 
data_cbbof 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             Ca3B5Be6O16F 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B5 Be6 Ca3 F O16' 
_chemical_formula_weight          503.35 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Li'  'Li'  -0.0003   0.0001 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Be'  'Be'   0.0005   0.0002 
 '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' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    P6(3)/m 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 'x, y, -z-1/2' 
 '-y, x-y, -z-1/2' 
 '-x+y, -x, -z-1/2' 
 
_cell_length_a                    8.9753(13) 
_cell_length_b                    8.9753(13) 
_cell_length_c                    7.7356(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      539.66(15) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     2344
_cell_measurement_theta_min       2.6205
_cell_measurement_theta_max       31.4816
 
_exptl_crystal_description        chip 
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.3250
_exptl_crystal_size_mid           0.3150
_exptl_crystal_size_min           0.2000 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.10 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              492 
_exptl_absorpt_coefficient_mu     1.667 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8862 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       153(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5363 
_diffrn_reflns_av_R_equivalents   0.0321 
_diffrn_reflns_av_sigmaI/netI     0.0168 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.62 
_diffrn_reflns_theta_max          31.48 
_reflns_number_total              642 
_reflns_number_gt                 632 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0255P)²+0.4518P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          642 
_refine_ls_number_parameters      53 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0264 
_refine_ls_R_factor_gt            0.0259 
_refine_ls_wR_factor_ref          0.0644 
_refine_ls_wR_factor_gt           0.0641 
_refine_ls_goodness_of_fit_ref    1.294 
_refine_ls_restrained_S_all       1.294 
_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 
Ca1 Ca 0.46368(5) 1.51200(5) 0.2500 0.00504(12) Uani 1 2 d S . . 
O1 O 0.0000 1.0000 0.2500 0.0033(4) Uani 1 6 d S . . 
O2 O 0.51710(12) 1.34172(13) 0.05572(14) 0.0061(2) Uani 1 1 d . . . 
O3 O 0.20287(12) 1.26703(12) 0.09915(13) 0.00510(19) Uani 1 1 d . . . 
O4 O 0.76652(17) 1.71059(18) 0.2500 0.0057(3) Uani 1 2 d S . . 
F1 F 0.3333 1.6667 0.2500 0.0097(4) Uani 1 6 d S . . 
B1 B 0.0882(3) 1.1963(3) 0.2500 0.0040(3) Uani 1 2 d S . . 
B2 B 0.6667 1.3333 0.0531(4) 0.0061(4) Uani 1 3 d S . . 
Be1 Be 0.1441(2) 1.3238(2) -0.0710(2) 0.0047(3) 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 
Ca1 F1 2.2180(5) . ? 
Ca1 O2 2.3573(11) . ? 
Ca1 O2 2.3573(11) 10_556 ? 
Ca1 O4 2.3917(15) . ? 
Ca1 O3 2.5551(11) . ? 
Ca1 O3 2.5551(11) 10_556 ? 
Ca1 O2 2.6683(11) 4_685 ? 
Ca1 O2 2.6683(11) 7_685 ? 
Ca1 Be1 2.9405(18) 8_455 ? 
Ca1 Be1 2.9405(18) 5_455 ? 
Ca1 B1 3.137(2) . ? 
Ca1 B2 3.228(2) 4_685 ? 
O1 B1 1.528(2) 2_675 ? 
O1 B1 1.528(2) . ? 
O1 B1 1.528(2) 3_465 ? 
O2 B2 1.3818(10) . ? 
O2 Be1 1.618(2) 8_455 ? 
O2 Ca1 2.6683(11) 7_685 ? 
O3 B1 1.4735(16) . ? 
O3 Be1 1.593(2) . ? 
O3 Be1 1.641(2) 8_455 ? 
O4 B1 1.489(2) 2_785 ? 
O4 Be1 1.7038(19) 4_685 ? 
O4 Be1 1.7038(19) 7_685 ? 
F1 Ca1 2.2180(5) 3_475 ? 
F1 Ca1 2.2180(5) 2_785 ? 
B1 O3 1.4735(16) 10_556 ? 
B1 O4 1.489(2) 3_475 ? 
B1 Ca1 3.246(2) 3_475 ? 
B2 O2 1.3818(10) 2_775 ? 
B2 O2 1.3818(10) 3_575 ? 
B2 Ca1 3.228(2) 9_765 ? 
B2 Ca1 3.228(2) 8_455 ? 
B2 Ca1 3.228(2) 7_685 ? 
Be1 O2 1.618(2) 9_665 ? 
Be1 O3 1.641(2) 9_665 ? 
Be1 O4 1.7038(19) 7_685 ? 
Be1 Ca1 2.9405(18) 9_665 ? 
Be1 Ca1 3.3604(18) 7_685 ? 
Be1 Ca1 3.4906(18) 3_475 ? 
 
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 
F1 Ca1 O2 138.39(3) . . ? 
F1 Ca1 O2 138.39(3) . 10_556 ? 
O2 Ca1 O2 79.22(5) . 10_556 ? 
F1 Ca1 O4 106.98(4) . . ? 
