 
data_123 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ?                                                                                     
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B10 Ca3 O23 V2' 
_chemical_formula_weight          698.22 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Ca'  'Ca'   0.2262   0.3064 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 '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' 
 
_symmetry_cell_setting            Triclinic                                                                       
_symmetry_space_group_name_H-M    P-1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    6.5251(3) 
_cell_length_b                    11.4616(4) 
_cell_length_c                    12.7135(5) 
_cell_angle_alpha                 114.1260(10) 
_cell_angle_beta                  103.6560(10) 
_cell_angle_gamma                 90.5940(10) 
_cell_volume                      837.09(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     1942 
_cell_measurement_theta_min       1.82  
_cell_measurement_theta_max       25.03  
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.11 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.770 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              680 
_exptl_absorpt_coefficient_mu     2.170 
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.6960 
_exptl_absorpt_correction_T_max   0.7962 
_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   'multiwire proportional' 
_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             5500 
_diffrn_reflns_av_R_equivalents   0.0210 
_diffrn_reflns_av_sigmaI/netI     0.0339 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          1.82 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              2960 
_reflns_number_gt                 2566 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker FRAMBO' 
_computing_cell_refinement        'Bruker FRAMBO' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL'

_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)+(0.0445P)²+15.0643P] 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(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2960 
_refine_ls_number_parameters      380 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0643 
_refine_ls_R_factor_gt            0.0561 
_refine_ls_wR_factor_ref          0.1361 
_refine_ls_wR_factor_gt           0.1293 
_refine_ls_goodness_of_fit_ref    0.925 
_refine_ls_restrained_S_all       0.925 
_refine_ls_shift/su_max           0 
_refine_ls_shift/su_mean          0
 
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 
Ca1 Ca 0.19317(17) 0.74537(10) -0.00137(9) 0.0061(3) Uani 1 1 d . . . 
Ca2 Ca 0.44988(18) 0.62255(11) 0.40278(11) 0.0128(3) Uani 1 1 d . . . 
Ca3 Ca 0.04658(18) 0.87798(11) 0.60161(10) 0.0127(3) Uani 1 1 d . . . 
V1 V 0.35861(18) 0.46299(11) 0.06860(10) 0.0226(3) Uani 1 1 d . . . 
V2 V -0.3150(2) 0.93816(17) 0.06553(12) 0.0559(6) Uani 1 1 d . . . 
B1 B 0.1981(10) 0.8785(6) 0.3213(6) 0.0119(13) Uani 1 1 d . . . 
B2 B 0.9164(10) 0.7602(6) 0.3459(6) 0.0108(13) Uani 1 1 d . . . 
B3 B 0.2710(10) 0.5989(6) 0.6339(6) 0.0120(13) Uani 1 1 d . . . 
B4 B -0.0706(10) 0.6612(6) 0.6753(6) 0.0113(13) Uani 1 1 d . . . 
B5 B -0.4121(10) 0.7465(6) 0.6622(6) 0.0098(12) Uani 1 1 d . . . 
B6 B -0.4730(10) 0.9437(6) 0.6307(6) 0.0111(13) Uani 1 1 d . . . 
B7 B 0.0503(11) 0.2925(7) -0.1476(6) 0.0193(15) Uani 1 1 d . . . 
B8 B -0.0161(10) 0.5636(6) 0.3818(6) 0.0114(13) Uani 1 1 d . . . 
B9 B 0.4177(10) 1.1407(6) 0.6270(6) 0.0117(13) Uani 1 1 d . . . 
B10 B -0.1850(11) 0.7976(6) -0.1446(6) 0.0156(14) Uani 1 1 d . . . 
O1 O -0.1281(7) 0.8615(4) -0.0225(4) 0.0235(10) Uani 1 1 d . . . 
O2 O -0.3671(7) 0.8120(4) -0.2110(4) 0.0171(9) Uani 1 1 d . . . 
O3 O 0.1141(7) 0.8050(4) 0.1906(4) 0.0178(9) Uani 1 1 d . . . 
O4 O 0.1077(7) 0.3625(5) -0.0257(4) 0.0279(11) Uani 1 1 d . . . 
O5 O 0.7308(6) 0.7842(4) 0.3963(4) 0.0144(9) Uani 1 1 d . . . 
O6 O 0.3809(6) 0.8184(4) 0.3620(4) 0.0148(9) Uani 1 1 d . . . 
O7 O 0.0371(6) 0.8823(4) 0.3820(3) 0.0114(8) Uani 1 1 d . . . 
O8 O 0.3675(6) 1.0232(4) 0.6271(4) 0.0138(9) Uani 1 1 d . . . 
O9 O -0.2680(6) 0.9869(4) 0.6524(4) 0.0144(9) Uani 1 1 d . . . 
O10 O -0.2221(6) 0.7220(4) 0.6190(3) 0.0104(8) Uani 1 1 d . . . 
O11 O 0.1315(6) 0.6847(4) 0.6510(4) 0.0142(9) Uani 1 1 d . . . 
O12 O 0.4618(6) 0.6165(4) 0.6129(4) 0.0132(9) Uani 1 1 d . . . 
O13 O 0.1317(6) 0.4804(4) 0.3716(4) 0.0131(8) Uani 1 1 d . . . 
