# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #TrackingRef '- Structure 5.cif' _audit_creation_date 08-04-08 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 1 _chemical_name_systematic ? _chemical_melting_point ? #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ? ; _publ_contact_author_name 'Mats Tilset' _publ_contact_author_address ; Centre for Theoretical and Computational Chemistry Department of Chemistry University of Oslo P. O. Box 1033 Blindern N-0315 Oslo, Norway. ; _publ_contact_author_phone '+47 2285 5502' _publ_contact_author_fax '+47 2285 5441' _publ_contact_author_email mats.tilset@kjemi.uio.no _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; # 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 _publ_author_footnote # Author 1 # Author 2 # Author 3 'Marianne Lenes Rosenberg' ; Department of Chemistry University of Oslo P.O.Box 1033 Blindern N-0315 Oslo. Norway # Address for author 1 ; ; ? # Footnote for author 1 ; 'Alexander Krivokapic' ; Department of Chemistry University of Oslo P.O.Box 1033 Blindern N-0315 Oslo. Norway. # Address 2 ; ; ? # Footnote 2 ; 'Mats Tilset' ; Centre for Theoretical and Computational Chemistry Department of Chemistry University of Oslo P. O. Box 1033 Blindern N-0315 Oslo, Norway. # Address 3 ; ; ? # Footnote 3 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 800306' #TrackingRef '- Structure 5.cif' _publ_section_exptl_refinement ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 11.1361(8) _cell_length_b 14.0517(11) _cell_length_c 17.3518(13) _cell_angle_alpha 90 _cell_angle_beta 100.9510(10) _cell_angle_gamma 90 _cell_volume 2665.8(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C30 H33.75 Cl1.25 N3.75 O1.25 Rh1.25 # Dc = 1.59 Fooo = 1216.00 Mu = 9.48 M = 639.82 # Found Formula = C25 H29 Cl3 N3 O1 Rh1 # Dc = 1.49 FOOO = 1216.00 Mu = 9.63 M = 596.79 _chemical_formula_sum 'C25 H29 Cl3 N3 O1 Rh1' _chemical_formula_moiety 'C24 H27 Cl N3 O Rh, C H2 Cl2' _chemical_compound_source ? _chemical_formula_weight 596.79 _cell_measurement_reflns_used 6725 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.81 _cell_measurement_temperature 105 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.963 # Sheldrick geometric approximatio 0.87 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device 'Bruker Kappa Apex2' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time none _diffrn_standards_interval_count none _diffrn_standards_number 0 _diffrn_standards_decay_% none _diffrn_ambient_temperature 105 _diffrn_reflns_number 23563 _reflns_number_total 6344 _diffrn_reflns_av_R_equivalents 0.038 # Number of reflections with Friedels Law is 6344 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6967 _diffrn_reflns_theta_min 1.879 _diffrn_reflns_theta_max 28.817 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.647 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 1.29 _oxford_diffrn_Wilson_scale 137.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.42 _refine_diff_density_max 0.47 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 4788 _refine_ls_number_restraints 0 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0255 _refine_ls_wR_factor_ref 0.0262 _refine_ls_goodness_of_fit_ref 1.1229 _refine_ls_shift/su_max 0.000733 # The values computed from all data _oxford_reflns_number_all 6320 _refine_ls_R_factor_all 0.0359 _refine_ls_wR_factor_all 0.0374 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5031 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_gt 0.0270 # 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 ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.117 0.309E-01 0.106E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Rh1 