# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_BMOF-dcppy-x(Ir) _database_code_depnum_ccdc_archive 'CCDC 875225' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BMOF-1-dcppy-Ir _chemical_melting_point ? _chemical_formula_moiety 'C34 H18 Ir0.11 N4 O8 Zn2' _chemical_formula_sum 'C34 H18 Ir0.11 N4 O8 Zn2' _chemical_formula_weight 761.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0368(15) _cell_length_b 15.1189(17) _cell_length_c 15.1242(17) _cell_angle_alpha 85.358(6) _cell_angle_beta 85.555(5) _cell_angle_gamma 86.350(6) _cell_volume 3184.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 5570 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 58.39 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 763.4 _exptl_crystal_F_000' 759.80 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 15103 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 58.91 _reflns_number_total 8026 _reflns_number_gt 5913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to the weak diffraction and fragility of the MOF crystal, the structure was collected at 230K and Cu X-ray source was used. In addition, we have tried our best to obtain a high completeness. But since the crystal was in triclinic unit cell, it is difficult to obtained high completeness and high redundancy. Due to disorders and weak diffraction, the structure was refined isotropically rather than anisotropically. The nitrogen atoms on dcppy ligand were refined as disordered over 2 positions, which has a ~50% occupancy each. We also attempted to refined the nitrogen as disordered over 4 positions and each position has a ~25% occupancy, but it resulted in an alert_A from check_Cif that there were wrong atoms assigments and high shift/su ratio. Only a model of nitrogen atom were refined as disodered over 4 positions which each has an occupancy of ~100% fit well. However, this is not possible. Since the occupancy of Ir was low ~<10% per dcppy ligand, we were unable to locate any other ligands that bound to Ir. Thus, checkCIF gave us an Alert_A on low/ unusual single bonded metal atoms. In addition, we do not use any restraint on Ir atom to ensure the corrected assigment (the bond distance Ir-C and Ir-N were found to be ~1.95 Angstrom). SQUEEZE protocol found 394 electrons that can be accounted for ~10 THF molecules in the pores. 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^)+(0.2000P)^2^+0.0000P] 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 'not measured' _refine_ls_number_reflns 8026 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.1074 _refine_ls_wR_factor_ref 0.3298 _refine_ls_wR_factor_gt 0.3089 _refine_ls_goodness_of_fit_ref 1.337 _refine_ls_restrained_S_all 1.337 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.019 0.001 -0.004 1804 394 ' ' _platon_squeeze_details ; ; 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 N1 N 0.0469(3) 0.6111(3) 0.3369(3) 0.0378(10) Uiso 1 1 d . . . O1 O -0.2700(3) 0.6173(3) 0.2143(3) 0.0588(11) Uiso 1 1 d . . . O7 O -0.2917(3) 0.6113(3) 0.4808(3) 0.0533(10) Uiso 1 1 d . . . O8 O -0.1336(3) 0.6096(3) 0.4653(3) 0.0540(10) Uiso 1 1 d . . . O2 O -0.1116(3) 0.5971(3) 0.2012(3) 0.0578(11) Uiso 1 1 d . . . C9 C 0.2427(4) 0.6158(4) 0.3397(4) 0.0434(13) Uiso 1 1 d . . . O5 O -0.2791(3) 0.4807(3) 0.3524(3) 0.0608(12) Uiso 1 1 d . . . O3 O -0.1312(4) 0.7381(3) 0.3163(3) 0.0677(12) Uiso 1 1 d . . . O6 O -0.1186(3) 0.4718(3) 0.3466(3) 0.0594(11) Uiso 1 1 d . . . O4 O -0.2912(4) 0.7473(3) 0.3404(3) 0.0670(12) Uiso 1 1 d . . . C8 C 0.1845(5) 0.6111(4) 0.4172(4) 0.0551(16) Uiso 1 1 d . . . H8 H 0.2111 0.6097 0.4725 0.066 Uiso 1 1 calc R . . C3 C -0.2126(4) 0.6110(4) 0.5114(4) 0.0395(13) Uiso 1 1 d . . . C2 C -0.1924(4) 0.6091(4) 0.1699(4) 0.0453(14) Uiso 1 1 d . . . C7 C 0.0884(5) 0.6087(4) 0.4134(4) 0.0510(15) Uiso 1 1 d . . . H7 H 0.0496 0.6051 0.4670 0.061 Uiso 1 1 calc R . . C1 C -0.1979(4) 0.4359(4) 0.3455(4) 0.0477(14) Uiso 1 1 d . . . C6 C 0.1042(5) 0.6176(4) 0.2610(4) 0.0548(16) Uiso 1 1 d . . . H6 H 0.0762 0.6207 0.2062 0.066 Uiso 1 1 calc R . . C5 C -0.1935(4) 0.6078(4) 0.0709(4) 0.0472(14) Uiso 1 1 d . . . C16 C -0.2007(5) 0.6112(5) -0.1107(5) 0.0647(18) Uiso 1 1 d . . . C10 C -0.1999(5) 0.3397(5) 0.3388(4) 0.0594(17) Uiso 1 1 d . . . C4 C 0.1994(5) 0.6198(5) 0.2610(5) 0.0590(17) Uiso 1 1 d . . . H4 H 0.2369 0.6241 0.2067 0.071 Uiso 1 1 calc R . . C19 C -0.2093(5) 0.8783(5) 0.3196(5) 0.0664(18) Uiso 1 1 d . . . C13 C -0.1141(6) 0.5903(5) 0.0188(5) 0.075(2) Uiso 1 1 d . . . H13 H -0.0554 0.5783 0.0445 0.090 Uiso 1 1 calc R . . C14 C -0.2773(7) 0.6286(6) 0.0317(6) 0.085(2) Uiso 1 1 d . . . H14 H -0.3346 0.6396 0.0665 0.102 Uiso 1 1 calc R . . C11 C -0.2848(7) 0.2977(6) 0.3428(6) 0.087(2) Uiso 1 1 d . . . H11 H -0.3434 0.3311 0.3500 0.104 Uiso 1 1 calc R . . C18 C -0.2108(5) 0.7817(4) 0.3264(4) 0.0516(15) Uiso 1 1 d . . . C12 C -0.1178(8) 0.2894(7) 0.3215(7) 0.101(3) Uiso 1 1 d . . . H12 H -0.0595 0.3171 0.3110 0.122 Uiso 1 1 calc R . . C15 C -0.2034(7) 0.1593(6) 0.3238(6) 0.085(2) Uiso 1 1 d . . . C23 C -0.2045(7) 0.0622(6) 0.3198(6) 0.089(2) Uiso 1 1 d . . . C20 C -0.2877(9) 0.9318(8) 0.3368(7) 0.117(4) Uiso 1 1 d . . . H20 H -0.3471 0.9062 0.3479 0.141 Uiso 1 1 calc R . . C24 C -0.1265(9) -0.0782(8) 0.2947(7) 0.112(3) Uiso 1 1 d . . . H24 H -0.0698 -0.1117 0.2789 0.135 Uiso 1 1 calc R A 2 N2 N -0.4540(3) 0.6149(3) 0.3462(3) 0.0353(10) Uiso 1 1 d . . . C17 C 0.3509(4) 0.6141(4) 0.3413(4) 0.0414(13) Uiso 1 1 d . . . C22 C -0.5104(7) 0.6009(6) 0.4162(6) 0.090(3) Uiso 1 1 d . . . H22 H -0.4830 0.5924 0.4712 0.108 Uiso 1 1 calc R . . C26 C 0.3948(8) 0.5977(7) 0.4165(7) 0.105(3) Uiso 1 1 d . . . H26 H 0.3587 0.5837 0.4702 0.126 Uiso 1 1 calc R . . C25 C 0.4072(9) 0.6237(8) 0.2698(8) 0.114(3) Uiso 1 1 d . . . H25 H 0.3795 0.6309 0.2148 0.137 Uiso 1 1 calc R . . C21 C -0.4930(9) 0.6240(8) 0.2694(8) 0.115(3) Uiso 1 1 d . . . H21 H -0.4549 0.6306 0.2156 0.138 Uiso 1 1 calc R . . C28 C -0.2112(4) 0.6148(4) 0.6112(4) 0.0475(14) Uiso 1 1 d . . . C30 C -0.2919(5) 0.6197(5) 0.6645(4) 0.0601(17) Uiso 1 1 d . . . H30 H -0.3512 0.6229 0.6392 0.072 Uiso 1 1 calc R . . C29 C -0.1219(5) 0.6085(5) 0.6492(5) 0.0604(17) Uiso 1 1 d . . . H29 H -0.0645 0.6060 0.6129 0.072 Uiso 1 1 calc R . . C27 C -0.2038(5) 0.6121(5) -0.2086(5) 0.0650(18) Uiso 1 1 d . . . Ir2 Ir -0.3829(6) 0.1190(5) 0.3372(5) 0.103(2) Uiso 0.06 1 d P . . Ir1 Ir -0.0354(17) 0.0910(15) 0.3290(14) 0.190(7) Uiso 0.05 1 d P . . Zn1 Zn -0.30756(5) 0.61515(5) 0.34728(4) 0.0375(4) Uani 1 1 d . . . Zn2 Zn -0.09796(5) 0.60461(5) 0.33369(4) 0.0374(4) Uani 1 1 d . . . N4A N -0.1252(9) 0.0110(8) 0.2925(8) 0.069(3) Uiso 0.510(10) 1 d P . 2 N6A N -0.2904(5) 0.6202(5) -0.2452(5) 0.028(2) Uiso 0.510(10) 1 d P . 2 N4B N -0.2845(9) 0.0214(9) 0.3386(8) 0.070(4) Uiso 0.490(10) 1 d P . 1 N6B N -0.1206(5) 0.6062(5) -0.2628(5) 0.026(2) Uiso 0.490(10) 1 d P . 1 C42 C -0.2765(7) 0.6331(6) -0.0567(6) 0.084(2) Uiso 1 1 d . . . H42 H -0.3334 0.6530 -0.0827 0.101 Uiso 1 1 calc R . . C43 C -0.1173(7) 0.5895(6) -0.0722(6) 0.090(3) Uiso 1 1 d . . . H43 H -0.0617 0.5739 -0.1075 0.108 Uiso 1 1 calc R . . C40 C -0.2845(7) 0.2078(6) 0.3364(6) 0.088(2) Uiso 1 1 d . . . C41 C -0.1183(9) 0.1988(9) 0.3190(8) 0.122(4) Uiso 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 Zn1 0.0277(5) 0.0466(6) 0.0385(5) -0.0056(3) -0.0028(3) -0.0014(3) Zn2 0.0273(5) 0.0472(6) 0.0381(5) -0.0060(3) -0.0019(3) -0.0019(3) _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 N1 C7 1.332(8) . ? N1 C6 1.350(8) . ? N1 Zn2 2.047(5) . ? O1 C2 1.239(7) . ? O1 Zn1 2.038(4) . ? O7 C3 1.236(7) . ? O7 Zn1 2.044(4) . ? O8 C3 1.263(7) . ? O8 Zn2 2.021(4) . ? O2 C2 1.260(7) . ? O2 Zn2 2.040(4) . ? C9 C4 1.374(9) . ? C9 C8 1.376(9) . ? C9 C17 1.520(10) . ? O5 C1 1.289(8) . ? O5 Zn1 2.043(5) . ? O3 C18 1.266(8) . ? O3 Zn2 2.043(5) . ? O6 C1 1.271(8) . ? O6 Zn2 2.039(5) . ? O4 C18 1.268(8) . ? O4 Zn1 2.019(5) . ? C8 C7 1.357(10) . ? C8 H8 0.9400 . ? C3 C28 1.517(8) . ? C2 C5 1.500(8) . ? C7 H7 0.9400 . ? C1 C10 1.468(10) . ? C6 C4 1.339(10) . ? C6 H6 0.9400 . ? C5 C13 1.339(10) . ? C5 C14 1.366(10) . ? C16 C42 1.332(11) . ? C16 C43 1.357(11) . ? C16 C27 1.483(11) . ? C10 C12 1.360(13) . ? C10 C11 1.381(11) . ? C4 H4 0.9400 . ? C19 C20 1.345(14) . ? C19 C24 1.384(14) 1_565 ? C19 C18 1.458(10) . ? C13 C43 1.381(12) . ? C13 H13 0.9400 . ? C14 C42 1.331(12) . ? C14 H14 0.9400 . ? C11 C40 1.370(13) . ? C11 H11 0.9400 . ? C12 C41 1.373(15) . ? C12 H12 0.9400 . ? C15 C40 1.324(12) . ? C15 C41 1.364(15) . ? C15 C23 1.475(14) . ? C15 Ir1 2.52(2) . ? C15 Ir2 2.619(11) . ? C23 N4B 1.317(16) . ? C23 N4A 1.371(15) . ? C23 Ir1 2.46(2) . ? C23 Ir2 2.596(12) . ? C20 N4B 1.361(17) 1_565 ? C20 H20 0.9400 . ? C24 N4A 1.348(16) . ? C24 C19 1.383(14) 1_545 ? C24 H24 0.9400 . ? N2 C22 1.283(11) . ? N2 C21 1.317(12) . ? N2 Zn1 2.057(5) . ? C17 C25 1.293(13) . ? C17 C26 1.334(12) . ? C22 C26 1.334(14) 1_455 ? C22 H22 0.9400 . ? C26 C22 1.334(14) 1_655 ? C26 H26 0.9400 . ? C25 C21 1.401(17) 1_655 ? C25 H25 0.9400 . ? C21 C25 1.401(17) 1_455 ? C21 H21 0.9400 . ? C28 C30 1.340(9) . ? C28 C29 1.414(9) . ? C30 N6A 1.367(10) 1_556 ? C30 H30 0.9400 . ? C29 N6B 1.330(10) 1_556 ? C29 H29 0.9400 . ? C27 N6A 1.369(10) . ? C27 N6B 1.377(11) . ? Ir2 N4B 1.955(15) . ? Ir2 C40 1.986(12) . ? Ir1 N4A 1.94(3) . ? Ir1 C41 1.94(3) . ? Zn1 Zn2 2.9284(10) . ? N6A C30 1.367(10) 1_554 ? N4B C20 1.361(17) 1_545 ? N6B C29 1.330(10) 1_554 ? C42 H42 0.9400 . ? C43 H43 0.9400 . ? 