data_hingganite-Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe0.54 Nd4 O20 H4 Si4, 4Be' _chemical_formula_sum 'Be4.08 Fe0.54 Nd3.21 O20 Si3.88' _chemical_formula_analytical ; Nd0.513 Ce0.401 Y0.395 Sm0.175 Gd0.145 Pr0.096 Dy0.068 La0.051 Ca0.041 Eu0.031 Er0.022 Tb0.014 Yb0.011 Ho0.009 Tm0.003 Th0.003 Lu0.001 Fe0.215 Mn0.007 Be1.967 B0.062 Si2 O10 H1.54 ; _chemical_formula_weight 959.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Be' 'Be' 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c 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 4.77193(15) _cell_length_b 7.6422(2) _cell_length_c 9.9299(2) _cell_angle_alpha 90.00 _cell_angle_beta 89.851(2) _cell_angle_gamma 90.00 _cell_volume 362.123(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26222 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 80.6 _exptl_crystal_description Prismatic _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 439 _exptl_absorpt_coefficient_mu 12.304 _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 Supernova _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 25451 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 40.29 _reflns_number_total 2256 _reflns_number_gt 2007 _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^)+(0.0443P)^2^+1.8022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0121(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2256 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _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 Nd1 Nd 0.00129(4) 0.11008(3) 0.331097(18) 0.01245(7) Uani 0.803(5) 1 d P . . Si1 Si 0.51967(17) 0.27494(11) 0.08016(8) 0.0100(2) Uani 0.969(9) 1 d P . . Be1 Be 0.4474(9) 0.4143(5) 0.3377(4) 0.0137(11) Uani 1.02(3) 1 d P . . Fe1 Fe 0.0000 0.0000 0.0000 0.0105(5) Uani 0.272(4) 2 d SP . . O1 O 0.7600(5) 0.4105(3) 0.0335(2) 0.0152(4) Uani 1 1 d . . . O2 O 0.3269(5) 0.2877(3) 0.4529(2) 0.0150(4) Uani 1 1 d . . . O3 O 0.3077(5) 0.3458(3) 0.1974(2) 0.0142(4) Uani 1 1 d . . . O4 O 0.6835(5) 0.1062(3) 0.1453(3) 0.0164(4) Uani 1 1 d . . . O5 O 0.7860(5) 0.4122(3) 0.3333(2) 0.0159(4) Uani 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 Nd1 0.01272(9) 0.01435(9) 0.01027(9) -0.00057(5) -0.00049(5) -0.00034(6) Si1 0.0110(4) 0.0108(3) 0.0083(3) -0.0002(2) 0.0003(2) -0.0001(2) Be1 0.0162(18) 0.0128(17) 0.0121(16) 0.0001(11) -0.0011(11) -0.0008(11) Fe1 0.0100(8) 0.0113(8) 0.0102(8) 0.0018(6) 0.0002(6) 0.0001(6) O1 0.0140(9) 0.0163(9) 0.0152(9) 0.0006(7) 0.0017(7) -0.0030(7) O2 0.0158(9) 0.0174(9) 0.0120(8) 0.0027(7) -0.0021(7) -0.0005(7) O3 