Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Daniel Leznoff' _publ_contact_author_address ; Department of Chemistry Simon Fraser University Burnaby BC V5A 1S6 CANADA ; _publ_contact_author_email DLEZNOFF@SFU.CA _publ_contact_author_phone 604-291-4887 _publ_contact_author_fax 604-291-3765 _publ_section_title ; Synthesis of mixed-donor amido/amino/siloxo ligands from symmetrical diamidosilylether ligands via a retro-Brook rearrangement and their chromium(II) complexes ; _publ_section_references ; Gabe, E.J.; White, P.S.; Enright, G.D. DIFRAC A Fortran 77 Control Routine for 4-Circle Diffractometers, N.R.C., Ottawa, 1995. Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # Insert your own references if required - in alphabetical order User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Straver, L. H. CAD4-EXPRESS, Nonius, Delft, The Netherlands (1992). North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. #Absorption Correction # Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; loop_ _publ_author_name 'Daniel Leznoff' 'Raymond J. Batchelor' 'James F. Britten' 'Farzad Haftbaradaran' 'Garry Mund' #========================================================================== #========================================================================== data_Me3PhNONCr _database_code_depnum_ccdc_archive 'CCDC 254124' #=============================================================================== _cell_length_a 11.349(3) _cell_length_b 11.513(3) _cell_length_c 20.346(4) _cell_angle_alpha 105.800(18) _cell_angle_beta 95.03(2) _cell_angle_gamma 103.31(2) _cell_volume 2457.0(11) _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' 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' 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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 '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 # Given Formula = C44 H68 Cr2 N4 O2 Si4 # Dc = 1.22 Fooo = 960.00 Mu = 5.77 M = 901.39 # Found Formula = C44 H68 Cr2 N4 O2 Si4 # Dc = 1.22 FOOO = 960.00 Mu = 5.77 M = 901.39 _chemical_formula_sum 'C44 H68 Cr2 N4 O2 Si4' _chemical_formula_moiety 'C44 H68 Cr2 N4 O2 Si4' _chemical_compound_source ? _chemical_formula_weight 901.39 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 16 _cell_measurement_theta_max 17 _cell_measurement_temperature 293 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.577 # Sheldrick geometric approximatio 0.89 0.84 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_method \w/2\q _computing_data_collection 'Cad4 Express, (Straver, 1992)' _computing_data_reduction 'RC93 (Watkin, Prout & Lilley, 1994)' _computing_cell_refinement 'Cad4 Express, (Straver, 1992)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _refine_special_details ; C11 and subsequent atoms were refined isotropically due to the limited Data. The principal atoms in the structure were still refined anisotropically. ; _diffrn_standards_interval_time 200 _diffrn_standards_interval_count 35 _diffrn_standards_number 2 _diffrn_standards_decay_% 1.10 _diffrn_ambient_temperature 293 _diffrn_reflns_number 6917 _reflns_number_total 6892 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections with Friedels Law is 6892 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6866 _diffrn_reflns_theta_min 2.104 _diffrn_reflns_theta_max 22.997 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.35 _refine_diff_density_max 0.44 _refine_ls_number_reflns 2974 _refine_ls_number_restraints 0 _refine_ls_number_parameters 328 #_refine_ls_R_factor_ref 0.0575 _refine_ls_wR_factor_ref 0.0520 _refine_ls_goodness_of_fit_ref 2.3920 #_reflns_number_all 6892 _refine_ls_R_factor_all 0.1737 _refine_ls_wR_factor_all 0.0557 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.50u(I) _reflns_number_gt 2974 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_gt 0.0520 _refine_ls_shift/su_max 0.000203 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.100E-01 0.00 0.00 0.00 0.00 1.00 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 0.38377(13) 0.98438(13) 0.24857(7) 0.0419 1.0000 Uani . . . . . . Cr2 Cr 0.24048(12) 1.10748(13) 0.25199(7) 0.0418 1.0000 Uani . . . . . . Si1 Si 0.4174(3) 0.7951(3) 0.30205(16) 0.0597 1.0000 Uani . . . . . . Si2 Si 0.4041(2) 1.0791(2) 0.39171(14) 0.0464 1.0000 Uani . . . . . . Si3 Si 0.2170(2) 1.0040(3) 0.10772(14) 0.0480 1.0000 Uani . . . . . . Si4 Si -0.0049(2) 1.0574(3) 0.19615(15) 0.0660 1.0000 Uani . . . . . . O1 O 0.4126(6) 0.9415(5) 0.3426(3) 0.0602 1.0000 Uani . . . . . . O2 O 0.1117(5) 1.0189(5) 0.1587(3) 0.0558 1.0000 Uani . . . . . . N1 N 0.3951(5) 1.1500(6) 0.3278(3) 0.0354 1.0000 Uani . . . . . . N2 N 0.3439(6) 1.0658(6) 0.1725(3) 0.0382 1.0000 Uani . . . . . . N3 N 0.3724(6) 0.7997(6) 0.2224(4) 0.0429 1.0000 Uani . . . . . . N4 N 0.0736(6) 1.1165(6) 0.2765(4) 0.0436 1.0000 Uani . . . . . . C1 C 0.3161(10) 0.6794(8) 0.3336(5) 0.0929 1.0000 Uani . . . . . . C2 C 0.5758(9) 0.7911(10) 0.3256(6) 0.1065 1.0000 Uani . . . . . . C3 C 0.5417(8) 1.1508(8) 0.4572(5) 0.0736 1.0000 Uani . . . . . . C4 C 0.2683(8) 1.0564(10) 0.4349(5) 0.0859 1.0000 Uani . . . . . . C5 C 0.2105(9) 1.0967(9) 0.0476(5) 0.0772 1.0000 Uani . . . . . . C6 C 0.1866(8) 0.8393(8) 0.0568(5) 0.0677 1.0000 Uani . . . . . . C7 C -0.1355(9) 0.9172(10) 0.1757(5) 0.1109 1.0000 Uani . . . . . . C8 C -0.0550(9) 1.1672(11) 0.1558(5) 0.1055 1.0000 Uani . . . . . . C11 C 0.4907(8) 1.2702(8) 0.3436(4) 0.042(2) 1.0000 Uiso . . . . . . C12 C 0.4672(8) 1.3795(8) 0.3807(4) 0.043(2) 1.0000 Uiso . . . . . . C13 C 0.5591(8) 1.4925(9) 0.3976(5) 0.062(3) 1.0000 Uiso . . . . . . C14 C 0.6710(9) 1.4929(9) 0.3777(5) 0.070(3) 1.0000 Uiso . . . . . . C15 C 0.6964(8) 1.3856(8) 0.3437(5) 0.060(3) 1.0000 Uiso . . . . . . C16 C 0.6079(8) 1.2704(8) 0.3262(4) 0.048(3) 1.0000 Uiso . . . . . . C21 C 0.4433(7) 1.1545(8) 0.1578(4) 0.040(2) 1.0000 Uiso . . . . . . C22 C 0.4496(8) 1.2843(8) 0.1762(4) 0.048(3) 1.0000 Uiso . . . . . . C23 C 0.5501(8) 1.3674(9) 0.1640(5) 0.065(3) 1.0000 Uiso . . . . . . C24 C 0.6381(9) 1.3219(10) 0.1323(5) 0.069(3) 1.0000 Uiso . . . . . . C25 C 0.6296(8) 1.1976(9) 0.1099(5) 0.061(3) 1.0000 Uiso . . . . . . C26 C 0.5324(8) 1.1117(8) 0.1219(4) 0.045(2) 1.0000 Uiso . . . . . . C31 C 0.3226(8) 0.6902(8) 0.1651(5) 0.048(2) 1.0000 Uiso . . . . . . C32 C 0.3971(8) 0.6342(8) 0.1211(5) 0.053(3) 1.0000 Uiso . . . . . . C33 C 0.3453(9) 0.5288(9) 0.0654(5) 0.068(3) 1.0000 Uiso . . . . . . C34 C 0.2210(9) 0.4760(9) 0.0521(5) 0.067(3) 1.0000 Uiso . . . . . . C35 C 0.1482(9) 0.5275(9) 0.0938(5) 0.068(3) 1.0000 Uiso . . . . . . C36 C 0.1947(9) 0.6322(9) 0.1496(5) 0.060(3) 1.0000 Uiso . . . . . . C41 C 0.0191(7) 1.1560(8) 0.3366(5) 0.043(2) 1.0000 Uiso . . . . . . C42 C 0.0154(7) 1.2807(8) 0.3615(5) 0.046(2) 1.0000 Uiso . . . . . . C43 C -0.0320(8) 1.3207(8) 0.4222(5) 0.055(3) 1.0000 Uiso . . . . . . C44 C -0.0745(8) 1.2397(9) 0.4586(5) 0.061(3) 1.0000 Uiso . . . . . . C45 