# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address R.A.Jones ; Department of Chemistry and Biochemistry, The University of Texas at Austin, 1 University Station A5300, Austin, Texas, 78712-0165 ; 'Xiaoping Yang' ; Department of Chemistry and Biochemistry, The University of Texas at Austin, 1 University Station A5300, Austin, Texas, 78712-0165 ; L.J.Anderson ;Department of Chemistry and Biochemistry, The University of Texas at Austin, 1 University Station A5300, Austin, Texas, 78712-0165 ; W.J.McCarty ; Department of Chemistry and Biochemistry, The University of Texas at Austin, 1 University Station A5300, Austin, Texas, 78712-0165 ; _publ_contact_author_name 'Richard Jones' _publ_contact_author_address ; Department of Chemistry and Biochemistry, The University of Texas at Austin, 1 University Station A5300, Austin, Texas, 78712-0165, USA. ; _publ_contact_author_email rajones@mail.utexas.edu _publ_contact_author_phone '+ 1 (512) 471 - 1706' _publ_section_title ; Dinuclear Rh (II) pyrazolates as CVD precursors for rhodium thin films ; # Attachment '- 3.CIF' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 772325' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Dirhodium(ii) tetrakis(3, 5-di(tert-butyl)pyrazolate))' _chemical_melting_point ? _chemical_formula_moiety 'C44 H76 N8 Rh2' _chemical_formula_sum 'C44 H76 N8 Rh2' _chemical_formula_weight 922.95 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.823(3) _cell_length_b 15.106(3) _cell_length_c 21.085(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.28(3) _cell_angle_gamma 90.00 _cell_volume 4727.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5122 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8375 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details 'Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7478 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4143 _reflns_number_gt 2882 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0079P)^2^+8.7027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4143 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.040201(11) 0.749682(16) 0.307210(8) 0.01349(8) Uani 1 1 d . . . N3 N 0.01698(15) 0.88208(15) 0.28470(10) 0.0179(5) Uani 1 1 d . . . C18 C 0.0000 1.0210(3) 0.2500 0.0272(10) Uani 1 2 d S . . H18A H 0.0000 1.0826 0.2500 0.041 Uiso 1 2 calc SR . . N4 N 0.13941(13) 0.75756(16) 0.26484(9) 0.0172(5) Uani 1 1 d . . . N2 N -0.09156(13) 0.74271(16) 0.30293(9) 0.0169(4) Uani 1 1 d . . . C17 C 0.02659(18) 0.96637(19) 0.30645(13) 0.0216(6) Uani 1 1 d . . . C3 C 0.1294(2) 0.5719(2) 0.42510(13) 0.0268(7) Uani 1 1 d . . . H3B H 0.1427 0.6300 0.4126 0.040 Uiso 1 1 calc R . . H3C H 0.1762 0.5536 0.4658 0.040 Uiso 1 1 calc R . . H3D H 0.0729 0.5731 0.4326 0.040 Uiso 1 1 calc R . . C11 C -0.14963(17) 0.73908(18) 0.33627(11) 0.0178(6) Uani 1 1 d . . . C15 C -0.0399(2) 0.9917(2) 0.39355(15) 0.0374(8) Uani 1 1 d . . . H15A H -0.0808 1.0329 0.3636 0.056 Uiso 1 1 calc R . . H15B H -0.0290 1.0090 0.4395 0.056 Uiso 1 1 calc R . . H15C H -0.0658 0.9335 0.3860 0.056 Uiso 1 1 calc R . . C9 C -0.1271(2) 0.60864(19) 0.40960(14) 0.0285(7) Uani 1 1 d . . . H9A H -0.0857 0.5849 0.3898 0.043 Uiso 1 1 calc R . . H9B H -0.1871 0.5896 0.3839 0.043 Uiso 1 1 calc R . . H9C H -0.1111 0.5879 0.4553 0.043 Uiso 1 1 calc R . . C12 C -0.23591(16) 0.7531(2) 0.29008(11) 0.0208(5) Uani 1 1 d . . . H12A H -0.2892 0.7546 0.2994 0.031 Uiso 1 1 calc R . . C2 C 0.21286(19) 0.5051(2) 0.35518(14) 0.0307(7) Uani 1 1 d . . . H2B H 0.2252 0.5629 0.3417 0.046 Uiso 1 1 calc R . . H2C H 0.2088 0.4634 0.3199 0.046 Uiso 1 1 calc R . . H2D H 0.2605 0.4878 0.3957 0.046 Uiso 1 1 calc R . . N1 N 0.03038(14) 0.61686(15) 0.28273(10) 0.0169(5) Uani 1 1 d . . . C23 C 0.22683(17) 0.76454(17) 0.27272(12) 0.0182(6) Uani 1 1 d . . . C4 C 0.12354(18) 0.50684(18) 0.36827(12) 0.0208(6) Uani 1 1 d . . . C21 C 0.39011(17) 0.7555(3) 0.33993(14) 0.0356(7) Uani 1 1 d . . . H21A H 0.3882 0.6921 0.3381 0.053 Uiso 1 1 calc R . . H21B H 0.4364 0.7743 0.3808 0.053 Uiso 1 1 calc R . . H21C H 0.4028 0.7781 0.3016 0.053 Uiso 1 1 calc R . . C10 C -0.12281(19) 0.71019(18) 0.40928(12) 0.0200(6) Uani 1 1 d . . . C22 C 0.29914(18) 0.79094(19) 0.33879(13) 0.0221(6) Uani 1 1 d . . . C5 C 0.04990(18) 0.53244(19) 0.30247(12) 0.0181(6) Uani 1 1 d . . . C14 C 0.0915(2) 1.0841(2) 0.39288(18) 0.0463(9) Uani 1 1 d . . . H14A H 0.0508 1.1259 0.3634 0.069 Uiso 1 1 calc