
H14 H 0.2721 0.0000 0.4475 0.208 Uiso 0.25 2 calc R U P A 1
C15 C 0.3076(8) 0.0000 0.3473(5) 0.168(8) Uani 0.5 2 d DS TU P A .
H15 H 0.2719 0.0000 0.3218 0.201 Uiso 0.5 2 calc R U P . .
C16 C 0.4686(8) 0.0000 0.4610(2) 0.173(10) Uani 0.25 2 d DS TU P A 1
H16D H 0.4909 -0.0346 0.4481 0.208 Uiso 0.25 1 d DR U P A 1
H16E H 0.4616 0.0000 0.5129 0.208 Uiso 0.25 2 d DR U P A 1
C17 C 0.3091(7) 0.0000 0.0257(13) 0.128(5) Uani 0.5 2 d DS TU P . .
C18 C 0.2446(7) 0.0000 0.041(2) 0.152(6) Uani 0.5 2 d DS TU P A .
C19 C 0.2250(9) 0.0000 0.1120(19) 0.165(6) Uani 0.5 2 d DS TU P A 1
H19 H 0.2521 0.0000 0.1504 0.198 Uiso 0.5 2 calc R U P A 1
C20 C 0.1658(11) 0.0000 0.1267(6) 0.177(7) Uani 0.5 2 d DS TU P A 1
H20 H 0.1527 0.0000 0.1750 0.213 Uiso 0.5 2 calc R U P A 1
C21 C 0.1260(5) 0.0000 0.0706(7) 0.189(7) Uani 0.5 2 d DS TU P . .
C22 C 0.1454(12) 0.0000 0.0000 0.179(7) Uani 1 4 d DS TU P A 2
H22 H 0.1182 0.0000 -0.0383 0.215 Uiso 0.5 2 calc R U P A 2
C23 C 0.2046(14) 0.0000 -0.0149(15) 0.167(6) Uani 0.5 2 d DS TU P A 2
H23 H 0.2178 0.0000 -0.0632 0.201 Uiso 0.5 2 calc R U P A 2
C24 C 0.0606(2) 0.0000 0.0798(12) 0.206(7) Uani 0.5 2 d DS TU P A .
C25 C 0.03024(18) 0.05232(15) 0.0798(12) 0.226(8) Uani 0.5 1 d D U P . .
C26 C 0.0629(8) 0.1086(6) 0.0798(12) 0.247(9) Uani 0.5 1 d D U P A .
H26A H 0.1035 0.0955 0.0751 0.297 Uiso 0.5 1 calc R U P . .
H26B H 0.0529 0.1248 0.0321 0.297 Uiso 0.5 1 calc R U P . .
C8A C 0.3387(7) 0.3421(4) 0.1471(10) 0.145(7) Uani 0.697(18) 1 d D U P B 2
H8A1 H 0.2993 0.3566 0.1398 0.218 Uiso 0.697(18) 1 calc R U P B 2
H8A2 H 0.3600 0.3437 0.1016 0.218 Uiso 0.697(18) 1 calc R U P B 2
H8A3 H 0.3585 0.3661 0.1830 0.218 Uiso 0.697(18) 1 calc R U P B 2
C16A C 0.2512(9) 0.0000 0.4612(3) 0.177(12) Uani 0.25 2 d DS TU P A 2
H16A H 0.2193 0.0000 0.4265 0.266 Uiso 0.25 2 calc R U P A 2
H16B H 0.2487 0.0347 0.4914 0.266 Uiso 0.125 1 calc R U P A 2
H16C H 0.2487 -0.0347 0.4914 0.266 Uiso 0.125 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 O7 2.152(9) . ?
Zr1 O7 2.152(9) 13_655 ?
Zr1 O8 2.180(10) . ?
Zr1 O8 2.180(10) 11 ?
Zr1 O1 2.217(5) . ?
Zr1 O1 2.217(5) 13_655 ?
Zr1 O1 2.217(5) 11 ?
Zr1 O1 2.217(5) 6_655 ?
Zr1 Zr2 3.4945(9) 11 ?
Zr1 Zr2 3.4945(9) 9_655 ?
Zr1 Zr2 3.4945(9) 3_655 ?
Zr1 Zr2 3.4945(9) . ?
Zr2 O3 2.00(4) . ?
Zr2 O5 2.08(3) . ?
Zr2 O8 2.120(5) 3_655 ?
Zr2 O8 2.120(5) . ?
Zr2 O7 2.125(6) . ?
Zr2 O7 2.125(6) 5 ?
Zr2 O2 2.231(6) 14 ?
Zr2 O2 2.231(6) . ?
Zr2 O9 2.428(18) . ?
Zr2 O6 2.50(3) 5 ?
Zr2 Zr2 3.477(3) 11 ?
O1 C7 1.247(11) . ?
O2 C7 1.260(11) . ?
O3 C9 1.311(10) . ?
O4 C9 1.305(10) . ?
O5 O6 0.89(4) 5 ?
O5 C17 1.312(10) . ?
O6 C17 1.323(10) . ?
O6 Zr2 2.50(3) 11 ?
O7 Zr2 2.125(6) 11 ?
O8 Zr2 2.120(5) 3_655 ?
N1 N2 1.217(10) . ?
N1 C26 1.493(10) . ?
N2 N3 1.146(10) . ?
C1 C2 1.386(7) . ?
C1 C6 1.388(7) . ?
C1 C1 1.493(12) 7 ?
C2 C3 1.389(7) . ?
C2 C8 1.506(9) . ?
C3 C4 1.390(7) . ?
C4 C5 1.384(7) . ?
C4 C7 1.502(10) . ?
C5 C6 1.397(7) . ?
C6 C8A 1.508(9) . ?
C9 C10 1.499(10) . ?
C10 C11 1.389(8) . ?
C10 C15 1.390(8) . ?
C11 C12 1.394(7) . ?
C12 C13 1.392(7) . ?
C12 C16 1.4951(17) . ?
C13 C14 1.394(7) . ?
C13 C13 1.508(9) 11_556 ?
C14 C15 1.390(8) . ?
C14 C16A 1.495(9) . ?
C16 C16 1.45(4) 3_655 ?
C16 C16 1.452(9) 5_556 ?
C17 O6 0.47(4) 5 ?
C17 C18 1.516(10) . ?
C17 C18 1.94(3) 5 ?
C18 C19 1.391(8) . ?
C18 C23 1.395(8) . ?
C18 O6 1.83(4) 5 ?
C19 C20 1.392(8) . ?
C20 C21 1.391(8) . ?
C21 C22 1.389(8) 5 ?
C21 C22 1.389(8) . ?
C21 C24 1.518(10) . ?
C22 C23 1.395(8) . ?
C24 C25 1.396(5) 14 ?
C24 C25 1.396(5) . ?
C25 C25 1.396(8) 13 ?
C25 C26 1.502(10) . ?

