# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Yun Wai Chan' 'Kin Shing Chan' _publ_contact_author_name 'Yun Wai Chan' _publ_contact_author_email yunwaichan@yahoo.com.hk data_YWC981 _database_code_depnum_ccdc_archive 'CCDC 797520' #TrackingRef '- Rh(ttp)(cycloheptatrienyl).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H42 N4 Rh' _chemical_formula_weight 861.84 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 15.4864(5) _cell_length_b 18.7106(6) _cell_length_c 16.4209(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.7630(10) _cell_angle_gamma 90.00 _cell_volume 4555.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 379 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6264 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42092 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8244 _reflns_number_gt 7013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.0627P)^2^+1.9217P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8244 _refine_ls_number_parameters 550 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.002 _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 Rh1 Rh 0.597993(12) 0.607474(10) 0.438487(12) 0.03769(9) Uani 1 1 d . . . N1 N 0.52898(14) 0.58681(12) 0.31626(13) 0.0420(5) Uani 1 1 d . . . N2 N 0.71456(15) 0.60415(11) 0.40748(14) 0.0423(5) Uani 1 1 d . . . N3 N 0.66683(14) 0.62702(12) 0.56094(13) 0.0414(5) Uani 1 1 d . . . N4 N 0.48404(14) 0.59343(12) 0.47246(13) 0.0417(5) Uani 1 1 d . . . C1 C 0.43680(17) 0.58466(14) 0.28363(16) 0.0418(5) Uani 1 1 d . . . C2 C 0.41328(19) 0.58592(16) 0.19219(17) 0.0507(6) Uani 1 1 d . . . H2A H 0.3552 0.5864 0.1550 0.061 Uiso 1 1 calc R . . C3 C 0.49108(19) 0.58629(17) 0.17038(18) 0.0522(7) Uani 1 1 d . . . H3A H 0.4964 0.5865 0.1154 0.063 Uiso 1 1 calc R . . C4 C 0.56385(18) 0.58628(15) 0.24773(16) 0.0456(6) Uani 1 1 d . . . C5 C 0.65504(18) 0.58682(15) 0.25269(17) 0.0465(6) Uani 1 1 d . . . C6 C 0.72425(18) 0.59355(15) 0.32781(18) 0.0455(6) Uani 1 1 d . . . C7 C 0.81948(19) 0.59105(18) 0.3344(2) 0.0557(7) Uani 1 1 d . . . H7A H 0.8444 0.5832 0.2901 0.067 Uiso 1 1 calc R . . C8 C 0.8652(2) 0.60206(17) 0.4164(2) 0.0555(7) Uani 1 1 d . . . H8A H 0.9276 0.6036 0.4388 0.067 Uiso 1 1 calc R . . C9 C 0.80054(18) 0.61099(14) 0.46307(18) 0.0445(6) Uani 1 1 d . . . C10 C 0.82137(17) 0.62978(14) 0.54881(17) 0.0435(6) Uani 1 1 d . . . C11 C 0.75734(16) 0.64117(14) 