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


data_x1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B3 Ca4.01 O10 Tb0.99'
_chemical_formula_weight         509.89

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cm

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

_cell_length_a                   8.0715(7)
_cell_length_b                   16.0000(15)
_cell_length_c                   3.5454(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2550(10)
_cell_angle_gamma                90.00
_cell_volume                     449.06(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    718
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.44

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             479
_exptl_absorpt_coefficient_mu    10.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4636
_exptl_absorpt_correction_T_max  0.5384
_exptl_absorpt_process_details   'APEX2 Software Suite (Bruker,2005)'

_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  'Bruker APEX2 CCD area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            1421
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         27.44
_reflns_number_total             718
_reflns_number_gt                717
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0194P)²+3.6467P] 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       0.033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_number_reflns         718
_refine_ls_number_parameters     83
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_restrained_S_all      1.465
_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
Tb1 Tb 0.00003(7) 0.0000 0.00041(7) 0.0071(3) Uani 0.96(2) 2 d SP . .
Tb2 Tb 0.1400(3) 0.38742(13) 0.3192(6) 0.0086(10) Uani 0.043(7) 1 d P . .
Ca1 Ca 0.00003(7) 0.0000 0.00041(7) 0.0071(3) Uani 0.04(2) 2 d SP . .
Ca2 Ca 0.1400(3) 0.38742(13) 0.3192(6) 0.0086(10) Uani 0.957(7) 1 d P . .
Ca3 Ca 0.2589(3) 0.18157(16) 0.6424(7) 0.0096(9) Uani 1 1 d . . .
O1 O 0.821(2) 0.0000 0.409(5) 0.009(4) Uani 1 2 d S . .
O2 O 0.4579(11) -0.0736(5) 0.735(3) 0.010(2) Uani 1 1 d . . .
O3 O 0.192(2) 0.0000 0.594(6) 0.014(4) Uani 1 2 d S . .
O4 O 0.0818(11) 0.1426(6) 0.064(3) 0.010(2) Uani 1 1 d . . .
O5 O 0.9665(13) 0.2688(6) 0.263(3) 0.014(2) Uani 1 1 d . . .
O6 O 0.7876(12) 0.1718(6) -0.130(3) 0.013(2) Uani 1 1 d . . .
B1 B 0.373(3) 0.0000 0.684(6) 0.008(4) Uiso 1 2 d S . .
B2 B 0.9486(19) 0.1945(10) 0.065(5) 0.011(3) Uiso 1 1 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
Tb1 O1 2.239(19) 1_455 ?
Tb1 O1 2.303(19) 1_454 ?
Tb1 O3 2.31(2) 1_554 ?
Tb1 O3 2.360(19) . ?
Tb1 O4 2.373(9) . ?
Tb1 O4 2.373(9) 2 ?
Tb1 Tb1 3.5454(3) 1_556 ?
Tb1 Ca1 3.5454(3) 1_556 ?
Tb1 Tb1 3.5454(3) 1_554 ?
Tb1 Ca1 3.5454(3) 1_554 ?
Tb1 Tb2 3.775(2) 3_445 ?
Tb1 Ca2 3.775(2) 3_445 ?
Tb2 O6 2.287(9) 4_456 ?
Tb2 O1 2.301(12) 3_455 ?
Tb2 O5 2.344(9) 1_455 ?
Tb2 O2 2.359(10) 3_455 ?
Tb2 O6 2.365(10) 4_455 ?
Tb2 O2 2.378(9) 3_454 ?
Tb2 Tb2 3.5454(3) 1_556 ?
Tb2 Ca2 3.5454(3) 1_556 ?
Tb2 Tb2 3.5454(3) 1_554 ?
Tb2 Ca2 3.5454(3) 1_554 ?
Tb2 Ca3 3.557(3) . ?
Tb2 Ca2 3.603(4) 2_565 ?
Ca3 O2 2.338(10) 2 ?
