 
data_1
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C2 H19 B12 K6 Na O29' 
_chemical_formula_weight          894.48

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'
 'B'  'B'   0.0010   0.0010
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'K'  'K'   0.2010   0.2490
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0360   0.0250
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0110   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            167
_space_group_name_H-M_alt         'R -3 c :H'
_space_group_name_Hall            '-R 3 2"c'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z+1/2'
 '-x, -x+y, -z+1/2'
 'x-y, -y, -z+1/2'
 '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'
 'y+2/3, x+1/3, -z+5/6'
 '-x+2/3, -x+y+1/3, -z+5/6'
 'x-y+2/3, -y+1/3, -z+5/6'
 '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'
 'y+1/3, x+2/3, -z+7/6'
 '-x+1/3, -x+y+2/3, -z+7/6'
 'x-y+1/3, -y+2/3, -z+7/6'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z-1/2'
 'x, x-y, z-1/2'
 '-x+y, y, z-1/2'
 '-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'
 '-y+2/3, -x+1/3, z-1/6'
 'x+2/3, x-y+1/3, z-1/6'
 '-x+y+2/3, y+1/3, z-1/6'
 '-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'
 '-y+1/3, -x+2/3, z+1/6'
 'x+1/3, x-y+2/3, z+1/6'
 '-x+y+1/3, y+2/3, z+1/6'
 
_cell_length_a                    11.0685(2)
_cell_length_b                    11.0685(2)
_cell_length_c                    40.5755(19)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4305.0(3)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     4944	
_cell_measurement_theta_min       2.9238
_cell_measurement_theta_max       26.3921
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     2.070          
_exptl_crystal_F_000              2688
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.14
_exptl_absorpt_coefficient_mu     1.041
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6663	
_exptl_absorpt_correction_T_max   0.7454
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube' 
_diffrn_measurement_device_type   bruker-CCD
_diffrn_measurement_method        'w scans'
_diffrn_detector_area_resol_mean  10.4167
_diffrn_reflns_number             7741
_diffrn_reflns_av_unetI/netI      0.0122
_diffrn_reflns_av_R_equivalents   0.0227
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -48
_diffrn_reflns_limit_l_max        50
_diffrn_reflns_theta_min          3.682
_diffrn_reflns_theta_max          26.391
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.989
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.989
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.989
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              978
_reflns_number_gt                 904
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SMART' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0613P)²+15.6693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0027(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          978
_refine_ls_number_parameters      110
_refine_ls_number_restraints      33
_refine_ls_R_factor_all           0.0382
_refine_ls_R_factor_gt            0.0351
_refine_ls_wR_factor_ref          0.1067
_refine_ls_wR_factor_gt           0.1037
_refine_ls_goodness_of_fit_ref    1.112
_refine_ls_restrained_S_all       1.102
_refine_ls_shift/su_max           0.001
_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_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
O1 O 0.6667 0.84949(18) 0.5833 0.0113(5) Uani 1 2 d S T P . .
O2 O 0.62686(15) 0.68067(16) 0.54099(3) 0.0166(4) Uani 1 1 d . . . . .
O3 O 0.49895(16) 0.60663(16) 0.59189(4) 0.0178(4) Uani 1 1 d . . . . .
O4 O 0.4088(2) 0.4750(2) 0.54284(4) 0.0331(5) Uani 1 1 d . . . . .
H4 H 0.3391 0.4379 0.5545 0.050 Uiso 1 1 calc R U . . .
O5 O 0.52706(15) 0.77883(16) 0.63211(3) 0.0149(4) Uani 1 1 d . . . . .
H5 H 0.4822 0.8101 0.6194 0.022 Uiso 1 1 d R U . . .
B1 B 0.5999(2) 0.7410(2) 0.60823(5) 0.0119(5) Uani 1 1 d . . . . .
B2 B 0.5129(3) 0.5882(3) 0.55890(6) 0.0182(5) Uani 1 1 d . . . . .
K1 K 0.60172(7) 0.77956(7) 0.48108(2) 0.0384(3) Uani 1 1 d . . . . .
Na1 Na 0.3333 0.6667 0.6667 0.0119(4) Uani 1 6 d S T P . .
O6 O 0.355(3) 0.697(2) 0.5096(3) 0.057(5) Uani 0.1667 1 d . U P A 1
H6 H 0.4088 0.7745 0.5156 0.085 Uiso 0.1667 1 d R U P A 1
O7 O 0.314(4) 0.659(7) 0.4540(2) 0.032(5) Uani 0.1667 1 d . U P B -1
H7 H 0.2435 0.6067 0.4686 0.049 Uiso 0.1667 1 d R U P B -1
C1 C 0.340(7) 0.655(6) 0.4239(2) 0.023(4) Uani 0.1667 1 d . U P B -1
H1A H 0.2978 0.5595 0.4158 0.028 Uiso 0.1667 1 calc R U P B -1
H1B H 0.4393 0.7032 0.4195 0.028 Uiso 0.1667 1 calc R U P B -1
C2 C 0.279(2) 0.722(2) 0.4112(5) 0.047(4) Uani 0.1667 1 d . U P B -1
H2A H 0.1880 0.6866 0.4210 0.071 Uiso 0.1667 1 calc R U P B -1
H2B H 0.2689 0.7075 0.3878 0.071 Uiso 0.1667 1 calc R U P B -1
H2C H 0.3346 0.8198 0.4158 0.071 Uiso 0.1667 1 calc R U P B -1
 