O14 O 0.0491(6) 0.6876(4) 0.4074(4) 0.0144(9) Uani 1 1 d . . . 
O15 O 0.7761(6) 0.5230(4) 0.3719(4) 0.0141(9) Uani 1 1 d . . . 
O16 O -0.0427(6) 0.7176(4) -0.1933(4) 0.0150(9) Uani 1 1 d . . . 
O17 O -0.5446(6) 0.8208(4) 0.6057(3) 0.0125(8) Uani 1 1 d . . . 
O18 O 0.1451(7) 0.3193(4) -0.2195(4) 0.0217(10) Uani 1 1 d . . . 
O19 O -0.3899(15) 0.8204(9) 0.1262(8) 0.026(2) Uani 0.50 1 d P . . 
O20 O -0.1850(9) 1.0385(5) 0.1921(4) 0.0383(13) Uani 1 1 d . . . 
O21 O -0.5984(14) 0.9273(9) -0.0030(8) 0.0213(19) Uani 0.50 1 d P . . 
O22 O 0.4106(14) 0.5717(8) 0.0034(8) 0.022(2) Uani 0.50 1 d P . . 
O23 O 0.3156(16) 0.5546(8) 0.2000(8) 0.024(2) Uani 0.50 1 d P . . 
O24 O -0.5091(15) 0.8618(11) 0.0473(11) 0.037(3) Uani 0.50 1 d P . . 
O25 O 0.5440(19) 0.3831(11) 0.0971(10) 0.046(3) Uani 0.50 1 d P . . 
O26 O 0.409(2) 0.4632(14) 0.1944(10) 0.049(3) Uani 0.50 1 d P . . 
O27 O 0.311(2) 0.6058(13) 0.0856(13) 0.056(4) Uani 0.50 1 d P . . 
 
 
_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 
Ca1 O24 2.154(10) 1_655 ? 
Ca1 O27 2.333(13) . ? 
Ca1 O22 2.469(9) . ? 
Ca1 O3 2.435(4) . ? 
Ca1 O25 2.482(12) 2_665 ? 
Ca1 O16 2.451(4) . ? 
Ca1 O4 2.473(5) 2_565 ? 
Ca1 O21 2.488(9) 1_655 ? 
Ca1 O1 2.515(4) . ? 
Ca1 O19 2.738(10) 1_655 ? 
Ca1 B7 2.894(8) 2_565 ? 
Ca1 B10 2.926(7) . ? 
Ca2 O23 2.301(9) . ? 
Ca2 O15 2.463(4) . ? 
Ca2 O13 2.477(4) . ? 
Ca2 O26 2.475(12) . ? 
Ca2 O6 2.524(4) . ? 
Ca2 O5 2.631(4) . ? 
Ca2 O17 2.642(4) 1_655 ? 
Ca2 O12 2.683(4) . ? 
Ca2 O14 2.734(4) . ? 
Ca2 O12 2.743(4) 2_666 ? 
Ca2 O10 2.836(4) 1_655 ? 
Ca2 B5 2.906(6) 1_655 ? 
Ca3 O20 2.329(5) 2_576 ? 
Ca3 O9 2.492(4) . ? 
Ca3 O8 2.535(4) . ? 
Ca3 O14 2.544(4) . ? 
Ca3 O11 2.571(4) . ? 
Ca3 O10 2.600(4) . ? 
Ca3 O5 2.709(4) 1_455 ? 
Ca3 O7 2.740(4) 2_576 ? 
Ca3 O17 2.747(4) 1_655 ? 
Ca3 O7 2.799(4) . ? 
Ca3 B2 2.863(7) 1_455 ? 
Ca3 B6 3.116(7) 1_655 ? 
V1 O26 1.554(11) . ? 
V1 O25 1.588(12) . ? 
V1 O23 1.663(9) . ? 
V1 O27 1.604(13) . ? 
V1 O4 1.830(5) . ? 
V1 O22 1.822(9) . ? 
V1 O22 1.905(9) 2_665 ? 
V2 O24 1.448(10) . ? 
V2 O20 1.567(5) . ? 
V2 O21 1.827(9) . ? 
V2 O1 1.837(5) . ? 
V2 O19 1.916(10) . ? 
V2 O21 2.034(10) 2_475 ? 
V2 Ca1 3.596(2) 1_455 ? 
B1 O7 1.433(8) . ? 
B1 O6 1.477(7) . ? 
B1 O3 1.480(8) . ? 
B1 O9 1.481(7) 2_576 ? 
B1 Ca3 3.146(6) 2_576 ? 
B2 O18 1.437(8) 2_665 ? 
B2 O7 1.439(7) 1_655 ? 
B2 O5 1.477(7) . ? 
B2 O14 1.510(7) 1_655 ? 
B2 Ca3 2.863(7) 1_655 ? 
B3 O11 1.334(8) . ? 
B3 O12 1.363(8) . ? 
B3 O15 1.396(8) 2_666 ? 
B3 Ca2 3.083(7) 2_666 ? 
B4 O10 1.437(8) . ? 
B4 O11 1.469(7) . ? 
B4 O16 1.487(7) 1_556 ? 
B4 O13 1.494(7) 2_566 ? 
