Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Chris Orvig' _publ_contact_author_address ; Department of Chemistry University of British Columbia 2036 Main Mall Vancouver BC V6T 1Z1 CANADA ; _publ_contact_author_email ORVIG@CHEM.UBC.CA _publ_section_title ; Coordination Chemistry of Bidentate PO-Phosphinophenolates with Ga3+ and In3+ ; loop_ _publ_author_name 'Chris Orvig' 'Brian O. Patrick' 'Katayoun Saatchi' #------------------------------------------------------------------------------ data_co248/KS-III-124 _database_code_depnum_ccdc_archive 'CCDC 262805' #------------------------------------------------------------------------------ _audit_creation_date 2000-06-05 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1996-1998). d*TREK. Area Detector Software. Version 4.4. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Burla, M.C., Cammalli, G., Cascarano, M., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, A. (1998). SIR97: a new tool for crystal structure determination and refinement. Submitted. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.0558(3) _cell_length_b 13.2211(7) _cell_length_c 18.694(2) _cell_angle_alpha 83.908(2) _cell_angle_beta 85.429(3) _cell_angle_gamma 64.939(2) _cell_volume 2459.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 9770 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 27.89 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description platelet _exptl_crystal_colour clear _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1167.84 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H42 Cl3 In2 O3 P3 ' _chemical_formula_moiety 'C54 H42 Cl3 In2 O3 P3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1168.00 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7242 _exptl_special_details ; Data were collected in 0.50\% oscillations with 12.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -19.0 and 23.0\% at \c = -90.0\%. The crystal-to-detector distance was 40.51 mm. The detector swing angle was -5.5\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 20441 _reflns_number_total 9328 _reflns_number_gt 5818 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06308 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 84 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 6 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 6 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; In 0 4 -0.936 1.310 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 6 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom In(1) 0.32965(4) 0.77949(3) 0.23338(2) 0.0244(1) 1.000 . Uani d ? In(2) 0.13194(4) 1.03802(3) 0.25216(2) 0.0205(1) 1.000 . Uani d ? Cl(1) 0.4833(2) 0.6835(1) 0.14050(9) 0.0428(5) 1.000 . Uani d ? Cl(2) 0.1576(2) 1.1497(1) 0.3366(1) 0.0430(5) 1.000 . Uani d ? Cl(3) -0.1045(1) 1.0827(1) 0.26468(9) 0.0345(4) 1.000 . Uani d ? P(1) 0.1827(1) 0.6667(1) 0.27242(8) 0.0245(4) 1.000 . Uani d ? P(2) 0.4999(1) 0.7379(1) 0.34207(8) 0.0245(4) 1.000 . Uani d ? P(3) 0.1295(1) 1.1488(1) 0.12433(8) 0.0233(4) 1.000 . Uani d ? O(1) 0.1823(3) 0.8789(3) 0.3168(2) 0.024(1) 1.000 . Uani d ? O(2) 0.3566(3) 0.9341(3) 0.2356(2) 0.023(1) 1.000 . Uani d ? O(3) 0.1676(3) 0.9115(3) 0.1721(2) 0.025(1) 1.000 . Uani d ? C(1) 0.0941(5) 0.7417(4) 0.3489(3) 0.022(1) 1.000 . Uani d ? C(2) 0.0126(6) 0.7052(4) 0.3960(3) 0.026(2) 1.000 . Uani d ? C(3) -0.0525(6) 0.7631(5) 0.4545(3) 0.028(2) 1.000 . Uani d ? C(4) -0.0391(6) 0.8594(5) 0.4666(3) 0.030(2) 1.000 . Uani d ? C(5) 0.0358(5) 0.8994(4) 0.4198(3) 0.027(2) 1.000 . Uani d ? C(6) 0.1057(5) 0.8403(4) 0.3609(3) 0.022(1) 1.000 . Uani d ? C(7) 0.2812(6) 0.5206(4) 0.3010(3) 0.030(2) 1.000 . Uani d ? C(8) 0.4176(6) 0.4769(5) 0.2882(4) 0.039(2) 1.000 . Uani d ? C(9) 0.4972(7) 0.3662(5) 0.3089(5) 0.054(2) 1.000 . Uani d ? C(10) 0.4390(8) 0.2992(5) 0.3433(4) 0.051(2) 1.000 . Uani d ? C(11) 0.3074(8) 0.3396(5) 0.3564(4) 0.051(2) 1.000 . Uani d ? C(12) 0.2253(7) 0.4519(5) 0.3338(4) 0.044(2) 1.000 . Uani d ? C(13) 0.0514(5) 0.6706(4) 0.2181(3) 0.025(2) 1.000 . Uani d ? C(14) 0.0570(6) 0.5778(5) 0.1888(4) 0.037(2) 1.000 . Uani d ? C(15) -0.0492(7) 0.5817(5) 0.1526(4) 0.041(2) 1.000 . Uani d ? C(16) -0.1622(6) 0.6801(6) 0.1446(3) 0.039(2) 1.000 . Uani d ? C(17) -0.1695(6) 0.7746(5) 0.1723(4) 0.039(2) 1.000 . Uani d ? C(18) -0.0628(6) 0.7697(5) 0.2092(3) 0.032(2) 1.000 . Uani d ? C(19) 0.5420(5) 0.8542(4) 0.3144(3) 0.022(1) 1.000 . Uani d ? C(20) 0.6528(5) 0.8608(4) 0.3415(3) 0.028(2) 1.000 . Uani d ? C(21) 0.6857(5) 0.9488(4) 0.3188(3) 0.027(2) 1.000 . Uani d ? C(22) 0.6087(6) 1.0315(4) 0.2677(4) 0.031(2) 1.000 . Uani d ? C(23) 0.4996(5) 1.0258(4) 0.2409(3) 0.027(2) 1.000 . Uani d ? C(24) 0.4641(5) 0.9375(4) 0.2640(3) 0.020(1) 1.000 . Uani d ? C(25) 0.4130(5) 0.7627(5) 0.4295(3) 0.028(2) 1.000 . Uani d ? C(26) 0.3776(7) 0.8616(5) 0.4603(4) 0.042(2) 1.000 . Uani d ? C(27) 0.3058(8) 0.8750(7) 0.5275(4) 0.060(2) 1.000 . Uani d ? C(28) 0.2711(7) 0.793(1) 0.5599(4) 0.069(3) 1.000 . Uani d ? C(29) 0.3092(8) 0.6953(9) 0.5287(4) 0.065(3) 1.000 . Uani d ? C(30) 0.3787(6) 0.6785(6) 0.4635(4) 0.042(2) 1.000 . Uani d ? C(31) 0.6567(6) 0.6182(4) 0.3587(3) 0.028(2) 1.000 . Uani d ? C(32) 0.7133(6) 0.5938(5) 0.4256(4) 0.040(2) 1.000 . Uani d ? C(33) 0.8357(7) 0.5033(6) 0.4378(4) 0.049(2) 1.000 . Uani d ? C(34) 0.9001(6) 0.4363(5) 0.3816(5) 0.049(2) 1.000 . Uani d ? C(35) 0.8464(7) 0.4593(5) 0.3164(4) 0.048(2) 1.000 . Uani d ? C(36) 0.7229(6) 0.5508(5) 0.3033(4) 0.038(2) 1.000 . Uani d ? C(37) 0.1503(5) 1.0406(4) 0.0674(3) 0.025(2) 1.000 . Uani d ? C(38) 0.1471(6) 1.0594(5) -0.0083(3) 0.033(2) 1.000 . Uani d ? C(39) 0.1654(6) 0.9742(6) -0.0507(3) 0.038(2) 1.000 . Uani d ? C(40) 0.1837(6) 0.8704(6) -0.0178(4) 0.041(2) 1.000 . Uani d ? C(41) 0.1845(5) 0.8486(5) 0.0561(4) 0.032(2) 1.000 . Uani d ? C(42) 0.1689(5) 0.9341(5) 0.1011(3) 0.026(2) 1.000 . Uani d ? C(43) 0.2646(5) 1.1924(4) 0.1013(3) 0.028(2) 1.000 . Uani d ? C(44) 0.3655(6) 1.1442(5) 0.0509(4) 0.038(2) 1.000 . Uani d ? C(45) 0.4671(6) 1.1809(6) 0.0374(4) 0.048(2) 1.000 . Uani d ? C(46) 0.4657(7) 1.2655(6) 0.0744(5) 0.052(2) 1.000 . Uani d ? C(47) 0.3671(6) 1.3117(5) 0.1263(4) 0.047(2) 1.000 . Uani d ? C(48) 0.2662(6) 1.2761(5) 0.1398(4) 0.034(2) 1.000 . Uani d ? C(49) -0.0183(5) 1.2744(4) 0.0984(3) 0.024(1) 1.000 . Uani d ? C(50) -0.0193(6) 1.3378(5) 0.0342(3) 0.035(2) 1.000 . Uani d ? C(51) -0.1343(7) 1.4318(5) 0.0138(3) 0.041(2) 1.000 . Uani d ? C(52) -0.2486(6) 1.4614(5) 0.0573(4) 0.040(2) 1.000 . Uani d ? C(53) -0.2483(6) 1.4014(5) 0.1221(4) 0.034(2) 1.000 . Uani d ? C(54) -0.1334(6) 1.3084(5) 0.1429(3) 0.031(2) 1.000 . Uani d ? H(1) 0.0013 0.6381 0.3870 0.030 1.000 . Uiso c ? H(2) -0.1071 0.7360 0.4879 0.034 1.000 . Uiso c ? H(3) -0.0844 0.8998 0.5089 0.036 1.000 . Uiso c ? H(4) 0.0402 0.9697 0.4282 0.032 1.000 . Uiso c ? H(5) 0.4587 0.5254 0.2644 0.044 1.000 . Uiso c ? H(6) 0.5942 0.3349 0.2983 0.066 1.000 . Uiso c ? H(7) 0.4944 0.2208 0.3581 0.061 1.000 . Uiso c ? H(8) 0.2666 0.2920 0.3823 0.063 1.000 . Uiso c ? H(9) 0.1284 0.4809 0.3422 0.052 1.000 . Uiso c ? H(10) 0.1385 0.5075 0.1935 0.044 1.000 . Uiso c ? H(11) -0.0442 0.5145 0.1324 0.049 1.000 . Uiso c ? H(12) -0.2374 0.6824 0.1188 0.048 1.000 . Uiso c ? H(13) -0.2498 0.8451 0.1662 0.047 1.000 . Uiso c ? H(14) -0.0683 0.8372 0.2293 0.036 1.000 . Uiso c ? H(15) 0.7081 0.8022 0.3770 0.034 1.000 . Uiso c ? H(16) 0.7617 0.9541 0.3385 0.032 1.000 . Uiso c ? H(17) 0.6340 1.0928 0.2509 0.036 1.000 . Uiso c ? H(18) 0.4455 1.0845 0.2055 0.031 1.000 . Uiso c ? H(19) 0.4028 0.9203 0.4373 0.050 1.000 . Uiso c ? H(20) 0.2786 0.9451 0.5506 0.072 1.000 . Uiso c ? H(21) 0.2204 0.8034 0.6061 0.083 1.000 . Uiso c ? H(22) 0.2855 0.6362 0.5524 0.076 1.000 . Uiso c ? H(23) 0.4040 0.6082 0.4412 0.049 1.000 . Uiso c ? H(24) 0.6649 0.6406 0.4649 0.049 1.000 . Uiso c ? H(25) 0.8772 0.4878 0.4846 0.058 1.000 . Uiso c ? H(26) 0.9843 0.3706 0.3901 0.058 1.000 . Uiso c ? H(27) 0.8955 0.4116 0.2777 0.058 1.000 . Uiso c ? H(28) 0.6847 0.5676 0.2556 0.043 1.000 . Uiso c ? H(29) 0.1304 1.1344 -0.0306 0.040 1.000 . Uiso c ? H(30) 0.1649 0.9877 -0.1036 0.045 1.000 . Uiso c ? H(31) 0.1957 0.8101 -0.0477 0.050 1.000 . Uiso c ? H(32) 0.1971 0.7741 0.0775 0.038 1.000 . Uiso c ? H(33) 0.3673 1.0831 0.0246 0.045 1.000 . Uiso c ? H(34) 0.5389 1.1471 0.0013 0.057 1.000 . Uiso c ? H(35) 0.5364 1.2919 0.0649 0.062 1.000 . Uiso c ? H(36) 0.3677 1.3711 0.1533 0.055 1.000 . Uiso c ? H(37) 0.1965 1.3091 0.1770 0.042 1.000 . Uiso c ? H(38) 0.0625 1.3165 0.0032 0.040 1.000 . Uiso c ? H(39) -0.1351 1.4765 -0.0315 0.049 1.000 . Uiso c ? H(40) -0.3308 1.5257 0.0427 0.048 1.000 . Uiso c ? H(41) -0.3292 1.4233 0.1532 0.041 1.000 . Uiso c ? H(42) -0.1338 1.2667 0.1895 0.038 1.000 . Uiso c ? 