Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 _database_code_CSD 412000 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Hoppe, Henning A.' 'Kotzyba, Gunter' 'Pottgen, Rainer' 'Schnick, Wolfgang' _publ_contact_author_name 'Prof Wolfgang Schnick' _publ_contact_author_address ; Department of Chemistry Ludwig-Maximilians University of Munich Butenandtstr. 5-13 (D) D-81377 Munich GERMANY ; _publ_contact_author_email 'WSC@CUP.UNI-MUENCHEN.DE' _publ_section_title ; High-Temperature Synthesis, Crystal Structure, Optical Properties, and Magnetism of the Carbidonitridosilicates Ho2[Si4N6C] and Tb2[Si4N6C] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'holmium carbidonitridosilicate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C Ho2 N6 Si4' _chemical_formula_weight 538.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ho' 'Ho' -0.2175 4.6783 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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 5.9314(1) _cell_length_b 9.8974(1) _cell_length_c 11.8859(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.58(1) _cell_angle_gamma 90.00 _cell_volume 606.825(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink/yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 26.610 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0282 _exptl_absorpt_correction_T_max 0.1377 _exptl_absorpt_process_details psi-scans _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 'kappaCCD area detector (Nonius)' _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 18069 _diffrn_reflns_av_R_equivalents 0.0905 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 32.49 _reflns_number_total 2187 _reflns_number_gt 2131 _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^)+(0.0316P)^2^+7.0620P] 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 0.0031(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2187 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.276 _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 Ho1 Ho 0.33162(5) 0.56439(3) 0.09506(3) 0.01058(10) Uani 1 1 d . . . Ho2 Ho 0.66039(5) 0.41486(3) 0.41946(3) 0.00862(10) Uani 1 1 d . . . Si1 Si 0.0051(3) 0.48040(17) 0.24924(16) 0.0077(3) Uani 1 1 d . . . Si2 Si 0.1654(3) 0.21365(19) 0.42073(16) 0.0076(3) Uani 1 1 d . . . Si3 Si 0.2018(3) 0.20588(19) 0.17632(16) 0.0080(3) Uani 1 1 d . . . Si4 Si 0.6767(3) 0.22813(19) 0.15900(16) 0.0080(3) Uani 1 1 d . . . N1 N 0.0426(11) 0.2110(7) 0.0089(5) 0.0145(11) Uani 1 1 d . . . N2 N 0.0592(10) 0.0456(6) 0.3995(5) 0.0093(9) Uani 1 1 d . . . N3 N 0.2407(10) 0.0356(6) 0.2234(5) 0.0099(9) Uani 1 1 d . . . N4 N 0.5068(11) 0.2910(6) 0.0016(5) 0.0115(9) Uani 1 1 d . . . N5 N 0.5173(11) 0.2646(6) 0.2452(6) 0.0110(10) Uani 1 1 d . . . N6 N 0.6998(10) 0.0532(6) 0.1373(5) 0.0095(9) Uani 1 1 d . . . C1 C 0.0224(11) 0.2916(6) 0.2519(6) 0.0076(9) 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 Ho1 0.00994(15) 0.01318(16) 0.00987(14) -0.00223(9) 0.00585(11) -0.00316(9) Ho2 0.00952(15) 0.00902(15) 0.00881(14) 0.00093(8) 0.00567(11) 0.00198(8) Si1 0.0086(7) 0.0069(7) 0.0091(7) 0.0007(5) 0.0055(6) -0.0005(5) Si2 0.0074(7) 0.0089(8) 0.0076(7) -0.0008(5) 0.0045(6) 0.0000(5) Si3 0.0089(7) 0.0086(7) 0.0083(7) -0.0003(5) 0.0055(6) -0.0004(6) Si4 0.0080(7) 0.0086(7) 0.0086(7) -0.0003(5) 0.0049(6) 0.0002(5) N1 0.014(3) 0.026(3) 0.007(2) -0.001(2) 0.008(2) -0.008(2) N2 0.008(2) 0.009(2) 0.012(2) 0.0023(17) 0.0056(18) 0.0004(17) N3 0.011(2) 0.007(2) 0.013(2) 0.0001(17) 0.0069(18) 0.0008(17) N4 0.007(2) 0.015(2) 0.011(2) 0.0033(18) 0.0034(18) -0.0011(18) N5 0.008(2) 0.012(2) 0.014(2) -0.0017(18) 0.007(2) -0.0028(18) N6 0.006(2) 0.009(2) 0.011(2) 0.0014(17) 0.0026(17) 0.0004(16) C1 0.007(2) 0.004(2) 0.012(2) 0.0002(18) 0.0048(19) 0.0001(18) _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 Ho1 N4 2.319(6) 3_665 ? Ho1 N2 2.343(5) 4_565 ? Ho1 N2 2.358(5) 2 ? Ho1 N3 2.402(5) 2_655 ? Ho1 N5 2.579(6) 2_655 ? Ho1 Si3 3.0950(18) 2_655 ? Ho1 Si2 3.2189(17) 2 ? Ho1 Si2 3.2896(19) 4_565 ? Ho1 Si1 3.3621(16) . ? Ho1 Si4 3.3639(17) 2_655 ? Ho1 Ho2 3.4745(4) 2_655 ? Ho1 Ho1 3.6648(6) 3_565 ? Ho2 N1 2.333(6) 4_666 ? Ho2 N6 2.339(5) 2_655 ? Ho2 N5 2.342(6) . ? Ho2 N3 2.375(5) 2_655 ? Ho2 N6 2.502(5) 4_566 ? Ho2 N4 2.610(6) 4_566 ? Ho2 Si4 3.1380(18) 4_566 ? Ho2 Si3 3.3434(18) 2_655 ? Ho2 Si3 3.3738(18) 4_666 ? Ho2 Ho1 3.4745(4) 2_645 ? Ho2 Ho2 3.7044(6) 3_666 ? Si1 N3 1.731(6) 2 ? Si1 N2 1.738(6) 2 ? Si1 N6 1.752(6) 2_655 ? Si1 C1 1.871(6) . ? Si2 N1 1.715(6) 4_566 ? Si2 N2 1.753(6) . ? Si2 N4 1.762(6) 4_566 ? Si2 C1 1.913(6) . ? Si2 Ho1 3.2189(17) 2_545 ? Si2 Ho1 3.2896(19) 4_566 ? Si3 N5 1.731(6) . ? Si3 N1 1.731(6) . ? Si3 N3 1.755(6) . ? Si3 C1 1.898(6) . ? Si3 Ho1 3.0950(18) 2_645 ? Si3 Ho2 3.3434(18) 2_645 ? Si3 Ho2 3.3738(18) 4_465 ? Si4 N5 1.741(6) . ? Si4 N4 1.744(6) . ? Si4 N6 1.766(6) . ? Si4 C1 1.893(6) 1_655 ? Si4 Ho2 3.1380(18) 4_565 ? Si4 Ho1 3.3639(17) 2_645 ? N1 Si2 1.715(6) 4_565 ? N1 Ho2 2.333(6) 4_465 ? N2 Si1 1.738(6) 2_545 ? N2 Ho1 2.343(5) 4_566 ? N2 Ho1 2.358(5) 2_545 ? N3 Si1 1.731(6) 2_545 ? N3 Ho2 2.375(5) 2_645 ? N3 Ho1 2.402(5) 2_645 ? N4 Si2 1.762(6) 4_565 ? N4 Ho1 2.319(6) 3_665 ? N4 Ho2 2.610(6) 4_565 ? N5 Ho1 2.579(6) 2_645 ? N6 Si1 1.752(5) 2_645 ? N6 Ho2 2.339(5) 2_645 ? N6 Ho2 2.502(5) 4_565 ? C1 Si4 1.893(6) 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 N4 Ho1 N2 92.7(2) 3_665 4_565 ? N4 Ho1 N2 135.6(2) 3_665 2 ? N2 Ho1 N2 77.5(2) 4_565 2 ? N4 Ho1 N3 90.40(19) 3_665 2_655 ? N2 Ho1 N3 137.85(19) 4_565 2_655 ? N2 Ho1 N3 125.64(18) 2 2_655 ? N4 Ho1 N5 79.2(2) 3_665 2_655 ? N2 Ho1 N5 154.94(19) 4_565 2_655 ? N2 Ho1 N5 91.71(18) 2 2_655 ? N3 Ho1 N5 66.47(18) 2_655 2_655 ? N4 Ho1 Si3 75.33(15) 3_665 2_655 ? N2 Ho1 Si3 163.96(13) 4_565 2_655 ? N2 Ho1 Si3 118.47(13) 2 2_655 ? N3 Ho1 Si3 34.40(14) 2_655 2_655 ? N5 Ho1 Si3 34.00(13) 2_655 2_655 ? N4 Ho1 Si2 106.18(15) 3_665 2 ? N2 Ho1 Si2 89.54(13) 4_565 2 ? N2 Ho1 Si2 32.16(14) 2 2 ? N3 Ho1 Si2 129.62(13) 2_655 2 ? N5 Ho1 Si2 70.48(13) 2_655 2 ? Si3 Ho1 Si2 103.87(5) 2_655 2 ? N4 Ho1 Si2 105.84(16) 3_665 4_565 ? N2 Ho1 Si2 30.81(14) 4_565 4_565 ? N2 Ho1 Si2 87.59(13) 2 4_565 ? N3 Ho1 Si2 108.77(14) 2_655 4_565 ? N5 Ho1 Si2 173.41(13) 2_655 4_565 ? Si3 Ho1 Si2 142.34(5) 2_655 4_565 ? Si2 Ho1 Si2 111.47(4) 2 4_565 ? N4 Ho1 Si1 155.94(16) 3_665 . ? N2 Ho1 Si1 97.18(13) 4_565 . ? N2 Ho1 Si1 29.19(14) 2 . ? N3 Ho1 Si1 96.78(13) 2_655 . ? N5 Ho1 Si1 82.71(13) 2_655 . ? Si3 Ho1 Si1 98.00(4) 2_655 . ? Si2 