Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_net97

_database_code_CSD	181898


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Ciani, Gianfranco'
'Carlucci, Lucia'
'Cozzi, Nicola'
'Moret, Massimo'
'Proserpio, David M.'
'Rizzato, Silvia'


_publ_contact_author_name     	'Prof Gianfranco Ciani'  
_publ_contact_author_address 
;
DCSSI
Universita' di Milano
vian venezian 21
Milano
20133
ITALY
;

_publ_contact_author_email       'DAVIDE@CSMTBO.MI.CNR.IT'

_publ_section_title		
;
A three-dimensional nanoporous flexible network of 'square-planar'
copper(II) centres with an unusual topology
;

_diffrn_measurement_domega        0.30
_diffrn_measurement_rtime         43

_chemical_formula_sum
'C24 H22 Cl4 Cu F6 N4 O7 S2'
_chemical_formula_weight          861.92

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'
'F'  'F'   0.0171   0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S'  'S'   0.1246   0.1234
'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'
'Cl'  'Cl'   0.1484   0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Tetragonal
_symmetry_space_group_name_H-M    'I41/acd'
_symmetry_Int_Tables_number	   142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, x+1/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'y+5/4, x+3/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-y-3/4, -x-1/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-y-1/4, -x+1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'

_cell_length_a                    28.484(8)
_cell_length_b                    28.484(8)
_cell_length_c                    18.219(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      14782(8)
_cell_formula_units_Z             16
_cell_measurement_temperature     203(2)
_cell_measurement_reflns_used     1024
_cell_measurement_theta_min       2
_cell_measurement_theta_max       25

_exptl_crystal_description        colum
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.34
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_diffrn     1.549
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              6928
_exptl_absorpt_coefficient_mu     1.067
_exptl_absorpt_correction_type    sadabs
_exptl_absorpt_correction_T_min   0.70
_exptl_absorpt_correction_T_max   1.00

_diffrn_ambient_temperature       203(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        SMART
_diffrn_detector_type             CCD_plate
_diffrn_measurement_method        omega-scan
_diffrn_standards_decay_%         10
_diffrn_reflns_number             39938
_diffrn_reflns_av_R_equivalents   0.0775
_diffrn_reflns_av_sigmaI/netI     0.0345
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -33
_diffrn_reflns_limit_k_max        33
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.43
_diffrn_reflns_theta_max          25.07
_reflns_number_total              3281
_reflns_number_observed           2634
_reflns_observed_criterion        >2sigma(I)

_computing_structure_solution     SIR92
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     SCHAKAL

_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^)+(0.1168P)^2^+136.5155P] 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_number_reflns          3281
_refine_ls_number_parameters      280
_refine_ls_number_restraints      180
_refine_ls_R_factor_all           0.1029
_refine_ls_R_factor_obs           0.0826
_refine_ls_wR_factor_all          0.2550
_refine_ls_wR_factor_obs          0.2307
_refine_ls_goodness_of_fit_all    1.134
_refine_ls_restrained_S_all       1.184
_refine_ls_shift/su_max           0.554
_refine_ls_shift/su_mean          0.070

