# CIF-file generated for BASH 1044-173 # Compound xx #=================================================================== data_global #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 6-Jul-06 _audit_creation_method 'PLATON option' _audit_update_record ; 6-Jul-06 Updated by the Author E.H. Text writing by E.H. Checkcif OK 17-Jul-06 Updated by the Author E.H. 28-Aug-06 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== # Name and address of author for X-ray correspondence _publ_contact_author_name ; Dr. Eberhardt Herdtweck ; _publ_contact_author_address ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_email 'eberhardt.herdtweck@ch.tum.de' _publ_contact_author_fax '+49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' _publ_requested_journal 'Organometallics' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission: August 2006 ; #=================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) #=================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=================================================================== # 3. TITLE AND AUTHOR LIST #=================================================================== _publ_section_title ; Chiral N-Heterocyclic Carbene with Restricted Flexibility in Asymmetric Catalysis ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Baskakov, D.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Herrmann, W. A.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Herdtweck, E.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; 'Hoffmann, S. D.' ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie mit Schwerpunkt Neue Materialen, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; #=================================================================== # 4. TEXT #=================================================================== _publ_section_synopsis ; ; _publ_section_abstract ; A novel chiral C2-symmetric diamine... ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_experimental ; ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Farrugia, L. J. (1999). WinGX (Version 1.70.01 January 2005), J. Appl. Cryst. 32, 837-838. Sheldrick, G. M. (1998). SHELXS-97, University of G\"ottingen, G\"ottingen, Germany. Sheldrick, G. M. (1998). SHELXL-97, University of G\"ottingen, G\"ottingen, Germany. Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Stoe (2004). X-AREA, Version 1.26, Stoe & Cie GmbH, Darmstadt, Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; #=================================================================== data_BASH-1044-173 #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C39 H36 Cl N2 Rh' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H36 Cl N2 Rh' _chemical_formula_weight 671.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 8.7505(4) _cell_length_b 17.5279(8) _cell_length_c 20.1836(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3095.