data_uk79p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H B Mn2 Na O11 Si3' _chemical_formula_weight 404.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Na' 'Na' 0.0362 0.0249 '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' 'Mn' 'Mn' 0.3368 0.7283 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8370(14) _cell_length_b 7.5750(15) _cell_length_c 8.8410(18) _cell_angle_alpha 99.91(3) _cell_angle_beta 102.19(3) _cell_angle_gamma 102.78(3) _cell_volume 424.81(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(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 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 197 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 4961 _diffrn_reflns_av_R_equivalents 0.0088 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.06 _reflns_number_total 2487 _reflns_number_gt 2409 _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 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^)+(0.0304P)^2^+0.3820P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2487 _refine_ls_number_parameters 171 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0174 _refine_ls_R_factor_gt 0.0168 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.953 _refine_ls_shift/su_mean 0.020 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 Na Na -0.12469(11) 0.64118(9) 0.81008(7) 0.01991(13) Uani 1 1 d . . . Mn1 Mn 0.12800(3) 0.87518(3) 0.60727(2) 0.00946(6) Uani 1 1 d . . . Mn2 Mn -0.38639(3) 0.86495(3) 0.59872(2) 0.01037(6) Uani 1 1 d . . . Si1 Si -0.27055(5) 0.52647(5) 0.38313(4) 0.00756(7) Uani 1 1 d . . . Si2 Si -0.53952(5) 0.74187(5) 0.21311(4) 0.00803(7) Uani 1 1 d . . . Si3 Si 0.01582(5) 0.73835(5) 0.22546(4) 0.00708(7) Uani 1 1 d . . . B B -0.27984(19) 0.87568(18) 0.02906(15) 0.0057(2) Uani 1 1 d . . . O1 O 0.44147(14) 1.07982(13) 0.63879(11) 0.01006(17) Uani 1 1 d . . . O2 O -0.18867(15) 0.68533(13) 0.54738(11) 0.01036(17) Uani 1 1 d . . . O3 O -0.48057(15) 0.78301(14) 0.05236(12) 0.01398(18) Uani 1 1 d . . . O4 O 0.08387(15) 0.92048(13) 0.36857(11) 0.01012(17) Uani 1 1 d . . . O5 O -0.12743(15) 0.77076(14) 0.06979(11) 0.01350(18) Uani 1 1 d . . . O6 O 0.32174(14) 0.68407(13) 0.59757(12) 0.01099(17) Uani 1 1 d . . . O7 O -0.09386(15) 