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 C7 N1 C6 117.5(5) . . ? C7 N1 Zn2 121.6(4) . . ? C6 N1 Zn2 120.9(4) . . ? C2 O1 Zn1 133.5(4) . . ? C3 O7 Zn1 122.5(4) . . ? C3 O8 Zn2 133.2(4) . . ? C2 O2 Zn2 120.6(4) . . ? C4 C9 C8 117.5(6) . . ? C4 C9 C17 121.3(6) . . ? C8 C9 C17 121.2(5) . . ? C1 O5 Zn1 129.5(4) . . ? C18 O3 Zn2 130.4(5) . . ? C1 O6 Zn2 126.4(4) . . ? C18 O4 Zn1 123.6(5) . . ? C7 C8 C9 119.6(6) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? O7 C3 O8 124.6(5) . . ? O7 C3 C28 117.2(5) . . ? O8 C3 C28 118.2(5) . . ? O1 C2 O2 125.4(6) . . ? O1 C2 C5 118.2(5) . . ? O2 C2 C5 116.2(5) . . ? N1 C7 C8 122.6(6) . . ? N1 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? O6 C1 O5 122.4(6) . . ? O6 C1 C10 120.3(6) . . ? O5 C1 C10 117.3(5) . . ? C4 C6 N1 122.3(6) . . ? C4 C6 H6 118.9 . . ? N1 C6 H6 118.9 . . ? C13 C5 C14 118.4(7) . . ? C13 C5 C2 122.3(6) . . ? C14 C5 C2 119.3(6) . . ? C42 C16 C43 116.6(8) . . ? C42 C16 C27 123.1(7) . . ? C43 C16 C27 120.2(8) . . ? C12 C10 C11 117.1(9) . . ? C12 C10 C1 120.9(7) . . ? C11 C10 C1 121.8(7) . . ? C6 C4 C9 120.5(7) . . ? C6 C4 H4 119.8 . . ? C9 C4 H4 119.8 . . ? C20 C19 C24 115.0(10) . 1_565 ? C20 C19 C18 122.8(8) . . ? C24 C19 C18 122.2(8) 1_565 . ? C5 C13 C43 121.0(8) . . ? C5 C13 H13 119.5 . . ? C43 C13 H13 119.5 . . ? C42 C14 C5 118.9(9) . . ? C42 C14 H14 120.5 . . ? C5 C14 H14 120.5 . . ? C40 C11 C10 120.6(9) . . ? C40 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? O3 C18 O4 124.7(7) . . ? O3 C18 C19 117.1(6) . . ? O4 C18 C19 118.2(6) . . ? C10 C12 C41 121.4(10) . . ? C10 C12 H12 119.3 . . ? C41 C12 H12 119.3 . . ? C40 C15 C41 119.6(11) . . ? C40 C15 C23 120.3(9) . . ? C41 C15 C23 120.0(10) . . ? C40 C15 Ir1 165.4(9) . . ? C41 C15 Ir1 50.0(8) . . ? C23 C15 Ir1 70.5(7) . . ? C40 C15 Ir2 47.7(5) . . ? C41 C15 Ir2 167.3(9) . . ? C23 C15 Ir2 72.7(6) . . ? Ir1 C15 Ir2 142.4(7) . . ? N4B C23 N4A 116.9(11) . . ? N4B C23 C15 120.5(10) . . ? N4A C23 C15 122.6(10) . . ? N4B C23 Ir1 157.0(9) . . ? N4A C23 Ir1 52.0(8) . . ? C15 C23 Ir1 75.0(7) . . ? N4B C23 Ir2 47.2(7) . . ? N4A C23 Ir2 158.8(8) . . ? C15 C23 Ir2 74.4(6) . . ? Ir1 C23 Ir2 148.4(7) . . ? C19 C20 N4B 122.8(12) . 1_565 ? C19 C20 H20 118.6 . . ? N4B C20 H20 118.6 1_565 . ? N4A C24 C19 121.5(11) . 1_545 ? N4A C24 H24 119.3 . . ? C19 C24 H24 119.3 1_545 . ? C22 N2 C21 117.0(8) . . ? C22 N2 Zn1 123.9(5) . . ? C21 N2 Zn1 119.0(6) . . ? C25 C17 C26 115.2(8) . . ? C25 C17 C9 122.6(7) . . ? C26 C17 C9 122.1(7) . . ? N2 C22 C26 124.8(9) . 1_455 ? N2 C22 H22 117.6 . . ? C26 C22 H22 117.6 1_455 . ? C17 C26 C22 120.5(10) . 1_655 ? C17 C26 H26 119.7 . . ? C22 C26 H26 119.7 1_655 . ? C17 C25 C21 123.8(11) . 1_655 ? C17 C25 H25 118.1 . . ? C21 C25 H25 118.1 1_655 . ? N2 C21 C25 118.3(11) . 1_455 ? N2 C21 H21 120.9 . . ? C25 C21 H21 120.9 1_455 . ? C30 C28 C29 119.3(6) . . ? C30 C28 C3 122.0(5) . . ? C29 C28 C3 118.6(5) . . ? C28 C30 N6A 121.8(7) . 1_556 ? C28 C30 H30 119.1 . . ? N6A C30 H30 119.1 1_556 . ? N6B C29 C28 118.8(7) 1_556 . ? N6B C29 H29 120.6 1_556 . ? C28 C29 H29 120.6 . . ? N6A C27 N6B 119.8(7) . . ? N6A C27 C16 119.6(7) . . ? N6B C27 C16 120.6(7) . . ? N4B Ir2 C40 91.2(6) . . ? N4B Ir2 C23 29.6(4) . . ? C40 Ir2 C23 62.4(4) . . ? N4B Ir2 C15 62.0(5) . . ? C40 Ir2 C15 29.6(3) . . ? C23 Ir2 C15 32.9(3) . . ? N4A Ir1 C41 97.0(12) . . ? N4A Ir1 C23 33.8(6) . . ? C41 Ir1 C23 66.8(8) . . ? N4A Ir1 C15 66.7(8) . . ? C41 Ir1 C15 32.5(6) . . ? C23 Ir1 C15 34.5(5) . . ? O4 Zn1 O1 88.68(19) . . ? O4 Zn1 O5 162.3(2) . . ? O1 Zn1 O5 87.34(18) . . ? O4 Zn1 O7 88.42(18) . . ? O1 Zn1 O7 158.84(19) . . ? O5 Zn1 O7 89.09(17) . . ? O4 Zn1 N2 100.06(19) . . ? O1 Zn1 N2 100.11(18) . . ? O5 Zn1 N2 97.66(18) . . ? O7 Zn1 N2 101.04(17) . . ? O4 Zn1 Zn2 83.29(14) . . ? O1 Zn1 Zn2 75.26(13) . . ? O5 Zn1 Zn2 78.98(13) . . ? O7 Zn1 Zn2 83.59(12) . . ? N2 Zn1 Zn2 174.31(13) . . ? O8 Zn2 O6 89.02(18) . . ? O8 Zn2 O2 160.26(19) . . ? O6 Zn2 O2 86.04(17) . . ? O8 Zn2 O3 89.22(18) . . ? O6 Zn2 O3 158.4(2) . . ? O2 Zn2 O3 88.41(18) . . ? O8 Zn2 N1 98.04(18) . . ? O6 Zn2 N1 104.10(18) . . ? O2 Zn2 N1 101.70(18) . . ? O3 Zn2 N1 97.43(19) . . ? O8 Zn2 Zn1 75.94(13) . . ? O6 Zn2 Zn1 81.65(13) . . ? O2 Zn2 Zn1 84.43(13) . . ? O3 Zn2 Zn1 77.07(14) . . ? N1 Zn2 Zn1 171.76(13) . . ? C24 N4A C23 121.4(11) . . ? C24 N4A Ir1 133.5(12) . . ? C23 N4A Ir1 94.2(10) . . ? C30 N6A C27 118.7(7) 1_554 . ? C23 N4B C20 121.9(12) . 1_545 ? C23 N4B Ir2 103.2(9) . . ? C20 N4B Ir2 133.2(10) 1_545 . ? C29 N6B C27 121.5(7) 1_554 . ? C14 C42 C16 124.6(9) . . ? C14 C42 H42 117.7 . . ? C16 C42 H42 117.7 . . ? C16 C43 C13 120.1(9) . . ? C16 C43 H43 119.9 . . ? C13 C43 H43 119.9 . . ? C15 C40 C11 121.3(9) . . ? C15 C40 Ir2 102.7(7) . . ? C11 C40 Ir2 136.0(8) . . ? C15 C41 C12 119.6(12) . . ? C15 C41 Ir1 97.5(11) . . ? C12 C41 Ir1 142.0(12) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 58.91 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 1.500 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.131 data_DMOF-1-dcppy(Rh) _database_code_depnum_ccdc_archive 'CCDC 875226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DMOF-1-dcppy(Rh) _chemical_melting_point ? _chemical_formula_moiety 'C26 H8 N10 O8 Rh Zn2' _chemical_formula_sum 'C26 H8 N10 O8 Rh Zn2' _chemical_formula_weight 822.07 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4/ m m m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' 'y, -x, z' 'x, -y, -z' '-x, y, -z' '-x, -y, z' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'y, -x, -z' '-y, x, -z' '-x, y, z' 'x, -y, z' 'x, y, -z' '-y, -x, z' 'y, x, z' _cell_length_a 15.093(6) _cell_length_b 15.093(6) _cell_length_c 9.620(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2191.5(15) _cell_formula_units_Z 1 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 2072 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 23.21 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.60 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 403 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7597 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.40 _reflns_number_total 1221 _reflns_number_gt 984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to the fragility of the crystal, the crystal was collected at 250 K using Mo X-ray source.The Rh atom was found disordered over two position by symmetry and each atom has an occupancy of ~6%. The carbon atoms of the dabco ligand are severely disorders. We strived our best to resolve the disorders and each carbon atom was found to have ~18.75% occupancy. In addition, the nitrogen atom of the phenylpyridine moiety was found to be disordered over 4 position and each has an occupancy of 50%. We tried to refined the nitrogen atom to have an occupancy of 25%, but the checkCif gave us errors on incorrected atom assigment. Due to the low occupancy and disorder of the Rh atom, we were unable to locate other ligands that coordinate to the Rh. In addition, since the Rh is disorder in the structure, it is inaccurate to comapre the occupancy with the ICP-MS analysis. SQUEEZE protocol found ~262 electrons that can be accounted to ~6 dichloromethane. 