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

data_ibrm2
_database_code_CSD                  181653

_audit_creation_date            2002-02-09T14:30:35-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FM

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Wright, P.'
'Bull, Ivor' 
'Lightfoot, Philip'
'Morris, Russell E.'
'Sastre, E.'
'Wheatley, Paul S.'

_publ_contact_author_name     	'Dr P Wright'  
_publ_contact_author_address 
;
School of Chemistry
St Andrews University
The Purdie Building
St Andrews
Fife
KY16 9ST
U.K.
;

_publ_contact_author_email       'PAW2@ST-ANDREWS.AC.UK'

_publ_section_title		
;
Synthesis and structure of the first scandium-containing open
framework solid
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic
;
?
;
_chemical_formula_moiety                'C8 N4 O4 P1 Sc1'
_chemical_formula_structural            'SC1 P1 O4 C8 N4'
_chemical_formula_sum                   'C1.60 H4 N0.80 O8.30 S2.20 Sc0.93'
_chemical_formula_weight                279.75
_chemical_compound_source               'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting                  cubic
_symmetry_space_group_name_H-M          'P n -3 n'
_symmetry_space_group_name_Hall         '-P 4a 2bc 3'
_symmetry_Int_Tables_number             222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'-y+1/2, x, z'
'y, x, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, -x+1/2, -z+1/2'
'y, z, x'
'-y+1/2, -z+1/2, x'
'y, -z+1/2, -x+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, y, x'
'-z+1/2, -y+1/2, -x+1/2'
'z, -y+1/2, x'
'z, y, -x+1/2'
'z, x, y'
'-z+1/2, x, -y+1/2'
'-z+1/2, -x+1/2, y'
'z, -x+1/2, -y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-x+1/2, z, y'
'x, -z+1/2, y'
'x, z, -y+1/2'
'-x, -y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'y-1/2, -x, -z'
'-y, -x, z-1/2'
'-y, x-1/2, -z'
'y-1/2, x-1/2, z-1/2'
'-y, -z, -x'
'y-1/2, z-1/2, -x'
'-y, z-1/2, x-1/2'
'y-1/2, -z, x-1/2'
'z-1/2, -y, -x'
'z-1/2, y-1/2, x-1/2'
'-z, y-1/2, -x'
'-z, -y, x-1/2'
'-z, -x, -y'
'z-1/2, -x, y-1/2'
'z-1/2, x-1/2, -y'
'-z, x-1/2, y-1/2'
'x-1/2, z-1/2, y-1/2'
'x-1/2, -z, -y'
'-x, z-1/2, -y'
'-x, -z, y-1/2'

_cell_length_a                          25.2469(3)
_cell_length_b                          25.2469(3)
_cell_length_c                          25.2469(3)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            16092.5(3)
_cell_formula_units_Z                   60
_cell_measurement_temperature           293(2)
_cell_measurement_reflns_used           0
_cell_measurement_theta_min             0
_cell_measurement_theta_max             0
_cell_measurement_wavelength            0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.05
_exptl_crystal_size_mid                 0.05
_exptl_crystal_size_min                 0.05
_exptl_crystal_density_diffrn           1.732
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    8424
_exptl_special_details
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu           1.093
_exptl_absorpt_correction_type          none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_reflns_av_unetI/netI            0.0761
_diffrn_reflns_number                   74745
_diffrn_reflns_limit_h_min              -28
_diffrn_reflns_limit_h_max              27
_diffrn_reflns_limit_k_min              -26
_diffrn_reflns_limit_k_max              28
_diffrn_reflns_limit_l_min              -28
_diffrn_reflns_limit_l_max              26
_diffrn_reflns_theta_min                1.61
_diffrn_reflns_theta_max                23.26
_diffrn_reflns_theta_full               23.26
_diffrn_measured_fraction_theta_full	0.999
_diffrn_measured_fraction_theta_max	0.999
_reflns_number_total                    1945
_reflns_number_gt                       1222
_reflns_threshold_expression            >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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^)+(0.1922P)^2^+175.6767P] 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                1945
_refine_ls_number_parameters            155
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.1816
_refine_ls_R_factor_gt                  0.1225
_refine_ls_wR_factor_ref                0.3897
_refine_ls_wR_factor_gt                 0.3397
_refine_ls_goodness_of_fit_ref          1.364
_refine_ls_restrained_S_all             1.364
_refine_ls_shift/su_max                 0.103
_refine_ls_shift/su_mean                0.015
_refine_diff_density_max                7.498
_refine_diff_density_min                -0.887
_refine_diff_density_rms                0.356

