# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Sc-pydc-1D
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H11 N2 O10 Sc'
_chemical_formula_weight         412.21

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   6.3313(6)
_cell_length_b                   33.114(4)
_cell_length_c                   7.5538(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.400(6)
_cell_angle_gamma                90.00
_cell_volume                     1580.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       acicular
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            11404
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.23
_diffrn_reflns_theta_max         28.39
_reflns_number_total             3952
_reflns_number_gt                2632
_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 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. 
;

_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)+(0.0912P)²+1.2062P] 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_extinction_coef       ?
_refine_ls_number_reflns         3952
_refine_ls_number_parameters     254
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2027
_refine_ls_wR_factor_gt          0.1815
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
C1 C 0.2598(7) -0.01518(14) 0.1569(5) 0.0196(9) Uani 1 1 d . . .
H1 H 0.2695 -0.0053 0.0424 0.024 Uiso 1 1 calc R . .
C2 C 0.2496(7) -0.05621(15) 0.1804(5) 0.0217(10) Uani 1 1 d . . .
H2 H 0.2513 -0.0736 0.0838 0.026 Uiso 1 1 calc R . .
C3 C 0.2367(6) -0.07130(13) 0.3499(6) 0.0197(9) Uani 1 1 d . . .
H3 H 0.2275 -0.0990 0.3689 0.024 Uiso 1 1 calc R . .
C4 C 0.2378(6) -0.04450(13) 0.4917(5) 0.0154(8) Uani 1 1 d . . .
C5 C 0.2483(6) -0.00350(13) 0.4556(5) 0.0140(8) Uani 1 1 d . . .
C6 C 0.2369(6) -0.06175(12) 0.6768(5) 0.0163(8) Uani 1 1 d . . .
C7 C 0.2487(6) 0.02867(13) 0.5979(5) 0.0140(8) Uani 1 1 d . . .
C8 C -0.0554(8) 0.15353(16) 0.0997(8) 0.0365(12) Uani 1 1 d . . .
H4 H -0.1309 0.1308 0.0603 0.044 Uiso 1 1 calc R . .
C9 C -0.1354(9) 0.19129(17) 0.0546(9) 0.0453(15) Uani 1 1 d . . .
H5 H -0.2615 0.1941 -0.0140 0.054 Uiso 1 1 calc R . .
C10 C -0.0233(9) 0.22425(17) 0.1139(8) 0.0411(14) Uani 1 1 d . . .
H6 H -0.0756 0.2499 0.0870 0.049 Uiso 1 1 calc R . .
C11 C 0.1669(8) 0.22041(14) 0.2134(7) 0.0301(11) Uani 1 1 d . . .
C12 C 0.2340(7) 0.18106(13) 0.2552(5) 0.0216(9) Uani 1 1 d . . .
C13 C 0.4277(8) 0.16798(15) 0.3684(6) 0.0267(10) Uani 1 1 d . . .
C14 C 0.2774(10) 0.26024(17) 0.2600(8) 0.0420(14) Uani 1 1 d . . .
H7 H 0.490(10) 0.235(2) 0.398(8) 0.051(19) Uiso 1 1 d . . .
N1 N 0.1247(6) 0.14821(11) 0.1970(6) 0.0252(9) Uani 1 1 d . . .
N2 N 0.2564(5) 0.01132(11) 0.2910(4) 0.0153(7) Uani 1 1 d . . .
O1 O 0.4376(5) 0.13054(10) 0.4036(5) 0.0320(8) Uani 1 1 d . . .
O2 O 0.5641(6) 0.19201(12) 0.4273(6) 0.0488(11) Uani 1 1 d . . .
O3 O 0.4535(8) 0.26057(14) 0.3526(7) 0.0641(14) Uani 1 1 d . . .
O4 O 0.1946(8) 0.29120(12) 0.2080(7) 0.0595(13) Uani 1 1 d . . .
O5 O 0.2666(5) 0.06521(9) 0.5426(4) 0.0190(6) Uani 1 1 d . . .
O6 O 0.2314(5) 0.01874(9) 0.7543(4) 0.0220(7) Uani 1 1 d . . .
O7 O 0.4108(4) -0.06701(10) 0.7624(4) 0.0213(7) Uani 1 1 d . . .
O8 O 0.0638(4) -0.07221(10) 0.7352(4) 0.0215(7) Uani 1 1 d . . .
O9 O 0.2420(5) 0.07918(10) -0.0055(4) 0.0229(7) Uani 1 1 d . . .
H9A H 0.2828 0.0993 -0.0648 0.034 Uiso 1 1 d R . .
H9B H 0.2355 0.0598 -0.0793 0.034 Uiso 1 1 d R . .
