# 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 1560585'
_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B3 Cd5 Cl O9'
_chemical_formula_weight         773.88

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'
Cl Cl 0.1484 0.1585 '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           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                   8.172(5)
_cell_length_b                   16.061(9)
_cell_length_c                   3.4741(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.294(8)
_cell_angle_gamma                90.00
_cell_volume                     450.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    671
_cell_measurement_theta_min      2.8621
_cell_measurement_theta_max      27.4934

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.0500
_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    11.951
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9331
_exptl_absorpt_process_details   ?

_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 Smart APEX II CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1487
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         28.29
_reflns_number_total             883
_reflns_number_gt                878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 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)+(0.0189P)²+0.0000P] 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       0.0061(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   0.00
_refine_ls_number_reflns         883
_refine_ls_number_parameters     89
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0145
_refine_ls_wR_factor_ref         0.0340
_refine_ls_wR_factor_gt          0.0339
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.087
_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 0.36140(4) 0.37188(2) 0.56920(8) 0.00921(10) Uani 1 1 d . . .
Cd2 Cd 0.48670(5) 0.17561(2) 0.91154(9) 0.01040(10) Uani 1 1 d . . .
Cd3 Cd 0.78934(7) 0.5000 0.31388(14) 0.01098(12) Uani 1 2 d S . .
Cl4 Cl 0.5512(2) 0.5000 0.7082(5) 0.0112(3) Uani 1 2 d S . .
O5 O 0.2009(5) 0.4244(2) 1.0207(11) 0.0132(8) Uani 1 1 d . . .
O4 O 0.4510(7) 0.0000 0.8758(17) 0.0232(15) Uani 1 2 d S . .
O1 O 0.8091(5) 0.6476(2) 0.3494(12) 0.0107(7) Uani 1 1 d . . .
O2 O 0.5163(5) 0.3204(2) 0.1258(12) 0.0124(8) Uani 1 1 d . . .
O3 O 0.1811(5) 0.2717(2) 0.5448(13) 0.0185(9) Uani 1 1 d . . .
B1 B 0.6225(9) 0.0000 0.978(2) 0.0059(14) Uani 1 2 d S . .
B2 B 0.1687(7) 0.1988(4) 0.3378(16) 0.0087(10) Uani 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
Cd1 O3 2.174(4) . ?
Cd1 O2 2.288(4) 1_556 ?
Cd1 O5 2.292(4) 1_554 ?
Cd1 O2 2.300(4) . ?
Cd1 O5 2.357(4) . ?
Cd1 Cl4 2.5751(15) . ?
Cd1 Cd2 3.4651(17) . ?
Cd1 Cd1 3.4741(19) 1_554 ?
Cd1 Cd1 3.4741(19) 1_556 ?
Cd2 O1 2.282(4) 3_445 ?
Cd2 O1 2.310(4) 3_446 ?
Cd2 O3 2.349(4) 4 ?
Cd2 O5 2.360(4) 4 ?
Cd2 O2 2.442(4) 1_556 ?
Cd2 O3 2.637(5) 4_556 ?
Cd2 B2 2.787(6) 4_556 ?
Cd2 Cd2 3.4741(19) 1_554 ?
Cd2 Cd2 3.4741(19) 1_556 ?
Cd3 O4 2.171(5) 3_554 ?
Cd3 O4 2.174(6) 3 ?
Cd3 O1 2.377(4) . ?
Cd3 O1 2.377(4) 2_565 ?
Cd3 Cl4 2.555(2) . ?
Cd3 Cl4 2.625(2) 1_554 ?
Cd3 Cd3 3.4741(19) 1_554 ?
Cd3 Cd3 3.4741(19) 1_556 ?
Cl4 Cd1 2.5751(15) 2_565 ?
Cl4 Cd3 2.625(2) 1_556 ?
O5 B1 1.370(5) 3_455 ?
