#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:49:31 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705219.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705219 loop_ _publ_author_name 'Kataoka, Yusuke' 'Kohara, Yoshihiro' 'Yano, Natsumi' 'Kawamoto, Tatsuya' _publ_section_title ; Unique Vapochromism of a Paddlewheel-type Dirhodium Complex Accompanied by Dynamic Structural and Phase Transitions ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02672G _journal_year 2020 _chemical_formula_sum 'C34 H54 N2 O8 Rh2' _chemical_formula_weight 824.61 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-07-23 deposited with the CCDC. 2020-08-19 downloaded from the CCDC. ; _cell_angle_alpha 113.792(5) _cell_angle_beta 99.705(4) _cell_angle_gamma 92.156(3) _cell_formula_units_Z 1 _cell_length_a 8.2724(3) _cell_length_b 10.7362(5) _cell_length_c 11.2851(6) _cell_measurement_reflns_used 5845 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.7670 _cell_measurement_theta_min 2.0600 _cell_volume 897.75(8) _computing_cell_refinement 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_molecular_graphics 'CrystalStructure 4.3 (Rigaku, 2018)' _computing_publication_material 'CrystalStructure 4.3 (Rigaku, 2018)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_unetI/netI 0.0504 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7716 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.452 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.72608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 426 _exptl_crystal_size_max 0.573 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.184 _refine_diff_density_max 1.265 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3153 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0379 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.6420P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.0956 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2971 _reflns_number_total 3153 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02672g2.cif _cod_data_source_block '[Rh2(HC)4(py)2]' _cod_database_code 7705219 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL koh-2-006-pyridine CELL 0.71075 8.27240 10.73620 11.28510 113.79200 99.70500 92.15600 ZERR 1 0.00030 0.00050 0.00060 0.00500 0.00400 0.00300 LATT 1 SFAC C H N O RH UNIT 34 54 2 8 2 SHEL 6.268407 0.840885 L.S. 50 FMAP 2 PLAN 5 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -123 ACTA SIMU 0.0200 0.0000 C10 C12 C11 WGHT 0.042800 1.642000 FVAR 1.42394 RH1 5 0.451073 0.103845 1.000774 11.00000 0.01751 0.01357 = 0.02021 0.00526 0.00343 0.00060 O2 4 0.582841 0.203200 1.188366 11.00000 0.02723 0.01771 = 0.02307 0.00564 0.00180 0.00280 O1 4 0.325289 -0.008069 0.812378 11.00000 0.02816 0.01708 = 0.02604 0.00781 0.00219 0.00206 O3 4 0.652329 0.133778 0.929304 11.00000 0.02534 0.01962 = 0.03393 0.01197 0.01054 0.00245 O4 4 0.256644 0.060962 1.072138 11.00000 0.02122 0.02146 = 0.03448 0.01203 0.00986 0.00391 N1 3 0.359973 0.298357 1.003464 11.00000 