# Copyright The Royal Society of Chemistry, 1998. data_ipds114 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H34 N4 O4 P Rh' _chemical_formula_weight 636.48 _chemical_melting_point '170-172 \% 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 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.298(2) _cell_length_b 11.928(2) _cell_length_c 33.903(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.232(12) _cell_angle_gamma 90.00 _cell_volume 6088.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method none _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Image Plate Detection System' _diffrn_measurement_method ; The reciprocical space was scanned with 133 images each of which with an exposure time of 5 min and a rotation angle of 1.5 degrees. ; _diffrn_standards_number 'max. 50 per image' _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% <1 _diffrn_reflns_number 25709 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 23.97 _reflns_number_total 4725 _reflns_number_observed 3410 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Stoe IPDS-software (STOE publication 4805-010, 1996) ; _computing_cell_refinement ; Stoe IPDS-software (STOE publication 4805-010, 1996) ; _computing_data_reduction ; Stoe IPDS-software (STOE publication 4805-010, 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 0 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^)+(0.1260P)^2^+46.1524P] 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 none _refine_ls_extinction_coef none _refine_ls_number_reflns 4725 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_obs 0.0649 _refine_ls_wR_factor_all 0.2269 _refine_ls_wR_factor_obs 0.2063 _refine_ls_goodness_of_fit_all 1.116 _refine_ls_goodness_of_fit_obs 1.206 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.206 _refine_ls_shift/esd_max -0.001 _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 Rh Rh 0.27740(4) 0.12161(6) 0.36746(2) 0.0326(3) Uani 1 d . . C1 C 0.1620(8) -0.1336(10) 0.4321(4) 0.067(3) Uani 1 d . . H1A H 0.2042(8) -0.1938(10) 0.4372(4) 0.080 Uiso 1 calc R . H1B H 0.1044(8) -0.1634(10) 0.4214(4) 0.080 Uiso 1 calc R . H1C H 0.1597(8) -0.0945(10) 0.4566(4) 0.080 Uiso 1 calc R . C2 C 0.1896(6) -0.0551(8) 0.4028(3) 0.039(2) Uani 1 d . . C3 C 0.1633(6) -0.0719(9) 0.3607(3) 0.046(2) Uani 1 d . . C4 C 0.0994(7) -0.1598(10) 0.3411(4) 0.062(3) Uani 1 d . . H4A H 0.0756(7) -0.2001(10) 0.3613(4) 0.075 Uiso 1 calc R . H4B H 0.1300(7) -0.2109(10) 0.3264(4) 0.075 Uiso 1 calc R . H4C H 0.0519(7) -0.1244(10) 0.3231(4) 0.075 Uiso 1 calc R . C5 C 0.4155(7) 0.3191(10) 0.2918(3) 0.056(3) Uani 1 d . . H5A H 0.4792(7) 0.3218(10) 0.2985(3) 0.067 Uiso 1 calc R . H5B H 0.3926(7) 0.3938(10) 0.2872(3) 0.067 Uiso 1 calc R . H5C H 0.3984(7) 0.2751(10) 0.2679(3) 0.067 Uiso 1 calc R . C6 C 0.3786(6) 0.2666(8) 0.3258(3) 0.039(2) Uani 1 d . . C7 C 0.3987(6) 0.3042(8) 