Ho1 Si1 52.26(4) 2 . ? Si2 Ho1 Si1 93.57(4) 4_565 . ? N4 Ho1 Si4 108.68(16) 3_665 2_655 ? N2 Ho1 Si4 141.90(13) 4_565 2_655 ? N2 Ho1 Si4 65.04(13) 2 2_655 ? N3 Ho1 Si4 74.85(13) 2_655 2_655 ? N5 Ho1 Si4 30.59(13) 2_655 2_655 ? Si3 Ho1 Si4 53.80(4) 2_655 2_655 ? Si2 Ho1 Si4 54.81(4) 2 2_655 ? Si2 Ho1 Si4 145.28(4) 4_565 2_655 ? Si1 Ho1 Si4 52.12(4) . 2_655 ? N4 Ho1 Ho2 48.70(16) 3_665 2_655 ? N2 Ho1 Ho2 115.73(14) 4_565 2_655 ? N2 Ho1 Ho2 96.77(14) 2 2_655 ? N3 Ho1 Ho2 97.41(13) 2_655 2_655 ? N5 Ho1 Ho2 42.39(13) 2_655 2_655 ? Si3 Ho1 Ho2 64.13(3) 2_655 2_655 ? Si2 Ho1 Ho2 64.75(3) 2 2_655 ? Si2 Ho1 Ho2 144.20(3) 4_565 2_655 ? Si1 Ho1 Ho2 107.43(3) . 2_655 ? Si4 Ho1 Ho2 64.44(3) 2_655 2_655 ? N4 Ho1 Ho1 119.32(14) 3_665 3_565 ? N2 Ho1 Ho1 38.92(13) 4_565 3_565 ? N2 Ho1 Ho1 38.63(13) 2 3_565 ? N3 Ho1 Ho1 148.09(13) 2_655 3_565 ? N5 Ho1 Ho1 126.75(13) 2_655 3_565 ? Si3 Ho1 Ho1 157.09(3) 2_655 3_565 ? Si2 Ho1 Ho1 56.65(3) 2 3_565 ? Si2 Ho1 Ho1 54.82(3) 4_565 3_565 ? Si1 Ho1 Ho1 61.20(3) . 3_565 ? Si4 Ho1 Ho1 103.39(3) 2_655 3_565 ? Ho2 Ho1 Ho1 110.696(13) 2_655 3_565 ? N1 Ho2 N6 171.03(19) 4_666 2_655 ? N1 Ho2 N5 84.9(2) 4_666 . ? N6 Ho2 N5 103.6(2) 2_655 . ? N1 Ho2 N3 93.8(2) 4_666 2_655 ? N6 Ho2 N3 90.71(19) 2_655 2_655 ? N5 Ho2 N3 78.28(19) . 2_655 ? N1 Ho2 N6 91.28(18) 4_666 4_566 ? N6 Ho2 N6 80.2(2) 2_655 4_566 ? N5 Ho2 N6 143.43(19) . 4_566 ? N3 Ho2 N6 138.29(19) 2_655 4_566 ? N1 Ho2 N4 81.5(2) 4_666 4_566 ? N6 Ho2 N4 97.28(19) 2_655 4_566 ? N5 Ho2 N4 78.11(19) . 4_566 ? N3 Ho2 N4 156.26(18) 2_655 4_566 ? N6 Ho2 N4 65.36(18) 4_566 4_566 ? N1 Ho2 Si4 75.99(15) 4_666 4_566 ? N6 Ho2 Si4 98.06(14) 2_655 4_566 ? N5 Ho2 Si4 110.56(14) . 4_566 ? N3 Ho2 Si4 165.45(14) 2_655 4_566 ? N6 Ho2 Si4 34.20(13) 4_566 4_566 ? N4 Ho2 Si4 33.76(13) 4_566 4_566 ? N1 Ho2 Si3 105.63(17) 4_666 2_655 ? N6 Ho2 Si3 74.91(14) 2_655 2_655 ? N5 Ho2 Si3 106.79(14) . 2_655 ? N3 Ho2 Si3 30.11(14) 2_655 2_655 ? N6 Ho2 Si3 109.25(13) 4_566 2_655 ? N4 Ho2 Si3 171.47(13) 4_566 2_655 ? Si4 Ho2 Si3 142.58(5) 4_566 2_655 ? N1 Ho2 Si3 28.55(14) 4_666 4_666 ? N6 Ho2 Si3 142.58(14) 2_655 4_666 ? N5 Ho2 Si3 110.05(15) . 