R . . H14B H 0.1472 1.0838 0.3843 0.069 Uiso 1 1 calc R . . H14C H 0.1028 1.1007 0.4390 0.069 Uiso 1 1 calc R . . C16 C 0.04949(19) 0.9914(2) 0.38005(14) 0.0275(7) Uani 1 1 d . . . C8 C -0.18912(18) 0.7477(2) 0.44082(12) 0.0279(6) Uani 1 1 d . . . H8A H -0.1864 0.8112 0.4409 0.042 Uiso 1 1 calc R . . H8B H -0.1734 0.7267 0.4864 0.042 Uiso 1 1 calc R . . H8C H -0.2491 0.7288 0.4149 0.042 Uiso 1 1 calc R . . C20 C 0.3034(2) 0.8924(2) 0.34233(15) 0.0348(8) Uani 1 1 d . . . H20A H 0.2464 0.9153 0.3415 0.052 Uiso 1 1 calc R . . H20B H 0.3167 0.9150 0.3043 0.052 Uiso 1 1 calc R . . H20C H 0.3498 0.9104 0.3834 0.052 Uiso 1 1 calc R . . C19 C 0.27960(18) 0.7548(2) 0.40013(12) 0.0292(6) Uani 1 1 d . . . H19A H 0.2226 0.7770 0.3997 0.044 Uiso 1 1 calc R . . H19B H 0.3262 0.7735 0.4408 0.044 Uiso 1 1 calc R . . H19C H 0.2778 0.6914 0.3983 0.044 Uiso 1 1 calc R . . C7 C -0.02825(18) 0.7404(2) 0.45167(12) 0.0277(7) Uani 1 1 d . . . H7A H -0.0254 0.8039 0.4513 0.042 Uiso 1 1 calc R . . H7B H 0.0143 0.7164 0.4331 0.042 Uiso 1 1 calc R . . H7C H -0.0140 0.7200 0.4973 0.042 Uiso 1 1 calc R . . C6 C 0.0000 0.4776(3) 0.2500 0.0215(9) Uani 1 2 d S . . H6A H 0.0000 0.4161 0.2500 0.032 Uiso 1 2 calc SR . . C13 C 0.1156(2) 0.9260(2) 0.42768(14) 0.0351(8) Uani 1 1 d . . . H13A H 0.1715 0.9268 0.4193 0.053 Uiso 1 1 calc R . . H13B H 0.0905 0.8674 0.4198 0.053 Uiso 1 1 calc R . . H13C H 0.1262 0.9427 0.4737 0.053 Uiso 1 1 calc R . . C1 C 0.1039(2) 0.4143(2) 0.38977(15) 0.0339(8) Uani 1 1 d . . . H1B H 0.1010 0.3725 0.3548 0.051 Uiso 1 1 calc R . . H1C H 0.0474 0.4151 0.3972 0.051 Uiso 1 1 calc R . . H1D H 0.1511 0.3975 0.4308 0.051 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 0.01228(11) 0.01804(12) 0.00886(11) -0.00040(10) 0.00204(7) 0.00007(10) N3 0.0160(12) 0.0219(14) 0.0144(10) -0.0016(9) 0.0035(9) -0.0004(10) C18 0.027(2) 0.018(2) 0.038(3) 0.000 0.014(2) 0.000 N4 0.0149(10) 0.0239(12) 0.0102(9) -0.0013(10) 0.0012(8) 0.0012(11) N2 0.0137(10) 0.0235(12) 0.0125(9) 0.0001(10) 0.0035(8) -0.0004(11) C17 0.0165(15) 0.0207(16) 0.0285(15) -0.0053(12) 0.0088(12) -0.0022(12) C3 0.0259(17) 0.0352(18) 0.0167(14) 0.0049(13) 0.0039(12) 0.0086(15) C11 0.0183(13) 0.0201(16) 0.0167(11) -0.0003(12) 0.0083(10) 0.0009(13) C15 0.0321(18) 0.054(2) 0.0290(16) -0.0069(15) 0.0138(14) 0.0083(17) C9 0.0337(17) 0.0270(16) 0.0265(15) 0.0055(13) 0.0125(13) 0.0021(14) C12 0.0150(12) 0.0269(14) 0.0224(12) 0.0001(14) 0.0088(10) 0.0002(15) C2 0.0237(16) 0.0404(19) 0.0259(15) -0.0001(14) 0.0058(12) 0.0070(15) N1 0.0157(12) 0.0205(13) 0.0125(10) 0.0001(9) 0.0023(9) -0.0004(10) C23 0.0149(13) 0.0168(17) 0.0217(12) -0.0001(11) 0.0049(10) -0.0009(11) C4 0.0184(14) 0.0240(15) 0.0185(13) 0.0047(11) 0.0046(11) 0.0038(12) C21 0.0169(14) 0.052(2) 0.0310(14) -0.0066(17) 0.0000(11) -0.0007(18) C10 0.0230(15) 0.0220(14) 0.0170(13) 0.0015(11) 0.0095(11) 0.0033(12) C22 0.0163(15) 0.0253(15) 0.0221(14) -0.0016(12) 0.0034(11) -0.0013(12) C5 0.0180(14) 0.0207(16) 0.0158(13) 0.0023(11) 0.0062(11) 0.0014(12) C14 0.044(2) 0.040(2) 0.053(2) -0.0260(18) 0.0137(17) -0.0099(18) C16 0.0215(16) 0.0319(17) 0.0289(15) -0.0134(13) 0.0086(12) -0.0008(14) C8 0.0318(15) 0.0356(16) 0.0211(12) 0.0011(15) 0.0153(11) 0.0063(18) C20 0.042(2) 0.0300(18) 0.0289(16) -0.0059(14) 0.0073(14) -0.0109(16) C19 0.0246(15) 0.0376(17) 0.0195(12) -0.0013(15) 0.0001(11) -0.0061(17) C7 0.0277(15) 0.0376(18) 0.0176(12) -0.0019(14) 0.0076(11) -0.0005(16) C6 0.022(2) 0.019(2) 0.021(2) 0.000 0.0053(17) 0.000 C13 0.0283(18) 0.050(2) 0.0228(16) -0.0111(15) 0.0034(13) 0.0041(16) C1 0.0377(19) 0.0288(18) 0.0296(16) 0.0120(14) 0.0046(14) 0.0031(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 2.058(2) . ? Rh1 N3 2.059(2) . ? Rh1 N4 2.061(2) . ? Rh1 N1 2.064(2) . ? Rh1 Rh1 2.3045(8) 2 ? N3 C17 1.344(4) . ? N3 N3 1.373(4) 2 ? C18 C17 1.388(4) 2 ? C18 C17 1.388(4) . ? C18 H18A 0.9300 . ? N4 C23 1.339(3) . ? N4 N2 1.384(3) 2 ? N2 C11 1.338(3) . ? N2 N4 1.384(3) 2 ? C17 C16 1.514(4) . ? C3 C4 1.528(4) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C11 C12 1.391(3) . ? C11 C10 1.513(3) . ? C15 C16 1.537(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C9 C10 1.536(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C12 C23 1.391(3) 2 ? C12 H12A 0.9300 . ? C2 C4 1.531(4) . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? N1 C5 1.344(3) . ? N1 N1 1.382(4) 2 ? C23 C12 1.391(3) 2 ? C23 C22 1.518(4) . ? C4 C5 1.520(3) . ? C4 C1 1.533(4) . ? C21 C22 1.528(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C10 C7 1.523(4) . ? C10 C8 1.532(4) . ? C22 C19 1.531(4) . ? C22 C20 1.535(4) . ? C5 C6 1.388(4) . ? C14 C16 1.534(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C13 1.534(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C6 C5 1.388(4) 2 ? C6 H6A 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 N3 86.70(9) . . ? N2 Rh1 N4 153.65(7) . . ? N3 Rh1 N4 86.90(9) . . ? N2 Rh1 N1 87.25(9) . . ? N3 Rh1 N1 153.45(7) . . ? N4 Rh1 N1 87.15(9) . . ? N2 Rh1 Rh1 76.75(6) . 2 ? N3 Rh1 Rh1 76.65(6) . 2 ? N4 Rh1 Rh1 76.90(5) . 2 ? N1 Rh1 Rh1 76.81(5) . 2 ? C17 N3 N3 108.66(15) . 2 ? C17 N3 Rh1 148.38(18) . . ? N3 N3 Rh1 102.61(6) 2 . ? C17 C18 C17 107.1(4) 2 . ? C17 C18 H18A 126.5 2 . ? C17 C18 H18A 126.5 . . ? C23 N4 N2 108.23(18) . 2 ? C23 N4 Rh1 149.32(16) . . ? N2 N4 Rh1 102.23(13) 2 . ? C11 N2 N4 108.64(19) . 2 ? C11 N2 Rh1 148.10(16) . . ? N4 N2 Rh1 102.73(13) 2 . ? N3 C17 C18 107.8(2) . . ? N3 C17 C16 123.0(2) . . ? C18 C17 C16 128.6(3) . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N2 C11 C12 108.2(2) . . ? N2 C11 C10 123.0(2) . . ? C12 C11 C10 128.1(2) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C12 C23 106.6(2) . 2 ? C11 C12 H12A 126.7 . . ? C23 C12 H12A 126.7 2 . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C5 N1 N1 108.36(14) . 2 ? C5 N1 Rh1 148.83(17) . . ? N1 N1 Rh1 102.46(6) 2 . ? N4 C23 C12 108.4(2) . 2 ? N4 C23 C22 123.5(2) . . ? C12 C23 C22 127.8(2) 2 . ? C5 C4 C3 111.8(2) . . ? C5 C4 C2 107.7(2) . . ? C3 C4 C2 110.1(2) . . ? C5 C4 C1 109.4(2) . . ? C3 C4 C1 108.5(2) . . ? C2 C4 C1 109.4(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C10 C7 112.5(2) . . ? C11 C10 C8 110.0(2) . . ? C7 C10 C8 108.4(2) . . ? C11 C10 C9 107.2(2) . . ? C7 C10 C9 109.4(2) . . ? C8 C10 C9 109.3(2) . . ? C23 C22 C21 109.2(2) . . ? C23 C22 C19 111.9(2) . . ? C21 C22 C19 109.1(2) . . ? C23 C22 C20 108.3(2) . . ? C21 C22 C20 108.9(3) . . ? C19 C22 C20 109.5(2) . . ? N1 C5 C6 108.2(2) . . ? N1 C5 C4 123.0(2) . . ? C6 C5 C4 128.3(3) . . ? C16 C14 H14A 109.5 . . ? C16 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C16 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C16 C14 110.1(3) . . ? C17 C16 C13 112.1(2) . . ? C14 C16 C13 108.5(3) . . ? C17 C16 C15 106.4(2) . . ? C14 C16 C15 109.6(3) . . ? C13 C16 C15 110.1(3) . . ? C10 C8 H8A 109.5 . . ? C10 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C10 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C22 C20 H20A 109.5 . . ? C22 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C19 H19A 109.5 . . ? C22 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C22 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C10 C7 H7A 109.5 . . ? C10 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C10 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C6 C5 106.8(4) . 2 ? C5 C6 H6A 126.6 . . ? C5 C6 H6A 126.6 2 . ? C16 C13 H13A 109.5 . . ? C16 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C16 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.325 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.058 # Attachment '- 1.cif' data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 840523' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Di-rhodium(ii) tetrakis (mu-(3,5- bis(trifluoromethyl)pyrazolate)) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H4 F24 N8 Rh2, H4 O2' _chemical_formula_sum 'C20 H8 F24 N8 O2 Rh2' _chemical_formula_weight 1054.16 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' 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' O O 0.0106 0.0060 '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 P21/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 9.2451(11) _cell_length_b 18.048(2) _cell_length_c 9.3478(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.683(3) _cell_angle_gamma 90.00 _cell_volume 1515.