Supplementary Material (ESI) for CrystEngComm This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Satoshi Takamizawa' 'Kenichi Kojima' 'Ei-ichi Nakata' 'Teruo Saito' _publ_contact_author_name 'Dr Satoshi Takamizawa' _publ_contact_author_address ; Graduate School of Integrated Science Yokohama City University Kanazawa-ku Yokohama Kanagawa 236-0027 JAPAN ; _publ_contact_author_email staka@yokohama-cu.ac.jp _publ_contact_author_phone +81-45-787-2187 _publ_contact_author_fax +81-45-787-2187 _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Structural determination of physisorbed sites for CO2 and Ar gases inside an organometallic framework ; data_306131 _database_code_depnum_ccdc_archive 'CCDC 221325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Rhodium(II) benzoate pyrazine' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.77 H24 N2 O9.54 Rh2' _chemical_formula_weight 804.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.572(2) _cell_length_b 10.424(2) _cell_length_c 10.977(2) _cell_angle_alpha 71.270(5) _cell_angle_beta 66.062(4) _cell_angle_gamma 63.155(4) _cell_volume 880.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 401 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7689 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_special_details ; Experimental was carried out in high pressure (ca.3.5MPa) of CO2 gas at room tempearature. ; _diffrn_ambient_temperature 298 _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 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3305 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 20.81 _reflns_number_total 1830 _reflns_number_gt 1208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+4.4565P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1830 _refine_ls_number_parameters 215 _refine_ls_number_restraints 330 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.073 _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 0.539(2) 0.1368(19) 0.2502(19) 0.050(2) Uani 1 1 d U . . C2 C 0.5634(18) 0.2106(17) 0.1091(15) 0.061(3) Uani 1 1 d DU . . C3 C 0.4750(17) 0.2085(16) 0.0361(15) 0.069(3) Uani 1 1 d DU . . H3 H 0.4004 0.1616 0.0771 0.082 Uiso 1 1 calc R . . C4 C 0.4989(19) 0.2770(18) -0.0991(16) 0.075(3) Uani 1 1 d DU . . H4 H 0.4397 0.2760 -0.1480 0.090 Uiso 1 1 calc R . . C5 C 0.611(2) 0.347(2) -0.1607(16) 0.079(3) Uani 1 1 d DU . . H5 H 