# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # 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_mar1672a _database_code_depnum_ccdc_archive 'CCDC 922079' #TrackingRef 'Complex2_922079_mar1672a_r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C37 H22 N3 O3 Re), C4 H10 O' _chemical_formula_sum 'C78 H54 N6 O7 Re2' _chemical_formula_weight 1559.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall ' -P 2ybc' _symmetry_Int_Tables_Number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.363(3) _cell_length_b 18.607(4) _cell_length_c 11.891(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.51(3) _cell_angle_gamma 90.00 _cell_volume 3318.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 24568 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.53 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 3.705 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(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 'Mar imaging plate system' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 24568 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.53 _reflns_number_total 5827 _reflns_number_gt 4812 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Mar data collection software (1996)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1995)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1995)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5827 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.495809(10) 0.271159(7) 0.852441(13) 0.03634(7) Uani 1 1 d . . . O1 O 0.3215(3) 0.2786(2) 0.9412(4) 0.0812(13) Uani 1 1 d . . . O2 O 0.4202(3) 0.14987(18) 0.6867(3) 0.0761(11) Uani 1 1 d . . . O3 O 0.5807(2) 0.15355(17) 1.0238(3) 0.0616(9) Uani 1 1 d . . . O4 O 0.0000 0.5000 0.0000 0.238(6) Uiso 1 2 d S . . N1 N 0.5520(2) 0.36714(16) 0.9454(3) 0.0389(7) Uani 1 1 d . . . N2 N 0.4572(2) 0.35998(17) 0.7329(3) 0.0369(7) Uani 1 1 d . . . N3 N 1.0477(3) 0.2890(2) 0.7195(5) 0.0731(13) Uani 1 1 d . . . C1 C 0.3839(3) 0.2798(3) 0.9102(4) 0.0523(12) Uani 1 1 d . . . C2 C 0.4481(3) 0.1956(2) 0.7499(4) 0.0506(11) Uani 1 1 d . . . C3 C 0.5467(3) 0.1977(2) 0.9628(4) 0.0455(10) Uani 1 1 d . . . C4 C 0.5982(3) 0.3678(2) 1.0555(4) 0.0494(11) Uani 1 1 d . . . H4 H 0.5992 0.3262 1.0992 0.059 Uiso 1 1 calc R . . C5 C 0.6438(3) 0.4266(3) 1.1061(4) 0.0652(13) Uani 1 1 d . . . H5 H 0.6756 0.4251 1.1821 0.078 Uiso 1 1 calc R . . C6 C 0.6413(4) 0.4881(3) 1.0417(4) 0.0720(15) Uani 1 1 d . . . H6 H 0.6714 0.5291 1.0739 0.086 Uiso 1 1 calc R . . C7 C 0.5939(3) 0.4889(2) 0.9293(4) 0.0592(12) Uani 1 1 d . . . H7 H 0.5919 0.5303 0.8850 0.071 Uiso 1 1 calc R . . C8 C 0.5498(3) 0.4280(2) 0.8831(3) 0.0420(9) Uani 1 1 d . . . C9 C 0.4944(3) 0.42506(19) 0.7654(3) 0.0387(9) Uani 1 1 d . . . C10 C 0.4764(3) 0.4827(2) 0.6920(4) 0.0517(11) Uani 1 1 d . . . H10 H 0.5016 0.5272 0.7152 0.062 Uiso 1 1 calc R . . C11 C 0.4216(3) 0.4758(2) 0.5847(4) 0.0553(12) Uani 1 1 d . . . H11 H 0.4101 0.5149 0.5350 0.066 Uiso 1 1 calc R . . C12 C 0.3847(3) 0.4107(2) 0.5525(4) 0.0520(11) Uani 1 1 d . . . H12 H 0.3471 0.4045 0.4805 0.062 Uiso 1 1 calc R . . C13 C 0.4038(3) 0.3538(2) 0.6285(3) 0.0449(10) Uani 1 1 d . . . H13 H 0.3784 0.3093 0.6060 0.054 Uiso 1 1 calc R . . C14 C 0.6221(3) 0.27147(19) 0.7967(4) 0.0392(9) Uani 1 1 d . . . C15 C 0.6894(3) 0.2742(2) 0.7773(4) 0.0483(11) Uani 1 1 d . . . C16 C 0.7809(3) 0.2786(2) 0.7593(4) 0.0518(11) Uani 1 1 d . . . C17 C 0.8081(4) 0.2440(3) 0.6689(6) 0.086(2) Uani 1 1 d . . . H17 H 0.7669 0.2172 0.6166 0.104 Uiso 1 1 calc R . . C18 C 0.8953(4) 0.2488(4) 0.6551(6) 0.0843(19) Uani 1 1 d . . . H18 H 0.9115 0.2265 0.5927 0.101 Uiso 1 1 calc R . . C19 C 0.9574(3) 0.2861(3) 0.7327(5) 0.0623(13) Uani 1 1 d . . . C20 C 0.9323(4) 0.3221(4) 0.8214(5) 0.0833(18) Uani 1 1 d . . . H20 H 0.9739 0.3494 0.8724 0.100 Uiso 1 1 calc R . . C21 C 0.8454(3) 0.3179(3) 0.8353(5) 0.0739(15) Uani 1 1 d . . . H21 H 0.8296 0.3418 0.8966 0.089 Uiso 1 1 calc R . . C22 C 1.0979(3) 0.2237(2) 0.7347(5) 0.0604(13) Uani 1 1 d . . . C23 C 1.0936(4) 0.1786(3) 0.8259(5) 0.0728(15) Uani 1 1 d . . . H23 H 1.0591 0.1913 0.8782 0.087 Uiso 1 1 calc R . . C24 C 1.1408(3) 0.1146(3) 0.8394(4) 0.0689(14) Uani 1 1 d . . . H24 H 1.1371 0.0845 0.9006 0.083 Uiso 1 1 calc R . . C25 C 1.1927(3) 0.0947(3) 0.7643(4) 0.0609(12) Uani 1 1 d . . . C26 C 1.1980(4) 0.1401(3) 0.6731(5) 0.0713(14) Uani 1 1 d . . . H26 H 1.2334 0.1274 0.6219 0.086 Uiso 1 1 calc R . . C27 C 1.1504(4) 0.2047(3) 0.6577(5) 0.0663(14) Uani 1 1 d . . . H27 H 1.1538 0.2348 0.5964 0.080 Uiso 1 1 calc R . . C28 C 1.2416(4) 0.0275(3) 0.7788(5) 0.0723(14) Uani 1 1 d . . . C29 C 1.2792(4) -0.0274(3) 0.7922(5) 0.0860(17) Uani 1 1 d . . . H29 H 1.3091 -0.0711 0.8029 0.103 Uiso 1 1 calc R . . C30 C 1.0851(3) 0.3554(3) 0.6959(4) 0.0586(12) Uani 1 1 d . . . C31 C 1.1758(3) 0.3664(3) 0.7191(4) 0.0580(12) Uani 1 1 d . . . H31 H 1.2142 0.3299 0.7526 0.070 Uiso 1 1 calc R . . C32 C 1.2097(3) 0.4308(3) 0.6930(4) 0.0604(12) Uani 1 1 d . . . H32 H 1.2713 0.4364 0.7079 0.072 Uiso 1 1 calc R . . C33 C 1.1565(4) 0.4877(3) 0.6457(4) 0.0601(12) Uani 1 1 d . . . C34 C 1.0642(4) 0.4771(3) 0.6266(5) 0.0746(15) Uani 1 1 d . . . H34 H 1.0260 0.5147 0.5975 0.089 Uiso 1 1 calc R . . C35 C 1.0284(3) 0.4120(3) 0.6498(4) 0.0697(15) Uani 1 1 d . . . H35 H 0.9669 0.4058 0.6350 0.084 Uiso 1 1 calc R . . C36 C 1.1919(4) 0.5545(3) 0.6162(4) 0.0720(15) Uani 1 1 d . . . C37 C 1.2227(5) 0.6082(4) 0.5920(6) 0.098(2) Uani 1 1 d . . . H37 H 1.2473 0.6509 0.5727 0.117 Uiso 1 1 calc R . . C38' C -0.0860(14) 0.5002(11) 0.0300(16) 0.148(7) Uiso 0.50 1 d P A 2 H38A H -0.0904 0.5447 0.0708 0.177 Uiso 0.50 1 calc PR A 2 H38B H -0.1305 0.5024 -0.0414 0.177 Uiso 0.50 1 calc PR A 2 C38 C -0.0215(13) 0.4645(12) 0.0817(18) 0.156(7) Uiso 0.50 1 d P A 1 H38C H 0.0066 0.4876 0.1535 0.187 Uiso 0.50 1 calc PR A 1 H38D H 0.0046 0.4170 0.0822 0.187 Uiso 0.50 1 calc PR A 1 C39 C -0.1058(10) 0.4563(9) 0.0821(12) 0.248(7) Uiso 1 1 d . . . H39D H -0.0588 0.4213 0.0991 0.298 Uiso 0.50 1 calc PR A 2 H39E H -0.1591 0.4338 0.0395 0.298 Uiso 0.50 1 calc PR A 2 H39F H -0.1166 0.4755 0.1527 0.298 