O10 O 0.4056(9) 0.13702(13) 0.8067(7) 0.0564(13) Uani 1 1 d D . .
Sc1 Sc 0.26577(11) 0.08232(2) 0.27613(10) 0.0153(2) Uani 1 1 d . . .
H10 H 0.336(11) 0.1585(14) 0.787(10) 0.080 Uiso 1 1 d D . .
H11 H 0.420(13) 0.129(2) 0.701(5) 0.080 Uiso 1 1 d D . .


_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
C1 N2 1.342(5) . ?
C1 C2 1.372(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(6) . ?
C4 C6 1.511(6) . ?
C5 N2 1.340(5) . ?
C5 C7 1.514(6) . ?
C6 O8 1.254(5) . ?
C6 O7 1.256(5) . ?
C7 O6 1.237(5) . ?
C7 O5 1.287(5) . ?
C8 N1 1.331(6) . ?
C8 C9 1.384(7) . ?
C8 H4 0.9300 . ?
C9 C10 1.363(8) . ?
C9 H5 0.9300 . ?
C10 C11 1.387(8) . ?
C10 H6 0.9300 . ?
C11 C12 1.401(7) . ?
C11 C14 1.524(7) . ?
C12 N1 1.349(6) . ?
C12 C13 1.516(6) . ?
C13 O2 1.237(6) . ?
C13 O1 1.269(6) . ?
C14 O4 1.207(7) . ?
C14 O3 1.281(7) . ?
N1 Sc1 2.419(4) . ?
N2 Sc1 2.355(4) . ?
O1 Sc1 2.130(3) . ?
O3 H7 0.93(7) . ?
O5 Sc1 2.091(3) . ?
O7 Sc1 2.146(3) 3_656 ?
O8 Sc1 2.110(3) 3_556 ?
O9 Sc1 2.126(3) . ?
O9 H9A 0.8507 . ?
O9 H9B 0.8500 . ?
O10 H10 0.84(2) . ?
O10 H11 0.85(2) . ?
Sc1 O8 2.110(3) 3_556 ?
Sc1 O7 2.146(3) 3_656 ?

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
N2 C1 C2 123.1(4) . . ?
N2 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.9(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 C6 123.7(4) . . ?
C3 C4 C6 118.1(4) . . ?
N2 C5 C4 123.1(4) . . ?
N2 C5 C7 113.8(4) . . ?
C4 C5 C7 123.2(3) . . ?
O8 C6 O7 122.6(4) . . ?
O8 C6 C4 118.8(4) . . ?
O7 C6 C4 118.5(3) . . ?
O6 C7 O5 125.1(4) . . ?
O6 C7 C5 119.6(4) . . ?
O5 C7 C5 115.3(3) . . ?
N1 C8 C9 123.0(5) . . ?
N1 C8 H4 118.5 . . ?
C9 C8 H4 118.5 . . ?
C10 C9 C8 117.8(5) . . ?
C10 C9 H5 121.1 . . ?
C8 C9 H5 121.1 . . ?
C9 C10 C11 121.5(5) . . ?
C9 C10 H6 119.2 . . ?
C11 C10 H6 119.2 . . ?
C10 C11 C12 116.7(5) . . ?
C10 C11 C14 114.7(5) . . ?
C12 C11 C14 128.6(5) . . ?
N1 C12 C11 122.3(4) . . ?
N1 C12 C13 109.6(4) . . ?
C11 C12 C13 128.1(4) . . ?
O2 C13 O1 121.9(5) . . ?
O2 C13 C12 122.9(5) . . ?
O1 C13 C12 115.2(4) . . ?
O4 C14 O3 121.2(6) . . ?
O4 C14 C11 118.4(6) . . ?
O3 C14 C11 120.4(5) . . ?
C8 N1 C12 118.6(4) . . ?
C8 N1 Sc1 123.2(3) . . ?
C12 N1 Sc1 118.2(3) . . ?
C5 N2 C1 117.7(4) . . ?
C5 N2 Sc1 114.4(3) . . ?
C1 N2 Sc1 128.0(3) . . ?
C13 O1 Sc1 128.3(3) . . ?
C14 O3 H7 113(4) . . ?
C7 O5 Sc1 124.9(3) . . ?
C6 O7 Sc1 141.0(3) . 3_656 ?
C6 O8 Sc1 155.8(3) . 3_556 ?
Sc1 O9 H9A 118.9 . . ?
Sc1 O9 H9B 133.7 . . ?
H9A O9 H9B 104.4 . . ?
H10 O10 H11 101(7) . . ?
O5 Sc1 O8 86.68(11) . 3_556 ?
