 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B11 Ca2 H7 O22' 
_chemical_formula_weight          558.13 
 
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'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'Ca'  'Ca'   0.2262   0.3064 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1) 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    6.5100(4) 
_cell_length_b                    20.4228(8) 
_cell_length_c                    6.6513(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  119.029(9) 
_cell_angle_gamma                 90.00 
_cell_volume                      773.21(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     3207 
_cell_measurement_theta_min       2.9862 
_cell_measurement_theta_max       29.2983 
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           0.1800 
_exptl_crystal_size_mid           0.1500 
_exptl_crystal_size_min           0.1200  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.397 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              556 
_exptl_absorpt_coefficient_mu     0.872 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.70808 
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details    'CrysAlisPro, Agilent Technologies' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'SuperNova, Dual, Cu at zero, Atlas' 
_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             5196 
_diffrn_reflns_av_R_equivalents   0.0266 
_diffrn_reflns_av_sigmaI/netI     0.0337 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -7 
_diffrn_reflns_limit_l_max        7 
_diffrn_reflns_theta_min          3.50 
_diffrn_reflns_theta_max          24.98 
_reflns_number_total              2415 
_reflns_number_gt                 2285 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrysAlisPro, Agilent Technologies' 
_computing_cell_refinement        'CrysAlisPro, Agilent Technologies' 
_computing_data_reduction         'CrysAlisPro, Agilent Technologies' 
_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)+(0.0658P)²+0.1916P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.31(4) 
_refine_ls_number_reflns          2415 
_refine_ls_number_parameters      317 
_refine_ls_number_restraints      13 
_refine_ls_R_factor_all           0.0403 
_refine_ls_R_factor_gt            0.0373 
_refine_ls_wR_factor_ref          0.1025 
_refine_ls_wR_factor_gt           0.0995 
_refine_ls_goodness_of_fit_ref    1.087 
_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 
Ca1 Ca 0.69336(16) 0.77196(4) 0.37557(16) 0.0173(3) Uani 1 1 d . . . 
Ca2 Ca 1.00434(16) 0.65639(4) 0.07703(17) 0.0155(2) Uani 1 1 d . . . 
B1 B 1.1967(9) 0.7993(2) 0.4771(9) 0.0093(10) Uani 1 1 d U . . 
B2 B 1.0198(8) 0.7969(2) 0.0586(9) 0.0074(10) Uani 1 1 d U . . 
B3 B 1.2840(9) 0.7806(3) 0.8812(10) 0.0139(11) Uani 1 1 d . . . 
B4 B 1.5973(8) 0.7728(2) 0.7875(9) 0.0129(10) Uani 1 1 d . . . 
B5 B 1.0984(9) 0.9019(3) 0.2501(10) 0.0158(11) Uani 1 1 d . . . 
B6 B 0.6762(10) 0.6215(3) 0.3884(10) 0.0153(12) Uani 1 1 d . . . 
B7 B 0.4970(9) 0.6209(3) -0.0329(9) 0.0142(12) Uani 1 1 d . . . 
B8 B 0.5978(10) 0.5172(3) 0.1835(10) 0.0188(12) Uani 1 1 d . . . 
B9 B 0.0966(9) 0.6442(2) -0.3418(9) 0.0118(11) Uani 1 1 d . . . 
B10 B 0.4144(9) 0.6374(2) -0.4327(9) 0.0111(10) Uani 1 1 d . . . 
B11 B 0.6907(10) 0.9227(3) 0.4213(11) 0.0239(13) Uani 1 1 d . . . 
O1W O 1.0281(6) 0.54509(18) 0.1262(6) 0.0278(9) Uani 1 1 d . . . 
H1WA H 1.0881 0.5274 0.2729 0.033 Uiso 1 1 calc R . . 
H1WB H 0.9779 0.5176 -0.0005 0.033 Uiso 1 1 calc R . . 
O1 O 0.7693(6) 0.88160(19) 0.6036(7) 0.0302(9) Uani 1 1 d . . . 
H1A H 0.8663 0.8564 0.6015 0.045 Uiso 1 1 calc R . . 
O2 O 0.6076(7) 0.88707(18) 0.2249(7) 0.0296(9) Uani 1 1 d . . . 
H2A H 0.5499 0.9117 0.1136 0.044 Uiso 1 1 calc R . . 
O3 O 0.5919(7) 0.44991(18) 0.1694(6) 0.0305(9) Uani 1 1 d . . . 
H3A H 0.6629 0.4343 0.2991 0.046 Uiso 1 1 calc R . . 
O4 O 0.4844(6) 0.54941(17) -0.0204(6) 0.0168(7) Uani 1 1 d . . . 
O5 O 1.2030(5) 0.87090(15) 0.4571(6) 0.0146(7) Uani 1 1 d . . . 
