# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Mueller, Christian' _publ_contact_author_email c.mueller@tue.nl _publ_section_title ; 2-(2\^a-pyridyl)-4,6-diphenylphosphinine versus 2-(2\^a-pyridyl)-4,6-diphenylpyridine: An evaluation of their coordination chemistry towards Rh(I) ; loop_ _publ_author_name C.Mueller 'A.Campos Carrasco' E.Pidko 'A.M.Masdeu Bulto' M.Lutz ; A.Spek ; D.Vogt # Attachment '- deposit.cif' data_s4321a _database_code_depnum_ccdc_archive 'CCDC 762388' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 N P Rh, B F4, 0.4(C H2 Cl2)' _chemical_formula_sum 'C30.40 H28.80 B Cl0.80 F4 N P Rh' _chemical_formula_weight 657.19 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7987(2) _cell_length_b 10.3575(2) _cell_length_c 14.5382(3) _cell_angle_alpha 84.8750(6) _cell_angle_beta 85.4051(6) _cell_angle_gamma 71.0572(8) _cell_volume 1387.95(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25271 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21889 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.58 _reflns_number_total 6367 _reflns_number_gt 5109 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, denzox, Sadabs' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0385P)^2^+1.3773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6367 _refine_ls_number_parameters 377 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.010 _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 0.32650(2) 0.52986(2) 0.245160(15) 0.02278(8) Uani 1 1 d . . . P1 P 0.48791(8) 0.37211(7) 0.16344(5) 0.02263(17) Uani 1 1 d . . . N1 N 0.2258(3) 0.5693(2) 0.11425(16) 0.0230(5) Uani 1 1 d . . . C1 C 0.6433(3) 0.2320(3) 0.1656(2) 0.0228(6) Uani 1 1 d . . . C2 C 0.6845(3) 0.1511(3) 0.0898(2) 0.0246(6) Uani 1 1 d . . . H2 H 0.7689 0.0736 0.0951 0.030 Uiso 1 1 calc R . . C3 C 0.6149(3) 0.1722(3) 0.0073(2) 0.0229(6) Uani 1 1 d . . . C4 C 0.4893(3) 0.2834(3) -0.0084(2) 0.0224(6) Uani 1 1 d . . . H4 H 0.4482 0.2947 -0.0668 0.027 Uiso 1 1 calc R . . C5 C 0.4215(3) 0.3782(3) 0.0565(2) 0.0218(6) Uani 1 1 d . . . C6 C 0.2847(3) 0.4893(3) 0.0417(2) 0.0217(6) Uani 1 1 d . . . C7 C 0.2147(3) 0.5106(3) -0.0405(2) 0.0254(6) Uani 1 1 d . . . H7 H 0.2580 0.4551 -0.0904 0.031 Uiso 1 1 calc R . . C8 C 0.0835(3) 0.6111(3) -0.0503(2) 0.0269(7) Uani 1 1 d . . . H8 H 0.0353 0.6254 -0.1063 0.032 Uiso 1 1 calc R . . C9 C 0.0234(3) 0.6906(3) 0.0229(2) 0.0275(7) Uani 1 1 d . . . H9 H -0.0674 0.7604 0.0185 0.033 Uiso 1 1 calc R . . C10 C 0.0972(3) 0.6671(3) 0.1028(2) 0.0263(7) Uani 1 1 d . . . H10 H 0.0550 0.7230 0.1526 0.032 Uiso 1 1 calc R . . C11 C 0.7339(3) 0.1990(3) 0.2467(2) 0.0258(6) Uani 1 1 d . . . C12 C 0.7839(3) 0.2980(3) 0.2785(2) 0.0262(7) Uani 1 1 d . . . H12 H 0.7533 0.3888 0.2511 0.031 Uiso 1 1 calc R . . C13 C 0.8774(3) 0.2651(3) 0.3493(2) 0.0331(7) Uani 1 1 d . . . H13 H 0.9122 0.3327 0.3697 0.040 Uiso 1 1 calc R . . C14 C 0.9206(4) 0.1334(4) 0.3908(2) 0.0432(9) Uani 1 1 d . . . H14 H 0.9853 0.1107 0.4394 0.052 Uiso 1 1 calc R . . C15 C 0.8695(4) 0.0352(4) 0.3613(3) 0.0480(10) Uani 1 1 d . . . H15 H 0.8976 -0.0545 0.3906 0.058 Uiso 1 1 calc R . . C16 C 0.7778(4) 0.0666(3) 0.2895(2) 0.0368(8) Uani 1 1 d . . . H16 H 0.7443 -0.0018 0.2690 0.044 Uiso 1 1 calc R . . C17 C 0.6726(3) 0.0752(3) -0.0662(2) 0.0237(6) Uani 1 1 d . . . C18 C 0.5790(3) 0.0386(3) -0.1184(2) 0.0260(6) Uani 1 1 d . . . H18 H 0.4775 0.0769 -0.1070 0.031 Uiso 1 1 calc R . . C19 C 0.6325(4) -0.0527(3) -0.1865(2) 0.0326(7) Uani 1 1 d . . . H19 H 0.5674 -0.0772 -0.2210 0.039 Uiso 1 1 calc R . . C20 C 0.7790(4) -0.1083(3) -0.2049(2) 0.0343(8) Uani 1 1 d . . . H20 H 0.8149 -0.1713 -0.2517 0.041 Uiso 1 1 calc R . . C21 C 0.8735(4) -0.0721(3) -0.1552(2) 0.0335(8) Uani 1 1 d . . . H21 H 0.9747 -0.1091 -0.1683 0.040 Uiso 1 1 calc R . . C22 C 0.8206(3) 0.0187(3) -0.0857(2) 0.0274(7) Uani 1 1 d . . . H22 H 0.8864 0.0424 -0.0513 0.033 Uiso 1 1 calc R . . C23 C 0.1282(3) 0.6478(3) 0.3261(2) 0.0270(7) Uani 1 1 d . . . H23 H 0.053(3) 0.644(3) 0.287(2) 0.028(8) Uiso 1 1 d . . . C24 C 0.2058(3) 0.7327(3) 0.2966(2) 0.0273(7) Uani 1 1 d . . . H24 H 0.182(3) 0.787(3) 0.240(2) 0.023(8) Uiso 1 1 d . . . C25 C 0.3048(4) 0.7737(3) 0.3534(2) 0.0345(8) Uani 1 1 d . . . H25A H 0.2456 0.8445 0.3946 0.041 Uiso 1 1 calc R . . H25B H 0.3662 0.8151 0.3114 0.041 