# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Philip Mountford' 'Michael G. Cushion' 'Robbert Duchateau' 'Alexander F. R. Kilpatrick' 'Shaneesh Vadake Kulangara' _publ_contact_author_name 'Philip Mountford' _publ_contact_author_email PHILIP.MOUNTFORD@CHEM.OX.AC.UK _publ_section_title ; Synthesis and ethylene trimerisation capability of new chromium(II) and chromium(III) heteroscorpionate complexes ; # Attachment 'B926333K.CIF' data_compound_10 _database_code_depnum_ccdc_archive 'CCDC 758105' #TrackingRef 'B926333K.CIF' # Local code mgc20 _chemical_name_systematic ; Cr{HC(Me2pz)2SiMe2N(H)iPr}Cl3 . 0.75(CH2Cl2) ; _publ_section_exptl_refinement ; The atoms of the SiMe2N(H) moiety were positionally disordered over two sites. The disorder was modelled adequately and refinement proceeded normally subject to similarity restraints applied to the positional and displacement parameters of the affected fragment. Residual electron density was modelled a 0.75 fractional occupancy CH2Cl2 molecule of crystallization ; _chemical_melting_point ? _cell_length_a 10.13760(10) _cell_length_b 14.1035(2) _cell_length_c 18.5130(3) _cell_angle_alpha 90 _cell_angle_beta 98.8488(6) _cell_angle_gamma 90 _cell_volume 2615.40(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C16.75 H30.50 Cl4.50 Cr1 N5 Si1' _chemical_formula_moiety 'C16 H29 Cl3 Cr1 N5 Si1, 0.75 (C H2 Cl2)' _chemical_compound_source ? _chemical_formula_weight 541.58 _cell_measurement_reflns_used 6176 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour 'lime green' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.83 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11908 _reflns_number_total 5950 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_min 5.140 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.928 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.39 _oxford_diffrn_Wilson_scale 19.08 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.60 _refine_diff_density_max 1.27 _refine_ls_number_reflns 4021 _refine_ls_number_restraints 44 _refine_ls_number_parameters 298 _refine_ls_wR_factor_ref 0.0497 _refine_ls_goodness_of_fit_ref 1.1094 _refine_ls_R_factor_all 0.0752 _refine_ls_wR_factor_all 0.0587 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4021 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_gt 0.0497 _refine_ls_shift/su_max 0.0002 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.05 1.06 1.10 0.435 0.355 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cr1 Cr 0.28745(4) 0.33627(3) 0.14677(3) 0.0201 1.0000 Uani . . . . . . N1 N 0.4980(2) 0.34683(17) 0.15088(13) 0.0214 1.0000 Uani . . . . . . N2 N 0.5699(2) 0.40609(19) 0.20106(15) 0.0269 1.0000 Uani . . . . . . N3 N 0.3220(2) 0.36058(18) 0.26142(14) 0.0245 1.0000 Uani . . . . . . N4 N 0.4287(3) 0.41509(19) 0.29106(14) 0.0260 1.0000 Uani . . . . . . N5 N 0.2840(9) 0.4854(7) 0.1193(4) 0.0198 0.5000 Uani D . . . . . N51 N 0.2594(8) 0.4897(7) 0.1416(5) 0.0214 0.5000 Uani D . . . . . Si1 Si 0.3674(3) 0.5563(2) 0.19225(16) 0.0286 0.5000 Uani D U . . . . Si11 Si 0.4071(3) 0.5552(2) 0.17187(15) 0.0225 0.5000 Uani D U . . . . C1 C 0.5892(3) 0.2982(2) 0.12043(17) 0.0244 1.0000 Uani . . . . . . C2 C 0.7177(3) 0.3273(2) 0.15123(18) 0.0307 1.0000 Uani . . . . . . C3 C 0.7032(3) 0.3953(3) 0.20232(19) 0.0314 1.0000 Uani . . . . . . C4 C 0.5581(3) 0.2248(3) 0.0627(2) 0.0344 1.0000 Uani . . . . . . C5 C 0.8064(4) 0.4500(4) 0.2524(3) 0.0539 1.0000 Uani . . . . . . C6 C 0.2760(3) 0.3220(2) 0.31940(18) 0.0287 1.0000 Uani . . . . . . C7 C 0.3530(4) 0.3520(2) 0.38401(18) 0.0333 1.0000 Uani . . . . . . C8 