B5 O2 1.425(7) 1_556 ? 
B5 O10 1.456(7) . ? 
B5 O17 1.487(7) . ? 
B5 O12 1.503(7) 1_455 ? 
B5 Ca2 2.906(6) 1_455 ? 
B6 O9 1.345(8) . ? 
B6 O17 1.361(8) . ? 
B6 O8 1.395(8) 1_455 ? 
B6 Ca3 3.116(7) 1_455 ? 
B7 O18 1.344(9) . ? 
B7 O4 1.374(8) . ? 
B7 O3 1.377(8) 2_565 ? 
B7 Ca1 2.894(8) 2_565 ? 
B8 O13 1.354(8) . ? 
B8 O14 1.360(8) . ? 
B8 O15 1.389(8) 1_455 ? 
B9 O6 1.347(8) 2_676 ? 
B9 O5 1.363(8) 2_676 ? 
B9 O8 1.384(8) . ? 
B9 Ca2 3.033(7) 2_676 ? 
B10 O2 1.341(8) . ? 
B10 O1 1.370(8) . ? 
B10 O16 1.383(8) . ? 
O2 B5 1.425(7) 1_554 ? 
O3 B7 1.377(8) 2_565 ? 
O4 Ca1 2.473(5) 2_565 ? 
O5 B9 1.363(8) 2_676 ? 
O5 Ca3 2.709(4) 1_655 ? 
O6 B9 1.347(8) 2_676 ? 
O7 B2 1.439(7) 1_455 ? 
O7 Ca3 2.740(4) 2_576 ? 
O8 B6 1.395(8) 1_655 ? 
O9 B1 1.481(7) 2_576 ? 
O10 Ca2 2.836(4) 1_455 ? 
O12 B5 1.503(7) 1_655 ? 
O12 Ca2 2.743(4) 2_666 ? 
O13 B4 1.494(7) 2_566 ? 
O14 B2 1.510(7) 1_455 ? 
O15 B8 1.389(8) 1_655 ? 
O15 B3 1.396(8) 2_666 ? 
O16 B4 1.487(7) 1_554 ? 
O17 Ca2 2.642(4) 1_455 ? 
O17 Ca3 2.747(4) 1_455 ? 
O18 B2 1.437(8) 2_665 ? 
O19 O24 1.365(14) . ? 
O19 Ca1 2.738(10) 1_455 ? 
O20 Ca3 2.329(5) 2_576 ? 
O21 O24 1.241(14) . ? 
O21 V2 2.034(10) 2_475 ? 
O21 Ca1 2.488(9) 1_455 ? 
O22 O27 1.288(15) . ? 
O22 O25 1.645(16) 2_665 ? 
O22 V1 1.905(9) 2_665 ? 
O23 O26 1.203(16) . ? 
O23 O27 1.772(16) . ? 
O24 Ca1 2.154(10) 1_455 ? 
O25 O22 1.645(16) 2_665 ? 
O25 O26 1.659(17) . ? 
O25 Ca1 2.482(12) 2_665 ? 
 
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 
O24 Ca1 O27 98.6(5) 1_655 . ? 
O24 Ca1 O22 85.8(4) 1_655 . ? 
O27 Ca1 O22 31.0(4) . . ? 
O24 Ca1 O3 102.5(3) 1_655 . ? 
O27 Ca1 O3 67.5(3) . . ? 
O22 Ca1 O3 97.7(2) . . ? 
O24 Ca1 O25 68.5(4) 1_655 2_665 ? 
O27 Ca1 O25 69.7(4) . 2_665 ? 
O22 Ca1 O25 38.8(4) . 2_665 ? 
O3 Ca1 O25 134.1(3) . 2_665 ? 
O24 Ca1 O16 113.9(3) 1_655 . ? 
O27 Ca1 O16 134.4(4) . . ? 
O22 Ca1 O16 118.2(2) . . ? 
O3 Ca1 O16 129.33(15) . . ? 
O25 Ca1 O16 92.8(3) 2_665 . ? 
O24 Ca1 O4 158.1(3) 1_655 2_565 ? 
O27 Ca1 O4 69.1(4) . 2_565 ? 
O22 Ca1 O4 90.9(2) . 2_565 ? 
O3 Ca1 O4 56.48(14) . 2_565 ? 
O25 Ca1 O4 120.1(3) 2_665 2_565 ? 
O16 Ca1 O4 86.64(15) . 2_565 ? 
O24 Ca1 O21 29.9(3) 1_655 1_655 ? 
O27 Ca1 O21 128.5(4) . 1_655 ? 
O22 Ca1 O21 112.1(3) . 1_655 ? 
O3 Ca1 O21 111.2(2) . 1_655 ? 
O25 Ca1 O21 83.5(4) 2_665 1_655 ? 
O16 Ca1 O21 88.3(2) . 1_655 ? 
O4 Ca1 O21 156.0(2) 2_565 1_655 ? 
O24 Ca1 O1 114.2(3) 1_655 . ? 
O27 Ca1 O1 136.6(3) . . ? 
O22 Ca1 O1 160.0(2) . . ? 
O3 Ca1 O1 77.94(15) . . ? 
O25 Ca1 O1 147.7(3) 2_665 . ? 
