# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_TCM-16
_database_code_depnum_ccdc_archive 'CCDC 1916002'
loop_
_audit_author_name
_audit_author_address
'Nian-Yong Zhu'
;Trinity College Dublin
Republic of Ireland
;
_audit_update_record             
;
2019-06-24 deposited with the CCDC.	2019-07-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_TCM-16              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The MOF crystal diffracted relativly weak because of high content of solent molecules in the lattice.
;
_vrf_PLAT250_TCM-16              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.0 Note
RESPONSE: The large U3/U1 ratio are from the C atoms of the organic linker, which indicate the statistic shifts of C atoms for maintaining the high symmetry.
;
_vrf_PLAT430_TCM-16              
;
PROBLEM: Short Inter D...A Contact  O4       ..O5       .       2.63 Ang.
RESPONSE: The short contacts are from the same Secondary-Building-Unit, and the atoms of O5/O6 are from the disordered carboxylate, for which some restrains (planarity) were applied for convergent structural refinements, these might be the main reasons for the slight short intra O..O contacts
;
_vrf_PLAT430_TCM-16_2            
;
PROBLEM: Short Inter D...A Contact  O4       ..O6       .       2.80 Ang.
RESPONSE: The short contacts are from the same Secondary-Building-Unit, and the atoms of O5/O6 are from the disordered carboxylate, for which some restrains (planarity) were applied for convergent structural refinements, these might be the main reasons for the slight short intra O..O contacts
;
# Added during the CSD deposition process: Monday 24 June 2019 12:28 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Zr6 (O)4 (OH)4 (H2O)4 (C33H15O6)4, 30(C3H7NO)'

# the 30(C3H7NO) dmf solvent molecules were estimated according to the Platon-squeeze
# routine, in which the void volume is 19021 A(3) with corresponding 2311 electron count
# in the unit cell

_chemical_formula_sum            'C222 H282 N30 O66 Zr6'
_chemical_formula_weight         4974.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zr Zr -0.1862 2.2449 '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'
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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

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

_cell_length_a                   33.102(3)
_cell_length_b                   33.102(3)
_cell_length_c                   21.711(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23790(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    215(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      45.69