O5 Sc1 O9 161.08(13) . . ?
O8 Sc1 O9 86.60(12) 3_556 . ?
O5 Sc1 O1 78.23(13) . . ?
O8 Sc1 O1 127.93(13) 3_556 . ?
O9 Sc1 O1 119.52(13) . . ?
O5 Sc1 O7 96.82(11) . 3_656 ?
O8 Sc1 O7 155.00(13) 3_556 3_656 ?
O9 Sc1 O7 82.19(11) . 3_656 ?
O1 Sc1 O7 76.85(13) . 3_656 ?
O5 Sc1 N2 71.46(12) . . ?
O8 Sc1 N2 79.40(12) 3_556 . ?
O9 Sc1 N2 89.92(12) . . ?
O1 Sc1 N2 137.78(13) . . ?
O7 Sc1 N2 78.32(12) 3_656 . ?
O5 Sc1 N1 117.52(13) . . ?
O8 Sc1 N1 77.49(13) 3_556 . ?
O9 Sc1 N1 78.09(13) . . ?
O1 Sc1 N1 66.84(13) . . ?
O7 Sc1 N1 121.38(13) 3_656 . ?
N2 Sc1 N1 154.48(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H7 O2 0.93(7) 1.52(7) 2.432(6) 167(6) .
O9 H9A O10 0.85 1.79 2.632(5) 171.0 1_554
O9 H9B O6 0.85 1.85 2.700(4) 177.3 1_554
O10 H10 O4 0.84(2) 1.97(2) 2.806(6) 171(8) 4_566
O10 H11 O1 0.85(2) 2.26(3) 3.072(6) 160(7) .
O10 H11 O5 0.85(2) 2.59(6) 3.194(6) 129(7) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.150
_database_code_depnum_ccdc_archive 'CCDC 976321'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Sc-pydc-2D
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 N3 O21 Sc2'
_chemical_formula_weight         737.30

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.817(4)
_cell_length_b                   27.839(8)
_cell_length_c                   8.017(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.42(2)
_cell_angle_gamma                90.00
_cell_volume                     2847.8(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       rodlike
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            7721
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.1241
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4734
_reflns_number_gt                2766
_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 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. 
;

_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)+(0.0866P)²+0.0000P] 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_extinction_coef       ?
_refine_ls_number_reflns         4734
_refine_ls_number_parameters     456
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1836
_refine_ls_wR_factor_gt          0.1604
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.043
_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
H43 H 0.596(6) -0.0298(19) 0.943(12) 0.09(4) Uiso 1 1 d D . .
H40 H 0.625(6) 0.013(2) 1.024(6) 0.06(3) Uiso 1 1 d D . .
H26 H 0.668(5) -0.040(3) 0.524(6) 0.07(3) Uiso 1 1 d D . .
H25 H 0.731(6) -0.0730(11) 0.633(9) 0.05(2) Uiso 1 1 d D . .
H24 H 0.464(4) 0.1720(17) -0.246(3) 0.000(13) Uiso 1 1 d D . .
H23 H 0.556(2) 0.167(3) -0.120(11) 0.09(4) Uiso 1 1 d D . .
O20 O 0.4108(4) 0.05177(16) 0.6815(6) 0.0337(12) Uani 1 1 d . . .
O21 O 0.0911(7) 0.6588(3) 0.7036(12) 0.129(3) Uani 1 1 d . . .
O22 O 0.1356(9) 0.7469(4) 0.610(3) 0.312(12) Uani 1 1 d . . .
O16 O 1.1721(4) -0.11437(16) 0.8342(6) 0.0419(13) Uani 1 1 d . . .
O6 O 1.2053(3) -0.06374(14) 1.0468(5) 0.0289(11) Uani 1 1 d . . .
C6 C 1.1597(5) -0.0755(2) 0.9034(8) 0.0256(15) Uani 1 1 d . . .
C19 C 1.0945(5) -0.0361(2) 0.8152(7) 0.0221(15) Uani 1 1 d . . .
C1 C 0.5506(5) 0.0820(2) 0.2212(8) 0.0228(15) Uani 1 1 d . . .
C2 C 0.2752(5) 0.2540(2) -0.0860(7) 0.0173(13) Uani 1 1 d . . .
C3 C 0.6883(5) 0.1628(2) 0.5478(8) 0.0324(17) Uani 1 1 d . . .
H3 H 0.7379 0.1620 0.6402 0.039 Uiso 1 1 calc R . .
C4 C 0.5795(5) 0.2063(2) 0.3446(8) 0.0294(16) Uani 1 1 d . . .
H4 H 0.5550 0.2358 0.3023 0.035 Uiso 1 1 calc R . .