0.01832 0.01543 = 0.02155 0.00580 0.00469 -0.00034 C1 1 0.664984 0.135725 1.241153 11.00000 0.02064 0.02267 = 0.02429 0.00957 0.00510 0.00067 C2 1 0.763095 0.211511 1.378674 11.00000 0.03224 0.02340 = 0.02413 0.00813 0.00077 0.00234 AFIX 23 H2A 2 0.881410 0.203835 1.375881 11.00000 -1.20000 H2B 2 0.733128 0.164927 1.433173 11.00000 -1.20000 AFIX 0 C3 1 0.742475 0.362503 1.448050 11.00000 0.03221 0.02285 = 0.02109 0.00625 0.00315 0.00259 AFIX 23 H3A 2 0.773631 0.410848 1.395356 11.00000 -1.20000 H3B 2 0.624878 0.371810 1.452881 11.00000 -1.20000 AFIX 0 C4 1 0.846851 0.429454 1.586245 11.00000 0.03239 0.02525 = 0.02191 0.00570 0.00425 0.00173 AFIX 23 H4A 2 0.963509 0.414824 1.581731 11.00000 -1.20000 H4B 2 0.810939 0.384521 1.640261 11.00000 -1.20000 AFIX 0 C5 1 0.835615 0.582359 1.653907 11.00000 0.04315 0.02518 = 0.02027 0.00733 0.00596 0.00747 AFIX 23 H5A 2 0.863903 0.626258 1.596787 11.00000 -1.20000 H5B 2 0.720287 0.596620 1.663988 11.00000 -1.20000 AFIX 0 C6 1 0.948610 0.651516 1.788337 11.00000 0.04190 0.02464 = 0.02520 0.00135 0.00910 0.00385 AFIX 33 H6A 2 0.936013 0.749464 1.826933 11.00000 -1.20000 H6B 2 0.919665 0.610120 1.846215 11.00000 -1.20000 H6C 2 1.063371 0.639776 1.778972 11.00000 -1.20000 AFIX 0 C7 1 0.751814 0.045572 0.907021 11.00000 0.02042 0.02278 = 0.02560 0.00685 0.00504 -0.00059 C8 1 0.895933 0.070008 0.848804 11.00000 0.02037 0.03233 = 0.04091 0.01821 0.01011 0.00146 AFIX 23 H8A 2 0.972906 0.148530 0.917102 11.00000 -1.20000 H8B 2 0.956211 -0.011805 0.824313 11.00000 -1.20000 AFIX 0 C9 1 0.844188 0.098887 0.729018 11.00000 0.04165 0.06733 = 0.03624 0.01805 0.00882 -0.00862 AFIX 23 H9A 2 0.801154 0.189030 0.758515 11.00000 -1.20000 H9B 2 0.944615 0.108337 0.695028 11.00000 -1.20000 AFIX 0 C10 1 0.719821 -0.000293 0.617049 11.00000 0.09885 0.09325 = 0.04899 0.01049 0.00729 -0.02384 AFIX 23 H10A 2 0.631141 -0.025749 0.654902 11.00000 -1.20000 H10B 2 0.670243 0.049401 0.565355 11.00000 -1.20000 AFIX 0 C12 1 0.635708 -0.226938 0.422638 11.00000 0.08330 0.07366 = 0.09528 -0.01145 0.02564 -0.01476 AFIX 33 H12A 2 0.691824 -0.303350 0.371246 11.00000 -1.20000 H12B 2 0.556419 -0.259945 0.461972 11.00000 -1.20000 H12C 2 0.577211 -0.188648 0.364426 11.00000 -1.20000 AFIX 0 C13 1 0.411546 0.419214 1.105349 11.00000 0.02358 0.02457 = 0.02816 0.01128 0.00442 0.00234 AFIX 43 H13 2 0.488741 0.422553 1.179456 11.00000 -1.20000 AFIX 0 C14 1 0.357054 0.539147 1.107032 11.00000 0.03076 0.01639 = 0.03244 0.00307 0.00795 0.00071 AFIX 43 H14 2 0.397692 0.623721 1.180712 11.00000 -1.20000 AFIX 0 C15 1 0.243719 0.536179 1.001838 11.00000 0.03131 0.02185 = 0.04074 0.01303 0.00764 0.00560 AFIX 43 H15 2 0.203907 0.617916 1.001511 11.00000 -1.20000 AFIX 0 C16 1 0.189028 0.410989 0.896320 11.00000 0.02842 0.02525 = 0.03330 0.01321 -0.00116 0.00244 AFIX 43 H16 2 0.110302 0.404814 0.821822 11.00000 -1.20000 AFIX 0 C17 1 0.250695 0.295371 0.901106 11.00000 0.02134 0.01799 = 0.02708 0.00663 0.00319 -0.00029 AFIX 43 H17 2 0.213509 0.209655 0.828025 11.00000 -1.20000 AFIX 0 C11 1 