# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Roderick Wasylishen' _publ_contact_author_email RODERICK.WASYLISHEN@UALBERTA.CA _publ_section_title ; Solid-State 115In NMR Study of Indium Coordination Complexes ; loop_ _publ_author_name 'R Wasylishen' 'R Cavell' 'Fu Chen.' 'Guibin Ma.' 'Victor V Terskikh' # Attachment 'ChemCommun.cif' # Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_1 _database_code_depnum_ccdc_archive 'CCDC 699098' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 I3 In O8 P2' _chemical_formula_sum 'C42 H42 I3 In O8 P2' _chemical_formula_weight 1232.22 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P -3 1 c' _symmetry_space_group_name_Hall '-P 3 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 12.9326(4) _cell_length_b 12.9326(4) _cell_length_c 15.5514(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2252.53(18) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7964 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2811 _exptl_absorpt_correction_T_max 0.5635 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19232 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0077 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1735 _reflns_number_gt 1704 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0301P)^2^+3.8507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1735 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.000 _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 I I 0.09062(2) 0.545308(12) 0.2500 0.04711(12) Uani 1 2 d S . . In In 0.3333 0.6667 0.2500 0.02223(11) Uani 1 6 d S . . P P 0.3333 0.6667 0.48894(6) 0.0223(2) Uani 1 3 d S . . O1 O 0.3333 0.6667 0.3928(2) 0.0345(7) Uani 1 3 d S . . O2 O 0.79825(17) 0.8231(2) 0.66049(13) 0.0370(5) Uani 1 1 d . . . C1 C 0.4793(2) 0.7231(2) 0.53405(15) 0.0232(4) Uani 1 1 d . . . C2 C 0.5197(2) 0.8043(2) 0.60242(15) 0.0250(5) Uani 1 1 d . . . H2 H 0.4724 0.8369 0.6219 0.030 Uiso 1 1 calc R . . C3 C 0.6277(2) 0.8376(2) 0.64189(16) 0.0267(5) Uani 1 1 d . . . H3 H 0.6554 0.8946 0.6871 0.032 Uiso 1 1 calc R . . C4 C 0.6957(2) 0.7876(2) 0.61531(16) 0.0266(5) Uani 1 1 d . . . C5 C 0.6579(2) 0.7074(2) 0.54689(16) 0.0294(5) Uani 1 1 d . . . H5 H 0.7053 0.6745 0.5280 0.035 Uiso 1 1 calc R . . C6 C 0.5503(2) 0.6760(2) 0.50651(16) 0.0277(5) Uani 1 1 d . . . H6 H 0.5246 0.6218 0.4595 0.033 Uiso 1 1 calc R . . C7 C 0.8730(3) 0.7762(4) 0.6352(3) 0.0550(10) Uani 1 1 d . . . H7A H 0.9427 0.8079 0.6732 0.066 Uiso 1 1 calc R . . H7B H 0.8994 0.7996 0.5758 0.066 Uiso 1 1 calc R . . H7C H 0.8281 0.6889 0.6395 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I 