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^)+(0.1967P)^2^+0.0000P] 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 'not measured' _refine_ls_number_reflns 1221 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2620 _refine_ls_wR_factor_gt 0.2529 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.001 -0.001 -0.026 1491 262 ' ' _platon_squeeze_details ; ; 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 N1 N 0.5000 0.5000 0.1319(9) 0.0346(19) Uani 1 8 d S . . O1 O 0.5000 0.3681(3) 0.3863(5) 0.0736(16) Uani 1 2 d S . . C1 C 0.5000 0.3326(6) 0.5000 0.058(2) Uani 1 4 d S . . C2 C 0.5000 0.2318(7) 0.5000 0.100(5) Uani 1 4 d S . . C4 C 0.5000 0.0491(7) 0.5000 0.107(5) Uani 1 4 d S . . N2 N 0.5000 0.0932(6) 0.3790(9) 0.175(6) Uani 1 2 d S . . C3 C 0.5000 0.1846(6) 0.3814(10) 0.170(8) Uani 1 2 d S . . H3 H 0.5000 0.2150 0.2972 0.204 Uiso 1 2 calc SR . . Rh1 Rh 0.5000 0.0000 0.2374(8) 0.357(11) Uani 0.24 4 d SP . . C5 C 0.5000 0.4113(11) 0.0817(19) 0.082(9) Uani 0.38 2 d SP . . C6 C 0.4377(12) 0.4377(12) 0.069(3) 0.083(7) Uani 0.38 2 d SP . . Zn1 Zn 0.5000 0.5000 0.34791(12) 0.0371(6) Uani 1 8 d S . . 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 N1 0.035(3) 0.035(3) 0.033(5) 0.000 0.000 0.000 O1 0.138(5) 0.042(2) 0.041(3) 0.002(2) 0.000 0.000 C1 0.095(7) 0.038(4) 0.041(5) 0.000 0.000 0.000 C2 0.215(16) 0.040(5) 0.045(6) 0.000 0.000 0.000 C4 0.202(16) 0.045(6) 0.073(8) 0.000 0.000 0.000 N2 0.40(2) 0.054(4) 0.069(5) -0.009(4) 0.000 0.000 C3 0.41(3) 0.050(5) 0.047(5) -0.005(4) 0.000 0.000 Rh1 0.88(4) 0.104(6) 0.084(5) 0.000 0.000 0.000 C5 0.19(3) 0.027(8) 0.029(10) -0.009(7) 0.000 0.000 C6 0.085(10) 0.085(10) 0.077(15) -0.020(8) -0.020(8) -0.017(13) Zn1 0.0436(7) 0.0436(7) 0.0240(7) 0.000 0.000 0.000 _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 N1 C5 1.423(17) . ? N1 C5 1.423(17) 2_655 ? N1 C5 1.423(17) 13_565 ? N1 C5 1.423(17) 3_565 ? N1 C6 1.46(2) 6_665 ? N1 C6 1.46(2) 2_655 ? N1 C6 1.46(2) 3_565 ? N1 C6 1.46(2) . ? N1 Zn1 2.078(9) . ? O1 C1 1.219(6) . ? O1 Zn1 2.024(5) . ? C1 O1 1.219(6) 5_656 ? C1 C2 1.520(12) . ? C2 C3 1.345(10) . ? C2 C3 1.345(10) 5_656 ? C4 N2 1.341(10) 5_656 ? C4 N2 1.341(10) . ? C4 C4 1.48(2) 9_656 ? N2 C3 1.380(12) . ? N2 Rh1 1.958(11) . ? C3 H3 0.9300 . ? Rh1 N2 1.958(11) 13 ? C5 C6 1.028(9) 2_655 ? C5 C6 1.028(9) . ? C5 C5 1.57(4) 5_655 ? C5 C6 1.78(2) 11_655 ? C5 C6 1.78(2) 14 ? C5 C5 1.89(2) 2_655 ? C5 C5 1.89(2) 3_565 ? C6 C5 1.028(9) 3_565 ? C6 C6 1.34(5) 14 ? C6 C5 1.78(2) 5_655 ? C6 C5 1.78(2) 10_565 ? C6 C6 1.88(4) 2_655 ? C6 C6 1.88(4) 3_565 ? Zn1 O1 2.024(5) 2_655 ? Zn1 O1 2.024(5) 13_565 ? Zn1 O1 2.024(5) 3_565 ? Zn1 Zn1 2.926(3) 9_666 ? 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 C5 N1 C5 83.4(5) . 2_655 ? C5 N1 C5 140.3(16) . 13_565 ? C5 N1 C5 83.4(5) 2_655 13_565 ? C5 N1 C5 83.4(5) . 3_565 ? C5 N1 C5 140.3(16) 2_655 3_565 ? C5 N1 C5 83.4(5) 13_565 3_565 ? C5 N1 C6 117.8(9) . 6_665 ? C5 N1 C6 41.8(2) 2_655 6_665 ? C5 N1 C6 41.8(2) 13_565 6_665 ? C5 N1 C6 117.8(9) 3_565 6_665 ? C5 N1 C6 41.8(2) . 2_655 ? C5 N1 C6 41.8(2) 2_655 2_655 ? C5 N1 C6 117.8(9) 13_565 2_655 ? C5 N1 C6 117.8(9) 3_565 2_655 ? C6 N1 C6 80.2(9) 6_665 2_655 ? C5 N1 C6 117.8(9) . 3_565 ? C5 N1 C6 117.8(9) 2_655 3_565 ? C5 N1 C6 41.8(2) 13_565 3_565 ? C5 N1 C6 41.8(2) 3_565 3_565 ? C6 N1 C6 80.2(9) 6_665 3_565 ? C6 N1 C6 131(2) 2_655 3_565 ? C5 N1 C6 41.8(2) . . ? C5 N1 C6 117.8(9) 2_655 . ? C5 N1 C6 117.8(9) 13_565 . ? C5 N1 C6 41.8(2) 3_565 . ? C6 N1 C6 131(2) 6_665 . ? C6 N1 C6 80.2(9) 2_655 . ? C6 N1 C6 80.2(9) 3_565 . ? C5 N1 Zn1 109.8(8) . . ? C5 N1 Zn1 109.8(8) 2_655 . ? C5 N1 Zn1 109.8(8) 13_565 . ? C5 N1 Zn1 109.8(8) 3_565 . ? C6 N1 Zn1 114.3(12) 6_665 . ? C6 N1 Zn1 114.3(12) 2_655 . ? C6 N1 Zn1 114.3(12) 3_565 . ? C6 N1 Zn1 114.3(12) . . ? C1 O1 Zn1 126.6(5) . . ? O1 C1 O1 127.7(8) 5_656 . ? O1 C1 C2 116.1(4) 5_656 . ? O1 C1 C2 116.1(4) . . ? C3 C2 C3 116.1(11) . 5_656 ? C3 C2 C1 122.0(5) . . ? C3 C2 C1 122.0(5) 5_656 . ? N2 C4 N2 120.4(11) 5_656 . ? N2 C4 C4 119.8(6) 5_656 9_656 ? N2 C4 C4 119.8(6) . 9_656 ? C4 N2 C3 118.9(9) . . ? C4 N2 Rh1 104.3(7) . . ? C3 N2 Rh1 136.9(8) . . ? C2 C3 N2 122.9(9) . . ? C2 C3 H3 118.5 . . ? N2 C3 H3 118.5 . . ? N2 Rh1 N2 91.9(7) 13 . ? C6 C5 C6 132(4) 2_655 . ? C6 C5 N1 71.0(17) 2_655 . ? C6 C5 N1 71.0(17) . . ? C6 C5 C5 83(2) 2_655 5_655 ? C6 C5 C5 83(2) . 5_655 ? N1 C5 C5 109.8(8) . 5_655 ? C6 C5 C6 48(2) 2_655 11_655 ? C6 C5 C6 108(3) . 11_655 ? N1 C5 C6 93.8(12) . 11_655 ? C5 C5 C6 35.1(5) 5_655 11_655 ? C6 C5 C6 108(3) 2_655 14 ? C6 C5 C6 48(2) . 14 ? N1 C5 C6 93.8(12) . 14 ? C5 C5 C6 35.1(5) 5_655 14 ? C6 C5 C6 63.9(13) 11_655 14 ? C6 C5 C5 22.9(17) 2_655 2_655 ? C6 C5 C5 111.9(18) . 2_655 ? N1 C5 C5 48.3(3) . 2_655 ? C5 C5 C5 90.001(3) 5_655 2_655 ? C6 C5 C5 57.8(6) 11_655 2_655 ? C6 C5 C5 102.4(10) 14 2_655 ? C6 C5 C5 111.9(18) 2_655 3_565 ? C6 C5 C5 22.9(17) . 3_565 ? N1 C5 C5 48.3(3) . 3_565 ? C5 C5 C5 90.001(1) 5_655 3_565 ? C6 C5 C5 102.4(10) 11_655 3_565 ? C6 C5 C5 57.8(6) 14 3_565 ? C5 C5 C5 90.001(1) 2_655 3_565 ? C5 C6 C5 134(3) . 3_565 ? C5 C6 C6 97(2) . 14 ? C5 C6 C6 97(2) 3_565 14 ? C5 C6 N1 67.2(17) . . ? C5 C6 N1 67.2(17) 3_565 . ? C6 C6 N1 114.3(12) 14 . ? C5 C6 C5 62(2) . 5_655 ? C5 C6 C5 120(3) 3_565 5_655 ? C6 C6 C5 35.1(5) 14 5_655 ? N1 C6 C5 98.1(15) . 5_655 ? C5 C6 C5 120(3) . 10_565 ? C5 C6 C5 62(2) 3_565 10_565 ? C6 C6 C5 35.1(5) 14 10_565 ? N1 C6 C5 98.1(15) . 10_565 ? C5 C6 C5 64.4(12) 5_655 10_565 ? C5 C6 C6 23.8(19) . 2_655 ? C5 C6 C6 112.8(18) 3_565 2_655 ? C6 C6 C6 90.000(8) 14 2_655 ? N1 C6 C6 49.9(5) . 2_655 ? C5 C6 C6 58.1(7) 5_655 2_655 ? C5 C6 C6 103.0(10) 10_565 2_655 ? C5 C6 C6 112.8(18) . 3_565 ? C5 C6 C6 23.8(19) 3_565 3_565 ? C6 C6 C6 90.000(1) 14 3_565 ? N1 C6 C6 49.9(5) . 3_565 ? C5 C6 C6 103.0(10) 5_655 3_565 ? C5 C6 C6 58.1(7) 10_565 3_565 ? C6 C6 C6 90.000(3) 2_655 3_565 ? O1 Zn1 O1 88.09(5) . 2_655 ? O1 Zn1 O1 159.0(3) . 13_565 ? O1 Zn1 O1 88.10(5) 2_655 13_565 ? O1 Zn1 O1 88.09(5) . 3_565 ? O1 Zn1 O1 159.0(3) 2_655 3_565 ? O1 Zn1 O1 88.09(5) 13_565 3_565 ? O1 Zn1 N1 100.51(15) . . ? O1 Zn1 N1 100.51(15) 2_655 . ? O1 Zn1 N1 100.51(15) 13_565 . ? O1 Zn1 N1 100.51(15) 3_565 . ? O1 Zn1 Zn1 79.49(15) . 9_666 ? O1 Zn1 Zn1 79.49(15) 2_655 9_666 ? O1 Zn1 Zn1 79.49(15) 13_565 9_666 ? O1 Zn1 Zn1 79.49(15) 3_565 9_666 ? N1 Zn1 Zn1 180.0 . 9_666 ? 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 Zn1 O1 C1 O1 0.000(1) . . . 5_656 ? Zn1 O1 C1 C2 180.000(1) . . . . ? O1 C1 C2 C3 180.000(2) 5_656 . . . ? O1 C1 C2 C3 0.000(2) . . . . ? O1 C1 C2 C3 0.000(2) 5_656 . . 5_656 ? O1 C1 C2 C3 180.000(2) . . . 5_656 ? N2 C4 N2 C3 0.000(2) 5_656 . . . ? C4 C4 N2 C3 180.000(2) 9_656 . . . ? N2 C4 N2 Rh1 180.0 5_656 . . . ? C4 C4 N2 Rh1 0.000(1) 9_656 . . . ? C3 C2 C3 N2 0.000(2) 5_656 . . . ? C1 C2 C3 N2 180.000(1) . . . . ? C4 N2 C3 C2 0.000(2) . . . . ? Rh1 N2 C3 C2 180.000(1) . . . . ? C4 N2 Rh1 N2 0.000(1) . . . 13 ? C3 N2 Rh1 N2 180.000(1) . . . 13 ? C5 N1 C5 C6 4(3) 2_655 . . 2_655 ? C5 N1 C5 C6 75(2) 13_565 . . 2_655 ? C5 N1 C5 C6 146.6(18) 3_565 . . 2_655 ? C6 N1 C5 C6 28.6(15) 6_665 . . 2_655 ? C6 N1 C5 C6 122(3) 3_565 . . 2_655 ? C6 N1 C5 C6 151(4) . . . 2_655 ? Zn1 N1 C5 C6 -105(2) . . . 2_655 ? C5 N1 C5 C6 -146.6(18) 2_655 . . . ? C5 N1 C5 C6 -75(2) 13_565 . . . ? C5 N1 C5 C6 -4(3) 3_565 . . . ? C6 N1 C5 C6 -122(3) 6_665 . . . ? C6 N1 C5 C6 -151(4) 2_655 . . . ? C6 N1 C5 C6 -28.6(15) 3_565 . . . ? Zn1 N1 C5 C6 105(2) . . . . ? C5 N1 C5 C5 -71.3(7) 2_655 . . 5_655 ? C5 N1 C5 C5 0.000(5) 13_565 . . 5_655 ? C5 N1 C5 C5 71.3(7) 3_565 . . 5_655 ? C6 N1 C5 C5 -46.8(10) 6_665 . . 5_655 ? C6 N1 C5 C5 -75(2) 2_655 . . 5_655 ? C6 N1 C5 C5 46.8(10) 3_565 . . 5_655 ? C6 N1 C5 C5 75(2) . . . 5_655 ? Zn1 N1 C5 C5 180.000(1) . . . 5_655 ? C5 N1 C5 C6 -39.2(11) 2_655 . . 11_655 ? C5 N1 C5 C6 32.0(7) 13_565 . . 11_655 ? C5 N1 C5 C6 103.3(8) 3_565 . . 11_655 ? C6 N1 C5 C6 -14.8(13) 6_665 . . 11_655 ? C6 N1 C5 C6 -43(2) 2_655 . . 11_655 ? C6 N1 C5 C6 78.8(12) 3_565 . . 11_655 ? C6 N1 C5 C6 107(2) . . . 11_655 ? Zn1 N1 C5 C6 -148.0(7) . . . 11_655 ? C5 N1 C5 C6 -103.3(8) 2_655 . . 