O6 O 0.1751(6) 0.63680(15) -0.5025(5) 0.0132(7) Uani 1 1 d . . . 
O7 O 1.4418(5) 0.77355(16) 0.5606(5) 0.0127(6) Uani 1 1 d . . . 
O8 O 0.2551(5) 0.64616(16) -0.1138(5) 0.0154(7) Uani 1 1 d . . . 
O9 O 1.5234(5) 0.77945(17) 0.9491(5) 0.0139(7) Uani 1 1 d . . . 
O10 O 1.8289(5) 0.76425(15) 0.8579(5) 0.0121(7) Uani 1 1 d . . . 
O12 O -0.1332(5) 0.65151(17) -0.4087(6) 0.0166(7) Uani 1 1 d . . . 
O13 O 1.1246(5) 0.78283(16) 0.6541(5) 0.0133(7) Uani 1 1 d . . . 
O14 O 0.5750(5) 0.63634(15) -0.2063(5) 0.0138(7) Uani 1 1 d . . . 
O15 O 1.2411(5) 0.77714(16) 1.0608(5) 0.0144(7) Uani 1 1 d . . . 
O16 O 0.7007(6) 0.54968(17) 0.3882(6) 0.0172(8) Uani 1 1 d . . . 
O17 O 1.0298(5) 0.76874(16) 0.2660(5) 0.0114(6) Uani 1 1 d . . . 
O18 O 0.6662(6) 0.65052(15) 0.1803(6) 0.0131(7) Uani 1 1 d . . . 
O19 O 0.9953(5) 0.86720(15) 0.0489(6) 0.0153(7) Uani 1 1 d . . . 
O20 O 1.0905(7) 0.96805(17) 0.2327(6) 0.0296(9) Uani 1 1 d . . . 
H20A H 1.1611 0.9842 0.3615 0.044 Uiso 1 1 calc R . . 
O23 O 0.6951(7) 0.98813(17) 0.4368(7) 0.0349(10) Uani 1 1 d . . . 
H23A H 0.6395 1.0041 0.3078 0.052 Uiso 1 1 calc R . . 
O11 O 0.4551(5) 0.63903(15) -0.6147(6) 0.0147(7) 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 O7 2.481(3) 1_455 ? 
Ca1 O9 2.500(3) 1_454 ? 
Ca1 O2 2.510(4) . ? 
Ca1 O13 2.513(3) . ? 
Ca1 O1 2.614(4) . ? 
Ca1 O17 2.623(3) . ? 
Ca1 O15 2.661(3) 1_454 ? 
Ca1 O18 2.765(3) . ? 
Ca1 O12 2.795(4) 1_656 ? 
Ca1 O10 2.889(3) 1_455 ? 
Ca1 B1 3.059(5) . ? 
Ca1 B3 3.073(6) 1_454 ? 
Ca2 O1W 2.291(4) . ? 
Ca2 O6 2.490(3) 1_656 ? 
Ca2 O8 2.516(3) 1_655 ? 
Ca2 O14 2.534(3) . ? 
Ca2 O10 2.582(3) 1_454 ? 
Ca2 O17 2.583(3) . ? 
Ca2 O18 2.608(3) . ? 
Ca2 O11 2.665(3) 1_656 ? 
Ca2 B2 2.876(5) . ? 
Ca2 O12 2.906(3) 1_655 ? 
Ca2 O15 2.938(3) 1_554 ? 
Ca2 B10 3.076(5) 1_656 ? 
B1 O17 1.435(6) . ? 
B1 O5 1.471(6) . ? 
B1 O13 1.502(5) . ? 
B1 O7 1.507(6) . ? 
B2 O19 1.442(6) . ? 
B2 O17 1.467(6) . ? 
B2 O10 1.470(6) 1_454 ? 
B2 O15 1.489(5) 1_554 ? 
B3 O15 1.354(6) . ? 
B3 O13 1.356(6) . ? 
B3 O9 1.397(6) . ? 
B3 Ca1 3.073(6) 1_656 ? 
B4 O7 1.349(6) . ? 
B4 O10 1.356(5) . ? 
B4 O9 1.381(6) . ? 
B4 Ca1 3.092(5) 1_655 ? 
B5 O20 1.355(6) . ? 
B5 O5 1.360(7) . ? 
B5 O19 1.368(6) . ? 
B6 O12 1.453(7) 1_656 ? 
B6 O11 1.473(6) 1_556 ? 
B6 O16 1.476(7) . ? 
B6 O18 1.478(6) . ? 
B7 O18 1.440(6) . ? 
B7 O4 1.467(7) . ? 
B7 O8 1.487(6) . ? 
B7 O14 1.502(6) . ? 
B8 O4 1.359(7) . ? 
B8 O16 1.363(7) . ? 
B8 O3 1.376(7) . ? 
B9 O12 1.346(6) . ? 