C -0.0738(8) 1.1172(9) 0.4334(5) 0.064(3) 1.0000 Uiso . . . . . . C46 C -0.0273(8) 1.0730(8) 0.3732(5) 0.053(3) 1.0000 Uiso . . . . . . C121 C 0.3476(8) 1.3823(8) 0.4061(5) 0.064(3) 1.0000 Uiso . . . . . . C141 C 0.7720(10) 1.6176(9) 0.3993(6) 0.106(4) 1.0000 Uiso . . . . . . C161 C 0.6483(8) 1.1552(7) 0.2929(5) 0.058(3) 1.0000 Uiso . . . . . . C221 C 0.3511(8) 1.3389(8) 0.2091(5) 0.058(3) 1.0000 Uiso . . . . . . C241 C 0.7488(10) 1.4183(10) 0.1208(6) 0.115(4) 1.0000 Uiso . . . . . . C261 C 0.5279(8) 0.9753(7) 0.0969(5) 0.062(3) 1.0000 Uiso . . . . . . C321 C 0.5345(8) 0.6890(8) 0.1328(5) 0.073(3) 1.0000 Uiso . . . . . . C341 C 0.1672(10) 0.3634(10) -0.0120(6) 0.112(4) 1.0000 Uiso . . . . . . C361 C 0.1095(9) 0.6870(9) 0.1938(5) 0.091(4) 1.0000 Uiso . . . . . . C421 C 0.0558(8) 1.3725(8) 0.3227(5) 0.065(3) 1.0000 Uiso . . . . . . C441 C -0.1220(9) 1.2875(9) 0.5259(5) 0.095(4) 1.0000 Uiso . . . . . . C461 C -0.0351(9) 0.9362(8) 0.3491(5) 0.079(3) 1.0000 Uiso . . . . . . H11 H 0.3213 0.5978 0.3097 0.130(9) 1.0000 Uiso R . . . . . H12 H 0.3421 0.6964 0.3818 0.130(9) 1.0000 Uiso R . . . . . H13 H 0.2344 0.6844 0.3257 0.130(9) 1.0000 Uiso R . . . . . H21 H 0.5841 0.7098 0.3044 0.155(9) 1.0000 Uiso R . . . . . H22 H 0.5942 0.8104 0.3747 0.155(9) 1.0000 Uiso R . . . . . H23 H 0.6298 0.8508 0.3108 0.155(9) 1.0000 Uiso R . . . . . H31 H 0.5365 1.2294 0.4853 0.107(9) 1.0000 Uiso R . . . . . H32 H 0.6119 1.1620 0.4351 0.107(9) 1.0000 Uiso R . . . . . H33 H 0.5476 1.0975 0.4850 0.107(9) 1.0000 Uiso R . . . . . H41 H 0.2633 1.1352 0.4631 0.127(9) 1.0000 Uiso R . . . . . H42 H 0.2755 1.0036 0.4629 0.127(9) 1.0000 Uiso R . . . . . H43 H 0.1966 1.0187 0.4011 0.127(9) 1.0000 Uiso R . . . . . H51 H 0.2712 1.0872 0.0187 0.112(9) 1.0000 Uiso R . . . . . H52 H 0.2251 1.1825 0.0730 0.112(9) 1.0000 Uiso R . . . . . H53 H 0.1316 1.0686 0.0195 0.112(9) 1.0000 Uiso R . . . . . H61 H 0.2470 0.8305 0.0276 0.097(9) 1.0000 Uiso R . . . . . H62 H 0.1075 0.8116 0.0293 0.097(9) 1.0000 Uiso R . . . . . H63 H 0.1905 0.7901 0.0872 0.097(9) 1.0000 Uiso R . . . . . H71 H -0.2022 0.9390 0.1968 0.128(9) 1.0000 Uiso R . . . . . H72 H -0.1604 0.8857 0.1268 0.128(9) 1.0000 Uiso R . . . . . H73 H -0.1121 0.8552 0.1922 0.128(9) 1.0000 Uiso R . . . . . H81 H -0.1209 1.1964 0.1747 0.141(9) 1.0000 Uiso R . . . . . H82 H 0.0129 1.2428 0.1630 0.141(9) 1.0000 Uiso R . . . . . H83 H -0.0792 1.1325 0.1066 0.141(9) 1.0000 Uiso R . . . . . H131 H 0.5424 1.5686 0.4222 0.115(13) 1.0000 Uiso R . . . . . H151 H 0.7755 1.3880 0.3308 0.116(13) 1.0000 Uiso R . . . . . H231 H 0.5547 1.4547 0.1771 0.119(13) 1.0000 Uiso R . . . . . H251 H 0.6902 1.1689 0.0852 0.116(13) 1.0000 Uiso R . . . . . H331 H 0.3973 0.4928 0.0362 0.124(13) 1.0000 Uiso R . . . . . H351 H 0.0620 0.4892 0.0844 0.123(13) 1.0000 Uiso R . . . . . H431 H -0.0349 1.4057 0.4386 0.108(13) 1.0000 Uiso R . . . . . H451 H -0.1057 1.0604 0.4580 0.117(13) 1.0000 Uiso R . . . . . H1211 H 0.3489 1.4658 0.4305 0.105(6) 1.0000 Uiso R . . . . . H1212 H 0.3350 1.3318 0.4362 0.105(6) 1.0000 Uiso R . . . . . H1213 H 0.2829 1.3502 0.3678 0.105(6) 1.0000 Uiso R . . . . . H1411 H 0.8447 1.6046 0.3826 0.148(6) 1.0000 Uiso R . . . . . H1412 H 0.7875 1.6511 0.4481 0.148(6) 1.0000 Uiso R . . . . . H1413 H 0.7437 1.6746 0.3797 0.148(6) 1.0000 Uiso R . . . . . H1611 H 0.7309 1.1783 0.2861 0.096(6) 1.0000 Uiso R . . . . . H1612 H 0.6409 1.1028 0.3221 0.096(6) 1.0000 Uiso R . . . . . H1613 H 0.5971 1.1109 0.2495 0.096(6) 1.0000 Uiso R . . . . . H2211 H 0.3736 1.4273 0.2174 0.098(6) 1.0000 Uiso R . . . . . H2212 H 0.3427 1.3212 0.2516 0.098(6) 1.0000 Uiso R . . . . . H2213 H 0.2754 1.3032 0.1784 0.098(6) 1.0000 Uiso R . . . . . H2411 H 0.8023 1.3735 0.0989 0.156(6) 1.0000 Uiso R . . . . . H2412 H 0.7906 1.4768 0.1634 0.156(6) 1.0000 Uiso R . . . . . H2413 H 0.7201 1.4612 0.0913 0.156(6) 1.0000 Uiso R . . . . . H2611 H 0.5964 0.9652 0.0745 0.102(6) 1.0000 Uiso R . . . . . H2612 H 0.5304 0.9433 0.1354 0.102(6) 1.0000 Uiso R . . . . . H2613 H 0.4543 0.9309 0.0655 0.102(6) 1.0000 Uiso R . . . . . H3211 H 0.5685 0.6390 0.0982 0.113(6) 1.0000 Uiso R . . . . . H3212 H 0.5529 0.7721 0.1303 0.113(6) 1.0000 Uiso R . . . . . H3213 H 0.5681 0.6885 0.1771 0.113(6) 1.0000 Uiso R . . . . . H3411 H 0.0811 0.3384 -0.0136 0.153(6) 1.0000 Uiso R . . . . . H3412 H 0.1847 0.3864 -0.0523 0.153(6) 1.0000 Uiso R . . . . . H3413 H 0.2014 0.2966 -0.0097 0.153(6) 1.0000 Uiso R . . . . . H3611 H 0.0274 0.6375 0.1768 0.129(6) 1.0000 Uiso R . . . . . H3612 H 0.1157 0.7699 0.1925 0.129(6) 1.0000 Uiso R . . . . . H3613 H 0.1317 0.6882 0.2402 0.129(6) 1.0000 Uiso R . . . . . H4211 H 0.0473 1.4519 0.3477 0.105(6) 1.0000 Uiso R . . . . . H4212 H 0.1390 1.3789 0.3173 0.105(6) 1.0000 Uiso R . . . . . H4213 H 0.0058 1.3440 0.2786 0.105(6) 1.0000 Uiso R . . . . . H4411 H -0.1485 1.2202 0.5445 0.132(6) 1.0000 Uiso R . . . . . H4412 H -0.0578 1.3507 0.5580 0.132(6) 1.0000 Uiso R . . . . . H4413 H -0.1887 1.3207 0.5172 0.132(6) 1.0000 Uiso R . . . . . H4611 H -0.0696 0.8981 0.3818 0.120(6) 1.0000 Uiso R . . . . . H4612 H 0.0447 0.9245 0.3461 0.120(6) 1.0000 Uiso R . . . . . H4613 H -0.0855 0.8984 0.3053 0.120(6) 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 0.0415(10) 0.0401(10) 0.0421(11) 0.0114(9) 0.0063(8) 0.0081(8) Cr2 0.0332(10) 0.0497(10) 0.0407(11) 0.0107(8) 0.0088(8) 0.0099(8) Si1 0.080(2) 0.0444(19) 0.058(2) 0.0187(17) 0.0107(18) 0.0207(17) Si2 0.0482(19) 0.0447(18) 0.040(2) 0.0109(16) 0.0008(15) 0.0053(15) Si3 0.0470(19) 0.060(2) 0.037(2) 0.0118(16) 0.0065(15) 0.0192(16) Si4 0.0351(18) 0.094(2) 0.055(2) -0.0013(19) 0.0047(16) 0.0195(17) O1 0.092(5) 0.047(4) 0.041(4) 0.016(4) -0.003(4) 0.018(4) O2 0.036(4) 0.081(5) 0.040(4) 0.000(3) 0.007(3) 0.017(3) N1 0.030(4) 0.036(4) 0.038(5) 0.009(4) 0.001(4) 0.007(3) N2 0.032(4) 0.039(4) 0.044(5) 0.013(4) 0.011(4) 0.011(4) N3 0.046(5) 0.035(4) 0.041(5) 0.007(4) 0.005(4) 0.004(4) N4 0.026(4) 0.049(5) 0.045(5) -0.002(4) 0.010(4) 0.006(4) C1 0.150(11) 0.052(7) 0.080(9) 0.031(7) 0.029(8) 0.016(7) C2 0.109(11) 0.132(11) 0.102(11) 0.053(9) -0.002(8) 0.062(9) C3 0.093(9) 0.075(7) 0.051(7) 0.027(6) -0.003(6) 0.015(6) C4 0.068(8) 0.128(10) 0.079(9) 0.054(8) 0.033(7) 0.026(7) C5 0.089(9) 0.093(9) 0.051(7) 0.019(7) -0.004(6) 0.037(7) C6 0.073(8) 0.072(8) 0.049(7) 0.009(6) 0.007(6) 0.016(6) C7 0.061(8) 0.153(12) 0.068(9) -0.026(8) 0.005(7) 0.005(8) C8 0.082(9) 0.166(12) 0.073(9) 0.020(9) -0.016(7) 0.072(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.084(2) 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 . Cr2 . 2.384(2) yes Cr1 . Si1 . 2.771(3) yes Cr1 . Si2 . 2.786(3) yes Cr1 . O1 . 2.119(6) yes Cr1 . N1 . 2.104(6) yes Cr1 . N2 . 2.083(7) yes Cr1 . N3 . 2.016(6) yes Cr2 . Si3 . 2.814(3) yes Cr2 . Si4 . 2.780(3) yes Cr2 . O2 . 2.133(6) yes Cr2 . N1 . 2.102(6) yes Cr2 . N2 . 2.095(6) yes Cr2 . N4 . 2.019(6) yes Si1 . O1 . 1.678(6) yes Si1 . N3 . 1.674(7) yes Si1 . C1 . 