Uiso 0.50 1 calc PR A 2 H39A H -0.1174 0.4057 0.0861 0.298 Uiso 0.50 1 d PR A 1 H39B H -0.1427 0.4759 0.0134 0.298 Uiso 0.50 1 d PR A 1 H39C H -0.1188 0.4799 0.1482 0.298 Uiso 0.50 1 d PR A 1 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 Re1 0.03753(11) 0.02488(10) 0.04758(11) 0.00297(6) 0.01134(7) 0.00224(7) O1 0.060(3) 0.115(4) 0.072(3) 0.028(2) 0.022(2) 0.025(2) O2 0.087(3) 0.0374(19) 0.096(3) -0.0207(19) 0.002(2) -0.0054(19) O3 0.070(2) 0.0399(17) 0.073(2) 0.0250(16) 0.0130(17) 0.0175(17) N1 0.044(2) 0.0281(17) 0.0440(18) 0.0001(13) 0.0072(15) 0.0043(15) N2 0.040(2) 0.0296(17) 0.0430(17) 0.0009(13) 0.0122(15) 0.0052(15) N3 0.045(3) 0.056(3) 0.123(4) 0.008(2) 0.030(3) 0.003(2) C1 0.026(2) 0.072(3) 0.057(3) 0.033(2) 0.003(2) -0.004(2) C2 0.052(3) 0.033(2) 0.067(3) 0.006(2) 0.012(2) 0.006(2) C3 0.041(2) 0.039(2) 0.060(3) -0.003(2) 0.018(2) -0.001(2) C4 0.052(3) 0.047(3) 0.047(2) -0.0022(19) 0.004(2) 0.006(2) C5 0.066(3) 0.065(3) 0.056(3) -0.014(2) -0.006(2) 0.005(3) C6 0.076(4) 0.050(3) 0.081(3) -0.019(3) -0.003(3) -0.013(3) C7 0.068(3) 0.039(3) 0.066(3) -0.003(2) 0.003(2) -0.006(2) C8 0.045(3) 0.029(2) 0.053(2) -0.0019(17) 0.0131(19) 0.0017(18) C9 0.045(2) 0.028(2) 0.045(2) 0.0023(16) 0.0119(17) 0.0027(18) C10 0.065(3) 0.030(2) 0.062(3) 0.0063(18) 0.018(2) -0.002(2) C11 0.070(3) 0.042(3) 0.056(3) 0.018(2) 0.019(2) 0.010(2) C12 0.053(3) 0.058(3) 0.044(2) 0.006(2) 0.008(2) 0.014(2) C13 0.046(3) 0.043(2) 0.045(2) -0.0019(18) 0.0073(19) 0.005(2) C14 0.045(3) 0.024(2) 0.049(2) -0.0005(15) 0.0100(19) 0.0082(18) C15 0.052(3) 0.033(2) 0.059(3) 0.0033(18) 0.011(2) 0.003(2) C16 0.044(3) 0.044(3) 0.068(3) 0.003(2) 0.016(2) 0.002(2) C17 0.051(3) 0.094(4) 0.119(6) -0.052(4) 0.032(3) -0.020(3) C18 0.056(4) 0.103(4) 0.103(5) -0.043(4) 0.036(3) -0.017(3) C19 0.043(3) 0.054(3) 0.093(4) -0.003(3) 0.020(3) -0.003(2) C20 0.051(3) 0.100(5) 0.100(4) -0.033(3) 0.018(3) -0.015(3) C21 0.054(3) 0.087(4) 0.083(3) -0.025(3) 0.020(3) -0.003(3) C22 0.041(3) 0.049(3) 0.092(4) 0.003(2) 0.016(3) -0.001(2) C23 0.061(3) 0.071(4) 0.092(4) 0.007(3) 0.028(3) 0.001(3) C24 0.062(3) 0.066(3) 0.077(3) 0.012(3) 0.012(3) -0.002(3) C25 0.051(3) 0.052(3) 0.075(3) -0.001(2) 0.004(2) -0.002(2) C26 0.066(4) 0.064(3) 0.086(4) -0.005(3) 0.020(3) 0.006(3) C27 0.059(3) 0.059(3) 0.084(4) 0.008(3) 0.023(3) 0.004(3) C28 0.069(4) 0.053(3) 0.086(4) -0.004(3) -0.002(3) 0.000(3) C29 0.084(4) 0.055(4) 0.109(4) -0.003(3) 0.000(4) 0.004(3) C30 0.043(3) 0.057(3) 0.076(3) 0.003(2) 0.015(2) 0.003(2) C31 0.044(3) 0.051(3) 0.078(3) 0.001(2) 0.012(2) 0.001(2) C32 0.051(3) 0.058(3) 0.073(3) -0.006(2) 0.015(2) -0.002(3) C33 0.063(3) 0.058(3) 0.060(3) -0.002(2) 0.013(2) -0.005(3) C34 0.071(4) 0.060(3) 0.086(4) 0.007(3) 0.001(3) 0.005(3) C35 0.048(3) 0.068(4) 0.089(4) 0.015(3) 0.005(3) 0.004(3) C36 0.086(4) 0.060(3) 0.069(3) 0.004(3) 0.015(3) -0.007(3) C37 0.119(6) 0.064(4) 0.115(5) 0.010(4) 0.036(4) -0.016(4) _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 Re1 C2 1.901(5) . ? Re1 C3 1.938(5) . ? Re1 C1 1.992(5) . ? Re1 N2 2.176(3) . ? Re1 N1 2.178(3) . ? Re1 C14 2.182(5) . ? O1 C1 1.099(6) . ? O2 C2 1.154(6) . ? O3 C3 1.145(5) . ? O4 C38 1.28(2) . ? O4 C38 1.28(2) 3_565 ? O4 C38' 1.441(19) 3_565 ? O4 C38' 1.441(19) . ? N1 C4 1.348(5) . ? N1 C8 1.349(5) . ? N2 C13 1.337(5) . ? N2 C9 1.359(5) . ? N3 C30 1.417(6) . ? N3 C22 1.430(6) . ? N3 C19 1.430(6) . ? C4 C5 1.368(7) . ? C5 C6 1.373(7) . ? C6 C7 1.377(6) . ? C7 C8 1.373(6) . ? C8 C9 1.473(5) . ? C9 C10 1.373(6) . ? C10 C11 1.374(6) . ? C11 C12 1.357(6) . ? C12 C13 1.381(6) . ? C14 C15 1.107(6) . ? C15 C16 1.469(7) . ? C16 C17 1.393(7) . ? C16 C21 1.395(7) . ? C17 C18 1.387(7) . ? C18 C19 1.365(8) . ? C19 C20 1.373(7) . ? C20 C21 1.383(7) . ? C22 C23 1.384(7) . ? C22 C27 1.390(7) . ? C23 C24 1.385(7) . ? C24 C25 1.370(7) . ? C25 C26 1.392(7) . ? C25 C28 1.449(7) . ? C26 C27 1.398(7) . ? C28 C29 1.167(7) . ? C30 C31 1.375(6) . ? C30 C35 1.401(7) . ? C31 C32 1.368(7) . ? C32 C33 1.382(7) . ? C33 C34 1.402(7) . ? C33 C36 1.429(7) . ? C34 C35 1.382(8) . ? C36 C37 1.168(8) . ? C38' C39 1.11(2) . ? C38 C39 1.305(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 87.5(2) . . ? C2 Re1 C1 92.2(2) . . ? C3 Re1 C1 94.30(17) . . ? C2 Re1 N2 97.48(17) . . ? C3 Re1 N2 172.03(15) . . ? C1 Re1 N2 91.76(14) . . ? C2 Re1 N1 170.90(15) . . ? C3 Re1 N1 100.22(16) . . ? C1 Re1 N1 92.07(17) . . ? N2 Re1 N1 74.37(12) . . ? C2 Re1 C14 92.98(17) . . ? C3 Re1 C14 87.27(16) . . ? C1 Re1 C14 174.62(18) . . ? N2 Re1 C14 86.23(13) . . ? N1 Re1 C14 82.58(13) . . ? C38 O4 C38 180.0(17) . 3_565 ? C38 O4 C38' 126.1(10) . 3_565 ? C38 O4 C38' 53.9(10) 3_565 3_565 ? C38 O4 C38' 53.9(10) . . ? C38 O4 C38' 126.1(10) 3_565 . ? C38' O4 C38' 180.0(4) 3_565 . ? C4 N1 C8 118.1(4) . . ? C4 N1 Re1 124.6(3) . . ? C8 N1 Re1 116.7(2) . . ? C13 N2 C9 118.4(3) . . ? C13 N2 Re1 124.5(3) . . ? C9 N2 Re1 116.9(3) . . ? C30 N3 C22 122.4(4) . . ? C30 N3 C19 120.0(4) . . ? C22 N3 C19 117.6(4) . . ? O1 C1 Re1 174.2(5) . . ? O2 C2 Re1 178.9(4) . . ? O3 C3 Re1 175.6(4) . . ? N1 C4 C5 123.1(4) . . ? C4 C5 C6 118.2(4) . . ? C5 C6 C7 119.7(5) . . ? C8 C7 C6 119.4(4) . . ? N1 C8 C7 121.5(4) . . ? N1 C8 C9 115.5(3) . . ? C7 C8 C9 122.9(4) . . ? N2 C9 C10 120.1(4) . . ? N2 C9 C8 115.1(3) . . ? C10 C9 C8 124.8(4) . . ? C9 C10 C11 121.0(4) . . ? C12 C11 C10 118.7(4) . . ? C11 C12 C13 118.9(4) . . ? N2 C13 C12 122.9(4) . . ? C15 C14 Re1 174.0(4) . . ? C14 C15 C16 176.4(6) . . ? C17 C16 C21 116.9(5) . . ? C17 C16 C15 122.9(5) . . ? C21 C16 C15 120.2(4) . . ? C18 C17 C16 121.4(5) . . ? C19 C18 C17 120.3(5) . . ? C18 C19 C20 119.7(5) . . ? C18 C19 N3 119.8(5) . . ? C20 C19 N3 120.4(5) . . ? C19 C20 C21 120.2(5) . . ? C20 C21 C16 121.5(5) . . ? C23 C22 C27 119.6(5) . . ? C23 C22 N3 119.9(5) . . ? C27 C22 N3 120.4(5) . . ? C22 C23 C24 120.0(5) . . ? C25 C24 C23 121.4(5) . . ? C24 C25 C26 119.0(5) . . ? C24 C25 C28 121.0(5) . . ? C26 C25 C28 120.0(5) . . ? C25 C26 C27 120.4(5) . . ? C22 C27 C26 119.6(5) . . ? C29 C28 C25 177.9(7) . . ? C31 C30 C35 119.0(5) . . ? C31 C30 N3 121.8(5) . . ? C35 C30 N3 119.2(4) . . ? C32 C31 C30 