#------------------------------------------------------------------------------ #$Date: 2014-07-11 19:33:45 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120075 $ #$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075776.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075776 loop_ _publ_author_name 'Tanaka, Shukichi' 'Dubs, Christian' 'Inagaki, Akiko' 'Akita, Munetaka' _publ_section_title ; Polynuclear Rhodium Complexes with Dinucleating PNNP Ligand:  Dynamic and Diverse M···M Interactions in [(\m-X)Rh2(PNNP)(CO)2]n+and [(\m4-X)Rh4(PNNP)2(CO)4]n+[X = H, O, C⋮C−R, R−C⋮C−R, C⋮C, CHCH2, SMe2;n= 0, 1:  PNNP = 3,5-bis(diphenylphosphinomethyl)pyrazolato] ; _journal_issue 1 _journal_name_full Organometallics _journal_page_first 163 _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C64 H50 N4 O4 P4 Rh4 ' _chemical_formula_sum 'C64 H50 N4 O4 P4 Rh4' _chemical_formula_weight 1474.64 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 38.916(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.608(3) _cell_length_b 19.320(3) _cell_length_c 22.188(1) _cell_measurement_reflns_used 23291 _cell_measurement_temperature 213.2 _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 3.1 _cell_volume 6088.0(14) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _computing_structure_refinement SHELXL97 _computing_structure_solution SHELXS86 _diffrn_detector_area_resol_mean 10.00 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 48675 _diffrn_reflns_theta_max 27.51 _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_crystal_colour unknown _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_description unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.77 _refine_diff_density_min -1.52 _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 721 _refine_ls_number_reflns 8137 _refine_ls_R_factor_gt 0.0680 _refine_ls_shift/su_max -0.0010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1926 _reflns_number_gt 8137 _reflns_number_total 13846 _reflns_threshold_expression >2.0sigma(I) _[local]_cod_data_source_file om049427vsi20040726_024341.cif _[local]_cod_data_source_block compound_9 _[local]_cod_chemical_formula_sum_orig 'C64 H50 N4 O4 P4 Rh4 ' _cod_original_cell_volume 6087(1) _cod_database_code 4075776 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z 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_calc_flag Rh(1) Rh 0.20493(5) 1.05942(3) 0.57747(5) 0.0344(2) Uani 1.00 d Rh(2) Rh 0.03185(4) 0.96202(3) 0.61421(4) 0.0309(2) Uani 1.00 d Rh(3) Rh -0.15789(5) 1.05681(3) 0.85125(4) 0.0333(2) Uani 1.00 d Rh(4) Rh 0.02564(5) 0.92306(3) 0.75799(5) 0.0329(2) Uani 1.00 d P(1) P 0.3594(2) 1.0866(1) 0.4491(2) 0.0424(5) Uani 1.00 d P(2) P 0.0650(2) 0.8983(1) 0.5069(2) 0.0331(4) Uani 1.00 d P(3) P -0.3140(2) 1.0715(1) 0.9895(2) 0.0366(5) Uani 1.00 d P(4) P 0.0075(2) 