B9 O8 1.359(6) . ? 
B9 O6 1.399(6) . ? 
B9 Ca2 3.132(5) 1_455 ? 
B10 O14 1.354(6) . ? 
B10 O11 1.359(6) . ? 
B10 O6 1.393(6) . ? 
B10 Ca2 3.076(5) 1_454 ? 
B11 O23 1.339(7) . ? 
B11 O1 1.355(7) . ? 
B11 O2 1.357(8) . ? 
O6 Ca2 2.490(3) 1_454 ? 
O7 Ca1 2.481(3) 1_655 ? 
O8 Ca2 2.516(3) 1_455 ? 
O9 Ca1 2.500(3) 1_656 ? 
O10 B2 1.470(6) 1_656 ? 
O10 Ca2 2.582(3) 1_656 ? 
O10 Ca1 2.889(3) 1_655 ? 
O12 B6 1.453(7) 1_454 ? 
O12 Ca1 2.795(4) 1_454 ? 
O12 Ca2 2.906(3) 1_455 ? 
O15 B2 1.489(5) 1_556 ? 
O15 Ca1 2.661(3) 1_656 ? 
O15 Ca2 2.938(3) 1_556 ? 
O11 B6 1.473(6) 1_554 ? 
O11 Ca2 2.665(3) 1_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 
O7 Ca1 O9 121.81(10) 1_455 1_454 ? 
O7 Ca1 O2 96.50(12) 1_455 . ? 
O9 Ca1 O2 66.39(12) 1_454 . ? 
O7 Ca1 O13 113.79(10) 1_455 . ? 
O9 Ca1 O13 123.51(10) 1_454 . ? 
O2 Ca1 O13 99.44(12) . . ? 
O7 Ca1 O1 71.66(12) 1_455 . ? 
O9 Ca1 O1 117.45(12) 1_454 . ? 
O2 Ca1 O1 51.09(12) . . ? 
O13 Ca1 O1 70.57(12) . . ? 
O7 Ca1 O17 168.33(10) 1_455 . ? 
O9 Ca1 O17 69.86(9) 1_454 . ? 
O2 Ca1 O17 88.08(11) . . ? 
O13 Ca1 O17 54.71(9) . . ? 
O1 Ca1 O17 103.55(11) . . ? 
O7 Ca1 O15 69.21(9) 1_455 1_454 ? 
O9 Ca1 O15 52.65(9) 1_454 1_454 ? 
O2 Ca1 O15 72.65(12) . 1_454 ? 
O13 Ca1 O15 171.99(12) . 1_454 ? 
O1 Ca1 O15 104.36(11) . 1_454 ? 
O17 Ca1 O15 122.45(9) . 1_454 ? 
O7 Ca1 O18 109.73(10) 1_455 . ? 
O9 Ca1 O18 68.26(11) 1_454 . ? 
O2 Ca1 O18 134.54(11) . . ? 
O13 Ca1 O18 102.68(11) . . ? 
O1 Ca1 O18 172.73(12) . . ? 
O17 Ca1 O18 73.67(9) . . ? 
O15 Ca1 O18 82.64(10) 1_454 . ? 
O7 Ca1 O12 87.50(10) 1_455 1_656 ? 
O9 Ca1 O12 118.85(11) 1_454 1_656 ? 
O2 Ca1 O12 170.21(13) . 1_656 ? 
O13 Ca1 O12 70.78(11) . 1_656 ? 
O1 Ca1 O12 122.72(11) . 1_656 ? 
O17 Ca1 O12 86.37(10) . 1_656 ? 
O15 Ca1 O12 117.14(10) 1_454 1_656 ? 
O18 Ca1 O12 50.92(10) . 1_656 ? 
O7 Ca1 O10 50.89(8) 1_455 1_455 ? 
O9 Ca1 O10 172.70(9) 1_454 1_455 ? 
O2 Ca1 O10 112.53(11) . 1_455 ? 
O13 Ca1 O10 63.67(9) . 1_455 ? 
O1 Ca1 O10 62.12(10) . 1_455 ? 
O17 Ca1 O10 117.44(9) . 1_455 ? 
O15 Ca1 O10 120.06(9) 1_454 1_455 ? 
O18 Ca1 O10 112.84(9) . 1_455 ? 
O12 Ca1 O10 63.42(9) 1_656 1_455 ? 
O7 Ca1 B1 141.48(12) 1_455 . ? 
O9 Ca1 B1 94.37(12) 1_454 . ? 
O2 Ca1 B1 85.66(14) . . ? 
O13 Ca1 B1 29.22(11) . . ? 
O1 Ca1 B1 80.50(13) . . ? 
O17 Ca1 B1 27.94(11) . . ? 
O15 Ca1 B1 145.51(12) 1_454 . ? 
O18 Ca1 B1 94.86(12) . . ? 