O5 Cd1 2.292(4) 1_556 ?
O5 Cd2 2.360(4) 4_455 ?
O4 B1 1.388(9) . ?
O4 Cd3 2.171(5) 3_446 ?
O4 Cd3 2.174(6) 3_445 ?
O1 B2 1.406(7) 3 ?
O1 Cd2 2.282(4) 3 ?
O1 Cd2 2.310(4) 3_554 ?
O2 B2 1.375(7) 4 ?
O2 Cd1 2.288(4) 1_554 ?
O2 Cd2 2.442(4) 1_554 ?
O3 B2 1.370(7) . ?
O3 Cd2 2.349(4) 4_455 ?
O3 Cd2 2.637(5) 4_454 ?
B1 O5 1.370(5) 4 ?
B1 O5 1.370(5) 3_545 ?
B2 O2 1.375(7) 4_455 ?
B2 O1 1.406(7) 3_445 ?
B2 Cd2 2.787(6) 4_454 ?

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 Cd1 O2 92.55(16) . 1_556 ?
O3 Cd1 O5 86.93(15) . 1_554 ?
O2 Cd1 O5 178.50(15) 1_556 1_554 ?
O3 Cd1 O2 98.67(14) . . ?
O2 Cd1 O2 98.45(15) 1_556 . ?
O5 Cd1 O2 83.02(14) 1_554 . ?
O3 Cd1 O5 81.02(14) . . ?
O2 Cd1 O5 81.85(14) 1_556 . ?
O5 Cd1 O5 96.68(15) 1_554 . ?
O2 Cd1 O5 179.58(15) . . ?
O3 Cd1 Cl4 169.28(11) . . ?
O2 Cd1 Cl4 84.03(10) 1_556 . ?
O5 Cd1 Cl4 96.24(10) 1_554 . ?
O2 Cd1 Cl4 91.89(10) . . ?
O5 Cd1 Cl4 88.43(11) . . ?
O3 Cd1 Cd2 60.06(12) . . ?
O2 Cd1 Cd2 44.65(9) 1_556 . ?
O5 Cd1 Cd2 135.85(9) 1_554 . ?
O2 Cd1 Cd2 74.85(10) . . ?
O5 Cd1 Cd2 105.20(9) . . ?
Cl4 Cd1 Cd2 121.80(5) . . ?
O3 Cd1 Cd1 94.04(11) . 1_554 ?
O2 Cd1 Cd1 139.10(10) 1_556 1_554 ?
O5 Cd1 Cd1 42.37(9) 1_554 1_554 ?
O2 Cd1 Cd1 40.65(10) . 1_554 ?
O5 Cd1 Cd1 139.05(10) . 1_554 ?
Cl4 Cd1 Cd1 95.18(4) . 1_554 ?
Cd2 Cd1 Cd1 107.188(15) . 1_554 ?
O3 Cd1 Cd1 85.96(11) . 1_556 ?
O2 Cd1 Cd1 40.90(10) 1_556 1_556 ?
O5 Cd1 Cd1 137.63(9) 1_554 1_556 ?
O2 Cd1 Cd1 139.35(10) . 1_556 ?
O5 Cd1 Cd1 40.95(10) . 1_556 ?
Cl4 Cd1 Cd1 84.82(4) . 1_556 ?
Cd2 Cd1 Cd1 72.813(16) . 1_556 ?
Cd1 Cd1 Cd1 180.00(3) 1_554 1_556 ?
O1 Cd2 O1 98.30(16) 3_445 3_446 ?
O1 Cd2 O3 89.97(16) 3_445 4 ?
O1 Cd2 O3 168.34(14) 3_446 4 ?
O1 Cd2 O5 110.86(13) 3_445 4 ?
O1 Cd2 O5 106.86(14) 3_446 4 ?
O3 Cd2 O5 77.49(13) 4 4 ?
O1 Cd2 O2 117.83(14) 3_445 1_556 ?