0.59264(16) 0.0418(5) Uani 1 1 d . . . C12 C 0.77601(18) 0.66680(15) 0.67817(17) 0.0480(6) Uani 1 1 d . . . H12A H 0.8321 0.6803 0.7135 0.058 Uiso 1 1 calc R . . C13 C 0.69778(18) 0.66782(15) 0.69801(17) 0.0471(6) Uani 1 1 d . . . H13A H 0.6896 0.6830 0.7492 0.056 Uiso 1 1 calc R . . C14 C 0.62909(16) 0.64114(14) 0.62583(16) 0.0413(5) Uani 1 1 d . . . C15 C 0.54019(18) 0.62634(15) 0.62358(17) 0.0443(6) Uani 1 1 d . . . C16 C 0.47534(17) 0.59837(14) 0.55318(17) 0.0436(6) Uani 1 1 d . . . C17 C 0.38617(18) 0.57548(18) 0.55174(18) 0.0526(7) Uani 1 1 d . . . H17A H 0.3642 0.5712 0.5986 0.063 Uiso 1 1 calc R . . C18 C 0.34048(18) 0.56147(17) 0.47059(18) 0.0516(7) Uani 1 1 d . . . H18A H 0.2809 0.5462 0.4509 0.062 Uiso 1 1 calc R . . C19 C 0.40024(16) 0.57442(15) 0.41986(17) 0.0440(6) Uani 1 1 d . . . C20 C 0.37588(16) 0.57705(14) 0.33084(16) 0.0423(5) Uani 1 1 d . . . C21 C 0.68092(18) 0.57910(17) 0.17182(17) 0.0488(6) Uani 1 1 d . . . C22 C 0.7249(2) 0.63400(19) 0.1436(2) 0.0617(8) Uani 1 1 d . . . H22A H 0.7364 0.6768 0.1735 0.074 Uiso 1 1 calc R . . C23 C 0.7519(2) 0.6253(2) 0.0706(2) 0.0660(8) Uani 1 1 d . . . H23A H 0.7825 0.6624 0.0533 0.079 Uiso 1 1 calc R . . C24 C 0.7349(2) 0.56406(19) 0.02343(19) 0.0589(8) Uani 1 1 d . . . C25 C 0.6907(2) 0.5099(2) 0.0515(2) 0.0673(9) Uani 1 1 d . . . H25A H 0.6784 0.4675 0.0208 0.081 Uiso 1 1 calc R . . C26 C 0.6641(2) 0.51727(18) 0.1250(2) 0.0612(8) Uani 1 1 d . . . H26A H 0.6344 0.4798 0.1426 0.073 Uiso 1 1 calc R . . C27 C 0.7651(3) 0.5563(3) -0.0558(2) 0.0815(11) Uani 1 1 d . . . H27A H 0.7468 0.5104 -0.0811 0.122 Uiso 1 1 calc R . . H27B H 0.8296 0.5602 -0.0410 0.122 Uiso 1 1 calc R . . H27C H 0.7381 0.5932 -0.0955 0.122 Uiso 1 1 calc R . . C31 C 0.91916(17) 0.63830(15) 0.59653(17) 0.0444(6) Uani 1 1 d . . . C32 C 0.95711(18) 0.70445(16) 0.62139(17) 0.0507(6) Uani 1 1 d . . . H32A H 0.9209 0.7450 0.6108 0.061 Uiso 1 1 calc R . . C33 C 1.0482(2) 0.71099(19) 0.6618(2) 0.0611(8) Uani 1 1 d . . . H33A H 1.0724 0.7561 0.6778 0.073 Uiso 1 1 calc R . . C34 C 1.1037(2) 0.6527(2) 0.6787(2) 0.0682(9) Uani 1 1 d . . . C35 C 1.0655(2) 0.5869(2) 0.6544(3) 0.0788(11) Uani 1 1 d . . . H35A H 1.1020 0.5465 0.6652 0.095 Uiso 1 1 calc R . . C36 C 0.9745(2) 0.57924(19) 0.6145(2) 0.0659(8) Uani 1 1 d . . . H36A H 0.9504 0.5339 0.5997 0.079 Uiso 1 1 calc R . . C37 C 1.2044(2) 0.6603(3) 0.7200(3) 0.1127(17) Uani 1 1 d . . . H37A H 1.2319 0.6139 0.7272 0.169 Uiso 1 1 calc R . . H37B H 1.2148 0.6829 0.7745 0.169 Uiso 1 1 calc R . . H37C H 1.2301 0.6890 0.6844 0.169 Uiso 1 1 calc R . . C41 C 0.51194(17) 0.64178(15) 0.70157(16) 0.0429(6) Uani 1 1 d . . . C42 C 0.45647(19) 0.69928(17) 0.70286(19) 0.0567(7) Uani 1 1 d . . . H42A H 0.4356 0.7275 0.6545 0.068 Uiso 1 1 calc R . . C43 C 0.4313(2) 0.71558(19) 0.7755(2) 0.0628(8) Uani 1 1 d . . . H43A H 0.3946 0.7549 0.7752 0.075 Uiso 1 1 calc R . . C44 C 0.4600(2) 0.67435(18) 0.8476(2) 0.0591(8) Uani 1 1 d . . . C45 C 0.5143(3) 0.61668(18) 0.8458(2) 0.0630(8) Uani 1 1 d . . . H45A H 0.5340 0.5877 0.8935 0.076 Uiso 1 1 calc R . . C46 C 0.5404(2) 0.60101(16) 0.77309(19) 0.0564(7) Uani 1 1 d . . . H46A H 0.5778 0.5621 0.7735 0.068 Uiso 1 1 calc R . . C47 C 0.4317(3) 0.6904(3) 0.9264(3) 0.0916(13) Uani 1 1 d . . . H47A H 0.4577 0.6557 0.9695 0.137 Uiso 1 1 calc R . . H47B H 0.3672 0.6886 0.9128 0.137 Uiso 1 1 calc R . . H47C H 0.4523 0.7373 0.9469 0.137 Uiso 1 1 calc R . . C51 C 0.27722(17) 0.57492(15) 0.28337(17) 0.0442(6) Uani 1 1 d . . . C52 C 0.2345(2) 0.63540(18) 0.2430(2) 0.0663(9) Uani 1 1 d . . . H52A H 0.2674 0.6766 0.2413 0.080 Uiso 1 1 calc R . . C53 C 0.1415(2) 0.6344(2) 0.2047(3) 0.0823(11) Uani 1 1 d . . . H53A H 0.1133 0.6752 0.1772 0.099 Uiso 1 1 calc R . . C54 C 0.0904(2) 0.5742(2) 0.2065(2) 0.0656(8) Uani 1 1 d . . . C55 C 0.1350(2) 0.51444(19) 0.2405(2) 0.0666(8) Uani 1 1 d . . . H55A H 0.1029 0.4721 0.2376 0.080 Uiso 1 1 calc R . . C56 C 0.22706(19) 0.51400(17) 0.2796(2) 0.0591(7) Uani 1 1 d . . . H56A H 0.2552 0.4719 0.3036 0.071 Uiso 1 1 calc R . . C57 C -0.0117(2) 0.5748(3) 0.1690(3) 0.0994(14) Uani 1 1 d . . . H57A H -0.0311 0.6217 0.1479 0.149 Uiso 1 1 calc R . . H57B H -0.0394 0.5620 0.2123 0.149 Uiso 1 1 calc R . . H57C H -0.0288 0.5409 0.1232 0.149 Uiso 1 1 calc R . . C61 C 0.5811(2) 0.71733(18) 0.4113(3) 0.0874(13) Uani 1 1 d D B . C62 C 0.6618(2) 0.76159(19) 0.4382(3) 0.1016(16) Uani 1 1 d D . . H62 H 0.7156 0.7383 0.4649 0.122 Uiso 1 1 calc R A 1 C63 C 0.6666(6) 0.8369(3) 0.4277(7) 0.094(3) Uani 0.50 1 d PD B 1 C63' C 0.6664(6) 0.8168(5) 0.5010(7) 0.125(5) Uani 0.50 1 d PD B 2 C64 C 0.6114(4) 0.8841(3) 0.4664(6) 0.164(3) Uani 1 1 d DU . . H64 H 0.6399 0.9205 0.5029 0.197 Uiso 1 1 calc R B 1 C65 C 0.5153(3) 0.8751(3) 0.4491(4) 0.120(2) Uani 1 1 d D B . H65 H 0.4834 0.9053 0.4749 0.144 Uiso 1 1 