C 0.4505(4) 0.4100(2) 0.36526(17) 0.0316 1.0000 Uani . . . . . . C9 C 0.1602(4) 0.2555(3) 0.3148(2) 0.0405 1.0000 Uani . . . . . . C10 C 0.5660(4) 0.4584(3) 0.41098(19) 0.0414 1.0000 Uani . . . . . . C11 C 0.4991(3) 0.4701(2) 0.24270(16) 0.0218 1.0000 Uani . . . . . . C12 C 0.4505(9) 0.6595(5) 0.1602(5) 0.0521 0.5000 Uani D U . . . . C13 C 0.2633(8) 0.5872(6) 0.2629(4) 0.0481 0.5000 Uani D U . . . . C14 C 0.1587(3) 0.5262(2) 0.07426(19) 0.0325 1.0000 Uani . . . . . . C15 C 0.0644(4) 0.5868(3) 0.1097(2) 0.0465 1.0000 Uani . . . . . . C16 C 0.2132(4) 0.5777(3) 0.0138(2) 0.0494 1.0000 Uani . . . . . . C101 C -0.0089(6) 0.6257(4) 0.4583(3) 0.0636 0.7500 Uani D U . . . . C121 C 0.5204(7) 0.5712(6) 0.1049(4) 0.0376 0.5000 Uani D U . . . . C131 C 0.3684(8) 0.6665(5) 0.2168(4) 0.0434 0.5000 Uani D U . . . . Cl1 Cl 0.25924(8) 0.31944(7) 0.02164(4) 0.0360 1.0000 Uani . . . . . . Cl2 Cl 0.06134(7) 0.33583(6) 0.14949(4) 0.0315 1.0000 Uani . . . . . . Cl3 Cl 0.30800(8) 0.17360(5) 0.16716(5) 0.0319 1.0000 Uani . . . . . . Cl101 Cl 0.0907(3) 0.5651(2) 0.40571(17) 0.1097 0.7500 Uani D U . . . . Cl102 Cl 0.0851(2) 0.65741(14) 0.54225(14) 0.0937 0.7500 Uani D U . . . . H1 H 0.3403 0.4873 0.0883 0.0330 0.5000 Uiso R . . . . . H11 H 0.2141 0.4990 0.1773 0.0338 0.5000 Uiso R . . . . . H21 H 0.8037 0.3030 0.1382 0.0367 1.0000 Uiso R . . . . . H41 H 0.6428 0.1990 0.0491 0.0422 1.0000 Uiso R . . . . . H42 H 0.5035 0.2539 0.0187 0.0422 1.0000 Uiso R . . . . . H43 H 0.5065 0.1723 0.0815 0.0422 1.0000 Uiso R . . . . . H51 H 0.8975 0.4303 0.2440 0.0657 1.0000 Uiso R . . . . . H52 H 0.7940 0.5193 0.2420 0.0657 1.0000 Uiso R . . . . . H53 H 0.7962 0.4372 0.3044 0.0657 1.0000 Uiso R . . . . . H71 H 0.3396 0.3347 0.4347 0.0402 1.0000 Uiso R . . . . . H91 H 0.1455 0.2368 0.3651 0.0504 1.0000 Uiso R . . . . . H92 H 0.0785 0.2877 0.2890 0.0504 1.0000 Uiso R . . . . . H93 H 0.1791 0.1976 0.2869 0.0504 1.0000 Uiso R . . . . . H101 H 0.5636 0.4462 0.4640 0.0482 1.0000 Uiso R . . . . . H102 H 0.5604 0.5282 0.4015 0.0482 1.0000 Uiso R . . . . . H103 H 0.6513 0.4333 0.3976 0.0482 1.0000 Uiso R . . . . . H111 H 0.5683 0.5082 0.2745 0.0265 1.0000 Uiso R . . . . . H121 H 0.3818 0.7037 0.1343 0.0608 0.5000 Uiso R . . . . . H122 H 0.5033 0.6930 0.2028 0.0608 0.5000 Uiso R . . . . . H123 H 0.5116 0.6384 0.1258 0.0608 0.5000 Uiso R . . . . . H131 H 0.1913 0.6321 0.2417 0.0552 0.5000 Uiso R . . . . . H132 H 0.3200 0.6177 0.3056 0.0552 0.5000 Uiso R . . . . . H133 H 0.2222 0.5281 0.2795 0.0552 0.5000 Uiso R . . . . . H141 H 0.1055 0.4714 0.0512 0.0377 1.0000 Uiso R . . . . . H151 H -0.0120 0.6073 0.0723 0.0550 1.0000 Uiso R . . . . . H152 H 0.1137 0.6439 0.1316 0.0550 1.0000 Uiso R . . . . . H153 H 0.0298 0.5500 0.1490 0.0550 1.0000 Uiso R . . . . . H161 H 0.1381 0.6071 -0.0202 0.0601 1.0000 Uiso R . . . . . H162 H 0.2758 0.6284 0.0358 0.0601 1.0000 Uiso R . . . . . H163 H 0.2623 0.5322 -0.0139 0.0601 1.0000 Uiso R . . . . . H1011 H -0.0448 0.6843 0.4318 0.0744 0.7500 Uiso R . . . . . H1012 H -0.0847 0.5842 0.4672 0.0744 0.7500 Uiso R . . . . . H1211 H 0.4789 0.6152 0.0655 0.0431 0.5000 Uiso R . . . . . H1212 H 0.6063 0.5989 0.1299 0.0431 0.5000 Uiso R . . . . . H1213 H 0.5383 0.5086 0.0829 0.0431 0.5000 Uiso R . . . . . H1311 H 0.3202 0.7107 0.1795 0.0473 0.5000 Uiso R . . . . . H1312 H 0.4532 0.6969 0.2406 0.0473 0.5000 Uiso R . . . . . H1313 H 0.3108 0.6522 0.2547 0.0473 0.5000 Uiso R . . . . . 