120.2(5) . . ? C31 C32 C33 122.9(5) . . ? C32 C33 C34 116.5(5) . . ? C32 C33 C36 123.0(5) . . ? C34 C33 C36 120.6(5) . . ? C35 C34 C33 121.6(5) . . ? C34 C35 C30 119.7(5) . . ? C37 C36 C33 178.3(7) . . ? C39 C38' O4 121(2) . . ? O4 C38 C39 119.0(19) . . ? C38' C39 C38 61.2(14) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 2.015 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.121 # start Validation Reply Form _vrf_PLAT029_mar1672a ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.938 RESPONSE: The data was collected using Marresearch imaging plate using phi scan only. As a result, may be due to the restriction of the orientation of the crystal, there is a cusp of data collected by the phi scan routine, thus the diffraction measured fraction collected is rather low, only 93.8% instead of the normal 95% or above. Unfortunately, this cannot be improved due to the instrument restriction. ; _vrf_PLAT057_mar1672a ; PROBLEM: Correction for Absorption Required RT(exp) ... 2.09 RESPONSE: As explained above, only the phi scan was collected, absorption correction was not applied even though the molecules consist of heavy metal atom, Re. ; _vrf_PLAT761_mar1672a ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: The CIF was generated without the C---H bond. However, the C-H bond distance could be calculated from the atomic coordinates. ; _vrf_PLAT762_mar1672a ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: The CIF was generated without the C---H bond. However, the X-Y-H or H-Y-H angles could still be calculated from the atomic coordinates. ; _vrf_PLAT230_mar1672a ; PROBLEM: Hirshfeld Test Diff for O3 -- C3 .. 8.3 su RESPONSE: The terminal O3 atom may exhibit larger thermal motion than the atom C3, thus large Hirshfeld test difference resulted. ; _vrf_PLAT202_mar1672a ; PROBLEM: Isotropic non-H Atoms in Anion/Solvent ......... 2 RESPONSE: The diethyl ether solvent molecule was found to be disordered. Due to the high mobility of the molecules & the high data collection temperature, 253K, the atoms of the solvent molecule exhibited large thermal parameter, thus isotropic instead of anisotropic refinement was used. ; _vrf_PLAT372_mar1672a ; PROBLEM: Short C(sp)-C(sp) Bond C14 - C15 ... 1.11 Ang. RESPONSE: The C14-C15 were both sp hybridized. However, due to the connecting conjugated system, the bond length was shorter than the default value of 1.25 Ang. ; _vrf_PLAT243_mar1672a ; PROBLEM: High 'Solvent' Ueq as Compared to Neighbors of O4 High 'Solvent' Ueq as Compared to Neighbors of C39 RESPONSE: The diethyl ether solvent molecule was found to be disordered. Due to the high mobility of the molecules & the high data collection temperature, 253K, the atoms of the solvent molecule exhibited large thermal parameter, thus isotropic instead of anisotropic refinement was used. ; _vrf_PLAT242_mar1672a ; PROBLEM: Check Low Ueq as Compared to Neighbors for C16 Check Low Ueq as Compared to Neighbors for C19 RESPONSE: The phenyl ring C16..C21 is exhibiting slight rocking motion along the pivot atoms/axis C16 and C19. Thus the Ueq of C16 and C19 are much smaller than their neighboring atoms. ; _vrf_PLAT241_mar1672a ; PROBLEM: Check High Ueq as Compared to Neighbors for C17 RESPONSE: The phenyl ring C16..C21 is exhibiting slight rocking motion along the pivot atoms/axis C16 and C19. Thus the Ueq of C16 and C19 are much smaller than their neighboring atoms. ; _vrf_PLAT005_mar1672a ; PROBLEM: No _iucr_refine_instructions_details in the CIF ? RESPONSE: . ; _vrf_PLAT232_mar1672a ; PROBLEM: Hirshfeld Test Diff (M-X) Re1 -- C2 .. 5.3 su Hirshfeld Test Diff (M-X) Re1 -- C3 .. 10.0 su RESPONSE: . ; _vrf_PLAT371_mar1672a ; PROBLEM: Long C(sp2)-C(sp1) Bond C15 - C16 ... 1.47 Ang. Long C(sp2)-C(sp1) Bond C25 - C28 ... 1.45 Ang. Long C(sp2)-C(sp1) Bond C33 - C36 ... 1.43 Ang. RESPONSE: The C15-C16, C25 - C28 and C33 - C36 were all sp2-sp1 hybridized. However, due to the connecting conjugated system, the bond length was longer than the default value of 1.47 Ang. ; data_mar1711 _database_code_depnum_ccdc_archive 'CCDC 922080' #TrackingRef 'Complex6_922080_mar1711_r.cif' _audit_update_record ; 2013-03-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H26 N3 O3 Re' _chemical_formula_sum 'C39 H26 N3 O3 Re' _chemical_formula_weight 770.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall ' -P 2yn' _symmetry_Int_Tables_Number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.543(3) _cell_length_b 12.047(2) _cell_length_c 18.937(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.57(3) _cell_angle_gamma 90.00 _cell_volume 3319.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 15572 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 25.65 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.702 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'Mar imaging plate system' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 15572 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_unetI/netI 0.0809 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.65 _reflns_number_total 5717 _reflns_number_gt 3829 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Mar data collection software (1996)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1995)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1995)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0091P)^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 ? _refine_ls_number_reflns 5717 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.503552(15) 0.756775(13) 0.145648(10) 0.04407(8) Uani 1 1 d . . . O1 O 0.3259(4) 0.8313(4) 0.1707(2) 0.0994(17) Uani 1 1 d . . . O2 O 0.6055(4) 0.7743(4) 0.3162(2) 0.0945(16) Uani 1 1 d . . . O3 O 0.5487(4) 0.9988(3) 0.1281(2) 0.1004(18) Uani 1 1 d . . . N1 N 0.4327(3) 0.7152(3) 0.0270(2) 0.0437(10) Uani 1 1 d . . . N2 N 0.4729(3) 0.5794(3) 0.1430(2) 0.0481(11) Uani 1 1 d . . . N3 N 1.0581(4) 0.6232(4) 0.1099(3) 0.0648(13) Uani 1 1 d . . . C1 C 0.3893(5) 0.8012(5) 0.1594(3) 0.0581(15) Uani 1 1 d . . . C2 C 0.5654(5) 0.7695(4) 0.2518(3) 0.0607(14) Uani 1 1 d . . . C3 C 