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
O1W O 0.4478(17) 0.2631(16) 0.094(2) 0.280(18) Uiso 0.50 1 d P . .
Cl1 Cl 0.8139(3) 0.4307(3) 0.0462(2) 0.229(3) Uani 1 1 d DU . .
C1W C 0.8430(4) 0.4070(4) 0.1250 0.150(8) Uani 1 2 d SDU . .
H1W1 H 0.8376 0.3734 0.1283 0.180 Uiso 0.50 1 calc PR . .
H1W2 H 0.8766 0.4124 0.1217 0.180 Uiso 0.50 1 calc PR . .
C2W C 0.2832(8) 0.9718(18) 0.1498(13) 0.27(3) Uani 0.50 1 d PDU . .
Cl2A Cl 0.3356(3) 0.9823(3) 0.0971(5) 0.149(3) Uani 0.50 1 d PD A 1
Cl2B Cl 0.3101(6) 1.0066(4) 0.1581(11) 0.268(9) Uani 0.50 1 d PD A 2
Cu Cu 0.49243(3) 0.0000 0.2500 0.0337(4) Uani 1 2 d S . .
O12 O 0.4901(3) -0.0537(3) 0.0063(3) 0.158(5) Uani 1 1 d DU . .
O11 O 0.49024(14) -0.05099(15) 0.1394(2) 0.0460(11) Uani 1 1 d DU . .
S1A S 0.50388(19) -0.07413(16) 0.0738(2) 0.0786(16) Uani 0.577(9) 1 d PDU B 1
O13A O 0.5532(3) -0.0847(4) 0.0738(5) 0.096(4) Uani 0.577(9) 1 d PDU B 1
C1A C 0.4754(6) -0.1313(6) 0.0770(6) 0.147(8) Uani 0.577(9) 1 d PDU B 1
F11A F 0.4887(9) -0.1480(10) 0.0111(11) 0.31(2) Uani 0.577(9) 1 d PDU B 1
F12A F 0.4957(10) -0.1531(10) 0.1343(12) 0.205(15) Uani 0.577(9) 1 d PDU B 1
F13A F 0.4287(5) -0.1257(8) 0.0840(13) 0.237(12) Uani 0.577(9) 1 d PDU B 1
S1B S 0.4727(2) -0.07061(18) 0.0728(2) 0.065(2) Uani 0.423(9) 1 d PDU B 2
O13B O 0.4219(3) -0.0706(5) 0.0728(6) 0.089(5) Uani 0.423(9) 1 d PDU B 2
C1B C 0.4884(5) -0.1328(6) 0.0775(7) 0.147(8) Uani 0.42 1 d PDU B 2
F11B F 0.4751(10) -0.1488(8) 0.1451(10) 0.152(13) Uani 0.423(9) 1 d PDU B 2
F12B F 0.4674(10) -0.1582(9) 0.0233(12) 0.190(14) Uani 0.423(9) 1 d PDU B 2
F13B F 0.5361(6) -0.1341(8) 0.0706(13) 0.167(10) Uani 0.423(9) 1 d PDU B 2
N12 N 0.44318(15) -0.04135(17) 0.2956(3) 0.0342(11) Uani 1 1 d . . .
N1 N 0.54248(15) 0.04136(16) 0.2051(3) 0.0340(12) Uani 1 1 d . . .
C2 C 0.5721(2) 0.0253(2) 0.1544(4) 0.0456(16) Uani 1 1 d . . .
H2 H 0.5702 -0.0060 0.1406 0.055 Uiso 1 1 calc R . .
C9 C 0.38137(19) -0.1054(2) 0.3584(3) 0.0367(13) Uani 1 1 d . B .
C4 C 0.60938(19) 0.0995(2) 0.1416(3) 0.0365(14) Uani 1 1 d . B .
C7 C 0.4450(2) -0.0516(2) 0.3678(4) 0.0425(15) Uani 1 1 d . . .
H7 H 0.4673 -0.0366 0.3968 0.051 Uiso 1 1 calc R . .
C6 C 0.5457(2) 0.0863(2) 0.2236(4) 0.0482(17) Uani 1 1 d . . .
H6 H 0.5249 0.0980 0.2585 0.058 Uiso 1 1 calc R . .
C11 C 0.4099(2) -0.0619(2) 0.2556(4) 0.0439(16) Uani 1 1 d . . .
H11 H 0.4077 -0.0542 0.2061 0.053 Uiso 1 1 calc R . .
C5 C 0.5782(2) 0.1161(2) 0.1938(4) 0.0495(17) Uani 1 1 d . . .
H5 H 0.5793 0.1474 0.2084 0.059 Uiso 1 1 calc R B .
C8 C 0.4156(2) -0.0833(2) 0.4001(4) 0.0431(15) Uani 1 1 d . . .
H8 H 0.4184 -0.0899 0.4499 0.052 Uiso 1 1 calc R B .
C10 C 0.3786(2) -0.0941(2) 0.2843(4) 0.0459(16) Uani 1 1 d . . .
H10 H 0.3561 -0.1080 0.2545 0.055 Uiso 1 1 calc R B .
C3 C 0.6053(2) 0.0531(2) 0.1216(4) 0.0494(17) Uani 1 1 d . . .
H3 H 0.6250 0.0406 0.0859 0.059 Uiso 1 1 calc R B .