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 In(1) 0.0147(2) 0.0165(2) 0.0400(3) -0.0035(2) -0.0001(2) -0.0080(2) In(2) 0.0127(2) 0.0148(2) 0.0348(3) -0.0058(1) 0.0003(2) -0.0061(2) Cl(1) 0.0282(9) 0.0410(8) 0.044(1) 0.0022(7) 0.0032(7) -0.0143(7) Cl(2) 0.048(1) 0.0403(8) 0.052(1) -0.0255(8) 0.0046(8) -0.0244(8) Cl(3) 0.0123(7) 0.0343(7) 0.054(1) -0.0090(6) 0.0011(7) 0.0042(7) P(1) 0.0178(7) 0.0183(6) 0.0328(9) -0.0033(6) 0.0006(6) -0.0015(6) P(2) 0.0237(8) 0.0202(7) 0.0295(9) -0.0091(6) 0.0036(6) -0.0048(6) P(3) 0.0134(7) 0.0265(7) 0.0271(9) -0.0039(6) -0.0013(6) -0.0094(6) O(1) 0.015(2) 0.019(2) 0.038(2) -0.007(2) -0.002(2) -0.001(2) O(2) 0.011(2) 0.019(2) 0.039(3) -0.005(1) -0.005(2) -0.006(2) O(3) 0.018(2) 0.020(2) 0.035(3) -0.004(2) -0.002(2) -0.011(2) C(1) 0.015(3) 0.022(3) 0.029(3) -0.008(2) 0.000(2) -0.001(2) C(2) 0.025(3) 0.024(3) 0.032(4) -0.013(2) -0.004(3) 0.004(2) C(3) 0.030(3) 0.032(3) 0.022(3) -0.014(3) 0.002(3) 0.006(3) C(4) 0.025(3) 0.037(3) 0.021(3) -0.006(3) -0.005(3) -0.002(3) C(5) 0.022(3) 0.030(3) 0.032(4) -0.011(2) -0.001(3) -0.010(3) C(6) 0.013(3) 0.021(3) 0.031(3) -0.006(2) -0.006(2) 0.001(2) C(7) 0.026(3) 0.022(3) 0.036(4) -0.005(2) -0.006(3) 0.001(3) C(8) 0.030(4) 0.027(3) 0.054(5) -0.006(3) -0.007(3) 0.001(3) C(9) 0.028(4) 0.030(3) 0.085(6) 0.004(3) -0.001(4) 0.002(4) C(10) 0.057(5) 0.020(3) 0.071(6) -0.010(3) -0.028(4) 0.009(3) C(11) 0.051(5) 0.030(3) 0.072(6) -0.017(3) -0.012(4) 0.003(3) C(12) 0.037(4) 0.022(3) 0.071(5) -0.012(3) -0.004(4) 0.005(3) C(13) 0.024(3) 0.025(3) 0.026(3) -0.010(2) 0.002(2) -0.006(2) C(14) 0.032(4) 0.034(3) 0.041(4) -0.007(3) -0.004(3) -0.005(3) C(15) 0.046(4) 0.045(4) 0.041(4) -0.024(3) 0.004(3) -0.019(3) C(16) 0.028(4) 0.058(4) 0.029(4) -0.019(3) 0.000(3) 0.002(3) C(17) 0.029(4) 0.043(4) 0.035(4) -0.005(3) -0.001(3) -0.005(3) C(18) 0.027(3) 0.031(3) 0.030(4) -0.004(3) -0.005(3) -0.003(3) C(19) 0.015(3) 0.024(3) 0.027(3) -0.008(2) -0.003(2) -0.004(2) C(20) 0.019(3) 0.028(3) 0.035(4) -0.006(2) -0.008(3) -0.001(3) C(21) 0.020(3) 0.026(3) 0.044(4) -0.015(2) -0.004(3) -0.009(3) C(22) 0.019(3) 0.025(3) 0.049(4) -0.011(2) -0.005(3) 0.001(3) C(23) 0.008(3) 0.025(3) 0.048(4) -0.007(2) -0.007(2) 0.005(3) C(24) 0.011(3) 0.022(2) 0.029(3) -0.007(2) -0.003(2) -0.002(2) C(25) 0.018(3) 0.036(3) 0.025(3) -0.006(2) -0.003(2) -0.001(3) C(26) 0.037(4) 0.036(3) 0.038(4) 0.000(3) -0.002(3) -0.012(3) C(27) 0.041(5) 0.069(5) 0.033(5) 0.016(4) -0.010(4) -0.019(4) C(28) 0.029(4) 0.125(8) 0.023(4) -0.004(5) -0.003(3) 0.000(5) C(29) 0.050(5) 0.118(8) 0.037(5) -0.047(5) 0.004(4) 0.006(5) C(30) 0.035(4) 0.061(4) 0.037(4) -0.029(3) -0.001(3) 0.003(3) C(31) 0.025(3) 0.018(3) 0.037(4) -0.007(2) 0.005(3) 0.005(2) C(32) 0.034(4) 0.026(3) 0.052(5) -0.005(3) 0.002(3) -0.002(3) C(33) 0.040(4) 0.039(4) 0.054(5) -0.005(3) -0.006(4) 0.014(3) C(34) 0.024(4) 0.027(3) 0.077(6) 0.002(3) 0.003(4) 0.015(3) C(35) 0.029(4) 0.034(3) 0.065(6) -0.001(3) 0.017(4) -0.004(3) C(36) 0.029(4) 0.036(3) 0.042(4) -0.008(3) 0.008(3) -0.005(3) C(37) 0.012(3) 0.027(3) 0.033(4) -0.005(2) -0.001(2) -0.010(2) C(38) 0.021(3) 0.048(4) 0.028(4) -0.009(3) -0.005(3) -0.014(3) C(39) 0.024(3) 0.056(4) 0.029(4) -0.010(3) 0.001(3) -0.020(3) C(40) 0.022(3) 0.054(4) 0.049(5) -0.013(3) -0.003(3) -0.031(4) C(41) 0.014(3) 0.034(3) 0.049(4) -0.008(2) 0.000(3) -0.023(3) C(42) 0.010(3) 0.035(3) 0.032(4) -0.005(2) -0.003(2) -0.011(3) C(43) 0.015(3) 0.026(3) 0.039(4) -0.004(2) -0.003(3) -0.005(3) C(44) 0.021(3) 0.047(4) 0.049(4) -0.014(3) 0.001(3) -0.017(3) C(45) 0.024(4) 0.069(5) 0.056(5) -0.024(3) 0.009(3) -0.016(4) C(46) 0.030(4) 0.046(4) 0.085(6) -0.023(3) -0.003(4) 0.006(4) C(47) 0.027(4) 0.033(3) 0.081(6) -0.010(3) -0.008(4) -0.014(3) C(48) 0.021(3) 0.029(3) 0.053(4) -0.008(3) 0.000(3) -0.014(3) C(49) 0.016(3) 0.023(3) 0.031(4) -0.004(2) -0.003(2) -0.011(2) C(50) 0.025(3) 0.037(3) 0.031(4) -0.001(3) 0.002(3) -0.006(3) C(51) 0.043(4) 0.042(4) 0.024(4) -0.004(3) -0.002(3) 0.002(3) C(52) 0.028(4) 0.035(3) 0.046(5) 0.002(3) -0.010(3) -0.013(3) C(53) 0.025(3) 0.031(3) 0.040(4) -0.004(3) 0.000(3) -0.011(3) C(54) 0.024(3) 0.028(3) 0.037(4) -0.005(2) 0.003(3) -0.010(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 9328 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_all 0.1135 _refine_ls_wR_factor_ref 0.1135 _refine_ls_goodness_of_fit_all 1.130 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_shift/su_max 0.0015 _refine_ls_shift/su_mean 0.0009 _refine_diff_density_min -1.35 _refine_diff_density_max 2.21 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 In(1) In(2) 3.2230(5) . . yes In(1) Cl(1) 2.384(2) . . yes In(1) P(1) 2.652(2) . . yes In(1) P(2) 2.733(2) . . yes In(1) O(1) 2.243(4) . . yes In(1) O(2) 2.193(3) . . yes In(1) O(3) 2.197(4) . . yes In(2) Cl(2) 2.381(1) . . yes In(2) Cl(3) 2.421(1) . . yes In(2) P(3) 2.663(2) . . yes In(2) O(1) 2.185(4) . . yes In(2) O(2) 2.287(3) . . yes In(2) O(3) 2.252(3) . . yes P(1) C(1) 1.800(5) . . yes P(1) C(7) 1.815(5) . . yes P(1) C(13) 1.816(6) . . yes P(2) C(19) 1.801(5) . . yes P(2) C(25) 1.816(6) . . yes P(2) C(31) 1.807(6) . . yes P(3) C(37) 1.799(5) . . yes P(3) C(43) 1.824(6) . . yes P(3) C(49) 1.822(5) . . yes O(1) C(6) 1.350(6) . . yes O(2) C(24) 1.359(6) . . yes O(3) C(42) 1.329(7) . . yes C(1) C(2) 1.404(7) . . yes C(1) C(6) 1.405(7) . . yes C(2) C(3) 1.373(8) . . yes C(2) H(1) 0.98 . . no C(3) C(4) 1.386(8) . . yes C(3) H(2) 0.98 . . no C(4) C(5) 1.374(8) . . yes C(4) H(3) 0.98 . . no C(5) C(6) 1.398(7) . . yes C(5) H(4) 0.98 . . no C(7) C(8) 1.378(8) . . yes C(7) C(12) 1.371(8) . . yes C(8) C(9) 1.382(8) . . yes C(8) H(5) 0.98 . . no C(9) C(10) 1.38(1) . . yes C(9) H(6) 0.98 . . no C(10) C(11) 1.33(1) . . yes C(10) H(7) 0.98 . . no C(11) C(12) 1.412(9) . . yes C(11) H(8) 0.99 . . no C(12) H(9) 0.98 . . no C(13) C(14) 1.372(8) . . yes C(13) C(18) 1.387(7) . . yes C(14) C(15) 1.382(9) . . yes C(14) H(10) 0.98 . . no C(15) C(16) 1.373(9) . . yes C(15) H(11) 0.98 . . no C(16) C(17) 1.372(9) . . yes C(16) H(12) 0.98 . . no C(17) C(18) 1.387(8) . . yes C(17) H(13) 0.98 . . no C(18) H(14) 0.98 . . no C(19) C(20) 1.402(7) . . yes C(19) C(24) 1.395(7) . . yes C(20) C(21) 1.376(7) . . yes C(20) H(15) 0.98 . . no C(21) C(22) 1.397(8) . . yes C(21) H(16) 0.98 . . no C(22) C(23) 1.375(7) . . yes C(22) H(17) 0.98 . . no C(23) C(24) 1.400(7) . . yes C(23) H(18) 0.98 . . no C(25) C(26) 1.372(8) . . yes C(25) C(30) 1.398(8) . . yes C(26) C(27) 1.42(1) . . yes C(26) H(19) 0.98 . . no C(27) C(28) 1.36(1) . . yes C(27) H(20) 0.98 . . no C(28) C(29) 1.36(1) . . yes C(28) H(21) 0.98 . . no C(29) C(30) 1.37(1) . . yes C(29) H(22) 0.98 . . no C(30) H(23) 0.98 . . no C(31) C(32) 1.387(9) . . yes C(31) C(36) 1.389(8) . . yes C(32) C(33) 1.392(9) . . yes C(32) H(24) 0.98 . . no C(33) C(34) 1.39(1) . . yes C(33) H(25) 0.98 . . no C(34) C(35) 1.35(1) . . yes C(34) H(26) 0.98 . . no C(35) C(36) 1.406(9) . . yes C(35) H(27) 0.98 . . no C(36) H(28) 0.98 . . no C(37) C(38) 1.412(8) . . yes C(37) C(42) 1.417(8) . . yes C(38) C(39) 1.381(8) . . yes C(38) H(29) 0.98 . . no C(39) C(40) 1.38(1) . . yes C(39) H(30) 0.99 . . no C(40) C(41) 1.381(9) . . yes C(40) H(31) 0.98 . . no C(41) C(42) 1.424(7) . . yes C(41) H(32) 0.98 . . no C(43) C(44) 1.377(8) . . yes C(43) C(48) 1.389(8) . . yes C(44) C(45) 1.397(9) . . yes C(44) H(33) 0.98 . . no C(45) C(46) 1.37(1) . . yes C(45) H(34) 0.98 . . no C(46) C(47) 1.38(1) . . yes C(46) H(35) 0.98 . . no C(47) C(48) 1.380(9) . . yes C(47) H(36) 0.98 . . no C(48) H(37) 0.98 . . no C(49) C(50) 1.387(9) . . yes C(49) C(54) 1.393(8) . . yes C(50) C(51) 1.395(8) . . yes C(50) H(38) 0.99 . . no C(51) C(52) 1.377(9) . . yes C(51) H(39) 0.98 . . no C(52) C(53) 1.375(9) . . yes C(52) H(40) 0.98 . . no C(53) C(54) 1.390(8) . . yes C(53) H(41) 0.98 . . no C(54) H(42) 0.98 . . no #------------------------------------------------------------------------------ 