0.5310(5) 0.9072(4) 0.1348(3) 0.0633(17) Uani 1 1 d . . . C4 C 0.6299(4) 0.7143(3) 0.1307(3) 0.0415(12) Uani 1 1 d . . . C5 C 0.7041(4) 0.6988(4) 0.1271(3) 0.0486(13) Uani 1 1 d . . . C6 C 0.7935(4) 0.6790(4) 0.1235(3) 0.0488(13) Uani 1 1 d . . . C7 C 0.8661(4) 0.6330(4) 0.1834(3) 0.0546(14) Uani 1 1 d . . . H7 H 0.8561 0.6132 0.2274 0.066 Uiso 1 1 calc R . . C8 C 0.9512(5) 0.6164(4) 0.1791(3) 0.0605(16) Uani 1 1 d . . . H8 H 0.9977 0.5869 0.2204 0.073 Uiso 1 1 calc R . . C9 C 0.9696(5) 0.6424(4) 0.1144(3) 0.0571(14) Uani 1 1 d . . . C10 C 0.8987(5) 0.6862(5) 0.0544(3) 0.0737(18) Uani 1 1 d . . . H10 H 0.9090 0.7039 0.0102 0.088 Uiso 1 1 calc R . . C11 C 0.8133(5) 0.7042(5) 0.0584(3) 0.0660(16) Uani 1 1 d . . . H11 H 0.7673 0.7339 0.0169 0.079 Uiso 1 1 calc R . . C12 C 1.0953(4) 0.5149(4) 0.1262(3) 0.0569(14) Uani 1 1 d . . . C13 C 1.0370(5) 0.4240(5) 0.1123(3) 0.0661(16) Uani 1 1 d . . . H13 H 0.9737 0.4347 0.0931 0.079 Uiso 1 1 calc R . . C14 C 1.0724(6) 0.3173(5) 0.1270(3) 0.0746(19) Uani 1 1 d . . . H14 H 1.0323 0.2574 0.1179 0.089 Uiso 1 1 calc R . . C15 C 1.1668(6) 0.2982(5) 0.1549(3) 0.0715(19) Uani 1 1 d . . . C16 C 1.2233(5) 0.3888(5) 0.1698(3) 0.0724(18) Uani 1 1 d . . . H16 H 1.2865 0.3782 0.1903 0.087 Uiso 1 1 calc R . . C17 C 1.1894(5) 0.4958(5) 0.1552(3) 0.0734(17) Uani 1 1 d . . . H17 H 1.2299 0.5555 0.1649 0.088 Uiso 1 1 calc R . . C18 C 1.2007(7) 0.1888(6) 0.1663(4) 0.098(3) Uani 1 1 d . . . C19 C 1.2288(7) 0.0995(7) 0.1719(4) 0.124(4) Uani 1 1 d . . . H19 H 1.2515 0.0275 0.1765 0.149 Uiso 1 1 calc R . . C20 C 1.0953(5) 0.7030(5) 0.0743(3) 0.0642(16) Uani 1 1 d . . . C21 C 1.1495(5) 0.6717(5) 0.0318(3) 0.0603(15) Uani 1 1 d . . . H21 H 1.1638 0.5973 0.0289 0.072 Uiso 1 1 calc R . . C22 C 1.1816(5) 0.7502(4) -0.0056(3) 0.0654(15) Uani 1 1 d . . . H22 H 1.2166 0.7272 -0.0339 0.078 Uiso 1 1 calc R . . C23 C 1.1635(5) 0.8625(5) -0.0025(4) 0.0725(18) Uani 1 1 d . . . C24 C 1.1116(6) 0.8926(5) 0.0413(4) 0.090(2) Uani 1 1 d . . . H24 H 1.0983 0.9673 0.0447 0.108 Uiso 1 1 calc R . . C25 C 1.0789(6) 0.8151(5) 0.0801(4) 0.084(2) Uani 1 1 d . . . H25 H 1.0460 0.8385 0.1100 0.101 Uiso 1 1 calc R . . C26 C 1.1978(6) 0.9448(6) -0.0418(4) 0.098(3) Uani 1 1 d . . . C27 C 1.2268(8) 1.0111(6) -0.0722(5) 0.145(4) Uani 1 1 d . . . H27 H 1.2500 1.0641 -0.0965 0.174 Uiso 1 1 calc R . . C28 C 0.4092(4) 0.7886(4) -0.0307(3) 0.0515(15) Uani 1 1 d . . . H28 H 0.4254 0.8627 -0.0203 0.062 Uiso 1 1 calc R . . C29 C 0.3622(4) 0.7581(4) -0.1044(3) 0.0557(14) Uani 1 1 d . . . H29 H 0.3463 0.8118 -0.1421 0.067 Uiso 1 1 calc R . . C30 C 0.3387(4) 0.6501(4) -0.1226(3) 0.0499(13) Uani 1 1 d . . . C31 C 0.3616(4) 0.5736(4) -0.0631(2) 0.0483(13) Uani 1 1 d . . . H31 H 0.3463 0.4992 -0.0730 0.058 Uiso 1 1 calc R . . C32 C 0.4066(4) 0.6082(3) 0.0098(2) 0.0417(11) Uani 1 1 d . . . C33 C 0.4310(4) 0.5312(3) 0.0744(3) 0.0430(12) Uani 1 1 d . . . C34 C 0.4137(4) 0.4192(3) 0.0676(3) 0.0507(14) Uani 1 1 d . . . H34 H 0.3857 0.3888 0.0198 0.061 Uiso 1 1 calc R . . C35 C 0.4369(5) 0.3507(4) 0.1298(3) 0.0591(15) Uani 1 1 d . . . C36 C 0.4776(5) 0.4010(4) 0.1991(3) 0.0664(17) Uani 1 1 d . . . H36 H 0.4936 0.3583 0.2428 0.080 Uiso 1 1 calc R . . C37 C 0.4949(5) 0.5131(4) 0.2046(3) 0.0618(16) Uani 1 1 d . . . H37 H 0.5225 0.5445 0.2521 0.074 Uiso 1 1 calc R . . C38 C 0.2897(5) 0.6131(4) -0.2026(3) 0.0690(18) Uani 1 1 d . . . H38A H 0.2708 0.6770 -0.2346 0.104 Uiso 1 1 calc R . . H38B H 0.2367 0.5701 -0.2052 0.104 Uiso 1 1 calc R . . H38C H 0.3304 0.5686 -0.2190 0.104 Uiso 1 1 calc R . . C39 C 0.4173(6) 0.2277(4) 0.1216(4) 0.083(2) Uani 1 1 d . . . H39A H 0.4050 0.2059 0.0703 0.124 Uiso 1 1 calc R . . H39B H 0.3647 0.2115 0.1353 0.124 Uiso 1 1 calc R . . H39C H 0.4695 0.1876 0.1542 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.04034(14) 0.04617(12) 0.04909(12) -0.00517(9) 0.01995(9) 0.00074(9) O1 0.061(4) 0.159(4) 0.082(3) -0.014(3) 0.029(3) 0.037(3) O2 0.074(4) 0.159(4) 0.049(3) -0.018(2) 0.020(2) -0.015(3) O3 0.129(6) 0.052(2) 0.121(4) -0.007(2) 0.043(3) -0.020(2) N1 0.042(3) 0.0380(18) 0.053(2) -0.0015(15) 0.019(2) 0.0013(17) N2 0.039(3) 0.056(2) 0.051(2) 0.0077(17) 0.018(2) 0.0002(19) N3 0.044(4) 0.080(3) 0.074(3) -0.006(2) 0.026(3) 0.002(2) C1 0.039(4) 0.084(3) 0.053(3) -0.010(3) 0.017(3) 0.013(3) C2 0.042(4) 0.080(4) 0.071(4) -0.002(3) 0.033(3) 0.001(3) C3 0.072(5) 0.051(3) 0.069(4) -0.010(2) 0.027(3) 0.002(3) C4 0.042(4) 0.039(2) 0.051(3) -0.0070(18) 0.027(3) -0.002(2) C5 0.051(4) 0.046(2) 0.051(3) -0.008(2) 0.021(3) -0.001(2) C6 0.041(4) 0.053(3) 0.058(3) -0.012(2) 0.024(3) 0.000(2) C7 0.046(4) 0.073(3) 0.050(3) -0.008(2) 0.024(3) 0.003(3) C8 0.056(5) 0.073(3) 0.051(3) -0.006(2) 0.017(3) 0.007(3) C9 0.039(4) 0.077(3) 0.059(3) -0.013(2) 0.022(3) 0.000(3) C10 0.055(5) 0.118(5) 0.056(4) 0.010(3) 0.029(3) 0.014(4) C11 0.041(4) 0.107(4) 0.050(3) 0.003(3) 0.015(3) 0.007(3) C12 0.041(4) 0.081(4) 0.052(3) -0.005(2) 0.022(3) -0.002(3) C13 0.048(5) 0.085(4) 0.069(4) -0.013(3) 0.025(3) 0.003(3) C14 0.072(6) 0.089(4) 0.070(4) -0.021(3) 0.035(4) -0.010(4) C15 0.073(6) 0.081(4) 0.067(4) 0.000(3) 0.032(4) 0.008(4) C16 0.043(5) 0.099(5) 0.075(4) 0.007(3) 0.020(3) 0.016(3) C17 0.042(5) 0.102(4) 0.078(4) 0.001(3) 0.023(3) -0.001(3) C18 0.119(9) 0.096(5) 0.082(5) 0.002(4) 0.041(5) 0.019(5) C19 0.156(12) 0.104(6) 0.111(6) 0.007(4) 0.044(6) 0.021(6) C20 0.054(5) 0.078(4) 0.061(4) -0.013(3) 0.021(3) 0.000(3) C21 0.045(4) 0.072(3) 0.064(4) -0.010(3) 0.019(3) -0.001(3) C22 0.051(4) 0.080(4) 0.068(3) -0.009(3) 0.025(3) 0.001(3) C23 0.056(5) 0.079(4) 0.086(5) -0.003(3) 0.029(4) -0.002(3) C24 0.080(7) 0.073(4) 0.117(6) -0.009(4) 0.035(5) 0.004(4) C25 0.083(7) 0.084(4) 0.093(5) -0.015(3) 0.042(5) 0.007(4) C26 0.112(9) 0.076(5) 0.121(6) 0.005(4) 0.061(6) 0.006(4) C27 0.210(14) 0.075(5) 0.200(9) 0.022(5) 0.133(9) 0.001(6) C28 0.063(5) 0.042(2) 0.053(3) 0.0086(19) 0.026(3) 0.002(2) C29 0.059(4) 0.054(3) 0.055(3) 0.012(2) 0.022(3) 0.008(2) C30 0.042(4) 0.059(3) 0.050(3) 0.000(2) 0.017(3) 0.006(2) C31 0.047(4) 0.048(2) 0.049(3) -0.0071(19) 0.016(3) 0.002(2) C32 0.032(3) 0.044(2) 0.053(3) -0.0001(18) 0.020(2) 