1.844(9) yes Si1 . C2 . 1.834(10) yes Si2 . O1 . 1.656(6) yes Si2 . N1 . 1.721(7) yes Si2 . C3 . 1.827(9) yes Si2 . C4 . 1.842(8) yes Si3 . O2 . 1.657(6) yes Si3 . N2 . 1.733(7) yes Si3 . C5 . 1.836(9) yes Si3 . C6 . 1.831(8) yes Si4 . O2 . 1.671(6) yes Si4 . N4 . 1.671(7) yes Si4 . C7 . 1.844(10) yes Si4 . C8 . 1.847(10) yes N1 . C11 . 1.483(9) yes N2 . C21 . 1.449(9) yes N3 . C31 . 1.423(10) yes N4 . C41 . 1.428(10) yes C1 . H11 . 0.951 no C1 . H12 . 0.951 no C1 . H13 . 0.945 no C2 . H21 . 0.948 no C2 . H22 . 0.955 no C2 . H23 . 0.943 no C3 . H31 . 0.948 no C3 . H32 . 0.949 no C3 . H33 . 0.950 no C4 . H41 . 0.949 no C4 . H42 . 0.951 no C4 . H43 . 0.949 no C5 . H51 . 0.950 no C5 . H52 . 0.950 no C5 . H53 . 0.954 no C6 . H61 . 0.951 no C6 . H62 . 0.951 no C6 . H63 . 0.950 no C7 . H71 . 0.952 no C7 . H72 . 0.953 no C7 . H73 . 0.946 no C8 . H81 . 0.957 no C8 . H82 . 0.987 no C8 . H83 . 0.959 no C11 . C12 . 1.378(10) yes C11 . C16 . 1.405(10) yes C12 . C13 . 1.403(10) yes C12 . C121 . 1.497(10) yes C13 . C14 . 1.366(11) yes C13 . H131 . 0.953 no C14 . C15 . 1.349(11) yes C14 . C141 . 1.542(12) yes C15 . C16 . 1.401(10) yes C15 . H151 . 0.954 no C16 . C161 . 1.509(10) yes C21 . C22 . 1.421(10) yes C21 . C26 . 1.401(10) yes C22 . C23 . 1.397(11) yes C22 . C221 . 1.523(10) yes C23 . C24 . 1.363(11) yes C23 . H231 . 0.955 no C24 . C25 . 1.357(11) yes C24 . C241 . 1.555(12) yes C25 . C26 . 1.390(11) yes C25 . H251 . 0.954 no C26 . C261 . 1.500(10) yes C31 . C32 . 1.415(11) yes C31 . C36 . 1.418(11) yes C32 . C33 . 1.381(11) yes C32 . C321 . 1.512(11) yes C33 . C34 . 1.371(11) yes C33 . H331 . 0.956 no C34 . C35 . 1.353(11) yes C34 . C341 . 1.526(12) yes C35 . C36 . 1.370(11) yes C35 . H351 . 0.954 no C36 . C361 . 1.505(11) yes C41 . C42 . 1.398(10) yes C41 . C46 . 1.404(11) yes C42 . C43 . 1.397(11) yes C42 . C421 . 1.497(11) yes C43 . C44 . 1.371(11) yes C43 . H431 . 0.953 no C44 . C45 . 1.364(11) yes C44 . C441 . 1.525(12) yes C45 . C46 . 1.392(11) yes C45 . H451 . 0.954 no C46 . C461 . 1.495(11) yes C121 . H1211 . 0.950 no C121 . H1212 . 0.951 no C121 . H1213 . 0.949 no C141 . H1411 . 0.947 no C141 . H1412 . 0.946 no C141 . H1413 . 0.954 no C161 . H1611 . 0.947 no C161 . H1612 . 0.951 no C161 . H1613 . 0.952 no C221 . H2211 . 0.953 no C221 . H2212 . 0.949 no C221 . H2213 . 0.949 no C241 . H2411 . 0.949 no C241 . H2412 . 0.945 no C241 . H2413 . 0.955 no C261 . H2611 . 0.949 no C261 . H2612 . 0.953 no C261 . H2613 . 0.948 no C321 . H3211 . 0.951 no C321 . H3212 . 0.948 no C321 . H3213 . 0.949 no C341 . H3411 . 0.948 no C341 . H3412 . 0.951 no C341 . H3413 . 0.948 no C361 . H3611 . 0.951 no C361 . H3612 . 0.949 no C361 . H3613 . 0.951 no C421 . H4211 . 0.949 no C421 . H4212 . 0.948 no C421 . H4213 . 0.948 no C441 . H4411 . 0.952 no C441 . H4412 . 0.949 no C441 . H4413 . 0.947 no C461 . H4611 . 0.956 no C461 . H4612 . 0.951 no C461 . H4613 . 0.946 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 Cr2 . Cr1 . Si1 . 136.57(9) yes Cr2 . Cr1 . Si2 . 81.55(8) yes Si1 . Cr1 . Si2 . 73.55(9) yes Cr2 . Cr1 . O1 . 111.47(17) yes Si1 . Cr1 . O1 . 37.22(16) yes Si2 . Cr1 . O1 . 36.36(16) yes Cr2 . Cr1 . N1 . 55.41(17) yes Si1 . Cr1 . N1 . 111.42(19) yes Si2 . Cr1 . N1 . 38.09(18) yes O1 . Cr1 . N1 . 74.2(2) yes Cr2 . Cr1 . N2 . 55.45(17) yes Si1 . Cr1 . N2 . 156.88(19) yes Si2 . Cr1 . N2 . 129.11(19) yes O1 . Cr1 . N2 . 165.3(2) yes N1 . Cr1 . N2 . 91.6(2) yes Cr2 . Cr1 . N3 . 135.4(2) yes Si1 . Cr1 . N3 . 36.8(2) yes Si2 . Cr1 . N3 . 109.4(2) yes O1 . Cr1 . N3 . 73.6(2) yes N1 . Cr1 . N3 . 147.4(3) yes N2 . Cr1 . N3 . 120.1(3) yes Cr1 . Cr2 . Si3 . 80.75(8) yes Cr1 . Cr2 . Si4 . 134.31(9) yes Si3 . Cr2 . Si4 . 72.18(9) yes Cr1 . Cr2 . O2 . 105.78(16) yes Si3 . Cr2 . O2 . 35.92(15) yes Si4 . Cr2 . O2 . 36.89(15) yes Cr1 . Cr2 . N1 . 55.52(17) yes Si3 . Cr2 . N1 . 128.58(18) yes Si4 . Cr2 . N1 . 158.35(19) yes O2 . Cr2 . N1 . 161.2(2) yes Cr1 . Cr2 . N2 . 54.96(18) yes Si3 . Cr2 . N2 . 37.90(18) yes Si4 . Cr2 . N2 . 109.94(19) yes O2 . Cr2 . N2 . 73.8(2) yes N1 . Cr2 . N2 . 91.3(3) yes Cr1 . Cr2 . N4 . 142.2(2) yes Si3 . Cr2 . N4 . 108.8(2) yes Si4 . Cr2 . N4 . 36.6(2) yes O2 . Cr2 . N4 . 73.2(2) yes N1 . Cr2 . N4 . 122.2(3) yes N2 . Cr2 . N4 . 146.5(3) yes Cr1 . Si1 . O1 . 49.8(2) yes Cr1 . Si1 . N3 . 46.3(2) yes O1 . Si1 . N3 . 95.3(3) yes Cr1 . Si1 . C1 . 134.3(4) yes O1 . Si1 . C1 . 111.5(4) yes N3 . Si1 . C1 . 117.0(4) yes Cr1 . Si1 . C2 . 117.2(4) yes O1 . Si1 . C2 . 105.3(4) yes N3 . Si1 . C2 . 118.7(4) yes C1 . Si1 . C2 . 107.7(5) yes Cr1 . Si2 . O1 . 49.3(2) yes Cr1 . Si2 . N1 . 49.0(2) yes O1 . Si2 . N1 . 98.0(3) yes Cr1 . Si2 . C3 . 129.4(3) yes O1 . Si2 . C3 . 109.5(4) yes N1 . Si2 . C3 . 114.5(4) yes Cr1 . Si2 . C4 . 121.0(3) yes O1 . Si2 . C4 . 109.2(4) yes N1 . Si2 . C4 . 115.7(4) yes C3 . Si2 . C4 . 109.2(5) yes Cr2 . Si3 . O2 . 49.0(2) yes Cr2 . Si3 . N2 . 48.0(2) yes O2 . Si3 . N2 . 96.9(3) yes Cr2 . Si3 . C5 . 122.7(3) yes O2 . Si3 . C5 . 110.6(4) yes N2 . Si3 . C5 . 113.8(4) yes Cr2 . Si3 . C6 . 128.6(3) yes O2 . Si3 . C6 . 109.0(4) yes N2 . Si3 . C6 . 117.6(4) yes C5 . Si3 . C6 . 108.2(4) yes Cr2 . Si4 . O2 . 50.0(2) yes Cr2 . Si4 . N4 . 46.1(2) yes O2 . Si4 . N4 . 95.7(3) yes Cr2 . Si4 . C7 . 132.8(4) yes O2 . Si4 . C7 . 109.4(4) yes N4 . Si4 . C7 . 119.0(5) yes Cr2 . Si4 . C8 . 119.5(4) yes O2 . Si4 . C8 . 107.2(4) yes N4 . Si4 . C8 . 117.5(4) yes C7 . Si4 . C8 . 106.8(5) yes Cr1 . O1 . Si1 . 93.0(3) yes Cr1 . O1 . Si2 . 94.3(3) yes Si1 . O1 . Si2 . 172.2(4) yes Cr2 . O2 . Si4 . 93.1(3) yes Cr2 . O2 . Si3 . 95.0(3) yes Si4 . O2 . Si3 . 163.9(4) yes Cr1 . N1 . Cr2 . 69.1(2) yes Cr1 . N1 . Si2 . 92.9(3) yes Cr2 . N1 . Si2 . 124.7(3) yes Cr1 . N1 . C11 . 126.3(5) yes Cr2 . N1 . C11 . 120.4(5) yes Si2 . N1 . C11 . 112.5(5) yes Cr2 . N2 . Cr1 . 69.6(2) yes Cr2 . N2 . Si3 . 94.1(3) yes Cr1 . N2 . Si3 . 124.6(3) yes Cr2 . N2 . C21 . 125.6(5) yes Cr1 . N2 . C21 . 118.1(5) yes Si3 . N2 . C21 . 114.3(5) yes Cr1 . N3 . Si1 . 96.9(3) yes Cr1 . N3 . C31 . 138.9(6) yes Si1 . N3 . C31 . 123.1(6) yes Cr2 . N4 . Si4 . 97.3(3) yes Cr2 . N4 . C41 . 139.0(6) yes Si4 . N4 . C41 . 123.7(5) yes Si1 . C1 . H11 . 109.203 no Si1 . C1 . H12 . 109.183 no H11 . C1 . H12 . 109.223 no Si1 . C1 . H13 . 109.585 no H11 . C1 . H13 . 109.791 no H12 . C1 . H13 . 109.838 no Si1 . C2 . H21 . 109.303 no Si1 . C2 . H22 . 109.060 no H21 . C2 . H22 . 109.261 no Si1 . C2 . H23 . 109.443 no H21 . C2 . H23 . 110.208 no H22 . C2 . H23 . 109.546 no Si2 . C3 . H31 . 109.379 no Si2 . C3 . H32 . 109.428 no H31 . C3 . H32 . 109.701 no Si2 . C3 . H33 . 109.151 no H31 . C3 . H33 . 109.632 no H32 . C3 . H33 . 109.533 no Si2 . C4 . H41 . 109.332 no Si2 . C4 . H42 . 109.320 no H41 . C4 . H42 . 109.498 no Si2 . C4 . H43 . 109.547 no H41 . C4 . H43 . 109.635 no H42 . C4 . H43 . 109.495 no Si3 . C5 . H51 . 109.616 no Si3 . C5 . H52 . 109.613 no H51 . C5 . H52 . 109.375 no Si3 . C5 . H53 . 109.796 no H51 . C5 . H53 . 109.131 no H52 . C5 . H53 . 