0.02593(14) 0.06485(19) 0.03757(17) 0.00933(12) 0.000 0.01296(7) In 0.02384(14) 0.02384(14) 0.01901(19) 0.000 0.000 0.01192(7) P 0.0241(3) 0.0241(3) 0.0188(5) 0.000 0.000 0.01203(15) O1 0.0415(12) 0.0415(12) 0.0204(14) 0.000 0.000 0.0207(6) O2 0.0287(10) 0.0487(12) 0.0388(11) -0.0119(9) -0.0081(8) 0.0232(9) C1 0.0219(11) 0.0228(11) 0.0225(11) 0.0010(9) 0.0015(8) 0.0094(9) C2 0.0276(12) 0.0245(11) 0.0243(11) -0.0016(9) 0.0008(9) 0.0142(10) C3 0.0293(12) 0.0258(11) 0.0244(11) -0.0046(9) -0.0016(9) 0.0134(10) C4 0.0235(11) 0.0294(12) 0.0255(11) 0.0015(9) 0.0010(9) 0.0121(10) C5 0.0299(12) 0.0347(13) 0.0281(11) -0.0037(10) 0.0024(10) 0.0197(11) C6 0.0291(12) 0.0300(12) 0.0243(11) -0.0050(9) 0.0015(9) 0.0151(10) C7 0.0399(17) 0.084(3) 0.058(2) -0.0209(19) -0.0120(15) 0.0432(19) _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 I In 2.7184(3) . ? In I 2.7184(3) 3_565 ? In I 2.7184(3) 2_665 ? In O1 2.221(3) 4_665 ? In O1 2.221(3) . ? P O1 1.495(3) . ? P C1 1.792(2) . ? P C1 1.792(2) 2_665 ? P C1 1.792(2) 3_565 ? O2 C4 1.361(3) . ? O2 C7 1.429(4) . ? C1 C6 1.398(3) . ? C1 C2 1.399(3) . ? C2 C3 1.383(4) . ? C3 C4 1.390(3) . ? C4 C5 1.392(4) . ? C5 C6 1.389(4) . ? 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 In O1 180.0 4_665 . ? O1 In I 90.0 4_665 3_565 ? O1 In I 90.0 . 3_565 ? O1 In I 90.0 4_665 . ? O1 In I 90.0 . . ? I In I 120.0 3_565 . ? O1 In I 90.0 4_665 2_665 ? O1 In I 90.0 . 2_665 ? I In I 120.0 3_565 2_665 ? I In I 120.0 . 2_665 ? O1 P C1 113.04(8) . . ? O1 P C1 113.04(8) . 2_665 ? C1 P C1 105.68(9) . 2_665 ? O1 P C1 113.04(8) . 3_565 ? C1 P C1 105.68(9) . 3_565 ? C1 P C1 105.68(9) 2_665 3_565 ? P O1 In 180.0 . . ? C4 O2 C7 117.8(2) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 P 119.37(18) . . ? C2 C1 P 121.65(19) . . ? C3 C2 C1 120.7(2) . . ? C2 C3 C4 119.9(2) . . ? O2 C4 C3 115.2(2) . . ? O2 C4 C5 124.4(2) . . ? C3 C4 C5 120.4(2) . . ? C6 C5 C4 119.4(2) . . ? C5 C6 C1 120.9(2) . . ? 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 C1 P O1 In -67(100) . . . . ? C1 P O1 In 53(100) 2_665 . . . ? C1 P O1 In 173(100) 3_565 . . . ? O1 In O1 P 0(73) 4_665 . . . ? I In O1 P 0(100) 3_565 . . . ? I In O1 P -120(100) . . . . ? I In O1 P 120(100) 2_665 . . . ? O1 P C1 C6 -51.6(2) . . . . ? C1 P C1 C6 -175.72(19) 2_665 . . . ? C1 P C1 C6 72.6(3) 3_565 . . . ? O1 P C1 C2 135.05(18) . . . . ? C1 P C1 C2 10.9(2) 2_665 . . . ? C1 P C1 C2 -100.81(15) 3_565 . . . ? C6 C1 C2 C3 0.1(4) . . . . ? P C1 C2 C3 173.53(19) . . . . ? C1 C2 C3 C4 -1.9(4) . . . . ? C7 O2 C4 C3 -179.0(3) . . . . ? C7 O2 C4 C5 0.9(4) . . . . ? C2 C3 C4 O2 -177.6(2) . . . . ? C2 