0.0038(19) C33 0.041(4) 0.040(2) 0.050(3) 0.0014(18) 0.018(2) 0.004(2) C34 0.046(4) 0.048(3) 0.054(3) 0.005(2) 0.012(3) 0.003(2) C35 0.058(5) 0.051(3) 0.071(4) 0.013(2) 0.026(3) 0.000(3) C36 0.055(5) 0.066(3) 0.078(4) 0.029(3) 0.022(3) 0.004(3) C37 0.060(5) 0.067(3) 0.057(3) 0.011(2) 0.018(3) 0.004(3) C38 0.058(5) 0.086(4) 0.055(3) -0.001(3) 0.009(3) 0.010(3) C39 0.086(6) 0.050(3) 0.111(5) 0.023(3) 0.033(4) 0.006(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 Re1 C3 1.890(6) . ? Re1 C2 1.906(6) . ? Re1 C1 1.957(6) . ? Re1 C4 2.142(6) . ? Re1 N1 2.184(4) . ? Re1 N2 2.186(4) . ? O1 C1 1.139(7) . ? O2 C2 1.160(7) . ? O3 C3 1.155(6) . ? N1 C28 1.352(6) . ? N1 C32 1.357(5) . ? N2 C37 1.354(5) . ? N2 C33 1.361(5) . ? N3 C20 1.410(7) . ? N3 C12 1.417(7) . ? N3 C9 1.426(8) . ? C4 C5 1.195(7) . ? C5 C6 1.434(8) . ? C6 C7 1.403(7) . ? C6 C11 1.403(7) . ? C7 C8 1.368(8) . ? C7 H7 0.9300 . ? C8 C9 1.388(7) . ? C8 H8 0.9300 . ? C9 C10 1.380(8) . ? C10 C11 1.373(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.386(8) . ? C12 C17 1.389(8) . ? C13 C14 1.387(8) . ? C13 H13 0.9300 . ? C14 C15 1.394(10) . ? C14 H14 0.9300 . ? C15 C16 1.367(9) . ? C15 C18 1.407(9) . ? C16 C17 1.383(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.152(10) . ? C19 H19 0.9300 . ? C20 C25 1.386(8) . ? C20 C21 1.406(8) . ? C21 C22 1.375(8) . ? C21 H21 0.9300 . ? C22 C23 1.388(7) . ? C22 H22 0.9300 . ? C23 C24 1.393(9) . ? C23 C26 1.449(9) . ? C24 C25 1.390(9) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.165(9) . ? C27 H27 0.9300 . ? C28 C29 1.378(7) . ? C28 H28 0.9300 . ? C29 C30 1.362(6) . ? C29 H29 0.9300 . ? C30 C31 1.401(6) . ? C30 C38 1.504(6) . ? C31 C32 1.375(6) . ? C31 H31 0.9300 . ? C32 C33 1.475(6) . ? C33 C34 1.374(6) . ? C34 C35 1.379(6) . ? C34 H34 0.9300 . ? C35 C36 1.381(7) . ? C35 C39 1.509(6) . ? C36 C37 1.374(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 C3 Re1 C2 89.3(2) . . ? C3 Re1 C1 90.1(3) . . ? C2 Re1 C1 89.0(2) . . ? C3 Re1 C4 87.9(2) . . ? C2 Re1 C4 90.7(2) . . ? C1 Re1 C4 178.0(2) . . ? C3 Re1 N1 99.17(18) . . ? C2 Re1 N1 171.36(17) . . ? C1 Re1 N1 92.7(2) . . ? C4 Re1 N1 87.94(17) . . ? C3 Re1 N2 172.23(18) . . ? C2 Re1 N2 97.35(18) . . ? C1 Re1 N2 94.0(2) . . ? C4 Re1 N2 88.05(17) . . ? N1 Re1 N2 74.07(13) . . ? C28 N1 C32 116.9(4) . . ? C28 N1 Re1 125.3(3) . . ? C32 N1 Re1 117.7(3) . . ? C37 N2 C33 117.5(4) . . ? C37 N2 Re1 124.7(3) . . ? C33 N2 Re1 117.8(3) . . ? C20 N3 C12 121.8(5) . . ? C20 N3 C9 118.9(5) . . ? C12 N3 C9 117.7(5) . . ? O1 C1 Re1 175.9(6) . . ? O2 C2 Re1 177.3(5) . . ? O3 C3 Re1 179.2(6) . . ? C5 C4 Re1 173.7(4) . . ? C4 C5 C6 179.2(6) . . ? C7 C6 C11 115.6(6) . . ? C7 C6 C5 123.0(5) . . ? C11 C6 C5 121.4(5) . . ? C8 C7 C6 121.9(5) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 121.5(6) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 117.4(6) . . ? C10 C9 N3 121.4(5) . . ? C8 C9 N3 121.2(6) . . ? C11 C10 C9 121.4(6) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C6 122.0(6) . . ? C10 C11 H11 119.0 . . ? C6 C11 H11 119.0 . . ? C13 C12 C17 118.2(6) . . ? C13 C12 N3 119.7(6) . . ? C17 C12 N3 122.1(6) . . ? C12 C13 C14 120.4(7) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 117.4(6) . . ? C16 C15 C18 122.5(8) . . ? C14 C15 C18 120.0(7) . . ? C15 C16 C17 122.1(7) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C12 120.5(6) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 C15 176.5(8) . . ? C18 C19 H19 180.0 . . ? C25 C20 C21 118.0(6) . . ? C25 C20 N3 120.6(6) . . ? C21 C20 N3 121.4(5) . . ? C22 C21 C20 120.7(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 122.2(6) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C24 116.6(6) . . ? C22 C23 C26 121.9(6) . . ? C24 C23 C26 121.5(6) . . ? C25 C24 C23 122.3(6) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C20 C25 C24 120.1(6) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C23 178.7(11) . . ? C26 C27 H27 180.0 . . ? N1 C28 C29 122.8(4) . . ? N1 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 117.1(4) . . ? C29 C30 C38 122.3(4) . . ? C31 C30 C38 120.7(4) . . ? C32 C31 C30 120.3(4) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? N1 C32 C31 122.2(4) . . ? N1 C32 C33 115.5(4) . . ? C31 C32 C33 122.3(4) . . ? N2 C33 C34 121.4(4) . . ? N2 C33 C32 114.9(4) . . ? C34 C33 C32 123.7(4) . . ? C33 C34 C35 121.6(5) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C36 116.4(4) . . ? C34 C35 C39 121.2(5) . . ? C36 C35 C39 122.5(5) . . ? C37 C36 C35 121.0(5) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? N2 C37 C36 122.1(5) . . ? N2 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C30 C38 H38A 109.5 . . ? C30 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C30 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.618 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.095 # start Validation Reply Form _vrf_PLAT029_mar1711 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.911 RESPONSE: The data was collected using Marresearch imaging plate using phi scan only. As a result, may be due to the restriction of the orientation of the crystal, there is a cusp of data collected by the phi scan routine, thus the diffraction measured fraction collected is rather low, only 91.1% instead of the normal 95% or above. Unfortunately, this cannot be improved due to the instrument restriction. ; _vrf_PLAT057_mar1711 ; PROBLEM: Correction for Absorption Required RT(exp) ... 1.66 RESPONSE: As explained above, only the phi scan was collected, absorption correction was not applied even though the molecules consist of heavy metal atom, Re. ; _vrf_PLAT220_mar1711 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.5 Ratio RESPONSE: The terminal O atom of the carbonyl group may exhibit larger thermal motion than the C atom, thus large non-solvent C Ueq(max)/Ueq(min) difference resulted. ; _vrf_PLAT234_mar1711 ; PROBLEM: Large Hirshfeld Difference C23 -- C24 .. 0.16 Ang. RESPONSE: The phenyl ring C20..C25 is exhibiting slight rocking motion along the pivot atoms/axis C20 and C23. Thus the Ueq of atom C23 are much smaller than the neighboring atom C24. ; _vrf_PLAT342_mar1711 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0089 Ang RESPONSE: ; _vrf_PLAT371_mar1711 ; PROBLEM: Long C(sp2)-C(sp1) Bond C5 - C6 ... 