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 24213 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 27.27 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method none _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details ; Numerical absorption correction after crystal shape optimization source: (Stoe, 2004) ; _exptl_special_details ; Diffractometer operator S. Hoffmann exposure_time 120 s per image exposure_run_1_phi 0 exposure_omega_range 1-180 exposure_delta_omega 1.0 exposure_run_2_phi 90 exposure_omega_range 1-180 exposure_delta_omega 1.0 exposure_sum_images 360 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Solution and refinements with the program WinGX; Farrugia (1999). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'IPDS 2T (Stoe)' _diffrn_measurement_method 'omega-rotation/oscillation ' _diffrn_detector 'image plate' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 39503 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 26.76 _reflns_number_total 6539 _reflns_number_gt 6300 # number of observed reflections (> n sig(I)) _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'X-AREA (Stoe, 2004)' _computing_cell_refinement 'X-AREA (Stoe, 2004)' _computing_data_reduction 'X-AREA (Stoe, 2004)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'PLATON (Spek, 2005)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0293P)^2^+1.0760P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(19) _chemical_absolute_configuration ad _refine_ls_number_reflns 6539 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.301 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.075 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Rh Rh Uani 0.03422(2) 0.40703(1) 0.08739(1) 1.000 0.0252(1) . . Cl Cl Uani -0.22783(7) 0.37117(4) 0.07552(3) 1.000 0.0345(2) . . N1 N Uani -0.0472(3) 0.51494(10) -0.02393(9) 1.000 0.0242(6) . . N2 N Uani -0.0105(2) 0.57944(10) 0.06420(8) 1.000 0.0236(6) . . C1 C Uani -0.0110(3) 0.50654(13) 0.04074(11) 1.000 0.0246(7) . . C2 C Uani -0.0715(3) 0.59130(14) -0.04149(10) 1.000 0.0239(6) . . C3 C Uani -0.0506(3) 0.63254(13) 0.01542(10) 1.000 0.0246(7) . . C4 C Uani -0.0710(3) 0.45066(13) -0.06998(11) 1.000 0.0271(7) . . C5 C Uani -0.2062(3) 0.47303(15) -0.11394(13) 1.000 0.0303(8) . . C6 C Uani -0.1778(3) 0.54862(15) -0.14749(12) 1.000 0.0269(7) . . C7 C Uani -0.1091(3) 0.60765(14) -0.11141(11) 1.000 0.0262(7) . . C8 C Uani -0.0711(3) 0.67628(15) -0.14288(12) 1.000 0.0302(8) . . C9 C Uani -0.1088(3) 0.68575(17) -0.20954(12) 1.000 0.0346(8) . . C10 C Uani -0.1802(3) 0.62884(17) -0.24443(12) 1.000 0.0353(8) . . C11 C Uani -0.2138(3) 0.56025(16) -0.21416(12) 1.000 0.0325(8) . . C12 C Uani -0.0083(3) 0.60196(14) 0.13438(10) 1.000 0.0258(7) . . C13 C