109.294 no Si3 . C6 . H61 . 109.164 no Si3 . C6 . H62 . 110.112 no H61 . C6 . H62 . 109.484 no Si3 . C6 . H63 . 109.305 no H61 . C6 . H63 . 109.313 no H62 . C6 . H63 . 109.446 no Si4 . C7 . H71 . 109.565 no Si4 . C7 . H72 . 108.970 no H71 . C7 . H72 . 109.051 no Si4 . C7 . H73 . 109.920 no H71 . C7 . H73 . 109.665 no H72 . C7 . H73 . 109.651 no Si4 . C8 . H81 . 113.485 no Si4 . C8 . H82 . 110.496 no H81 . C8 . H82 . 105.850 no Si4 . C8 . H83 . 112.790 no H81 . C8 . H83 . 108.034 no H82 . C8 . H83 . 105.664 no N1 . C11 . C12 . 119.5(7) yes N1 . C11 . C16 . 119.8(7) yes C12 . C11 . C16 . 120.4(8) yes C11 . C12 . C13 . 119.4(8) yes C11 . C12 . C121 . 122.5(8) yes C13 . C12 . C121 . 118.1(8) yes C12 . C13 . C14 . 119.8(9) yes C12 . C13 . H131 . 119.634 no C14 . C13 . H131 . 120.571 no C13 . C14 . C15 . 121.1(10) yes C13 . C14 . C141 . 118.7(9) yes C15 . C14 . C141 . 120.0(9) yes C14 . C15 . C16 . 121.1(9) yes C14 . C15 . H151 . 119.684 no C16 . C15 . H151 . 119.224 no C11 . C16 . C15 . 118.0(8) yes C11 . C16 . C161 . 125.1(8) yes C15 . C16 . C161 . 116.8(8) yes N2 . C21 . C22 . 121.5(7) yes N2 . C21 . C26 . 119.7(7) yes C22 . C21 . C26 . 118.7(8) yes C21 . C22 . C23 . 119.6(8) yes C21 . C22 . C221 . 123.0(8) yes C23 . C22 . C221 . 117.5(8) yes C22 . C23 . C24 . 119.4(9) yes C22 . C23 . H231 . 119.292 no C24 . C23 . H231 . 121.334 no C23 . C24 . C25 . 122.1(10) yes C23 . C24 . C241 . 117.4(9) yes C25 . C24 . C241 . 120.5(10) yes C24 . C25 . C26 . 120.4(9) yes C24 . C25 . H251 . 119.724 no C26 . C25 . H251 . 119.823 no C21 . C26 . C25 . 119.5(8) yes C21 . C26 . C261 . 122.0(8) yes C25 . C26 . C261 . 118.5(8) yes N3 . C31 . C32 . 122.1(8) yes N3 . C31 . C36 . 120.9(8) yes C32 . C31 . C36 . 116.9(9) yes C31 . C32 . C33 . 120.5(9) yes C31 . C32 . C321 . 121.2(8) yes C33 . C32 . C321 . 118.3(9) yes C32 . C33 . C34 . 120.7(10) yes C32 . C33 . H331 . 119.095 no C34 . C33 . H331 . 120.236 no C33 . C34 . C35 . 119.8(10) yes C33 . C34 . C341 . 118.8(10) yes C35 . C34 . C341 . 121.3(10) yes C34 . C35 . C36 . 121.9(10) yes C34 . C35 . H351 . 119.022 no C36 . C35 . H351 . 119.026 no C31 . C36 . C35 . 120.1(9) yes C31 . C36 . C361 . 120.0(9) yes C35 . C36 . C361 . 119.9(9) yes N4 . C41 . C42 . 120.0(8) yes N4 . C41 . C46 . 121.3(8) yes C42 . C41 . C46 . 118.7(8) yes C41 . C42 . C43 . 119.9(9) yes C41 . C42 . C421 . 121.6(8) yes C43 . C42 . C421 . 118.4(8) yes C42 . C43 . C44 . 121.1(9) yes C42 . C43 . H431 . 119.393 no C44 . C43 . H431 . 119.555 no C43 . C44 . C45 . 119.1(10) yes C43 . C44 . C441 . 119.6(9) yes C45 . C44 . C441 . 121.3(9) yes C44 . C45 . C46 . 121.9(10) yes C44 . C45 . H451 . 119.000 no C46 . C45 . H451 . 119.063 no C41 . C46 . C45 . 119.3(9) yes C41 . C46 . C461 . 123.3(8) yes C45 . C46 . C461 . 117.4(9) yes C12 . C121 . H1211 . 109.975 no C12 . C121 . H1212 . 109.100 no H1211 . C121 . H1212 . 109.363 no C12 . C121 . H1213 . 109.402 no H1211 . C121 . H1213 . 109.582 no H1212 . C121 . H1213 . 109.403 no C14 . C141 . H1411 . 110.076 no C14 . C141 . H1412 . 109.668 no H1411 . C141 . H1412 . 110.077 no C14 . C141 . H1413 . 108.279 no H1411 . C141 . H1413 . 109.374 no H1412 . C141 . H1413 . 109.336 no C16 . C161 . H1611 . 110.055 no C16 . C161 . H1612 . 109.186 no H1611 . C161 . H1612 . 109.568 no C16 . C161 . H1613 . 109.231 no H1611 . C161 . H1613 . 109.598 no H1612 . C161 . H1613 . 109.185 no C22 . C221 . H2211 . 109.280 no C22 . C221 . H2212 . 110.176 no H2211 . C221 . H2212 . 109.349 no C22 . C221 . H2213 . 109.135 no H2211 . C221 . H2213 . 109.300 no H2212 . C221 . H2213 . 109.584 no C24 . C241 . H2411 . 107.851 no C24 . C241 . H2412 . 110.730 no H2411 . C241 . H2412 . 110.068 no C24 . C241 . H2413 . 109.370 no H2411 . C241 . H2413 . 109.208 no H2412 . C241 . H2413 . 109.579 no C26 . C261 . H2611 . 109.526 no C26 . C261 . H2612 . 109.334 no H2611 . C261 . H2612 . 109.279 no C26 . C261 . H2613 . 109.651 no H2611 . C261 . H2613 . 109.686 no H2612 . C261 . H2613 . 109.350 no C32 . C321 . H3211 . 108.972 no C32 . C321 . H3212 . 110.089 no H3211 . C321 . H3212 . 109.549 no C32 . C321 . H3213 . 109.000 no H3211 . C321 . H3213 . 109.385 no H3212 . C321 . H3213 . 109.825 no C34 . C341 . H3411 . 108.268 no C34 . C341 . H3412 . 109.529 no H3411 . C341 . H3412 . 109.603 no C34 . C341 . H3413 . 110.053 no H3411 . C341 . H3413 . 109.830 no H3412 . C341 . H3413 . 109.537 no C36 . C361 . H3611 . 109.656 no C36 . C361 . H3612 . 109.488 no H3611 . C361 . H3612 . 109.468 no C36 . C361 . H3613 . 109.370 no H3611 . C361 . H3613 . 109.413 no H3612 . C361 . H3613 . 109.431 no C42 . C421 . H4211 . 109.383 no C42 . C421 . H4212 . 109.600 no H4211 . C421 . H4212 . 109.654 no C42 . C421 . H4213 . 108.788 no H4211 . C421 . H4213 . 109.683 no H4212 . C421 . H4213 . 109.715 no C44 . C441 . H4411 . 109.390 no C44 . C441 . H4412 . 109.126 no H4411 . C441 . H4412 . 109.364 no C44 . C441 . H4413 . 109.681 no H4411 . C441 . H4413 . 109.456 no H4412 . C441 . H4413 . 109.809 no C46 . C461 . H4611 . 108.925 no C46 . C461 . H4612 . 109.801 no H4611 . C461 . H4612 . 108.919 no C46 . C461 . H4613 . 110.045 no H4611 . C461 . H4613 . 109.358 no H4612 . C461 . H4613 . 109.769 no #============================================================================= #============================================================================= data_Me3PhNNOCr _database_code_depnum_ccdc_archive 'CCDC 254125' #============================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H84 Cr2 N4 O4 Si4 , C4 H8 O , C4 H8 O' _chemical_formula_sum 'C60 H100 Cr2 N4 O6 Si4' _chemical_formula_weight 1189.79 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.146(3) _cell_length_b 27.506(7) _cell_length_c 22.192(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.630(4) _cell_angle_gamma 90.00 _cell_volume 6708(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 963 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23870 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7682 _reflns_number_gt 5187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Disorder in coordinated THF modelled sith refined occupancies. Badly disordered solvent was removed from the model. The diffraction data was processed with SQUEEZE (Sluis, P. v.d. & Spek, A. L. (1990) Acta Cryst. A46, 194-201.) to remove the diffraction contribution of the solvent. 