# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1550155'
_audit_update_record             
;
2017-06-19 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Cd O4 Sc'
_chemical_formula_weight         232.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   9.921(9)
_cell_length_b                   3.372(3)
_cell_length_c                   9.469(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     316.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    418
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    8.685
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_process_details   face-indexed

_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  '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            1819
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         27.44
_reflns_number_total             418
_reflns_number_gt                383
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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)+(0.0220P)²+4.4671P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0084(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         418
_refine_ls_number_parameters     46
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0258
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_restrained_S_all      1.262
_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
Cd1 Cd 1.09094(7) 1.2500 0.67300(8) 0.0111(3) Uani 0.7405(11) 2 d SP . .
Sc1 Sc 1.09094(7) 1.2500 0.67300(8) 0.0111(3) Uani 0.2595(11) 2 d SP . .
Cd2 Cd 0.88642(12) 0.7500 0.92397(14) 0.0144(4) Uani 0.2590(10) 2 d SP . .
Sc2 Sc 0.88642(12) 0.7500 0.92397(14) 0.0144(4) Uani 0.7410(10) 2 d SP . .
O1 O 0.9934(6) 0.7500 1.1142(6) 0.0142(13) Uani 1 2 d S . .
O3 O 0.7447(7) 0.7500 0.7517(7) 0.0214(15) Uani 1 2 d S . .
O2 O 0.7476(7) 0.2500 0.9991(7) 0.0232(16) Uani 1 2 d S . .
O4 O 0.9534(7) 0.7500 0.6293(10) 0.041(2) Uani 1 2 d S . .
B1 B 0.8161(10) 0.7500 0.6250(11) 0.0142(19) Uani 1 2 d S . .


_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
Cd1 O1 2.181(6) 5_777 ?
Cd1 O4 2.208(5) . ?
Cd1 O4 2.208(5) 1_565 ?
Cd1 O2 2.252(6) 6_667 ?
Cd1 O3 2.382(5) 6_667 ?
Cd1 O3 2.382(5) 6_657 ?
Cd1 Cd1 3.372(3) 1_545 ?
Cd1 Cd1 3.372(3) 1_565 ?
Cd1 Sc1 3.372(3) 1_545 ?
Cd1 Sc1 3.372(3) 1_565 ?
Cd1 Sc2 3.504(3) 6_667 ?
Cd1 Sc2 3.504(3) 6_657 ?
Cd2 O1 2.091(6) . ?
Cd2 O1 2.097(4) 5_777 ?
Cd2 O1 2.097(4) 5_767 ?
Cd2 O3 2.153(7) . ?
Cd2 O2 2.290(5) . ?
Cd2 O2 2.290(5) 1_565 ?
Cd2 Sc2 3.161(3) 5_777 ?
Cd2 Cd2 3.161(3) 5_777 ?
Cd2 Sc2 3.161(3) 5_767 ?
Cd2 Cd2 3.161(3) 5_767 ?
Cd2 Cd2 3.372(3) 1_565 ?
Cd2 Cd2 3.372(3) 1_545 ?
O1 Sc2 2.097(4) 5_777 ?
O1 Cd2 2.097(4) 5_777 ?
O1 Sc2 2.097(4) 5_767 ?
O1 Cd2 2.097(4) 5_767 ?
O1 Cd1 2.181(6) 5_777 ?
O1 Sc1 2.181(6) 5_777 ?
O3 B1 1.394(12) . ?
O3 Sc1 2.382(5) 6_547 ?
O3 Cd1 2.382(5) 6_547 ?
O3 Sc1 2.382(5) 6_557 ?
O3 Cd1 2.382(5) 6_557 ?
O2 B1 1.349(12) 2_665 ?
O2 Sc1 2.252(6) 6_547 ?
O2 Cd1 2.252(6) 6_547 ?
O2 Cd2 2.290(5) 1_545 ?
O2 Sc2 2.290(5) 1_545 ?
O4 B1 1.363(12) . ?
O4 Sc1 2.208(5) 1_545 ?
O4 Cd1 2.208(5) 1_545 ?
B1 O2 1.349(12) 2_664 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O4 86.3(3) 5_777 . ?
O1 Cd1 O4 86.3(3) 5_777 1_565 ?
