# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_ya0104 _database_code_CSD 186292 _audit_creation_method Xtal3.7.1 _audit_creation_date 01-07-13 _audit_update_record ? _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Yagasaki, Atsushi' 'Ozawa, Y.' 'Taguchi, M.' _publ_contact_author_name 'Prof Atsushi Yagasaki' _publ_contact_author_address ; Department of Chemistry Kwansei Gakuin University 2-1 Gakuen Sanda Hyogo 669-1337 JAPAN ; _publ_contact_author_email 'YAGASAKI@KWANSEI.AC.JP' _publ_section_title ; Isolation of a new mixed valence Pt molecular oxide using phosphine as protecting group ; # Formula sums constructed from STARTX celcon lines and and ADDATM # atom sites disagree! Which formula sum is more correct? # C18 H72 N4 O21 P6 Pt4 _chemical_formula_sum 'C18 H72 N4 O24 P6 Pt4' _chemical_formula_moiety ; ((Pt (O H)6) (Pt (P (C H3)3)2)3) 1+, (N O3 1-)4, 6(H2 O) ; _chemical_formula_weight 1694.94 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.311(8) _cell_length_b 16.218(3) _cell_length_c 22.777(9) _cell_angle_alpha 90.00000 _cell_angle_beta 94.21(2) _cell_angle_gamma 90.00000 _cell_volume 4904(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 220 _exptl_absorpt_coefficient_mu 11.637 _exptl_crystal_description prism _exptl_crystal_size_max .325 _exptl_crystal_size_mid .175 _exptl_crystal_size_min .150 _exptl_crystal_size_rad ? _exptl_crystal_colour lemon_yellow _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.0381 _exptl_absorpt_correction_T_max 0.2283 _diffrn_reflns_number 12265 _reflns_number_total 11953 _reflns_Friedel_coverage 0 _reflns_number_gt 4393 _reflns_threshold_expression 'Fsqd > 3.00 sig(Fsqd)' _diffrn_reflns_theta_max 30.7 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .054 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .067 _refine_ls_wR_factor_ref .144 _refine_ls_goodness_of_fit_ref 1.337 _refine_ls_number_reflns 4393 _refine_ls_number_parameters 505 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max .036 _refine_diff_density_min -3.239 _refine_diff_density_max 3.454 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection CAD4_DATCOL _computing_cell_refinement CAD4_CELDIM _computing_data_reduction xtal _computing_structure_solution SHELX-97S _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal_ORTEP _computing_publication_material 'xtal CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 240 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 84 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 24 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Pt ? 