0.6283 0.3908 -0.2511 0.095 Uiso 1 1 calc R . . C6 C 0.697(2) 0.351(2) -0.0873(16) 0.075(3) Uani 1 1 d DU . . H6 H 0.7686 0.4013 -0.1271 0.090 Uiso 1 1 calc R . . C7 C 0.6771(19) 0.2785(18) 0.0470(15) 0.069(3) Uani 1 1 d DU . . H7 H 0.7397 0.2760 0.0947 0.082 Uiso 1 1 calc R . . C8 C 0.3318(18) 0.2520(17) 0.5759(17) 0.042(3) Uani 1 1 d U . . C9 C 0.2319(14) 0.4027(14) 0.6154(15) 0.045(2) Uani 1 1 d DU . . C10 C 0.0638(14) 0.4625(14) 0.6408(14) 0.051(3) Uani 1 1 d DU . . H10 H 0.0108 0.4111 0.6327 0.062 Uiso 1 1 calc R . . C11 C -0.0258(15) 0.5980(14) 0.6779(16) 0.058(3) Uani 1 1 d DU . . H11 H -0.1391 0.6390 0.6938 0.069 Uiso 1 1 calc R . . C12 C 0.0529(15) 0.6729(15) 0.6916(18) 0.059(3) Uani 1 1 d DU . . H12 H -0.0077 0.7632 0.7197 0.070 Uiso 1 1 calc R . . C13 C 0.2204(15) 0.6143(15) 0.6637(18) 0.054(3) Uani 1 1 d DU . . H13 H 0.2738 0.6668 0.6694 0.065 Uiso 1 1 calc R . . C14 C 0.3101(15) 0.4787(14) 0.6276(17) 0.049(3) Uani 1 1 d DU . . H14 H 0.4234 0.4382 0.6114 0.059 Uiso 1 1 calc R . . C15 C 0.0025(17) 0.0542(16) 0.5923(16) 0.036(3) Uani 1 1 d U . . H15 H 0.0005 0.0947 0.6573 0.044 Uiso 1 1 calc R . . C16 C 0.1428(18) -0.0619(17) 0.4119(17) 0.037(3) Uani 1 1 d U . . H16 H 0.2410 -0.1045 0.3477 0.044 Uiso 1 1 calc R . . C1S C 0.0000 0.5000 0.0000 0.22(2) Uani 0.77(5) 2 d SPU . . N1 N 0.1449(14) -0.0099(14) 0.5052(14) 0.035(3) Uani 1 1 d U . . O1 O 0.4173(12) 0.0972(12) 0.3061(11) 0.047(2) Uani 1 1 d U . . O2 O 0.6469(12) 0.1115(11) 0.3033(11) 0.044(2) Uani 1 1 d U . . O3 O 0.2545(12) 0.1885(11) 0.5631(11) 0.041(2) Uani 1 1 d U . . O4 O 0.5145(11) -0.2006(11) 0.4396(11) 0.039(3) Uani 1 1 d U . . O1S O -0.003(5) 0.589(4) 0.012(4) 0.22(2) Uani 0.77(5) 1 d PU . . Rh1 Rh 0.37726(15) -0.00617(15) 0.50248(16) 0.0349(6) Uani 1 1 d U . . 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 0.048(3) 0.053(3) 0.054(3) -0.007(3) -0.019(3) -0.021(3) C2 0.060(3) 0.063(3) 0.062(3) -0.009(3) -0.021(3) -0.024(3) C3 0.068(4) 0.070(4) 0.067(4) -0.008(3) -0.022(3) -0.026(3) C4 0.075(4) 0.076(4) 0.072(4) -0.009(3) -0.024(3) -0.027(3) C5 0.078(4) 0.078(4) 0.074(4) -0.008(3) -0.022(3) -0.027(3) C6 0.075(4) 0.074(4) 0.072(4) -0.009(3) -0.022(3) -0.028(3) C7 0.068(4) 0.068(4) 0.067(4) -0.009(3) -0.021(3) -0.025(3) C8 0.040(3) 0.043(4) 0.046(4) -0.007(3) -0.016(3) -0.016(3) C9 0.046(3) 0.046(3) 0.048(3) -0.009(3) -0.016(3) -0.018(3) C10 0.051(3) 0.050(4) 