Supplementary Material (ESI) for Dalton Transactions This journal is (c) THe Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _audit_creation_method\tab 'maXus' _publ_contact_author_name 'Michel ETIENNE' _publ_contact_author_address ; Laboratoire de chimie de coordination ( CNRS , UPR 8241 ) 205 route de Narbonne 31077 Toulouse Cedex 4 France ; _publ_contact_author_email 'etienne@lcc-toulouse.fr' _publ_contact_author_fax '(33)561553003' _publ_contact_author_phone '(33)561333176' loop_ _publ_author_name _publ_author_address 'Emmanuelle Teuma' ; Laboratoire de Catalyse, Chimie fine et Polymeres ENSCT 118 route de Narbonne 31077 Toulouse Cedex 4 France ; 'Francois Malbosc' ; Laboratoire de Catalyse, Chimie fine et Polymeres ENSCT 118 route de Narbonne 31077 Toulouse Cedex 4 France ; 'Vincent Pons' ; Laboratoire de Catalyse, Chimie fine et Polymeres ENSCT 118 route de Narbonne 31077 Toulouse Cedex 4 France ; 'Carole Leberre' ; Laboratoire de Catalyse, Chimie fine et Polymeres ENSCT 118 route de Narbonne 31077 Toulouse Cedex 4 France ; 'Philippe Kalck' ; Laboratoire de Catalyse, Chimie fine et Polymeres ENSCT 118 route de Narbonne 31077 Toulouse Cedex 4 France ; 'Joel Jaud' ; Centre d'elaboration des materiaux et d'etudes structurales (CNRS) 29 rue Jeanne Marvig BP 4347 , 31055 Toulouse Cedex 4 France ; 'Michel Etienne' ; Laboratoire de chimie de coordination ( CNRS , UPR 8241 ) 205 route de Narbonne 31077 Toulouse Cedex 4 France ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Waasmaier, D. & Kirfel, A. (1995). Acta Cryst. A51, 416-431. ; data_1 _database_code_CSD 161062 #Crystal and molecular structure of [ C21 H34 N7 Cl3 B1 Rh1 ] , [ (CH3)2 CO] _chemical_formula_moiety '[ C21 H34 N7 Cl3 B1 Rh1 ] , [ (CH3)2 CO]' _chemical_formula_sum 'C24 H40 B Cl3 N7 O Rh' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Colourless' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _publ_requested_journal 'J. Chem. Soc., Dalton Transactions' _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 631.762 _diffrn_radiation_type ' MoK\\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X,-Y,-Z' '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting 'Monoclinic' _chemical_formula_moiety 'C24 H40 B Cl3 N7 O Rh ' _chemical_formula_sum 'C24 H40 B Cl3 N7 O Rh ' _chemical_name_systematic ; ? ; _cell_length_a 12.3405(3) _cell_length_b 12.3544(4) _cell_length_c 21.1247(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.838(2) _cell_angle_gamma 90.00 _cell_volume 3173.3(2) _diffrn_reflns_number 14125 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_av_R_equivalents 0.021 _cell_measurement_reflns_used 73205 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? _exptl_absorpt_coefficient_mu 0.66 _exptl_crystal_F_000 1312 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'B ' 'B ' 0.0013 0.0007 'Waasmaier & Kirfel, 1995' 'N ' 'N ' 0.0061 0.0033 'Waasmaier & Kirfel, 1995' 'O ' 'O ' 0.0106 0.0060 'Waasmaier & Kirfel, 1995' 'Cl' 'Cl' 0.1484 0.1585 'Waasmaier & Kirfel, 1995' 'Rh' 'Rh' -1.1178 0.9187 'Waasmaier & Kirfel, 1995' _reflns_number_total 7213 _reflns_number_gt 4971 _reflns_threshold_expression 'I> 3.00 sigma(I)' _reflns_d_resolution_low 1.77 _reflns_d_resolution_high 0.62 _reflns_limit_h_max 16 _reflns_limit_h_min 0 _reflns_limit_k_max 16 _reflns_limit_k_min 0 _reflns_limit_l_max 16 _reflns_limit_l_min -4 _refine_ls_matrix_type full _refine_ls_R_factor_all 0.075 _refine_ls_wR_factor_all 0.166 _refine_ls_R_factor_gt 0.040 _refine_ls_wR_factor_gt 0.040 _refine_ls_wR_factor_ref 0.040 _refine_ls_goodness_of_fit_gt 1.695 _refine_ls_goodness_of_fit_ref 1.695 _refine_ls_goodness_of_fit_all 3.459 _refine_ls_number_parameters 334 _refine_ls_number_reflns 4971 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^) ; _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; equ(22) p292 'Crystallographic Computing' (1970) ; _refine_ls_extinction_coef 3444(0) _computing_structure_refinement 'maxus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maxus(Mackay et al., 1999)' _atom_sites_solution_hydrogens 'geom, diff' _refine_diff_density_max 0.50 _refine_diff_density_min -0.59 _refine_diff_density_rms 0.07 #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 Rh1 0.202633(3) 0.161536(3) 