# Copyright The Royal Society of Chemistry, 1998. #================================================================ data_stadi121 _publ_contact_author ; Prof. Dr. Dirk Steinborn Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; _publ_contact_author_phone '049 345 55-25620' _publ_contact_author_fax '049 345 55-27028' _publ_contact_author_email 'steinborn@chemie.uni-halle.de' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #================================================================ _publ_section_title ; Syntheses and structures of novel cyclic and dinuclear organorhodoximes - a homologous series of di- to pentamethylene-bridged complexes ; loop_ _publ_author_name _publ_author_address 'Steinborn, Dirk' ; Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; 'Rausch, Mario' ; Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; 'Bruhn, Clemens' ; Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; 'Schmidt, Harry' ; Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; 'Str\"ohl, Dieter' ; Institut f\"ur Anorganische Chemie Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle(Saale) Bundesrepublik Deutschland ; #================================================================ _audit_creation_method SHELXL _chemical_name_systematic ; \m-ethane-1,2-diyl-bis[bis(dimethylglyoximato-N,N')(triphenylphos phine) rhodium(III)] ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H62 N8 O8 P2 Rh2' _chemical_formula_weight 1218.88 _chemical_melting_point '215-220 \%C decomp.' _chemical_compound_source 'see text' 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.5199(15) _cell_length_b 9.931(2) _cell_length_c 16.721(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.278(11) _cell_angle_gamma 90.00 _cell_volume 2699.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 79 _cell_measurement_theta_min 10.25 _cell_measurement_theta_max 40.41 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method none _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type 'empirical via \y-scans' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'STOE Stadi4 4-circle-diffractometer' _diffrn_measurement_method '\w/2q' _diffrn_standards_number 1 _diffrn_standards_interval_count none _diffrn_standards_interval_time 1h _diffrn_standards_decay_% <1 _diffrn_reflns_number 8879 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4737 _reflns_number_observed 3678 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 ver. 1.05c (STOE, 1996)' _computing_cell_refinement 'STADI4 ver. 1.05c (STOE, 1996)' _computing_data_reduction 'X-red ver. 1.05 (STOE,1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEPIII (Johnson, C. K., 1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+1.1243P] 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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00091(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4732 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_obs 0.0318 _refine_ls_wR_factor_all 0.0836 _refine_ls_wR_factor_obs 0.0718 _refine_ls_goodness_of_fit_all 1.111 