0.8229(1) 0.8200(2) 0.0361(5) Uani 1.00 d O(01) O 0.1771(6) 1.1118(5) 0.7237(6) 0.081(3) Uani 1.00 d O(02) O -0.1709(5) 0.9258(4) 0.7656(5) 0.058(2) Uani 1.00 d O(03) O -0.1302(6) 1.1897(4) 0.7639(6) 0.087(3) Uani 1.00 d O(04) O 0.2272(5) 0.8852(3) 0.5881(5) 0.053(2) Uani 1.00 d N(1) N 0.2307(4) 1.0276(4) 0.4715(4) 0.035(1) Uani 1.00 d N(2) N 0.1685(5) 0.9931(3) 0.4858(4) 0.033(1) Uani 1.00 d N(3) N -0.1835(5) 0.9703(4) 0.9218(5) 0.037(2) Uani 1.00 d N(4) N -0.1159(5) 0.9283(3) 0.8917(5) 0.035(2) Uani 1.00 d C(1) C 0.0681(6) 1.0292(4) 0.6755(6) 0.033(2) Uani 1.00 d C(01) C 0.1873(7) 1.0918(5) 0.6675(7) 0.050(2) Uani 1.00 d C(2) C -0.0177(6) 1.0291(4) 0.7393(6) 0.036(2) Uani 1.00 d C(02) C -0.0929(7) 0.9383(4) 0.7108(6) 0.042(2) Uani 1.00 d C(03) C -0.1403(7) 1.1378(5) 0.7975(7) 0.052(2) Uani 1.00 d C(04) C 0.1499(7) 0.9043(4) 0.6515(6) 0.039(2) Uani 1.00 d C(11) C 0.3092(6) 1.0427(4) 0.3763(5) 0.036(2) Uani 1.00 d C(12) C 0.2943(6) 1.0178(5) 0.3291(6) 0.042(2) Uani 1.00 d C(13) C 0.2067(6) 0.9858(5) 0.3990(6) 0.038(2) Uani 1.00 d C(14) C 0.3852(7) 1.0820(5) 0.3475(7) 0.051(2) Uani 1.00 d C(15) C 0.1490(7) 0.9523(4) 0.3975(6) 0.042(2) Uani 1.00 d C(21) C -0.2686(6) 0.9509(4) 1.0116(6) 0.037(2) Uani 1.00 d C(22) C -0.2570(6) 0.8971(5) 1.0422(6) 0.041(2) Uani 1.00 d C(23) C -0.1608(7) 0.8842(5) 0.9659(6) 0.041(2) Uani 1.00 d C(24) C -0.3519(6) 0.9881(5) 1.0536(7) 0.045(2) Uani 1.00 d C(25) C -0.1004(7) 0.8344(5) 0.9517(6) 0.044(2) Uani 1.00 d C(31) C 0.4042(6) 1.1703(5) 0.4380(6) 0.047(2) Uani 1.00 d C(32) C 0.4609(10) 1.1758(6) 0.4426(10) 0.073(3) Uani 1.00 d C(33) C 0.492(1) 1.2423(7) 0.439(1) 0.096(5) Uani 1.00 d C(34) C 0.4652(9) 1.2981(7) 0.4321(9) 0.078(4) Uani 1.00 d C(35) C 0.4078(10) 1.2951(6) 0.4253(9) 0.082(4) Uani 1.00 d C(36) C 0.3765(8) 1.2304(6) 0.4304(9) 0.065(3) Uani 1.00 d C(41) C 0.4378(7) 1.0229(6) 0.4224(7) 0.055(3) Uani 1.00 d C(42) C 0.5321(9) 1.0171(8) 0.3332(10) 0.083(4) Uani 1.00 d C(43) C 0.5871(9) 0.9657(9) 0.320(1) 0.094(5) Uani 1.00 d C(44) C 0.551(1) 0.9247(9) 0.392(1) 0.094(5) Uani 1.00 d C(45) C 0.460(1) 0.9322(7) 0.478(1) 0.085(4) Uani 1.00 d C(46) C 0.4038(8) 0.9801(6) 0.4940(9) 0.059(3) Uani 1.00 d C(51) C -0.0238(6) 0.8652(4) 0.5260(6) 0.037(2) Uani 1.00 d C(52) C -0.0277(7) 0.8812(5) 0.4685(6) 0.044(2) Uani 1.00 d C(53) C -0.0976(8) 0.8536(5) 0.4876(8) 0.057(3) Uani 1.00 d C(54) C -0.1624(7) 0.8094(5) 0.5629(8) 0.055(3) Uani 1.00 d C(55) C -0.1595(7) 0.7922(5) 0.6210(8) 0.055(3) Uani 1.00 d C(56) C -0.0895(7) 0.8189(5) 0.6014(6) 0.044(2) Uani 1.00 d C(61) C 0.1354(6) 0.8215(4) 0.4668(6) 0.036(2) Uani 1.00 d C(62) C 0.1743(7) 0.8137(5) 0.4928(7) 0.043(2) Uani 1.00 d C(63) C 0.2289(7) 0.7553(5) 0.4625(7) 0.047(2) Uani 1.00 d C(64) C 0.2469(7) 0.7069(5) 0.4051(7) 0.048(2) Uani 1.00 d C(65) C 0.2105(7) 0.7143(5) 0.3773(7) 0.050(2) Uani 1.00 d C(66) C 