4_666 ? N3 Ho2 Si3 111.37(13) 2_655 4_666 ? N6 Ho2 Si3 63.09(12) 4_566 4_666 ? N4 Ho2 Si3 74.76(13) 4_566 4_666 ? Si4 Ho2 Si3 55.25(4) 4_566 4_666 ? Si3 Ho2 Si3 109.25(4) 2_655 4_666 ? N1 Ho2 Ho1 57.01(18) 4_666 2_645 ? N6 Ho2 Ho1 127.07(14) 2_655 2_645 ? N5 Ho2 Ho1 47.93(14) . 2_645 ? N3 Ho2 Ho1 116.90(13) 2_655 2_645 ? N6 Ho2 Ho1 100.43(13) 4_566 2_645 ? N4 Ho2 Ho1 41.86(12) 4_566 2_645 ? Si4 Ho2 Ho1 66.41(3) 4_566 2_645 ? Si3 Ho2 Ho1 146.26(3) 2_655 2_645 ? Si3 Ho2 Ho1 70.19(3) 4_666 2_645 ? N1 Ho2 Ho1 126.00(13) 4_666 . ? N6 Ho2 Ho1 61.61(14) 2_655 . ? N5 Ho2 Ho1 63.51(15) . . ? N3 Ho2 Ho1 40.15(13) 2_655 . ? N6 Ho2 Ho1 140.07(13) 4_566 . ? N4 Ho2 Ho1 127.30(12) 4_566 . ? Si4 Ho2 Ho1 153.97(3) 4_566 . ? Si3 Ho2 Ho1 52.16(3) 2_655 . ? Si3 Ho2 Ho1 150.38(3) 4_666 . ? Ho1 Ho2 Ho1 111.349(9) 2_645 . ? N1 Ho2 Ho2 129.70(13) 4_666 3_666 ? N6 Ho2 Ho2 41.73(13) 2_655 3_666 ? N5 Ho2 Ho2 133.74(14) . 3_666 ? N3 Ho2 Ho2 120.80(13) 2_655 3_666 ? N6 Ho2 Ho2 38.48(12) 4_566 3_666 ? N4 Ho2 Ho2 78.37(12) 4_566 3_666 ? Si4 Ho2 Ho2 61.96(3) 4_566 3_666 ? Si3 Ho2 Ho2 93.34(3) 2_655 3_666 ? Si3 Ho2 Ho2 101.29(3) 4_666 3_666 ? Ho1 Ho2 Ho2 120.195(14) 2_645 3_666 ? Ho1 Ho2 Ho2 102.574(12) . 3_666 ? N3 Si1 N2 107.0(3) 2 2 ? N3 Si1 N6 109.8(3) 2 2_655 ? N2 Si1 N6 105.3(3) 2 2_655 ? N3 Si1 C1 110.8(3) 2 . ? N2 Si1 C1 111.7(3) 2 . ? N6 Si1 C1 111.8(3) 2_655 . ? N3 Si1 Ho1 142.1(2) 2 . ? N2 Si1 Ho1 41.41(18) 2 . ? N6 Si1 Ho1 72.11(19) 2_655 . ? C1 Si1 Ho1 102.40(19) . . ? N1 Si2 N2 105.7(3) 4_566 . ? N1 Si2 N4 113.5(3) 4_566 4_566 ? N2 Si2 N4 106.8(3) . 4_566 ? N1 Si2 C1 111.3(3) 4_566 . ? N2 Si2 C1 106.9(3) . . ? N4 Si2 C1 112.2(3) 4_566 . ? N1 Si2 Ho1 65.3(2) 4_566 2_545 ? N2 Si2 Ho1 45.74(18) . 2_545 ? N4 Si2 Ho1 142.4(2) 4_566 2_545 ? C1 Si2 Ho1 101.82(19) . 2_545 ? N1 Si2 Ho1 93.7(2) 4_566 4_566 ? N2 Si2 Ho1 43.21(18) . 4_566 ? N4 Si2 Ho1 74.2(2) 4_566 4_566 ? C1 Si2 Ho1 146.9(2) . 4_566 ? Ho1 Si2 Ho1 68.53(4) 2_545 4_566 ? N5 Si3 N1 112.5(3) . . ? N5 Si3 N3 103.3(3) . . ? N1 Si3 N3 107.8(3) . . ? N5 Si3 C1 110.7(3) . . ? N1 Si3 C1 114.5(3) . . ? N3 Si3 C1 107.1(3) . . ? N5 Si3 Ho1 56.4(2) . 2_645 ? N1 Si3 Ho1 140.0(2) . 2_645 ? N3 Si3 Ho1 50.63(18) . 