calc R . . C66 C 0.4675(3) 0.8192(2) 0.3916(4) 0.125(2) Uani 1 1 d D . . H66A H 0.4184 0.8329 0.3466 0.150 Uiso 1 1 calc R B . C67 C 0.4909(2) 0.74406(19) 0.3996(4) 0.0999(15) Uani 1 1 d D B . H67A H 0.4452 0.7112 0.3971 0.120 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 Rh1 0.02950(12) 0.04330(14) 0.04015(13) -0.00425(8) 0.00983(9) -0.00039(7) N1 0.0349(11) 0.0489(12) 0.0417(11) -0.0006(9) 0.0103(9) -0.0009(9) N2 0.0361(11) 0.0464(12) 0.0452(12) -0.0055(9) 0.0127(9) 0.0003(9) N3 0.0323(10) 0.0485(12) 0.0437(11) -0.0062(9) 0.0114(9) -0.0024(9) N4 0.0347(11) 0.0493(12) 0.0405(11) -0.0021(9) 0.0097(9) -0.0001(9) C1 0.0381(13) 0.0423(13) 0.0429(13) -0.0036(11) 0.0084(11) -0.0010(11) C2 0.0441(15) 0.0577(16) 0.0457(14) 0.0012(13) 0.0056(12) -0.0010(13) C3 0.0488(16) 0.0667(18) 0.0405(14) 0.0020(13) 0.0122(12) -0.0018(14) C4 0.0450(14) 0.0519(15) 0.0405(13) -0.0025(12) 0.0132(11) -0.0012(12) C5 0.0437(14) 0.0508(15) 0.0477(15) -0.0026(12) 0.0178(12) -0.0008(12) C6 0.0409(14) 0.0479(15) 0.0509(15) -0.0059(12) 0.0185(12) 0.0017(11) C7 0.0414(15) 0.074(2) 0.0574(17) -0.0097(15) 0.0228(13) 0.0019(13) C8 0.0361(14) 0.073(2) 0.0596(18) -0.0082(14) 0.0172(13) 0.0041(12) C9 0.0321(13) 0.0497(15) 0.0528(15) -0.0066(11) 0.0137(11) 0.0016(10) C10 0.0348(13) 0.0421(14) 0.0524(15) -0.0017(11) 0.0107(11) 0.0000(11) C11 0.0349(12) 0.0426(14) 0.0456(13) -0.0037(11) 0.0080(10) -0.0011(10) C12 0.0389(13) 0.0546(16) 0.0472(14) -0.0064(12) 0.0069(11) -0.0059(12) C13 0.0449(14) 0.0528(16) 0.0426(14) -0.0088(12) 0.0111(11) -0.0035(12) C14 0.0379(13) 0.0416(14) 0.0443(13) -0.0053(11) 0.0118(10) -0.0002(11) C15 0.0384(13) 0.0515(15) 0.0442(14) -0.0024(11) 0.0140(11) 0.0010(11) C16 0.0340(13) 0.0534(16) 0.0437(14) -0.0042(11) 0.0119(11) -0.0007(11) C17 0.0401(14) 0.0693(19) 0.0526(16) -0.0054(14) 0.0201(12) -0.0069(13) C18 0.0345(13) 0.0698(19) 0.0514(15) -0.0025(14) 0.0137(11) -0.0072(12) C19 0.0331(12) 0.0501(15) 0.0488(14) -0.0031(12) 0.0117(11) -0.0018(11) C20 0.0347(13) 0.0429(14) 0.0462(14) -0.0029(11) 0.0071(11) -0.0022(11) C21 0.0441(14) 0.0602(17) 0.0442(14) -0.0022(13) 0.0163(12) -0.0009(13) C22 0.0659(19) 0.0622(19) 0.0614(18) -0.0054(15) 0.0254(15) -0.0073(16) C23 0.065(2) 0.077(2) 0.0627(19) 0.0090(17) 0.0292(16) -0.0094(17) C24 0.0451(15) 0.084(2) 0.0486(16) -0.0010(15) 0.0156(13) 0.0013(15) C25 0.072(2) 0.078(2) 0.0588(18) -0.0156(16) 0.0290(16) -0.0077(17) C26 