0 16 -2.352 8.388 'Int Tables Vol IV Tables 2.2B and 2.3.1' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 .67398(7) .67383(6) .60851(4) .0245(5) Uani ? ? 1.00000 ? ? Pt2 .80996(8) .57683(6) .70529(5) .0291(6) Uani ? ? 1.00000 ? ? Pt3 .43848(8) .64542(6) .60434(5) .0290(6) Uani ? ? 1.00000 ? ? Pt4 .77807(8) .78596(6) .51605(4) .0271(5) Uani ? ? 1.00000 ? ? P1 .9192(6) .6192(5) .7766(3) .039(4) Uani ? ? 1.00000 ? ? P2 .8339(7) .4431(5) .7231(3) .040(4) Uani ? ? 1.00000 ? ? P3 .3284(6) .6634(5) .6721(3) .038(4) Uani ? ? 1.00000 ? ? P4 .3323(6) .5832(5) .5378(3) .041(5) Uani ? ? 1.00000 ? ? P5 .9027(6) .7657(5) .4586(3) .039(4) Uani ? ? 1.00000 ? ? P6 .7514(6) .9145(4) .4879(3) .038(4) Uani ? ? 1.00000 ? ? O1 .6958(15) .5571(11) .6392(7) .038(11) Uani ? ? 1.00000 ? ? O2 .7767(14) .6974(10) .6767(7) .031(10) Uani ? ? 1.00000 ? ? O3 .5610(14) .6373(11) .5487(7) .028(10) Uani ? ? 1.00000 ? ? O4 .5609(15) .6928(11) .6617(8) .039(12) Uani ? ? 1.00000 ? ? O5 .7784(13) .6640(11) .5493(7) .030(10) Uani ? ? 1.00000 ? ? O6 .6717(15) .7913(11) .5806(7) .034(11) Uani ? ? 1.00000 ? ? O7 1.0679(18) .5317(15) .6234(10) .065(16) Uani ? ? 1.00000 ? ? O8 .924(2) .508(2) .5775(14) .11(3) Uani ? ? 1.00000 ? ? O9 .975(2) .6341(14) .5868(10) .067(17) Uani ? ? 1.00000 ? ? O10 .435(4) .888(2) .6286(14) .13(3) Uani ? ? 1.00000 ? ? O11 .319(2) .8595(15) .5627(13) .08(2) Uani ? ? 1.00000 ? ? O12 .476(2) .839(2) .5503(12) .09(2) Uani ? ? 1.00000 ? ? O13 .585(5) .551(3) .804(2) .20(5) Uani ? ? 1.00000 ? ? O14 .626(3) .674(2) .7811(15) .11(3) Uani ? ? 1.00000 ? ? O15 .662(3) .613(4) .8684(15) .17(4) Uani ? ? 1.00000 ? ? O16 .569(3) .648(2) .3482(16) .11(3) Uani ? ? 1.00000 ? ? O17 .684(3) .728(2) .3366(18) .13(3) Uani ? ? 1.00000 ? ? O18 .656(7) .635(4) .276(2) .23(7) Uani ? ? 1.00000 ? ? O19 .9434(19) .7748(15) .6522(10) .067(17) Uani ? ? 1.00000 ? ? O20 .544(2) .7398(16) .4523(9) .066(17) Uani ? ? 1.00000 ? ? O21 .207(3) .9332(16) .6698(12) .10(2) Uani ? ? 1.00000 ? ? O22 .555(2) .4816(17) .6938(11) .075(18) Uani ? ? 1.00000 ? ? O23 1.005(2) .9335(16) .6257(10) .08(2) Uani ? ? 1.00000 ? ? O24 .328(3) .7881(17) .4407(10) .09(2) Uani ? ? 1.00000 ? ? N1 .990(2) .5535(15) .5965(11) .043(15) Uani ? ? 1.00000 ? ? N2 .406(3) .8645(17) .5822(16) .07(2) Uani ? ? 1.00000 ? ? N3 .621(3) .619(3) .819(2) .09(3) Uani ? ? 1.00000 ? ? N4 .639(3) .673(2) .320(2) .08(3) Uani ? ? 1.00000 ? ? C1 .915(3) .565(2) .8475(12) .05(2) Uani ? ? 1.00000 ? ? C2 1.051(3) .615(2) .7601(15) .06(2) Uani ? ? 1.00000 ? ? C3 .893(3) .7238(18) .7940(14) .06(2) Uani ? ? 1.00000 ? ? C4 .775(3) .399(2) .7871(14) .07(3) Uani ? ? 1.00000 ? ? C5 .962(4) .410(2) .7292(14) .08(3) Uani ? ? 1.00000 ? ? C6 .784(3) .387(2) .6585(14) .07(3) Uani ? ? 