0.308837(2) 0.03747(2) 1.00 Uij Cl1 -0.08982(1) -0.12643(1) 0.445041(7) 0.07379(9) 1.00 Uij Cl2 0.20978(1) -0.13351(1) 0.092269(6) 0.06530(8) 1.00 Uij Cl3 0.66473(1) 0.08163(1) 0.447976(8) 0.08154(9) 1.00 Uij N1 0.36059(3) 0.10249(3) 0.36187(2) 0.0381(2) 1.00 Uij N2 0.37019(3) -0.00589(3) 0.37408(2) 0.0381(2) 1.00 Uij N3 0.17210(3) -0.05785(3) 0.37569(2) 0.0380(2) 1.00 Uij N4 0.11893(3) 0.04058(3) 0.36606(2) 0.0377(2) 1.00 Uij N5 0.24714(3) -0.06505(3) 0.27291(2) 0.0371(2) 1.00 Uij N6 0.21544(3) 0.03489(3) 0.24794(2) 0.0373(2) 1.00 Uij N7 0.17143(3) 0.30522(3) 0.35493(2) 0.0393(2) 1.00 Uij C1 0.11144(4) -0.12959(4) 0.40427(2) 0.0426(2) 1.00 Uij C2 0.01814(4) -0.07524(4) 0.41244(2) 0.0452(3) 1.00 Uij C3 0.02332(4) 0.02895(4) 0.38852(2) 0.0433(3) 1.00 Uij C4 0.14444(4) -0.24308(4) 0.42074(3) 0.0621(3) 1.00 Uij C5 -0.06226(4) 0.11369(4) 0.38562(3) 0.0596(3) 1.00 Uij C6 0.25016(3) -0.13756(3) 0.22490(2) 0.0398(2) 1.00 Uij C7 0.21918(3) -0.08231(4) 0.16872(2) 0.0423(2) 1.00 Uij C8 0.19870(4) 0.02480(4) 0.18405(2) 0.0404(2) 1.00 Uij C9 0.28396(4) -0.25235(4) 0.23588(2) 0.0589(3) 1.00 Uij C10 0.16677(5) 0.11757(4) 0.13922(2) 0.0638(3) 1.00 Uij C11 0.47304(4) -0.02996(4) 0.40463(2) 0.0451(3) 1.00 Uij C12 0.52945(4) 0.06595(4) 0.41183(2) 0.0489(3) 1.00 Uij C13 0.45867(3) 0.14693(4) 0.38468(2) 0.0441(3) 1.00 Uij C14 0.51151(4) -0.14214(5) 0.42434(3) 0.0707(3) 1.00 Uij C15 0.48286(4) 0.26380(4) 0.37776(3) 0.0647(3) 1.00 Uij C16 0.06148(4) 0.23112(4) 0.26244(2) 0.0473(3) 1.00 Uij C17 0.06829(3) 0.32975(4) 0.30632(2) 0.0451(3) 1.00 Uij C18 0.07672(5) 0.43710(4) 0.27305(3) 0.0666(3) 1.00 Uij C19 0.15872(4) 0.31337(4) 0.42316(2) 0.0475(3) 1.00 Uij C20 0.26046(4) 0.27615(5) 0.46719(2) 0.0628(3) 1.00 Uij C21 0.12477(5) 0.42731(5) 0.44013(3) 0.0810(4) 1.00 Uij B2 0.27476(4) -0.08126(4) 0.34674(3) 0.0417(3) 1.00 Uij O22 0.34762(5) -0.00763(5) 0.83619(3) 0.1372(4) 1.00 Uij C23 0.42740(9) -0.01708(8) 0.81197(8) 0.181(1) 1.00 Uij C24 0.4267(2) 0.0278(1) 0.74608(9) 0.386(2) 1.00 Uij C25 0.52158(9) -0.06870(9) 0.8426(1) 0.449(2) 1.00 Uij H4A 0.214838 -0.257193 0.408917 0.081001 1.00 Uiso H4B 0.090720 -0.291492 0.397837 0.081001 1.00 Uiso H4C 0.148978 -0.253965 0.466113 0.081001 1.00 Uiso H5A -0.038526 0.178383 0.366847 0.079368 1.00 Uiso H5B -0.074658 0.129003 0.428361 0.079368 1.00 Uiso H5C -0.129295 0.088340 0.360036 0.079368 1.00 Uiso H14A 0.452086 -0.192153 0.412090 0.088530 1.00 Uiso H14B 0.534449 -0.144357 0.470099 0.088530 1.00 Uiso H14C 0.572116 -0.161747 0.403618 0.088530 1.00 Uiso H15A 0.417490 0.299636 0.356728 0.083958 1.00 Uiso H15B 0.540083 0.272128 0.352540 0.083958 1.00 Uiso H15C 0.506060 0.295210 0.419438 0.083958 1.00 Uiso H9A 0.301480 -0.265608 0.281261 0.077727 1.00 Uiso H9B 0.284 -0.287 0.197 0.077727 1.00 Uiso H9C 0.227 -0.295 0.249 0.077727 1.00 Uiso H10A 0.157739 0.181547 0.163585 0.083203 1.00 Uiso H10B 0.098909 0.101283 0.111264 0.083203 1.00 Uiso H10C 0.223501 0.129470 0.114051 0.083203 1.00 Uiso H16A -0.005294 0.192262 0.264245 0.066159 1.00 Uiso H16B 0.061611 0.255164 0.219240 0.066159 1.00 Uiso H17 0.006984 0.333886 0.328731 0.063904 1.00 Uiso H7 0.231644 0.354303 0.354593 0.058366 1.00 Uiso H19 0.099138 0.266295 0.428659 0.066862 1.00 Uiso H20A 0.278889 0.204090 0.455739 0.081755 1.00 Uiso H20B 0.248796 0.276968 0.510964 0.081755 1.00 Uiso H20C 0.319580 0.324410 0.462555 0.081755 1.00 Uiso H21A 0.058791 0.448130 0.411749 0.099523 1.00 Uiso H21B 0.182933 0.476608 0.435306 0.099523 1.00 Uiso H21C 0.112149 0.429167 0.483716 0.099523 1.00 Uiso H18A 0.081123 0.494891 0.303768 0.084723 1.00 Uiso H18B 0.013325 0.447395 0.240317 0.084723 1.00 Uiso H18C 0.141814 0.436878 0.253827 0.084723 1.00 Uiso H25A 0.513159 -0.093971 0.884418 0.463713 1.00 Uiso H25B 0.582538 -0.019443 0.846478 0.463713 1.00 Uiso H25C 0.534979 -0.129158 0.816412 0.463713 1.00 Uiso H24A 0.358257 0.063010 0.729702 0.421445 1.00 Uiso H24B 0.438220 -0.030752 0.718128 0.421445 1.00 Uiso H24C 0.485779 0.078964 0.748194 0.421445 1.00 Uiso H1 0.262149 0.236431 0.261281 0.056776 1.00 Uiso H2 0.297205 -0.155708 0.355765 0.060704 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.03799(2) 0.03514(2) 0.03720(2) 0.00410(2) 0.00108(1) 0.00364(2) Cl1 0.07444(9) 0.0759(1) 0.07220(9) -.02794(8) 0.03140(8) -.00181(7) Cl2 0.08094(9) 