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 Cr1 0.0156(2) 0.0212(2) 0.0230(2) -0.00039(19) 0.00123(17) 0.00096(18) N1 0.0178(11) 0.0241(13) 0.0220(12) 0.0002(10) 0.0015(9) -0.0026(10) N2 0.0172(12) 0.0329(14) 0.0311(14) -0.0100(11) 0.0056(10) -0.0031(10) N3 0.0202(12) 0.0297(13) 0.0240(13) 0.0016(10) 0.0051(10) -0.0034(10) N4 0.0270(13) 0.0311(14) 0.0201(13) 0.0020(10) 0.0039(10) -0.0062(11) N5 0.022(4) 0.024(3) 0.013(4) 0.003(3) 0.001(3) 0.001(3) N51 0.027(4) 0.025(3) 0.014(4) 0.000(3) 0.008(3) 0.004(3) Si1 0.0313(16) 0.0197(10) 0.0316(15) 0.0021(10) -0.0052(10) -0.0023(11) Si11 0.0197(12) 0.0219(9) 0.0259(13) 0.0032(9) 0.0031(8) 0.0010(9) C1 0.0234(14) 0.0259(15) 0.0248(15) -0.0003(12) 0.0070(12) 0.0015(12) C2 0.0188(14) 0.0396(18) 0.0350(17) -0.0047(15) 0.0086(12) 0.0003(13) C3 0.0179(15) 0.0392(18) 0.0375(18) -0.0072(15) 0.0060(13) -0.0043(13) C4 0.0277(16) 0.0368(18) 0.0394(19) -0.0097(15) 0.0076(14) 0.0051(14) C5 0.0238(18) 0.072(3) 0.066(3) -0.033(2) 0.0068(18) -0.0087(18) C6 0.0267(15) 0.0324(17) 0.0286(15) 0.0035(13) 0.0088(12) 0.0005(13) C7 0.0396(18) 0.0375(19) 0.0244(16) 0.0053(14) 0.0097(14) -0.0025(15) C8 0.0396(19) 0.0334(17) 0.0217(16) 0.0029(13) 0.0045(14) -0.0033(14) C9 0.0325(18) 0.049(2) 0.042(2) 0.0102(17) 0.0109(15) -0.0112(16) C10 0.051(2) 0.045(2) 0.0250(17) 0.0020(15) -0.0040(15) -0.0119(17) C11 0.0205(13) 0.0237(14) 0.0215(14) -0.0007(11) 0.0047(11) -0.0013(11) C12 0.052(4) 0.040(4) 0.056(4) 0.012(4) -0.018(4) -0.012(3) C13 0.054(4) 0.048(4) 0.040(4) -0.016(3) -0.001(3) 0.021(3) C14 0.0267(16) 0.0273(16) 0.0391(19) 0.0064(14) -0.0089(14) 0.0023(13) C15 0.040(2) 0.043(2) 0.052(2) 0.0009(18) -0.0058(18) 0.0076(17) C16 0.044(2) 0.046(2) 0.056(3) 0.015(2) 0.0019(19) 0.0011(18) C101 0.041(3) 0.050(3) 0.093(5) 0.029(3) -0.010(3) 0.000(3) C121 0.029(3) 0.047(4) 0.037(4) 0.018(3) 0.008(3) 0.000(3) C131 0.044(4) 0.035(3) 0.045(4) -0.013(3) -0.013(3) 0.009(3) Cl1 0.0324(4) 0.0493(5) 0.0243(4) -0.0069(3) -0.0014(3) 0.0106(4) Cl2 0.0165(3) 0.0382(4) 0.0396(4) 0.0035(3) 0.0035(3) -0.0001(3) Cl3 0.0283(4) 0.0218(4) 0.0443(5) 0.0015(3) 0.0015(3) 0.0012(3) Cl101 0.1051(18) 0.1002(17) 0.127(2) -0.0142(15) 0.0275(15) -0.0227(14) Cl102 0.0749(12) 0.0614(11) 0.1279(18) -0.0104(11) -0.0377(12) 0.0133(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2178(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 . N1 . 2.129(2) yes Cr1 . N3 . 2.125(3) yes Cr1 . N5 . 2.163(10) yes Cr1 . N51 . 2.182(11) yes Cr1 . Cl1 . 2.3023(9) yes Cr1 . Cl2 . 2.3005(8) yes Cr1 . Cl3 . 2.3292(9) yes N1 . N2 . 1.373(3) yes N1 . C1 . 1.343(4) yes N2 . C3 . 1.357(4) yes N2 . C11 . 1.447(4) yes N3 . N4 . 1.371(4) yes N3 . C6 . 1.349(4) yes N4 . C8 . 1.359(4) yes N4 . C11 . 1.452(4) yes N5 . Si1 . 1.786(6) yes N5 . C14 . 1.521(10) yes N5 . H1 . 0.870 no N51 . Si11 . 1.776(7) yes N51 . C14 . 1.572(11) yes N51 . H11 . 0.870 no Si1 . C11 . 1.937(4) yes Si1 . C12 . 1.826(7) yes Si1 . C13 . 1.855(7) yes Si11 . C11 . 1.912(4) yes Si11 . C121 . 1.829(6) yes Si11 . C131 . 1.847(6) yes C1 . C2 . 1.401(4) yes C1 . C4 . 1.485(4) yes C2 . C3 . 1.370(5) yes C2 . H21 . 1.000 no C3 . C5 . 1.500(5) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C4 . H43 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.390(5) yes C6 . C9 . 1.494(5) yes C7 . C8 . 1.369(5) yes C7 . H71 . 1.000 no C8 . C10 . 1.499(5) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . H111 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C14 . C15 . 1.506(5) yes C14 . C16 . 1.509(5) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C15 . H152 . 1.000 no C15 . H153 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C101 . Cl101 . 1.733(6) yes C101 . Cl102 . 1.751(6) yes C101 . H1011 . 1.000 no C101 . H1012 . 1.000 no C121 . H1211 . 