# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1814 #=============================================================================== data_global #=============================================================================== _audit_creation_date 25-05-00 # 1. SUBMISSION DETAILS _publ_contact_author_name ; P. Braunstein ; _publ_contact_author_address ;Insitut Le Bel - Universite Louis Pasteur - 4 rue Blaise Pascal F-67070 STRASBOURG (France) ; _publ_contact_author_phone '(++33) 388 41 60 30' _publ_contact_author_fax '(++33) 388 41 60 30' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_requested_journal ? _publ_contact_letter ; ; _publ_requested_category ? #============================================================================ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ? ? # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st632 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'compound 7' _chemical_formula_moiety 'C42 H70 N4 Pt2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H70 N4 Pt2' _chemical_formula_weight 1021.23 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 Pt ? -2.352 8.388 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.829(1) _cell_length_b 22.615(1) _cell_length_c 10.618(1) _cell_angle_alpha 90 _cell_angle_beta 117.474(5) _cell_angle_gamma 90 _cell_volume 2094.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12114 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 28.3 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.62 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 6.705 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12114 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 30 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = -6.40 Omega = 0.00 Kappa = 0.00 91 frames Friedel pairs were averaged. Internal R = 0.07 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12114 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4933 _reflns_number_gt 3184 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3184 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.085 _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_all 0.164 _refine_ls_wR_factor_ref 0.068 _refine_ls_goodness_of_fit_all 3.166 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_shift/su_max 0.011 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 2.825 _refine_diff_density_min -0.475 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PT 0.13413(3) 0.10092(1) 0.91730(3) 0.0322(2) Uani ? ? Pt N1 0.3550(7) 0.0859(3) 1.0788(6) 0.028(3) Uani ? ? N C1 0.4320(8) 0.0439(3) 1.0503(7) 0.025(3) Uani ? ? C C2 0.3624(7) 0.0282(3) 0.8931(6) 0.022(3) Uani ? ? C C3 0.4348(9) -0.0146(4) 0.8538(7) 0.031(4) Uani ? ? C N2 0.2349(7) 0.0571(3) 0.8090(6) 0.028(3) Uani ? ? N C4 0.423(1) 0.1120(3) 1.2202(8) 0.037(4) Uani ? ? C C5 0.525(1) 0.1664(4) 1.2398(8) 0.041(4) Uani ? ? C C6 0.448(2) 0.2094(5) 1.117(1) 