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Interwoven Metal-Organic Framework on a Periodic Minimal Surface with Extra Large Pores
B. Chen, M. Eddaoudi, S.T. Hyde, M. O'keeffe, O.M. Yaghi
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Supplementary Material
Experimental details
As-synthesized MOF-14 [Cu3(BTB)2(H2O)3•(DMF)9(H2O)2]: Elemental microanalysis, Calc: C, 53.72; H, 5.69; N, 6.96%. Found: C, 54.02; H, 5.58; N, 6.91%. (b) At -116° ± 2°C MOF-14 is cubic, space group Im-3, a = 26.946(2) Å, V = 19556(2) Å3, Z = 8. R = 0.0472, goodness of fit indicator = 0.980, and max./min. peak in the final difference map = 0.413/-0.333 e-/Å3. Evacuated MOF-14 [Cu3(BTB)2(H2O)3•H2O]: Elemental microanalysis, Calc: C, 57.21; H, 3.38; N, 0.00%. Found: C, 57.13; H, 3.60; N, 0.23%. At -116° ± 2°C evacuated MOF-14 is cubic, space group Im-3, a = 26.919(1) Å, V = 19507(1) Å3, Z = 12. R = 0.0601, goodness of fit indicator = 0.985, and max./min. peak in the final difference map = 0.306/-0.379 e-/Å3 (see below for details). Solvent exchanged MOF-14: Calculated and found elemental microanalysis for the family Cu3(BTB)2(H2O)3•(solvent)n(H2O)2 where (solvent)n = (tetrahydrofuran)7: Calc, C, 59.46; H, 5.80; N, 0.00%. Found: C, 59.44; H, 5.91; N, 0.20%, (ethanol)8: Calc, C, 55.26; H, 6.84; N, 0.00%. Found: C, 55.00; H, 6.52; N, 0.12%, (chloroform)4: Calc, C, 42.76; H, 2.7; N, 0.00%. Found: C, 42.52; H, 2.71; N, 0.20%, and (benzene)6: Calc, C, 66.71; H, 4.69; N, 0.00%. Found: C, 67.03; H, 4.65; N, 0.44%.
Crystallographic data for as-synthesized MOF-14 (in CIF format)
data_cuttb
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C84 H84 Cu3 N6 O24'
_chemical_formula_weight 1752.19
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'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu' 'Cu' 0.3201 1.2651
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting cubic
_symmetry_space_group_name_H-M Im-3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
_cell_length_a 26.9464(15)
_cell_length_b 26.9464(15)
_cell_length_c 26.9464(15)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 19566.0(19)
_cell_formula_units_Z 8
_cell_measurement_temperature 179(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.190
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 7272
_exptl_absorpt_coefficient_mu 0.714
_exptl_absorpt_correction_type 'empirical (SADABS)'
_exptl_absorpt_correction_T_min 0.86
_exptl_absorpt_correction_T_max 0.93
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 179(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 ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14620
_diffrn_reflns_av_R_equivalents 0.0840
_diffrn_reflns_av_sigmaI/netI 0.0710
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 1.85
_diffrn_reflns_theta_max 20.78
_reflns_number_total 1849
_reflns_number_gt 1348
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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_extinction_coef ?
_refine_ls_number_reflns 1849
_refine_ls_number_parameters 171
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0741
_refine_ls_R_factor_gt 0.0472
_refine_ls_wR_factor_ref 0.1210
_refine_ls_wR_factor_gt 0.1105
_refine_ls_goodness_of_fit_ref 0.980
_refine_ls_restrained_S_all 0.980
_refine_ls_shift/su_max 0.018
_refine_ls_shift/su_mean 0.002
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 0.14219(6) 0.5000 0.0000 0.0317(5) Uani 1 4 d S . .
Cu2 Cu 0.24015(6) 0.5000 0.0000 0.0358(5) Uani 1 4 d S . .
O1 O 0.0637(4) 0.5000 0.0112(7) 0.034(6) Uani 0.50 2 d SP . .
O2 O 0.3201(4) 0.5000 0.0000 0.077(4) Uani 1 4 d S . .
O3 O 0.15001(19) 0.44765(17) 0.05083(17) 0.0418(13) Uani 1 1 d . . .
O4 O 0.23263(19) 0.44878(18) 0.0501(2) 0.0530(14) Uani 1 1 d . . .
C1 C 0.1924(3) 0.4306(3) 0.0625(3) 0.0380(18) Uani 1 1 d . . .
C2 C 0.1931(3) 0.3841(3) 0.0925(2) 0.040(2) Uani 1 1 d . . .
C3 C 0.1499(3) 0.3602(3) 0.1080(3) 0.051(2) Uani 1 1 d . . .
H3A H 0.1184 0.3740 0.1002 0.061 Uiso 1 1 calc R . .
C4 C 0.1527(3) 0.3170(3) 0.1342(3) 0.049(2) Uani 1 1 d . . .
H4A H 0.1232 0.3011 0.1451 0.059 Uiso 1 1 calc R . .
C5 C 0.1998(3) 0.2956(3) 0.1453(3) 0.050(2) Uani 1 1 d . . .
C6 C 0.2408(3) 0.3199(3) 0.1307(3) 0.050(2) Uani 1 1 d . . .
H6A H 0.2724 0.3064 0.1390 0.061 Uiso 1 1 calc R . .
C7 C 0.2388(3) 0.3636(3) 0.1042(3) 0.051(2) Uani 1 1 d . . .