Uani 0.0846(3) 0.67565(15) 0.13748(12) 1.000 0.0293(7) . . C14 C Uani 0.0121(3) 0.73596(13) 0.09398(11) 1.000 0.0272(7) . . C15 C Uani -0.0595(3) 0.71305(14) 0.03465(11) 1.000 0.0256(7) . . C16 C Uani -0.1388(3) 0.76775(14) -0.00281(13) 1.000 0.0326(8) . . C17 C Uani -0.1374(4) 0.84390(16) 0.01567(14) 1.000 0.0395(9) . . C18 C Uani -0.0593(3) 0.86625(15) 0.07213(13) 1.000 0.0394(9) . . C19 C Uani 0.0118(3) 0.81226(15) 0.11156(12) 1.000 0.0336(8) . . C20 C Uani 0.0742(3) 0.42895(14) -0.10631(11) 1.000 0.0269(7) . . C21 C Uani 0.1085(3) 0.35127(15) -0.11264(13) 1.000 0.0336(8) . . C22 C Uani 0.2400(4) 0.32677(17) -0.14526(15) 1.000 0.0414(9) . . C23 C Uani 0.3385(4) 0.37922(18) -0.17157(14) 1.000 0.0431(9) . . C24 C Uani 0.3076(4) 0.45648(18) -0.16583(15) 1.000 0.0423(10) . . C25 C Uani 0.1760(3) 0.48119(15) -0.13368(13) 1.000 0.0344(8) . . C26 C Uani -0.1714(3) 0.60877(13) 0.16029(11) 1.000 0.0275(7) . . C27 C Uani -0.2902(3) 0.56908(17) 0.13097(14) 1.000 0.0370(8) . . C28 C Uani -0.4370(3) 0.57224(18) 0.15664(15) 1.000 0.0444(10) . . C29 C Uani -0.4674(4) 0.61447(16) 0.21243(14) 1.000 0.0406(8) . . C30 C Uani -0.3510(3) 0.65480(16) 0.24161(13) 1.000 0.0375(8) . . C31 C Uani -0.2052(3) 0.65253(15) 0.21623(12) 1.000 0.0325(8) . . C32 C Uani 0.2504(3) 0.44686(16) 0.12013(14) 1.000 0.0346(8) . . C33 C Uani 0.2649(3) 0.41392(19) 0.05710(13) 1.000 0.0371(8) . . C34 C Uani 0.3285(4) 0.3349(2) 0.04252(16) 1.000 0.0486(10) . . C35 C Uani 0.2653(4) 0.27255(18) 0.08716(18) 1.000 0.0519(10) . . C36 C Uani 0.1036(4) 0.28732(15) 0.11064(14) 1.000 0.0389(8) . . C37 C Uani 0.0693(3) 0.32387(14) 0.16855(13) 1.000 0.0344(8) . . C38 C Uani 0.1793(4) 0.35968(18) 0.21616(14) 1.000 0.0440(10) . . C39 C Uani 0.3033(4) 0.4079(2) 0.18358(13) 1.000 0.0426(9) . . H41 H Uiso -0.10310 0.40560 -0.04300 1.000 0.0320 calc R H51 H Uiso -0.22260 0.43310 -0.14790 1.000 0.0360 calc R H52 H Uiso -0.29990 0.47650 -0.08660 1.000 0.0360 calc R H81 H Uiso -0.02060 0.71580 -0.11920 1.000 0.0360 calc R H91 H Uiso -0.08450 0.73240 -0.23110 1.000 0.0420 calc R H101 H Uiso -0.20660 0.63670 -0.28960 1.000 0.0420 calc R H111 H Uiso -0.26180 0.52080 -0.23880 1.000 0.0390 calc R H121 H Uiso 0.04620 0.56170 0.16030 1.000 0.0310 calc R H131 H Uiso 0.08910 0.69410 0.18380 1.000 0.0350 calc R H132 H Uiso 0.19040 0.66570 0.12240 1.000 0.0350 calc R H161 H Uiso -0.19380 0.75240 -0.04110 1.000 0.0390 calc R H171 H Uiso -0.19000 0.88070 -0.01030 1.000 0.0470 calc R H181 H Uiso -0.05460 0.91870 0.08380 1.000 0.0470 calc R H191 H Uiso 0.06120 0.82780 0.15120 1.000 0.0400 calc R H211 H Uiso 0.04080 0.31450 -0.09430 1.000 0.0400 calc R H221 H Uiso 0.26110 0.27380 -0.14920 1.000 0.0500 calc R H231 H Uiso 0.42830 0.36270 -0.19380 1.000 0.0520 calc R H241 H Uiso 0.37660 0.49270 -0.18400 1.000 0.0510 calc R H251 H Uiso 0.15540 0.53430 -0.13040 