0.0679(1) 0.04536(7) 0.00487(7) 0.01168(6) -.01498(6) Cl3 0.03498(7) 0.0975(1) 0.1055(1) 0.00013(7) -.01317(7) -.0022(1) N1 0.0328(2) 0.0328(2) 0.0465(2) 0.0025(2) 0.0008(2) 0.0038(2) N2 0.0337(2) 0.0354(2) 0.0423(2) 0.0061(2) -.0034(2) 0.0054(2) N3 0.0378(2) 0.0361(2) 0.0378(2) 0.0006(2) -.0002(2) 0.0052(2) N4 0.0369(2) 0.0353(2) 0.0386(2) 0.0000(2) 0.0008(2) 0.0033(2) N5 0.0382(2) 0.0308(2) 0.0397(2) 0.0048(2) -.0010(2) 0.0039(2) N6 0.0428(2) 0.0326(2) 0.0348(2) 0.0055(2) 0.0037(2) 0.0033(2) N7 0.0413(2) 0.0413(2) 0.0325(2) 0.0047(2) -.0032(2) 0.0022(2) C1 0.0525(3) 0.0409(3) 0.0311(2) -.0099(2) -.0052(2) 0.0067(2) C2 0.0465(3) 0.0491(3) 0.0393(3) -.0129(2) 0.0098(2) -.0026(2) C3 0.0421(3) 0.0485(3) 0.0377(3) -.0037(2) 0.0048(2) -.0048(2) C4 0.0736(4) 0.0453(3) 0.0641(4) -.0106(3) 0.0048(3) 0.0161(3) C5 0.0410(3) 0.0639(3) 0.0732(4) 0.0007(2) 0.0161(3) 0.0002(3) C6 0.0350(2) 0.0363(3) 0.0466(3) 0.0015(2) 0.0047(2) -.0042(2) C7 0.0388(3) 0.0505(3) 0.0365(3) 0.0016(2) 0.0067(2) -.0066(2) C8 0.0419(3) 0.0428(3) 0.0348(3) 0.0042(2) 0.0043(2) 0.0033(2) C9 0.0826(4) 0.0359(3) 0.0547(3) 0.0073(3) 0.0034(3) -.0083(2) C10 0.0907(4) 0.0588(3) 0.0401(3) 0.0169(3) 0.0125(3) 0.0092(2) C11 0.0382(3) 0.0508(3) 0.0436(3) 0.0111(2) -.0019(2) 0.0054(2) C12 0.0312(3) 0.0601(3) 0.0526(3) 0.0014(2) -.0008(2) -.0026(3) C13 0.0365(2) 0.0450(3) 0.0493(3) 0.0011(2) 0.0066(2) -.0016(2) C14 0.0586(3) 0.0702(4) 0.0767(4) 0.0237(3) -.0140(3) 0.0127(3) C15 0.0458(3) 0.0525(3) 0.0935(4) -.0100(3) 0.0106(3) 0.0002(3) C16 0.0474(3) 0.0491(3) 0.0420(3) 0.0126(2) -.0044(2) -.0013(2) C17 0.0426(2) 0.0470(3) 0.0421(2) 0.0133(2) -.0055(2) 0.0020(2) C18 0.0823(4) 0.0498(3) 0.0621(4) 0.0166(3) -.0074(3) 0.0186(3) C19 0.0516(3) 0.0526(3) 0.0365(3) 0.0057(2) 0.0041(2) -.0013(2) C20 0.0629(3) 0.0860(4) 0.0364(3) 0.0133(3) -.0013(2) 0.0058(3) C21 0.1114(5) 0.0713(4) 0.0558(4) 0.0242(4) 0.0040(3) -.0200(3) B2 0.0468(3) 0.0321(3) 0.0432(3) 0.0054(2) -.0019(2) 0.0055(2) O22 0.0937(4) 0.1237(5) 0.1938(6) -.0121(4) 0.0469(4) -.0374(4) C23 0.1204(9) 0.0903(7) 0.336(2) -.0545(6) 0.097(1) -.1070(9) C24 0.600(4) 0.280(2) 0.313(2) -.261(2) 0.352(2) -.198(2) C25 0.0707(7) 0.1058(9) 1.149(6) -.0061(7) 0.087(2) 0.051(2) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 2.2012(3) . . ? Rh1 N4 2.2794(3) . . ? Rh1 N6 2.0488(3) . . ? Rh1 N7 2.0918(3) . . ? Rh1 C16 2.0372(4) . . ? Cl1 C2 1.7212(4) . . ? Cl2 C7 1.7199(4) . . ? Cl3 C12 1.7239(4) . . ? N1 N2 1.3650(4) . . ? N1 C13 1.3412(5) . . ? N2 C11 1.3550(5) . . ? N2 B2 1.5346(6) . . ? N3 N4 1.3801(4) . . ? N3 C1 1.3655(5) . . ? N3 B2 1.5255(6) . . ? N4 C3 1.3523(5) . . ? N5 N6 1.3729(4) . . ? N5 C6 1.3583(5) . . ? N5 B2 1.5515(6) . . ? N6 C8 1.3358(5) . . ? N7 C19 1.4795(5) . . ? C1 C2 1.3690(6) . . ? C1 C4 1.4847(6) . . ? C2 C3 1.3882(6) . . ? C3 C5 1.4809(6) . . ? C6 C7 1.3659(6) . . ? C6 C9 1.4851(6) . . ? C7 C8 1.3956(6) . . ? C8 C10 1.4960(6) . . ? C11 C12 1.3695(6) . . ? C12 C13 1.3861(6) . . ? C13 C15 1.4867(7) . . ? O22 C23 1.1903(9) . . ? C23 C24 1.497(2) . . ? C23 C25 1.385(2) . . ? Rh1 H1 1.6300(4) . . ? N7 H7 0.9600(3) . . ? C4 H4A 0.9600(5) . . ? C4 H4B 0.9600(5) . . ? C4 H4C 0.9600(5) . . ? C5 H5A 0.9600(5) . . ? C5 H5B 0.9600(5) . . ? C5 H5C 0.9600(5) . . ? C9 H9A 0.9600(5) . . ? C9 H9B 0.9600(5) . . ? C9 H9C 0.9600(5) . . ? C10 H10A 0.9600(5) . . ? C10 H10B 0.9600(5) . . ? C10 H10C 0.9600(5) . . ? C14 H14A 0.9600(6) . . ? C14 H14B 0.9600(5) . . ? C14 H14C 0.9600(5) . . ? C15 H15A 0.9600(5) . . ? C15 H15B 0.9600(5) . . ? C15 H15C 0.9600(5) . . ? C16 H16A 0.9600(5) . . ? C16 H16B 0.9600(4) . . ? C17 H17 0.9600(4) . . ? C18 H18A 0.9600(6) . . ? C18 H18B 0.9600(5) . . ? C18 H18C 0.9600(6) . . ? C19 H19 0.9600(4) . . ? C20 H20A 0.9600(5) . . ? C20 H20B 0.9600(4) . . ? C20 H20C 0.9600(5) . . ? C21 H21A 0.9600(6) . . ? C21 H21B 0.9600(7) . . ? C21 H21C 0.9600(6) . . ? B2 H2 0.9700(5) . . ? C24 H24A 0.960(3) . . ? C24 H24B 0.960(1) . . ? C24 H24C 0.960(1) . . ? C25 H25A 0.960(3) . . ? C25 H25B 0.960(1) . . ? C25 H25C 0.960(2) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Rh1 N7 168.7(1) . . . ? N6 Rh1 C16 99.9(1) . . . ? N7 Rh1 C16 69.9(1) . . . ? N2 N1 C13 106.8(1) . . . ? N1 N2 C11 110.4(1) . . . ? N1 N2 B2 119.2(1) . . . ? C11 N2 B2 130.0(1) . . . ? N4 N3 C1 