# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1978 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Regine Herbst-Irmer Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; _publ_contact_author_phone '049 551 393007' _publ_contact_author_fax '049 551 392582' _publ_contact_author_email rherbst@shelx.uni-ac.gwdg.de _publ_requested_journal ; Dalton Transactions ; _publ_requested_coeditor_name ? _publ_contact_letter ; Here you find the crystallographic data of the publication 'Cis-1.3-diamino-1.3-dichloro-2.4-bis(silyl)cyclodisilazane - synthesis and crystal structure' which is submitted to the journal 'Dalton Transactions', paper ref. B002634O. Sincerely Regine Herbst-Irmer ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Cis-1.3-diamino-1.3-dichloro-2.4-bis(silyl)cyclodisilazane - synthesis and crystal structure ; loop_ _publ_author_name _publ_author_address 'Jaschke, Bettina' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Herbst-Irmer, Regine' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Klingebiel, Uwe' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; 'Pape, Thomas' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 37077 G\"ottingen Germany ; #============================================================================== data_Mol1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H56 Cl2 N4 O Si4' _chemical_formula_weight 575.97 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.733(3) _cell_length_b 22.687(2) _cell_length_c 8.719(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3309.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 10 _cell_measurement_theta_max 25 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7606 _exptl_absorpt_correction_T_max 0.8992 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe-Siemens-Huber four circle diffractometer' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean '8.192 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37478 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2999 _reflns_number_gt 2680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (V. 4.050, Siemens 1996)' _computing_cell_refinement 'Siemens SMART (V. 4.050, Siemens 1996)' _computing_data_reduction 'Siemens SAINT (V. 4.050, Siemens 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (V. 5.05)' _computing_publication_material 'SHELXL-97 (Scheldrick, 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^)+(0.0347P)^2^+2.9875P] 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 0.0014(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2999 _refine_ls_number_parameters 178 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.130 _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 Si1 Si 0.34505(3) 0.38003(2) 0.29172(6) 0.02147(15) Uani 1 1 d . . . Si2 Si 0.28364(4) 0.2500 0.24542(9) 0.02092(18) Uani 1 2 d S . . Si3 Si 0.39887(4) 0.2500 0.41810(9) 0.01996(18) Uani 1 2 d S . . Cl1 Cl 0.37683(5) 0.2500 0.65265(8) 0.03022(19) Uani 1 2 d S . . Cl2 Cl 0.16995(4) 0.2500 0.34076(9) 0.03117(19) Uani 1 2 d S . . N1 N 0.34425(9) 0.30393(7) 0.32519(18) 0.0205(4) Uani 1 1 d . . . N2 N 0.26569(16) 0.2500 0.0569(3) 0.0289(6) Uani 1 2 d SD . . HN1 H 0.2203(15) 0.2500 0.013(4) 0.041(5) Uiso 1 2 d SD . . HN2 H 0.3028(17) 0.2500 -0.010(4) 0.041(5) Uiso 1 2 d SD . . N3 N 0.49854(15) 0.2500 0.4060(3) 0.0281(6) Uani 1 2 d SD . . HN3 H 0.520(2) 0.2500 0.317(3) 0.041(5) Uiso 1 2 d SD . . HN4 H 0.5288(19) 0.2500 0.485(3) 0.041(5) Uiso 1 2 d SD . . C1 C 0.24207(12) 0.39906(9) 0.2168(3) 0.0300(5) Uani 1 1 d . . . H1A H 0.2355 0.3827 0.1136 0.045 Uiso 1 1 calc R . . H1B H 0.2360 0.4420 0.2130 0.045 Uiso 1 1 calc R . . H1C H 0.2015 0.3823 0.2851 0.045 Uiso 1 1 calc R . . C2 C 0.36021(12) 0.42195(9) 0.4788(2) 0.0265(5) Uani 1 1 d . . . C3 C 0.28830(15) 0.40879(11) 0.5840(3) 0.0390(6) Uani 1 1 d . . . H3A H 0.2844 0.3662 0.6011 0.058 Uiso 1 1 calc R . . H3B H 0.2391 0.4229 0.5352 0.058 Uiso 1 1 calc R . . H3C H 0.2956 0.4289 0.6825 0.058 Uiso 1 1 calc R . . C4 C 0.36255(15) 0.48893(10) 0.4488(3) 0.0372(6) Uani 1 1 d . . . H4A H 0.3638 0.5100 0.5468 0.056 Uiso 1 1 calc R . . H4B H 0.3149 0.5006 0.3911 0.056 Uiso 1 1 calc R . . H4C H 0.4105 0.4987 0.3893 0.056 Uiso 1 1 calc R . . C5 C 0.43680(14) 0.40511(10) 0.5647(3) 0.0345(5) Uani 1 1 d . . . H5A H 0.4834 0.4149 0.5015 0.052 Uiso 1 1 calc R . . H5B H 0.4365 0.3627 0.5860 0.052 Uiso 1 1 calc R . . H5C H 0.4395 0.4270 0.6615 0.052 Uiso 1 1 calc R . . C6 C 0.42105(13) 0.39907(9) 0.1346(2) 0.0285(5) Uani 1 1 d . . . C7 C 0.50758(14) 0.40330(11) 0.1920(3) 0.0397(6) Uani 1 1 d . . . H7A H 0.5436 0.4082 0.1043 0.059 Uiso 1 1 calc R . . H7B H 0.5215 0.3672 0.2474 0.059 Uiso 1 1 calc R . . H7C H 0.5128 0.4372 0.2608 0.059 Uiso 1 1 calc R . . C8 C 0.39865(16) 0.45775(10) 0.0555(3) 0.0406(6) Uani 1 1 d . . . H8A H 0.4003 0.4898 0.1309 0.061 Uiso 1 1 calc R . . H8B H 0.3447 0.4547 0.0127 0.061 Uiso 1 1 calc R . . H8C H 0.4368 0.4660 -0.0270 0.061 Uiso 1 1 calc R . . C9 C 0.41779(16) 0.35103(11) 0.0096(3) 0.0400(6) Uani 1 1 d . . . H9A H 0.4528 0.3621 -0.0757 0.060 Uiso 1 1 calc R . . H9B H 0.3628 0.3470 -0.0277 0.060 Uiso 1 1 calc R . . H9C H 0.4357 0.3134 0.0528 0.060 Uiso 1 1 calc R . . C1E C 0.10594(15) 0.30222(10) 0.7487(3) 0.0363(5) Uani 1 1 d . . . H1E1 H 0.0475 0.3047 0.7318 0.044 Uiso 1 1 calc R . . H1E2 H 0.1326 0.3013 0.6474 0.044 Uiso 1 1 calc R . . C2E C 0.13399(15) 0.35486(10) 0.8386(3) 0.0391(6) Uani 1 1 d . . . H2E1 H 0.1092 0.3545 0.9404 0.059 Uiso 1 1 calc R . . H2E2 H 0.1188 0.3910 0.7844 0.059 Uiso 1 1 calc R . . H2E3 H 0.1922 0.3534 0.8495 0.059 Uiso 1 1 calc R . . O1E O 0.12471(12) 0.2500 0.8325(2) 0.0277(5) Uani 1 2 d S . . 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 Si1 0.0235(3) 0.0166(3) 0.0243(3) 0.0006(2) 0.0002(2) 0.0010(2) Si2 0.0211(4) 0.0186(4) 0.0231(4) 0.000 -0.0018(3) 0.000 Si3 0.0220(4) 0.0180(4) 0.0198(4) 0.000 -0.0011(3) 0.000 Cl1 0.0429(4) 0.0275(4) 0.0202(3) 0.000 0.0014(3) 0.000 Cl2 0.0227(4) 0.0347(4) 0.0361(4) 0.000 0.0017(3) 0.000 N1 0.0210(8) 0.0184(9) 0.0222(8) -0.0012(7) -0.0014(7) -0.0007(6) N2 0.0311(14) 0.0334(14) 0.0222(13) 0.000 -0.0063(11) 0.000 N3 0.0240(13) 0.0348(15) 0.0256(14) 0.000 -0.0035(11) 0.000 C1 0.0274(11) 0.0193(10) 