H7A H 0.2686 0.3796 0.0940 0.061 Uiso 1 1 calc R . .
C8 C 0.2033(3) 0.2495(3) 0.1777(3) 0.050(3) Uani 1 1 d . . .
C9 C 0.1707(3) 0.2415(3) 0.2168(3) 0.055(2) Uani 1 1 d . . .
H9A H 0.1451 0.2655 0.2230 0.066 Uiso 1 1 d R . .
O5 O 0.311(2) 0.251(4) 0.0000 0.52(3) Uiso 1 2 d S . .
O6 O 0.3420(9) 0.3963(12) 0.0212(10) 0.264(14) Uiso 0.50 1 d P . .
O7 O 0.2769(17) 0.0000 0.103(2) 0.46(2) Uiso 1 2 d S . .
O8 O 0.331(3) 0.191(3) 0.0000 0.52(3) Uiso 1 2 d S . .
O9 O 0.3205(17) 0.316(2) 0.0000 0.398(12) Uiso 0.82(5) 2 d SP . .
O10 O 0.344(3) 0.0000 0.084(6) 0.398(12) Uiso 0.50(13) 2 d SP . .
O11 O 0.3510(14) 0.4551(17) 0.0000 0.398(12) Uiso 0.83(4) 2 d SP . .
O12 O 0.230(3) 0.0000 0.177(2) 0.398(12) Uiso 0.68(6) 2 d SP . .
O13 O 0.4165(13) 0.0273(11) 0.0000 0.398(12) Uiso 0.83(3) 2 d SP . .
O14 O 0.264(5) 0.157(6) 0.0000 0.398(12) Uiso 0.26(3) 2 d SP . .
O15 O 0.351(2) 0.0000 0.048(4) 0.398(12) Uiso 0.73(14) 2 d SP . .
O16 O 0.287(3) 0.092(3) 0.0000 0.398(12) Uiso 0.52(4) 2 d SP . .
O17 O 0.1279(10) 0.1279(10) 0.1279(10) 0.398(12) Uiso 0.78(4) 3 d SP . .
O18 O 0.432(3) 0.124(2) 0.0000 0.398(12) Uiso 0.52(4) 2 d SP . .
O19 O 0.279(2) 0.0000 0.162(2) 0.398(12) Uiso 0.86(6) 2 d SP . .
O20 O 0.266(4) 0.0000 0.238(5) 0.398(12) Uiso 0.32(3) 2 d SP . .
O21 O 0.372(3) 0.140(3) 0.0000 0.398(12) Uiso 0.58(5) 2 d SP . .
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 0.0367(11) 0.0289(12) 0.0296(12) 0.000 0.000 0.000
Cu2 0.0370(11) 0.0354(13) 0.0350(13) 0.000 0.000 0.000
O1 0.042(7) 0.044(7) 0.02(2) 0.000 0.007(6) 0.000
O2 0.050(7) 0.091(10) 0.090(10) 0.000 0.000 0.000
O3 0.049(3) 0.041(3) 0.036(3) 0.008(2) 0.006(3) 0.005(3)
O4 0.040(4) 0.053(4) 0.066(4) 0.021(3) 0.000(3) 0.003(3)
C1 0.043(5) 0.047(5) 0.023(4) -0.001(3) 0.000(4) 0.014(5)
C2 0.041(5) 0.037(5) 0.041(5) 0.016(4) 0.004(4) 0.018(5)
C3 0.048(6) 0.055(6) 0.049(5) 0.012(5) 0.008(4) 0.013(4)
C4 0.051(6) 0.044(5) 0.053(5) 0.019(4) 0.012(4) 0.006(4)
C5 0.057(6) 0.054(6) 0.040(5) 0.014(4) 0.017(4) 0.021(5)
C6 0.028(5) 0.061(7) 0.062(6) 0.016(5) 0.018(4) 0.018(5)
C7 0.054(6) 0.041(5) 0.057(6) 0.017(5) 0.017(4) -0.001(5)
C8 0.056(6) 0.052(6) 0.044(5) 0.014(4) 0.013(5) 0.030(5)
C9 0.052(6) 0.053(6) 0.060(6) 0.014(5) 0.029(5) 0.022(4)
_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 O3 1.978(4) . ?
Cu1 O3 1.978(4) 27_565 ?
Cu1 O3 1.978(4) 26 ?
Cu1 O3 1.978(4) 4_565 ?
Cu1 O1 2.135(11) . ?
Cu1 O1 2.135(11) 26 ?
Cu1 Cu2 2.640(2) . ?
Cu2 O4 1.942(5) 26 ?
Cu2 O4 1.942(5) 27_565 ?
Cu2 O4 1.942(5) 4_565 ?
Cu2 O4 1.942(5) . ?
Cu2 O2 2.154(11) . ?
O1 O1 0.61(4) 26 ?
O2 O11 1.47(4) . ?
O2 O11 1.47(4) 27_565 ?
O3 C1 1.270(8) . ?
O4 C1 1.235(8) . ?
C1 C2 1.493(9) . ?
C2 C7 1.387(9) . ?
C2 C3 1.393(9) . ?
C3 C4 1.364(9) . ?
C4 C5 1.425(10) . ?
C5 C6 1.343(10) . ?
C5 C8 1.521(10) . ?
C6 C7 1.380(10) . ?
C8 C9 1.367(9) 9 ?
C8 C9 1.390(9) . ?
C9 C8 1.367(9) 5 ?
O5 O8 1.70(6) . ?
O5 O9 1.75(7) . ?