1.43 Ang. Long C(sp2)-C(sp1) Bond C23 - C26 ... 1.45 Ang. RESPONSE: The C5-C6 and C23 - C26 were all sp2-sp1 hybridized. However, due to the connecting conjugated system, the bond length was longer than the default value of 1.43 Ang. ; data_mar1395 _database_code_depnum_ccdc_archive 'CCDC 922081' #TrackingRef 'Complex7_922081_mar1395_r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H38 N3 O3 Re, 2(C H2 Cl2)' _chemical_formula_sum 'C43 H42 Cl4 N3 O3 Re' _chemical_formula_weight 976.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall ' -C 2yc' _symmetry_Int_Tables_Number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.572(7) _cell_length_b 12.522(3) _cell_length_c 23.379(5) _cell_angle_alpha 90.00 _cell_angle_beta 124.77(3) _cell_angle_gamma 90.00 _cell_volume 8795(3) _cell_formula_units_Z 8 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 25191 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 25.45 _exptl_crystal_description prism _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 3.046 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'Mar imaging plate system' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 25191 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0827 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.45 _reflns_number_total 7207 _reflns_number_gt 4789 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Mar data collection software (1996)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1995)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1995)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7207 _refine_ls_number_parameters 457 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.241875(10) 0.940798(18) 0.857875(14) 0.04789(12) Uani 1 1 d . . . O1 O 0.3081(2) 1.0969(5) 0.9751(3) 0.105(2) Uani 1 1 d . . . O2 O 0.1731(2) 1.1200(4) 0.7907(3) 0.0851(18) Uani 1 1 d . . . O3 O 0.2050(2) 0.8763(5) 0.9422(3) 0.099(2) Uani 1 1 d . . . N1 N 0.28991(17) 0.8115(4) 0.8899(3) 0.0477(13) Uani 1 1 d . . . N2 N 0.26837(18) 0.9563(4) 0.7953(3) 0.0461(13) Uani 1 1 d . . . N3 N 0.0662(2) 0.4457(4) 0.5367(3) 0.0663(17) Uani 1 1 d . . . C1 C 0.2844(3) 1.0384(6) 0.9315(4) 0.065(2) Uani 1 1 d . . . C2 C 0.1990(3) 1.0524(6) 0.8171(4) 0.0605(19) Uani 1 1 d . . . C3 C 0.2185(3) 0.9017(6) 0.9104(4) 0.067(2) Uani 1 1 d . . . C4 C 0.1963(2) 0.8328(5) 0.7773(4) 0.0525(17) Uani 1 1 d . . . C5 C 0.1719(2) 0.7706(5) 0.7321(4) 0.0563(18) Uani 1 1 d . . . C6 C 0.1429(2) 0.6946(5) 0.6798(4) 0.0550(17) Uani 1 1 d . . . C7 C 0.1502(2) 0.6610(5) 0.6312(4) 0.0634(19) Uani 1 1 d . . . H7 H 0.1724 0.6941 0.6296 0.076 Uiso 1 1 calc R . . C8 C 0.1257(2) 0.5795(5) 0.5846(4) 0.0581(18) Uani 1 1 d . . . H8 H 0.1321 0.5573 0.5533 0.070 Uiso 1 1 calc R . . C9 C 0.0912(3) 0.5304(5) 0.5845(4) 0.061(2) Uani 1 1 d . . . C10 C 0.0828(2) 0.5659(5) 0.6319(4) 0.065(2) Uani 1 1 d . . . H10 H 0.0595 0.5360 0.6317 0.078 Uiso 1 1 calc R . . C11 C 0.1088(2) 0.6458(5) 0.6801(4) 0.0592(18) Uani 1 1 d . . . H11 H 0.1032 0.6667 0.7127 0.071 Uiso 1 1 calc R . . C12 C 0.0490(2) 0.3601(5) 0.5535(4) 0.065(2) Uani 1 1 d . . . C13 C 0.0692(3) 0.3263(6) 0.6223(4) 0.073(2) Uani 1 1 d . . . H13 H 0.0951 0.3587 0.6586 0.087 Uiso 1 1 calc R . . C14 C 0.0504(3) 0.2461(7) 0.6349(5) 0.094(3) Uani 1 1 d . . . H14 H 0.0634 0.2244 0.6807 0.113 Uiso 1 1 calc R . . C15 C 0.0127(4) 0.1951(7) 0.5828(7) 0.105(3) Uani 1 1 d . . . H15 H 0.0004 0.1404 0.5936 0.126 Uiso 1 1 calc R . . C16 C -0.0069(3) 0.2244(7) 0.5150(6) 0.101(3) Uani 1 1 d . . . H16 H -0.0322 0.1894 0.4794 0.121 Uiso 1 1 calc R . . C17 C 0.0114(3) 0.3059(6) 0.5005(5) 0.081(2) Uani 1 1 d . . . H17 H -0.0014 0.3256 0.4544 0.097 Uiso 1 1 calc R . . C18 C 0.0614(3) 0.4453(5) 0.4725(4) 0.065(2) Uani 1 1 d . . . C19 C 0.0810(3) 0.3638(7) 0.4578(5) 0.101(3) Uani 1 1 d . . . H19 H 0.0964 0.3092 0.4898 0.122 Uiso 1 1 calc R . . C20 C 0.0774(5) 0.3645(10) 0.3957(7) 0.145(5) Uani 1 1 d . . . H20 H 0.0903 0.3098 0.3859 0.174 Uiso 1 1 calc R . . C21 C 0.0551(5) 0.4450(12) 0.3485(6) 0.138(5) Uani 1 1 d . . . H21 H 0.0534 0.4455 0.3073 0.166 Uiso 1 1 calc R . . C22 C 0.0348(4) 0.5264(10) 0.3617(6) 0.114(4) Uani 1 1 d . . . H22 H 0.0191 0.5801 0.3291 0.137 Uiso 1 1 calc R . . C23 C 0.0384(3) 0.5261(7) 0.4240(5) 0.086(3) Uani 1 1 d . . . H23 H 0.0254 0.5806 0.4335 0.103 Uiso 1 1 calc R . . C24 C 0.3021(2) 0.7439(5) 0.9427(3) 0.0560(18) Uani 1 1 d . . . H24 H 0.2918 0.7563 0.9703 0.067 Uiso 1 1 calc R . . C25 C 0.3291(2) 0.6577(5) 0.9575(4) 0.0626(19) Uani 1 1 d . . . H25 H 0.3364 0.6130 0.9944 0.075 Uiso 1 1 calc R . . C26 C 0.3457(2) 0.6362(5) 0.9180(3) 0.0518(17) Uani 1 1 d . . . C27 C 0.3337(2) 0.7088(5) 0.8647(3) 0.0514(17) Uani 1 1 d . . . H27 H 0.3444 0.6992 0.8373 0.062 Uiso 1 1 calc R . . C28 C 0.3066(2) 0.7937(5) 0.8518(3) 0.0444(15) Uani 1 1 d . . . C29 C 0.2933(2) 0.8741(5) 0.7960(3) 0.0449(15) Uani 1 1 d . . . C30 C 0.3052(2) 0.8700(5) 0.7506(3) 0.0482(16) Uani 1 1 d . . . H30 H 0.3215 0.8118 0.7520 0.058 Uiso 1 1 calc R . . C31 C 0.2937(2) 0.9502(5) 0.7021(3) 0.0507(16) Uani 1 1 d . . . C32 C 0.2702(2) 1.0367(5) 0.7042(4) 0.0568(18) Uani 1 1 d . . . H32 H 0.2629 1.0947 0.6747 0.068 Uiso 1 1 calc R . . C33 C 0.2579(2) 1.0358(5) 0.7498(4) 0.0521(17) Uani 1 1 d . . . H33 H 0.2415 1.0932 0.7492 0.063 Uiso 1 1 calc R . . C34 C 0.3758(3) 0.5398(5) 0.9353(4) 0.065(2) Uani 1 1 d . . . C35 C 0.3525(4) 0.4377(6) 0.9362(6) 0.113(4) Uani 1 1 d . . . H35A H 0.3715 0.3772 0.9469 0.169 Uiso 1 1 calc R . . H35B H 0.3251 0.4278 0.8914 0.169 Uiso 1 1 calc R . . H35C H 0.3464 0.4446 0.9710 0.169 Uiso 1 1 calc R . . C36 C 0.4185(3) 0.5557(6) 1.0064(5) 0.109(4) Uani 1 1 d . . . H36A H 0.4377 0.4953 1.0177 0.164 Uiso 1 1 calc R . . H36B H 0.4119 0.5628 1.0405 0.164 Uiso 1 1 calc R . . H36C H 0.4332 0.6192 1.0062 0.164 Uiso 1 1 calc R . . C37 C 0.3877(4) 0.5234(8) 0.8838(5) 0.116(4) Uani 1 1 d . . . H37A H 0.4065 0.4617 0.8970 0.174 Uiso 1 1 calc R . . H37B