Ca3 O4 2.345(10) 1_556 ?
Ca3 O4 2.345(9) . ?
Ca3 O5 2.475(10) 4_455 ?
Ca3 O6 2.477(9) 4_456 ?
Ca3 O5 2.615(10) 4_456 ?
Ca3 B2 2.760(16) 4_456 ?
Ca3 O5 2.845(11) 1_455 ?
Ca3 B2 2.917(15) 1_455 ?
Ca3 O3 2.953(4) . ?
Ca3 B1 3.043(7) . ?
Ca3 B2 3.166(17) 1_456 ?
O1 Ca1 2.239(19) 1_655 ?
O1 Tb1 2.239(19) 1_655 ?
O1 Ca2 2.301(12) 3_545 ?
O1 Tb2 2.301(12) 3_545 ?
O1 Ca2 2.301(12) 4 ?
O1 Tb2 2.301(12) 4 ?
O1 Tb1 2.303(19) 1_656 ?
O1 Ca1 2.303(19) 1_656 ?
O2 B1 1.356(14) . ?
O2 Ca3 2.338(10) 2 ?
O2 Tb2 2.359(10) 3_545 ?
O2 Ca2 2.359(10) 3_545 ?
O2 Tb2 2.378(9) 3_546 ?
O2 Ca2 2.378(9) 3_546 ?
O3 B1 1.43(3) . ?
O3 Ca1 2.31(2) 1_556 ?
O3 Tb1 2.31(2) 1_556 ?
O3 Ca3 2.953(4) 2 ?
O4 B2 1.360(18) 1_455 ?
O4 Ca3 2.345(10) 1_554 ?
O5 B2 1.373(18) . ?
O5 Ca2 2.344(9) 1_655 ?
O5 Tb2 2.344(9) 1_655 ?
O5 Ca3 2.475(10) 4 ?
O5 Ca3 2.615(10) 4_554 ?
O5 Ca3 2.845(11) 1_655 ?
O6 B2 1.394(17) . ?
O6 Ca2 2.287(9) 4_554 ?
O6 Tb2 2.287(9) 4_554 ?
O6 Ca2 2.365(10) 4 ?
O6 Tb2 2.365(10) 4 ?
O6 Ca3 2.477(9) 4_554 ?
B1 O2 1.356(14) 2 ?
B1 Ca3 3.043(7) 2 ?
B1 Ca2 3.263(18) 4 ?
B1 Ca2 3.263(18) 3_545 ?
B2 O4 1.360(18) 1_655 ?
B2 Ca3 2.760(15) 4_554 ?
B2 Ca3 2.917(15) 1_655 ?
B2 Ca2 3.101(16) 4 ?
B2 Ca1 3.154(15) 1_655 ?
B2 Ca3 3.166(17) 1_654 ?

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 Tb1 O1 102.6(8) 1_455 1_454 ?
O1 Tb1 O3 178.2(9) 1_455 1_554 ?
O1 Tb1 O3 79.2(6) 1_454 1_554 ?
O1 Tb1 O3 79.5(7) 1_455 . ?
O1 Tb1 O3 177.9(9) 1_454 . ?
O3 Tb1 O3 98.7(7) 1_554 . ?
O1 Tb1 O4 98.2(3) 1_455 . ?
O1 Tb1 O4 101.5(2) 1_454 . ?
O3 Tb1 O4 81.4(3) 1_554 . ?
O3 Tb1 O4 78.1(2) . . ?
O1 Tb1 O4 98.2(3) 1_455 2 ?
O1 Tb1 O4 101.5(2) 1_454 2 ?
O3 Tb1 O4 81.4(3) 1_554 2 ?
O3 Tb1 O4 78.1(2) . 2 ?
O4 Tb1 O4 148.0(4) . 2 ?
O1 Tb1 Tb1 39.3(5) 1_455 1_556 ?
O1 Tb1 Tb1 141.9(5) 1_454 1_556 ?