O4 Cd1 O4 99.5(3) . 1_565 ?
O1 Cd1 O2 158.9(2) 5_777 6_667 ?
O4 Cd1 O2 106.9(3) . 6_667 ?
O4 Cd1 O2 106.9(3) 1_565 6_667 ?
O1 Cd1 O3 88.23(19) 5_777 6_667 ?
O4 Cd1 O3 172.7(3) . 6_667 ?
O4 Cd1 O3 84.9(2) 1_565 6_667 ?
O2 Cd1 O3 77.0(2) 6_667 6_667 ?
O1 Cd1 O3 88.23(19) 5_777 6_657 ?
O4 Cd1 O3 84.9(2) . 6_657 ?
O4 Cd1 O3 172.7(3) 1_565 6_657 ?
O2 Cd1 O3 77.0(2) 6_667 6_657 ?
O3 Cd1 O3 90.1(2) 6_667 6_657 ?
O1 Cd1 Cd1 90.000(1) 5_777 1_545 ?
O4 Cd1 Cd1 40.23(15) . 1_545 ?
O4 Cd1 Cd1 139.77(15) 1_565 1_545 ?
O2 Cd1 Cd1 90.0 6_667 1_545 ?
O3 Cd1 Cd1 135.04(12) 6_667 1_545 ?
O3 Cd1 Cd1 44.96(12) 6_657 1_545 ?
O1 Cd1 Cd1 90.000(1) 5_777 1_565 ?
O4 Cd1 Cd1 139.77(15) . 1_565 ?
O4 Cd1 Cd1 40.23(15) 1_565 1_565 ?
O2 Cd1 Cd1 90.0 6_667 1_565 ?
O3 Cd1 Cd1 44.96(12) 6_667 1_565 ?
O3 Cd1 Cd1 135.04(12) 6_657 1_565 ?
Cd1 Cd1 Cd1 180.00(5) 1_545 1_565 ?
O1 Cd1 Sc1 90.000(1) 5_777 1_545 ?
O4 Cd1 Sc1 40.23(15) . 1_545 ?
O4 Cd1 Sc1 139.77(15) 1_565 1_545 ?
O2 Cd1 Sc1 90.0 6_667 1_545 ?
O3 Cd1 Sc1 135.04(12) 6_667 1_545 ?
O3 Cd1 Sc1 44.96(12) 6_657 1_545 ?
Cd1 Cd1 Sc1 0.00(3) 1_545 1_545 ?
Cd1 Cd1 Sc1 180.00(5) 1_565 1_545 ?
O1 Cd1 Sc1 90.000(1) 5_777 1_565 ?
O4 Cd1 Sc1 139.77(15) . 1_565 ?
O4 Cd1 Sc1 40.23(15) 1_565 1_565 ?
O2 Cd1 Sc1 90.0 6_667 1_565 ?
O3 Cd1 Sc1 44.96(12) 6_667 1_565 ?
O3 Cd1 Sc1 135.04(12) 6_657 1_565 ?
Cd1 Cd1 Sc1 180.00(5) 1_545 1_565 ?
Cd1 Cd1 Sc1 0.00(4) 1_565 1_565 ?
Sc1 Cd1 Sc1 180.00(5) 1_545 1_565 ?
O1 Cd1 Sc2 124.25(14) 5_777 6_667 ?
O4 Cd1 Sc2 146.6(2) . 6_667 ?
O4 Cd1 Sc2 95.78(18) 1_565 6_667 ?
O2 Cd1 Sc2 39.92(12) 6_667 6_667 ?
O3 Cd1 Sc2 37.10(16) 6_667 6_667 ?
O3 Cd1 Sc2 83.30(15) 6_657 6_667 ?
Cd1 Cd1 Sc2 118.76(3) 1_545 6_667 ?
Cd1 Cd1 Sc2 61.24(3) 1_565 6_667 ?
Sc1 Cd1 Sc2 118.76(3) 1_545 6_667 ?
Sc1 Cd1 Sc2 61.24(3) 1_565 6_667 ?
O1 Cd1 Sc2 124.25(13) 5_777 6_657 ?
O4 Cd1 Sc2 95.78(18) . 6_657 ?