1.000 no C121 . H1212 . 1.000 no C121 . H1213 . 1.000 no C131 . H1311 . 1.000 no C131 . H1312 . 1.000 no C131 . H1313 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Cr1 . N3 . 86.72(9) yes N1 . Cr1 . N5 . 85.4(2) yes N3 . Cr1 . N5 . 94.15(19) yes N1 . Cr1 . N51 . 93.2(2) yes N3 . Cr1 . N51 . 83.3(2) yes N5 . Cr1 . N51 . 13.7(2) yes N1 . Cr1 . Cl1 . 90.68(7) yes N3 . Cr1 . Cl1 . 175.88(8) yes N5 . Cr1 . Cl1 . 82.44(18) yes N51 . Cr1 . Cl1 . 93.6(2) yes N1 . Cr1 . Cl2 . 174.95(7) yes N3 . Cr1 . Cl2 . 89.44(7) yes N5 . Cr1 . Cl2 . 91.6(2) yes N51 . Cr1 . Cl2 . 83.10(19) yes Cl1 . Cr1 . Cl2 . 92.97(3) yes N1 . Cr1 . Cl3 . 89.94(7) yes N3 . Cr1 . Cl3 . 90.01(7) yes N5 . Cr1 . Cl3 . 173.6(2) yes N51 . Cr1 . Cl3 . 172.47(19) yes Cl1 . Cr1 . Cl3 . 93.19(4) yes Cl2 . Cr1 . Cl3 . 93.35(3) yes Cr1 . N1 . N2 . 119.47(18) yes Cr1 . N1 . C1 . 134.5(2) yes N2 . N1 . C1 . 105.5(2) yes N1 . N2 . C3 . 111.6(2) yes N1 . N2 . C11 . 119.0(2) yes C3 . N2 . C11 . 129.4(3) yes Cr1 . N3 . N4 . 119.27(18) yes Cr1 . N3 . C6 . 134.9(2) yes N4 . N3 . C6 . 104.8(2) yes N3 . N4 . C8 . 111.8(3) yes N3 . N4 . C11 . 119.0(2) yes C8 . N4 . C11 . 129.2(3) yes Cr1 . N5 . Si1 . 112.2(5) yes Cr1 . N5 . C14 . 118.6(4) yes Si1 . N5 . C14 . 117.4(6) yes Cr1 . N5 . H1 . 101.3 no Si1 . N5 . H1 . 101.5 no C14 . N5 . H1 . 101.8 no Cr1 . N51 . Si11 . 113.8(5) yes Cr1 . N51 . C14 . 115.1(4) yes Si11 . N51 . C14 . 119.5(6) yes Cr1 . N51 . H11 . 101.4 no Si11 . N51 . H11 . 101.5 no C14 . N51 . H11 . 101.4 no N5 . Si1 . C11 . 102.9(4) yes N5 . Si1 . C12 . 112.9(4) yes C11 . Si1 . C12 . 109.8(3) yes N5 . Si1 . C13 . 114.2(4) yes C11 . Si1 . C13 . 103.4(3) yes C12 . Si1 . C13 . 112.5(5) yes N51 . Si11 . C11 . 100.9(4) yes N51 . Si11 . C121 . 116.0(4) yes C11 . Si11 . C121 . 104.6(3) yes N51 . Si11 . C131 . 110.9(4) yes C11 . Si11 . C131 . 109.9(3) yes C121 . Si11 . C131 . 113.5(4) yes N1 . C1 . C2 . 109.7(3) yes N1 . C1 . C4 . 125.0(3) yes C2 . C1 . C4 . 125.3(3) yes C1 . C2 . C3 . 107.1(3) yes C1 . C2 . H21 . 126.3 no C3 . C2 . H21 . 126.5 no C2 . C3 . N2 . 106.2(3) yes C2 . C3 . C5 . 130.4(3) yes N2 . C3 . C5 . 123.4(3) yes C1 . C4 . H41 . 109.9 no C1 . C4 . H42 . 109.2 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.3 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.5 no C3 . C5 . H52 . 109.2 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.7 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 110.1(3) yes N3 . C6 . C9 . 124.9(3) yes C7 . C6 . C9 . 124.9(3) yes C6 . C7 . C8 . 107.2(3) yes C6 . C7 . H71 . 126.4 no C8 . C7 . H71 . 126.3 no C7 . C8 . N4 . 106.0(3) yes C7 . C8 . C10 . 131.4(3) yes N4 . C8 . C10 . 122.6(3) yes C6 . C9 . H91 . 109.9 no C6 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.9 no C8 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.2 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N4 . C11 . N2 . 109.1(2) yes N4 . C11 . Si1 . 105.3(2) yes N2 . C11 . Si1 . 119.8(2) yes N4 . C11 . Si11 . 121.6(2) yes N2 . C11 . Si11 . 104.8(2) yes Si1 . C11 . Si11 . 17.70(8) yes N4 . C11 . H111 . 106.9 no N2 . C11 . H111 . 106.8 no Si1 . C11 . H111 . 108.4 no Si11 . C11 . H111 . 106.9 no Si1 . C12 . H121 . 109.3 no Si1 . C12 . H122 . 109.8 no H121 . C12 . H122 . 109.5 no Si1 . C12 . H123 . 109.3 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no Si1 . C13 . H131 . 109.4 no Si1 . C13 . H132 . 109.8 no H131 . C13 . H132 . 109.5 no Si1 . C13 . H133 . 109.3 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N5 . C14 . N51 . 19.2(3) yes N5 . C14 . C15 . 120.5(4) yes N51 . C14 . C15 . 102.6(4) yes N5 . C14 . C16 . 102.6(4) yes N51 . C14 . C16 . 