Uiso 1 1 calc R . . C26 C 0.4024(3) 0.6552(3) 0.4123(2) 0.0343(8) Uani 1 1 d . . . H26A H 0.4904 0.6768 0.4242 0.041 Uiso 1 1 calc R . . H26B H 0.3511 0.6451 0.4726 0.041 Uiso 1 1 calc R . . C27 C 0.4462(3) 0.5208(3) 0.3659(2) 0.0300(7) Uani 1 1 d . . . H27 H 0.552(4) 0.491(3) 0.349(2) 0.033(9) Uiso 1 1 d . . . C28 C 0.3743(4) 0.4244(3) 0.3788(2) 0.0318(7) Uani 1 1 d . . . H28 H 0.433(3) 0.329(3) 0.368(2) 0.031(9) Uiso 1 1 d . . . C29 C 0.2336(4) 0.4391(3) 0.4335(2) 0.0397(8) Uani 1 1 d . . . H29A H 0.2533 0.4152 0.4997 0.048 Uiso 1 1 calc R . . H29B H 0.1901 0.3734 0.4129 0.048 Uiso 1 1 calc R . . C30 C 0.1242(4) 0.5840(3) 0.4234(2) 0.0355(8) Uani 1 1 d . . . H30A H 0.0258 0.5797 0.4403 0.043 Uiso 1 1 calc R . . H30B H 0.1458 0.6424 0.4667 0.043 Uiso 1 1 calc R . . F1 F 0.3733(2) 0.3310(2) 0.77321(14) 0.0427(5) Uani 1 1 d . . . F2 F 0.2235(2) 0.2061(2) 0.81621(15) 0.0460(5) Uani 1 1 d . . . F3 F 0.1325(2) 0.4251(2) 0.76042(18) 0.0555(6) Uani 1 1 d . . . F4 F 0.2611(3) 0.2605(3) 0.66530(16) 0.0699(7) Uani 1 1 d . . . B1 B 0.2493(4) 0.3044(4) 0.7521(3) 0.0341(9) Uani 1 1 d . . . C31 C 0.5035(11) 0.0651(9) 0.5104(7) 0.078(4) Uani 0.40 1 d PD . . H31A H 0.5624 0.1174 0.4764 0.093 Uiso 0.40 1 calc PR . . H31B H 0.4503 0.1212 0.5615 0.093 Uiso 0.40 1 calc PR . . Cl1 Cl 0.3801(2) 0.06880(17) 0.43956(12) 0.0844(5) Uani 0.80 1 d PD . . 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 0.02397(14) 0.02194(13) 0.01905(13) -0.00220(8) -0.00144(9) -0.00242(9) P1 0.0230(4) 0.0211(4) 0.0208(4) -0.0035(3) -0.0022(3) -0.0022(3) N1 0.0237(13) 0.0205(12) 0.0217(13) -0.0017(9) -0.0015(10) -0.0026(10) C1 0.0238(15) 0.0192(14) 0.0230(15) -0.0007(11) -0.0020(12) -0.0035(12) C2 0.0230(15) 0.0196(14) 0.0281(16) 0.0001(12) -0.0022(12) -0.0029(12) C3 0.0252(15) 0.0214(14) 0.0215(15) -0.0019(11) -0.0004(12) -0.0066(12) C4 0.0240(15) 0.0214(14) 0.0201(15) -0.0013(11) -0.0013(12) -0.0048(12) C5 0.0220(15) 0.0186(13) 0.0235(15) -0.0010(11) 0.0001(12) -0.0053(12) C6 0.0239(15) 0.0193(13) 0.0218(15) -0.0017(11) 0.0007(12) -0.0073(12) C7 0.0278(16) 0.0230(14) 0.0226(15) -0.0027(11) -0.0007(12) -0.0040(13) C8 0.0286(16) 0.0254(15) 0.0242(16) 0.0002(12) -0.0054(13) -0.0048(13) C9 0.0240(16) 0.0240(15) 0.0298(17) -0.0005(12) -0.0028(13) -0.0012(13) C10 0.0275(16) 0.0229(14) 0.0234(16) -0.0043(12) -0.0005(13) -0.0007(13) C11 0.0259(16) 0.0239(15) 0.0230(16) -0.0043(12) -0.0024(12) -0.0008(12) C12 0.0266(16) 0.0248(15) 0.0230(16) -0.0052(12) -0.0005(13) -0.0015(13) C13 0.0290(17) 0.0382(18) 0.0303(18) -0.0143(14) -0.0011(14) -0.0055(14) C14 0.044(2) 0.048(2) 0.0268(18) -0.0061(15) -0.0152(16) 0.0038(17) C15 0.064(3) 0.0299(18) 0.039(2) 0.0006(15) -0.0174(19) 0.0024(18) C16 0.048(2) 0.0239(16) 0.0334(19) -0.0022(13) -0.0117(16) -0.0031(15) C17 0.0293(16) 0.0190(14) 0.0199(15) -0.0013(11) -0.0005(12) -0.0038(12) C18 0.0252(16) 0.0243(15) 0.0268(16) -0.0026(12) 0.0006(13) -0.0057(13) C19 0.0401(19) 0.0303(16) 0.0291(18) -0.0081(13) 0.0009(15) -0.0125(15) C20 0.045(2) 0.0257(16) 0.0260(17) -0.0086(13) 0.0035(15) -0.0025(15) C21 0.0335(18) 0.0263(16) 0.0302(18) -0.0008(13) 0.0013(14) 0.0039(14) C22 0.0281(16) 0.0219(14) 0.0283(17) 0.0000(12) -0.0034(13) -0.0025(13) C23 0.0202(15) 0.0320(16) 0.0217(16) -0.0062(12) -0.0010(13) 0.0027(13) C24 0.0283(17) 0.0215(15) 0.0245(17) -0.0060(12) -0.0018(13) 0.0039(13) C25 0.0398(19) 0.0304(17) 0.0348(19) -0.0105(14) -0.0011(15) -0.0115(15) C26 0.0300(17) 0.0456(19) 0.0290(18) -0.0139(15) -0.0043(14) -0.0108(15) C27 0.0246(17) 0.0374(18) 0.0199(16) -0.0040(13) -0.0051(13) 0.0028(14) C28 0.0363(18) 0.0282(17) 0.0227(16) 0.0040(13) -0.0029(14) -0.0002(15) C29 0.040(2) 0.0414(19) 0.034(2) 0.0075(15) 0.0014(16) -0.0120(16) C30 0.0304(17) 0.048(2) 0.0256(17) -0.0033(14) 0.0053(14) -0.0105(15) F1 0.0350(11) 0.0527(12) 0.0436(12) -0.0050(9) -0.0032(9) -0.0178(9) F2 0.0448(12) 0.0392(11) 0.0521(13) -0.0037(9) 0.0091(10) -0.0135(9) F3 0.0413(12) 0.0344(11) 0.0912(18) -0.0040(11) -0.0220(12) -0.0085(10) F4 0.102(2) 0.0859(18) 0.0354(13) -0.0198(12) -0.0028(13) -0.0445(16) B1 0.038(2) 0.034(2) 0.031(2) -0.0063(16) -0.0054(17) -0.0113(17) C31 0.133(11) 0.036(6) 0.061(7) -0.034(5) 0.009(7) -0.019(6) Cl1 0.1106(14) 0.0829(11) 0.0735(11) 0.0208(9) -0.0349(10) -0.0498(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C28 2.150(3) . ? Rh1 N1 2.159(2) . ? Rh1 C27 2.167(3) . ? Rh1 C24 2.213(3) . ? Rh1 P1 2.2250(8) . ? Rh1 C23 2.236(3) . ? P1 C5 1.721(3) . ? P1 C1 1.729(3) . ? N1 C10 1.348(4) . ? N1 C6 1.372(3) . ? C1 C2 1.397(4) . ? C1 C11 1.481(4) . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C3 C4 1.404(4) . ? C3 C17 1.481(4) . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.472(4) . ? C6 C7 1.390(4) . ? C7 C8 1.375(4) . ? C7 H7 0.9500 . ? C8 C9 1.379(4) . ? C8 H8 0.9500 . ? C9 C10 1.378(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.398(4) . ? C11 C16 1.400(4) . ? C12 C13 1.379(4) . ? C12 H12 0.9500 . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 C16 1.379(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(4) . ? C17 C18 1.397(4) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 C20 1.377(5) . ? C19 H19 0.9500 . ? C20 C21 1.379(5) . ? C20 H20 0.9500 . ? C21 C22 1.394(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.361(5) . ? C23 C30 1.510(4) . ? C23 H23 0.98(3) . ? C24 C25 1.504(4) . ? C24 H24 0.96(3) . ? C25 C26 1.527(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.520(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.390(5) . ? C27 H27 0.99(3) . ? C28 C29 1.505(5) . ? C28 H28 0.99(3) . ? C29 C30 1.537(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? F1 B1 1.392(4) . ? F2 B1 1.389(4) . ? F3 B1 1.401(4) . ? F4 B1 1.363(4) . ? C31 Cl1 1.637(6) 2_656 ? C31 Cl1 1.639(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? Cl1 C31 1.637(6) 2_656 ? 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 C28 Rh1 N1 153.72(12) . . ? C28 Rh1 C27 37.55(13) . . ? N1 Rh1 C27 168.71(11) . . ? C28 Rh1 C24 96.28(12) . . ? N1 Rh1 C24 95.25(10) . . ? C27 Rh1 C24 80.49(11) . . ? C28 Rh1 P1 96.71(9) . . ? N1 Rh1 P1 79.76(6) . . ? C27 Rh1 P1 100.56(8) . . ? C24 Rh1 P1 159.44(9) . . ? C28 Rh1 C23 80.95(12) . . ? N1 Rh1 C23 95.15(10) . . ? C27 Rh1 C23 87.45(11) . . ? C24 Rh1 C23 35.60(12) . . ? P1 Rh1 C23 163.71(9) . . ? C5 P1 C1 105.25(14) . . ? C5 P1 Rh1 107.89(10) . . ? C1 P1 Rh1 146.23(10) . . ? C10 N1 C6 117.2(2) . . ? C10 N1 Rh1 121.23(19) . . ? C6 N1 Rh1 121.35(18) . . ? C2 C1 C11 120.0(2) . . ? C2 C1 P1 119.8(2) . . ? C11 C1 P1 120.2(2) . . ? C3 C2 C1 126.8(3) . . ? C3 C2 H2 116.6 . . ? C1 C2 H2 116.6 . . ? C2 C3 C4 121.6(3) . . ? C2 C3 C17 119.9(2) . . ? C4 C3 C17 118.5(2) . . ? C5 C4 C3 123.9(3) . . ? C5 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? C4 C5 C6 123.4(3) . . ? C4 C5 P1 122.6(2) . . ? C6 C5 P1 113.9(2) . . ? N1 C6 C7 120.9(3) . . ? N1 C6 C5 116.8(2) . . ? C7 C6 C5 122.2(3) . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 118.5(3) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N1 C10 C9 123.7(3) . . ? N1 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C12 C11 C16 118.8(3) . . ? C12 C11 C1 120.3(3) . . ? C16 C11 C1 120.9(3) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 120.2(3) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C22 C17 C18 118.1(3) . . ? C22 C17 C3 121.4(3) . . ? C18 C17 C3 120.5(3) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.6(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.8(3) . . ? C17 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C30 124.6(3) . . ? C24 C23 Rh1 71.28(17) . . ? C30 C23 Rh1 110.73(19) . . ? C24 C23 H23 118.3(19) . . ? C30 C23 H23 115.5(19) . . ? Rh1 C23 H23 100.9(18) . . ? C23 C24 C25 126.1(3) . . ? C23 C24 Rh1 73.12(17) . . ? C25 C24 Rh1 107.90(19) . . ? C23 C24 H24 118.2(18) . . ? C25 C24 H24 114.4(18) . . ? Rh1 C24 H24 101.1(18) . . ? C24 C25 C26 113.9(3) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 112.4(2) . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 125.4(3) . . ? C28 C27 Rh1 70.57(18) . . ? C26 C27 Rh1 113.4(2) . . ? C28 C27 H27 119.6(19) . . ? C26 C27 H27 110.0(19) . . ? Rh1 C27 H27 109.6(18) . . ? C27 C28 C29 126.6(3) . . ? C27 C28 Rh1 71.87(18) . . ? C29 C28 Rh1 108.2(2) . . ? C27 C28 H28 116.4(19) . . ? C29 C28 H28 114.3(19) . . ? Rh1 C28 H28 107.0(18) . . ? C28 C29 C30 113.4(3) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C23 C30 C29 112.0(3) . . ? C23 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? C23 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? F4 B1 F2 109.5(3) . . ? F4 B1 F1 111.8(3) . . ? F2 B1 F1 109.5(3) . . ? F4 B1 F3 110.4(3) . . ? F2 B1 F3 107.7(3) . . ? F1 B1 F3 107.8(3) . . ? Cl1 C31 Cl1 128.2(6) 2_656 . ? Cl1 C31 H31A 105.2 2_656 . ? Cl1 C31 H31A 105.2 . . ? Cl1 C31 H31B 105.2 2_656 . ? Cl1 C31 H31B 105.2 . . ? H31A C31 H31B 106.0 . . ? C31 Cl1 C31 51.8(6) 2_656 . ? 