data_vmx1_220k_up_abs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H B Ca O5 Si' _chemical_formula_weight 159.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.83280(10) _cell_length_b 7.60780(10) _cell_length_c 9.63130(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.173(2) _cell_angle_gamma 90.00 _cell_volume 354.112(9) _cell_formula_units_Z 4 _cell_measurement_temperature 493(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 1.999 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 8566 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 40.07 _reflns_number_total 2204 _reflns_number_gt 1921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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 0.086(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2204 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0472 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.526 _refine_ls_restrained_S_all 1.526 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.99167(3) 0.10622(2) 0.336076(17) 0.00503(4) Uani 1 1 d . . . Si Si 0.46923(5) 0.26636(3) 0.08431(2) 0.00350(5) Uani 1 1 d . . . B B 0.56861(19) 0.41070(11) 0.34077(10) 0.00437(14) Uani 1 1 d . . . O1 O 0.24094(13) 0.40154(8) 0.03724(7) 0.00609(10) Uani 1 1 d . . . O2 O 0.67052(12) 0.30091(8) 0.45754(6) 0.00530(10) Uani 1 1 d . . . O3 O 0.67570(12) 0.33461(8) 0.21059(6) 0.00513(10) Uani 1 1 d . . . O4 O 0.31487(13) 0.08806(7) 0.14589(7) 0.00558(10) Uani 1 1 d . . . O5 O 0.25888(13) 0.41333(8) 0.33645(7) 0.00602(10) Uani 1 1 d . . . H H 0.213(3) 0.448(2) 0.4034(18) 0.030(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.00532(7) 0.00561(6) 0.00415(7) -0.00006(5) 0.00047(5) -0.00031(5) Si 0.00430(9) 0.00358(9) 0.00263(9) -0.00023(7) 0.00020(7) 0.00025(7) B 0.0049(3) 0.0051(3) 0.0031(3) -0.0004(2) 0.0006(3) -0.0001(3) O1 0.0065(2) 0.0063(2) 0.0054(2) -0.00026(19) -0.0005(2) 0.00191(18) O2 0.0058(2) 0.0062(2) 0.0039(2) 0.00123(18) 0.00069(19) 0.00073(18) O3 0.0051(2) 0.0069(2) 0.0034(2) -0.00095(18) 0.00037(18) 0.00019(18) O4 0.0063(2) 0.0041(2) 0.0063(3) 0.00072(18) 0.00191(19) 0.00007(17) O5 0.0044(2) 0.0086(2) 0.0050(3) -0.00111(19) 0.00061(19) 0.00078(19) _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 Ca O1 2.2771(6) 2_645 ? Ca O1 2.2791(6) 4_666 ? Ca O4 2.4148(7) 1_655 ? Ca O2 2.4458(6) . ? Ca O5 2.5236(7) 2_645 ? Ca O3 2.6077(6) . ? Ca O3 2.6572(6) 2_745 ? Ca O5 2.6695(7) 1_655 ? Si O1 1.5740(6) . ? Si O2 1.6451(7) 4_565 ? Si O3 1.6544(6) . ? Si O4 1.6586(6) . ? B O4 1.4676(11) 2_655 ? B O3 1.4761(11) . ? B O2 1.4838(11) . ? B O5 1.4974(11) . ? O1 Ca 2.2771(6) 2_655 ? O1 Ca 2.2791(6) 4_465 ? O2 Si 1.6451(7) 4_566 ? O3 Ca 2.6572(6) 2_755 ? O4 B 1.4676(11) 2_645 ? O4 Ca 2.4148(7) 1_455 ? O5 Ca 2.5236(7) 2_655 ? O5 Ca 2.6695(7) 1_455 ? 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 Ca O1 77.72(2) 2_645 4_666 ? O1 Ca O4 133.54(2) 2_645 1_655 ? O1 Ca O4 107.57(2) 4_666 1_655 ? O1 Ca O2 80.96(2) 2_645 . ? O1 Ca O2 86.77(2) 4_666 . ? O4 Ca O2 144.13(2) 1_655 . ? O1 Ca O5 73.65(2) 2_645 2_645 ? O1 Ca O5 142.75(2) 4_666 2_645 ? O4 Ca O5 77.14(2) 1_655 2_645 ? O2 Ca O5 111.29(2) . 2_645 ? O1 Ca O3 114.50(2) 2_645 . ? O1 Ca O3 135.93(2) 4_666 . ? O4 Ca O3 93.77(2) 1_655 . ? O2 Ca O3 56.40(2) . . ? O5 Ca O3 78.65(2) 2_645 . ? O1 Ca O3 81.88(2) 2_645 2_745 ? O1 Ca O3 78.76(2) 4_666 2_745 ? O4 Ca O3 55.539(19) 1_655 2_745 ? O2 Ca O3 159.55(2) . 2_745 ? O5 Ca O3 74.08(2) 2_645 2_745 ? O3 Ca O3 142.511(10) . 2_745 ? O1 Ca O5 146.86(2) 2_645 1_655 ? O1 Ca O5 76.53(2) 4_666 1_655 ? O4 Ca O5 74.76(2) 1_655 1_655 ? O2 Ca O5 77.12(2) . 1_655 ? O5 Ca O5 137.814(14) 2_645 1_655 ? O3 Ca O5 72.547(19) . 1_655 ? O3 Ca O5 112.83(2) 2_745 1_655 ? O1 Si O2 113.89(3) . 4_565 ? O1 Si O3 115.30(3) . . ? O2 Si O3 106.65(3) 4_565 . ? O1 Si O4 108.77(3) . . ? O2 Si O4 106.18(3) 4_565 . ? O3 Si O4 105.35(3) . . ? O4 B O3 107.43(7) 2_655 . ? O4 B O2 108.96(6) 2_655 . ? O3 B O2 107.85(7) . . ? O4 B O5 111.93(7) 2_655 . ? O3 B O5 109.55(6) . . ? O2 B O5 110.98(7) . . ? Si O1 Ca 129.73(4) . 2_655 ? Si O1 Ca 126.60(3) . 4_465 ? Ca O1 Ca 102.28(2) 2_655 4_465 ? B O2 Si 122.82(5) . 4_566 ? B O2 Ca 100.84(5) . . ? Si O2 Ca 122.97(3) 4_566 . ? B O3 Si 122.36(5) . . ? B O3 Ca 94.24(4) . . ? Si O3 Ca 118.86(3) . . ? B O3 Ca 93.01(4) . 2_755 ? Si O3 Ca 118.92(3) . 2_755 ? Ca O3 Ca 104.05(2) . 2_755 ? B O4 Si 127.62(6) 2_645 . ? B O4 Ca 103.60(5) 2_645 1_455 ? Si O4 Ca 121.14(3) . 1_455 ? B O5 Ca 120.24(5) . 2_655 ? B O5 Ca 118.16(5) . 1_455 ? Ca O5 Ca 106.08(2) 2_655 1_455 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 40.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.536 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.110