O3 Tb1 Tb1 138.9(5) 1_554 1_556 ?
O3 Tb1 Tb1 40.2(5) . 1_556 ?
O4 Tb1 Tb1 87.7(2) . 1_556 ?
O4 Tb1 Tb1 87.7(2) 2 1_556 ?
O1 Tb1 Ca1 39.3(5) 1_455 1_556 ?
O1 Tb1 Ca1 141.9(5) 1_454 1_556 ?
O3 Tb1 Ca1 138.9(5) 1_554 1_556 ?
O3 Tb1 Ca1 40.2(5) . 1_556 ?
O4 Tb1 Ca1 87.7(2) . 1_556 ?
O4 Tb1 Ca1 87.7(2) 2 1_556 ?
Tb1 Tb1 Ca1 0.000(17) 1_556 1_556 ?
O1 Tb1 Tb1 140.7(5) 1_455 1_554 ?
O1 Tb1 Tb1 38.1(5) 1_454 1_554 ?
O3 Tb1 Tb1 41.1(5) 1_554 1_554 ?
O3 Tb1 Tb1 139.8(5) . 1_554 ?
O4 Tb1 Tb1 92.3(2) . 1_554 ?
O4 Tb1 Tb1 92.3(2) 2 1_554 ?
Tb1 Tb1 Tb1 180.0 1_556 1_554 ?
Ca1 Tb1 Tb1 180.0 1_556 1_554 ?
O1 Tb1 Ca1 140.7(5) 1_455 1_554 ?
O1 Tb1 Ca1 38.1(5) 1_454 1_554 ?
O3 Tb1 Ca1 41.1(5) 1_554 1_554 ?
O3 Tb1 Ca1 139.8(5) . 1_554 ?
O4 Tb1 Ca1 92.3(2) . 1_554 ?
O4 Tb1 Ca1 92.3(2) 2 1_554 ?
Tb1 Tb1 Ca1 180.0 1_556 1_554 ?
Ca1 Tb1 Ca1 180.0 1_556 1_554 ?
Tb1 Tb1 Ca1 0.000(17) 1_554 1_554 ?
O1 Tb1 Tb2 34.3(3) 1_455 3_445 ?
O1 Tb1 Tb2 83.6(4) 1_454 3_445 ?
O3 Tb1 Tb2 146.7(2) 1_554 3_445 ?
O3 Tb1 Tb2 98.3(5) . 3_445 ?
O4 Tb1 Tb2 130.3(2) . 3_445 ?
O4 Tb1 Tb2 74.3(2) 2 3_445 ?
Tb1 Tb1 Tb2 63.28(3) 1_556 3_445 ?
Ca1 Tb1 Tb2 63.28(3) 1_556 3_445 ?
Tb1 Tb1 Tb2 116.72(3) 1_554 3_445 ?
Ca1 Tb1 Tb2 116.72(3) 1_554 3_445 ?
O1 Tb1 Ca2 34.3(3) 1_455 3_445 ?
O1 Tb1 Ca2 83.6(4) 1_454 3_445 ?
O3 Tb1 Ca2 146.7(2) 1_554 3_445 ?
O3 Tb1 Ca2 98.3(5) . 3_445 ?
O4 Tb1 Ca2 130.3(2) . 3_445 ?
O4 Tb1 Ca2 74.3(2) 2 3_445 ?
Tb1 Tb1 Ca2 63.28(3) 1_556 3_445 ?
Ca1 Tb1 Ca2 63.28(3) 1_556 3_445 ?
Tb1 Tb1 Ca2 116.72(3) 1_554 3_445 ?
Ca1 Tb1 Ca2 116.72(3) 1_554 3_445 ?
Tb2 Tb1 Ca2 0.00(6) 3_445 3_445 ?
O6 Tb2 O1 89.7(5) 4_456 3_455 ?
O6 Tb2 O5 86.6(4) 4_456 1_455 ?