C3 C4 C5 2.5(4) . . . . ? O2 C4 C5 C6 178.8(2) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C4 C5 C6 C1 -0.5(4) . . . . ? C2 C1 C6 C5 1.1(4) . . . . ? P C1 C6 C5 -172.5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.029 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.083 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 699099' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Cl3 In O9 P' _chemical_formula_weight 753.67 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' In In -0.7276 1.3100 '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 10.7470(11) _cell_length_b 12.3980(13) _cell_length_c 14.0806(15) _cell_angle_alpha 93.5129(14) _cell_angle_beta 112.0704(12) _cell_angle_gamma 108.9252(13) _cell_volume 1608.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7726 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5583 _exptl_absorpt_correction_T_max 0.7374 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14214 _diffrn_reflns_av_R_equivalents 0.0102 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7293 _reflns_number_gt 6840 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0463P)^2^+1.0965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7293 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 In In 0.204724(16) 0.296600(13) 0.180862(11) 0.03112(6) Uani 1 1 d . . . Cl1 Cl 0.09699(7) 0.26049(5) -0.00751(4) 0.04190(13) Uani 1 1 d . . . Cl2 Cl 0.43221(6) 0.45702(6) 0.23493(6) 0.04977(16) Uani 1 1 d . . . Cl3 Cl 0.26536(8) 0.13187(6) 0.22511(5) 0.05188(16) Uani 1 1 d . . . P P 0.04854(5) 0.34047(4) 0.26232(3) 0.02043(9) Uani 1 1 d . . . O11 O -0.09646(17) 0.12459(12) 0.12422(12) 0.0331(3) Uani 1 1 d . . . O12 O -0.53226(19) 0.16537(17) -0.09605(14) 0.0527(5) Uani 1 1 d . . . O13 O -0.16414(16) 0.46758(13) 0.20073(11) 0.0312(3) Uani 1 1 d . . . O21 O 0.12138(16) 0.50699(13) 0.14835(11) 0.0310(3) Uani 1 1 d . . . O22 O 0.3323(2) 0.85428(13) 0.42106(15) 0.0459(4) Uani 1 1 d . . . O23 O 0.12882(18) 0.47965(13) 0.47895(11) 0.0337(3) Uani 1 1 d . . . O31 O 0.30057(15) 0.33755(13) 0.41839(12) 0.0323(3) Uani 1 1 d . . . O32 O 0.11107(19) 0.12361(16) 0.63370(13) 0.0441(4) Uani 1 1 d . . . O33 O -0.20070(15) 0.19709(14) 0.31604(12) 0.0367(4) Uani 1 1 d . . . C11 C -0.13143(19) 0.29521(16) 0.16002(14) 0.0228(3) Uani 1 1 d . . . C12 C -0.1861(2) 0.18455(17) 0.09534(15) 0.0270(4) Uani 1 1 d . . . C13 C -0.3208(2) 0.14197(19) 0.01010(17) 0.0356(5) Uani 1 1 d . . . H13 H -0.3558 0.0675 -0.0335 0.043 Uiso 1 1 calc R . . C14 C -0.4029(2) 0.2115(2) -0.00960(16) 0.0348(4) Uani 1 1 d . . . C15 C -0.3554(2) 