Rh 0.441131(14) 0.755714(11) 0.478721(8) 0.0131 1.0000 Uani . . . . . . . Cl1 Cl 0.59535(5) 0.77827(4) 0.59097(3) 0.0204 1.0000 Uani . . . . . . . Cl2 Cl 0.14212(8) 0.99370(8) 0.47093(7) 0.0722 1.0000 Uani . . . . . . . Cl3 Cl 0.25883(9) 0.98645(6) 0.33469(5) 0.0562 1.0000 Uani . . . . . . . N1 N 0.31227(15) 0.70260(12) 0.54443(10) 0.0137 1.0000 Uani . . . . . . . N2 N 0.19593(16) 0.70148(13) 0.42339(10) 0.0156 1.0000 Uani . . . . . . . N3 N 0.26651(16) 0.72725(13) 0.31801(10) 0.0179 1.0000 Uani . . . . . . . C1 C 0.30052(18) 0.73059(14) 0.39683(11) 0.0151 1.0000 Uani . . . . . . . C2 C 0.10199(19) 0.67893(16) 0.36012(12) 0.0197 1.0000 Uani . . . . . . . C3 C 0.1463(2) 0.69600(17) 0.29508(13) 0.0217 1.0000 Uani . . . . . . . C4 C 0.3458(2) 0.75085(19) 0.26243(12) 0.0247 1.0000 Uani . . . . . . . C5 C 0.20426(18) 0.68968(14) 0.50400(11) 0.0142 1.0000 Uani . . . . . . . C6 C 0.08859(19) 0.66899(16) 0.53177(12) 0.0180 1.0000 Uani . . . . . . . C7 C -0.0127(2) 0.72615(17) 0.50310(13) 0.0231 1.0000 Uani . . . . . . . C8 C -0.1225(2) 0.71113(19) 0.52815(14) 0.0271 1.0000 Uani . . . . . . . C9 C -0.1311(2) 0.63898(19) 0.58109(15) 0.0289 1.0000 Uani . . . . . . . C10 C -0.0306(2) 0.58330(17) 0.61068(14) 0.0261 1.0000 Uani . . . . . . . C11 C 0.0798(2) 0.59827(16) 0.58646(13) 0.0209 1.0000 Uani . . . . . . . C12 C 0.33619(18) 0.68816(14) 0.62850(11) 0.0134 1.0000 Uani . . . . . . . C13 C 0.29327(18) 0.75322(15) 0.67824(11) 0.0161 1.0000 Uani . . . . . . . C14 C 0.3140(2) 0.73157(16) 0.75839(12) 0.0207 1.0000 Uani . . . . . . . C15 C 0.3776(2) 0.65098(16) 0.78781(12) 0.0212 1.0000 Uani . . . . . . . C16 C 0.4260(2) 0.59107(15) 0.73763(12) 0.0195 1.0000 Uani . . . . . . . C17 C 0.40637(18) 0.60853(14) 0.65702(12) 0.0152 1.0000 Uani . . . . . . . C18 C 0.2316(2) 0.84599(15) 0.64906(14) 0.0215 1.0000 Uani . . . . . . . C19 C 0.3170(2) 0.92973(17) 0.67668(17) 0.0329 1.0000 Uani . . . . . . . C20 C 0.1086(2) 0.85734(18) 0.67500(15) 0.0293 1.0000 Uani . . . . . . . C21 C 0.4566(2) 0.54116(15) 0.60238(12) 0.0180 1.0000 Uani . . . . . . . C22 C 0.5827(2) 0.50243(17) 0.63879(14) 0.0250 1.0000 Uani . . . . . . . C23 C 0.3671(2) 0.45976(17) 0.57543(15) 0.0262 1.0000 Uani . . . . . . . C24 C 0.5394(2) 0.80275(16) 0.41517(13) 0.0217 1.0000 Uani . . . . . . . C25 C 0.2829(3) 0.99518(19) 0.43744(16) 0.0347 1.0000 Uani . . . . . . . O1 O 0.60441(17) 0.83224(15) 0.37733(11) 0.0377 1.0000 Uani . . . . . . . H21 H 0.0241 0.6569 0.3648 0.0239 1.0000 Uiso R . . . . . . H31 H 0.1072 0.6895 0.2426 0.0263 1.0000 Uiso R . . . . . . H42 H 0.3032 0.7332 0.2111 0.0400 1.0000 Uiso R . . . . . . H41 H 0.3633 0.8183 0.2644 0.0402 1.0000 Uiso R . . . . . . H43 H 0.4209 0.7147 0.2764 0.0403 1.0000 Uiso R . . . . . . H71 H -0.0055 0.7759 0.4669 0.0281 1.0000 Uiso R . . . . . . H81 H -0.1910 0.7500 0.5091 0.0335 1.0000 Uiso R . . . . . . H91 H -0.2062 0.6274 0.5968 0.0354 1.0000 Uiso R . . . . . . H101 H -0.0370 0.5350 0.6474 0.0319 1.0000 Uiso R . . . . . . H111 H 0.1485 0.5611 0.6064 0.0259 1.0000 Uiso R . . . . . . H141 H 0.2842 0.7732 0.7932 0.0251 1.0000 Uiso R . . . . . . H151 H 0.3878 0.6364 0.8417 0.0252 1.0000 Uiso R . . . . . . H161 H 0.4717 0.5383 0.7583 0.0244 1.0000 Uiso R . . . . . . H181 H 0.2179 0.8461 0.5912 0.0265 1.0000 Uiso R . . . . . . H191 H 0.2799 0.9883 0.6553 0.0494 1.0000 Uiso R . . . . . . H193 H 0.3339 0.9324 0.7339 0.0498 1.0000 Uiso R . . . . . . H192 H 0.3938 0.9207 0.6590 0.0497 1.0000 Uiso R . . . . . . H201 H 0.0656 0.9115 0.6495 0.0447 1.0000 Uiso R . . . . . . H203 H 0.1228 0.8675 0.7311 0.0446 1.0000 Uiso R . . . . . . H202 H 0.0575 0.8019 0.6627 0.0450 1.0000 Uiso R . . . . . . H211 H 0.4673 0.5791 0.5559 0.0221 1.0000 Uiso R . . . . . . H221 H 0.6163 0.4700 0.5983 0.0380 1.0000 Uiso R . . . . . . H223 H 0.6349 0.5553 0.6598 0.0382 1.0000 Uiso R . . . . . . H222 H 0.5761 0.4574 0.6812 0.0381 1.0000 Uiso R . . . . . . H231 H 0.4016 0.4153 0.5432 0.0393 1.0000 Uiso R . . . . . . H233 H 0.3488 0.4251 0.6202 0.0393 1.0000 Uiso R . . . . . . H232 H 0.2920 0.4830 0.5451 0.0398 1.0000 Uiso R . . . . . . H251 H 0.3227 1.0559 0.4529 0.0402 1.0000 Uiso R . . . . . . H252 H 0.3311 0.9407 0.4602 0.0405 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 Rh1 0.01254(7) 0.01612(7) 0.01074(7) 0.00119(6) 0.00279(5) 0.00020(6) Cl1 0.0161(2) 0.0305(3) 0.0141(2) -0.00081(19) 0.00153(18) -0.00387(19) Cl2 0.0407(5) 0.0917(7) 0.0842(7) 0.0506(6) 0.0120(4) 0.0153(5) Cl3 0.0851(6) 0.0378(4) 0.0364(4) -0.0058(3) -0.0115(4) 0.0020(4) N1 0.0135(8) 0.0157(8) 0.0118(8) 0.0010(6) 0.0026(6) 0.0011(6) N2 0.0135(8) 0.0209(8) 0.0120(8) 0.0020(7) 0.0011(6) 0.0008(7) N3 0.0193(9) 0.0219(9) 0.0123(8) 0.0029(7) 0.0024(7) 0.0010(7) C1 0.0163(9) 0.0162(9) 0.0134(9) 0.0032(7) 0.0039(7) 0.0014(7) C2 0.0151(10) 0.0270(11) 0.0160(10) -0.0008(8) 0.0007(8) -0.0024(8) C3 0.0194(11) 0.0292(11) 0.0151(10) -0.0005(8) 0.0000(8) -0.0013(9) C4 0.0254(11) 0.0363(12) 0.0132(9) 0.0011(9) 0.0060(8) -0.0037(10) C5 0.0160(10) 0.0143(9) 0.0136(9) 0.0010(7) 0.0058(7) 0.0005(7) C6 0.0151(10) 0.0233(10) 0.0163(10) -0.0041(8) 0.0049(8) -0.0019(8) C7 0.0171(10) 0.0320(12) 0.0196(10) -0.0008(9) 0.0016(8) 0.0029(9) C8 0.0168(11) 0.0397(13) 0.0239(11) -0.0073(10) 0.0019(9) 0.0012(9) C9 0.0196(11) 0.0401(14) 0.0297(13) -0.0123(11) 0.0117(10) -0.0087(10) C10 0.0300(13) 0.0245(11) 0.0265(12) -0.0030(9) 0.0124(10) -0.0091(9) C11 0.0210(11) 0.0217(10) 0.0214(11) -0.0020(8) 0.0077(9) -0.0015(8) C12 0.0125(9) 0.0160(9) 0.0124(9) 0.0015(7) 0.0039(7) -0.0018(7) C13 0.0168(9) 0.0159(9) 0.0164(9) -0.0015(8) 0.0049(7) -0.0021(8) C14 0.0240(11) 0.0238(11) 0.0153(10) -0.0047(8) 0.0064(8) -0.0042(8) C15 0.0273(12) 0.0239(11) 0.0117(9) 0.0008(8) 0.0022(8) -0.0062(9) C16 0.0240(11) 0.0178(10) 0.0157(10) 0.0056(8) 0.0015(8) -0.0020(8) C17 0.0156(10) 0.0150(9) 0.0148(9) 0.0002(7) 0.0023(7) -0.0027(7) C18 0.0248(11) 0.0170(10) 0.0234(11) -0.0023(8) 0.0059(9) 0.0038(8) C19 0.0333(14) 0.0191(11) 0.0455(16) -0.0018(10) 0.0055(12) -0.0001(10) C20 0.0260(13) 0.0312(12) 0.0307(13) -0.0090(10) 0.0056(10) 0.0087(10) C21 0.0211(11) 0.0155(9) 0.0174(10) 0.0013(8) 0.0035(8) 0.0032(8) C22 0.0236(12) 0.0239(11) 0.0270(11) 0.0006(9) 0.0036(9) 0.0048(9) C23 0.0270(12) 0.0228(11) 0.0291(12) -0.0093(9) 0.0058(10) 0.0017(9) C24 0.0202(11) 0.0261(11) 0.0175(10) -0.0001(9) 0.0003(8) -0.0034(9) C25 0.0363(14) 0.0289(13) 0.0346(14) 0.0035(11) -0.0041(11) -0.0031(11) O1 0.0308(10) 0.0565(12) 0.0280(9) 0.0053(9) 0.0115(8) -0.0155(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.09369(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rh1 . Cl1 . 2.3606(5) yes Rh1 . N1 . 2.1302(17) yes Rh1 . C1 . 1.937(2) yes Rh1 . C24 . 1.819(2) yes Cl2 . C25 . 1.773(3) yes Cl3 . C25 . 1.756(3) yes N1 . C5 . 1.285(3) yes N1 . C12 . 1.447(2) yes N2 . C1 . 1.393(3) yes N2 . C2 . 1.401(3) yes N2 . C5 . 1.394(2) yes N3 . C1 . 1.349(2) yes N3 . C3 . 1.393(3) yes N3 . C4 . 1.464(3) yes C2 . C3 . 1.336(3) yes C2 . H21 . 0.939 no C3 . H31 . 0.936 no C4 . H42 . 0.959 no C4 . H41 . 0.967 no C4 . H43 . 0.970 no C5 . C6 . 1.487(3) yes C6 . C7 . 1.397(3) yes C6 . C11 . 1.390(3) yes C7 . C8 . 1.389(3) yes C7 . H71 . 0.953 no C8 . C9 . 1.384(4) yes C8 . H81 . 0.945 no C9 . C10 . 1.382(4) yes C9 . H91 . 0.941 no C10 . C11 . 1.389(3) yes C10 . H101 . 0.943 no C11 . H111 . 0.936 no C12 . C13 . 1.402(3) yes C12 . C17 . 1.400(3) yes C13 . C14 . 1.399(3) yes C13 . C18 . 1.515(3) yes C14 . C15 . 