O4 Cd1 Sc2 146.6(2) 1_565 6_657 ?
O2 Cd1 Sc2 39.92(11) 6_667 6_657 ?
O3 Cd1 Sc2 83.30(15) 6_667 6_657 ?
O3 Cd1 Sc2 37.10(16) 6_657 6_657 ?
Cd1 Cd1 Sc2 61.24(3) 1_545 6_657 ?
Cd1 Cd1 Sc2 118.76(3) 1_565 6_657 ?
Sc1 Cd1 Sc2 61.24(3) 1_545 6_657 ?
Sc1 Cd1 Sc2 118.76(3) 1_565 6_657 ?
Sc2 Cd1 Sc2 57.52(6) 6_667 6_657 ?
O1 Cd2 O1 82.0(2) . 5_777 ?
O1 Cd2 O1 82.0(2) . 5_767 ?
O1 Cd2 O1 107.0(3) 5_777 5_767 ?
O1 Cd2 O3 169.7(3) . . ?
O1 Cd2 O3 103.9(2) 5_777 . ?
O1 Cd2 O3 103.9(2) 5_767 . ?
O1 Cd2 O2 92.1(2) . . ?
O1 Cd2 O2 171.0(2) 5_777 . ?
O1 Cd2 O2 78.68(19) 5_767 . ?
O3 Cd2 O2 80.9(2) . . ?
O1 Cd2 O2 92.1(2) . 1_565 ?
O1 Cd2 O2 78.68(19) 5_777 1_565 ?
O1 Cd2 O2 171.0(2) 5_767 1_565 ?
O3 Cd2 O2 80.9(2) . 1_565 ?
O2 Cd2 O2 94.8(3) . 1_565 ?
O1 Cd2 Sc2 41.05(10) . 5_777 ?
O1 Cd2 Sc2 40.91(17) 5_777 5_777 ?
O1 Cd2 Sc2 95.85(17) 5_767 5_777 ?
O3 Cd2 Sc2 144.14(9) . 5_777 ?
O2 Cd2 Sc2 132.82(17) . 5_777 ?
O2 Cd2 Sc2 83.95(16) 1_565 5_777 ?
O1 Cd2 Cd2 41.05(10) . 5_777 ?
O1 Cd2 Cd2 40.91(17) 5_777 5_777 ?
O1 Cd2 Cd2 95.85(17) 5_767 5_777 ?
O3 Cd2 Cd2 144.14(9) . 5_777 ?
O2 Cd2 Cd2 132.82(17) . 5_777 ?
O2 Cd2 Cd2 83.95(16) 1_565 5_777 ?
Sc2 Cd2 Cd2 0.00(4) 5_777 5_777 ?
O1 Cd2 Sc2 41.05(10) . 5_767 ?
O1 Cd2 Sc2 95.85(17) 5_777 5_767 ?
O1 Cd2 Sc2 40.91(17) 5_767 5_767 ?
O3 Cd2 Sc2 144.14(9) . 5_767 ?
O2 Cd2 Sc2 83.95(16) . 5_767 ?
O2 Cd2 Sc2 132.82(17) 1_565 5_767 ?
Sc2 Cd2 Sc2 64.45(7) 5_777 5_767 ?
Cd2 Cd2 Sc2 64.45(7) 5_777 5_767 ?
O1 Cd2 Cd2 41.05(10) . 5_767 ?
O1 Cd2 Cd2 95.85(17) 5_777 5_767 ?
O1 Cd2 Cd2 40.91(17) 5_767 5_767 ?
O3 Cd2 Cd2 144.14(9) . 5_767 ?
O2 Cd2 Cd2 83.95(16) . 5_767 ?
O2 Cd2 Cd2 132.82(17) 1_565 5_767 ?
Sc2 Cd2 Cd2 64.45(7) 5_777 5_767 ?
Cd2 Cd2 Cd2 64.45(7) 5_777 5_767 ?
Sc2 Cd2 Cd2 0.00(4) 5_767 5_767 ?
O1 Cd2 Cd2 90.000(1) . 1_565 ?
O1 Cd2 Cd2 36.48(14) 5_777 1_565 ?
O1 Cd2 Cd2 143.52(14) 5_767 1_565 ?
O3 Cd2 Cd2 90.000(1) . 1_565 ?