0.1546(7) 0.7726(5) 0.4070(7) 0.046(2) Uani 1.00 d C(71) C -0.3464(6) 1.1337(5) 1.0723(6) 0.041(2) Uani 1.00 d C(72) C -0.3200(8) 1.1218(6) 1.1100(8) 0.065(3) Uani 1.00 d C(73) C -0.3365(10) 1.1692(7) 1.1684(9) 0.081(4) Uani 1.00 d C(74) C -0.380(1) 1.2312(6) 1.1894(9) 0.078(4) Uani 1.00 d C(75) C -0.4089(10) 1.2427(6) 1.1560(9) 0.080(4) Uani 1.00 d C(76) C -0.3927(8) 1.1962(5) 1.0968(7) 0.061(3) Uani 1.00 d C(81) C -0.3940(7) 1.0861(5) 0.9907(7) 0.046(2) Uani 1.00 d C(82) C -0.4900(8) 1.0896(7) 1.0749(8) 0.071(3) Uani 1.00 d C(83) C -0.5489(8) 1.0975(8) 1.073(1) 0.086(4) Uani 1.00 d C(84) C -0.513(1) 1.1040(7) 0.987(1) 0.082(4) Uani 1.00 d C(85) C -0.416(1) 1.0992(7) 0.903(1) 0.079(4) Uani 1.00 d C(86) C -0.3594(8) 1.0901(6) 0.9060(8) 0.061(3) Uani 1.00 d C(91) C 0.0994(6) 0.7905(5) 0.7977(6) 0.041(2) Uani 1.00 d C(92) C 0.109(1) 0.817(1) 0.846(1) 0.150(9) Uani 1.00 d C(93) C 0.183(1) 0.794(1) 0.824(2) 0.18(1) Uani 1.00 d C(94) C 0.243(1) 0.7474(8) 0.759(1) 0.088(4) Uani 1.00 d C(95) C 0.2273(9) 0.7185(7) 0.719(1) 0.082(4) Uani 1.00 d C(96) C 0.1560(9) 0.7365(6) 0.7388(9) 0.072(3) Uani 1.00 d C(101) C -0.0198(6) 0.7478(4) 0.7949(6) 0.037(2) Uani 1.00 d C(102) C -0.0070(7) 0.7535(5) 0.7226(7) 0.046(2) Uani 1.00 d C(103) C -0.0271(8) 0.6985(6) 0.7021(8) 0.059(3) Uani 1.00 d C(104) C -0.0597(8) 0.6367(5) 0.7531(8) 0.056(3) Uani 1.00 d C(105) C -0.0725(8) 0.6309(5) 0.8228(8) 0.058(3) Uani 1.00 d C(106) C -0.0522(7) 0.6865(5) 0.8446(7) 0.050(2) Uani 1.00 d H(1) H 0.3358 1.0222 0.2621 0.0500 Uiso 1.00 calc H(2) H 0.3891 1.1280 0.3277 0.0625 Uiso 1.00 calc H(3) H 0.4447 1.0598 0.2936 0.0625 Uiso 1.00 calc H(4) H 0.1868 0.9245 0.3409 0.0508 Uiso 1.00 calc H(5) H 0.1166 0.9860 0.3988 0.0508 Uiso 1.00 calc H(6) H 0.4795 1.1336 0.4495 0.0852 Uiso 1.00 calc H(7) H 0.5333 1.2450 0.4410 0.1131 Uiso 1.00 calc H(8) H 0.4848 1.3426 0.4318 0.0941 Uiso 1.00 calc H(9) H 0.3911 1.3373 0.4170 0.0995 Uiso 1.00 calc H(10) H 0.3339 1.2268 0.4293 0.0775 Uiso 1.00 calc H(11) H 0.5602 1.0487 0.2808 0.1013 Uiso 1.00 calc H(12) H 0.6533 0.9594 0.2564 0.1168 Uiso 1.00 calc H(13) H 0.5883 0.8894 0.3834 0.1139 Uiso 1.00 calc H(14) H 0.4318 0.9031 0.5321 0.1040 Uiso 1.00 calc H(15) H 0.3373 0.9842 0.5583 0.0721 Uiso 1.00 calc H(16) H 0.0184 0.9119 0.4145 0.0545 Uiso 1.00 calc H(17) H -0.1001 0.8654 0.4469 0.0682 Uiso 1.00 calc H(18) H -0.2113 0.7902 0.5769 0.0664 Uiso 1.00 calc H(19) H -0.2061 0.7613 0.6748 0.0651 Uiso 1.00 calc H(20) H -0.0869 0.8061 0.6417 0.0530 Uiso 1.00 calc H(21) H 0.1629 0.8487 0.5322 0.0511 Uiso 1.00 calc H(22) H 0.2541 0.7496 0.4829 0.0581 Uiso 1.00 calc H(23) H 0.2865 0.6674 0.3827 0.0579 Uiso 1.00 calc H(24) H 0.2215 0.6789 0.3380 0.0589 Uiso 1.00 calc H(25) H 0.1312 0.7791 0.3851 0.0551 Uiso 1.00 calc H(26) H -0.3049 0.8730 1.1026 0.0488 Uiso 1.00 calc H(27) H -0.3950 0.9974 1.1202 