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.118 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.1129(3) 0.3814(4) -0.0364(3) 0.0596(12) Uani 1 d . . H1A H 0.0971(3) 0.3832(4) -0.0945(3) 0.072 Uiso 1 calc R . H1B H 0.1599(3) 0.4384(4) -0.0203(3) 0.072 Uiso 1 calc R . H1C H 0.0681(3) 0.4133(4) -0.0120(3) 0.072 Uiso 1 calc R . C2 C 0.1339(2) 0.2403(4) -0.0090(2) 0.0356(8) Uani 1 d . . C3 C 0.1604(2) 0.1356(4) -0.0605(2) 0.0347(8) Uani 1 d . . C4 C 0.1675(3) 0.1543(4) -0.1473(2) 0.0616(12) Uani 1 d . . H4A H 0.1614(3) 0.2479(4) -0.1612(2) 0.074 Uiso 1 calc R . H4B H 0.1253(3) 0.1034(4) -0.1811(2) 0.074 Uiso 1 calc R . H4C H 0.2205(3) 0.1235(4) -0.1556(2) 0.074 Uiso 1 calc R . C5 C 0.1124(3) -0.3821(4) 0.1870(3) 0.0585(11) Uani 1 d . . H5A H 0.0572(3) -0.3986(4) 0.1953(3) 0.070 Uiso 1 calc R . H5B H 0.1505(3) -0.4049(4) 0.2354(3) 0.070 Uiso 1 calc R . H5C H 0.1235(3) -0.4362(4) 0.1426(3) 0.070 Uiso 1 calc R . C6 C 0.1216(2) -0.2371(4) 0.1677(2) 0.0360(8) Uani 1 d . . C7 C 0.0994(2) -0.1307(4) 0.2204(2) 0.0348(8) Uani 1 d . . C8 C 0.0704(2) -0.1576(4) 0.2984(2) 0.0526(10) Uani 1 d . . H8A H 0.1157(2) -0.1889(4) 0.3383(2) 0.063 Uiso 1 calc R . H8B H 0.0281(2) -0.2250(4) 0.2898(2) 0.063 Uiso 1 calc R . H8C H 0.0488(2) -0.0761(4) 0.3173(2) 0.063 Uiso 1 calc R . C9 C 0.3319(2) 0.2099(4) 0.1497(2) 0.0322(7) Uani 1 d . . C10 C 0.4072(2) 0.2351(4) 0.1258(2) 0.0513(10) Uani 1 d . . H10 H 0.4385(2) 0.1635(4) 0.1123(2) 0.062 Uiso 1 calc R . C11 C 0.4360(3) 0.3657(5) 0.1220(3) 0.0690(14) Uani 1 d . . H11 H 0.4865(3) 0.3807(5) 0.1062(3) 0.083 Uiso 1 calc R . C12 C 0.3919(3) 0.4704(5) 0.1409(3) 0.0696(14) Uani 1 d . . H12 H 0.4118(3) 0.5576(5) 0.1384(3) 0.084 Uiso 1 calc R . C13 C 0.3173(3) 0.4486(5) 0.1638(3) 0.076(2) Uani 1 d . . H13 H 0.2864(3) 0.5216(5) 0.1761(3) 0.092 Uiso 1 calc R . C14 C 0.2874(2) 0.3183(4) 0.1688(3) 0.0550(11) Uani 1 d . . H14 H 0.2371(2) 0.3047(4) 0.1852(3) 0.066 Uiso 1 calc R . C15 C 0.3716(2) -0.0614(4) 0.1210(2) 0.0375(8) Uani 1 d . . C16 C 0.3697(2) -0.0881(5) 0.0403(2) 0.0511(11) Uani 1 d . . H16 H 0.3238(2) -0.0640(5) 0.0024(2) 0.061 Uiso 1 calc R . C17 C 0.4354(3) -0.1504(5) 0.0148(3) 0.0690(14) Uani 1 d . . H17 H 0.4340(3) -0.1653(5) -0.0404(3) 0.083 Uiso 1 calc R . C18 C 0.5019(3) -0.1901(5) 0.0695(3) 0.0717(14) Uani 1 d . . H18 H 0.5454(3) -0.2340(5) 0.0521(3) 0.086 Uiso 1 calc R . C19 C 0.5048(3) -0.1654(7) 0.1498(3) 0.090(2) Uani 1 d . . H19 H 0.5505(3) -0.1918(7) 0.1874(3) 0.108 Uiso 1 calc R . C20 C 0.4403(2) -0.1015(6) 0.1757(3) 0.0680(14) Uani 1 d . . H20 H 0.4428(2) -0.0850(6) 0.2308(3) 0.082 Uiso 1 calc R . C21 C 0.3031(2) -0.0037(4) 0.2611(2) 0.0336(7) Uani 1 d . . C22 C 0.2930(2) -0.1375(4) 0.2807(2) 0.0475(10) Uani 1 d . . H22 H 0.2852(2) -0.2017(4) 0.2396(2) 0.057 Uiso 1 calc R . C23 C 0.2943(2) -0.1775(5) 0.3599(3) 0.0611(13) Uani 1 d . . H23 H 0.2871(2) -0.2676(5) 0.3720(3) 0.073 Uiso 1 calc R . C24 C 0.3063(3) -0.0821(6) 0.4209(3) 0.0695(14) Uani 1 d . . H24 H 0.3067(3) -0.1078(6) 0.4744(3) 0.083 Uiso 1 calc R . C25 C 0.3174(3) 0.0486(6) 0.4031(2) 0.0667(13) Uani 1 d . . H25 H 0.3266(3) 