0.55404(13) 0.28046(11) 0.01169(17) Uani 1 1 d . . . O8 O -0.79254(14) 0.67852(13) 0.16777(11) 0.01089(17) Uani 1 1 d . . . O9 O -0.47640(15) 0.56219(13) 0.26884(12) 0.01332(18) Uani 1 1 d . . . OH10 O 0.19850(15) 0.92900(14) 0.86885(12) 0.01274(18) Uani 1 1 d D . . OH11 O -0.3053(2) 0.88051(18) 0.86090(13) 0.0244(3) Uani 1 1 d D . . H1 H 0.287(3) 0.855(3) 0.914(3) 0.053(8) Uiso 1 1 d D . . H2 H -0.417(9) 0.766(7) 0.843(14) 0.39(6) Uiso 1 1 d 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 Na 0.0315(3) 0.0176(3) 0.0158(3) 0.0050(2) 0.0101(2) 0.0123(3) Mn1 0.00913(10) 0.01007(10) 0.00847(10) 0.00136(7) 0.00180(7) 0.00222(7) Mn2 0.01000(10) 0.00983(10) 0.01042(10) 0.00088(7) 0.00130(7) 0.00331(7) Si1 0.00756(15) 0.00623(15) 0.00831(15) 0.00084(11) 0.00175(11) 0.00159(11) Si2 0.00617(15) 0.00776(15) 0.00903(15) 0.00010(12) 0.00117(11) 0.00176(11) Si3 0.00647(15) 0.00763(15) 0.00663(15) 0.00072(11) 0.00146(11) 0.00180(11) B 0.0043(5) 0.0073(5) 0.0046(5) -0.0011(4) 0.0008(4) 0.0020(4) O1 0.0103(4) 0.0086(4) 0.0095(4) 0.0000(3) 0.0012(3) 0.0017(3) O2 0.0110(4) 0.0090(4) 0.0099(4) 0.0003(3) 0.0023(3) 0.0021(3) O3 0.0111(4) 0.0160(4) 0.0128(4) -0.0004(3) 0.0053(3) 0.0004(3) O4 0.0119(4) 0.0088(4) 0.0085(4) 0.0002(3) 0.0021(3) 0.0022(3) O5 0.0144(4) 0.0162(4) 0.0096(4) 0.0009(3) -0.0005(3) 0.0087(4) O6 0.0100(4) 0.0080(4) 0.0155(4) 0.0034(3) 0.0042(3) 0.0021(3) O7 0.0133(4) 0.0095(4) 0.0136(4) 0.0028(3) 0.0072(3) 0.0022(3) O8 0.0067(4) 0.0125(4) 0.0124(4) 0.0000(3) 0.0024(3) 0.0028(3) O9 0.0116(4) 0.0095(4) 0.0161(4) 0.0010(3) -0.0022(3) 0.0041(3) OH10 0.0134(4) 0.0118(4) 0.0123(4) 0.0021(3) 0.0020(3) 0.0037(3) OH11 0.0424(7) 0.0320(6) 0.0092(4) 0.0084(4) 0.0091(4) 0.0259(6) _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 Na O5 2.3423(13) 1_556 ? Na O2 2.3665(12) . ? Na O8 2.4139(13) 2_466 ? Na OH11 2.4407(14) . ? Na O7 2.4770(13) 2_566 ? Na OH10 2.6268(16) . ? Na O9 2.6955(16) 2_466 ? Na B 2.9234(16) 1_556 ? Na Si3 3.1069(10) 2_566 ? Na Si2 3.2220(14) 2_466 ? Na Mn1 3.2232(11) . ? Na Mn2 3.2537(12) . ? Mn1 O4 2.1653(11) . ? Mn1 O6 2.1706(11) . ? Mn1 OH10 2.2056(11) . ? Mn1 O2 2.2164(13) . ? Mn1 O1 2.2810(13) . ? Mn1 O4 2.3556(11) 2_576 ? Mn2 O6 2.1532(12) 1_455 ? Mn2 O2 2.1783(11) . ? Mn2 