O12 Ca1 B1 85.67(12) 1_656 . ? 
O10 Ca1 B1 92.73(11) 1_455 . ? 
O7 Ca1 B3 95.26(12) 1_455 1_454 ? 
O9 Ca1 B3 26.57(11) 1_454 1_454 ? 
O2 Ca1 B3 67.02(14) . 1_454 ? 
O13 Ca1 B3 149.58(12) . 1_454 ? 
O1 Ca1 B3 113.17(13) . 1_454 ? 
O17 Ca1 B3 96.41(11) . 1_454 ? 
O15 Ca1 B3 26.08(11) 1_454 1_454 ? 
O18 Ca1 B3 74.00(12) . 1_454 ? 
O12 Ca1 B3 121.64(12) 1_656 1_454 ? 
O10 Ca1 B3 146.13(11) 1_455 1_454 ? 
B1 Ca1 B3 120.37(14) . 1_454 ? 
O1W Ca2 O6 73.61(12) . 1_656 ? 
O1W Ca2 O8 88.52(12) . 1_655 ? 
O6 Ca2 O8 120.53(11) 1_656 1_655 ? 
O1W Ca2 O14 85.39(12) . . ? 
O6 Ca2 O14 122.66(10) 1_656 . ? 
O8 Ca2 O14 111.28(10) 1_655 . ? 
O1W Ca2 O10 155.21(12) . 1_454 ? 
O6 Ca2 O10 127.24(10) 1_656 1_454 ? 
O8 Ca2 O10 90.21(10) 1_655 1_454 ? 
O14 Ca2 O10 72.05(10) . 1_454 ? 
O1W Ca2 O17 145.90(12) . . ? 
O6 Ca2 O17 73.01(10) 1_656 . ? 
O8 Ca2 O17 114.54(11) 1_655 . ? 
O14 Ca2 O17 107.01(10) . . ? 
O10 Ca2 O17 54.76(9) 1_454 . ? 
O1W Ca2 O18 85.65(12) . . ? 
O6 Ca2 O18 70.77(11) 1_656 . ? 
O8 Ca2 O18 165.10(11) 1_655 . ? 
O14 Ca2 O18 54.61(10) . . ? 
O10 Ca2 O18 89.37(10) 1_454 . ? 
O17 Ca2 O18 77.03(9) . . ? 
O1W Ca2 O11 77.60(12) . 1_656 ? 
O6 Ca2 O11 52.38(9) 1_656 1_656 ? 
O8 Ca2 O11 68.62(10) 1_655 1_656 ? 
O14 Ca2 O11 162.99(11) . 1_656 ? 
O10 Ca2 O11 124.63(10) 1_454 1_656 ? 
O17 Ca2 O11 87.54(10) . 1_656 ? 
O18 Ca2 O11 123.12(10) . 1_656 ? 
O1W Ca2 B2 174.09(14) . . ? 
O6 Ca2 B2 101.67(13) 1_656 . ? 
O8 Ca2 B2 90.96(12) 1_655 . ? 
O14 Ca2 B2 100.27(12) . . ? 
O10 Ca2 B2 30.65(12) 1_454 . ? 
O17 Ca2 B2 30.57(12) . . ? 
O18 Ca2 B2 96.23(12) . . ? 
O11 Ca2 B2 96.73(12) 1_656 . ? 
O1W Ca2 O12 95.03(12) . 1_655 ? 
O6 Ca2 O12 166.44(10) 1_656 1_655 ? 
O8 Ca2 O12 50.31(9) 1_655 1_655 ? 
O14 Ca2 O12 62.22(9) . 1_655 ? 
O10 Ca2 O12 65.70(9) 1_454 1_655 ? 
O17 Ca2 O12 118.95(10) . 1_655 ? 
O18 Ca2 O12 116.57(9) . 1_655 ? 
O11 Ca2 O12 118.76(9) 1_656 1_655 ? 
B2 Ca2 O12 89.15(13) . 1_655 ? 
O1W Ca2 O15 146.91(12) . 1_554 ? 
O6 Ca2 O15 102.70(10) 1_656 1_554 ? 
O8 Ca2 O15 64.58(9) 1_655 1_554 ? 
O14 Ca2 O15 121.16(10) . 1_554 ? 
O10 Ca2 O15 50.16(8) 1_454 1_554 ? 
O17 Ca2 O15 50.30(9) . 1_554 ? 
O18 Ca2 O15 124.98(10) . 1_554 ? 
O11 Ca2 O15 74.84(9) 1_656 1_554 ? 
B2 Ca2 O15 29.66(11) . 1_554 ? 
O12 Ca2 O15 82.64(9) 1_655 1_554 ? 
O1W Ca2 B10 76.12(13) . 1_656 ? 
O6 Ca2 B10 26.40(11) 1_656 1_656 ? 