C5 C 0.1048(5) 0.2209(2) -0.2772(9) 0.0351(18) Uani 1 1 d . . .
H5 H 0.0467 0.2086 -0.3415 0.042 Uiso 1 1 calc R . .
C7 C 0.5819(5) 0.1243(2) 0.3307(7) 0.0192(14) Uani 1 1 d . . .
C8 C 0.2091(5) 0.2869(2) -0.1706(7) 0.0201(14) Uani 1 1 d . . .
C9 C 0.9876(5) -0.0303(2) 0.8193(7) 0.0196(14) Uani 1 1 d . . .
C10 C 0.2318(5) 0.3402(2) -0.1704(8) 0.0233(15) Uani 1 1 d . . .
C11 C 0.6505(5) 0.2060(2) 0.4833(9) 0.0369(18) Uani 1 1 d . . .
H11A H 0.6731 0.2348 0.5337 0.044 Uiso 1 1 calc R . .
C12 C 0.3668(5) 0.2679(2) 0.0323(7) 0.0203(14) Uani 1 1 d . . .
C13 C 0.6513(5) 0.1209(2) 0.4733(7) 0.0219(14) Uani 1 1 d . . .
C14 C 0.1750(5) 0.1907(2) -0.1927(8) 0.0308(17) Uani 1 1 d . . .
H14 H 0.1632 0.1578 -0.2021 0.037 Uiso 1 1 calc R . .
C15 C 1.0948(5) 0.0360(2) 0.6542(8) 0.0270(15) Uani 1 1 d . . .
H20 H 1.1303 0.0590 0.5969 0.032 Uiso 1 1 calc R . .
C16 C 0.1210(5) 0.2703(2) -0.2665(8) 0.0301(16) Uani 1 1 d . . .
H16 H 0.0738 0.2916 -0.3223 0.036 Uiso 1 1 calc R . .
C17 C 0.9896(5) 0.0399(2) 0.6638(8) 0.0274(16) Uani 1 1 d . . .
H17 H 0.9541 0.0661 0.6136 0.033 Uiso 1 1 calc R . .
C18 C 1.1474(5) -0.0019(2) 0.7293(8) 0.0270(16) Uani 1 1 d . . .
H18 H 1.2192 -0.0048 0.7232 0.032 Uiso 1 1 calc R . .
C20 C 0.9203(5) -0.0631(2) 0.9145(7) 0.0218(15) Uani 1 1 d . . .
C21 C 0.6826(5) 0.0754(2) 0.5609(8) 0.0263(16) Uani 1 1 d . . .
N1 N 0.9352(4) 0.00716(18) 0.7437(6) 0.0239(12) Uani 1 1 d . . .
N2 N 0.5438(4) 0.16651(16) 0.2675(6) 0.0216(12) Uani 1 1 d . . .
N3 N 0.2593(4) 0.20568(16) -0.0978(6) 0.0201(12) Uani 1 1 d . . .
O2 O 0.3846(3) 0.31017(14) 0.0650(5) 0.0264(10) Uani 1 1 d . . .
O3 O 0.3024(4) 0.35374(14) -0.2612(5) 0.0284(11) Uani 1 1 d . . .
O4 O 0.5992(3) 0.04325(15) 0.2411(6) 0.0320(12) Uani 1 1 d . . .
O5 O 0.3029(4) 0.10658(15) -0.0945(6) 0.0238(10) Uani 1 1 d D . .
O7 O 0.6307(4) -0.00416(16) 0.9362(6) 0.0299(11) Uani 1 1 d D . .
O8 O 0.7088(4) -0.04467(17) 0.6130(6) 0.0364(12) Uani 1 1 d D . .
O9 O 0.8238(3) -0.04880(14) 0.9145(5) 0.0241(10) Uani 1 1 d . . .
O10 O 0.4747(3) 0.08923(14) 0.1078(5) 0.0272(11) Uani 1 1 d . . .
O11 O 0.9571(4) -0.09900(16) 0.9828(6) 0.0395(13) Uani 1 1 d . . .
O12 O 0.7768(3) 0.06169(16) 0.5715(6) 0.0341(12) Uani 1 1 d . . .
O13 O 0.6197(3) 0.05295(16) 0.6424(6) 0.0368(12) Uani 1 1 d . . .
O14 O 0.4198(3) 0.23247(14) 0.0987(6) 0.0320(12) Uani 1 1 d . . .
O15 O 0.1788(4) 0.36812(16) -0.0952(6) 0.0393(13) Uani 1 1 d . . .
O17 O 0.4915(4) 0.16317(18) -0.1502(6) 0.0357(12) Uani 1 1 d D . .