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.694
_exptl_crystal_F_000             5184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.406
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2276
_exptl_absorpt_correction_T_max  0.7490
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      215(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39877
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.434
_diffrn_reflns_theta_max         45.813
_diffrn_reflns_theta_full        45.813
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5175
_reflns_number_gt                4098
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0950P)²+67.0649P] 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         5175
_refine_ls_number_parameters     220
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1762
_refine_ls_wR_factor_gt          0.1643
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_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 0.500000 0.500000 0.11330(4) 0.0365(4) Uani 1 4 d S T P . .
Zr2 Zr 0.54090(2) 0.43671(2) 0.000000 0.0438(3) Uani 1 2 d S T P . .
O1 O 0.48862(10) 0.44799(13) 0.05517(18) 0.0799(15) Uani 1 1 d . . . . .
O2 O 0.52432(19) 0.37150(16) 0.000000 0.0779(19) Uani 1 2 d S T P . .
O3 O 0.54723(11) 0.53047(10) 0.16555(17) 0.0445(10) Uani 1 1 d . . . . .
O4 O 0.58938(12) 0.55591(13) 0.0943(2) 0.0749(14) Uani 1 1 d . . . . .
O5 O 0.92420(18) 0.89608(18) 0.500000 0.0719(18) Uani 1 2 d S T P . .
O6 O 0.9467(3) 0.8677(3) 0.5932(5) 0.106(4) Uani 0.5 1 d . . P . .
C1 C 0.5782(2) 0.55002(19) 0.1498(3) 0.0591(18) Uani 1 1 d . U . . .
C2 C 0.60316(16) 0.56806(17) 0.1994(2) 0.092(3) Uani 1 1 d G U . . .
C3 C 0.63637(17) 0.59200(18) 0.18520(19) 0.119(3) Uani 1 1 d G U . . .
H3 H 0.643292 0.596709 0.143827 0.143 Uiso 1 1 calc R U . . .
C4 C 0.65933(15) 0.60899(19) 0.2321(3) 0.147(4) Uani 1 1 d G U . . .
H4 H 0.681788 0.625181 0.222488 0.177 Uiso 1 1 calc R U . . .
C5 C 0.64909(19) 0.6020(2) 0.2933(2) 0.157(5) Uani 1 1 d G U . . .
C6 C 0.6159(2) 0.5781(2) 0.30755(17) 0.196(6) Uani 1 1 d G U . . .
H6 H 0.608964 0.573382 0.348923 0.236 Uiso 1 1 calc R U . . .
C7 C 0.59292(16) 0.56110(18) 0.2606(2) 0.156(5) Uani 1 1 d G U . . .
H7 H 0.570467 0.544909 0.270262 0.187 Uiso 1 1 calc R U . . .
C8 C 0.6707(3) 0.6185(4) 0.3440(5) 0.182(6) Uani 1 1 d . U . . .
C9 C 0.6882(4) 0.6313(4) 0.3878(4) 0.180(6) Uani 1 1 d . U . . .
C10 C 0.6908(4) 0.6310(5) 0.500000 0.180(8) Uani 1 2 d S TU P . .
H10 H 0.669882 0.611772 0.500000 0.216 Uiso 1 2 calc R U P . .
C11 C 0.7067(3) 0.6456(3) 0.4450(4) 0.174(5) Uani 1 1 d . U . . .
C12 C 0.7367(2) 0.6754(3) 0.4440(4) 0.169(5) Uani 1 1 d . U . . .
H12 H 0.746300 0.686042 0.406665 0.203 Uiso 1 1 calc R U . . .
C13 C 0.7520(4) 0.6885(4) 0.500000 0.135(5) Uani 1 2 d S TU P . .
C14 C 0.7813(4) 0.7182(5) 0.500000 0.165(7) Uani 1 2 d S TU P . .
C15 C 0.8074(5) 0.7432(4) 0.500000 0.156(6) Uani 1 2 d S TU P . .
C16 C 0.8367(3) 0.7772(3) 0.5194(6) 0.110(7) Uani 0.5 1 d G U P . .