O8 Ca2 B10 94.75(12) 1_655 1_656 ? 
O14 Ca2 B10 147.66(12) . 1_656 ? 
O10 Ca2 B10 128.64(12) 1_454 1_656 ? 
O17 Ca2 B10 77.18(11) . 1_656 ? 
O18 Ca2 B10 97.14(12) . 1_656 ? 
O11 Ca2 B10 26.16(11) 1_656 1_656 ? 
B2 Ca2 B10 98.07(13) . 1_656 ? 
O12 Ca2 B10 144.60(11) 1_655 1_656 ? 
O15 Ca2 B10 86.77(11) 1_554 1_656 ? 
O17 B1 O5 112.6(4) . . ? 
O17 B1 O13 107.0(4) . . ? 
O5 B1 O13 109.1(4) . . ? 
O17 B1 O7 111.9(4) . . ? 
O5 B1 O7 108.0(4) . . ? 
O13 B1 O7 108.1(4) . . ? 
O17 B1 Ca1 58.9(2) . . ? 
O5 B1 Ca1 103.6(3) . . ? 
O13 B1 Ca1 54.78(19) . . ? 
O7 B1 Ca1 147.9(3) . . ? 
O19 B2 O17 112.7(4) . . ? 
O19 B2 O10 112.6(4) . 1_454 ? 
O17 B2 O10 107.9(3) . 1_454 ? 
O19 B2 O15 110.8(4) . 1_554 ? 
O17 B2 O15 106.5(3) . 1_554 ? 
O10 B2 O15 105.9(4) 1_454 1_554 ? 
O19 B2 Ca2 171.7(3) . . ? 
O17 B2 Ca2 63.6(2) . . ? 
O10 B2 Ca2 63.5(2) 1_454 . ? 
O15 B2 Ca2 77.5(2) 1_554 . ? 
O15 B3 O13 127.6(4) . . ? 
O15 B3 O9 112.9(4) . . ? 
O13 B3 O9 119.4(4) . . ? 
O15 B3 Ca1 59.7(2) . 1_656 ? 
O13 B3 Ca1 172.5(3) . 1_656 ? 
O9 B3 Ca1 53.2(2) . 1_656 ? 
O7 B4 O10 119.5(4) . . ? 
O7 B4 O9 120.9(4) . . ? 
O10 B4 O9 119.5(4) . . ? 
O7 B4 Ca1 51.2(2) . 1_655 ? 
O10 B4 Ca1 68.7(2) . 1_655 ? 
O9 B4 Ca1 170.7(3) . 1_655 ? 
O20 B5 O5 122.0(5) . . ? 
O20 B5 O19 116.9(5) . . ? 
O5 B5 O19 121.0(4) . . ? 
O12 B6 O11 107.4(4) 1_656 1_556 ? 
O12 B6 O16 112.1(4) 1_656 . ? 
O11 B6 O16 110.3(4) 1_556 . ? 
O12 B6 O18 109.3(4) 1_656 . ? 
O11 B6 O18 106.9(4) 1_556 . ? 
O16 B6 O18 110.7(4) . . ? 
O12 B6 Ca1 65.1(2) 1_656 . ? 
O11 B6 Ca1 78.8(3) 1_556 . ? 
O16 B6 Ca1 170.8(3) . . ? 
O18 B6 Ca1 63.9(2) . . ? 
O18 B7 O4 113.5(4) . . ? 
O18 B7 O8 112.4(4) . . ? 
O4 B7 O8 106.7(4) . . ? 
O18 B7 O14 106.6(4) . . ? 
O4 B7 O14 107.5(4) . . ? 
O8 B7 O14 110.0(4) . . ? 
O18 B7 Ca2 56.7(2) . . ? 
O4 B7 Ca2 107.5(3) . . ? 
O8 B7 Ca2 145.4(3) . . ? 
O14 B7 Ca2 54.1(2) . . ? 
O4 B8 O16 121.8(5) . . ? 
O4 B8 O3 115.6(5) . . ? 
O16 B8 O3 122.6(5) . . ? 
O12 B9 O8 119.1(4) . . ? 
O12 B9 O6 121.2(4) . . ? 
O8 B9 O6 119.7(4) . . ? 
O12 B9 Ca2 67.9(2) . 1_455 ? 
O8 B9 Ca2 51.3(2) . 1_455 ? 
O6 B9 Ca2 170.8(3) . 1_455 ? 
O14 B10 O11 127.7(4) . . ? 
O14 B10 O6 120.4(4) . . ? 
O11 B10 O6 111.9(4) . . ? 
O14 B10 Ca2 170.3(3) . 1_454 ? 
O11 B10 Ca2 59.8(2) . 1_454 ? 
O6 B10 Ca2 52.6(2) . 1_454 ? 
O23 B11 O1 124.4(6) . . ? 