O16 Ca1 O1 55.85(14) . . ? 
O4 Ca1 O1 70.27(17) 2_565 . ? 
O21 Ca1 O1 87.5(2) 1_655 . ? 
O24 Ca1 O19 29.4(3) 1_655 1_655 ? 
O27 Ca1 O19 69.7(4) . 1_655 ? 
O22 Ca1 O19 63.6(3) . 1_655 ? 
O3 Ca1 O19 86.2(2) . 1_655 ? 
O25 Ca1 O19 64.0(3) 2_665 1_655 ? 
O16 Ca1 O19 140.4(2) . 1_655 ? 
O4 Ca1 O19 132.4(2) 2_565 1_655 ? 
O21 Ca1 O19 59.0(3) 1_655 1_655 ? 
O1 Ca1 O19 134.5(2) . 1_655 ? 
O24 Ca1 B7 130.2(3) 1_655 2_565 ? 
O27 Ca1 B7 63.1(3) . 2_565 ? 
O22 Ca1 B7 92.9(3) . 2_565 ? 
O3 Ca1 B7 28.30(17) . 2_565 ? 
O25 Ca1 B7 130.9(3) 2_665 2_565 ? 
O16 Ca1 B7 110.33(17) . 2_565 ? 
O4 Ca1 B7 28.30(17) 2_565 2_565 ? 
O21 Ca1 B7 137.4(2) 1_655 2_565 ? 
O1 Ca1 B7 73.93(19) . 2_565 ? 
O19 Ca1 B7 109.0(2) 1_655 2_565 ? 
O24 Ca1 B10 119.1(3) 1_655 . ? 
O27 Ca1 B10 142.3(4) . . ? 
O22 Ca1 B10 142.3(2) . . ? 
O3 Ca1 B10 103.22(17) . . ? 
O25 Ca1 B10 120.8(3) 2_665 . ? 
O16 Ca1 B10 28.06(17) . . ? 
O4 Ca1 B10 75.51(18) 2_565 . ? 
O21 Ca1 B10 89.2(2) 1_655 . ? 
O1 Ca1 B10 27.87(17) . . ? 
O19 Ca1 B10 147.9(2) 1_655 . ? 
B7 Ca1 B10 91.0(2) 2_565 . ? 
O23 Ca2 O15 90.7(3) . . ? 
O23 Ca2 O13 81.0(3) . . ? 
O15 Ca2 O13 117.67(14) . . ? 
O23 Ca2 O26 28.9(4) . . ? 
O15 Ca2 O26 67.1(3) . . ? 
O13 Ca2 O26 79.2(3) . . ? 
O23 Ca2 O6 71.8(2) . . ? 
O15 Ca2 O6 119.21(14) . . ? 
O13 Ca2 O6 116.13(14) . . ? 
O26 Ca2 O6 98.1(3) . . ? 
O23 Ca2 O5 87.9(3) . . ? 
O15 Ca2 O5 69.47(13) . . ? 
O13 Ca2 O5 166.72(14) . . ? 
O26 Ca2 O5 94.6(3) . . ? 
O6 Ca2 O5 52.70(13) . . ? 
O23 Ca2 O17 140.0(3) . 1_655 ? 
O15 Ca2 O17 120.51(14) . 1_655 ? 
O13 Ca2 O17 102.33(13) . 1_655 ? 
O26 Ca2 O17 168.8(3) . 1_655 ? 
O6 Ca2 O17 71.18(13) . 1_655 ? 
O5 Ca2 O17 81.51(13) . 1_655 ? 
O23 Ca2 O12 153.4(3) . . ? 
O15 Ca2 O12 97.86(13) . . ? 
O13 Ca2 O12 72.71(13) . . ? 
O26 Ca2 O12 136.7(3) . . ? 
O6 Ca2 O12 123.59(13) . . ? 
O5 Ca2 O12 118.66(13) . . ? 
O17 Ca2 O12 53.10(12) 1_655 . ? 
O23 Ca2 O14 83.0(3) . . ? 
O15 Ca2 O14 169.13(14) . . ? 
O13 Ca2 O14 52.68(12) . . ? 
O26 Ca2 O14 104.1(3) . . ? 
O6 Ca2 O14 67.18(13) . . ? 
O5 Ca2 O14 118.89(13) . . ? 
O17 Ca2 O14 69.20(12) 1_655 . ? 
O12 Ca2 O14 84.24(13) . . ? 
O23 Ca2 O12 94.7(2) . 2_666 ? 
O15 Ca2 O12 52.42(12) . 2_666 ? 
O13 Ca2 O12 66.79(12) . 2_666 ? 
O26 Ca2 O12 67.4(3) . 2_666 ? 
O6 Ca2 O12 164.85(14) . 2_666 ? 
O5 Ca2 O12 121.83(13) . 2_666 ? 
O17 Ca2 O12 123.57(13) 1_655 2_666 ? 
O12 Ca2 O12 71.53(14) . 2_666 ? 
O14 Ca2 O12 119.10(12) . 2_666 ? 
O23 Ca2 O10 154.1(3) . 1_655 ? 
O15 Ca2 O10 69.40(13) . 1_655 ? 
O13 Ca2 O10 122.43(13) . 1_655 ? 