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
Cl1 0.304(8) 0.257(7) 0.126(4) -0.026(4) -0.002(4) 0.118(6)
C1W 0.144(12) 0.144(12) 0.16(2) -0.014(11) -0.014(11) -0.008(15)
C2W 0.32(7) 0.21(6) 0.27(8) -0.01(5) -0.09(6) 0.05(4)
Cl2A 0.187(9) 0.123(6) 0.136(7) -0.019(5) -0.031(6) -0.042(6)
Cl2B 0.203(14) 0.173(13) 0.43(3) -0.002(15) -0.037(16) -0.058(11)
Cu 0.0157(5) 0.0337(6) 0.0516(7) 0.0274(4) 0.000 0.000
O12 0.208(11) 0.211(12) 0.056(5) 0.021(6) 0.023(6) 0.064(9)
O11 0.046(3) 0.044(2) 0.048(3) 0.007(2) 0.000(2) -0.0015(19)
S1A 0.066(3) 0.100(3) 0.070(3) -0.023(2) -0.006(2) 0.013(2)
O13A 0.066(7) 0.134(12) 0.089(9) -0.037(8) 0.009(6) 0.020(7)
C1A 0.16(2) 0.098(11) 0.185(19) -0.042(12) -0.064(16) 0.022(13)
F11A 0.28(3) 0.32(4) 0.32(3) -0.26(3) 0.01(2) -0.12(3)
F12A 0.26(3) 0.116(16) 0.23(3) -0.020(16) -0.08(2) 0.059(18)
F13A 0.136(15) 0.24(3) 0.34(3) -0.05(2) -0.063(18) -0.087(16)
S1B 0.073(5) 0.066(3) 0.057(3) -0.007(2) -0.001(3) 0.003(3)
O13B 0.060(9) 0.118(14) 0.090(11) -0.010(9) -0.030(8) -0.019(9)
C1B 0.16(2) 0.098(11) 0.185(19) -0.042(12) -0.064(16) 0.022(13)
F11B 0.19(3) 0.053(12) 0.21(3) 0.040(14) -0.01(2) -0.047(15)
F12B 0.22(3) 0.103(15) 0.25(3) -0.105(18) -0.03(2) -0.051(18)
F13B 0.132(17) 0.137(18) 0.23(3) 0.010(18) 0.060(17) 0.060(15)
N12 0.021(2) 0.040(3) 0.042(3) 0.025(2) -0.0028(19) -0.0045(19)
N1 0.017(2) 0.033(2) 0.052(3) 0.021(2) 0.003(2) -0.0032(18)
C2 0.039(3) 0.029(3) 0.069(4) 0.006(3) 0.015(3) -0.005(3)
C9 0.025(3) 0.037(3) 0.048(4) 0.016(3) 0.006(2) -0.005(2)
C4 0.030(3) 0.032(3) 0.047(4) 0.010(3) 0.010(2) -0.005(2)
C7 0.032(3) 0.046(4) 0.049(4) 0.016(3) -0.002(3) -0.013(3)
C6 0.043(4) 0.036(3) 0.066(4) 0.010(3) 0.024(3) -0.002(3)
C11 0.027(3) 0.055(4) 0.049(4) 0.029(3) -0.004(3) -0.010(3)
C5 0.049(4) 0.029(3) 0.070(5) 0.006(3) 0.028(3) -0.005(3)
C8 0.038(3) 0.050(4) 0.042(3) 0.017(3) 0.004(3) -0.014(3)
C10 0.032(3) 0.057(4) 0.049(4) 0.018(3) -0.004(3) -0.015(3)
C3 0.047(4) 0.035(3) 0.067(4) -0.002(3) 0.028(3) -0.007(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
Cl1 C1W 1.790(9) . ?
C1W Cl1 1.790(9) 5_665 ?
C2W Cl2B 1.795(11) 5_665 ?
C2W Cl2A 1.69(5) 5_665 ?
C2W Cl2A 1.799(11) . ?
Cl2A C2W 1.69(5) 5_665 ?
Cl2B C2W 1.795(11) 5_665 ?
Cu N12 2.012(4) . ?
Cu N12 2.012(4) 3 ?
Cu N1 2.022(4) 3 ?
Cu N1 2.022(4) . ?
Cu O11 2.485(4) . ?
Cu O11 2.485(4) 3 ?
O12 S1B 1.395(6) . ?
O12 S1A 1.416(6) . ?
O11 S1A 1.418(5) . ?
O11 S1B 1.426(6) . ?
S1A O13A 1.436(7) . ?
S1A C1A 1.821(19) . ?
C1A F13A 1.343(12) . ?
C1A F11A 1.346(12) . ?
C1A F12A 1.344(12) . ?
S1B O13B 1.446(7) . ?
S1B C1B 1.83(2) . ?
C1B F11B 1.367(12) . ?