O1 2.1828(11) 2_576 ? Mn2 O1 2.2327(11) 1_455 ? Mn2 OH11 2.2424(12) . ? Mn2 O4 2.2587(13) 2_576 ? Si1 O6 1.6022(10) 2_566 ? Si1 O2 1.6210(12) . ? Si1 O9 1.6544(11) . ? Si1 O7 1.6564(11) . ? Si2 O1 1.6149(12) 2_576 ? Si2 O3 1.6181(11) . ? Si2 O8 1.6301(11) . ? Si2 O9 1.6379(11) . ? Si2 Na 3.2220(14) 2_466 ? Si3 O5 1.6022(11) . ? Si3 O4 1.6085(12) . ? Si3 O8 1.6272(10) 1_655 ? Si3 O7 1.6348(11) . ? Si3 Na 3.1069(10) 2_566 ? Si3 Na 3.4954(12) 1_554 ? B O5 1.4675(16) . ? B OH11 1.4677(16) 1_554 ? B O3 1.4703(16) . ? B OH10 1.5090(17) 2_576 ? B Na 2.9233(16) 1_554 ? O1 Si2 1.6149(12) 2_576 ? O1 Mn2 2.1828(11) 2_576 ? O1 Mn2 2.2327(11) 1_655 ? O4 Mn2 2.2587(13) 2_576 ? O4 Mn1 2.3556(11) 2_576 ? O5 Na 2.3423(13) 1_554 ? O6 Si1 1.6022(10) 2_566 ? O6 Mn2 2.1532(12) 1_655 ? O7 Na 2.4770(13) 2_566 ? O8 Si3 1.6272(10) 1_455 ? O8 Na 2.4140(13) 2_466 ? O9 Na 2.6955(16) 2_466 ? OH10 B 1.5091(17) 2_576 ? OH11 B 1.4677(16) 1_556 ? 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 O5 Na O2 143.17(4) 1_556 . ? O5 Na O8 96.14(5) 1_556 2_466 ? O2 Na O8 115.38(5) . 2_466 ? O5 Na OH11 59.31(4) 1_556 . ? O2 Na OH11 84.99(5) . . ? O8 Na OH11 130.26(5) 2_466 . ? O5 Na O7 129.06(5) 1_556 2_566 ? O2 Na O7 84.41(4) . 2_566 ? O8 Na O7 62.59(4) 2_466 2_566 ? OH11 Na O7 166.35(5) . 2_566 ? O5 Na OH10 82.51(5) 1_556 . ? O2 Na OH10 84.68(5) . . ? O8 Na OH10 140.01(4) 2_466 . ? OH11 Na OH10 83.17(5) . . ? O7 Na OH10 87.30(4) 2_566 . ? O5 Na O9 93.92(5) 1_556 2_466 ? O2 Na O9 86.64(5) . 2_466 ? O8 Na O9 59.79(4) 2_466 2_466 ? OH11 Na O9 78.18(5) . 2_466 ? O7 Na O9 109.71(4) 2_566 2_466 ? OH10 Na O9 160.03(4) . 2_466 ? O5 Na B 29.84(4) 1_556 1_556 ? O2 Na B 115.06(5) . 1_556 ? O8 Na B 112.02(5) 2_466 1_556 ? OH11 Na B 30.08(4) . 1_556 ? O7 Na B 158.74(4) 2_566 1_556 ? OH10 Na B 86.22(5) . 1_556 ? O9 Na B 81.23(5) 2_466 1_556 ? O5 Na Si3 113.52(4) 1_556 2_566 ? O2 Na Si3 103.25(4) . 2_566 ? O8 Na Si3 31.19(2) 2_466 2_566 ? OH11 Na Si3 161.43(4) . 2_566 ? O7 Na Si3 31.55(3) 2_566 2_566 ? OH10 Na Si3 113.85(4) . 2_566 ? O9 Na Si3 85.64(4) 2_466 2_566 ? B Na Si3 138.41(4) 1_556 2_566 ? O5 Na Si2 93.77(5) 1_556 2_466 ? O2 Na Si2 104.38(5) . 2_466 ? O8 Na Si2 29.41(3) 2_466 2_466 ? OH11 Na Si2 104.26(4) . 