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^)+(0.0728P)^2^+0.0000P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00013(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7682 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 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 Cr1 Cr 0.49335(3) 0.082592(13) 0.317387(15) 0.02804(12) Uani 1 1 d . . . Si1 Si 0.72852(6) 0.05414(2) 0.42268(3) 0.03382(17) Uani 1 1 d . B . Si2 Si 0.74961(5) 0.04440(3) 0.28754(3) 0.03520(17) Uani 1 1 d . B . O1 O 0.61741(13) 0.06943(6) 0.26297(7) 0.0324(4) Uani 1 1 d . . . O2 O 0.34307(14) 0.10713(6) 0.35461(7) 0.0383(4) Uani 1 1 d . . . N1 N 0.61107(17) 0.09322(7) 0.39770(8) 0.0332(4) Uani 1 1 d . . . N2 N 0.74878(16) 0.01878(7) 0.35923(8) 0.0326(4) Uani 1 1 d . . . C1 C 0.7128(3) 0.00773(10) 0.48322(11) 0.0502(7) Uani 1 1 d . . . H1A H 0.6419 -0.0129 0.4693 0.075 Uiso 1 1 calc R B . H1B H 0.7023 0.0244 0.5210 0.075 Uiso 1 1 calc R . . H1C H 0.7862 -0.0125 0.4908 0.075 Uiso 1 1 calc R . . C2 C 0.8674(2) 0.09040(10) 0.45564(14) 0.0532(7) Uani 1 1 d . . . H2A H 0.8818 0.1156 0.4265 0.080 Uiso 1 1 calc R B . H2B H 0.9381 0.0688 0.4637 0.080 Uiso 1 1 calc R . . H2C H 0.8544 0.1057 0.4939 0.080 Uiso 1 1 calc R . . C3 C 0.7816(3) -0.00448(11) 0.23450(12) 0.0533(7) Uani 1 1 d . . . H3A H 0.7179 -0.0293 0.2315 0.080 Uiso 1 1 calc R B . H3B H 0.8607 -0.0193 0.2501 0.080 Uiso 1 1 calc R . . H3C H 0.7832 0.0094 0.1940 0.080 Uiso 1 1 calc R . . C4 C 0.8720(2) 0.09128(11) 0.29287(14) 0.0549(8) Uani 1 1 d . . . H4A H 0.8559 0.1172 0.3207 0.082 Uiso 1 1 calc R B . H4B H 0.8736 0.1050 0.2523 0.082 Uiso 1 1 calc R . . H4C H 0.9508 0.0762 0.3084 0.082 Uiso 1 1 calc R . . C5 C 0.2974(3) 0.08468(11) 0.40513(14) 0.0622(8) Uani 1 1 d . B . H5A H 0.3652 0.0711 0.4349 0.075 Uiso 1 1 calc R A 1 H5B H 0.2400 0.0581 0.3904 0.075 Uiso 1 1 calc R A 1 C6 C 0.2338(4) 0.12437(15) 0.43415(18) 0.0841(11) Uani 0.77(2) 1 d P B 1 H6A H 0.1619 0.1115 0.4498 0.101 Uiso 0.77(2) 1 calc PR B 1 H6B H 0.2894 0.1397 0.4684 0.101 Uiso 0.77(2) 1 calc PR B 1 C6A C 0.2338(4) 0.12437(15) 0.43415(18) 0.0841(11) Uani 0.23(2) 1 d P B 2 H6AA H 0.1452 0.1179 0.4288 0.101 Uiso 0.23(2) 1 calc PR B 2 H6AB H 0.2662 0.1267 0.4784 0.101 Uiso 0.23(2) 1 calc PR B 2 C7 C 0.1964(7) 0.1600(3) 0.3839(3) 0.0629(17) Uani 0.77(2) 1 d P B 1 H7A H 0.1886 0.1931 0.4001 0.076 Uiso 0.77(2) 1 calc PR B 1 H7B H 0.1182 0.1505 0.3585 0.076 Uiso 0.77(2) 1 calc PR B 1 C7A C 0.258(4) 0.1693(8) 0.4028(18) 0.091(10) Uani 0.23(2) 1 d P B 2 H7AA H 0.1820 0.1887 0.3931 0.109 Uiso 0.23(2) 1 calc PR B 2 H7AB H 0.3191 0.1891 0.4295 0.109 Uiso 0.23(2) 1 calc PR B 2 C8 C 0.3018(2) 0.15695(10) 0.34730(13) 0.0496(7) Uani 0.77(2) 1 d P B 1 H8A H 0.2733 0.1646 0.3037 0.059 Uiso 0.77(2) 1 calc PR B 1 H8B H 0.3678 0.1798 0.3639 0.059 Uiso 0.77(2) 1 calc PR B 1 C8A C 0.3018(2) 0.15695(10) 0.34730(13) 0.0496(7) Uani 0.23(2) 1 d P B 2 H8AA H 0.3696 0.1787 0.3413 0.059 Uiso 0.23(2) 1 calc PR B 2 H8AB H 0.2359 0.1600 0.3116 0.059 Uiso 0.23(2) 1 calc PR B 2 C11 C 0.5995(2) 0.13886(9) 0.42714(11) 0.0382(6) Uani 1 1 d . B . C12 C 0.5741(3) 0.14236(10) 0.48707(12) 0.0496(7) Uani 1 1 d . . . C13 C 0.5626(3) 0.18794(12) 0.51311(14) 0.0629(9) Uani 1 1 d . B . H13A H 0.5443 0.1892 0.5534 0.075 Uiso 1 1 calc R . . C14 C 0.5761(3) 0.23100(11) 0.48379(15) 0.0587(8) Uani 1 1 d . . . C15 C 0.5991(2) 0.22752(10) 0.42486(15) 0.0552(8) Uani 1 1 d . B . H15A H 0.6077 0.2566 0.4029 0.066 Uiso 1 1 calc R . . C16 C 0.6103(2) 0.18327(9) 0.39612(13) 0.0451(6) Uani 1 1 d . . . C21 C 0.7593(2) -0.03346(8) 0.36593(10) 0.0333(5) Uani 1 1 d . B . C22 C 0.8739(2) -0.05538(9) 0.38310(12) 0.0420(6) Uani 1 1 d . . . C23 C 0.8798(2) -0.10553(10) 0.39254(13) 0.0500(7) Uani 1 1 d . B . H23A H 0.9571 -0.1201 0.4052 0.060 Uiso 1 1 calc R . . C24 C 0.7762(3) -0.13530(9) 0.38409(13) 0.0480(7) Uani 1 1 d . . . C25 C 0.6656(2) -0.11274(9) 0.36573(12) 0.0431(6) Uani 1 1 d . B . H25A H 0.5941 -0.1321 0.3587 0.052 Uiso 1 1 calc R . . C26 C 0.6546(2) -0.06263(9) 0.35702(10) 0.0341(5) Uani 1 1 d . . . C121 C 0.5566(4) 0.09809(13) 0.52447(15) 0.0813(11) Uani 1 1 d . B . H12A H 0.5393 0.1082 0.5645 0.122 Uiso 1 1 calc R . . H12B H 0.6308 0.0783 0.5300 0.122 Uiso 1 1 calc R . . H12C H 0.4883 0.0789 0.5033 0.122 Uiso 1 1 calc R . . C141 C 0.5675(3) 0.27983(12) 0.51450(19) 0.0877(13) Uani 1 1 d . B . H14A H 0.5510 0.2748 0.5561 0.132 Uiso 1 1 calc R . . H14B H 0.5014 0.2989 0.4910 0.132 Uiso 1 1 calc R . . H14C H 0.6445 0.2974 0.5163 0.132 Uiso 1 1 calc R . . C161 C 0.6352(4) 0.18335(11) 0.33082(16) 0.0725(10) Uani 1 1 d . B . H16A H 0.6400 0.2170 0.3168 0.109 Uiso 1 1 calc R . . H16B H 0.5692 0.1664 0.3043 0.109 Uiso 1 1 calc R . . H16C H 0.7125 0.1668 0.3293 0.109 Uiso 1 1 calc R . . C221 C 0.9891(2) -0.02561(11) 0.39187(14) 0.0564(8) Uani 1 1 d . B . H22A H 1.0594 -0.0470 0.4037 0.085 Uiso 1 1 calc R . . H22B H 0.9864 -0.0015 0.4241 0.085 Uiso 1 1 calc R . . H22C H 0.9964 -0.0090 0.3536 0.085 Uiso 1 1 calc R . . C241 C 0.7846(3) -0.18952(11) 0.39550(18) 0.0737(10) Uani 1 1 d . B . H24A H 0.7029 -0.2038 0.3872 0.111 Uiso 1 1 calc R . . H24B H 0.8209 -0.1956 0.4382 0.111 Uiso 1 1 calc R . . H24C H 0.8354 -0.2043 0.3685 0.111 Uiso 1 1 calc R . . C261 C 0.5303(2) -0.04031(9) 0.33879(12) 0.0405(6) Uani 1 1 d . B . H26A H 0.4684 -0.0659 0.3347 0.061 Uiso 1 1 calc R . . H26B H 0.5264 -0.0234 0.2997 0.061 Uiso 1 1 calc R . . H26C H 0.5152 -0.0171 0.3702 0.061 Uiso 1 1 calc 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 0.0307(2) 0.0317(2) 0.02196(19) -0.00121(14) 0.00502(13) -0.00217(14) Si1 0.0401(4) 0.0333(4) 0.0256(3) 0.0017(3) -0.0018(3) -0.0081(3) Si2 0.0275(3) 0.0484(4) 0.0298(3) 0.0072(3) 0.0052(3) 0.0006(3) O1 0.0286(8) 0.0433(10) 0.0257(8) 0.0038(7) 0.0054(6) 0.0011(7) O2 0.0413(9) 0.0418(10) 0.0340(9) 0.0002(7) 0.0131(7) 0.0016(7) N1 0.0402(11) 0.0327(11) 0.0256(10) -0.0024(8) 0.0022(8) -0.0063(8) N2 0.0320(10) 0.0365(11) 0.0276(10) 0.0029(8) 0.0000(8) -0.0027(8) C1 0.079(2) 0.0418(15) 0.0287(13) 0.0028(11) 0.0052(13) -0.0029(13) C2 0.0505(16) 0.0472(17) 0.0552(17) -0.0047(13) -0.0104(13) -0.0102(12) C3 0.0498(16) 0.075(2) 0.0363(14) 0.0032(14) 0.0122(12) 0.0225(14) C4 0.0342(14) 0.072(2) 0.0588(18) 0.0246(15) 0.0083(12) -0.0085(13) C5 0.081(2) 0.061(2) 0.0541(18) -0.0009(15) 0.0416(17) -0.0092(16) C6 0.088(3) 0.098(3) 0.079(3) -0.016(2) 0.051(2) 0.005(2) C6A 0.088(3) 0.098(3) 0.079(3) -0.016(2) 0.051(2) 0.005(2) C7 0.045(3) 0.068(3) 0.080(4) -0.022(3) 0.022(3) 0.006(3) C7A 0.08(2) 0.059(13) 0.14(2) 0.002(13) 0.055(18) 0.014(11) C8 0.0503(16) 0.0429(16) 0.0569(17) -0.0069(13) 0.0129(13) 0.0077(12) C8A 0.0503(16) 0.0429(16) 0.0569(17) -0.0069(13) 0.0129(13) 0.0077(12) C11 0.0392(13) 0.0392(14) 0.0341(13) -0.0080(10) 0.0002(10) -0.0066(10) C12 0.0617(18) 0.0525(17) 0.0341(14) -0.0066(12) 0.0065(12) 0.0044(13) C13 0.072(2) 0.070(2) 0.0441(17) -0.0220(15) 0.0007(14) 0.0142(16) C14 0.0484(17) 0.0506(18) 0.070(2) -0.0251(16) -0.0100(14) 0.0047(13) C15 0.0516(17) 0.0361(15) 0.077(2) -0.0088(14) 0.0080(15) -0.0092(12) C16 0.0452(15) 0.0364(14) 0.0538(16) -0.0041(12) 0.0084(12) -0.0076(11) C21 0.0367(12) 0.0362(13) 0.0258(11) 0.0001(9) 0.0019(9) 0.0024(10) C22 0.0352(13) 0.0478(16) 0.0408(14) 0.0024(11) -0.0003(10) 0.0036(11) C23 0.0468(16) 0.0498(17) 0.0512(17) 0.0050(13) 0.0019(12) 0.0143(13) C24 0.0565(17) 0.0371(15) 0.0493(16) 0.0005(12) 0.0054(13) 0.0081(12) C25 0.0464(15) 0.0390(15) 0.0415(14) -0.0036(11) 0.0001(11) -0.0032(11) C26 0.0363(12) 0.0361(13) 0.0285(12) -0.0024(10) 0.0009(9) -0.0008(10) C121 0.131(3) 