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 In(2) In(1) Cl(1) 134.17(5) . . . yes In(2) In(1) P(1) 105.09(3) . . . yes In(2) In(1) P(2) 100.67(3) . . . yes In(2) In(1) O(1) 42.58(9) . . . yes In(2) In(1) O(2) 45.17(9) . . . yes In(2) In(1) O(3) 44.27(9) . . . yes Cl(1) In(1) P(1) 106.86(5) . . . yes Cl(1) In(1) P(2) 100.60(5) . . . yes Cl(1) In(1) O(1) 176.8(1) . . . yes Cl(1) In(1) O(2) 104.0(1) . . . yes Cl(1) In(1) O(3) 102.4(1) . . . yes P(1) In(1) P(2) 106.72(5) . . . yes P(1) In(1) O(1) 75.31(9) . . . yes P(1) In(1) O(2) 148.1(1) . . . yes P(1) In(1) O(3) 92.3(1) . . . yes P(2) In(1) O(1) 80.9(1) . . . yes P(2) In(1) O(2) 74.8(1) . . . yes P(2) In(1) O(3) 144.23(9) . . . yes O(1) In(1) O(2) 73.5(1) . . . yes O(1) In(1) O(3) 75.0(1) . . . yes O(2) In(1) O(3) 73.3(1) . . . yes In(1) In(2) Cl(2) 124.83(5) . . . yes In(1) In(2) Cl(3) 116.45(4) . . . yes In(1) In(2) P(3) 106.49(3) . . . yes In(1) In(2) O(1) 44.01(9) . . . yes In(1) In(2) O(2) 42.83(8) . . . yes In(1) In(2) O(3) 42.90(9) . . . yes Cl(2) In(2) Cl(3) 102.55(6) . . . yes Cl(2) In(2) P(3) 105.02(5) . . . yes Cl(2) In(2) O(1) 101.2(1) . . . yes Cl(2) In(2) O(2) 94.18(9) . . . yes Cl(2) In(2) O(3) 164.7(1) . . . yes Cl(3) In(2) P(3) 97.74(5) . . . yes Cl(3) In(2) O(1) 91.8(1) . . . yes Cl(3) In(2) O(2) 159.24(9) . . . yes Cl(3) In(2) O(3) 92.5(1) . . . yes P(3) In(2) O(1) 149.3(1) . . . yes P(3) In(2) O(2) 89.6(1) . . . yes P(3) In(2) O(3) 75.5(1) . . . yes O(1) In(2) O(2) 72.8(1) . . . yes O(1) In(2) O(3) 75.0(1) . . . yes O(2) In(2) O(3) 70.5(1) . . . yes In(1) P(1) C(1) 98.4(2) . . . yes In(1) P(1) C(7) 113.3(2) . . . yes In(1) P(1) C(13) 123.1(2) . . . yes C(1) P(1) C(7) 110.0(3) . . . yes C(1) P(1) C(13) 104.1(2) . . . yes C(7) P(1) C(13) 106.8(3) . . . yes In(1) P(2) C(19) 95.3(2) . . . yes In(1) P(2) C(25) 112.3(2) . . . yes In(1) P(2) C(31) 128.4(2) . . . yes C(19) P(2) C(25) 107.8(3) . . . yes C(19) P(2) C(31) 105.9(2) . . . yes C(25) P(2) C(31) 105.1(3) . . . yes In(2) P(3) C(37) 99.1(2) . . . yes In(2) P(3) C(43) 117.7(2) . . . yes In(2) P(3) C(49) 119.9(2) . . . yes C(37) P(3) C(43) 107.9(3) . . . yes C(37) P(3) C(49) 109.0(2) . . . yes C(43) P(3) C(49) 102.7(3) . . . yes In(1) O(1) In(2) 93.4(1) . . . yes In(1) O(1) C(6) 124.0(3) . . . yes In(2) O(1) C(6) 131.1(3) . . . yes In(1) O(2) In(2) 92.0(1) . . . yes In(1) O(2) C(24) 123.2(3) . . . yes In(2) O(2) C(24) 131.9(3) . . . yes In(1) O(3) In(2) 92.8(1) . . . yes In(1) O(3) C(42) 125.8(3) . . . yes In(2) O(3) C(42) 124.1(3) . . . yes P(1) C(1) C(2) 121.8(4) . . . yes P(1) C(1) C(6) 118.8(4) . . . yes C(2) C(1) C(6) 119.3(5) . . . yes C(1) C(2) C(3) 120.7(5) . . . yes C(1) C(2) H(1) 119.9 . . . no C(3) C(2) H(1) 119.4 . . . no C(2) C(3) C(4) 119.7(5) . . . yes C(2) C(3) H(2) 120.3 . . . no C(4) C(3) H(2) 120.0 . . . no C(3) C(4) C(5) 120.8(5) . . . yes C(3) C(4) H(3) 119.5 . . . no C(5) C(4) H(3) 119.7 . . . no C(4) C(5) C(6) 120.5(5) . . . yes C(4) C(5) H(4) 119.3 . . . no C(6) C(5) H(4) 120.2 . . . no O(1) C(6) C(1) 121.4(5) . . . yes O(1) C(6) C(5) 119.6(4) . . . yes C(1) C(6) C(5) 118.9(5) . . . yes P(1) C(7) C(8) 118.4(4) . . . yes P(1) C(7) C(12) 122.7(5) . . . yes C(8) C(7) C(12) 118.8(5) . . . yes C(7) C(8) C(9) 120.7(6) . . . yes C(7) C(8) H(5) 119.5 . . . no C(9) C(8) H(5) 119.8 . . . no C(8) C(9) C(10) 119.4(6) . . . yes C(8) C(9) H(6) 120.3 . . . no C(10) C(9) H(6) 120.2 . . . no C(9) C(10) C(11) 121.0(6) . . . yes C(9) C(10) H(7) 120.1 . . . no C(11) C(10) H(7) 118.9 . . . no C(10) C(11) C(12) 119.8(7) . . . yes C(10) C(11) H(8) 120.7 . . . no C(12) C(11) H(8) 119.5 . . . no C(7) C(12) C(11) 120.2(6) . . . yes C(7) C(12) H(9) 120.0 . . . no C(11) C(12) H(9) 119.8 . . . no P(1) C(13) C(14) 122.7(4) . . . yes P(1) C(13) C(18) 118.9(4) . . . yes C(14) C(13) C(18) 118.3(5) . . . yes C(13) C(14) C(15) 121.1(6) . . . yes C(13) C(14) H(10) 119.2 . . . no C(15) C(14) H(10) 119.7 . . . no C(14) C(15) C(16) 120.0(6) . . . yes C(14) C(15) H(11) 120.2 . . . no C(16) C(15) H(11) 119.8 . . . no C(15) C(16) C(17) 120.1(6) . . . yes C(15) C(16) H(12) 119.7 . . . no C(17) C(16) H(12) 120.2 . . . no C(16) C(17) C(18) 119.6(6) . . . yes C(16) C(17) H(13) 120.1 . . . no C(18) C(17) H(13) 120.3 . . . no C(13) C(18) C(17) 120.9(5) . . . yes C(13) C(18) H(14) 119.6 . . . no C(17) C(18) H(14) 119.5 . . . no P(2) C(19) C(20) 121.1(4) . . . yes P(2) C(19) C(24) 119.1(4) . . . yes C(20) C(19) C(24) 119.8(5) . . . yes C(19) C(20) C(21) 120.5(5) . . . yes C(19) C(20) H(15) 120.1 . . . no C(21) C(20) H(15) 119.3 . . . no C(20) C(21) C(22) 119.7(5) . . . yes C(20) C(21) H(16) 120.4 . . . no C(22) C(21) H(16) 119.9 . . . no C(21) C(22) C(23) 120.1(5) . . . yes C(21) C(22) H(17) 119.2 . . . no C(23) C(22) H(17) 120.6 . . . no C(22) C(23) C(24) 120.9(5) . . . yes C(22) C(23) H(18) 119.7 . . . no C(24) C(23) H(18) 119.4 . . . no O(2) C(24) C(19) 122.0(4) . . . yes O(2) C(24) C(23) 119.0(5) . . . yes C(19) C(24) C(23) 118.9(5) . . . yes P(2) C(25) C(26) 121.7(5) . . . yes P(2) C(25) C(30) 117.4(4) . . . yes C(26) C(25) C(30) 120.9(6) . . . yes C(25) C(26) C(27) 117.8(7) . . . yes C(25) C(26) H(19) 121.3 . . . no C(27) C(26) H(19) 120.9 . . . no C(26) C(27) C(28) 121.1(7) . . . yes C(26) C(27) H(20) 119.6 . . . no C(28) C(27) H(20) 119.2 . . . no C(27) C(28) C(29) 119.9(7) . . . yes C(27) C(28) H(21) 120.9 . . . no C(29) C(28) H(21) 119.2 . . . no C(28) C(29) C(30) 121.0(8) . . . yes C(28) C(29) H(22) 119.9 . . . no C(30) C(29) H(22) 119.1 . . . no C(25) C(30) C(29) 119.3(7) . . . yes C(25) C(30) H(23) 120.5 . . . no C(29) C(30) H(23) 120.2 . . . no P(2) C(31) C(32) 121.1(5) . . . yes P(2) C(31) C(36) 119.4(5) . . . yes C(32) C(31) C(36) 119.5(6) . . . yes C(31) C(32) C(33) 121.0(6) . . . yes C(31) C(32) H(24) 119.1 . . . no C(33) C(32) H(24) 119.9 . . . no C(32) C(33) C(34) 118.6(7) . . . yes C(32) C(33) H(25) 120.9 . . . no C(34) C(33) H(25) 120.5 . . . no C(33) C(34) C(35) 120.9(6) . . . yes C(33) C(34) H(26) 119.3 . . . no C(35) C(34) H(26) 119.7 . . . no C(34) C(35) C(36) 121.0(6) . . . yes C(34) C(35) H(27) 118.7 . . . no C(36) C(35) H(27) 120.2 . . . no C(31) C(36) C(35) 118.9(6) . . . yes C(31) C(36) H(28) 120.4 . . . no C(35) C(36) H(28) 120.7 . . . no P(3) C(37) C(38) 122.2(4) . . . yes P(3) C(37) C(42) 117.8(4) . . . yes C(38) C(37) C(42) 120.1(5) . . . yes C(37) C(38) C(39) 120.9(6) . . . yes C(37) C(38) H(29) 119.0 . . . no C(39) C(38) H(29) 120.1 . . . no C(38) C(39) C(40) 119.0(6) . . . yes C(38) C(39) H(30) 120.4 . . . no C(40) C(39) H(30) 120.7 . . . no C(39) C(40) C(41) 122.2(5) . . . yes C(39) C(40) H(31) 119.2 . . . no C(41) C(40) H(31) 118.6 . . . no C(40) C(41) C(42) 120.0(6) . . . yes C(40) C(41) H(32) 119.9 . . . no C(42) C(41) H(32) 120.1 . . . no O(3) C(42) C(37) 123.5(5) . . . yes O(3) C(42) C(41) 118.7(5) . . . yes C(37) C(42) C(41) 117.8(6) . . . yes P(3) C(43) C(44) 123.8(4) . . . yes P(3) C(43) C(48) 116.7(4) . . . yes C(44) C(43) C(48) 119.5(5) . . . yes C(43) C(44) C(45) 120.2(6) . . . yes C(43) C(44) H(33) 120.3 . . . no C(45) C(44) H(33) 119.5 . . . no C(44) C(45) C(46) 119.7(6) . . . yes C(44) C(45) H(34) 120.5 . . . no C(46) C(45) H(34) 119.8 . . . no C(45) C(46) C(47) 120.2(6) . . . yes C(45) C(46) H(35) 120.1 . . . no C(47) C(46) H(35) 119.7 . . . no C(46) C(47) C(48) 120.3(6) . . . yes C(46) C(47) H(36) 119.9 . . . no C(48) C(47) H(36) 119.7 . . . no C(43) C(48) C(47) 119.9(6) . . . yes C(43) C(48) H(37) 120.2 . . . no C(47) C(48) H(37) 119.9 . . . no P(3) C(49) C(50) 121.1(4) . . . yes P(3) C(49) C(54) 120.3(5) . . . yes C(50) C(49) C(54) 118.6(5) . . . yes C(49) C(50) C(51) 120.7(6) . . . yes C(49) C(50) H(38) 119.4 . . . no C(51) C(50) H(38) 119.9 . . . no C(50) C(51) C(52) 119.8(6) . . . yes C(50) C(51) H(39) 120.7 . . . no C(52) C(51) H(39) 119.5 . . . no C(51) C(52) C(53) 120.3(6) . . . yes C(51) C(52) H(40) 120.4 . . . no C(53) C(52) H(40) 119.2 . . . no C(52) C(53) C(54) 120.0(6) . . . yes C(52) C(53) H(41) 120.1 . . . no C(54) C(53) H(41) 119.9 . . . no C(49) C(54) C(53) 120.6(6) . . . yes C(49) C(54) H(42) 120.0 . . . no C(53) C(54) H(42) 119.4 . . . no #------------------------------------------------------------------------------ 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 Cl(1) C(52) 3.563(6) . 1_645 no Cl(3) C(21) 3.502(5) . 1_455 no Cl(3) C(22) 3.507(5) . 