O1 Cd2 O2 91.53(13) 3_446 1_556 ?
O3 Cd2 O2 77.28(13) 4 1_556 ?
O5 Cd2 O2 124.37(13) 4 1_556 ?
O1 Cd2 O3 172.60(13) 3_445 4_556 ?
O1 Cd2 O3 82.60(14) 3_446 4_556 ?
O3 Cd2 O3 88.16(14) 4 4_556 ?
O5 Cd2 O3 75.70(12) 4 4_556 ?
O2 Cd2 O3 54.78(12) 1_556 4_556 ?
O1 Cd2 B2 143.98(15) 3_445 4_556 ?
O1 Cd2 B2 97.44(14) 3_446 4_556 ?
O3 Cd2 B2 71.19(15) 4 4_556 ?
O5 Cd2 B2 95.10(15) 4 4_556 ?
O2 Cd2 B2 29.57(15) 1_556 4_556 ?
O3 Cd2 B2 29.10(14) 4_556 4_556 ?
O1 Cd2 Cd1 76.94(10) 3_445 . ?
O1 Cd2 Cd1 102.77(10) 3_446 . ?
O3 Cd2 Cd1 70.99(9) 4 . ?
O5 Cd2 Cd1 147.61(9) 4 . ?
O2 Cd2 Cd1 41.19(9) 1_556 . ?
O3 Cd2 Cd1 95.69(8) 4_556 . ?
B2 Cd2 Cd1 68.06(13) 4_556 . ?
O1 Cd2 Cd2 41.15(10) 3_445 1_554 ?
O1 Cd2 Cd2 139.45(11) 3_446 1_554 ?
O3 Cd2 Cd2 49.33(11) 4 1_554 ?
O5 Cd2 Cd2 92.35(9) 4 1_554 ?
O2 Cd2 Cd2 106.79(9) 1_556 1_554 ?
O3 Cd2 Cd2 137.49(8) 4_556 1_554 ?
B2 Cd2 Cd2 116.43(11) 4_556 1_554 ?
Cd1 Cd2 Cd2 72.812(16) . 1_554 ?
O1 Cd2 Cd2 138.85(10) 3_445 1_556 ?
O1 Cd2 Cd2 40.55(11) 3_446 1_556 ?
O3 Cd2 Cd2 130.67(11) 4 1_556 ?
O5 Cd2 Cd2 87.65(9) 4 1_556 ?
O2 Cd2 Cd2 73.21(9) 1_556 1_556 ?
O3 Cd2 Cd2 42.51(8) 4_556 1_556 ?
B2 Cd2 Cd2 63.57(11) 4_556 1_556 ?
Cd1 Cd2 Cd2 107.188(16) . 1_556 ?
Cd2 Cd2 Cd2 180.00(3) 1_554 1_556 ?
O4 Cd3 O4 106.2(2) 3_554 3 ?
O4 Cd3 O1 89.57(9) 3_554 . ?
O4 Cd3 O1 85.82(11) 3 . ?
O4 Cd3 O1 89.57(9) 3_554 2_565 ?
O4 Cd3 O1 85.82(11) 3 2_565 ?
O1 Cd3 O1 171.0(2) . 2_565 ?
O4 Cd3 Cl4 168.18(16) 3_554 . ?
O4 Cd3 Cl4 85.62(15) 3 . ?
O1 Cd3 Cl4 91.33(9) . . ?
O1 Cd3 Cl4 91.33(9) 2_565 . ?
O4 Cd3 Cl4 83.95(16) 3_554 1_554 ?
O4 Cd3 Cl4 169.85(14) 3 1_554 ?
O1 Cd3 Cl4 94.41(10) . 1_554 ?
O1 Cd3 Cl4 94.41(11) 2_565 1_554 ?
Cl4 Cd3 Cl4 84.23(7) . 1_554 ?