0.077(2) 0.0446(18) 0.0068(16) 0.040(2) 0.026(2) C141 0.080(2) 0.066(2) 0.106(3) -0.047(2) -0.016(2) 0.0084(18) C161 0.111(3) 0.0389(17) 0.078(2) 0.0106(15) 0.044(2) -0.0115(17) C221 0.0354(14) 0.065(2) 0.0650(19) 0.0121(15) -0.0030(13) -0.0002(13) C241 0.081(2) 0.0425(18) 0.093(3) 0.0043(17) 0.0028(19) 0.0113(16) C261 0.0335(13) 0.0401(14) 0.0458(15) 0.0037(11) 0.0012(10) -0.0036(10) _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 Cr1 O1 2.0151(16) . ? Cr1 O1 2.0244(15) 2_655 ? Cr1 N1 2.0498(18) . ? Cr1 O2 2.0993(17) . ? Si1 N1 1.713(2) . ? Si1 N2 1.757(2) . ? Si1 C1 1.882(3) . ? Si1 C2 1.883(3) . ? Si2 O1 1.6351(16) . ? Si2 N2 1.7415(19) . ? Si2 C3 1.861(3) . ? Si2 C4 1.867(3) . ? O1 Cr1 2.0244(15) 2_655 ? O2 C8 1.446(3) . ? O2 C5 1.445(3) . ? N1 C11 1.431(3) . ? N2 C21 1.447(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.504(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.491(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.538(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C11 C12 1.409(4) . ? C11 C16 1.417(4) . ? C12 C13 1.395(4) . ? C12 C121 1.505(4) . ? C13 C14 1.372(4) . ? C13 H13A 0.9500 . ? C14 C15 1.378(4) . ? C14 C141 1.517(4) . ? C15 C16 1.389(4) . ? C15 H15A 0.9500 . ? C16 C161 1.521(4) . ? C21 C26 1.403(3) . ? C21 C22 1.406(3) . ? C22 C23 1.395(4) . ? C22 C221 1.508(3) . ? C23 C24 1.402(4) . ? C23 H23A 0.9500 . ? C24 C25 1.379(4) . ? C24 C241 1.513(4) . ? C25 C26 1.394(3) . ? C25 H25A 0.9500 . ? C26 C261 1.508(3) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C161 H16A 0.9800 . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C261 H26A 0.9800 . ? C261 H26B 0.9800 . ? C261 H26C 0.9800 . ? 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 Cr1 O1 79.54(7) . 2_655 ? O1 Cr1 N1 98.23(7) . . ? O1 Cr1 N1 177.15(7) 2_655 . ? O1 Cr1 O2 165.10(6) . . ? O1 Cr1 O2 89.71(6) 2_655 . ? N1 Cr1 O2 92.80(7) . . ? N1 Si1 N2 106.37(9) . . ? N1 Si1 C1 119.96(12) . . ? N2 Si1 C1 103.68(11) . . ? N1 Si1 C2 109.10(11) . . ? N2 Si1 C2 113.40(12) . . ? C1 Si1 C2 104.49(13) . . ? O1 Si2 N2 109.44(9) . . ? O1 Si2 C3 110.54(10) . . ? N2 Si2 C3 108.44(11) . . ? O1 Si2 C4 109.80(11) . . ? N2 Si2 C4 109.71(11) . . ? C3 Si2 C4 108.89(14) . . ? Si2 O1 Cr1 123.10(8) . . ? Si2 O1 Cr1 138.75(9) . 2_655 ? Cr1 O1 Cr1 96.73(6) . 2_655 ? C8 O2 C5 110.2(2) . . ? C8 O2 Cr1 121.36(15) . . ? C5 O2 Cr1 125.13(17) . . ? C11 N1 Si1 121.69(15) . . ? C11 N1 Cr1 115.38(14) . . ? Si1 N1 Cr1 122.36(10) . . ? C21 N2 Si2 118.87(15) . . ? C21 N2 Si1 119.11(15) . . ? Si2 N2 Si1 121.95(11) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C6 105.9(3) . . ? O2 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? O2 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C7 C6 C5 104.4(3) . . ? C7 C6 H6A 110.9 . . ? C5 C6 H6A 110.9 . . ? C7 C6 H6B 110.9 . . ? C5 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C6 C7 C8 102.5(4) . . ? C6 C7 H7A 111.3 . . ? C8 C7 H7A 111.3 . . ? C6 C7 H7B 111.3 . . ? C8 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? H7AA C7A H7AB 108.3 . . ? O2 C8 C7 104.4(3) . . ? O2 C8 H8A 110.9 . . ? C7 C8 H8A 110.9 . . ? O2 C8 H8B 110.9 . . ? C7 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C12 C11 C16 116.5(2) . . ? C12 C11 N1 122.6(2) . . ? C16 C11 N1 120.9(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 C121 118.0(3) . . ? C11 C12 C121 122.0(2) . . ? C14 C13 C12 123.7(3) . . ? C14 C13 H13A 118.2 . . ? C12 C13 H13A 118.2 . . ? C13 C14 C15 116.3(3) . . ? C13 C14 C141 122.1(3) . . ? C15 C14 C141 121.6(3) . . ? C14 C15 C16 122.8(3) . . ? C14 C15 H15A 118.6 . . ? C16 C15 H15A 118.6 . . ? C15 C16 C11 120.7(3) . . ? C15 C16 C161 118.7(3) . . ? C11 C16 C161 120.5(2) . . ? C26 C21 C22 119.3(2) . . ? C26 C21 N2 120.13(19) . . ? C22 C21 N2 120.5(2) . . ? C23 C22 C21 118.8(2) . . ? C23 C22 C221 120.0(2) . . ? C21 C22 C221 121.1(2) . . ? C22 C23 C24 122.7(2) . . ? C22 C23 H23A 118.6 . . ? C24 C23 H23A 118.6 . . ? C25 C24 C23 116.9(2) . . ? C25 C24 C241 121.3(3) . . ? C23 C24 C241 121.8(2) . . ? C24 C25 C26 122.6(2) . . ? C24 C25 H25A 118.7 . . ? C26 C25 H25A 118.7 . . ? C25 C26 C21 119.6(2) . . ? C25 C26 C261 119.7(2) . . ? C21 C26 C261 120.7(2) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.350 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.052 #============================================================================= #============================================================================= data_Pr2PhNNOCr _database_code_depnum_ccdc_archive 'CCDC 254126' #============================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H92 Cr2 N4 O2 Si4' _chemical_formula_weight 1069.69 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.727(4) _cell_length_b 15.844(6) _cell_length_c 19.010(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.599(6) _cell_angle_gamma 90.00 _cell_volume 2879.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.27 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15641 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4955 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0588P)^2^+2.0616P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4955 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cr1 Cr 0.48671(7) 0.03071(4) 0.92637(3) 0.01633(19) Uani 1 1 d . . . Si1 Si 0.61747(12) 0.21462(6) 0.88307(6) 0.0163(3) Uani 1 1 d . . . Si2 Si 0.70897(12) 0.13695(6) 1.02917(6) 0.0165(3) Uani 1 1 d . . . O1 O 0.5947(3) 0.05946(15) 1.02096(14) 0.0171(6) Uani 1 1 d . . . N1 N 0.5595(3) 0.11440(18) 0.86646(17) 0.0157(7) Uani 1 1 d . . . N2 N 0.6423(3) 0.22159(18) 0.97596(16) 0.0147(7) Uani 1 1 d . . . C1 C 0.7825(4) 0.2347(2) 0.8495(2) 0.0247(10) Uani 1 1 d . . . H1A H 0.8521 0.1919 0.8688 0.037 Uiso 1 1 calc R . . H1B H 0.8183 0.2908 0.8649 0.037 Uiso 1 1 calc R . . H1C H 0.7642 0.2319 0.7971 0.037 Uiso 1 1 calc R . . C2 C 0.4960(5) 0.2998(2) 0.8425(2) 0.0268(10) Uani 1 1 d . . . H2A H 0.4060 0.2934 0.8581 0.040 Uiso 1 1 calc R . . H2B H 0.4819 0.2959 0.7902 0.040 Uiso 1 1 calc R . . H2C H 0.5364 0.3550 0.8579 0.040 Uiso 1 1 calc R . . C3 C 0.8700(4) 0.0968(3) 1.0021(2) 0.0288(11) Uani 1 1 d . . . H3A H 0.8489 0.0793 0.9518 0.043 Uiso 1 1 calc R . . H3B H 0.9055 0.0484 1.0321 0.043 Uiso 1 1 calc R . . H3C H 0.9408 0.1415 1.0080 0.043 Uiso 1 1 calc R . . C4 C 0.7482(5) 0.1699(3) 1.1233(2) 0.0279(11) Uani 1 1 d . . . H4A H 0.6628 0.1912 1.1376 0.042 Uiso 1 1 calc R . . H4B H 0.8191 0.2145 1.1293 0.042 Uiso 1 1 calc R . . H4C H 0.7837 0.1215 1.1534 0.042 Uiso 1 1 calc R . . C11 C 0.4986(4) 0.0628(2) 0.8103(2) 0.0169(9) Uani 1 1 d . . . C12 C 0.5787(5) 0.0074(2) 0.7747(2) 0.0221(10) Uani 1 1 d . . . C121 C 0.7351(4) 0.0188(2) 0.7838(2) 0.0244(10) Uani 1 1 d . . . H12A H 0.7668 0.0549 0.8269 0.029 Uiso 1 1 calc R . . C122 C 0.7699(5) 0.0644(3) 0.7185(3) 0.0418(13) Uani 1 1 d . . . H12B H 0.7186 0.1179 0.7117 0.063 Uiso 1 1 calc R . . H12C H 0.7429 0.0290 0.6760 0.063 Uiso 1 1 calc R . . H12D