1_455 no C(4) C(27) 3.507(9) . 2_576 no C(9) C(28) 3.52(1) . 2_666 no C(10) C(28) 3.49(1) . 2_666 no C(15) C(51) 3.554(9) . 2_575 no C(17) C(21) 3.589(8) . 1_455 no C(18) C(21) 3.476(8) . 1_455 no C(29) C(33) 3.59(1) . 2_666 no C(37) C(40) 3.537(8) . 2_575 no C(38) C(40) 3.378(8) . 2_575 no C(38) C(41) 3.498(8) . 2_575 no C(39) C(42) 3.540(8) . 2_575 no C(39) C(41) 3.577(8) . 2_575 no #------------------------------------------------------------------------------ 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 In(1) In(2) P(3) C(37) . . . . 32.8(2) no In(1) In(2) P(3) C(43) . . . . -83.0(2) no In(1) In(2) P(3) C(49) . . . . 151.0(2) no In(1) In(2) O(1) C(6) . . . . -142.7(5) no In(1) In(2) O(2) C(24) . . . . -140.2(5) no In(1) In(2) O(3) C(42) . . . . -137.7(4) no In(1) P(1) C(1) C(2) . . . . -171.6(4) no In(1) P(1) C(1) C(6) . . . . 9.2(4) no In(1) P(1) C(7) C(8) . . . . -11.3(6) no In(1) P(1) C(7) C(12) . . . . 169.5(5) no In(1) P(1) C(13) C(14) . . . . 116.1(5) no In(1) P(1) C(13) C(18) . . . . -67.8(5) no In(1) P(2) C(19) C(20) . . . . -164.8(4) no In(1) P(2) C(19) C(24) . . . . 13.9(4) no In(1) P(2) C(25) C(26) . . . . -97.2(5) no In(1) P(2) C(25) C(30) . . . . 80.5(5) no In(1) P(2) C(31) C(32) . . . . -162.0(4) no In(1) P(2) C(31) C(36) . . . . 19.2(6) no In(1) O(1) In(2) Cl(2) . . . . -129.29(9) no In(1) O(1) In(2) Cl(3) . . . . 127.5(1) no In(1) O(1) In(2) P(3) . . . . 19.1(2) no In(1) O(1) In(2) O(2) . . . . -38.3(1) no In(1) O(1) In(2) O(3) . . . . 35.5(1) no In(1) O(1) C(6) C(1) . . . . -12.2(7) no In(1) O(1) C(6) C(5) . . . . 168.0(4) no In(1) O(2) In(2) Cl(2) . . . . 139.8(1) no In(1) O(2) In(2) Cl(3) . . . . -4.1(4) no In(1) O(2) In(2) P(3) . . . . -115.2(1) no In(1) O(2) In(2) O(1) . . . . 39.3(1) no In(1) O(2) In(2) O(3) . . . . -40.4(1) no In(1) O(2) C(24) C(19) . . . . -21.8(7) no In(1) O(2) C(24) C(23) . . . . 156.7(4) no In(1) O(3) In(2) Cl(2) . . . . 41.1(5) no In(1) O(3) In(2) Cl(3) . . . . -127.5(1) no In(1) O(3) In(2) P(3) . . . . 135.1(1) no In(1) O(3) In(2) O(1) . . . . -36.3(1) no In(1) O(3) In(2) O(2) . . . . 40.4(1) no In(1) O(3) C(42) C(37) . . . . -122.9(5) no In(1) O(3) C(42) C(41) . . . . 59.6(6) no In(2) In(1) P(1) C(1) . . . . -40.8(2) no In(2) In(1) P(1) C(7) . . . . -156.8(2) no In(2) In(1) P(1) C(13) . . . . 72.2(2) no In(2) In(1) P(2) C(19) . . . . -53.5(2) no In(2) In(1) P(2) C(25) . . . . 58.2(2) no In(2) In(1) P(2) C(31) . . . . -168.7(2) no In(2) In(1) O(1) C(6) . . . . 146.6(4) no In(2) In(1) O(2) C(24) . . . . 145.3(4) no In(2) In(1) O(3) C(42) . . . . 136.7(4) no In(2) P(3) C(37) C(38) . . . . 175.8(4) no In(2) P(3) C(37) C(42) . . . . -3.4(4) no In(2) P(3) C(43) C(44) . . . . 108.2(5) no In(2) P(3) C(43) C(48) . . . . -69.0(5) no In(2) P(3) C(49) C(50) . . . . 175.8(4) no In(2) P(3) C(49) C(54) . . . . -4.5(5) no In(2) O(1) In(1) Cl(1) . . . . -1(2) no In(2) O(1) In(1) P(1) . . . . -133.1(1) no In(2) O(1) In(1) P(2) . . . . 116.8(1) no In(2) O(1) In(1) O(2) . . . . 40.1(1) no In(2) O(1) In(1) O(3) . . . . -36.5(1) no In(2) O(1) C(6) C(1) . . . . 120.9(5) no In(2) O(1) C(6) C(5) . . . . -58.9(7) no In(2) O(2) In(1) Cl(1) . . . . 139.85(9) no In(2) O(2) In(1) P(1) . . . . -25.5(3) no In(2) O(2) In(1) P(2) . . . . -122.8(1) no In(2) O(2) In(1) O(1) . . . . -38.0(1) no In(2) O(2) In(1) O(3) . . . . 40.9(1) no In(2) O(2) C(24) C(19) . . . . 108.3(5) no In(2) O(2) C(24) C(23) . . . . -73.2(6) no In(2) O(3) In(1) Cl(1) . . . . -142.8(1) no In(2) O(3) In(1) P(1) . . . . 109.4(1) no In(2) O(3) In(1) P(2) . . . . -14.0(2) no In(2) O(3) In(1) O(1) . . . . 35.2(1) no In(2) O(3) In(1) O(2) . . . . -41.7(1) no In(2) O(3) C(42) C(37) . . . . 1.2(7) no In(2) O(3) C(42) C(41) . . . . -176.2(3) no Cl(1) In(1) In(2) Cl(2) . . . . -112.40(8) no Cl(1) In(1) In(2) Cl(3) . . . . 117.67(8) no Cl(1) In(1) In(2) P(3) . . . . 9.96(7) no Cl(1) In(1) In(2) O(1) . . . . 179.9(1) no Cl(1) In(1) In(2) O(2) . . . . -60.7(2) no Cl(1) In(1) In(2) O(3) . . . . 55.4(2) no Cl(1) In(1) P(1) C(1) . . . . 172.5(2) no Cl(1) In(1) P(1) C(7) . . . . 56.5(2) no Cl(1) In(1) P(1) C(13) . . . . -74.5(2) no Cl(1) In(1) P(2) C(19) . . . . 85.7(2) no Cl(1) In(1) P(2) C(25) . . . . -162.6(2) no Cl(1) In(1) P(2) C(31) . . . . -29.5(2) no Cl(1) In(1) O(1) C(6) . . . . 146(2) no Cl(1) In(1) O(2) C(24) . . . . -74.8(4) no Cl(1) In(1) O(3) C(42) . . . . -6.2(4) no Cl(2) In(2) In(1) P(1) . . . . 114.70(6) no Cl(2) In(2) In(1) P(2) . . . . 3.96(6) no Cl(2) In(2) In(1) O(1) . . . . 67.7(1) no Cl(2) In(2) In(1) O(2) . . . . -51.7(2) no Cl(2) In(2) In(1) O(3) . . . . -167.8(1) no Cl(2) In(2) P(3) C(37) . . . . 166.9(2) no Cl(2) In(2) P(3) C(43) . . . . 51.2(2) no Cl(2) In(2) P(3) C(49) . . . . -74.9(2) no Cl(2) In(2) O(1) C(6) . . . . 88.1(4) no Cl(2) In(2) O(2) C(24) . . . . -0.4(4) no Cl(2) In(2) O(3) C(42) . . . . -96.6(5) no Cl(3) In(2) In(1) P(1) . . . . -15.23(6) no Cl(3) In(2) In(1) P(2) . . . . -125.96(6) no Cl(3) In(2) In(1) O(1) . . . . -62.3(1) no Cl(3) In(2) In(1) O(2) . . . . 178.4(2) no Cl(3) In(2) In(1) O(3) . . . . 62.3(1) no Cl(3) In(2) P(3) C(37) . . . . -87.8(2) no Cl(3) In(2) P(3) C(43) . . . . 156.4(2) no Cl(3) In(2) P(3) C(49) . . . . 30.4(2) no Cl(3) In(2) O(1) C(6) . . . . -15.1(4) no Cl(3) In(2) O(2) C(24) . . . . -144.3(4) no Cl(3) In(2) O(3) C(42) . . . . 94.8(4) no P(1) In(1) In(2) P(3) . . . . -122.94(5) no P(1) In(1) In(2) O(1) . . . . 47.0(1) no P(1) In(1) In(2) O(2) . . . . 166.4(1) no P(1) In(1) In(2) O(3) . . . . -77.5(1) no P(1) In(1) P(2) C(19) . . . . -163.0(2) no P(1) In(1) P(2) C(25) . . . . -51.2(2) no P(1) In(1) P(2) C(31) . . . . 81.9(2) no P(1) In(1) O(1) C(6) . . . . 13.5(3) no P(1) In(1) O(2) C(24) . . . . 119.9(3) no P(1) In(1) O(3) C(42) . . . . -114.0(4) no P(1) C(1) C(2) C(3) . . . . 179.1(5) no P(1) C(1) C(6) O(1) . . . . -0.5(7) no P(1) C(1) C(6) C(5) . . . . 179.3(4) no P(1) C(7) C(8) C(9) . . . . 180.0(6) no P(1) C(7) C(12) C(11) . . . . -178.5(6) no P(1) C(13) C(14) C(15) . . . . 174.8(5) no P(1) C(13) C(18) C(17) . . . . -175.6(5) no P(2) In(1) In(2) P(3) . . . . 126.32(5) no P(2) In(1) In(2) O(1) . . . . -63.7(1) no P(2) In(1) In(2) O(2) . . . . 55.7(1) no P(2) In(1) In(2) O(3) . . . . 171.8(1) no P(2) In(1) P(1) C(1) . . . . 65.6(2) no P(2) In(1) P(1) C(7) . . . . -50.5(2) no P(2) In(1) P(1) C(13) . . . . 178.5(2) no P(2) In(1) O(1) C(6) . . . . -96.6(4) no P(2) In(1) O(2) C(24) . . . . 22.6(4) no P(2) In(1) O(3) C(42) . . . . 122.7(4) no P(2) C(19) C(20) C(21) . . . . 178.6(4) no P(2) C(19) C(24) O(2) . . . . 0.5(7) no P(2) C(19) C(24) C(23) . . . . -178.0(4) no P(2) C(25) C(26) C(27) . . . . 177.8(5) no P(2) C(25) C(30) C(29) . . . . -178.0(5) no P(2) C(31) C(32) C(33) . . . . -178.3(5) no P(2) C(31) C(36) C(35) . . . . 178.6(5) no P(3) In(2) In(1) O(1) . . . . -170.0(1) no P(3) In(2) In(1) O(2) . . . . 70.7(1) no P(3) In(2) In(1) O(3) . . . . -45.4(1) no P(3) In(2) O(1) C(6) . . . . -123.5(4) no P(3) In(2) O(2) C(24) . . . . 104.6(4) no P(3) In(2) O(3) C(42) . . . . -2.6(3) no P(3) C(37) C(38) C(39) . . . . 179.0(4) no P(3) C(37) C(42) O(3) . . . . 2.1(7) no P(3) C(37) C(42) C(41) . . . . 179.6(4) no P(3) C(43) C(44) C(45) . . . . -178.6(5) no P(3) C(43) C(48) C(47) . . . . 178.6(5) no P(3) C(49) C(50) C(51) . . . . 178.0(5) no P(3) C(49) C(54) C(53) . . . . -177.3(4) no O(1) In(1) In(2) O(2) . . . . 119.4(2) no O(1) In(1) In(2) O(3) . . . . -124.5(2) no O(1) In(1) P(1) C(1) . . . . -10.0(2) no O(1) In(1) P(1) C(7) . . . . -126.0(2) no O(1) In(1) P(1) C(13) . . . . 103.0(2) no O(1) In(1) P(2) C(19) . . . . -91.4(2) no O(1) In(1) P(2) C(25) . . . . 20.3(2) no O(1) In(1) P(2) C(31) . . . . 153.4(2) no O(1) In(1) O(2) C(24) . . . . 107.4(4) no O(1) In(1) O(3) C(42) . . . . 171.9(4) no O(1) In(2) In(1) O(2) . . . . -119.4(2) no O(1) In(2) In(1) O(3) . . . . 124.5(2) no O(1) In(2) P(3) C(37) . . . . 19.1(3) no O(1) In(2) P(3) C(43) . . . . -96.7(3) no O(1) In(2) P(3) C(49) . . . . 137.3(3) no O(1) In(2) O(2) C(24) . . . . -100.9(4) no O(1) In(2) O(3) C(42) . . . . -174.1(4) no O(1) C(6) C(1) C(2) . . . . -179.7(5) no O(1) C(6) C(5) C(4) . . . . -177.8(5) no O(2) In(1) In(2) O(3) . . . . 116.1(2) no O(2) In(1) P(1) C(1) . . . . -22.4(3) no O(2) In(1) P(1) C(7) . . . . -138.4(3) no O(2) In(1) P(1) C(13) . . . . 90.6(3) no O(2) In(1) P(2) C(19) . . . . -16.2(2) no O(2) In(1) P(2) C(25) . . . . 