0.052(4) -0.008(3) -0.016(3) -0.017(3) C11 0.056(4) 0.054(4) 0.055(4) -0.007(3) -0.017(3) -0.017(3) C12 0.060(4) 0.054(4) 0.056(4) -0.008(3) -0.016(3) -0.018(3) C13 0.057(4) 0.051(4) 0.055(4) -0.009(3) -0.016(3) -0.020(3) C14 0.051(3) 0.048(4) 0.051(4) -0.009(3) -0.017(3) -0.019(3) C15 0.036(4) 0.037(4) 0.039(4) -0.007(3) -0.013(3) -0.015(3) C16 0.034(4) 0.037(4) 0.039(4) -0.009(3) -0.010(3) -0.013(3) C1S 0.22(2) 0.22(2) 0.22(2) -0.037(6) -0.068(8) -0.082(9) N1 0.033(4) 0.037(4) 0.037(4) -0.007(3) -0.012(3) -0.015(3) O1 0.043(3) 0.052(4) 0.051(4) -0.004(3) -0.020(3) -0.019(3) O2 0.043(3) 0.048(4) 0.050(4) -0.006(3) -0.017(3) -0.022(3) O3 0.038(3) 0.042(4) 0.048(4) -0.008(3) -0.016(3) -0.015(3) O4 0.030(4) 0.040(4) 0.049(5) -0.009(4) -0.015(3) -0.013(3) O1S 0.22(2) 0.22(2) 0.22(2) -0.037(6) -0.068(8) -0.083(9) Rh1 0.0217(7) 0.0346(8) 0.0549(10) -0.0060(6) -0.0200(6) -0.0097(5) _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 O1 1.264(18) . ? C1 O2 1.271(18) . ? C1 C2 1.47(2) . ? C2 C7 1.391(13) . ? C2 C3 1.391(13) . ? C3 C4 1.399(13) . ? C4 C5 1.394(13) . ? C5 C6 1.388(13) . ? C6 C7 1.402(13) . ? C8 O3 1.262(17) . ? C8 O4 1.274(16) 2_656 ? C8 C9 1.522(19) . ? C9 C14 1.375(12) . ? C9 C10 1.377(12) . ? C10 C11 1.375(12) . ? C11 C12 1.377(12) . ? C12 C13 1.370(12) . ? C13 C14 1.371(12) . ? C15 N1 1.322(17) . ? C15 C16 1.37(2) 2_556 ? C16 N1 1.314(18) . ? C16 C15 1.37(2) 2_556 ? C1S O1S 0.96(4) 2_565 ? C1S O1S 0.96(4) . ? N1 Rh1 2.230(12) . ? O1 Rh1 2.041(11) . ? O2 Rh1 2.033(11) 2_656 ? O3 Rh1 2.005(10) . ? O4 C8 1.274(16) 2_656 ? O4 Rh1 2.017(10) . ? Rh1 O2 2.033(11) 2_656 ? Rh1 Rh1 2.389(2) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 125.7(17) . . ? O1 C1 C2 116.9(15) . . ? O2 C1 C2 117.3(14) . . ? C7 C2 C3 120.1(9) . . ? C7 C2 C1 120.5(12) . . ? C3 C2 C1 119.3(12) . . ? C2 C3 C4 119.7(9) . . ? C5 C4 C3 120.2(9) . . ? C6 C5 C4 120.0(9) . . ? C5 C6 C7 119.8(9) . . ? C2 C7 C6 120.1(9) . . ? O3 C8 O4 125.9(14) . 2_656 ? O3 C8 C9 117.0(13) . . ? O4 C8 C9 117.1(12) 2_656 . ? C14 C9 C10 119.9(8) . . ? C14 C9 C8 119.6(10) . . ? C10 C9 C8 120.5(10) . . ? C11 C10 C9 120.1(9) . . ? C10 C11 C12 119.7(9) . . ? C13 C12 C11 119.9(9) . . ? C12 C13 C14 120.5(9) . . ? C13 C14 C9 119.8(9) . . ? N1 C15 C16 121.0(14) . 2_556 ? N1 C16 C15 121.0(14) . 2_556 ? O1S C1S O1S 180(5) 2_565 . ? C16 N1 C15 117.9(13) . . ? C16 N1 Rh1 121.1(10) . . ? C15 N1 Rh1 120.7(11) . . ? C1 O1 Rh1 118.7(11) . . ? C1 O2 Rh1 119.2(11) . 