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Sc1 Sc 0 0.5 0 0.0129(16) Uani 1 6 d S . .
Sc2 Sc 0.10248(11) 0.66834(11) 0.04225(12) 0.0153(10) Uani 1 1 d . . .
S1 S 0.06848(16) 0.55307(15) 0.10239(16) 0.0167(11) Uani 1 1 d . . .
S2 S 0.09555(16) 0.78838(15) -0.01626(16) 0.0173(11) Uani 1 1 d . . .
S3 S 0.1425(2) 0.75 0.1425(2) 0.065(3) Uani 1 2 d S . .
O1 O 0.0974(5) 0.6031(4) 0.0913(5) 0.025(3) Uani 1 1 d . . .
O2 O 0.0585(4) 0.5254(4) 0.0528(5) 0.025(3) Uani 1 1 d . . .
O3 O 0.1152(5) 0.7338(4) -0.0053(5) 0.032(3) Uani 1 1 d . . .
O4 O 0.1776(5) 0.6423(5) 0.0208(6) 0.038(3) Uani 1 1 d . . .
O5 O 0.0654(6) 0.7897(5) -0.0655(5) 0.042(4) Uani 1 1 d . . .
H5 H 0.0392 0.7706 -0.0626 0.064 Uiso 1 1 calc R . .
O6 O 0.0283(4) 0.6940(5) 0.0629(5) 0.030(3) Uani 1 1 d . . .
O7 O 0.1010(5) 0.5205(5) 0.1362(5) 0.042(4) Uani 1 1 d . . .
H7 H 0.1293 0.5144 0.1215 0.062 Uiso 1 1 calc R . .
O8 O 0.0185(5) 0.5659(5) 0.1283(5) 0.034(3) Uani 1 1 d . . .
O9 O 0.141(2) 0.1957(11) 0.7681(9) 0.36(4) Uani 1 1 d . . .
O10 O 0.1363(5) 0.7061(5) 0.1059(5) 0.042(4) Uani 1 1 d . . .
C1 C 0.1291(8) 0.7649(6) 0.8361(7) 0.028(4) Uani 1 1 d . . .
H1A H 0.1489 0.7781 0.8663 0.034 Uiso 1 1 calc R . .
H1B H 0.1535 0.7617 0.8066 0.034 Uiso 1 1 calc R . .
C2 C 0.1074(8) 0.7094(6) 0.8497(7) 0.029(5) Uani 1 1 d . . .
H2A H 0.0785 0.7135 0.8747 0.035 Uiso 1 1 calc R . .
H2B H 0.1352 0.6895 0.8673 0.035 Uiso 1 1 calc R . .
N1 N 0.0880(6) 0.8037(5) 0.8224(5) 0.024(3) Uani 1 1 d . . .
H3 H 0.0554 0.8003 0.8318 0.14(15) Uiso 1 1 calc R . .
O14 O 0.25 0.75 0.25 0.080(17) Uani 1 8 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
Sc1 0.0129(16) 0.0129(16) 0.0129(16) -0.0017(17) 0.0017(17) -0.0017(17)
Sc2 0.0142(18) 0.0100(17) 0.0218(19) -0.0038(13) 0.0056(13) -0.0010(12)
S1 0.018(2) 0.015(2) 0.017(2) -0.0010(17) -0.0021(17) -0.0027(17)
S2 0.022(2) 0.013(2) 0.017(2) -0.0006(17) 0.0063(17) -0.0023(17)
S3 0.079(5) 0.035(4) 0.079(5) -0.036(4) -0.060(5) 0.036(4)
O1 0.029(7) 0.017(6) 0.028(7) 0.006(5) -0.004(5) -0.008(5)
O2 0.023(7) 0.020(6) 0.031(7) -0.005(5) -0.001(5) -0.007(5)
O3 0.028(7) 0.012(6) 0.057(9) 0.004(6) 0.017(6) 0.002(5)
O4 0.026(7) 0.021(7) 0.066(10) -0.004(6) 0.022(7) 0.011(5)
O5 0.056(9) 0.046(9) 0.025(7) -0.001(6) -0.003(6) -0.021(7)
O6 0.019(7) 0.024(7) 0.045(8) -0.003(6) 0.010(6) 0.009(5)
O7 0.054(9) 0.024(7) 0.047(9) 0.001(6) -0.020(7) 0.005(6)
O8 0.030(7) 0.041(8) 0.031(7) -0.006(6) 0.011(6) -0.005(6)
O9 0.84(11) 0.15(3) 0.08(2) 0.074(19) -0.20(4) -0.33(5)
O10 0.056(9) 0.032(8) 0.039(8) -0.025(6) -0.007(7) -0.003(7)
C1 0.047(12) 0.017(10) 0.021(10) 0.000(7) 0.008(8) -0.007(8)
C2 0.052(13) 0.015(9) 0.020(10) -0.001(7) 0.002(8) -0.011(8)
N1 0.031(9) 0.023(8) 0.020(8) 0.005(6) 0.016(7) 0.005(6)
O14 0.029(15) 0.18(6) 0.029(15) 0 0 0