95.6(2) no O(2) In(1) P(2) C(31) . . . . -131.3(3) no O(2) In(1) O(1) C(6) . . . . -173.3(4) no O(2) In(1) O(3) C(42) . . . . 95.0(4) no O(2) In(2) In(1) O(3) . . . . -116.1(2) no O(2) In(2) P(3) C(37) . . . . 72.7(2) no O(2) In(2) P(3) C(43) . . . . -43.1(2) no O(2) In(2) P(3) C(49) . . . . -169.1(2) no O(2) In(2) O(1) C(6) . . . . 179.0(4) no O(2) In(2) O(3) C(42) . . . . -97.4(4) no O(2) C(24) C(19) C(20) . . . . 179.2(5) no O(2) C(24) C(23) C(22) . . . . -179.1(5) no O(3) In(1) P(1) C(1) . . . . -83.8(2) no O(3) In(1) P(1) C(7) . . . . 160.2(2) no O(3) In(1) P(1) C(13) . . . . 29.2(2) no O(3) In(1) P(2) C(19) . . . . -43.6(3) no O(3) In(1) P(2) C(25) . . . . 68.1(3) no O(3) In(1) P(2) C(31) . . . . -158.8(3) no O(3) In(1) O(1) C(6) . . . . 110.0(4) no O(3) In(1) O(2) C(24) . . . . -173.8(4) no O(3) In(2) P(3) C(37) . . . . 2.7(2) no O(3) In(2) P(3) C(43) . . . . -113.0(2) no O(3) In(2) P(3) C(49) . . . . 120.9(2) no O(3) In(2) O(1) C(6) . . . . -107.2(4) no O(3) In(2) O(2) C(24) . . . . 179.4(5) no O(3) C(42) C(37) C(38) . . . . -177.2(5) no O(3) C(42) C(41) C(40) . . . . 178.8(5) no C(1) P(1) C(7) C(8) . . . . -120.4(5) no C(1) P(1) C(7) C(12) . . . . 60.4(6) no C(1) P(1) C(13) C(14) . . . . -133.8(5) no C(1) P(1) C(13) C(18) . . . . 42.4(5) no C(1) C(2) C(3) C(4) . . . . 0.8(9) no C(1) C(6) C(5) C(4) . . . . 2.4(8) no C(2) C(1) P(1) C(7) . . . . -53.0(5) no C(2) C(1) P(1) C(13) . . . . 61.0(5) no C(2) C(1) C(6) C(5) . . . . 0.1(8) no C(2) C(3) C(4) C(5) . . . . 1.8(9) no C(3) C(2) C(1) C(6) . . . . -1.7(8) no C(3) C(4) C(5) C(6) . . . . -3.4(9) no C(6) C(1) P(1) C(7) . . . . 127.9(4) no C(6) C(1) P(1) C(13) . . . . -118.1(4) no C(7) P(1) C(13) C(14) . . . . -17.5(6) no C(7) P(1) C(13) C(18) . . . . 158.7(5) no C(7) C(8) C(9) C(10) . . . . -1(1) no C(7) C(12) C(11) C(10) . . . . -3(1) no C(8) C(7) P(1) C(13) . . . . 127.3(5) no C(8) C(7) C(12) C(11) . . . . 2(1) no C(8) C(9) C(10) C(11) . . . . 0(1) no C(9) C(8) C(7) C(12) . . . . -1(1) no C(9) C(10) C(11) C(12) . . . . 1(1) no C(12) C(7) P(1) C(13) . . . . -51.9(6) no C(13) C(14) C(15) C(16) . . . . 1(1) no C(13) C(18) C(17) C(16) . . . . 0(1) no C(14) C(13) C(18) C(17) . . . . 0.7(9) no C(14) C(15) C(16) C(17) . . . . 0(1) no C(15) C(14) C(13) C(18) . . . . -1(1) no C(15) C(16) C(17) C(18) . . . . -1(1) no C(19) P(2) C(25) C(26) . . . . 6.5(6) no C(19) P(2) C(25) C(30) . . . . -175.8(5) no C(19) P(2) C(31) C(32) . . . . 87.5(5) no C(19) P(2) C(31) C(36) . . . . -91.3(5) no C(19) C(20) C(21) C(22) . . . . -0.7(9) no C(19) C(24) C(23) C(22) . . . . -0.6(9) no C(20) C(19) P(2) C(25) . . . . 79.8(5) no C(20) C(19) P(2) C(31) . . . . -32.3(5) no C(20) C(19) C(24) C(23) . . . . 0.7(8) no C(20) C(21) C(22) C(23) . . . . 0.8(9) no C(21) C(20) C(19) C(24) . . . . -0.1(8) no C(21) C(22) C(23) C(24) . . . . -0.2(9) no C(24) C(19) P(2) C(25) . . . . -101.6(5) no C(24) C(19) P(2) C(31) . . . . 146.4(4) no C(25) P(2) C(31) C(32) . . . . -26.4(6) no C(25) P(2) C(31) C(36) . . . . 154.8(5) no C(25) C(26) C(27) C(28) . . . . -1(1) no C(25) C(30) C(29) C(28) . . . . 1(1) no C(26) C(25) P(2) C(31) . . . . 119.1(5) no C(26) C(25) C(30) C(29) . . . . 0(1) no C(26) C(27) C(28) C(29) . . . . 2(1) no C(27) C(26) C(25) C(30) . . . . 0.2(9) no C(27) C(28) C(29) C(30) . . . . -2(1) no C(30) C(25) P(2) C(31) . . . . -63.2(5) no C(31) C(32) C(33) C(34) . . . . -1(1) no C(31) C(36) C(35) C(34) . . . . 0(1) no C(32) C(31) C(36) C(35) . . . . -0.3(9) no C(32) C(33) C(34) C(35) . . . . 1(1) no C(33) C(32) C(31) C(36) . . . . 0.5(9) no C(33) C(34) C(35) C(36) . . . . -1(1) no C(37) P(3) C(43) C(44) . . . . -2.6(6) no C(37) P(3) C(43) C(48) . . . . -179.9(5) no C(37) P(3) C(49) C(50) . . . . -71.2(5) no C(37) P(3) C(49) C(54) . . . . 108.5(5) no C(37) C(38) C(39) C(40) . . . . 1.6(9) no C(37) C(42) C(41) C(40) . . . . 1.2(8) no C(38) C(37) P(3) C(43) . . . . -61.1(5) no C(38) C(37) P(3) C(49) . . . . 49.8(5) no C(38) C(37) C(42) C(41) . . . . 0.3(8) no C(38) C(39) C(40) C(41) . . . . -0.1(9) no C(39) C(38) C(37) C(42) . . . . -1.7(8) no C(39) C(40) C(41) C(42) . . . . -1.3(9) no C(42) C(37) P(3) C(43) . . . . 119.7(4) no C(42) C(37) P(3) C(49) . . . . -129.5(4) no C(43) P(3) C(49) C(50) . . . . 43.0(5) no C(43) P(3) C(49) C(54) . . . . -137.3(4) no C(43) C(44) C(45) C(46) . . . . 0(1) no C(43) C(48) C(47) C(46) . . . . 1(1) no C(44) C(43) P(3) C(49) . . . . -117.7(6) no C(44) C(43) C(48) C(47) . . . . 1(1) no C(44) C(45) C(46) C(47) . . . . 2(1) no C(45) C(44) C(43) C(48) . . . . -1(1) no C(45) C(46) C(47) C(48) . . . . -2(1) no C(48) C(43) P(3) C(49) . . . . 65.0(5) no C(49) C(50) C(51) C(52) . . . . -1(1) no C(49) C(54) C(53) C(52) . . . . -0.7(9) no C(50) C(49) C(54) C(53) . . . . 2.5(8) no C(50) C(51) C(52) C(53) . . . . 3(1) no C(51) C(50) C(49) C(54) . . . . -1.7(9) no C(51) C(52) C(53) C(54) . . . . -1.9(9) no #------------------------------------------------------------------------------ data_co249/ks-iii-175 _database_code_depnum_ccdc_archive 'CCDC 262806' #------------------------------------------------------------------------------ _audit_creation_date 2004-11-23 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1996-1998). d*TREK. Area Detector Software. Version 4.4. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Burla, M.C., Cammalli, G., Cascarano, M., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, A. (1998). SIR97: a new tool for crystal structure determination and refinement. Submitted. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 10.3320(4) _cell_length_b 10.5387(4) _cell_length_c 12.722(2) _cell_angle_alpha 105.611(2) _cell_angle_beta 103.913(2) _cell_angle_gamma 103.526(2) _cell_volume 1227.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 7752 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.90 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description prism _exptl_crystal_colour clear _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1138.29 _chemical_formula_analytical ? _chemical_formula_sum 'C46 H56 Cl4 In2 O6 P2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 576.00 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7311 _exptl_special_details ; Data were collected in 0.50\% oscillations with 58.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -19.0 and 23.0\% at \c = -90.0\%. The crystal-to-detector distance was 40.47 mm. The detector swing angle was -5.5\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 10523 _reflns_number_total 4679 _reflns_number_gt 4242 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03762 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_max 0.796 _diffrn_measured_fraction_theta_full 0.796 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.92 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 46 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 56 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 6 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; In 0 2 -0.936 1.310 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom In(1) 0.94617(1) 0.08083(1) 0.61661(1) 0.00926(5) 1.000 . Uani d ? Cl(1) 0.95986(7) -0.10831(6) 0.69241(5) 0.0219(1) 1.000 . Uani d ? Cl(2) 0.75863(6) 0.13947(6) 0.67944(5) 0.0236(1) 1.000 . Uani d ? P(1) 1.15719(6) 0.27484(6) 0.78404(4) 0.0105(1) 1.000 . Uani d ? O(1) 1.1361(1) 0.0734(2) 0.5580(1) 0.0112(3) 1.000 . Uani d ? O(2) 0.9379(2) 0.2280(2) 0.5178(1) 0.0163(4) 1.000 . Uani d ? O(3) 0.6879(2) 0.2542(2) 0.4275(2) 0.0264(5) 1.000 . Uani d ? C(1) 1.2593(2) 0.1791(2) 0.6073(2) 0.0111(5) 1.000 . Uani d ? C(2) 1.3620(2) 0.1875(2) 0.5527(2) 0.0171(5) 1.000 . Uani d ? C(3) 1.4895(2) 0.2927(3) 0.6036(2) 0.0199(6) 1.000 . Uani d ? C(4) 1.5206(2) 0.3976(3) 0.7091(2) 0.0196(6) 1.000 . Uani d ? C(5) 1.4188(2) 0.3911(2) 0.7629(2) 0.0165(5) 1.000 . Uani d ? C(6) 1.2893(2) 0.2830(2) 0.7142(2) 0.0115(5) 1.000 . Uani d ? C(7) 1.6607(3) 0.5121(3) 0.7608(2) 0.0353(7) 1.000 . Uani d ? C(8) 1.2148(2) 0.2225(2) 0.9074(2) 0.0159(5) 1.000 . Uani d ? C(9) 1.1180(3) 0.1858(3) 0.9617(2) 0.0246(6) 1.000 . Uani d ? C(10) 1.1546(3) 0.1389(3) 1.0538(2) 0.0337(7) 1.000 . Uani d ? C(11) 1.2863(4) 0.1271(3) 1.0894(2) 0.0417(8) 1.000 . Uani d ? C(12) 1.3834(4) 0.1650(4) 1.0368(3) 0.0439(9) 1.000 . Uani d ? C(13) 1.3480(3) 0.2132(3) 0.9459(2) 