1.381(3) yes C14 . H141 . 0.946 no C15 . C16 . 1.391(3) yes C15 . H151 . 0.943 no C16 . C17 . 1.396(3) yes C16 . H161 . 0.931 no C17 . C21 . 1.520(3) yes C18 . C19 . 1.531(3) yes C18 . C20 . 1.529(3) yes C18 . H181 . 0.986 no C19 . H191 . 0.963 no C19 . H193 . 0.975 no C19 . H192 . 0.971 no C20 . H201 . 0.961 no C20 . H203 . 0.966 no C20 . H202 . 0.965 no C21 . C22 . 1.526(3) yes C21 . C23 . 1.531(3) yes C21 . H211 . 0.993 no C22 . H221 . 0.970 no C22 . H223 . 0.971 no C22 . H222 . 0.984 no C23 . H231 . 0.966 no C23 . H233 . 0.972 no C23 . H232 . 0.957 no C24 . O1 . 1.143(3) yes C25 . H251 . 0.975 no C25 . H252 . 0.975 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 Cl1 . Rh1 . N1 . 93.67(5) yes Cl1 . Rh1 . C1 . 171.88(6) yes N1 . Rh1 . C1 . 78.22(7) yes Cl1 . Rh1 . C24 . 91.38(7) yes N1 . Rh1 . C24 . 174.74(8) yes C1 . Rh1 . C24 . 96.74(9) yes Rh1 . N1 . C5 . 114.40(13) yes Rh1 . N1 . C12 . 125.11(12) yes C5 . N1 . C12 . 120.31(17) yes C1 . N2 . C2 . 110.73(17) yes C1 . N2 . C5 . 117.80(17) yes C2 . N2 . C5 . 131.05(18) yes C1 . N3 . C3 . 111.71(17) yes C1 . N3 . C4 . 124.88(18) yes C3 . N3 . C4 . 123.40(18) yes N2 . C1 . N3 . 103.52(17) yes N2 . C1 . Rh1 . 114.91(14) yes N3 . C1 . Rh1 . 141.49(15) yes N2 . C2 . C3 . 106.30(19) yes N2 . C2 . H21 . 124.8 no C3 . C2 . H21 . 128.9 no N3 . C3 . C2 . 107.72(19) yes N3 . C3 . H31 . 123.6 no C2 . C3 . H31 . 128.7 no N3 . C4 . H42 . 107.5 no N3 . C4 . H41 . 109.9 no H42 . C4 . H41 . 110.3 no N3 . C4 . H43 . 108.5 no H42 . C4 . H43 . 110.3 no H41 . C4 . H43 . 110.2 no N2 . C5 . N1 . 114.08(17) yes N2 . C5 . C6 . 116.85(17) yes N1 . C5 . C6 . 128.99(18) yes C5 . C6 . C7 . 117.57(19) yes C5 . C6 . C11 . 122.57(19) yes C7 . C6 . C11 . 119.8(2) yes C6 . C7 . C8 . 120.0(2) yes C6 . C7 . H71 . 119.5 no C8 . C7 . H71 . 120.5 no C7 . C8 . C9 . 119.7(2) yes C7 . C8 . H81 . 120.2 no C9 . C8 . H81 . 120.1 no C8 . C9 . C10 . 120.5(2) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 119.7 no C9 . C10 . C11 . 120.2(2) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.9 no C6 . C11 . C10 . 119.7(2) yes C6 . C11 . H111 . 119.6 no C10 . C11 . H111 . 120.7 no N1 . C12 . C13 . 120.69(17) yes N1 . C12 . C17 . 116.87(17) yes C13 . C12 . C17 . 122.42(18) yes C12 . C13 . C14 . 117.31(19) yes C12 . C13 . C18 . 122.77(18) yes C14 . C13 . C18 . 119.86(19) yes C13 . C14 . C15 . 121.5(2) yes C13 . C14 . H141 . 119.3 no C15 . C14 . H141 . 119.3 no C14 . C15 . C16 . 119.81(19) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 120.0 no C15 . C16 . C17 . 121.0(2) yes C15 . C16 . H161 . 119.2 no C17 . C16 . H161 . 119.8 no C12 . C17 . C16 . 117.73(19) yes C12 . C17 . C21 . 121.61(18) yes C16 . C17 . C21 . 120.63(19) yes C13 . C18 . C19 . 109.96(19) yes C13 . C18 . C20 . 111.47(19) yes C19 . C18 . C20 . 111.42(19) yes C13 . C18 . H181 . 108.3 no C19 . C18 . H181 . 106.5 no C20 . C18 . H181 . 109.0 no C18 . C19 . H191 . 109.9 no C18 . C19 . H193 . 109.7 no H191 . C19 . H193 . 110.2 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.2 no H193 . C19 . H192 . 108.4 no C18 . C20 . H201 . 110.0 no C18 . C20 . H203 . 109.1 no H201 . C20 . H203 . 108.6 no C18 . C20 . H202 . 112.0 no H201 . C20 . H202 . 108.4 no H203 . C20 . H202 . 108.5 no C17 . C21 . C22 . 112.49(18) yes C17 . C21 . C23 . 111.13(18) yes C22 . C21 . C23 . 110.76(18) yes C17 . C21 . H211 . 106.7 no C22 . C21 . H211 . 106.6 no C23 . C21 . H211 . 108.9 no C21 . C22 . H221 . 108.6 no C21 . C22 . H223 . 108.7 no H221 . C22 . H223 . 110.2 no C21 . C22 . H222 . 110.2 no H221 . C22 . H222 . 109.6 no H223 . C22 . H222 . 109.6 no C21 . C23 . H231 . 110.7 no C21 . C23 . H233 . 110.7 no H231 . C23 . H233 . 107.8 no C21 . C23 . H232 . 111.3 no H231 . C23 . H232 . 