0.0144(9) 0.0177(9) 0.0107(8) -0.0019(7) 0.0013(6) 0.0016(7) O4 0.0185(10) 0.0141(9) 0.0166(9) 0.0023(7) -0.0018(7) 0.0019(7) O5 0.0143(9) 0.0207(10) 0.0129(8) -0.0010(7) 0.0000(7) 0.0001(7) _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 Nd1 O1 2.319(2) 4_466 ? Nd1 O1 2.332(2) 2_645 ? Nd1 O4 2.392(3) 1_455 ? Nd1 O2 2.394(2) . ? Nd1 O5 2.444(2) 2_645 ? Nd1 O3 2.517(2) 2_545 ? Nd1 O5 2.527(3) 1_455 ? Nd1 O3 2.671(2) . ? Nd1 Be1 3.107(4) 2_545 ? Nd1 Be1 3.153(4) . ? Nd1 Fe1 3.39371(19) . ? Nd1 Fe1 3.4194(2) 2 ? Si1 O1 1.612(2) . ? Si1 O3 1.633(2) . ? Si1 O2 1.637(2) 4_565 ? Si1 O4 1.642(2) . ? Be1 O4 1.603(5) 2_655 ? Be1 O2 1.603(5) . ? Be1 O5 1.616(5) . ? Be1 O3 1.632(5) . ? Be1 Fe1 2.751(4) 2 ? Be1 Nd1 3.107(4) 2 ? Fe1 O5 2.059(2) 4_465 ? Fe1 O5 2.059(2) 2_645 ? Fe1 O4 2.238(3) 1_455 ? Fe1 O4 2.238(3) 3_655 ? Fe1 O2 2.298(2) 4_565 ? Fe1 O2 2.298(2) 2_545 ? Fe1 Be1 2.751(4) 2_545 ? Fe1 Be1 2.751(4) 4_565 ? Fe1 Nd1 3.39371(19) 3 ? Fe1 Nd1 3.4194(2) 4_565 ? Fe1 Nd1 3.4194(2) 2_545 ? O1 Nd1 2.319(2) 4_665 ? O1 Nd1 2.332(2) 2_655 ? O2 Si1 1.637(2) 4_566 ? O2 Fe1 2.298(2) 2 ? O3 Nd1 2.517(2) 2 ? O4 Be1 1.603(5) 2_645 ? O4 Fe1 2.238(3) 1_655 ? O4 Nd1 2.392(3) 1_655 ? O5 Fe1 2.059(2) 2_655 ? O5 Nd1 2.444(2) 2_655 ? O5 Nd1 2.527(3) 1_655 ? 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 Nd1 O1 72.44(9) 4_466 2_645 ? O1 Nd1 O4 110.71(9) 4_466 1_455 ? O1 Nd1 O4 138.43(8) 2_645 1_455 ? O1 Nd1 O2 85.53(8) 4_466 . ? O1 Nd1 O2 76.17(8) 2_645 . ? O4 Nd1 O2 144.15(8) 1_455 . ? O1 Nd1 O5 137.85(8) 4_466 2_645 ? O1 Nd1 O5 77.16(8) 2_645 2_645 ? O4 Nd1 O5 74.92(8) 1_455 2_645 ? O2 Nd1 O5 114.79(8) . 2_645 ? O1 Nd1 O3 75.73(8) 4_466 2_545 ? O1 Nd1 O3 80.05(8) 2_645 2_545 ? O4 Nd1 O3 61.99(8) 1_455 2_545 ? O2 Nd1 O3 153.27(7) . 2_545 ? O5 Nd1 O3 70.78(8) 2_645 2_545 ? O1 Nd1 O5 81.56(8) 4_466 1_455 ? O1 Nd1 O5 142.33(8) 2_645 1_455 ? O4 Nd1 O5 76.09(8) 1_455 1_455 ? O2 Nd1 O5 75.04(8) . 1_455 ? O5 Nd1 O5 137.67(5) 2_645 1_455 ? O3 Nd1 O5 119.72(8) 2_545 1_455 ? O1 Nd1 O3 138.27(8) 4_466 . ? O1 Nd1 O3 117.38(8) 2_645 . ? O4 Nd1 O3 88.42(8) 1_455 . ? O2 Nd1 O3 60.88(7) . . ? O5 Nd1 O3 81.91(8) 2_645 . ? O3 Nd1 O3 143.64(3) 2_545 . ? O5 Nd1 O3 67.07(7) 1_455 . ? O1 Nd1 Be1 95.38(10) 4_466 2_545 ? O1 Nd1 Be1 109.54(10) 2_645 2_545 ? O4 Nd1 Be1 30.51(9) 1_455 2_545 ? O2 Nd1 Be1 174.23(9) . 2_545 ? O5 Nd1 Be1 68.11(10) 2_645 2_545 ? O3 Nd1 Be1 31.58(9) 2_545 2_545 ? O5 Nd1 Be1 99.43(9) 1_455 2_545 ? O3 Nd1 Be1 115.71(9) . 