O18 O 0.3022(4) 0.8245(2) 0.0460(7) 0.0624(17) Uani 1 1 d . . .
O19 O 0.9556(5) 0.1522(2) 0.4402(7) 0.0681(18) Uani 1 1 d . . .
Sc1 Sc 0.39799(9) 0.15875(4) 0.05601(15) 0.0208(3) Uani 1 1 d . . .
Sc2 Sc 0.75775(9) 0.01161(4) 0.78004(15) 0.0221(3) Uani 1 1 d . . .
H41 H 0.338(5) 0.093(2) -0.163(7) 0.06(3) Uiso 1 1 d D . .
H42 H 0.256(4) 0.091(2) -0.049(8) 0.03(2) Uiso 1 1 d D . .


_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
O16 C6 1.232(7) . ?
O6 C6 1.282(7) . ?
O6 Sc2 2.033(4) 3_757 ?
C6 C19 1.514(9) . ?
C19 C9 1.383(9) . ?
C19 C18 1.390(9) . ?
C1 O4 1.248(7) . ?
C1 O10 1.283(7) . ?
C1 C7 1.502(8) . ?
C2 N3 1.362(7) . ?
C2 C8 1.382(8) . ?
C2 C12 1.490(8) . ?
C3 C13 1.374(8) . ?
C3 C11 1.379(9) . ?
C3 H3 0.9300 . ?
C4 N2 1.329(7) . ?
C4 C11 1.369(9) . ?
C4 H4 0.9300 . ?
C5 C14 1.363(9) . ?
C5 C16 1.392(9) . ?
C5 H5 0.9300 . ?
C7 N2 1.352(7) . ?
C7 C13 1.384(8) . ?
C8 C16 1.385(8) . ?
C8 C10 1.512(8) . ?
C9 N1 1.353(7) . ?
C9 C20 1.512(9) . ?
C10 O15 1.228(7) . ?
C10 O3 1.270(8) . ?
C11 H11A 0.9300 . ?
C12 O2 1.222(7) . ?
C12 O14 1.284(7) . ?
C13 C21 1.486(8) . ?
C14 N3 1.329(8) . ?
C14 H14 0.9300 . ?
C15 C18 1.361(9) . ?
C15 C17 1.363(9) . ?
C15 H20 0.9300 . ?
C16 H16 0.9300 . ?
C17 N1 1.347(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C20 O11 1.213(7) . ?
C20 O9 1.300(7) . ?
C21 O13 1.251(8) . ?
C21 O12 1.261(8) . ?
N1 Sc2 2.323(5) . ?
N2 Sc1 2.411(5) . ?
N3 Sc1 2.444(5) . ?
O3 Sc1 2.027(5) 4_565 ?
O5 Sc1 2.185(4) . ?
O5 H41 0.846(10) . ?
O5 H42 0.849(10) . ?
O7 Sc2 2.190(5) . ?
O7 H43 0.849(10) . ?
O7 H40 0.855(10) . ?
O8 H26 0.851(10) . ?
O8 Sc2 2.117(5) . ?
O8 H26 0.851(10) . ?
O8 H25 0.850(10) . ?
O9 Sc2 2.129(4) . ?
O10 Sc1 2.193(4) . ?
O12 Sc2 2.208(4) . ?
O13 Sc2 2.303(4) . ?
O14 Sc1 2.095(4) . ?
O17 Sc1 2.135(5) . ?
O17 H24 0.849(10) . ?
O17 H23 0.849(10) . ?
Sc1 O3 2.027(5) 4_566 ?
Sc2 O6 2.033(4) 3_757 ?

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
C6 O6 Sc2 148.4(4) . 3_757 ?
O16 C6 O6 124.1(6) . . ?
O16 C6 C19 121.0(6) . . ?
O6 C6 C19 114.7(5) . . ?
C9 C19 C18 117.6(6) . . ?
C9 C19 C6 125.3(6) . . ?
C18 C19 C6 117.0(6) . . ?
O4 C1 O10 124.3(6) . . ?
O4 C1 C7 120.1(5) . . ?
O10 C1 C7 115.6(5) . . ?
N3 C2 C8 122.7(5) . . ?
N3 C2 C12 113.9(5) . . ?
C8 C2 C12 123.3(5) . . ?
C13 C3 C11 118.9(6) . . ?
C13 C3 H3 120.6 . . ?
C11 C3 H3 120.6 . . ?
N2 C4 C11 123.1(6) . . ?
N2 C4 H4 118.4 . . ?
C11 C4 H4 118.4 . . ?
C14 C5 C16 119.4(6) . . ?