O2 Cd2 Cd2 137.40(13) . 1_565 ?
O2 Cd2 Cd2 42.60(13) 1_565 1_565 ?
Sc2 Cd2 Cd2 57.77(4) 5_777 1_565 ?
Cd2 Cd2 Cd2 57.77(4) 5_777 1_565 ?
Sc2 Cd2 Cd2 122.23(4) 5_767 1_565 ?
Cd2 Cd2 Cd2 122.23(4) 5_767 1_565 ?
O1 Cd2 Cd2 90.000(1) . 1_545 ?
O1 Cd2 Cd2 143.52(14) 5_777 1_545 ?
O1 Cd2 Cd2 36.48(14) 5_767 1_545 ?
O3 Cd2 Cd2 90.000(1) . 1_545 ?
O2 Cd2 Cd2 42.60(13) . 1_545 ?
O2 Cd2 Cd2 137.40(13) 1_565 1_545 ?
Sc2 Cd2 Cd2 122.23(4) 5_777 1_545 ?
Cd2 Cd2 Cd2 122.23(4) 5_777 1_545 ?
Sc2 Cd2 Cd2 57.77(4) 5_767 1_545 ?
Cd2 Cd2 Cd2 57.77(4) 5_767 1_545 ?
Cd2 Cd2 Cd2 180.00(8) 1_565 1_545 ?
Cd2 O1 Sc2 98.0(2) . 5_777 ?
Cd2 O1 Cd2 98.0(2) . 5_777 ?
Sc2 O1 Cd2 0.00(7) 5_777 5_777 ?
Cd2 O1 Sc2 98.0(2) . 5_767 ?
Sc2 O1 Sc2 107.0(3) 5_777 5_767 ?
Cd2 O1 Sc2 107.0(3) 5_777 5_767 ?
Cd2 O1 Cd2 98.0(2) . 5_767 ?
Sc2 O1 Cd2 107.0(3) 5_777 5_767 ?
Cd2 O1 Cd2 107.0(3) 5_777 5_767 ?
Sc2 O1 Cd2 0.00(7) 5_767 5_767 ?
Cd2 O1 Cd1 127.0(3) . 5_777 ?
Sc2 O1 Cd1 112.2(2) 5_777 5_777 ?
Cd2 O1 Cd1 112.2(2) 5_777 5_777 ?
Sc2 O1 Cd1 112.2(2) 5_767 5_777 ?
Cd2 O1 Cd1 112.2(2) 5_767 5_777 ?
Cd2 O1 Sc1 127.0(3) . 5_777 ?
Sc2 O1 Sc1 112.2(2) 5_777 5_777 ?
Cd2 O1 Sc1 112.2(2) 5_777 5_777 ?
Sc2 O1 Sc1 112.2(2) 5_767 5_777 ?
Cd2 O1 Sc1 112.2(2) 5_767 5_777 ?
Cd1 O1 Sc1 0.00(3) 5_777 5_777 ?
B1 O3 Cd2 108.7(6) . . ?
B1 O3 Sc1 125.7(3) . 6_547 ?
Cd2 O3 Sc1 101.0(2) . 6_547 ?
B1 O3 Cd1 125.7(3) . 6_547 ?
Cd2 O3 Cd1 101.0(2) . 6_547 ?
Sc1 O3 Cd1 0.00(3) 6_547 6_547 ?
B1 O3 Sc1 125.7(3) . 6_557 ?
Cd2 O3 Sc1 101.0(2) . 6_557 ?
Sc1 O3 Sc1 90.1(2) 6_547 6_557 ?
Cd1 O3 Sc1 90.1(2) 6_547 6_557 ?
B1 O3 Cd1 125.7(3) . 6_557 ?
Cd2 O3 Cd1 101.0(2) . 6_557 ?
Sc1 O3 Cd1 90.1(2) 6_547 6_557 ?
Cd1 O3 Cd1 90.1(2) 6_547 6_557 ?
Sc1 O3 Cd1 0.00(5) 6_557 6_557 ?
B1 O2 Sc1 108.4(6) 2_665 6_547 ?
B1 O2 Cd1 108.4(6) 2_665 6_547 ?