O2 Ca1 O4 87.67(4) . . ? 
O2 Ca1 O4 87.67(4) 10_556 . ? 
F1 Ca1 O3 89.75(3) . . ? 
O2 Ca1 O3 63.05(3) . . ? 
O2 Ca1 O3 97.42(4) 10_556 . ? 
O4 Ca1 O3 148.44(3) . . ? 
F1 Ca1 O3 89.75(3) . 10_556 ? 
O2 Ca1 O3 97.42(4) . 10_556 ? 
O2 Ca1 O3 63.05(3) 10_556 10_556 ? 
O4 Ca1 O3 148.44(3) . 10_556 ? 
O3 Ca1 O3 54.35(5) . 10_556 ? 
F1 Ca1 O2 67.46(2) . 4_685 ? 
O2 Ca1 O2 154.15(3) . 4_685 ? 
O2 Ca1 O2 76.69(4) 10_556 4_685 ? 
O4 Ca1 O2 82.16(3) . 4_685 ? 
O3 Ca1 O2 129.36(3) . 4_685 ? 
O3 Ca1 O2 79.90(3) 10_556 4_685 ? 
F1 Ca1 O2 67.46(2) . 7_685 ? 
O2 Ca1 O2 76.69(4) . 7_685 ? 
O2 Ca1 O2 154.15(3) 10_556 7_685 ? 
O4 Ca1 O2 82.16(3) . 7_685 ? 
O3 Ca1 O2 79.90(3) . 7_685 ? 
O3 Ca1 O2 129.36(3) 10_556 7_685 ? 
O2 Ca1 O2 124.83(5) 4_685 7_685 ? 
F1 Ca1 Be1 122.93(4) . 8_455 ? 
O2 Ca1 Be1 33.30(4) . 8_455 ? 
O2 Ca1 Be1 76.39(4) 10_556 8_455 ? 
O4 Ca1 Be1 120.38(4) . 8_455 ? 
O3 Ca1 Be1 33.82(4) . 8_455 ? 
O3 Ca1 Be1 66.38(4) 10_556 8_455 ? 
O2 Ca1 Be1 143.73(4) 4_685 8_455 ? 
O2 Ca1 Be1 88.37(4) 7_685 8_455 ? 
F1 Ca1 Be1 122.93(4) . 5_455 ? 
O2 Ca1 Be1 76.39(4) . 5_455 ? 
O2 Ca1 Be1 33.30(4) 10_556 5_455 ? 
O4 Ca1 Be1 120.38(4) . 5_455 ? 
O3 Ca1 Be1 66.38(4) . 5_455 ? 
O3 Ca1 Be1 33.82(4) 10_556 5_455 ? 
O2 Ca1 Be1 88.37(4) 4_685 5_455 ? 
O2 Ca1 Be1 143.73(4) 7_685 5_455 ? 
Be1 Ca1 Be1 56.19(7) 8_455 5_455 ? 
F1 Ca1 B1 84.30(4) . . ? 
O2 Ca1 B1 83.64(4) . . ? 
O2 Ca1 B1 83.64(4) 10_556 . ? 
O4 Ca1 B1 168.72(5) . . ? 
O3 Ca1 B1 27.67(2) . . ? 
O3 Ca1 B1 27.67(2) 10_556 . ? 
O2 Ca1 B1 102.73(3) 4_685 . ? 
O2 Ca1 B1 102.73(3) 7_685 . ? 
Be1 Ca1 B1 50.40(4) 8_455 . ? 
Be1 Ca1 B1 50.40(4) 5_455 . ? 
F1 Ca1 B2 46.59(3) . 4_685 ? 
O2 Ca1 B2 167.67(3) . 4_685 ? 
O2 Ca1 B2 92.90(4) 10_556 4_685 ? 
O4 Ca1 B2 101.58(3) . 4_685 ? 
O3 Ca1 B2 109.19(3) . 4_685 ? 
O3 Ca1 B2 70.44(3) 10_556 4_685 ? 
O2 Ca1 B2 24.86(3) 4_685 4_685 ? 
O2 Ca1 B2 112.36(4) 7_685 4_685 ? 
Be1 Ca1 B2 135.70(4) 8_455 4_685 ? 
Be1 Ca1 B2 91.80(4) 5_455 4_685 ? 
B1 Ca1 B2 86.09(3) . 4_685 ? 
B1 O1 B1 120.0 2_675 . ? 
B1 O1 B1 120.000(1) 2_675 3_465 ? 
B1 O1 B1 120.000(1) . 3_465 ? 
B2 O2 Be1 125.91(9) . 8_455 ? 
B2 O2 Ca1 124.25(10) . . ? 
Be1 O2 Ca1 93.55(7) 8_455 . ? 
B2 O2 Ca1 100.85(11) . 7_685 ? 
Be1 O2 Ca1 106.48(8) 8_455 7_685 ? 
Ca1 O2 Ca1 103.31(4) . 7_685 ? 
B1 O3 Be1 121.36(11) . . ? 
B1 O3 Be1 112.69(11) . 8_455 ? 
Be1 O3 Be1 116.54(8) . 8_455 ? 