H 0.8706 0.0757 0.7260 0.063 Uiso 1 1 calc R . . C123 C 0.8143(5) -0.0640(3) 0.7942(3) 0.0487(15) Uani 1 1 d . . . H12E H 0.7919 -0.0934 0.8361 0.073 Uiso 1 1 calc R . . H12F H 0.9151 -0.0528 0.8017 0.073 Uiso 1 1 calc R . . H12G H 0.7873 -0.0994 0.7516 0.073 Uiso 1 1 calc R . . C13 C 0.5128(5) -0.0540(3) 0.7301(2) 0.0283(11) Uani 1 1 d . . . H13A H 0.5669 -0.0912 0.7070 0.034 Uiso 1 1 calc R . . C14 C 0.3683(5) -0.0630(3) 0.7181(2) 0.0311(11) Uani 1 1 d . . . H14A H 0.3246 -0.1067 0.6876 0.037 Uiso 1 1 calc R . . C15 C 0.2901(5) -0.0099(3) 0.7496(2) 0.0290(11) Uani 1 1 d . . . H15A H 0.1912 -0.0159 0.7400 0.035 Uiso 1 1 calc R . . C16 C 0.3502(4) 0.0539(2) 0.7959(2) 0.0216(10) Uani 1 1 d . . . C161 C 0.2546(4) 0.1181(2) 0.8210(2) 0.0239(10) Uani 1 1 d . . . H16A H 0.3141 0.1567 0.8555 0.029 Uiso 1 1 calc R . . C162 C 0.1467(5) 0.0778(3) 0.8600(3) 0.0368(12) Uani 1 1 d . . . H16B H 0.1948 0.0437 0.9001 0.055 Uiso 1 1 calc R . . H16C H 0.0837 0.0417 0.8267 0.055 Uiso 1 1 calc R . . H16D H 0.0924 0.1222 0.8782 0.055 Uiso 1 1 calc R . . C163 C 0.1830(6) 0.1712(3) 0.7578(3) 0.0443(14) Uani 1 1 d . . . H16E H 0.2540 0.1962 0.7336 0.067 Uiso 1 1 calc R . . H16F H 0.1286 0.2162 0.7751 0.067 Uiso 1 1 calc R . . H16G H 0.1206 0.1353 0.7240 0.067 Uiso 1 1 calc R . . C21 C 0.6011(4) 0.2964(2) 1.0106(2) 0.0190(9) Uani 1 1 d . . . C22 C 0.6968(4) 0.3609(2) 1.0317(2) 0.0195(9) Uani 1 1 d . . . C221 C 0.8443(4) 0.3587(2) 1.0173(2) 0.0247(10) Uani 1 1 d . . . H22A H 0.8608 0.3017 0.9978 0.030 Uiso 1 1 calc R . . C222 C 0.8613(5) 0.4241(3) 0.9613(2) 0.0342(12) Uani 1 1 d . . . H22B H 0.7911 0.4143 0.9180 0.051 Uiso 1 1 calc R . . H22C H 0.9551 0.4195 0.9497 0.051 Uiso 1 1 calc R . . H22D H 0.8485 0.4806 0.9799 0.051 Uiso 1 1 calc R . . C223 C 0.9524(5) 0.3724(3) 1.0851(3) 0.0351(12) Uani 1 1 d . . . H22E H 0.9399 0.3299 1.1208 0.053 Uiso 1 1 calc R . . H22F H 0.9404 0.4289 1.1042 0.053 Uiso 1 1 calc R . . H22G H 1.0466 0.3674 1.0740 0.053 Uiso 1 1 calc R . . C23 C 0.6546(5) 0.4318(3) 1.0656(2) 0.0287(11) Uani 1 1 d . . . H23A H 0.7195 0.4762 1.0797 0.034 Uiso 1 1 calc R . . C24 C 0.5223(5) 0.4386(3) 1.0791(3) 0.0350(12) Uani 1 1 d . . . H24A H 0.4957 0.4871 1.1028 0.042 Uiso 1 1 calc R . . C25 C 0.4275(5) 0.3752(3) 1.0585(2) 0.0328(11) Uani 1 1 d . . . H25A H 0.3354 0.3804 1.0681 0.039 Uiso 1 1 calc R . . C26 C 0.4636(5) 0.3033(2) 1.0238(2) 0.0233(10) Uani 1 1 d . . . C261 C 0.3546(5) 0.2364(3) 1.0031(2) 0.0299(11) Uani 1 1 d . . . H26A H 0.3907 0.1962 0.9702 0.036 Uiso 1 1 calc R . . C262 C 0.3301(6) 0.1863(3) 1.0684(3) 0.0484(14) Uani 1 1 d . . . H26D H 0.4192 0.1635 1.0937 0.073 Uiso 1 1 calc R . . H26E H 0.2652 0.1398 1.0528 0.073 Uiso 1 1 calc R . . H26B H 0.2901 0.2235 1.1006 0.073 Uiso 1 1 calc R . . C263 C 0.2152(5) 0.2725(3) 0.9625(3) 0.0477(14) Uani 1 1 d . . . H26C H 0.2321 0.3046 0.9208 0.072 Uiso 1 1 calc R . . H26H H 0.1744 0.3099 0.9943 0.072 Uiso 1 1 calc R . . H26F H 0.1503 0.2261 0.9465 0.072 Uiso 1 1 calc 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 0.0182(4) 0.0147(3) 0.0158(4) 0.0007(3) 0.0024(3) -0.0046(3) Si1 0.0175(6) 0.0135(5) 0.0184(6) 0.0013(5) 0.0045(5) -0.0022(5) Si2 0.0172(6) 0.0146(5) 0.0172(6) 0.0002(5) 0.0015(5) -0.0042(5) O1 0.0197(15) 0.0152(12) 0.0162(15) 0.0007(11) 0.0034(12) -0.0054(12) N1 0.0185(18) 0.0146(15) 0.0139(18) 0.0005(14) 0.0028(14) -0.0027(15) N2 0.0172(18) 0.0137(15) 0.0138(18) -0.0005(14) 0.0043(14) 0.0015(14) C1 0.027(2) 0.023(2) 0.026(3) 0.0006(19) 0.009(2) -0.010(2) C2 0.030(3) 0.020(2) 0.031(3) 0.0084(19) 0.006(2) -0.001(2) C3 0.022(2) 0.031(2) 0.033(3) 0.004(2) 0.004(2) 0.001(2) C4 0.040(3) 0.022(2) 0.018(2) -0.0007(18) -0.004(2) -0.010(2) C11 0.019(2) 0.0183(18) 0.012(2) 0.0029(17) 0.0007(17) -0.0042(18) C12 0.031(3) 0.0196(19) 0.016(2) 0.0005(17) 0.0031(19) -0.001(2) C121 0.027(2) 0.024(2) 0.023(3) -0.0073(19) 0.007(2) -0.003(2) C122 0.039(3) 0.054(3) 0.034(3) -0.002(3) 0.010(2) -0.015(3) C123 0.036(3) 0.037(3) 0.074(4) -0.002(3) 0.013(3) 0.004(3) C13 0.038(3) 0.030(2) 0.019(3) -0.0075(19) 0.008(2) -0.002(2) C14 0.038(3) 0.029(2) 0.025(3) -0.005(2) 0.002(2) -0.016(2) C15 0.031(3) 0.031(2) 0.022(3) 0.002(2) -0.001(2) -0.012(2) C16 0.028(2) 0.021(2) 0.014(2) 0.0024(17) 0.0006(19) -0.0022(19) C161 0.020(2) 0.024(2) 0.027(3) 0.0026(19) 0.0027(19) -0.003(2) C162 0.025(3) 0.036(3) 0.052(3) 0.004(2) 0.014(2) -0.002(2) C163 0.052(3) 0.037(3) 0.041(3) 0.011(2) 0.001(3) 0.003(3) C21 0.023(2) 0.0180(19) 0.018(2) 0.0021(17) 0.0080(18) 0.0058(19) C22 0.027(2) 0.0158(19) 0.015(2) 0.0018(17) 0.0026(18) -0.0001(19) C221 0.028(2) 0.0189(19) 0.027(3) -0.0044(18) 0.006(2) -0.007(2) C222 0.039(3) 0.030(2) 0.034(3) -0.001(2) 0.007(2) -0.015(2) C223 0.033(3) 0.037(3) 0.034(3) -0.004(2) 0.005(2) -0.011(2) C23 0.040(3) 0.018(2) 0.028(3) -0.0023(19) 0.007(2) -0.001(2) C24 0.051(3) 0.023(2) 0.031(3) -0.002(2) 0.010(2) 0.014(3) C25 0.027(3) 0.040(3) 0.034(3) -0.002(2) 0.011(2) 0.010(2) C26 0.029(2) 0.022(2) 0.020(2) -0.0020(18) 0.0055(19) 0.001(2) C261 0.026(3) 0.033(2) 0.033(3) -0.011(2) 0.014(2) -0.006(2) C262 0.046(3) 0.048(3) 0.057(4) -0.002(3) 0.025(3) -0.012(3) C263 0.025(3) 0.067(4) 0.051(4) -0.016(3) 0.008(2) 0.003(3) _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 Cr1 O1 1.962(3) . ? Cr1 N1 1.963(3) . ? Cr1 O1 1.990(3) 3_657 ? Cr1 C11 2.287(4) . ? Cr1 Cr1 2.9298(16) 3_657 ? Si1 N1 1.695(3) . ? Si1 N2 1.741(3) . ? Si1 C1 1.861(4) . ? Si1 C2 1.865(4) . ? Si2 O1 1.644(3) . ? Si2 N2 1.732(3) . ? Si2 C4 1.836(4) . ? Si2 C3 1.849(4) . ? O1 Cr1 1.990(3) 3_657 ? N1 C11 1.387(5) . ? N2 C21 1.448(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 C12 1.425(6) . ? C11 C16 1.427(6) . ? C12 C13 1.369(6) . ? C12 C121 1.509(6) . ? C121 C123 1.517(6) . ? C121 C122 1.526(6) . ? C121 H12A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C13 C14 1.389(6) . ? C13 H13A 0.9500 . ? C14 C15 1.347(6) . ? C14 H14A 0.9500 . ? C15 C16 1.396(6) . ? C15 H15A 0.9500 . ? C16 C161 1.513(6) . ? C161 C163 1.527(6) . ? C161 C162 1.531(6) . ? C161 H16A 1.0000 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C163 H16G 0.9800 . ? C21 C22 1.390(5) . ? C21 C26 1.409(6) . ? C22 C23 1.395(5) . ? C22 C221 1.509(6) . ? C221 C222 1.517(6) . ? C221 C223 1.521(6) . ? C221 H22A 1.0000 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C222 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C23 C24 1.363(6) . ? C23 H23A 0.9500 . ? C24 C25 1.370(6) . ? C24 H24A 0.9500 . ? C25 C26 1.394(6) . ? C25 H25A 0.9500 . ? C26 C261 1.500(6) . ? C261 C262 1.530(7) . ? C261 C263 1.542(6) . ? C261 H26A 1.0000 . ? C262 H26D 0.9800 . ? C262 H26E 0.9800 . ? C262 H26B 0.9800 . ? C263 H26C 0.9800 . ? C263 H26H 0.9800 . ? C263 H26F 0.9800 . ? 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 Cr1 N1 100.69(12) . . ? O1 Cr1 O1 84.32(11) . 3_657 ? N1 Cr1 O1 174.85(12) . 3_657 ? O1 Cr1 C11 135.94(13) . . ? N1 Cr1 C11 37.11(13) . . ? O1 Cr1 C11 137.74(12) 3_657 . ? O1 Cr1 Cr1 42.54(8) . 