107.7 no H233 . C23 . H232 . 108.5 no Rh1 . C24 . O1 . 177.7(2) yes Cl2 . C25 . Cl3 . 110.97(15) yes Cl2 . C25 . H251 . 107.6 no Cl3 . C25 . H251 . 108.4 no Cl2 . C25 . H252 . 108.1 no Cl3 . C25 . H252 . 108.8 no H251 . C25 . H252 . 112.9 no # Attachment '- Structure 7.cif' data_nsg_el_27 _database_code_depnum_ccdc_archive 'CCDC 800307' #TrackingRef '- Structure 7.cif' # start Validation Reply Form _vrf_PLAT071_nsg_el_27 ; PROBLEM: Uninterpretable Atom Label on Input ............ Cl RESPONSE: This must be a checking error, the atom label Cl01 is used througout for the chlorine atom. ; _vrf_PLAT230_nsg_el_27 ; PROBLEM: Hirshfeld Test Diff for O009 -- C008 .. 5.17 su RESPONSE: This is due to thermal montion in the carbonyl ligand. ; _vrf_PLAT232_nsg_el_27 ; PROBLEM: Hirshfeld Test Diff (M-X) Rh01 -- C008 .. 9.02 su RESPONSE: This is due to thermal montion in the carbonyl ligand. ; # end Validation Reply Form _audit_update_record ; 2009-10-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H25 Cl N3 O Rh' _chemical_formula_sum 'C23 H25 Cl N3 O Rh' _chemical_formula_weight 497.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 19.6410(7) _cell_length_b 47.2800(14) _cell_length_c 9.725(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9031(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_pressure 101(1) _cell_measurement_reflns_used 5446 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 28.6 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8331 _exptl_absorpt_correction_T_max 0.9478 _exptl_absorpt_process_details 'SADABS (Bruker,2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 101(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD' _diffrn_measurement_method 'Sets of exposures each taken over 0.5\% \w rotation' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19450 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -63 _diffrn_reflns_limit_k_max 63 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.62 _reflns_number_total 5446 _reflns_number_gt 5106 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT-plus (Bruker, 2007)' _computing_data_reduction 'SAINT-plus (Bruker, 2007)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0288P)^2^+1.0369P] 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 none _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 0.014(19) _refine_ls_number_reflns 5446 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Rh01 Rh 0.318440(8) 0.193935(3) 0.865675(17) 0.03553(5) Uani 1 1 d . . . Cl01 Cl 0.32654(3) 0.183271(19) 0.63015(7) 0.05857(16) Uani 1 1 d . . . N003 N 0.23741(9) 0.18472(4) 1.09865(19) 0.0414(4) Uani 1 1 d . . . N004 N 0.32198(10) 0.20748(4) 1.1867(2) 0.0424(4) Uani 1 1 d . . . N005 N 0.21607(8) 0.18003(3) 0.8721(2) 0.0361(3) Uani 1 1 d . . . C001 C 0.19317(12) 0.17634(5) 0.9938(3) 0.0383(5) Uani 1 1 d . . . C007 C 0.15197(12) 0.19688(5) 0.6767(2) 0.0418(5) Uani 1 1 d . . . C008 C 0.40656(12) 0.20478(5) 0.8585(3) 0.0523(5) Uani 1 1 d . . . O009 O 0.46230(10) 0.21135(6) 0.8424(3) 0.0902(8) Uani 1 1 d . . . C010 C 0.16194(11) 0.14597(5) 0.7139(3) 0.0448(5) Uani 1 1 d . . . C011 C 0.27665(14) 0.20035(6) 1.2930(3) 0.0541(6) Uani 1 1 d . . . H011 H 0.2825 0.2046 1.3857 0.065 Uiso 1 1 calc R . . C012 C 0.06672(12) 0.17835(6) 0.9963(3) 0.0501(6) Uani 1 1 d . . . H012 H 0.0688 0.1941 0.9393 0.060 Uiso 1 1 calc R . . C013 C 0.38542(13) 0.22430(5) 1.2107(3) 0.0474(5) Uani 1 1 d . . . C014 C 0.12581(12) 0.16485(5) 1.0355(2) 0.0405(5) Uani 1 1 d . . . C015 C 0.17450(11) 0.17381(5) 0.7533(3) 0.0366(5) Uani 1 1 d . . . C016 C 0.12206(14) 0.14100(6) 1.1181(4) 0.0599(7) Uani 1 1 d . . . H016 H 0.1616 0.1317 1.1451 0.072 Uiso 1 1 calc R . . C017 C 0.29855(13) 0.19766(5) 