0.0529 Uiso 1.00 calc H(28) H -0.3828 0.9607 1.0489 0.0529 Uiso 1.00 calc H(29) H -0.1327 0.7910 0.9822 0.0532 Uiso 1.00 calc H(30) H -0.0854 0.8517 0.9790 0.0532 Uiso 1.00 calc H(31) H -0.2914 1.0776 1.0973 0.0768 Uiso 1.00 calc H(32) H -0.3178 1.1591 1.1951 0.0948 Uiso 1.00 calc H(33) H -0.3894 1.2659 1.2280 0.0914 Uiso 1.00 calc H(34) H -0.4417 1.2862 1.1731 0.0926 Uiso 1.00 calc H(35) H -0.4138 1.2063 1.0727 0.0755 Uiso 1.00 calc H(36) H -0.5161 1.0869 1.1363 0.0857 Uiso 1.00 calc H(37) H -0.6168 1.0987 1.1330 0.1049 Uiso 1.00 calc H(38) H -0.5525 1.1116 0.9850 0.1019 Uiso 1.00 calc H(39) H -0.3867 1.1037 0.8393 0.0969 Uiso 1.00 calc H(40) H -0.2915 1.0864 0.8462 0.0737 Uiso 1.00 calc H(41) H 0.0602 0.8474 0.9005 0.1711 Uiso 1.00 calc H(42) H 0.1894 0.8128 0.8596 0.2210 Uiso 1.00 calc H(43) H 0.2962 0.7331 0.7401 0.1030 Uiso 1.00 calc H(44) H 0.2691 0.6815 0.6725 0.0959 Uiso 1.00 calc H(45) H 0.1459 0.7118 0.7092 0.0852 Uiso 1.00 calc H(46) H 0.0153 0.7969 0.6876 0.0553 Uiso 1.00 calc H(47) H -0.0199 0.7024 0.6533 0.0715 Uiso 1.00 calc H(48) H -0.0727 0.5978 0.7372 0.0666 Uiso 1.00 calc H(49) H -0.0954 0.5884 0.8581 0.0707 Uiso 1.00 calc H(50) H -0.0627 0.6829 0.8962 0.0587 Uiso 1.00 calc 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 Rh(1) 0.0304(4) 0.0326(3) 0.0324(3) -0.0037(3) -0.0225(3) 0.0033(3) Rh(2) 0.0309(3) 0.0274(3) 0.0300(3) -0.0019(3) -0.0226(3) 0.0012(2) Rh(3) 0.0295(3) 0.0302(3) 0.0296(3) 0.0012(3) -0.0203(3) 0.0000(3) Rh(4) 0.0355(4) 0.0282(3) 0.0340(3) 0.0016(3) -0.0268(3) -0.0003(3) P(1) 0.029(1) 0.046(1) 0.038(1) -0.007(1) -0.022(1) 0.001(1) P(2) 0.035(1) 0.030(1) 0.034(1) 0.0009(9) -0.026(1) -0.0015(8) P(3) 0.029(1) 0.038(1) 0.033(1) 0.0014(9) -0.021(1) 0.0016(9) P(4) 0.043(1) 0.029(1) 0.040(1) 0.0016(9) -0.033(1) 0.0005(9) O(01) 0.100(7) 0.096(6) 0.064(5) -0.022(5) -0.068(6) 0.001(5) O(02) 0.027(4) 0.061(5) 0.039(4) -0.012(3) -0.014(3) -0.006(3) O(03) 0.076(6) 0.055(5) 0.078(6) 0.005(4) -0.047(5) 0.026(4) O(04) 0.045(4) 0.043(4) 0.058(4) 0.003(3) -0.036(4) -0.004(3) N(1) 0.022(3) 0.035(4) 0.027(3) -0.006(3) -0.014(3) 0.002(3) N(2) 0.029(4) 0.033(4) 0.026(3) -0.002(3) -0.019(3) 0.001(3) N(3) 0.036(4) 0.032(4) 0.039(4) 0.002(3) -0.028(4) 0.000(3) N(4) 0.037(4) 0.025(3) 0.044(4) 0.003(3) -0.031(4) 0.004(3) C(1) 0.035(5) 0.021(4) 0.038(4) -0.007(3) -0.027(4) 0.007(3) C(01) 0.039(5) 0.040(5) 0.059(6) -0.012(4) -0.035(5) 0.005(4) C(2) 0.044(5) 0.031(4) 0.034(4) 0.003(4) -0.031(4) -0.003(3) C(02) 0.052(6) 0.032(4) 0.037(5) -0.005(4) -0.033(5) 0.000(4) C(03) 0.038(5) 0.054(6) 0.036(5) 0.010(5) -0.022(5) -0.004(4) C(04) 0.042(5) 0.031(4) 0.039(5) -0.006(4) -0.030(5) 0.006(4) C(11) 0.027(4) 0.042(5) 0.019(3) 0.002(4) -0.013(4) -0.001(3) C(12) 0.029(5) 0.044(5) 0.025(4) -0.007(4) -0.014(4) 0.006(4) C(13) 0.040(5) 0.041(5) 0.031(4) -0.006(4) -0.027(4) 