1.000 0.0410 calc R H271 H Uiso -0.27080 0.53920 0.09260 1.000 0.0440 calc R H281 H Uiso -0.51720 0.54500 0.13550 1.000 0.0530 calc R H291 H Uiso -0.56760 0.61580 0.23060 1.000 0.0490 calc R H301 H Uiso -0.37140 0.68470 0.27990 1.000 0.0450 calc R H311 H Uiso -0.12640 0.68110 0.23700 1.000 0.0390 calc R H321 H Uiso 0.20520 0.49600 0.12340 1.000 0.0410 calc R H331 H Uiso 0.23210 0.44350 0.02030 1.000 0.0440 calc R H341 H Uiso 0.30540 0.32170 -0.00410 1.000 0.0580 calc R H342 H Uiso 0.44100 0.33630 0.04740 1.000 0.0580 calc R H351 H Uiso 0.26760 0.22350 0.06280 1.000 0.0620 calc R H352 H Uiso 0.33270 0.26730 0.12630 1.000 0.0620 calc R H361 H Uiso 0.02160 0.27020 0.08360 1.000 0.0470 calc R H371 H Uiso -0.03590 0.32690 0.17990 1.000 0.0410 calc R H381 H Uiso 0.22880 0.31880 0.24230 1.000 0.0530 calc R H382 H Uiso 0.12130 0.39230 0.24740 1.000 0.0530 calc R H391 H Uiso 0.33790 0.44730 0.21540 1.000 0.0510 calc R H392 H Uiso 0.39200 0.37480 0.17330 1.000 0.0510 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 Rh 0.0255(1) 0.0244(1) 0.0258(1) 0.0038(1) -0.0017(1) -0.0002(1) Cl 0.0298(3) 0.0390(3) 0.0348(3) 0.0049(3) -0.0008(2) -0.0078(3) N1 0.0292(11) 0.0209(9) 0.0226(9) -0.0008(7) -0.0006(8) 0.0005(9) N2 0.0254(11) 0.0255(10) 0.0198(8) 0.0018(7) -0.0016(7) 0.0005(8) C1 0.0244(13) 0.0263(11) 0.0232(10) 0.0010(9) 0.0002(9) 0.0015(10) C2 0.0258(12) 0.0235(10) 0.0224(10) 0.0001(10) -0.0009(8) 0.0019(10) C3 0.0255(13) 0.0261(11) 0.0222(10) 0.0015(9) -0.0013(9) 0.0008(10) C4 0.0323(15) 0.0223(11) 0.0266(11) -0.0028(9) 0.0000(9) -0.0010(10) C5 0.0280(14) 0.0302(13) 0.0326(12) -0.0049(11) -0.0039(10) -0.0026(11) C6 0.0251(13) 0.0316(13) 0.0241(11) -0.0024(10) -0.0005(9) 0.0054(10) C7 0.0267(13) 0.0298(14) 0.0222(10) 0.0001(9) 0.0014(9) 0.0039(10) C8 0.0340(16) 0.0278(12) 0.0288(12) 0.0006(10) 0.0005(10) 0.0018(11) C9 0.0398(16) 0.0356(14) 0.0284(12) 0.0079(11) 0.0036(11) 0.0058(12) C10 0.0363(16) 0.0496(16) 0.0200(11) 0.0031(11) -0.0005(10) 0.0120(13) C11 0.0330(15) 0.0387(14) 0.0258(12) -0.0097(11) -0.0032(10) 0.0082(12) C12 0.0317(14) 0.0279(12) 0.0178(9) 0.0009(9) -0.0013(8) -0.0015(10) C13 0.0284(13) 0.0356(14) 0.0239(11) -0.0017(10) -0.0028(9) -0.0059(11) C14 0.0261(13) 0.0293(11) 0.0263(10) -0.0023(9) 0.0024(10) -0.0052(9) C15 0.0259(14) 0.0246(11) 0.0263(10) 0.0017(9) 0.0004(9) -0.0009(10) C16 0.0385(16) 0.0287(13) 0.0305(12) -0.0033(10) -0.0053(11) 0.0048(11) C17 0.0455(18) 0.0298(13) 0.0432(15) -0.0030(11) -0.0069(13) 0.0082(13) C18 0.0423(18) 0.0286(12) 0.0472(15) -0.0112(11) -0.0025(12) 0.0034(12) C19 0.0354(16) 0.0333(13) 0.0321(11) -0.0089(10) -0.0011(10) -0.0066(12) C20 0.0317(14) 0.0267(12) 0.0224(10) -0.0018(9) -0.0051(9) 0.0019(10) C21 0.0350(15) 0.0274(13) 0.0384(13) -0.0048(11) -0.0048(11) 0.0019(11) C22 0.0451(18) 0.0353(15) 0.0439(16) -0.0084(13) -0.0045(13) 