0.3671(3) 0.038(2) Uani 1 d . . C8 C 0.4582(7) 0.4015(9) 0.3816(4) 0.061(3) Uani 1 d . . H8A H 0.4497(7) 0.4598(9) 0.3617(4) 0.074 Uiso 1 calc R . H8B H 0.5191(7) 0.3774(9) 0.3860(4) 0.074 Uiso 1 calc R . H8C H 0.4439(7) 0.4295(9) 0.4062(4) 0.074 Uiso 1 calc R . C9 C 0.0552(5) 0.2451(8) 0.3189(2) 0.037(2) Uani 1 d . . C10 C 0.0148(6) 0.1425(9) 0.3126(3) 0.050(3) Uani 1 d . . H10 H 0.0407(6) 0.0802(9) 0.3266(3) 0.060 Uiso 1 calc R . C11 C -0.0653(7) 0.1302(10) 0.2853(3) 0.064(3) Uani 1 d . . H11 H -0.0915(7) 0.0599(10) 0.2810(3) 0.077 Uiso 1 calc R . C12 C -0.1046(6) 0.2209(11) 0.2653(3) 0.057(3) Uani 1 d . . H12 H -0.1576(6) 0.2130(11) 0.2472(3) 0.069 Uiso 1 calc R . C13 C -0.0646(7) 0.3257(11) 0.2721(3) 0.056(3) Uani 1 d . . H13 H -0.0912(7) 0.3883(11) 0.2586(3) 0.067 Uiso 1 calc R . C14 C 0.0141(6) 0.3368(10) 0.2986(3) 0.051(3) Uani 1 d . . H14 H 0.0401(6) 0.4072(10) 0.3030(3) 0.061 Uiso 1 calc R . C15 C 0.1924(6) 0.3985(8) 0.3523(3) 0.041(2) Uani 1 d . . C16 C 0.2153(6) 0.4266(9) 0.3146(3) 0.048(2) Uani 1 d . . H16 H 0.2067(6) 0.3745(9) 0.2939(3) 0.058 Uiso 1 calc R . C17 C 0.2505(7) 0.5320(10) 0.3086(3) 0.058(3) Uani 1 d . . H17 H 0.2641(7) 0.5500(10) 0.2837(3) 0.069 Uiso 1 calc R . C18 C 0.2653(7) 0.6099(10) 0.3393(4) 0.065(3) Uani 1 d . . H18 H 0.2890(7) 0.6800(10) 0.3354(4) 0.078 Uiso 1 calc R . C19 C 0.2442(8) 0.5814(11) 0.3759(4) 0.069(3) Uani 1 d . . H19 H 0.2544(8) 0.6332(11) 0.3967(4) 0.082 Uiso 1 calc R . C20 C 0.2080(7) 0.4767(9) 0.3828(3) 0.051(3) Uani 1 d . . H20 H 0.1946(7) 0.4600(9) 0.4078(3) 0.061 Uiso 1 calc R . C21 C 0.1012(6) 0.2664(8) 0.4044(2) 0.037(2) Uani 1 d . . C22 C 0.1530(6) 0.2419(9) 0.4410(2) 0.045(2) Uani 1 d . . H22 H 0.2129(6) 0.2253(9) 0.4425(2) 0.054 Uiso 1 calc R . C23 C 0.1161(7) 0.2417(10) 0.4759(3) 0.056(3) Uani 1 d . . H23 H 0.1511(7) 0.2232(10) 0.5004(3) 0.068 Uiso 1 calc R . C24 C 0.0287(7) 0.2689(10) 0.4740(3) 0.061(3) Uani 1 d . . H24 H 0.0041(7) 0.2692(10) 0.4972(3) 0.074 Uiso 1 calc R . C25 C -0.0232(7) 0.2958(10) 0.4376(3) 0.060(3) Uani 1 d . . H25 H -0.0824(7) 0.3155(10) 0.4363(3) 0.072 Uiso 1 calc R . C26 C 0.0132(7) 0.2935(10) 0.4025(3) 0.053(3) Uani 1 d . . H26 H -0.0222(7) 0.3103(10) 0.3779(3) 0.064 Uiso 1 calc R . C27 C 0.3887(6) 0.0138(9) 0.3817(3) 0.047(2) Uani 1 d . . H27A H 0.3708(6) -0.0625(9) 0.3743(3) 0.056 Uiso 1 calc R . H27B H 0.4337(6) 0.0356(9) 0.3663(3) 0.056 Uiso 1 calc R . C28 C 0.4286(7) 0.0189(10) 0.4274(3) 0.058(3) Uani 1 d . . H28A H 0.4833(7) -0.0241(10) 0.4319(3) 0.070 Uiso 1 calc R . H28B H 0.4442(7) 0.0962(10) 0.4342(3) 0.070 Uiso 1 calc R . C29 C 0.3703(7) -0.0234(10) 0.4558(3) 0.057(3) Uani 1 d . . H29A H 0.3579(7) -0.1023(10) 0.4505(3) 0.068 Uiso 1 calc R . H29B H 0.4026(7) -0.0170(10) 0.4831(3) 0.068 Uiso 1 calc R . N1 N 0.2410(4) 0.0307(6) 0.4122(2) 0.037(2) Uani 1 d . . N2 N 0.2028(5) -0.0034(7) 0.3390(2) 0.044(2) Uani 1 d . . N3 