O26 Ca2 O10 136.5(3) . 1_655 ? 
O6 Ca2 O10 102.91(13) . 1_655 ? 
O5 Ca2 O10 69.99(12) . 1_655 ? 
O17 Ca2 O10 51.90(11) 1_655 1_655 ? 
O12 Ca2 O10 50.29(11) . 1_655 ? 
O14 Ca2 O10 119.08(12) . 1_655 ? 
O12 Ca2 O10 86.21(12) 2_666 1_655 ? 
O23 Ca2 B5 170.6(3) . 1_655 ? 
O15 Ca2 B5 96.64(16) . 1_655 ? 
O13 Ca2 B5 100.57(16) . 1_655 ? 
O26 Ca2 B5 160.5(4) . 1_655 ? 
O6 Ca2 B5 99.43(16) . 1_655 ? 
O5 Ca2 B5 89.19(16) . 1_655 ? 
O17 Ca2 B5 30.61(15) 1_655 1_655 ? 
O12 Ca2 B5 30.87(15) . 1_655 ? 
O14 Ca2 B5 90.62(16) . 1_655 ? 
O12 Ca2 B5 94.40(15) 2_666 1_655 ? 
O10 Ca2 B5 29.34(14) 1_655 1_655 ? 
O20 Ca3 O9 84.22(18) 2_576 . ? 
O20 Ca3 O8 80.05(17) 2_576 . ? 
O9 Ca3 O8 116.02(13) . . ? 
O20 Ca3 O14 142.62(18) 2_576 . ? 
O9 Ca3 O14 126.39(14) . . ? 
O8 Ca3 O14 100.37(13) . . ? 
O20 Ca3 O11 73.54(18) 2_576 . ? 
O9 Ca3 O11 118.61(13) . . ? 
O8 Ca3 O11 115.17(13) . . ? 
O14 Ca3 O11 72.66(13) . . ? 
O20 Ca3 O10 88.23(16) 2_576 . ? 
O9 Ca3 O10 69.88(13) . . ? 
O8 Ca3 O10 166.00(14) . . ? 
O14 Ca3 O10 84.30(13) . . ? 
O11 Ca3 O10 53.37(12) . . ? 
O20 Ca3 O5 154.66(17) 2_576 1_455 ? 
O9 Ca3 O5 73.91(13) . 1_455 ? 
O8 Ca3 O5 120.88(13) . 1_455 ? 
O14 Ca3 O5 53.41(12) . 1_455 ? 
O11 Ca3 O5 105.67(13) . 1_455 ? 
O10 Ca3 O5 72.50(12) . 1_455 ? 
O20 Ca3 O7 90.64(17) 2_576 2_576 ? 
O9 Ca3 O7 53.06(12) . 2_576 ? 
O8 Ca3 O7 65.51(12) . 2_576 ? 
O14 Ca3 O7 123.93(13) . 2_576 ? 
O11 Ca3 O7 163.40(13) . 2_576 ? 
O10 Ca3 O7 122.71(12) . 2_576 ? 
O5 Ca3 O7 86.39(12) 1_455 2_576 ? 
O20 Ca3 O17 81.75(17) 2_576 1_655 ? 
O9 Ca3 O17 162.93(14) . 1_655 ? 
O8 Ca3 O17 51.84(12) . 1_655 ? 
O14 Ca3 O17 70.39(12) . 1_655 ? 
O11 Ca3 O17 66.29(12) . 1_655 ? 
O10 Ca3 O17 119.14(12) . 1_655 ? 
O5 Ca3 O17 121.78(13) 1_455 1_655 ? 
O7 Ca3 O17 117.30(12) 2_576 1_655 ? 
O20 Ca3 O7 150.25(17) 2_576 . ? 
O9 Ca3 O7 102.79(13) . . ? 
O8 Ca3 O7 70.85(12) . . ? 
O14 Ca3 O7 52.67(12) . . ? 
O11 Ca3 O7 124.42(13) . . ? 
O10 Ca3 O7 121.43(12) . . ? 
O5 Ca3 O7 50.79(12) 1_455 . ? 
O7 Ca3 O7 72.03(13) 2_576 . ? 
O17 Ca3 O7 85.03(12) 1_655 . ? 
O20 Ca3 B2 173.7(2) 2_576 1_455 ? 
O9 Ca3 B2 102.04(16) . 1_455 ? 
O8 Ca3 B2 97.68(16) . 1_455 ? 
O14 Ca3 B2 31.74(15) . 1_455 ? 
O11 Ca3 B2 102.40(16) . 1_455 ? 
O10 Ca3 B2 93.17(16) . 1_455 ? 
O5 Ca3 B2 30.58(15) 1_455 1_455 ? 
O7 Ca3 B2 93.77(16) 2_576 1_455 ? 
O17 Ca3 B2 92.21(15) 1_655 1_455 ? 
O7 Ca3 B2 29.42(15) . 1_455 ? 
O20 Ca3 B6 77.98(18) 2_576 1_655 ? 
O9 Ca3 B6 140.23(16) . 1_655 ? 
O8 Ca3 B6 26.08(15) . 1_655 ? 
O14 Ca3 B6 86.51(15) . 1_655 ? 