H 0.4032 0.5852 0.8836 0.174 Uiso 1 1 calc R . . H37C H 0.3610 0.5128 0.8382 0.174 Uiso 1 1 calc R . . C38 C 0.3051(3) 0.9441(5) 0.6485(4) 0.063(2) Uani 1 1 d . . . C39 C 0.2715(3) 0.8680(8) 0.5915(4) 0.112(4) Uani 1 1 d . . . H39A H 0.2420 0.8952 0.5707 0.168 Uiso 1 1 calc R . . H39B H 0.2740 0.7990 0.6114 0.168 Uiso 1 1 calc R . . H39C H 0.2775 0.8618 0.5566 0.168 Uiso 1 1 calc R . . C40 C 0.3517(3) 0.9025(7) 0.6818(4) 0.087(3) Uani 1 1 d . . . H40A H 0.3582 0.8986 0.6475 0.131 Uiso 1 1 calc R . . H40B H 0.3540 0.8326 0.7005 0.131 Uiso 1 1 calc R . . H40C H 0.3724 0.9497 0.7186 0.131 Uiso 1 1 calc R . . C41 C 0.3018(4) 1.0537(6) 0.6165(5) 0.099(3) Uani 1 1 d . . . H41A H 0.2724 1.0819 0.5953 0.148 Uiso 1 1 calc R . . H41B H 0.3079 1.0462 0.5818 0.148 Uiso 1 1 calc R . . H41C H 0.3231 1.1016 0.6523 0.148 Uiso 1 1 calc R . . C42 C 0.1005(9) 1.226(3) 0.9009(14) 0.51(3) Uiso 1 1 d D . . H42A H 0.0958 1.2137 0.9372 0.611 Uiso 1 1 calc R . . H42B H 0.1076 1.3008 0.9002 0.611 Uiso 1 1 calc R . . C43 C 0.0626(11) 0.9798(19) 0.7504(12) 0.51(2) Uiso 1 1 d D . . H43A H 0.0826 1.0331 0.7525 0.618 Uiso 1 1 calc R . . H43B H 0.0417 1.0116 0.7585 0.618 Uiso 1 1 calc R . . Cl3 Cl 0.0898(4) 0.8652(11) 0.8012(6) 0.505(7) Uiso 1 1 d D . . Cl4 Cl 0.0362(3) 0.8926(9) 0.6721(5) 0.393(5) Uiso 1 1 d D . . Cl1 Cl 0.1399(5) 1.1340(12) 0.9035(8) 0.564(8) Uiso 1 1 d D . . Cl2 Cl 0.0567(5) 1.1770(11) 0.8180(8) 0.559(8) Uiso 1 1 d 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 Re1 0.0617(2) 0.04872(17) 0.04466(18) -0.00373(13) 0.03707(16) -0.00409(14) O1 0.115(5) 0.133(5) 0.091(5) -0.070(4) 0.073(4) -0.060(4) O2 0.113(5) 0.066(3) 0.100(5) 0.016(3) 0.075(4) 0.029(3) O3 0.119(5) 0.129(5) 0.095(5) 0.022(4) 0.089(5) -0.005(4) N1 0.055(4) 0.051(3) 0.041(3) 0.002(2) 0.030(3) -0.004(2) N2 0.055(4) 0.046(3) 0.044(3) -0.002(2) 0.032(3) -0.006(2) N3 0.071(4) 0.060(4) 0.061(4) -0.013(3) 0.034(4) -0.019(3) C1 0.071(6) 0.090(5) 0.056(5) -0.011(4) 0.049(5) -0.014(4) C2 0.083(6) 0.069(5) 0.055(5) -0.006(4) 0.055(5) -0.006(4) C3 0.072(6) 0.065(4) 0.069(5) -0.004(4) 0.044(5) -0.010(4) C4 0.058(5) 0.054(4) 0.055(5) 0.012(3) 0.037(4) 0.003(3) C5 0.058(5) 0.048(4) 0.060(5) -0.004(3) 0.031(4) -0.005(3) C6 0.056(5) 0.046(4) 0.057(5) 0.000(3) 0.029(4) -0.001(3) C7 0.065(5) 0.067(4) 0.059(5) -0.006(4) 0.036(4) -0.007(4) C8 0.057(5) 0.061(4) 0.062(5) -0.004(3) 0.037(4) -0.005(3) C9 0.060(5) 0.053(4) 0.048(5) -0.005(3) 0.018(4) 0.003(3) C10 0.052(5) 0.072(5) 0.066(5) -0.003(4) 0.031(4) -0.008(4) C11 0.060(5) 0.058(4) 0.060(5) -0.003(3) 0.034(4) 0.000(4) C12 0.048(5) 0.058(4) 0.076(6) -0.016(4) 0.027(4) -0.004(3) C13 0.073(6) 0.068(5) 0.068(6) 0.003(4) 0.035(5) 0.000(4) C14 0.104(8) 0.082(6) 0.099(7) 0.014(5) 0.060(7) -0.009(5) C15 0.112(9) 0.076(6) 0.149(11) -0.016(7) 0.087(9) -0.023(6) C16 0.079(7) 0.092(7) 0.110(9) -0.030(6) 0.041(7) -0.030(5) C17 0.063(6) 0.076(5) 0.081(6) -0.006(4) 0.028(5) -0.005(4) C18 0.067(5) 0.064(5) 0.044(4) -0.003(4) 0.019(4) -0.005(4) C19 0.132(9) 0.090(6) 0.084(7) -0.005(5) 0.063(7) 0.031(6) C20 0.196(14) 0.132(10) 0.120(11) -0.033(8) 0.098(11) 0.025(9) C21 0.165(13) 0.181(14) 0.068(8) -0.003(8) 0.065(9) 0.003(10) C22 0.136(11) 0.128(8) 0.074(8) 0.009(6) 0.056(8) 0.005(7) C23 0.072(6) 0.091(6) 0.069(6) 0.000(5) 0.026(5) -0.001(5) C24 0.069(5) 0.061(4) 0.048(4) 0.009(3) 0.039(4) 0.003(4) C25 0.076(6) 0.060(4) 0.052(5) 0.014(3) 0.036(4) 0.002(4) C26 0.058(5) 0.047(4) 0.050(4) 0.004(3) 0.030(4) 0.001(3) C27 0.057(5) 0.055(4) 0.048(4) 0.000(3) 0.033(4) -0.002(3) C28 0.048(4) 0.051(4) 0.036(4) 0.004(3) 0.025(3) -0.002(3) C29 0.052(4) 0.045(4) 0.041(4) -0.005(3) 0.029(4) -0.005(3) C30 0.053(4) 0.051(4) 0.046(4) 0.004(3) 0.031(4) 0.006(3) C31 0.056(4) 0.063(4) 0.042(4) -0.003(3) 0.033(4) -0.002(3) C32 0.066(5) 0.060(4) 0.050(4) 0.008(3) 0.037(4) 0.000(3) C33 0.068(5) 0.052(4) 0.051(4) 0.008(3) 0.042(4) 0.005(3) C34 0.070(5) 0.056(4) 0.065(5) 0.008(3) 0.037(5) 0.009(3) C35 0.127(9) 0.060(6) 0.145(10) 0.016(5) 0.074(8) 0.002(5) C36 0.089(7) 0.089(7) 0.090(7) 0.004(5) 0.016(6) 0.026(5) C37 0.153(11) 0.110(7) 0.118(9) 0.040(6) 0.097(9) 0.063(7) C38 0.077(6) 0.081(5) 0.053(5) 0.014(4) 0.049(4) 0.014(4) C39 0.124(9) 0.169(9) 0.062(6) -0.044(6) 0.065(6) -0.035(7) C40 0.094(7) 0.122(7) 0.077(6) 0.023(5) 0.067(6) 0.021(6) C41 0.151(10) 0.106(7) 0.094(7) 0.031(5) 0.102(8) 0.024(6) _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 Re1 C2 1.901(8) . ? Re1 C3 1.916(8) . ? Re1 C1 1.956(8) . ? Re1 C4 2.139(7) . ? Re1 N2 2.175(5) . ? Re1 N1 2.183(5) . ? O1 C1 1.149(8) . ? O2 C2 1.153(8) . ? O3 C3 1.150(8) . ? N1 C24 1.345(7) . ? N1 C28 1.354(7) . ? N2 C33 1.344(7) . ? N2 C29 1.370(7) . ? N3 C12 1.408(9) . ? N3 C18 1.408(9) . ? N3 C9 1.429(8) . ? C4 C5 1.202(9) . ? C5 C6 1.431(9) . ? C6 C7 1.374(9) . ? C6 C11 1.392(9) . ? C7 C8 1.385(9) . ? C8 C9 1.402(10) . ? C9 C10 1.382(10) . ? C10 C11 1.398(9) . ? C12 C17 1.394(10) . ? C12 C13 1.399(10) . ? C13 C14 1.342(10) . ? C14 C15 1.370(13) . ? C15 C16 1.365(13) . ? C16 C17 1.366(11) . ? C18 C23 1.389(10) . ? C18 C19 1.396(11) . ? C19 C20 1.381(13) . ? C20 C21 1.369(15) . ? C21 C22 1.394(15) . ? C22 C23 1.386(13) . ? C24 C25 1.367(9) . ? C25 C26 1.391(9) . ? C26 C27 1.396(8) . ? C26 C34 1.523(9) . ? C27 C28 1.365(8) . ? C28 C29 1.493(8) . ? C29 C30 1.360(8) . ? C30 C31 1.388(8) . ? C31 C32 1.401(8) . ? C31 C38 1.531(9) . ? C32 C33 1.374(9) . ? C34 C37 1.509(11) . ? C34 C36 1.510(11) . ? C34 C35 1.544(10) . ? C38 C40 1.505(11) . ? C38 C39 1.525(11) . ? C38 C41 1.535(9) . ? C42 Cl2 1.779(18) . ? C42 Cl1 1.821(18) . ? C43 Cl3 1.764(19) . ? C43 Cl4 1.860(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 88.2(3) . . ? C2 Re1 C1 89.8(3) . . ? C3 Re1 C1 91.0(3) . . ? C2 Re1 C4 91.0(3) . . ? C3 Re1 C4 89.7(3) . . ? C1 Re1 C4 178.9(3) . . ? C2 Re1 N2 98.8(2) . . ? C3 Re1 N2 170.3(2) . . ? C1 Re1 N2 95.7(2) . . ? C4 Re1 N2 83.5(2) . . ? C2 Re1 N1 171.5(2) . . ? C3 Re1 N1 99.0(3) . . ? C1 Re1 N1 94.6(3) . . ? C4 Re1 N1 84.5(2) . . ? N2 Re1 N1 73.56(18) . . ? C24 N1 C28 117.4(5) . . ? C24 N1 Re1 124.3(4) . . ? C28 N1 Re1 118.2(4) . . ? C33 N2 C29 117.0(5) . . ? C33 