# 1. SUBMISSION DETAILS _publ_contact_author ; Martin Nieger Laboratory of Inorganic Chemistry Department of Chemistry Universitity of Helsinki P.O. Box 55 FIN-00014 University of Helsinki Finland ; _publ_contact_author_phone '++358 2941 50192' _publ_contact_author_fax ? _publ_contact_author_email 'martin.nieger@helsinki.fi' _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? _publ_contact_letter ; enclosed you will find the necessary data for our publication in Orgtanometallics ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Bis(imino)phosphanes - Synthesis and Coordination Chemistry ; loop_ _publ_author_name _publ_author_address 'van Dijk, Tom' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Rong, Mark K. ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Borger, Jaap E.' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Boom, Devin H. A.' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Nieger, Martin' ; Laboratory of Inorganic Chemistry Department of Chemistry Universitity of Helsinki P.O. Box 55 FIN-00014 University of Helsinki Finland ; 'Slootweg, J. Chris' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Lamertsma, Koops' ; Department of Chemistry Univeristy of Johannesburg Auckland Park Johannesburg, 2006 South Africa ; #============================================================================== data_jcs011_m_compound_5d _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Z)-N-(1-(((E)-2,2-dimethyl-1-(phenylimino)propyl)(phenyl)phosphino)- 2,2-dimethylpropylidene)-2,4,6-trimethylaniline ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H39 N2 P' _chemical_formula_sum 'C31 H39 N2 P' _chemical_formula_weight 470.61 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' 'P' 'P' 0.1023 0.0942 '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 14.0810(10) _cell_length_b 11.9795(11) _cell_length_c 15.9550(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.047(7) _cell_angle_gamma 90.00 _cell_volume 2691.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 486 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.9955 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; dx = 35 mm, 60 sec./deg., 2 deg., 12 sets, 456 frames ; _diffrn_ambient_temperature 123(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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 2 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64257 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6159 _reflns_number_gt 5140 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement EVALCCD _computing_data_reduction EVALCCd _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0368P)^2^+1.5401P] 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 6159 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 P1 P 0.76604(2) 0.28686(3) 0.73602(2) 0.01539(8) Uani 1 1 d . . . N1 N 0.62036(7) 0.26560(9) 0.62972(7) 0.0168(2) Uani 1 1 d . . . N2 N 0.86239(8) 0.29105(9) 0.57797(7) 0.0179(2) Uani 1 1 d . . . C1 C 0.63684(9) 0.27697(10) 0.70795(8) 0.0154(2) Uani 1 1 d . . . C2 C 0.56549(9) 0.27756(11) 0.78156(8) 0.0177(3) Uani 1 1 d . . . C3 C 0.47128(10) 0.33544(12) 0.75924(9) 0.0239(3) Uani 1 1 d . . . H3A H 0.4836 0.4135 0.7444 0.036 Uiso 1 1 calc R . . H3B H 0.4284 0.3325 0.8075 0.036 Uiso 1 1 calc R . . H3C H 0.4418 0.2972 0.7115 0.036 Uiso 1 1 calc R . . C4 C 0.60656(11) 0.33737(14) 0.85895(9) 0.0276(3) Uani 1 1 d . . . H4A H 0.6668 0.3024 0.8749 0.041 Uiso 1 1 calc R . . H4B H 0.5616 0.3316 0.9056 0.041 Uiso 1 1 calc R . . H4C H 0.6174 0.4162 0.8457 0.041 Uiso 1 1 calc R . . C5 C 0.54711(10) 0.15478(12) 0.80500(9) 0.0234(3) Uani 1 1 d . . . H5A H 0.6074 0.1185 0.8191 0.035 Uiso 1 1 calc R . . H5B H 0.5178 0.1162 0.7574 0.035 Uiso 1 1 calc R . . H5C H 0.5044 0.1515 0.8534 0.035 Uiso 1 1 calc R . . C6 C 0.53081(9) 0.24994(11) 0.59084(8) 0.0173(3) Uani 1 1 d . . . C7 C 0.49283(9) 0.14308(12) 0.58173(8) 0.0195(3) Uani 1 1 d . . . H7 H 0.5244 0.0808 0.6059 0.023 Uiso 1 1 calc R . . C8 C 0.40880(10) 0.12764(12) 0.53731(9) 0.0232(3) Uani 1 1 d . . . H8 H 0.3828 0.0548 0.5317 0.028 Uiso 1 1 calc R . . C9 C 0.36265(10) 0.21801(13) 0.50107(9) 0.0246(3) Uani 1 1 d . . . H9 H 0.3048 0.2074 0.4714 0.030 Uiso 1 1 calc R . . C10 C 0.40166(10) 0.32390(13) 0.50845(9) 0.0231(3) Uani 1 1 d . . . H10 H 0.3705 0.3858 0.4833 0.028 Uiso 1 1 calc R . . C11 C 0.48586(9) 0.34048(12) 0.55217(8) 0.0206(3) Uani 1 1 d . . . H11 H 0.5128 0.4130 0.5558 0.025 Uiso 1 1 calc R . . C12 C 0.81744(8) 0.23773(11) 0.63412(8) 0.0157(2) Uani 1 1 d . . . C13 C 0.81810(9) 0.10861(11) 0.62201(8) 0.0187(3) Uani 1 1 d . . . C14 C 0.78166(11) 0.08255(12) 0.53353(9) 0.0278(3) Uani 1 1 d . . . H14A H 0.8188 0.1247 0.4924 0.042 Uiso 1 1 calc R . . H14B H 0.7146 0.1038 0.5292 0.042 Uiso 1 1 calc R . . H14C H 0.7882 0.0024 0.5225 0.042 Uiso 1 1 calc R . . C15 C 0.75929(10) 0.04208(12) 0.68557(9) 0.0259(3) Uani 1 1 d . . . H15A H 0.7820 0.0581 0.7424 0.039 Uiso 1 1 calc R . . H15B H 0.7659 -0.0379 0.6741 0.039 Uiso 1 1 calc R . . H15C H 0.6923 0.0635 0.6808 0.039 Uiso 1 1 calc R . . C16 C 0.92245(10) 0.07229(12) 0.62998(10) 0.0266(3) Uani 1 1 d . . . H16A H 0.9612 0.1141 0.5897 0.040 Uiso 1 1 calc R . . H16B H 0.9277 -0.0078 0.6183 0.040 Uiso 1 1 calc R . . H16C H 0.9450 0.0875 0.6870 0.040 Uiso 1 1 calc R . . C17 C 0.87999(9) 0.40725(11) 0.57632(8) 0.0169(3) Uani 1 1 d . . . C18 C 0.95377(9) 0.45301(11) 0.62458(8) 0.0183(3) Uani 1 1 d . . . C19 C 0.97069(9) 0.56709(12) 0.61848(9) 0.0207(3) Uani 1 1 d . . . H19 H 1.0194 0.5993 0.6518 0.025 Uiso 1 1 calc R . . C20 C 0.91855(10) 0.63546(11) 0.56515(9) 0.0219(3) Uani 1 1 d . . . C21 C 0.85044(10) 0.58626(12) 0.51413(8) 0.0211(3) Uani 1 1 d . . . H21 H 0.8163 0.6316 0.4757 0.025 Uiso 1 1 calc R . . C22 C 0.83074(9) 0.47241(11) 0.51763(8) 0.0191(3) Uani 1 1 d . . . C23 C 1.01392(10) 0.37968(12) 0.67996(9) 0.0243(3) Uani 1 1 d . . . H23A H 1.0691 0.4220 0.6998 0.036 Uiso 1 1 calc R . . H23B H 1.0355 0.3146 0.6480 0.036 Uiso 1 1 calc R . . H23C H 0.9763 0.3548 0.7281 0.036 Uiso 1 1 calc R . . C24 C 0.93715(12) 0.75944(12) 0.56304(11) 0.0330(4) Uani 1 1 d . . . H24A H 0.8943 0.7948 0.5225 0.050 Uiso 1 1 calc R . . H24B H 1.0032 0.7730 0.5465 0.050 Uiso 1 1 calc R . . H24C H 0.9260 0.7911 0.6188 0.050 Uiso 1 1 calc R . . C25 C 0.75828(10) 0.41911(13) 0.46069(9) 0.0263(3) Uani 1 1 d . . . H25A H 0.7318 0.4758 