O6 O6 1.14(6) 26 ?
O6 O11 1.70(4) . ?
O7 O19 1.61(5) . ?
O8 O21 1.76(7) . ?
O10 O15 0.98(11) . ?
O11 O6 1.70(4) 26 ?
O12 O19 1.38(6) . ?
O13 O13 1.47(6) 27 ?
O18 O21 1.68(8) . ?
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
O3 Cu1 O3 91.0(3) . 27_565 ?
O3 Cu1 O3 87.7(3) . 26 ?
O3 Cu1 O3 167.8(3) 27_565 26 ?
O3 Cu1 O3 167.8(3) . 4_565 ?
O3 Cu1 O3 87.7(3) 27_565 4_565 ?
O3 Cu1 O3 91.0(3) 26 4_565 ?
O3 Cu1 O1 90.4(4) . . ?
O3 Cu1 O1 90.4(4) 27_565 . ?
O3 Cu1 O1 101.8(4) 26 . ?
O3 Cu1 O1 101.8(4) 4_565 . ?
O3 Cu1 O1 101.8(4) . 26 ?
O3 Cu1 O1 101.8(4) 27_565 26 ?
O3 Cu1 O1 90.4(4) 26 26 ?
O3 Cu1 O1 90.4(4) 4_565 26 ?
O1 Cu1 O1 16.3(10) . 26 ?
O3 Cu1 Cu2 83.88(15) . . ?
O3 Cu1 Cu2 83.88(15) 27_565 . ?
O3 Cu1 Cu2 83.88(15) 26 . ?
O3 Cu1 Cu2 83.88(15) 4_565 . ?
O1 Cu1 Cu2 171.8(5) . . ?
O1 Cu1 Cu2 171.8(5) 26 . ?
O4 Cu2 O4 168.0(3) 26 27_565 ?
O4 Cu2 O4 90.6(3) 26 4_565 ?
O4 Cu2 O4 88.2(3) 27_565 4_565 ?
O4 Cu2 O4 88.2(3) 26 . ?
O4 Cu2 O4 90.6(3) 27_565 . ?
O4 Cu2 O4 168.0(3) 4_565 . ?
O4 Cu2 O2 95.99(16) 26 . ?
O4 Cu2 O2 95.99(16) 27_565 . ?
O4 Cu2 O2 95.99(16) 4_565 . ?
O4 Cu2 O2 96.00(16) . . ?
O4 Cu2 Cu1 84.01(16) 26 . ?
O4 Cu2 Cu1 84.01(16) 27_565 . ?
O4 Cu2 Cu1 84.01(16) 4_565 . ?
O4 Cu2 Cu1 84.00(16) . . ?
O2 Cu2 Cu1 180.0 . . ?
O1 O1 Cu1 81.8(5) 26 . ?
O11 O2 O11 111(4) . 27_565 ?
O11 O2 Cu2 124.5(18) . . ?
O11 O2 Cu2 124.5(18) 27_565 . ?
C1 O3 Cu1 121.6(4) . . ?
C1 O4 Cu2 124.1(4) . . ?
O4 C1 O3 125.4(6) . . ?
O4 C1 C2 117.9(7) . . ?
O3 C1 C2 116.6(7) . . ?
C7 C2 C3 119.4(6) . . ?
C7 C2 C1 117.9(7) . . ?
C3 C2 C1 122.7(7) . . ?
C4 C3 C2 120.2(7) . . ?
C3 C4 C5 120.2(7) . . ?
C6 C5 C4 118.4(7) . . ?
C6 C5 C8 120.9(7) . . ?
C4 C5 C8 120.4(7) . . ?
C5 C6 C7 122.3(7) . . ?
C6 C7 C2 119.5(7) . . ?
C9 C8 C9 118.7(8) 9 . ?
C9 C8 C5 119.6(7) 9 . ?
C9 C8 C5 121.5(7) . . ?
C8 C9 C8 121.3(8) 5 . ?
O8 O5 O9 153(6) . . ?
O6 O6 O11 70.4(11) 26 . ?
O5 O8 O21 161(7) . . ?
O2 O11 O6 133(3) . 26 ?
O2 O11 O6 133(3) . . ?
O6 O11 O6 39(2) 26 . ?
O12 O19 O7 104(5) . . ?
O18 O21 O8 143(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Cu1 Cu2 O4 88.5(2) . . . 26 ?
O3 Cu1 Cu2 O4 -179.8(2) 27_565 . . 26 ?
O3 Cu1 Cu2 O4 0.2(2) 26 . . 26 ?
O3 Cu1 Cu2 O4 -91.5(2) 4_565 . . 26 ?
O1 Cu1 Cu2 O4 134.39(17) . . . 26 ?
O1 Cu1 Cu2 O4 -45.61(17) 26 . . 26 ?
O3 Cu1 Cu2 O4 -91.5(2) . . . 27_565 ?
O3 Cu1 Cu2 O4 0.2(2) 27_565 . . 27_565 ?
O3 Cu1 Cu2 O4 -179.8(2) 26 . . 27_565 ?
O3 Cu1 Cu2 O4 88.5(2) 4_565 . . 27_565 ?
O1 Cu1 Cu2 O4 -45.61(17) . . . 27_565 ?
O1 Cu1 Cu2 O4 134.39(17) 26 . . 27_565 ?
O3 Cu1 Cu2 O4 179.8(2) . . . 4_565 ?
O3 Cu1 Cu2 O4 -88.5(2) 27_565 . . 4_565 ?