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Sc1 O2 2.089(11) 25_565 ?
Sc1 O2 2.089(11) . ?
Sc1 O2 2.089(11) 34_565 ?
Sc1 O2 2.089(11) 44_565 ?
Sc1 O2 2.089(11) 20 ?
Sc1 O2 2.089(11) 10 ?
Sc2 O8 2.055(12) 34_565 ?
Sc2 O1 2.064(11) . ?
Sc2 O10 2.054(12) . ?
Sc2 O6 2.049(11) . ?
Sc2 O3 2.067(12) . ?
Sc2 O4 2.078(11) . ?
S1 O7 1.442(13) . ?
S1 O2 1.456(12) . ?
S1 O8 1.458(12) . ?
S1 O1 1.487(11) . ?
S2 O5 1.458(13) . ?
S2 O6 1.464(12) 15_565 ?
S2 O4 1.466(12) 29_565 ?
S2 O3 1.492(12) . ?
S3 O9 1.42(3) 9 ?
S3 O9 1.42(3) 23_565 ?
S3 O10 1.452(12) . ?
S3 O10 1.452(12) 15_565 ?
O4 S2 1.466(12) 31_665 ?
O6 S2 1.464(12) 15_565 ?
O8 Sc2 2.055(12) 44_565 ?
O9 S3 1.42(3) 17 ?
C1 N1 1.47(2) . ?
C1 C2 1.54(2) . ?
C2 N1 1.49(2) 23_565 ?
N1 C2 1.49(2) 24_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
O2 Sc1 O2 180.0(7) 25_565 . ?
O2 Sc1 O2 87.8(4) 25_565 34_565 ?
O2 Sc1 O2 92.2(4) . 34_565 ?
O2 Sc1 O2 87.8(4) 25_565 44_565 ?
O2 Sc1 O2 92.2(4) . 44_565 ?
O2 Sc1 O2 87.8(4) 34_565 44_565 ?
O2 Sc1 O2 92.2(4) 25_565 20 ?
O2 Sc1 O2 87.8(4) . 20 ?
O2 Sc1 O2 92.2(4) 34_565 20 ?
O2 Sc1 O2 180.0000 44_565 20 ?
O2 Sc1 O2 92.2(4) 25_565 10 ?
O2 Sc1 O2 87.8(4) . 10 ?
O2 Sc1 O2 180.0(6) 34_565 10 ?
O2 Sc1 O2 92.2(4) 44_565 10 ?
O2 Sc1 O2 87.8(4) 20 10 ?
O8 Sc2 O1 91.6(5) 34_565 . ?
O8 Sc2 O10 176.7(5) 34_565 . ?
O1 Sc2 O10 85.7(5) . . ?
O8 Sc2 O6 86.3(5) 34_565 . ?
O1 Sc2 O6 92.4(5) . . ?
O10 Sc2 O6 91.9(5) . . ?
O8 Sc2 O3 91.7(5) 34_565 . ?
O1 Sc2 O3 174.5(5) . . ?
O10 Sc2 O3 91.1(5) . . ?
O6 Sc2 O3 92.1(5) . . ?
O8 Sc2 O4 93.4(5) 34_565 . ?
O1 Sc2 O4 87.8(5) . . ?
O10 Sc2 O4 88.4(5) . . ?
O6 Sc2 O4 179.6(6) . . ?
O3 Sc2 O4 87.7(5) . . ?
O7 S1 O2 109.6(7) . . ?
O7 S1 O8 110.7(8) . . ?
O2 S1 O8 110.1(7) . . ?
O7 S1 O1 108.5(7) . . ?
O2 S1 O1 109.4(7) . . ?
O8 S1 O1 108.7(7) . . ?
O5 S2 O6 110.7(8) . 15_565 ?
O5 S2 O4 110.0(8) . 29_565 ?
O6 S2 O4 109.6(8) 15_565 29_565 ?
O5 S2 O3 110.6(8) . . ?
O6 S2 O3 109.0(7) 15_565 . ?
O4 S2 O3 106.8(7) 29_565 . ?
O9 S3 O9 99(4) 9 23_565 ?
O9 S3 O10 109.2(17) 9 . ?
O9 S3 O10 110.6(11) 23_565 . ?
O9 S3 O10 110.6(11) 9 15_565 ?
O9 S3 O10 109.2(17) 23_565 15_565 ?
O10 S3 O10 116.5(12) . 15_565 ?
S1 O1 Sc2 145.2(7) . . ?
S1 O2 Sc1 144.9(8) . . ?
S2 O3 Sc2 142.6(7) . . ?
S2 O4 Sc2 144.1(8) 31_665 . ?
S2 O6 Sc2 160.3(9) 15_565 . ?
S1 O8 Sc2 165.1(8) . 44_565 ?
S3 O10 Sc2 153.8(9) . . ?
N1 C1 C2 114.1(15) . . ?
C1 C2 N1 115.6(14) . 23_565 ?
C1 N1 C2 114.4(14) . 24_556 ?