3_657 ? N1 Cr1 Cr1 143.21(10) . 3_657 ? O1 Cr1 Cr1 41.79(8) 3_657 3_657 ? C11 Cr1 Cr1 169.75(11) . 3_657 ? N1 Si1 N2 103.16(15) . . ? N1 Si1 C1 111.99(17) . . ? N2 Si1 C1 111.69(18) . . ? N1 Si1 C2 115.95(18) . . ? N2 Si1 C2 109.43(18) . . ? C1 Si1 C2 104.79(19) . . ? O1 Si2 N2 110.41(15) . . ? O1 Si2 C4 108.68(17) . . ? N2 Si2 C4 109.75(18) . . ? O1 Si2 C3 108.01(17) . . ? N2 Si2 C3 110.41(18) . . ? C4 Si2 C3 109.5(2) . . ? Si2 O1 Cr1 119.93(15) . . ? Si2 O1 Cr1 144.36(16) . 3_657 ? Cr1 O1 Cr1 95.68(11) . 3_657 ? C11 N1 Si1 140.8(3) . . ? C11 N1 Cr1 84.2(2) . . ? Si1 N1 Cr1 131.90(19) . . ? C21 N2 Si2 118.3(2) . . ? C21 N2 Si1 121.0(2) . . ? Si2 N2 Si1 120.68(17) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C11 C12 122.4(4) . . ? N1 C11 C16 118.7(4) . . ? C12 C11 C16 118.0(4) . . ? N1 C11 Cr1 58.64(19) . . ? C12 C11 Cr1 116.8(3) . . ? C16 C11 Cr1 86.2(2) . . ? C13 C12 C11 119.8(4) . . ? C13 C12 C121 120.2(4) . . ? C11 C12 C121 119.9(4) . . ? C12 C121 C123 112.9(4) . . ? C12 C121 C122 109.4(4) . . ? C123 C121 C122 109.4(4) . . ? C12 C121 H12A 108.3 . . ? C123 C121 H12A 108.3 . . ? C122 C121 H12A 108.3 . . ? C121 C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C123 H12G 109.5 . . ? H12E C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 121.9(4) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C15 C16 C11 119.0(4) . . ? C15 C16 C161 118.4(4) . . ? C11 C16 C161 122.1(4) . . ? C16 C161 C163 109.9(4) . . ? C16 C161 C162 112.9(3) . . ? C163 C161 C162 110.9(4) . . ? C16 C161 H16A 107.7 . . ? C163 C161 H16A 107.7 . . ? C162 C161 H16A 107.7 . . ? C161 C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C163 H16G 109.5 . . ? H16E C163 H16G 109.5 . . ? H16F C163 H16G 109.5 . . ? C22 C21 C26 119.9(4) . . ? C22 C21 N2 120.3(3) . . ? C26 C21 N2 119.7(3) . . ? C21 C22 C23 119.1(4) . . ? C21 C22 C221 122.7(3) . . ? C23 C22 C221 118.2(4) . . ? C22 C221 C222 109.9(4) . . ? C22 C221 C223 112.1(4) . . ? C222 C221 C223 110.5(4) . . ? C22 C221 H22A 108.1 . . ? C222 C221 H22A 108.1 . . ? C223 C221 H22A 108.1 . . ? C221 C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? H22B C222 H22D 109.5 . . ? H22C C222 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C223 H22G 109.5 . . ? H22E C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C24 C23 C22 121.3(4) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 119.8(4) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 121.3(4) . . ? C24 C25 H25A 119.4 . . ? C26 C25 H25A 119.4 . . ? C25 C26 C21 118.6(4) . . ? C25 C26 C261 118.3(4) . . ? C21 C26 C261 123.2(4) . . ? C26 C261 C262 111.2(4) . . ? C26 C261 C263 112.6(4) . . ? C262 C261 C263 110.2(4) . . ? C26 C261 H26A 107.5 . . ? C262 C261 H26A 107.5 . . ? C263 C261 H26A 107.5 . . ? C261 C262 H26D 109.5 . . ? C261 C262 H26E 109.5 . . ? H26D C262 H26E 109.5 . . ? C261 C262 H26B 109.5 . . ? H26D C262 H26B 109.5 . . ? H26E C262 H26B 109.5 . . ? C261 C263 H26C 109.5 . . ? C261 C263 H26H 109.5 . . ? H26C C263 H26H 109.5 . . ? C261 C263 H26F 109.5 . . ? H26C C263 H26F 109.5 . . ? H26H C263 H26F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Si2 O1 Cr1 41.4(2) . . . . ? C4 Si2 O1 Cr1 161.82(19) . . . . ? C3 Si2 O1 Cr1 -79.4(2) . . . . ? N2 Si2 O1 Cr1 -141.1(3) . . . 3_657 ? C4 Si2 O1 Cr1 -20.7(3) . . . 3_657 ? C3 Si2 O1 Cr1 98.1(3) . . . 3_657 ? N1 Cr1 O1 Si2 -0.29(19) . . . . ? O1 Cr1 O1 Si2 178.5(2) 3_657 . . . ? C11 Cr1 O1 Si2 13.3(3) . . . . ? Cr1 Cr1 O1 Si2 178.5(2) 3_657 . . . ? N1 Cr1 O1 Cr1 -178.81(12) . . . 3_657 ? O1 Cr1 O1 Cr1 0.0 3_657 . . 3_657 ? C11 Cr1 O1 Cr1 -165.20(15) . . . 3_657 ? N2 Si1 N1 C11 167.7(4) . . . . ? C1 Si1 N1 C11 -72.1(5) . . . . ? C2 Si1 N1 C11 48.1(5) . . . . ? N2 Si1 N1 Cr1 15.0(3) . . . . ? C1 Si1 N1 Cr1 135.3(2) . . . . ? C2 Si1 N1 Cr1 -104.6(3) . . . . ? O1 Cr1 N1 C11 164.3(2) . . . . ? O1 Cr1 N1 C11 -2.4(15) 3_657 . . . ? Cr1 Cr1 N1 C11 162.92(18) 3_657 . . . ? O1 Cr1 N1 Si1 -32.7(3) . . . . ? O1 Cr1 N1 Si1 160.6(12) 3_657 . . . ? C11 Cr1 N1 Si1 163.1(4) . . . . ? Cr1 Cr1 N1 Si1 -34.0(3) 3_657 . . . ? O1 Si2 N2 C21 107.7(3) . . . . ? C4 Si2 N2 C21 -12.1(3) . . . . ? C3 Si2 N2 C21 -133.0(3) . . . . ? O1 Si2 N2 Si1 -69.1(2) . . . . ? C4 Si2 N2 Si1 171.1(2) . . . . ? C3 Si2 N2 Si1 50.2(3) . . . . ? N1 Si1 N2 C21 -138.4(3) . . . . ? C1 Si1 N2 C21 101.2(3) . . . . ? C2 Si1 N2 C21 -14.4(3) . . . . ? N1 Si1 N2 Si2 38.4(2) . . . . ? C1 Si1 N2 Si2 -82.1(2) . . . . ? C2 Si1 N2 Si2 162.3(2) . . . . ? Si1 N1 C11 C12 96.3(5) . . . . ? Cr1 N1 C11 C12 -103.8(3) . . . . ? Si1 N1 C11 C16 -94.8(5) . . . . ? Cr1 N1 C11 C16 65.1(3) . . . . ? Si1 N1 C11 Cr1 -159.9(5) . . . . ? O1 Cr1 C11 N1 -22.5(3) . . . . ? O1 Cr1 C11 N1 179.7(2) 3_657 . . . ? Cr1 Cr1 C11 N1 -98.6(6) 3_657 . . . ? O1 Cr1 C11 C12 90.7(3) . . . . ? N1 Cr1 C11 C12 113.2(4) . . . . ? O1 Cr1 C11 C12 -67.1(4) 3_657 . . . ? Cr1 Cr1 C11 C12 14.6(8) 3_657 . . . ? O1 Cr1 C11 C16 -149.7(2) . . . . ? N1 Cr1 C11 C16 -127.1(3) . . . . ? O1 Cr1 C11 C16 52.5(3) 3_657 . . . ? Cr1 Cr1 C11 C16 134.2(5) 3_657 . . . ? N1 C11 C12 C13 166.7(4) . . . . ? C16 C11 C12 C13 -2.3(6) . . . . ? Cr1 C11 C12 C13 98.4(4) . . . . ? N1 C11 C12 C121 -15.8(6) . . . . ? C16 C11 C12 C121 175.3(4) . . . . ? Cr1 C11 C12 C121 -84.0(4) . . . . ? C13 C12 C121 C123 -45.2(6) . . . . ? C11 C12 C121 C123 137.2(4) . . . . ? C13 C12 C121 C122 76.9(5) . . . . ? C11 C12 C121 C122 -100.7(4) . . . . ? C11 C12 C13 C14 0.8(6) . . . . ? C121 C12 C13 C14 -176.7(4) . . . . ? C12 C13 C14 C15 1.1(7) . . . . ? C13 C14 C15 C16 -1.4(7) . . . . ? C14 C15 C16 C11 -0.1(6) . . . . ? C14 C15 C16 C161 171.8(4) . . . . ? N1 C11 C16 C15 -167.4(4) . . . . ? C12 C11 C16 C15 2.0(6) . . . . ? Cr1 C11 C16 C15 -116.5(4) . . . . ? N1 C11 C16 C161 21.0(6) . . . . ? C12 C11 C16 C161 -169.6(4) . . . . ? Cr1 C11 C16 C161 71.9(4) . . . . ? C15 C16 C161 C163 -66.0(5) . . . . ? C11 C16 C161 C163 105.7(4) . . . . ? C15 C16 C161 C162 58.3(5) . . . . ? C11 C16 C161 C162 -130.0(4) . . . . ? Si2 N2 C21 C22 90.1(4) . . . . ? Si1 N2 C21 C22 -93.1(4) . . . . ? Si2 N2 C21 C26 -89.0(4) . . . . ? Si1 N2 C21 C26 87.8(4) . . . . ? C26 C21 C22 C23 -0.1(6) . . . . ? N2 C21 C22 C23 -179.2(3) . . . . ? C26 C21 C22 C221 -178.2(4) . . . . ? N2 C21 C22 C221 2.6(6) . . . . ? C21 C22 C221 C222 109.9(4) . . . . ? C23 C22 C221 C222 -68.3(5) . . . . ? C21 C22 C221 C223 -126.9(4) . . . . ? C23 C22 C221 C223 54.9(5) . . . . ? C21 C22 C23 C24 0.7(6) . . . . ? C221 C22 C23 C24 178.9(4) . . . . ? C22 C23 C24 C25 -0.6(7) . . . . ? C23 C24 C25 C26 0.0(7) . . . . ? C24 C25 C26 C21 0.5(6) . . . . ? C24 C25 C26 C261 179.8(4) . . . . ? C22 C21 C26 C25 -0.5(6) . . . . ? N2 C21 C26 C25 178.7(4) . . . . ? C22 C21 C26 C261 -179.7(4) . . . . ? N2 C21 C26 C261 -0.5(6) . . . . ? C25 C26 C261 C262 -74.3(5) . . . . ? C21 C26 C261 C262 104.9(5) . . . . ? C25 C26 C261 C263 50.0(6) . . . . ? C21 C26 C261 C263 -130.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.357 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.079