1.00000 ? ? C7 .384(3) .732(3) .7283(13) .07(3) Uani ? ? 1.00000 ? ? C8 .210(3) .714(2) .6513(16) .07(2) Uani ? ? 1.00000 ? ? C9 .294(3) .572(2) .7127(13) .06(2) Uani ? ? 1.00000 ? ? C10 .390(2) .5690(18) .4666(11) .038(17) Uani ? ? 1.00000 ? ? C11 .312(4) .474(2) .5645(14) .10(3) Uani ? ? 1.00000 ? ? C12 .214(2) .629(2) .5184(11) .05(2) Uani ? ? 1.00000 ? ? C13 .917(3) .658(2) .4347(17) .07(2) Uani ? ? 1.00000 ? ? C14 .904(3) .815(3) .3857(12) .06(2) Uani ? ? 1.00000 ? ? C15 1.024(3) .797(2) .495(2) .08(3) Uani ? ? 1.00000 ? ? C16 .677(3) .967(2) .5381(16) .08(3) Uani ? ? 1.00000 ? ? C17 .859(3) .982(2) .4844(14) .06(2) Uani ? ? 1.00000 ? ? C18 .687(2) .920(2) .4153(13) .05(2) Uani ? ? 1.00000 ? ? 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 Pt1 .0208(5) .0149(4) .0381(6) -.0012(4) .0047(4) .0006(4) Pt2 .0269(6) .0184(5) .0418(7) -.0015(4) .0013(4) .0038(4) Pt3 .0217(5) .0195(5) .0461(7) -.0025(4) .0037(4) -.0014(4) Pt4 .0239(5) .0173(5) .0408(7) -.0016(4) .0079(4) .0012(4) P1 .030(4) .035(4) .052(5) -.003(3) .004(3) .003(3) P2 .048(5) .025(4) .046(5) .001(3) -.004(3) .010(3) P3 .023(4) .030(4) .063(5) -.005(3) .006(3) .005(3) P4 .032(4) .033(4) .057(5) -.005(4) -.002(3) -.003(3) P5 .035(5) .024(4) .060(5) -.002(3) .018(3) -.003(3) P6 .041(5) .018(4) .056(5) -.002(3) .008(3) .003(3) O1 .052(14) .031(11) .030(11) -.011(10) -.012(8) -.008(8) O2 .041(12) .024(10) .027(10) -.007(8) .005(7) -.006(7) O3 .028(10) .024(9) .032(10) .002(8) .001(7) .002(7) O4 .034(12) .023(10) .062(13) -.009(9) .012(9) -.004(8) O5 .037(11) .034(11) .021(10) .011(9) .012(7) .005(7) O6 .055(13) .020(9) .027(10) -.003(9) .002(8) .005(7) O7 .032(14) .054(16) .11(2) .019(12) .016(12) .007(12) O8 .06(2) .07(2) .20(3) -.048(19) -.011(19) -.026(19) O9 .07(2) .030(13) .10(2) .009(12) .012(13) -.008(11) O10 .22(5) .08(2) .09(2) -.01(3) -.09(3) -.021(18) O11 .06(2) .024(13) .16(3) .008(13) .050(17) .022(13) O12 .06(2) .12(3) .10(2) .03(2) .012(15) -.020(18) O13 .23(7) .13(5) .24(5) -.13(5) .08(4) -.02(3) O14 .10(3) .07(2) .15(3) -.00(2) .01(2) .02(2) O15 .07(3) .35(8) .09(3) .09(4) .022(18) .06(3) O16 .07(3) .06(2) .18(4) -.01(2) -.01(2) .029(19) O17 .07(3) .05(2) .28(5) -.03(2) -.02(2) .01(2) O18 .39(11) .14(5) .19(5) .06(6) .16(5) -.00(3) O19 .046(16) .044(15) .12(2) -.012(12) .025(12) -.007(12) O20 .063(18) .065(18) .071(16) -.026(14) .002(12) .013(12) O21 .16(3) .040(16) .11(2) -.010(18) .042(19) .026(14) O22 .052(18) .063(18) .11(2) -.018(14) .024(13) .026(14) O23 .11(2) .044(16) .09(2) -.015(15) .044(15) -.005(12) O24 .14(3) .060(18) .072(18) .02(2) .024(16) -.003(13) N1 .025(14) .029(14) .076(19) .005(11) .007(11) -.002(11) N2 .04(2) .016(14) .13(3) -.007(13) -.029(19) .019(14) N3 .04(2) .07(3) .15(4) .02(2) .06(2) .05(3) N4 .05(2) .04(2) .15(4) .007(18) .03(2) .03(2) C1 .06(2) .06(2) .035(19) .000(19) .005(14) .002(14) C2 .04(2) .04(2) .09(3) -.008(16) .018(16) -.006(16) C3 .07(3) .018(16) .09(3) -.020(16) -.013(18) -.001(14) C4 .09(3) .06(2) .05(2) -.02(2) -.001(18) -.002(17) C5 .14(4) .023(17) .06(2) .03(2) -.01(2) -.012(14) C6 .10(4) .04(2) .06(2) -.01(2) .01(2) -.007(16) C7 .05(2) .12(3) .03(2) -.00(2) .007(14) -.009(18) C8 .04(2) .04(2) .12(3) .016(17) .019(18) -.008(18) C9 .08(3) .05(2) .05(2) .030(18) .035(16) .027(15) C10 .036(17) .041(17) .041(17) -.015(14) .020(12) .002(12) C11 .18(5) .06(3) .05(2) -.08(3) .03(2) -.010(17) C12 .038(18) .10(3) .015(16) .022(18) .007(11) .005(14) C13 .05(2) .017(17) .13(3) .003(15) .03(2) -.006(15) C14 .07(3) .10(3) .023(17) -.01(2) .008(15) .027(17) C15 .02(2) .028(19) .19(4) -.020(15) .001(19) -.02(2) C16 .11(4) .05(2) .08(3) .03(2) .07(2) .013(19) C17 .08(3) .034(18) .06(2) -.009(18) -.003(18) .022(15) C18 .030(18) .06(2) .05(2) .009(17) -.003(13) .001(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter y(es) for value to be published Pt1 Pt2 . . 3.1661(16) ? Pt1 Pt3 . . 3.163(2) ? Pt1 Pt4 . . 3.1765(16) ? Pt1 O1 . . 2.032(18) ? Pt1 O2 . . 2.030(16) ? Pt1 O3 . . 2.042(16) ? Pt1 O4 . . 2.02(2) ? Pt1 O5 . . 2.013(17) ? Pt1 O6 . . 2.009(17) ? Pt2 P1 . . 2.208(8) ? Pt2 P2 . . 2.226(8) ? Pt2 O1 . . 2.084(18) ? Pt2 O2 . . 2.098(16) ? Pt3 P3 . . 2.225(8) ? Pt3 P4 . . 2.235(8) ? Pt3 O3 . . 2.141(18) ? Pt3 O4 . . 2.154(19) ? Pt4 P5 . . 2.212(8) ? Pt4 P6 . . 2.202(7) ? Pt4 O5 . . 2.118(18) ? Pt4 O6 . . 2.116(19) ? P1 C1 . . 1.84(3) ? P1 C2 . . 1.82(4) ? P1 C3 . . 1.78(3) ? P2 C4 . . 1.85(4) ? P2 C5 . . 1.78(5) ? P2 C6 . . 1.81(4) ? P3 C7 . . 1.81(4) ? P3 C8 . . 1.81(4) ? P3 C9 . . 1.82(3) ? P4 C10 . . 1.86(3) ? P4 C11 . . 1.90(4) ? P4 C12 . . 1.77(3) ? P5 C13 . . 1.84(3) ? P5 C14 . . 1.84(3) ? P5 C15 . . 1.83(4) ? P6 C16 . . 1.79(4) ? P6 C17 . . 1.81(4) ? P6 C18 . . 1.81(3) ? O16 N4 . . 1.24(6) ? O17 N4 . . 1.12(5) ? O18 N4 . . 1.21(7) ? O10 N2 . . 1.16(5) ? O11 N2 . . 1.21(5) ? O12 N2 . . 1.29(5) ? O7 N1 . . 1.22(3) ? O8 N1 . . 1.20(4) ? O9 N1 . . 1.34(3) ? O13 N3 . . 1.24(7) ? O14 N3 . . 1.25(6) ? O15 N3 . . 1.21(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter yes for value to be published Pt2 Pt1 Pt3 . . . 117.59(5) ? Pt2 Pt1 Pt4 . . . 119.42(5) ? Pt2 Pt1 O1 . . . 40.3(5) ? Pt2 Pt1 O2 . . . 40.7(5) ? Pt2 Pt1 O3 . . . 132.5(5) ? Pt2 Pt1 O4 . . . 94.1(5) ? Pt2 Pt1 O5 . . . 92.3(5) ? Pt2 Pt1 O6 . . . 133.3(5) ? Pt3 Pt1 Pt4 . . . 122.89(4) ? Pt3 Pt1 O1 . . . 89.5(6) ? Pt3 Pt1 O2 . . . 131.4(5) ? Pt3 Pt1 O3 . . . 