14 ? C5 N1 C5 C6 -32.0(7) 13_565 . . 14 ? C5 N1 C5 C6 39.2(11) 3_565 . . 14 ? C6 N1 C5 C6 -78.8(12) 6_665 . . 14 ? C6 N1 C5 C6 -107(2) 2_655 . . 14 ? C6 N1 C5 C6 14.8(13) 3_565 . . 14 ? C6 N1 C5 C6 43(2) . . . 14 ? Zn1 N1 C5 C6 148.0(7) . . . 14 ? C5 N1 C5 C5 71.3(7) 13_565 . . 2_655 ? C5 N1 C5 C5 142.5(13) 3_565 . . 2_655 ? C6 N1 C5 C5 24.5(11) 6_665 . . 2_655 ? C6 N1 C5 C5 -4(3) 2_655 . . 2_655 ? C6 N1 C5 C5 118.0(13) 3_565 . . 2_655 ? C6 N1 C5 C5 146.6(18) . . . 2_655 ? Zn1 N1 C5 C5 -108.7(7) . . . 2_655 ? C5 N1 C5 C5 -142.5(13) 2_655 . . 3_565 ? C5 N1 C5 C5 -71.3(7) 13_565 . . 3_565 ? C6 N1 C5 C5 -118.0(13) 6_665 . . 3_565 ? C6 N1 C5 C5 -146.6(18) 2_655 . . 3_565 ? C6 N1 C5 C5 -24.5(11) 3_565 . . 3_565 ? C6 N1 C5 C5 4(3) . . . 3_565 ? Zn1 N1 C5 C5 108.7(7) . . . 3_565 ? C6 C5 C6 C5 -31(9) 2_655 . . 3_565 ? N1 C5 C6 C5 8(5) . . . 3_565 ? C5 C5 C6 C5 -106(5) 5_655 . . 3_565 ? C6 C5 C6 C5 -80(5) 11_655 . . 3_565 ? C6 C5 C6 C5 -106(5) 14 . . 3_565 ? C5 C5 C6 C5 -18(6) 2_655 . . 3_565 ? C6 C5 C6 C6 75(5) 2_655 . . 14 ? N1 C5 C6 C6 113.6(8) . . . 14 ? C5 C5 C6 C6 -0.001(3) 5_655 . . 14 ? C6 C5 C6 C6 25.7(14) 11_655 . . 14 ? C5 C5 C6 C6 87.3(8) 2_655 . . 14 ? C5 C5 C6 C6 106(5) 3_565 . . 14 ? C6 C5 C6 N1 -39(5) 2_655 . . . ? C5 C5 C6 N1 -113.6(8) 5_655 . . . ? C6 C5 C6 N1 -88.0(12) 11_655 . . . ? C6 C5 C6 N1 -113.6(8) 14 . . . ? C5 C5 C6 N1 -26.3(12) 2_655 . . . ? C5 C5 C6 N1 -8(5) 3_565 . . . ? C6 C5 C6 C5 75(5) 2_655 . . 5_655 ? N1 C5 C6 C5 113.6(8) . . . 5_655 ? C6 C5 C6 C5 25.7(14) 11_655 . . 5_655 ? C6 C5 C6 C5 0.001(3) 14 . . 5_655 ? C5 C5 C6 C5 87.3(8) 2_655 . . 5_655 ? C5 C5 C6 C5 106(5) 3_565 . . 5_655 ? C6 C5 C6 C5 47(6) 2_655 . . 10_565 ? N1 C5 C6 C5 86.1(19) . . . 10_565 ? C5 C5 C6 C5 -27.6(16) 5_655 . . 10_565 ? C6 C5 C6 C5 -2(3) 11_655 . . 10_565 ? C6 C5 C6 C5 -27.6(16) 14 . . 10_565 ? C5 C5 C6 C5 60(2) 2_655 . . 10_565 ? C5 C5 C6 C5 78(5) 3_565 . . 10_565 ? N1 C5 C6 C6 39(5) . . . 2_655 ? C5 C5 C6 C6 -75(5) 5_655 . . 2_655 ? C6 C5 C6 C6 -49(4) 11_655 . . 2_655 ? C6 C5 C6 C6 -75(5) 14 . . 2_655 ? C5 C5 C6 C6 12(4) 2_655 . . 2_655 ? C5 C5 C6 C6 31(9) 3_565 . . 2_655 ? C6 C5 C6 C6 -18(5) 2_655 . . 3_565 ? N1 C5 C6 C6 20.9(9) . . . 3_565 ? C5 C5 C6 C6 -92.8(9) 5_655 . . 3_565 ? C6 C5 C6 C6 -67.1(15) 11_655 . . 3_565 ? C6 C5 C6 C6 -92.8(9) 14 . . 3_565 ? C5 C5 C6 C6 -5.4(17) 2_655 . . 3_565 ? C5 C5 C6 C6 13(4) 3_565 . . 3_565 ? C5 N1 C6 C5 38(2) 2_655 . . . ? C5 N1 C6 C5 136(2) 13_565 . . . ? C5 N1 C6 C5 174(4) 3_565 . . . ? C6 N1 C6 C5 87.0(19) 6_665 . . . ? C6 N1 C6 C5 19(3) 2_655 . . . ? C6 N1 C6 C5 154.6(13) 3_565 . . . ? Zn1 N1 C6 C5 -93.0(19) . . . . ? C5 N1 C6 C5 -174(4) . . . 3_565 ? C5 N1 C6 C5 -136(2) 2_655 . . 3_565 ? C5 N1 C6 C5 -38(2) 13_565 . . 3_565 ? C6 N1 C6 C5 -87.0(19) 6_665 . . 3_565 ? C6 N1 C6 C5 -154.6(13) 2_655 . . 3_565 ? C6 N1 C6 C5 -19(3) 3_565 . . 3_565 ? Zn1 N1 C6 C5 93.0(19) . . . 3_565 ? C5 N1 C6 C6 -87.0(19) . . . 14 ? C5 N1 C6 C6 -48.8(8) 2_655 . . 14 ? C5 N1 C6 C6 48.8(8) 13_565 . . 14 ? C5 N1 C6 C6 87.0(19) 3_565 . . 14 ? C6 N1 C6 C6 0.000(5) 6_665 . . 14 ? C6 N1 C6 C6 -67.6(9) 2_655 . . 14 ? C6 N1 C6 C6 67.6(9) 3_565 . . 14 ? Zn1 N1 C6 C6 180.000(2) . . . 14 ? C5 N1 C6 C5 -54.4(16) . . . 5_655 ? C5 N1 C6 C5 -16.2(13) 2_655 . . 5_655 ? C5 N1 C6 C5 81.3(8) 13_565 . . 5_655 ? C5 N1 C6 C5 120(2) 3_565 . . 5_655 ? C6 N1 C6 C5 32.5(7) 6_665 . . 5_655 ? C6 N1 C6 C5 -35.1(16) 2_655 . . 5_655 ? C6 N1 C6 C5 100.2(7) 3_565 . . 5_655 ? Zn1 N1 C6 C5 -147.5(7) . . . 5_655 ? C5 N1 C6 C5 -120(2) . . . 10_565 ? C5 N1 C6 C5 -81.3(8) 2_655 . . 10_565 ? C5 N1 C6 C5 16.2(13) 13_565 . . 10_565 ? C5 N1 C6 C5 54.4(16) 3_565 . . 10_565 ? C6 N1 C6 C5 -32.5(7) 6_665 . . 10_565 ? C6 N1 C6 C5 -100.2(7) 2_655 . . 10_565 ? C6 N1 C6 C5 35.1(16) 3_565 . . 10_565 ? Zn1 N1 C6 C5 147.5(7) . . . 10_565 ? C5 N1 C6 C6 -19(3) . . . 2_655 ? C5 N1 C6 C6 18.9(8) 2_655 . . 2_655 ? C5 N1 C6 C6 116.4(15) 13_565 . . 2_655 ? C5 N1 C6 C6 154.6(13) 3_565 . . 2_655 ? C6 N1 C6 C6 67.6(9) 6_665 . . 2_655 ? C6 N1 C6 C6 135.3(19) 3_565 . . 2_655 ? Zn1 N1 C6 C6 -112.4(9) . . . 2_655 ? C5 N1 C6 C6 -154.6(13) . . . 3_565 ? C5 N1 C6 C6 -116.4(15) 2_655 . . 3_565 ? C5 N1 C6 C6 -18.9(8) 13_565 . . 3_565 ? C5 N1 C6 C6 19(3) 3_565 . . 3_565 ? C6 N1 C6 C6 -67.6(9) 6_665 . . 3_565 ? C6 N1 C6 C6 -135.3(19) 2_655 . . 3_565 ? Zn1 N1 C6 C6 112.4(9) . . . 3_565 ? C1 O1 Zn1 O1 79.67(14) . . . 2_655 ? C1 O1 Zn1 O1 -0.001(3) . . . 13_565 ? C1 O1 Zn1 O1 -79.67(14) . . . 3_565 ? C1 O1 Zn1 N1 180.000(1) . . . . ? C1 O1 Zn1 Zn1 0.000(1) . . . 9_666 ? C5 N1 Zn1 O1 0.000(1) . . . . ? C5 N1 Zn1 O1 -90.0 2_655 . . . ? C5 N1 Zn1 O1 180.000(1) 13_565 . . . ? C5 N1 Zn1 O1 90.0 3_565 . . . ? C6 N1 Zn1 O1 -135.0 6_665 . . . ? C6 N1 Zn1 O1 -45.0 2_655 . . . ? C6 N1 Zn1 O1 135.000(1) 3_565 . . . ? C6 N1 Zn1 O1 45.0 . . . . ? C5 N1 Zn1 O1 90.0 . . . 2_655 ? C5 N1 Zn1 O1 0.0 2_655 . . 2_655 ? C5 N1 Zn1 O1 -90.000(1) 13_565 . . 2_655 ? C5 N1 Zn1 O1 180.0 3_565 . . 2_655 ? C6 N1 Zn1 O1 -45.0 6_665 . . 2_655 ? C6 N1 Zn1 O1 45.0 2_655 . . 2_655 ? C6 N1 Zn1 O1 -135.000(1) 3_565 . . 2_655 ? C6 N1 Zn1 O1 135.0 . . . 2_655 ? C5 N1 Zn1 O1 180.000(1) . . . 13_565 ? C5 N1 Zn1 O1 90.0 2_655 . . 13_565 ? C5 N1 Zn1 O1 0.000(2) 13_565 . . 13_565 ? C5 N1 Zn1 O1 -90.0 3_565 . . 13_565 ? C6 N1 Zn1 O1 45.000(1) 6_665 . . 13_565 ? C6 N1 Zn1 O1 135.000(1) 2_655 . . 13_565 ? C6 N1 Zn1 O1 -45.000(1) 3_565 . . 13_565 ? C6 N1 Zn1 O1 -135.0 . . . 13_565 ? C5 N1 Zn1 O1 -90.000(1) . . . 3_565 ? C5 N1 Zn1 O1 180.0 2_655 . . 3_565 ? C5 N1 Zn1 O1 90.000(1) 13_565 . . 3_565 ? C5 N1 Zn1 O1 0.0 3_565 . . 3_565 ? C6 N1 Zn1 O1 135.0 6_665 . . 3_565 ? C6 N1 Zn1 O1 -135.0 2_655 . . 3_565 ? C6 N1 Zn1 O1 45.0 3_565 . . 3_565 ? C6 N1 Zn1 O1 -45.0 . . . 3_565 ? C5 N1 Zn1 Zn1 -88(100) . . . 9_666 ? C5 N1 Zn1 Zn1 -178(100) 2_655 . . 9_666 ? C5 N1 Zn1 Zn1 92(61) 13_565 . . 9_666 ? C5 N1 Zn1 Zn1 2(61) 3_565 . . 9_666 ? C6 N1 Zn1 Zn1 137(61) 6_665 . . 9_666 ? C6 N1 Zn1 Zn1 -133(100) 2_655 . . 9_666 ? C6 N1 Zn1 Zn1 47(61) 3_565 . . 9_666 ? C6 N1 Zn1 Zn1 -43(61) . . . 9_666 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.218 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.133 data_BMOF-1-dcppy(Rh) _database_code_depnum_ccdc_archive 'CCDC 887472' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common BMOF-1-dcppy(Rh) _chemical_melting_point ? _chemical_formula_moiety 'C36 H21 N4 O8 Rh0.15 Zn2' _chemical_formula_sum 'C36 H21 N4 O8 Rh0.15 Zn2' _chemical_formula_weight 768.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0869(13) _cell_length_b 15.1333(17) _cell_length_c 15.1402(15) _cell_angle_alpha 86.517(7) _cell_angle_beta 87.286(5) _cell_angle_gamma 86.896(5) _cell_volume 3213.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 8141 _cell_measurement_theta_min 4.20 _cell_measurement_theta_max 70.57 _exptl_crystal_description needle _exptl_crystal_colour 'clear yellow' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10145 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 70.57 _reflns_number_total 10145 _reflns_number_gt 8182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to the weak diffraction and the fragility of the crystal, the data was collected at 230 K using Cu source. The Rh atom was refined to have ~7.5% occupancy. The structure was rather ordered than the BMOF-1-dcppyIr structure. In addition, due to the low occupancy of Rh, we were unable to locate any other ligands bound to Rh. Due to the weak diffraction, the data completeness can only go upto 82.30%. We have tried several crystals but the completeness and resolution cannot be improved. SQUEEZE protocol found ~197 e that can be accounted for ~5.5 THF molecules 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^)+(0.1076P)^2^+0.0000P] 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 'not measured' _refine_ls_number_reflns 10145 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 0.000 0.027 1798 197 ' ' _platon_squeeze_details ; ; 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 N1 N 0.95202(14) 0.38968(15) 0.15803(15) 0.0375(5) Uani 1 1 d . . . N2 N 1.45067(15) 0.38891(16) 0.15373(16) 0.0408(5) Uani 1 1 d . . . O1 O 1.12686(13) 0.39408(15) 0.02911(12) 0.0488(5) Uani 1 1 d . . . O3 O 1.27017(14) 0.38379(16) 0.28459(12) 