0.011(4) C(14) 0.040(5) 0.063(6) 0.040(5) -0.016(5) -0.029(5) 0.009(4) C(15) 0.053(6) 0.033(5) 0.045(5) 0.004(4) -0.040(5) -0.002(4) C(21) 0.034(5) 0.034(4) 0.028(4) 0.001(4) -0.020(4) 0.001(3) C(22) 0.039(5) 0.036(5) 0.030(4) -0.004(4) -0.022(4) 0.007(3) C(23) 0.050(6) 0.037(5) 0.037(5) -0.005(4) -0.034(5) 0.007(4) C(24) 0.032(5) 0.040(5) 0.047(5) -0.003(4) -0.027(5) 0.004(4) C(25) 0.050(6) 0.039(5) 0.040(5) 0.005(4) -0.035(5) -0.001(4) C(31) 0.028(5) 0.053(6) 0.039(5) -0.003(4) -0.021(4) -0.003(4) C(32) 0.092(10) 0.051(7) 0.100(9) -0.019(6) -0.081(9) 0.009(6) C(33) 0.12(1) 0.057(8) 0.15(1) -0.021(8) -0.11(1) 0.007(9) C(34) 0.062(8) 0.056(8) 0.069(8) -0.019(6) -0.038(7) -0.003(6) C(35) 0.084(10) 0.040(6) 0.063(8) 0.009(6) -0.042(8) -0.007(5) C(36) 0.062(7) 0.047(6) 0.079(8) -0.005(5) -0.053(7) -0.001(5) C(41) 0.033(5) 0.065(7) 0.054(6) 0.006(5) -0.030(5) -0.024(5) C(42) 0.057(8) 0.10(1) 0.076(8) 0.009(7) -0.048(8) -0.019(8) C(43) 0.042(7) 0.12(1) 0.09(1) 0.030(8) -0.042(8) -0.037(9) C(44) 0.09(1) 0.11(1) 0.10(1) 0.030(10) -0.08(1) -0.031(10) C(45) 0.11(1) 0.068(8) 0.13(1) 0.021(8) -0.10(1) -0.025(8) C(46) 0.068(7) 0.055(6) 0.078(7) 0.001(5) -0.062(7) -0.002(6) C(51) 0.039(5) 0.032(4) 0.042(5) 0.005(4) -0.032(4) -0.006(4) C(52) 0.049(6) 0.045(5) 0.044(5) 0.003(4) -0.038(5) -0.002(4) C(53) 0.079(8) 0.045(6) 0.086(8) 0.002(5) -0.074(7) -0.004(5) C(54) 0.049(6) 0.053(6) 0.069(7) -0.005(5) -0.048(6) -0.007(5) C(55) 0.047(6) 0.052(6) 0.063(6) -0.010(5) -0.042(6) 0.002(5) C(56) 0.044(5) 0.041(5) 0.043(5) -0.003(4) -0.033(5) -0.001(4) C(61) 0.036(5) 0.030(4) 0.041(5) 0.003(3) -0.030(4) -0.001(3) C(62) 0.046(6) 0.043(5) 0.049(5) 0.002(4) -0.040(5) -0.002(4) C(63) 0.048(6) 0.042(5) 0.062(6) 0.008(4) -0.045(6) -0.004(4) C(64) 0.038(5) 0.038(5) 0.054(6) 0.006(4) -0.032(5) -0.004(4) C(65) 0.047(6) 0.049(6) 0.052(6) 0.015(5) -0.038(5) -0.018(5) C(66) 0.050(6) 0.051(6) 0.049(5) 0.009(4) -0.042(5) -0.013(4) C(71) 0.030(5) 0.039(5) 0.037(5) -0.004(4) -0.022(4) 0.006(4) C(72) 0.059(7) 0.066(7) 0.069(7) 0.018(6) -0.049(7) -0.022(6) C(73) 0.088(10) 0.085(10) 0.075(8) 0.013(8) -0.065(8) -0.032(7) C(74) 0.10(1) 0.056(7) 0.057(7) -0.008(7) -0.054(8) -0.006(6) C(75) 0.087(10) 0.051(7) 0.062(7) 0.023(7) -0.047(8) -0.018(6) C(76) 0.069(7) 0.045(6) 0.047(6) 0.010(5) -0.040(6) -0.002(5) C(81) 0.038(5) 0.040(5) 0.050(5) 0.005(4) -0.032(5) 0.000(4) C(82) 0.045(6) 0.098(9) 0.067(7) -0.015(6) -0.042(6) 0.034(7) C(83) 0.043(7) 0.12(1) 0.093(10) -0.006(7) -0.053(8) 0.027(9) C(84) 0.10(1) 0.075(8) 0.13(1) -0.003(8) -0.11(1) 0.012(8) C(85) 0.09(1) 0.087(9) 0.093(10) 0.024(8) -0.082(10) -0.025(8) C(86) 0.061(7) 0.079(8) 0.057(6) 0.026(6) -0.049(6) -0.017(6) C(91) 0.045(5) 0.035(5) 0.048(5) 0.004(4) -0.038(5) -0.004(4) C(92) 0.13(1) 0.22(2) 0.19(2) 0.12(1) -0.14(1) -0.16(2) C(93) 0.14(2) 0.28(3) 0.24(2) 