O23 B11 O2 126.4(5) . . ? 
O1 B11 O2 109.2(5) . . ? 
O23 B11 Ca1 177.6(4) . . ? 
O1 B11 Ca1 56.9(3) . . ? 
O2 B11 Ca1 52.4(3) . . ? 
B11 O1 Ca1 97.4(3) . . ? 
B11 O2 Ca1 102.2(3) . . ? 
B8 O4 B7 121.3(4) . . ? 
B5 O5 B1 122.2(4) . . ? 
B10 O6 B9 120.5(4) . . ? 
B10 O6 Ca2 101.0(3) . 1_454 ? 
B9 O6 Ca2 135.3(3) . 1_454 ? 
B4 O7 B1 120.1(3) . . ? 
B4 O7 Ca1 103.7(2) . 1_655 ? 
B1 O7 Ca1 131.1(2) . 1_655 ? 
B9 O8 B7 119.4(4) . . ? 
B9 O8 Ca2 103.8(3) . 1_455 ? 
B7 O8 Ca2 132.7(3) . 1_455 ? 
B4 O9 B3 120.4(4) . . ? 
B4 O9 Ca1 138.4(3) . 1_656 ? 
B3 O9 Ca1 100.3(3) . 1_656 ? 
B4 O10 B2 124.3(4) . 1_656 ? 
B4 O10 Ca2 114.7(3) . 1_656 ? 
B2 O10 Ca2 85.8(2) 1_656 1_656 ? 
B4 O10 Ca1 85.4(3) . 1_655 ? 
B2 O10 Ca1 130.7(2) 1_656 1_655 ? 
Ca2 O10 Ca1 119.10(11) 1_656 1_655 ? 
B9 O12 B6 124.9(4) . 1_454 ? 
B9 O12 Ca1 112.0(3) . 1_454 ? 
B6 O12 Ca1 86.8(3) 1_454 1_454 ? 
B9 O12 Ca2 86.7(3) . 1_455 ? 
B6 O12 Ca2 135.3(3) 1_454 1_455 ? 
Ca1 O12 Ca2 111.74(11) 1_454 1_455 ? 
B3 O13 B1 121.3(4) . . ? 
B3 O13 Ca1 142.7(3) . . ? 
B1 O13 Ca1 96.0(2) . . ? 
B10 O14 B7 119.4(4) . . ? 
B10 O14 Ca2 143.4(3) . . ? 
B7 O14 Ca2 97.2(3) . . ? 
B3 O15 B2 126.1(4) . 1_556 ? 
B3 O15 Ca1 94.2(3) . 1_656 ? 
B2 O15 Ca1 135.6(3) 1_556 1_656 ? 
B3 O15 Ca2 114.4(3) . 1_556 ? 
B2 O15 Ca2 72.9(2) 1_556 1_556 ? 
Ca1 O15 Ca2 109.73(11) 1_656 1_556 ? 
B8 O16 B6 118.9(4) . . ? 
B1 O17 B2 114.6(4) . . ? 
B1 O17 Ca2 134.5(3) . . ? 
B2 O17 Ca2 85.8(2) . . ? 
B1 O17 Ca1 93.2(2) . . ? 
B2 O17 Ca1 126.1(2) . . ? 
Ca2 O17 Ca1 107.01(11) . . ? 
B7 O18 B6 114.8(4) . . ? 
B7 O18 Ca2 95.8(2) . . ? 
B6 O18 Ca2 127.3(3) . . ? 
B7 O18 Ca1 133.1(3) . . ? 
B6 O18 Ca1 87.5(3) . . ? 
Ca2 O18 Ca1 102.28(10) . . ? 
B5 O19 B2 118.7(4) . . ? 
B10 O11 B6 126.3(4) . 1_554 ? 
B10 O11 Ca2 94.1(3) . 1_454 ? 