0.4230 0.039 Uiso 1 1 calc R . . H25B H 0.7072 0.3866 0.4945 0.039 Uiso 1 1 calc R . . H25C H 0.7888 0.3603 0.4275 0.039 Uiso 1 1 calc R . . C26 C 0.77311(8) 0.43965(11) 0.74388(8) 0.0158(2) Uani 1 1 d . . . C27 C 0.72107(9) 0.51378(11) 0.69411(8) 0.0177(3) Uani 1 1 d . . . H27 H 0.6841 0.4860 0.6489 0.021 Uiso 1 1 calc R . . C28 C 0.72294(10) 0.62764(12) 0.71020(9) 0.0229(3) Uani 1 1 d . . . H28 H 0.6881 0.6774 0.6755 0.028 Uiso 1 1 calc R . . C29 C 0.77585(10) 0.66923(12) 0.77714(9) 0.0262(3) Uani 1 1 d . . . H29 H 0.7766 0.7471 0.7884 0.031 Uiso 1 1 calc R . . C30 C 0.82717(10) 0.59672(13) 0.82698(9) 0.0247(3) Uani 1 1 d . . . H30 H 0.8634 0.6249 0.8726 0.030 Uiso 1 1 calc R . . C31 C 0.82605(9) 0.48258(12) 0.81069(8) 0.0199(3) Uani 1 1 d . . . H31 H 0.8616 0.4334 0.8453 0.024 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 P1 0.01604(15) 0.01546(16) 0.01466(15) -0.00050(12) -0.00220(11) 0.00011(12) N1 0.0158(5) 0.0171(5) 0.0174(5) -0.0006(4) -0.0014(4) -0.0007(4) N2 0.0178(5) 0.0163(5) 0.0196(5) -0.0017(4) 0.0002(4) 0.0014(4) C1 0.0167(6) 0.0118(6) 0.0176(6) 0.0000(5) 0.0004(5) -0.0004(5) C2 0.0197(6) 0.0177(6) 0.0158(6) -0.0012(5) 0.0025(5) -0.0017(5) C3 0.0227(7) 0.0242(7) 0.0247(7) 0.0002(6) 0.0058(5) 0.0033(6) C4 0.0273(7) 0.0371(9) 0.0186(7) -0.0078(6) 0.0055(5) -0.0075(6) C5 0.0270(7) 0.0213(7) 0.0220(7) 0.0042(5) 0.0043(5) -0.0015(6) C6 0.0149(6) 0.0231(6) 0.0137(6) -0.0011(5) 0.0011(4) -0.0003(5) C7 0.0198(6) 0.0207(7) 0.0180(6) 0.0012(5) -0.0009(5) 0.0003(5) C8 0.0235(7) 0.0245(7) 0.0217(7) -0.0010(6) -0.0022(5) -0.0068(6) C9 0.0175(6) 0.0353(8) 0.0211(7) 0.0016(6) -0.0043(5) -0.0026(6) C10 0.0202(6) 0.0282(7) 0.0210(7) 0.0048(6) -0.0014(5) 0.0039(6) C11 0.0210(6) 0.0202(7) 0.0207(6) 0.0013(5) 0.0000(5) -0.0011(5) C12 0.0142(6) 0.0163(6) 0.0165(6) -0.0016(5) -0.0038(4) 0.0023(5) C13 0.0191(6) 0.0143(6) 0.0228(7) -0.0026(5) -0.0020(5) 0.0013(5) C14 0.0369(8) 0.0200(7) 0.0263(7) -0.0065(6) -0.0070(6) -0.0024(6) C15 0.0290(7) 0.0156(7) 0.0330(8) 0.0017(6) 0.0026(6) -0.0004(5) C16 0.0229(7) 0.0168(7) 0.0400(8) -0.0008(6) -0.0026(6) 0.0043(5) C17 0.0170(6) 0.0169(6) 0.0168(6) -0.0010(5) 0.0052(5) 0.0019(5) C18 0.0157(6) 0.0193(7) 0.0199(6) -0.0009(5) 0.0044(5) 0.0020(5) C19 0.0172(6) 0.0214(7) 0.0235(7) -0.0027(5) 0.0044(5) -0.0028(5) C20 0.0233(7) 0.0180(6) 0.0246(7) 0.0007(5) 0.0097(5) -0.0003(5) C21 0.0229(7) 0.0216(7) 0.0188(6) 0.0035(5) 0.0057(5) 0.0049(5) C22 0.0200(6) 0.0209(7) 0.0163(6) -0.0009(5) 0.0048(5) 0.0018(5) C23 0.0203(6) 0.0226(7) 0.0300(8) 0.0004(6) -0.0040(5) 0.0014(5) C24 0.0390(9) 0.0193(7) 0.0409(9) 0.0040(6) 0.0035(7) -0.0039(6) C25 0.0304(7) 0.0267(7) 0.0218(7) -0.0016(6) -0.0046(6) 0.0029(6) C26 0.0141(6) 0.0170(6) 0.0164(6) -0.0028(5) 0.0024(4) -0.0009(5) C27 0.0162(6) 0.0201(6) 0.0169(6) -0.0012(5) 0.0001(5) -0.0005(5) C28 0.0214(7) 0.0200(7) 0.0273(7) 0.0006(5) 0.0021(5) 0.0022(5) C29 0.0264(7) 0.0186(7) 0.0338(8) -0.0083(6) 0.0050(6) -0.0035(6) C30 0.0219(7) 0.0285(8) 0.0238(7) -0.0093(6) 0.0006(5) -0.0056(6) C31 0.0166(6) 0.0239(7) 0.0191(6) -0.0019(5) 0.0003(5) -0.0016(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 P1 C26 1.8374(13) . ? P1 C12 1.8749(13) . ? P1 C1 1.8770(13) . ? N1 C1 1.2767(16) . ? N1 C6 1.4173(16) . ? N2 C12 1.2697(17) . ? N2 C17 1.4141(17) . ? C1 C2 1.5462(17) . ? C2 C3 1.5385(19) . ? C2 C5 1.5397(18) . ? C2 C4 1.5397(18) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.3949(19) . ? C6 C11 1.3989(19) . ? C7 C8 1.3911(18) . ? C7 H7 0.9500 . ? C8 C9 1.389(2) . ? C8 H8 0.9500 . ? C9 C10 1.387(2) . ? C9 H9 0.9500 . ? C10 C11 1.3893(19) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.5588(17) . ? C13 C15 1.5332(19) . ? C13 C14 1.5339(19) . ? C13 C16 1.5376(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.4021(18) . ? C17 C18 1.4041(18) . ? C18 C19 1.3906(19) . ? C18 C23 1.5062(19) . ? C19 C20 1.390(2) . ? C19 H19 0.9500 . ? C20 C21 1.389(2) . ? C20 C24 1.508(2) . ? C21 C22 1.3929(19) . ? C21 H21 0.9500 . ? C22 C25 1.5076(19) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C31 1.3982(18) . ? C26 C27 1.3983(18) . ? C27 C28 1.3881(19) . ? C27 H27 0.9500 . ? C28 C29 1.394(2) . ? C28 H28 0.9500 . ? C29 C30 1.381(2) . ? C29 H29 0.9500 . ? C30 C31 1.392(2) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? 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 C26 P1 C12 110.55(6) . . ? C26 P1 C1 97.56(6) . . ? C12 P1 C1 98.51(5) . . ? C1 N1 C6 127.08(11) . . ? C12 N2 C17 126.58(11) . . ? N1 C1 C2 128.72(11) . . ? N1 C1 P1 114.54(9) . . ? C2 C1 P1 116.67(9) . . ? C3 C2 C5 109.98(11) . . ? C3 C2 C4 107.41(11) . . ? C5 C2 C4 108.23(11) . . ? C3 C2 C1 112.76(11) . . ? C5 C2 C1 106.83(10) . . ? C4 C2 C1 111.55(11) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.49(12) . . ? C7 C6 N1 120.53(12) . . ? C11 C6 N1 119.50(12) . . ? C8 C7 C6 120.06(13) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.40(13) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.50(12) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.73(13) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C6 119.75(13) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? N2 C12 C13 114.13(11) . . ? N2 C12 P1 130.30(10) . . ? C13 C12 P1 114.92(9) . . ? C15 C13 C14 108.81(11) . . ? C15 C13 C16 108.36(11) . . ? C14 C13 C16 109.72(12) . . ? C15 C13 C12 115.50(11) . . ? C14 C13 C12 108.30(11) . . ? C16 C13 C12 106.04(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 120.94(12) . . ? C22 C17 N2 118.29(12) . . ? C18 C17 N2 120.24(12) . . ? C19 C18 C17 118.16(12) . . ? C19 C18 C23 121.19(12) . . ? C17 C18 C23 120.63(12) . . ? C20 C19 C18 122.11(13) . . ? C20 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C21 C20 C19 118.21(13) . . ? C21 C20 C24 121.64(13) . . ? C19 C20 C24 120.15(13) . . ? C20 C21 C22 121.98(13) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C17 118.26(12) . . ? C21 C22 C25 121.69(12) . . ? C17 C22 C25 120.05(12) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 118.57(12) . . ? C31 C26 P1 116.57(10) . . ? C27 C26 P1 124.44(10) . . ? C28 C27 C26 120.61(12) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.20(13) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.70(13) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.29(13) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 120.63(13) . . ? C30 C31 H31 119.7 . . ? C26 C31 H31 119.7 . . ? 