0.0282(7) 1.000 . Uani d ? C(14) 1.1552(2) 0.4519(2) 0.8417(2) 0.0162(5) 1.000 . Uani d ? C(15) 1.2342(3) 0.5370(3) 0.9532(2) 0.0381(8) 1.000 . Uani d ? C(16) 1.2358(4) 0.6746(3) 0.9925(3) 0.0503(9) 1.000 . Uani d ? C(17) 1.1593(4) 0.7259(3) 0.9191(3) 0.0412(9) 1.000 . Uani d ? C(18) 1.0800(4) 0.6410(3) 0.8088(3) 0.047(1) 1.000 . Uani d ? C(19) 1.0755(3) 0.5030(3) 0.7692(2) 0.0341(7) 1.000 . Uani d ? C(20) 0.7786(4) 0.4967(3) 0.4720(3) 0.0426(9) 1.000 . Uani d ? C(21) 0.6710(3) 0.3647(3) 0.3877(3) 0.0397(8) 1.000 . Uani d ? C(22) 0.5792(3) 0.1218(3) 0.3653(3) 0.0331(7) 1.000 . Uani d ? C(23) 0.6029(4) 0.0416(4) 0.2594(3) 0.0459(9) 1.000 . Uani d ? H(1) 1.3430 0.1181 0.4772 0.021 1.000 . Uiso c ? H(2) 1.5608 0.2938 0.5647 0.024 1.000 . Uiso c ? H(3) 1.4376 0.4635 0.8368 0.020 1.000 . Uiso c ? H(4) 1.7370 0.4722 0.7738 0.042 1.000 . Uiso c ? H(5) 1.6712 0.5632 0.7073 0.042 1.000 . Uiso c ? H(6) 1.6646 0.5765 0.8341 0.042 1.000 . Uiso c ? H(7) 1.0233 0.1928 0.9354 0.029 1.000 . Uiso c ? H(8) 1.0861 0.1147 1.0929 0.040 1.000 . Uiso c ? H(9) 1.3111 0.0915 1.1526 0.050 1.000 . Uiso c ? H(10) 1.4779 0.1583 1.0638 0.053 1.000 . Uiso c ? H(11) 1.4177 0.2404 0.9088 0.034 1.000 . Uiso c ? H(12) 1.2896 0.5013 1.0048 0.046 1.000 . Uiso c ? H(13) 1.2910 0.7347 1.0719 0.059 1.000 . Uiso c ? H(14) 1.1616 0.8227 0.9467 0.049 1.000 . Uiso c ? H(15) 1.0257 0.6778 0.7566 0.057 1.000 . Uiso c ? H(16) 1.0165 0.4420 0.6907 0.041 1.000 . Uiso c ? H(17) 0.8728 0.4900 0.4783 0.052 1.000 . Uiso c ? H(18) 0.7681 0.5741 0.4455 0.052 1.000 . Uiso c ? H(19) 0.7650 0.5131 0.5476 0.052 1.000 . Uiso c ? H(20) 0.6841 0.3475 0.3118 0.048 1.000 . Uiso c ? H(21) 0.5763 0.3706 0.3810 0.048 1.000 . Uiso c ? H(22) 0.5771 0.0669 0.4163 0.040 1.000 . Uiso c ? H(23) 0.4886 0.1380 0.3426 0.040 1.000 . Uiso c ? H(24) 0.5264 -0.0472 0.2206 0.056 1.000 . Uiso c ? H(25) 0.6042 0.0952 0.2074 0.056 1.000 . Uiso c ? H(26) 0.6928 0.0242 0.2811 0.056 1.000 . Uiso c ? H(27) 0.865(4) 0.246(4) 0.488(3) 0.047(9) 1.000 . Uiso d ? H(28) 0.967(3) 0.219(4) 0.478(3) 0.023(8) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 In(1) 0.0100(1) 0.00900(9) 0.00818(8) 0.00277(6) 0.00377(6) 0.00152(6) Cl(1) 0.0380(3) 0.0176(3) 0.0175(2) 0.0115(2) 0.0140(2) 0.0110(2) Cl(2) 0.0171(3) 0.0247(3) 0.0262(3) 0.0077(2) 0.0125(2) -0.0011(2) P(1) 0.0121(3) 0.0102(3) 0.0077(2) 0.0031(2) 0.0034(2) 0.0009(2) O(1) 0.0082(7) 0.0120(7) 0.0099(6) 0.0012(6) 0.0040(5) -0.0008(6) O(2) 0.0197(9) 0.0173(8) 0.0157(8) 0.0092(7) 0.0070(7) 0.0077(7) O(3) 0.0249(9) 0.028(1) 0.0271(9) 0.0115(8) 0.0054(7) 0.0102(8) C(1) 0.010(1) 0.010(1) 0.0107(9) 0.0024(8) 0.0015(7) 0.0023(8) C(2) 0.018(1) 0.014(1) 0.0152(9) 0.0033(9) 0.0083(8) -0.0010(9) C(3) 0.014(1) 0.021(1) 0.020(1) 0.0010(9) 0.0093(9) 0.001(1) C(4) 0.014(1) 0.017(1) 0.020(1) -0.0015(9) 0.0052(8) 0.000(1) C(5) 0.018(1) 0.013(1) 0.0125(9) 0.0008(9) 0.0039(8) -0.0014(9) C(6) 0.013(1) 0.012(1) 0.0106(9) 0.0051(8) 0.0046(7) 0.0038(8) C(7) 0.023(1) 0.031(2) 0.030(1) -0.012(1) 0.011(1) -0.008(1) C(8) 0.023(1) 0.012(1) 0.0072(8) 0.0033(9) 0.0014(8) 0.0001(8) C(9) 0.022(1) 0.026(1) 0.016(1) -0.004(1) 0.0027(9) 0.006(1) C(10) 0.046(2) 0.025(1) 0.014(1) -0.010(1) 0.005(1) 0.006(1) C(11) 0.072(2) 0.033(2) 0.014(1) 0.014(2) 0.001(1) 0.013(1) C(12) 0.055(2) 0.060(2) 0.026(1) 0.037(2) 0.006(1) 0.020(2) C(13) 0.032(1) 0.039(2) 0.019(1) 0.018(1) 0.007(1) 0.012(1) C(14) 0.018(1) 0.012(1) 0.018(1) 0.0040(9) 0.0100(8) 0.0011(9) C(15) 0.045(2) 0.025(1) 0.029(1) 0.013(1) 0.000(1) -0.005(1) C(16) 0.054(2) 0.026(2) 0.046(2) 0.012(2) 0.005(2) -0.017(1) C(17) 0.048(2) 0.016(1) 0.060(2) 0.013(1) 0.027(2) 0.003(1) C(18) 0.070(2) 0.026(2) 0.053(2) 0.030(2) 0.021(2) 0.015(2) C(19) 0.056(2) 0.020(1) 0.026(1) 0.020(1) 0.007(1) 0.005(1) C(20) 0.054(2) 0.031(2) 0.053(2) 0.016(1) 0.021(2) 0.026(2) C(21) 0.040(2) 0.042(2) 0.046(2) 0.017(1) 0.008(1) 0.031(2) C(22) 0.028(1) 0.033(2) 0.036(1) 0.008(1) 0.008(1) 0.010(1) C(23) 0.053(2) 0.047(2) 0.033(1) 0.028(2) 0.004(1) 0.004(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4679 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.024 _refine_ls_wR_factor_all 0.0680 _refine_ls_wR_factor_ref 0.068 _refine_ls_goodness_of_fit_all 1.107 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_shift/su_max 0.0020 _refine_ls_shift/su_mean 0.0008 _refine_diff_density_min -0.85 _refine_diff_density_max 0.59 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 In(1) Cl(1) 2.4544(5) . . yes In(1) Cl(2) 2.4114(6) . . yes In(1) P(1) 2.6093(5) . . yes In(1) O(1) 2.271(1) . . yes In(1) O(1) 2.191(1) . 2_756 yes In(1) O(2) 2.247(2) . . yes P(1) C(6) 1.797(2) . . yes P(1) C(8) 1.814(2) . . yes P(1) C(14) 1.819(2) . . yes O(1) C(1) 1.353(2) . . yes O(2) H(27) 0.84(4) . . no O(2) H(28) 0.65(3) . . no O(3) C(21) 1.419(3) . . yes O(3) C(22) 1.443(4) . . yes C(1) C(2) 1.400(3) . . yes C(1) C(6) 1.408(3) . . yes C(2) C(3) 1.380(3) . . yes C(2) H(1) 0.98 . . no C(3) C(4) 1.398(3) . . yes C(3) H(2) 0.98 . . no C(4) C(5) 1.384(3) . . yes C(4) C(7) 1.511(3) . . yes C(5) C(6) 1.407(3) . . yes C(5) H(3) 0.98 . . no C(7) H(4) 0.98 . . no C(7) H(5) 0.98 . . no C(7) H(6) 0.98 . . no C(8) C(9) 1.387(3) . . yes C(8) C(13) 1.381(3) . . yes C(9) C(10) 1.394(4) . . yes C(9) H(7) 0.98 . . no C(10) C(11) 1.373(5) . . yes C(10) H(8) 0.98 . . no C(11) C(12) 1.375(5) . . yes C(11) H(9) 0.98 . . no C(12) C(13) 1.389(4) . . yes C(12) H(10) 0.98 . . no C(13) H(11) 0.98 . . no C(14) C(15) 1.378(4) . . yes C(14) C(19) 1.388(3) . . yes C(15) C(16) 1.396(4) . . yes C(15) H(12) 0.98 . . no C(16) C(17) 1.380(5) . . yes C(16) H(13) 0.98 . . no C(17) C(18) 1.367(5) . . yes C(17) H(14) 0.98 . . no C(18) C(19) 1.391(4) . . yes C(18) H(15) 0.98 . . no C(19) H(16) 0.98 . . no C(20) C(21) 1.491(5) . . yes C(20) H(17) 0.98 . . no C(20) H(18) 0.98 . . no C(20) H(19) 0.98 . . no C(21) H(20) 0.98 . . no C(21) H(21) 0.98 . . no C(22) C(23) 1.494(4) . . yes C(22) H(22) 0.98 . . no C(22) H(23) 0.98 . . no C(23) H(24) 0.98 . . no C(23) H(25) 0.98 . . no C(23) H(26) 0.98 . . no #------------------------------------------------------------------------------ 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 Cl(1) In(1) Cl(2) 99.41(2) . . . yes Cl(1) In(1) P(1) 96.55(2) . . . yes Cl(1) In(1) O(1) 91.82(4) . . . yes Cl(1) In(1) O(1) 88.54(4) . . 2_756 yes Cl(1) In(1) O(2) 169.30(5) . . . yes Cl(2) In(1) P(1) 97.92(2) . . . yes Cl(2) In(1) O(1) 167.67(4) . . . yes Cl(2) In(1) O(1) 111.06(4) . . 2_756 yes Cl(2) In(1) O(2) 88.51(5) . . . yes P(1) In(1) O(1) 75.60(4) . . . yes P(1) In(1) O(1) 149.36(4) . . 2_756 yes P(1) In(1) O(2) 89.40(4) . . . yes O(1) In(1) O(1) 74.05(6) . . 2_756 yes O(1) In(1) O(2) 81.02(6) . . . yes O(1) In(1) O(2) 81.88(6) 2_756 . . yes In(1) P(1) C(6) 99.44(7) . . . yes In(1) P(1) C(8) 112.81(7) . . . yes In(1) P(1) C(14) 122.41(8) . . . yes C(6) P(1) C(8) 108.2(1) . . . yes C(6) P(1) C(14) 106.5(1) . . . yes C(8) P(1) C(14) 106.3(1) . . . yes In(1) O(1) In(1) 105.95(6) . . 2_756 yes In(1) O(1) C(1) 121.9(1) . . . yes In(1) O(1) C(1) 128.2(1) 2_756 . . yes In(1) O(2) H(27) 125(3) . . . no In(1) O(2) H(28) 115(3) . . . no H(27) O(2) H(28) 104(4) . . . no C(21) O(3) C(22) 115.8(2) . . . yes O(1) C(1) C(2) 120.4(2) . . . yes O(1) C(1) C(6) 121.8(2) . . . yes C(2) C(1) C(6) 117.8(2) . . . yes C(1) C(2) C(3) 120.9(2) . . . yes C(1) C(2) H(1) 119.6 . . . no C(3) C(2) H(1) 119.5 . . . no C(2) C(3) C(4) 122.1(2) . . . yes C(2) C(3) H(2) 119.0 . . . no C(4) C(3) H(2) 118.9 . . . no C(3) C(4) C(5) 117.4(2) . . . yes C(3) C(4) C(7) 120.4(2) . . . yes C(5) C(4) C(7) 122.3(2) . . . yes C(4) C(5) C(6) 121.7(2) . . . yes C(4) C(5) H(3) 119.1 . . . no C(6) C(5) H(3) 119.2 . . . no P(1) C(6) C(1) 118.2(2) . . . yes P(1) C(6) C(5) 121.6(2) . . . yes C(1) C(6) C(5) 120.1(2) . . . yes C(4) C(7) H(4) 109.8 . . . no C(4) C(7) H(5) 109.3 . . . no C(4) C(7) H(6) 109.5 . . . no H(4) C(7) H(5) 109.3 . . . no H(4) C(7) H(6) 109.8 . . . no H(5) C(7) H(6) 109.1 . . . no P(1) C(8) C(9) 117.8(2) . . . yes P(1) C(8) C(13) 122.8(2) . . . yes C(9) C(8) C(13) 119.4(2) . . . yes C(8) C(9) C(10) 120.2(2) . . . yes C(8) C(9) H(7) 120.0 . . . no C(10) C(9) H(7) 119.8 . . . no C(9) C(10) C(11) 119.7(3) . . . yes C(9) C(10) H(8) 119.9 . . . no C(11) C(10) H(8) 120.4 . . . no C(10) C(11) C(12) 120.3(2) . . . yes C(10) C(11) H(9) 