# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_zn-mof-crown
_audit_block_doi                 10.5517/cc1k1tq4
_database_code_depnum_ccdc_archive 'CCDC 1431726'
_audit_update_record             
;
2015-12-02 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 O25 Zn4'
_chemical_formula_weight         949.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.2657(8)
_cell_length_b                   18.2657(8)
_cell_length_c                   22.3708(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6463.8(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    516
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      25.48

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15406
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1811
_reflns_number_gt                952
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;


# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.022 -0.015 -0.001 3964 494 ' '
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0320P)²+36.4392P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1811
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.1969
_refine_ls_wR_factor_gt          0.1782
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.3333 0.6667 0.07962(10) 0.0558(7) Uani 0.50 6 d SP . .
Zn2 Zn 0.44924(8) 0.72462(4) 0.13770(6) 0.0563(5) Uani 0.50 2 d SP . .
O1 O 0.3333 0.6667 0.1667 0.0311(17) Uani 1 12 d S . .
O3 O 0.4312(3) 0.8625(6) 0.1295(5) 0.087(3) Uani 0.50 2 d SP . .
O2 O 0.4713(4) 0.8220(4) 0.0889(3) 0.088(2) Uani 0.50 1 d P . .
O4 O 0.3910(3) 0.7820(6) 0.0492(4) 0.088(3) Uani 0.50 2 d SP . .
C2 C 0.4640(5) 0.9280(10) 0.0385(5) 0.095(3) Uani 1 2 d S . .
C1 C 0.4259(2) 0.8518(5) 0.0736(4) 0.086(2) Uani 1 2 d S . .
C3 C 0.5373(13) 0.9925(15) 0.0469(10) 0.153(8) Uani 0.50 1 d P . .
C4 C 0.505(2) 0.9337(13) -0.0010(16) 0.192(14) Uani 0.50 1 d P . .
O5 O 0.5891(19) 0.9972(14) 0.093(2) 0.53(2) Uani 0.50 1 d P . .
O6 O 0.5211(19) 0.888(2) -0.0270(11) 0.54(3) Uani 0.50 1 d 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
Zn1 O1 1.947(2) . ?
Zn1 O4 1.948(9) 2_665 ?
Zn1 O4 1.948(9) . ?
Zn1 O4 1.948(9) 3_565 ?
Zn1 Zn2 2.2471(19) 2_665 ?
Zn1 Zn2 2.247(2) . ?
Zn1 Zn2 2.247(2) 3_565 ?
Zn2 O1 1.9446(13) . ?
Zn2 O3 1.946(9) 26_455 ?
Zn2 O2 1.950(6) 24_565 ?
Zn2 O2 1.950(6) . ?
Zn2 Zn2 2.2453(19) 26_455 ?
Zn2 Zn2 2.2454(19) 27 ?
O1 Zn2 1.9446(13) 26_455 ?
O1 Zn2 1.9446(13) 2_665 ?
O1 Zn2 1.9446(13) 3_565 ?
O1 Zn2 1.9447(13) 27 ?
O1 Zn2 1.9447(13) 25_565 ?
O1 Zn1 1.947(2) 25_565 ?
O3 C1 1.261(12) . ?
O3 O2 1.564(10) 23 ?
O3 O2 1.564(10) . ?
O3 Zn2 1.946(9) 27 ?
O2 C1 1.246(7) . ?
O2 O4 1.551(10) . ?
O4 C1 1.232(11) . ?
O4 O2 1.551(10) 23 ?
C2 C4 1.13(3) 23 ?
C2 C4 1.13(3) . ?
C2 C3 1.28(2) 23 ?
C2 C3 1.28(2) . ?
C2 C1 1.438(13) . ?
C1 O2 1.246(7) 23 ?
C3 O5 1.38(5) . ?
C3 C4 1.42(3) . ?
C3 C3 1.50(5) 23 ?
C3 C4 1.56(3) 5_675 ?
C3 C4 2.03(2) 23 ?
C4 O6 1.16(5) . ?
C4 C4 1.40(6) 23 ?
C4 C3 1.56(3) 5_675 ?
C4 C3 2.03(2) 23 ?

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 Zn1 O4 110.4(3) . 2_665 ?
O1 Zn1 O4 110.4(3) . . ?