2_656 ? C8 O3 Rh1 119.8(10) . . ? C8 O4 Rh1 117.8(9) 2_656 . ? O3 Rh1 O4 176.3(4) . . ? O3 Rh1 O2 91.3(4) . 2_656 ? O4 Rh1 O2 89.1(4) . 2_656 ? O3 Rh1 O1 89.5(4) . . ? O4 Rh1 O1 90.0(4) . . ? O2 Rh1 O1 176.1(4) 2_656 . ? O3 Rh1 N1 90.8(4) . . ? O4 Rh1 N1 92.8(4) . . ? O2 Rh1 N1 93.0(5) 2_656 . ? O1 Rh1 N1 90.8(5) . . ? O3 Rh1 Rh1 87.6(3) . 2_656 ? O4 Rh1 Rh1 88.7(3) . 2_656 ? O2 Rh1 Rh1 88.0(3) 2_656 2_656 ? O1 Rh1 Rh1 88.2(3) . 2_656 ? N1 Rh1 Rh1 178.2(4) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 169.4(15) . . . . ? O2 C1 C2 C7 -14(2) . . . . ? O1 C1 C2 C3 -13(2) . . . . ? O2 C1 C2 C3 164.0(13) . . . . ? C7 C2 C3 C4 -1.1(16) . . . . ? C1 C2 C3 C4 -179.2(15) . . . . ? C2 C3 C4 C5 0.2(16) . . . . ? C3 C4 C5 C6 -1(3) . . . . ? C4 C5 C6 C7 3(3) . . . . ? C3 C2 C7 C6 3(2) . . . . ? C1 C2 C7 C6 -179.0(17) . . . . ? C5 C6 C7 C2 -4(3) . . . . ? O3 C8 C9 C14 -178.4(15) . . . . ? O4 C8 C9 C14 2(2) 2_656 . . . ? O3 C8 C9 C10 3(2) . . . . ? O4 C8 C9 C10 -176.7(13) 2_656 . . . ? C14 C9 C10 C11 0.2(16) . . . . ? C8 C9 C10 C11 179.2(15) . . . . ? C9 C10 C11 C12 -0.9(16) . . . . ? C10 C11 C12 C13 2(2) . . . . ? C11 C12 C13 C14 -3(3) . . . . ? C12 C13 C14 C9 2(3) . . . . ? C10 C9 C14 C13 -1(2) . . . . ? C8 C9 C14 C13 -179.7(15) . . . . ? C15 C16 N1 C15 -2(3) 2_556 . . . ? C15 C16 N1 Rh1 -175.1(11) 2_556 . . . ? C16 C15 N1 C16 2(3) 2_556 . . . ? C16 C15 N1 Rh1 175.1(11) 2_556 . . . ? O2 C1 O1 Rh1 4(2) . . . . ? C2 C1 O1 Rh1 180.0(11) . . . . ? O1 C1 O2 Rh1 -3(2) . . . 2_656 ? C2 C1 O2 Rh1 -178.9(11) . . . 2_656 ? O4 C8 O3 Rh1 -4(2) 2_656 . . . ? C9 C8 O3 Rh1 177.0(10) . . . . ? C8 O3 Rh1 O4 -6(8) . . . . ? C8 O3 Rh1 O2 89.3(13) . . . 2_656 ? C8 O3 Rh1 O1 -86.9(13) . . . . ? C8 O3 Rh1 N1 -177.7(13) . . . . ? C8 O3 Rh1 Rh1 1.4(12) . . . 2_656 ? C8 O4 Rh1 O3 9(8) 2_656 . . . ? C8 O4 Rh1 O2 -85.7(12) 2_656 . . 2_656 ? C8 O4 Rh1 O1 90.6(12) 2_656 . . . ? C8 O4 Rh1 N1 -178.6(12) 2_656 . . . ? C8 O4 Rh1 Rh1 2.4(11) 2_656 . . 2_656 ? C1 O1 Rh1 O3 85.1(12) . . . . ? C1 O1 Rh1 O4 -91.3(12) . . . . ? C1 O1 Rh1 O2 -16(7) . . . 2_656 ? C1 O1 Rh1 N1 175.9(12) . . . . ? C1 O1 Rh1 Rh1 -2.6(12) . . . 2_656 ? C16 N1 Rh1 O3 141.6(12) . . . . ? C15 N1 Rh1 O3 -31.2(12) . . . . ? C16 N1 Rh1 O4 -37.9(13) . . . . ? C15 N1 Rh1 O4 149.4(12) . . . . ? C16 N1 Rh1 O2 -127.1(12) . . . 