118.6(4) yes C15 . C14 . C16 . 112.4(3) yes N5 . C14 . H141 . 106.9 no N51 . C14 . H141 . 109.1 no C15 . C14 . H141 . 106.8 no C16 . C14 . H141 . 106.8 no C14 . C15 . H151 . 109.7 no C14 . C15 . H152 . 108.8 no H151 . C15 . H152 . 109.5 no C14 . C15 . H153 . 109.9 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no C14 . C16 . H161 . 109.6 no C14 . C16 . H162 . 108.9 no H161 . C16 . H162 . 109.5 no C14 . C16 . H163 . 109.9 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Cl101 . C101 . Cl102 . 109.9(3) yes Cl101 . C101 . H1011 . 109.4 no Cl102 . C101 . H1011 . 109.4 no Cl101 . C101 . H1012 . 109.4 no Cl102 . C101 . H1012 . 109.3 no H1011 . C101 . H1012 . 109.5 no Si11 . C121 . H1211 . 109.5 no Si11 . C121 . H1212 . 109.1 no H1211 . C121 . H1212 . 109.5 no Si11 . C121 . H1213 . 109.8 no H1211 . C121 . H1213 . 109.5 no H1212 . C121 . H1213 . 109.5 no Si11 . C131 . H1311 . 109.5 no Si11 . C131 . H1312 . 109.5 no H1311 . C131 . H1312 . 109.5 no Si11 . C131 . H1313 . 109.4 no H1311 . C131 . H1313 . 109.5 no H1312 . C131 . H1313 . 109.5 no #===end data_compound_11 _database_code_depnum_ccdc_archive 'CCDC 758106' #TrackingRef 'B926333K.CIF' # Local code mgc23 _chemical_name_systematic ; Cr{HC(Me2pz)2SiMe2N(H)Ph}Cl3 .CH2Cl2 ; _chemical_melting_point ? _publ_section_exptl_refinement ; C-H atoms were placed in calculated positions with methyl group orientations checked against a Fourier difference map. H(1) was located from a Fourier difference synthesis and positionally and isotropically refined ; _cell_length_a 8.5884(2) _cell_length_b 11.9779(4) _cell_length_c 13.6741(5) _cell_angle_alpha 75.1113(14) _cell_angle_beta 76.7912(14) _cell_angle_gamma 76.1372(17) _cell_volume 1298.79(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cr 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C20 H29 Cl5 Cr1 N5 Si1' _chemical_formula_moiety 'C18 H27 Cl3 Cr1 N5 Si1, CH2Cl2' _chemical_compound_source ? _chemical_formula_weight 596.83 _cell_measurement_reflns_used 5667 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10110 _reflns_number_total 5903 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_min 5.135 _diffrn_reflns_theta_max 27.489 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.939 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -10 _reflns_limit_h_max 11 _reflns_limit_k_min -14 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 2.58 _oxford_diffrn_Wilson_scale 3.39 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.40 _refine_diff_density_max 1.15 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4369 _refine_ls_number_restraints 0 _refine_ls_number_parameters 293 _oxford_refine_ls_R_factor_ref 0.0450 _refine_ls_wR_factor_ref 0.0448 _refine_ls_goodness_of_fit_ref 1.1225 _refine_ls_shift/su_max 0.000314 # The values computed from all data _oxford_reflns_number_all 5903 _refine_ls_R_factor_all 0.0669 _refine_ls_wR_factor_all 0.0578 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4716 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_gt 0.0467 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.893 0.239 0.725 0.786E-01 0.247 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cr1 Cr 0.22246(5) 0.17722(4) 0.22817(4) 0.0248 1.0000 Uani . . . . . . . N1 N 0.1399(3) 0.2462(2) 0.0851(2) 0.0270 1.0000 Uani . . . . . . . N2 N -0.0201(3) 0.3046(2) 0.08495(19) 0.0253 1.0000 Uani . . . . . . . N3 N 0.0341(3) 0.3092(2) 0.28641(19) 0.0262 1.0000 Uani . . . . . . . N4 N -0.1120(3) 0.3431(2) 0.25217(19) 0.0257 1.0000 Uani . . . . . . . N5 N 0.0451(3) 0.0609(2) 0.2701(3) 0.0375 1.0000 Uani . . . . . . . Si1 Si -0.14761(9) 0.12246(7) 0.22930(7) 0.0261 1.0000 Uani . . . . . . . C1 C 0.2130(4) 0.2664(3) -0.0145(2) 0.0318 1.0000 Uani . . . . . . . C2 C 0.0994(4) 0.3350(3) -0.0757(3) 0.0333 1.0000 Uani . . . . . . . C3 C -0.0466(4) 0.3587(3) -0.0113(2) 0.0294 1.0000 Uani . . . . . . . C4 C 0.3893(4) 0.2237(3) -0.0502(3) 0.0427 1.0000 Uani . . . . . . . C5 C -0.2073(4) 0.4308(3) -0.0327(3) 0.0384 1.0000 Uani . . . . . . . C6 C 0.0263(4) 0.3819(3) 0.3489(2) 0.0293 1.0000 Uani . . . . . . . C7 C -0.1242(4) 0.4591(3) 0.3543(2) 0.0319 1.0000 Uani . . . . . . . C8 C -0.2106(4) 0.4339(3) 0.2925(2) 0.0276 1.0000 Uani . . . . . . . C9 C 0.1593(4) 0.3773(3) 0.4045(3) 0.0387 1.0000 Uani . . . . . . . C10 C -0.3765(4) 0.4861(3) 0.2679(3) 0.0348 1.0000 Uani . . . . . . . C11 C -0.1395(3) 0.2853(3) 0.1784(2) 0.0251 1.0000 Uani . . . . . . . C12 C -0.1742(4) 0.0725(3) 0.1187(3) 0.0337 1.0000 Uani . . . . . . . C13 C -0.3025(4) 0.1049(3) 0.3461(3) 0.0376 1.0000 Uani . . . . . . . C14 C 0.0982(3) -0.0641(3) 0.2724(2) 0.0291 1.0000 Uani . . . . . . . C15 C 0.1521(4) -0.1023(4) 0.1798(3) 0.0468 1.0000 Uani . . . . . . . C16 C 0.1973(5) -0.2176(4) 0.1763(4) 0.0532 1.0000 Uani . . . . . . . C17 C 0.1953(5) -0.2987(4) 0.2678(4) 0.0537 1.0000 Uani . . . . . . . C18 C 0.1463(5) -0.2705(4) 0.3622(4) 0.0510 1.0000 Uani . . . . . . . C19 C 0.0936(4) -0.1472(4) 0.3651(3) 0.0511 1.0000 Uani . . . . . . . Cl1 Cl 0.42132(9) 0.03364(7) 0.17031(7) 0.0365 1.0000 Uani . . . . . . . Cl2 Cl 0.26486(9) 0.09805(7) 0.39648(6) 0.0339 1.0000 Uani . . . . . . . Cl3 Cl 0.40381(9) 0.30634(7) 0.18188(6) 0.0318 1.0000 Uani . . . . . . . H1 H 0.053(12) 0.057(9) 0.346(8) 0.20(4) 1.0000 Uiso . . . . . . . H21 H 0.1195 0.3603 -0.1485 0.0409 1.0000 Uiso R . . . . . . H41 H 0.4150 0.2477 -0.1229 0.0513 1.0000 Uiso R . . . . . . H42 H 0.4523 0.2555 -0.0193 0.0513 1.0000 Uiso R . . . . . . H43 H 0.4132 0.1402 -0.0310 0.0513 1.0000 Uiso R . . . . . . H51 H -0.2006 0.4612 -0.1046 0.0462 1.0000 Uiso R . . . . . . H52 H -0.2366 0.4941 0.0020 0.0462 1.0000 Uiso R . . . . . . H53 H -0.2875 0.3827 -0.0090 0.0462 1.0000 Uiso R . . . . . . H71 H -0.1604 0.5183 0.3936 0.0394 1.0000 Uiso R . . . . . . H91 H 0.1275 0.4367 0.4436 0.0502 1.0000 Uiso R . . . . . . H92 H 0.2554 0.3899 0.3560 0.0502 1.0000 Uiso R . . . . . . H93 H 0.1797 0.3023 0.4490 0.0502 1.0000 Uiso R . . . . . . H101 H -0.4254 0.5481 0.3031 0.0432 1.0000 Uiso R . . . . . . H102 H -0.3687 0.5162 0.1959 0.0432 1.0000 Uiso R . . . . . . H103 H -0.4414 0.4272 0.2890 0.0432 1.0000 Uiso R . . . . . . H111 H -0.2429 0.3236 0.1609 0.0317 1.0000 Uiso R . . . . . . H121 H -0.2786 0.1089 0.1019 0.0423 1.0000 Uiso R . . . . . . H122 H -0.1654 -0.0106 0.1357 0.0423 1.0000 Uiso R . . . . . . H123 H -0.0923 0.0933 0.0614 0.0423 1.0000 Uiso R . . . . . . H131 H -0.4078 0.1363 0.3289 0.0444 1.0000 Uiso R . . . . . . H132 H -0.2850 0.1457 0.3925 0.0444 1.0000 Uiso R . . . . . . H133 H -0.2950 0.0237 0.3775 0.0444 1.0000 Uiso R . . . . . . H151 H 0.1577 -0.0449 0.1172 0.0640 1.0000 Uiso R . . . . . . H161 H 0.2290 -0.2417 0.1125 0.0683 1.0000 Uiso R . . . . . . H171 H 0.2301 -0.3795 0.2652 0.0627 1.0000 Uiso R . . . . . . H181 H 0.1478 -0.3299 0.4235 0.0647 1.0000 Uiso R . . . . . . H191 H 0.0557 -0.1229 0.4287 0.0662 1.0000 Uiso R . . . . . . C101 C 0.5357(5) 0.8102(4) 0.3960(4) 0.0623 1.0000 Uani . . . . . . . Cl101 Cl 0.48956(11) 0.67728(8) 0.47584(7) 0.0454 1.0000 Uani . . . . . . . Cl102 Cl 0.72606(11) 0.78851(8) 0.31605(7) 0.0446 1.0000 Uani . . . . . . . H1011 H 0.5360 0.8624 0.4379 0.0651 1.0000 Uiso R . . . . . . H1012 H 0.4544 0.8442 0.3544 0.0651 1.0000 Uiso R . . . . . . 