C14 C5 H5 120.3 . . ?
C16 C5 H5 120.3 . . ?
N2 C7 C13 123.4(5) . . ?
N2 C7 C1 113.3(5) . . ?
C13 C7 C1 123.0(5) . . ?
C2 C8 C16 118.7(6) . . ?
C2 C8 C10 122.8(5) . . ?
C16 C8 C10 118.4(5) . . ?
N1 C9 C19 122.0(6) . . ?
N1 C9 C20 114.2(5) . . ?
C19 C9 C20 123.8(5) . . ?
O15 C10 O3 123.4(6) . . ?
O15 C10 C8 120.4(6) . . ?
O3 C10 C8 116.0(5) . . ?
C4 C11 C3 119.5(6) . . ?
C4 C11 H11A 120.3 . . ?
C3 C11 H11A 120.3 . . ?
O2 C12 O14 124.7(6) . . ?
O2 C12 C2 120.5(5) . . ?
O14 C12 C2 114.7(5) . . ?
C3 C13 C7 118.0(6) . . ?
C3 C13 C21 116.8(5) . . ?
C7 C13 C21 124.9(5) . . ?
N3 C14 C5 123.6(6) . . ?
N3 C14 H14 118.2 . . ?
C5 C14 H14 118.2 . . ?
C18 C15 C17 119.2(6) . . ?
C18 C15 H20 120.4 . . ?
C17 C15 H20 120.4 . . ?
C8 C16 C5 118.2(6) . . ?
C8 C16 H16 120.9 . . ?
C5 C16 H16 120.9 . . ?
N1 C17 C15 122.2(6) . . ?
N1 C17 H17 118.9 . . ?
C15 C17 H17 118.9 . . ?
C15 C18 C19 120.4(6) . . ?
C15 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
O11 C20 O9 125.7(6) . . ?
O11 C20 C9 120.6(6) . . ?
O9 C20 C9 113.8(5) . . ?
O13 C21 O12 118.3(6) . . ?
O13 C21 C13 120.9(6) . . ?
O12 C21 C13 120.2(6) . . ?
C17 N1 C9 118.6(5) . . ?
C17 N1 Sc2 125.5(4) . . ?
C9 N1 Sc2 115.8(4) . . ?
C4 N2 C7 117.0(5) . . ?
C4 N2 Sc1 127.7(4) . . ?
C7 N2 Sc1 114.5(4) . . ?
C14 N3 C2 117.2(5) . . ?
C14 N3 Sc1 129.4(4) . . ?
C2 N3 Sc1 113.3(4) . . ?
C10 O3 Sc1 151.0(4) . 4_565 ?
Sc1 O5 H41 111(5) . . ?
Sc1 O5 H42 119(5) . . ?
H41 O5 H42 119(7) . . ?
Sc2 O7 H43 129(7) . . ?
Sc2 O7 H40 119(5) . . ?
H43 O7 H40 109(8) . . ?
H26 O8 Sc2 122(6) . . ?
H26 O8 H26 0(10) . . ?
Sc2 O8 H26 122(6) . . ?
H26 O8 H25 119(8) . . ?
Sc2 O8 H25 119(5) . . ?
H26 O8 H25 119(8) . . ?
C20 O9 Sc2 125.1(4) . . ?
C1 O10 Sc1 124.8(4) . . ?
C21 O12 Sc2 93.9(4) . . ?
C21 O13 Sc2 89.8(4) . . ?
C12 O14 Sc1 128.9(4) . . ?
Sc1 O17 H24 120(3) . . ?
Sc1 O17 H23 113(7) . . ?
H24 O17 H23 122(7) . . ?
O3 Sc1 O14 97.51(18) 4_566 . ?
O3 Sc1 O17 172.52(19) 4_566 . ?
O14 Sc1 O17 89.6(2) . . ?
O3 Sc1 O5 86.63(18) 4_566 . ?
O14 Sc1 O5 143.16(17) . . ?
O17 Sc1 O5 86.3(2) . . ?
O3 Sc1 O10 90.15(17) 4_566 . ?
O14 Sc1 O10 141.53(16) . . ?
O17 Sc1 O10 85.59(18) . . ?
O5 Sc1 O10 74.63(16) . . ?
O3 Sc1 N2 89.33(18) 4_566 . ?
O14 Sc1 N2 73.42(16) . . ?
O17 Sc1 N2 94.87(19) . . ?
O5 Sc1 N2 143.40(17) . . ?
O10 Sc1 N2 69.02(15) . . ?
O3 Sc1 N3 89.76(17) 4_566 . ?
O14 Sc1 N3 68.79(15) . . ?
O17 Sc1 N3 90.76(18) . . ?