O3 Cu1 Cu2 O4 91.5(2) 26 . . 4_565 ?
O3 Cu1 Cu2 O4 -0.2(2) 4_565 . . 4_565 ?
O1 Cu1 Cu2 O4 -134.39(17) . . . 4_565 ?
O1 Cu1 Cu2 O4 45.61(17) 26 . . 4_565 ?
O3 Cu1 Cu2 O4 -0.2(2) . . . . ?
O3 Cu1 Cu2 O4 91.5(2) 27_565 . . . ?
O3 Cu1 Cu2 O4 -88.5(2) 26 . . . ?
O3 Cu1 Cu2 O4 179.8(2) 4_565 . . . ?
O1 Cu1 Cu2 O4 45.61(17) . . . . ?
O1 Cu1 Cu2 O4 -134.39(17) 26 . . . ?
O3 Cu1 Cu2 O2 0.0 . . . . ?
O3 Cu1 Cu2 O2 0.0 27_565 . . . ?
O3 Cu1 Cu2 O2 0.0 26 . . . ?
O3 Cu1 Cu2 O2 0.0 4_565 . . . ?
O1 Cu1 Cu2 O2 0.0 . . . . ?
O1 Cu1 Cu2 O2 0.0 26 . . . ?
O3 Cu1 O1 O1 -134.49(14) . . . 26 ?
O3 Cu1 O1 O1 134.48(14) 27_565 . . 26 ?
O3 Cu1 O1 O1 -46.78(17) 26 . . 26 ?
O3 Cu1 O1 O1 46.78(17) 4_565 . . 26 ?
Cu2 Cu1 O1 O1 180.0 . . . 26 ?
O4 Cu2 O2 O11 -44.39(17) 26 . . . ?
O4 Cu2 O2 O11 135.61(17) 27_565 . . . ?
O4 Cu2 O2 O11 -135.61(17) 4_565 . . . ?
O4 Cu2 O2 O11 44.39(17) . . . . ?
Cu1 Cu2 O2 O11 0.0 . . . . ?
O4 Cu2 O2 O11 135.61(17) 26 . . 27_565 ?
O4 Cu2 O2 O11 -44.39(17) 27_565 . . 27_565 ?
O4 Cu2 O2 O11 44.39(17) 4_565 . . 27_565 ?
O4 Cu2 O2 O11 -135.61(17) . . . 27_565 ?
Cu1 Cu2 O2 O11 0.0 . . . 27_565 ?
O3 Cu1 O3 C1 -88.7(6) 27_565 . . . ?
O3 Cu1 O3 C1 79.1(6) 26 . . . ?
O3 Cu1 O3 C1 -5.0(5) 4_565 . . . ?
O1 Cu1 O3 C1 -179.2(6) . . . . ?
O1 Cu1 O3 C1 169.0(6) 26 . . . ?
Cu2 Cu1 O3 C1 -5.0(5) . . . . ?
O4 Cu2 O4 C1 -78.3(7) 26 . . . ?
O4 Cu2 O4 C1 89.8(6) 27_565 . . . ?
O4 Cu2 O4 C1 5.9(6) 4_565 . . . ?
O2 Cu2 O4 C1 -174.1(6) . . . . ?
Cu1 Cu2 O4 C1 5.9(6) . . . . ?
Cu2 O4 C1 O3 -12.2(11) . . . . ?
Cu2 O4 C1 C2 166.2(5) . . . . ?
Cu1 O3 C1 O4 11.5(11) . . . . ?
Cu1 O3 C1 C2 -166.9(4) . . . . ?
O4 C1 C2 C7 -1.0(10) . . . . ?
O3 C1 C2 C7 177.6(7) . . . . ?
O4 C1 C2 C3 -179.2(7) . . . . ?
O3 C1 C2 C3 -0.7(11) . . . . ?
C7 C2 C3 C4 -0.1(11) . . . . ?
C1 C2 C3 C4 178.1(7) . . . . ?
C2 C3 C4 C5 -1.0(11) . . . . ?
C3 C4 C5 C6 2.0(11) . . . . ?
C3 C4 C5 C8 175.6(7) . . . . ?
C4 C5 C6 C7 -2.0(12) . . . . ?
C8 C5 C6 C7 -175.5(7) . . . . ?
C5 C6 C7 C2 1.0(12) . . . . ?
C3 C2 C7 C6 0.2(11) . . . . ?
C1 C2 C7 C6 -178.2(7) . . . . ?
C6 C5 C8 C9 -36.3(12) . . . 9 ?
C4 C5 C8 C9 150.3(8) . . . 9 ?
C6 C5 C8 C9 138.7(9) . . . . ?
C4 C5 C8 C9 -34.7(12) . . . . ?
C9 C8 C9 C8 3.2(18) 9 . . 5 ?
C5 C8 C9 C8 -171.9(6) . . . 5 ?
O9 O5 O8 O21 0.0 . . . . ?
O11 O2 O11 O6 -152(2) 27_565 . . 26 ?
Cu2 O2 O11 O6 28(2) . . . 26 ?
O11 O2 O11 O6 152(2) 27_565 . . . ?
Cu2 O2 O11 O6 -28(2) . . . . ?
O6 O6 O11 O2 110(2) 26 . . . ?