0.0123(14) C23 0.0395(17) 0.0523(17) 0.0376(14) -0.0081(13) 0.0037(12) 0.0130(15) C24 0.0399(18) 0.0434(16) 0.0436(16) 0.0035(13) 0.0120(13) 0.0004(14) C25 0.0411(17) 0.0268(13) 0.0354(13) -0.0003(11) 0.0068(12) 0.0035(12) C26 0.0328(14) 0.0255(12) 0.0241(11) 0.0027(9) 0.0004(9) -0.0027(10) C27 0.0350(15) 0.0413(15) 0.0346(13) -0.0095(11) 0.0045(11) -0.0081(12) C28 0.0312(17) 0.0518(18) 0.0502(16) -0.0055(13) 0.0022(12) -0.0123(13) C29 0.0338(14) 0.0404(14) 0.0476(14) 0.0046(12) 0.0119(14) 0.0009(13) C30 0.0449(16) 0.0368(14) 0.0307(13) -0.0017(11) 0.0068(12) 0.0065(13) C31 0.0377(15) 0.0321(13) 0.0276(12) -0.0033(10) -0.0025(11) 0.0017(11) C32 0.0238(14) 0.0338(14) 0.0461(15) 0.0055(12) -0.0031(11) 0.0008(11) C33 0.0230(13) 0.0485(16) 0.0397(13) 0.0099(14) -0.0035(10) 0.0038(13) C34 0.0354(17) 0.066(2) 0.0444(16) -0.0022(15) -0.0005(13) 0.0150(16) C35 0.055(2) 0.0470(17) 0.0537(17) -0.0037(17) -0.0034(17) 0.0238(15) C36 0.0473(17) 0.0263(12) 0.0432(14) 0.0055(11) -0.0079(12) 0.0043(12) C37 0.0398(17) 0.0289(13) 0.0346(13) 0.0091(11) -0.0048(11) 0.0003(11) C38 0.058(2) 0.0408(16) 0.0332(14) 0.0078(12) -0.0098(13) 0.0012(14) C39 0.0395(16) 0.0503(16) 0.0380(14) -0.0032(14) -0.0126(11) -0.0011(15) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl 2.3897(7) . . yes Rh C1 2.021(2) . . yes Rh C32 2.122(3) . . yes Rh C33 2.113(3) . . yes Rh C36 2.234(3) . . yes Rh C37 2.214(3) . . yes N1 C1 1.351(3) . . yes N1 C2 1.401(3) . . yes N1 C4 1.475(3) . . yes N2 C1 1.363(3) . . yes N2 C3 1.400(3) . . yes N2 C12 1.471(3) . . yes C2 C3 1.369(3) . . no C2 C7 1.477(3) . . no C3 C15 1.466(3) . . no C4 C5 1.530(4) . . no C4 C20 1.516(4) . . no C5 C6 1.509(4) . . no C6 C7 1.401(4) . . no C6 C11 1.397(3) . . no C7 C8 1.400(4) . . no C8 C9 1.395(3) . . no C9 C10 1.372(4) . . no C10 C11 1.380(4) . . no C12 C13 1.527(4) . . no C12 C26 1.525(4) . . no C13 C14 1.514(3) . . no C14 C15 1.410(3) . . no C14 C19 1.384(3) . . no C15 C16 1.404(4) . . no C16 C17 1.386(4) . . no C17 C18 1.385(4) . . no C18 C19 1.384(4) . . no C20 C21 1.400(4) . . no C20 C25 1.392(4) . . no C21 C22 1.394(4) . . no C22 C23 1.368(5) . . no C23 C24 1.386(4) . . no C24 C25 1.391(4) . . no C26 C27 1.384(4) . . no C26 C31 1.397(3) . . no C27 C28 1.386(4) . . no C28 C29 1.374(4) . . no C29 C30 1.373(4) . . no C30 C31 1.375(4) . . no C32 C33 1.403(4) . . no C32 C39 1.523(4) . . no C33 C34 1.521(5) . . no C34 C35 1.521(5) . . no C35 C36 1.515(5) . . no C36 C37 1.366(4) . . no C37 C38 1.498(4) . . no C38 C39 1.525(5) . . no C4 H41 0.9996 . . no C5 H51 0.9901 . . no C5 H52 0.9902 . . no C8 H81 0.9505 . . no C9 H91 0.9504 . . no C10 H101 0.9505 . . no C11 H111 0.9497 . . no C12 H121 0.9996 . . no C13 H131 0.9900 . . no C13 H132 0.9900 . . no C16 H161 0.9494 . . no C17 H171 0.9501 . . no C18 H181 0.9499 . . no C19 H191 0.9493 . . no C21 H211 