1.0643(2) 0.0379(5) Uani 1 1 d . . . C018 C 0.00082(16) 0.14479(8) 1.1209(4) 0.0774(9) Uani 1 1 d . . . H018 H -0.0415 0.1380 1.1482 0.093 Uiso 1 1 calc R . . C019 C 0.10041(13) 0.16394(7) 0.5192(3) 0.0602(8) Uani 1 1 d . . . H019 H 0.0746 0.1606 0.4408 0.072 Uiso 1 1 calc R . . C020 C 0.11430(14) 0.19126(6) 0.5577(3) 0.0548(7) Uani 1 1 d . . . H020 H 0.0985 0.2062 0.5041 0.066 Uiso 1 1 calc R . . C021 C 0.00459(14) 0.16855(8) 1.0414(3) 0.0700(8) Uani 1 1 d . . . H021 H -0.0350 0.1782 1.0176 0.084 Uiso 1 1 calc R . . C022 C 0.12380(13) 0.14199(6) 0.5936(3) 0.0551(7) Uani 1 1 d . . . H022 H 0.1144 0.1237 0.5645 0.066 Uiso 1 1 calc R . . C023 C 0.22450(14) 0.18667(6) 1.2394(3) 0.0533(6) Uani 1 1 d . . . H023 H 0.1867 0.1797 1.2860 0.064 Uiso 1 1 calc R . . C024 C 0.38585(16) 0.24951(5) 1.1128(4) 0.0694(7) Uani 1 1 d . . . H02A H 0.3465 0.2610 1.1296 0.104 Uiso 1 1 calc R . . H02B H 0.3850 0.2429 1.0195 0.104 Uiso 1 1 calc R . . H02C H 0.4263 0.2605 1.1276 0.104 Uiso 1 1 calc R . . C025 C 0.44617(15) 0.20477(7) 1.1922(3) 0.0665(8) Uani 1 1 d . . . H02D H 0.4432 0.1894 1.2566 0.100 Uiso 1 1 calc R . . H02E H 0.4874 0.2151 1.2081 0.100 Uiso 1 1 calc R . . H02F H 0.4463 0.1974 1.1002 0.100 Uiso 1 1 calc R . . C026 C 0.05855(19) 0.13093(7) 1.1606(3) 0.0767(10) Uani 1 1 d . . . H026 H 0.0556 0.1149 1.2157 0.092 Uiso 1 1 calc R . . C027 C 0.38600(16) 0.23570(6) 1.3564(3) 0.0716(8) Uani 1 1 d . . . H02G H 0.3861 0.2202 1.4202 0.107 Uiso 1 1 calc R . . H02H H 0.3462 0.2471 1.3712 0.107 Uiso 1 1 calc R . . H02I H 0.4260 0.2470 1.3700 0.107 Uiso 1 1 calc R . . C028 C 0.18845(15) 0.12103(6) 0.7937(4) 0.0724(9) Uani 1 1 d . . . H02J H 0.1739 0.1038 0.7502 0.109 Uiso 1 1 calc R . . H02K H 0.1710 0.1217 0.8859 0.109 Uiso 1 1 calc R . . H02L H 0.2373 0.1217 0.7960 0.109 Uiso 1 1 calc R . . C029 C 0.16648(16) 0.22645(6) 0.7187(3) 0.0639(7) Uani 1 1 d . . . H02M H 0.1464 0.2392 0.6536 0.096 Uiso 1 1 calc R . . H02N H 0.2148 0.2294 0.7214 0.096 Uiso 1 1 calc R . . H02O H 0.1476 0.2299 0.8082 0.096 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 Rh01 0.03366(7) 0.04243(8) 0.03050(7) 0.00038(7) -0.00133(7) -0.00433(6) Cl01 0.0471(3) 0.0958(5) 0.0328(3) -0.0078(3) 0.0042(3) -0.0100(3) N003 0.0404(9) 0.0554(10) 0.0284(10) 0.0038(8) -0.0001(8) -0.0041(8) N004 0.0431(11) 0.0500(11) 0.0340(10) 0.0009(8) -0.0038(8) -0.0019(9) N005 0.0338(8) 0.0412(8) 0.0332(8) -0.0015(9) -0.0024(9) -0.0027(7) C001 0.0361(11) 0.0414(13) 0.0375(12) 0.0054(9) -0.0032(10) -0.0003(10) C007 0.0352(11) 0.0558(14) 0.0342(11) 0.0030(10) 0.0015(9) -0.0048(10) C008 0.0453(12) 0.0725(15) 0.0390(12) -0.0060(14) -0.0018(12) -0.0072(11) O009 0.0445(10) 0.150(2) 0.0756(17) -0.0140(15) 0.0060(11) -0.0354(12) C010 0.0325(11) 0.0475(12) 0.0543(15) -0.0123(11) 0.0053(10) -0.0026(9) C011 0.0583(16) 0.0767(18) 0.0272(12) 0.0035(11) -0.0020(11) -0.0046(13) C012 0.0440(13) 0.0603(16) 0.0460(14) 0.0076(12) 0.0028(11) -0.0015(11) C013 0.0517(14) 0.0478(12) 0.0426(13) -0.0068(10) -0.0094(11) -0.0083(10) C014 0.0382(11) 0.0508(13) 0.0324(11) 0.0042(9) 0.0000(9) -0.0056(10) C015 0.0295(10) 0.0460(13) 0.0342(11) -0.0045(9) 0.0022(9) -0.0014(8) C016 0.0616(15) 0.0605(15) 0.0577(16) 0.0184(17) -0.0044(18) -0.0094(12) C017 0.0375(11) 0.0425(12) 0.0338(11) 0.0027(9) -0.0044(9) -0.0002(9) C018 0.0602(16) 0.125(3) 0.0473(15) 0.011(2) 0.0066(17) -0.0401(17) C019 0.0425(13) 0.102(2) 0.0360(13) -0.0131(14) 0.0002(11) -0.0189(14) C020 0.0443(14) 0.085(2) 0.0356(13) 0.0108(12) -0.0014(10) -0.0085(13) C021 0.0404(14) 0.112(3) 0.0579(17) 0.0088(17) 0.0064(13) -0.0050(15) C022 0.0414(12) 0.0672(16) 0.0567(18) -0.0298(14) 0.0069(13) -0.0137(11) C023 0.0521(15) 0.0754(18) 0.0323(12) 0.0098(11) 0.0002(11) -0.0097(13) C024 