0.0670(19) 0.0621(19) 0.0619(18) -0.0070(15) 0.0302(15) -0.0076(15) C27 0.077(2) 0.118(3) 0.058(2) -0.003(2) 0.0326(18) -0.006(2) C31 0.0346(13) 0.0503(15) 0.0482(14) 0.0015(12) 0.0117(11) 0.0014(11) C32 0.0425(14) 0.0554(16) 0.0523(15) 0.0005(13) 0.0105(12) -0.0039(12) C33 0.0476(16) 0.070(2) 0.0631(18) -0.0044(15) 0.0121(14) -0.0177(15) C34 0.0380(15) 0.091(3) 0.070(2) 0.0109(18) 0.0064(14) -0.0053(16) C35 0.0447(18) 0.081(2) 0.104(3) 0.017(2) 0.0098(18) 0.0186(17) C36 0.0493(17) 0.0509(17) 0.092(2) -0.0001(17) 0.0114(16) 0.0018(14) C37 0.0415(19) 0.165(5) 0.115(4) 0.005(3) -0.004(2) -0.007(2) C41 0.0375(13) 0.0477(15) 0.0440(14) -0.0060(11) 0.0123(11) -0.0039(11) C42 0.0492(16) 0.0683(19) 0.0532(16) 0.0022(14) 0.0157(13) 0.0129(14) C43 0.0532(17) 0.071(2) 0.070(2) -0.0133(16) 0.0273(15) 0.0067(15) C44 0.0571(17) 0.070(2) 0.0575(17) -0.0181(15) 0.0281(14) -0.0152(15) C45 0.073(2) 0.070(2) 0.0495(17) 0.0039(14) 0.0241(16) -0.0037(16) C46 0.0646(19) 0.0558(18) 0.0520(17) -0.0010(13) 0.0222(15) 0.0085(14) C47 0.103(3) 0.112(3) 0.078(2) -0.026(2) 0.054(2) -0.013(3) C51 0.0370(13) 0.0486(15) 0.0450(14) -0.0037(12) 0.0087(11) -0.0011(11) C52 0.0515(17) 0.0545(18) 0.084(2) 0.0058(17) 0.0056(16) -0.0029(15) C53 0.053(2) 0.073(2) 0.103(3) 0.007(2) -0.0053(19) 0.0125(18) C54 0.0382(15) 0.085(2) 0.0664(19) -0.0063(18) 0.0044(14) -0.0009(16) C55 0.0463(16) 0.073(2) 0.074(2) -0.0044(17) 0.0071(15) -0.0185(15) C56 0.0447(15) 0.0523(17) 0.0717(19) -0.0007(14) 0.0034(14) -0.0024(13) C57 0.0417(19) 0.137(4) 0.109(3) -0.004(3) 0.005(2) 0.000(2) C61 0.0465(17) 0.0445(18) 0.158(4) 0.012(2) 0.009(2) 0.0041(14) C62 0.0461(19) 0.055(2) 0.194(5) 0.015(3) 0.019(2) -0.0008(16) C63 0.079(5) 0.065(5) 0.147(9) 0.010(5) 0.047(6) -0.010(4) C63' 0.077(6) 0.099(7) 0.170(11) -0.077(8) -0.011(7) 0.007(5) C64 0.127(5) 0.086(4) 0.271(7) -0.047(4) 0.042(5) 0.000(3) C65 0.089(3) 0.075(3) 0.193(6) -0.029(3) 0.033(4) 0.018(2) C66 0.085(3) 0.088(3) 0.159(5) -0.037(3) -0.033(3) 0.040(3) C67 0.0486(19) 0.056(2) 0.187(5) 0.006(3) 0.021(2) 0.0041(16) _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 Rh1 N2 2.013(2) . ? Rh1 N4 2.016(2) . ? Rh1 N3 2.019(2) . ? Rh1 N1 2.021(2) . ? Rh1 C61 2.104(3) . ? N1 C1 1.373(3) . ? N1 C4 1.382(3) . ? N2 C6 1.374(3) . ? N2 C9 1.386(4) . ? N3 C11 1.373(3) . ? N3 C14 1.381(3) . ? N4 C16 1.374(3) . ? N4 C19 1.382(3) . ? C1 C20 1.391(4) . ? C1 