110.7(1) . . . ? N4 N3 B2 121.0(1) . . . ? C1 N3 B2 127.6(1) . . . ? N3 N4 C3 106.0(1) . . . ? N6 N5 C6 110.4(1) . . . ? N6 N5 B2 120.1(1) . . . ? C6 N5 B2 129.5(1) . . . ? Rh1 N6 N5 119.5(1) . . . ? Rh1 N6 C8 133.7(1) . . . ? N5 N6 C8 106.8(1) . . . ? Rh1 N7 C19 124.7(1) . . . ? N3 C1 C2 105.9(1) . . . ? N3 C1 C4 124.6(1) . . . ? C2 C1 C4 129.5(1) . . . ? Cl1 C2 C1 126.5(1) . . . ? Cl1 C2 C3 125.0(1) . . . ? C1 C2 C3 108.5(1) . . . ? N4 C3 C2 108.9(1) . . . ? N4 C3 C5 124.7(1) . . . ? C2 C3 C5 126.4(1) . . . ? N5 C6 C7 106.2(1) . . . ? N5 C6 C9 123.8(1) . . . ? C7 C6 C9 130.0(1) . . . ? Cl2 C7 C6 126.6(1) . . . ? Cl2 C7 C8 125.5(1) . . . ? C6 C7 C8 107.9(1) . . . ? N6 C8 C7 108.7(1) . . . ? N6 C8 C10 123.1(1) . . . ? C7 C8 C10 128.2(1) . . . ? N2 C11 C12 106.3(1) . . . ? Cl3 C12 C11 125.6(1) . . . ? Cl3 C12 C13 126.6(1) . . . ? C11 C12 C13 107.8(1) . . . ? N1 C13 C12 108.6(1) . . . ? N1 C13 C15 123.1(1) . . . ? C12 C13 C15 128.2(1) . . . ? N2 B2 N3 111.7(1) . . . ? N2 B2 N5 108.8(1) . . . ? N3 B2 N5 108.9(1) . . . ? O22 C23 C24 119.3(2) . . . ? O22 C23 C25 122.3(2) . . . ? C24 C23 C25 118.4(2) . . . ? N6 Rh1 H1 87.4(1) . . . ? N7 Rh1 H1 86.8(1) . . . ? C16 Rh1 H1 84.4(1) . . . ? Rh1 N7 H7 109.2(1) . . . ? C19 N7 H7 100.1(1) . . . ? C1 C4 H4A 109.6(1) . . . ? C1 C4 H4B 109.4(1) . . . ? C1 C4 H4C 109.5(1) . . . ? H4A C4 H4B 109.5(1) . . . ? H4A C4 H4C 109.5(1) . . . ? H4B C4 H4C 109.5(1) . . . ? C3 C5 H5A 109.9(1) . . . ? C3 C5 H5B 109.1(1) . . . ? C3 C5 H5C 109.4(1) . . . ? H5A C5 H5B 109.5(1) . . . ? H5A C5 H5C 109.5(1) . . . ? H5B C5 H5C 109.5(1) . . . ? C6 C9 H9A 109.2(1) . . . ? C6 C9 H9B 109.7(1) . . . ? C6 C9 H9C 111.7(1) . . . ? H9A C9 H9B 141.0(1) . . . ? H9A C9 H9C 70.6(1) . . . ? H9B C9 H9C 97.0(1) . . . ? C8 C10 H10A 109.5(1) . . . ? C8 C10 H10B 109.7(1) . . . ? C8 C10 H10C 109.3(1) . . . ? H10A C10 H10B 109.5(1) . . . ? H10A C10 H10C 109.5(1) . . . ? H10B C10 H10C 109.5(1) . . . ? H14A C14 H14B 109.5(1) . . . ? H14A C14 H14C 109.5(1) . . . ? H14B C14 H14C 109.5(1) . . . ? C13 C15 H15A 109.0(1) . . . ? C13 C15 H15B 109.7(1) . . . ? C13 C15 H15C 109.6(1) . . . ? H15A C15 H15B 109.5(1) . . . ? H15A C15 H15C 109.5(1) . . . ? H15B C15 H15C 109.5(1) . . . ? Rh1 C16 H16A 116.0(1) . . . ? Rh1 C16 H16B 116.6(1) . . . ? H16A C16 H16B 109.5(1) . . . ? H18A C18 H18B 109.5(1) . . . ? H18A C18 H18C 109.5(1) . . . ? H18B C18 H18C 109.5(1) . . . ? N7 C19 H19 106.7(1) . . . ? H20A C20 H20B 109.5(1) . . . ? H20A C20 H20C 109.5(1) . . . ? H20B C20 H20C 109.5(1) . . . ? H21A C21 H21B 109.5(1) . . . ? H21A C21 H21C 109.5(1) . . . ? H21B C21 H21C 109.5(1) . . . ? N2 B2 H2 109.0(1) . . . ? N3 B2 H2 109.3(1) . . . ? N5 B2 H2 109.0(1) . . . ? C23 C24 H24A 111.6(2) . . . ? C23 C24 H24B 108.3(2) . . . ? C23 C24 H24C 108.5(2) . . . ? H24A C24 H24B 109.5(2) . . . ? H24A C24 H24C 109.5(2) . . . ? H24B C24 H24C 109.5(2) . . . ? C23 C25 H25A 111.4(2) . . . ? C23 C25 H25B 109.3(2) . . . ? C23 C25 H25C 107.6(3) . . . ? H25A C25 H25B 109.5(3) . . . ? H25A C25 H25C 109.5(2) . . . ? H25B C25 H25C 109.5(2) . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Rh1 C18 4.5306 1_555 3_545 ? Cl1 C3 3.6743 1_555 2_556 ? Cl1 C5 3.7483 1_555 2_556 ? Cl1 C10 3.6735 1_555 3_545 ? Cl1 C20 3.5535 1_555 2_556 ? Cl2 C5 3.6846 1_555 3_545 ? C2 C18 3.8963 1_555 3_545 ? C2 H18B 3.1960 1_555 3_545 ? C3 C18 3.6086 1_555 3_545 ? C3 H18B 2.8647 1_555 3_545 ? C5 C9 3.7964 1_555 3_555 ? C5 C18 3.9777 1_555 3_545 ? C6 C17 3.8929 1_555 3_545 ? C7 C17 3.8317 1_555 3_545 ? C7 C25 3.746(1) 1_555 2_656 ? C7 H17 2.9858 1_555 3_545 ? C7 H25B 2.8176 1_555 2_656 ? C8 C18 3.8208 1_555 3_545 ? C8 C25 3.632(1) 1_555 2_656 ? C8 H25B 2.8815 1_555 2_656 ? C9 C23 3.5858 1_555 4_555 ? C9 C24 3.821(1) 1_555 4_555 ? C9 H15B 3.1115 1_555 3_645 ? C10 C25 3.847(1) 1_555 2_656 ? C11 C12 3.9080 1_555 2_656 ? C11 C24 3.608(1) 1_555 2_656 ? C11 H24B 3.0753 1_555 2_656 ? C12 C14 3.7036 1_555 2_656 ? C12 C24 3.658(1) 1_555 2_656 ? C12 H14B 2.9075 1_555 2_656 ? C12 H24B 2.8739 1_555 2_656 ? C13 C14 3.9885 1_555 2_656 ? C13 C24 3.953(1) 1_555 2_656 ? C13 H14B 3.0547 1_555 2_656 ? C13 H24B 3.0561 1_555 2_656 ? C14 C20 3.7022 1_555 2_656 ? C14 C25 3.979(2) 1_555 4_555 ? C15 O22 3.4827 1_555 4_565 ? C15 C23 3.4447 1_555 4_565 ? C15 C24 3.766(1) 1_555 4_565 ? C15 C25 