Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data__MAKIURA5 _database_code_CSD 155325 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ikeda, Ryuichi' 'Ishimaru, S.' 'Kimura, Noriyoshi' 'Kitagawa, Hiroshi' 'Makiura, Rie' 'Nagasawa, Isoroku' _publ_contact_author_name 'Dr Isoroku Nagasawa' _publ_contact_author_address ;Department of Chemistry, Fukuoka University of Education Akama 729-1, Munakata, Fukuoka 811-4192, Japan ; _publ_contact_author_email iso@fukuoka-edu.ac.jp _publ_contact_author_fax '+81 940-35-1711' _publ_contact_author_phone '+81 940-35-1368' _publ_requested_journal 'Chemical Communication' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF for database ; #========================================================================== #data__MAKIURA5 #========================================================================== _computing_data_collection 'CAD4_(Enraf-Nonius,_1977)' _computing_cell_refinement 'CAD4_(Enraf-Nonius,_1977)' _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'LSFM_MolEN_(Fair,_1990)' _computing_publication_material 'BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990)' #-------------------------------------------------------------------------- _cell_length_a 8.6718(4) _cell_length_b 10.7317(5) _cell_length_c 30.9849(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2883.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.0 _cell_measurement_theta_max 25.5 #-------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #-------------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.895 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1256.80 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H32 I6 P4 Pt ' _chemical_formula_moiety 'C12 H32 I6 P4 Pt' _chemical_formula_structural '[Pt I (C6 H12 P2)2 (I2)].I3' _chemical_compound_source ? _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 11.510 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.316 _exptl_special_details ; ? ; #========================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'CAD4' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -4 -13 2 4 -13 -5 0 -6 _diffrn_reflns_number 4933 _reflns_number_total 4933 _reflns_number_gt 2734 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.084 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.4 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00472 _diffrn_orient_matrix_UB_12 -0.09145 _diffrn_orient_matrix_UB_13 0.00608 _diffrn_orient_matrix_UB_21 -0.02460 _diffrn_orient_matrix_UB_22 -0.01788 _diffrn_orient_matrix_UB_23 -0.03093 _diffrn_orient_matrix_UB_31 0.11256 _diffrn_orient_matrix_UB_32 -0.00007 _diffrn_orient_matrix_UB_33 -0.00694 #---------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.002 0.002 ;International Tables for X-Ray Crystallography (1974, Vol. IV) ; H 0 128 0.000 0.000 ;International Tables for Crystallography (1974, Vol. IV) ; I 0 24 -0.726 1.812 ;International Tables for Crystallography (1974, Vol. IV) ; P 0 16 0.090 0.095 ;International Tables for Crystallography (1974, Vol. IV) ; Pt 0 4 -2.352 8.388 ;International Tables for Crystallography (1974, Vol. IV) ; #========================================================================== # 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.37810(4) 0.7500 0.87686(1) 0.0222(1) S Uani d y I(1) 0.1160(1) 0.7500 0.82349(3) 0.0468(4) S Uani d y I(2) 0.63310(8) 0.7500 0.93320(2) 0.0336(3) S Uani d y I(3) 0.87510(8) 0.7500 1.00510(2) 0.0349(3) S Uani d y I(4) 0.2276(1) 0.7500 0.09219(3) 0.0466(4) S Uani d y I(5) 0.01711(9) 0.7500 0.16761(2) 0.0384(4) S Uani d y I(6) -0.1790(1) 0.7500 0.24267(3) 0.0493(4) S Uani d y P(1) 0.4852(3) 0.9134(2) 0.83508(6) 0.0312(9) . Uani d y P(2) 0.2795(2) 0.9138(2) 0.92035(6) 0.0278(8) . Uani d y C(1) 0.404(1) 1.0575(7) 0.8562(3) 0.043(4) . Uani d y C(2) 0.389(1) 1.0520(7) 0.9049(3) 0.040(4) . Uani d y C(3) 0.691(1) 0.9353(9) 0.8371(3) 0.058(6) . Uani d y C(4) 0.442(1) 0.9194(9) 0.7784(3) 0.054(5) . Uani d y C(5) 0.298(1) 0.9092(8) 0.9788(2) 0.042(4) . Uani d y C(6) 0.080(1) 0.9514(8) 0.9124(3) 0.042(4) . Uani d y H(1a) 0.3041 1.0713 0.8437 0.0633 . Uiso c n H(1b) 0.4686 1.1263 0.8484 