O1 Tb2 O5 176.3(5) 3_455 1_455 ?
O6 Tb2 O2 82.0(3) 4_456 3_455 ?
O1 Tb2 O2 99.3(5) 3_455 3_455 ?
O5 Tb2 O2 80.4(3) 1_455 3_455 ?
O6 Tb2 O6 99.3(3) 4_456 4_455 ?
O1 Tb2 O6 91.0(5) 3_455 4_455 ?
O5 Tb2 O6 89.4(3) 1_455 4_455 ?
O2 Tb2 O6 169.6(3) 3_455 4_455 ?
O6 Tb2 O2 169.7(4) 4_456 3_454 ?
O1 Tb2 O2 100.5(5) 3_455 3_454 ?
O5 Tb2 O2 83.2(3) 1_455 3_454 ?
O2 Tb2 O2 96.9(3) 3_455 3_454 ?
O6 Tb2 O2 80.0(3) 4_455 3_454 ?
O6 Tb2 Tb2 41.2(2) 4_456 1_556 ?
O1 Tb2 Tb2 89.1(5) 3_455 1_556 ?
O5 Tb2 Tb2 88.2(2) 1_455 1_556 ?
O2 Tb2 Tb2 41.8(2) 3_455 1_556 ?
O6 Tb2 Tb2 140.5(2) 4_455 1_556 ?
O2 Tb2 Tb2 138.7(2) 3_454 1_556 ?
O6 Tb2 Ca2 41.2(2) 4_456 1_556 ?
O1 Tb2 Ca2 89.1(5) 3_455 1_556 ?
O5 Tb2 Ca2 88.2(2) 1_455 1_556 ?
O2 Tb2 Ca2 41.8(2) 3_455 1_556 ?
O6 Tb2 Ca2 140.5(2) 4_455 1_556 ?
O2 Tb2 Ca2 138.7(2) 3_454 1_556 ?
Tb2 Tb2 Ca2 0.00(10) 1_556 1_556 ?
O6 Tb2 Tb2 138.8(2) 4_456 1_554 ?
O1 Tb2 Tb2 90.9(5) 3_455 1_554 ?
O5 Tb2 Tb2 91.8(2) 1_455 1_554 ?
O2 Tb2 Tb2 138.2(2) 3_455 1_554 ?
O6 Tb2 Tb2 39.5(2) 4_455 1_554 ?
O2 Tb2 Tb2 41.3(2) 3_454 1_554 ?
Tb2 Tb2 Tb2 180.00(14) 1_556 1_554 ?
Ca2 Tb2 Tb2 180.00(14) 1_556 1_554 ?
O6 Tb2 Ca2 138.8(2) 4_456 1_554 ?
O1 Tb2 Ca2 90.9(5) 3_455 1_554 ?
O5 Tb2 Ca2 91.8(2) 1_455 1_554 ?
O2 Tb2 Ca2 138.2(2) 3_455 1_554 ?
O6 Tb2 Ca2 39.5(2) 4_455 1_554 ?
O2 Tb2 Ca2 41.3(2) 3_454 1_554 ?
Tb2 Tb2 Ca2 180.00(14) 1_556 1_554 ?
Ca2 Tb2 Ca2 180.00(14) 1_556 1_554 ?
Tb2 Tb2 Ca2 0.0 1_554 1_554 ?
O6 Tb2 Ca3 43.8(2) 4_456 . ?
O1 Tb2 Ca3 123.8(4) 3_455 . ?
O5 Tb2 Ca3 52.9(3) 1_455 . ?
O2 Tb2 Ca3 101.9(2) 3_455 . ?
O6 Tb2 Ca3 72.9(2) 4_455 . ?
O2 Tb2 Ca3 127.3(2) 3_454 . ?
Tb2 Tb2 Ca3 74.37(5) 1_556 . ?
Ca2 Tb2 Ca3 74.37(5) 1_556 . ?