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 C6 N1 C1 C2 -0.3(2) . . . . ? C6 N1 C1 P1 176.27(10) . . . . ? C26 P1 C1 N1 98.17(10) . . . . ? C12 P1 C1 N1 -14.04(11) . . . . ? C26 P1 C1 C2 -84.80(10) . . . . ? C12 P1 C1 C2 163.00(9) . . . . ? N1 C1 C2 C3 -36.78(18) . . . . ? P1 C1 C2 C3 146.68(10) . . . . ? N1 C1 C2 C5 84.16(16) . . . . ? P1 C1 C2 C5 -92.38(11) . . . . ? N1 C1 C2 C4 -157.75(13) . . . . ? P1 C1 C2 C4 25.71(14) . . . . ? C1 N1 C6 C7 -86.91(17) . . . . ? C1 N1 C6 C11 101.08(16) . . . . ? C11 C6 C7 C8 -2.58(19) . . . . ? N1 C6 C7 C8 -174.59(12) . . . . ? C6 C7 C8 C9 0.6(2) . . . . ? C7 C8 C9 C10 0.9(2) . . . . ? C8 C9 C10 C11 -0.5(2) . . . . ? C9 C10 C11 C6 -1.5(2) . . . . ? C7 C6 C11 C10 2.98(19) . . . . ? N1 C6 C11 C10 175.08(12) . . . . ? C17 N2 C12 C13 -174.70(11) . . . . ? C17 N2 C12 P1 -4.6(2) . . . . ? C26 P1 C12 N2 8.02(14) . . . . ? C1 P1 C12 N2 109.46(12) . . . . ? C26 P1 C12 C13 178.11(9) . . . . ? C1 P1 C12 C13 -80.45(9) . . . . ? N2 C12 C13 C15 -176.32(11) . . . . ? P1 C12 C13 C15 11.95(14) . . . . ? N2 C12 C13 C14 -54.04(15) . . . . ? P1 C12 C13 C14 134.23(10) . . . . ? N2 C12 C13 C16 63.66(14) . . . . ? P1 C12 C13 C16 -108.06(11) . . . . ? C12 N2 C17 C22 -108.33(15) . . . . ? C12 N2 C17 C18 79.90(17) . . . . ? C22 C17 C18 C19 6.05(18) . . . . ? N2 C17 C18 C19 177.60(11) . . . . ? C22 C17 C18 C23 -172.72(12) . . . . ? N2 C17 C18 C23 -1.18(18) . . . . ? C17 C18 C19 C20 -1.47(19) . . . . ? C23 C18 C19 C20 177.30(12) . . . . ? C18 C19 C20 C21 -2.82(19) . . . . ? C18 C19 C20 C24 177.76(13) . . . . ? C19 C20 C21 C22 2.68(19) . . . . ? C24 C20 C21 C22 -177.91(13) . . . . ? C20 C21 C22 C17 1.73(19) . . . . ? C20 C21 C22 C25 -178.59(12) . . . . ? C18 C17 C22 C21 -6.18(18) . . . . ? N2 C17 C22 C21 -177.89(11) . . . . ? C18 C17 C22 C25 174.13(12) . . . . ? N2 C17 C22 C25 2.42(18) . . . . ? C12 P1 C26 C31 -119.60(10) . . . . ? C1 P1 C26 C31 138.32(10) . . . . ? C12 P1 C26 C27 68.02(12) . . . . ? C1 P1 C26 C27 -34.06(12) . . . . ? C31 C26 C27 C28 0.77(19) . . . . ? P1 C26 C27 C28 173.01(10) . . . . ? C26 C27 C28 C29 -0.9(2) . . . . ? C27 C28 C29 C30 0.6(2) . . . . ? C28 C29 C30 C31 -0.1(2) . . . . ? C29 C30 C31 C26 0.0(2) . . . . ? C27 C26 C31 C30 -0.29(19) . . . . ? P1 C26 C31 C30 -173.14(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.335 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.045 _iucr_refine_instructions_details ; TITL jcs011 in P2(1)/c (sadabs 0.8995/0.9955) CELL 0.71073 14.0810 11.9795 15.9550 90.000 90.047 90.000 ZERR 4.00 0.0010 0.0011 0.0014 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N P UNIT 124 156 8 4 SHEL 7.0 0.77 OMIT 4 4 4 OMIT 4 2 6 L.S. 12 BOND BOND $H ACTA CONF SIZE 0.15 0.30 0.50 rem yellow-orange blocks TEMP -150 FMAP 2 PLAN 20 MPLA 5 P1 C1 C2 N1 C6 MPLA 5 P1 C12 C13 N2 C17 MPLA 6 C6 C7 C8 C9 C10 C11 MPLA 6 C26 C27 C28 C29 C30 C31 c17 c18 c19 c20 c21 c22 c23 c24 c25 MPLA 6 c17 c18 c19 c20 c21 c22 c23 c24 c25 C26 C27 C28 C29 C30 C31 MPLA 6 C6 C7 C8 C9 C10 C11 WGHT 0.036800 1.540100 FVAR 0.14492 P1 4 0.766043 0.286861 0.736018 11.00000 0.01604 0.01546 = 0.01466 -0.00050 -0.00220 0.00011 N1 3 0.620365 0.265596 0.629718 11.00000 0.01582 0.01709 = 0.01737 -0.00057 -0.00137 -0.00072 N2 3 0.862386 0.291053 0.577971 11.00000 0.01784 0.01629 = 0.01961 -0.00169 0.00024 0.00142 C1 1 0.636840 0.276965 0.707953 11.00000 0.01668 0.01181 = 0.01759 0.00002 0.00040 -0.00045 C2 1 0.565490 0.277560 0.781565 11.00000 0.01966 0.01771 = 0.01583 -0.00117 0.00251 -0.00170 C3 1 0.471276 0.335441 0.759235 11.00000 0.02274 0.02420 = 0.02468 0.00019 0.00579 0.00328 AFIX 33 H3A 2 0.483581 0.413497 0.744409 11.00000 -1.50000 H3B 2 0.428400 0.332495 0.807537 11.00000 -1.50000 H3C 2 0.441832 0.297201 0.711536 11.00000 -1.50000 AFIX 0 C4 1 0.606557 0.337365 0.858947 11.00000 0.02725 0.03709 = 0.01861 -0.00778 0.00548 -0.00751 AFIX 33 H4A 2 0.666837 0.302365 0.874863 11.00000 -1.50000 H4B 2 0.561569 0.331589 0.905579 11.00000 -1.50000 H4C 2 0.617402 0.416206 0.845651 11.00000 -1.50000 AFIX 0 C5 1 0.547107 0.154776 0.805004 11.00000 0.02699 0.02129 = 0.02198 0.00425 0.00426 -0.00148 AFIX 33 H5A 2 0.607424 0.118528 0.819132 11.00000 -1.50000 H5B 2 0.517811 0.116171 0.757400 11.00000 -1.50000 H5C 2 0.504385 0.151477 0.853398 11.00000 -1.50000 AFIX 0 C6 1 0.530808 0.249938 0.590843 11.00000 0.01491 0.02312 = 0.01375 -0.00111 0.00111 -0.00033 C7 1 0.492831 0.143078 0.581726 11.00000 0.01981 0.02067 = 0.01802 0.00121 -0.00090 0.00026 AFIX 43 H7 2 0.524383 0.080781 0.605875 11.00000 -1.20000 AFIX 0 C8 1 0.408801 0.127642 0.537306 11.00000 0.02346 0.02454 = 0.02172 -0.00096 -0.00217 -0.00682 AFIX 43 H8 2 0.382832 0.054825 0.531729 11.00000 -1.20000 AFIX 0 C9 1 0.362650 0.218014 0.501070 11.00000 0.01752 0.03530 = 0.02105 0.00156 -0.00432 -0.00258 AFIX 43 H9 2 0.304797 0.207415 0.471448 11.00000 -1.20000 AFIX 0 C10 1 0.401664 0.323904 0.508451 11.00000 0.02016 0.02822 = 0.02105 0.00476 -0.00141 0.00392 AFIX 43 H10 2 0.370463 0.385764 0.483334 11.00000 -1.20000 AFIX 0 C11 1 0.485859 0.340475 0.552170 11.00000 0.02096 0.02021 = 0.02070 0.00128 0.00003 -0.00108 AFIX 43 H11 2 0.512806 0.413019 0.555790 11.00000 -1.20000 AFIX 0 C12 1 0.817439 0.237725 0.634122 11.00000 0.01416 0.01628 = 0.01655 -0.00165 -0.00377 0.00234 C13 1 0.818098 0.108608 0.622013 11.00000 0.01910 0.01430 = 0.02280 -0.00261 -0.00202 0.00132 C14 1 0.781659 0.082547 0.533527 11.00000 0.03690 0.02004 = 0.02631 -0.00650 -0.00699 -0.00240 AFIX 33 H14A 2 0.818822 0.124697 0.492379 11.00000 -1.50000 H14B 2 0.714636 0.103843 0.529195 11.00000 -1.50000 H14C 2 0.788235 0.002449 0.522474 11.00000 -1.50000 AFIX 0 C15 1 0.759285 0.042079 0.685569 11.00000 0.02905 0.01557 = 0.03301 0.00168 0.00260 -0.00035 AFIX 33 H15A 2 0.782019 0.058146 0.742372 11.00000 -1.50000 H15B 2 0.765922 -0.037913 0.674118 11.00000 -1.50000 H15C 2 0.692320 0.063478 0.680843 11.00000 -1.50000 AFIX 0 C16 1 0.922453 0.072291 0.629981 11.00000 0.02294 0.01681 = 0.03999 -0.00082 -0.00256 0.00428 AFIX 33 H16A 2 0.961160 0.114053 0.589728 11.00000 -1.50000 H16B 2 0.927690 -0.007791 0.618319 11.00000 -1.50000 H16C 2 0.945018 0.087463 0.686975 11.00000 -1.50000 AFIX 0 C17 1 0.879987 0.407250 0.576317 11.00000 0.01700 0.01689 = 0.01678 -0.00096 0.00516 0.00195 C18 1 0.953770 0.453014 0.624581 11.00000 0.01575 0.01934 = 0.01993 -0.00090 