 
_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
O1 B1 1.457(2) . ?
O1 B1 1.457(2) 17_655 ?
O2 B2 1.370(3) . ?
O2 B1 1.487(3) 17_655 ?
O3 B2 1.374(3) . ?
O3 B1 1.496(3) . ?
O4 B2 1.370(3) . ?
O4 H4 0.8200 . ?
O5 B1 1.449(2) . ?
O5 H5 0.8970 . ?
B1 O2 1.488(3) 17_655 ?
O6 O6 0.52(4) 2_665 ?
O6 O6 0.52(3) 3_565 ?
O6 H6 0.7984 . ?
O7 C1 1.261(19) . ?
O7 H7 0.9166 . ?
C1 C2 1.34(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
 
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
B1 O1 B1 110.4(2) . 17_655 ?
B2 O2 B1 116.95(16) . 17_655 ?
B2 O3 B1 119.74(16) . . ?
B2 O4 H4 109.5 . . ?
B1 O5 H5 102.9 . . ?
O5 B1 O1 110.59(17) . . ?
O5 B1 O2 108.92(16) . 17_655 ?
O1 B1 O2 109.96(15) . 17_655 ?
O5 B1 O3 109.69(16) . . ?
O1 B1 O3 109.33(15) . . ?
O2 B1 O3 108.31(17) 17_655 . ?
O2 B2 O4 118.0(2) . . ?
O2 B2 O3 122.4(2) . . ?
O4 B2 O3 119.6(2) . . ?
O6 O6 O6 60.00(3) 2_665 3_565 ?
O6 O6 H6 144.9 2_665 . ?
O6 O6 H6 146.2 3_565 . ?
C1 O7 H7 137.6 . . ?
O7 C1 C2 99(3) . . ?
O7 C1 H1A 111.9 . . ?
C2 C1 H1A 111.9 . . ?
O7 C1 H1B 111.9 . . ?
C2 C1 H1B 111.9 . . ?
H1A C1 H1B 109.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
B1 O1 B1 O5 -177.0(2) 17_655 . . . ?
B1 O1 B1 O2 62.66(13) 17_655 . . 17_655 ?
B1 O1 B1 O3 -56.13(12) 17_655 . . . ?
B2 O3 B1 O5 142.31(19) . . . . ?
B2 O3 B1 O1 20.9(3) . . . . ?
B2 O3 B1 O2 -98.9(2) . . . 17_655 ?
B1 O2 B2 O4 175.7(2) 17_655 . . . ?
B1 O2 B2 O3 -3.1(3) 17_655 . . . ?
B1 O3 B2 O2 8.9(3) . . . . ?
B1 O3 B2 O4 -169.8(2) . . . . ?
 
_refine_diff_density_max    0.949
_refine_diff_density_min   -0.269
_refine_diff_density_rms    0.080



