# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Martin Jansen' _publ_contact_author_address ; MPI fur Festkorperforschung Stuttgart D-70569 GERMANY ; _publ_contact_author_email M.JANSEN@FKF.MPG.DE _publ_section_title ; Towards continuous processes for the synthesis of precursors of amorphous Si/B/N/C ceramics ; loop_ _publ_author_name 'M. Jansen' 'Thomas Jaschke' 'Matthias Kroschel' 'Jurgen Nuss' 'Markus Weinmann' data_wei10_m _database_code_depnum_ccdc_archive 'CCDC 656264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C H3 B Cl5 N Si' _chemical_formula_sum 'C H3 B Cl5 N Si' _chemical_formula_weight 245.19 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.0996(13) _cell_length_b 6.8561(12) _cell_length_c 8.9728(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.854(3) _cell_angle_gamma 90.00 _cell_volume 435.19(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4649 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 34.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 1.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6266 _exptl_absorpt_correction_T_max 0.7826 _exptl_absorpt_process_details ; semi empirical absorption correction with SADABS, G.M. Sheldrick, Bruker AXS, Inc. Madison, WI (2003). ; _exptl_special_details ? _diffrn_ambient_temperature 100(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 'SMART APEX, Bruker AXS' _diffrn_measurement_method \wscan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7668 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 34.62 _reflns_number_total 1894 _reflns_number_gt 1697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART32 (Bruker AXS)' _computing_cell_refinement 'SAINT32 (Bruker AXS)' _computing_data_reduction 'SAINT32 (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0327P)^2^+0.1936P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1894 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Cl1 Cl 0.40134(7) 0.2500 1.05566(4) 0.02864(10) Uani 1 2 d S . . Cl2 Cl 0.11437(4) 0.00948(4) 0.82206(3) 0.02473(8) Uani 1 1 d . . . Si Si 0.27900(6) 0.2500 0.84357(5) 0.01784(9) Uani 1 2 d S . . Cl3 Cl 0.16381(6) 0.2500 0.48667(5) 0.02916(10) Uani 1 2 d S . . Cl4 Cl 0.57489(7) 0.2500 0.43389(5) 0.02723(10) Uani 1 2 d S . . N N 0.44899(18) 0.2500 0.71736(14) 0.0180(2) Uani 1 2 d S . . B B 0.4007(3) 0.2500 0.56260(19) 0.0197(3) Uani 1 2 d S . . C C 0.6542(2) 0.2500 0.7713(2) 0.0272(3) Uani 1 2 d S . . H1 H 0.675(5) 0.2500 0.872(4) 0.069(11) Uiso 1 2 d S . . H2 H 0.715(3) 0.141(3) 0.742(2) 0.058(7) 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 Cl1 0.0351(2) 0.0362(2) 0.01410(16) 0.000 -0.00101(14) 0.000 Cl2 0.02346(13) 0.02344(13) 0.02775(14) 0.00089(9) 0.00479(10) -0.00407(9) Si 0.01841(18) 0.02061(19) 0.01456(18) 0.000 0.00176(13) 0.000 Cl3 0.02834(19) 0.0379(2) 0.01972(18) 0.000 -0.00685(14) 0.000 Cl4 0.0366(2) 0.02668(19) 0.01993(17) 0.000 0.01155(15) 0.000 N 0.0166(5) 0.0220(6) 0.0151(5) 0.000 0.0005(4) 0.000 B 0.0238(7) 0.0198(7) 0.0156(7) 0.000 0.0028(6) 0.000 C 0.0165(6) 0.0409(10) 0.0240(8) 0.000 0.0002(5) 0.000 _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 Cl1 Si 2.0240(7) . ? Cl2 Si 2.0210(5) . ? Si N 1.7234(14) . ? Si Cl2 2.0210(4) 4_565 ? Cl3 B 1.7604(19) . ? Cl4 B 1.7620(18) . ? N B 1.402(2) . ? N C 1.496(2) . ? 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 N Si Cl2 111.64(3) . . ? N Si Cl2 111.64(3) . 4_565 ? Cl2 Si Cl2 109.36(3) . 4_565 ? N Si Cl1 110.44(5) . . ? Cl2 Si Cl1 106.768(18) . . ? Cl2 Si Cl1 106.768(18) 4_565 . ? B N C 118.06(13) . . ? B N Si 121.65(11) . . ? C N Si 120.29(11) . . ? N B Cl3 121.93(12) . . ? N B Cl4 121.53(13) . . ? Cl3 B Cl4 116.54(10) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 34.62 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.567 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.083