0.0534(5) Uani 1 1 d . . . O2 O 1.28497(13) 0.39170(15) 0.02073(12) 0.0486(5) Uani 1 1 d . . . O7 O 1.27715(14) 0.52093(12) 0.15040(16) 0.0529(5) Uani 1 1 d . . . O4 O 1.11209(14) 0.40123(17) 0.29279(13) 0.0566(6) Uani 1 1 d . . . O8 O 1.11881(14) 0.52938(12) 0.15223(16) 0.0526(5) Uani 1 1 d . . . O6 O 1.29095(15) 0.25483(13) 0.15665(17) 0.0576(5) Uani 1 1 d . . . C3 C 0.75430(18) 0.3873(2) 0.1570(2) 0.0444(6) Uani 1 1 d . . . O5 O 1.13300(15) 0.26441(13) 0.17418(19) 0.0618(6) Uani 1 1 d . . . C2 C 0.80903(18) 0.3922(2) 0.0790(2) 0.0484(7) Uani 1 1 d . . . H2 H 0.7804 0.3944 0.0247 0.058 Uiso 1 1 calc R . . C8 C 1.1990(2) 0.66069(18) 0.1620(2) 0.0515(7) Uani 1 1 d . . . C5 C 0.89890(19) 0.3833(2) 0.23468(19) 0.0531(8) Uani 1 1 d . . . H5 H 0.9292 0.3799 0.2881 0.064 Uiso 1 1 calc R . . C7 C 1.20430(19) 0.38839(19) -0.11145(18) 0.0428(6) Uani 1 1 d . . . C9 C 1.1934(2) 0.3911(2) 0.42513(18) 0.0482(7) Uani 1 1 d . . . C4 C 0.80084(19) 0.3817(3) 0.2360(2) 0.0573(8) Uani 1 1 d . . . H4 H 0.7662 0.3769 0.2897 0.069 Uiso 1 1 calc R . . C1 C 0.90686(17) 0.3938(2) 0.08240(19) 0.0440(6) Uani 1 1 d . . . H1 H 0.9429 0.3980 0.0294 0.053 Uiso 1 1 calc R . . C6 C 1.20573(18) 0.39090(17) -0.01316(17) 0.0380(5) Uani 1 1 d . . . C10 C 1.19798(19) 0.56296(17) 0.15429(18) 0.0403(6) Uani 1 1 d . . . N4 N 1.1161(2) 0.3948(2) -0.24409(19) 0.0704(8) Uani 1 1 d . . . C21 C 1.2853(2) 0.3793(3) -0.25319(19) 0.0568(8) Uani 1 1 d . . . H21 H 1.3419 0.3738 -0.2870 0.068 Uiso 1 1 calc R . . C26 C 1.2113(2) 0.22184(18) 0.1677(2) 0.0483(7) Uani 1 1 d . . . C22 C 1.2872(2) 0.3797(2) -0.1637(2) 0.0551(8) Uani 1 1 d . . . H22 H 1.3455 0.3739 -0.1369 0.066 Uiso 1 1 calc R . . C20 C 1.1183(2) 0.3958(2) -0.15432(19) 0.0505(7) Uani 1 1 d . . . H20 H 1.0614 0.4016 -0.1209 0.061 Uiso 1 1 calc R . . C14 C 1.19214(19) 0.39210(18) 0.32644(17) 0.0413(6) Uani 1 1 d . . . C25 C 0.64856(17) 0.3881(2) 0.15601(19) 0.0439(6) Uani 1 1 d . . . C23 C 1.1993(2) 0.3872(2) -0.29440(19) 0.0520(7) Uani 1 1 d . . . C19 C 1.1972(2) 0.3885(3) 0.6082(2) 0.0590(8) Uani 1 1 d . . . C16 C 1.2743(3) 0.3697(4) 0.4686(2) 0.0845(14) Uani 1 1 d . . . H16 H 1.3298 0.3544 0.4361 0.101 Uiso 1 1 calc R . . C27 C 1.2092(2) 0.1229(2) 0.1734(3) 0.0616(9) Uani 1 1 d . . . C17 C 1.2764(2) 0.3699(4) 0.5584(2) 0.0825(14) Uani 1 1 d . . . H17 H 1.3336 0.3569 0.5857 0.099 Uiso 1 1 calc R . . C18 C 1.1166(3) 0.4085(4) 0.5664(2) 0.0858(15) Uani 1 1 d . . . H18 H 1.0610 0.4219 0.5996 0.103 Uiso 1 1 calc R . . C15 C 1.1138(3) 0.4097(4) 0.4764(2) 0.0860(14) Uani 1 1 d . . . H15 H 1.0564 0.4235 0.4497 0.103 Uiso 1 1 calc R . . C12 C 1.2811(3) 0.7044(2) 0.1567(4) 0.0812(13) Uani 1 1 d . . . H12 H 1.3384 0.6718 0.1488 0.097 Uiso 1 1 calc R . . N3 N 1.2859(3) -0.0206(2) 0.1633(4) 0.1030(15) Uani 1 1 d . . . C28 C 1.2877(3) 0.0693(2) 0.1611(4) 0.0844(14) Uani 1 1 d . . . H28 H 1.3459 0.0950 0.1506 0.101 Uiso 1 1 calc R . . C11 C 1.1179(3) 0.7125(3) 0.1714(5) 0.105(2) Uani 1 1 d . . . H11 H 1.0596 0.6863 0.1728 0.126 Uiso 1 1 calc R . . C13 C 1.2833(3) 0.7937(2) 0.1624(4) 0.0849(14) Uani 1 1 d . . . C34 C 1.2019(3) 0.8427(2) 0.1750(4) 0.0786(12) Uani 1 1 d . . . C32 C 1.2042(3) -0.0597(2) 0.1795(4) 0.0807(13) Uani 1 1 d . . . C33 C 1.1190(3) 0.8014(3) 0.1789(6) 0.123(3) Uani 1 1 d . . . H33 H 1.0619 0.8343 0.1867 0.148 Uiso 1 1 calc R . . C30 C 1.1255(3) 0.0824(3) 0.1931(6) 0.136(3) Uani 1 1 d . . . H30 H 1.0699 0.1165 0.2046 0.163 Uiso 1 1 calc R . . C31 C 1.1236(4) -0.0083(3) 0.1959(7) 0.150(3) Uani 1 1 d . . . H31 H 1.0664 -0.0352 0.2093 0.180 Uiso 1 1 calc R . . Rh1 Rh 1.3779(3) -0.1218(3) 0.1564(6) 0.115(2) Uani 0.08 1 d P . . C37 C 1.4975(4) 0.3500(6) 0.2217(4) 0.065(2) Uani 0.590(9) 1 d P . 2 H37 H 1.4627 0.3224 0.2683 0.079 Uiso 0.590(9) 1 calc PR . 2 C38 C 1.5018(4) 0.4262(6) 0.0884(4) 0.065(2) Uani 0.590(9) 1 d P . 2 H38 H 1.4707 0.4534 0.0404 0.078 Uiso 0.590(9) 1 calc PR . 2 C36 C 0.5994(4) 0.4265(6) 0.0881(4) 0.064(2) Uani 0.590(9) 1 d P . 2 H36 H 0.6323 0.4537 0.0401 0.076 Uiso 0.590(9) 1 calc PR . 2 C35 C 0.5954(4) 0.3491(7) 0.2257(4) 0.072(3) Uani 0.590(9) 1 d P . 2 H35 H 0.6253 0.3225 0.2747 0.086 Uiso 0.590(9) 1 calc PR . 2 C37A C 1.4944(5) 0.4176(9) 0.2170(6) 0.058(3) Uani 0.410(9) 1 d P . 1 H37A H 1.4574 0.4404 0.2637 0.069 Uiso 0.410(9) 1 calc PR . 1 C38A C 1.5058(5) 0.3571(9) 0.0859(6) 0.060(3) Uani 0.410(9) 1 d P . 1 H38A H 1.4761 0.3350 0.0390 0.072 Uiso 0.410(9) 1 calc PR . 1 C36A C 0.6042(5) 0.3558(8) 0.0830(6) 0.061(3) Uani 0.410(9) 1 d P . 1 H36A H 0.6400 0.3345 0.0350 0.074 Uiso 0.410(9) 1 calc PR . 1 C35A C 0.5924(5) 0.4176(9) 0.2223(7) 0.061(3) Uani 0.410(9) 1 d P . 1 H35A H 0.6188 0.4381 0.2719 0.074 Uiso 0.410(9) 1 calc PR . 1 Zn1 Zn 1.095996(19) 0.39643(2) 0.16095(2) 0.03018(12) Uani 1 1 d . . . Zn2 Zn 1.306032(19) 0.38717(2) 0.15279(2) 0.03029(12) 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 N1 0.0229(9) 0.0474(12) 0.0419(12) 0.0005(10) -0.0013(8) -0.0021(8) N2 0.0255(10) 0.0495(13) 0.0477(12) -0.0034(10) -0.0013(9) -0.0046(9) O1 0.0374(9) 0.0747(14) 0.0348(9) -0.0070(9) 0.0023(8) -0.0061(9) O3 0.0421(10) 0.0855(16) 0.0331(9) -0.0038(10) -0.0007(8) -0.0096(10) O2 0.0396(10) 0.0740(14) 0.0323(9) -0.0060(9) -0.0050(8) 0.0006(9) O7 0.0463(11) 0.0317(9) 0.0809(15) -0.0075(10) -0.0014(10) 0.0004(8) O4 0.0457(11) 0.0917(16) 0.0324(10) -0.0029(10) -0.0078(8) 0.0023(11) O8 0.0472(11) 0.0349(9) 0.0764(14) -0.0045(10) -0.0043(10) -0.0057(8) O6 0.0539(12) 0.0345(10) 0.0843(16) -0.0057(10) 0.0046(11) -0.0059(9) C3 0.0268(12) 0.0572(16) 0.0490(15) 0.0034(13) -0.0049(11) -0.0052(11) O5 0.0506(11) 0.0307(9) 0.1040(19) 0.0008(11) -0.0120(12) 0.0011(8) C2 0.0299(12) 0.0717(19) 0.0442(15) -0.0001(14) -0.0082(11) -0.0054(12) C8 0.0530(16) 0.0318(13) 0.0699(19) -0.0027(13) -0.0065(14) -0.0019(12) C5 0.0310(13) 0.089(2) 0.0391(14) 0.0016(15) -0.0040(11) -0.0043(14) C7 0.0425(13) 0.0530(15) 0.0335(13) -0.0053(12) -0.0013(11) -0.0037(12) C9 0.0478(15) 0.0636(18) 0.0334(13) -0.0037(12) -0.0024(11) -0.0019(13) C4 0.0304(13) 0.098(3) 0.0429(15) 0.0024(16) -0.0010(11) -0.0087(14) C1 0.0260(11) 0.0642(17) 0.0417(14) -0.0022(13) 0.0002(10) -0.0032(11) C6 0.0387(13) 0.0432(13) 0.0324(12) -0.0031(11) -0.0015(10) -0.0023(10) C10 0.0464(14) 0.0334(12) 0.0415(13) -0.0008(11) -0.0019(11) -0.0054(11) N4 0.0652(17) 0.100(2) 0.0481(15) -0.0032(15) -0.0098(13) -0.0190(16) C21 0.0447(15) 0.093(2) 0.0326(14) -0.0117(15) 0.0045(11) 0.0017(15) C26 0.0526(16) 0.0354(14) 0.0570(17) -0.0032(13) -0.0054(13) -0.0015(12) C22 0.0439(15) 0.080(2) 0.0419(15) -0.0078(15) 0.0003(12) 0.0005(15) C20 0.0413(14) 0.074(2) 0.0368(14) -0.0017(13) -0.0028(11) -0.0116(14) C14 0.0456(14) 0.0477(14) 0.0309(12) -0.0019(11) -0.0033(11) -0.0038(11) C25 0.0255(12) 0.0596(17) 0.0468(15) -0.0004(13) -0.0034(10) -0.0047(11) C23 0.0521(16) 0.070(2) 0.0348(14) -0.0067(13) -0.0005(12) -0.0063(14) C19 0.0587(18) 0.083(2) 0.0359(15) -0.0050(15) -0.0011(13) -0.0080(16) C16 0.0519(18) 0.161(4) 0.0396(17) -0.008(2) -0.0060(14) 0.008(2) C27 0.0562(17) 0.0351(15) 0.094(3) -0.0071(16) -0.0097(17) -0.0027(13) C17 0.0470(17) 0.163(4) 0.0371(17) -0.008(2) -0.0076(13) 0.008(2) C18 0.0512(18) 0.167(5) 0.0364(17) -0.014(2) 0.0031(14) 0.021(2) C15 0.0550(19) 0.162(5) 0.0396(18) -0.012(2) -0.0023(15) 0.015(2) C12 0.062(2) 0.0396(17) 0.143(4) -0.015(2) 0.003(2) -0.0066(15) N3 0.079(2) 0.0469(17) 0.181(5) -0.014(2) 0.013(3) 0.0016(16) C28 0.061(2) 0.0412(17) 0.149(4) -0.009(2) 0.014(2) -0.0036(15) C11 0.056(2) 0.0453(19) 0.216(7) -0.025(3) -0.008(3) -0.0048(16) C13 0.071(2) 0.0389(17) 0.148(4) -0.019(2) -0.003(2) -0.0137(16) C34 0.076(2) 0.0374(17) 0.124(4) -0.012(2) -0.015(2) -0.0001(16) C32 0.069(2) 0.0361(16) 0.139(4) -0.007(2) -0.015(2) -0.0066(15) C33 0.055(2) 0.0385(18) 0.277(9) -0.026(3) -0.003(3) 0.0084(16) C30 0.060(2) 0.045(2) 0.300(10) -0.012(3) 0.011(4) -0.0069(18) C31 0.073(3) 0.040(2) 0.338(11) -0.013(4) 0.004(4) -0.0179(19) Rh1 0.073(3) 0.066(2) 0.207(7) -0.020(3) -0.003(3) -0.006(2) C37 0.031(3) 0.098(6) 0.063(4) 0.027(4) -0.001(2) -0.005(3) C38 0.036(3) 0.096(6) 0.058(3) 0.034(4) -0.008(2) -0.016(3) C36 0.031(2) 0.099(6) 0.058(3) 0.029(4) -0.002(2) -0.010(3) C35 0.031(3) 0.123(7) 0.057(3) 0.037(4) -0.004(2) -0.005(3) C37A 0.023(3) 0.107(9) 0.047(4) -0.033(5) 