0.084(8) Uani ? ? C C7 0.674(1) 0.1503(6) 1.243(2) 0.090(8) Uani ? ? C C8 0.550(2) 0.1979(6) 1.378(1) 0.112(9) Uani ? ? C C9 0.1652(9) 0.0516(4) 0.6560(7) 0.033(4) Uani ? ? C C10 0.217(1) 0.0990(4) 0.582(1) 0.049(5) Uani ? ? C C11 0.173(1) 0.1606(5) 0.605(1) 0.083(7) Uani ? ? C C12 0.388(1) 0.0973(6) 0.636(1) 0.106(7) Uani ? ? C C13 0.125(2) 0.0877(7) 0.424(1) 0.078(8) Uani ? ? C C14 0.0445(9) 0.1575(4) 1.0229(8) 0.040(4) Uani ? ? C C15 0.026(2) 0.1014(5) 1.055(1) 0.070(7) Uani ? ? C C16 -0.128(1) 0.0673(7) 0.993(1) 0.100(7) Uani ? ? C C17 -0.209(1) 0.0530(6) 0.849(1) 0.075(7) Uani ? ? C C18 -0.164(2) 0.0768(6) 0.756(1) 0.121(9) Uani ? ? C C19 -0.081(1) 0.1223(5) 0.7441(9) 0.046(5) Uani ? ? C C20 -0.127(1) 0.1849(5) 0.772(1) 0.066(7) Uani ? ? C C21 -0.077(2) 0.1976(5) 0.920(1) 0.085(7) Uani ? ? C H1 0.6081 0.0249 1.2438 0.0423 Uiso calc ? H H2 0.4833 0.0826 1.2864 0.0468 Uiso calc C4 H H3 0.3417 0.1237 1.2401 0.0468 Uiso calc C4 H H4 0.5135 0.2424 1.1313 0.1306 Uiso calc C6 H H5 0.4295 0.1901 1.0308 0.1306 Uiso calc C6 H H6 0.3539 0.2224 1.1116 0.1306 Uiso calc C6 H H7 0.7334 0.1851 1.2551 0.1486 Uiso calc C7 H H8 0.7289 0.1240 1.3195 0.1486 Uiso calc C7 H H9 0.6551 0.1317 1.1561 0.1486 Uiso calc C7 H H10 0.6125 0.2318 1.3929 0.1468 Uiso calc C8 H H11 0.4531 0.2098 1.3700 0.1468 Uiso calc C8 H H12 0.5980 0.1716 1.4559 0.1468 Uiso calc C8 H H13 0.0571 0.0545 0.6196 0.0432 Uiso calc C9 H H14 0.1905 0.0138 0.6339 0.0432 Uiso calc C9 H H15 0.2060 0.1885 0.5584 0.1077 Uiso calc C11 H H16 0.0646 0.1630 0.5680 0.1077 Uiso calc C11 H H17 0.2203 0.1690 0.7041 0.1077 Uiso calc C11 H H18 0.4170 0.1267 0.5892 0.1355 Uiso calc C12 H H19 0.4378 0.1047 0.7354 0.1355 Uiso calc C12 H H20 0.4172 0.0595 0.6181 0.1355 Uiso calc C12 H H21 0.1529 0.1159 0.3739 0.1121 Uiso calc C13 H H22 0.1464 0.0490 0.4034 0.1121 Uiso calc C13 H H23 0.0190 0.0912 0.3972 0.1121 Uiso calc C13 H H24 0.1453 0.1733 1.0707 0.0552 Uiso calc C14 H H25 0.1147 0.0811 1.1215 0.0965 Uiso calc C15 H H26 -0.1955 0.0903 1.0141 0.1185 Uiso calc C16 H H27 -0.1072 0.0309 1.0426 0.1185 Uiso calc C16 H H28 -0.2361 0.1878 0.7226 0.0979 Uiso calc C20 H H29 -0.0840 0.2135 0.7352 0.0979 Uiso calc C20 H H30 -0.0384 0.2368 0.9375 0.1266 Uiso calc C21 H H31 -0.1640 0.1950 0.9365 0.1266 Uiso calc C21 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PT 0.0226(1) 0.0385(2) 0.0382(2) 0.0078(1) 0.0122(1) 0.0009(1) Pt N1 0.019(3) 0.034(3) 0.036(4) 0.005(2) 0.007(2) -0.002(3) N C1 0.020(3) 0.030(4) 0.026(3) -0.003(3) 0.009(2) -0.003(3) C C2 0.023(3) 0.023(3) 0.019(3) 0.003(3) 0.013(2) 0.002(3) C C3 0.026(3) 0.035(4) 0.033(3) 0.004(3) 0.011(2) 0.002(3) C N2 0.026(3) 0.038(4) 0.024(3) 0.003(3) 0.010(2) -0.003(3) N C4 0.046(4) 0.027(4) 0.042(4) 0.005(3) 0.027(3) -0.001(3) C C5 0.045(4) 0.046(5) 0.033(4) -0.016(4) 0.017(3) -0.014(4) C C6 0.085(8) 0.053(6) 0.129(9) -0.018(6) 0.020(7) 0.036(6) C C7 0.062(7) 0.053(7) 0.22(1) -0.025(6) 