B6 O11 Ca2 138.3(3) 1_554 1_454 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              24.98 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.474 
_refine_diff_density_min   -0.381 
_refine_diff_density_rms    0.086 

#==========================================================================end

data_2

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B18 Ba4 H30 O46' 
_chemical_formula_weight          1510.14 
 
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'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ba'  'Ba'  -0.3244   2.2819 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 '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            orthorhombic 
_symmetry_space_group_name_H-M    Pmn21 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y, z' 
 'x+1/2, -y, z+1/2' 
 
_cell_length_a                    10.1679(5) 
_cell_length_b                    16.2316(9) 
_cell_length_c                    7.5544(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1246.79(14) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used           3342
_cell_measurement_theta_min             2.3603
_cell_measurement_theta_max             27.4816
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colour  
_exptl_crystal_size_max           0.1800 
_exptl_crystal_size_mid           0.1500 
_exptl_crystal_size_min           0.1200 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.011 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              712 
_exptl_absorpt_coefficient_mu     3.227 
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.6144
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Saturn724+ (2x2 bin mode)' 
_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             7924 
_diffrn_reflns_av_R_equivalents   0.0689 
_diffrn_reflns_av_sigmaI/netI     0.0721 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        8 
_diffrn_reflns_theta_min          3.59 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              2235 
_reflns_number_gt                 2026 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection         'CrystalClear (Rigaku Inc., 2007)' 
_computing_cell_refinement         'CrystalClear (Rigaku Inc., 2007)' 
_computing_data_reduction          'CrystalClear (Rigaku Inc., 2007)' 
_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)+(0.1128P)²+17.8845P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.013(2) 
_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    0.44(8) 
_refine_ls_number_reflns          2235 
_refine_ls_number_parameters      180 
_refine_ls_number_restraints      67 
_refine_ls_R_factor_all           0.0824 
_refine_ls_R_factor_gt            0.0757 
_refine_ls_wR_factor_ref          0.2040 
_refine_ls_wR_factor_gt           0.1956 
_refine_ls_goodness_of_fit_ref    1.061 
_refine_ls_restrained_S_all       1.050 
_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 
Ba1 Ba -0.5000 0.07951(6) 0.32146(17) 0.0180(4) Uani 1 2 d S . . 
Ba2 Ba -0.3659(2) -0.42218(14) 0.1047(3) 0.0443(7) Uani 0.50 1 d P . . 
B1 B -0.2260(12) -0.0128(8) 0.2044(18) 0.010(2) Uani 1 1 d U . . 
B2 B -0.5000 0.0552(10) -0.213(2) 0.003(3) Uani 1 2 d SU . . 
B3 B -0.5000 -0.1937(11) -0.014(2) 0.011(4) Uani 1 2 d SU . . 
B4 B -0.3707(14) -0.0688(8) -0.052(2) 0.012(3) Uani 1 1 d U . . 
B5 B -0.5000 -0.5674(18) -0.533(4) 0.034(6) Uani 1 2 d S . . 
B6 B -0.389(3) -0.483(3) -0.301(6) 0.114(17) Uani 1 1 d . . . 
O1 O -0.5000 -0.4440(13) -0.251(3) 0.061(6) Uani 1 2 d S . . 
O2 O -0.5000 -0.5262(14) -0.696(4) 0.075(6) Uani 1 2 d S . . 
H2A H -0.5751 -0.5249 -0.7353 0.112 Uiso 0.50 1 d PR . . 
O3 O -0.3837(9) 0.0571(6) -0.3302(14) 0.021(2) Uani 1 1 d U . . 
O4 O -0.3435(8) -0.0259(6) 0.1172(13) 0.0179(19) Uani 1 1 d U . . 
O5 O -0.3873(18) -0.5460(13) -0.414(3) 0.118(10) Uani 1 1 d . . . 
O6 O -0.2309(8) 0.0440(5) 0.3175(19) 0.0228(17) Uani 1 1 d U . . 
O7 O -0.3840(8) -0.1548(5) -0.0275(12) 0.0156(18) Uani 1 1 d U . . 
O8 O -0.5000 -0.6611(14) -0.547(4) 0.073(7) Uani 1 2 d S . . 
O9 O -0.5000 -0.2783(9) 0.002(2) 0.032(3) Uani 1 2 d SU . . 
H9A H -0.5760 -0.2950 0.0090 0.048 Uiso 0.50 1 d PR . . 
O10 O -0.5000 -0.0334(7) -0.1242(13) 0.007(2) Uani 1 2 d SU . . 
O11 O -0.5000 0.1121(8) -0.0750(19) 0.021(3) Uani 1 2 d S . . 
H11A H -0.4605 0.0929 0.0102 0.032 Uiso 0.50 1 d PR . . 
O12 O -0.253(2) -0.4349(13) -0.279(3) 0.051(6) Uani 0.60 1 d PU . . 
H12A H -0.2062 -0.4202 -0.3608 0.077 Uiso 1 1 d R . . 
O13 O -0.5000 -0.0888(13) 0.461(4) 0.079(8) Uani 1 2 d S . . 
H13A H -0.4822 -0.0838 0.5664 0.119 Uiso 0.50 1 d PR . . 
O1W O -0.3581(16) 0.2268(9) 0.286(5) 0.167(16) Uani 1 1 d . . . 
H1WA H -0.2777 0.2263 0.2601 0.201 Uiso 1 1 d R . . 
H1WB H -0.3953 0.2724 0.3090 0.201 Uiso 1 1 d R . . 
O2W O -0.366(5) -0.590(2) 0.006(6) 0.25(2) Uani 1 1 d . . . 
H2WA H -0.3707 -0.6010 -0.1034 0.298 Uiso 1 1 d R . . 
H2WB H -0.3639 -0.6286 0.0820 0.298 Uiso 1 1 d R . . 