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
O7 Zr1 O7 108.8(7) . 13_655 ?
O7 Zr1 O8 70.0(2) . . ?
O7 Zr1 O8 70.0(2) 13_655 . ?
O7 Zr1 O8 70.0(2) . 11 ?
O7 Zr1 O8 70.0(2) 13_655 11 ?
O8 Zr1 O8 108.1(6) . 11 ?
O7 Zr1 O1 78.7(3) . . ?
O7 Zr1 O1 142.28(18) 13_655 . ?
O8 Zr1 O1 78.9(3) . . ?
O8 Zr1 O1 142.41(16) 11 . ?
O7 Zr1 O1 142.28(18) . 13_655 ?
O7 Zr1 O1 78.7(3) 13_655 13_655 ?
O8 Zr1 O1 78.9(3) . 13_655 ?
O8 Zr1 O1 142.41(16) 11 13_655 ?
O1 Zr1 O1 74.8(3) . 13_655 ?
O7 Zr1 O1 78.7(3) . 11 ?
O7 Zr1 O1 142.28(18) 13_655 11 ?
O8 Zr1 O1 142.41(16) . 11 ?
O8 Zr1 O1 78.9(3) 11 11 ?
O1 Zr1 O1 75.0(3) . 11 ?
O1 Zr1 O1 118.6(3) 13_655 11 ?
O7 Zr1 O1 142.28(18) . 6_655 ?
O7 Zr1 O1 78.7(3) 13_655 6_655 ?
O8 Zr1 O1 142.41(16) . 6_655 ?
O8 Zr1 O1 78.9(3) 11 6_655 ?
O1 Zr1 O1 118.6(3) . 6_655 ?
O1 Zr1 O1 75.0(3) 13_655 6_655 ?
O1 Zr1 O1 74.8(3) 11 6_655 ?
O7 Zr1 Zr2 34.95(17) . 11 ?
O7 Zr1 Zr2 89.7(3) 13_655 11 ?
O8 Zr1 Zr2 89.2(3) . 11 ?
O8 Zr1 Zr2 35.07(15) 11 11 ?
O1 Zr1 Zr2 111.10(15) . 11 ?
O1 Zr1 Zr2 165.59(14) 13_655 11 ?
O1 Zr1 Zr2 75.78(14) 11 11 ?
O1 Zr1 Zr2 111.28(17) 6_655 11 ?
O7 Zr1 Zr2 89.7(3) . 9_655 ?
O7 Zr1 Zr2 34.95(17) 13_655 9_655 ?
O8 Zr1 Zr2 89.2(3) . 9_655 ?
O8 Zr1 Zr2 35.07(15) 11 9_655 ?
O1 Zr1 Zr2 165.59(14) . 9_655 ?
O1 Zr1 Zr2 111.10(15) 13_655 9_655 ?
O1 Zr1 Zr2 111.28(17) 11 9_655 ?
O1 Zr1 Zr2 75.78(14) 6_655 9_655 ?
Zr2 Zr1 Zr2 60.12(4) 11 9_655 ?
O7 Zr1 Zr2 89.7(3) . 3_655 ?
O7 Zr1 Zr2 34.95(17) 13_655 3_655 ?
O8 Zr1 Zr2 35.07(15) . 3_655 ?
O8 Zr1 Zr2 89.2(3) 11 3_655 ?
O1 Zr1 Zr2 111.28(17) . 3_655 ?
O1 Zr1 Zr2 75.78(14) 13_655 3_655 ?
O1 Zr1 Zr2 165.59(14) 11 3_655 ?
O1 Zr1 Zr2 111.10(15) 6_655 3_655 ?
Zr2 Zr1 Zr2 89.81(3) 11 3_655 ?
Zr2 Zr1 Zr2 59.66(4) 9_655 3_655 ?
O7 Zr1 Zr2 34.95(17) . . ?
O7 Zr1 Zr2 89.7(3) 13_655 . ?
O8 Zr1 Zr2 35.07(15) . . ?
O8 Zr1 Zr2 89.2(3) 11 . ?
O1 Zr1 Zr2 75.78(14) . . ?
O1 Zr1 Zr2 111.28(17) 13_655 . ?
O1 Zr1 Zr2 111.10(15) 11 . ?
O1 Zr1 Zr2 165.59(14) 6_655 . ?
Zr2 Zr1 Zr2 59.66(4) 11 . ?
Zr2 Zr1 Zr2 89.81(3) 9_655 . ?
Zr2 Zr1 Zr2 60.12(4) 3_655 . ?
O3 Zr2 O5 83.2(11) . . ?
O3 Zr2 O8 96.7(8) . 3_655 ?
O5 Zr2 O8 145.7(2) . 3_655 ?
O3 Zr2 O8 96.7(8) . . ?
O5 Zr2 O8 145.7(2) . . ?
O8 Zr2 O8 68.6(4) 3_655 . ?
O3 Zr2 O7 143.9(3) . . ?
O5 Zr2 O7 88.3(6) . . ?
O8 Zr2 O7 109.5(5) 3_655 . ?
O8 Zr2 O7 71.7(4) . . ?
O3 Zr2 O7 143.9(3) . 5 ?
O5 Zr2 O7 88.3(6) . 5 ?
O8 Zr2 O7 71.7(4) 3_655 5 ?
O8 Zr2 O7 109.5(5) . 5 ?
O7 Zr2 O7 70.2(4) . 5 ?
O3 Zr2 O2 68.8(3) . 14 ?
O5 Zr2 O2 72.1(3) . 14 ?
O8 Zr2 O2 75.9(3) 3_655 14 ?
O8 Zr2 O2 139.8(3) . 14 ?
O7 Zr2 O2 140.5(3) . 14 ?
O7 Zr2 O2 75.2(3) 5 14 ?
O3 Zr2 O2 68.8(3) . . ?
O5 Zr2 O2 72.1(3) . . ?
O8 Zr2 O2 139.8(3) 3_655 . ?
O8 Zr2 O2 75.9(3) . . ?
O7 Zr2 O2 75.2(3) . . ?
O7 Zr2 O2 140.5(3) 5 . ?
O2 Zr2 O2 126.6(3) 14 . ?
O5 Zr2 O9 105.1(9) . . ?
O8 Zr2 O9 78.6(7) 3_655 . ?
O8 Zr2 O9 78.6(7) . . ?
O7 Zr2 O9 142.9(3) . . ?
O7 Zr2 O9 142.9(3) 5 . ?
O2 Zr2 O9 76.4(4) 14 . ?
O2 Zr2 O9 76.4(4) . . ?
O3 Zr2 O6 103.1(11) . 5 ?
O5 Zr2 O6 19.9(10) . 5 ?
O8 Zr2 O6 140.4(3) 3_655 5 ?
O8 Zr2 O6 140.4(3) . 5 ?
O7 Zr2 O6 72.1(6) . 5 ?
O7 Zr2 O6 72.1(6) 5 5 ?
O2 Zr2 O6 79.8(4) 14 5 ?
O2 Zr2 O6 79.8(4) . 5 ?
O9 Zr2 O6 125.1(9) . 5 ?
O3 Zr2 Zr2 171.0(9) . 11 ?
O5 Zr2 Zr2 87.8(6) . 11 ?
O8 Zr2 Zr2 90.7(3) 3_655 11 ?
O8 Zr2 Zr2 90.7(3) . 11 ?
O7 Zr2 Zr2 35.1(2) . 11 ?
O7 Zr2 Zr2 35.1(2) 5 11 ?
O2 Zr2 Zr2 108.4(3) 14 11 ?
O2 Zr2 Zr2 108.4(3) . 11 ?
O9 Zr2 Zr2 167.0(7) . 11 ?
O6 Zr2 Zr2 67.9(6) 5 11 ?
O3 Zr2 Zr1 124.7(5) . . ?
O5 Zr2 Zr1 118.8(4) . . ?
O8 Zr2 Zr1 89.5(3) 3_655 . ?
O8 Zr2 Zr1 36.2(3) . . ?
O7 Zr2 Zr1 35.5(2) . . ?
O7 Zr2 Zr1 90.0(3) 5 . ?
O2 Zr2 Zr1 161.77(17) 14 . ?
O2 Zr2 Zr1 71.59(17) . . ?
O9 Zr2 Zr1 111.8(4) . . ?
O6 Zr2 Zr1 106.1(4) 5 . ?
Zr2 Zr2 Zr1 60.17(2) 11 . ?
C7 O1 Zr1 129.9(5) . . ?
C7 O2 Zr2 135.5(6) . . ?
C9 O3 Zr2 124(3) . . ?
O6 O5 C17 11(3) 5 . ?
O6 O5 Zr2 107(3) 5 . ?
C17 O5 Zr2 118.0(18) . . ?
C17 O6 Zr2 127(2) . 11 ?
Zr2 O7 Zr2 109.8(4) . 11 ?
Zr2 O7 Zr1 109.6(4) . . ?
Zr2 O7 Zr1 109.6(4) 11 . ?
Zr2 O8 Zr2 111.3(4) 3_655 . ?
Zr2 O8 Zr1 108.7(4) 3_655 . ?
Zr2 O8 Zr1 108.7(4) . . ?
N2 N1 C26 123.9(14) . . ?
N3 N2 N1 159(4) . . ?
C2 C1 C6 120.2(5) . . ?
C2 C1 C1 116.9(7) . 7 ?
C6 C1 C1 122.8(7) . 7 ?
C1 C2 C3 120.0(5) . . ?
C1 C2 C8 123.4(12) . . ?
C3 C2 C8 116.6(12) . . ?
C2 C3 C4 120.0(5) . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 C7 120.3(7) . . ?
C3 C4 C7 119.5(7) . . ?
C4 C5 C6 120.0(5) . . ?
C1 C6 C5 119.7(5) . . ?
C1 C6 C8A 123.5(9) . . ?
C5 C6 C8A 116.8(9) . . ?
O1 C7 O2 127.1(8) . . ?
O1 C7 C4 117.9(8) . . ?
O2 C7 C4 115.0(8) . . ?
O4 C9 O3 136(3) . . ?
O4 C9 C10 109(2) . . ?
O3 C9 C10 115(2) . . ?
C11 C10 C15 120.1(5) . . ?
C11 C10 C9 120.3(9) . . ?
C15 C10 C9 119.6(9) . . ?
C10 C11 C12 119.9(5) . . ?
C13 C12 C11 120.2(5) . . ?
C13 C12 C16 120.5(3) . . ?
C11 C12 C16 119.4(4) . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 C13 120.3(3) . 11_556 ?
C14 C13 C13 120.1(3) . 11_556 ?
C15 C14 C13 120.3(5) . . ?
C15 C14 C16A 119.1(6) . . ?
C13 C14 C16A 120.6(6) . . ?
C10 C15 C14 119.9(5) . . ?
C16 C16 C16 89.997(1) 3_655 5_556 ?
C16 C16 C12 150.77(14) 3_655 . ?
C16 C16 C12 119.23(14) 5_556 . ?
O6 C17 O5 21(5) 5 . ?
O6 C17 O6 118(6) 5 . ?
O5 C17 O6 139(2) . . ?
O6 C17 C18 126(6) 5 . ?
O5 C17 C18 105(3) . . ?
O6 C17 C18 116(3) . . ?
O6 C17 C18 177(6) 5 5 ?
O5 C17 C18 156(2) . 5 ?
O6 C17 C18 65(2) . 5 ?
C18 C17 C18 51(3) . 5 ?
C19 C18 C17 120(3) . . ?
C23 C18 C17 120(3) . . ?
C19 C18 O6 108(3) . 5 ?
C23 C18 O6 132(3) . 5 ?
C17 C18 O6 12.0(16) . 5 ?
C18 C19 C20 120.2(5) . . ?
C21 C20 C19 120.1(5) . . ?
C22 C21 C22 0(2) 5 . ?
C22 C21 C24 115.3(18) 5 . ?
C22 C21 C24 115.3(18) . . ?
C20 C21 C24 124.9(18) . . ?
C21 C22 C23 120.3(5) . . ?
C18 C23 C22 119.9(5) . . ?
C25 C24 C25 119.7(4) 14 . ?
C25 C24 C21 119.9(2) 14 . ?
C25 C24 C21 119.9(2) . . ?
C25 C25 C24 120.1(2) 13 . ?
C25 C25 C26 120.1(8) 13 . ?
C24 C25 C26 119.8(9) . . ?
N1 C26 C25 139.8(11) . . ?