2_656 ? C15 N1 Rh1 O2 60.2(12) . . . 2_656 ? C16 N1 Rh1 O1 52.1(13) . . . . ? C15 N1 Rh1 O1 -120.6(12) . . . . ? C16 N1 Rh1 Rh1 109(12) . . . 2_656 ? C15 N1 Rh1 Rh1 -64(13) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.353 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.174 #===END data_306201 _database_code_depnum_ccdc_archive 'CCDC 221326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'rhodium benzoate pyrazine' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Ar1.12 N2 O8 Rh2' _chemical_formula_weight 814.70 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' Ar Ar 0.1743 0.2003 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.588(2) _cell_length_b 10.322(3) _cell_length_c 10.861(3) _cell_angle_alpha 72.139(5) _cell_angle_beta 64.783(5) _cell_angle_gamma 62.722(5) _cell_volume 856.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7667 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_special_details ; Experiment was carried out in high pressure (ca.8MPa) of Ar gas at room temperature. ; _diffrn_ambient_temperature 298 _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 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3229 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 20.80 _reflns_number_total 1778 _reflns_number_gt 1138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1778 _refine_ls_number_parameters 209 _refine_ls_number_restraints 319 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2139 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.045 _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 Ar1S Ar 0.649(3) 0.172(2) 0.4580(19) 0.214(12) Uani 0.56(2) 1 d PU . . C1 C 0.827(2) 0.2626(18) 0.0766(16) 0.0477(14) Uani 1 1 d U . . C2 C 0.7302(15) 0.4124(14) 0.1175(16) 0.0487(14) Uani 1 1 d DU . . C3 C 0.8069(15) 0.4856(14) 0.1368(16) 0.0494(15) Uani 1 1 d DU . . H3 H 0.9209 0.4425 0.1211 0.059 Uiso 1 1 calc R . . C4 C 0.7154(15) 0.6226(15) 0.1792(16) 0.0501(15) Uani 1 1 d DU . . H4 H 0.7680 0.6739 0.1884 0.060 Uiso 1 1 calc R . . C5 C 0.5453(15) 0.6829(15) 0.2079(16) 0.0505(15) Uani 1 1 d DU . . H5 H 0.4823 0.7729 0.2414 0.061 Uiso 1 1 calc R . . C6 C 0.4687(15) 0.6116(14) 0.1876(16) 0.0502(15) Uani 1 1 d DU . . H6 H 0.3546 0.6548 0.2036 0.060 Uiso 1 1 calc R . . C7 C 0.5604(15) 0.4761(14) 0.1436(16) 0.0494(15) Uani 1 1 d DU . . H7 H 0.5077 0.4269 0.1313 0.059 Uiso 1 1 