0.31950(19) 0.05369(16) 0.0305(4) Uani 1 1 d . . . H15 H -0.4147 0.3642 0.0401 0.037 Uiso 1 1 calc R . . C16 C -0.2190(2) 0.36165(17) 0.13768(14) 0.0250(4) Uani 1 1 d . . . C17 C -0.1376(3) 0.0160(2) 0.0561(2) 0.0436(5) Uani 1 1 d . . . H17A H -0.0649 -0.0184 0.0858 0.052 Uiso 1 1 calc R . . H17B H -0.1439 0.0300 -0.0130 0.052 Uiso 1 1 calc R . . H17C H -0.2320 -0.0375 0.0492 0.052 Uiso 1 1 calc R . . C18 C -0.6145(3) 0.2375(3) -0.1262(2) 0.0596(8) Uani 1 1 d . . . H18A H -0.7063 0.1934 -0.1868 0.072 Uiso 1 1 calc R . . H18B H -0.5595 0.3061 -0.1449 0.072 Uiso 1 1 calc R . . H18C H -0.6341 0.2625 -0.0678 0.072 Uiso 1 1 calc R . . C19 C -0.2367(3) 0.5465(2) 0.17146(19) 0.0370(5) Uani 1 1 d . . . H19A H -0.1839 0.6193 0.2245 0.044 Uiso 1 1 calc R . . H19B H -0.3354 0.5115 0.1664 0.044 Uiso 1 1 calc R . . H19C H -0.2404 0.5630 0.1034 0.044 Uiso 1 1 calc R . . C21 C 0.12677(19) 0.49518(15) 0.31335(14) 0.0224(3) Uani 1 1 d . . . C22 C 0.1614(2) 0.56619(17) 0.24626(15) 0.0257(4) Uani 1 1 d . . . C23 C 0.2299(2) 0.68682(18) 0.27777(17) 0.0322(4) Uani 1 1 d . . . H23 H 0.2526 0.7334 0.2310 0.039 Uiso 1 1 calc R . . C24 C 0.2641(2) 0.73705(17) 0.37969(18) 0.0323(4) Uani 1 1 d . . . C25 C 0.2316(2) 0.67002(17) 0.44929(16) 0.0295(4) Uani 1 1 d . . . H25 H 0.2559 0.7062 0.5187 0.035 Uiso 1 1 calc R . . C26 C 0.1635(2) 0.55006(16) 0.41615(15) 0.0251(4) Uani 1 1 d . . . C27 C 0.1751(3) 0.5709(2) 0.08077(18) 0.0391(5) Uani 1 1 d . . . H27A H 0.1405 0.5186 0.0135 0.047 Uiso 1 1 calc R . . H27B H 0.2813 0.6027 0.1137 0.047 Uiso 1 1 calc R . . H27C H 0.1401 0.6349 0.0692 0.047 Uiso 1 1 calc R . . C28 C 0.3754(4) 0.9271(2) 0.3554(3) 0.0659(9) Uani 1 1 d . . . H28A H 0.4220 1.0087 0.3930 0.079 Uiso 1 1 calc R . . H28B H 0.2900 0.9179 0.2917 0.079 Uiso 1 1 calc R . . H28C H 0.4438 0.9048 0.3363 0.079 Uiso 1 1 calc R . . C29 C 0.1864(3) 0.5258(2) 0.58866(16) 0.0401(5) Uani 1 1 d . . . H29A H 0.1522 0.4639 0.6234 0.048 Uiso 1 1 calc R . . H29B H 0.1540 0.5889 0.5997 0.048 Uiso 1 1 calc R . . H29C H 0.2925 0.5562 0.6181 0.048 Uiso 1 1 calc R . . C31 C 0.0510(2) 0.26306(15) 0.36671(14) 0.0224(3) Uani 1 1 d . . . C32 C 0.1888(2) 0.27286(16) 0.43982(15) 0.0260(4) Uani 1 1 d . . . C33 C 0.2064(2) 0.22424(19) 0.52744(16) 0.0319(4) Uani 1 1 d . . . H33 H 0.2998 0.2308 0.5754 0.038 Uiso 1 1 calc R . . C34 C 0.0839(2) 0.16546(18) 0.54377(16) 0.0317(4) Uani 1 1 d . . . C35 C -0.0543(2) 0.15190(18) 0.47302(16) 0.0292(4) Uani 1 1 d . . . H35 H -0.1369 0.1098 0.4844 0.035 Uiso 1 1 calc R . . C36 C -0.0692(2) 0.20142(16) 0.38501(15) 0.0253(4) Uani 1 1 d . . . C37 C 0.4427(2) 0.3408(2) 0.4806(2) 