_refine_diff_density_max         1.870
_refine_diff_density_min         -2.440
_refine_diff_density_rms         0.150



_exptl_crystal_recrystallization_method 'Solvothermal Reaction'
####################################################################### 
# 
# 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_LIFM-92
_database_code_depnum_ccdc_archive 'CCDC 1544324'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            LIFM-92
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H74 N6 O32 Zr6'
_chemical_formula_sum            'C102 H74 N6 O32 Zr6'
_chemical_formula_weight         2442.99

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+1/2'
'-x, -y, z'
'y, -x, z+1/2'
'x, -y, -z'
'-x, y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y, -x, -z-1/2'
'x, y, -z'
'-y, x, -z-1/2'
'-x, y, z'
'x, -y, z'
'-y, -x, z-1/2'
'y, x, z-1/2'

_cell_length_a                   23.10920(10)
_cell_length_b                   23.10920(10)
_cell_length_c                   18.7957(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10037.57(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9339
_cell_measurement_theta_min      4.2640
_cell_measurement_theta_max      65.0930

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.808
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.825
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.70854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_reflns_number            19865
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.826
_diffrn_reflns_theta_max         65.044
_diffrn_reflns_theta_full        65.044
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             4585
_reflns_number_gt                3886
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1258P)²+22.3044P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4585
_refine_ls_number_parameters     222
_refine_ls_number_restraints     291
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.2037
_refine_ls_wR_factor_gt          0.1892
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.255
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.42456(2) 0.0000 0.09255(3) 0.0285(2) Uani 1 2 d S T P . .
Zr2 Zr 0.5000 0.10789(3) 0.0000 0.0181(2) Uani 1 4 d S T P . .
O1 O 0.39157(19) 0.08352(17) 0.1349(2) 0.0641(13) Uani 1 1 d . . . . .
O2 O 0.44111(16) 0.15618(15) 0.0728(2) 0.0444(9) Uani 1 1 d . . . . .
O3 O 0.4456(4) 0.0000 0.2057(3) 0.092(3) Uani 1 2 d S TU P . .
O4 O 0.3320(2) 0.0000 0.0621(4) 0.074(2) Uani 1 2 d S TU P . .
O5 O 0.5000 0.0536(3) 0.0930(4) 0.0619(19) Uani 1 2 d S T P . .
O6 O 0.4251(3) 0.0536(3) 0.0000 0.071(2) Uani 1 2 d S T P . .
N1 N 0.0000 0.1526(4) 0.0000 0.403(9) Uani 1 4 d DS TU P A 1
N2 N 0.0178(10) 0.2030(5) 0.0000 0.428(10) Uani 0.5 2 d DS TU P A 1
N3 N 0.0000 0.2505(5) 0.0000 0.444(11) Uani 1 4 d DS TU P A 1
C1 C 0.3006(2) 0.2601(2) 0.2310(3) 0.098(2) Uani 1 1 d D U . . .
C2 C 0.3001(3) 0.2027(3) 0.2508(3) 0.114(2) Uani 1 1 d D U . . .
H2 H 0.2765 0.1904 0.2893 0.137 Uiso 0.667(12) 1 calc R U P B 2
C3 C 0.3344(3) 0.1627(2) 0.2146(3) 0.105(2) Uani 1 1 d D U . . .
H3 H 0.3341 0.1231 0.2283 0.126 Uiso 1 1 calc R U . . .
C4 C 0.3690(3) 0.1809(2) 0.1584(3) 0.0724(17) Uani 1 1 d D U . . .
C5 C 0.3698(3) 0.2385(2) 0.1386(3) 0.086(2) Uani 1 1 d D U . . .
H5 H 0.3939 0.2509 0.1005 0.103 Uiso 1 1 calc R U . . .
C6 C 0.3352(3) 0.2786(2) 0.1748(4) 0.102(2) Uani 1 1 d D U . . .
H6 H 0.3353 0.3182 0.1611 0.122 Uiso 0.333(12) 1 calc R U P B 1
C7 C 0.4034(3) 0.1362(3) 0.1185(4) 0.0569(15) Uani 1 1 d . U . . .
C8 C 0.2647(6) 0.1768(9) 0.3109(6) 0.134(4) Uani 0.333(12) 1 d D U P B 1
H8A H 0.2723 0.1351 0.3138 0.201 Uiso 0.333(12) 1 calc R U P B 1
H8B H 0.2755 0.1952 0.3559 0.201 Uiso 0.333(12) 1 calc R U P B 1
H8C H 0.2235 0.1832 0.3017 0.201 Uiso 0.333(12) 1 calc R U P B 1
C9 C 0.5000 0.0000 0.2326(6) 0.120(4) Uani 1 4 d DS TU P . .
C10 C 0.5000 0.0000 0.3118(4) 0.147(5) Uani 1 4 d DS TU P . .
C11 C 0.4550(4) 0.0265(6) 0.3485(4) 0.171(6) Uani 0.5 1 d D U P D .
H11 H 0.4243 0.0445 0.3231 0.205 Uiso 0.5 1 calc R U P . .
C12 C 0.4550(4) 0.0265(6) 0.4228(5) 0.185(7) Uani 0.5 1 d D U P . .
H12 H 0.4243 0.0446 0.4481 0.222 Uiso 0.25 1 calc R U P C 2
C13 C 0.5000 0.0000 0.4600(2) 0.195(7) Uani 1 4 d DS TU P D .
C14 C 0.4052(9) 0.0558(13) 0.4593(10) 0.204(11) Uani 0.25 1 d D U P D 1
H14A H 0.3787 0.0715 0.4235 0.306 Uiso 0.25 1 calc R U P D 1
H14B H 0.3847 0.0277 0.4891 0.306 Uiso 0.25 1 calc R U P D 1
H14C H 0.4199 0.0874 0.4891 0.306 Uiso 0.25 1 calc R U P D 1
C15 C 0.3090(4) 0.0000 0.0000 0.098(3) Uani 1 4 d DS TU P . .
C16 C 0.2447(3) 0.0000 0.0000 0.141(4) Uani 1 4 d DS TU P . .
C17 C 0.2151(4) 0.0000 0.0641(2) 0.187(5) Uani 1 2 d DS TU P . .
H17 H 0.2358 0.0000 0.1077 0.225 Uiso 1 2 calc R U P . .
C18 C 0.1547(4) 0.0000 0.0641(2) 0.231(6) Uani 1 2 d DS TU P . .
H18 H 0.1342 0.0000 0.1079 0.277 Uiso 1 2 calc R U P . .
C19 C 0.1246(3) 0.0000 0.0000 0.265(7) Uani 1 4 d DS TU P . .
C20 C 0.06013(18) 0.0000 0.0000 0.298(7) Uani 1 4 d DS TU P . .
C21 C 0.03088(17) 0.05177(14) 0.0000 0.335(8) Uani 1 2 d DS TU P . .
H21 H 0.0516 0.0873 0.0000 0.402 Uiso 0.5 2 calc R U P E 2
C22 C 0.0540(5) 0.1146(4) 0.0000 0.374(9) Uani 0.5 2 d DS TU P A 1
H22A H 0.0777 0.1221 0.0428 0.449 Uiso 0.25 1 calc R U P A 1
H22B H 0.0777 0.1221 -0.0428 0.449 Uiso 0.25 1 calc R U P A 1
C8A C 0.3383(5) 0.3408(4) 0.1487(6) 0.134(4) Uani 0.667(12) 1 d D U P B 2
H8A1 H 0.3654 0.3433 0.1088 0.201 Uiso 0.667(12) 1 calc R U P B 2
H8A2 H 0.2998 0.3533 0.1331 0.201 Uiso 0.667(12) 1 calc R U P B 2
H8A3 H 0.3516 0.3658 0.1875 0.201 Uiso 0.667(12) 1 calc R U P B 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 O6 2.135(4) . ?
Zr1 O6 2.135(4) 5 ?
Zr1 O5 2.138(3) 3_655 ?
Zr1 O5 2.138(3) . ?
Zr1 O3 2.182(7) . ?
Zr1 O4 2.214(6) . ?
Zr1 O1 2.222(4) 14 ?
Zr1 O1 2.222(4) . ?
Zr1 Zr1 3.4790(11) 11 ?
Zr1 Zr1 3.4869(10) 3_655 ?
Zr1 Zr2 3.5045(5) 9_655 ?
Zr1 Zr2 3.5046(5) . ?
Zr2 O6 2.138(5) 13_655 ?
Zr2 O6 2.138(5) . ?
Zr2 O5 2.152(5) . ?
Zr2 O5 2.152(5) 11 ?
Zr2 O2 2.230(3) . ?
Zr2 O2 2.230(3) 13_655 ?
Zr2 O2 2.230(3) 11 ?
Zr2 O2 2.230(3) 6_655 ?
Zr2 Zr1 3.5046(5) 11 ?
Zr2 Zr1 3.5046(5) 9_655 ?
Zr2 Zr1 3.5046(5) 3_655 ?
O1 C7 1.286(7) . ?
O2 C7 1.307(7) . ?
O3 C9 1.354(10) . ?
O4 C15 1.284(8) . ?
O5 Zr1 2.138(3) 3_655 ?
O6 Zr1 2.135(4) 11 ?
N1 N2 1.235(10) . ?
N1 N2 1.235(10) 13 ?
N1 C22 1.524(8) . ?
N1 C22 1.524(8) 13 ?
N2 N2 0.82(5) 13 ?
N2 N3 1.172(10) . ?
N3 N2 1.172(10) 13 ?
C1 C2 1.379(6) . ?
C1 C6 1.391(6) . ?
C1 C1 1.504(9) 7 ?
C2 C3 1.394(6) . ?
C2 C8 1.518(9) . ?
C3 C4 1.390(6) . ?
C4 C5 1.383(6) . ?
C4 C7 1.504(7) . ?
C5 C6 1.402(6) . ?
C6 C8A 1.519(8) . ?
C9 O3 1.354(10) 3_655 ?
C9 C10 1.488(9) . ?
C10 C11 1.391(6) 13_655 ?
C10 C11 1.391(6) 3_655 ?
C10 C11 1.391(6) 14 ?
C10 C11 1.391(6) . ?
C11 C12 1.397(7) . ?
C11 C12 1.858(18) 14 ?
C12 C13 1.395(6) . ?
C12 C14 1.500(10) . ?
C12 C11 1.858(18) 14 ?
C13 C12 1.395(6) 14 ?
C13 C12 1.395(6) 13_655 ?
C13 C12 1.395(6) 3_655 ?
C13 C13 1.503(9) 5_556 ?
C15 O4 1.284(8) 11 ?
C15 C16 1.484(8) . ?
C16 C17 1.385(5) 5 ?
C16 C17 1.385(5) . ?
C17 C18 1.395(7) . ?
C18 C19 1.391(6) . ?
C19 C18 1.391(6) 5 ?
C19 C20 1.491(8) . ?
C20 C21 1.374(4) 14 ?
C20 C21 1.374(4) . ?
C21 C21 1.427(8) 6 ?
C21 C22 1.547(10) . ?