0.091(2) 0.0529(14) 0.0645(17) -0.0054(17) -0.002(2) -0.0155(13) C025 0.0522(16) 0.082(2) 0.0652(19) -0.0083(16) -0.0179(14) -0.0003(15) C026 0.100(3) 0.074(2) 0.0559(18) 0.0207(14) 0.0010(16) -0.0381(18) C027 0.085(2) 0.0767(18) 0.0530(15) -0.0160(16) -0.0085(17) -0.0235(15) C028 0.0663(18) 0.0478(16) 0.103(2) -0.0098(15) -0.0040(17) 0.0121(13) C029 0.0782(19) 0.0476(14) 0.0658(19) 0.0131(13) -0.0092(15) -0.0020(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Rh01 C008 1.806(2) . ? Rh01 C017 1.979(2) . ? Rh01 N005 2.1164(16) . ? Rh01 Cl01 2.3507(10) . ? N003 C017 1.389(3) . ? N003 C023 1.395(3) . ? N003 C001 1.397(3) . ? N004 C017 1.358(3) . ? N004 C011 1.405(3) . ? N004 C013 1.497(3) . ? N005 C001 1.278(3) . ? N005 C015 1.445(3) . ? C001 C014 1.487(3) . ? C007 C015 1.393(3) . ? C007 C020 1.399(3) . ? C007 C029 1.484(4) . ? C008 O009 1.149(3) . ? C010 C015 1.393(3) . ? C010 C022 1.401(4) . ? C010 C028 1.505(4) . ? C011 C023 1.319(4) . ? C011 H011 0.9300 . ? C012 C021 1.377(4) . ? C012 C014 1.378(3) . ? C012 H012 0.9300 . ? C013 C027 1.516(4) . ? C013 C025 1.520(4) . ? C013 C024 1.525(4) . ? C014 C016 1.386(3) . ? C016 C026 1.398(4) . ? C016 H016 0.9300 . ? C018 C026 1.366(5) . ? C018 C021 1.366(5) . ? C018 H018 0.9300 . ? C019 C022 1.346(4) . ? C019 C020 1.372(4) . ? C019 H019 0.9300 . ? C020 H020 0.9300 . ? C021 H021 0.9300 . ? C022 H022 0.9300 . ? C023 H023 0.9300 . ? C024 H02A 0.9600 . ? C024 H02B 0.9600 . ? C024 H02C 0.9600 . ? C025 H02D 0.9600 . ? C025 H02E 0.9600 . ? C025 H02F 0.9600 . ? C026 H026 0.9300 . ? C027 H02G 0.9600 . ? C027 H02H 0.9600 . ? C027 H02I 0.9600 . ? C028 H02J 0.9600 . ? C028 H02K 0.9600 . ? C028 H02L 0.9600 . ? C029 H02M 0.9600 . ? C029 H02N 0.9600 . ? C029 H02O 0.9600 . ? 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 C008 Rh01 C017 101.62(12) . . ? C008 Rh01 N005 178.32(10) . . ? C017 Rh01 N005 79.13(9) . . ? C008 Rh01 Cl01 87.63(10) . . ? C017 Rh01 Cl01 169.65(7) . . ? N005 Rh01 Cl01 91.50(6) . . ? C017 N003 C023 111.34(19) . . ? C017 N003 C001 119.17(19) . . ? C023 N003 C001 128.5(2) . . ? C017 N004 C011 110.38(19) . . ? C017 N004 C013 126.90(19) . . ? C011 N004 C013 122.7(2) . . ? C001 N005 C015 120.93(19) . . ? C001 N005 Rh01 113.81(16) . . ? C015 N005 Rh01 125.22(15) . . ? N005 C001 N003 114.7(2) . . ? N005 C001 C014 128.0(2) . . ? N003 C001 C014 117.3(2) . . ? C015 C007 C020 117.5(2) . . ? C015 C007 C029 122.0(2) . . ? C020 C007 C029 120.6(2) . . ? O009 C008 Rh01 174.3(3) . . ? C015 C010 C022 116.8(2) . . ? C015 C010 C028 122.5(2) . . ? C022 C010 C028 120.7(2) . . ? C023 C011 N004 108.6(2) . . ? C023 C011 H011 125.7 . . ? N004 C011 H011 125.7 . . ? C021 C012 C014 120.2(3) . . ? C021 C012 H012 119.9 . . ? C014 C012 H012 119.9 . . ? N004 C013 C027 109.9(2) . . ? N004 C013 C025 108.2(2) . . ? C027 C013 C025 108.7(2) . . ? N004 C013 C024 108.8(2) . . ? C027 C013 C024 107.8(2) . . ? C025 C013 C024 113.4(2) . . ? C012 C014 C016 119.5(2) . . ? C012 C014 C001 120.3(2) . . ? C016 C014 C001 120.2(2) . . ? C010 C015 C007 122.4(2) . . ? C010 C015 N005 120.8(2) . . ? C007 C015 N005 116.6(2) . . ? C014 C016 C026 119.7(3) . . ? C014 C016 H016 120.1 . . ? C026 C016 H016 120.1 . . ? N004 C017 N003 103.47(19) . . ? N004 C017 Rh01 145.01(18) . . ? N003 C017 Rh01 111.48(16) . . ? C026 C018 C021 120.7(3) . . ? C026 C018 H018 119.7 . . ? C021 C018 H018 119.7 . . ? C022 C019 C020 120.7(3) . . ? C022 C019 H019 119.6 . . ? C020 C019 H019 119.6 . . ? C019 C020 C007 120.6(3) . . ? C019 C020 H020 119.7 . . ? C007 C020 H020 119.7 . . ? C018 C021 C012 120.3(3) . . ? C018 C021 H021 119.8 . . ? C012 C021 H021 119.8 . . ? C019 C022 C010 121.8(2) . . ? C019 C022 H022 119.1 . . ? C010 C022 H022 119.1 . . ? C011 C023 N003 