0.001(3) -0.004(4) C38A 0.022(3) 0.108(9) 0.052(4) -0.034(5) 0.003(3) -0.005(4) C36A 0.038(4) 0.093(8) 0.057(5) -0.029(5) -0.003(3) -0.005(4) C35A 0.031(4) 0.098(8) 0.060(5) -0.029(6) -0.007(3) -0.009(4) Zn1 0.02228(18) 0.03465(19) 0.03379(19) -0.00271(13) -0.00190(12) -0.00169(12) Zn2 0.02186(18) 0.0352(2) 0.03406(19) -0.00315(14) -0.00161(12) -0.00234(12) _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 N1 C1 1.333(4) . ? N1 C5 1.352(4) . ? N1 Zn1 2.039(2) . ? N2 C37A 1.273(8) . ? N2 C38 1.313(6) . ? N2 C37 1.338(6) . ? N2 C38A 1.354(8) . ? N2 Zn2 2.040(2) . ? O1 C6 1.256(3) . ? O1 Zn1 2.0248(19) . ? O3 C14 1.247(3) . ? O3 Zn2 2.0334(19) . ? O2 C6 1.251(3) . ? O2 Zn2 2.0317(19) . ? O7 C10 1.254(3) . ? O7 Zn2 2.0414(19) . ? O4 C14 1.257(3) . ? O4 Zn1 2.026(2) . ? O8 C10 1.253(3) . ? O8 Zn1 2.0501(19) . ? O6 C26 1.252(3) . ? O6 Zn2 2.022(2) . ? C3 C2 1.381(4) . ? C3 C4 1.386(4) . ? C3 C25 1.490(4) . ? O5 C26 1.250(3) . ? O5 Zn1 2.0375(19) . ? C2 C1 1.383(4) . ? C2 H2 0.9300 . ? C8 C11 1.358(5) . ? C8 C12 1.359(5) . ? C8 C10 1.492(4) . ? C5 C4 1.382(4) . ? C5 H5 0.9300 . ? C7 C22 1.384(4) . ? C7 C20 1.398(4) . ? C7 C6 1.492(4) . ? C9 C16 1.356(4) . ? C9 C15 1.361(5) . ? C9 C14 1.494(4) . ? C4 H4 0.9300 . ? C1 H1 0.9300 . ? N4 C20 1.362(4) . ? N4 C23 1.371(4) . ? C21 C22 1.357(4) . ? C21 C23 1.384(4) . ? C21 H21 0.9300 . ? C26 C27 1.497(4) . ? C22 H22 0.9300 . ? C20 H20 0.9300 . ? C25 C35A 1.331(9) . ? C25 C36 1.351(6) . ? C25 C35 1.385(6) . ? C25 C36A 1.420(9) . ? C23 C19 1.476(4) 1_554 ? C19 C18 1.337(5) . ? C19 C17 1.343(5) . ? C19 C23 1.476(4) 1_556 ? C16 C17 1.361(5) . ? C16 H16 0.9300 . ? C27 C28 1.347(5) . ? C27 C30 1.370(6) . ? C17 H17 0.9300 . ? C18 C15 1.364(5) . ? C18 H18 0.9300 . ? C15 H15 0.9300 . ? C12 C13 1.362(5) . ? C12 H12 0.9300 . ? N3 C32 1.328(5) . ? N3 C28 1.360(5) . ? N3 Rh1 1.957(6) . ? C28 H28 0.9300 . ? C11 C33 1.356(5) . ? C11 H11 0.9300 . ? C13 C34 1.344(5) . ? C13 Rh1 1.892(6) 1_565 ? C34 C33 1.351(6) . ? C34 C32 1.485(5) 1_565 ? C34 Rh1 2.565(6) 1_565 ? C32 C31 1.362(6) . ? C32 C34 1.485(5) 1_545 ? C32 Rh1 2.589(6) . ? C33 H33 0.9300 . ? C30 C31 1.373(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? Rh1 C13 1.892(6) 1_545 ? Rh1 C34 2.565(6) 1_545 ? C37 C35 1.383(8) 1_655 ? C37 H37 0.9300 . ? C38 C36 1.375(7) 1_655 ? C38 H38 0.9300 . ? C36 C38 1.375(7) 1_455 ? C36 H36 0.9300 . ? C35 C37 1.383(8) 1_455 ? C35 H35 0.9300 . ? C37A C35A 1.387(10) 1_655 ? C37A H37A 0.9300 . ? C38A C36A 1.384(10) 1_655 ? C38A H38A 0.9300 . ? C36A C38A 1.384(10) 1_455 ? C36A H36A 0.9300 . ? C35A C37A 1.387(10) 1_455 ? C35A H35A 0.9300 . ? Zn1 Zn2 2.9516(5) . ? 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 C1 N1 C5 117.8(2) . . ? C1 N1 Zn1 122.24(18) . . ? C5 N1 Zn1 119.90(18) . . ? C37A N2 C38 97.3(5) . . ? C37A N2 C37 45.9(5) . . ? C38 N2 C37 117.2(4) . . ? C37A N2 C38A 116.2(5) . . ? C38 N2 C38A 46.2(5) . . ? C37 N2 C38A 99.2(5) . . ? C37A N2 Zn2 123.2(4) . . ? C38 N2 Zn2 122.4(3) . . ? C37 N2 Zn2 120.4(3) . . ? C38A N2 Zn2 120.5(3) . . ? C6 O1 Zn1 130.41(17) . . ? C14 O3 Zn2 132.33(17) . . ? C6 O2 Zn2 125.17(17) . . ? C10 O7 Zn2 128.94(17) . . ? C14 O4 Zn1 122.37(18) . . ? C10 O8 Zn1 125.75(17) . . ? C26 O6 Zn2 122.17(19) . . ? C2 C3 C4 117.9(2) . . ? C2 C3 C25 120.8(3) . . ? C4 C3 C25 121.3(3) . . ? C26 O5 Zn1 132.39(19) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C11 C8 C12 115.4(3) . . ? C11 C8 C10 122.3(3) . . ? C12 C8 C10 122.3(3) . . ? N1 C5 C4 121.9(3) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C22 C7 C20 117.5(3) . . ? C22 C7 C6 121.8(2) . . ? C20 C7 C6 120.7(2) . . ? C16 C9 C15 116.3(3) . . ? C16 C9 C14 121.5(3) . . ? C15 C9 C14 122.2(3) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? O2 C6 O1 125.0(2) . . ? O2 C6 C7 117.8(2) . . ? O1 C6 C7 117.2(2) . . ? O8 C10 O7 125.2(2) . . ? O8 C10 C8 117.9(2) . . ? O7 C10 C8 116.9(2) . . ? C20 N4 C23 120.1(3) . . ? C22 C21 C23 120.3(3) . . ? C22 C21 H21 119.9 . . ? C23 C21 H21 119.9 . . ? O5 C26 O6 125.7(3) . . ? O5 C26 C27 116.9(3) . . ? O6 C26 C27 117.5(3) . . ? C21 C22 C7 121.4(3) . . ? C21 C22 H22 119.3 . . ? C7 C22 H22 119.3 . . ? N4 C20 C7 121.3(3) . . ? N4 C20 H20 119.4 . . ? C7 C20 H20 119.4 . . ? O3 C14 O4 125.6(2) . . ? O3 C14 C9 117.5(2) . . ? O4 C14 C9 116.9(2) . . ? C35A C25 C36 98.1(6) . . ? C35A C25 C35 44.7(5) . . ? C36 C25 C35 116.5(4) . . ? C35A C25 C36A 117.6(5) . . ? C36 C25 C36A 45.6(5) . . ? C35 C25 C36A 100.3(5) . . ? C35A C25 C3 122.4(4) . . ? C36 C25 C3 122.4(3) . . ? C35 C25 C3 121.1(3) . . ? C36A C25 C3 120.1(4) . . ? N4 C23 C21 119.5(3) . . ? N4 C23 C19 120.1(3) . 1_554 ? C21 C23 C19 120.3(3) . 1_554 ? C18 C19 C17 117.7(3) . . ? C18 C19 C23 121.2(3) . 1_556 ? C17 C19 C23 121.0(3) . 1_556 ? C9 C16 C17 121.9(3) . . ? C9 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C28 C27 C30 116.7(3) . . ? C28 C27 C26 122.9(3) . . ? C30 C27 C26 120.4(3) . . ? C19 C17 C16 121.1(3) . . ? C19 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C15 121.7(3) . . ? C19 C18 H18 119.1 . . ? C15 C18 H18 119.1 . . ? C9 C15 C18 121.2(3) . . ? C9 C15 H15 119.4 . . ? C18 C15 H15 119.4 . . ? C8 C12 C13 123.1(4) . . ? C8 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C32 N3 C28 120.1(3) . . ? C32 N3 Rh1 102.3(3) . . ? C28 N3 Rh1 137.5(3) . . ? C27 C28 N3 123.2(4) . . ? C27 C28 H28 118.4 . . ? N3 C28 H28 118.4 . . ? C33 C11 C8 122.2(4) . . ? C33 C11 H11 118.9 . . ? C8 C11 H11 118.9 . . ? C34 C13 C12 120.0(4) . . ? C34 C13 Rh1 103.6(3) . 1_565 ? C12 C13 Rh1 136.4(4) . 1_565 ? C13 C34 C33 118.2(3) . . ? C13 C34 C32 120.0(4) . 1_565 ? C33 C34 C32 121.7(4) . 1_565 ? C13 C34 Rh1 45.8(2) . 1_565 ? C33 C34 Rh1 163.9(3) . 1_565 ? C32 C34 Rh1 74.2(3) 1_565 1_565 ? N3 C32 C31 118.8(3) . . ? N3 C32 C34 119.5(4) . 1_545 ? C31 C32 C34 121.6(4) . 1_545 ? N3 C32 Rh1 47.6(2) . . ? C31 C32 Rh1 165.7(3) . . ? C34 C32 Rh1 72.4(2) 1_545 . ? C34 C33 C11 121.0(4) . . ? C34 C33 H33 119.5 . . ? C11 C33 H33 119.5 . . ? C27 C30 C31 120.1(4) . . ? C27 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 121.0(4) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C13 Rh1 N3 93.9(3) 1_545 . ? C13 Rh1 C34 30.63(16) 1_545 1_545 ? N3 Rh1 C34 63.39(19) . 1_545 ? C13 Rh1 C32 64.1(2) 1_545 . ? N3 Rh1 C32 30.07(15) . . ? C34 Rh1 C32 33.48(12) 1_545 . ? N2 C37 C35 122.8(5) . 1_655 ? N2 C37 H37 118.6 . . ? C35 C37 H37 118.6 1_655 . ? N2 C38 C36 122.7(5) . 1_655 ? N2 C38 H38 118.6 . . ? C36 C38 H38 118.6 1_655 . ? C25 C36 C38 121.4(5) . 1_455 ? C25 C36 H36 119.3 . . ? C38 C36 H36 119.3 1_455 . ? C37 C35 C25 119.4(5) 1_455 . ? C37 C35 H35 120.3 1_455 . ? C25 C35 H35 120.3 . . ? N2 C37A C35A 125.5(7) . 1_655 ? N2 C37A H37A 117.2 . . ? C35A C37A H37A 117.2 1_655 . ? N2 C38A C36A 123.3(7) . 1_655 ? N2 C38A H38A 118.4 . . ? C36A C38A H38A 118.4 1_655 . ? C38A C36A C25 117.7(7) 1_455 . ? C38A C36A H36A 121.2 1_455 . ? C25 C36A H36A 121.2 . . ? C25 C35A C37A 119.7(7) . 1_455 ? C25 C35A H35A 120.2 . . ? C37A C35A H35A 120.2 1_455 . ? O1 Zn1 O4 161.11(8) . . ? O1 Zn1 O5 89.36(10) . . ? O4 Zn1 O5 87.77(11) . . ? O1 Zn1 N1 98.15(8) . . ? O4 Zn1 N1 100.74(9) . . ? O5 Zn1 N1 99.16(9) . . ? O1 Zn1 O8 88.59(9) . . ? O4 Zn1 O8 86.50(10) . . ? O5 Zn1 O8 156.01(9) . . ? N1 Zn1 O8 104.79(8) . . ? O1 Zn1 Zn2 77.79(5) . . ? O4 Zn1 Zn2 83.42(6) . . ? O5 Zn1 Zn2 75.44(6) . . ? N1 Zn1 Zn2 173.16(7) . . ? O8 Zn1 Zn2 80.77(6) . . ? O6 Zn2 O2 88.56(10) . . ? O6 Zn2 O3 88.36(10) . . ? O2 Zn2 O3 157.26(8) . . ? O6 Zn2 N2 99.80(9) . . ? O2 Zn2 N2 101.42(9) . . ? O3 Zn2 N2 101.31(9) . . ? O6 Zn2 O7 162.52(9) . . ? O2 Zn2 O7 88.75(9) . . ? O3 Zn2 O7 87.47(10) . . ? N2 Zn2 O7 97.66(9) . . ? O6 Zn2 Zn1 83.74(6) . . ? O2 Zn2 Zn1 81.48(5) . . ? O3 Zn2 Zn1 75.80(6) . . ? N2 Zn2 Zn1 175.43(7) . . ? O7 Zn2 Zn1 78.78(6) . . ? 