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 C28 Rh1 P1 C5 149.65(14) . . . . ? N1 Rh1 P1 C5 -4.01(12) . . . . ? C27 Rh1 P1 C5 -172.54(14) . . . . ? C24 Rh1 P1 C5 -81.5(3) . . . . ? C23 Rh1 P1 C5 69.0(3) . . . . ? C28 Rh1 P1 C1 -18.9(2) . . . . ? N1 Rh1 P1 C1 -172.6(2) . . . . ? C27 Rh1 P1 C1 18.9(2) . . . . ? C24 Rh1 P1 C1 110.0(3) . . . . ? C23 Rh1 P1 C1 -99.6(3) . . . . ? C28 Rh1 N1 C10 94.3(3) . . . . ? C27 Rh1 N1 C10 -88.6(6) . . . . ? C24 Rh1 N1 C10 -21.5(2) . . . . ? P1 Rh1 N1 C10 178.7(2) . . . . ? C23 Rh1 N1 C10 14.3(2) . . . . ? C28 Rh1 N1 C6 -80.8(3) . . . . ? C27 Rh1 N1 C6 96.3(5) . . . . ? C24 Rh1 N1 C6 163.5(2) . . . . ? P1 Rh1 N1 C6 3.6(2) . . . . ? C23 Rh1 N1 C6 -160.7(2) . . . . ? C5 P1 C1 C2 -1.9(3) . . . . ? Rh1 P1 C1 C2 166.84(16) . . . . ? C5 P1 C1 C11 177.1(2) . . . . ? Rh1 P1 C1 C11 -14.2(4) . . . . ? C11 C1 C2 C3 -177.0(3) . . . . ? P1 C1 C2 C3 2.0(4) . . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C1 C2 C3 C17 -179.5(3) . . . . ? C2 C3 C4 C5 -2.2(5) . . . . ? C17 C3 C4 C5 177.3(3) . . . . ? C3 C4 C5 C6 -175.9(3) . . . . ? C3 C4 C5 P1 1.9(4) . . . . ? C1 P1 C5 C4 0.1(3) . . . . ? Rh1 P1 C5 C4 -173.4(2) . . . . ? C1 P1 C5 C6 178.1(2) . . . . ? Rh1 P1 C5 C6 4.6(2) . . . . ? C10 N1 C6 C7 1.0(4) . . . . ? Rh1 N1 C6 C7 176.2(2) . . . . ? C10 N1 C6 C5 -176.9(3) . . . . ? Rh1 N1 C6 C5 -1.7(3) . . . . ? C4 C5 C6 N1 175.8(3) . . . . ? P1 C5 C6 N1 -2.2(3) . . . . ? C4 C5 C6 C7 -2.1(4) . . . . ? P1 C5 C6 C7 179.9(2) . . . . ? N1 C6 C7 C8 -1.1(4) . . . . ? C5 C6 C7 C8 176.8(3) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C6 N1 C10 C9 -0.2(4) . . . . ? Rh1 N1 C10 C9 -175.5(2) . . . . ? C8 C9 C10 N1 -0.5(5) . . . . ? C2 C1 C11 C12 125.2(3) . . . . ? P1 C1 C11 C12 -53.8(4) . . . . ? C2 C1 C11 C16 -51.2(4) . . . . ? P1 C1 C11 C16 129.9(3) . . . . ? C16 C11 C12 C13 1.5(5) . . . . ? C1 C11 C12 C13 -174.9(3) . . . . ? C11 C12 C13 C14 -1.1(5) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? C13 C14 C15 C16 1.3(6) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? C12 C11 C16 C15 -0.4(5) . . . . ? C1 C11 C16 C15 176.0(3) . . . . ? C2 C3 C17 C22 -39.0(4) . . . . ? C4 C3 C17 C22 141.5(3) . . . . ? C2 C3 C17 C18 141.4(3) . . . . ? C4 C3 C17 C18 -38.1(4) . . . . ? C22 C17 C18 C19 0.9(4) . . . . ? C3 C17 C18 C19 -179.5(3) . . . . ? C17 C18 C19 C20 -0.7(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C22 1.0(5) . . . . ? C18 C17 C22 C21 -0.3(4) . . . . ? C3 C17 C22 C21 -179.8(3) . . . . ? C20 C21 C22 C17 -0.7(5) . . . . ? C28 Rh1 C23 C24 114.4(2) . . . . ? N1 Rh1 C23 C24 -91.82(19) . . . . ? C27 Rh1 C23 C24 77.2(2) . . . . ? P1 Rh1 C23 C24 -162.7(2) . . . . ? C28 Rh1 C23 C30 -6.5(2) . . . . ? N1 Rh1 C23 C30 147.3(2) . . . . ? C27 Rh1 C23 C30 -43.7(2) . . . . ? C24 Rh1 C23 C30 -120.9(3) . . . . ? P1 Rh1 C23 C30 76.4(4) . . . . ? C30 C23 C24 C25 2.6(5) . . . . ? Rh1 C23 C24 C25 -100.2(3) . . . . ? C30 C23 C24 Rh1 102.7(3) . . . . ? C28 Rh1 C24 C23 -64.8(2) . . . . ? N1 Rh1 C24 C23 91.53(19) . . . . ? C27 Rh1 C24 C23 -99.0(2) . . . . ? P1 Rh1 C24 C23 166.26(18) . . . . ? C28 Rh1 C24 C25 58.5(2) . . . . ? N1 Rh1 C24 C25 -145.2(2) . . . . ? C27 Rh1 C24 C25 24.3(2) . . . . ? P1 Rh1 C24 C25 -70.5(3) . . . . ? C23 Rh1 C24 C25 123.3(3) . . . . ? C23 C24 C25 C26 43.6(4) . . . . ? Rh1 C24 C25 C26 -38.2(3) . . . . ? C24 C25 C26 C27 33.3(4) . . . . ? C25 C26 C27 C28 -93.0(4) . . . . ? C25 C26 C27 Rh1 -10.9(4) . . . . ? N1 Rh1 C27 C28 -177.9(4) . . . . ? C24 Rh1 C27 C28 113.6(2) . . . . ? P1 Rh1 C27 C28 -87.27(18) . . . . ? C23 Rh1 C27 C28 78.4(2) . . . . ? C28 Rh1 C27 C26 -121.1(3) . . . . ? N1 Rh1 C27 C26 61.0(6) . . . . ? C24 Rh1 C27 C26 -7.5(2) . . . . ? P1 Rh1 C27 C26 151.7(2) . . . . ? C23 Rh1 C27 C26 -42.6(2) . . . . ? C26 C27 C28 C29 5.9(5) . . . . ? Rh1 C27 C28 C29 -99.5(3) . . . . ? C26 C27 C28 Rh1 105.4(3) . . . . ? N1 Rh1 C28 C27 179.07(19) . . . . ? C24 Rh1 C28 C27 -65.4(2) . . . . ? P1 Rh1 C28 C27 98.62(18) . . . . ? C23 Rh1 C28 C27 -97.7(2) . . . . ? N1 Rh1 C28 C29 -57.4(4) . . . . ? C27 Rh1 C28 C29 123.5(3) . . . . ? C24 Rh1 C28 C29 58.1(2) . . . . ? P1 Rh1 C28 C29 -137.9(2) . . . . ? C23 Rh1 C28 C29 25.9(2) . . . . ? C27 C28 C29 C30 38.0(5) . . . . ? Rh1 C28 C29 C30 -42.5(3) . . . . ? C24 C23 C30 C29 -95.3(4) . . . . ? Rh1 C23 C30 C29 -14.2(3) . . . . ? C28 C29 C30 C23 38.1(4) . . . . ? Cl1 C31 Cl1 C31 0.000(2) 2_656 . . 