0.1117(6) 0.4448(2) 0.080 Uiso 1 calc R . C26 C 0.3154(2) 0.0902(4) 0.3231(2) 0.0482(10) Uani 1 d . . H26 H 0.3223(2) 0.1806(4) 0.3115(2) 0.058 Uiso 1 calc R . C27A C 0.0139(8) -0.0075(12) 0.0432(8) 0.026(2) Uani 0.50 d P . H27A H -0.0051(8) -0.0940(12) 0.0595(8) 0.031 Uiso 0.50 calc PR . H27B H -0.0124(8) 0.0615(12) 0.0707(8) 0.031 Uiso 0.50 calc PR . C27B C 0.0248(9) -0.0525(12) 0.0259(10) 0.039(3) Uani 0.50 d P . H27C H 0.0302(9) -0.1299(12) -0.0081(10) 0.047 Uiso 0.50 calc PR . H27D H -0.0063(9) -0.0813(12) 0.0669(10) 0.047 Uiso 0.50 calc PR . N1 N 0.1250(2) 0.1968(3) 0.0616(2) 0.0315(6) Uani 1 d . . N2 N 0.1693(2) 0.0167(3) -0.0266(2) 0.0316(6) Uani 1 d . . N3 N 0.1490(2) -0.1931(3) 0.1049(2) 0.0349(7) Uani 1 d . . N4 N 0.1070(2) -0.0094(3) 0.1928(2) 0.0311(6) Uani 1 d . . O1 O 0.09412(14) 0.2804(3) 0.1143(2) 0.0441(6) Uani 1 d . . H1 H 0.10142(14) 0.2463(3) 0.1596(2) 0.053 Uiso 1 calc R . O2 O 0.18611(15) -0.0919(2) -0.06563(14) 0.0417(6) Uani 1 d . . O3 O 0.1700(2) -0.2815(3) 0.0487(2) 0.0537(7) Uani 1 d . . H3 H 0.1768(2) -0.2399(3) 0.0080(2) 0.064 Uiso 1 calc R . O4 O 0.0874(2) 0.1001(3) 0.22982(14) 0.0446(6) Uani 1 d . . P P 0.29028(5) 0.03887(9) 0.15299(5) 0.0277(2) Uani 1 d . . Rh Rh 0.145511(14) 0.00455(3) 0.086290(14) 0.02544(10) Uani 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 0.075(3) 0.042(2) 0.064(3) 0.019(2) 0.018(2) 0.006(2) C2 0.033(2) 0.032(2) 0.042(2) 0.003(2) 0.0055(15) -0.006(2) C3 0.034(2) 0.039(2) 0.031(2) 0.000(2) 0.0053(14) -0.006(2) C4 0.091(3) 0.054(3) 0.043(2) 0.005(2) 0.020(2) -0.004(3) C5 0.071(3) 0.036(2) 0.072(3) 0.009(2) 0.021(2) 0.000(2) C6 0.032(2) 0.032(2) 0.043(2) 0.003(2) 0.0045(15) -0.002(2) C7 0.028(2) 0.037(2) 0.039(2) 0.005(2) 0.0071(14) 0.000(2) C8 0.056(2) 0.054(3) 0.052(2) 0.012(2) 0.022(2) -0.001(2) C9 0.029(2) 0.040(2) 0.026(2) -0.0008(14) 0.0001(13) -0.006(2) C10 0.056(2) 0.053(3) 0.051(2) -0.011(2) 0.027(2) -0.015(2) C11 0.081(3) 0.076(4) 0.056(3) -0.003(2) 0.028(2) -0.042(3) C12 0.085(4) 0.050(3) 0.068(3) 0.009(2) -0.003(3) -0.024(3) C13 0.062(3) 0.037(3) 0.119(4) -0.009(3) -0.013(3) 0.003(2) C14 0.040(2) 0.043(2) 0.078(3) -0.010(2) -0.001(2) -0.003(2) C15 0.026(2) 0.043(2) 0.044(2) -0.005(2) 0.0084(14) 0.002(2) C16 0.032(2) 0.075(3) 0.046(2) -0.013(2) 0.006(2) 0.003(2) C17 0.048(2) 0.101(4) 0.061(3) -0.033(3) 0.019(2) -0.001(3) C18 0.048(2) 0.086(4) 0.085(3) -0.019(3) 0.020(2) 0.023(3) C19 0.055(3) 0.141(6) 0.074(3) 0.007(3) 0.011(2) 0.054(3) C20 0.050(2) 0.106(4) 0.047(2) 0.002(2) 0.004(2) 0.034(3) C21 0.0247(15) 0.041(2) 0.034(2) 0.006(2) 0.0025(12) -0.005(2) C22 0.044(2) 0.051(3) 0.044(2) 0.009(2) -0.002(2) -0.008(2) C23 0.055(3) 0.068(3) 0.057(3) 0.031(2) -0.001(2) -0.011(2) C24 0.063(3) 0.105(4) 0.040(2) 0.030(3) 0.008(2) -0.015(3) C25 0.077(3) 0.089(4) 0.034(2) -0.003(2) 0.009(2) -0.011(3) C26 0.052(2) 0.059(3) 0.035(2) -0.003(2) 0.010(2) -0.010(2) C27A 0.017(4) 0.024(7) 0.037(6) 0.001(5) 0.002(3) -0.001(5) C27B 0.024(5) 0.026(8) 0.064(9) 0.001(5) -0.003(5) -0.003(5) N1 0.0288(14) 0.030(2) 0.036(2) -0.0028(12) 0.0054(12) -0.0001(12) N2 0.0286(13) 