# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2014

####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1014612'
_audit_update_record             
;
2014-10-17 deposited with the CCDC.
2014-12-26 downloaded from the CCDC.
;
_audit_creation_date             2014-10-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'B6 Bi3 H3 O15'
_chemical_formula_sum            'C0 H3 B6 Bi3 O15'
_chemical_formula_weight         934.82
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Bi Bi -4.1077 10.2566 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_H-M_alt        'P 31'
_space_group_name_Hall           'P 31'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   6.62214(10)
_cell_length_b                   6.62214(10)
_cell_length_c                   6.65264(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     252.652(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    52.218
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    6.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             402
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            546
_diffrn_reflns_point_group_measured_fraction_full 0.604
_diffrn_reflns_point_group_measured_fraction_max 0.505
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.995
_diffrn_reflns_theta_min         3.553
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.173
_reflns_Friedel_fraction_full    0.211
_reflns_Friedel_fraction_max     0.149
_reflns_number_gt                428
_reflns_number_total             448
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         3.151
_refine_diff_density_min         -3.026
_refine_diff_density_rms         0.719
_refine_ls_abs_structure_details 
;
 Flack x determined using 64 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         448
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0461P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0934
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(O1) = Uiso(O2) = Uiso(O3) = Uiso(O4)
3. Others
 Fixed X: H(0.204519)
 Fixed Y: H(0.615221)
 Fixed Z: H(0.518291)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.4654(2) 1.0395(2) -0.5020(8) 0.0018(3) Uani 1 1 d . . . . .
O1 O 0.652(4) 0.811(4) -0.472(4) 0.004(3) Uiso 1 1 d . . . . .
O2 O 0.342(4) 0.148(4) -0.895(3) 0.004(3) Uiso 1 1 d . . . . .
O3 O 0.589(4) 1.433(4) -0.529(3) 0.004(3) Uiso 1 1 d . . . . .
O4 O 1.076(4) 1.038(4) -0.389(3) 0.004(3) Uiso 1 1 d . . . . .
B2 B 0.609(7) 0.603(6) -0.363(5) 0.001(7) Uiso 1 1 d . . . . .
O5 O 0.384(4) 0.490(4) -0.260(3) 0.000(5) Uiso 1 1 d . . . . .
H H 0.2045 0.6152 0.5183 0.000 Uiso 1 1 d R . . . .
B1 B 0.882(9) 0.989(9) -0.531(7) 0.022(11) 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
Bi1 O1 2.39(2) . ?
Bi1 O2 2.27(2) 2_665 ?
Bi1 O3 2.31(2) . ?
Bi1 O3 2.16(2) 2_775 ?
Bi1 O4 2.68(2) 1_455 ?
Bi1 O5 2.69(2) 3_564 ?
O1 B2 1.45(4) . ?
O1 B1 1.44(6) . ?
O2 Bi1 2.27(2) 3_564 ?
O2 B2 1.47(4) 2_654 ?
O2 B1 1.48(6) 3_564 ?
O3 Bi1 2.16(2) 3_574 ?
O3 B2 1.54(4) 1_565 ?
O4 Bi1 2.68(2) 1_655 ?
O4 B1 1.52(5) 2_765 ?
O4 B1 1.50(6) . ?
B2 O2 1.47(4) 3_665 ?
B2 O3 1.54(4) 1_545 ?
B2 O5 1.46(4) . ?
O5 Bi1 2.69(2) 2_665 ?
B1 O2 1.48(6) 2_665 ?
B1 O4 1.52(5) 3_674 ?

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 Bi1 O4 140.7(8) . 1_455 ?
O1 Bi1 O5 80.1(7) . 3_564 ?
O2 Bi1 O1 58.4(9) 2_665 . ?
O2 Bi1 O3 78.1(8) 2_665 . ?
O2 Bi1 O4 156.6(8) 2_665 1_455 ?
O2 Bi1 O5 130.0(8) 2_665 3_564 ?
O3 Bi1 O1 88.9(9) 2_775 . ?
O3 Bi1 O1 135.5(8) . . ?
O3 Bi1 O2 85.6(8) 2_775 2_665 ?
O3 Bi1 O3 78.4(8) 2_775 . ?
O3 Bi1 O4 82.1(8) 2_775 1_455 ?
O3 Bi1 O4 80.0(8) . 1_455 ?
O3 Bi1 O5 142.0(7) . 3_564 ?
O3 Bi1 O5 122.7(8) 2_775 3_564 ?
O4 Bi1 O5 73.2(7) 1_455 3_564 ?
B2 O1 Bi1 136(2) . . ?
B1 O1 Bi1 97(2) . . ?
B1 O1 B2 123(3) . . ?
B2 O2 Bi1 126(2) 2_654 3_564 ?
B2 O2 B1 125(3) 2_654 3_564 ?
B1 O2 Bi1 102(2) 3_564 3_564 ?
Bi1 O3 Bi1 112.2(10) 3_574 . ?
B2 O3 Bi1 116.5(18) 1_565 3_574 ?
B2 O3 Bi1 128.6(18) 1_565 . ?
B1 O4 Bi1 102(2) 2_765 1_655 ?
B1 O4 Bi1 123(2) . 1_655 ?
B1 O4 B1 116.8(18) . 2_765 ?
O1 B2 O2 110(3) . 3_665 ?
O1 B2 O3 104(2) . 1_545 ?
O1 B2 O5 113(3) . . ?
O2 B2 O3 111(3) 3_665 1_545 ?
O5 B2 O2 113(2) . 3_665 ?
O5 B2 O3 106(3) . 1_545 ?
B2 O5 Bi1 154.4(19) . 2_665 ?
O1 B1 O2 103(3) . 2_665 ?
O1 B1 O4 112(4) . 3_674 ?
O1 B1 O4 117(4) . . ?
O2 B1 O4 113(3) 2_665 . ?
O2 B1 O4 112(3) 2_665 3_674 ?
O4 B1 O4 102(3) . 3_674 ?

_olex2_submission_special_instructions 'No special instructions were received'