O4 Zn1 O4 108.5(3) 2_665 . ?
O1 Zn1 O4 110.4(3) . 3_565 ?
O4 Zn1 O4 108.5(3) 2_665 3_565 ?
O4 Zn1 O4 108.5(3) . 3_565 ?
O1 Zn1 Zn2 54.68(6) . 2_665 ?
O4 Zn1 Zn2 79.6(2) 2_665 2_665 ?
O4 Zn1 Zn2 79.6(2) . 2_665 ?
O4 Zn1 Zn2 165.1(3) 3_565 2_665 ?
O1 Zn1 Zn2 54.68(6) . . ?
O4 Zn1 Zn2 165.1(3) 2_665 . ?
O4 Zn1 Zn2 79.6(2) . . ?
O4 Zn1 Zn2 79.6(2) 3_565 . ?
Zn2 Zn1 Zn2 89.92(9) 2_665 . ?
O1 Zn1 Zn2 54.68(6) . 3_565 ?
O4 Zn1 Zn2 79.6(2) 2_665 3_565 ?
O4 Zn1 Zn2 165.1(3) . 3_565 ?
O4 Zn1 Zn2 79.6(2) 3_565 3_565 ?
Zn2 Zn1 Zn2 89.92(9) 2_665 3_565 ?
Zn2 Zn1 Zn2 89.92(9) . 3_565 ?
O1 Zn2 O3 111.0(3) . 26_455 ?
O1 Zn2 O2 110.8(2) . 24_565 ?
O3 Zn2 O2 108.0(3) 26_455 24_565 ?
O1 Zn2 O2 110.8(2) . . ?
O3 Zn2 O2 108.0(3) 26_455 . ?
O2 Zn2 O2 108.0(5) 24_565 . ?
O1 Zn2 Zn2 54.74(2) . 26_455 ?
O3 Zn2 Zn2 80.0(2) 26_455 26_455 ?
O2 Zn2 Zn2 79.9(2) 24_565 26_455 ?
O2 Zn2 Zn2 165.6(2) . 26_455 ?
O1 Zn2 Zn2 54.74(2) . 27 ?
O3 Zn2 Zn2 80.0(2) 26_455 27 ?
O2 Zn2 Zn2 165.6(2) 24_565 27 ?
O2 Zn2 Zn2 79.9(2) . 27 ?
Zn2 Zn2 Zn2 90.01(9) 26_455 27 ?
O1 Zn2 Zn1 54.79(6) . . ?
O3 Zn2 Zn1 165.8(3) 26_455 . ?
O2 Zn2 Zn1 79.8(2) 24_565 . ?
O2 Zn2 Zn1 79.8(2) . . ?
Zn2 Zn2 Zn1 90.04(5) 26_455 . ?
Zn2 Zn2 Zn1 90.04(5) 27 . ?
Zn2 O1 Zn2 180.0 26_455 2_665 ?
Zn2 O1 Zn2 70.53(4) 26_455 3_565 ?
Zn2 O1 Zn2 109.48(4) 2_665 3_565 ?
Zn2 O1 Zn2 70.53(4) 26_455 . ?
Zn2 O1 Zn2 109.48(4) 2_665 . ?
Zn2 O1 Zn2 109.48(4) 3_565 . ?
Zn2 O1 Zn2 109.48(4) 26_455 27 ?
Zn2 O1 Zn2 70.52(4) 2_665 27 ?
Zn2 O1 Zn2 180.0 3_565 27 ?
Zn2 O1 Zn2 70.53(4) . 27 ?
Zn2 O1 Zn2 109.48(4) 26_455 25_565 ?
Zn2 O1 Zn2 70.52(4) 2_665 25_565 ?
Zn2 O1 Zn2 70.53(4) 3_565 25_565 ?
Zn2 O1 Zn2 180.0 . 25_565 ?
Zn2 O1 Zn2 109.47(4) 27 25_565 ?
Zn2 O1 Zn1 109.47(4) 26_455 . ?
Zn2 O1 Zn1 70.53(4) 2_665 . ?
Zn2 O1 Zn1 70.53(4) 3_565 . ?
Zn2 O1 Zn1 70.53(4) . . ?
Zn2 O1 Zn1 109.47(4) 27 . ?