2_656 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.034 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.093 #===END data_s4340a _database_code_depnum_ccdc_archive 'CCDC 762389' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 N2 Rh, B F4' _chemical_formula_sum 'C30 H28 B F4 N2 Rh' _chemical_formula_weight 606.26 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4699(7) _cell_length_b 13.7427(12) _cell_length_c 24.527(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.250(5) _cell_angle_gamma 90.00 _cell_volume 2477.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50900 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 27.53 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.7489 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61166 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5685 _reflns_number_gt 4994 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'Eval15, Sadabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0238P)^2^+2.3234P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5685 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _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 0.486646(17) 0.767203(10) 0.906504(5) 0.01507(5) Uani 1 1 d . . . N1 N 0.47279(18) 0.69924(11) 0.82628(6) 0.0148(3) Uani 1 1 d . . . N2 N 0.35337(19) 0.87244(11) 0.85319(6) 0.0176(3) Uani 1 1 d . . . C1 C 0.5410(2) 0.61359(12) 0.81194(7) 0.0157(3) Uani 1 1 d . . . C2 C 0.4647(2) 0.56318(13) 0.76445(7) 0.0169(3) Uani 1 1 d . . . H2 H 0.5107 0.5009 0.7574 0.020 Uiso 1 1 calc R . . C3 C 0.3220(2) 0.60279(13) 0.72715(7) 0.0167(3) Uani 1 1 d . . . C4 C 0.2571(2) 0.69318(13) 0.74041(7) 0.0180(3) Uani 1 1 d . . . H4 H 0.1602 0.7233 0.7159 0.022 Uiso 1 1 calc R . . C5 C 0.3336(2) 0.73915(13) 0.78925(7) 0.0156(3) Uani 1 1 d . . . C6 C 0.2767(2) 0.83822(13) 0.80263(7) 0.0163(3) Uani 1 1 d . . . C7 C 0.1617(2) 0.89610(14) 0.76502(7) 0.0207(4) Uani 1 1 d . . . H7 H 0.1044 0.8702 0.7304 0.025 Uiso 1 1 calc R . . C8 C 0.1319(2) 0.99157(14) 0.77869(8) 0.0230(4) Uani 1 1 d . . . H8 H 0.0528 1.0317 0.7536 0.028 Uiso 1 1 calc R . . C9 C 0.2177(3) 1.02827(14) 0.82897(8) 0.0241(4) Uani 1 1 d . . . H9 H 0.2032 1.0945 0.8384 0.029 Uiso 1 1 calc R . . C10 C 0.3252(3) 0.96615(14) 0.86526(8) 0.0230(4) Uani 1 1 d . . . H10 H 0.3818 0.9907 0.9003 0.028 Uiso 1 1 calc R . . C11 C 0.7156(2) 0.57625(12) 0.84395(7) 0.0158(3) Uani 1 1 d . . . C12 C 0.8728(2) 0.63161(13) 0.84556(7) 0.0195(3) Uani 1 1 d . . . H12 H 0.8656 0.6945 0.8293 0.023 Uiso 1 1 calc R . . C13 C 1.0400(2) 0.59469(15) 0.87097(8) 0.0248(4) Uani 1 1 d . . . H13 H 1.1473 0.6323 0.8721 0.030 Uiso 1 1 calc R . . C14 C 1.0500(3) 0.50270(16) 0.89466(8) 0.0289(4) Uani 1 1 d . . . H14 H 1.1641 0.4777 0.9125 0.035 Uiso 1 1 calc R . . C15 C 0.8942(3) 0.44719(15) 0.89246(8) 0.0277(4) Uani 1 1 d . . . H15 H 0.9018 0.3843 0.9088 0.033 Uiso 1 1 calc R . . C16 C 0.7266(2) 0.48302(13) 0.86648(7) 0.0207(4) Uani 1 1 d . . . H16 H 0.6203 0.4442 0.8641 0.025 Uiso 1 1 calc R . . C17 C 0.2515(2) 0.55408(13) 0.67386(7) 0.0179(3) Uani 1 1 d . . . C18 C 0.2074(3) 0.60964(14) 0.62581(7) 0.0237(4) Uani 1 1 d . . . H18 H 0.2196 0.6784 0.6276 0.028 Uiso 1 1 calc R . . C19 C 0.1457(3) 0.56471(15) 0.57537(8) 0.0282(4) Uani 1 1 d . . . H19 H 0.1165 0.6027 0.5426 0.034 Uiso 1 1 calc R . . C20 C 0.1267(3) 0.46446(15) 0.57260(8) 0.0256(4) Uani 1 1 d . . . H20 H 0.0838 0.4339 0.5380 0.031 Uiso 1 1 calc R . . C21 C 0.1700(2) 0.40860(14) 0.62009(8) 0.0229(4) Uani 1 1 d . . . H21 H 0.1557 0.3399 0.6180 0.027 Uiso 1 1 calc R . . C22 C 0.2342(2) 0.45284(13) 0.67073(7) 0.0198(3) Uani 1 1 d . . . H22 H 0.2663 0.4144 0.7032 0.024 Uiso 1 1 calc R . . C23 C 0.3348(3) 0.80797(14) 0.96761(7) 0.0217(4) Uani 1 1 d . . . H23 H 0.239(3) 0.8472(16) 0.9493(9) 0.025(6) Uiso 1 1 d . . . C24 C 0.5071(3) 0.85065(14) 0.98118(7) 0.0211(4) Uani 1 1 d . . . H24 H 0.521(3) 0.9152(17) 0.9703(9) 0.029(6) Uiso 1 1 d . . . C25 C 0.6516(3) 0.81623(15) 1.02871(7) 