0.9504 . . no C22 H221 0.9500 . . no C23 H231 0.9501 . . no C24 H241 0.9498 . . no C25 H251 0.9505 . . no C27 H271 0.9502 . . no C28 H281 0.9500 . . no C29 H291 0.9507 . . no C30 H301 0.9507 . . no C31 H311 0.9497 . . no C32 H321 0.9501 . . no C33 H331 0.9502 . . no C34 H341 0.9898 . . no C34 H342 0.9897 . . no C35 H351 0.9906 . . no C35 H352 0.9901 . . no C36 H361 0.9501 . . no C37 H371 0.9501 . . no C38 H381 0.9897 . . no C38 H382 0.9910 . . no C39 H391 0.9905 . . no C39 H392 0.9910 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Rh C1 89.57(8) . . . yes Cl Rh C32 166.71(8) . . . yes Cl Rh C33 154.54(8) . . . yes Cl Rh C36 91.99(9) . . . yes Cl Rh C37 91.95(7) . . . yes C1 Rh C32 92.05(10) . . . yes C1 Rh C33 90.17(11) . . . yes C1 Rh C36 164.05(10) . . . yes C1 Rh C37 160.03(9) . . . yes C32 Rh C33 38.69(11) . . . yes C32 Rh C36 90.08(11) . . . yes C32 Rh C37 82.10(10) . . . yes C33 Rh C36 81.65(12) . . . yes C33 Rh C37 96.85(11) . . . yes C36 Rh C37 35.77(10) . . . yes C1 N1 C2 112.59(18) . . . yes C1 N1 C4 123.95(18) . . . yes C2 N1 C4 123.29(18) . . . yes C1 N2 C3 112.23(17) . . . yes C1 N2 C12 125.90(18) . . . yes C3 N2 C12 120.16(18) . . . yes Rh C1 N1 126.15(16) . . . yes Rh C1 N2 130.29(16) . . . yes N1 C1 N2 103.55(18) . . . yes N1 C2 C3 105.77(18) . . . yes N1 C2 C7 117.5(2) . . . yes C3 C2 C7 136.8(2) . . . no N2 C3 C2 105.81(19) . . . yes N2 C3 C15 117.86(18) . . . yes C2 C3 C15 136.3(2) . . . no N1 C4 C5 106.2(2) . . . yes N1 C4 C20 112.2(2) . . . yes C5 C4 C20 115.60(19) . . . no C4 C5 C6 111.0(2) . . . no C5 C6 C7 119.1(2) . . . no C5 C6 C11 121.6(2) . . . no C7 C6 C11 119.3(2) . . . no C2 C7 C6 116.7(2) . . . no C2 C7 C8 123.2(2) . . . no C6 C7 C8 120.0(2) . . . no C7 C8 C9 118.9(2) . . . no C8 C9 C10 121.1(3) . . . no C9 C10 C11 120.2(2) . . . no C6 C11 C10 120.4(2) . . . no N2 C12 C13 105.87(18) . . . yes N2 C12 C26 109.82(19) . . . yes C13 C12 C26 114.7(2) . . . no C12 C13 C14 110.1(2) . . . no C13 C14 C15 118.7(2) . . . no C13 C14 C19 121.8(2) . . . no C15 C14 C19 119.5(2) . . . no C3 C15 C14 118.4(2) . . . no C3 C15 C16 122.8(2) . . . no C14 C15 C16 118.8(2) . . . no C15 C16 C17 120.5(2) . . . no C16 C17 C18 119.9(3) . . . no C17 C18 C19 120.1(2) . . . no C14 C19 C18 121.0(2) . . . no C4 C20 C21 117.9(2) . . . no C4 C20 C25 124.3(2) . . . no C21 C20 C25 117.8(2) . . . no C20 C21 C22 121.3(2) . . . no C21 C22 C23 119.8(3) . . . no C22 C23 C24 120.1(3) . . . no C23 C24 C25 120.3(3) . . . no C20 C25 C24 120.7(3) . . . no C12 C26 C27 121.1(2) . . . no C12 C26 C31 121.2(2) . . . no C27 C26 C31 117.6(2) . . . no C26 C27 C28 121.1(3) . . . no C27 C28 C29 120.5(3) . . . no C28 C29 C30 119.1(3) . . . no C29 C30 C31 120.9(3) . . . no C26 C31 C30 120.9(2) . . . no Rh C32 C33 70.29(16) . . . yes Rh C32 C39 112.7(2) . . . yes C33 C32 C39 123.4(3) . . . no Rh C33 