O11 Ca3 B6 90.03(15) . 1_655 ? 
O10 Ca3 B6 143.34(15) . 1_655 ? 
O5 Ca3 B6 127.22(15) 1_455 1_655 ? 
O7 Ca3 B6 91.59(15) 2_576 1_655 ? 
O17 Ca3 B6 25.88(15) 1_655 1_655 ? 
O7 Ca3 B6 78.52(14) . 1_655 ? 
B2 Ca3 B6 97.37(17) 1_455 1_655 ? 
O26 V1 O25 63.7(7) . . ? 
O26 V1 O23 43.7(6) . . ? 
O25 V1 O23 105.3(5) . . ? 
O26 V1 O27 107.0(7) . . ? 
O25 V1 O27 142.3(7) . . ? 
O23 V1 O27 65.6(6) . . ? 
O26 V1 O4 110.4(5) . . ? 
O25 V1 O4 113.5(4) . . ? 
O23 V1 O4 106.6(4) . . ? 
O27 V1 O4 104.0(6) . . ? 
O26 V1 O22 137.6(6) . . ? 
O25 V1 O22 117.4(6) . . ? 
O23 V1 O22 106.4(4) . . ? 
O27 V1 O22 43.6(5) . . ? 
O4 V1 O22 107.0(3) . . ? 
O26 V1 O22 114.0(6) . 2_665 ? 
O25 V1 O22 55.3(5) . 2_665 ? 
O23 V1 O22 138.6(4) . 2_665 ? 
O27 V1 O22 106.0(5) . 2_665 ? 
O4 V1 O22 114.6(3) . 2_665 ? 
O22 V1 O22 65.2(5) . 2_665 ? 
O26 V1 Ca2 26.5(5) . . ? 
O25 V1 Ca2 84.0(4) . . ? 
O23 V1 Ca2 21.5(3) . . ? 
O27 V1 Ca2 80.5(5) . . ? 
O4 V1 Ca2 119.84(15) . . ? 
O22 V1 Ca2 114.3(3) . . ? 
O22 V1 Ca2 121.5(3) 2_665 . ? 
O24 V2 O20 122.5(5) . . ? 
O24 V2 O21 42.6(5) . . ? 
O20 V2 O21 127.0(4) . . ? 
O24 V2 O1 118.5(5) . . ? 
O20 V2 O1 108.6(3) . . ? 
O21 V2 O1 122.3(3) . . ? 
O24 V2 O19 45.3(5) . . ? 
O20 V2 O19 92.9(4) . . ? 
O21 V2 O19 87.3(4) . . ? 
O1 V2 O19 105.7(3) . . ? 
O24 V2 O21 106.6(5) . 2_475 ? 
O20 V2 O21 94.6(3) . 2_475 ? 
O21 V2 O21 64.1(5) . 2_475 ? 
O1 V2 O21 100.5(3) . 2_475 ? 
O19 V2 O21 148.8(4) . 2_475 ? 
O24 V2 Ca1 4.1(5) . 1_455 ? 
O20 V2 Ca1 126.3(2) . 1_455 ? 
O21 V2 Ca1 39.9(3) . 1_455 ? 
O1 V2 Ca1 116.45(16) . 1_455 ? 
O19 V2 Ca1 48.6(3) . 1_455 ? 
O21 V2 Ca1 104.1(2) 2_475 1_455 ? 
O7 B1 O6 111.4(5) . . ? 
O7 B1 O3 111.3(5) . . ? 
O6 B1 O3 108.2(5) . . ? 
O7 B1 O9 107.2(5) . 2_576 ? 
O6 B1 O9 109.9(5) . 2_576 ? 
O3 B1 O9 108.8(5) . 2_576 ? 
O7 B1 Ca3 60.5(3) . 2_576 ? 
O6 B1 Ca3 144.0(4) . 2_576 ? 
O3 B1 Ca3 107.1(4) . 2_576 ? 
O9 B1 Ca3 50.9(3) 2_576 2_576 ? 
O18 B2 O7 115.3(5) 2_665 1_655 ? 
O18 B2 O5 111.7(5) 2_665 . ? 
O7 B2 O5 108.3(5) 1_655 . ? 
O18 B2 O14 108.6(5) 2_665 1_655 ? 
O7 B2 O14 107.7(5) 1_655 1_655 ? 
O5 B2 O14 104.7(4) . 1_655 ? 
O18 B2 Ca3 170.2(4) 2_665 1_655 ? 
O7 B2 Ca3 72.8(3) 1_655 1_655 ? 
O5 B2 Ca3 68.9(3) . 1_655 ? 
O14 B2 Ca3 62.4(3) 1_655 1_655 ? 
O11 B3 O12 124.7(5) . . ? 
O11 B3 O15 121.2(5) . 2_666 ? 
O12 B3 O15 113.9(5) . 2_666 ? 
O11 B3 Ca2 172.5(4) . 2_666 ? 
O12 B3 Ca2 62.8(3) . 2_666 ? 
O15 B3 Ca2 51.3(3) 2_666 2_666 ? 
O10 B4 O11 106.1(5) . . ? 
O10 B4 O16 111.6(5) . 1_556 ? 
O11 B4 O16 109.2(5) . 1_556 ? 