O5 O8 O21 O18 0.0 . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 20.78
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.413
_refine_diff_density_min -0.333
_refine_diff_density_rms 0.062
Crystallographic data for evacuated MOF-14 (in CIF format)
data_im3
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C46 H26.67 Cu2 O10'
_chemical_formula_weight 866.42
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 Cubic
_symmetry_space_group_name_H-M Im-3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
_cell_length_a 26.9193(10)
_cell_length_b 26.9193(10)
_cell_length_c 26.9193(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 19507.0(13)
_cell_formula_units_Z 12
_cell_measurement_temperature 179(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 0.885
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5288
_exptl_absorpt_coefficient_mu 0.691
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min 0.8629
_exptl_absorpt_correction_T_max 0.8975
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 179(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 40010
_diffrn_reflns_av_R_equivalents 0.1825
_diffrn_reflns_av_sigmaI/netI 0.1081
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.39
_diffrn_reflns_theta_max 23.28
_reflns_number_total 2512
_reflns_number_gt 1384
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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_extinction_coef ?
_refine_ls_number_reflns 2512
_refine_ls_number_parameters 111
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1236
_refine_ls_R_factor_gt 0.0601
_refine_ls_wR_factor_ref 0.1475
_refine_ls_wR_factor_gt 0.1315
_refine_ls_goodness_of_fit_ref 0.985
_refine_ls_restrained_S_all 0.985
_refine_ls_shift/su_max 0.010
_refine_ls_shift/su_mean 0.001
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 0.0000 0.14174(6) 0.5000 0.0445(5) Uani 1 4 d S . .
Cu2 Cu 0.0000 0.23920(6) 0.5000 0.0480(5) Uani 1 4 d S . .
O1 O 0.0000 0.0631(4) 0.5000 0.150(6) Uani 1 4 d S . .
O2 O 0.0000 0.3219(4) 0.5000 0.136(5) Uani 1 4 d S . .
O3 O 0.05045(17) 0.14949(17) 0.44786(16) 0.0547(13) Uani 1 1 d . . .
O4 O 0.05007(19) 0.23223(17) 0.44842(18) 0.0659(14) Uani 1 1 d . . .
C1 C 0.0624(3) 0.1917(3) 0.4311(3) 0.0551(19) Uiso 1 1 d . . .
C2 C 0.0929(2) 0.1932(3) 0.3838(2) 0.055(2) Uiso 1 1 d . . .
C3 C 0.1074(2) 0.1487(3) 0.3602(3) 0.061(2) Uiso 1 1 d . . .
C4 C 0.1338(3) 0.1515(3) 0.3160(3) 0.068(2) Uiso 1 1 d . . .
C5 C 0.1451(2) 0.1978(3) 0.2946(3) 0.0569(19) Uiso 1 1 d . . .
C6 C 0.1300(3) 0.2413(3) 0.3187(3) 0.067(2) Uiso 1 1 d . . .
C7 C 0.1043(3) 0.2397(3) 0.3644(3) 0.060(2) Uiso 1 1 d . . .
C8 C 0.1770(3) 0.2025(3) 0.2491(3) 0.062(2) Uiso 1 1 d . . .
C9 C 0.2166(3) 0.1695(3) 0.2422(3) 0.066(2) Uiso 1 1 d . . .
C10 C 0.0197(10) 0.3530(11) 0.5448(12) 0.075(10) Uiso 0.25 1 d P . .
C201 C 0.0000 0.3481(14) 0.5885(18) 0.167(14) Uiso 0.50 2 d SP . .
C202 C 0.0000 0.3156(12) 0.697(2) 0.150 Uiso 0.63(4) 2 d SP . .
C203 C 0.0000 0.177(3) 0.735(3) 0.150 Uiso 0.24(3) 2 d SP . .
C204 C 0.0000 0.0000 0.420(4) 0.150 Uiso 0.23(3) 4 d SP . .
C205 C 0.0000 0.3084(13) 0.737(2) 0.150 Uiso 0.61(4) 2 d SP . .
C206 C 0.0000 0.237(3) 0.735(3) 0.150 Uiso 0.32(3) 2 d SP . .
C207 C 0.0000 0.251(4) 0.782(4) 0.150 Uiso 0.20(3) 2 d SP . .
C208 C 0.0000 0.3227(15) 0.781(2) 0.150 Uiso 0.54(3) 2 d SP . .
C209 C 0.0000 0.295(5) 0.825(4) 0.150 Uiso 0.18(3) 2 d SP . .
C210 C 0.0000 0.334(2) 0.645(3) 0.150 Uiso 0.34(3) 2 d SP . .
C211 C 0.0604(13) 0.3995(13) 0.5000 0.150 Uiso 0.46(3) 2 d SP . .
C212 C 0.0000 0.351(2) 0.825(2) 0.150 Uiso 0.37(3) 2 d SP . .
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 0.0458(12) 0.0441(11) 0.0436(12) 0.000 0.000 0.000
Cu2 0.0523(13) 0.0439(11) 0.0479(12) 0.000 0.000 0.000
O1 0.167(14) 0.058(8) 0.223(18) 0.000 0.000 0.000
O2 0.229(18) 0.059(8) 0.118(12) 0.000 0.000 0.000
O3 0.055(3) 0.061(3) 0.048(3) 0.002(3) 0.008(2) 0.002(3)
O4 0.074(4) 0.059(3) 0.065(4) 0.004(3) 0.020(3) -0.003(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
Cu1 O3 1.964(4) 28 ?
Cu1 O3 1.964(4) 26_556 ?
Cu1 O3 1.964(4) 3_556 ?
Cu1 O3 1.964(4) . ?
Cu1 O1 2.116(11) . ?
Cu1 Cu2 2.624(2) . ?
