# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_tet_mof
_database_code_depnum_ccdc_archive 'CCDC 1420151'
_audit_update_record             
;
2015-08-21 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 C9 H5 Cu2 O7 2(H2 O)
;
_chemical_formula_sum            
;
 C9 H9 Cu2 O9 
;
_chemical_formula_weight         388.24

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'
H H 0.0000 0.0000 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4/nmm

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

_cell_length_a                   19.2100(5)
_cell_length_b                   19.210
_cell_length_c                   6.9158(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2552.10(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_exptl_absorpt_coefficient_mu    3.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and ψ scans'
_diffrn_reflns_number            27000
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         27.59
_reflns_number_total             1626
_reflns_number_gt                1475
_reflns_threshold_expression     >2sigma(I)

_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. 
 O5 and O6 are part of water molecules residing in pores; H-atoms of these 
 could not be located and were therefore not included in refinement. 
;

_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)+(0.0500P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1626
_refine_ls_number_parameters     107
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.031
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.67264(2) 0.17264(2) -0.5000 0.01689(18) Uani 1 2 d S . .
Cu2 Cu 0.53003(2) 0.53003(2) 0.35189(8) 0.00882(17) Uani 1 2 d S . .
O1 O 0.63198(16) 0.19197(13) -0.2665(4) 0.0232(6) Uani 1 1 d . . .
O2 O 0.53227(18) 0.43386(14) 0.2615(4) 0.0301(7) Uani 1 1 d . . .
O3 O 0.4841(2) 0.38177(15) 0.5124(4) 0.0407(10) Uani 1 1 d . . .
C1 C 0.6153(3) 0.2500 -0.1982(7) 0.0135(9) Uani 1 2 d S . .
C2 C 0.5742(3) 0.2500 -0.0145(7) 0.0134(9) Uani 1 2 d S . .
C3 C 0.55650(18) 0.31241(17) 0.0724(5) 0.0131(6) Uani 1 1 d . . .
H3 H 0.5659 0.3551 0.0083 0.016 Uiso 1 1 calc R . .
C4 C 0.52472(17) 0.31270(18) 0.2546(5) 0.0119(6) Uani 1 1 d . . .
C5 C 0.5092(3) 0.2500 0.3468(7) 0.0130(9) Uani 1 2 d S . .
H5 H 0.4884 0.2500 0.4714 0.016 Uiso 1 2 calc SR . .
C6 C 0.51203(17) 0.38111(17) 0.3508(5) 0.0112(6) Uani 1 1 d . . .
O4 O 0.57098(13) 0.57098(13) 0.0860(5) 0.0174(7) Uani 1 2 d SD . .
H4A H 0.6025(9) 0.6025(9) 0.055(9) 0.049(17) Uiso 1 2 d SD . .
H4B H 0.559(2) 0.559(2) -0.030(5) 0.049(17) Uiso 1 2 d SD . .
O5 O 0.6771(4) 0.6771(4) 0.056(3) 0.195(8) Uani 1 2 d S . .
O6 O 0.6767(4) 0.6767(4) 0.546(3) 0.208(8) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0189(2) 0.0189(2) 0.0129(3) -0.00577(17) 0.00577(17) -0.0007(2)
Cu2 0.0094(2) 0.0094(2) 0.0076(3) 0.00000(14) 0.00000(14) -0.0002(2)
O1 0.0369(17) 0.0123(13) 0.0203(13) -0.0033(10) 0.0168(12) -0.0019(11)
O2 0.058(2) 0.0097(12) 0.0230(14) -0.0001(10) 0.0252(14) 0.0017(12)
O3 0.083(3) 0.0141(13) 0.0254(15) -0.0082(12) 0.0334(17) -0.0153(15)
C1 0.014(2) 0.015(2) 0.011(2) 0.000 -0.0006(18) 0.000
C2 0.015(2) 0.015(2) 0.011(2) 0.000 0.0001(18) 0.000
C3 0.0153(16) 0.0107(15) 0.0133(15) 0.0005(12) 0.0008(13) -0.0004(13)
C4 0.0111(15) 0.0148(16) 0.0100(14) -0.0015(12) -0.0012(12) 0.0004(13)
C5 0.014(2) 0.014(2) 0.011(2) 0.000 0.0013(17) 0.000
C6 0.0107(14) 0.0115(14) 0.0116(14) -0.0015(12) -0.0009(11) -0.0004(12)
O4 0.0200(11) 0.0200(11) 0.0122(16) 0.0020(10) 0.0020(10) -0.0031(15)
O5 0.091(5) 0.091(5) 0.40(2) 0.038(8) 0.038(8) -0.009(6)
O6 0.153(9) 0.153(9) 0.32(2) -0.006(8) -0.006(8) -0.075(10)