O10 B4 O13 112.9(5) . 2_566 ? 
O11 B4 O13 109.6(5) . 2_566 ? 
O16 B4 O13 107.4(5) 1_556 2_566 ? 
O10 B4 Ca3 55.2(3) . . ? 
O11 B4 Ca3 54.3(3) . . ? 
O16 B4 Ca3 109.3(3) 1_556 . ? 
O13 B4 Ca3 143.2(4) 2_566 . ? 
O2 B5 O10 113.3(5) 1_556 . ? 
O2 B5 O17 110.1(5) 1_556 . ? 
O10 B5 O17 109.6(5) . . ? 
O2 B5 O12 112.8(5) 1_556 1_455 ? 
O10 B5 O12 105.1(4) . 1_455 ? 
O17 B5 O12 105.6(4) . 1_455 ? 
O2 B5 Ca2 173.6(4) 1_556 1_455 ? 
O10 B5 Ca2 72.7(3) . 1_455 ? 
O17 B5 Ca2 64.8(3) . 1_455 ? 
O12 B5 Ca2 66.3(3) 1_455 1_455 ? 
O9 B6 O17 124.4(5) . . ? 
O9 B6 O8 121.2(5) . 1_455 ? 
O17 B6 O8 114.4(5) . 1_455 ? 
O9 B6 Ca3 172.9(4) . 1_455 ? 
O17 B6 Ca3 61.8(3) . 1_455 ? 
O8 B6 Ca3 53.0(3) 1_455 1_455 ? 
O18 B7 O4 122.2(6) . . ? 
O18 B7 O3 122.6(6) . 2_565 ? 
O4 B7 O3 115.1(6) . 2_565 ? 
O18 B7 Ca1 172.9(5) . 2_565 ? 
O4 B7 Ca1 58.6(3) . 2_565 ? 
O3 B7 Ca1 57.0(3) 2_565 2_565 ? 
O13 B8 O14 117.7(5) . . ? 
O13 B8 O15 120.1(5) . 1_455 ? 
O14 B8 O15 122.1(5) . 1_455 ? 
O13 B8 Ca2 53.4(3) . . ? 
O14 B8 Ca2 64.4(3) . . ? 
O15 B8 Ca2 173.4(4) 1_455 . ? 
O6 B9 O5 115.4(5) 2_676 2_676 ? 
O6 B9 O8 120.8(5) 2_676 . ? 
O5 B9 O8 123.5(5) 2_676 . ? 
O6 B9 Ca2 55.4(3) 2_676 2_676 ? 
O5 B9 Ca2 60.0(3) 2_676 2_676 ? 
O8 B9 Ca2 172.1(4) . 2_676 ? 
O2 B10 O1 121.7(6) . . ? 
O2 B10 O16 122.9(6) . . ? 
O1 B10 O16 115.4(6) . . ? 
O2 B10 Ca1 175.0(5) . . ? 
O1 B10 Ca1 59.1(3) . . ? 
O16 B10 Ca1 56.5(3) . . ? 
B10 O1 V2 123.5(4) . . ? 
B10 O1 Ca1 93.0(4) . . ? 
V2 O1 Ca1 137.9(2) . . ? 
B10 O2 B5 118.7(5) . 1_554 ? 
B7 O3 B1 118.8(5) 2_565 . ? 
B7 O3 Ca1 94.7(4) 2_565 . ? 
B1 O3 Ca1 144.5(4) . . ? 
B7 O4 V1 128.0(4) . . ? 
B7 O4 Ca1 93.1(4) . 2_565 ? 
V1 O4 Ca1 137.1(2) . 2_565 ? 
B9 O5 B2 123.2(5) 2_676 . ? 
B9 O5 Ca2 93.3(3) 2_676 . ? 
B2 O5 Ca2 130.5(3) . . ? 
B9 O5 Ca3 120.9(4) 2_676 1_655 ? 
B2 O5 Ca3 80.5(3) . 1_655 ? 
Ca2 O5 Ca3 110.22(14) . 1_655 ? 
B9 O6 B1 122.2(5) 2_676 . ? 
B9 O6 Ca2 98.6(3) 2_676 . ? 
B1 O6 Ca2 138.7(3) . . ? 
B1 O7 B2 115.1(4) . 1_455 ? 
B1 O7 Ca3 92.5(3) . 2_576 ? 
B2 O7 Ca3 137.0(3) 1_455 2_576 ? 
B1 O7 Ca3 132.9(3) . . ? 
B2 O7 Ca3 77.8(3) 1_455 . ? 
Ca3 O7 Ca3 107.97(13) 2_576 . ? 
B6 O8 B9 118.7(5) 1_655 . ? 
B6 O8 Ca3 100.9(3) 1_655 . ? 
B9 O8 Ca3 140.1(4) . . ? 
B6 O9 B1 122.3(5) . 2_576 ? 
B6 O9 Ca3 133.3(4) . . ? 
B1 O9 Ca3 101.7(3) 2_576 . ? 
B4 O10 B5 115.0(4) . . ? 
B4 O10 Ca3 97.8(3) . . ? 
B5 O10 Ca3 130.2(3) . . ? 
B4 O10 Ca2 132.2(3) . 1_455 ? 