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22309 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9273 _exptl_absorpt_correction_T_max 0.9627 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27098 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3456 _reflns_number_gt 3152 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction ; 'CrystalClear (Rigaku Inc., 2008)' ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0000P)^2^+3.4419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3456 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _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 C1 C 0.2621(3) -0.10006(13) -0.2904(3) 0.0140(5) Uani 1 1 d . . . C2 C 0.1029(3) -0.09261(13) -0.2847(2) 0.0115(4) Uani 1 1 d . . . C3 C -0.0246(3) -0.11710(14) -0.3855(3) 0.0146(5) Uani 1 1 d . . . H3 H -0.0306 -0.1438 -0.4718 0.018 Uiso 1 1 calc R . . C4 C 0.2859(3) -0.17638(13) 0.2407(3) 0.0143(5) Uani 1 1 d . . . C5 C 0.1236(3) -0.15871(13) 0.1987(2) 0.0117(4) Uani 1 1 d . . . C6 C 0.3045(3) 0.10160(15) 0.3840(3) 0.0168(5) Uani 1 1 d . . . C7 C 0.1408(3) 0.09207(13) 0.3264(2) 0.0123(4) Uani 1 1 d . . . C8 C 0.2813(3) 0.16800(13) -0.1468(3) 0.0125(4) Uani 1 1 d . . . C9 C 0.1197(2) 0.15509(12) -0.1562(2) 0.0106(4) Uani 1 1 d . . . C10 C -0.0028(3) 0.19759(13) -0.2244(3) 0.0129(4) Uani 1 1 d . . . H4 H -0.0035 0.2419 -0.2754 0.016 Uiso 1 1 calc R . . F1 F 0.27569(16) -0.14269(9) -0.40341(16) 0.0224(3) Uani 1 1 d . . . F2 F 0.32429(16) -0.03430(9) -0.30607(18) 0.0233(3) Uani 1 1 d . . . F3 F 0.34657(16) -0.13036(9) -0.16708(16) 0.0218(3) Uani 1 1 d . . . F4 F 0.31405(16) -0.23428(8) 0.33229(18) 0.0241(3) Uani 1 1 d . . . F5 F 0.34029(17) -0.19268(10) 0.12353(17) 0.0278(4) Uani 1 1 d . . . F6 F 0.36774(16) -0.11917(9) 0.30847(18) 0.0231(3) Uani 1 1 d . . . F7 F 0.33452(19) 0.14696(14) 0.4985(2) 0.0553(7) Uani 1 1 d . . . F8 F 0.37429(18) 0.03769(10) 0.4228(2) 0.0378(5) Uani 1 1 d . . . F9 F 0.36986(17) 0.13027(10) 0.28226(18) 0.0276(4) Uani 1 1 d . . . F10 F 0.30133(16) 0.22114(8) -0.23927(17) 0.0215(3) Uani 1 1 d . . . F11 F 0.35717(17) 0.18758(12) -0.01204(17) 0.0333(4) Uani 1 1 d . . . F12 F 0.34834(17) 0.10664(8) -0.1813(2) 0.0276(4) Uani 1 1 d . . . N1 N 0.0650(2) -0.05592(10) -0.1740(2) 0.0101(4) Uani 1 1 d . . . N2 N 0.0764(2) -0.09685(10) 0.1208(2) 0.0102(4) Uani 1 1 d . . . N3 N 0.0867(2) 0.05533(11) 0.2005(2) 0.0105(4) Uani 1 1 d . . . N4 N 0.0745(2) 0.09491(10) -0.0939(2) 0.0093(4) Uani 1 1 d . . . O1 O 0.38416(19) -0.00544(10) 0.0817(2) 0.0191(4) Uani 1 1 d . . . Rh1 Rh 0.130220(17) -0.001291(9) 0.024515(17) 0.00777(6) Uani 1 1 d . . . H1 H 0.4121 0.0371 0.0817 0.068 Uiso 1 1 d . . . H2 H 0.4318 -0.0137 0.1640 0.074(16) Uiso 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 C1 0.0133(11) 0.0158(11) 0.0139(11) -0.0049(9) 0.0053(9) -0.0004(9) C2 0.0100(11) 0.0121(11) 0.0136(10) -0.0003(8) 0.0050(8) 0.0006(8) C3 0.0110(11) 0.0212(12) 0.0118(10) -0.0050(9) 0.0030(9) -0.0017(9) C4 0.0121(11) 0.0146(11) 0.0161(11) 0.0054(9) 0.0030(9) 0.0027(9) C5 0.0107(11) 0.0116(11) 0.0127(10) 0.0007(8) 0.0029(8) 0.0016(8) C6 0.0104(11) 0.0252(13) 0.0143(11) -0.0054(9) 0.0017(9) 0.0005(9) C7 0.0097(11) 0.0160(11) 0.0106(10) -0.0009(9) 0.0009(8) -0.0009(9) C8 0.0117(11) 0.0115(11) 0.0149(10) 0.0010(8) 0.0046(8) 0.0011(8) C9 0.0096(10) 0.0110(10) 0.0116(10) -0.0002(8) 0.0034(8) -0.0010(8) C10 0.0117(11) 0.0116(11) 0.0154(10) 0.0021(9) 0.0030(8) 0.0005(9) F1 0.0171(7) 0.0306(8) 0.0224(8) -0.0128(6) 0.0102(6) 0.0009(6) F2 0.0157(7) 0.0194(8) 0.0376(9) -0.0012(7) 0.0121(7) -0.0035(6) F3 0.0119(7) 0.0324(9) 0.0202(7) 0.0023(6) 0.0021(6) 0.0074(6) F4 0.0141(7) 0.0216(8) 0.0351(9) 0.0157(7) 0.0028(6) 0.0060(6) F5 0.0170(8) 0.0437(10) 0.0253(8) 0.0013(7) 0.0101(6) 0.0102(7) F6 0.0115(7) 0.0216(8) 0.0321(8) 0.0018(6) -0.0029(6) -0.0029(6) F7 0.0139(8) 0.1058(19) 0.0420(11) -0.0540(12) -0.0014(8) -0.0035(10) F8 0.0142(8) 0.0383(10) 0.0564(12) 0.0269(9) -0.0004(8) 0.0050(7) F9 0.0136(7) 0.0366(10) 0.0322(9) 0.0090(7) 0.0045(6) -0.0070(7) F10 0.0161(7) 0.0171(7) 0.0341(8) 0.0101(6) 0.0115(6) -0.0013(6) F11 0.0146(8) 0.0674(13) 0.0173(8) -0.0088(8) 0.0025(6) -0.0121(8) F12 0.0177(8) 0.0134(7) 0.0568(11) -0.0007(7) 0.0193(8) 0.0026(6) N1 0.0060(8) 0.0132(9) 0.0117(9) -0.0012(7) 0.0032(7) -0.0002(7) N2 0.0058(9) 0.0116(9) 0.0131(9) 0.0012(7) 0.0024(7) -0.0004(7) N3 0.0072(9) 0.0131(9) 0.0109(9) -0.0013(7) 0.0018(7) 0.0001(7) N4 0.0056(8) 0.0106(9) 0.0115(8) 0.0013(7) 0.0017(7) 0.0007(7) O1 0.0116(8) 0.0235(9) 0.0214(9) 0.0033(7) 0.0024(7) -0.0006(7) Rh1 0.00520(9) 0.00956(9) 0.00867(9) 0.00014(6) 0.00189(6) 0.00056(6) _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 C1 F1 1.337(3) . ? C1 F2 1.342(3) . ? C1 F3 1.346(3) . ? C1 C2 1.491(3) . ? C2 N1 1.343(3) . ? C2 C3 1.395(3) . ? C3 C7 1.394(3) 3 ? C3 H3 0.9300 . ? C4 F4 1.337(3) . ? C4 F5 1.342(3) . ? C4 F6 1.347(3) . ? C4 C5 1.493(3) . ? C5 N2 1.348(3) . ? C5 C10 1.387(3) 3 ? C6 F7 1.324(3) . ? C6 F8 1.329(3) . ? C6 F9 1.345(3) . ? C6 C7 1.492(3) . ? C7 N3 1.341(3) . ? C7 C3 1.394(3) 3 ? C8 F10 1.333(3) . ? C8 F11 1.337(3) . ? C8 F12 1.345(3) . ? C8 C9 1.494(3) . ? C9 N4 1.345(3) . ? C9 C10 1.391(3) . ? C10 C5 1.387(3) 3 ? C10 H4 0.9300 . ? N1 N3 1.365(3) 3 ? N1 Rh1 2.0613(19) . ? N2 N4 1.359(2) 3 ? N2 Rh1 2.0600(19) . ? N3 N1 1.365(3) 3 ? N3 Rh1 2.0555(19) . ? N4 N2 1.359(2) 3 ? N4 Rh1 2.0578(18) . ? O1 Rh1 2.2824(17) . ? O1 H1 0.8100(18) . ? O1 H2 0.8049(18) . ? Rh1 Rh1 2.3426(4) 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 F1 C1 F2 107.45(19) . . ? F1 C1 F3 107.39(19) . . ? F2 C1 F3 106.01(19) . . ? F1 C1 C2 111.02(19) . . ? F2 C1 C2 112.1(2) . . ? F3 C1 C2 112.56(19) . . ? N1 C2 C3 110.2(2) . . ? N1 C2 C1 120.8(2) . . ? C3 C2 C1 129.0(2) . . ? C7 C3 C2 103.7(2) 3 . ? C7 C3 H3 128.2 3 . ? C2 C3 H3 128.2 . . ? F4 C4 F5 107.31(19) . . ? F4 C4 F6 107.16(19) . . ? F5 C4 F6 105.94(19) . . ? F4 C4 C5 111.52(19) . . ? F5 C4 C5 112.34(19) . . ? F6 C4 C5 112.21(19) . . ? N2 C5 C10 110.0(2) . 3 ? N2 C5 C4 119.7(2) . . ? C10 C5 C4 130.3(2) 3 . ? F7 C6 F8 108.7(2) . . ? F7 C6 F9 106.9(2) . . ? F8 C6 F9 104.9(2) . . ? F7 C6 C7 111.3(2) . . ? F8 C6 C7 112.6(2) . . ? F9 C6 C7 112.1(2) . . ? N3 C7 C3 110.2(2) . 3 ? N3 C7 C6 120.6(2) . . ? C3 C7 C6 129.1(2) 3 . ? F10 C8 F11 107.35(19) . . ? F10 C8 F12 107.12(18) . . ? F11 C8 F12 105.9(2) . . ? F10 C8 C9 111.40(19) . . ? F11 C8 C9 113.04(19) . . ? F12 C8 C9 111.64(19) . . ? N4 C9 C10 110.0(2) . . ? N4 C9 C8 120.6(2) . . ? C10 C9 C8 129.4(2) . . ? C5 C10 C9 104.1(2) 3 . ? C5 C10 H4 128.0 3 . ? C9 C10 H4 128.0 . . ? C2 N1 N3 107.93(18) . 3 ? C2 N1 Rh1 148.82(16) . . ? N3 N1 Rh1 103.22(13) 3 . ? C5 N2 N4 107.95(18) . 3 ? C5 N2 Rh1 148.09(16) . . ? N4 N2 Rh1 103.95(13) 3 . ? C7 N3 N1 108.01(18) . 3 ? C7 N3 Rh1 147.74(16) . . ? N1 N3 Rh1 104.24(13) 3 . ? C9 N4 N2 108.03(18) . 3 ? C9 N4 Rh1 148.26(16) . . ? N2 N4 Rh1 103.70(13) 3 . ? Rh1 O1 H1 106.22(14) . . ? Rh1 O1 H2 121.99(15) . . ? H1 O1 H2 94.20(19) . . ? N3 Rh1 N4 86.52(7) . . ? N3 Rh1 N2 87.33(7) . . ? N4 Rh1 N2 152.34(7) . . ? N3 Rh1 N1 152.51(7) . . ? N4 Rh1 N1 86.38(7) . . ? N2 Rh1 N1 86.76(7) . . ? N3 Rh1 O1 102.38(7) . . ? N4 Rh1 O1 105.45(7) . . ? N2 Rh1 O1 102.21(7) . . ? N1 Rh1 O1 105.11(7) . . ? N3 Rh1 Rh1 76.10(5) . 3 ? N4 Rh1 Rh1 76.29(5) . 3 ? N2 Rh1 Rh1 76.05(5) . 3 ? N1 Rh1 Rh1 76.42(5) . 3 ? O1 Rh1 Rh1 177.68(5) . 3 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 F9 0.8100(18) 2.6156(18) 3.106(3) 120.51(13) . O1 H2 F6 0.8049(18) 2.4852(16) 2.980(2) 120.97(13) . O1 H2 F2 0.8049(18) 2.4865(15) 3.083(2) 131.91(13) 3_655 O1 H2 F12 0.8049(18) 2.6108(15) 3.038(2) 114.85(13) 3_655 O1 H1 O1 0.8100(18) 2.7511(18) 2.917(3) 93.63(13) 3_655 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.446 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.083 # Attachment '- 2.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 840524' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Di-rhodium(ii)tetrakis (mu-(3,5- bis(trifluoromethyl)pyrazolate))bis(acetonitrile) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H4 F24 N8 Rh2, C4 H6 N2' _chemical_formula_sum 'C24 H10 F24 N10 Rh2' _chemical_formula_weight 1100.24 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' F F 0.0171 0.0103 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.359 _cell_length_b 9.434 _cell_length_c 10.913 _cell_angle_alpha 109.56 _cell_angle_beta 102.23 _cell_angle_gamma 92.58 _cell_volume 880.270 _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9248 _cell_measurement_theta_min 6.02 _cell_measurement_theta_max 54.86 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8884 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Rigaku AFC-12 with Saturn 724+CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25948 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4017 _reflns_number_gt 3798 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0216P)^2^+1.1928P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4017 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 0.558839(14) 0.022150(14) 0.612455(13) 0.01123(5) Uani 1 1 d . . . N5 N 0.67303(18) 0.06943(19) 0.81741(16) 0.0192(3) Uani 1 1 d . . . F2 F 0.96528(13) 0.00496(13) 0.72739(12) 0.0227(2) Uani 1 1 d . . . F5 F 0.70951(13) 0.42988(14) 0.85938(12) 0.0262(3) Uani 1 1 d . . . F4 F 0.89430(12) 0.32262(13) 0.80148(12) 0.0231(2) Uani 1 1 d . . . F1 F 0.88257(16) -0.22392(15) 0.69128(14) 0.0359(3) Uani 1 1 d . . . F6 F 0.86987(15) 0.54880(14) 0.80077(13) 0.0314(3) Uani 1 1 d . . . F3 F 1.06607(15) -0.17715(18) 0.61322(14) 0.0388(3) Uani 1 1 d . . . F9 F 0.20927(15) 0.28249(18) 0.90410(13) 0.0403(4) Uani 1 1 d . . . F11 F 0.60079(14) -0.29614(15) 0.75529(13) 0.0295(3) Uani 1 1 d . . . F7 F 0.43902(15) 0.32381(17) 0.90911(13) 0.0367(3) Uani 1 1 d . . . F10 F 0.40777(17) -0.20796(18) 0.80953(13) 0.0392(3) Uani 1 1 d . . . N4 N 0.43824(17) -0.18829(17) 0.54978(15) 0.0148(3) Uani 1 1 d . . . N3 N 0.36364(17) 0.11093(17) 0.62400(15) 0.0150(3) Uani 1 1 d . . . F8 F 0.34513(18) 0.10288(16) 0.88611(13) 0.0388(3) Uani 1 1 d . . . N2 N 0.62913(16) 0.21387(17) 0.58012(15) 0.0143(3) Uani 1 1 d . . . N1 N 0.70465(17) -0.08570(17) 0.50565(15) 0.0146(3) Uani 1 1 d . . . C5 C 0.7097(2) 0.3511(2) 0.63041(19) 0.0162(3) Uani 1 1 d . . . F12 F 0.40753(18) -0.45007(17) 0.71943(15) 0.0438(4) Uani 1 1 d . . . C10 C 0.3992(2) -0.3096(2) 0.57915(19) 0.0177(4) Uani 1 1 d . . . C11 C 0.7519(2) 0.1108(2) 0.9207(2) 0.0216(4) Uani 1 1 d . . . C2 C 0.8343(2) -0.1419(2) 0.50689(19) 0.0167(3) Uani 1 1 d . . . C8 C 0.2765(2) 0.1826(2) 0.70166(19) 0.0173(4) Uani 1 1 d . . . C6 C 0.6956(2) 0.4172(2) 0.5324(2) 0.0187(4) Uani 1 1 d . . . H6 H 0.7393 0.5112 0.5399 0.022 Uiso 1 1 calc R . . C1 C 0.9362(2) -0.1347(2) 0.6339(2) 0.0193(4) Uani 1 1 d . . . C4 C 0.7946(2) 0.4132(2) 0.7729(2) 0.0181(4) Uani 1 1 d . . . C3 C 0.8514(2) -0.2060(2) 0.3770(2) 0.0193(4) Uani 1 1 d . . . H3 H 0.9299 -0.2534 0.3493 0.023 Uiso 1 1 calc R . . C9 C 0.4539(2) -0.3152(2) 0.7157(2) 0.0217(4) Uani 1 1 d . . . C7 C 0.3186(2) 0.2237(2) 0.8503(2) 0.0215(4) Uani 1 1 d . . . C12 C 0.8584(3) 0.1672(4) 1.0508(2) 0.0420(6) Uani 1 1 d . . . H12A H 0.9562 0.1751 1.0376 0.063 Uiso 1 1 calc R . . H12B H 0.8505 0.0983 1.0975 0.063 Uiso 1 1 calc R . . H12C H 0.8383 0.2652 1.1027 0.063 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 0.01161(7) 0.01030(7) 0.00929(7) 0.00224(5) -0.00032(5) -0.00058(5) N5 0.0206(8) 0.0211(8) 0.0146(8) 0.0064(6) 0.0019(7) -0.0001(6) F2 0.0234(6) 0.0185(5) 0.0200(6) 0.0039(5) -0.0021(5) -0.0021(4) F5 0.0254(6) 0.0287(6) 0.0173(6) -0.0006(5) 0.0045(5) 0.0024(5) F4 0.0189(6) 0.0245(6) 0.0230(6) 0.0079(5) -0.0002(5) 0.0045(5) F1 0.0389(7) 0.0313(7) 0.0346(7) 0.0234(6) -0.0125(6) -0.0141(6) F6 0.0358(7) 0.0184(6) 0.0290(7) 0.0069(5) -0.0094(6) -0.0144(5) F3 0.0238(7) 0.0520(9) 0.0315(7) 0.0056(6) -0.0008(6) 0.0203(6) F9 0.0292(7) 0.0607(10) 0.0204(7) -0.0019(6) 0.0092(5) 0.0127(7) F11 0.0259(6) 0.0356(7) 0.0254(6) 0.0138(6) -0.0019(5) 0.0044(5) F7 0.0320(7) 0.0439(8) 0.0206(6) 0.0014(6) -0.0019(5) -0.0157(6) F10 0.0505(9) 0.0518(9) 0.0215(7) 0.0143(6) 0.0155(6) 0.0243(7) N4 0.0159(7) 0.0132(7) 0.0134(7) 0.0042(6) 0.0008(6) -0.0007(6) N3 0.0153(7) 0.0147(7) 0.0121(7) 0.0030(6) 0.0001(6) -0.0006(6) F8 0.0652(10) 0.0338(7) 0.0196(7) 0.0126(6) 0.0093(6) 0.0076(7) N2 0.0147(7) 0.0130(7) 0.0128(7) 0.0037(6) 0.0003(6) -0.0005(5) N1 0.0144(7) 0.0139(7) 0.0131(7) 0.0036(6) 0.0006(6) 0.0001(5) C5 0.0151(8) 0.0126(8) 0.0169(9) 0.0026(7) 0.0005(7) -0.0001(6) F12 0.0573(10) 0.0356(8) 0.0377(8) 0.0263(7) -0.0073(7) -0.0177(7) C10 0.0187(9) 0.0157(8) 0.0186(9) 0.0067(7) 0.0033(7) 0.0013(7) C11 0.0196(9) 0.0254(10) 0.0196(10) 0.0089(8) 0.0040(8) -0.0019(7) C2 0.0150(8) 0.0144(8) 0.0187(9) 0.0051(7) 0.0016(7) 0.0001(6) C8 0.0182(9) 0.0147(8) 0.0161(9) 0.0028(7) 0.0028(7) -0.0007(7) C6 0.0196(9) 0.0128(8) 0.0223(10) 0.0058(7) 0.0036(7) -0.0024(7) C1 0.0166(9) 0.0167(9) 0.0219(10) 0.0056(7) 0.0007(7) 0.0022(7) C4 0.0173(9) 0.0125(8) 0.0209(10) 0.0039(7) 0.0008(7) -0.0018(7) C3 0.0173(9) 0.0182(9) 0.0216(10) 0.0050(7) 0.0057(7) 0.0036(7) C9 0.0252(10) 0.0180(9) 0.0220(10) 0.0093(8) 0.0030(8) 0.0001(7) C7 0.0199(9) 0.0226(10) 0.0178(10) 0.0018(8) 0.0049(8) 0.0003(7) C12 0.0319(13) 0.0645(18) 0.0195(11) 0.0130(11) -0.0077(10) -0.0147(12) _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 N3 2.0542(15) . ? Rh1 N4 2.0603(15) . ? Rh1 N2 2.0609(15) . ? Rh1 N1 2.0642(15) . ? Rh1 N5 2.1494(16) . ? Rh1 Rh1 2.3533(3) 2_656 ? N5 C11 1.138(3) . ? F2 C1 1.342(2) . ? F5 C4 1.334(2) . ? F4 C4 1.351(2) . ? F1 C1 1.342(2) . ? F6 C4 1.339(2) . ? F3 C1 1.337(2) . ? F9 C7 1.336(2) . ? F11 C9 1.336(2) . ? F7 C7 1.329(2) . ? F10 C9 1.338(2) . ? N4 C10 1.343(2) . ? N4 N2 1.358(2) 2_656 ? N3 C8 1.342(2) . ? N3 N1 1.358(2) 2_656 ? F8 C7 1.340(2) . ? N2 