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
O6 Zr1 O6 70.9(3) . 5 ?
O6 Zr1 O5 109.5(3) . 3_655 ?
O6 Zr1 O5 70.3(2) 5 3_655 ?
O6 Zr1 O5 70.3(2) . . ?
O6 Zr1 O5 109.5(3) 5 . ?
O5 Zr1 O5 70.7(3) 3_655 . ?
O6 Zr1 O3 142.45(14) . . ?
O6 Zr1 O3 142.45(14) 5 . ?
O5 Zr1 O3 79.3(3) 3_655 . ?
O5 Zr1 O3 79.3(3) . . ?
O6 Zr1 O4 78.2(3) . . ?
O6 Zr1 O4 78.2(3) 5 . ?
O5 Zr1 O4 142.07(13) 3_655 . ?
O5 Zr1 O4 142.07(13) . . ?
O3 Zr1 O4 117.9(3) . . ?
O6 Zr1 O1 142.86(18) . 14 ?
O6 Zr1 O1 77.9(2) 5 14 ?
O5 Zr1 O1 77.03(19) 3_655 14 ?
O5 Zr1 O1 141.36(17) . 14 ?
O3 Zr1 O1 74.20(17) . 14 ?
O4 Zr1 O1 76.17(16) . 14 ?
O6 Zr1 O1 77.9(2) . . ?
O6 Zr1 O1 142.86(18) 5 . ?
O5 Zr1 O1 141.36(17) 3_655 . ?
O5 Zr1 O1 77.03(19) . . ?
O3 Zr1 O1 74.20(17) . . ?
O4 Zr1 O1 76.17(16) . . ?
O1 Zr1 O1 120.6(2) 14 . ?
O6 Zr1 Zr1 35.43(14) . 11 ?
O6 Zr1 Zr1 35.43(14) 5 11 ?
O5 Zr1 Zr1 90.22(18) 3_655 11 ?
O5 Zr1 Zr1 90.22(18) . 11 ?
O3 Zr1 Zr1 167.1(3) . 11 ?
O4 Zr1 Zr1 75.0(2) . 11 ?
O1 Zr1 Zr1 110.97(12) 14 11 ?
O1 Zr1 Zr1 110.97(12) . 11 ?
O6 Zr1 Zr1 89.64(19) . 3_655 ?
O6 Zr1 Zr1 89.64(19) 5 3_655 ?
O5 Zr1 Zr1 35.37(13) 3_655 3_655 ?
O5 Zr1 Zr1 35.37(13) . 3_655 ?
O3 Zr1 Zr1 77.1(3) . 3_655 ?
O4 Zr1 Zr1 165.0(2) . 3_655 ?
O1 Zr1 Zr1 110.06(12) 14 3_655 ?
O1 Zr1 Zr1 110.06(12) . 3_655 ?
Zr1 Zr1 Zr1 90.0 11 3_655 ?
O6 Zr1 Zr2 90.28(19) . 9_655 ?
O6 Zr1 Zr2 34.91(14) 5 9_655 ?
O5 Zr1 Zr2 35.35(15) 3_655 9_655 ?
O5 Zr1 Zr2 90.46(17) . 9_655 ?
O3 Zr1 Zr2 111.89(17) . 9_655 ?
O4 Zr1 Zr2 110.64(14) . 9_655 ?
O1 Zr1 Zr2 74.36(11) 14 9_655 ?
O1 Zr1 Zr2 165.05(11) . 9_655 ?
Zr1 Zr1 Zr2 60.241(9) 11 9_655 ?
Zr1 Zr1 Zr2 60.167(9) 3_655 9_655 ?
O6 Zr1 Zr2 34.92(14) . . ?
O6 Zr1 Zr2 90.28(19) 5 . ?
O5 Zr1 Zr2 90.46(17) 3_655 . ?
O5 Zr1 Zr2 35.35(15) . . ?
O3 Zr1 Zr2 111.89(17) . . ?
O4 Zr1 Zr2 110.64(14) . . ?
O1 Zr1 Zr2 165.05(11) 14 . ?
O1 Zr1 Zr2 74.36(11) . . ?
Zr1 Zr1 Zr2 60.241(9) 11 . ?
Zr1 Zr1 Zr2 60.167(9) 3_655 . ?
Zr2 Zr1 Zr2 90.704(18) 9_655 . ?
O6 Zr2 O6 108.0(4) 13_655 . ?
O6 Zr2 O5 69.96(14) 13_655 . ?
O6 Zr2 O5 69.95(14) . . ?
O6 Zr2 O5 69.95(14) 13_655 11 ?
O6 Zr2 O5 69.95(14) . 11 ?
O5 Zr2 O5 108.6(4) . 11 ?
O6 Zr2 O2 141.99(10) 13_655 . ?
O6 Zr2 O2 78.47(19) . . ?
O5 Zr2 O2 78.07(18) . . ?
O5 Zr2 O2 142.25(10) 11 . ?
O6 Zr2 O2 78.47(19) 13_655 13_655 ?
O6 Zr2 O2 141.99(10) . 13_655 ?
O5 Zr2 O2 78.07(18) . 13_655 ?
O5 Zr2 O2 142.25(10) 11 13_655 ?
O2 Zr2 O2 75.22(19) . 13_655 ?
O6 Zr2 O2 141.99(10) 13_655 11 ?
O6 Zr2 O2 78.47(19) . 11 ?
O5 Zr2 O2 142.25(10) . 11 ?
O5 Zr2 O2 78.07(18) 11 11 ?
O2 Zr2 O2 75.8(2) . 11 ?
O2 Zr2 O2 119.9(2) 13_655 11 ?
O6 Zr2 O2 78.47(19) 13_655 6_655 ?
O6 Zr2 O2 141.99(10) . 6_655 ?
O5 Zr2 O2 142.25(10) . 6_655 ?
O5 Zr2 O2 78.07(18) 11 6_655 ?
O2 Zr2 O2 119.9(2) . 6_655 ?
O2 Zr2 O2 75.8(2) 13_655 6_655 ?
O2 Zr2 O2 75.22(19) 11 6_655 ?
O6 Zr2 Zr1 89.12(19) 13_655 . ?
O6 Zr2 Zr1 34.86(11) . . ?
O5 Zr2 Zr1 35.09(10) . . ?
O5 Zr2 Zr1 89.31(17) 11 . ?
O2 Zr2 Zr1 75.38(10) . . ?
O2 Zr2 Zr1 110.79(10) 13_655 . ?
O2 Zr2 Zr1 110.93(10) 11 . ?
O2 Zr2 Zr1 164.68(10) 6_655 . ?
O6 Zr2 Zr1 89.12(19) 13_655 11 ?
O6 Zr2 Zr1 34.86(11) . 11 ?
O5 Zr2 Zr1 89.31(17) . 11 ?
O5 Zr2 Zr1 35.09(10) 11 11 ?
O2 Zr2 Zr1 110.93(10) . 11 ?
O2 Zr2 Zr1 164.68(10) 13_655 11 ?
O2 Zr2 Zr1 75.38(10) 11 11 ?
O2 Zr2 Zr1 110.79(10) 6_655 11 ?
Zr1 Zr2 Zr1 59.518(19) . 11 ?
O6 Zr2 Zr1 34.86(11) 13_655 9_655 ?
O6 Zr2 Zr1 89.12(19) . 9_655 ?
O5 Zr2 Zr1 89.31(17) . 9_655 ?
O5 Zr2 Zr1 35.09(10) 11 9_655 ?
O2 Zr2 Zr1 164.68(10) . 9_655 ?
O2 Zr2 Zr1 110.93(10) 13_655 9_655 ?
O2 Zr2 Zr1 110.79(10) 11 9_655 ?
O2 Zr2 Zr1 75.38(10) 6_655 9_655 ?
Zr1 Zr2 Zr1 89.295(18) . 9_655 ?
Zr1 Zr2 Zr1 59.666(19) 11 9_655 ?
O6 Zr2 Zr1 34.86(11) 13_655 3_655 ?
O6 Zr2 Zr1 89.12(19) . 3_655 ?
O5 Zr2 Zr1 35.09(10) . 3_655 ?
O5 Zr2 Zr1 89.31(17) 11 3_655 ?
O2 Zr2 Zr1 110.79(10) . 3_655 ?
O2 Zr2 Zr1 75.38(10) 13_655 3_655 ?
O2 Zr2 Zr1 164.68(10) 11 3_655 ?
O2 Zr2 Zr1 110.93(10) 6_655 3_655 ?
Zr1 Zr2 Zr1 59.666(19) . 3_655 ?
Zr1 Zr2 Zr1 89.296(18) 11 3_655 ?
Zr1 Zr2 Zr1 59.519(19) 9_655 3_655 ?
C7 O1 Zr1 131.6(3) . . ?
C7 O2 Zr2 129.3(3) . . ?
C9 O3 Zr1 124.8(7) . . ?
C15 O4 Zr1 129.5(6) . . ?
Zr1 O5 Zr1 109.3(3) 3_655 . ?
Zr1 O5 Zr2 109.6(2) 3_655 . ?
Zr1 O5 Zr2 109.6(2) . . ?
Zr1 O6 Zr1 109.1(3) . 11 ?
Zr1 O6 Zr2 110.2(2) . . ?
Zr1 O6 Zr2 110.2(2) 11 . ?
N2 N1 N2 39(2) . 13 ?
N2 N1 C22 105.7(11) . . ?
N2 N1 C22 144.5(12) 13 . ?
N2 N1 C22 144.5(12) . 13 ?
N2 N1 C22 105.7(11) 13 13 ?
C22 N1 C22 109.8(10) . 13 ?
N2 N2 N3 69.5(11) 13 . ?
N2 N2 N1 70.6(11) 13 . ?
N3 N2 N1 140(2) . . ?
N2 N3 N2 41(2) . 13 ?
C2 C1 C6 120.4(4) . . ?
C2 C1 C1 117.7(5) . 7 ?
C6 C1 C1 121.8(5) . 7 ?
C1 C2 C3 120.1(4) . . ?
C1 C2 C8 125.9(9) . . ?
C3 C2 C8 114.1(9) . . ?
C4 C3 C2 119.8(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 C7 121.3(5) . . ?
C3 C4 C7 118.4(5) . . ?
C4 C5 C6 119.8(4) . . ?
C1 C6 C5 119.6(4) . . ?
C1 C6 C8A 124.2(6) . . ?
C5 C6 C8A 116.2(6) . . ?
O1 C7 O2 129.3(5) . . ?
O1 C7 C4 114.8(5) . . ?
O2 C7 C4 116.0(5) . . ?
O3 C9 O3 136.2(11) . 3_655 ?
O3 C9 C10 111.9(5) . . ?
O3 C9 C10 111.9(5) 3_655 . ?
C11 C10 C11 52.2(12) 13_655 3_655 ?
C11 C10 C11 120.5(6) 13_655 14 ?
C11 C10 C11 96.9(11) 3_655 14 ?
C11 C10 C11 96.9(11) 13_655 . ?
C11 C10 C11 120.5(6) 3_655 . ?
C11 C10 C11 52.2(12) 14 . ?
C11 C10 C9 119.8(3) 13_655 . ?
C11 C10 C9 119.8(3) 3_655 . ?
C11 C10 C9 119.8(3) 14 . ?
C11 C10 C9 119.8(3) . . ?
C10 C11 C12 119.8(5) . . ?
C10 C11 C12 94.8(8) . 14 ?
C12 C11 C12 41.3(7) . 14 ?
C13 C12 C11 120.1(4) . . ?
C13 C12 C14 122.7(9) . . ?
C11 C12 C14 117.2(8) . . ?
C13 C12 C11 95.0(8) . 14 ?
C11 C12 C11 41.2(7) . 14 ?
C14 C12 C11 129.9(8) . 14 ?
C12 C13 C12 52.1(12) 14 . ?
C12 C13 C12 119.9(6) 14 13_655 ?
C12 C13 C12 96.4(10) . 13_655 ?
C12 C13 C12 96.4(10) 14 3_655 ?
C12 C13 C12 119.9(6) . 3_655 ?
C12 C13 C12 52.1(12) 13_655 3_655 ?
C12 C13 C13 120.1(3) 14 5_556 ?
C12 C13 C13 120.1(3) . 5_556 ?
C12 C13 C13 120.1(3) 13_655 5_556 ?
C12 C13 C13 120.1(3) 3_655 5_556 ?
O4 C15 O4 131.0(9) . 11 ?
O4 C15 C16 114.5(5) . . ?
O4 C15 C16 114.5(5) 11 . ?
C17 C16 C17 120.8(6) 5 . ?
C17 C16 C15 119.6(3) 5 . ?
C17 C16 C15 119.6(3) . . ?
C16 C17 C18 119.7(4) . . ?
C19 C18 C17 119.9(4) . . ?
C18 C19 C18 120.1(6) . 5 ?
C18 C19 C20 120.0(3) . . ?
C18 C19 C20 120.0(3) 5 . ?
C21 C20 C21 121.1(4) 14 . ?
C21 C20 C19 119.5(2) 14 . ?
C21 C20 C19 119.5(2) . . ?
C20 C21 C21 119.5(2) . 6 ?
C20 C21 C22 130.4(5) . . ?
C21 C21 C22 110.2(4) 6 . ?
N1 C22 C21 104.9(8) . . ?