2_545 ? O1 Nd1 Be1 111.44(10) 4_466 . ? O1 Nd1 Be1 98.02(10) 2_645 . ? O4 Nd1 Be1 117.04(9) 1_455 . ? O2 Nd1 Be1 29.78(9) . . ? O5 Nd1 Be1 101.00(10) 2_645 . ? O3 Nd1 Be1 171.77(9) 2_545 . ? O5 Nd1 Be1 66.46(10) 1_455 . ? O3 Nd1 Be1 31.17(9) . . ? Be1 Nd1 Be1 146.37(7) 2_545 . ? O1 Nd1 Fe1 145.15(6) 4_466 . ? O1 Nd1 Fe1 113.48(6) 2_645 . ? O4 Nd1 Fe1 41.12(6) 1_455 . ? O2 Nd1 Fe1 129.26(6) . . ? O5 Nd1 Fe1 36.99(6) 2_645 . ? O3 Nd1 Fe1 71.91(5) 2_545 . ? O5 Nd1 Fe1 103.49(5) 1_455 . ? O3 Nd1 Fe1 71.83(5) . . ? Be1 Nd1 Fe1 49.83(8) 2_545 . ? Be1 Nd1 Fe1 101.88(7) . . ? O1 Nd1 Fe1 68.51(6) 4_466 2 ? O1 Nd1 Fe1 106.71(6) 2_645 2 ? O4 Nd1 Fe1 112.89(6) 1_455 2 ? O2 Nd1 Fe1 42.13(6) . 2 ? O5 Nd1 Fe1 150.11(6) 2_645 2 ? O3 Nd1 Fe1 138.95(5) 2_545 2 ? O5 Nd1 Fe1 36.80(6) 1_455 2 ? O3 Nd1 Fe1 69.90(5) . 2 ? Be1 Nd1 Fe1 133.15(8) 2_545 2 ? Be1 Nd1 Fe1 49.27(8) . 2 ? Fe1 Nd1 Fe1 133.725(6) . 2 ? O1 Si1 O3 115.51(13) . . ? O1 Si1 O2 111.52(13) . 4_565 ? O3 Si1 O2 107.43(12) . 4_565 ? O1 Si1 O4 106.18(13) . . ? O3 Si1 O4 105.92(13) . . ? O2 Si1 O4 110.08(13) 4_565 . ? O4 Be1 O2 109.7(3) 2_655 . ? O4 Be1 O5 113.7(3) 2_655 . ? O2 Be1 O5 111.7(3) . . ? O4 Be1 O3 102.9(3) 2_655 . ? O2 Be1 O3 105.6(3) . . ? O5 Be1 O3 112.6(3) . . ? O4 Be1 Fe1 54.45(16) 2_655 2 ? O2 Be1 Fe1 56.60(15) . 2 ? O5 Be1 Fe1 142.4(2) . 2 ? O3 Be1 Fe1 105.0(2) . 2 ? O4 Be1 Nd1 49.26(14) 2_655 2 ? O2 Be1 Nd1 115.4(2) . 2 ? O5 Be1 Nd1 132.9(2) . 2 ? O3 Be1 Nd1 53.89(15) . 2 ? Fe1 Be1 Nd1 70.52(10) 2 2 ? O4 Be1 Nd1 114.4(2) 2_655 . ? O2 Be1 Nd1 47.86(14) . . ? O5 Be1 Nd1 131.8(2) . . ? O3 Be1 Nd1 57.88(15) . . ? Fe1 Be1 Nd1 70.41(10) 2 . ? Nd1 Be1 Nd1 82.97(10) 2 . ? O5 Fe1 O5 180.00(15) 4_465 2_645 ? O5 Fe1 O4 93.70(9) 4_465 1_455 ? O5 Fe1 O4 86.30(9) 2_645 1_455 ? O5 Fe1 O4 86.30(9) 4_465 3_655 ? O5 Fe1 O4 93.70(9) 2_645 3_655 ? O4 Fe1 O4 180.00(14) 1_455 3_655 ? O5 Fe1 O2 86.80(9) 4_465 4_565 ? O5 Fe1 O2 93.20(9) 2_645 4_565 ? O4 Fe1 O2 109.38(8) 1_455 4_565 ? O4 Fe1 O2 70.62(8) 3_655 4_565 ? O5 Fe1 O2 93.20(9) 4_465 2_545 ? O5 Fe1 O2 86.80(9) 2_645 2_545 ? O4 Fe1 O2 70.62(8) 1_455 2_545 ? O4 Fe1 O2 109.38(8) 3_655 2_545 ? O2 Fe1 O2 180.00(14) 4_565 2_545 ? O5 Fe1 Be1 99.35(11) 4_465 2_545 ? O5 Fe1 Be1 80.65(11) 2_645 2_545 ? O4 Fe1 Be1 35.64(10) 1_455 2_545 ? O4 Fe1 Be1 144.36(10) 3_655 2_545 ? O2 Fe1 Be1 144.37(10) 4_565 2_545 ? O2 Fe1 Be1 35.63(10) 2_545 2_545 ? O5 Fe1 Be1 80.65(11) 4_465 4_565 ? O5 Fe1 Be1 99.35(11) 2_645 4_565 ? O4 Fe1 Be1 144.36(10) 1_455 4_565 ? O4 Fe1 Be1 35.64(10) 3_655 4_565 ? O2 Fe1 Be1 35.63(10) 4_565 4_565 ? O2 Fe1 Be1 144.37(10) 2_545 4_565 ? Be1 Fe1 Be1 180.00(18) 2_545 4_565 ? O5 Fe1 Nd1 134.42(7) 4_465 . ? O5 Fe1 Nd1 45.58(7) 2_645 . ? O4 Fe1 Nd1 44.65(7) 1_455 . ? O4 Fe1 Nd1 135.35(7) 3_655 . ? O2 Fe1 Nd1 91.11(6) 4_565 . ? O2 Fe1 Nd1 88.89(6) 2_545 . ? Be1 Fe1 Nd1 59.65(8) 2_545 . ? Be1 Fe1 Nd1 120.35(8) 4_565 . ? O5 Fe1 Nd1 45.58(7) 4_465 3 ? O5 Fe1 Nd1 134.42(7) 2_645 3 ? O4 Fe1 Nd1 135.35(7) 1_455 3 ? O4 Fe1 Nd1 44.65(7) 3_655 3 ? O2 Fe1 Nd1 88.89(6) 4_565 3 ? O2 Fe1 Nd1 91.11(6) 2_545 3 ? Be1 Fe1 Nd1 120.35(8) 2_545 3 ? Be1 Fe1 Nd1 59.65(8) 4_565 3 ? Nd1 Fe1 Nd1 180.000(2) . 3 ? O5 Fe1 Nd1 47.32(7) 4_465 4_565 ? O5 Fe1 Nd1 132.68(7) 2_645 4_565 ? O4 Fe1 Nd1 90.03(6) 1_455 4_565 ? O4 Fe1 Nd1 89.97(6) 3_655 4_565 ? O2 Fe1 Nd1 44.32(6) 4_565 4_565 ? O2 Fe1 Nd1 135.68(6) 2_545 4_565 ? Be1 Fe1 Nd1 119.68(8) 2_545 4_565 ? Be1 Fe1 Nd1 60.32(8) 4_565 4_565 ? Nd1 Fe1 Nd1 105.020(3) . 4_565 ? Nd1 Fe1 Nd1 74.980(3) 3 4_565 ? O5 Fe1 Nd1 132.68(7) 4_465 2_545 ? O5 Fe1 Nd1 47.32(7) 2_645 2_545 ? O4 Fe1 Nd1 89.97(6) 1_455 2_545 ? O4 Fe1 Nd1 90.03(6) 3_655 2_545 ? O2 Fe1 Nd1 135.68(6) 4_565 2_545 ? O2 Fe1 Nd1 44.32(6) 2_545 2_545 ? Be1 Fe1 Nd1 60.32(8) 2_545 2_545 ? Be1 Fe1 Nd1 119.68(8) 4_565 2_545 ? Nd1 Fe1 Nd1 74.980(3) . 2_545 ? Nd1 Fe1 Nd1 105.020(3) 3 2_545 ? Nd1 Fe1 Nd1 180.0 4_565 2_545 ? Si1 O1 Nd1 123.82(13) . 4_665 ? Si1 O1 Nd1 127.06(13) . 2_655 ? Nd1 O1 Nd1 107.56(9) 4_665 2_655 ? Be1 O2 Si1 121.8(2) . 4_566 ? Be1 O2 Fe1 87.77(18) . 2 ? Si1 O2 Fe1 115.59(12) 4_566 2 ? Be1 O2 Nd1 102.35(18) . . ? Si1 O2 Nd1 126.23(13) 4_566 . ? Fe1 O2 Nd1 93.55(8) 2 . ? Be1 O3 Si1 117.5(2) . . ? Be1 O3 Nd1 94.53(18) . 2 ? Si1 O3 Nd1 123.20(12) . 2 ? Be1 O3 Nd1 90.96(17) . . ? Si1 O3 Nd1 117.92(12) . . ? Nd1 O3 Nd1 106.08(8) 2 . ? Be1 O4 Si1 125.1(2) 2_645 . ? Be1 O4 Fe1 89.92(18) 2_645 1_655 ? Si1 O4 Fe1 110.64(13) . 1_655 ? Be1 O4 Nd1 100.24(18) 2_645 1_655 ? Si1 O4 Nd1 126.70(13) . 1_655 ? Fe1 O4 Nd1 94.23(9) 1_655 1_655 ? Be1 O5 Fe1 118.23(19) . 2_655 ? Be1 O5 Nd1 115.15(19) . 2_655 ? Fe1 O5 Nd1 97.42(10) 2_655 2_655 ? Be1 O5 Nd1 114.58(19) . 1_655 ? Fe1 O5 Nd1 95.87(9) 2_655 1_655 ? Nd1 O5 Nd1 113.03(9) 2_655 1_655 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 40.29 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.816 _refine_diff_density_min -2.778 _refine_diff_density_rms 0.308 # start Validation Reply Form _vrf_PLAT075_hingganite-Nd ; PROBLEM: Occupancy 1.020 Greater Than 1.0 for ...... BE1 RESPONSE: This site features partial substitution with B atoms in agreement with the chemical analysis. Refinement of the partial site occupancy factors was not possible from XRD data. ; # end Validation Reply Form