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 C4 C3 C2 C1 -1.7(5) . . . . ? C25 C3 C2 C1 178.2(3) . . . . ? C1 N1 C5 C4 -0.5(5) . . . . ? Zn1 N1 C5 C4 177.7(3) . . . . ? N1 C5 C4 C3 -0.4(6) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C25 C3 C4 C5 -178.4(3) . . . . ? C5 N1 C1 C2 0.2(5) . . . . ? Zn1 N1 C1 C2 -177.9(2) . . . . ? C3 C2 C1 N1 0.9(5) . . . . ? Zn2 O2 C6 O1 5.8(4) . . . . ? Zn2 O2 C6 C7 -175.90(18) . . . . ? Zn1 O1 C6 O2 -2.7(4) . . . . ? Zn1 O1 C6 C7 178.94(18) . . . . ? C22 C7 C6 O2 5.4(4) . . . . ? C20 C7 C6 O2 -173.9(3) . . . . ? C22 C7 C6 O1 -176.2(3) . . . . ? C20 C7 C6 O1 4.5(4) . . . . ? Zn1 O8 C10 O7 9.9(4) . . . . ? Zn1 O8 C10 C8 -170.1(2) . . . . ? Zn2 O7 C10 O8 -7.1(4) . . . . ? Zn2 O7 C10 C8 172.8(2) . . . . ? C11 C8 C10 O8 3.5(6) . . . . ? C12 C8 C10 O8 -173.9(4) . . . . ? C11 C8 C10 O7 -176.5(4) . . . . ? C12 C8 C10 O7 6.1(5) . . . . ? Zn1 O5 C26 O6 5.6(5) . . . . ? Zn1 O5 C26 C27 -174.2(2) . . . . ? Zn2 O6 C26 O5 2.9(5) . . . . ? Zn2 O6 C26 C27 -177.4(2) . . . . ? C23 C21 C22 C7 -0.4(6) . . . . ? C20 C7 C22 C21 0.7(5) . . . . ? C6 C7 C22 C21 -178.6(3) . . . . ? C23 N4 C20 C7 -0.7(5) . . . . ? C22 C7 C20 N4 -0.2(5) . . . . ? C6 C7 C20 N4 179.1(3) . . . . ? Zn2 O3 C14 O4 3.6(5) . . . . ? Zn2 O3 C14 C9 -176.4(2) . . . . ? Zn1 O4 C14 O3 3.9(4) . . . . ? Zn1 O4 C14 C9 -176.1(2) . . . . ? C16 C9 C14 O3 -9.1(5) . . . . ? C15 C9 C14 O3 172.3(4) . . . . ? C16 C9 C14 O4 170.9(4) . . . . ? C15 C9 C14 O4 -7.7(5) . . . . ? C2 C3 C25 C35A -153.2(7) . . . . ? C4 C3 C25 C35A 26.8(8) . . . . ? C2 C3 C25 C36 -26.3(7) . . . . ? C4 C3 C25 C36 153.6(5) . . . . ? C2 C3 C25 C35 153.8(6) . . . . ? C4 C3 C25 C35 -26.3(7) . . . . ? C2 C3 C25 C36A 27.5(7) . . . . ? C4 C3 C25 C36A -152.5(7) . . . . ? C20 N4 C23 C21 1.0(6) . . . . ? C20 N4 C23 C19 -178.4(3) . . . 1_554 ? C22 C21 C23 N4 -0.4(6) . . . . ? C22 C21 C23 C19 178.9(4) . . . 1_554 ? C15 C9 C16 C17 -2.3(7) . . . . ? C14 C9 C16 C17 179.0(4) . . . . ? O5 C26 C27 C28 175.1(4) . . . . ? O6 C26 C27 C28 -4.7(6) . . . . ? O5 C26 C27 C30 -5.9(6) . . . . ? O6 C26 C27 C30 174.3(5) . . . . ? C18 C19 C17 C16 -1.3(8) . . . . ? C23 C19 C17 C16 179.0(5) 1_556 . . . ? C9 C16 C17 C19 2.4(8) . . . . ? C17 C19 C18 C15 0.4(8) . . . . ? C23 C19 C18 C15 -179.9(5) 1_556 . . . ? C16 C9 C15 C18 1.4(7) . . . . ? C14 C9 C15 C18 -180.0(4) . . . . ? C19 C18 C15 C9 -0.5(8) . . . . ? C11 C8 C12 C13 1.5(8) . . . . ? C10 C8 C12 C13 179.1(4) . . . . ? C30 C27 C28 N3 3.2(8) . . . . ? C26 C27 C28 N3 -177.7(5) . . . . ? C32 N3 C28 C27 -1.1(8) . . . . ? Rh1 N3 C28 C27 -175.6(6) . . . . ? C12 C8 C11 C33 -2.8(9) . . . . ? C10 C8 C11 C33 179.7(6) . . . . ? C8 C12 C13 C34 0.9(8) . . . . ? C8 C12 C13 Rh1 -178.6(6) . . . 1_565 ? C12 C13 C34 C33 -2.0(9) . . . . ? Rh1 C13 C34 C33 177.6(6) 1_565 . . . ? C12 C13 C34 C32 -178.9(5) . . . 1_565 ? Rh1 C13 C34 C32 0.8(6) 1_565 . . 1_565 ? C12 C13 C34 Rh1 -179.6(8) . . . 1_565 ? C28 N3 C32 C31 -1.6(9) . . . . ? Rh1 N3 C32 C31 174.6(6) . . . . ? C28 N3 C32 C34 175.4(5) . . . 1_545 ? Rh1 N3 C32 C34 -8.4(6) . . . 1_545 ? C28 N3 C32 Rh1 -176.2(7) . . . . ? C13 C34 C33 C11 0.8(10) . . . . ? C32 C34 C33 C11 177.6(6) 1_565 . . . ? Rh1 C34 C33 C11 7(2) 1_565 . . . ? C8 C11 C33 C34 1.7(11) . . . . ? C28 C27 C30 C31 -2.6(10) . . . . ? C26 C27 C30 C31 178.3(6) . . . . ? N3 C32 C31 C30 2.1(11) . . . . ? C34 C32 C31 C30 -174.9(7) 1_545 . . . ? Rh1 C32 C31 C30 18(3) . . . . ? C27 C30 C31 C32 0.1(12) . . . . ? C32 N3 Rh1 C13 7.3(5) . . . 1_545 ? C28 N3 Rh1 C13 -177.6(6) . . . 1_545 ? C32 N3 Rh1 C34 4.7(3) . . . 1_545 ? C28 N3 Rh1 C34 179.9(7) . . . 1_545 ? C28 N3 Rh1 C32 175.1(9) . . . . ? N3 C32 Rh1 C13 -171.9(6) . . . 1_545 ? C31 C32 Rh1 C13 169(2) . . . 1_545 ? C34 C32 Rh1 C13 0.4(3) 1_545 . . 1_545 ? C31 C32 Rh1 N3 -20(2) . . . . ? C34 C32 Rh1 N3 172.3(6) 1_545 . . . ? N3 C32 Rh1 C34 -172.3(6) . . . 1_545 ? C31 C32 Rh1 C34 168(2) . . . 1_545 ? C37A N2 C37 C35 -71.7(9) . . . 1_655 ? C38 N2 C37 C35 1.0(11) . . . 1_655 ? C38A N2 C37 C35 46.2(10) . . . 1_655 ? Zn2 N2 C37 C35 179.9(7) . . . 1_655 ? C37A N2 C38 C36 43.5(10) . . . 1_655 ? C37 N2 C38 C36 -0.2(11) . . . 1_655 ? C38A N2 C38 C36 -76.1(9) . . . 1_655 ? Zn2 N2 C38 C36 -179.1(6) . . . 1_655 ? C35A C25 C36 C38 -43.3(9) . . . 1_455 ? C35 C25 C36 C38 -0.3(11) . . . 1_455 ? C36A C25 C36 C38 77.7(9) . . . 1_455 ? C3 C25 C36 C38 179.8(6) . . . 1_455 ? C35A C25 C35 C37 74.8(9) . . . 1_455 ? C36 C25 C35 C37 1.1(11) . . . 1_455 ? C36A C25 C35 C37 -44.2(10) . . . 1_455 ? C3 C25 C35 C37 -179.0(7) . . . 1_455 ? C38 N2 C37A C35A -45.2(12) . . . 1_655 ? C37 N2 C37A C35A 75.9(12) . . . 1_655 ? C38A N2 C37A C35A -0.9(15) . . . 1_655 ? Zn2 N2 C37A C35A 177.8(9) . . . 1_655 ? C37A N2 C38A C36A -0.8(14) . . . 1_655 ? C38 N2 C38A C36A 73.2(11) . . . 1_655 ? C37 N2 C38A C36A -45.8(12) . . . 1_655 ? Zn2 N2 C38A C36A -179.5(8) . . . 1_655 ? C35A C25 C36A C38A -0.1(13) . . . 1_455 ? C36 C25 C36A C38A -73.3(10) . . . 1_455 ? C35 C25 C36A C38A 43.8(11) . . . 1_455 ? C3 C25 C36A C38A 179.3(8) . . . 1_455 ? C36 C25 C35A C37A 42.3(11) . . . 1_455 ? C35 C25 C35A C37A -77.5(10) . . . 1_455 ? C36A C25 C35A C37A -1.4(14) . . . 1_455 ? C3 C25 C35A C37A 179.3(8) . . . 1_455 ? C6 O1 Zn1 O4 5.4(5) . . . . ? C6 O1 Zn1 O5 -75.8(3) . . . . ? C6 O1 Zn1 N1 -174.9(2) . . . . ? C6 O1 Zn1 O8 80.3(3) . . . . ? C6 O1 Zn1 Zn2 -0.5(2) . . . . ? C14 O4 Zn1 O1 -11.7(4) . . . . ? C14 O4 Zn1 O5 69.8(2) . . . . ? C14 O4 Zn1 N1 168.7(2) . . . . ? C14 O4 Zn1 O8 -86.9(2) . . . . ? C14 O4 Zn1 Zn2 -5.8(2) . . . . ? C26 O5 Zn1 O1 70.2(3) . . . . ? C26 O5 Zn1 O4 -91.1(3) . . . . ? C26 O5 Zn1 N1 168.3(3) . . . . ? C26 O5 Zn1 O8 -14.9(5) . . . . ? C26 O5 Zn1 Zn2 -7.4(3) . . . . ? C1 N1 Zn1 O1 -6.4(2) . . . . ? C5 N1 Zn1 O1 175.5(2) . . . . ? C1 N1 Zn1 O4 173.5(2) . . . . ? C5 N1 Zn1 O4 -4.6(3) . . . . ? C1 N1 Zn1 O5 -97.1(2) . . . . ? C5 N1 Zn1 O5 84.9(2) . . . . ? C1 N1 Zn1 O8 84.3(2) . . . . ? C5 N1 Zn1 O8 -93.8(2) . . . . ? C1 N1 Zn1 Zn2 -59.5(6) . . . . ? C5 N1 Zn1 Zn2 122.4(5) . . . . ? C10 O8 Zn1 O1 -84.1(2) . . . . ? C10 O8 Zn1 O4 77.6(2) . . . . ? C10 O8 Zn1 O5 1.1(4) . . . . ? C10 O8 Zn1 N1 177.8(2) . . . . ? C10 O8 Zn1 Zn2 -6.2(2) . . . . ? C26 O6 Zn2 O2 -87.4(2) . . . . ? C26 O6 Zn2 O3 70.1(3) . . . . ? C26 O6 Zn2 N2 171.3(2) . . . . ? C26 O6 Zn2 O7 -6.2(5) . . . . ? C26 O6 Zn2 Zn1 -5.8(2) . . . . ? C6 O2 Zn2 O6 79.4(2) . . . . ? C6 O2 Zn2 O3 -2.9(4) . . . . ? C6 O2 Zn2 N2 179.1(2) . . . . ? C6 O2 Zn2 O7 -83.3(2) . . . . ? C6 O2 Zn2 Zn1 -4.5(2) . . . . ? C14 O3 Zn2 O6 -89.9(3) . . . . ? C14 O3 Zn2 O2 -7.6(4) . . . . ? C14 O3 Zn2 N2 170.4(3) . . . . ? C14 O3 Zn2 O7 73.1(3) . . . . ? C14 O3 Zn2 Zn1 -6.0(3) . . . . ? C37A N2 Zn2 O6 -115.0(7) . . . . ? C38 N2 Zn2 O6 118.3(6) . . . . ? C37 N2 Zn2 O6 -60.5(5) . . . . ? C38A N2 Zn2 O6 63.6(7) . . . . ? C37A N2 Zn2 O2 154.5(7) . . . . ? C38 N2 Zn2 O2 27.8(6) . . . . ? C37 N2 Zn2 O2 -151.0(5) . . . . ? C38A N2 Zn2 O2 -26.9(7) . . . . ? C37A N2 Zn2 O3 -24.7(7) . . . . ? C38 N2 Zn2 O3 -151.4(6) . . . . ? C37 N2 Zn2 O3 29.7(5) . . . . ? C38A N2 Zn2 O3 153.9(7) . . . . ? C37A N2 Zn2 O7 64.2(7) . . . . ? C38 N2 Zn2 O7 -62.4(6) . . . . ? C37 N2 Zn2 O7 118.7(5) . . . . ? C38A N2 Zn2 O7 -117.2(7) . . . . ? C37A N2 Zn2 Zn1 25.6(12) . . . . ? C38 N2 Zn2 Zn1 -101.1(10) . . . . ? C37 N2 Zn2 Zn1 80.1(10) . . . . ? C38A N2 Zn2 Zn1 -155.8(9) . . . . ? C10 O7 Zn2 O6 2.0(5) . . . . ? C10 O7 Zn2 O2 83.2(3) . . . . ? C10 O7 Zn2 O3 -74.4(3) . . . . ? C10 O7 Zn2 N2 -175.5(3) . . . . ? C10 O7 Zn2 Zn1 1.6(2) . . . . ? O1 Zn1 Zn2 O6 -87.50(10) . . . . ? O4 Zn1 Zn2 O6 94.44(10) . . . . ? O5 Zn1 Zn2 O6 5.04(11) . . . . ? N1 Zn1 Zn2 O6 -33.4(5) . . . . ? O8 Zn1 Zn2 O6 -178.05(9) . . . . ? O1 Zn1 Zn2 O2 1.98(9) . . . . ? O4 Zn1 Zn2 O2 -176.08(9) . . . . ? O5 Zn1 Zn2 O2 94.52(10) . . . . ? N1 Zn1 Zn2 O2 56.1(5) . . . . ? O8 Zn1 Zn2 O2 -88.58(9) . . . . ? O1 Zn1 Zn2 O3 -177.39(9) . . . . ? O4 Zn1 Zn2 O3 4.55(10) . . . . ? O5 Zn1 Zn2 O3 -84.85(11) . . . . ? N1 Zn1 Zn2 O3 -123.3(5) . . . . ? O8 Zn1 Zn2 O3 92.05(10) . . . . ? O1 Zn1 Zn2 N2 131.5(8) . . . . ? O4 Zn1 Zn2 N2 -46.6(8) . . . . ? O5 Zn1 Zn2 N2 -136.0(8) . . . . ? N1 Zn1 Zn2 N2 -174.4(9) . . . . ? O8 Zn1 Zn2 N2 40.9(8) . . . . ? O1 Zn1 Zn2 O7 92.39(10) . . . . ? O4 Zn1 Zn2 O7 -85.67(10) . . . . ? O5 Zn1 Zn2 O7 -175.07(10) . . . . ? N1 Zn1 Zn2 O7 146.5(5) . . . . ? O8 Zn1 Zn2 O7 1.84(10) . . . . ? _diffrn_measured_fraction_theta_max 0.823 _diffrn_reflns_theta_full 70.57 _diffrn_measured_fraction_theta_full 0.823 _refine_diff_density_max 0.667 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.069 data_DMOF-1-dcppy-x(Ir) _database_code_depnum_ccdc_archive 'CCDC 887681' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DMOF-1-dcppy(Ir) _chemical_melting_point ? _chemical_formula_moiety 