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
O7 S1 O1 Sc2 162.2(13) . . . . ?
O2 S1 O1 Sc2 42.8(15) . . . . ?
O8 S1 O1 Sc2 -77.4(15) . . . . ?
O8 Sc2 O1 S1 -23.9(14) 34_565 . . . ?
O10 Sc2 O1 S1 154.2(14) . . . . ?
O6 Sc2 O1 S1 62.5(14) . . . . ?
O3 Sc2 O1 S1 -151(5) . . . . ?
O4 Sc2 O1 S1 -117.2(14) . . . . ?
O7 S1 O2 Sc1 127.7(12) . . . . ?
O8 S1 O2 Sc1 5.7(15) . . . . ?
O1 S1 O2 Sc1 -113.6(12) . . . . ?
O2 Sc1 O2 S1 -5E1(8) 25_565 . . . ?
O2 Sc1 O2 S1 112.2(15) 34_565 . . . ?
O2 Sc1 O2 S1 24.3(12) 44_565 . . . ?
O2 Sc1 O2 S1 -155.7(12) 20 . . . ?
O2 Sc1 O2 S1 -67.8(15) 10 . . . ?
O5 S2 O3 Sc2 -105.5(14) . . . . ?
O6 S2 O3 Sc2 16.5(16) 15_565 . . . ?
O4 S2 O3 Sc2 134.8(13) 29_565 . . . ?
O8 Sc2 O3 S2 103.7(14) 34_565 . . . ?
O1 Sc2 O3 S2 -130(5) . . . . ?
O10 Sc2 O3 S2 -74.6(14) . . . . ?
O6 Sc2 O3 S2 17.4(14) . . . . ?
O4 Sc2 O3 S2 -162.9(14) . . . . ?
O8 Sc2 O4 S2 -65.9(16) 34_565 . . 31_665 ?
O1 Sc2 O4 S2 25.6(16) . . . 31_665 ?
O10 Sc2 O4 S2 111.4(16) . . . 31_665 ?
O6 Sc2 O4 S2 -10E1(7) . . . 31_665 ?
O3 Sc2 O4 S2 -157.4(16) . . . 31_665 ?
O8 Sc2 O6 S2 148(2) 34_565 . . 15_565 ?
O1 Sc2 O6 S2 57(2) . . . 15_565 ?
O10 Sc2 O6 S2 -29(2) . . . 15_565 ?
O3 Sc2 O6 S2 -120(2) . . . 15_565 ?
O4 Sc2 O6 S2 18E1(10) . . . 15_565 ?
O7 S1 O8 Sc2 102(4) . . . 44_565 ?
O2 S1 O8 Sc2 -137(3) . . . 44_565 ?
O1 S1 O8 Sc2 -17(4) . . . 44_565 ?
O9 S3 O10 Sc2 -122(3) 9 . . . ?
O9 S3 O10 Sc2 129(3) 23_565 . . . ?
O10 S3 O10 Sc2 3.9(17) 15_565 . . . ?
O8 Sc2 O10 S3 -97(10) 34_565 . . . ?
O1 Sc2 O10 S3 -133(2) . . . . ?
O6 Sc2 O10 S3 -41(2) . . . . ?
O3 Sc2 O10 S3 51(2) . . . . ?
O4 Sc2 O10 S3 139(2) . . . . ?
N1 C1 C2 N1 74(2) . . . 23_565 ?
C2 C1 N1 C2 -158.3(15) . . . 24_556 ?