Zn2 O1 Zn1 109.47(4) 25_565 . ?
Zn2 O1 Zn1 70.53(4) 26_455 25_565 ?
Zn2 O1 Zn1 109.46(4) 2_665 25_565 ?
Zn2 O1 Zn1 109.47(4) 3_565 25_565 ?
Zn2 O1 Zn1 109.47(4) . 25_565 ?
Zn2 O1 Zn1 70.53(4) 27 25_565 ?
Zn2 O1 Zn1 70.53(4) 25_565 25_565 ?
Zn1 O1 Zn1 180.0 . 25_565 ?
C1 O3 O2 51.0(4) . 23 ?
C1 O3 O2 51.0(4) . . ?
O2 O3 O2 89.6(8) 23 . ?
C1 O3 Zn2 131.9(7) . 27 ?
O2 O3 Zn2 100.1(4) 23 27 ?
O2 O3 Zn2 100.1(4) . 27 ?
C1 O2 O4 50.9(6) . . ?
C1 O2 O3 51.8(6) . . ?
O4 O2 O3 89.9(6) . . ?
C1 O2 Zn2 132.3(5) . . ?
O4 O2 Zn2 100.1(5) . . ?
O3 O2 Zn2 100.0(5) . . ?
C1 O4 O2 51.7(4) . 23 ?
C1 O4 O2 51.7(4) . . ?
O2 O4 O2 90.5(8) 23 . ?
C1 O4 Zn1 133.2(7) . . ?
O2 O4 Zn1 100.5(5) 23 . ?
O2 O4 Zn1 100.5(5) . . ?
C4 C2 C4 77(3) 23 . ?
C4 C2 C3 71.9(18) 23 23 ?
C4 C2 C3 114.5(16) . 23 ?
C4 C2 C3 114.5(16) 23 . ?
C4 C2 C3 71.9(18) . . ?
C3 C2 C3 72(3) 23 . ?
C4 C2 C1 119.5(17) 23 . ?
C4 C2 C1 119.5(17) . . ?
C3 C2 C1 126.0(10) 23 . ?
C3 C2 C1 126.0(10) . . ?
O4 C1 O2 77.5(6) . 23 ?
O4 C1 O2 77.5(6) . . ?
O2 C1 O2 124.2(8) 23 . ?
O4 C1 O3 124.0(8) . . ?
O2 C1 O3 77.2(6) 23 . ?
O2 C1 O3 77.2(6) . . ?
O4 C1 C2 120.6(11) . . ?
O2 C1 C2 117.8(4) 23 . ?
O2 C1 C2 117.8(4) . . ?
O3 C1 C2 115.5(11) . . ?
C2 C3 O5 122.5(18) . . ?
C2 C3 C4 49.2(16) . . ?
O5 C3 C4 129(3) . . ?
C2 C3 C3 54.1(14) . 23 ?
O5 C3 C3 131(2) . 23 ?
C4 C3 C3 88.1(16) . 23 ?
C2 C3 C4 118.9(15) . 5_675 ?
O5 C3 C4 118(2) . 5_675 ?
C4 C3 C4 89.6(16) . 5_675 ?
C3 C3 C4 88.2(15) 23 5_675 ?
C2 C3 C4 30.5(11) . 23 ?
O5 C3 C4 153(2) . 23 ?
C4 C3 C4 44(2) . 23 ?
C3 C3 C4 44.4(11) 23 23 ?
C4 C3 C4 88.5(10) 5_675 23 ?
C2 C4 O6 136(3) . . ?
C2 C4 C4 51.7(17) . 23 ?
O6 C4 C4 127(3) . 23 ?
C2 C4 C3 58.9(18) . . ?
O6 C4 C3 140(4) . . ?
C4 C4 C3 91.9(16) 23 . ?
C2 C4 C3 126.4(17) . 5_675 ?
O6 C4 C3 96(3) . 5_675 ?
C4 C4 C3 91.8(15) 23 5_675 ?
C3 C4 C3 90.3(18) . 5_675 ?
C2 C4 C3 35.0(11) . 23 ?
O6 C4 C3 169(3) . 23 ?
C4 C4 C3 44.4(11) 23 23 ?
C3 C4 C3 47.6(19) . 23 ?
C3 C4 C3 91.5(10) 5_675 23 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.060