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 Cr1 0.0196(2) 0.0238(2) 0.0325(3) -0.00703(19) -0.00847(18) -0.00251(17) N1 0.0210(12) 0.0289(13) 0.0327(13) -0.0117(11) -0.0068(10) -0.0004(10) N2 0.0227(11) 0.0250(12) 0.0287(13) -0.0074(10) -0.0068(10) -0.0014(9) N3 0.0206(11) 0.0282(13) 0.0322(13) -0.0082(10) -0.0100(10) -0.0020(9) N4 0.0207(11) 0.0253(12) 0.0325(13) -0.0094(10) -0.0082(10) -0.0007(9) N5 0.0269(13) 0.0266(13) 0.063(2) -0.0092(13) -0.0170(13) -0.0042(11) Si1 0.0208(4) 0.0250(4) 0.0342(4) -0.0070(3) -0.0075(3) -0.0043(3) C1 0.0293(15) 0.0344(16) 0.0339(17) -0.0120(13) -0.0042(13) -0.0063(13) C2 0.0373(17) 0.0356(17) 0.0289(16) -0.0073(13) -0.0073(13) -0.0086(14) C3 0.0342(16) 0.0276(15) 0.0301(16) -0.0088(12) -0.0082(13) -0.0077(12) C4 0.0314(17) 0.054(2) 0.0399(19) -0.0148(17) -0.0007(14) -0.0020(15) C5 0.0395(18) 0.0333(17) 0.0414(19) -0.0050(14) -0.0158(15) -0.0002(14) C6 0.0317(15) 0.0280(15) 0.0317(16) -0.0088(12) -0.0117(13) -0.0040(12) C7 0.0343(16) 0.0292(15) 0.0355(17) -0.0127(13) -0.0097(13) -0.0029(13) C8 0.0245(14) 0.0244(14) 0.0324(16) -0.0073(12) -0.0048(12) -0.0010(11) C9 0.0399(18) 0.0399(18) 0.045(2) -0.0191(15) -0.0181(15) -0.0025(15) C10 0.0279(15) 0.0346(17) 0.0435(19) -0.0153(14) -0.0103(14) 0.0024(13) C11 0.0200(13) 0.0277(14) 0.0300(15) -0.0101(12) -0.0067(11) -0.0027(11) C12 0.0299(16) 0.0334(16) 0.0402(18) -0.0093(14) -0.0080(13) -0.0074(13) C13 0.0344(17) 0.0387(18) 0.0383(18) -0.0056(14) -0.0070(14) -0.0067(14) C14 0.0224(14) 0.0276(15) 0.0384(17) -0.0072(13) -0.0063(12) -0.0056(11) C15 0.0341(18) 0.055(2) 0.061(2) -0.0290(19) -0.0055(17) -0.0112(16) C16 0.047(2) 0.049(2) 0.071(3) -0.024(2) -0.014(2) -0.0055(18) C17 0.037(2) 0.051(2) 0.067(3) -0.005(2) -0.0107(19) -0.0050(17) C18 0.041(2) 0.044(2) 0.070(3) -0.0097(19) -0.0113(19) -0.0127(17) C19 0.0343(19) 0.061(2) 0.060(3) -0.004(2) -0.0152(17) -0.0147(17) Cl1 0.0242(3) 0.0301(4) 0.0536(5) -0.0122(3) -0.0047(3) -0.0011(3) Cl2 0.0320(4) 0.0329(4) 0.0393(4) -0.0058(3) -0.0156(3) -0.0040(3) Cl3 0.0274(4) 0.0304(4) 0.0404(4) -0.0054(3) -0.0110(3) -0.0087(3) C101 0.045(2) 0.036(2) 0.081(3) 0.001(2) 0.012(2) 0.0015(17) Cl101 0.0456(5) 0.0483(5) 0.0436(5) -0.0085(4) -0.0054(4) -0.0155(4) Cl102 0.0372(4) 0.0406(5) 0.0505(5) -0.0083(4) -0.0010(4) -0.0050(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4699(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 . N1 . 2.129(3) yes Cr1 . N3 . 2.141(2) yes Cr1 . N5 . 2.190(3) yes Cr1 . Cl1 . 2.2747(9) yes Cr1 . Cl2 . 2.3291(9) yes Cr1 . Cl3 . 2.3280(8) yes N1 . N2 . 1.385(3) yes N1 . C1 . 1.349(4) yes N2 . C3 . 1.354(4) yes N2 . C11 . 1.450(4) yes N3 . N4 . 1.373(3) yes N3 . C6 . 1.350(4) yes N4 . C8 . 1.363(4) yes N4 . C11 . 1.448(4) yes N5 . Si1 . 1.794(3) yes N5 . C14 . 1.451(4) yes N5 . H1 . 1.04(10) yes Si1 . C11 . 1.908(3) yes Si1 . C12 . 1.840(3) yes Si1 . C13 . 1.832(3) yes C1 . C2 . 1.402(4) yes C1 . C4 . 1.488(4) yes C2 . C3 . 1.371(5) yes C2 . H21 . 0.950 no C3 . C5 . 1.490(4) yes C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.950 no C6 . C7 . 1.397(4) yes C6 . C9 . 1.493(4) yes C7 . C8 . 1.372(4) yes C7 . H71 . 0.950 no C8 . C10 . 1.490(4) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . H111 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.398(5) yes C14 . C19 . 1.396(5) yes C15 . C16 . 1.352(5) yes C15 . H151 . 0.950 no C16 . C17 . 1.372(6) yes C16 . H161 . 0.950 no C17 . C18 . 1.367(6) yes C17 . H171 . 0.950 no C18 . C19 . 1.445(6) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no C101 . Cl101 . 