0.035(2) 0.0314(14) -0.0037(12) 0.0051(11) -0.0017(12) N3 0.037(2) 0.032(2) 0.035(2) -0.0026(13) 0.0042(13) -0.0003(13) N4 0.0246(12) 0.036(2) 0.0337(14) 0.0002(13) 0.0076(11) 0.0001(12) O1 0.0452(14) 0.0395(15) 0.0507(15) -0.0046(12) 0.0165(12) 0.0058(12) O2 0.0494(14) 0.0404(15) 0.0369(13) -0.0100(11) 0.0121(11) 0.0004(12) O3 0.076(2) 0.038(2) 0.052(2) -0.0102(13) 0.0253(14) 0.0003(14) O4 0.054(2) 0.0395(15) 0.0446(14) -0.0038(12) 0.0210(12) 0.0062(13) P 0.0237(4) 0.0325(5) 0.0270(4) -0.0006(3) 0.0044(3) -0.0008(3) Rh 0.02325(14) 0.0265(2) 0.02626(14) 0.00013(11) 0.00349(9) -0.00109(11) _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 C2 1.497(5) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 N1 1.291(4) . ? C2 C3 1.466(5) . ? C3 N2 1.307(4) . ? C3 C4 1.488(5) . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.489(5) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 N3 1.293(4) . ? C6 C7 1.464(5) . ? C7 N4 1.304(4) . ? C7 C8 1.491(5) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C14 1.374(5) . ? C9 C10 1.395(5) . ? C9 P 1.837(4) . ? C10 C11 1.386(6) . ? C10 H10 0.93 . ? C11 C12 1.340(7) . ? C11 H11 0.93 . ? C12 C13 1.372(7) . ? C12 H12 0.93 . ? C13 C14 1.393(6) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C16 1.370(5) . ? C15 C20 1.382(5) . ? C15 P 1.827(3) . ? C16 C17 1.382(5) . ? C16 H16 0.93 . ? C17 C18 1.357(6) . ? C17 H17 0.93 . ? C18 C19 1.357(6) . ? C18 H18 0.93 . ? C19 C20 1.376(6) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C26 1.382(5) . ? C21 C22 1.386(5) . ? C21 P 1.831(3) . ? C22 C23 1.378(5) . ? C22 H22 0.93 . ? C23 C24 1.380(7) . ? C23 H23 0.93 . ? C24 C25 1.351(7) . ? C24 H24 0.93 . ? C25 C26 1.395(5) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27A C27A 1.44(3) 3 ? C27A Rh 2.168(14) . ? C27A H27A 0.97 . ? C27A H27B 0.97 . ? C27B C27B 1.50(3) 3 ? C27B Rh 2.145(15) . ? C27B H27C 0.97 . ? C27B H27D 0.97 . ? N1 O1 1.372(3) . ? N1 Rh 1.970(3) . ? N2 O2 1.316(3) . ? N2 Rh 1.999(3) . ? N3 O3 1.375(4) . ? N3 Rh 1.987(3) . ? N4 O4 1.320(3) . ? N4 Rh 1.999(3) . ? O1 H1 0.82 . ? O3 H3 0.82 . ? P Rh 2.4755(9) . ? 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 C2 C1 H1A 109.5(2) . . ? C2 C1 H1B 109.5(2) . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5(2) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 113.3(3) . . ? N1 C2 C1 122.3(3) . . ? C3 C2 C1 124.2(3) . . ? N2 C3 C2 114.0(3) . . ? N2 C3 C4 120.9(3) . . ? C2 C3 C4 124.7(3) . . ? C3 C4 H4A 109.5(2) . . ? C3 C4 H4B 109.5(2) . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5(2) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 H5A 109.5(2) . . ? C6 C5 H5B 109.5(2) . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5(2) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 114.0(3) . . ? N3 C6 C5 124.5(3) . . ? C7 C6 C5 121.5(3) . . ? N4 C7 C6 113.8(3) . . ? N4 C7 C8 122.8(3) . . ? C6 C7 C8 123.4(3) . . ? C7 C8 H8A 109.5(2) . . ? C7 C8 H8B 109.5(2) . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5(2) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 117.9(4) . . ? C14 C9 P 119.9(3) . . ? C10 C9 P 122.2(3) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6(3) . . ? C9 C10 H10 119.6(2) . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11 119.7(3) . . ? C10 C11 H11 119.7(3) . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12 120.1(3) . . ? C13 C12 H12 120.1(3) . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7(3) . . ? C14 C13 H13 119.7(3) . . ? C9 C14 C13 120.2(4) . . ? C9 C14 H14 119.9(2) . . ? C13 C14 H14 119.9(3) . . ? C16 C15 C20 117.8(3) . . ? C16 C15 P 120.3(3) . . ? C20 C15 P 121.5(3) . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16 119.6(2) . . ? C17 C16 H16 119.6(3) . . ? C18 C17 C16 120.5(4) . . ? C18 C17 H17 119.8(3) . . ? C16 C17 H17 119.8(3) . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1(3) . . ? C17 C18 H18 120.1(3) . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19 119.9(3) . . ? C20 C19 H19 119.9(3) . . ? C19 C20 C15 121.1(4) . . ? C19 C20 H20 119.5(3) . . ? C15 C20 H20 119.5(2) . . ? C26 C21 C22 118.4(3) . . ? C26 C21 P 124.1(3) . . ? C22 C21 P 117.3(3) . . ? C23 C22 C21 121.5(4) . . ? C23 C22 H22 119.2(3) . . ? C21 C22 H22 119.2(2) . . ? C22 C23 C24 119.1(4) . . ? C22 C23 H23 120.4(3) . . ? C24 C23 H23 120.4(3) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.9(3) . . ? C23 C24 H24 119.9(3) . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25 119.5(3) . . ? C26 C25 H25 119.5(3) . . ? C21 C26 C25 119.7(4) . . ? C21 C26 H26 120.2(2) . . ? C25 C26 H26 120.2(3) . . ? C27A C27A Rh 116.6(12) 3 . ? C27A C27A H27A 108.1(10) 3 . ? Rh C27A H27A 108.1(4) . . ? C27A C27A H27B 108.1(8) 3 . ? Rh C27A H27B 108.1(3) . . ? H27A C27A H27B 107.3 . . ? C27B C27B Rh 117.0(13) 3 . ? C27B C27B H27C 108.1(10) 3 . ? Rh C27B H27C 108.1(3) . . ? C27B C27B H27D 108.1(12) 3 . ? Rh C27B H27D 108.1(5) . . ? H27C C27B H27D 107.3 . . ? C2 N1 O1 120.1(3) . . ? C2 N1 Rh 118.1(2) . . ? O1 N1 Rh 121.5(2) . . ? C3 N2 O2 122.8(3) . . ? C3 N2 Rh 116.1(2) . . ? O2 N2 Rh 120.9(2) . . ? C6 N3 O3 120.5(3) . . ? C6 N3 Rh 117.2(2) . . ? O3 N3 Rh 121.9(2) . . ? C7 N4 O4 123.1(3) . . ? C7 N4 Rh 116.5(2) . . ? O4 N4 Rh 120.3(2) . . ? N1 O1 H1 109.5(2) . . ? N3 O3 H3 109.5(2) . . ? C15 P C21 101.6(2) . . ? C15 P C9 101.3(2) . . ? C21 P C9 105.38(15) . . ? C15 P Rh 119.67(11) . . ? C21 P Rh 110.19(10) . . ? C9 P Rh 116.79(10) . . ? N1 Rh N3 171.71(11) . . ? N1 Rh N2 78.43(11) . . ? N3 Rh N2 101.66(11) . . ? N1 Rh N4 100.55(11) . . ? N3 Rh N4 78.32(11) . . ? N2 Rh N4 172.92(10) . . ? N1 Rh C27B 92.7(4) . . ? N3 Rh C27B 79.1(4) . . ? N2 Rh C27B 84.0(5) . . ? N4 Rh C27B 89.1(5) . . ? N1 Rh C27A 81.9(4) . . ? N3 Rh C27A 89.8(4) . . ? N2 Rh C27A 92.6(4) . . ? N4 Rh C27A 80.4(4) . . ? C27B Rh C27A 15.4(3) . . ? N1 Rh P 94.44(8) . . ? N3 Rh P 93.82(8) . . ? N2 Rh P 94.59(8) . . ? N4 Rh P 92.48(7) . . ? C27B Rh P 172.3(3) . . ? C27A Rh P 171.2(3) . . ? 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 Rh C27A C27A Rh 180.0 . . 3 3 ? _refine_diff_density_max 0.456 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.065 #================================================================ #=END