Sc1 O2 Cd1 0.00(3) 6_547 6_547 ?
B1 O2 Cd2 123.8(3) 2_665 . ?
Sc1 O2 Cd2 101.0(2) 6_547 . ?
Cd1 O2 Cd2 101.0(2) 6_547 . ?
B1 O2 Cd2 123.8(3) 2_665 1_545 ?
Sc1 O2 Cd2 101.0(2) 6_547 1_545 ?
Cd1 O2 Cd2 101.0(2) 6_547 1_545 ?
Cd2 O2 Cd2 94.8(3) . 1_545 ?
B1 O2 Sc2 123.8(3) 2_665 1_545 ?
Sc1 O2 Sc2 101.0(2) 6_547 1_545 ?
Cd1 O2 Sc2 101.0(2) 6_547 1_545 ?
Cd2 O2 Sc2 94.8(3) . 1_545 ?
Cd2 O2 Sc2 0.00(6) 1_545 1_545 ?
B1 O4 Cd1 128.6(2) . . ?
B1 O4 Sc1 128.6(2) . 1_545 ?
Cd1 O4 Sc1 99.5(3) . 1_545 ?
B1 O4 Cd1 128.6(2) . 1_545 ?
Cd1 O4 Cd1 99.5(3) . 1_545 ?
Sc1 O4 Cd1 0.00(4) 1_545 1_545 ?
O2 B1 O4 119.7(9) 2_664 . ?
O2 B1 O3 121.5(8) 2_664 . ?
O4 B1 O3 118.8(9) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.319
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1550159'
_audit_update_record             
;
2017-05-15 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B Ca O4 Sc'
_chemical_formula_weight         159.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Ca Ca 0.2262 0.3064 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   10.283(4)
_cell_length_b                   3.3636(13)
_cell_length_c                   9.432(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     326.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    438
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             312
_exptl_absorpt_coefficient_mu    3.662
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_process_details   face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            1857
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.47
_reflns_number_total             438
_reflns_number_gt                395
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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)+(0.0252P)²+0.1446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         438
_refine_ls_number_parameters     44
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0152
_refine_ls_wR_factor_ref         0.0480
_refine_ls_wR_factor_gt          0.0460
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.174
_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 0.38994(4) 1.2500 0.57162(5) 0.00806(17) Uani 1 2 d S . .
Ca1 Ca 0.58870(5) 0.7500 0.84087(5) 0.00786(16) Uani 1 2 d S . .
B1 B 0.3046(3) 1.2500 0.8649(3) 0.0084(5) Uani 1 2 d S . .
O1 O 0.50199(16) 0.7500 0.61564(17) 0.0079(4) Uani 1 2 d S . .
O2 O 0.24343(17) 1.2500 0.73431(18) 0.0107(4) Uani 1 2 d S . .
O3 O 0.26621(17) 0.7500 0.48923(17) 0.0106(4) Uani 1 2 d S . .
O4 O 0.43786(18) 0.2500 0.8747(2) 0.0158(4) Uani 1 2 d S . .


_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 O1 2.0805(12) 1_565 ?
Sc1 O1 2.0805(11) . ?
Sc1 O1 2.0868(18) 5_676 ?
Sc1 O2 2.1505(18) . ?
Sc1 O3 2.2475(13) . ?
Sc1 O3 2.2475(13) 1_565 ?
Sc1 Sc1 3.1269(11) 5_686 ?
Sc1 Sc1 3.1269(11) 5_676 ?
Sc1 Sc1 3.3636(13) 1_545 ?
Sc1 Sc1 3.3636(13) 1_565 ?
Sc1 Ca1 3.6203(12) 6_557 ?
Sc1 Ca1 3.6203(12) 6_567 ?
Ca1 O1 2.3039(19) . ?
Ca1 O4 2.3101(14) . ?
Ca1 O4 2.3101(14) 1_565 ?
Ca1 O2 2.4214(14) 6_657 ?
Ca1 O2 2.4214(14) 6_647 ?
Ca1 O3 2.4290(19) 6_657 ?
Ca1 O4 2.696(2) 5_667 ?
Ca1 B1 2.984(3) 5_677 ?
Ca1 Ca1 3.3636(13) 1_545 ?
Ca1 Ca1 3.3636(13) 1_565 ?