0.0245(4) Uani 1 1 d . . . H25A H 0.5920 0.7879 1.0580 0.029 Uiso 1 1 calc R . . H25B H 0.7251 0.8726 1.0448 0.029 Uiso 1 1 calc R . . C26 C 0.7772(3) 0.73990(14) 1.00977(8) 0.0235(4) Uani 1 1 d . . . H26A H 0.8852 0.7732 1.0003 0.028 Uiso 1 1 calc R . . H26B H 0.8201 0.6950 1.0410 0.028 Uiso 1 1 calc R . . C27 C 0.6874(2) 0.68116(13) 0.96041(7) 0.0195(4) Uani 1 1 d . . . H27 H 0.769(3) 0.6575(16) 0.9372(9) 0.025(6) Uiso 1 1 d . . . C28 C 0.5199(2) 0.63513(13) 0.95587(7) 0.0197(3) Uani 1 1 d . . . H28 H 0.492(3) 0.5870(16) 0.9293(9) 0.023(5) Uiso 1 1 d . . . C29 C 0.4094(3) 0.63570(15) 1.00216(8) 0.0253(4) Uani 1 1 d . . . H29A H 0.4928 0.6412 1.0382 0.030 Uiso 1 1 calc R . . H29B H 0.3429 0.5733 1.0019 0.030 Uiso 1 1 calc R . . C30 C 0.2728(3) 0.71999(15) 0.99625(8) 0.0269(4) Uani 1 1 d . . . H30A H 0.1551 0.6972 0.9750 0.032 Uiso 1 1 calc R . . H30B H 0.2524 0.7394 1.0336 0.032 Uiso 1 1 calc R . . F1 F 0.2776(2) 0.40035(10) 0.81274(7) 0.0508(4) Uani 1 1 d . . . F2 F 0.4490(2) 0.27257(13) 0.84995(6) 0.0537(4) Uani 1 1 d . . . F3 F 0.14215(17) 0.26792(9) 0.84234(6) 0.0374(3) Uani 1 1 d . . . F4 F 0.2710(3) 0.26005(12) 0.76574(6) 0.0610(5) Uani 1 1 d . . . B1 B 0.2857(3) 0.30030(17) 0.81774(9) 0.0259(4) Uani 1 1 d . . . 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 0.01642(7) 0.01592(7) 0.01282(7) -0.00033(5) 0.00246(5) 0.00342(5) N1 0.0152(6) 0.0165(7) 0.0128(6) 0.0007(5) 0.0027(5) 0.0011(5) N2 0.0193(7) 0.0157(7) 0.0180(7) 0.0007(6) 0.0040(6) 0.0029(6) C1 0.0149(7) 0.0176(8) 0.0150(8) 0.0021(6) 0.0035(6) 0.0015(6) C2 0.0176(8) 0.0163(8) 0.0174(8) -0.0010(6) 0.0048(6) 0.0015(6) C3 0.0162(8) 0.0196(9) 0.0147(8) 0.0001(6) 0.0040(6) -0.0025(6) C4 0.0166(8) 0.0203(9) 0.0165(8) 0.0024(7) 0.0008(6) 0.0014(7) C5 0.0153(7) 0.0174(8) 0.0148(8) 0.0027(6) 0.0045(6) 0.0018(6) C6 0.0155(8) 0.0170(8) 0.0173(8) 0.0025(6) 0.0053(6) 0.0011(6) C7 0.0197(8) 0.0255(10) 0.0176(8) 0.0043(7) 0.0049(7) 0.0037(7) C8 0.0229(9) 0.0233(9) 0.0249(9) 0.0101(7) 0.0097(7) 0.0077(7) C9 0.0274(9) 0.0173(9) 0.0300(10) 0.0043(7) 0.0110(8) 0.0049(7) C10 0.0260(9) 0.0197(9) 0.0238(9) -0.0018(7) 0.0055(7) 0.0028(7) C11 0.0163(8) 0.0181(8) 0.0126(7) -0.0039(6) 0.0016(6) 0.0035(6) C12 0.0212(8) 0.0202(9) 0.0175(8) -0.0024(7) 0.0043(7) 0.0002(7) C13 0.0172(8) 0.0339(11) 0.0235(9) -0.0040(8) 0.0042(7) -0.0019(8) C14 0.0185(9) 0.0359(12) 0.0305(10) 0.0010(8) -0.0010(8) 0.0078(8) C15 0.0281(10) 0.0236(10) 0.0296(10) 0.0049(8) 0.0006(8) 0.0071(8) C16 0.0208(8) 0.0196(9) 0.0214(9) -0.0002(7) 0.0027(7) 0.0009(7) C17 0.0149(8) 0.0221(9) 0.0163(8) -0.0005(7) 0.0019(6) 0.0000(7) C18 0.0298(10) 0.0203(9) 0.0192(9) 0.0012(7) -0.0007(7) -0.0047(7) C19 0.0366(11) 0.0289(11) 0.0162(9) 0.0040(7) -0.0030(8) -0.0054(8) C20 0.0267(9) 0.0303(11) 0.0181(9) -0.0066(7) -0.0003(7) -0.0023(8) C21 0.0236(9) 0.0203(9) 0.0244(9) -0.0038(7) 0.0037(7) 0.0005(7) C22 0.0193(8) 0.0213(9) 0.0186(8) 0.0010(7) 0.0025(7) 0.0032(7) C23 0.0230(9) 0.0256(10) 0.0177(8) -0.0022(7) 0.0065(7) 0.0084(8) C24 0.0270(9) 0.0204(9) 0.0166(8) -0.0033(7) 0.0056(7) 0.0046(7) C25 0.0275(9) 0.0280(10) 0.0170(8) -0.0050(7) 0.0011(7) 0.0024(8) C26 0.0216(9) 0.0277(10) 0.0193(9) -0.0009(7) -0.0011(7) 0.0047(7) C27 0.0206(8) 0.0228(9) 0.0146(8) 0.0026(7) 0.0019(6) 0.0084(7) C28 0.0252(9) 0.0165(9) 0.0176(8) 0.0004(7) 0.0043(7) 0.0047(7) C29 0.0294(10) 0.0262(10) 0.0225(9) 0.0038(7) 0.0108(8) 0.0007(8) C30 0.0245(9) 0.0333(11) 0.0259(10) -0.0023(8) 0.0126(8) 0.0011(8) F1 0.0665(10) 0.0244(7) 0.0681(10) 0.0039(7) 0.0296(8) -0.0052(7) F2 0.0326(7) 0.0820(12) 0.0439(8) 0.0197(8) -0.0005(6) 0.0049(7) F3 0.0331(7) 0.0316(7) 0.0486(8) 0.0066(6) 0.0103(6) -0.0038(5) F4 0.0895(13) 0.0648(11) 0.0275(7) -0.0138(7) 0.0071(8) 0.0131(9) B1 0.0312(11) 0.0245(11) 0.0222(10) 0.0017(8) 0.0048(9) 0.0018(9) _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 2.0807(14) . ? Rh1 C23 2.1097(17) . ? Rh1 C24 2.1433(18) . ? Rh1 N1 2.1639(14) . ? Rh1 C27 2.1653(17) . ? Rh1 C28 2.1714(18) . ? N1 C1 1.353(2) . ? N1 C5 1.368(2) . ? N2 C10 1.346(2) . ? N2 C6 1.354(2) . ? C1 C2 1.387(2) . ? C1 C11 1.489(2) . ? C2 C3 1.386(2) . ? C2 H2 0.9500 . ? C3 C4 1.393(2) . ? C3 C17 1.479(2) . ? C4 C5 1.384(2) . ? C4 H4 0.9500 . ? C5 C6 1.480(2) . ? C6 C7 1.393(2) . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.380(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.392(2) . ? C11 C12 1.394(2) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.390(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.394(2) . ? C17 C22 1.398(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C19 C20 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.389(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.399(3) . ? C23 C30 1.512(3) . ? C23 H23 0.94(2) . ? C24 C25 1.517(3) . ? C24 H24 0.94(2) . ? C25 C26 1.533(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.510(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.389(3) . ? C27 H27 0.96(2) . ? C28 C29 1.518(2) . ? C28 H28 0.93(2) . ? C29 C30 1.533(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? F1 B1 1.381(3) . ? F2 B1 1.384(3) . ? F3 B1 1.394(3) . ? F4 B1 1.376(3) . ? 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 C23 90.25(7) . . ? N2 Rh1 C24 96.81(7) . . ? C23 Rh1 C24 38.41(7) . . ? N2 Rh1 N1 77.79(6) . . ? C23 Rh1 N1 144.67(7) . . ? C24 Rh1 N1 173.05(7) . . ? N2 Rh1 C27 164.83(7) . . ? C23 Rh1 C27 96.46(7) . . ? C24 Rh1 C27 80.45(7) . . ? N1 Rh1 C27 103.61(6) . . ? N2 Rh1 C28 157.80(7) . . ? C23 Rh1 C28 81.28(7) . . ? C24 Rh1 C28 89.26(7) . . ? N1 Rh1 C28 97.38(6) . . ? C27 Rh1 C28 37.35(7) . . ? C1 N1 C5 116.93(14) . . ? C1 N1 Rh1 130.71(11) . . ? C5 N1 Rh1 109.78(11) . . ? C10 N2 C6 118.44(15) . . ? C10 N2 Rh1 127.07(12) . . ? C6 N2 Rh1 114.28(11) . . ? N1 C1 C2 122.35(15) . . ? N1 C1 C11 119.84(15) . . ? C2 C1 C11 117.44(15) . . ? C3 C2 C1 120.70(16) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 117.05(15) . . ? C2 C3 C17 121.08(16) . . ? C4 C3 C17 121.73(15) . . ? C5 C4 C3 120.12(16) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 122.64(16) . . ? N1 C5 C6 115.84(15) . . ? C4 C5 C6 121.40(15) . . ? N2 C6 C7 121.24(16) . . ? N2 C6 C5 115.54(14) . . ? C7 C6 C5 123.09(16) . . ? C8 C7 C6 119.25(17) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 119.64(17) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.27(18) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 123.01(18) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C16 C11 C12 120.08(16) . . ? C16 C11 C1 120.72(16) . . ? C12 C11 C1 118.78(16) . . ? C13 C12 C11 119.95(17) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 119.85(18) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.22(18) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.35(19) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 119.52(17) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? C18 C17 C22 119.54(16) . . ? C18 C17 C3 119.52(16) . . ? C22 C17 C3 120.90(16) . . ? C19 C18 C17 120.12(18) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.12(18) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.23(17) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.09(18) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 119.89(17) . . ? C21 C22 H22 120.1 . . ? C17 C22 H22 120.1 . . ? C24 C23 C30 124.73(17) . . ? C24 C23 Rh1 72.09(10) . . ? C30 C23 Rh1 111.46(12) . . ? C24 C23 H23 117.4(14) . . ? C30 C23 H23 114.2(14) . . ? Rh1 C23 H23 105.6(13) . . ? C23 C24 C25 123.42(18) . . ? C23 C24 Rh1 69.50(10) . . ? C25 C24 Rh1 115.01(12) . . ? C23 C24 H24 118.1(14) . . ? C25 C24 H24 114.6(14) . . ? Rh1 C24 H24 104.9(14) . . ? C24 C25 C26 111.76(15) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 113.57(15) . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 125.00(16) . . ? C28 C27 Rh1 71.56(10) . . ? C26 C27 Rh1 111.01(12) . . ? C28 C27 H27 117.1(13) . . ? C26 C27 H27 114.7(13) . . ? Rh1 C27 H27 105.4(13) . . ? C27 C28 C29 122.67(17) . . ? C27 C28 Rh1 71.08(10) . . ? C29 C28 Rh1 112.91(12) . . ? C27 C28 H28 118.1(13) . . ? C29 C28 H28 116.4(14) . . ? Rh1 C28 H28 102.4(13) . . ? C28 C29 C30 112.00(15) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C23 C30 C29 113.20(15) . . ? C23 C30 H30A 108.9 . . ? C29 C30 H30A 108.9 . . ? C23 C30 H30B 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.8 . . ? F4 B1 F1 108.84(18) . . ? F4 B1 F2 109.61(19) . . ? F1 B1 F2 110.22(19) . . ? F4 B1 F3 109.37(19) . . ? F1 B1 F3 109.33(18) . . ? F2 B1 F3 109.45(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Rh1 N1 C1 176.20(16) . . . . ? C23 Rh1 N1 C1 -111.12(17) . . . . ? C27 Rh1 N1 C1 11.70(16) . . . . ? C28 