3.885(1) 1_555 4_565 ? C18 O22 3.4913 1_555 4_565 ? C20 H14B 3.1089 1_555 2_656 ? O22 H7 2.4449 1_555 4_566 ? C23 H15A 2.8574 1_555 4_566 ? C23 H9A 3.1142 1_555 4_556 ? C24 H15A 3.180(1) 1_555 4_566 ? Rh1 C18 4.5306 1_555 3_545 ? Cl1 C3 3.6743 1_555 2_556 ? Cl1 C5 3.7483 1_555 2_556 ? Cl1 C10 3.6735 1_555 3_545 ? Cl1 C20 3.5535 1_555 2_556 ? Cl2 C5 3.6846 1_555 3_545 ? C2 C18 3.8963 1_555 3_545 ? C2 H18B 3.1960 1_555 3_545 ? C3 C18 3.6086 1_555 3_545 ? C3 H18B 2.8647 1_555 3_545 ? C5 C9 3.7964 1_555 3_555 ? C5 C18 3.9777 1_555 3_545 ? C6 C17 3.8929 1_555 3_545 ? C7 C17 3.8317 1_555 3_545 ? C7 C25 3.746(1) 1_555 2_656 ? C7 H17 2.9858 1_555 3_545 ? C7 H25B 2.8176 1_555 2_656 ? C8 C18 3.8208 1_555 3_545 ? C8 C25 3.632(1) 1_555 2_656 ? C8 H25B 2.8815 1_555 2_656 ? C9 C23 3.5858 1_555 4_555 ? C9 C24 3.821(1) 1_555 4_555 ? C9 H15B 3.1115 1_555 3_645 ? C10 C25 3.847(1) 1_555 2_656 ? C11 C12 3.9080 1_555 2_656 ? C11 C24 3.608(1) 1_555 2_656 ? C11 H24B 3.0753 1_555 2_656 ? C12 C14 3.7036 1_555 2_656 ? C12 C24 3.658(1) 1_555 2_656 ? C12 H14B 2.9075 1_555 2_656 ? C12 H24B 2.8739 1_555 2_656 ? C13 C14 3.9885 1_555 2_656 ? C13 C24 3.953(1) 1_555 2_656 ? C13 H14B 3.0547 1_555 2_656 ? C13 H24B 3.0561 1_555 2_656 ? C14 C20 3.7022 1_555 2_656 ? C14 C25 3.979(2) 1_555 4_555 ? C15 O22 3.4827 1_555 4_565 ? C15 C23 3.4447 1_555 4_565 ? C15 C24 3.766(1) 1_555 4_565 ? C15 C25 3.885(1) 1_555 4_565 ? C18 O22 3.4913 1_555 4_565 ? C20 H14B 3.1089 1_555 2_656 ? O22 H7 2.4449 1_555 4_566 ? C23 H15A 2.8574 1_555 4_566 ? C23 H9A 3.1142 1_555 4_556 ? C24 H15A 3.180(1) 1_555 4_566 ? #=================================================== #END #=================================================== data_2 _database_code_CSD 161063 #Crystal and molecular structure of [ C21 H33 N7 Cl4 B1 Rh1 ] , [ (CH3)2 CO] _chemical_formula_moiety '[ C21 H33 N7 Cl4 B1 Rh1 ] , [ (CH3)2 CO]' _chemical_formula_sum 'C24 H39 B Cl4 N7 O Rh ' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'Cube' _exptl_crystal_colour 'Orange' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'noref' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 697.152 _diffrn_radiation_type ' MoK\\a' 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' _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_cell_setting 'Monoclinic' _chemical_formula_moiety 'C24 H39 B Cl4 N7 O Rh ' _chemical_formula_sum 'C24 H39 B Cl4 N7 O Rh ' _chemical_name_systematic ; ? ; _cell_length_a 12.2538(3) _cell_length_b 12.4285(5) _cell_length_c 20.5888(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.547(2) _cell_angle_gamma 90.00 _cell_volume 3125.7(2) _diffrn_reflns_number 11966 _diffrn_reflns_theta_max 26.09 _diffrn_reflns_av_R_equivalents 0.030 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type 'sphere' _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_coefficient_mu 0.91 _exptl_crystal_F_000 1316 _exptl_absorpt_process_details ; Sphere (Maslen, 1992) ; 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'N ' 'N ' 0.0061 0.0033 'Waasmaier & Kirfel, 1995' 'Cl' 'Cl' 0.1484 0.1585 'Waasmaier & Kirfel, 1995' 'B ' 'B ' 0.0013 0.0007 'Waasmaier & Kirfel, 1995' 'Rh' 'Rh' -1.1178 0.9187 'Waasmaier & Kirfel, 1995' 'O ' 'O ' 0.0106 0.0060 'Waasmaier & Kirfel, 1995' # Refinement statistics _reflns_number_total 6069 _reflns_number_gt 5000 _reflns_threshold_expression 'I> 3.00 sigma(I)' _reflns_d_resolution_low 2.33 _reflns_d_resolution_high 0.64 _reflns_limit_h_max 15 _reflns_limit_h_min 0 _reflns_limit_k_max 15 _reflns_limit_k_min 0 _reflns_limit_l_max 15 _reflns_limit_l_min 0 _refine_ls_matrix_type full _refine_ls_R_factor_all 0.094 _refine_ls_wR_factor_all 0.147 _refine_ls_R_factor_gt 0.062 _refine_ls_wR_factor_gt 0.083 _refine_ls_wR_factor_ref 0.083 _refine_ls_goodness_of_fit_gt 2.308 _refine_ls_goodness_of_fit_ref 2.308 _refine_ls_goodness_of_fit_all 3.443 _refine_ls_number_parameters 344 _refine_ls_number_reflns 5000 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^) ; _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; equ(22) p292 'Crystallographic Computing' (1970) ; _refine_ls_extinction_coef 20764(229) _computing_structure_refinement 'maxus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maxus(Mackay et al., 1999)' _atom_sites_solution_hydrogens geom _refine_diff_density_max 1.32 _refine_diff_density_min -1.42 _refine_diff_density_rms 0.18 #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 Rh1 0.54918(3) 0.02984(3) 0.19888(2) 0.0386(2) 1.00 Uij Cl1 0.44212(14) 0.14177(13) 0.25950(8) 0.0618(9) 1.00 Uij Cl2 0.84489(14) -0.24527(15) 0.05293(9) 0.0726(10) 1.00 Uij Cl3 0.09880(13) -0.05001(15) 0.06230(9) 0.0685(9) 1.00 Uij Cl4 0.53805(15) -0.26175(14) 0.42432(7) 0.0649(9) 1.00 Uij O50 0.4076(7) 0.4205(8) 0.1413(5) 0.177(7) 1.00 Uij N1 0.6339(4) -0.0834(3) 0.1452(2) 0.040(2) 1.00 Uij N2 0.5797(4) -0.1820(3) 0.1359(2) 0.041(2) 1.00 Uij N3 0.3940(4) -0.0261(4) 0.1447(2) 0.043(2) 1.00 Uij N4 0.3806(3) -0.1355(3) 0.1415(2) 0.037(2) 1.00 Uij N5 0.5314(3) -0.0938(3) 0.2651(2) 0.041(2) 1.00 Uij N6 0.4977(3) -0.1916(3) 0.2412(2) 0.040(2) 1.00 Uij N7 0.5863(3) 0.1697(3) 0.1478(2) 0.041(2) 1.00 Uij C1 0.6427(4) -0.2510(4) 0.1032(3) 0.042(3) 1.00 Uij C2 0.7357(5) -0.1973(5) 0.0917(3) 0.048(3) 1.00 Uij C3 0.7291(4) -0.0937(5) 0.1184(3) 0.047(3) 1.00 Uij C4 0.6113(6) -0.3643(6) 0.0866(4) 0.067(4) 1.00 Uij C5 0.8188(5) -0.0120(5) 0.1190(4) 0.068(4) 1.00 Uij C6 0.3008(4) 0.0171(5) 0.1188(3) 0.045(3) 1.00 Uij C7 0.2296(4) -0.0642(5) 0.0988(3) 0.045(3) 1.00 Uij C8 0.2793(4) -0.1616(5) 0.1145(3) 0.042(3) 1.00 Uij C9 0.2814(5) 0.1364(5) 0.1148(4) 0.067(4) 1.00 Uij C10 0.2365(5) -0.2738(5) 0.1065(3) 0.058(3) 1.00 Uij C11 0.4950(4) -0.2601(5) 0.2918(3) 0.047(3) 1.00 Uij C12 0.5278(4) -0.2100(5) 0.3467(3) 0.047(3) 1.00 Uij C13 0.5504(4) -0.1029(5) 0.3299(3) 0.043(3) 1.00 Uij C14 0.4597(5) -0.3786(5) 0.2812(3) 0.060(4) 1.00 Uij C15 0.5890(6) -0.0142(5) 0.3751(3) 0.061(4) 1.00 Uij C16 0.6862(5) 0.1020(5) 0.2438(3) 0.053(3) 1.00 Uij C17 0.6064(5) 0.1788(5) 0.0786(3) 0.057(3) 1.00 Uij C18 0.5206(8) 0.1313(7) 0.0339(4) 0.091(5) 1.00 Uij C19 0.6338(7) 0.2926(7) 0.0617(4) 0.091(5) 1.00 Uij C20 0.6845(5) 0.1984(5) 0.1959(3) 0.054(3) 1.00 Uij C21 0.6684(7) 0.3082(6) 0.2273(4) 0.077(5) 1.00 Uij C51 0.3125(8) 0.4207(7) 0.1514(5) 0.094(3) 1.00 Uiso C52 0.2790(8) 0.3994(8) 0.2154(5) 0.109(3) 1.00 Uiso C53 0.2273(10) 0.4356(9) 0.0986(6) 0.126(4) 1.00 Uiso B1 0.4748(5) -0.2089(5) 0.1681(3) 0.043(3) 1.00 Uij H1 0.455347 -0.282303 0.158353 0.060121 1.00 Uiso H4A 0.539997 -0.378880 0.101350 0.080896 1.00 Uiso H4B 0.663571 -0.412862 0.107043 0.080896 1.00 Uiso H4C 0.608093 -0.372981 0.040158 0.080896 1.00 Uiso H5A 0.796779 0.052267 0.139599 0.088012 1.00 Uiso H5B 0.834293 0.003543 0.074777 0.088012 1.00 Uiso H5C 0.883777 -0.040456 0.142185 0.088012 1.00 Uiso H7 0.525656 0.217100 0.153408 0.056054 1.00 Uiso H9A 0.345913 0.173213 0.132609 0.074824 1.00 Uiso H9B 0.220525 0.154928 0.138619 0.074824 1.00 Uiso H9C 0.266936 0.156124 0.069720 0.074824 1.00 Uiso H10A 0.291735 -0.324587 0.122296 0.072662 1.00 Uiso H10B 0.216524 -0.287583 0.061184 0.072662 1.00 Uiso H10C 0.173234 -0.281879 0.130792 0.072662 1.00 Uiso H14A 0.439896 -0.390847 0.235490 0.074979 1.00 Uiso H14B 0.397591 -0.394349 0.305299 0.074979 1.00 Uiso H14C 0.519215 -0.425159 0.295399 0.074979 1.00 Uiso H15A 0.599044 0.050242 0.350761 0.079298 1.00 Uiso H15B 0.657818 -0.034656 0.397654 0.079298 1.00 Uiso H15C 0.535924 -0.002659 0.405872 0.079298 1.00 Uiso H16A 0.753410 0.063225 0.242877 0.069928 1.00 Uiso H16B 0.679191 0.129533 0.286874 0.069928 1.00 Uiso H17 0.671936 0.137761 0.073727 0.072460 1.00 Uiso H18A 0.506103 0.058200 0.045570 0.109115 1.00 Uiso H18B 0.542002 0.132689 -0.010328 0.109115 1.00 Uiso H18C 0.456317 0.173977 0.036571 0.109115 1.00 Uiso H19A 0.692004 0.317723 0.091740 0.108865 1.00 Uiso H19B 0.569993 0.336624 0.065037 0.108865 1.00 Uiso H19C 0.655705 0.295321 0.018225 0.108865 1.00 Uiso H20 0.749179 0.201306 0.172375 0.069674 1.00 Uiso H21A 0.669589 0.363033 0.194410 0.092984 1.00 Uiso H21B 0.725794 0.322358 0.260898 0.092984 1.00 Uiso H21C 0.599178 0.308657 0.245699 0.092984 1.00 Uiso H52A 0.342568 0.391658 0.245773 0.130449 1.00 Uiso H52B 0.236760 0.334266 0.215169 0.130449 1.00 Uiso H52C 0.235077 0.458031 0.229562 0.130449 1.00 Uiso H53A 0.157537 0.429150 0.115646 0.148008 1.00 Uiso H53B 0.234258 0.380946 0.065638 0.148008 1.00 Uiso H53C 0.234356 0.505031 0.079046 0.148008 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.0384(2) 0.0400(3) 0.0374(2) -.00333(19) 0.00291(15) 0.00119(18) Cl1 