_refine_diff_density_max         1.583
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.124



_vrf_PLAT220_LIFM-92             
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range
        6.6 Ratio 
RESPONSE: The crystal of insertion is not perfect. The 
phenyl rings and functional groups of the ligands can rotate
and result in high Ueq. We have used best crystal, Cu radiation
and long exposure time to acquire the best data.
;

_exptl_crystal_recrystallization_method 'Solvothermal Reaction'
####################################################################### 
# 
# 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_LIFM-90
_database_code_depnum_ccdc_archive 'CCDC 1544323'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            LIFM-90
_chemical_melting_point          ?
_chemical_formula_moiety         'C101 H73 N3 O32 Zr6'
_chemical_formula_sum            'C101 H73 N3 O32 Zr6'
_chemical_formula_weight         2387.94

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+1/2'
'-x, -y, z'
'y, -x, z+1/2'
'x, -y, -z'
'-x, y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y, -x, -z-1/2'
'x, y, -z'
'-y, x, -z-1/2'
'-x, y, z'
'x, -y, z'
'-y, -x, z-1/2'
'y, x, z-1/2'

_cell_length_a                   23.08420(10)
_cell_length_b                   23.08420(10)
_cell_length_c                   18.7738(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10004.19(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10693
_cell_measurement_theta_min      4.2560
_cell_measurement_theta_max      65.0210