O5 Sc1 N3 74.66(16) . . ?
O10 Sc1 N3 149.24(16) . . ?
N2 Sc1 N3 141.73(16) . . ?
O6 Sc2 O8 174.9(2) 3_757 . ?
O6 Sc2 O9 99.34(17) 3_757 . ?
O8 Sc2 O9 79.36(17) . . ?
O6 Sc2 O7 83.71(18) 3_757 . ?
O8 Sc2 O7 91.2(2) . . ?
O9 Sc2 O7 80.42(17) . . ?
O6 Sc2 O12 91.78(18) 3_757 . ?
O8 Sc2 O12 92.06(19) . . ?
O9 Sc2 O12 144.58(17) . . ?
O7 Sc2 O12 134.49(17) . . ?
O6 Sc2 O13 95.12(17) 3_757 . ?
O8 Sc2 O13 84.18(19) . . ?
O9 Sc2 O13 152.61(17) . . ?
O7 Sc2 O13 78.19(18) . . ?
O12 Sc2 O13 57.08(17) . . ?
O6 Sc2 N1 87.48(18) 3_757 . ?
O8 Sc2 N1 96.68(19) . . ?
O9 Sc2 N1 70.99(17) . . ?
O7 Sc2 N1 148.24(18) . . ?
O12 Sc2 N1 76.08(17) . . ?
O13 Sc2 N1 133.12(18) . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 976322'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Sc-pydc-3D
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H5 N2 O8 Sc'
_chemical_formula_weight         290.09

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'
Sc Sc 0.2519 0.3716 '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-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'

_cell_length_a                   23.2465(9)
_cell_length_b                   23.2465(9)
_cell_length_c                   10.2390(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4791.8(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            11833
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         28.28
_reflns_number_total             2637
_reflns_number_gt                2254
_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 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. 
;

_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)+(0.0018P)²+122.6964P] 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_extinction_coef       ?
_refine_ls_number_reflns         2637
_refine_ls_number_parameters     169
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.1924
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.206
_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
Sc1 Sc 0.27423(5) 0.07034(5) -0.12034(9) 0.0177(2) Uani 1 1 d . . .
O1 O 0.35224(18) 0.0838(2) 0.0093(4) 0.0251(8) Uani 1 1 d . . .
O6 O 0.1694(2) 0.0462(2) -0.1524(4) 0.0348(10) Uani 1 1 d . . .
O5 O 0.2327(2) 0.0690(2) -0.3182(4) 0.0348(10) Uani 1 1 d . . .
O2 O 0.39277(18) 0.09222(19) 0.2100(3) 0.0242(8) Uani 1 1 d . . .
O3 O 0.3661(2) 0.16566(18) 0.4428(4) 0.0291(9) Uani 1 1 d . . .
O4 O 0.3272(2) 0.05951(19) 0.4876(4) 0.0276(8) Uani 1 1 d . . .
O8 O 0.3523(2) 0.0862(2) -0.2487(4) 0.0262(8) Uani 1 1 d D . .
O7 O 0.1315(2) 0.0486(3) -0.3447(5) 0.0493(13) Uani 1 1 d . . .
N1 N 0.2374(2) 0.0625(2) 0.0936(4) 0.0228(9) Uani 1 1 d . . .
C1 C 0.1785(3) 0.0517(3) 0.1337(6) 0.0295(12) Uani 1 1 d . . .
H1 H 0.1453 0.0406 0.0717 0.035 Uiso 1 1 calc R . .
C4 C 0.2753(3) 0.0853(2) 0.3171(5) 0.0215(10) Uani 1 1 d . . .
C2 C 0.1640(3) 0.0563(3) 0.2638(6) 0.0332(13) Uani 1 1 d . . .
H2 H 0.1217 0.0470 0.2882 0.040 Uiso 1 1 calc R . .
C3 C 0.2132(3) 0.0747(3) 0.3556(5) 0.0312(12) Uani 1 1 d . . .
H3 H 0.2052 0.0801 0.4425 0.037 Uiso 1 1 calc R . .
C5 C 0.2844(2) 0.0780(2) 0.1885(5) 0.0158(9) Uani 1 1 d . . .
C7 C 0.3486(2) 0.0858(2) 0.1305(5) 0.0188(9) Uani 1 1 d . . .
N2 N 0.1762(2) 0.0547(2) -0.2763(5) 0.0279(10) Uani 1 1 d . . .
C6 C 0.3276(3) 0.1040(3) 0.4221(5) 0.0206(10) Uani 1 1 d . . .
H4 H 0.348(5) 0.081(5) -0.331(2) 0.080 Uiso 1 1 d D . .