0.0667(10) 0.0603(10) 0.0587(9) 0.0032(8) 0.0154(7) -.0088(7) Cl2 0.0609(10) 0.0789(13) 0.0795(11) 0.0212(9) 0.0281(8) -.0007(9) Cl3 0.0398(8) 0.0866(13) 0.0774(11) 0.0080(8) -.0110(7) -.0151(9) Cl4 0.0803(11) 0.0697(11) 0.0445(8) -.0007(9) 0.0065(7) 0.0190(7) O50 0.113(6) 0.225(10) 0.199(10) -.032(6) 0.076(6) -.036(7) N1 0.039(2) 0.041(3) 0.041(2) -.002(2) 0.0035(18) 0.003(2) N2 0.041(2) 0.037(3) 0.044(2) 0.004(2) 0.0009(19) 0.0005(19) N3 0.041(3) 0.038(3) 0.048(3) 0.002(2) -.0016(19) -.001(2) N4 0.032(2) 0.036(3) 0.042(2) -.0009(18) -.0008(18) 0.0036(19) N5 0.040(2) 0.041(3) 0.041(2) -.006(2) 0.0089(19) 0.003(2) N6 0.039(2) 0.041(3) 0.040(2) -.004(2) 0.0056(18) 0.008(2) N7 0.041(2) 0.037(3) 0.046(3) -.0074(19) 0.0000(19) 0.0007(19) C1 0.043(3) 0.045(3) 0.038(3) 0.012(3) 0.003(2) -.003(2) C2 0.041(3) 0.057(4) 0.048(3) 0.014(3) 0.007(2) 0.002(3) C3 0.040(3) 0.053(4) 0.048(3) 0.003(3) 0.008(2) 0.012(3) C4 0.057(4) 0.068(5) 0.075(5) 0.009(3) 0.006(3) -.016(4) C5 0.046(4) 0.060(4) 0.098(5) -.007(3) 0.028(3) 0.000(4) C6 0.037(3) 0.049(4) 0.050(3) 0.006(3) 0.004(2) -.001(3) C7 0.034(3) 0.053(4) 0.047(3) 0.002(2) -.001(2) -.003(3) C8 0.034(3) 0.051(4) 0.040(3) -.005(2) 0.004(2) -.001(2) C9 0.051(4) 0.057(4) 0.092(5) 0.010(3) -.004(3) 0.002(4) C10 0.054(4) 0.049(4) 0.070(4) -.021(3) 0.005(3) -.003(3) C11 0.037(3) 0.069(4) 0.035(3) 0.014(3) 0.011(2) 0.023(3) C12 0.041(3) 0.058(4) 0.043(3) 0.000(3) 0.007(2) 0.010(3) C13 0.042(3) 0.048(4) 0.040(3) -.001(2) 0.004(2) 0.000(2) C14 0.072(4) 0.042(4) 0.066(4) -.011(3) 0.010(3) 0.010(3) C15 0.077(4) 0.063(4) 0.041(3) -.010(3) 0.002(3) 0.002(3) C16 0.055(4) 0.054(4) 0.049(3) -.021(3) 0.000(3) 0.002(3) C17 0.064(4) 0.060(4) 0.047(3) 0.005(3) 0.007(3) 0.006(3) C18 0.123(7) 0.101(6) 0.048(4) -.037(5) 0.009(4) 0.005(4) C19 0.105(6) 0.100(6) 0.068(5) -.022(5) 0.011(4) 0.031(4) C20 0.053(4) 0.050(4) 0.059(4) -.013(3) -.002(3) 0.001(3) C21 0.092(6) 0.066(5) 0.071(5) -.029(4) -.010(4) -.009(4) B1 0.045(4) 0.036(4) 0.046(3) 0.004(3) -.001(3) -.003(3) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 Cl1 2.340(2) . . ? Rh1 N1 2.112(5) . . ? Rh1 N3 2.238(4) . . ? Rh1 N5 2.078(4) . . ? Rh1 N7 2.100(4) . . ? Rh1 C16 2.057(5) . . ? Cl2 C2 1.718(6) . . ? Cl3 C7 1.724(5) . . ? Cl4 C12 1.719(6) . . ? O50 C51 1.200(11) . . ? N1 N2 1.399(6) . . ? N1 C3 1.336(7) . . ? N2 C1 1.366(7) . . ? N2 B1 1.530(8) . . ? N3 N4 1.370(6) . . ? N3 C6 1.334(7) . . ? N4 C8 1.360(6) . . ? N4 B1 1.537(7) . . ? N5 N6 1.363(6) . . ? N5 C13 1.341(7) . . ? N6 C11 1.348(6) . . ? N6 B1 1.525(8) . . ? N7 C17 1.469(8) . . ? N7 C20 1.538(7) . . ? C1 C2 1.358(8) . . ? C1 C4 1.493(8) . . ? C2 C3 1.405(8) . . ? C3 C5 1.496(8) . . ? C6 C7 1.377(7) . . ? C6 C9 1.503(8) . . ? C7 C8 1.382(7) . . ? C8 C10 1.494(8) . . ? C11 C12 1.323(8) . . ? C11 C14 1.546(8) . . ? C12 C13 1.408(8) . . ? C13 C15 1.495(8) . . ? C16 C20 1.551(8) . . ? C17 C18 1.466(10) . . ? C17 C19 1.501(10) . . ? C20 C21 1.529(9) . . ? C51 C52 1.434(14) . . ? C51 C53 1.458(13) . . ? N7 H7 0.962(5) . . ? C4 H4A 0.965(7) . . ? C4 H4B 0.954(7) . . ? C4 H4C 0.959(7) . . ? C5 H5A 0.953(7) . . ? C5 H5B 0.964(8) . . ? C5 H5C 0.963(7) . . ? C9 H9A 0.960(7) . . ? C9 H9B 0.953(7) . . ? C9 H9C 0.963(8) . . ? C10 H10A 0.963(7) . . ? C10 H10B 0.961(7) . . ? C10 H10C 0.961(7) . . ? C14 H14A 0.965(7) . . ? C14 H14B 0.961(7) . . ? C14 H14C 0.958(7) . . ? C15 H15A 0.957(6) . . ? C15 H15B 0.964(7) . . ? C15 H15C 0.955(7) . . ? C16 H16A 0.956(7) . . ? C16 H16B 0.961(6) . . ? C17 H17 0.963(7) . . ? C18 H18A 0.960(8) . . ? C18 H18B 0.967(8) . . ? C18 H18C 0.955(10) . . ? C19 H19A 0.958(9) . . ? C19 H19B 0.961(10) . . ? C19 H19C 0.956(8) . . ? C20 H20 0.962(7) . . ? C21 H21A 0.962(8) . . ? C21 H21B 0.963(7) . . ? C21 H21C 0.956(9) . . ? C52 H52A 0.965(10) . . ? C52 H52B 0.960(10) . . ? C52 H52C 0.965(10) . . ? C53 H53A 0.952(12) . . ? C53 H53B 0.969(12) . . ? C53 H53C 0.960(11) . . ? B1 H1 0.960(6) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Rh1 N1 174.22(12) . . . ? Cl1 Rh1 N3 87.73(13) . . . ? Cl1 Rh1 N5 89.83(13) . . . ? Cl1 Rh1 N7 85.85(13) . . . ? Cl1 Rh1 C16 88.5(2) . . . ? N1 Rh1 N3 88.0(2) . . . ? N1 Rh1 N5 86.1(2) . . . ? N1 Rh1 N7 98.9(2) . . . ? N1 Rh1 C16 96.2(2) . . . ? N3 Rh1 N5 88.2(2) . . . ? N3 Rh1 N7 102.5(2) . . . ? N3 Rh1 C16 