'C24 H8 Ir0.29 N6 O8 Zn2' _chemical_formula_sum 'C24 H8 Ir0.29 N6 O8 Zn2' _chemical_formula_weight 694.07 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4/ m m m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' 'y, -x, z' 'x, -y, -z' '-x, y, -z' '-x, -y, z' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'y, -x, -z' '-y, x, -z' '-x, y, z' 'x, -y, z' 'x, y, -z' '-y, -x, z' 'y, x, z' _cell_length_a 15.093(6) _cell_length_b 15.093(6) _cell_length_c 9.620(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2191.5(15) _cell_formula_units_Z 1 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 2072 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 23.21 _exptl_crystal_description 'retangular block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 341.1 _exptl_crystal_F_000' 339.86 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8255 _exptl_absorpt_correction_T_max 0.9069 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 7597 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.40 _reflns_number_total 1221 _reflns_number_gt 981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to the fragility of the crystal, the data was collected at 250K. The structure was refined isotropically due to the weak diffraction and severely disoders of dabco ligand and the nitrogen atom of dcppy ligand. We have strived our best to assign the occupancy and resolved the disordered carbon atoms of dabco ligand (most of this were in alert_C). The nitrogen atom of dcppy ligand was refined as disordered over 4 positions and the occupancy was 25% for each. Since the occupancy of Ir was low ~<10% per dcppy ligand, we were unable to locate any other ligands that bound to Ir. Thus, checkCIF gave us an Alert_A on low/ unusual single bonded metal atoms. In addition, we do not use any restraint on Ir atom to ensure the corrected assigment (the bond distance Ir-C and Ir-N were found to be ~2.04 Angstrom). Also, due to the severe disorder of dabco, alert_A on short N1-N1 distance is also reported by checkCif. The R-factor of the structure is fairly large and it is highly due to the disorder of the dabco ligand in the structure. SQEEZE protocol was applied to the structure and found 217 electrons that can be account for ~5 dichloromethane molecules. 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^)+(0.2000P)^2^+0.0000P] 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 'not measured' _refine_ls_number_reflns 1221 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1677 _refine_ls_R_factor_gt 0.1567 _refine_ls_wR_factor_ref 0.3458 _refine_ls_wR_factor_gt 0.3555 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.001 -0.001 -0.026 1497 217 ' ' _platon_squeeze_details ; ; 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 N1 N 0.5000 0.5000 0.1322(16) 0.036(3) Uiso 1 8 d S . . O1 O 0.5000 0.3666(6) 0.3861(10) 0.069(2) Uiso 1 2 d S . . C1 C 0.5000 0.3304(11) 0.5000 0.057(4) Uiso 1 4 d S . . C2 C 0.5000 0.2328(14) 0.5000 0.076(5) Uiso 1 4 d S . . C4 C 0.5000 0.0489(15) 0.5000 0.083(6) Uiso 1 4 d S . . C3 C 0.5000 0.1795(13) 0.379(2) 0.099(5) Uiso 1 2 d S . . H3 H 0.5000 0.2080 0.2919 0.119 Uiso 1 2 calc SR . . N2 N 0.5000 0.0958(14) 0.381(2) 0.062(5) Uiso 0.50 2 d SP . . Ir1 Ir 0.5000 0.0000 0.232(2) 0.125(6) Uiso 0.07 4 d SP . . C5 C 0.5000 0.409(2) 0.084(4) 0.040(8) Uiso 0.25 2 d SP . . C6 C 0.436(2) 0.436(2) 0.076(5) 0.055(10) Uiso 0.25 2 d SP . . Zn1 Zn 0.5000 0.5000 0.34806(19) 0.0368(10) Uani 1 8 d S . . 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 Zn1 0.0428(11) 0.0428(11) 0.0249(13) 0.000 0.000 0.000 _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 N1 C5 1.45(4) 2_655 ? N1 C5 1.45(4) 3_565 ? N1 C5 1.45(4) . ? N1 C5 1.45(4) 13_565 ? N1 C6 1.48(4) . ? N1 C6 1.48(4) 6_665 ? N1 C6 1.48(4) 2_655 ? N1 C6 1.48(4) 3_565 ? N1 Zn1 2.077(16) . ? O1 C1 1.224(12) . ? O1 Zn1 2.046(9) . ? C1 O1 1.224(12) 5_656 ? C1 C2 1.47(3) . ? C2 C3 1.42(2) . ? C2 C3 1.42(2) 5_656 ? C4 N2 1.34(2) 5_656 ? C4 N2 1.34(2) . ? C4 C4 1.48(4) 9_656 ? C3 N2 1.26(3) . ? C3 H3 0.9400 . ? N2 Ir1 2.04(3) . ? Ir1 N2 2.04(3) 13 ? C5 C6 1.06(2) 2_655 ? C5 C6 1.06(2) . ? C5 C5 1.62(7) 5_655 ? C5 C6 1.86(5) 11_655 ? C5 C6 1.86(5) 14 ? C5 C5 1.95(5) 2_655 ? C5 C5 1.95(5) 3_565 ? C6 C5 1.06(2) 3_565 ? C6 C6 1.46(10) 14 ? C6 C5 1.86(5) 10_565 ? C6 C5 1.86(5) 5_655 ? C6 C6 1.94(6) 2_655 ? C6 C6 1.94(6) 3_565 ? Zn1 O1 2.046(9) 13_565 ? Zn1 O1 2.046(9) 2_655 ? Zn1 O1 2.046(9) 3_565 ? Zn1 Zn1 2.923(4) 9_666 ? 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 C5 N1 C5 143(3) 2_655 3_565 ? C5 N1 C5 84.2(10) 2_655 . ? C5 N1 C5 84.2(10) 3_565 . ? C5 N1 C5 84.2(10) 2_655 13_565 ? C5 N1 C5 84.2(10) 3_565 13_565 ? C5 N1 C5 143(3) . 13_565 ? C5 N1 C6 120.4(17) 2_655 . ? C5 N1 C6 42.2(4) 3_565 . ? C5 N1 C6 42.2(4) . . ? C5 N1 C6 120.4(17) 13_565 . ? C5 N1 C6 42.2(4) 2_655 6_665 ? C5 N1 C6 120.4(17) 3_565 6_665 ? C5 N1 C6 120.4(17) . 6_665 ? C5 N1 C6 42.2(4) 13_565 6_665 ? C6 N1 C6 137(4) . 6_665 ? C5 N1 C6 42.2(4) 2_655 2_655 ? C5 N1 C6 120.4(17) 3_565 2_655 ? C5 N1 C6 42.2(4) . 2_655 ? C5 N1 C6 120.4(17) 13_565 2_655 ? C6 N1 C6 82.2(14) . 2_655 ? C6 N1 C6 82.2(14) 6_665 2_655 ? C5 N1 C6 120.4(17) 2_655 3_565 ? C5 N1 C6 42.2(4) 3_565 3_565 ? C5 N1 C6 120.4(17) . 3_565 ? C5 N1 C6 42.2(4) 13_565 3_565 ? C6 N1 C6 82.2(14) . 3_565 ? C6 N1 C6 82.2(14) 6_665 3_565 ? C6 N1 C6 137(4) 2_655 3_565 ? C5 N1 Zn1 108.5(16) 2_655 . ? C5 N1 Zn1 108.5(16) 3_565 . ? C5 N1 Zn1 108.5(16) . . ? C5 N1 Zn1 108.5(16) 13_565 . ? C6 N1 Zn1 112(2) . . ? C6 N1 Zn1 112(2) 6_665 . ? C6 N1 Zn1 112(2) 2_655 . ? C6 N1 Zn1 112(2) 3_565 . ? C1 O1 Zn1 126.8(10) . . ? O1 C1 O1 126.9(17) . 5_656 ? O1 C1 C2 116.5(8) . . ? O1 C1 C2 116.5(8) 5_656 . ? C3 C2 C3 111(2) . 5_656 ? C3 C2 C1 124.6(11) . . ? C3 C2 C1 124.6(11) 5_656 . ? N2 C4 N2 116(3) 5_656 . ? N2 C4 C4 121.8(13) 5_656 9_656 ? N2 C4 C4 121.8(13) . 9_656 ? N2 C3 C2 124(2) . . ? N2 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 N2 C4 123(2) . . ? C3 N2 Ir1 134.1(19) . . ? C4 N2 Ir1 103.0(14) . . ? N2 Ir1 N2 90.4(15) 13 . ? C6 C5 C6 134(6) 2_655 . ? C6 C5 N1 70(3) 2_655 . ? C6 C5 N1 70(3) . . ? C6 C5 C5 85(3) 2_655 5_655 ? C6 C5 C5 85(3) . 5_655 ? N1 C5 C5 108.5(16) . 5_655 ? C6 C5 C6 51(4) 2_655 11_655 ? C6 C5 C6 109(4) . 11_655 ? N1 C5 C6 93(2) . 11_655 ? C5 C5 C6 34.4(12) 5_655 11_655 ? C6 C5 C6 109(4) 2_655 14 ? C6 C5 C6 51(4) . 14 ? N1 C5 C6 93(2) . 14 ? C5 C5 C6 34.4(12) 5_655 14 ? C6 C5 C6 63(3) 11_655 14 ? C6 C5 C5 23(3) 2_655 2_655 ? C6 C5 C5 112(3) . 2_655 ? N1 C5 C5 47.9(5) . 2_655 ? C5 C5 C5 89.999(4) 5_655 2_655 ? C6 C5 C5 58.5(12) 11_655 2_655 ? C6 C5 C5 102.3(16) 14 2_655 ? C6 C5 C5 112(3) 2_655 3_565 ? C6 C5 C5 23(3) . 3_565 ? N1 C5 C5 47.9(5) . 3_565 ? C5 C5 C5 90.001(1) 5_655 3_565 ? C6 C5 C5 102.3(16) 11_655 3_565 ? C6 C5 C5 58.5(12) 14 3_565 ? C5 C5 C5 89.999(1) 2_655 3_565 ? C5 C6 C5 135(6) 3_565 . ? C5 C6 C6 95(3) 3_565 14 ? C5 C6 C6 95(3) . 14 ? C5 C6 N1 68(3) 3_565 . ? C5 C6 N1 68(3) . . ? C6 C6 N1 111.6(19) 14 . ? C5 C6 C5 60(3) 3_565 10_565 ? C5 C6 C5 118(4) . 10_565 ? C6 C6 C5 34.4(12) 14 10_565 ? N1 C6 C5 96(2) . 10_565 ? C5 C6 C5 118(4) 3_565 5_655 ? C5 C6 C5 60(3) . 5_655 ? C6 C6 C5 34.4(12) 14 5_655 ? N1 C6 C5 96(2) . 5_655 ? C5 C6 C5 63(2) 10_565 5_655 ? C5 C6 C6 113(3) 3_565 2_655 ? C5 C6 C6 23(3) . 2_655 ? C6 C6 C6 90.000(12) 14 2_655 ? N1 C6 C6 48.9(7) . 2_655 ? C5 C6 C6 102.6(16) 10_565 2_655 ? C5 C6 C6 58.6(13) 5_655 2_655 ? C5 C6 C6 23(3) 3_565 3_565 ? C5 C6 C6 113(3) . 3_565 ? C6 C6 C6 90.002(3) 14 3_565 ? N1 C6 C6 48.9(7) . 3_565 ? C5 C6 C6 58.6(13) 10_565 3_565 ? C5 C6 C6 102.6(16) 5_655 3_565 ? C6 C6 C6 90.001(6) 2_655 3_565 ? O1 Zn1 O1 88.16(10) 13_565 2_655 ? O1 Zn1 O1 159.4(6) 13_565 . ? O1 Zn1 O1 88.16(10) 2_655 . ? O1 Zn1 O1 88.17(10) 13_565 3_565 ? O1 Zn1 O1 159.4(6) 2_655 3_565 ? O1 Zn1 O1 88.16(10) . 3_565 ? O1 Zn1 N1 100.3(3) 13_565 . ? O1 Zn1 N1 100.3(3) 2_655 . ? O1 Zn1 N1 100.3(3) . . ? O1 Zn1 N1 100.3(3) 3_565 . ? O1 Zn1 Zn1 79.7(3) 13_565 9_666 ? O1 Zn1 Zn1 79.7(3) 2_655 9_666 ? O1 Zn1 Zn1 79.7(3) . 9_666 ? O1 Zn1 Zn1 79.7(3) 3_565 9_666 ? N1 Zn1 Zn1 179.999(1) . 9_666 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.872 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.198