N2 Re1 124.3(4) . . ? C29 N2 Re1 118.3(4) . . ? C12 N3 C18 119.4(6) . . ? C12 N3 C9 122.3(6) . . ? C18 N3 C9 118.2(6) . . ? O1 C1 Re1 177.3(7) . . ? O2 C2 Re1 178.0(6) . . ? O3 C3 Re1 178.6(7) . . ? C5 C4 Re1 177.9(6) . . ? C4 C5 C6 178.4(7) . . ? C7 C6 C11 117.9(6) . . ? C7 C6 C5 120.7(7) . . ? C11 C6 C5 121.1(7) . . ? C6 C7 C8 122.1(7) . . ? C7 C8 C9 120.2(7) . . ? C10 C9 C8 118.0(7) . . ? C10 C9 N3 122.0(7) . . ? C8 C9 N3 120.0(7) . . ? C9 C10 C11 121.2(7) . . ? C6 C11 C10 120.5(7) . . ? C17 C12 C13 118.7(8) . . ? C17 C12 N3 119.6(8) . . ? C13 C12 N3 121.7(7) . . ? C14 C13 C12 118.6(8) . . ? C13 C14 C15 122.4(9) . . ? C16 C15 C14 120.2(9) . . ? C15 C16 C17 118.8(9) . . ? C16 C17 C12 121.2(9) . . ? C23 C18 C19 119.2(8) . . ? C23 C18 N3 121.0(8) . . ? C19 C18 N3 119.7(7) . . ? C20 C19 C18 120.0(9) . . ? C21 C20 C19 120.5(11) . . ? C20 C21 C22 120.5(11) . . ? C23 C22 C21 119.1(11) . . ? C22 C23 C18 120.6(10) . . ? N1 C24 C25 123.0(6) . . ? C24 C25 C26 120.7(6) . . ? C25 C26 C27 115.5(6) . . ? C25 C26 C34 120.0(6) . . ? C27 C26 C34 124.5(6) . . ? C28 C27 C26 121.6(6) . . ? N1 C28 C27 121.8(5) . . ? N1 C28 C29 114.8(5) . . ? C27 C28 C29 123.4(6) . . ? C30 C29 N2 121.8(5) . . ? C30 C29 C28 124.6(6) . . ? N2 C29 C28 113.5(5) . . ? C29 C30 C31 121.9(6) . . ? C30 C31 C32 115.9(6) . . ? C30 C31 C38 122.3(6) . . ? C32 C31 C38 121.7(6) . . ? C33 C32 C31 120.0(6) . . ? N2 C33 C32 123.3(6) . . ? C37 C34 C36 107.9(8) . . ? C37 C34 C26 112.9(6) . . ? C36 C34 C26 109.0(6) . . ? C37 C34 C35 108.1(7) . . ? C36 C34 C35 109.1(7) . . ? C26 C34 C35 109.8(7) . . ? C40 C38 C39 110.2(7) . . ? C40 C38 C31 110.5(6) . . ? C39 C38 C31 106.6(6) . . ? C40 C38 C41 108.2(7) . . ? C39 C38 C41 109.4(7) . . ? C31 C38 C41 111.9(6) . . ? Cl2 C42 Cl1 91.1(11) . . ? Cl3 C43 Cl4 87.8(11) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 1.173 _refine_diff_density_min -2.015 _refine_diff_density_rms 0.116 # start Validation Reply Form _vrf_PLAT029_mar1395 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.885 RESPONSE: The data was collected using Marresearch imaging plate using phi scan only. As a result, may be due to the restriction of the orientation of the crystal, there is a cusp of data collected by the phi scan routine, thus the diffraction measured fraction collected is rather low, only 88.5% instead of the normal 95% or above. Unfortunately, this cannot be improved due to the instrument restriction. ; _vrf_PLAT005_mar1395 ; PROBLEM: No _iucr_refine_instructions_details in the CIF ? RESPONSE: . ; _vrf_PLAT761_mar1395 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: The CIF was generated without the C---H bond. However, the C-H bond distance could be calculated from the atomic coordinates. ; _vrf_PLAT762_mar1395 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: The CIF was generated without the C---H bond. However, the X-Y-H or H-Y-H angles could still be calculated from the atomic coordinates. ; _vrf_PLAT057_mar1395 ; PROBLEM: Correction for Absorption Required RT(exp) ... 2.12 RESPONSE: As explained above, only the phi scan was collected, absorption correction was not applied even though the molecules consist of heavy metal atom, Re. ; _vrf_PLAT202_mar1395 ; PROBLEM: Isotropic non-H Atoms in Anion/Solvent ......... 6 RESPONSE: The data set was collected at room temperature, 301 K. The solvent molecule, dichlormethane, exhibiting high thermal mobility at room temperature. ; _vrf_PLAT220_mar1395 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.3 Ratio RESPONSE: . ; _vrf_PLAT234_mar1395 ; PROBLEM: Large Hirshfeld Difference O3 -- C3 .. 0.17 Ang. Large Hirshfeld Difference C8 -- C9 .. 0.18 Ang. RESPONSE: . ; _vrf_PLAT241_mar1395 ; PROBLEM: Check High Ueq as Compared to Neighbors for C20 RESPONSE: . ; _vrf_PLAT242_mar1395 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C18 Check Low Ueq as Compared to Neighbors for C34 Check Low Ueq as Compared to Neighbors for C38 RESPONSE: The atoms C34 and C38 were the pivot atoms of a tertiary butyl group. Hence, the atoms C34 and C38 showing lower Ueq than the neighbouring terminal atoms. ; _vrf_PLAT243_mar1395 ; PROBLEM: High 'Solvent' Ueq as Compared to Neighbors of C43 RESPONSE: The data set was collected at room temperature, 301 K. The solvent molecule, dichlormethane, exhibiting high thermal mobility at room temperature. ; _vrf_PLAT244_mar1395 ; PROBLEM: Low 'Solvent' Ueq as Compared to Neighbors of C42 RESPONSE: The data set was collected at room temperature, 301 K. The solvent molecule, dichlormethane, exhibiting high thermal mobility at room temperature. ; _vrf_PLAT342_mar1395 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0129 Ang RESPONSE: The data set was collected at room temperature, 301 K. Thus, the C-C bonds could not be determined precisly due to larger thermal motion of the atoms in general. ; _vrf_PLAT860_mar1395 ; PROBLEM: Note: Number of Least-Squares Restraints ....... 5 RESPONSE: The bond distances of the solvent molecules, C---Cl, were restrained. The Cl...Cl distance is also restrained. ; _vrf_PLAT371_mar1395 ; PROBLEM: Long C(sp2)-C(sp1) Bond C5 - C6 ... 1.43 Ang. RESPONSE: The C5-C6 was sp2-sp1 hybridized. However, due to the connecting conjugated system, the bond length was longer than the default value. ; _vrf_PLAT152_mar1395 ; PROBLEM: The Supplied and Calc. Volume s.1. Differ by ... 2 Units RESPONSE: This may be related to the trancation system of the software used in calculating the cell volume. ; _vrf_PLAT790_mar1395 ; PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 2 C H2 Cl2 RESPONSE: ; _vrf_PLAT950_mar1395 ; PROBLEM: Reported and Calculated Hmax Values Differ by .. 3 RESPONSE: This discrepancy may be due to the very weak data at high angle. ; _vrf_PLAT951_mar1395 ; PROBLEM: Reported and Calculated Kmax Values Differ by .. 3 RESPONSE: This discrepancy may be due to the very weak data at high angle. ; _vrf_PLAT002_mar1395 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 6 RESPONSE: The atoms C43, C44, Cl1, Cl2, Cl3 and Cl4 were restrained. ; # end Validation Reply Form