106.2(2) . . ? C011 C023 H023 126.9 . . ? N003 C023 H023 126.9 . . ? C013 C024 H02A 109.5 . . ? C013 C024 H02B 109.5 . . ? H02A C024 H02B 109.5 . . ? C013 C024 H02C 109.5 . . ? H02A C024 H02C 109.5 . . ? H02B C024 H02C 109.5 . . ? C013 C025 H02D 109.5 . . ? C013 C025 H02E 109.5 . . ? H02D C025 H02E 109.5 . . ? C013 C025 H02F 109.5 . . ? H02D C025 H02F 109.5 . . ? H02E C025 H02F 109.5 . . ? C018 C026 C016 119.6(3) . . ? C018 C026 H026 120.2 . . ? C016 C026 H026 120.2 . . ? C013 C027 H02G 109.5 . . ? C013 C027 H02H 109.5 . . ? H02G C027 H02H 109.5 . . ? C013 C027 H02I 109.5 . . ? H02G C027 H02I 109.5 . . ? H02H C027 H02I 109.5 . . ? C010 C028 H02J 109.5 . . ? C010 C028 H02K 109.5 . . ? H02J C028 H02K 109.5 . . ? C010 C028 H02L 109.5 . . ? H02J C028 H02L 109.5 . . ? H02K C028 H02L 109.5 . . ? C007 C029 H02M 109.5 . . ? C007 C029 H02N 109.5 . . ? H02M C029 H02N 109.5 . . ? C007 C029 H02O 109.5 . . ? H02M C029 H02O 109.5 . . ? H02N C029 H02O 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 C017 Rh01 N005 C001 -9.81(17) . . . . ? Cl01 Rh01 N005 C001 165.74(16) . . . . ? C017 Rh01 N005 C015 172.68(18) . . . . ? Cl01 Rh01 N005 C015 -11.76(17) . . . . ? C015 N005 C001 N003 -176.5(2) . . . . ? Rh01 N005 C001 N003 5.8(3) . . . . ? C015 N005 C001 C014 2.4(3) . . . . ? Rh01 N005 C001 C014 -175.2(2) . . . . ? C017 N003 C001 N005 4.2(3) . . . . ? C023 N003 C001 N005 171.4(2) . . . . ? C017 N003 C001 C014 -174.9(2) . . . . ? C023 N003 C001 C014 -7.6(4) . . . . ? C017 N004 C011 C023 -1.1(3) . . . . ? C013 N004 C011 C023 177.3(2) . . . . ? C017 N004 C013 C027 169.3(2) . . . . ? C011 N004 C013 C027 -8.8(3) . . . . ? C017 N004 C013 C025 -72.2(3) . . . . ? C011 N004 C013 C025 109.8(3) . . . . ? C017 N004 C013 C024 51.4(3) . . . . ? C011 N004 C013 C024 -126.7(3) . . . . ? C021 C012 C014 C016 1.4(4) . . . . ? C021 C012 C014 C001 -176.4(3) . . . . ? N005 C001 C014 C012 -60.6(4) . . . . ? N003 C001 C014 C012 118.3(3) . . . . ? N005 C001 C014 C016 121.6(3) . . . . ? N003 C001 C014 C016 -59.5(3) . . . . ? C022 C010 C015 C007 -1.4(3) . . . . ? C028 C010 C015 C007 177.7(2) . . . . ? C022 C010 C015 N005 -177.0(2) . . . . ? C028 C010 C015 N005 2.0(4) . . . . ? C020 C007 C015 C010 1.3(3) . . . . ? C029 C007 C015 C010 -179.1(2) . . . . ? C020 C007 C015 N005 177.1(2) . . . . ? C029 C007 C015 N005 -3.3(3) . . . . ? C001 N005 C015 C010 -74.3(3) . . . . ? Rh01 N005 C015 C010 103.0(2) . . . . ? C001 N005 C015 C007 109.8(2) . . . . ? Rh01 N005 C015 C007 -72.8(2) . . . . ? C012 C014 C016 C026 0.0(4) . . . . ? C001 C014 C016 C026 177.8(3) . . . . ? C011 N004 C017 N003 0.7(3) . . . . ? C013 N004 C017 N003 -177.5(2) . . . . ? C011 N004 C017 Rh01 -176.7(3) . . . . ? C013 N004 C017 Rh01 5.0(5) . . . . ? C023 N003 C017 N004 -0.1(3) . . . . ? C001 N003 C017 N004 169.1(2) . . . . ? C023 N003 C017 Rh01 178.28(17) . . . . ? C001 N003 C017 Rh01 -12.4(3) . . . . ? C008 Rh01 C017 N004 10.0(3) . . . . ? N005 Rh01 C017 N004 -171.5(3) . . . . ? Cl01 Rh01 C017 N004 163.0(2) . . . . ? C008 Rh01 C017 N003 -167.30(17) . . . . ? N005 Rh01 C017 N003 11.16(15) . . . . ? Cl01 Rh01 C017 N003 -14.4(6) . . . . ? C022 C019 C020 C007 -1.3(4) . . . . ? C015 C007 C020 C019 0.1(4) . . . . ? C029 C007 C020 C019 -179.5(3) . . . . ? C026 C018 C021 C012 2.2(6) . . . . ? C014 C012 C021 C018 -2.5(5) . . . . ? C020 C019 C022 C010 1.2(4) . . . . ? C015 C010 C022 C019 0.1(4) . . . . ? C028 C010 C022 C019 -178.9(3) . . . . ? N004 C011 C023 N003 0.9(3) . . . . ? C017 N003 C023 C011 -0.5(3) . . . . ? C001 N003 C023 C011 -168.5(2) . . . . ? C021 C018 C026 C016 -0.7(6) . . . . ? C014 C016 C026 C018 -0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.290 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.055