0.761086 -0.117744 0.530518 11.00000 0.08331 0.07367 = 0.09530 -0.01146 0.02564 -0.01475 AFIX 23 H11A 2 0.821258 -0.162180 0.583472 11.00000 -1.20000 H11B 2 0.841879 -0.091469 0.486729 11.00000 -1.20000 AFIX 0 HKLF 4 REM koh-2-006-pyridine REM R1 = 0.0379 for 2971 Fo > 4sig(Fo) and 0.0397 for all 3153 data REM 208 parameters refined using 12 restraints END WGHT 0.0428 1.6420 REM Instructions for potential hydrogen bonds HTAB C13 O2 HTAB C17 O1 REM Highest difference peak 1.265, deepest hole -1.097, 1-sigma level 0.107 Q1 1 0.7611 -0.0811 0.6393 11.00000 0.05 1.26 Q2 1 0.6532 -0.1127 0.5732 11.00000 0.05 1.04 Q3 1 0.7015 -0.0732 0.4729 11.00000 0.05 0.97 Q4 1 0.8762 -0.0195 0.7069 11.00000 0.05 0.85 Q5 1 0.8208 -0.0318 0.5814 11.00000 0.05 0.82 ; _shelx_res_checksum 68982 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.45107(3) 0.10384(2) 1.00077(3) 0.01776(12) Uani 1 1 d . . . . . O2 O 0.5828(3) 0.2032(2) 1.1884(3) 0.0240(6) Uani 1 1 d . . . . . O1 O 0.3253(3) -0.0081(2) 0.8124(3) 0.0246(6) Uani 1 1 d . . . . . O3 O 0.6523(3) 0.1338(2) 0.9293(3) 0.0254(6) Uani 1 1 d . . . . . O4 O 0.2566(3) 0.0610(2) 1.0721(3) 0.0250(6) Uani 1 1 d . . . . . N1 N 0.3600(3) 0.2984(3) 1.0035(3) 0.0190(6) Uani 1 1 d . . . . . C1 C 0.6650(4) 0.1357(4) 1.2412(4) 0.0226(8) Uani 1 1 d . . . . . C2 C 0.7631(5) 0.2115(4) 1.3787(4) 0.0278(8) Uani 1 1 d . . . . . H2A H 0.8814 0.2038 1.3759 0.033 Uiso 1 1 calc R U . . . H2B H 0.7331 0.1649 1.4332 0.033 Uiso 1 1 calc R U . . . C3 C 0.7425(5) 0.3625(4) 1.4481(4) 0.0266(8) Uani 1 1 d . . . . . H3A H 0.7736 0.4108 1.3954 0.032 Uiso 1 1 calc R U . . . H3B H 0.6249 0.3718 1.4529 0.032 Uiso 1 1 calc R U . . . C4 C 0.8469(5) 0.4295(4) 1.5862(4) 0.0281(8) Uani 1 1 d . . . . . H4A H 0.9635 0.4148 1.5817 0.034 Uiso 1 1 calc R U . . . H4B H 0.8109 0.3845 1.6403 0.034 Uiso 1 1 calc R U . . . C5 C 0.8356(5) 0.5824(4) 1.6539(4) 0.0302(9) Uani 1 1 d . . . . . H5A H 0.8639 0.6263 1.5968 0.036 Uiso 1 1 calc R U . . . H5B H 0.7203 0.5966 1.6640 0.036 Uiso 1 1 calc R U . . . C6 C 0.9486(5) 0.6515(4) 1.7883(4) 0.0333(9) Uani 1 1 d . . . . . H6A H 0.9360 0.7495 1.8269 0.040 Uiso 1 1 calc R U . . . H6B H 0.9197 0.6101 1.8462 0.040 Uiso 1 1 calc R U . . . H6C H 1.0634 0.6398 1.7790 0.040 Uiso 1 1 calc R U . . . C7 C 0.7518(4) 0.0456(4) 0.9070(4) 0.0240(8) Uani 1 1 d . . . . . C8 C 0.8959(4) 0.0700(4) 0.8488(4) 0.0298(9) Uani 1 1 d . . . . . H8A H 0.9729 0.1485 0.9171 0.036 Uiso 1 1 calc R U . . . H8B H 0.9562 -0.0118 0.8243 0.036 Uiso 1 1 calc R U . . . C9 C 0.8442(6) 0.0989(6) 0.7290(5) 0.0499(13) Uani 1 1 d . . . . . H9A H 0.8012 0.1890 0.7585 0.060 Uiso 1 1 calc R U . . . H9B H 0.9446 0.1083 0.6950 0.060 Uiso 1 1 calc R U . . . C10 C 0.7198(9) -0.0003(8) 0.6170(6) 0.089(2) Uani 1 1 d . U . . . H10A H 0.6311 -0.0257 0.6549 0.106 Uiso 1 1 calc R U . . . H10B H 0.6702 0.0494 0.5654 0.106 Uiso 1 1 calc R U . . . C12 C 0.6357(9) -0.2269(7) 0.4226(8) 0.0992(13) Uani 1 1 d . U . . . H12A H 0.6918 -0.3033 0.3712 0.119 Uiso 1 1 calc R U . . . H12B H 0.5564 -0.2599 0.4620 0.119 