calc R . . C8 C 0.944(2) -0.125(2) 0.256(2) 0.070(2) Uani 1 1 d U . . C9 C 0.920(2) -0.2044(18) 0.4005(15) 0.0717(19) Uani 1 1 d DU . . C10 C 1.0185(18) -0.2171(16) 0.4678(15) 0.073(2) Uani 1 1 d DU . . H10 H 1.1007 -0.1780 0.4248 0.087 Uiso 1 1 calc R . . C11 C 0.9943(19) -0.2886(18) 0.5998(15) 0.073(2) Uani 1 1 d DU . . H11 H 1.0569 -0.2943 0.6486 0.088 Uiso 1 1 calc R . . C12 C 0.880(2) -0.3506(19) 0.6591(15) 0.073(2) Uani 1 1 d DU . . H12 H 0.8733 -0.4077 0.7448 0.088 Uiso 1 1 calc R . . C13 C 0.776(2) -0.3313(19) 0.5962(15) 0.073(2) Uani 1 1 d DU . . H13 H 0.6899 -0.3653 0.6421 0.088 Uiso 1 1 calc R . . C14 C 0.799(2) -0.2605(19) 0.4629(16) 0.073(2) Uani 1 1 d DU . . H14 H 0.7328 -0.2514 0.4163 0.087 Uiso 1 1 calc R . . C15 C 1.5038(17) -0.0653(16) -0.0883(15) 0.039(2) Uani 1 1 d DU . . H15 H 1.5097 -0.1151 -0.1497 0.047 Uiso 1 1 calc R . . C16 C 1.3527(19) 0.0677(16) 0.0881(15) 0.039(2) Uani 1 1 d DU . . H16 H 1.2513 0.1133 0.1531 0.047 Uiso 1 1 calc R . . N1 N 1.3575(15) 0.0061(13) -0.0034(12) 0.039(2) Uani 1 1 d DU . . O1 O 0.9826(12) 0.2062(10) 0.0593(10) 0.0469(15) Uani 1 1 d DU . . O2 O 0.7515(13) 0.1992(11) 0.0596(10) 0.0474(15) Uani 1 1 d U . . O3 O 1.0692(16) -0.0916(13) 0.1995(11) 0.069(2) Uani 1 1 d DU . . O4 O 1.1622(12) 0.0981(10) -0.2010(9) 0.042(3) Uani 1 1 d DU . . Rh1 Rh 1.12324(15) 0.00361(14) -0.00175(14) 0.0374(6) Uani 1 1 d DU . . 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 Ar1S 0.214(12) 0.214(12) 0.213(12) -0.030(2) -0.072(4) -0.081(5) C1 0.0475(15) 0.0480(15) 0.0480(15) -0.0067(7) -0.0164(8) -0.0182(8) C2 0.0487(15) 0.0488(15) 0.0488(15) -0.0067(6) -0.0166(7) -0.0186(8) C3 0.0495(15) 0.0493(15) 0.0493(15) -0.0068(7) -0.0166(8) -0.0187(8) C4 0.0501(16) 0.0498(16) 0.0499(16) -0.0067(7) -0.0167(8) -0.0189(8) C5 0.0504(16) 0.0500(16) 0.0501(16) -0.0067(7) -0.0167(8) -0.0188(8) C6 0.0500(16) 0.0499(16) 0.0500(16) -0.0066(7) -0.0167(8) -0.0187(8) C7 0.0493(15) 0.0494(15) 0.0494(15) -0.0067(7) -0.0167(8) -0.0187(8) C8 0.070(2) 0.071(2) 0.071(2) -0.0098(8) -0.0241(9) -0.0271(10) C9 0.072(2) 0.072(2) 0.072(2) -0.0098(7) -0.0243(9) -0.0274(9) C10 0.072(2) 0.073(2) 0.072(2) -0.0098(7) -0.0245(9) -0.0274(10) C11 0.073(2) 0.073(2) 0.073(2) -0.0098(8) -0.0246(9) -0.0275(10) C12 0.073(2) 0.073(2) 0.073(2) -0.0098(8) -0.0245(9) -0.0277(10) C13 0.073(2) 0.073(2) 0.073(2) -0.0098(8) -0.0244(9) -0.0279(10) C14 