B5 O10 Ca2 78.0(3) . 1_455 ? 
Ca3 O10 Ca2 107.29(13) . 1_455 ? 
B3 O11 B4 122.3(5) . . ? 
B3 O11 Ca3 137.3(4) . . ? 
B4 O11 Ca3 98.1(3) . . ? 
B3 O12 B5 123.0(5) . 1_655 ? 
B3 O12 Ca2 116.6(3) . . ? 
B5 O12 Ca2 82.8(3) 1_655 . ? 
B3 O12 Ca2 91.0(3) . 2_666 ? 
B5 O12 Ca2 135.5(3) 1_655 2_666 ? 
Ca2 O12 Ca2 108.47(14) . 2_666 ? 
B8 O13 B4 121.5(5) . 2_566 ? 
B8 O13 Ca2 100.6(3) . . ? 
B4 O13 Ca2 136.4(3) 2_566 . ? 
B8 O14 B2 121.0(5) . 1_455 ? 
B8 O14 Ca3 123.6(4) . . ? 
B2 O14 Ca3 85.9(3) 1_455 . ? 
B8 O14 Ca2 89.0(3) . . ? 
B2 O14 Ca2 129.3(3) 1_455 . ? 
Ca3 O14 Ca2 111.90(15) . . ? 
B8 O15 B3 118.9(5) 1_655 2_666 ? 
B8 O15 Ca2 137.2(4) 1_655 . ? 
B3 O15 Ca2 102.5(3) 2_666 . ? 
B10 O16 B4 119.6(5) . 1_554 ? 
B10 O16 Ca1 95.4(4) . . ? 
B4 O16 Ca1 144.7(4) 1_554 . ? 
B6 O17 B5 120.3(5) . . ? 
B6 O17 Ca2 123.0(3) . 1_455 ? 
B5 O17 Ca2 84.5(3) . 1_455 ? 
B6 O17 Ca3 92.4(3) . 1_455 ? 
B5 O17 Ca3 131.0(3) . 1_455 ? 
Ca2 O17 Ca3 108.51(14) 1_455 1_455 ? 
B7 O18 B2 119.7(5) . 2_665 ? 
O24 O19 V2 48.9(5) . . ? 
O24 O19 Ca1 50.8(5) . 1_455 ? 
V2 O19 Ca1 99.7(4) . 1_455 ? 
V2 O20 Ca3 156.2(3) . 2_576 ? 
O24 O21 V2 52.2(6) . . ? 
O24 O21 V2 167.4(8) . 2_475 ? 
V2 O21 V2 115.9(5) . 2_475 ? 
O24 O21 Ca1 60.0(6) . 1_455 ? 
V2 O21 Ca1 112.0(4) . 1_455 ? 
V2 O21 Ca1 132.2(4) 2_475 1_455 ? 
O27 O22 O25 139.4(10) . 2_665 ? 
O27 O22 V1 59.2(7) . . ? 
O25 O22 V1 158.3(7) 2_665 . ? 
O27 O22 V1 159.3(10) . 2_665 ? 
O25 O22 V1 52.5(5) 2_665 2_665 ? 
V1 O22 V1 114.8(5) . 2_665 ? 
O27 O22 Ca1 68.7(7) . . ? 
O25 O22 Ca1 71.0(5) 2_665 . ? 
V1 O22 Ca1 123.7(4) . . ? 
V1 O22 Ca1 121.5(4) 2_665 . ? 
O26 O23 V1 63.3(7) . . ? 
O26 O23 O27 115.9(10) . . ? 
V1 O23 O27 55.6(5) . . ? 
O26 O23 Ca2 83.6(7) . . ? 
V1 O23 Ca2 143.1(6) . . ? 
O27 O23 Ca2 140.8(7) . . ? 
O21 O24 O19 165.1(12) . . ? 
O21 O24 V2 85.3(7) . . ? 
O19 O24 V2 85.8(7) . . ? 
O21 O24 Ca1 90.1(7) . 1_455 ? 
O19 O24 Ca1 99.7(7) . 1_455 ? 
V2 O24 Ca1 173.2(8) . 1_455 ? 
O22 O25 V1 72.2(6) 2_665 . ? 
O22 O25 O26 123.3(9) 2_665 . ? 
V1 O25 O26 57.2(6) . . ? 
O22 O25 Ca1 70.2(5) 2_665 2_665 ? 
V1 O25 Ca1 139.2(7) . 2_665 ? 
O26 O25 Ca1 163.5(8) . 2_665 ? 
O23 O26 V1 73.0(8) . . ? 
O23 O26 O25 128.4(11) . . ? 
V1 O26 O25 59.1(6) . . ? 
O23 O26 Ca2 67.5(7) . . ? 
V1 O26 Ca2 137.2(8) . . ? 
O25 O26 Ca2 143.3(8) . . ? 
O22 O27 V1 77.2(8) . . ? 
O22 O27 O23 131.1(11) . . ? 
V1 O27 O23 58.8(5) . . ? 
O22 O27 Ca1 80.3(8) . . ? 
V1 O27 Ca1 148.5(8) . . ? 
O23 O27 Ca1 148.4(8) . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    1.608 
_refine_diff_density_min   -2.689 
_refine_diff_density_rms    0.164 