Cu2 O4 1.944(4) 28 ?
Cu2 O4 1.944(4) 26_556 ?
Cu2 O4 1.944(4) 3_556 ?
Cu2 O4 1.944(4) . ?
Cu2 O2 2.225(11) . ?
O2 C10 1.56(3) . ?
O2 C10 1.56(3) 3_556 ?
O2 C10 1.56(3) 26_556 ?
O2 C10 1.56(3) 28 ?
O3 C1 1.263(8) . ?
O4 C1 1.232(8) . ?
C1 C2 1.518(9) . ?
C2 C7 1.391(8) . ?
C2 C3 1.410(9) . ?
C3 C4 1.387(9) . ?
C4 C5 1.408(9) . ?
C5 C6 1.400(9) . ?
C5 C8 1.500(10) . ?
C6 C7 1.413(9) . ?
C8 C9 1.395(9) 9 ?
C8 C9 1.400(8) . ?
C9 C8 1.395(9) 5 ?
C10 C10 1.06(6) 28 ?
C10 C201 1.30(4) . ?
C201 C10 1.30(4) 28 ?
C201 C210 1.58(6) . ?
C202 C205 1.09(4) . ?
C202 C210 1.47(6) . ?
C203 C206 1.64(9) . ?
C205 C208 1.26(5) . ?
C205 C206 1.91(7) . ?
C205 C207 1.97(11) . ?
C206 C207 1.32(10) . ?
C207 C209 1.66(14) . ?
C207 C208 1.93(10) . ?
C208 C209 1.38(11) . ?
C208 C212 1.41(6) . ?
C209 C212 1.51(11) . ?
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
O3 Cu1 O3 167.8(3) 28 26_556 ?
O3 Cu1 O3 91.2(3) 28 3_556 ?
O3 Cu1 O3 87.5(3) 26_556 3_556 ?
O3 Cu1 O3 87.5(3) 28 . ?
O3 Cu1 O3 91.2(3) 26_556 . ?
O3 Cu1 O3 167.8(3) 3_556 . ?
O3 Cu1 O1 96.10(14) 28 . ?
O3 Cu1 O1 96.10(14) 26_556 . ?
O3 Cu1 O1 96.10(14) 3_556 . ?
O3 Cu1 O1 96.10(14) . . ?
O3 Cu1 Cu2 83.90(14) 28 . ?
O3 Cu1 Cu2 83.90(14) 26_556 . ?
O3 Cu1 Cu2 83.90(14) 3_556 . ?
O3 Cu1 Cu2 83.90(14) . . ?
O1 Cu1 Cu2 180.000(1) . . ?
O4 Cu2 O4 168.9(3) 28 26_556 ?
O4 Cu2 O4 91.2(3) 28 3_556 ?
O4 Cu2 O4 87.8(3) 26_556 3_556 ?
O4 Cu2 O4 87.8(3) 28 . ?
O4 Cu2 O4 91.2(3) 26_556 . ?
O4 Cu2 O4 168.9(3) 3_556 . ?
O4 Cu2 O2 95.54(14) 28 . ?
O4 Cu2 O2 95.54(14) 26_556 . ?
O4 Cu2 O2 95.54(14) 3_556 . ?
O4 Cu2 O2 95.54(14) . . ?
O4 Cu2 Cu1 84.46(14) 28 . ?
O4 Cu2 Cu1 84.46(14) 26_556 . ?
O4 Cu2 Cu1 84.46(14) 3_556 . ?
O4 Cu2 Cu1 84.46(14) . . ?
O2 Cu2 Cu1 180.000(1) . . ?
C10 O2 C10 115(2) . 3_556 ?
C10 O2 C10 101(2) . 26_556 ?
C10 O2 C10 40(2) 3_556 26_556 ?
C10 O2 C10 40(2) . 28 ?
C10 O2 C10 101(2) 3_556 28 ?
C10 O2 C10 115(2) 26_556 28 ?
C10 O2 Cu2 122.5(11) . . ?
C10 O2 Cu2 122.5(11) 3_556 . ?
C10 O2 Cu2 122.5(11) 26_556 . ?
C10 O2 Cu2 122.5(11) 28 . ?
C1 O3 Cu1 121.7(4) . . ?
C1 O4 Cu2 122.8(4) . . ?
O4 C1 O3 126.4(6) . . ?
O4 C1 C2 116.0(7) . . ?
O3 C1 C2 117.5(7) . . ?
C7 C2 C3 122.3(6) . . ?
C7 C2 C1 117.3(7) . . ?
C3 C2 C1 120.4(7) . . ?
C4 C3 C2 118.9(7) . . ?
C3 C4 C5 120.6(7) . . ?
C6 C5 C4 119.3(7) . . ?
C6 C5 C8 118.4(6) . . ?
C4 C5 C8 122.1(7) . . ?
C5 C6 C7 121.4(7) . . ?
C2 C7 C6 117.6(7) . . ?
C9 C8 C9 120.7(8) 9 . ?
C9 C8 C5 119.6(7) 9 . ?
C9 C8 C5 119.4(7) . . ?
C8 C9 C8 119.3(8) 5 . ?
C10 C10 C201 65.8(15) 28 . ?
C10 C10 O2 70.1(10) 28 . ?
C201 C10 O2 120(3) . . ?
C10 C201 C10 48(3) 28 . ?
C10 C201 C210 154.8(19) 28 . ?
C10 C201 C210 154.8(19) . . ?
C205 C202 C210 170(5) . . ?
C202 C205 C208 152(5) . . ?