0.00438 0.00198 C19 1 0.970687 0.567085 0.618477 11.00000 0.01723 0.02144 = 0.02350 -0.00268 0.00445 -0.00282 AFIX 43 H19 2 1.019430 0.599322 0.651813 11.00000 -1.20000 AFIX 0 C20 1 0.918554 0.635463 0.565153 11.00000 0.02327 0.01798 = 0.02457 0.00075 0.00967 -0.00028 C21 1 0.850440 0.586257 0.514131 11.00000 0.02292 0.02158 = 0.01878 0.00351 0.00566 0.00492 AFIX 43 H21 2 0.816256 0.631607 0.475692 11.00000 -1.20000 AFIX 0 C22 1 0.830744 0.472410 0.517629 11.00000 0.01999 0.02093 = 0.01634 -0.00093 0.00480 0.00177 C23 1 1.013925 0.379684 0.679955 11.00000 0.02027 0.02262 = 0.02998 0.00044 -0.00395 0.00135 AFIX 137 H23A 2 1.069137 0.421964 0.699761 11.00000 -1.50000 H23B 2 1.035460 0.314568 0.648015 11.00000 -1.50000 H23C 2 0.976318 0.354808 0.728118 11.00000 -1.50000 AFIX 0 C24 1 0.937146 0.759437 0.563043 11.00000 0.03899 0.01925 = 0.04086 0.00403 0.00345 -0.00391 AFIX 137 H24A 2 0.894346 0.794769 0.522487 11.00000 -1.50000 H24B 2 1.003152 0.772952 0.546468 11.00000 -1.50000 H24C 2 0.926017 0.791134 0.618801 11.00000 -1.50000 AFIX 0 C25 1 0.758280 0.419107 0.460686 11.00000 0.03037 0.02674 = 0.02179 -0.00156 -0.00461 0.00287 AFIX 137 H25A 2 0.731771 0.475759 0.423037 11.00000 -1.50000 H25B 2 0.707211 0.386584 0.494488 11.00000 -1.50000 H25C 2 0.788754 0.360326 0.427518 11.00000 -1.50000 AFIX 0 C26 1 0.773112 0.439654 0.743881 11.00000 0.01410 0.01700 = 0.01635 -0.00275 0.00240 -0.00090 C27 1 0.721066 0.513782 0.694115 11.00000 0.01620 0.02010 = 0.01690 -0.00118 0.00014 -0.00049 AFIX 43 H27 2 0.684085 0.485968 0.648878 11.00000 -1.20000 AFIX 0 C28 1 0.722939 0.627637 0.710200 11.00000 0.02144 0.02002 = 0.02731 0.00059 0.00211 0.00225 AFIX 43 H28 2 0.688051 0.677357 0.675482 11.00000 -1.20000 AFIX 0 C29 1 0.775850 0.669227 0.777135 11.00000 0.02635 0.01859 = 0.03376 -0.00828 0.00502 -0.00345 AFIX 43 H29 2 0.776617 0.747084 0.788429 11.00000 -1.20000 AFIX 0 C30 1 0.827167 0.596724 0.826976 11.00000 0.02194 0.02845 = 0.02377 -0.00927 0.00057 -0.00564 AFIX 43 H30 2 0.863387 0.624887 0.872569 11.00000 -1.20000 AFIX 0 C31 1 0.826046 0.482579 0.810694 11.00000 0.01658 0.02385 = 0.01913 -0.00191 0.00030 -0.00160 AFIX 43 H31 2 0.861586 0.433369 0.845308 11.00000 -1.20000 HKLF 4 REM jcs011 in P2(1)/c (sadabs 0.8995/0.9955) REM R1 = 0.0371 for 5140 Fo > 4sig(Fo) and 0.0498 for all 6159 data REM 310 parameters refined using 0 restraints END WGHT 0.0368 1.5401 REM Highest difference peak 0.335, deepest hole -0.217, 1-sigma level 0.045 Q1 1 0.7702 0.3696 0.7394 11.00000 0.05 0.34 Q2 1 0.6979 0.2779 0.7243 11.00000 0.05 0.31 Q3 1 0.7919 0.2598 0.6799 11.00000 0.05 0.29 Q4 1 0.5998 0.2816 0.7451 11.00000 0.05 0.28 Q5 1 0.5560 0.2166 0.7959 11.00000 0.05 0.27 Q6 1 0.9801 0.4172 0.6539 11.00000 0.05 0.27 Q7 1 0.7459 0.6397 0.7504 11.00000 0.05 0.26 Q8 1 0.9035 0.4319 0.6150 11.00000 0.05 0.26 Q9 1 0.8182 0.1700 0.6300 11.00000 0.05 0.26 Q10 1 0.8449 0.4442 0.5595 11.00000 0.05 0.26 Q11 1 0.8004 0.4465 0.4902 11.00000 0.05 0.25 Q12 1 0.9755 0.5006 0.6077 11.00000 0.05 0.23 Q13 1 0.8975 0.6024 0.5269 11.00000 0.05 0.23 Q14 1 0.5201 0.3041 0.7698 11.00000 0.05 0.23 Q15 1 0.4556 0.3199 0.5177 11.00000 0.05 0.23 Q16 1 0.9885 0.7804 0.5956 11.00000 0.05 0.23 Q17 1 0.9345 0.4221 0.5889 11.00000 0.05 0.23 Q18 1 0.7958 0.0926 0.5807 11.00000 0.05 0.23 Q19 1 0.5208 0.1936 0.5774 11.00000 0.05 0.23 Q20 1 0.8353 0.5415 0.8081 11.00000 0.05 0.22 ; #============================================================================== data_jcs013_compound_6 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H49 Cl N P Rh2, C H2 Cl2' _chemical_formula_sum 'C37 H51 Cl3 N P Rh2' _chemical_formula_weight 852.92 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.428(1) _cell_length_b 11.901(1) _cell_length_c 14.709(1) _cell_angle_alpha 86.78(1) _cell_angle_beta 87.00(1) _cell_angle_gamma 87.00(1) _cell_volume 1817.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 216 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_density_meas . _exptl_crystal_density_method . _exptl_crystal_density_diffrn 1.558 _exptl_crystal_F_000 872 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 1.199 _shelx_estimated_absorpt_T_min 0.762 _shelx_estimated_absorpt_T_max 0.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8124 _exptl_absorpt_correction_T_max 0.9281 _exptl_absorpt_process_details 'SADABS (Shelcrick, 2008)' _exptl_special_details ; dx = 40 mm, 80 sec./deg., 2 deg., 7 sets, 368 frames ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'rotation in \f and \w, 2\%' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31559 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.777 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 8322 _reflns_number_gt 7446 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection Collect _computing_cell_refinement EVALCCD _computing_data_reduction EVALCCD _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.4336P] 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 8322 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.72924(2) 0.72015(2) 0.91749(2) 0.01468(4) Uani 1 1 d . . . . . Cl1 Cl 0.89265(5) 0.83314(4) 0.84463(3) 0.01837(10) Uani 1 1 d . . . . . Rh2 Rh 0.76052(2) 0.58750(2) 0.68300(2) 0.01401(4) Uani 1 1 d . . . . . P1 P 0.63870(5) 0.70422(4) 0.78003(3) 0.01231(10) Uani 1 1 d . . . . . N1 N 0.73769(16) 0.75139(14) 0.62418(11) 0.0137(3) Uani 1 1 d . . . . . C1 C 0.67012(19) 0.80978(16) 0.68256(13) 0.0135(4) Uani 1 1 d . . . . . C2 C 0.6191(2) 0.93303(17) 0.67411(15) 0.0195(4) Uani 1 1 d . . . . . C3 C 0.4924(2) 0.9361(2) 0.62473(18) 0.0313(5) Uani 1 1 d . . . . . H3A H 0.5090 0.9079 0.5637 0.047 Uiso 1 1 calc R U . . . H3B H 0.4563 1.0138 0.6196 0.047 Uiso 1 1 calc R U . . . H3C H 0.4312 0.8885 0.6595 0.047 Uiso 1 1 calc R U . . . C4 C 0.5933(3) 0.97746(19) 0.76926(16) 0.0274(5) Uani 1 1 d . . . . . H4A H 0.6740 0.9754 0.8008 0.041 Uiso 1 1 calc R U . . . H4B H 0.5318 0.9302 0.8041 0.041 Uiso 1 1 calc R U . . . H4C H 0.5575 1.0552 0.7639 0.041 Uiso 1 1 calc R U . . . C5 C 0.7127(3) 1.01083(19) 0.62119(19) 0.0338(6) Uani 1 1 d . . . . . H5A H 0.7305 0.9844 0.5597 0.051 Uiso 1 1 calc R U . . . H5B H 0.7930 1.0101 0.6529 0.051 Uiso 1 1 calc R U . . . H5C H 0.6742 1.0878 0.6171 0.051 Uiso 1 1 calc R U . . . C6 C 0.7843(2) 0.78971(16) 0.53412(13) 0.0145(4) Uani 1 1 d . . . . . C7 C 0.9091(2) 0.82784(16) 