0.13(2) -0.18(2) -0.17(2) C(94) 0.077(10) 0.10(1) 0.11(1) 0.022(8) -0.078(10) -0.005(9) C(95) 0.056(8) 0.062(8) 0.11(1) 0.022(6) -0.059(8) -0.017(7) C(96) 0.071(8) 0.061(7) 0.094(9) 0.026(6) -0.067(8) -0.038(7) C(101) 0.040(5) 0.038(5) 0.037(4) -0.002(4) -0.031(4) 0.003(4) C(102) 0.052(6) 0.043(5) 0.046(5) -0.010(4) -0.039(5) 0.009(4) C(103) 0.078(8) 0.053(6) 0.065(7) -0.010(6) -0.061(7) 0.002(5) C(104) 0.075(8) 0.034(5) 0.076(7) -0.008(5) -0.063(7) 0.002(5) C(105) 0.068(7) 0.034(5) 0.073(7) -0.005(5) -0.056(7) 0.009(5) C(106) 0.061(7) 0.042(5) 0.061(6) -0.007(5) -0.051(6) 0.009(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag P(1) Rh(1) N(1) 80.8(2) yes P(1) Rh(1) C(1) 169.6(4) yes P(1) Rh(1) C(01) 96.2(3) yes N(1) Rh(1) C(1) 88.8(5) yes N(1) Rh(1) C(01) 176.6(3) yes C(1) Rh(1) C(01) 94.1(5) yes P(2) Rh(2) N(2) 77.9(3) yes P(2) Rh(2) C(1) 155.6(2) yes P(2) Rh(2) C(2) 175.2(3) yes P(2) Rh(2) C(02) 92.5(5) yes N(2) Rh(2) C(1) 79.9(4) yes N(2) Rh(2) C(2) 106.7(4) yes N(2) Rh(2) C(02) 165.7(7) yes C(1) Rh(2) C(2) 29.2(3) yes C(1) Rh(2) C(02) 111.2(5) yes C(2) Rh(2) C(02) 82.8(5) yes P(3) Rh(3) N(3) 81.4(2) yes P(3) Rh(3) C(2) 169.1(4) yes P(3) Rh(3) C(03) 95.5(3) yes N(3) Rh(3) C(2) 87.9(3) yes N(3) Rh(3) C(03) 175.2(5) yes C(2) Rh(3) C(03) 95.0(4) yes P(4) Rh(4) N(4) 79.6(2) yes P(4) Rh(4) C(1) 172.0(3) yes P(4) Rh(4) C(2) 158.7(2) yes P(4) Rh(4) C(04) 89.1(3) yes N(4) Rh(4) C(1) 107.9(3) yes N(4) Rh(4) C(2) 79.9(3) yes N(4) Rh(4) C(04) 168.4(5) yes C(1) Rh(4) C(2) 29.2(3) yes C(1) Rh(4) C(04) 83.2(4) yes C(2) Rh(4) C(04) 111.5(4) yes Rh(1) P(1) C(14) 103.9(4) yes Rh(1) P(1) C(31) 121.9(2) yes Rh(1) P(1) C(41) 114.0(3) yes C(14) P(1) C(31) 105.4(6) yes C(14) P(1) C(41) 105.5(6) yes C(31) P(1) C(41) 104.8(7) yes Rh(2) P(2) C(15) 103.8(4) yes Rh(2) P(2) C(51) 123.6(3) yes Rh(2) P(2) C(61) 114.2(6) yes C(15) P(2) C(51) 109.0(7) yes C(15) P(2) C(61) 101.8(4) yes C(51) P(2) C(61) 102.4(5) yes Rh(3) P(3) C(24) 103.5(3) yes Rh(3) P(3) C(71) 115.7(4) yes Rh(3) P(3) C(81) 121.8(4) yes C(24) P(3) C(71) 102.7(6) yes C(24) P(3) C(81) 105.2(6) yes C(71) P(3) C(81) 105.7(6) yes Rh(4) P(4) C(25) 104.7(3) yes Rh(4) P(4) C(91) 120.5(3) yes Rh(4) P(4) C(101) 116.5(5) yes C(25) P(4) C(91) 107.0(7) yes C(25) P(4) C(101) 103.4(5) yes C(91) P(4) C(101) 103.2(6) yes Rh(1) N(1) N(2) 124.7(4) yes Rh(1) N(1) C(11) 125.8(9) yes N(2) N(1) C(11) 109(1) yes Rh(2) N(2) N(1) 128.9(7) yes Rh(2) N(2) C(13) 122.3(9) yes N(1) N(2) C(13) 108.5(7) yes Rh(3) N(3) N(4) 124.9(4) yes Rh(3) N(3) C(21) 125.6(7) yes N(4) N(3) C(21) 108.9(9) yes Rh(4) N(4) N(3) 128.8(7) yes Rh(4) N(4) C(23) 124.6(7) yes N(3) N(4) C(23) 106.5(7) yes Rh(1) C(1) Rh(2) 116.5(4) yes Rh(1) C(1) Rh(4) 115.7(6) yes Rh(1) C(1) C(2) 163.4(7) yes Rh(2) C(1) Rh(4) 82.0(3) yes Rh(2) C(1) C(2) 74.0(10) yes Rh(4) C(1) C(2) 77.4(6) yes Rh(1) C(01) O(01) 179(1) yes