Ca1 Sc1 3.6203(12) 6_657 ?
Ca1 Sc1 3.6203(12) 6_647 ?
B1 O4 1.373(3) 1_565 ?
B1 O3 1.381(3) 2_575 ?
B1 O2 1.383(3) . ?
B1 Ca1 2.984(3) 5_677 ?
O1 Sc1 2.0805(11) 1_545 ?
O1 Sc1 2.0868(18) 5_676 ?
O2 Ca1 2.4214(14) 6_557 ?
O2 Ca1 2.4214(14) 6_567 ?
O3 B1 1.381(3) 2_574 ?
O3 Sc1 2.2475(13) 1_545 ?
O3 Ca1 2.4290(19) 6_557 ?
O4 B1 1.373(3) 1_545 ?
O4 Ca1 2.3101(14) 1_545 ?
O4 Ca1 2.696(2) 5_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sc1 O1 107.88(8) 1_565 . ?
O1 Sc1 O1 82.76(6) 1_565 5_676 ?
O1 Sc1 O1 82.76(6) . 5_676 ?
O1 Sc1 O2 104.22(6) 1_565 . ?
O1 Sc1 O2 104.22(6) . . ?
O1 Sc1 O2 167.70(7) 5_676 . ?
O1 Sc1 O3 170.91(6) 1_565 . ?
O1 Sc1 O3 77.15(6) . . ?
O1 Sc1 O3 90.51(6) 5_676 . ?
O2 Sc1 O3 81.38(6) . . ?
O1 Sc1 O3 77.15(6) 1_565 1_565 ?
O1 Sc1 O3 170.91(6) . 1_565 ?
O1 Sc1 O3 90.51(6) 5_676 1_565 ?
O2 Sc1 O3 81.38(6) . 1_565 ?
O3 Sc1 O3 96.89(7) . 1_565 ?
O1 Sc1 Sc1 41.46(5) 1_565 5_686 ?
O1 Sc1 Sc1 96.90(5) . 5_686 ?
O1 Sc1 Sc1 41.30(3) 5_676 5_686 ?
O2 Sc1 Sc1 144.63(2) . 5_686 ?
O3 Sc1 Sc1 131.52(5) . 5_686 ?
O3 Sc1 Sc1 81.83(5) 1_565 5_686 ?
O1 Sc1 Sc1 96.90(5) 1_565 5_676 ?
O1 Sc1 Sc1 41.46(5) . 5_676 ?
O1 Sc1 Sc1 41.30(3) 5_676 5_676 ?
O2 Sc1 Sc1 144.63(2) . 5_676 ?
O3 Sc1 Sc1 81.83(5) . 5_676 ?
O3 Sc1 Sc1 131.52(5) 1_565 5_676 ?
Sc1 Sc1 Sc1 65.08(3) 5_686 5_676 ?
O1 Sc1 Sc1 143.94(4) 1_565 1_545 ?
O1 Sc1 Sc1 36.06(4) . 1_545 ?
O1 Sc1 Sc1 90.0 5_676 1_545 ?
O2 Sc1 Sc1 90.0 . 1_545 ?
O3 Sc1 Sc1 41.56(4) . 1_545 ?
O3 Sc1 Sc1 138.44(4) 1_565 1_545 ?
Sc1 Sc1 Sc1 122.538(15) 5_686 1_545 ?
Sc1 Sc1 Sc1 57.462(15) 5_676 1_545 ?
O1 Sc1 Sc1 36.06(4) 1_565 1_565 ?
O1 Sc1 Sc1 143.94(4) . 1_565 ?
O1 Sc1 Sc1 90.0 5_676 1_565 ?
O2 Sc1 Sc1 90.0 . 1_565 ?
O3 Sc1 Sc1 138.44(4) . 1_565 ?
O3 Sc1 Sc1 41.56(4) 1_565 1_565 ?
Sc1 Sc1 Sc1 57.462(15) 5_686 1_565 ?
Sc1 Sc1 Sc1 122.538(15) 5_676 1_565 ?
Sc1 Sc1 Sc1 180.00(3) 1_545 1_565 ?
O1 Sc1 Ca1 143.51(5) 1_565 6_557 ?