0.073(2) 0.073(2) 0.072(2) -0.0098(7) -0.0244(9) -0.0277(10) C15 0.039(2) 0.039(2) 0.039(2) -0.0054(9) -0.0132(10) -0.0149(11) C16 0.039(2) 0.039(2) 0.039(2) -0.0055(9) -0.0132(10) -0.0148(11) N1 0.039(2) 0.039(2) 0.039(2) -0.0055(8) -0.0132(10) -0.0149(10) O1 0.0467(16) 0.0475(16) 0.0477(16) -0.0069(8) -0.0164(9) -0.0183(9) O2 0.0472(16) 0.0477(16) 0.0478(16) -0.0068(8) -0.0164(9) -0.0181(9) O3 0.069(2) 0.070(2) 0.070(2) -0.0098(9) -0.0239(10) -0.0270(11) O4 0.042(3) 0.042(3) 0.042(3) -0.0052(11) -0.0141(13) -0.0164(14) Rh1 0.0236(7) 0.0453(8) 0.0498(9) -0.0070(5) -0.0158(5) -0.0150(5) _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 O2 1.266(16) . ? C1 O1 1.280(17) . ? C1 C2 1.484(19) . ? C2 C3 1.376(12) . ? C2 C7 1.380(12) . ? C3 C4 1.378(12) . ? C4 C5 1.378(12) . ? C5 C6 1.365(12) . ? C6 C7 1.372(12) . ? C8 O3 1.25(2) . ? C8 O4 1.28(2) 2_755 ? C8 C9 1.51(2) . ? C9 C14 1.353(13) . ? C9 C10 1.365(13) . ? C10 C11 1.371(13) . ? C11 C12 1.343(13) . ? C12 C13 1.349(13) . ? C13 C14 1.380(13) . ? C15 N1 1.315(14) . ? C15 C16 1.37(2) 2_855 ? C16 N1 1.310(14) . ? C16 C15 1.37(2) 2_855 ? N1 Rh1 2.250(12) . ? O1 Rh1 2.034(9) . ? O2 Rh1 2.019(10) 2_755 ? O3 Rh1 2.049(11) . ? O4 C8 1.28(2) 2_755 ? O4 Rh1 2.031(9) . ? Rh1 O2 2.019(10) 2_755 ? Rh1 Rh1 2.382(2) 2_755 ? 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 O2 C1 O1 124.0(15) . . ? O2 C1 C2 118.7(14) . . ? O1 C1 C2 117.3(13) . . ? C3 C2 C7 119.4(9) . . ? C3 C2 C1 120.7(11) . . ? C7 C2 C1 119.9(11) . . ? C2 C3 C4 120.3(9) . . ? C5 C4 C3 119.5(9) . . ? C6 C5 C4 120.5(9) . . ? C5 C6 C7 119.9(9) . . ? C6 C7 C2 120.4(9) . . ? O3 C8 O4 125.5(19) . 2_755 ? O3 C8 C9 116.2(16) . . ? O4 C8 C9 118.3(16) 2_755 . ? C14 C9 C10 120.8(10) . . ? C14 C9 C8 119.9(13) . . ? C10 C9 C8 119.3(13) . . ? C9 C10 C11 118.8(10) . . ? C12 C11 C10 120.3(10) . . ? C11 C12 C13 121.0(10) . . ? C12 C13 C14 119.2(10) . . ? C9 C14 C13 119.6(10) . . ? N1 C15 C16 121.3(13) . 2_855 ? N1 C16 C15 120.2(13) . 2_855 ? C16 N1 C15 118.3(13) . . ? C16 N1 Rh1 120.7(10) . . ? C15 N1 Rh1 120.7(10) . . ? C1 O1 Rh1 119.3(10) . . ? C1 O2 Rh1 120.4(10) . 2_755 ? C8 O3 Rh1 119.3(13) . . ? C8 O4 Rh1 118.9(12) 2_755 . ? O2 Rh1 O4 90.9(4) 2_755 . ? O2 Rh1 O1 176.1(4) 2_755 . ? O4 Rh1 O1 89.8(4) . . ? O2 Rh1 O3 89.2(4) 2_755 . ? O4 Rh1 O3 176.1(4) . . ? O1 Rh1 O3 89.9(4) . . ? O2 Rh1 N1 91.1(4) 2_755 . ? O4 Rh1 N1 92.3(4) . . ? O1 Rh1 N1 92.6(4) . . ? O3 Rh1 N1 91.6(5) . . ? O2 Rh1 Rh1 88.1(3) 2_755 2_755 ? O4 Rh1 Rh1 88.4(3) . 