Rh(2) C(2) Rh(3) 115.4(7) yes Rh(2) C(2) Rh(4) 81.7(2) yes Rh(2) C(2) C(1) 76.8(8) yes Rh(3) C(2) Rh(4) 117.2(3) yes Rh(3) C(2) C(1) 164.0(8) yes Rh(4) C(2) C(1) 73.3(7) yes Rh(2) C(02) O(02) 173(1) yes Rh(3) C(03) O(03) 179.2(9) yes Rh(4) C(04) O(04) 172.4(9) yes N(1) C(11) C(12) 107.6(9) yes N(1) C(11) C(14) 116(1) yes C(12) C(11) C(14) 135.7(8) yes C(11) C(12) C(13) 106.3(10) yes N(2) C(13) C(12) 108(1) yes N(2) C(13) C(15) 118.2(7) yes C(12) C(13) C(15) 133(1) yes P(1) C(14) C(11) 109.7(7) yes P(2) C(15) C(13) 103(1) yes N(3) C(21) C(22) 109.6(9) yes N(3) C(21) C(24) 116(1) yes C(22) C(21) C(24) 133.9(7) yes C(21) C(22) C(23) 104.7(8) yes N(4) C(23) C(22) 110(1) yes N(4) C(23) C(25) 116.7(7) yes C(22) C(23) C(25) 133.1(10) yes P(3) C(24) C(21) 109.5(6) yes P(4) C(25) C(23) 106.1(9) yes P(1) C(31) C(32) 121.0(10) yes P(1) C(31) C(36) 120(1) yes C(32) C(31) C(36) 118(1) yes C(31) C(32) C(33) 120(1) yes C(32) C(33) C(34) 120(2) yes C(33) C(34) C(35) 121(1) yes C(34) C(35) C(36) 118(1) yes C(31) C(36) C(35) 120(2) yes P(1) C(41) C(42) 122(1) yes P(1) C(41) C(46) 119.9(7) yes C(42) C(41) C(46) 117(1) yes C(41) C(42) C(43) 118(1) yes C(42) C(43) C(44) 122(1) yes C(43) C(44) C(45) 118(2) yes C(44) C(45) C(46) 121(2) yes C(41) C(46) C(45) 122(1) yes P(2) C(51) C(52) 124.0(6) yes P(2) C(51) C(56) 117(1) yes C(52) C(51) C(56) 118(1) yes C(51) C(52) C(53) 120.5(10) yes C(52) C(53) C(54) 119(2) yes C(53) C(54) C(55) 120(1) yes C(54) C(55) C(56) 119.6(10) yes C(51) C(56) C(55) 120(1) yes P(2) C(61) C(62) 118.9(8) yes P(2) C(61) C(66) 121(1) yes C(62) C(61) C(66) 119(1) yes C(61) C(62) C(63) 119(1) yes C(62) C(63) C(64) 120(1) yes C(63) C(64) C(65) 120(1) yes C(64) C(65) C(66) 120(1) yes C(61) C(66) C(65) 119(1) yes P(3) C(71) C(72) 118.9(8) yes P(3) C(71) C(76) 123(1) yes C(72) C(71) C(76) 117(1) yes C(71) C(72) C(73) 122(1) yes C(72) C(73) C(74) 119(2) yes C(73) C(74) C(75) 119(1) yes C(74) C(75) C(76) 122(1) yes C(71) C(76) C(75) 119(1) yes P(3) C(81) C(82) 122(1) yes P(3) C(81) C(86) 119.5(9) yes C(82) C(81) C(86) 118(1) yes C(81) C(82) C(83) 120(1) yes C(82) C(83) C(84) 120(1) yes C(83) C(84) C(85) 118(2) yes C(84) C(85) C(86) 119(2) yes C(81) C(86) C(85) 121(1) yes P(4) C(91) C(92) 120(1) yes P(4) C(91) C(96) 123(1) yes C(92) C(91) C(96) 116(1) yes C(91) C(92) C(93) 119(1) yes C(92) C(93) C(94) 121(3) yes C(93) C(94) C(95) 117(2) yes C(94) C(95) C(96) 123(1) yes C(91) C(96) C(95) 120(2) yes P(4) C(101) C(102) 118.1(7) yes P(4) C(101) C(106) 122(1) yes C(102) C(101) C(106) 119(1) yes C(101) C(102) C(103) 119(1) yes C(102) C(103) C(104) 119(1) yes C(103) C(104) C(105) 120(1) yes C(104) C(105) C(106) 120(1) yes C(101) C(106) C(105) 119(1) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Rh(1) P(1) 2.259(2) yes Rh(1) N(1) 2.03(1) yes Rh(1) C(1) 2.042(9) yes Rh(1) C(01) 1.82(2) yes