N 0.3223(5) 0.1839(7) 0.3204(2) 0.039(2) Uani 1 d . . N4 N 0.3573(4) 0.2502(6) 0.3920(2) 0.035(2) Uani 1 d . . O1 O 0.2854(4) 0.0372(6) 0.4528(2) 0.050(2) Uani 1 d . . O2 O 0.1909(4) -0.0114(6) 0.2990(2) 0.057(2) Uani 1 d . . O3 O 0.2976(5) 0.1412(6) 0.2822(2) 0.055(2) Uani 1 d . . H3 H 0.2622(5) 0.0897(6) 0.2826(2) 0.066 Uiso 1 calc R . O4 O 0.3676(4) 0.2796(6) 0.4295(2) 0.052(2) Uani 1 d . . P P 0.15276(15) 0.2576(2) 0.35906(6) 0.0351(6) 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 Rh 0.0346(4) 0.0432(5) 0.0192(4) -0.0018(3) 0.0026(3) 0.0002(3) C1 0.069(7) 0.053(7) 0.084(9) 0.014(6) 0.028(6) -0.001(6) C2 0.038(5) 0.046(6) 0.036(5) -0.001(4) 0.012(4) 0.005(4) C3 0.036(5) 0.048(6) 0.052(6) -0.006(5) 0.005(4) 0.002(5) C4 0.049(6) 0.058(7) 0.080(8) -0.013(6) 0.012(6) -0.009(5) C5 0.052(6) 0.073(8) 0.048(6) 0.013(6) 0.023(5) 0.010(6) C6 0.040(5) 0.042(6) 0.035(5) 0.009(4) 0.009(4) 0.010(4) C7 0.039(5) 0.047(6) 0.029(5) 0.004(4) 0.005(4) -0.001(4) C8 0.056(6) 0.063(8) 0.068(7) -0.001(6) 0.017(5) -0.017(5) C9 0.034(5) 0.057(6) 0.020(4) 0.005(4) 0.000(3) 0.005(4) C10 0.039(5) 0.063(7) 0.044(6) 0.006(5) -0.005(4) -0.006(5) C11 0.056(7) 0.071(8) 0.059(7) 0.000(6) -0.005(5) -0.014(6) C12 0.035(5) 0.093(10) 0.038(6) -0.002(6) -0.009(4) 0.005(6) C13 0.051(6) 0.087(9) 0.026(5) 0.006(5) -0.005(4) 0.019(6) C14 0.048(6) 0.073(8) 0.032(5) 0.003(5) 0.008(4) 0.007(5) C15 0.033(5) 0.053(7) 0.035(5) 0.005(4) 0.000(4) 0.008(4) C16 0.050(6) 0.057(7) 0.039(5) 0.002(5) 0.011(4) 0.007(5) C17 0.055(6) 0.056(7) 0.064(7) 0.017(6) 0.017(5) 0.014(5) C18 0.055(7) 0.054(8) 0.086(9) 0.016(7) 0.012(6) 0.006(5) C19 0.062(7) 0.065(8) 0.076(9) -0.023(7) 0.004(6) -0.005(6) C20 0.054(6) 0.056(7) 0.043(6) -0.010(5) 0.009(4) -0.003(5) C21 0.040(5) 0.047(6) 0.024(4) 0.002(4) 0.004(4) 0.000(4) C22 0.048(5) 0.062(7) 0.025(5) -0.001(4) 0.004(4) 0.010(5) C23 0.062(7) 0.079(8) 0.025(5) -0.002(5) 0.001(4) 0.013(6) C24 0.072(7) 0.080(9) 0.037(6) -0.001(6) 0.024(5) 0.003(6) C25 0.046(6) 0.092(9) 0.046(6) -0.002(6) 0.017(5) 0.010(6) C26 0.053(6) 0.075(8) 0.033(5) 0.010(5) 0.013(4) 0.016(5) C27 0.048(5) 0.047(6) 0.045(5) 0.001(5) 0.006(4) 0.008(5) C28 0.048(6) 0.065(8) 0.058(7) 0.011(6) 0.001(5) 0.006(5) C29 0.057(6) 0.070(8) 0.037(5) 0.009(5) -0.007(4) 0.009(6) N1 0.038(4) 0.047(5) 0.024(4) -0.002(3) 0.002(3) 0.003(4) N2 0.038(4) 0.054(5) 0.038(4) -0.013(4) 0.002(3) -0.002(4) N3 0.045(4) 0.053(5) 0.017(4) -0.003(3) 0.006(3) 0.010(4) N4 0.040(4) 0.043(5) 0.021(4) -0.004(3) 0.001(3) 0.001(3) O1 0.061(4) 0.060(5) 0.028(3) 0.004(3) 0.004(3) 0.007(3) O2 0.064(4) 0.077(5) 0.027(3) -0.019(3) -0.001(3) -0.009(4) O3 0.066(4) 0.079(5) 0.020(3) -0.008(3) 0.004(3) -0.002(4) O4 0.061(4) 0.063(5) 0.030(4) -0.007(3) 0.002(3) -0.007(4) P 0.0368(12) 0.048(2) 0.0191(10) 0.0005(10) 0.0013(8) 0.0035(10) _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 Rh N3 1.989(7) . ? Rh