119.8 . . . no C(12) C(11) H(9) 119.9 . . . no C(11) C(12) C(13) 120.2(3) . . . yes C(11) C(12) H(10) 119.9 . . . no C(13) C(12) H(10) 119.9 . . . no C(8) C(13) C(12) 120.1(3) . . . yes C(8) C(13) H(11) 120.0 . . . no C(12) C(13) H(11) 119.9 . . . no P(1) C(14) C(15) 121.8(2) . . . yes P(1) C(14) C(19) 118.5(2) . . . yes C(15) C(14) C(19) 119.7(2) . . . yes C(14) C(15) C(16) 120.2(3) . . . yes C(14) C(15) H(12) 120.1 . . . no C(16) C(15) H(12) 119.8 . . . no C(15) C(16) C(17) 119.8(3) . . . yes C(15) C(16) H(13) 120.2 . . . no C(17) C(16) H(13) 120.0 . . . no C(16) C(17) C(18) 120.0(3) . . . yes C(16) C(17) H(14) 119.6 . . . no C(18) C(17) H(14) 120.4 . . . no C(17) C(18) C(19) 120.7(3) . . . yes C(17) C(18) H(15) 119.8 . . . no C(19) C(18) H(15) 119.5 . . . no C(14) C(19) C(18) 119.6(3) . . . yes C(14) C(19) H(16) 120.1 . . . no C(18) C(19) H(16) 120.3 . . . no C(21) C(20) H(17) 109.6 . . . no C(21) C(20) H(18) 109.4 . . . no C(21) C(20) H(19) 109.4 . . . no H(17) C(20) H(18) 109.5 . . . no H(17) C(20) H(19) 109.6 . . . no H(18) C(20) H(19) 109.3 . . . no O(3) C(21) C(20) 108.5(2) . . . yes O(3) C(21) H(20) 109.5 . . . no O(3) C(21) H(21) 109.7 . . . no C(20) C(21) H(20) 109.8 . . . no C(20) C(21) H(21) 110.1 . . . no H(20) C(21) H(21) 109.3 . . . no O(3) C(22) C(23) 112.5(3) . . . yes O(3) C(22) H(22) 108.6 . . . no O(3) C(22) H(23) 108.7 . . . no C(23) C(22) H(22) 108.7 . . . no C(23) C(22) H(23) 108.7 . . . no H(22) C(22) H(23) 109.6 . . . no C(22) C(23) H(24) 109.2 . . . no C(22) C(23) H(25) 109.4 . . . no C(22) C(23) H(26) 109.5 . . . no H(24) C(23) H(25) 109.5 . . . no H(24) C(23) H(26) 109.6 . . . no H(25) C(23) H(26) 109.7 . . . no #------------------------------------------------------------------------------ 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 Cl(2) C(3) 3.594(3) . 1_455 no O(2) O(3) 2.673(2) . . no O(2) C(22) 3.491(3) . . no O(2) C(20) 3.557(4) . 2_766 no O(3) C(3) 3.390(3) . 1_455 no C(1) C(23) 3.580(4) . 2_756 no C(3) C(22) 3.533(4) . 1_655 no C(7) C(10) 3.551(4) . 2_867 no C(10) C(10) 3.467(5) . 2_757 no C(13) C(23) 3.434(4) . 2_756 no #------------------------------------------------------------------------------ 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 In(1) P(1) C(6) C(1) . . . . -10.2(2) no In(1) P(1) C(6) C(5) . . . . 168.7(2) no In(1) P(1) C(8) C(9) . . . . -59.7(2) no In(1) P(1) C(8) C(13) . . . . 117.8(2) no In(1) P(1) C(14) C(15) . . . . 153.8(2) no In(1) P(1) C(14) C(19) . . . . -28.5(2) no In(1) O(1) In(1) Cl(1) . . 2_756 2_756 92.31(5) no In(1) O(1) In(1) Cl(2) . . 2_756 2_756 -168.16(4) no In(1) O(1) In(1) P(1) . . 2_756 2_756 -8.1(1) no In(1) O(1) In(1) O(1) . . 2_756 2_756 0.0000 no In(1) O(1) In(1) O(2) . . 2_756 2_756 -82.92(7) no In(1) O(1) C(1) C(2) . . . . -164.4(1) no In(1) O(1) C(1) C(6) . . . . 15.9(2) no In(1) O(1) In(1) Cl(1) . 2_756 2_756 2_756 -87.96(5) no In(1) O(1) In(1) Cl(2) . 2_756 2_756 2_756 116.3(2) no In(1) O(1) In(1) P(1) . 2_756 2_756 2_756 175.75(6) no In(1) O(1) In(1) O(1) . 2_756 2_756 . 0.0000 no In(1) O(1) In(1) O(2) . 2_756 2_756 2_756 84.05(7) no In(1) O(1) C(1) C(2) . 2_756 2_756 2_756 10.1(3) no In(1) O(1) C(1) C(6) . 2_756 2_756 2_756 -170.2(1) no Cl(1) In(1) P(1) C(6) . . . . 102.07(7) no Cl(1) In(1) P(1) C(8) . . . . -12.41(8) no Cl(1) In(1) P(1) C(14) . . . . -141.36(8) no Cl(1) In(1) O(1) C(1) . . . . -112.8(1) no Cl(1) In(1) O(1) C(1) . . 2_756 2_756 65.2(2) no Cl(2) In(1) P(1) C(6) . . . . -157.43(7) no Cl(2) In(1) P(1) C(8) . . . . 88.09(8) no Cl(2) In(1) P(1) C(14) . . . . -40.86(9) no Cl(2) In(1) O(1) C(1) . . . . 43.0(3) no Cl(2) In(1) O(1) C(1) . . 2_756 2_756 -34.3(2) no P(1) In(1) O(1) C(1) . . . . -16.5(1) no P(1) In(1) O(1) C(1) . . 2_756 2_756 165.6(1) no P(1) C(6) C(1) O(1) . . . . -1.3(3) no P(1) C(6) C(1) C(2) . . . . 179.0(2) no P(1) C(6) C(5) C(4) . . . . -179.9(2) no P(1) C(8) C(9) C(10) . . . . 177.2(2) no P(1) C(8) C(13) C(12) . . . . -176.3(2) no P(1) C(14) C(15) C(16) . . . . 176.7(3) no P(1) C(14) C(19) C(18) . . . . -175.6(3) no O(1) In(1) P(1) C(6) . . . . 11.86(8) no O(1) In(1) P(1) C(8) . . . . -102.61(9) no O(1) In(1) P(1) C(14) . . . . 128.44(9) no O(1) In(1) O(1) In(1) . . 2_756 2_756 0.0000 no O(1) In(1) O(1) C(1) . . 2_756 2_756 157.5(2) no O(1) In(1) P(1) C(6) . 2_756 2_756 2_756 -3.8(1) no O(1) In(1) P(1) C(8) . 2_756 2_756 2_756 110.7(1) no O(1) In(1) P(1) C(14) . 2_756 2_756 2_756 -120.4(1) no O(1) In(1) O(1) In(1) . 2_756 2_756 . 0.0000 no O(1) In(1) O(1) C(1) . 2_756 2_756 2_756 -159.2(2) no O(1) C(1) C(2) C(3) . . . . -178.2(2) no O(1) C(1) C(6) C(5) . . . . 179.8(2) no O(2) In(1) P(1) C(6) . . . . -69.02(8) no O(2) In(1) P(1) C(8) . . . . 176.5(1) no O(2) In(1) P(1) C(14) . . . . 47.6(1) no O(2) In(1) O(1) C(1) . . . . 75.2(1) no O(2) In(1) O(1) C(1) . . 2_756 2_756 -119.6(2) no C(1) C(2) C(3) C(4) . . . . -2.2(4) no C(1) C(6) P(1) C(8) . . . . 107.8(2) no C(1) C(6) P(1) C(14) . . . . -138.2(2) no C(1) C(6) C(5) C(4) . . . . -1.1(3) no C(2) C(1) C(6) C(5) . . . . 0.1(3) no C(2) C(3) C(4) C(5) . . . . 1.3(4) no C(2) C(3) C(4) C(7) . . . . -179.0(2) no C(3) C(2) C(1) C(6) . . . . 1.5(3) no C(3) C(4) C(5) C(6) . . . . 0.3(4) no C(5) C(6) P(1) C(8) . . . . -73.4(2) no C(5) C(6) P(1) C(14) . . . . 40.6(2) no C(6) P(1) C(8) C(9) . . . . -168.8(2) no C(6) P(1) C(8) C(13) . . . . 8.8(2) no C(6) P(1) C(14) C(15) . . . . -93.1(2) no C(6) P(1) C(14) C(19) . . . . 84.5(2) no C(6) C(5) C(4) C(7) . . . . -179.3(2) no C(8) P(1) C(14) C(15) . . . . 22.2(3) no C(8) P(1) C(14) C(19) . . . . -160.2(2) no C(8) C(9) C(10) C(11) . . . . -1.0(4) no C(8) C(13) C(12) C(11) . . . . -0.4(5) no C(9) C(8) P(1) C(14) . . . . 77.1(2) no C(9) C(8) C(13) C(12) . . . . 1.1(4) no C(9) C(10) C(11) C(12) . . . . 1.8(4) no C(10) C(9) C(8) C(13) . . . . -0.4(4) no C(10) C(11) C(12) C(13) . . . . -1.1(5) no C(13) C(8) P(1) C(14) . . . . -105.4(2) no C(14) C(15) C(16) C(17) . . . . -0.8(6) no C(14) C(19) C(18) C(17) . . . . -1.6(5) no C(15) C(14) C(19) C(18) . . . . 2.1(5) no C(15) C(16) C(17) C(18) . . . . 1.4(6) no C(16) C(15) C(14) C(19) . . . . -1.0(5) no C(16) C(17) C(18) C(19) . . . . -0.2(6) no C(20) C(21) O(3) C(22) . . . . 171.1(2) no C(21) O(3) C(22) C(23) . . . . 83.9(3) no data_copy _database_code_depnum_ccdc_archive 'CCDC 262807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.50 H16 Cl4 Ga O P' _chemical_formula_weight 496.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2856(5) _cell_length_b 9.8663(7) _cell_length_c 12.5628(5) _cell_angle_alpha 102.024(3) _cell_angle_beta 108.807(2) _cell_angle_gamma 94.664(3) _cell_volume 1051.79(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6155 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 28.69 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4272 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.69 _reflns_number_total 4272 _reflns_number_gt 3703 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.7082P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4272 _refine_ls_number_parameters 252 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.057 _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 Ga1 Ga 0.76695(3) 0.86164(3) 0.79635(2) 0.01793(9) Uani 1 1 d . . . Cl1 Cl 0.65019(8) 0.93793(8) 0.91619(6) 0.03073(16) Uani 1 1 d . . . Cl2 Cl 0.60192(8) 0.72880(7) 0.63639(6) 0.03429(17) Uani 1 1 d . . . Cl3 Cl 0.95388(8) 0.75629(7) 0.87466(6) 0.03204(16) Uani 1 1 d . . . P1 P 1.10821(7) 1.22978(6) 0.82809(5) 0.01556(13) Uani 1 1 d . . . O1 O 0.86429(19) 1.01244(18) 0.76793(16) 0.0213(4) Uani 1 1 d . . . C1 C 1.1698(3) 1.1124(3) 0.7294(2) 0.0185(5) Uani 1 1 d . . . C2 C 1.2258(3) 0.9939(3) 0.7588(2) 0.0285(6) Uani 1 1 d . . . H2 H 1.2341 0.9770 0.8321 0.034 Uiso 1 1 calc R . . C3 C 1.2698(3) 0.9003(3) 0.6807(3) 0.0371(7) Uani 1 1 d . . . H3 H 1.3084 0.8192 0.7005 0.045 Uiso 1 1 calc R . . C4 C 1.2574(3) 0.9253(3) 0.5740(3) 0.0328(6) Uani 1 1 d . . . H4 H 1.2874 0.8608 0.5207 0.039 Uiso 1 1 calc R . . C5 C 1.2021(3) 1.0423(3) 0.5445(2) 0.0304(6) Uani 1 1 d . . . H5 H 1.1953 1.0591 0.4714 0.036 Uiso 1 1 calc R . . C6 C 1.1563(3) 1.1362(3) 0.6214(2) 0.0259(5) Uani 1 1 d . . . H6 H 1.1160 1.2162 0.6005 0.031 Uiso 1 1 calc R . . C7 C 1.2238(3) 1.4002(3) 0.8793(2) 0.0190(5) Uani 1 1 d . . . C8 C 1.3246(3) 1.4429(3) 0.8276(3) 0.0305(6) Uani 1 1 d . . . H8 H 1.3393 1.3793 0.7654 0.037 Uiso 1 1 calc R . . C9 C 1.4045(3) 1.5800(3) 0.8677(3) 0.0360(7) Uani 1 1 d . . . H9 H 1.4736 1.6098 0.8324 0.043 Uiso 1 1 calc R . . C10 C 1.3838(3) 1.6721(3) 0.9579(2) 0.0306(6) Uani 1 1 d . . . H10 H 1.4373 1.7657 0.9839 0.037 Uiso 1 1 calc R . . C11 C 1.2853(3) 1.6289(3) 1.0110(2) 0.0286(6) Uani 1 1 d . . . H11 H 1.2728 1.6926 1.0742 0.034 Uiso 1 1 calc R . . C12 C 1.2049(3) 1.4935(3) 0.9726(2) 0.0242(5) Uani 1 1 d . . . H12 H 1.1374 1.4640 1.0092 0.029 Uiso 1 1 calc R . . C13 C 0.9117(3) 1.2472(2) 0.7656(2) 0.0159(4) Uani 1 1 d . . . C14 C 0.8627(3) 1.3706(3) 0.7386(2) 0.0214(5) Uani 1 1 d . . . H14 H 0.9357 1.4522 0.7549 0.026 Uiso 1 1 calc R . . C15 C 0.7066(3) 1.3722(3) 0.6878(2) 0.0258(5) Uani 1 1 d . . . H15 H 0.6719 1.4549 0.6685 0.031 Uiso 1 1 calc R . . C16 C 0.6011(3) 1.2527(3) 0.6652(2) 0.0224(5) Uani 1 1 d . . . H16 H 0.4943 1.2549 0.6307 0.027 Uiso 1 1 calc R . . C17 C 0.6481(3) 1.1297(3) 0.6919(2) 0.0198(5) Uani 1 1 d . . . H17 H 0.5741 1.0491 0.6761 0.024 Uiso 1 1 calc R . . C18 C 0.8045(3) 1.1258(2) 0.74190(19) 0.0156(4) Uani 1 1 d . . . Cl4A Cl 0.1649(4) 0.4911(4) 0.5292(3) 0.1216(14) Uani 0.726(8) 1 d PD . 