C1B F13B 1.363(12) . ?
C1B F12B 1.364(12) . ?
N12 C11 1.330(8) . ?
N12 C7 1.349(8) . ?
N1 C6 1.326(8) . ?
N1 C2 1.333(8) . ?
C2 C3 1.368(8) . ?
C9 C8 1.387(9) . ?
C9 C10 1.392(9) . ?
C9 C4 1.482(7) 29_545 ?
C4 C5 1.384(9) . ?
C4 C3 1.377(9) . ?
C4 C9 1.482(7) 21_655 ?
C7 C8 1.365(8) . ?
C6 C5 1.370(8) . ?
C11 C10 1.382(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
Cl1 C1W Cl1 107.0(8) 5_665 . ?
C2W C2W Cl2B 109(4) 5_665 . ?
Cl2B C2W Cl2B 148(3) 5_665 . ?
Cl2A C2W Cl2B 156(4) 5_665 . ?
Cl2B C2W Cl2A 107.1(8) 5_665 . ?
Cl2A C2W Cl2A 113(2) 5_665 . ?
N12 Cu N12 91.6(2) . 3 ?
N12 Cu N1 89.05(17) . 3 ?
N12 Cu N1 179.31(19) 3 3 ?
N12 Cu N1 179.31(19) . . ?
N12 Cu N1 89.05(17) 3 . ?
N1 Cu N1 90.3(2) 3 . ?
N12 Cu O11 88.59(18) . . ?
N12 Cu O11 89.40(19) 3 . ?
N1 Cu O11 90.30(18) 3 . ?
N1 Cu O11 91.73(18) . . ?
N12 Cu O11 89.40(19) . 3 ?
N12 Cu O11 88.59(18) 3 3 ?
N1 Cu O11 91.73(18) 3 3 ?
N1 Cu O11 90.30(18) . 3 ?
O11 Cu O11 177.13(19) . 3 ?
S1A O11 Cu 161.4(3) . . ?
S1B O11 Cu 158.1(3) . . ?
O12 S1A O11 117.7(5) . . ?
O12 S1A O13A 110.9(5) . . ?
O11 S1A O13A 111.4(4) . . ?
O12 S1A C1A 105.7(5) . . ?
O11 S1A C1A 105.4(4) . . ?
O13A S1A C1A 104.4(5) . . ?
F13A C1A F11A 113.9(10) . . ?
F13A C1A F12A 114.2(11) . . ?
F11A C1A F12A 114.1(10) . . ?
F13A C1A S1A 109.7(13) . . ?
F11A C1A S1A 99.2(15) . . ?
F12A C1A S1A 104.1(17) . . ?
O12 S1B O11 118.6(5) . . ?
O12 S1B O13B 110.8(5) . . ?
O11 S1B O13B 110.5(5) . . ?
O12 S1B C1B 106.7(5) . . ?
O11 S1B C1B 104.7(5) . . ?
O13B S1B C1B 104.2(5) . . ?
F11B C1B F13B 110.5(11) . . ?
F11B C1B F12B 110.7(10) . . ?
F13B C1B F12B 110.8(10) . . ?
F11B C1B S1B 107.3(13) . . ?
F13B C1B S1B 105.5(13) . . ?
F12B C1B S1B 111.9(15) . . ?
C11 N12 C7 117.9(5) . . ?
C11 N12 Cu 121.8(4) . . ?
C7 N12 Cu 120.2(4) . . ?
C6 N1 C2 117.6(5) . . ?
C6 N1 Cu 120.5(4) . . ?
C2 N1 Cu 121.9(4) . . ?
N1 C2 C3 122.8(6) . . ?
N1 C2 Cu 35.6(3) . . ?
C3 C2 Cu 158.4(5) . . ?
C8 C9 C10 117.7(5) . . ?
C8 C9 C4 121.0(5) . 29_545 ?
C10 C9 C4 121.3(6) . 29_545 ?
C5 C4 C3 117.1(5) . . ?
C5 C4 C9 120.4(5) . 21_655 ?
C3 C4 C9 122.5(5) . 21_655 ?
N12 C7 C8 122.7(6) . . ?
N12 C7 Cu 36.4(3) . . ?
C8 C7 Cu 158.5(5) . . ?
N1 C6 C5 123.0(6) . . ?
N1 C6 Cu 36.5(3) . . ?
C5 C6 Cu 159.5(5) . . ?
N12 C11 C10 122.9(6) . . ?
N12 C11 Cu 35.6(3) . . ?
C10 C11 Cu 158.0(5) . . ?
C6 C5 C4 119.6(6) . . ?
C7 C8 C9 119.7(6) . . ?
C11 C10 C9 119.1(6) . . ?
C2 C3 C4 119.9(6) . . ?

_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.07
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.038
_refine_diff_density_min   -0.838
_refine_diff_density_rms    0.124

# END