C202 C205 C206 99(5) . . ?
C208 C205 C206 109(4) . . ?
C202 C205 C207 139(5) . . ?
C208 C205 C207 69(5) . . ?
C206 C205 C207 40(3) . . ?
C207 C206 C203 106(8) . . ?
C207 C206 C205 72(6) . . ?
C203 C206 C205 179(6) . . ?
C206 C207 C209 150(9) . . ?
C206 C207 C208 106(7) . . ?
C209 C207 C208 45(5) . . ?
C206 C207 C205 68(6) . . ?
C209 C207 C205 82(6) . . ?
C208 C207 C205 38(2) . . ?
C205 C208 C209 130(7) . . ?
C205 C208 C212 165(5) . . ?
C209 C208 C212 65(5) . . ?
C205 C208 C207 73(5) . . ?
C209 C208 C207 57(5) . . ?
C212 C208 C207 123(5) . . ?
C208 C209 C212 58(5) . . ?
C208 C209 C207 78(7) . . ?
C212 C209 C207 136(9) . . ?
C202 C210 C201 174(5) . . ?
C208 C212 C209 57(5) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Cu1 Cu2 O4 0.1(2) 28 . . 28 ?
O3 Cu1 Cu2 O4 -179.9(2) 26_556 . . 28 ?
O3 Cu1 Cu2 O4 -91.8(2) 3_556 . . 28 ?
O3 Cu1 Cu2 O4 88.2(2) . . . 28 ?
O1 Cu1 Cu2 O4 0(33) . . . 28 ?
O3 Cu1 Cu2 O4 -179.9(2) 28 . . 26_556 ?
O3 Cu1 Cu2 O4 0.1(2) 26_556 . . 26_556 ?
O3 Cu1 Cu2 O4 88.2(2) 3_556 . . 26_556 ?
O3 Cu1 Cu2 O4 -91.8(2) . . . 26_556 ?
O1 Cu1 Cu2 O4 0(33) . . . 26_556 ?
O3 Cu1 Cu2 O4 91.8(2) 28 . . 3_556 ?
O3 Cu1 Cu2 O4 -88.2(2) 26_556 . . 3_556 ?
O3 Cu1 Cu2 O4 -0.1(2) 3_556 . . 3_556 ?
O3 Cu1 Cu2 O4 179.9(2) . . . 3_556 ?
O1 Cu1 Cu2 O4 0(33) . . . 3_556 ?
O3 Cu1 Cu2 O4 -88.2(2) 28 . . . ?
O3 Cu1 Cu2 O4 91.8(2) 26_556 . . . ?
O3 Cu1 Cu2 O4 179.9(2) 3_556 . . . ?
O3 Cu1 Cu2 O4 -0.1(2) . . . . ?
O1 Cu1 Cu2 O4 0(33) . . . . ?
O3 Cu1 Cu2 O2 0(100) 28 . . . ?
O3 Cu1 Cu2 O2 0(85) 26_556 . . . ?
O3 Cu1 Cu2 O2 0(100) 3_556 . . . ?
O3 Cu1 Cu2 O2 0(85) . . . . ?
O1 Cu1 Cu2 O2 0(43) . . . . ?
O4 Cu2 O2 C10 159.6(13) 28 . . . ?
O4 Cu2 O2 C10 -20.4(13) 26_556 . . . ?
O4 Cu2 O2 C10 67.9(13) 3_556 . . . ?
O4 Cu2 O2 C10 -112.1(13) . . . . ?
Cu1 Cu2 O2 C10 0(100) . . . . ?
O4 Cu2 O2 C10 -20.4(13) 28 . . 3_556 ?
O4 Cu2 O2 C10 159.6(13) 26_556 . . 3_556 ?
O4 Cu2 O2 C10 -112.1(13) 3_556 . . 3_556 ?
O4 Cu2 O2 C10 67.9(13) . . . 3_556 ?
Cu1 Cu2 O2 C10 0(100) . . . 3_556 ?
O4 Cu2 O2 C10 -67.9(13) 28 . . 26_556 ?
O4 Cu2 O2 C10 112.1(13) 26_556 . . 26_556 ?
O4 Cu2 O2 C10 -159.6(13) 3_556 . . 26_556 ?
O4 Cu2 O2 C10 20.4(13) . . . 26_556 ?
Cu1 Cu2 O2 C10 0(100) . . . 26_556 ?
O4 Cu2 O2 C10 112.1(13) 28 . . 28 ?
O4 Cu2 O2 C10 -67.9(13) 26_556 . . 28 ?
O4 Cu2 O2 C10 20.4(13) 3_556 . . 28 ?
O4 Cu2 O2 C10 -159.6(13) . . . 28 ?
Cu1 Cu2 O2 C10 0(100) . . . 28 ?
O3 Cu1 O3 C1 79.7(6) 28 . . . ?
O3 Cu1 O3 C1 -88.2(6) 26_556 . . . ?
O3 Cu1 O3 C1 -4.4(5) 3_556 . . . ?
O1 Cu1 O3 C1 175.6(5) . . . . ?
Cu2 Cu1 O3 C1 -4.4(5) . . . . ?
O4 Cu2 O4 C1 -79.8(6) 28 . . . ?
O4 Cu2 O4 C1 89.1(6) 26_556 . . . ?
O4 Cu2 O4 C1 4.8(6) 3_556 . . . ?
O2 Cu2 O4 C1 -175.2(6) . . . . ?
Cu1 Cu2 O4 C1 4.8(6) . . . . ?