C32 71.01(15) . . . yes Rh C33 C34 110.7(2) . . . yes C32 C33 C34 125.7(3) . . . no C33 C34 C35 114.0(3) . . . no C34 C35 C36 113.7(3) . . . no Rh C36 C35 110.41(19) . . . yes Rh C36 C37 71.31(15) . . . yes C35 C36 C37 123.6(3) . . . no Rh C37 C36 72.92(16) . . . yes Rh C37 C38 106.73(17) . . . yes C36 C37 C38 127.2(3) . . . no C37 C38 C39 114.4(2) . . . no C32 C39 C38 113.3(3) . . . no N1 C4 H41 107.45 . . . no C5 C4 H41 107.53 . . . no C20 C4 H41 107.50 . . . no C4 C5 H51 109.42 . . . no C4 C5 H52 109.44 . . . no C6 C5 H51 109.51 . . . no C6 C5 H52 109.43 . . . no H51 C5 H52 108.01 . . . no C7 C8 H81 120.55 . . . no C9 C8 H81 120.54 . . . no C8 C9 H91 119.41 . . . no C10 C9 H91 119.51 . . . no C9 C10 H101 119.85 . . . no C11 C10 H101 119.94 . . . no C6 C11 H111 119.86 . . . no C10 C11 H111 119.78 . . . no N2 C12 H121 108.72 . . . no C13 C12 H121 108.76 . . . no C26 C12 H121 108.81 . . . no C12 C13 H131 109.64 . . . no C12 C13 H132 109.64 . . . no C14 C13 H131 109.65 . . . no C14 C13 H132 109.67 . . . no H131 C13 H132 108.10 . . . no C15 C16 H161 119.69 . . . no C17 C16 H161 119.77 . . . no C16 C17 H171 120.07 . . . no C18 C17 H171 120.06 . . . no C17 C18 H181 119.93 . . . no C19 C18 H181 119.98 . . . no C14 C19 H191 119.51 . . . no C18 C19 H191 119.54 . . . no C20 C21 H211 119.36 . . . no C22 C21 H211 119.32 . . . no C21 C22 H221 120.08 . . . no C23 C22 H221 120.13 . . . no C22 C23 H231 119.99 . . . no C24 C23 H231 119.91 . . . no C23 C24 H241 119.79 . . . no C25 C24 H241 119.89 . . . no C20 C25 H251 119.69 . . . no C24 C25 H251 119.63 . . . no C26 C27 H271 119.44 . . . no C28 C27 H271 119.49 . . . no C27 C28 H281 119.77 . . . no C29 C28 H281 119.73 . . . no C28 C29 H291 120.54 . . . no C30 C29 H291 120.41 . . . no C29 C30 H301 119.56 . . . no C31 C30 H301 119.53 . . . no C26 C31 H311 119.52 . . . no C30 C31 H311 119.59 . . . no Rh C32 H321 87.06 . . . no C33 C32 H321 118.28 . . . no C39 C32 H321 118.33 . . . no Rh C33 H331 88.21 . . . no C32 C33 H331 117.19 . . . no C34 C33 H331 117.13 . . . no C33 C34 H341 108.78 . . . no C33 C34 H342 108.79 . . . no C35 C34 H341 108.72 . . . no C35 C34 H342 108.70 . . . no H341 C34 H342 107.67 . . . no C34 C35 H351 108.80 . . . no C34 C35 H352 108.84 . . . no C36 C35 H351 108.82 . . . no C36 C35 H352 108.83 . . . no H351 C35 H352 107.65 . . . no Rh C36 H361 88.32 . . . no C35 C36 H361 118.15 . . . no C37 C36 H361 118.27 . . . no Rh C37 H371 90.42 . . . no C36 C37 H371 116.44 . . . no C38 C37 H371 116.39 . . . no C37 C38 H381 108.65 . . . no C37 C38 H382 108.71 . . . no C39 C38 H381 108.65 . . . no C39 C38 H382 108.61 . . . no H381 C38 H382 107.62 . . . no C32 C39 H391 108.99 . . . no C32 C39 H392 108.93 . . . no C38 C39 H391 108.93 . . . no C38 C39 H392 108.86 . . . no H391 C39 H392 107.73 . . . no # End of Crystallographic Information File