O4 Cd3 Cd3 36.93(15) 3_554 1_554 ?
O4 Cd3 Cd3 143.13(14) 3 1_554 ?
O1 Cd3 Cd3 92.35(10) . 1_554 ?
O1 Cd3 Cd3 92.35(10) 2_565 1_554 ?
Cl4 Cd3 Cd3 131.25(5) . 1_554 ?
Cl4 Cd3 Cd3 47.02(5) 1_554 1_554 ?
O4 Cd3 Cd3 143.07(15) 3_554 1_556 ?
O4 Cd3 Cd3 36.87(14) 3 1_556 ?
O1 Cd3 Cd3 87.65(10) . 1_556 ?
O1 Cd3 Cd3 87.65(10) 2_565 1_556 ?
Cl4 Cd3 Cd3 48.75(5) . 1_556 ?
Cl4 Cd3 Cd3 132.98(5) 1_554 1_556 ?
Cd3 Cd3 Cd3 180.00(4) 1_554 1_556 ?
Cd3 Cl4 Cd1 112.79(5) . . ?
Cd3 Cl4 Cd1 112.79(5) . 2_565 ?
Cd1 Cl4 Cd1 106.08(8) . 2_565 ?
Cd3 Cl4 Cd3 84.23(7) . 1_556 ?
Cd1 Cl4 Cd3 119.76(5) . 1_556 ?
Cd1 Cl4 Cd3 119.76(5) 2_565 1_556 ?
B1 O5 Cd1 127.7(4) 3_455 1_556 ?
B1 O5 Cd1 123.0(4) 3_455 . ?
Cd1 O5 Cd1 96.68(15) 1_556 . ?
B1 O5 Cd2 105.3(4) 3_455 4_455 ?
Cd1 O5 Cd2 101.16(14) 1_556 4_455 ?
Cd1 O5 Cd2 97.34(14) . 4_455 ?
B1 O4 Cd3 121.7(5) . 3_446 ?
B1 O4 Cd3 132.1(5) . 3_445 ?
Cd3 O4 Cd3 106.2(2) 3_446 3_445 ?
B2 O1 Cd2 108.2(3) 3 3 ?
B2 O1 Cd2 117.6(3) 3 3_554 ?
Cd2 O1 Cd2 98.30(15) 3 3_554 ?
B2 O1 Cd3 122.2(3) 3 . ?
Cd2 O1 Cd3 105.64(16) 3 . ?
Cd2 O1 Cd3 101.81(14) 3_554 . ?
B2 O2 Cd1 149.6(3) 4 1_554 ?
B2 O2 Cd1 105.7(3) 4 . ?
Cd1 O2 Cd1 98.45(15) 1_554 . ?
B2 O2 Cd2 89.2(3) 4 1_554 ?
Cd1 O2 Cd2 94.16(14) 1_554 1_554 ?
Cd1 O2 Cd2 120.57(16) . 1_554 ?
B2 O3 Cd1 130.2(3) . . ?
B2 O3 Cd2 126.4(3) . 4_455 ?
Cd1 O3 Cd2 103.05(14) . 4_455 ?
B2 O3 Cd2 81.5(3) . 4_454 ?
Cd1 O3 Cd2 96.21(15) . 4_454 ?
Cd2 O3 Cd2 88.16(14) 4_455 4_454 ?
O5 B1 O5 124.9(7) 4 3_545 ?
O5 B1 O4 117.6(3) 4 . ?
O5 B1 O4 117.6(3) 3_545 . ?
O3 B2 O2 117.1(5) . 4_455 ?
O3 B2 O1 119.6(5) . 3_445 ?
O2 B2 O1 123.3(5) 4_455 3_445 ?
O3 B2 Cd2 69.4(3) . 4_454 ?
O2 B2 Cd2 61.2(3) 4_455 4_454 ?
O1 B2 Cd2 143.3(3) 3_445 4_454 ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.157