Tb2 Tb2 Ca3 105.63(5) 1_554 . ?
Ca2 Tb2 Ca3 105.63(5) 1_554 . ?
O6 Tb2 Ca2 114.5(2) 4_456 2_565 ?
O1 Tb2 Ca2 38.5(4) 3_455 2_565 ?
O5 Tb2 Ca2 144.1(3) 1_455 2_565 ?
O2 Tb2 Ca2 74.7(2) 3_455 2_565 ?
O6 Tb2 Ca2 113.6(2) 4_455 2_565 ?
O2 Tb2 Ca2 74.8(2) 3_454 2_565 ?
Tb2 Tb2 Ca2 90.0 1_556 2_565 ?
Ca2 Tb2 Ca2 90.0 1_556 2_565 ?
Tb2 Tb2 Ca2 90.0 1_554 2_565 ?
Ca2 Tb2 Ca2 90.0 1_554 2_565 ?
Ca3 Tb2 Ca2 157.81(5) . 2_565 ?
O2 Ca3 O4 101.6(3) 2 1_556 ?
O2 Ca3 O4 102.2(3) 2 . ?
O4 Ca3 O4 98.2(4) 1_556 . ?
O2 Ca3 O5 78.1(3) 2 4_455 ?
O4 Ca3 O5 173.3(3) 1_556 4_455 ?
O4 Ca3 O5 88.4(3) . 4_455 ?
O2 Ca3 O6 129.5(3) 2 4_456 ?
O4 Ca3 O6 94.2(3) 1_556 4_456 ?
O4 Ca3 O6 122.7(3) . 4_456 ?
O5 Ca3 O6 81.0(3) 4_455 4_456 ?
O2 Ca3 O5 78.3(3) 2 4_456 ?
O4 Ca3 O5 85.1(3) 1_556 4_456 ?
O4 Ca3 O5 176.4(3) . 4_456 ?
O5 Ca3 O5 88.3(3) 4_455 4_456 ?
O6 Ca3 O5 55.5(3) 4_456 4_456 ?
O2 Ca3 B2 99.3(4) 2 4_456 ?
O4 Ca3 B2 100.8(4) 1_556 4_456 ?
O4 Ca3 B2 147.6(4) . 4_456 ?
O5 Ca3 B2 72.7(4) 4_455 4_456 ?
O6 Ca3 B2 30.3(4) 4_456 4_456 ?
O5 Ca3 B2 29.4(4) 4_456 4_456 ?
O2 Ca3 O5 155.9(3) 2 1_455 ?
O4 Ca3 O5 83.0(3) 1_556 1_455 ?
O4 Ca3 O5 53.7(3) . 1_455 ?
O5 Ca3 O5 99.9(3) 4_455 1_455 ?
O6 Ca3 O5 72.9(3) 4_456 1_455 ?
O5 Ca3 O5 125.8(2) 4_456 1_455 ?
B2 Ca3 O5 103.0(4) 4_456 1_455 ?
O2 Ca3 B2 128.5(4) 2 1_455 ?
O4 Ca3 B2 85.4(4) 1_556 1_455 ?
O4 Ca3 B2 27.3(4) . 1_455 ?
O5 Ca3 B2 100.1(4) 4_455 1_455 ?
O6 Ca3 B2 100.1(4) 4_456 1_455 ?
O5 Ca3 B2 152.9(4) 4_456 1_455 ?
B2 Ca3 B2 129.7(2) 4_456 1_455 ?
O5 Ca3 B2 27.5(4) 1_455 1_455 ?
O2 Ca3 O3 52.6(4) 2 . ?
O4 Ca3 O3 69.4(5) 1_556 . ?
O4 Ca3 O3 67.3(4) . . ?
O5 Ca3 O3 114.8(5) 4_455 . ?
O6 Ca3 O3 162.7(5) 4_456 . ?
O5 Ca3 O3 115.3(4) 4_456 . ?