B1 O3 Ca1 98.70(8) . . ? 
Be1 O3 Ca1 114.17(8) . . ? 
Be1 O3 Ca1 86.08(7) 8_455 . ? 
B1 O4 Be1 109.23(9) 2_785 4_685 ? 
B1 O4 Be1 109.23(9) 2_785 7_685 ? 
Be1 O4 Be1 108.72(14) 4_685 7_685 ? 
B1 O4 Ca1 111.40(10) 2_785 . ? 
Be1 O4 Ca1 109.12(8) 4_685 . ? 
Be1 O4 Ca1 109.12(8) 7_685 . ? 
Ca1 F1 Ca1 120.0 3_475 2_785 ? 
Ca1 F1 Ca1 120.000(1) 3_475 . ? 
Ca1 F1 Ca1 120.0 2_785 . ? 
O3 B1 O3 104.73(15) 10_556 . ? 
O3 B1 O4 113.67(10) 10_556 3_475 ? 
O3 B1 O4 113.67(10) . 3_475 ? 
O3 B1 O1 110.14(10) 10_556 . ? 
O3 B1 O1 110.14(10) . . ? 
O4 B1 O1 104.56(13) 3_475 . ? 
O3 B1 Ca1 53.63(7) 10_556 . ? 
O3 B1 Ca1 53.63(7) . . ? 
O4 B1 Ca1 117.32(11) 3_475 . ? 
O1 B1 Ca1 138.12(11) . . ? 
O3 B1 Ca1 88.65(9) 10_556 3_475 ? 
O3 B1 Ca1 88.65(9) . 3_475 ? 
O4 B1 Ca1 43.32(8) 3_475 3_475 ? 
O1 B1 Ca1 147.89(11) . 3_475 ? 
Ca1 B1 Ca1 74.00(5) . 3_475 ? 
O2 B2 O2 119.979(7) 2_775 3_575 ? 
O2 B2 O2 119.979(7) 2_775 . ? 
O2 B2 O2 119.979(6) 3_575 . ? 
O2 B2 Ca1 90.53(9) 2_775 9_765 ? 
O2 B2 Ca1 54.29(9) 3_575 9_765 ? 
O2 B2 Ca1 127.33(13) . 9_765 ? 
O2 B2 Ca1 54.29(9) 2_775 8_455 ? 
O2 B2 Ca1 127.33(13) 3_575 8_455 ? 
O2 B2 Ca1 90.53(9) . 8_455 ? 
Ca1 B2 Ca1 73.05(5) 9_765 8_455 ? 
O2 B2 Ca1 127.33(13) 2_775 7_685 ? 
O2 B2 Ca1 90.53(9) 3_575 7_685 ? 
O2 B2 Ca1 54.29(9) . 7_685 ? 
Ca1 B2 Ca1 73.05(5) 9_765 7_685 ? 
Ca1 B2 Ca1 73.05(5) 8_455 7_685 ? 
O3 Be1 O2 112.02(11) . 9_665 ? 
O3 Be1 O3 110.36(11) . 9_665 ? 
O2 Be1 O3 104.38(11) 9_665 9_665 ? 
O3 Be1 O4 110.64(11) . 7_685 ? 
O2 Be1 O4 114.13(11) 9_665 7_685 ? 
O3 Be1 O4 104.84(11) 9_665 7_685 ? 
O3 Be1 Ca1 152.19(10) . 9_665 ? 
O2 Be1 Ca1 53.14(6) 9_665 9_665 ? 
O3 Be1 Ca1 60.10(6) 9_665 9_665 ? 
O4 Be1 Ca1 97.17(8) 7_685 9_665 ? 
O3 Be1 Ca1 92.24(8) . 7_685 ? 
O2 Be1 Ca1 88.73(7) 9_665 7_685 ? 
O3 Be1 Ca1 146.38(9) 9_665 7_685 ? 
O4 Be1 Ca1 42.26(6) 7_685 7_685 ? 
Ca1 Be1 Ca1 109.20(5) 9_665 7_685 ? 
O3 Be1 Ca1 78.36(7) . 3_475 ? 
O2 Be1 Ca1 47.14(6) 9_665 3_475 ? 
O3 Be1 Ca1 86.87(7) 9_665 3_475 ? 
O4 Be1 Ca1 160.72(9) 7_685 3_475 ? 
Ca1 Be1 Ca1 75.16(4) 9_665 3_475 ? 
Ca1 Be1 Ca1 122.93(5) 7_685 3_475 ? 
O3 Be1 Ca1 41.45(6) . . ? 
O2 Be1 Ca1 76.77(7) 9_665 . ? 
O3 Be1 Ca1 142.78(9) 9_665 . ? 
O4 Be1 Ca1 108.41(8) 7_685 . ? 
Ca1 Be1 Ca1 129.69(6) 9_665 . ? 
Ca1 Be1 Ca1 69.93(3) 7_685 . ? 
Ca1 Be1 Ca1 66.44(3) 3_475 . ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              31.48 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.325 
_refine_diff_density_min   -0.444 
_refine_diff_density_rms    0.112 