0.52199(14) 0.0155(4) Uani 1 1 d . . . . . C8 C 0.9502(2) 0.86672(17) 0.43456(14) 0.0186(4) Uani 1 1 d . . . . . H8 H 1.0336 0.8952 0.4256 0.022 Uiso 1 1 calc R U . . . C9 C 0.8738(2) 0.86532(17) 0.36012(14) 0.0209(4) Uani 1 1 d . . . . . C10 C 0.7545(2) 0.81882(18) 0.37401(14) 0.0205(4) Uani 1 1 d . . . . . H10 H 0.7026 0.8141 0.3233 0.025 Uiso 1 1 calc R U . . . C11 C 0.7082(2) 0.77872(17) 0.46017(14) 0.0175(4) Uani 1 1 d . . . . . C12 C 0.9972(2) 0.82827(19) 0.59980(15) 0.0208(4) Uani 1 1 d . . . . . H12A H 0.9505 0.8607 0.6524 0.031 Uiso 1 1 calc R U . . . H12B H 1.0709 0.8735 0.5813 0.031 Uiso 1 1 calc R U . . . H12C H 1.0276 0.7509 0.6163 0.031 Uiso 1 1 calc R U . . . C13 C 0.9195(3) 0.9115(2) 0.26656(15) 0.0316(6) Uani 1 1 d . . . . . H13A H 1.0103 0.9286 0.2674 0.047 Uiso 1 1 calc R U . . . H13B H 0.8685 0.9805 0.2502 0.047 Uiso 1 1 calc R U . . . H13C H 0.9092 0.8554 0.2216 0.047 Uiso 1 1 calc R U . . . C14 C 0.5807(2) 0.7232(2) 0.46942(15) 0.0247(5) Uani 1 1 d . . . . . H14A H 0.5671 0.6913 0.5319 0.037 Uiso 1 1 calc R U . . . H14B H 0.5811 0.6629 0.4266 0.037 Uiso 1 1 calc R U . . . H14C H 0.5113 0.7793 0.4558 0.037 Uiso 1 1 calc R U . . . C15 C 0.4661(2) 0.68452(18) 0.76830(14) 0.0180(4) Uani 1 1 d . . . . . C16 C 0.4296(2) 0.6038(2) 0.71027(15) 0.0257(5) Uani 1 1 d . . . . . H16 H 0.4937 0.5589 0.6790 0.031 Uiso 1 1 calc R U . . . C17 C 0.3001(3) 0.5888(3) 0.69799(19) 0.0376(6) Uani 1 1 d . . . . . H17 H 0.2764 0.5340 0.6582 0.045 Uiso 1 1 calc R U . . . C18 C 0.2063(2) 0.6532(3) 0.7433(2) 0.0396(7) Uani 1 1 d . . . . . H18 H 0.1182 0.6424 0.7348 0.048 Uiso 1 1 calc R U . . . C19 C 0.2399(2) 0.7333(2) 0.80099(19) 0.0351(6) Uani 1 1 d . . . . . H19 H 0.1751 0.7778 0.8320 0.042 Uiso 1 1 calc R U . . . C20 C 0.3694(2) 0.7485(2) 0.81351(16) 0.0244(5) Uani 1 1 d . . . . . H20 H 0.3921 0.8034 0.8535 0.029 Uiso 1 1 calc R U . . . C21 C 0.5616(2) 0.6860(2) 0.99917(15) 0.0229(5) Uani 1 1 d . . . . . H21 H 0.5141 0.7286 0.9545 0.027 Uiso 1 1 calc R U . . . C22 C 0.6216(2) 0.58322(19) 0.97376(15) 0.0211(4) Uani 1 1 d . . . . . H22 H 0.6141 0.5624 0.9129 0.025 Uiso 1 1 calc R U . . . C23 C 0.6977(3) 0.5033(2) 1.03736(17) 0.0323(6) Uani 1 1 d . . . . . H23A H 0.6866 0.4248 1.0214 0.039 Uiso 1 1 calc R U . . . H23B H 0.6629 0.5113 1.1007 0.039 Uiso 1 1 calc R U . . . C24 C 0.8403(3) 0.5253(2) 1.0325(2) 0.0373(6) Uani 1 1 d . . . . . H24A H 0.8768 0.4994 1.0913 0.045 Uiso 1 1 calc R U . . . H24B H 0.8839 0.4801 0.9844 0.045 Uiso 1 1 calc R U . . . C25 C 0.8685(2) 0.6480(2) 1.01244(17) 0.0314(6) Uani 1 1 d . . . . . H25 H 0.9352 0.6639 0.9678 0.038 Uiso 1 1 calc R U . . . C26 C 0.8070(3) 0.7379(2) 1.05258(15) 0.0320(6) Uani 1 1 d . . . . . H26 H 0.8314 0.8112 1.0321 0.038 Uiso 1 1 calc R U . . . C27 C 0.7019(3) 0.7286(3) 1.12799(17) 0.0481(8) Uani 1 1 d . . . . . H27A H 0.7086 0.7903 1.1696 0.058 Uiso 1 1 calc R U . . . H27B H 0.7157 0.6563 1.1637 0.058 Uiso 1 1 calc R U . . . C28 C 0.5663(3) 0.7345(3) 1.09173(17) 0.0379(6) Uani 1 1 d . . . . . H28A H 0.5086 0.6928 1.1356 0.045 Uiso 1 1 calc R U . . . H28B H 0.5338 0.8141 1.0876 0.045 Uiso 1 1 calc R U . . . C29 C 0.9208(2) 0.51350(18) 0.59736(15) 0.0224(5) Uani 1 1 d . . . . . H29 H 0.9547 0.5861 0.5884 0.027 Uiso 1 1 calc R U . . . C30 C 0.8060(2) 0.4963(2) 0.56035(15) 0.0245(5) Uani 1 1 d . . . . . H30 H 0.7665 0.5580 0.5266 0.029 Uiso 1 1 calc R U . . . C31 C 0.7371(3) 0.3879(2) 0.56875(19) 0.0344(6) Uani 1 1 d . . . . . H31A H 0.7844 0.3325 0.5300 0.041 Uiso 1 1 calc R U . . . H31B H 0.6503 0.4020 0.5451 0.041 Uiso 1 1 calc R U . . . C32 C 0.7236(3) 0.3367(2) 0.66539(19) 0.0358(6) Uani 1 1 d . . . . . H32A H 0.7979 0.2831 0.6760 0.043 Uiso 1 1 calc R U . . . H32B H 0.6449 0.2933 0.6715 0.043 Uiso 1 1 calc R U . . . C33 C 0.7164(2) 0.42276(18) 0.73897(16) 0.0249(5) Uani 1 1 d . . . . . H33 H 0.6346 0.4538 0.7588 0.030 Uiso 1 1 calc R U . . . C34 C 0.8251(2) 0.45718(18) 0.77776(15) 0.0229(5) Uani 1 1 d . . . . . H34 H 0.8112 0.5093 0.8243 0.027 Uiso 1 1 calc R U . . . C35 C 0.9628(3) 0.4211(2) 0.75422(19) 0.0355(6) Uani 1 1 d . . . . . H35A H 0.9799 0.3436 0.7802 0.043 Uiso 1 1 calc R U . . . H35B H 1.0197 0.4712 0.7831 0.043 Uiso 1 1 calc R U . . . C36 C 0.9968(2) 0.4238(2) 0.65152(18) 0.0295(5) Uani 1 1 d . . . . . H36A H 1.0896 0.4368 0.6412 0.035 Uiso 1 1 calc R U . . . H36B H 0.9815 0.3493 0.6286 0.035 Uiso 1 1 calc R U . . . C1C C 0.8298(4) 1.0802(3) 0.9746(2) 0.0537(9) Uani 1 1 d . . . . . H1C1 H 0.8900 1.0902 1.0230 0.064 Uiso 1 1 calc R U . . . H1C2 H 0.8701 1.0241 0.9333 0.064 Uiso 1 1 calc R U . . . Cl2 Cl 0.80250(9) 1.20976(7) 0.91268(7) 0.0562(2) Uani 1 1 d . . . . . Cl3 Cl 0.68469(12) 1.02944(7) 1.02442(7) 0.0768(3) Uani 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 Rh1 0.01530(8) 0.01765(8) 0.01131(8) 0.00109(6) -0.00037(6) -0.00511(6) Cl1 0.0168(2) 0.0199(2) 0.0183(2) 0.00074(18) 0.00329(18) -0.00596(18) Rh2 0.01777(8) 0.01100(7) 0.01298(8) -0.00072(5) 0.00217(6) -0.00098(6) P1 0.0126(2) 0.0127(2) 0.0113(2) 0.00087(17) 0.00076(18) -0.00101(18) N1 0.0154(8) 0.0136(8) 0.0118(8) 0.0019(6) 0.0004(6) -0.0022(6) C1 0.0128(9) 0.0137(9) 0.0140(9) 0.0010(7) -0.0009(7) -0.0019(7) C2 0.0225(11) 0.0134(9) 0.0213(10) 0.0028(8) 0.0040(8) 0.0021(8) C3 0.0314(13) 0.0261(12) 0.0346(13) 0.0079(10) -0.0079(11) 0.0100(10) C4 0.0368(14) 0.0163(10) 0.0277(12) -0.0034(9) 0.0041(10) 0.0069(9) C5 0.0410(15) 0.0130(10) 0.0451(15) 0.0019(10) 0.0177(12) -0.0025(10) C6 0.0186(10) 0.0131(9) 0.0114(9) 0.0006(7) 0.0028(7) -0.0017(7) C7 0.0182(10) 0.0123(9) 0.0159(9) -0.0012(7) 0.0017(8) -0.0004(7) C8 0.0208(11) 0.0160(9) 0.0187(10) -0.0007(8) 0.0060(8) -0.0042(8) C9 0.0317(12) 0.0164(10) 0.0139(10) -0.0003(8) 0.0056(8) -0.0034(8) C10 0.0270(12) 0.0211(10) 0.0136(10) -0.0001(8) -0.0023(8) -0.0020(8) C11 0.0189(10) 0.0180(10) 0.0152(9) 0.0012(7) 0.0003(8) -0.0014(8) C12 0.0205(11) 0.0219(10) 0.0205(10) 0.0002(8) -0.0029(8) -0.0042(8) C13 0.0473(16) 0.0326(13) 0.0148(10) 0.0029(9) 0.0052(10) -0.0137(11) C14 0.0229(11) 0.0319(12) 0.0202(11) 0.0007(9) -0.0041(9) -0.0075(9) C15 0.0143(10) 0.0236(10) 0.0154(9) 0.0086(8) -0.0017(8) -0.0033(8) C16 0.0256(12) 0.0331(12) 0.0190(11) 0.0038(9) -0.0046(9) -0.0095(10) C17 0.0322(14) 0.0500(16) 0.0322(14) 0.0098(12) -0.0140(11) -0.0186(12) C18 0.0196(12) 0.0524(17) 0.0458(16) 0.0274(14) -0.0148(11) -0.0114(11) C19 0.0184(12) 