1 C19A C 0.0268(9) 0.5830(19) 0.5717(15) 0.107(6) Uiso 0.363(4) 1 d PD . 1 H19A H 0.0489 0.6834 0.5735 0.128 Uiso 0.363(4) 1 calc PR . 1 H19B H 0.0338 0.5762 0.6507 0.128 Uiso 0.363(4) 1 calc PR . 1 Cl4B Cl 0.0482(13) 0.3929(9) 0.4326(8) 0.075(3) Uiso 0.163(6) 1 d PD . 2 C19B C 0.1097(19) 0.510(2) 0.5755(14) 0.004(4) Uiso 0.082(3) 1 d PD . 2 H19C H 0.1245 0.4578 0.6362 0.005 Uiso 0.082(3) 1 calc PR . 2 H19D H 0.2067 0.5736 0.5916 0.005 Uiso 0.082(3) 1 calc PR . 2 Cl4C Cl 0.1272(15) 0.4179(15) 0.4750(12) 0.045(4) Uiso 0.099(7) 1 d PD . 3 C19C C 0.072(2) 0.570(3) 0.548(3) 0.004(4) Uiso 0.049(4) 1 d PD . 3 H19E H 0.1154 0.6520 0.5269 0.005 Uiso 0.049(4) 1 calc PR . 3 H19F H 0.1251 0.5828 0.6320 0.005 Uiso 0.049(4) 1 calc PR . 3 H1 H 1.125(3) 1.172(3) 0.919(3) 0.028(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.02356(15) 0.01309(15) 0.01919(15) 0.00734(10) 0.00845(10) 0.00143(9) Cl1 0.0330(3) 0.0405(4) 0.0249(3) 0.0099(3) 0.0171(3) 0.0061(3) Cl2 0.0418(4) 0.0212(3) 0.0277(3) -0.0003(3) 0.0003(3) 0.0038(3) Cl3 0.0341(4) 0.0272(4) 0.0390(4) 0.0181(3) 0.0104(3) 0.0121(3) P1 0.0184(3) 0.0158(3) 0.0145(3) 0.0037(2) 0.0085(2) 0.0031(2) O1 0.0219(9) 0.0161(9) 0.0329(10) 0.0122(7) 0.0145(7) 0.0061(6) C1 0.0168(11) 0.0210(12) 0.0162(11) 0.0001(9) 0.0073(8) 0.0011(8) C2 0.0322(14) 0.0326(16) 0.0227(13) 0.0067(11) 0.0103(10) 0.0143(11) C3 0.0386(17) 0.0363(17) 0.0365(17) 0.0025(13) 0.0134(13) 0.0219(13) C4 0.0254(14) 0.0398(17) 0.0284(14) -0.0075(12) 0.0125(11) 0.0060(11) C5 0.0345(15) 0.0356(16) 0.0201(13) -0.0009(11) 0.0153(11) -0.0035(11) C6 0.0329(14) 0.0227(14) 0.0216(13) 0.0044(11) 0.0104(10) 0.0014(10) C7 0.0191(11) 0.0186(12) 0.0177(11) 0.0026(9) 0.0061(8) 0.0003(8) C8 0.0342(15) 0.0286(15) 0.0303(14) -0.0010(12) 0.0208(11) -0.0039(11) C9 0.0368(16) 0.0328(16) 0.0416(17) 0.0055(13) 0.0233(13) -0.0076(12) C10 0.0294(14) 0.0221(14) 0.0332(15) 0.0015(12) 0.0070(11) -0.0053(10) C11 0.0275(14) 0.0264(15) 0.0263(14) -0.0032(11) 0.0087(10) 0.0014(10) C12 0.0241(13) 0.0259(14) 0.0228(13) 0.0015(10) 0.0119(9) 0.0023(10) C13 0.0195(11) 0.0138(11) 0.0170(11) 0.0043(9) 0.0093(8) 0.0025(8) C14 0.0268(13) 0.0135(12) 0.0255(13) 0.0057(10) 0.0109(10) 0.0020(9) C15 0.0317(14) 0.0191(13) 0.0307(14) 0.0112(11) 0.0112(11) 0.0120(10) C16 0.0218(12) 0.0273(14) 0.0217(12) 0.0084(10) 0.0097(9) 0.0089(10) C17 0.0198(12) 0.0194(12) 0.0211(12) 0.0051(10) 0.0090(9) 0.0009(9) C18 0.0241(12) 0.0125(11) 0.0152(11) 0.0050(9) 0.0124(9) 0.0041(8) Cl4A 0.164(3) 0.104(3) 0.105(3) 0.047(2) 0.0499(19) -0.006(2) _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 Ga1 O1 1.8354(17) . ? Ga1 Cl3 2.1633(7) . ? Ga1 Cl2 2.1667(7) . ? Ga1 Cl1 2.1730(7) . ? P1 C13 1.777(2) . ? P1 C1 1.781(2) . ? P1 C7 1.790(2) . ? P1 H1 1.35(3) . ? O1 C18 1.343(3) . ? C1 C2 1.389(4) . ? C1 C6 1.393(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(5) . ? C4 H4 0.9500 . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.384(3) . ? C7 C12 1.400(4) . ? C8 C9 1.395(4) . ? C8 H8 0.9500 . ? C9 C10 1.374(4) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.403(3) . ? C13 C18 1.407(3) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.392(4) . ? C16 H16 0.9500 . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? Cl4A C19A 1.784(10) . ? Cl4A C19A 1.805(9) 2_566 ? C19A Cl4A 1.805(9) 2_566 ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? Cl4B C19B 1.800(10) 2_566 ? Cl4B C19B 1.805(10) . ? C19B Cl4B 1.800(10) 2_566 ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? Cl4C C19C 1.791(10) . ? Cl4C C19C 1.797(10) 2_566 ? C19C Cl4C 1.797(10) 2_566 ? C19C H19E 0.9900 . ? C19C H19F 0.9900 . ? 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 O1 Ga1 Cl3 103.57(6) . . ? O1 Ga1 Cl2 110.63(6) . . ? Cl3 Ga1 Cl2 112.26(3) . . ? O1 Ga1 Cl1 108.96(6) . . ? Cl3 Ga1 Cl1 111.31(3) . . ? Cl2 Ga1 Cl1 109.93(3) . . ? C13 P1 C1 111.84(11) . . ? C13 P1 C7 109.05(11) . . ? C1 P1 C7 112.27(11) . . ? C13 P1 H1 109.2(12) . . ? C1 P1 H1 105.6(13) . . ? C7 P1 H1 108.8(13) . . ? C18 O1 Ga1 126.90(15) . . ? C2 C1 C6 120.0(2) . . ? C2 C1 P1 119.66(19) . . ? C6 C1 P1 120.3(2) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C8 C7 C12 120.0(2) . . ? C8 C7 P1 122.5(2) . . ? C12 C7 P1 117.43(19) . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.5(2) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 120.8(2) . . ? C14 C13 P1 123.86(18) . . ? C18 C13 P1 115.32(17) . . ? C15 C14 C13 119.3(2) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 119.8(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 121.5(2) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 119.5(2) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? O1 C18 C17 125.0(2) . . ? O1 C18 C13 115.8(2) . . ? C17 C18 C13 119.1(2) . . ? C19A Cl4A C19A 70.0(8) . 2_566 ? Cl4A C19A Cl4A 110.0(8) . 2_566 ? Cl4A C19A H19A 109.7 . . ? Cl4A C19A H19A 109.7 2_566 . ? Cl4A C19A H19B 109.7 . . ? Cl4A C19A H19B 109.7 2_566 . ? H19A C19A H19B 108.2 . . ? C19B Cl4B C19B 77.3(10) 2_566 . ? Cl4B C19B Cl4B 102.7(10) 2_566 . ? Cl4B C19B H19C 111.2 2_566 . ? Cl4B C19B H19C 111.2 . . ? Cl4B C19B H19D 111.2 2_566 . ? Cl4B C19B H19D 111.2 . . ? H19C C19B H19D 109.1 . . ? C19C Cl4C C19C 59.1(15) . 2_566 ? Cl4C C19C Cl4C 120.9(15) . 2_566 ? Cl4C C19C H19E 107.1 . . ? Cl4C C19C H19E 107.1 2_566 . ? Cl4C C19C H19F 107.1 . . ? Cl4C C19C H19F 107.1 2_566 . ? H19E C19C H19F 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl3 Ga1 O1 C18 -165.40(18) . . . . ? Cl2 Ga1 O1 C18 74.12(19) . . . . ? Cl1 Ga1 O1 C18 -46.8(2) . . . . ? C13 P1 C1 C2 -120.9(2) . . . . ? C7 P1 C1 C2 116.1(2) . . . . ? C13 P1 C1 C6 56.6(2) . . . . ? C7 P1 C1 C6 -66.3(2) . . . . ? C6 C1 C2 C3 0.7(4) . . . . ? P1 C1 C2 C3 178.2(2) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C1 1.3(4) . . . . ? C2 C1 C6 C5 -1.3(4) . . . . ? P1 C1 C6 C5 -178.8(2) . . . . ? C13 P1 C7 C8 -110.9(2) . . . . ? C1 P1 C7 C8 13.7(3) . . . . ? C13 P1 C7 C12 66.8(2) . . . . ? C1 P1 C7 C12 -168.72(19) . . . . ? C12 C7 C8 C9 -1.3(4) . . . . ? P1 C7 C8 C9 176.3(2) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C9 C10 C11 C12 -1.1(4) . . . . ? C10 C11 C12 C7 -0.1(4) . . . . ? C8 C7 C12 C11 1.3(4) . . . . ? P1 C7 C12 C11 -176.4(2) . . . . ? C1 P1 C13 C14 -111.9(2) . . . . ? C7 P1 C13 C14 12.9(2) . . . . ? C1 P1 C13 C18 67.0(2) . . . . ? C7 P1 C13 C18 -168.25(17) . . . . ? C18 C13 C14 C15 -0.1(4) . . . . ? P1 C13 C14 C15 178.7(2) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C17 -0.3(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? Ga1 O1 C18 C17 -24.3(3) . . . . ? Ga1 O1 C18 C13 157.36(16) . . . . ? C16 C17 C18 O1 -177.6(2) . . . . ? C16 C17 C18 C13 0.7(3) . . . . ? C14 C13 C18 O1 178.0(2) . . . . ? P1 C13 C18 O1 -0.9(3) . . . . ? C14 C13 C18 C17 -0.5(3) . . . . ? P1 C13 C18 C17 -179.39(18) . . . . ? C19A Cl4A C19A Cl4A 0.0 2_566 . . 2_566 ? C19B Cl4B C19B Cl4B 0.0 2_566 . . 2_566 ? C19C Cl4C C19C Cl4C 0.000(2) 2_566 . . 2_566 ? _diffrn_measured_fraction_theta_max 0.785 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.785 _refine_diff_density_max 0.644 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.073