0.062(7) -0.024(8) C C8 0.17(1) 0.089(9) 0.090(7) -0.053(9) 0.074(6) -0.041(6) C C9 0.032(4) 0.044(5) 0.025(3) 0.002(3) 0.014(2) 0.001(3) C C10 0.043(5) 0.051(6) 0.055(5) 0.007(4) 0.017(4) 0.024(4) C C11 0.108(7) 0.050(6) 0.107(6) 0.002(6) 0.063(5) 0.030(5) C C12 0.066(5) 0.15(1) 0.117(5) 0.024(5) 0.062(3) 0.094(5) C C13 0.11(1) 0.10(1) 0.044(6) 0.018(7) 0.030(6) 0.024(5) C C14 0.033(4) 0.045(5) 0.043(4) 0.006(4) 0.012(3) -0.004(4) C C15 0.061(7) 0.074(8) 0.075(7) -0.002(6) 0.021(5) 0.002(5) C C16 0.085(6) 0.11(1) 0.111(6) -0.028(6) 0.069(4) -0.000(7) C C17 0.059(6) 0.079(8) 0.090(7) -0.013(6) 0.028(5) 0.005(6) C C18 0.33(2) 0.051(7) 0.105(7) -0.054(9) 0.127(7) -0.037(6) C C19 0.032(4) 0.058(5) 0.052(5) 0.006(4) 0.015(3) -0.001(5) C C20 0.086(7) 0.038(5) 0.087(7) 0.026(5) 0.027(5) 0.009(5) C C21 0.112(8) 0.088(7) 0.063(6) 0.071(5) 0.015(5) 0.004(6) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT N1 2.082(7) . . ? PT N2 2.083(7) . . ? PT C14 2.140(9) . . ? PT C15 2.17(2) . . ? PT C19 2.12(1) . . ? N1 C1 1.33(1) . . ? N1 C4 1.46(1) . . ? C1 C2 1.53(1) . . ? C1 C3 1.40(1) . 3_657 ? C2 C3 1.37(1) . . ? C2 N2 1.33(1) . . ? N2 C9 1.45(1) . . ? C4 C5 1.54(1) . . ? C5 C6 1.52(2) . . ? C5 C7 1.50(2) . . ? C5 C8 1.55(2) . . ? C9 C10 1.55(1) . . ? C10 C11 1.51(2) . . ? C10 C12 1.51(2) . . ? C10 C13 1.51(2) . . ? C14 C15 1.35(1) . . ? C14 C21 1.50(1) . . ? C15 C16 1.55(2) . . ? C16 C17 1.39(2) . . ? C17 C18 1.37(2) . . ? C18 C19 1.36(2) . . ? C19 C20 1.56(2) . . ? C20 C21 1.44(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 PT N2 78.2(3) . . . ? N1 PT C14 101.0(3) . . . ? N1 PT C15 95.5(4) . . . ? N1 PT C19 174.2(4) . . . ? N2 PT C14 171.6(3) . . . ? N2 PT C15 151.7(4) . . . ? N2 PT C19 99.6(3) . . . ? C14 PT C15 36.4(4) . . . ? C14 PT C19 80.4(4) . . . ? C15 PT C19 89.0(5) . . . ? PT N1 C1 114.5(6) . . . ? PT N1 C4 126.1(6) . . . ? C1 N1 C4 119.1(7) . . . ? N1 C1 C2 113.5(7) . . . ? N1 C1 C3 127.6(7) . . 3_657 ? C2 C1 C3 118.9(7) . . 3_657 ? C1 C2 C3 117.5(7) . . . ? C1 C2 N2 115.4(6) . . . ? C3 C2 N2 127.1(7) . . . ? C1 C3 C2 123.6(7) . 3_657 . ? PT N2 C2 113.9(5) . . . ? PT N2 C9 124.1(5) . . . ? C2 N2 C9 121.6(7) . . . ? N1 C4 C5 114.9(8) . . . ? C4 C5 C6 111.0(9) . . . ? C4 C5 C7 112.4(9) . . . ? C4 C5 C8 107.5(9) . . . ? C6 C5 C7 105(1) . . . ? C6 C5 C8 108(1) . . . ? C7 C5 C8 111(1) . . . ? N2 C9 C10 114.5(8) . . . ? C9 C10 C11 111(1) . . . ? C9 C10 C12 111.0(8) . . . ? C9 C10 C13 106(1) . . . ? C11 C10 C12 108(1) . . . ? C11 C10 C13 105(1) . . . ? C12 C10 C13 114(1) . . . ? PT C14 C15 72.9(8) . . . ? PT C14 C21 111.2(7) . . . ? C15 C14 C21 126(1) . . . ? PT C15 C14 70.6(8) . . . ? PT C15 C16 113(1) . . . ? C14 C15 C16 125(1) . . . ? C15 C16 C17 122(1) . . . ? C16 C17 C18 118(1) . . . ? C17 C18 C19 141(1) . . . ? PT C19 C18 98(1) . . . ? PT C19 C20 107.9(8) . . . ? C18 C19 C20 115(1) . . . ? C19 C20 C21 113(1) . . . ? C14 C21 C20 115(1) . . . ?