0.0633 . Uiso c n H(2a) 0.4885 1.0491 0.9177 0.0633 . Uiso c n H(2b) 0.3364 1.1248 0.9153 0.0633 . Uiso c n H(3a) 0.7227 0.9326 0.8672 0.0633 . Uiso c n H(3b) 0.7403 0.8690 0.8225 0.0633 . Uiso c n H(3c) 0.7174 1.0121 0.8254 0.0633 . Uiso c n H(4a) 0.3326 0.9075 0.7742 0.0633 . Uiso c n H(4b) 0.4711 0.9963 0.7666 0.0633 . Uiso c n H(4c) 0.4940 0.8532 0.7637 0.0633 . Uiso c n H(5a) 0.4011 0.8885 0.9872 0.0633 . Uiso c n H(5b) 0.2710 0.9869 0.9915 0.0633 . Uiso c n H(5c) 0.2306 0.8461 0.9908 0.0633 . Uiso c n H(6a) 0.0577 0.9567 0.8824 0.0633 . Uiso c n H(6b) 0.0166 0.8886 0.9250 0.0633 . Uiso c n H(6c) 0.0570 1.0294 0.9257 0.0633 . Uiso c n 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 Pt(1) 0.0238(2) 0.0218(1) 0.0212(1) 0.0000 -0.0012(2) 0.0000 I(1) 0.0411(4) 0.0700(5) 0.0356(4) 0.0000 -0.0151(3) 0.0000 I(2) 0.0278(3) 0.0369(3) 0.0369(3) 0.0000 -0.0022(3) 0.0000 I(3) 0.0337(3) 0.0386(4) 0.0326(3) 0.0000 -0.0043(3) 0.0000 I(4) 0.0451(4) 0.0606(5) 0.0371(4) 0.0000 0.0043(4) 0.0000 I(5) 0.0393(4) 0.0395(4) 0.0366(3) 0.0000 -0.0043(3) 0.0000 I(6) 0.0477(4) 0.0556(5) 0.0451(4) 0.0000 0.0084(4) 0.0000 P(1) 0.038(1) 0.0277(9) 0.0286(8) -0.0008(8) 0.0064(9) 0.0038(8) P(2) 0.0295(9) 0.0264(8) 0.0274(8) 0.0031(8) 0.0014(8) -0.0023(7) C(1) 0.063(5) 0.030(4) 0.042(4) 0.006(4) 0.014(4) 0.007(3) C(2) 0.054(5) 0.027(4) 0.043(4) -0.003(4) 0.015(4) -0.002(3) C(3) 0.036(5) 0.055(5) 0.096(7) -0.005(5) 0.012(5) 0.021(5) C(4) 0.089(7) 0.054(5) 0.034(4) -0.006(6) 0.012(5) 0.009(4) C(5) 0.053(5) 0.050(5) 0.029(4) 0.012(4) -0.006(4) -0.006(4) C(6) 0.036(4) 0.040(4) 0.050(5) 0.011(4) 0.007(4) 0.001(4) #========================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00E+00 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2734 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.033 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_all 0.040 _refine_ls_wR_factor_ref 0.040 _refine_ls_goodness_of_fit_all 1.346 _refine_ls_goodness_of_fit_ref 1.35 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean ? _refine_diff_density_min 0.0000 _refine_diff_density_max 0.7778 #========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Pt1 I1 2.8106(9) y Pt1 I2 2.8173(8) y Pt1 P1 2.369(2) y Pt1 P2 2.374(2) y I2 I3 3.061(1) y I4 I5 2.965(1) y I5 I6 2.881(1) y P1 C1 1.821(8) y P1 C3 1.800(9) y P1 C4 1.797(8) y P2 C2 1.823(8) y P2 C5 1.817(7) y P2 C6 1.798(9) y C1 C2 1.52(1) y C1 H1a 0.9575 n C1 H1b 0.9593 n C2 H2a 0.9534 n C2 H2b 0.9585 n C3 H3a 0.9750 n C3 H3b 0.9456 n C3 H3c 0.9288 n C4 H4a 0.9696 n C4 H4b 0.9363 n C4 H4c 0.9549 n C5 H5a 0.9606 n C5 H5b 0.9503 n C5 H5c 0.9685 n C6 H6a 0.9507 n C6 H6b 0.9516 n C6 H6c 0.9522 n #-------------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag I1 Pt1 I2 177.75(3) y I1 Pt1 P1 89.73(5) y I1 Pt1 P2 92.45(5) y I2 Pt1 P1 91.78(5) y I2 Pt1 P2 86.04(5) y P1 Pt1 P2 84.46(6) y Pt1 I2 I3 171.58(3) y I4 I5 I6 178.18(4) y Pt1 P1 C1 106.3(3) y Pt1 P1 C3 117.8(3) y Pt1 P1 C4 118.7(3) y C1 P1 C3 105.1(4) y C1 P1 C4 103.9(4) y C3 P1 C4 103.5(5) y Pt1 P2 C2 105.5(3) y Pt1 P2 C5 120.9(3) y Pt1 P2 C6 115.9(3) y C2 P2 C5 103.8(4) y C2 P2 C6 106.4(4) y C5 P2 C6 103.1(4) y P1 C1 C2 110.9(6) y P1 C1 H1a 109.69 n P1 C1 H1b 109.66 n C2 C1 H1a 109.13 n C2 C1 H1b 109.31 n H1a C1 H1b 108.06 n P2 C2 C1 109.8(6) n P2 C2 H2a 109.64 n P2 C2 H2b 109.32 n C1 C2 H2a 109.60 n C1 C2 H2b 110.02 n H2a C2 H2b 108.47 n P1 C3 H3a 108.10 n P1 C3 H3b 109.62 n P1 C3 H3c 110.44 n H3a C3 H3b 107.74 n H3a C3 H3c 109.12 n H3b C3 H3c 111.71 n P1 C4 H4a 109.12 n P1 C4 H4b 110.98 n P1 C4 H4c 110.04 n H4a C4 H4b 108.96 n H4a C4 H4c 107.43 n H4b C4 H4c 110.22 n P2 C5 H5a 111.04 n P2 C5 H5b 111.58 n P2 C5 H5c 110.56 n H5a C5 H5b 108.55 n H5a C5 H5c 107.06 n H5b C5 H5c 107.89 n P2 C6 H6a 109.83 n P2 C6 H6b 109.71 n P2 C6 H6c 109.66 n H6a C6 H6b 109.27 n H6a C6 H6c 109.22 n H6b C6 H6c 109.14 n #-------------------------------------------------------------------------- #========================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #========================================================================== # End of CIF #=========================================================================