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.793
_exptl_crystal_F_000             2392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.822
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.65152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_reflns_number            18268
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.830
_diffrn_reflns_theta_max         65.058
_diffrn_reflns_theta_full        65.058
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4546
_reflns_number_gt                4093
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1332P)²+24.6595P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4546
_refine_ls_number_parameters     282
_refine_ls_number_restraints     337
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1996
_refine_ls_wR_factor_gt          0.1943
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.39199(2) 0.0000 0.0000 0.0193(2) Uani 1 4 d S T P . .
Zr2 Zr 0.5000 0.07559(2) 0.09260(3) 0.0328(2) Uani 1 2 d S T P . .
O1 O 0.5000 0.1687(2) 0.0628(4) 0.0791(18) Uani 1 2 d S TU P . .
O2 O 0.4470(3) 0.0000 0.0922(4) 0.0668(18) Uani 1 2 d S T P . .
O3 O 0.34376(15) 0.05892(15) 0.07300(19) 0.0478(8) Uani 1 1 d . . . . .
O4 O 0.4468(3) 0.0748(3) 0.0000 0.074(2) Uani 1 2 d S T P . .
O5 O 0.5000 0.0549(4) 0.2068(4) 0.097(2) Uani 1 2 d S TU P . .
O6 O 0.41614(17) 0.1082(2) 0.1345(2) 0.0726(13) Uani 1 1 d . . . . .
N1 N 0.340(3) 0.4548(17) 0.0667(15) 0.256(11) Uani 0.0625 1 d D U P A 1
N2 N 0.320(3) 0.421(4) 0.109(4) 0.256(12) Uani 0.0625 1 d D U P A 1
N3 N 0.304(6) 0.383(4) 0.142(4) 0.256(16) Uani 0.0625 1 d D U P A 1
C1 C 0.2394(2) 0.1988(2) 0.2311(3) 0.090(2) Uani 1 1 d D . . . .
C2 C 0.2971(3) 0.1991(3) 0.2511(3) 0.130(4) Uani 1 1 d D . . . .
H2 H 0.3095 0.2229 0.2896 0.156 Uiso 0.734(15) 1 calc R U P B 2
C3 C 0.3370(2) 0.1648(3) 0.2152(3) 0.126(4) Uani 1 1 d D . . . .
H3 H 0.3765 0.1651 0.2291 0.151 Uiso 1 1 calc R U . . .
C4 C 0.3189(2) 0.1302(2) 0.1590(3) 0.0725(19) Uani 1 1 d D . . . .
C5 C 0.2613(2) 0.1295(3) 0.1391(3) 0.090(3) Uani 1 1 d D . . . .
H5 H 0.2491 0.1055 0.1009 0.108 Uiso 1 1 calc R U . . .
C6 C 0.2210(2) 0.1641(3) 0.1749(4) 0.107(3) Uani 1 1 d D . . . .
H6 H 0.1815 0.1639 0.1610 0.128 Uiso 0.266(15) 1 calc R U P B 1
C7 C 0.3636(2) 0.0959(3) 0.1191(3) 0.0606(16) Uani 1 1 d . . . . .
C8 C 0.3213(10) 0.2352(6) 0.3113(7) 0.220(12) Uani 0.266(15) 1 d D . P B 1
H8A H 0.3630 0.2283 0.3155 0.330 Uiso 0.266(15) 1 calc R U P B 1
H8B H 0.3143 0.2763 0.3015 0.330 Uiso 0.266(15) 1 calc R U P B 1
H8C H 0.3021 0.2244 0.3560 0.330 Uiso 0.266(15) 1 calc R U P B 1
C9 C 0.5000 0.0000 0.2322(6) 0.125(4) Uani 1 4 d DS TU P . .
C10 C 0.5000 0.0000 0.3118(4) 0.144(4) Uani 1 4 d DS TU P . .
C11 C 0.5281(6) 0.0441(4) 0.3487(5) 0.168(5) Uani 0.5 1 d D U P D .
H11 H 0.5473 0.0741 0.3234 0.202 Uiso 0.5 1 calc R U P . .
C12 C 0.5281(6) 0.0441(4) 0.4232(5) 0.184(6) Uani 0.5 1 d D U P . .
H12 H 0.5473 0.0741 0.4485 0.220 Uiso 0.25 1 calc R U P C 2
C13 C 0.5000 0.0000 0.4601(3) 0.192(7) Uani 1 4 d DS TU P D .
C14 C 0.5589(12) 0.0922(9) 0.4609(10) 0.200(11) Uani 0.25 1 d D U P D 1
H14A H 0.5758 0.1187 0.4258 0.300 Uiso 0.25 1 calc R U P D 1
H14B H 0.5314 0.1134 0.4908 0.300 Uiso 0.25 1 calc R U P D 1
H14C H 0.5898 0.0761 0.4908 0.300 Uiso 0.25 1 calc R U P D 1
C15 C 0.5000 0.1906(6) 0.0000 0.114(4) Uani 1 4 d DS TU P . .
C16 C 0.5000 0.2553(5) 0.0000 0.148(4) Uani 1 4 d DS TU P . .
C17 C 0.5000 0.2848(5) 0.0642(2) 0.189(5) Uani 1 2 d DS TU P . .
H17 H 0.5000 0.2641 0.1079 0.227 Uiso 1 2 calc R U P . .
C18 C 0.5000 0.3456(5) 0.0642(2) 0.216(5) Uani 1 2 d DS TU P . .
H18 H 0.5000 0.3661 0.1081 0.259 Uiso 1 2 calc R U P . .
C19 C 0.5000 0.3762(4) 0.0000 0.239(6) Uani 1 4 d DS TU P . .
C20 C 0.4800(11) 0.43956(18) 0.0000 0.251(7) Uani 0.5 2 d DS TU P . .
C21 C 0.5322(11) 0.46988(19) 0.0000 0.258(8) Uani 0.5 2 d DS TU P . .
H21 H 0.5679 0.4493 0.0000 0.310 Uiso 0.375 2 calc R U P E 4
C22 C 0.4276(11) 0.46993(18) 0.0000 0.256(8) Uani 0.5 2 d DS TU P . .
H22 H 0.3920 0.4494 0.0000 0.307 Uiso 0.375 2 calc R U P F 2
C23 C 0.3714(12) 0.4375(7) 0.0000 0.256(9) Uani 0.125 2 d DS TU P A 1
H23A H 0.3786(15) 0.3952(6) 0.0000 0.384 Uiso 0.125 2 d DS U P G 1
H23B H 0.3482(13) 0.4480(15) -0.0425(11) 0.384 Uiso 0.0625 1 d D U P H 1
C24 C 0.5886(12) 0.4372(7) 0.0000 0.261(9) Uani 0.125 2 d DS TU P I 3
C8A C 0.1591(4) 0.1612(6) 0.1493(7) 0.220(12) Uani 0.734(15) 1 d D . P B 2
H8A1 H 0.1563 0.1341 0.1094 0.330 Uiso 0.734(15) 1 calc R U P B 2
H8A2 H 0.1341 0.1480 0.1883 0.330 Uiso 0.734(15) 1 calc R U P B 2
H8A3 H 0.1466 0.1998 0.1337 0.330 Uiso 0.734(15) 1 calc R U P B 2
N4 N 0.6327(18) 0.464(3) -0.0495(10) 0.263(10) Uani 0.0625 1 d D U P I 3
N5 N 0.678(2) 0.483(2) -0.028(5) 0.265(11) Uani 0.0625 1 d D U P I 3
N6 N 0.7183(14) 0.5000 0.0000 0.267(12) Uani 0.25 4 d DS TU P I 3
H24A H 0.6046(13) 0.4363(15) 0.0489(3) 0.400 Uiso 0.0625 1 d D U P J 3
H24B H 0.5816(15) 0.3965(7) -0.014(2) 0.400 Uiso 0.0625 1 d D U P K 3


_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 O4 2.141(5) . ?
Zr1 O4 2.141(5) 5 ?
Zr1 O2 2.148(5) 11 ?
Zr1 O2 2.148(5) . ?
Zr1 O3 2.229(3) . ?
Zr1 O3 2.229(3) 5 ?
Zr1 O3 2.229(3) 14 ?
Zr1 O3 2.229(3) 11 ?
Zr1 Zr2 3.5047(5) . ?
Zr1 Zr2 3.5047(5) 11 ?
Zr1 Zr2 3.5047(5) 3_655 ?
Zr1 Zr2 3.5047(5) 9_655 ?
Zr2 O4 2.129(4) 13_655 ?
Zr2 O4 2.129(4) . ?
Zr2 O2 2.131(3) . ?
Zr2 O2 2.131(3) 3_655 ?
Zr2 O5 2.196(7) . ?
Zr2 O1 2.221(6) . ?
Zr2 O6 2.221(4) . ?
Zr2 O6 2.221(4) 13_655 ?
Zr2 Zr2 3.4769(10) 11 ?
Zr2 Zr2 3.4898(10) 3_655 ?
Zr2 Zr1 3.5047(5) 9_655 ?
O1 C15 1.283(9) . ?
O2 Zr2 2.131(3) 3_655 ?
O3 C7 1.300(7) . ?
O4 Zr2 2.129(4) 11 ?
O5 C9 1.354(10) . ?
O6 C7 1.279(7) . ?
N1 N2 1.210(10) . ?
N1 C23 1.498(10) . ?
N2 N3 1.133(10) . ?
C1 C2 1.384(6) . ?
C1 C6 1.392(6) . ?
C1 C1 1.501(9) 7 ?
C2 C3 1.389(6) . ?
C2 C8 1.510(9) . ?
C3 C4 1.389(6) . ?
C4 C5 1.380(6) . ?
C4 C7 1.500(6) . ?
C5 C6 1.398(6) . ?
C6 C8A 1.510(8) . ?
C9 O5 1.354(10) 3_655 ?
C9 C10 1.493(9) . ?
C10 C11 1.392(6) . ?
C10 C11 1.392(6) 3_655 ?
C10 C11 1.392(6) 13_655 ?
C10 C11 1.392(6) 14 ?
C11 C12 1.398(7) . ?
C11 C12 1.909(18) 13_655 ?
C12 C13 1.392(6) . ?
C12 C14 1.498(10) . ?
C12 C11 1.909(18) 13_655 ?
C13 C12 1.392(6) 3_655 ?
C13 C12 1.392(6) 14 ?
C13 C12 1.392(6) 13_655 ?
C13 C13 1.498(9) 5_556 ?
C15 O1 1.283(9) 11 ?
C15 C16 1.494(9) . ?
C16 C17 1.383(6) . ?
C16 C17 1.383(6) 6_655 ?
C17 C18 1.404(7) . ?
C18 C19 1.396(6) . ?
C19 C18 1.396(6) 6_655 ?
C19 C20 1.534(9) 6_655 ?
C19 C20 1.534(9) . ?
C20 C21 1.395(7) . ?
C20 C22 1.397(7) . ?
C21 C21 1.391(9) 5_565 ?
C21 C24 1.504(9) . ?
C22 C22 1.388(8) 5_565 ?
C22 C23 1.499(9) . ?
C23 N1 1.498(10) 11 ?
C24 C22 0.84(3) 6_655 ?
C24 N4 1.508(10) 11 ?
C24 N4 1.508(10) . ?
C24 C20 1.58(5) 6_655 ?
N4 N5 1.209(10) . ?
N4 N5 1.66(7) 14_565 ?
N4 N4 1.68(13) 14_565 ?
N4 C22 1.68(6) 6_655 ?
N4 N5 1.84(10) 11 ?
N4 N4 1.86(4) 11 ?
N5 N5 0.77(9) 14_565 ?
N5 N5 1.0(2) 11 ?
N5 N6 1.134(10) . ?
N5 N5 1.29(13) 5_565 ?
N5 N4 1.66(7) 14_565 ?
N5 N4 1.84(10) 11 ?
N6 N5 1.134(10) 14_565 ?
N6 N5 1.134(10) 11 ?
N6 N5 1.134(10) 5_565 ?