O1 Sc1 Ca1 93.03(5) . 6_557 ?
O1 Sc1 Ca1 130.44(4) 5_676 6_557 ?
O2 Sc1 Ca1 40.34(4) . 6_557 ?
O3 Sc1 Ca1 41.13(4) . 6_557 ?
O3 Sc1 Ca1 86.68(5) 1_565 6_557 ?
Sc1 Sc1 Ca1 165.42(2) 5_686 6_557 ?
Sc1 Sc1 Ca1 117.91(3) 5_676 6_557 ?
Sc1 Sc1 Ca1 62.319(13) 1_545 6_557 ?
Sc1 Sc1 Ca1 117.681(13) 1_565 6_557 ?
O1 Sc1 Ca1 93.03(5) 1_565 6_567 ?
O1 Sc1 Ca1 143.51(5) . 6_567 ?
O1 Sc1 Ca1 130.44(4) 5_676 6_567 ?
O2 Sc1 Ca1 40.34(4) . 6_567 ?
O3 Sc1 Ca1 86.68(5) . 6_567 ?
O3 Sc1 Ca1 41.13(4) 1_565 6_567 ?
Sc1 Sc1 Ca1 117.91(3) 5_686 6_567 ?
Sc1 Sc1 Ca1 165.42(2) 5_676 6_567 ?
Sc1 Sc1 Ca1 117.681(13) 1_545 6_567 ?
Sc1 Sc1 Ca1 62.319(13) 1_565 6_567 ?
Ca1 Sc1 Ca1 55.36(3) 6_557 6_567 ?
O1 Ca1 O4 82.39(6) . . ?
O1 Ca1 O4 82.39(6) . 1_565 ?
O4 Ca1 O4 93.44(7) . 1_565 ?
O1 Ca1 O2 89.10(5) . 6_657 ?
O4 Ca1 O2 170.89(6) . 6_657 ?
O4 Ca1 O2 88.63(5) 1_565 6_657 ?
O1 Ca1 O2 89.10(5) . 6_647 ?
O4 Ca1 O2 88.63(5) . 6_647 ?
O4 Ca1 O2 170.89(6) 1_565 6_647 ?
O2 Ca1 O2 87.98(7) 6_657 6_647 ?
O1 Ca1 O3 154.05(6) . 6_657 ?
O4 Ca1 O3 114.42(6) . 6_657 ?
O4 Ca1 O3 114.42(6) 1_565 6_657 ?
O2 Ca1 O3 72.50(5) 6_657 6_657 ?
O2 Ca1 O3 72.50(5) 6_647 6_657 ?
O1 Ca1 O4 151.42(6) . 5_667 ?
O4 Ca1 O4 78.14(6) . 5_667 ?
O4 Ca1 O4 78.14(6) 1_565 5_667 ?
O2 Ca1 O4 110.97(5) 6_657 5_667 ?
O2 Ca1 O4 110.97(5) 6_647 5_667 ?
O3 Ca1 O4 54.54(6) 6_657 5_667 ?
O1 Ca1 B1 178.79(7) . 5_677 ?
O4 Ca1 B1 96.79(6) . 5_677 ?
O4 Ca1 B1 96.79(6) 1_565 5_677 ?
O2 Ca1 B1 91.77(6) 6_657 5_677 ?
O2 Ca1 B1 91.77(6) 6_647 5_677 ?
O3 Ca1 B1 27.16(7) 6_657 5_677 ?
O4 Ca1 B1 27.38(6) 5_667 5_677 ?
O1 Ca1 Ca1 90.0 . 1_545 ?
O4 Ca1 Ca1 43.28(4) . 1_545 ?
O4 Ca1 Ca1 136.72(4) 1_565 1_545 ?
O2 Ca1 Ca1 133.99(3) 6_657 1_545 ?
O2 Ca1 Ca1 46.01(3) 6_647 1_545 ?
O3 Ca1 Ca1 90.0 6_657 1_545 ?
O4 Ca1 Ca1 90.0 5_667 1_545 ?
B1 Ca1 Ca1 90.0 5_677 1_545 ?
O1 Ca1 Ca1 90.0 . 1_565 ?
O4 Ca1 Ca1 136.72(4) . 1_565 ?