0.0398(14) 0.0433(15) 0.0218(12) 0.0027(10) 0.0050(10) C20 0.0180(11) 0.0264(11) 0.0268(11) 0.0094(9) 0.0021(9) 0.0026(9) C21 0.0229(11) 0.0309(12) 0.0148(10) 0.0022(8) 0.0047(8) -0.0107(9) C22 0.0214(11) 0.0261(11) 0.0160(10) 0.0071(8) -0.0012(8) -0.0115(9) C23 0.0335(14) 0.0351(13) 0.0283(12) 0.0168(10) -0.0110(10) -0.0130(11) C24 0.0339(14) 0.0388(14) 0.0398(15) 0.0203(12) -0.0198(12) -0.0118(11) C25 0.0281(13) 0.0395(14) 0.0276(12) 0.0146(10) -0.0147(10) -0.0145(11) C26 0.0384(14) 0.0457(15) 0.0144(10) 0.0027(10) -0.0082(10) -0.0232(12) C27 0.061(2) 0.072(2) 0.0147(12) -0.0053(12) 0.0012(12) -0.0356(17) C28 0.0434(16) 0.0515(17) 0.0199(12) -0.0091(11) 0.0124(11) -0.0196(13) C29 0.0255(12) 0.0174(10) 0.0239(11) -0.0074(8) 0.0093(9) -0.0006(8) C30 0.0305(12) 0.0246(11) 0.0186(10) -0.0088(8) 0.0013(9) 0.0044(9) C31 0.0328(14) 0.0334(14) 0.0395(15) -0.0175(11) -0.0029(11) -0.0071(11) C32 0.0459(16) 0.0186(11) 0.0447(15) -0.0027(10) -0.0092(13) -0.0101(11) C33 0.0316(13) 0.0121(10) 0.0303(12) 0.0056(8) 0.0001(10) -0.0028(9) C34 0.0328(13) 0.0141(10) 0.0209(11) 0.0042(8) -0.0021(9) 0.0028(9) C35 0.0315(14) 0.0322(13) 0.0417(15) 0.0055(11) -0.0068(11) 0.0049(11) C36 0.0207(12) 0.0289(12) 0.0393(14) -0.0102(10) -0.0009(10) 0.0033(9) C1C 0.070(2) 0.0382(16) 0.0517(19) -0.0100(14) 0.0079(17) 0.0115(15) Cl2 0.0566(5) 0.0401(4) 0.0697(6) 0.0018(4) 0.0128(4) -0.0035(3) Cl3 0.1151(9) 0.0353(4) 0.0749(6) -0.0096(4) 0.0516(6) -0.0042(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 Rh1 C21 2.113(2) . ? Rh1 C22 2.131(2) . ? Rh1 C25 2.178(2) . ? Rh1 C26 2.210(2) . ? Rh1 P1 2.2972(6) . ? Rh1 Cl1 2.3975(6) . ? Rh2 N1 2.0959(16) . ? Rh2 C34 2.132(2) . ? Rh2 C33 2.146(2) . ? Rh2 C30 2.176(2) . ? Rh2 C29 2.215(2) . ? Rh2 P1 2.3299(6) . ? P1 C15 1.845(2) . ? P1 C1 1.880(2) . ? N1 C1 1.292(3) . ? N1 C6 1.445(2) . ? C1 C2 1.535(3) . ? C2 C4 1.530(3) . ? C2 C5 1.533(3) . ? C2 C3 1.539(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.396(3) . ? C6 C7 1.399(3) . ? C7 C8 1.396(3) . ? C7 C12 1.505(3) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.388(3) . ? C9 C13 1.516(3) . ? C10 C11 1.400(3) . ? C10 H10 0.9500 . ? C11 C14 1.512(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.395(3) . ? C15 C16 1.400(3) . ? C16 C17 1.394(3) . ? C16 H16 0.9500 . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.405(3) . ? C21 C28 1.512(3) . ? C21 H21 0.9500 . ? C22 C23 1.519(3) . ? C22 H22 0.9500 . ? C23 C24 1.520(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.515(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.365(4) . ? C25 H25 0.9500 . ? C26 C27 1.522(4) . ? C26 H26 0.9500 . ? C27 C28 1.534(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.371(3) . ? C29 C36 1.512(3) . ? C29 H29 0.9500 . ? C30 C31 1.506(3) . ? C30 H30 0.9500 . ? C31 C32 1.517(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.528(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.386(3) . ? C33 H33 0.9500 . ? C34 C35 1.505(3) . ? C34 H34 0.9500 . ? C35 C36 1.532(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C1C Cl2 1.764(3) . ? C1C Cl3 1.767(4) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? 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 C21 Rh1 C22 38.67(9) . . ? C21 Rh1 C25 97.39(9) . . ? C22 Rh1 C25 81.78(9) . . ? C21 Rh1 C26 81.56(9) . . ? C22 Rh1 C26 89.34(9) . . ? C25 Rh1 C26 36.25(11) . . ? C21 Rh1 P1 95.97(6) . . ? C22 Rh1 P1 89.52(6) . . ? C25 Rh1 P1 145.93(8) . . ? C26 Rh1 P1 177.22(8) . . ? C21 Rh1 Cl1 156.68(7) . . ? C22 Rh1 Cl1 164.25(7) . . ? C25 Rh1 Cl1 89.45(7) . . ? C26 Rh1 Cl1 91.28(6) . . ? P1 Rh1 Cl1 90.51(2) . . ? N1 Rh2 C34 157.29(8) . . ? N1 Rh2 C33 160.99(8) . . ? C34 Rh2 C33 37.80(9) . . ? N1 Rh2 C30 99.47(8) . . ? C34 Rh2 C30 96.76(9) . . ? C33 Rh2 C30 82.44(9) . . ? N1 Rh2 C29 102.43(7) . . ? C34 Rh2 C29 81.63(9) . . ? C33 Rh2 C29 90.36(9) . . ? C30 Rh2 C29 36.37(9) . . ? N1 Rh2 P1 68.89(5) . . ? C34 Rh2 P1 100.75(6) . . ? C33 Rh2 P1 102.11(7) . . ? C30 Rh2 P1 156.54(7) . . ? C29 Rh2 P1 162.60(6) . . ? C15 P1 C1 100.31(9) . . ? C15 P1 Rh1 123.66(7) . . ? C1 P1 Rh1 120.55(6) . . ? C15 P1 Rh2 109.62(7) . . ? C1 P1 Rh2 81.22(6) . . ? Rh1 P1 Rh2 113.27(2) . . ? C1 N1 C6 126.93(17) . . ? C1 N1 Rh2 106.77(12) . . ? C6 N1 Rh2 126.26(13) . . ? N1 C1 C2 129.48(17) . . ? N1 C1 P1 103.12(13) . . ? C2 C1 P1 127.30(14) . . ? C4 C2 C5 107.80(19) . . ? C4 C2 C1 109.51(17) . . ? C5 C2 C1 113.30(18) . . ? C4 C2 C3 109.45(19) . . ? C5 C2 C3 109.2(2) . . ? C1 C2 C3 107.57(18) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.45(18) . . ? C11 C6 N1 119.14(18) . . ? C7 C6 N1 119.17(18) . . ? C8 C7 C6 117.75(19) . . ? C8 C7 C12 120.32(19) . . ? C6 C7 C12 121.93(18) . . ? C9 C8 C7 122.5(2) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C10 C9 C8 117.73(19) . . ? C10 C9 C13 121.0(2) . . ? C8 C9 C13 121.2(2) . . ? C9 C10 C11 122.2(2) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C6 C11 C10 117.92(19) . . ? C6 C11 C14 122.71(18) . . ? C10 C11 C14 119.35(19) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.1(2) . . ? C20 C15 P1 122.77(18) . . ? C16 C15 P1 119.12(17) . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C15 121.1(2) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C22 C21 C28 125.4(2) . . ? C22 C21 Rh1 71.38(12) . . ? C28 C21 Rh1 111.04(16) . . ? C22 C21 H21 117.3 . . ? C28 C21 H21 117.3 . . ? Rh1 C21 H21 87.5 . . ? C21 C22 C23 124.2(2) . . ? C21 C22 Rh1 69.95(12) . . ? C23 C22 Rh1 113.10(15) . . ? C21 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? Rh1 C22 H22 87.0 . . ? C22 C23 C24 112.64(19) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 113.7(2) . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 126.0(2) . . ? C26 C25 Rh1 73.15(14) . . ? C24 C25 Rh1 107.87(15) . . ? C26 C25 H25 117.0 . . ? C24 C25 H25 117.0 . . ? Rh1 C25 H25 88.9 . . ? C25 C26 C27 124.4(2) . . ? C25 C26 Rh1 70.60(14) . . ? C27 C26 Rh1 111.07(17) . . ? C25 C26 H26 117.8 . . ? C27 C26 H26 117.8 . . ? Rh1 C26 H26 88.3 . . ? C26 C27 C28 113.0(2) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C21 C28 C27 113.2(2) . . ? C21 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C21 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C36 123.9(2) . . ? C30 C29 Rh2 70.24(13) . . ? C36 C29 Rh2 110.73(15) . . ? C30 C29 H29 118.1 . . ? C36 C29 H29 118.1 . . ? Rh2 C29 H29 89.0 . . ? C29 C30 C31 125.4(2) . . ? C29 C30 Rh2 73.39(13) . . ? C31 C30 Rh2 108.52(16) . . ? C29 C30 H30 117.3 . . ? C31 C30 H30 117.3 . . ? Rh2 C30 H30 88.0 . . ? C30 C31 C32 114.1(2) . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C31 C32 C33 114.2(2) . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 122.3(2) . . ? C34 C33 Rh2 70.56(12) . . ? C32 C33 Rh2 111.48(16) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? Rh2 C33 H33 88.0 . . ? C33 C34 C35 127.2(2) . . ? C33 C34 Rh2 71.64(12) . . ? C35 C34 Rh2 110.18(15) . . ? C33 C34 H34 116.4 . . ? C35 C34 H34 116.4 . . ? Rh2 C34 H34 88.1 . . ? C34 C35 C36 113.8(2) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C29 C36 C35 113.69(19) . . ? C29 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C29 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? Cl2 C1C Cl3 111.2(2) . . ? Cl2 C1C H1C1 109.4 . . ? Cl3 C1C H1C1 109.4 . . ? Cl2 C1C H1C2 109.4 . . ? Cl3 C1C H1C2 109.4 . . ? H1C1 C1C H1C2 108.0 . . ? 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 C6 N1 C1 C2 0.7(3) . . . . ? Rh2 N1 C1 C2 -176.90(18) . . . . ? C6 N1 C1 P1 177.23(16) . . . . ? Rh2 N1 C1 P1 -0.42(14) . . . . ? C15 P1 C1 N1 -108.13(15) . . . . ? Rh1 P1 C1 N1 112.27(13) . . . . ? Rh2 P1 C1 N1 0.37(12) . . . . ? C15 P1 C1 C2 68.45(19) . . . . ? Rh1 P1 C1 C2 -71.14(19) . . . . ? Rh2 P1 C1 C2 176.96(18) . . . . ? N1 C1 C2 C4 -157.3(2) . . . . ? P1 C1 C2 C4 27.0(3) . . . . ? N1 C1 C2 C5 -36.9(3) . . . . ? P1 C1 C2 C5 147.37(18) . . . . ? N1 C1 C2 C3 83.8(3) . . . . ? P1 C1 C2 C3 -91.9(2) . . . . ? C1 N1 C6 C11 -90.3(3) . . . . ? Rh2 N1 C6 C11 86.9(2) . . . . ? C1 N1 C6 C7 95.2(3) . . . . ? Rh2 N1 C6 C7 -87.6(2) . . . . ? C11 C6 C7 C8 7.1(3) . . . . ? N1 C6 C7 C8 -178.54(17) . . . . ? C11 C6 C7 C12 -173.31(19) . . . . ? N1 C6 C7 C12 1.1(3) . . . . ? C6 C7 C8 C9 -2.1(3) . . . . ? C12 C7 C8 C9 178.3(2) . . . . ? C7 C8 C9 C10 -2.7(3) . . . . ? C7 C8 C9 C13 178.1(2) . . . . ? C8 C9 C10 C11 2.8(3) . . . . ? C13 C9 C10 C11 -178.0(2) . . . . ? C7 C6 C11 C10 -7.0(3) . . . . ? N1 C6 C11 C10 178.61(18) . . . . ? C7 C6 C11 C14 171.5(2) . . . . ? N1 C6 C11 C14 -2.9(3) . . . . ? C9 C10 C11 C6 1.9(3) . . . . ? C9 C10 C11 C14 -176.6(2) . . . . ? C1 P1 C15 C20 -91.43(18) . . . . ? Rh1 P1 C15 C20 46.5(2) . . . . ? Rh2 P1 C15 C20 -175.70(15) . . . . ? C1 P1 C15 C16 87.18(17) . . . . ? Rh1 P1 C15 C16 -134.94(15) . . . . ? Rh2 P1 C15 C16 2.91(18) . . . . ? C20 C15 C16 C17 0.4(3) . . . . ? P1 C15 C16 C17 -178.32(18) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C18 C19 C20 C15 0.4(3) . . . . ? C16 C15 C20 C19 -0.4(3) . . . . ? P1 C15 C20 C19 178.22(17) . . . . ? C28 C21 C22 C23 1.9(3) . . . . ? Rh1 C21 C22 C23 104.9(2) . . . . ? C28 C21 C22 Rh1 -103.0(2) . . . . ? C21 C22 C23 C24 -92.0(3) . . . . ? Rh1 C22 C23 C24 -11.3(3) . . . . ? C22 C23 C24 C25 32.2(3) . . . . ? C23 C24 C25 C26 45.4(3) . . . . ? C23 C24 C25 Rh1 -36.4(3) . . . . ? C24 C25 C26 C27 2.6(4) . . . . ? Rh1 C25 C26 C27 102.8(2) . . . . ? C24 C25 C26 Rh1 -100.1(2) . . . . ? C25 C26 C27 C28 -92.5(3) . . . . ? Rh1 C26 C27 C28 -12.1(3) . . . . ? C22 C21 C28 C27 45.9(3) . . . . ? Rh1 C21 C28 C27 -35.6(3) . . . . ? C26 C27 C28 C21 31.4(4) . . . . ? C36 C29 C30 C31 1.0(4) . . . . ? Rh2 C29 C30 C31 -101.2(2) . . . . ? C36 C29 C30 Rh2 102.2(2) . . . . ? C29 C30 C31 C32 48.9(3) . . . . ? Rh2 C30 C31 C32 -33.5(3) . . . . ? C30 C31 C32 C33 29.5(3) . . . . ? C31 C32 C33 C34 -89.8(3) . . . . ? C31 C32 C33 Rh2 -9.9(3) . . . . ? C32 C33 C34 C35 1.9(3) . . . . ? Rh2 C33 C34 C35 -101.8(2) . . . . ? C32 C33 C34 Rh2 103.7(2) . . . . ? C33 C34 C35 C36 46.5(3) . . . . ? Rh2 C34 C35 C36 -35.3(3) . . . . ? C30 C29 C36 C35 -90.5(3) . . . . ? Rh2 C29 C36 C35 -11.0(3) . . . . ? C34 C35 C36 C29 30.8(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 C1C H1C2 Cl1 0.99 2.68 3.609(3) 157.0 . _refine_diff_density_max 0.754 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.072 _shelxl_version_number 2013-2 _shelx_res_file ; TITL jcs013 in P-1 - sadabs 0.8124/0.9281 CELL 0.71073 10.428 11.901 14.709 86.78 87.00 87.00 ZERR 2.00 0.001 0.001 0.001 0.01 0.01 0.01 LATT 1 SFAC C H N P CL RH UNIT 74 102 2 2 6 4 SHEL 15 0.77 L.S. 24 BOND BOND $H ACTA CONF SIZE 0.06 0.12 0.24 rem orange blocks TEMP -150 FMAP 2 PLAN 20 HTAB C1C CL1 WGHT 0.019000 2.433600 FVAR 0.17410 RH1 6 0.729236 0.720146 0.917495 11.00000 0.01530 0.01765 = 0.01131 0.00109 -0.00037 -0.00511 CL1 5 0.892649 0.833144 0.844626 11.00000 0.01681 0.01987 = 0.01833 0.00074 0.00329 -0.00596 RH2 6 0.760516 0.587503 0.683002 11.00000 0.01777 0.01100 = 0.01298 -0.00072 0.00217 -0.00098 P1 4 0.638695 0.704221 0.780029 11.00000 0.01262 0.01274 = 0.01130 0.00087 0.00076 -0.00101 N1 3 0.737688 0.751391 0.624184 11.00000 0.01542 0.01355 = 0.01184 0.00194 0.00038 -0.00220 C1 1 0.670118 0.809777 0.682557 11.00000 0.01278 0.01372 = 0.01402 0.00105 -0.00092 -0.00191 C2 1 0.619122 0.933032 0.674106 11.00000 0.02255 0.01341 = 0.02133 0.00280 0.00397 0.00214 C3 1 0.492414 0.936088 0.624734 11.00000 0.03143 0.02610 = 0.03462 0.00791 -0.00790 0.00998 AFIX 33 H3A 2 0.508991 0.907938 0.563668 11.00000 -1.50000 H3B 2 0.456336 1.013758 0.619601 11.00000 -1.50000 H3C 2 0.431205 0.888514 0.659484 11.00000 -1.50000 AFIX 0 C4 1 0.593294 0.977457 0.769263 11.00000 0.03677 0.01634 = 0.02773 -0.00344 0.00409 0.00690 AFIX 33 H4A 2 0.673964 0.975403 0.800769 11.00000 -1.50000 H4B 2 0.531837 0.930216 0.804103 11.00000 -1.50000 H4C 2 0.557534 1.055214 0.763879 11.00000 -1.50000 AFIX 0 C5 1 0.712663 1.010834 0.621192 11.00000 0.04095 0.01300 = 0.04507 0.00194 0.01769 -0.00254 AFIX 33 H5A 2 0.730538 0.984405 0.559683 11.00000 -1.50000 H5B 2 0.793048 1.010088 0.652930 11.00000 -1.50000 H5C 2 0.674219 1.087762 0.617127 11.00000 -1.50000 AFIX 0 C6 1 0.784341 0.789706 0.534116 11.00000 0.01857 0.01312 = 0.01136 0.00061 0.00281 -0.00169 C7 1 0.909091 0.827838 0.521990 11.00000 0.01817 0.01232 = 0.01587 -0.00121 0.00167 -0.00039 C8 1 0.950172 0.866717 0.434564 11.00000 0.02082 0.01597 = 0.01875 -0.00070 0.00596 -0.00423 AFIX 43 H8 2 1.033566 0.895219 0.425632 11.00000 -1.20000 AFIX 0 C9 1 0.873761 0.865321 0.360117 11.00000 0.03169 0.01642 = 0.01395 -0.00032 0.00563 -0.00340 C10 1 0.754494 0.818823 0.374009 11.00000 0.02699 0.02109 = 0.01357 -0.00010 -0.00227 -0.00198 AFIX 43 H10 2 0.702558 0.814064 0.323326 11.00000 -1.20000 AFIX 0 C11 1 0.708190 0.778718 0.460171 