Uiso 1 1 calc R U . . . H12C H 0.5772 -0.1886 0.3644 0.119 Uiso 1 1 calc R U . . . C13 C 0.4115(4) 0.4192(4) 1.1053(4) 0.0254(8) Uani 1 1 d . . . . . H13 H 0.4887 0.4226 1.1795 0.031 Uiso 1 1 calc R U . . . C14 C 0.3571(5) 0.5391(4) 1.1070(4) 0.0287(9) Uani 1 1 d . . . . . H14 H 0.3977 0.6237 1.1807 0.034 Uiso 1 1 calc R U . . . C15 C 0.2437(5) 0.5362(4) 1.0018(4) 0.0312(9) Uani 1 1 d . . . . . H15 H 0.2039 0.6179 1.0015 0.037 Uiso 1 1 calc R U . . . C16 C 0.1890(5) 0.4110(4) 0.8963(4) 0.0296(9) Uani 1 1 d . . . . . H16 H 0.1103 0.4048 0.8218 0.036 Uiso 1 1 calc R U . . . C17 C 0.2507(4) 0.2954(4) 0.9011(4) 0.0233(8) Uani 1 1 d . . . . . H17 H 0.2135 0.2097 0.8280 0.028 Uiso 1 1 calc R U . . . C11 C 0.7611(9) -0.1177(7) 0.5305(8) 0.0992(13) Uani 1 1 d . U . . . H11A H 0.8213 -0.1622 0.5835 0.119 Uiso 1 1 calc R U . . . H11B H 0.8419 -0.0915 0.4867 0.119 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01751(18) 0.01357(17) 0.02021(19) 0.00526(13) 0.00343(12) 0.00060(11) O2 0.0272(13) 0.0177(12) 0.0231(14) 0.0056(11) 0.0018(11) 0.0028(10) O1 0.0282(13) 0.0171(12) 0.0260(14) 0.0078(11) 0.0022(11) 0.0021(10) O3 0.0253(13) 0.0196(12) 0.0339(15) 0.0120(12) 0.0105(11) 0.0025(11) O4 0.0212(13) 0.0215(13) 0.0345(15) 0.0120(12) 0.0099(11) 0.0039(10) N1 0.0183(14) 0.0154(14) 0.0216(16) 0.0058(13) 0.0047(12) -0.0003(11) C1 0.0206(17) 0.0227(18) 0.0243(19) 0.0096(16) 0.0051(15) 0.0007(14) C2 0.032(2) 0.0234(19) 0.024(2) 0.0081(16) 0.0008(16) 0.0023(16) C3 0.032(2) 0.0228(18) 0.0211(19) 0.0062(16) 0.0031(16) 0.0026(15) C4 0.032(2) 0.0253(19) 0.022(2) 0.0057(16) 0.0042(16) 0.0017(16) C5 0.043(2) 0.0252(19) 0.020(2) 0.0073(16) 0.0060(17) 0.0075(17) C6 0.042(2) 0.0246(19) 0.025(2) 0.0013(17) 0.0091(18) 0.0039(17) C7 0.0204(17) 0.0228(18) 0.026(2) 0.0068(16) 0.0050(15) -0.0006(15) C8 0.0204(18) 0.032(2) 0.041(2) 0.0182(19) 0.0101(17) 0.0015(15) C9 0.042(3) 0.067(3) 0.036(3) 0.018(2) 0.009(2) -0.009(2) C10 0.099(5) 0.093(5) 0.049(4) 0.010(4) 0.007(3) -0.024(4) C12 0.083(2) 0.074(2) 0.095(2) -0.011(2) 0.0256(19) -0.0148(19) C13 0.0236(18) 0.0246(18) 0.028(2) 0.0113(17) 0.0044(15) 0.0023(15) C14 0.031(2) 0.0164(17) 0.032(2) 0.0031(16) 0.0079(17) 0.0007(15) C15 0.031(2) 0.0219(19) 0.041(2) 0.0130(18) 0.0076(18) 0.0056(16) C16 0.028(2) 0.0252(19) 0.033(2) 0.0132(17) -0.0012(17) 0.0024(16) C17 0.0213(17) 0.0180(17) 0.027(2) 0.0066(15) 0.0032(15) -0.0003(14) C11 0.083(2) 0.074(2) 0.095(2) -0.011(2) 0.0256(19) -0.0148(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rh1 O4 89.77(11) . . ? O2 Rh1 O1 175.98(9) . . ? O4 Rh1 O1 90.22(11) . . ? O2 Rh1 O3 90.04(11) . . ? O4 Rh1 O3 175.73(9) . . ? O1 Rh1 O3 89.67(11) . . ? O2 Rh1 N1 91.49(10) . . ? O4 Rh1 N1 92.19(10) . . ? O1 Rh1 N1 92.53(10) . . ? O3 Rh1 N1 92.08(10) . . ? O2 Rh1 Rh1 88.21(7) . 2_657 ? O4 Rh1 Rh1 87.69(7) . 2_657 ? O1 Rh1 Rh1 87.77(7) . 2_657 ? O3 Rh1 Rh1 88.04(7) . 2_657 ? N1 Rh1 Rh1 179.68(8) . 2_657 ? C1 O2 Rh1 119.0(2) . . ? C1 O1 Rh1 119.0(2) 2_657 . ? C7 O3 Rh1 118.7(2) . . ? C7 O4 Rh1 119.2(2) 2_657 . ? C17 N1 C13 118.0(3) . . ? C17 N1 Rh1 119.9(2) . . ? C13 N1 Rh1 122.1(3) . . ? O2 C1 O1 126.0(3) . 