Rh(2) P(2) 2.230(4) yes Rh(2) N(2) 2.079(5) yes Rh(2) C(1) 2.44(2) yes Rh(2) C(2) 2.41(1) yes Rh(2) C(02) 1.83(1) yes Rh(3) P(3) 2.258(2) yes Rh(3) N(3) 2.042(9) yes Rh(3) C(2) 2.062(9) yes Rh(3) C(03) 1.81(1) yes Rh(4) P(4) 2.219(3) yes Rh(4) N(4) 2.069(6) yes Rh(4) C(1) 2.396(9) yes Rh(4) C(2) 2.44(1) yes Rh(4) C(04) 1.810(8) yes P(1) C(14) 1.84(2) yes P(1) C(31) 1.82(1) yes P(1) C(41) 1.84(2) yes P(2) C(15) 1.847(9) yes P(2) C(51) 1.81(2) yes P(2) C(61) 1.822(10) yes P(3) C(24) 1.86(1) yes P(3) C(71) 1.80(1) yes P(3) C(81) 1.81(2) yes P(4) C(25) 1.856(8) yes P(4) C(91) 1.83(2) yes P(4) C(101) 1.83(1) yes O(01) C(01) 1.15(2) yes O(02) C(02) 1.14(1) yes O(03) C(03) 1.16(2) yes O(04) C(04) 1.16(1) yes N(1) N(2) 1.35(2) yes N(1) C(11) 1.365(9) yes N(2) C(13) 1.37(2) yes N(3) N(4) 1.36(1) yes N(3) C(21) 1.359(8) yes N(4) C(23) 1.37(1) yes C(1) C(2) 1.22(1) yes C(11) C(12) 1.41(2) yes C(11) C(14) 1.49(2) yes C(12) C(13) 1.39(1) yes C(13) C(15) 1.48(2) yes C(21) C(22) 1.37(2) yes C(21) C(24) 1.48(2) yes C(22) C(23) 1.39(1) yes C(23) C(25) 1.49(2) yes C(31) C(32) 1.37(3) yes C(31) C(36) 1.39(2) yes C(32) C(33) 1.43(2) yes C(33) C(34) 1.29(3) yes C(34) C(35) 1.42(4) yes C(35) C(36) 1.40(2) yes C(41) C(42) 1.38(1) yes C(41) C(46) 1.38(2) yes C(42) C(43) 1.43(3) yes C(43) C(44) 1.35(3) yes C(44) C(45) 1.33(2) yes C(45) C(46) 1.37(3) yes C(51) C(52) 1.38(2) yes C(51) C(56) 1.39(1) yes C(52) C(53) 1.39(3) yes C(53) C(54) 1.36(1) yes C(54) C(55) 1.38(3) yes C(55) C(56) 1.37(2) yes C(61) C(62) 1.39(3) yes C(61) C(66) 1.39(2) yes C(62) C(63) 1.40(2) yes C(63) C(64) 1.36(2) yes C(64) C(65) 1.37(3) yes C(65) C(66) 1.42(2) yes C(71) C(72) 1.37(3) yes C(71) C(76) 1.40(2) yes C(72) C(73) 1.38(3) yes C(73) C(74) 1.38(2) yes C(74) C(75) 1.33(4) yes C(75) C(76) 1.39(3) yes C(81) C(82) 1.38(1) yes C(81) C(86) 1.37(2) yes C(82) C(83) 1.37(3) yes C(83) C(84) 1.37(4) yes C(84) C(85) 1.38(2) yes C(85) C(86) 1.35(4) yes C(91) C(92) 1.34(4) yes C(91) C(96) 1.35(1) yes C(92) C(93) 1.40(5) yes C(93) C(94) 1.30(3) yes C(94) C(95) 1.30(4) yes C(95) C(96) 1.35(3) yes C(101) C(102) 1.40(2) yes C(101) C(106) 1.38(1) yes C(102) C(103) 1.37(2) yes C(103) C(104) 1.40(2) yes C(104) C(105) 1.34(3) yes C(105) C(106) 1.40(2) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 Rh(2) C(52) 3.58(1) 3_576 O(01) C(94) 3.38(3) 2_556 O(01) C(34) 3.59(1) 4_475 O(02) C(65) 3.21(1) 4_465 O(02) C(64) 3.26(1) 4_465 O(03) C(52) 3.54(1) 3_576 N(1) C(53) 3.30(2) 3_576 N(2) C(53) 3.20(1) 3_576 N(2) C(52) 3.47(2) 3_576 C(13) C(53) 3.52(1) 3_576 C(22) C(63) 3.57(2) 4_465 C(22) C(64) 3.59(2) 4_465 C(33) C(93) 3.45(3) 2_556 C(34) C(93) 3.50(3) 2_556 C(35) C(74) 3.59(1) 1_654 C(54) C(76) 3.47(2) 2_446 C(63) C(106) 3.53(2) 4_564 C(63) C(105) 3.60(2) 4_564 C(64) C(102) 3.59(1) 4_564 C(65) C(84) 3.56(2) 2_446 _journal_paper_doi 10.1021/om049427v