_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
Cu1 O1 1.832(3) . ?
Cu1 O1 1.832(3) 7_544 ?
Cu1 Cu1 2.9723(9) 11_664 ?
Cu1 Cu1 2.9723(9) 12_654 ?
Cu2 O2 1.951(3) . ?
Cu2 O2 1.951(3) 16 ?
Cu2 O3 1.956(3) 8_666 ?
Cu2 O3 1.956(3) 9_666 ?
Cu2 O4 2.150(3) . ?
Cu2 Cu2 2.6189(11) 9_666 ?
O1 C1 1.252(3) . ?
O2 C6 1.249(4) . ?
O3 C6 1.240(4) . ?
O3 Cu2 1.956(3) 9_666 ?
C1 O1 1.252(3) 13_565 ?
C1 C2 1.496(6) . ?
C2 C3 1.383(4) 13_565 ?
C2 C3 1.383(4) . ?
C3 C4 1.401(5) . ?
C4 C5 1.395(4) . ?
C4 C6 1.493(5) . ?
C5 C4 1.395(4) 13_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
O1 Cu1 O1 161.80(18) . 7_544 ?
O1 Cu1 Cu1 78.30(8) . 11_664 ?
O1 Cu1 Cu1 115.23(10) 7_544 11_664 ?
O1 Cu1 Cu1 115.23(10) . 12_654 ?
O1 Cu1 Cu1 78.30(8) 7_544 12_654 ?
Cu1 Cu1 Cu1 90.0 11_664 12_654 ?
O2 Cu2 O2 86.5(2) . 16 ?
O2 Cu2 O3 90.20(16) . 8_666 ?
O2 Cu2 O3 167.77(11) 16 8_666 ?
O2 Cu2 O3 167.77(11) . 9_666 ?
O2 Cu2 O3 90.20(16) 16 9_666 ?
O3 Cu2 O3 90.5(3) 8_666 9_666 ?
O2 Cu2 O4 93.69(11) . . ?
O2 Cu2 O4 93.69(11) 16 . ?
O3 Cu2 O4 98.29(11) 8_666 . ?
O3 Cu2 O4 98.29(11) 9_666 . ?
O2 Cu2 Cu2 80.98(8) . 9_666 ?
O2 Cu2 Cu2 80.98(8) 16 9_666 ?
O3 Cu2 Cu2 86.87(8) 8_666 9_666 ?
O3 Cu2 Cu2 86.87(8) 9_666 9_666 ?
O4 Cu2 Cu2 172.64(11) . 9_666 ?
C1 O1 Cu1 128.5(3) . . ?
C6 O2 Cu2 127.1(2) . . ?
C6 O3 Cu2 120.1(2) . 9_666 ?
O1 C1 O1 125.8(5) 13_565 . ?
O1 C1 C2 117.1(2) 13_565 . ?
O1 C1 C2 117.1(2) . . ?
C3 C2 C3 120.2(4) 13_565 . ?
C3 C2 C1 119.9(2) 13_565 . ?
C3 C2 C1 119.9(2) . . ?
C2 C3 C4 120.1(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 C6 121.4(3) . . ?
C3 C4 C6 118.4(3) . . ?
C4 C5 C4 119.4(4) 13_565 . ?
O3 C6 O2 124.9(3) . . ?
O3 C6 C4 118.8(3) . . ?
O2 C6 C4 116.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.120