2_755 ? O1 Rh1 Rh1 88.2(3) . 2_755 ? O3 Rh1 Rh1 87.8(4) . 2_755 ? N1 Rh1 Rh1 179.0(3) . 2_755 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -179.8(14) . . . . ? O1 C1 C2 C3 -1(2) . . . . ? O2 C1 C2 C7 4(2) . . . . ? O1 C1 C2 C7 -177.1(15) . . . . ? C7 C2 C3 C4 -1(2) . . . . ? C1 C2 C3 C4 -177.8(15) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C3 C4 C5 C6 -4(2) . . . . ? C4 C5 C6 C7 3(2) . . . . ? C5 C6 C7 C2 -1(2) . . . . ? C3 C2 C7 C6 0(2) . . . . ? C1 C2 C7 C6 176.9(15) . . . . ? O3 C8 C9 C14 -172.0(15) . . . . ? O4 C8 C9 C14 8(2) 2_755 . . . ? O3 C8 C9 C10 9(2) . . . . ? O4 C8 C9 C10 -171.3(14) 2_755 . . . ? C14 C9 C10 C11 0.4(17) . . . . ? C8 C9 C10 C11 179.6(16) . . . . ? C9 C10 C11 C12 3.0(17) . . . . ? C10 C11 C12 C13 -7(3) . . . . ? C11 C12 C13 C14 7(3) . . . . ? C10 C9 C14 C13 0(2) . . . . ? C8 C9 C14 C13 -179.2(16) . . . . ? C12 C13 C14 C9 -4(3) . . . . ? C15 C16 N1 C15 4(2) 2_855 . . . ? C15 C16 N1 Rh1 178.3(10) 2_855 . . . ? C16 C15 N1 C16 -4(2) 2_855 . . . ? C16 C15 N1 Rh1 -178.3(11) 2_855 . . . ? O2 C1 O1 Rh1 1(2) . . . . ? C2 C1 O1 Rh1 -178.3(10) . . . . ? O1 C1 O2 Rh1 0(2) . . . 2_755 ? C2 C1 O2 Rh1 179.2(11) . . . 2_755 ? O4 C8 O3 Rh1 -4(2) 2_755 . . . ? C9 C8 O3 Rh1 175.8(11) . . . . ? C8 O4 Rh1 O2 89.7(12) 2_755 . . 2_755 ? C8 O4 Rh1 O1 -86.5(12) 2_755 . . . ? C8 O4 Rh1 O3 -1(7) 2_755 . . . ? C8 O4 Rh1 N1 -179.2(12) 2_755 . . . ? C8 O4 Rh1 Rh1 1.6(12) 2_755 . . 2_755 ? C1 O1 Rh1 O2 -12(7) . . . 2_755 ? C1 O1 Rh1 O4 87.3(12) . . . . ? C1 O1 Rh1 O3 -88.8(12) . . . . ? C1 O1 Rh1 N1 179.6(12) . . . . ? C1 O1 Rh1 Rh1 -1.1(11) . . . 2_755 ? C8 O3 Rh1 O2 -86.0(13) . . . 2_755 ? C8 O3 Rh1 O4 5(7) . . . . ? C8 O3 Rh1 O1 90.2(13) . . . . ? C8 O3 Rh1 N1 -177.1(13) . . . . ? C8 O3 Rh1 Rh1 2.1(13) . . . 2_755 ? C16 N1 Rh1 O2 -143.5(12) . . . 2_755 ? C15 N1 Rh1 O2 30.4(12) . . . 2_755 ? C16 N1 Rh1 O4 125.5(11) . . . . ? C15 N1 Rh1 O4 -60.5(12) . . . . ? C16 N1 Rh1 O1 35.7(12) . . . . ? C15 N1 Rh1 O1 -150.4(12) . . . . ? C16 N1 Rh1 O3 -54.3(12) . . . . ? C15 N1 Rh1 O3 119.6(12) . . . . ? C16 N1 Rh1 Rh1 -104(18) . . . 2_755 ? C15 N1 Rh1 Rh1 70(19) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.80 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.043 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.264