0.0434(13) 0.0037(9) -0.0047(10) 0.0061(8) C2 0.0324(11) 0.0189(10) 0.0282(11) -0.0026(8) 0.0047(9) 0.0002(8) C3 0.0460(14) 0.0349(13) 0.0359(12) -0.0058(11) 0.0141(11) -0.0014(11) C4 0.0473(14) 0.0215(11) 0.0429(14) -0.0067(10) 0.0054(11) 0.0002(10) C5 0.0449(13) 0.0296(12) 0.0290(11) -0.0028(10) -0.0047(10) -0.0046(10) C6 0.0353(11) 0.0226(11) 0.0277(11) 0.0020(9) 0.0044(9) -0.0027(9) C7 0.0301(12) 0.0445(14) 0.0444(14) 0.0064(12) 0.0094(10) -0.0032(11) C8 0.0557(15) 0.0285(12) 0.0375(13) 0.0107(10) 0.0046(12) -0.0035(11) C9 0.0544(15) 0.0337(13) 0.0319(12) -0.0025(10) 0.0154(11) -0.0057(11) C1E 0.0469(13) 0.0296(12) 0.0325(11) 0.0044(10) -0.0036(11) 0.0020(10) C2E 0.0444(14) 0.0275(12) 0.0453(14) -0.0011(11) 0.0040(11) -0.0018(10) O1E 0.0299(11) 0.0260(11) 0.0273(11) 0.000 -0.0021(9) 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 Si1 N1 1.7509(17) . ? Si1 C1 1.893(2) . ? Si1 C2 1.905(2) . ? Si1 C6 1.919(2) . ? Si2 N2 1.671(3) . ? Si2 N1 1.7348(16) . ? Si2 N1 1.7348(16) 7_565 ? Si2 Cl2 2.0760(11) . ? Si2 Si3 2.4464(11) . ? Si3 N3 1.671(3) . ? Si3 N1 1.7287(17) 7_565 ? Si3 N1 1.7287(17) . ? Si3 Cl1 2.0780(11) . ? N2 HN1 0.85(2) . ? N2 HN2 0.85(2) . ? N3 HN4 0.86(2) . ? N3 HN3 0.86(2) . ? C2 C5 1.533(3) . ? C2 C3 1.542(3) . ? C2 C4 1.542(3) . ? C6 C7 1.535(3) . ? C6 C9 1.542(3) . ? C6 C8 1.545(3) . ? C1E O1E 1.427(2) . ? C1E C2E 1.504(3) . ? O1E C1E 1.427(2) 7_565 ? 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 N1 Si1 C1 106.00(9) . . ? N1 Si1 C2 110.53(9) . . ? C1 Si1 C2 107.62(10) . . ? N1 Si1 C6 110.25(9) . . ? C1 Si1 C6 107.79(10) . . ? C2 Si1 C6 114.25(9) . . ? N2 Si2 N1 119.97(8) . . ? N2 Si2 N1 119.97(8) . 7_565 ? N1 Si2 N1 89.71(11) . 7_565 ? N2 Si2 Cl2 103.25(10) . . ? N1 Si2 Cl2 112.04(6) . . ? N1 Si2 Cl2 112.04(6) 7_565 . ? N2 Si2 Si3 138.34(10) . . ? N1 Si2 Si3 44.96(6) . . ? N1 Si2 Si3 44.96(6) 7_565 . ? Cl2 Si2 Si3 118.41(5) . . ? N3 Si3 N1 119.87(8) . 7_565 ? N3 Si3 N1 119.87(8) . . ? N1 Si3 N1 90.11(11) 7_565 . ? N3 Si3 Cl1 103.84(10) . . ? N1 Si3 Cl1 111.55(6) 7_565 . ? N1 Si3 Cl1 111.55(6) . . ? N3 Si3 Si2 138.39(10) . . ? N1 Si3 Si2 45.16(5) 7_565 . ? N1 Si3 Si2 45.16(5) . . ? Cl1 Si3 Si2 117.76(4) . . ? Si3 N1 Si2 89.87(8) . . ? Si3 N1 Si1 140.53(10) . . ? Si2 N1 Si1 129.27(10) . . ? HN1 N2 HN2 110(3) . . ? HN1 N2 Si2 127(3) . . ? HN2 N2 Si2 123(3) . . ? HN4 N3 HN3 119(3) . . ? HN4 N3 Si3 123(2) . . ? HN3 N3 Si3 119(2) . . ? C5 C2 C3 108.26(19) . . ? C5 C2 C4 107.89(18) . . ? C3 C2 C4 108.15(18) . . ? C5 C2 Si1 113.91(14) . . ? C3 C2 Si1 107.98(15) . . ? C4 C2 Si1 110.50(15) . . ? C7 C6 C9 107.93(19) . . ? C7 C6 C8 108.68(19) . . ? C9 C6 C8 106.57(19) . . ? C7 C6 Si1 113.99(15) . . ? C9 C6 Si1 108.78(15) . . ? C8 C6 Si1 110.59(15) . . ? O1E C1E C2E 108.90(19) . . ? C1E O1E C1E 112.3(2) 7_565 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 HN1 O1E 0.85(2) 2.25(2) 3.065(3) 162(3) 1_554 N3 HN3 Cl2 0.86(2) 2.86(3) 3.586(3) 144(3) 6_656 N3 HN4 O1E 0.86(2) 2.26(2) 3.107(3) 171(3) 6_657 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.321 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.051 ### END