42.1(5) ? Pt3 Pt1 O4 . . . 42.4(5) ? Pt3 Pt1 O5 . . . 134.4(5) ? Pt3 Pt1 O6 . . . 97.9(6) ? Pt4 Pt1 O1 . . . 134.7(6) ? Pt4 Pt1 O2 . . . 95.6(5) ? Pt4 Pt1 O3 . . . 93.4(5) ? Pt4 Pt1 O4 . . . 133.6(5) ? Pt4 Pt1 O5 . . . 41.0(5) ? Pt4 Pt1 O6 . . . 40.9(5) ? O1 Pt1 O2 . . . 80.8(7) ? O1 Pt1 O3 . . . 92.2(7) ? O1 Pt1 O4 . . . 91.7(7) ? O1 Pt1 O5 . . . 93.9(7) ? O1 Pt1 O6 . . . 172.6(8) ? O2 Pt1 O3 . . . 170.9(7) ? O2 Pt1 O4 . . . 90.1(7) ? O2 Pt1 O5 . . . 93.9(7) ? O2 Pt1 O6 . . . 93.3(7) ? O3 Pt1 O4 . . . 84.2(7) ? O3 Pt1 O5 . . . 92.4(7) ? O3 Pt1 O6 . . . 94.1(7) ? O4 Pt1 O5 . . . 173.6(7) ? O4 Pt1 O6 . . . 92.9(7) ? O5 Pt1 O6 . . . 81.9(7) ? Pt1 Pt2 P1 . . . 132.0(2) ? Pt1 Pt2 P2 . . . 132.7(2) ? Pt1 Pt2 O1 . . . 39.1(5) ? Pt1 Pt2 O2 . . . 39.1(4) ? P1 Pt2 P2 . . . 95.3(3) ? P1 Pt2 O1 . . . 170.0(6) ? P1 Pt2 O2 . . . 92.9(5) ? P2 Pt2 O1 . . . 93.9(5) ? P2 Pt2 O2 . . . 171.6(5) ? O1 Pt2 O2 . . . 78.1(7) ? Pt1 Pt3 P3 . . . 131.5(2) ? Pt1 Pt3 P4 . . . 131.5(2) ? Pt1 Pt3 O3 . . . 39.7(4) ? Pt1 Pt3 O4 . . . 39.3(5) ? P3 Pt3 P4 . . . 96.5(3) ? P3 Pt3 O3 . . . 171.1(5) ? P3 Pt3 O4 . . . 92.3(6) ? P4 Pt3 O3 . . . 92.4(5) ? P4 Pt3 O4 . . . 169.9(6) ? O3 Pt3 O4 . . . 78.8(7) ? Pt1 Pt4 P5 . . . 133.6(2) ? Pt1 Pt4 P6 . . . 131.8(2) ? Pt1 Pt4 O5 . . . 38.5(5) ? Pt1 Pt4 O6 . . . 38.4(5) ? P5 Pt4 P6 . . . 94.6(3) ? P5 Pt4 O5 . . . 95.2(5) ? P5 Pt4 O6 . . . 170.5(5) ? P6 Pt4 O5 . . . 169.8(5) ? P6 Pt4 O6 . . . 93.5(5) ? O5 Pt4 O6 . . . 76.9(7) ? Pt2 P1 C1 . . . 116.0(11) ? Pt2 P1 C2 . . . 115.4(11) ? Pt2 P1 C3 . . . 109.3(12) ? C1 P1 C2 . . . 104.7(16) ? C1 P1 C3 . . . 103.8(16) ? C2 P1 C3 . . . 106.6(17) ? Pt2 P2 C4 . . . 117.1(13) ? Pt2 P2 C5 . . . 115.7(12) ? Pt2 P2 C6 . . . 107.7(12) ? C4 P2 C5 . . . 106.2(17) ? C4 P2 C6 . . . 107.3(18) ? C5 P2 C6 . . . 101.5(18) ? Pt3 P3 C7 . . . 108.4(12) ? Pt3 P3 C8 . . . 118.9(12) ? Pt3 P3 C9 . . . 116.6(11) ? C7 P3 C8 . . . 102.1(17) ? C7 P3 C9 . . . 104.1(16) ? C8 P3 C9 . . . 104.8(17) ? Pt3 P4 C10 . . . 111.5(10) ? Pt3 P4 C11 . . . 107.5(13) ? Pt3 P4 C12 . . . 119.3(11) ? C10 P4 C11 . . . 103.9(16) ? C10 P4 C12 . . . 104.5(12) ? C11 P4 C12 . . . 109(2) ? Pt4 P5 C13 . . . 114.3(13) ? Pt4 P5 C14 . . . 121.5(13) ? Pt4 P5 C15 . . . 111.4(14) ? C13 P5 C14 . . . 97.8(17) ? C13 P5 C15 . . . 106.9(17) ? C14 P5 C15 . . . 103.2(18) ? Pt4 P6 C16 . . . 110.7(12) ? Pt4 P6 C17 . . . 118.4(12) ? Pt4 P6 C18 . . . 111.9(12) ? C16 P6 C17 . . . 102.4(18) ? C16 P6 C18 . . . 108.0(17) ? C17 P6 C18 . . . 104.7(15) ? Pt1 O1 Pt2 . . . 100.6(8) ? Pt1 O2 Pt2 . . . 100.2(7) ? Pt1 O3 Pt3 . . . 98.2(7) ? Pt1 O4 Pt3 . . . 98.4(8) ? Pt1 O5 Pt4 . . . 100.5(8) ? Pt1 O6 Pt4 . . . 100.7(8) ? O16 N4 O17 . . . 