C17 C 0.8409(3) 0.8083(4) 0.4768(5) 0.150(9) Uani 0.5 1 d G U P . .
H17 H 0.823750 0.809570 0.442404 0.180 Uiso 0.5 1 calc R U P . .
C18 C 0.8705(4) 0.8376(3) 0.4852(5) 0.085(6) Uani 0.5 1 d G U P . .
H18 H 0.873344 0.858658 0.456472 0.102 Uiso 0.5 1 calc R U P . .
C19 C 0.8959(3) 0.8358(2) 0.5362(5) 0.073(5) Uani 0.5 1 d G U P . .
C20 C 0.8917(3) 0.8047(3) 0.5787(5) 0.144(8) Uani 0.5 1 d G U P . .
H20 H 0.908849 0.803475 0.613130 0.172 Uiso 0.5 1 calc R U P . .
C21 C 0.8621(4) 0.7754(3) 0.5703(5) 0.141(8) Uani 0.5 1 d G U P . .
H21 H 0.859255 0.754386 0.599063 0.170 Uiso 0.5 1 calc R U P . .
C22 C 0.9250(4) 0.8673(4) 0.5439(8) 0.076(4) Uani 0.5 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.168(4) 4_565 ?
Zr1 O1 2.168(4) 3_655 ?
Zr1 O1 2.168(4) 2_665 ?
Zr1 O1 2.168(4) . ?
Zr1 O3 2.179(4) 3_655 ?
Zr1 O3 2.179(4) 2_665 ?
Zr1 O3 2.179(4) 4_565 ?
Zr1 O3 2.179(4) . ?
Zr2 O1 2.127(4) 3_655 ?
Zr2 O1 2.127(4) 12_655 ?
Zr2 O5 2.127(6) 7_644 ?
Zr2 O1 2.137(4) . ?
Zr2 O1 2.138(4) 10 ?
Zr2 O2 2.228(5) . ?
Zr2 O4 2.277(4) 11_565 ?
Zr2 O4 2.277(4) 4_565 ?
O3 C1 1.260(7) . ?
O4 C1 1.274(7) . ?
O5 C22 1.349(14) . ?
O5 C22 1.349(14) 10_556 ?
O6 C22 1.290(16) . ?
C1 C2 1.484(7) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9400 . ?
C4 C5 1.3900 . ?
C4 H4 0.9400 . ?
C5 C6 1.3900 . ?
C5 C8 1.422(10) . ?
C6 C7 1.3900 . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?
C8 C9 1.189(11) . ?
C9 C11 1.463(12) . ?
C10 C11 1.392(9) . ?
C10 C11 1.392(9) 10_556 ?
C10 H10 0.9400 . ?
C11 C12 1.402(10) . ?
C12 C13 1.386(8) . ?
C12 H12 0.9400 . ?
C13 C14 1.381(15) . ?
C14 C15 1.197(15) . ?
C15 C16 1.544(15) . ?
C15 C16 1.544(15) 10_556 ?
C16 C16 0.84(2) 10_556 ?
C16 C17 1.0422(17) 10_556 ?
C16 C17 1.3900 . ?
C16 C21 1.3900 . ?
C17 C18 1.3900 . ?
C17 H17 0.9400 . ?
C18 C19 1.3900 . ?
C18 H18 0.9400 . ?
C19 C20 1.3900 . ?
C19 C22 1.429(13) . ?
C19 C19 1.57(2) 10_556 ?
C20 C21 1.3900 . ?
C20 H20 0.9400 . ?
C21 H21 0.9400 . ?
C22 C22 1.91(3) 10_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O1 108.8(2) 4_565 3_655 ?
O1 Zr1 O1 70.19(13) 4_565 2_665 ?
O1 Zr1 O1 70.19(13) 3_655 2_665 ?
O1 Zr1 O1 70.19(13) 4_565 . ?
O1 Zr1 O1 70.18(13) 3_655 . ?
O1 Zr1 O1 108.8(2) 2_665 . ?
O1 Zr1 O3 79.09(15) 4_565 3_655 ?
O1 Zr1 O3 142.70(12) 3_655 3_655 ?
O1 Zr1 O3 79.27(14) 2_665 3_655 ?
O1 Zr1 O3 142.42(12) . 3_655 ?
O1 Zr1 O3 79.27(14) 4_565 2_665 ?
O1 Zr1 O3 142.42(12) 3_655 2_665 ?
O1 Zr1 O3 142.70(12) 2_665 2_665 ?
O1 Zr1 O3 79.10(15) . 2_665 ?
O3 Zr1 O3 74.27(10) 3_655 2_665 ?
O1 Zr1 O3 142.70(12) 4_565 4_565 ?
O1 Zr1 O3 79.09(15) 3_655 4_565 ?
O1 Zr1 O3 142.42(12) 2_665 4_565 ?
O1 Zr1 O3 79.26(14) . 4_565 ?
O3 Zr1 O3 117.2(2) 3_655 4_565 ?
O3 Zr1 O3 74.27(10) 2_665 4_565 ?
O1 Zr1 O3 142.42(12) 4_565 . ?
O1 Zr1 O3 79.26(14) 3_655 . ?
O1 Zr1 O3 79.09(15) 2_665 . ?
O1 Zr1 O3 142.69(12) . . ?
O3 Zr1 O3 74.28(10) 3_655 . ?
O3 Zr1 O3 117.3(2) 2_665 . ?
O3 Zr1 O3 74.27(10) 4_565 . ?
O1 Zr2 O1 68.6(2) 3_655 12_655 ?
O1 Zr2 O5 89.29(19) 3_655 7_644 ?