C2 1.439(4) . ? C2 C3 1.352(4) . ? C3 C4 1.434(4) . ? C4 C5 1.391(4) . ? C5 C6 1.387(4) . ? C5 C21 1.501(4) . ? C6 C7 1.448(4) . ? C7 C8 1.343(4) . ? C8 C9 1.436(4) . ? C9 C10 1.396(4) . ? C10 C11 1.399(4) . ? C10 C31 1.500(4) . ? C11 C12 1.432(4) . ? C12 C13 1.342(4) . ? C13 C14 1.435(4) . ? C14 C15 1.394(4) . ? C15 C16 1.396(4) . ? C15 C41 1.496(3) . ? C16 C17 1.439(4) . ? C17 C18 1.342(4) . ? C18 C19 1.433(4) . ? C19 C20 1.401(4) . ? C20 C51 1.502(3) . ? C21 C26 1.372(4) . ? C21 C22 1.385(4) . ? C22 C23 1.387(4) . ? C23 C24 1.366(5) . ? C24 C25 1.375(5) . ? C24 C27 1.511(4) . ? C25 C26 1.389(4) . ? C31 C36 1.377(4) . ? C31 C32 1.380(4) . ? C32 C33 1.381(4) . ? C33 C34 1.366(5) . ? C34 C35 1.374(6) . ? C34 C37 1.517(5) . ? C35 C36 1.380(5) . ? C41 C46 1.363(4) . ? C41 C42 1.381(4) . ? C42 C43 1.391(4) . ? C43 C44 1.376(5) . ? C44 C45 1.374(5) . ? C44 C47 1.510(4) . ? C45 C46 1.397(4) . ? C51 C56 1.371(4) . ? C51 C52 1.381(4) . ? C52 C53 1.394(5) . ? C53 C54 1.381(5) . ? C54 C55 1.349(5) . ? C54 C57 1.522(4) . ? C55 C56 1.384(4) . ? C61 C67 1.444(4) . ? C61 C62 1.458(4) . ? C62 C63 1.425(6) . ? C62 C63' 1.447(7) . ? C63 C64 1.492(8) . ? C63' C64 1.533(8) . ? C64 C65 1.442(6) . ? C65 C66 1.459(6) . ? C66 C67 1.449(5) . ? 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 N2 Rh1 N4 170.62(9) . . ? N2 Rh1 N3 90.18(9) . . ? N4 Rh1 N3 90.05(8) . . ? N2 Rh1 N1 89.94(9) . . ? N4 Rh1 N1 89.74(9) . . ? N3 Rh1 N1 179.39(9) . . ? N2 Rh1 C61 92.42(12) . . ? N4 Rh1 C61 96.94(12) . . ? N3 Rh1 C61 91.85(15) . . ? N1 Rh1 C61 88.75(15) . . ? C1 N1 C4 106.8(2) . . ? C1 N1 Rh1 125.87(17) . . ? C4 N1 Rh1 126.26(17) . . ? C6 N2 C9 107.0(2) . . ? C6 N2 Rh1 126.70(18) . . ? C9 N2 Rh1 126.29(18) . . ? C11 N3 C14 106.5(2) . . ? C11 N3 Rh1 126.91(17) . . ? C14 N3 Rh1 125.72(16) . . ? C16 N4 C19 106.5(2) . . ? C16 N4 Rh1 126.56(17) . . ? C19 N4 Rh1 126.86(17) . . ? N1 C1 C20 125.6(2) . . ? N1 C1 C2 109.2(2) . . ? C20 C1 C2 125.1(2) . . ? C3 C2 C1 107.4(2) . . ? C2 C3 C4 107.3(2) . . ? N1 C4 C5 125.5(2) . . ? N1 C4 C3 109.2(2) . . ? C5 C4 C3 125.2(2) . . ? C6 C5 C4 124.3(2) . . ? C6 C5 C21 117.4(2) . . ? C4 C5 C21 118.2(2) . . ? N2 C6 C5 126.3(2) . . ? N2 C6 C7 108.8(2) . . ? C5 C6 C7 125.0(3) . . ? C8 C7 C6 107.6(3) . . ? C7 C8 C9 107.8(3) . . ? N2 C9 C10 125.9(2) . . ? N2 C9 C8 108.8(2) . . ? C10 C9 C8 125.0(3) . . ? C9 C10 C11 124.4(2) . . ? C9 C10 C31 117.3(2) . . ? C11 