2_466 ? O7 Na Si2 86.71(3) 2_566 2_466 ? OH10 Na Si2 168.59(3) . 2_466 ? O9 Na Si2 30.51(3) 2_466 2_466 ? B Na Si2 95.93(4) 1_556 2_466 ? Si3 Na Si2 57.78(2) 2_566 2_466 ? O5 Na Mn1 122.17(4) 1_556 . ? O2 Na Mn1 43.44(3) . . ? O8 Na Mn1 135.68(4) 2_466 . ? OH11 Na Mn1 91.04(4) . . ? O7 Na Mn1 75.34(3) 2_566 . ? OH10 Na Mn1 42.80(3) . . ? O9 Na Mn1 129.91(4) 2_466 . ? B Na Mn1 112.25(4) 1_556 . ? Si3 Na Mn1 106.44(3) 2_566 . ? Si2 Na Mn1 143.61(3) 2_466 . ? O5 Na Mn2 102.83(4) 1_556 . ? O2 Na Mn2 42.01(3) . . ? O8 Na Mn2 131.36(4) 2_466 . ? OH11 Na Mn2 43.53(3) . . ? O7 Na Mn2 126.42(4) 2_566 . ? OH10 Na Mn2 87.16(4) . . ? O9 Na Mn2 74.43(4) 2_466 . ? B Na Mn2 73.44(3) 1_556 . ? Si3 Na Mn2 139.55(3) 2_566 . ? Si2 Na Mn2 104.20(3) 2_466 . ? Mn1 Na Mn2 65.10(2) . . ? O4 Mn1 O6 100.40(4) . . ? O4 Mn1 OH10 161.23(4) . . ? O6 Mn1 OH10 92.05(5) . . ? O4 Mn1 O2 91.72(5) . . ? O6 Mn1 O2 102.69(4) . . ? OH10 Mn1 O2 99.24(5) . . ? O4 Mn1 O1 81.18(5) . . ? O6 Mn1 O1 80.04(4) . . ? OH10 Mn1 O1 87.27(5) . . ? O2 Mn1 O1 172.78(3) . . ? O4 Mn1 O4 82.70(4) . 2_576 ? O6 Mn1 O4 176.86(3) . 2_576 ? OH10 Mn1 O4 85.06(4) . 2_576 ? O2 Mn1 O4 76.63(4) . 2_576 ? O1 Mn1 O4 101.00(4) . 2_576 ? O4 Mn1 Na 138.95(4) . . ? O6 Mn1 Na 90.18(3) . . ? OH10 Mn1 Na 54.02(4) . . ? O2 Mn1 Na 47.24(3) . . ? O1 Mn1 Na 139.86(3) . . ? O4 Mn1 Na 87.14(3) 2_576 . ? O6 Mn2 O2 106.31(4) 1_455 . ? O6 Mn2 O1 103.66(5) 1_455 2_576 ? O2 Mn2 O1 93.13(4) . 2_576 ? O6 Mn2 O1 81.51(4) 1_455 1_455 ? O2 Mn2 O1 171.59(4) . 1_455 ? O1 Mn2 O1 81.82(4) 2_576 1_455 ? O6 Mn2 OH11 84.62(6) 1_455 . ? O2 Mn2 OH11 94.55(5) . . ? O1 Mn2 OH11 166.65(4) 2_576 . ? O1 Mn2 OH11 89.21(5) 1_455 . ? O6 Mn2 O4 171.95(4) 1_455 2_576 ? O2 Mn2 O4 79.46(4) . 2_576 ? O1 Mn2 O4 81.31(5) 2_576 2_576 ? O1 Mn2 O4 93.08(4) 1_455 2_576 ? OH11 Mn2 O4 89.37(6) . 2_576 ? O6 Mn2 Na 92.00(4) 1_455 . ? O2 Mn2 Na 46.65(3) . . ? O1 Mn2 Na 139.73(3) 2_576 . ? O1 Mn2 Na 137.76(3) 1_455 . ? OH11 Mn2 Na 48.56(4) . . ? O4 Mn2 Na 88.02(4) 2_576 . ? O6 Si1 O2 115.70(6) 2_566 . ? O6 Si1 O9 109.76(6) 2_566 . ? O2 Si1 O9 109.51(6) . . ? O6 Si1 O7 108.32(6) 2_566 . ? O2 Si1 O7 108.80(6) . . ? O9 Si1 O7 104.09(6) . . ? O1 Si2 O3 112.18(6) 2_576 . ? O1 Si2 O8 112.53(6) 2_576 . ? O3 Si2 O8 105.30(6) . . ? O1 Si2 O9 108.24(6) 2_576 . ? O3 Si2 O9 115.25(6) . . ? O8 Si2 O9 103.04(6) . . ? O1 Si2 Na 128.59(5) 2_576 2_466 ? O3 Si2 Na 118.55(5) . 