O1 Zr2 O5 89.29(19) 12_655 7_644 ?
O1 Zr2 O1 71.5(2) 3_655 . ?
O1 Zr2 O1 108.3(3) 12_655 . ?
O5 Zr2 O1 145.91(10) 7_644 . ?
O1 Zr2 O1 108.3(3) 3_655 10 ?
O1 Zr2 O1 71.5(2) 12_655 10 ?
O5 Zr2 O1 145.91(10) 7_644 10 ?
O1 Zr2 O1 68.2(2) . 10 ?
O1 Zr2 O2 145.66(10) 3_655 . ?
O1 Zr2 O2 145.66(10) 12_655 . ?
O5 Zr2 O2 93.0(2) 7_644 . ?
O1 Zr2 O2 88.26(18) . . ?
O1 Zr2 O2 88.26(18) 10 . ?
O1 Zr2 O4 140.83(15) 3_655 11_565 ?
O1 Zr2 O4 76.24(16) 12_655 11_565 ?
O5 Zr2 O4 73.28(13) 7_644 11_565 ?
O1 Zr2 O4 138.30(15) . 11_565 ?
O1 Zr2 O4 74.86(15) 10 11_565 ?
O2 Zr2 O4 71.71(13) . 11_565 ?
O1 Zr2 O4 76.24(16) 3_655 4_565 ?
O1 Zr2 O4 140.83(15) 12_655 4_565 ?
O5 Zr2 O4 73.28(13) 7_644 4_565 ?
O1 Zr2 O4 74.86(15) . 4_565 ?
O1 Zr2 O4 138.30(15) 10 4_565 ?
O2 Zr2 O4 71.71(13) . 4_565 ?
O4 Zr2 O4 128.1(2) 11_565 4_565 ?
Zr2 O1 Zr2 111.64(18) 4_565 . ?
Zr2 O1 Zr1 109.33(17) 4_565 . ?
Zr2 O1 Zr1 108.92(18) . . ?
C1 O3 Zr1 132.8(4) . . ?
C1 O4 Zr2 134.9(4) . 3_655 ?
C22 O5 C22 90.0(13) . 10_556 ?
C22 O5 Zr2 133.6(7) . 15_565 ?
C22 O5 Zr2 133.6(7) 10_556 15_565 ?
O3 C1 O4 124.9(5) . . ?
O3 C1 C2 117.5(6) . . ?
O4 C1 C2 117.6(6) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 120.5(5) . . ?
C7 C2 C1 119.5(5) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 123.6(5) . . ?
C6 C5 C8 116.4(5) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C9 C8 C5 177.5(10) . . ?
C8 C9 C11 174.9(9) . . ?
C11 C10 C11 118.3(11) . 10_556 ?
C11 C10 H10 120.8 . . ?
C11 C10 H10 120.8 10_556 . ?
C10 C11 C12 121.6(8) . . ?
C10 C11 C9 117.3(7) . . ?
C12 C11 C9 120.9(7) . . ?
C13 C12 C11 117.9(8) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C14 C13 C12 118.7(5) . 10_556 ?
C14 C13 C12 118.7(5) . . ?
C12 C13 C12 122.5(9) 10_556 . ?
C15 C14 C13 178.6(19) . . ?
C14 C15 C16 163.3(7) . . ?
C14 C15 C16 163.3(7) . 10_556 ?
C16 C15 C16 31.6(10) . 10_556 ?
C16 C16 C17 94.5(12) 10_556 10_556 ?
C16 C16 C17 48.4(4) 10_556 . ?
C17 C16 C17 46.2(11) 10_556 . ?
C16 C16 C21 142.7(4) 10_556 . ?
C17 C16 C21 84.2(9) 10_556 . ?
C17 C16 C21 120.0 . . ?
C16 C16 C15 74.2(5) 10_556 . ?
C17 C16 C15 145.7(11) 10_556 . ?
C17 C16 C15 115.0(9) . . ?
C21 C16 C15 124.4(9) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C18 23.8(11) 10_556 . ?
C18 C19 C20 106.2(7) 10_556 . ?
C18 C19 C20 120.0 . . ?
C18 C19 C22 126.9(11) 10_556 . ?
C18 C19 C22 118.0(10) . . ?
C20 C19 C22 122.0(10) . . ?
C18 C19 C19 61.1(11) 10_556 10_556 ?
C18 C19 C19 37.3 . 10_556 ?
C20 C19 C19 131.6 . 10_556 ?
C22 C19 C19 96.8(10) . 10_556 ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C16 120.0 . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
O6 C22 O5 126.1(11) . . ?
O6 C22 C19 118.8(13) . . ?
O5 C22 C19 114.8(12) . . ?
O6 C22 C22 146.1(8) . 10_556 ?
O5 C22 C22 45.0(7) . 10_556 ?
C19 C22 C22 83.2(8) . 10_556 ?

_refine_diff_density_max         0.491
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.058



_exptl_crystal_recrystallization_method 'solvothermal reaction'
_chemical_properties_physical    'easily lost solvent'