B2 Ca3 O3 144.4(5) 4_456 . ?
O5 Ca3 O3 109.3(4) 1_455 . ?
B2 Ca3 O3 84.7(5) 1_455 . ?
O2 Ca3 B1 25.1(4) 2 . ?
O4 Ca3 B1 86.1(5) 1_556 . ?
O4 Ca3 B1 85.2(4) . . ?
O5 Ca3 B1 95.9(5) 4_455 . ?
O6 Ca3 B1 151.7(4) 4_456 . ?
O5 Ca3 B1 96.4(4) 4_456 . ?
B2 Ca3 B1 121.9(5) 4_456 . ?
O5 Ca3 B1 135.0(4) 1_455 . ?
B2 Ca3 B1 108.2(5) 1_455 . ?
O3 Ca3 B1 27.6(5) . . ?
O2 Ca3 B2 124.6(4) 2 1_456 ?
O4 Ca3 B2 22.9(4) 1_556 1_456 ?
O4 Ca3 B2 91.6(4) . 1_456 ?
O5 Ca3 B2 156.6(4) 4_455 1_456 ?
O6 Ca3 B2 79.4(4) 4_456 1_456 ?
O5 Ca3 B2 91.1(4) 4_456 1_456 ?
B2 Ca3 B2 95.9(4) 4_456 1_456 ?
O5 Ca3 B2 62.1(3) 1_455 1_456 ?
B2 Ca3 B2 71.2(4) 1_455 1_456 ?
O3 Ca3 B2 86.5(5) . 1_456 ?
B1 Ca3 B2 107.4(5) . 1_456 ?
Ca1 O1 Tb1 0.00(2) 1_655 1_655 ?
Ca1 O1 Ca2 112.5(6) 1_655 3_545 ?
Tb1 O1 Ca2 112.5(6) 1_655 3_545 ?
Ca1 O1 Tb2 112.5(6) 1_655 3_545 ?
Tb1 O1 Tb2 112.5(6) 1_655 3_545 ?
Ca2 O1 Tb2 0.00(7) 3_545 3_545 ?
Ca1 O1 Ca2 112.5(6) 1_655 4 ?
Tb1 O1 Ca2 112.5(6) 1_655 4 ?
Ca2 O1 Ca2 103.1(8) 3_545 4 ?
Tb2 O1 Ca2 103.1(8) 3_545 4 ?
Ca1 O1 Tb2 112.5(6) 1_655 4 ?
Tb1 O1 Tb2 112.5(6) 1_655 4 ?
Ca2 O1 Tb2 103.1(8) 3_545 4 ?
Tb2 O1 Tb2 103.1(8) 3_545 4 ?
Ca2 O1 Tb2 0.00(15) 4 4 ?
Ca1 O1 Tb1 102.6(8) 1_655 1_656 ?
Tb1 O1 Tb1 102.6(8) 1_655 1_656 ?
Ca2 O1 Tb1 113.3(6) 3_545 1_656 ?
Tb2 O1 Tb1 113.3(6) 3_545 1_656 ?
Ca2 O1 Tb1 113.3(6) 4 1_656 ?
Tb2 O1 Tb1 113.3(6) 4 1_656 ?
Ca1 O1 Ca1 102.6(8) 1_655 1_656 ?
Tb1 O1 Ca1 102.6(8) 1_655 1_656 ?
Ca2 O1 Ca1 113.3(6) 3_545 1_656 ?
Tb2 O1 Ca1 113.3(6) 3_545 1_656 ?
Ca2 O1 Ca1 113.3(6) 4 1_656 ?
Tb2 O1 Ca1 113.3(6) 4 1_656 ?
Tb1 O1 Ca1 0.0 1_656 1_656 ?
B1 O2 Ca3 108.0(10) . 2 ?
B1 O2 Tb2 120.5(11) . 3_545 ?