H5 H 0.377(4) 0.079(5) -0.198(8) 0.080 Uiso 1 1 d D . .


_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 O3 2.030(4) 13 ?
Sc1 O8 2.119(4) . ?
Sc1 O2 2.120(4) 8_544 ?
Sc1 O1 2.140(4) . ?
Sc1 O6 2.234(4) . ?
Sc1 O5 2.238(4) . ?
Sc1 N1 2.326(4) . ?
Sc1 H5 2.42(8) . ?
O1 C7 1.246(6) . ?
O6 N2 1.281(6) . ?
O5 N2 1.257(6) . ?
O2 C7 1.260(6) . ?
O2 Sc1 2.120(4) 6 ?
O3 C6 1.272(6) . ?
O3 Sc1 2.030(4) 13 ?
O4 C6 1.229(6) . ?
O8 H4 0.85(2) . ?
O8 H5 0.84(2) . ?
O7 N2 1.202(6) . ?
N1 C1 1.327(7) . ?
N1 C5 1.368(6) . ?
C1 C2 1.391(8) . ?
C1 H1 0.9300 . ?
C4 C5 1.357(7) . ?
C4 C3 1.395(8) . ?
C4 C6 1.516(7) . ?
C2 C3 1.372(8) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C5 C7 1.531(7) . ?

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 Sc1 O8 94.92(17) 13 . ?
O3 Sc1 O2 176.08(17) 13 8_544 ?
O8 Sc1 O2 89.00(15) . 8_544 ?
O3 Sc1 O1 92.41(16) 13 . ?
O8 Sc1 O1 76.66(15) . . ?
O2 Sc1 O1 88.63(15) 8_544 . ?
O3 Sc1 O6 88.33(17) 13 . ?
O8 Sc1 O6 133.21(16) . . ?
O2 Sc1 O6 88.88(16) 8_544 . ?
O1 Sc1 O6 149.97(15) . . ?
O3 Sc1 O5 87.30(17) 13 . ?
O8 Sc1 O5 76.55(15) . . ?
O2 Sc1 O5 93.48(16) 8_544 . ?
O1 Sc1 O5 153.08(15) . . ?
O6 Sc1 O5 56.95(15) . . ?
O3 Sc1 N1 85.98(16) 13 . ?
O8 Sc1 N1 147.95(15) . . ?
O2 Sc1 N1 90.78(15) 8_544 . ?
O1 Sc1 N1 71.30(15) . . ?
O6 Sc1 N1 78.82(15) . . ?
O5 Sc1 N1 135.41(16) . . ?
O3 Sc1 H5 101(2) 13 . ?
O8 Sc1 H5 20.0(12) . . ?
O2 Sc1 H5 83(2) 8_544 . ?
O1 Sc1 H5 57.7(14) . . ?
O6 Sc1 H5 151.2(16) . . ?
O5 Sc1 H5 96.0(13) . . ?
N1 Sc1 H5 128.6(13) . . ?
C7 O1 Sc1 123.7(3) . . ?
N2 O6 Sc1 94.1(3) . . ?
N2 O5 Sc1 94.6(3) . . ?
C7 O2 Sc1 134.0(3) . 6 ?
C6 O3 Sc1 156.3(4) . 13 ?
Sc1 O8 H4 124(7) . . ?
Sc1 O8 H5 101(7) . . ?
H4 O8 H5 128(9) . . ?
C1 N1 C5 116.2(4) . . ?
C1 N1 Sc1 127.6(4) . . ?
C5 N1 Sc1 115.7(3) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C5 C4 C3 117.7(5) . . ?
C5 C4 C6 124.8(5) . . ?
C3 C4 C6 117.5(5) . . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.2(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C4 C5 N1 124.6(4) . . ?
C4 C5 C7 124.4(4) . . ?
N1 C5 C7 111.0(4) . . ?
O1 C7 O2 125.6(5) . . ?
O1 C7 C5 117.6(4) . . ?
O2 C7 C5 116.9(4) . . ?
O7 N2 O5 124.0(5) . . ?
O7 N2 O6 121.8(5) . . ?
O5 N2 O6 114.2(4) . . ?
O4 C6 O3 124.3(5) . . ?
O4 C6 C4 118.6(5) . . ?
O3 C6 C4 116.9(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O8 H5 O1 0.84(2) 2.21(9) 2.642(5) 111(8) .
O8 H5 O4 0.84(2) 2.01(7) 2.676(5) 135(9) 6_554
O8 H4 O4 0.85(2) 1.92(3) 2.766(5) 172(10) 1_554

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.136
_database_code_depnum_ccdc_archive 'CCDC 976323'