11.00000 0.01893 0.01799 = 0.01522 0.00118 0.00026 -0.00140 C12 1 0.997198 0.828275 0.599798 11.00000 0.02051 0.02185 = 0.02046 0.00018 -0.00295 -0.00416 AFIX 137 H12A 2 0.950451 0.860712 0.652432 11.00000 -1.50000 H12B 2 1.070941 0.873530 0.581305 11.00000 -1.50000 H12C 2 1.027572 0.750868 0.616320 11.00000 -1.50000 AFIX 0 C13 1 0.919489 0.911523 0.266558 11.00000 0.04734 0.03256 = 0.01484 0.00288 0.00521 -0.01371 AFIX 137 H13A 2 1.010339 0.928555 0.267408 11.00000 -1.50000 H13B 2 0.868458 0.980502 0.250212 11.00000 -1.50000 H13C 2 0.909237 0.855385 0.221561 11.00000 -1.50000 AFIX 0 C14 1 0.580693 0.723184 0.469421 11.00000 0.02285 0.03189 = 0.02022 0.00066 -0.00411 -0.00747 AFIX 137 H14A 2 0.567065 0.691323 0.531863 11.00000 -1.50000 H14B 2 0.581119 0.662924 0.426639 11.00000 -1.50000 H14C 2 0.511254 0.779309 0.455757 11.00000 -1.50000 AFIX 0 C15 1 0.466131 0.684520 0.768304 11.00000 0.01431 0.02357 = 0.01541 0.00859 -0.00169 -0.00333 C16 1 0.429616 0.603828 0.710268 11.00000 0.02558 0.03312 = 0.01904 0.00379 -0.00459 -0.00952 AFIX 43 H16 2 0.493698 0.558895 0.678969 11.00000 -1.20000 AFIX 0 C17 1 0.300104 0.588816 0.697989 11.00000 0.03223 0.04997 = 0.03224 0.00983 -0.01402 -0.01863 AFIX 43 H17 2 0.276432 0.534035 0.658244 11.00000 -1.20000 AFIX 0 C18 1 0.206323 0.653161 0.743304 11.00000 0.01956 0.05242 = 0.04581 0.02737 -0.01480 -0.01140 AFIX 43 H18 2 0.118192 0.642414 0.734847 11.00000 -1.20000 AFIX 0 C19 1 0.239933 0.733250 0.800993 11.00000 0.01843 0.03983 = 0.04327 0.02185 0.00274 0.00502 AFIX 43 H19 2 0.175140 0.777754 0.832002 11.00000 -1.20000 AFIX 0 C20 1 0.369405 0.748483 0.813510 11.00000 0.01801 0.02643 = 0.02683 0.00936 0.00206 0.00264 AFIX 43 H20 2 0.392101 0.803357 0.853506 11.00000 -1.20000 AFIX 0 C21 1 0.561584 0.686024 0.999171 11.00000 0.02288 0.03095 = 0.01481 0.00219 0.00466 -0.01073 AFIX 43 H21 2 0.514129 0.728566 0.954545 11.00000 -1.20000 AFIX 0 C22 1 0.621602 0.583222 0.973757 11.00000 0.02137 0.02615 = 0.01598 0.00712 -0.00117 -0.01148 AFIX 43 H22 2 0.614097 0.562356 0.912934 11.00000 -1.20000 AFIX 0 C23 1 0.697723 0.503332 1.037361 11.00000 0.03350 0.03510 = 0.02825 0.01677 -0.01097 -0.01297 AFIX 23 H23A 2 0.686592 0.424839 1.021396 11.00000 -1.20000 H23B 2 0.662927 0.511346 1.100714 11.00000 -1.20000 AFIX 0 C24 1 0.840269 0.525281 1.032497 11.00000 0.03389 0.03876 = 0.03978 0.02029 -0.01982 -0.01179 AFIX 23 H24A 2 0.876839 0.499439 1.091285 11.00000 -1.20000 H24B 2 0.883900 0.480052 0.984428 11.00000 -1.20000 AFIX 0 C25 1 0.868520 0.648018 1.012437 11.00000 0.02805 0.03947 = 0.02764 0.01461 -0.01471 -0.01454 AFIX 43 H25 2 0.935208 0.663907 0.967799 11.00000 -1.20000 AFIX 0 C26 1 0.807001 0.737915 1.052579 11.00000 0.03838 0.04570 = 0.01439 0.00274 -0.00818 -0.02322 AFIX 43 H26 2 0.831444 0.811203 1.032053 11.00000 -1.20000 AFIX 0 C27 1 0.701914 0.728570 1.127990 11.00000 0.06104 0.07189 = 0.01467 -0.00532 0.00120 -0.03560 AFIX 23 H27A 2 0.708561 0.790291 1.169645 11.00000 -1.20000 H27B 2 0.715684 0.656297 1.163669 11.00000 -1.20000 AFIX 0 C28 1 0.566349 0.734471 1.091726 11.00000 0.04339 0.05148 = 0.01989 -0.00912 0.01242 -0.01957 AFIX 23 H28A 2 0.508594 0.692830 1.135639 11.00000 -1.20000 H28B 2 0.533773 0.814144 1.087620 11.00000 -1.20000 AFIX 0 C29 1 0.920824 0.513499 0.597356 11.00000 0.02554 0.01739 = 0.02394 -0.00737 0.00925 -0.00059 AFIX 43 H29 2 0.954663 0.586094 0.588428 11.00000 -1.20000 AFIX 0 C30 1 0.805963 0.496320 0.560349 11.00000 0.03047 0.02458 = 0.01856 -0.00885 0.00135 0.00442 AFIX 43 H30 2 0.766531 0.557963 0.526605 11.00000 -1.20000 AFIX 0 C31 1 0.737134 0.387854 0.568753 11.00000 0.03284 0.03343 = 0.03950 -0.01748 -0.00292 -0.00706 AFIX 23 H31A 2 0.784380 0.332540 0.529983 11.00000 -1.20000 H31B 2 0.650303 0.401971 0.545059 11.00000 -1.20000 AFIX 0 C32 1 0.723646 0.336696 0.665386 11.00000 0.04588 0.01865 = 0.04467 -0.00270 -0.00915 -0.01012 AFIX 23 H32A 2 0.797899 0.283136 0.676008 11.00000 -1.20000 H32B 2 0.644932 0.293292 0.671489 11.00000 -1.20000 AFIX 0 C33 1 0.716390 0.422763 0.738966 11.00000 0.03162 0.01208 = 0.03032 0.00559 0.00013 -0.00275 AFIX 43 H33 2 0.634558 0.453753 0.758809 11.00000 -1.20000 AFIX 0 C34 1 0.825086 0.457184 0.777760 11.00000 0.03276 0.01412 = 0.02092 0.00419 -0.00208 0.00277 AFIX 43 H34 2 0.811164 0.509269 0.824334 11.00000 -1.20000 AFIX 0 C35 1 0.962792 0.421114 0.754216 11.00000 0.03148 0.03224 = 0.04173 0.00549 -0.00680 0.00492 AFIX 23 H35A 2 0.979890 0.343573 0.780236 11.00000 -1.20000 H35B 2 1.019734 0.471170 0.783118 11.00000 -1.20000 AFIX 0 C36 1 0.996831 0.423796 0.651524 11.00000 0.02066 0.02894 = 0.03931 -0.01019 -0.00095 0.00327 AFIX 23 H36A 2 1.089580 0.436795 0.641197 11.00000 -1.20000 H36B 2 0.981507 0.349287 0.628556 11.00000 -1.20000 AFIX 0 C1C 1 0.829806 1.080164 0.974610 11.00000 0.06965 0.03815 = 0.05166 -0.01001 0.00792 0.01151 AFIX 23 H1C1 2 0.890023 1.090159 1.023042 11.00000 -1.20000 H1C2 2 0.870064 1.024119 0.933287 11.00000 -1.20000 AFIX 0 CL2 5 0.802504 1.209764 0.912679 11.00000 0.05657 0.04007 = 0.06973 0.00176 0.01279 -0.00348 CL3 5 0.684687 1.029441 1.024418 11.00000 0.11511 0.03532 = 0.07491 -0.00958 0.05157 -0.00425 HKLF 4 REM jcs013 in P-1 - sadabs 0.8124/0.9281 REM R1 = 0.0238 for 7446 Fo > 4sig(Fo) and 0.0295 for all 8322 data REM 400 parameters refined using 0 restraints END WGHT 0.0190 2.4336 REM Highest difference peak 0.754, deepest hole -0.694, 1-sigma level 0.072 Q1 1 0.6428 0.3571 0.6773 11.00000 0.05 0.75 Q2 1 0.9323 0.3681 0.7284 11.00000 0.05 0.63 Q3 1 0.4704 0.6981 0.9726 11.00000 0.05 0.52 Q4 1 0.5712 0.5405 0.9314 11.00000 0.05 0.52 Q5 1 0.7057 0.7810 0.9293 11.00000 0.05 0.42 Q6 1 0.7572 0.3425 0.6012 11.00000 0.05 0.41 Q7 1 0.9708 0.7814 0.6465 11.00000 0.05 0.41 Q8 1 0.7968 0.6985 0.9307 11.00000 0.05 0.40 Q9 1 0.8051 0.4766 0.8552 11.00000 0.05 0.40 Q10 1 0.8042 0.5934 1.0974 11.00000 0.05 0.40 Q11 1 0.6433 0.4146 0.7767 11.00000 0.05 0.39 Q12 1 0.7365 0.8058 0.4965 11.00000 0.05 0.37 Q13 1 0.9198 0.8561 0.4804 11.00000 0.05 0.37 Q14 1 0.9805 0.5659 0.5614 11.00000 0.05 0.36 Q15 1 0.6459 0.8761 0.6772 11.00000 0.05 0.35 Q16 1 0.9525 0.9855 0.2582 11.00000 0.05 0.35 Q17 1 0.7451 0.7868 0.4200 11.00000 0.05 0.34 Q18 1 0.9008 0.8246 0.8690 11.00000 0.05 0.34 Q19 1 0.8652 0.8056 1.0557 11.00000 0.05 0.34 Q20 1 0.7506 0.7002 0.6375 11.00000 0.05 0.33 ; _shelx_res_checksum 15457