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
O4 Zr1 O4 107.5(4) . 5 ?
O4 Zr1 O2 69.54(14) . 11 ?
O4 Zr1 O2 69.54(14) 5 11 ?
O4 Zr1 O2 69.54(14) . . ?
O4 Zr1 O2 69.53(14) 5 . ?
O2 Zr1 O2 107.5(4) 11 . ?
O4 Zr1 O3 78.63(19) . . ?
O4 Zr1 O3 141.95(10) 5 . ?
O2 Zr1 O3 142.30(9) 11 . ?
O2 Zr1 O3 78.45(18) . . ?
O4 Zr1 O3 141.95(10) . 5 ?
O4 Zr1 O3 78.63(19) 5 5 ?
O2 Zr1 O3 78.45(18) 11 5 ?
O2 Zr1 O3 142.30(9) . 5 ?
O3 Zr1 O3 120.1(2) . 5 ?
O4 Zr1 O3 141.95(10) . 14 ?
O4 Zr1 O3 78.63(19) 5 14 ?
O2 Zr1 O3 142.30(9) 11 14 ?
O2 Zr1 O3 78.46(18) . 14 ?
O3 Zr1 O3 75.22(19) . 14 ?
O3 Zr1 O3 75.9(2) 5 14 ?
O4 Zr1 O3 78.63(19) . 11 ?
O4 Zr1 O3 141.95(10) 5 11 ?
O2 Zr1 O3 78.45(18) 11 11 ?
O2 Zr1 O3 142.30(9) . 11 ?
O3 Zr1 O3 75.9(2) . 11 ?
O3 Zr1 O3 75.22(19) 5 11 ?
O3 Zr1 O3 120.1(2) 14 11 ?
O4 Zr1 Zr2 34.71(11) . . ?
O4 Zr1 Zr2 88.92(19) 5 . ?
O2 Zr1 Zr2 88.80(17) 11 . ?
O2 Zr1 Zr2 34.84(10) . . ?
O3 Zr1 Zr2 75.32(10) . . ?
O3 Zr1 Zr2 164.62(10) 5 . ?
O3 Zr1 Zr2 110.75(10) 14 . ?
O3 Zr1 Zr2 110.89(9) 11 . ?
O4 Zr1 Zr2 34.71(11) . 11 ?
O4 Zr1 Zr2 88.92(19) 5 11 ?
O2 Zr1 Zr2 34.84(10) 11 11 ?
O2 Zr1 Zr2 88.80(17) . 11 ?
O3 Zr1 Zr2 110.89(9) . 11 ?
O3 Zr1 Zr2 110.75(10) 5 11 ?
O3 Zr1 Zr2 164.62(10) 14 11 ?
O3 Zr1 Zr2 75.32(10) 11 11 ?
Zr2 Zr1 Zr2 59.476(18) . 11 ?
O4 Zr1 Zr2 88.92(19) . 3_655 ?
O4 Zr1 Zr2 34.71(11) 5 3_655 ?
O2 Zr1 Zr2 88.80(17) 11 3_655 ?
O2 Zr1 Zr2 34.84(10) . 3_655 ?
O3 Zr1 Zr2 110.74(10) . 3_655 ?
O3 Zr1 Zr2 110.89(9) 5 3_655 ?
O3 Zr1 Zr2 75.32(10) 14 3_655 ?
O3 Zr1 Zr2 164.62(10) 11 3_655 ?
Zr2 Zr1 Zr2 59.717(19) . 3_655 ?
Zr2 Zr1 Zr2 89.303(17) 11 3_655 ?
O4 Zr1 Zr2 88.93(19) . 9_655 ?
O4 Zr1 Zr2 34.71(11) 5 9_655 ?
O2 Zr1 Zr2 34.84(10) 11 9_655 ?
O2 Zr1 Zr2 88.80(17) . 9_655 ?
O3 Zr1 Zr2 164.62(10) . 9_655 ?
O3 Zr1 Zr2 75.32(10) 5 9_655 ?
O3 Zr1 Zr2 110.89(9) 14 9_655 ?
O3 Zr1 Zr2 110.75(10) 11 9_655 ?
Zr2 Zr1 Zr2 89.303(17) . 9_655 ?
Zr2 Zr1 Zr2 59.718(19) 11 9_655 ?
Zr2 Zr1 Zr2 59.475(18) 3_655 9_655 ?
O4 Zr2 O4 70.5(3) 13_655 . ?
O4 Zr2 O2 108.8(3) 13_655 . ?
O4 Zr2 O2 70.1(2) . . ?
O4 Zr2 O2 70.1(2) 13_655 3_655 ?
O4 Zr2 O2 108.8(3) . 3_655 ?
O2 Zr2 O2 70.0(3) . 3_655 ?
O4 Zr2 O5 142.68(14) 13_655 . ?
O4 Zr2 O5 142.68(14) . . ?
O2 Zr2 O5 79.9(3) . . ?
O2 Zr2 O5 79.9(3) 3_655 . ?
O4 Zr2 O1 78.6(2) 13_655 . ?
O4 Zr2 O1 78.6(2) . . ?
O2 Zr2 O1 142.35(13) . . ?
O2 Zr2 O1 142.35(13) 3_655 . ?
O5 Zr2 O1 117.2(3) . . ?
O4 Zr2 O6 142.65(18) 13_655 . ?
O4 Zr2 O6 77.8(2) . . ?
O2 Zr2 O6 77.2(2) . . ?
O2 Zr2 O6 141.18(18) 3_655 . ?
O5 Zr2 O6 74.23(17) . . ?
O1 Zr2 O6 76.16(16) . . ?
O4 Zr2 O6 77.8(2) 13_655 13_655 ?
O4 Zr2 O6 142.65(18) . 13_655 ?
O2 Zr2 O6 141.18(18) . 13_655 ?
O2 Zr2 O6 77.2(2) 3_655 13_655 ?
O5 Zr2 O6 74.23(17) . 13_655 ?
O1 Zr2 O6 76.17(16) . 13_655 ?
O6 Zr2 O6 121.3(2) . 13_655 ?
O4 Zr2 Zr2 35.24(14) 13_655 11 ?
O4 Zr2 Zr2 35.25(14) . 11 ?
O2 Zr2 Zr2 89.82(18) . 11 ?
O2 Zr2 Zr2 89.82(18) 3_655 11 ?
O5 Zr2 Zr2 167.4(3) . 11 ?
O1 Zr2 Zr2 75.4(2) . 11 ?
O6 Zr2 Zr2 110.74(13) . 11 ?
O6 Zr2 Zr2 110.74(13) 13_655 11 ?
O4 Zr2 Zr2 89.51(19) 13_655 3_655 ?
O4 Zr2 Zr2 89.51(19) . 3_655 ?
O2 Zr2 Zr2 35.02(13) . 3_655 ?
O2 Zr2 Zr2 35.02(13) 3_655 3_655 ?
O5 Zr2 Zr2 77.4(3) . 3_655 ?
O1 Zr2 Zr2 165.4(2) . 3_655 ?
O6 Zr2 Zr2 109.84(13) . 3_655 ?
O6 Zr2 Zr2 109.83(13) 13_655 3_655 ?
Zr2 Zr2 Zr2 90.0 11 3_655 ?
O4 Zr2 Zr1 34.93(14) 13_655 9_655 ?
O4 Zr2 Zr1 90.07(19) . 9_655 ?
O2 Zr2 Zr1 89.94(17) . 9_655 ?
O2 Zr2 Zr1 35.16(15) 3_655 9_655 ?
O5 Zr2 Zr1 112.08(17) . 9_655 ?
O1 Zr2 Zr1 110.90(13) . 9_655 ?
O6 Zr2 Zr1 164.70(11) . 9_655 ?
O6 Zr2 Zr1 74.01(11) 13_655 9_655 ?
Zr2 Zr2 Zr1 60.262(9) 11 9_655 ?
Zr2 Zr2 Zr1 60.141(9) 3_655 9_655 ?
O4 Zr2 Zr1 90.07(19) 13_655 . ?
O4 Zr2 Zr1 34.93(14) . . ?
O2 Zr2 Zr1 35.16(15) . . ?
O2 Zr2 Zr1 89.94(17) 3_655 . ?
O5 Zr2 Zr1 112.08(17) . . ?
O1 Zr2 Zr1 110.90(13) . . ?
O6 Zr2 Zr1 74.01(11) . . ?
O6 Zr2 Zr1 164.70(11) 13_655 . ?
Zr2 Zr2 Zr1 60.262(9) 11 . ?
Zr2 Zr2 Zr1 60.141(9) 3_655 . ?
Zr1 Zr2 Zr1 90.697(17) 9_655 . ?
C15 O1 Zr2 127.9(7) . . ?
Zr2 O2 Zr2 110.0(3) . 3_655 ?
Zr2 O2 Zr1 110.0(2) . . ?
Zr2 O2 Zr1 110.0(2) 3_655 . ?
C7 O3 Zr1 129.4(3) . . ?