2_645 ? C1 Si3 Ho1 104.71(19) . 2_645 ? N5 Si3 Ho2 93.5(2) . 2_645 ? N1 Si3 Ho2 73.8(2) . 2_645 ? N3 Si3 Ho2 42.73(18) . 2_645 ? C1 Si3 Ho2 146.6(2) . 2_645 ? Ho1 Si3 Ho2 69.29(4) 2_645 2_645 ? N5 Si3 Ho2 150.6(2) . 4_465 ? N1 Si3 Ho2 40.1(2) . 4_465 ? N3 Si3 Ho2 82.24(19) . 4_465 ? C1 Si3 Ho2 94.65(19) . 4_465 ? Ho1 Si3 Ho2 132.33(6) 2_645 4_465 ? Ho2 Si3 Ho2 70.75(4) 2_645 4_465 ? N5 Si4 N4 111.3(3) . . ? N5 Si4 N6 113.1(3) . . ? N4 Si4 N6 103.8(3) . . ? N5 Si4 C1 109.5(3) . 1_655 ? N4 Si4 C1 113.2(3) . 1_655 ? N6 Si4 C1 105.7(3) . 1_655 ? N5 Si4 Ho2 147.7(2) . 4_565 ? N4 Si4 Ho2 56.3(2) . 4_565 ? N6 Si4 Ho2 52.77(18) . 4_565 ? C1 Si4 Ho2 102.60(19) 1_655 4_565 ? N5 Si4 Ho1 48.9(2) . 2_645 ? N4 Si4 Ho1 148.8(2) . 2_645 ? N6 Si4 Ho1 71.95(19) . 2_645 ? C1 Si4 Ho1 97.43(19) 1_655 2_645 ? Ho2 Si4 Ho1 124.34(6) 4_565 2_645 ? Si2 N1 Si3 124.0(3) 4_565 . ? Si2 N1 Ho2 124.3(3) 4_565 4_465 ? Si3 N1 Ho2 111.4(3) . 4_465 ? Si1 N2 Si2 112.4(3) 2_545 . ? Si1 N2 Ho1 122.3(3) 2_545 4_566 ? Si2 N2 Ho1 106.0(3) . 4_566 ? Si1 N2 Ho1 109.4(3) 2_545 2_545 ? Si2 N2 Ho1 102.1(2) . 2_545 ? Ho1 N2 Ho1 102.5(2) 4_566 2_545 ? Si1 N3 Si3 111.9(3) 2_545 . ? Si1 N3 Ho2 120.3(3) 2_545 2_645 ? Si3 N3 Ho2 107.2(3) . 2_645 ? Si1 N3 Ho1 118.9(3) 2_545 2_645 ? Si3 N3 Ho1 95.0(2) . 2_645 ? Ho2 N3 Ho1 100.25(19) 2_645 2_645 ? Si4 N4 Si2 118.4(3) . 4_565 ? Si4 N4 Ho1 126.2(3) . 3_665 ? Si2 N4 Ho1 113.0(3) 4_565 3_665 ? Si4 N4 Ho2 90.0(3) . 4_565 ? Si2 N4 Ho2 107.1(3) 4_565 4_565 ? Ho1 N4 Ho2 89.44(19) 3_665 4_565 ? Si3 N5 Si4 115.2(3) . . ? Si3 N5 Ho2 117.8(3) . . ? Si4 N5 Ho2 125.9(3) . . ? Si3 N5 Ho1 89.6(2) . 2_645 ? Si4 N5 Ho1 100.5(3) . 2_645 ? Ho2 N5 Ho1 89.7(2) . 2_645 ? Si1 N6 Si4 114.3(3) 2_645 . ? Si1 N6 Ho2 113.9(3) 2_645 2_645 ? Si4 N6 Ho2 119.3(3) . 2_645 ? Si1 N6 Ho2 113.3(3) 2_645 4_565 ? Si4 N6 Ho2 93.0(2) . 4_565 ? Ho2 N6 Ho2 99.8(2) 2_645 4_565 ? Si1 C1 Si4 106.7(3) . 1_455 ? Si1 C1 Si3 118.5(3) . . ? Si4 C1 Si3 105.9(3) 1_455 . ? Si1 C1 Si2 114.4(3) . . ? Si4 C1 Si2 105.6(3) 1_455 . ? Si3 C1 Si2 104.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.205 _refine_diff_density_min -4.715 _refine_diff_density_rms 0.498