Ca3 O2 Tb2 102.2(4) 2 3_545 ?
B1 O2 Ca2 120.5(11) . 3_545 ?
Ca3 O2 Ca2 102.2(4) 2 3_545 ?
Tb2 O2 Ca2 0.00(15) 3_545 3_545 ?
B1 O2 Tb2 123.6(10) . 3_546 ?
Ca3 O2 Tb2 102.6(4) 2 3_546 ?
Tb2 O2 Tb2 96.9(3) 3_545 3_546 ?
Ca2 O2 Tb2 96.9(3) 3_545 3_546 ?
B1 O2 Ca2 123.6(10) . 3_546 ?
Ca3 O2 Ca2 102.6(4) 2 3_546 ?
Tb2 O2 Ca2 96.9(3) 3_545 3_546 ?
Ca2 O2 Ca2 96.9(3) 3_545 3_546 ?
Tb2 O2 Ca2 0.00(12) 3_546 3_546 ?
B1 O3 Ca1 129.8(15) . 1_556 ?
B1 O3 Tb1 129.8(15) . 1_556 ?
Ca1 O3 Tb1 0.000(17) 1_556 1_556 ?
B1 O3 Tb1 131.5(16) . . ?
Ca1 O3 Tb1 98.7(7) 1_556 . ?
Tb1 O3 Tb1 98.7(7) 1_556 . ?
B1 O3 Ca3 79.7(4) . . ?
Ca1 O3 Ca3 95.8(4) 1_556 . ?
Tb1 O3 Ca3 95.8(4) 1_556 . ?
Tb1 O3 Ca3 97.6(4) . . ?
B1 O3 Ca3 79.7(4) . 2 ?
Ca1 O3 Ca3 95.8(4) 1_556 2 ?
Tb1 O3 Ca3 95.8(4) 1_556 2 ?
Tb1 O3 Ca3 97.6(4) . 2 ?
Ca3 O3 Ca3 159.3(7) . 2 ?
B2 O4 Ca3 114.8(9) 1_455 1_554 ?
B2 O4 Ca3 100.5(8) 1_455 . ?
Ca3 O4 Ca3 98.2(4) 1_554 . ?
B2 O4 Tb1 112.5(8) 1_455 . ?
Ca3 O4 Tb1 112.9(4) 1_554 . ?
Ca3 O4 Tb1 116.7(4) . . ?
B2 O5 Ca2 138.2(9) . 1_655 ?
B2 O5 Tb2 138.2(9) . 1_655 ?
Ca2 O5 Tb2 0.00(12) 1_655 1_655 ?
B2 O5 Ca3 122.7(8) . 4 ?
Ca2 O5 Ca3 98.6(4) 1_655 4 ?
Tb2 O5 Ca3 98.6(4) 1_655 4 ?
B2 O5 Ca3 81.2(8) . 4_554 ?
Ca2 O5 Ca3 95.7(3) 1_655 4_554 ?
Tb2 O5 Ca3 95.7(3) 1_655 4_554 ?
Ca3 O5 Ca3 88.3(3) 4 4_554 ?
B2 O5 Ca3 79.2(8) . 1_655 ?
Ca2 O5 Ca3 86.0(3) 1_655 1_655 ?
Tb2 O5 Ca3 86.0(3) 1_655 1_655 ?
Ca3 O5 Ca3 119.2(4) 4 1_655 ?
Ca3 O5 Ca3 152.0(4) 4_554 1_655 ?
B2 O6 Ca2 144.1(9) . 4_554 ?
B2 O6 Tb2 144.1(9) . 4_554 ?
Ca2 O6 Tb2 0.00(17) 4_554 4_554 ?
B2 O6 Ca2 108.4(9) . 4 ?
Ca2 O6 Ca2 99.3(3) 4_554 4 ?
Tb2 O6 Ca2 99.3(3) 4_554 4 ?
B2 O6 Tb2 108.4(9) . 4 ?