Cu2 O4 C1 O3 -10.4(12) . . . . ?
Cu2 O4 C1 C2 166.8(5) . . . . ?
Cu1 O3 C1 O4 10.1(11) . . . . ?
Cu1 O3 C1 C2 -167.0(4) . . . . ?
O4 C1 C2 C7 0.1(10) . . . . ?
O3 C1 C2 C7 177.5(6) . . . . ?
O4 C1 C2 C3 -177.9(7) . . . . ?
O3 C1 C2 C3 -0.5(11) . . . . ?
C7 C2 C3 C4 -0.2(11) . . . . ?
C1 C2 C3 C4 177.7(6) . . . . ?
C2 C3 C4 C5 -1.1(11) . . . . ?
C3 C4 C5 C6 0.8(11) . . . . ?
C3 C4 C5 C8 175.1(7) . . . . ?
C4 C5 C6 C7 1.0(11) . . . . ?
C8 C5 C6 C7 -173.5(7) . . . . ?
C3 C2 C7 C6 1.9(11) . . . . ?
C1 C2 C7 C6 -176.0(7) . . . . ?
C5 C6 C7 C2 -2.3(11) . . . . ?
C6 C5 C8 C9 -35.1(10) . . . 9 ?
C4 C5 C8 C9 150.6(8) . . . 9 ?
C6 C5 C8 C9 139.3(7) . . . . ?
C4 C5 C8 C9 -35.1(11) . . . . ?
C9 C8 C9 C8 0.6(16) 9 . . 5 ?
C5 C8 C9 C8 -173.6(5) . . . 5 ?
C10 O2 C10 C10 76.7(9) 3_556 . . 28 ?
C10 O2 C10 C10 116.1(14) 26_556 . . 28 ?
Cu2 O2 C10 C10 -103.3(9) . . . 28 ?
C10 O2 C10 C201 121(3) 3_556 . . . ?
C10 O2 C10 C201 160.3(19) 26_556 . . . ?
C10 O2 C10 C201 44(3) 28 . . . ?
Cu2 O2 C10 C201 -59(3) . . . . ?
O2 C10 C201 C10 -46(3) . . . 28 ?
C10 C10 C201 C210 162(10) 28 . . . ?
O2 C10 C201 C210 116(9) . . . . ?
C210 C202 C205 C208 0.00(13) . . . . ?
C210 C202 C205 C206 180.00(10) . . . . ?
C210 C202 C205 C207 180.00(10) . . . . ?
C202 C205 C206 C207 180.00(3) . . . . ?
C208 C205 C206 C207 0.00(3) . . . . ?
C202 C205 C206 C203 180.0(11) . . . . ?
C208 C205 C206 C203 0.0(11) . . . . ?
C207 C205 C206 C203 0.0(10) . . . . ?
C203 C206 C207 C209 180.00(5) . . . . ?
C205 C206 C207 C209 0.00(6) . . . . ?
C203 C206 C207 C208 180.000(12) . . . . ?
C205 C206 C207 C208 0.000(13) . . . . ?
C203 C206 C207 C205 180.000(18) . . . . ?
C202 C205 C207 C206 0.00(2) . . . . ?
C208 C205 C207 C206 180.000(19) . . . . ?
C202 C205 C207 C209 180.00(4) . . . . ?
C208 C205 C207 C209 0.00(3) . . . . ?
C206 C205 C207 C209 180.00(3) . . . . ?
C202 C205 C207 C208 180.00(5) . . . . ?
C206 C205 C207 C208 180.000(12) . . . . ?
C202 C205 C208 C209 180.00(4) . . . . ?
C206 C205 C208 C209 0.00(4) . . . . ?
C207 C205 C208 C209 0.00(3) . . . . ?
C202 C205 C208 C212 0.00(8) . . . . ?
C206 C205 C208 C212 180.00(5) . . . . ?
C207 C205 C208 C212 180.00(6) . . . . ?
C202 C205 C208 C207 180.00(4) . . . . ?
C206 C205 C208 C207 0.000(19) . . . . ?
C206 C207 C208 C205 0.00(3) . . . . ?
C209 C207 C208 C205 180.00(3) . . . . ?
C206 C207 C208 C209 180.00(3) . . . . ?
C205 C207 C208 C209 180.00(3) . . . . ?
C206 C207 C208 C212 180.00(3) . . . . ?
C209 C207 C208 C212 0.00(4) . . . . ?
C205 C207 C208 C212 180.00(3) . . . . ?
C205 C208 C209 C212 180.00(5) . . . . ?
C207 C208 C209 C212 180.000(13) . . . . ?
C205 C208 C209 C207 0.00(3) . . . . ?
C212 C208 C209 C207 180.00(2) . . . . ?
C206 C207 C209 C208 0.00(5) . . . . ?
C205 C207 C209 C208 0.00(2) . . . . ?
C206 C207 C209 C212 0.00(7) . . . . ?
C208 C207 C209 C212 0.00(3) . . . . ?
C205 C207 C209 C212 0.00(3) . . . . ?
C205 C202 C210 C201 180.00(10) . . . . ?
C10 C201 C210 C202 74(9) 28 . . . ?
C10 C201 C210 C202 -74(9) . . . . ?
C205 C208 C212 C209 180.00(7) . . . . ?
C207 C208 C212 C209 0.00(3) . . . . ?
C207 C209 C212 C208 0.00(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 23.28
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.306
_refine_diff_density_min -0.379
_refine_diff_density_rms 0.076