N2 2.016(8) . ? Rh N1 2.022(7) . ? Rh N4 2.044(7) . ? Rh C27 2.120(9) . ? Rh P 2.481(2) . ? C1 C2 1.480(14) . ? C2 N1 1.295(12) . ? C2 C3 1.426(13) . ? C3 N2 1.314(13) . ? C3 C4 1.505(14) . ? C5 C6 1.510(13) . ? C6 N3 1.300(12) . ? C6 C7 1.451(12) . ? C7 N4 1.309(11) . ? C7 C8 1.502(13) . ? C9 C10 1.371(13) . ? C9 C14 1.382(13) . ? C9 P 1.838(8) . ? C10 C11 1.406(13) . ? C11 C12 1.36(2) . ? C12 C13 1.39(2) . ? C13 C14 1.376(13) . ? C15 C20 1.382(13) . ? C15 C16 1.424(13) . ? C15 P 1.816(10) . ? C16 C17 1.397(15) . ? C17 C18 1.39(2) . ? C18 C19 1.38(2) . ? C19 C20 1.40(2) . ? C21 C26 1.375(13) . ? C21 C22 1.381(12) . ? C21 P 1.850(8) . ? C22 C23 1.398(13) . ? C23 C24 1.367(14) . ? C24 C25 1.384(14) . ? C25 C26 1.399(13) . ? C27 C28 1.563(13) . ? C28 C29 1.514(14) . ? C29 O1 1.474(12) . ? N1 O1 1.424(9) . ? N2 O2 1.339(9) . ? N3 O3 1.380(9) . ? N4 O4 1.303(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 N3 Rh N2 98.1(3) . . ? N3 Rh N1 169.2(3) . . ? N2 Rh N1 75.7(3) . . ? N3 Rh N4 77.2(3) . . ? N2 Rh N4 175.2(3) . . ? N1 Rh N4 108.8(3) . . ? N3 Rh C27 91.7(3) . . ? N2 Rh C27 91.3(4) . . ? N1 Rh C27 79.7(3) . . ? N4 Rh C27 88.0(3) . . ? N3 Rh P 91.8(2) . . ? N2 Rh P 94.0(2) . . ? N1 Rh P 97.4(2) . . ? N4 Rh P 87.0(2) . . ? C27 Rh P 173.1(3) . . ? N1 C2 C3 114.2(8) . . ? N1 C2 C1 124.5(9) . . ? C3 C2 C1 121.3(10) . . ? N2 C3 C2 113.3(8) . . ? N2 C3 C4 120.9(9) . . ? C2 C3 C4 125.8(10) . . ? N3 C6 C7 113.1(8) . . ? N3 C6 C5 122.4(9) . . ? C7 C6 C5 124.5(9) . . ? N4 C7 C6 115.1(8) . . ? N4 C7 C8 120.4(8) . . ? C6 C7 C8 124.4(8) . . ? C10 C9 C14 118.4(8) . . ? C10 C9 P 118.1(7) . . ? C14 C9 P 122.9(8) . . ? C9 C10 C11 120.8(10) . . ? C12 C11 C10 120.2(11) . . ? C11 C12 C13 119.3(9) . . ? C14 C13 C12 120.2(10) . . ? C13 C14 C9 121.2(11) . . ? C20 C15 C16 118.4(10) . . ? C20 C15 P 123.2(8) . . ? C16 C15 P 118.2(8) . . ? C17 C16 C15 120.4(10) . . ? C18 C17 C16 120.6(11) . . ? C19 C18 C17 118.6(11) . . ? C18 C19 C20 122.1(11) . . ? C15 C20 C19 119.8(10) . . ? C26 C21 C22 119.5(8) . . ? C26 C21 P 122.2(6) . . ? C22 C21 P 118.3(7) . . ? C21 C22 C23 120.5(9) . . ? C24 C23 C22 120.0(9) . . ? C23 C24 C25 119.8(9) . . ? C24 C25 C26 120.3(10) . . ? C21 C26 C25 119.9(9) . . ? C28 C27 Rh 111.0(7) . . ? C29 C28 C27 116.6(8) . . ? O1 C29 C28 113.8(8) . . ? C2 N1 O1 116.5(7) . . ? C2 N1 Rh 118.3(6) . . ? O1 N1 Rh 123.2(5) . . ? C3 N2 O2 121.9(8) . . ? C3 N2 Rh 118.1(6) . . ? O2 N2 Rh 120.0(6) . . ? C6 N3 O3 118.5(7) . . ? C6 N3 Rh 119.0(6) . . ? O3 N3 Rh 122.5(6) . . ? O4 N4 C7 120.5(7) . . ? O4 N4 Rh 124.0(5) . . ? C7 N4 Rh 115.5(6) . . ? N1 O1 C29 107.7(6) . . ? C15 P C9 103.1(4) . . ? C15 P C21 104.7(4) . . ? C9 P C21 102.1(4) . . ? C15 P Rh 110.7(3) . . ? C9 P Rh 122.6(3) . . ? C21 P Rh 112.0(3) . . ? _refine_diff_density_max 2.199 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.174 #=================================END