C10 C31 118.3(2) . . ? N3 C11 C10 125.0(2) . . ? N3 C11 C12 109.4(2) . . ? C10 C11 C12 125.6(2) . . ? C13 C12 C11 107.6(2) . . ? C12 C13 C14 107.5(2) . . ? N3 C14 C15 125.2(2) . . ? N3 C14 C13 109.0(2) . . ? C15 C14 C13 125.6(2) . . ? C14 C15 C16 124.4(2) . . ? C14 C15 C41 118.0(2) . . ? C16 C15 C41 117.6(2) . . ? N4 C16 C15 125.2(2) . . ? N4 C16 C17 108.9(2) . . ? C15 C16 C17 125.6(2) . . ? C18 C17 C16 107.6(2) . . ? C17 C18 C19 107.5(2) . . ? N4 C19 C20 124.4(2) . . ? N4 C19 C18 109.1(2) . . ? C20 C19 C18 126.0(2) . . ? C1 C20 C19 124.3(2) . . ? C1 C20 C51 117.7(2) . . ? C19 C20 C51 117.9(2) . . ? C26 C21 C22 118.0(3) . . ? C26 C21 C5 121.4(3) . . ? C22 C21 C5 120.5(3) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 122.1(3) . . ? C23 C24 C25 117.4(3) . . ? C23 C24 C27 120.9(3) . . ? C25 C24 C27 121.7(3) . . ? C24 C25 C26 121.3(3) . . ? C21 C26 C25 121.0(3) . . ? C36 C31 C32 118.1(3) . . ? C36 C31 C10 119.9(3) . . ? C32 C31 C10 122.0(2) . . ? C31 C32 C33 120.7(3) . . ? C34 C33 C32 121.5(3) . . ? C33 C34 C35 117.6(3) . . ? C33 C34 C37 121.4(4) . . ? C35 C34 C37 121.0(4) . . ? C34 C35 C36 121.8(3) . . ? C31 C36 C35 120.4(3) . . ? C46 C41 C42 118.1(3) . . ? C46 C41 C15 121.9(2) . . ? C42 C41 C15 120.0(2) . . ? C41 C42 C43 120.9(3) . . ? C44 C43 C42 121.0(3) . . ? C45 C44 C43 117.9(3) . . ? C45 C44 C47 120.4(3) . . ? C43 C44 C47 121.7(3) . . ? C44 C45 C46 120.9(3) . . ? C41 C46 C45 121.2(3) . . ? C56 C51 C52 118.2(3) . . ? C56 C51 C20 121.6(3) . . ? C52 C51 C20 120.2(3) . . ? C51 C52 C53 119.7(3) . . ? C54 C53 C52 121.7(3) . . ? C55 C54 C53 117.1(3) . . ? C55 C54 C57 121.4(4) . . ? C53 C54 C57 121.4(4) . . ? C54 C55 C56 122.2(3) . . ? C51 C56 C55 120.7(3) . . ? C67 C61 C62 123.8(3) . . ? C67 C61 Rh1 115.0(2) . . ? C62 C61 Rh1 116.6(2) . . ? C63 C62 C63' 52.1(6) . . ? C63 C62 C61 126.5(5) . . ? C63' C62 C61 118.9(6) . . ? C62 C63 C64 118.5(6) . . ? C62 C63' C64 114.5(6) . . ? C65 C64 C63 122.2(6) . . ? C65 C64 C63' 114.1(6) . . ? C63 C64 C63' 49.3(6) . . ? C64 C65 C66 120.9(5) . . ? C67 C66 C65 124.7(4) . . ? C61 C67 C66 123.8(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.750 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.057 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.171 0.682 0.450 115.9 35.7 2 0.329 0.182 0.050 115.9 36.8 3 0.671 0.818 0.950 115.9 35.2 4 0.829 0.318 0.550 115.9 37.4 _platon_squeeze_details ; ;