O4 Ca1 Ca1 43.28(4) 1_565 1_565 ?
O2 Ca1 Ca1 46.01(3) 6_657 1_565 ?
O2 Ca1 Ca1 133.99(3) 6_647 1_565 ?
O3 Ca1 Ca1 90.0 6_657 1_565 ?
O4 Ca1 Ca1 90.0 5_667 1_565 ?
B1 Ca1 Ca1 90.0 5_677 1_565 ?
Ca1 Ca1 Ca1 180.0 1_545 1_565 ?
O1 Ca1 Sc1 122.78(4) . 6_657 ?
O4 Ca1 Sc1 151.79(5) . 6_657 ?
O4 Ca1 Sc1 101.82(5) 1_565 6_657 ?
O2 Ca1 Sc1 35.09(4) 6_657 6_657 ?
O2 Ca1 Sc1 80.04(4) 6_647 6_657 ?
O3 Ca1 Sc1 37.49(3) 6_657 6_657 ?
O4 Ca1 Sc1 81.95(4) 5_667 6_657 ?
B1 Ca1 Sc1 58.23(5) 5_677 6_657 ?
Ca1 Ca1 Sc1 117.681(13) 1_545 6_657 ?
Ca1 Ca1 Sc1 62.319(13) 1_565 6_657 ?
O1 Ca1 Sc1 122.78(4) . 6_647 ?
O4 Ca1 Sc1 101.82(5) . 6_647 ?
O4 Ca1 Sc1 151.79(5) 1_565 6_647 ?
O2 Ca1 Sc1 80.04(4) 6_657 6_647 ?
O2 Ca1 Sc1 35.09(4) 6_647 6_647 ?
O3 Ca1 Sc1 37.49(3) 6_657 6_647 ?
O4 Ca1 Sc1 81.95(4) 5_667 6_647 ?
B1 Ca1 Sc1 58.23(5) 5_677 6_647 ?
Ca1 Ca1 Sc1 62.319(13) 1_545 6_647 ?
Ca1 Ca1 Sc1 117.681(13) 1_565 6_647 ?
Sc1 Ca1 Sc1 55.36(3) 6_657 6_647 ?
O4 B1 O3 118.0(2) 1_565 2_575 ?
O4 B1 O2 121.0(2) 1_565 . ?
O3 B1 O2 121.1(2) 2_575 . ?
O4 B1 Ca1 64.55(13) 1_565 5_677 ?
O3 B1 Ca1 53.41(12) 2_575 5_677 ?
O2 B1 Ca1 174.49(18) . 5_677 ?
Sc1 O1 Sc1 107.88(8) 1_545 . ?
Sc1 O1 Sc1 97.24(6) 1_545 5_676 ?
Sc1 O1 Sc1 97.24(6) . 5_676 ?
Sc1 O1 Ca1 113.48(5) 1_545 . ?
Sc1 O1 Ca1 113.48(5) . . ?
Sc1 O1 Ca1 125.05(8) 5_676 . ?
B1 O2 Sc1 108.45(15) . . ?
B1 O2 Ca1 124.05(9) . 6_557 ?
Sc1 O2 Ca1 104.56(6) . 6_557 ?
B1 O2 Ca1 124.05(9) . 6_567 ?
Sc1 O2 Ca1 104.56(6) . 6_567 ?
Ca1 O2 Ca1 87.98(6) 6_557 6_567 ?
B1 O3 Sc1 126.33(7) 2_574 . ?
B1 O3 Sc1 126.33(7) 2_574 1_545 ?
Sc1 O3 Sc1 96.89(7) . 1_545 ?
B1 O3 Ca1 99.43(15) 2_574 6_557 ?
Sc1 O3 Ca1 101.38(6) . 6_557 ?
Sc1 O3 Ca1 101.38(6) 1_545 6_557 ?
B1 O4 Ca1 131.34(6) 1_545 . ?
B1 O4 Ca1 131.34(6) 1_545 1_545 ?
Ca1 O4 Ca1 93.44(7) . 1_545 ?
B1 O4 Ca1 88.08(14) 1_545 5_667 ?
Ca1 O4 Ca1 101.86(6) . 5_667 ?
Ca1 O4 Ca1 101.86(6) 1_545 5_667 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.078