O12' O -0.289(3) -0.4786(19) -0.185(7) 0.058(7) Uiso 0.40 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 
Ba2 O12' 2.50(5) . ? 
Ba2 Ba2 2.728(5) 3_455 ? 
B1 O6 1.257(17) . ? 
B1 O3 1.353(16) 2_455 ? 
B1 O4 1.380(16) . ? 
B2 O11 1.39(2) . ? 
B2 O3 1.479(14) 3_455 ? 
B2 O3 1.479(14) . ? 
B2 O10 1.586(18) . ? 
B3 O7 1.341(12) 3_455 ? 
B3 O7 1.341(12) . ? 
B3 O9 1.38(2) . ? 
B4 O7 1.414(15) . ? 
B4 O6 1.485(18) 2_454 ? 
B4 O4 1.481(17) . ? 
B4 O10 1.536(15) . ? 
B5 O2 1.40(4) . ? 
B5 O5 1.50(3) . ? 
B5 O5 1.50(3) 3_455 ? 
B5 O8 1.52(3) . ? 
B6 O5 1.33(4) . ? 
B6 O1 1.35(3) . ? 
B6 O12' 1.35(5) . ? 
B6 O12 1.60(5) . ? 
O1 B6 1.35(3) 3_455 ? 
O2 H2A 0.8200 . ? 
O3 B1 1.353(16) 2_454 ? 
O6 B4 1.485(18) 2_455 ? 
O9 H9A 0.8200 . ? 
O10 B4 1.536(15) 3_455 ? 
O11 H11A 0.8200 . ? 
O12 O12' 1.07(4) . ? 
O12 H12A 0.8200 . ? 
O13 H13A 0.8200 . ? 
O1W H1WA 0.8398 . ? 
O1W H1WB 0.8500 . ? 
O2W H2WA 0.8500 . ? 
O2W H2WB 0.8500 . ? 
 
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 
O12' Ba2 Ba2 108.2(8) . 3_455 ? 
O6 B1 O3 123.6(11) . 2_455 ? 
O6 B1 O4 113.8(10) . . ? 
O3 B1 O4 122.6(11) 2_455 . ? 
O11 B2 O3 115.8(8) . 3_455 ? 
O11 B2 O3 115.8(8) . . ? 
O3 B2 O3 106.3(13) 3_455 . ? 
O11 B2 O10 106.6(12) . . ? 
O3 B2 O10 105.8(8) 3_455 . ? 
O3 B2 O10 105.8(8) . . ? 
O7 B3 O7 123.1(16) 3_455 . ? 
O7 B3 O9 118.4(8) 3_455 . ? 
O7 B3 O9 118.4(8) . . ? 
O7 B4 O6 114.9(10) . 2_454 ? 
O7 B4 O4 111.7(11) . . ? 
O6 B4 O4 108.4(10) 2_454 . ? 
O7 B4 O10 109.5(10) . . ? 
O6 B4 O10 104.9(10) 2_454 . ? 
O4 B4 O10 106.9(10) . . ? 
O2 B5 O5 114.6(19) . . ? 
O2 B5 O5 114.6(19) . 3_455 ? 
O5 B5 O5 100(3) . 3_455 ? 
O2 B5 O8 115(3) . . ? 
O5 B5 O8 105.9(18) . . ? 
O5 B5 O8 105.9(18) 3_455 . ? 
O5 B6 O1 124(3) . . ? 
O5 B6 O12' 117(3) . . ? 
O1 B6 O12' 115(3) . . ? 
O5 B6 O12 115(3) . . ? 
O1 B6 O12 117(3) . . ? 
O12' B6 O12 41(2) . . ? 
B6 O1 B6 113(4) 3_455 . ? 
B5 O2 H2A 109.4 . . ? 
B1 O3 B2 122.2(11) 2_454 . ? 
B1 O4 B4 130.2(10) . . ? 
B6 O5 B5 123.5(18) . . ? 
B1 O6 B4 128.6(10) . 2_455 ? 
B3 O7 B4 123.9(11) . . ? 
B3 O9 H9A 109.5 . . ? 
B4 O10 B4 117.8(13) 3_455 . ? 
B4 O10 B2 119.3(6) 3_455 . ? 
B4 O10 B2 119.3(6) . . ? 
B2 O11 H11A 109.6 . . ? 
O12' O12 B6 57(3) . . ? 
O12' O12 H12A 153.6 . . ? 
B6 O12 H12A 124.8 . . ? 
H1WA O1W H1WB 119.4 . . ? 
H2WA O2W H2WB 120.0 . . ? 
O12 O12' B6 82(4) . . ? 
O12 O12' Ba2 116(3) . . ? 
B6 O12' Ba2 111(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    1.810 
_refine_diff_density_min   -2.460 
_refine_diff_density_rms    0.270 