Zr2 O4 Zr2 109.5(3) 11 . ?
Zr2 O4 Zr1 110.4(2) 11 . ?
Zr2 O4 Zr1 110.4(2) . . ?
C9 O5 Zr2 123.2(7) . . ?
C7 O6 Zr2 132.2(3) . . ?
N2 N1 C23 124(5) . . ?
N3 N2 N1 171(9) . . ?
C2 C1 C6 120.1(4) . . ?
C2 C1 C1 118.0(5) . 7 ?
C6 C1 C1 121.8(5) . 7 ?
C1 C2 C3 120.2(4) . . ?
C1 C2 C8 124.1(10) . . ?
C3 C2 C8 115.6(10) . . ?
C2 C3 C4 119.9(4) . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 C7 121.5(5) . . ?
C3 C4 C7 118.5(5) . . ?
C4 C5 C6 120.3(4) . . ?
C1 C6 C5 119.4(4) . . ?
C1 C6 C8A 123.7(6) . . ?
C5 C6 C8A 116.9(6) . . ?
O6 C7 O3 129.1(5) . . ?
O6 C7 C4 115.0(5) . . ?
O3 C7 C4 115.9(5) . . ?
O5 C9 O5 138.7(11) . 3_655 ?
O5 C9 C10 110.7(6) . . ?
O5 C9 C10 110.7(6) 3_655 . ?
C11 C10 C11 120.3(7) . 3_655 ?
C11 C10 C11 55.6(12) . 13_655 ?
C11 C10 C11 93.9(11) 3_655 13_655 ?
C11 C10 C11 93.9(11) . 14 ?
C11 C10 C11 55.6(12) 3_655 14 ?
C11 C10 C11 120.3(7) 13_655 14 ?
C11 C10 C9 119.9(3) . . ?
C11 C10 C9 119.9(3) 3_655 . ?
C11 C10 C9 119.9(3) 13_655 . ?
C11 C10 C9 119.9(3) 14 . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 C12 92.7(8) . 13_655 ?
C12 C11 C12 42.9(6) . 13_655 ?
C13 C12 C11 119.9(4) . . ?
C13 C12 C14 121.9(9) . . ?
C11 C12 C14 118.2(8) . . ?
C13 C12 C11 92.7(8) . 13_655 ?
C11 C12 C11 42.9(6) . 13_655 ?
C14 C12 C11 132.0(8) . 13_655 ?
C12 C13 C12 55.7(12) 3_655 14 ?
C12 C13 C12 120.2(6) 3_655 . ?
C12 C13 C12 93.9(11) 14 . ?
C12 C13 C12 93.9(11) 3_655 13_655 ?
C12 C13 C12 120.2(6) 14 13_655 ?
C12 C13 C12 55.7(12) . 13_655 ?
C12 C13 C13 119.9(3) 3_655 5_556 ?
C12 C13 C13 119.9(3) 14 5_556 ?
C12 C13 C13 119.9(3) . 5_556 ?
C12 C13 C13 119.9(3) 13_655 5_556 ?
O1 C15 O1 133.5(12) . 11 ?
O1 C15 C16 113.3(6) . . ?
O1 C15 C16 113.3(6) 11 . ?
C17 C16 C17 121.1(7) . 6_655 ?
C17 C16 C15 119.5(3) . . ?
C17 C16 C15 119.5(3) 6_655 . ?
C16 C17 C18 119.5(5) . . ?
C19 C18 C17 120.4(5) . . ?
C18 C19 C18 119.3(7) 6_655 . ?
C18 C19 C20 118.8(3) 6_655 6_655 ?
C18 C19 C20 118.8(3) . 6_655 ?
C18 C19 C20 118.8(3) 6_655 . ?
C18 C19 C20 118.8(3) . . ?
C20 C19 C20 35.1(19) 6_655 . ?
C21 C20 C22 119.8(4) . . ?
C21 C20 C19 102.6(10) . . ?
C22 C20 C19 137.7(10) . . ?
C21 C21 C20 120.1(2) 5_565 . ?
C21 C21 C24 120.1(8) 5_565 . ?
C20 C21 C24 119.8(8) . . ?
C22 C22 C20 120.1(3) 5_565 . ?
C22 C22 C23 120.0(7) 5_565 . ?
C20 C22 C23 119.9(8) . . ?
N1 C23 N1 113(4) . 11 ?
N1 C23 C22 106(3) . . ?
N1 C23 C22 106(3) 11 . ?
C22 C24 C21 34(3) 6_655 . ?
C22 C24 N4 86(4) 6_655 11 ?
C21 C24 N4 112(2) . 11 ?
C22 C24 N4 86(4) 6_655 . ?
C21 C24 N4 112(2) . . ?
N4 C24 N4 76.1(16) 11 . ?
C22 C24 C20 62(3) 6_655 6_655 ?
C21 C24 C20 28.1(3) . 6_655 ?
N4 C24 C20 131.4(16) 11 6_655 ?
N4 C24 C20 131.4(16) . 6_655 ?
N5 N4 C24 122(6) . . ?
N5 N4 N5 25(2) . 14_565 ?
C24 N4 N5 125(4) . 14_565 ?
N5 N4 N4 68(2) . 14_565 ?
C24 N4 N4 114(3) . 14_565 ?
N5 N4 N4 43(3) 14_565 14_565 ?
N5 N4 C22 120(5) . 6_655 ?
C24 N4 C22 30.1(9) . 6_655 ?
N5 N4 C22 109(5) 14_565 6_655 ?
N4 N4 C22 85(2) 14_565 6_655 ?
N5 N4 N5 32(6) . 11 ?
C24 N4 N5 89.9(13) . 11 ?
N5 N4 N5 43(3) 14_565 11 ?
N4 N4 N5 75.8(9) 14_565 11 ?
C22 N4 N5 90.8(19) 6_655 11 ?
N5 N4 N4 70(5) . 11 ?
C24 N4 N4 52.0(8) . 11 ?
N5 N4 N4 76(3) 14_565 11 ?
N4 N4 N4 90.002(6) 14_565 11 ?
C22 N4 N4 56.4(11) 6_655 11 ?
N5 N4 N4 38.2(10) 11 11 ?
N5 N5 N5 90.00(2) 14_565 11 ?
N5 N5 N6 70(3) 14_565 . ?
N5 N5 N6 63(6) 11 . ?
N5 N5 N4 112(2) 14_565 . ?
N5 N5 N4 110(5) 11 . ?
N6 N5 N4 173(10) . . ?
N5 N5 N5 53(8) 14_565 5_565 ?
N5 N5 N5 37(8) 11 5_565 ?
N6 N5 N5 55(4) . 5_565 ?
N4 N5 N5 120(5) . 5_565 ?
N5 N5 N4 43(3) 14_565 14_565 ?
N5 N5 N4 104(3) 11 14_565 ?
N6 N5 N4 112(5) . 14_565 ?
N4 N5 N4 70(4) . 14_565 ?
N5 N5 N4 76(4) 5_565 14_565 ?
N5 N5 N4 104.2(9) 14_565 11 ?
N5 N5 N4 38.2(10) 11 11 ?
N6 N5 N4 101(6) . 11 ?
N4 N5 N4 72(5) . 11 ?
N5 N5 N4 61(6) 5_565 11 ?
N4 N5 N4 91(4) 14_565 11 ?
N5 N6 N5 70(8) 14_565 11 ?
N5 N6 N5 54(10) 14_565 5_565 ?
N5 N6 N5 40(5) 11 5_565 ?
N5 N6 N5 40(5) 14_565 . ?
N5 N6 N5 54(10) 11 . ?
N5 N6 N5 70(8) 5_565 . ?

_refine_diff_density_max         0.775
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.126



_exptl_crystal_recrystallization_method 'Solvothermal Reaction'