Rh1 N1 C1 -25.80(15) . . . . ? N2 Rh1 N1 C5 -22.99(11) . . . . ? C23 Rh1 N1 C5 49.68(17) . . . . ? C27 Rh1 N1 C5 172.50(11) . . . . ? C28 Rh1 N1 C5 135.00(12) . . . . ? C23 Rh1 N2 C10 47.64(16) . . . . ? C24 Rh1 N2 C10 9.69(16) . . . . ? N1 Rh1 N2 C10 -165.87(16) . . . . ? C27 Rh1 N2 C10 -68.9(3) . . . . ? C28 Rh1 N2 C10 114.6(2) . . . . ? C23 Rh1 N2 C6 -126.94(13) . . . . ? C24 Rh1 N2 C6 -164.88(12) . . . . ? N1 Rh1 N2 C6 19.55(11) . . . . ? C27 Rh1 N2 C6 116.6(2) . . . . ? C28 Rh1 N2 C6 -59.9(2) . . . . ? C5 N1 C1 C2 -5.6(2) . . . . ? Rh1 N1 C1 C2 154.08(13) . . . . ? C5 N1 C1 C11 167.22(15) . . . . ? Rh1 N1 C1 C11 -33.1(2) . . . . ? N1 C1 C2 C3 5.0(3) . . . . ? C11 C1 C2 C3 -168.01(15) . . . . ? C1 C2 C3 C4 -1.7(2) . . . . ? C1 C2 C3 C17 174.04(16) . . . . ? C2 C3 C4 C5 -0.5(2) . . . . ? C17 C3 C4 C5 -176.24(16) . . . . ? C1 N1 C5 C4 3.3(2) . . . . ? Rh1 N1 C5 C4 -160.47(14) . . . . ? C1 N1 C5 C6 -172.77(14) . . . . ? Rh1 N1 C5 C6 23.47(17) . . . . ? C3 C4 C5 N1 -0.3(3) . . . . ? C3 C4 C5 C6 175.56(15) . . . . ? C10 N2 C6 C7 -4.1(2) . . . . ? Rh1 N2 C6 C7 170.98(13) . . . . ? C10 N2 C6 C5 171.88(15) . . . . ? Rh1 N2 C6 C5 -13.04(18) . . . . ? N1 C5 C6 N2 -8.0(2) . . . . ? C4 C5 C6 N2 175.91(16) . . . . ? N1 C5 C6 C7 167.92(16) . . . . ? C4 C5 C6 C7 -8.2(3) . . . . ? N2 C6 C7 C8 2.9(3) . . . . ? C5 C6 C7 C8 -172.75(16) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? C7 C8 C9 C10 -2.9(3) . . . . ? C6 N2 C10 C9 1.8(3) . . . . ? Rh1 N2 C10 C9 -172.59(14) . . . . ? C8 C9 C10 N2 1.7(3) . . . . ? N1 C1 C11 C16 126.30(18) . . . . ? C2 C1 C11 C16 -60.5(2) . . . . ? N1 C1 C11 C12 -61.1(2) . . . . ? C2 C1 C11 C12 112.08(18) . . . . ? C16 C11 C12 C13 -1.7(3) . . . . ? C1 C11 C12 C13 -174.36(16) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C12 C13 C14 C15 0.8(3) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C14 C15 C16 C11 -1.7(3) . . . . ? C12 C11 C16 C15 2.5(3) . . . . ? C1 C11 C16 C15 175.03(17) . . . . ? C2 C3 C17 C18 -138.40(18) . . . . ? C4 C3 C17 C18 37.1(2) . . . . ? C2 C3 C17 C22 39.5(2) . . . . ? C4 C3 C17 C22 -144.95(18) . . . . ? C22 C17 C18 C19 0.4(3) . . . . ? C3 C17 C18 C19 178.31(17) . . . . ? C17 C18 C19 C20 0.4(3) . . . . ? C18 C19 C20 C21 -0.3(3) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C20 C21 C22 C17 1.3(3) . . . . ? C18 C17 C22 C21 -1.2(3) . . . . ? C3 C17 C22 C21 -179.15(16) . . . . ? N2 Rh1 C23 C24 -100.68(11) . . . . ? N1 Rh1 C23 C24 -169.60(11) . . . . ? C27 Rh1 C23 C24 65.69(12) . . . . ? C28 Rh1 C23 C24 99.92(12) . . . . ? N2 Rh1 C23 C30 138.24(14) . . . . ? C24 Rh1 C23 C30 -121.08(18) . . . . ? N1 Rh1 C23 C30 69.32(18) . . . . ? C27 Rh1 C23 C30 -55.39(14) . . . . ? C28 Rh1 C23 C30 -21.16(13) . . . . ? C30 C23 C24 C25 -3.0(3) . . . . ? Rh1 C23 C24 C25 -107.09(17) . . . . ? C30 C23 C24 Rh1 104.11(17) . . . . ? N2 Rh1 C24 C23 81.75(12) . . . . ? C27 Rh1 C24 C23 -113.33(12) . . . . ? C28 Rh1 C24 C23 -76.84(12) . . . . ? N2 Rh1 C24 C25 -159.93(14) . . . . ? C23 Rh1 C24 C25 118.32(19) . . . . ? C27 Rh1 C24 C25 5.00(14) . . . . ? C28 Rh1 C24 C25 41.48(15) . . . . ? C23 C24 C25 C26 91.7(2) . . . . ? Rh1 C24 C25 C26 10.7(2) . . . . ? C24 C25 C26 C27 -27.9(2) . . . . ? C25 C26 C27 C28 -49.8(3) . . . . ? C25 C26 C27 Rh1 31.9(2) . . . . ? N2 Rh1 C27 C28 -177.8(2) . . . . ? C23 Rh1 C27 C28 66.42(12) . . . . ? C24 Rh1 C27 C28 101.47(11) . . . . ? N1 Rh1 C27 C28 -84.29(11) . . . . ? N2 Rh1 C27 C26 60.9(3) . . . . ? C23 Rh1 C27 C26 -54.89(14) . . . . ? C24 Rh1 C27 C26 -19.85(13) . . . . ? N1 Rh1 C27 C26 154.39(12) . . . . ? C28 Rh1 C27 C26 -121.31(18) . . . . ? C26 C27 C28 C29 -2.4(3) . . . . ? Rh1 C27 C28 C29 -105.62(17) . . . . ? C26 C27 C28 Rh1 103.17(17) . . . . ? N2 Rh1 C28 C27 178.49(14) . . . . ? C23 Rh1 C28 C27 -112.87(11) . . . . ? C24 Rh1 C28 C27 -75.14(11) . . . . ? N1 Rh1 C28 C27 102.80(11) . . . . ? N2 Rh1 C28 C29 -63.2(2) . . . . ? C23 Rh1 C28 C29 5.46(14) . . . . ? C24 Rh1 C28 C29 43.20(14) . . . . ? N1 Rh1 C28 C29 -138.87(13) . . . . ? C27 Rh1 C28 C29 118.34(18) . . . . ? C27 C28 C29 C30 92.7(2) . . . . ? Rh1 C28 C29 C30 11.1(2) . . . . ? C24 C23 C30 C29 -48.7(2) . . . . ? Rh1 C23 C30 C29 33.9(2) . . . . ? C28 C29 C30 C23 -29.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.750 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.062 #===END