119(4) ? O16 N4 O18 . . . 117(5) ? O17 N4 O18 . . . 124(6) ? O10 N2 O11 . . . 127(4) ? O10 N2 O12 . . . 114(4) ? O11 N2 O12 . . . 119(3) ? O7 N1 O8 . . . 125(3) ? O7 N1 O9 . . . 119(2) ? O8 N1 O9 . . . 116(3) ? O13 N3 O14 . . . 119(4) ? O13 N3 O15 . . . 109(5) ? O14 N3 O15 . . . 131(5) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter yes for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter yes for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 P1 O2 3.121(18) . . ? P2 O1 3.15(2) . . ? P3 O4 3.16(2) . . ? P4 O3 3.16(2) . . ? P5 O5 3.198(19) . . ? P6 O6 3.147(19) . . ? O1 O2 2.63(2) . . ? O1 O3 2.94(2) . . ? O1 O4 2.91(3) . . ? O1 O5 2.96(2) . . ? O1 O22 2.62(3) . . ? O1 C6 3.02(4) . . ? O2 O4 2.87(3) . . ? O2 O5 2.95(2) . . ? O2 O6 2.94(2) . . ? O2 O19 2.64(3) . . ? O2 C3 3.02(4) . . ? O3 O4 2.73(2) . . ? O3 O5 2.93(3) . . ? O3 O6 2.96(2) . . ? O3 O20 2.75(3) . . ? O3 C10 3.05(3) . . ? O4 O6 2.92(3) . . ? O4 O14 2.81(4) . . ? O4 C7 2.96(4) . . ? O5 O6 2.63(3) . . ? O5 O9 2.73(3) . . ? O6 O12 2.76(4) . . ? O6 C16 3.02(4) . . ? O7 O8 2.15(4) . . ? O7 O9 2.20(3) . . ? O8 O9 2.16(4) . . ? O9 O19 2.77(3) . . ? O10 O11 2.13(5) . . ? O10 O12 2.06(5) . . ? O11 O12 2.15(4) . . ? O11 O21 3.18(4) . . ? O11 O24 3.02(4) . . ? O12 O20 2.95(4) . . ? O12 O24 3.17(4) . . ? O13 O14 2.14(7) . . ? O13 O15 2.00(7) . . ? O13 O22 2.76(5) . . ? O13 O23 2.81(6) . '2 646' ? O14 O15 2.24(5) . . ? O15 O24 3.10(5) . '4 565' ? O16 O17 2.03(5) . . ? O16 O18 2.09(8) . . ? O16 O20 2.84(4) . . ? O16 O22 2.80(4) . '3 666' ? O16 C11 3.15(5) . '3 666' ? O17 O18 2.06(7) . . ? O18 O21 2.79(7) . '4 564' ? O19 O23 2.78(4) . . ? O20 O24 2.98(4) . . ? O21 O23 2.80(5) . '1 455' ? C1 C2 2.90(5) . . ? C1 C3 2.85(5) . . ? C2 C3 2.89(5) . . ? C4 C5 2.90(6) . . ? C4 C6 2.95(5) . . ? C5 C6 2.78(6) . . ? C7 C8 2.81(5) . . ? C7 C9 2.86(5) . . ? C8 C9 2.88(5) . . ? C10 C11 2.96(5) . . ? C10 C12 2.87(4) . . ? C11 C12 2.99(5) . . ? C13 C14 2.78(5) . . ? C13 C15 2.95(5) . . ? C14 C15 2.88(5) . . ? C16 C17 2.80(6) . . ? C16 C18 2.91(5) . . ? C17 C18 2.86(5) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3064 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 1 _reflns_limit_l_max 31 _reflns_number_observed ? _reflns_d_resolution_high .696 _reflns_d_resolution_low 9.275 _diffrn_reflns_av_sigmaI/netI .311 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 220 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_radiation_detector ? _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .26 _refine_ls_wR_factor_all .199 _refine_ls_goodness_of_fit_all 1.088 _refine_ls_shift/su_mean .003 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end