Ca2 O6 Tb2 99.3(3) 4_554 4 ?
Tb2 O6 Tb2 99.3(3) 4_554 4 ?
Ca2 O6 Tb2 0.00(13) 4 4 ?
B2 O6 Ca3 86.2(8) . 4_554 ?
Ca2 O6 Ca3 96.5(3) 4_554 4_554 ?
Tb2 O6 Ca3 96.5(3) 4_554 4_554 ?
Ca2 O6 Ca3 124.9(4) 4 4_554 ?
Tb2 O6 Ca3 124.9(4) 4 4_554 ?
O2 B1 O2 120.5(18) 2 . ?
O2 B1 O3 119.7(9) 2 . ?
O2 B1 O3 119.7(9) . . ?
O2 B1 Ca3 167.4(12) 2 2 ?
O2 B1 Ca3 47.0(6) . 2 ?
O3 B1 Ca3 72.7(4) . 2 ?
O2 B1 Ca3 47.0(6) 2 . ?
O2 B1 Ca3 167.4(12) . . ?
O3 B1 Ca3 72.7(4) . . ?
Ca3 B1 Ca3 145.4(8) 2 . ?
O2 B1 Ca2 38.5(8) 2 4 ?
O2 B1 Ca2 100.2(12) . 4 ?
O3 B1 Ca2 129.4(10) . 4 ?
Ca3 B1 Ca2 136.5(6) 2 4 ?
Ca3 B1 Ca2 70.8(2) . 4 ?
O2 B1 Ca2 100.2(12) 2 3_545 ?
O2 B1 Ca2 38.5(8) . 3_545 ?
O3 B1 Ca2 129.4(10) . 3_545 ?
Ca3 B1 Ca2 70.8(2) 2 3_545 ?
Ca3 B1 Ca2 136.5(6) . 3_545 ?
Ca2 B1 Ca2 67.0(4) 4 3_545 ?
O4 B2 O5 121.7(12) 1_655 . ?
O4 B2 O6 120.0(13) 1_655 . ?
O5 B2 O6 118.2(13) . . ?
O4 B2 Ca3 142.4(11) 1_655 4_554 ?
O5 B2 Ca3 69.4(8) . 4_554 ?
O6 B2 Ca3 63.6(7) . 4_554 ?
O4 B2 Ca3 52.2(6) 1_655 1_655 ?
O5 B2 Ca3 73.3(7) . 1_655 ?
O6 B2 Ca3 156.6(10) . 1_655 ?
Ca3 B2 Ca3 137.8(6) 4_554 1_655 ?
O4 B2 Ca2 115.0(9) 1_655 4 ?
O5 B2 Ca2 103.1(9) . 4 ?
O6 B2 Ca2 46.4(7) . 4 ?
Ca3 B2 Ca2 94.0(5) 4_554 4 ?
Ca3 B2 Ca2 113.2(5) 1_655 4 ?
O4 B2 Ca1 44.0(6) 1_655 1_655 ?
O5 B2 Ca1 152.7(10) . 1_655 ?
O6 B2 Ca1 80.2(8) . 1_655 ?
Ca3 B2 Ca1 137.4(6) 4_554 1_655 ?
Ca3 B2 Ca1 82.7(4) 1_655 1_655 ?
Ca2 B2 Ca1 74.2(3) 4 1_655 ?
O4 B2 Ca3 42.2(7) 1_655 1_654 ?
O5 B2 Ca3 106.5(9) . 1_654 ?
O6 B2 Ca3 119.7(10) . 1_654 ?
Ca3 B2 Ca3 101.3(5) 4_554 1_654 ?
Ca3 B2 Ca3 71.2(4) 1_655 1_654 ?
Ca2 B2 Ca3 149.8(5) 4 1_654 ?
Ca1 B2 Ca3 76.9(4) 1_655 1_654 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.386
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.220
_database_code_depnum_ccdc_archive 'CCDC 985948'