2_657 ? O2 C1 C2 118.0(3) . . ? O1 C1 C2 116.0(3) 2_657 . ? C1 C2 C3 116.6(3) . . ? C1 C2 H2A 108.1 . . ? C3 C2 H2A 108.1 . . ? C1 C2 H2B 108.1 . . ? C3 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C2 112.4(3) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 113.0(3) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 113.2(3) . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 O4 126.4(3) . 2_657 ? O3 C7 C8 116.5(3) . . ? O4 C7 C8 117.1(3) 2_657 . ? C9 C8 C7 113.2(3) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 118.7(5) . . ? C10 C9 H9A 107.7 . . ? C8 C9 H9A 107.7 . . ? C10 C9 H9B 107.7 . . ? C8 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 H10A 107.0 . . ? C9 C10 H10A 107.0 . . ? C11 C10 H10B 107.0 . . ? C9 C10 H10B 107.0 . . ? H10A C10 H10B 106.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.4(4) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 118.2(4) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C17 C16 C15 118.8(4) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? N1 C17 C16 122.9(3) . . ? N1 C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? C10 C11 C12 122.8(7) . . ? C10 C11 H11A 106.6 . . ? C12 C11 H11A 106.6 . . ? C10 C11 H11B 106.6 . . ? C12 C11 H11B 106.6 . . ? H11A C11 H11B 106.6 . . ? 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 O2 2.030(3) . ? Rh1 O4 2.032(2) . ? Rh1 O1 2.036(3) . ? Rh1 O3 2.036(2) . ? Rh1 N1 2.237(3) . ? Rh1 Rh1 2.3951(5) 2_657 ? O2 C1 1.261(4) . ? O1 C1 1.267(4) 2_657 ? O3 C7 1.254(4) . ? O4 C7 1.259(5) 2_657 ? N1 C17 1.330(5) . ? N1 C13 1.333(5) . ? C1 O1 1.267(4) 2_657 ? C1 C2 1.495(5) . ? C2 C3 1.520(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.512(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O4 1.259(4) 2_657 ? C7 C8 1.517(5) . ? C8 C9 1.503(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.477(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.346(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C11 1.504(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.372(6) . ? C14 H14 0.9500 . ? C15 C16 1.382(6) . ? C15 H15 0.9500 . ? C16 C17 1.377(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? 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 Rh1 O2 C1 O1 0.2(5) . . . 2_657 ? Rh1 O2 C1 C2 179.1(2) . . . . ? O2 C1 C2 C3 5.5(5) . . . . ? O1 C1 C2 C3 -175.5(3) 2_657 . . . ? C1 C2 C3 C4 -180.0(3) . . . . ? C2 C3 C4 C5 176.5(3) . . . . ? C3 C4 C5 C6 -176.1(3) . . . . ? Rh1 O3 C7 O4 -2.1(5) . . . 2_657 ? Rh1 O3 C7 C8 177.7(2) . . . . ? O3 C7 C8 C9 -50.9(5) . . . . ? O4 C7 C8 C9 128.9(4) 2_657 . . . ? C7 C8 C9 C10 -54.5(6) . . . . ? C8 C9 C10 C11 -78.5(9) . . . . ? C17 N1 C13 C14 -0.6(5) . . . . ? Rh1 N1 C13 C14 179.4(3) . . . . ? N1 C13 C14 C15 1.0(6) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C17 -0.2(6) . . . . ? C13 N1 C17 C16 -0.1(5) . . . . ? Rh1 N1 C17 C16 179.8(3) . . . . ? C15 C16 C17 N1 0.6(6) . . . . ? C9 C10 C11 C12 174.4(7) . . . . ?