2_466 ? O8 Si2 Na 46.65(4) . 2_466 ? O9 Si2 Na 56.68(4) . 2_466 ? O5 Si3 O4 110.79(6) . . ? O5 Si3 O8 104.94(6) . 1_655 ? O4 Si3 O8 114.72(6) . 1_655 ? O5 Si3 O7 112.63(6) . . ? O4 Si3 O7 111.09(6) . . ? O8 Si3 O7 102.33(5) 1_655 . ? O5 Si3 Na 116.00(5) . 2_566 ? O4 Si3 Na 133.13(4) . 2_566 ? O8 Si3 Na 50.19(4) 1_655 2_566 ? O7 Si3 Na 52.46(4) . 2_566 ? O5 Si3 Na 33.88(4) . 1_554 ? O4 Si3 Na 136.68(4) . 1_554 ? O8 Si3 Na 73.38(4) 1_655 1_554 ? O7 Si3 Na 107.94(5) . 1_554 ? Na Si3 Na 86.19(4) 2_566 1_554 ? O5 B OH11 107.56(10) . 1_554 ? O5 B O3 110.25(10) . . ? OH11 B O3 109.30(11) 1_554 . ? O5 B OH10 109.08(10) . 2_576 ? OH11 B OH10 109.83(11) 1_554 2_576 ? O3 B OH10 110.76(10) . 2_576 ? O5 B Na 52.58(6) . 1_554 ? OH11 B Na 56.44(6) 1_554 1_554 ? O3 B Na 114.18(8) . 1_554 ? OH10 B Na 135.01(8) 2_576 1_554 ? Si2 O1 Mn2 116.83(6) 2_576 2_576 ? Si2 O1 Mn2 120.13(6) 2_576 1_655 ? Mn2 O1 Mn2 98.18(4) 2_576 1_655 ? Si2 O1 Mn1 122.50(6) 2_576 . ? Mn2 O1 Mn1 98.08(5) 2_576 . ? Mn2 O1 Mn1 96.00(4) 1_655 . ? Si1 O2 Mn2 118.00(6) . . ? Si1 O2 Mn1 119.36(6) . . ? Mn2 O2 Mn1 104.93(4) . . ? Si1 O2 Na 127.48(6) . . ? Mn2 O2 Na 91.34(4) . . ? Mn1 O2 Na 89.33(5) . . ? B O3 Si2 129.70(9) . . ? Si3 O4 Mn1 116.72(6) . . ? Si3 O4 Mn2 119.13(6) . 2_576 ? Mn1 O4 Mn2 99.27(5) . 2_576 ? Si3 O4 Mn1 121.73(6) . 2_576 ? Mn1 O4 Mn1 97.30(4) . 2_576 ? Mn2 O4 Mn1 98.07(4) 2_576 2_576 ? B O5 Si3 138.69(8) . . ? B O5 Na 97.57(7) . 1_554 ? Si3 O5 Na 123.70(6) . 1_554 ? Si1 O6 Mn2 129.20(6) 2_566 1_655 ? Si1 O6 Mn1 128.20(6) 2_566 . ? Mn2 O6 Mn1 101.76(4) 1_655 . ? Si3 O7 Si1 129.83(6) . . ? Si3 O7 Na 95.99(5) . 2_566 ? Si1 O7 Na 133.75(5) . 2_566 ? Si3 O8 Si2 139.86(7) 1_455 . ? Si3 O8 Na 98.62(5) 1_455 2_466 ? Si2 O8 Na 103.95(6) . 2_466 ? Si2 O9 Si1 135.85(7) . . ? Si2 O9 Na 92.81(5) . 2_466 ? Si1 O9 Na 128.66(6) . 2_466 ? B OH10 Mn1 121.42(8) 2_576 . ? B OH10 Na 138.72(8) 2_576 . ? Mn1 OH10 Na 83.18(5) . . ? B OH11 Mn2 172.54(11) 1_556 . ? B OH11 Na 93.48(8) 1_556 . ? Mn2 OH11 Na 87.91(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.444 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.084