172.1(2) . . . ? N5 Rh1 N7 168.3(2) . . . ? N5 Rh1 C16 98.8(2) . . . ? N7 Rh1 C16 70.3(2) . . . ? Rh1 N1 N2 114.1(3) . . . ? Rh1 N1 C3 139.6(4) . . . ? N2 N1 C3 106.3(4) . . . ? N1 N2 C1 109.7(5) . . . ? N1 N2 B1 122.6(4) . . . ? C1 N2 B1 127.1(5) . . . ? Rh1 N3 N4 115.2(3) . . . ? Rh1 N3 C6 137.8(4) . . . ? N4 N3 C6 106.6(4) . . . ? N3 N4 C8 111.0(4) . . . ? N3 N4 B1 119.2(4) . . . ? C8 N4 B1 129.7(5) . . . ? Rh1 N5 N6 117.8(3) . . . ? Rh1 N5 C13 134.2(4) . . . ? N6 N5 C13 108.0(4) . . . ? N5 N6 C11 107.9(5) . . . ? N5 N6 B1 120.6(4) . . . ? C11 N6 B1 131.4(5) . . . ? Rh1 N7 C17 127.5(4) . . . ? Rh1 N7 C20 93.4(3) . . . ? C17 N7 C20 115.0(4) . . . ? N2 C1 C2 107.0(5) . . . ? N2 C1 C4 124.0(5) . . . ? C2 C1 C4 128.9(5) . . . ? Cl2 C2 C1 127.3(5) . . . ? Cl2 C2 C3 124.8(5) . . . ? C1 C2 C3 107.9(5) . . . ? N1 C3 C2 109.2(5) . . . ? N1 C3 C5 126.6(6) . . . ? C2 C3 C5 124.1(5) . . . ? N3 C6 C7 109.0(5) . . . ? N3 C6 C9 123.1(5) . . . ? C7 C6 C9 127.9(5) . . . ? Cl3 C7 C6 126.9(4) . . . ? Cl3 C7 C8 124.7(4) . . . ? C6 C7 C8 108.4(5) . . . ? N4 C8 C7 104.9(5) . . . ? N4 C8 C10 124.7(5) . . . ? C7 C8 C10 130.4(5) . . . ? N6 C11 C12 109.8(6) . . . ? N6 C11 C14 121.0(5) . . . ? C12 C11 C14 129.1(5) . . . ? Cl4 C12 C11 127.8(5) . . . ? Cl4 C12 C13 125.4(4) . . . ? C11 C12 C13 106.7(5) . . . ? N5 C13 C12 107.5(5) . . . ? N5 C13 C15 125.3(5) . . . ? C12 C13 C15 127.2(5) . . . ? Rh1 C16 C20 94.7(3) . . . ? N7 C17 C18 114.3(6) . . . ? N7 C17 C19 110.8(5) . . . ? C18 C17 C19 113.3(6) . . . ? N7 C20 C16 101.6(4) . . . ? N7 C20 C21 111.0(5) . . . ? C16 C20 C21 114.6(6) . . . ? O50 C51 C52 120.8(10) . . . ? O50 C51 C53 121.2(11) . . . ? C52 C51 C53 117.9(10) . . . ? N2 B1 N4 110.4(5) . . . ? N2 B1 N6 107.5(4) . . . ? N4 B1 N6 110.0(5) . . . ? Rh1 N7 H7 104.3(3) . . . ? C17 N7 H7 105.1(4) . . . ? C20 N7 H7 110.7(4) . . . ? C1 C4 H4A 109.2(6) . . . ? C1 C4 H4B 110.1(6) . . . ? C1 C4 H4C 108.9(7) . . . ? H4A C4 H4B 109.5(8) . . . ? H4A C4 H4C 109.1(6) . . . ? H4B C4 H4C 110.0(7) . . . ? C3 C5 H5A 109.8(6) . . . ? C3 C5 H5B 109.1(6) . . . ? C3 C5 H5C 109.4(6) . . . ? H5A C5 H5B 109.7(7) . . . ? H5A C5 H5C 109.8(7) . . . ? H5B C5 H5C 108.9(6) . . . ? C6 C9 H9A 109.1(5) . . . ? C6 C9 H9B 109.7(6) . . . ? C6 C9 H9C 108.7(6) . . . ? H9A C9 H9B 110.1(7) . . . ? H9A C9 H9C 109.3(7) . . . ? H9B C9 H9C 110.0(6) . . . ? C8 C10 H10A 110.1(5) . . . ? C8 C10 H10B 109.5(5) . . . ? C8 C10 H10C 109.3(6) . . . ? H10A C10 H10B 109.2(7) . . . ? H10A C10 H10C 109.3(6) . . . ? H10B C10 H10C 109.4(6) . . . ? C11 C14 H14A 109.5(5) . . . ? C11 C14 H14B 110.2(6) . . . ? C11 C14 H14C 109.5(5) . . . ? H14A C14 H14B 108.9(6) . . . ? H14A C14 H14C 109.2(7) . . . ? H14B C14 H14C 109.6(6) . . . ? C13 C15 H15A 109.9(5) . . . ? C13 C15 H15B 109.1(6) . . . ? C13 C15 H15C 108.9(6) . . . ? H15A C15 H15B 109.3(6) . . . ? H15A C15 H15C 110.1(7) . . . ? H15B C15 H15C 109.6(6) . . . ? Rh1 C16 H16A 116.4(4) . . . ? Rh1 C16 H16B 116.1(5) . . . ? C20 C16 H16A 110.2(5) . . . ? C20 C16 H16B 108.3(5) . . . ? H16A C16 H16B 109.7(5) . . . ? N7 C17 H17 105.5(5) . . . ? C18 C17 H17 106.5(6) . . . ? C19 C17 H17 105.7(6) . . . ? C17 C18 H18A 111.2(7) . . . ? C17 C18 H18B 110.5(7) . . . ? C17 C18 H18C 107.1(7) . . . ? H18A C18 H18B 108.8(8) . . . ? H18A C18 H18C 110.0(8) . . . ? H18B C18 H18C 109.3(8) . . . ? C17 C19 H19A 109.0(7) . . . ? C17 C19 H19B 108.8(7) . . . ? C17 C19 H19C 109.6(8) . . . ? H19A C19 H19B 109.7(9) . . . ? H19A C19 H19C 110.0(8) . . . ? H19B C19 H19C 109.7(8) . . . ? N7 C20 H20 108.6(5) . . . ? C16 C20 H20 112.3(6) . . . ? C21 C20 H20 108.6(6) . . . ? C20 C21 H21A 109.0(7) . . . ? C20 C21 H21B 110.9(7) . . . ? C20 C21 H21C 108.8(6) . . . ? H21A C21 H21B 108.9(7) . . . ? H21A C21 H21C 109.7(8) . . . ? H21B C21 H21C 109.5(8) . . . ? C51 C52 H52A 109.8(10) . . . ? C51 C52 H52B 110.2(10) . . . ? C51 C52 H52C 110.2(10) . . . ? H52A C52 H52B 109.0(10) . . . ? H52A C52 H52C 108.6(10) . . . ? H52B C52 H52C 109.0(10) . . . ? C51 C53 H53A 109.0(11) . . . ? C51 C53 H53B 109.7(10) . . . ? C51 C53 H53C 110.1(10) . . . ? H53A C53 H53B 109.3(11) . . . ? H53A C53 H53C 110.1(11) . . . ? H53B C53 H53C 108.6(12) . . . ? N2 B1 H1 108.7(5) . . . ? N4 B1 H1 108.9(5) . . . ? N6 B1 H1 111.2(6) . . . ? #===================================================