C5 1.344(2) . ? N2 N4 1.358(2) 2_656 ? N1 C2 1.345(2) . ? N1 N3 1.358(2) 2_656 ? C5 C6 1.395(3) . ? C5 C4 1.489(3) . ? F12 C9 1.342(2) . ? C10 C6 1.390(3) 2_656 ? C10 C9 1.489(3) . ? C11 C12 1.462(3) . ? C2 C3 1.389(3) . ? C2 C1 1.485(3) . ? C8 C3 1.390(3) 2_656 ? C8 C7 1.494(3) . ? C6 C10 1.390(3) 2_656 ? C6 H6 0.9300 . ? C3 C8 1.390(3) 2_656 ? C3 H3 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh1 N4 86.84(6) . . ? N3 Rh1 N2 86.47(6) . . ? N4 Rh1 N2 152.05(6) . . ? N3 Rh1 N1 152.03(6) . . ? N4 Rh1 N1 86.52(6) . . ? N2 Rh1 N1 86.79(6) . . ? N3 Rh1 N5 104.56(6) . . ? N4 Rh1 N5 106.05(6) . . ? N2 Rh1 N5 101.90(6) . . ? N1 Rh1 N5 103.39(6) . . ? N3 Rh1 Rh1 76.29(4) . 2_656 ? N4 Rh1 Rh1 76.18(4) . 2_656 ? N2 Rh1 Rh1 75.86(4) . 2_656 ? N1 Rh1 Rh1 75.74(4) . 2_656 ? N5 Rh1 Rh1 177.60(4) . 2_656 ? C11 N5 Rh1 167.22(16) . . ? C10 N4 N2 108.16(15) . 2_656 ? C10 N4 Rh1 148.10(13) . . ? N2 N4 Rh1 103.72(10) 2_656 . ? C8 N3 N1 108.22(15) . 2_656 ? C8 N3 Rh1 147.86(13) . . ? N1 N3 Rh1 103.91(11) 2_656 . ? C5 N2 N4 107.94(14) . 2_656 ? C5 N2 Rh1 147.82(13) . . ? N4 N2 Rh1 104.23(10) 2_656 . ? C2 N1 N3 107.70(15) . 2_656 ? C2 N1 Rh1 148.25(13) . . ? N3 N1 Rh1 104.05(11) 2_656 . ? N2 C5 C6 110.04(16) . . ? N2 C5 C4 120.72(16) . . ? C6 C5 C4 129.22(17) . . ? N4 C10 C6 110.09(16) . 2_656 ? N4 C10 C9 121.12(17) . . ? C6 C10 C9 128.78(17) 2_656 . ? N5 C11 C12 177.2(2) . . ? N1 C2 C3 110.26(16) . . ? N1 C2 C1 121.56(17) . . ? C3 C2 C1 128.17(17) . . ? N3 C8 C3 110.08(16) . 2_656 ? N3 C8 C7 121.59(17) . . ? C3 C8 C7 128.31(18) 2_656 . ? C10 C6 C5 103.76(16) 2_656 . ? C10 C6 H6 128.1 2_656 . ? C5 C6 H6 128.1 . . ? F3 C1 F1 107.58(16) . . ? F3 C1 F2 106.40(16) . . ? F1 C1 F2 105.55(16) . . ? F3 C1 C2 111.03(17) . . ? F1 C1 C2 112.65(16) . . ? F2 C1 C2 113.21(15) . . ? F5 C4 F6 107.67(16) . . ? F5 C4 F4 106.15(15) . . ? F6 C4 F4 106.75(15) . . ? F5 C4 C5 113.07(15) . . ? F6 C4 C5 110.81(16) . . ? F4 C4 C5 112.03(15) . . ? C2 C3 C8 103.74(16) . 2_656 ? C2 C3 H3 128.1 . . ? C8 C3 H3 128.1 2_656 . ? F11 C9 F10 106.07(17) . . ? F11 C9 F12 106.72(16) . . ? F10 C9 F12 107.60(17) . . ? F11 C9 C10 112.92(16) . . ? F10 C9 C10 112.61(16) . . ? F12 C9 C10 110.57(17) . . ? F7 C7 F9 107.84(17) . . ? F7 C7 F8 106.45(17) . . ? F9 C7 F8 106.56(17) . . ? F7 C7 C8 113.05(16) . . ? F9 C7 C8 110.43(17) . . ? F8 C7 C8 112.18(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.563 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.069 # Attachment '- 4.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 840525' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ;Dirhodium(ii) tetrakis(3-(trifluoromethyl), 5-(tert- butyl)pyrazolate)) ; _chemical_formula_moiety 'C32 H40 F12 N8 Rh2' _chemical_formula_sum 'C32 H40 F12 N8 Rh2' _exptl_crystal_recrystallization_method 'slow evaporation' _chemical_melting_point . _exptl_crystal_description block _exptl_crystal_colour green _chemical_formula_weight 970.54 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' F F 0.0171 0.0103 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_int_tables_number 88 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 19.3600(10) _cell_length_b 19.3600(10) _cell_length_c 10.1730(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3812.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5592 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9272 _exptl_absorpt_correction_T_max 0.9626 _exptl_absorpt_process_details 'Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9981 _diffrn_reflns_av_R_equivalents 0.0862 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2188 _reflns_number_gt 1260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _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^)+(0.0480P)^2^+18.2738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2188 _refine_ls_number_parameters 151 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 C2 C 0.8556(3) 0.3399(3) 0.5250(6) 0.0518(16) Uani 1 1 d . A . C3 C 0.8203(3) 0.3616(3) 0.6339(8) 0.0585(17) Uani 1 1 d . . . H3 H 0.7797 0.3873 0.6357 0.070 Uiso 1 1 calc R . . C4 C 0.9124(3) 0.1073(3) 0.5088(7) 0.0526(17) Uani 1 1 d . . . C5 C 0.9074(4) 0.0935(4) 0.3635(7) 0.065(2) Uani 1 1 d . . . C6 C 0.8331(4) 0.0757(5) 0.3263(9) 0.109(4) Uani 1 1 d . . . H6A H 0.8304 0.0676 0.2333 0.163 Uiso 1 1 calc R . . H6B H 0.8033 0.1134 0.3495 0.163 Uiso 1 1 calc R . . H6C H 0.8189 0.0349 0.3725 0.163 Uiso 1 1 calc R . . C7 C 0.9297(6) 0.1556(5) 0.2844(8) 0.113(4) Uani 1 1 d . . . H7A H 0.9258 0.1455 0.1924 0.169 Uiso 1 1 calc R . . H7B H 0.9768 0.1667 0.3049 0.169 Uiso 1 1 calc R . . H7C H 0.9007 0.1943 0.3057 0.169 Uiso 1 1 calc R . . C8 C 0.9536(4) 0.0330(5) 0.3271(9) 0.090(3) Uani 1 1 d . . . H8A H 0.9506 0.0247 0.2342 0.135 Uiso 1 1 calc R . . H8B H 0.9390 -0.0075 0.3739 0.135 Uiso 1 1 calc R . . H8C H 1.0006 0.0437 0.3500 0.135 Uiso 1 1 calc R . . N1 N 0.9113(3) 0.3038(3) 0.5603(5) 0.0462(12) Uani 1 1 d . . . N2 N 0.9475(3) 0.1623(3) 0.5552(5) 0.0463(13) Uani 1 1 d . . . C1 C 0.8364(4) 0.3506(4) 0.3848(8) 0.069(2) Uani 1 1 d D . . F1 F 0.8017(4) 0.3006(3) 0.3325(5) 0.091(2) Uani 0.851(11) 1 d PDU A 1 F2 F 0.7996(4) 0.4081(3) 0.3697(7) 0.105(3) Uani 0.851(11) 1 d PDU A 1 F3 F 0.8920(3) 0.3601(5) 0.3103(6) 0.111(3) Uani 0.851(11) 1 d PDU A 1 F1A F 0.7672(8) 0.3486(19) 0.381(4) 0.101(13) Uani 0.149(11) 1 d PDU A 2 F2A F 0.8558(19) 0.2979(12) 0.310(3) 0.094(12) Uani 0.149(11) 1 d PDU A 2 F3A F 0.8543(17) 0.4061(10) 0.324(3) 0.066(10) Uani 0.149(11) 1 d PDU A 2 Rh1 Rh 1.0000 0.2500 0.51154(6) 0.0445(3) Uani 1 2 d S . . 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 C2 0.049(4) 0.058(4) 0.048(4) 0.002(3) -0.007(3) 0.002(3) C3 0.044(4) 0.052(4) 0.079(5) -0.005(4) 0.001(4) 0.000(3) C4 0.046(4) 0.052(4) 0.060(5) -0.010(3) -0.010(3) 0.007(3) C5 0.075(5) 0.067(5) 0.054(4) -0.022(4) -0.021(4) 0.010(4) C6 0.075(6) 0.157(9) 0.095(7) -0.064(6) -0.041(5) 0.036(6) C7 0.191(11) 0.108(8) 0.039(5) -0.019(5) -0.018(6) 0.017(7) C8 0.083(6) 0.106(7) 0.082(6) -0.048(5) -0.013(5) 0.024(5) N1 0.054(3) 0.056(3) 0.029(3) -0.005(2) -0.002(2) 0.002(3) N2 0.051(3) 0.051(3) 0.036(3) -0.005(2) -0.007(2) -0.001(3) C1 0.058(5) 0.083(5) 0.067(5) 0.002(5) -0.021(4) 0.009(4) F1 0.130(5) 0.078(4) 0.066(4) 0.004(3) -0.035(3) -0.033(4) F2 0.127(5) 0.078(4) 0.111(5) 0.003(3) -0.054(4) 0.026(4) F3 0.092(4) 0.180(7) 0.061(3) 0.041(4) -0.019(3) -0.009(4) F1A 0.092(15) 0.115(16) 0.095(15) 0.007(10) -0.002(10) 0.003(10) F2A 0.106(15) 0.095(15) 0.079(14) -0.004(10) -0.011(10) 0.010(10) F3A 0.082(13) 0.057(12) 0.060(12) 0.005(9) 0.003(9) -0.012(9) Rh1 0.0547(5) 0.0539(5) 0.0250(3) 0.000 0.000 0.0037(4) _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 C2 N1 1.335(8) . ? C2 C3 1.368(9) . ? C2 C1 1.488(10) . ? C3 C4 1.386(10) 15_666 ? C3 H3 0.9300 . ? C4 N2 1.349(8) . ? C4 C3 1.386(10) 16_646 ? C4 C5 1.505(9) . ? C5 C7 1.511(12) . ? C5 C8 1.520(10) . ? C5 C6 1.526(10) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 N2 1.369(6) 15_666 ? N1 Rh1 2.068(5) . ? N2 N1 1.369(6) 16_646 ? N2 Rh1 2.028(5) . ? C1 F3A 1.289(13) . ? C1 F1 1.293(8) . ? C1 F3 1.330(8) . ? C1 F2A 1.325(14) . ? C1 F2 1.332(8) . ? C1 F1A 1.342(14) . ? Rh1 N2 2.028(5) 2_755 ? Rh1 N1 2.068(5) 2_755 ? Rh1 Rh1 2.3085(12) 15_666 ? 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 N1 C2 C3 110.3(6) . . ? N1 C2 C1 122.2(6) . . ? C3 C2 C1 127.5(7) . . ? C2 C3 C4 106.1(6) . 15_666 ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 15_666 . ? N2 C4 C3 107.6(6) . 16_646 ? N2 C4 C5 121.1(7) . . ? C3 C4 C5 131.3(7) 16_646 . ? C4 C5 C7 111.3(6) . . ? C4 C5 C8 109.7(6) . . ? C7 C5 C8 108.3(7) . . ? C4 C5 C6 110.2(7) . . ? C7 C5 C6 108.5(8) . . ? C8 C5 C6 108.7(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 N1 N2 106.9(5) . 15_666 ? C2 N1 Rh1 150.5(5) . . ? N2 N1 Rh1 102.7(4) 15_666 . ? C4 N2 N1 109.2(5) . 16_646 ? C4 N2 Rh1 146.8(5) . . ? N1 N2 Rh1 103.9(4) 16_646 . ? F3A C1 F1 124.5(15) . . ? F3A C1 F3 52.6(13) . . ? F1 C1 F3 106.9(7) . . ? F3A C1 F2A 106.9(13) . . ? F1 C1 F2A 48.3(14) . . ? F3 C1 F2A 63.4(14) . . ? F3A C1 F2 52.4(14) . . ? F1 C1 F2 107.5(6) . . ? F3 C1 F2 104.6(7) . . ? F2A C1 F2 136.8(16) . . ? F3A C1 F1A 106.0(13) . . ? F1 C1 F1A 56.4(15) . . ? F3 C1 F1A 142.7(17) . . ? F2A C1 F1A 104.0(13) . . ? F2 C1 F1A 59.0(14) . . ? F3A C1 C2 120.7(14) . . ? F1 C1 C2 114.8(6) . . ? F3 C1 C2 111.3(6) . . ? F2A C1 C2 111.8(16) . . ? F2 C1 C2 111.1(6) . . ? F1A C1 C2 106.0(16) . . ? N2 Rh1 N2 154.7(3) 2_755 . ? N2 Rh1 N1 86.7(2) 2_755 . ? N2 Rh1 N1 87.3(2) . . ? N2 Rh1 N1 87.3(2) 2_755 2_755 ? N2 Rh1 N1 86.7(2) . 2_755 ? N1 Rh1 N1 152.2(3) . 2_755 ? N2 Rh1 Rh1 77.35(14) 2_755 15_666 ? N2 Rh1 Rh1 77.35(14) . 15_666 ? N1 Rh1 Rh1 76.12(14) . 15_666 ? N1 Rh1 Rh1 76.12(14) 2_755 15_666 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.067 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.180