1.759(4) yes C101 . Cl102 . 1.750(4) yes C101 . H1011 . 0.950 no C101 . H1012 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Cr1 . N3 . 86.54(9) yes N1 . Cr1 . N5 . 88.12(11) yes N3 . Cr1 . N5 . 88.27(10) yes N1 . Cr1 . Cl1 . 94.65(7) yes N3 . Cr1 . Cl1 . 178.49(8) yes N5 . Cr1 . Cl1 . 90.83(8) yes N1 . Cr1 . Cl2 . 169.78(7) yes N3 . Cr1 . Cl2 . 87.63(7) yes N5 . Cr1 . Cl2 . 83.33(9) yes Cl1 . Cr1 . Cl2 . 91.06(3) yes N1 . Cr1 . Cl3 . 90.56(7) yes N3 . Cr1 . Cl3 . 90.15(7) yes N5 . Cr1 . Cl3 . 178.00(8) yes Cl1 . Cr1 . Cl3 . 90.77(3) yes Cl2 . Cr1 . Cl3 . 97.84(3) yes Cr1 . N1 . N2 . 118.98(18) yes Cr1 . N1 . C1 . 135.0(2) yes N2 . N1 . C1 . 104.9(2) yes N1 . N2 . C3 . 111.7(2) yes N1 . N2 . C11 . 119.2(2) yes C3 . N2 . C11 . 128.1(2) yes Cr1 . N3 . N4 . 120.80(18) yes Cr1 . N3 . C6 . 133.76(19) yes N4 . N3 . C6 . 105.2(2) yes N3 . N4 . C8 . 111.8(2) yes N3 . N4 . C11 . 119.0(2) yes C8 . N4 . C11 . 129.1(2) yes Cr1 . N5 . Si1 . 116.33(14) yes Cr1 . N5 . C14 . 120.64(19) yes Si1 . N5 . C14 . 113.8(2) yes Cr1 . N5 . H1 . 85(6) yes Si1 . N5 . H1 . 118(6) yes C14 . N5 . H1 . 97(6) yes N5 . Si1 . C11 . 103.39(12) yes N5 . Si1 . C12 . 114.65(15) yes C11 . Si1 . C12 . 104.64(14) yes N5 . Si1 . C13 . 105.96(16) yes C11 . Si1 . C13 . 109.47(15) yes C12 . Si1 . C13 . 117.75(16) yes N1 . C1 . C2 . 109.8(3) yes N1 . C1 . C4 . 123.6(3) yes C2 . C1 . C4 . 126.7(3) yes C1 . C2 . C3 . 107.4(3) yes C1 . C2 . H21 . 126.4 no C3 . C2 . H21 . 126.3 no C2 . C3 . N2 . 106.2(3) yes C2 . C3 . C5 . 131.2(3) yes N2 . C3 . C5 . 122.6(3) yes C1 . C4 . H41 . 109.7 no C1 . C4 . H42 . 109.5 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.2 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.6 no C3 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.5 no C3 . C5 . H53 . 109.2 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no N3 . C6 . C7 . 109.7(3) yes N3 . C6 . C9 . 124.3(3) yes C7 . C6 . C9 . 126.0(3) yes C6 . C7 . C8 . 107.5(3) yes C6 . C7 . H71 . 126.3 no C8 . C7 . H71 . 126.2 no C7 . C8 . N4 . 105.8(3) yes C7 . C8 . C10 . 132.0(3) yes N4 . C8 . C10 . 122.3(3) yes C6 . C9 . H91 . 109.7 no C6 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.5 no C6 . C9 . H93 . 109.3 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.5 no C8 . C10 . H102 . 109.6 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.3 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . N4 . 109.6(2) yes N2 . C11 . Si1 . 111.84(19) yes N4 . C11 . Si1 . 114.5(2) yes N2 . C11 . H111 . 106.7 no N4 . C11 . H111 . 106.8 no Si1 . C11 . H111 . 106.9 no Si1 . C12 . H121 . 109.5 no Si1 . C12 . H122 . 109.5 no H121 . C12 . H122 . 109.5 no Si1 . C12 . H123 . 109.4 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no Si1 . C13 . H131 . 109.6 no Si1 . C13 . H132 . 109.3 no H131 . C13 . H132 . 109.5 no Si1 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N5 . C14 . C15 . 119.4(3) yes N5 . C14 . C19 . 121.3(3) yes C15 . C14 . C19 . 119.3(3) yes C14 . C15 . C16 . 122.4(4) yes C14 . C15 . H151 . 118.6 no C16 . C15 . H151 . 119.0 no C15 . C16 . C17 . 118.0(4) yes C15 . C16 . H161 . 121.0 no C17 . C16 . H161 . 121.0 no C16 . C17 . C18 . 124.1(4) yes C16 . C17 . H171 . 117.9 no C18 . C17 . H171 . 118.0 no C17 . C18 . C19 . 117.5(4) yes C17 . C18 . H181 . 121.1 no C19 . C18 . H181 . 121.5 no C18 . C19 . C14 . 118.7(4) yes C18 . C19 . H191 . 120.9 no C14 . C19 . H191 . 120.4 no Cl101 . C101 . Cl102 . 111.8(2) yes Cl101 . C101 . H1011 . 108.9 no Cl102 . C101 . H1011 . 109.0 no Cl101 . C101 . H1012 . 108.8 no Cl102 . C101 . H1012 . 108.8 no H1011 . C101 . H1012 . 109.5 no #===end