0.0434(5) Uani 1 1 d . . . H37A H 0.5114 0.3884 0.4553 0.052 Uiso 1 1 calc R . . H37B H 0.4420 0.2614 0.4750 0.052 Uiso 1 1 calc R . . H37C H 0.4721 0.3748 0.5540 0.052 Uiso 1 1 calc R . . C38 C -0.0074(3) 0.0718(3) 0.6612(2) 0.0482(6) Uani 1 1 d . . . H38A H 0.0286 0.0505 0.7294 0.058 Uiso 1 1 calc R . . H38B H -0.0788 0.0019 0.6079 0.058 Uiso 1 1 calc R . . H38C H -0.0530 0.1278 0.6652 0.058 Uiso 1 1 calc R . . C39 C -0.3266(3) 0.1000(2) 0.3006(2) 0.0490(6) Uani 1 1 d . . . H39A H -0.4126 0.1098 0.2504 0.059 Uiso 1 1 calc R . . H39B H -0.3342 0.0948 0.3676 0.059 Uiso 1 1 calc R . . H39C H -0.3200 0.0284 0.2733 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In 0.03537(9) 0.03632(9) 0.03433(9) 0.01295(6) 0.02136(7) 0.01996(7) Cl1 0.0661(4) 0.0401(3) 0.0335(3) 0.0127(2) 0.0299(3) 0.0255(3) Cl2 0.0286(3) 0.0619(4) 0.0624(4) 0.0265(3) 0.0229(3) 0.0145(3) Cl3 0.0706(4) 0.0487(3) 0.0503(3) 0.0160(3) 0.0219(3) 0.0425(3) P 0.0211(2) 0.0220(2) 0.0194(2) 0.00629(16) 0.00895(17) 0.00872(17) O11 0.0407(8) 0.0262(7) 0.0300(7) 0.0025(6) 0.0102(6) 0.0158(6) O12 0.0358(9) 0.0510(10) 0.0413(9) 0.0018(8) -0.0082(7) 0.0097(8) O13 0.0309(7) 0.0318(7) 0.0313(7) 0.0030(6) 0.0089(6) 0.0178(6) O21 0.0372(8) 0.0319(7) 0.0243(7) 0.0117(6) 0.0156(6) 0.0092(6) O22 0.0493(10) 0.0226(7) 0.0534(10) 0.0050(7) 0.0180(8) 0.0029(7) O23 0.0504(9) 0.0290(7) 0.0243(7) 0.0065(5) 0.0205(7) 0.0121(6) O31 0.0209(6) 0.0412(8) 0.0347(7) 0.0170(6) 0.0105(6) 0.0112(6) O32 0.0408(9) 0.0563(10) 0.0307(8) 0.0257(7) 0.0120(7) 0.0133(8) O33 0.0210(7) 0.0504(9) 0.0365(8) 0.0223(7) 0.0110(6) 0.0096(7) C11 0.0219(8) 0.0267(9) 0.0189(8) 0.0064(7) 0.0074(7) 0.0088(7) C12 0.0306(9) 0.0265(9) 0.0230(8) 0.0069(7) 0.0108(8) 0.0098(7) C13 0.0366(11) 0.0295(10) 0.0278(10) 0.0013(8) 0.0058(9) 0.0064(8) C14 0.0265(10) 0.0384(11) 0.0274(10) 0.0085(8) 0.0035(8) 0.0065(8) C15 0.0250(9) 0.0376(10) 0.0293(9) 0.0131(8) 0.0098(8) 0.0130(8) C16 0.0263(9) 0.0291(9) 0.0221(8) 0.0090(7) 0.0118(7) 0.0109(7) C17 0.0561(15) 0.0279(10) 0.0450(13) 0.0005(9) 0.0197(11) 0.0168(10) C18 0.0349(13) 0.0645(18) 0.0535(16) 0.0159(14) -0.0065(12) 0.0157(12) C19 0.0457(12) 0.0375(11) 0.0402(11) 0.0141(9) 0.0213(10) 0.0259(10) C21 0.0208(8) 0.0218(8) 0.0236(8) 0.0055(7) 0.0088(7) 0.0072(6) C22 0.0237(8) 0.0285(9) 0.0255(9) 0.0093(7) 0.0103(7) 0.0100(7) C23 0.0311(10) 0.0284(10) 0.0375(11) 0.0142(8) 0.0156(9) 0.0090(8) C24 0.0269(9) 0.0232(9) 0.0416(11) 0.0057(8) 0.0114(9) 0.0067(7) C25 0.0283(9) 0.0276(9) 0.0297(9) 0.0024(7) 0.0101(8) 0.0100(8) C26 0.0235(8) 0.0276(9) 0.0256(9) 0.0067(7) 0.0107(7) 0.0108(7) C27 0.0494(13) 0.0442(12) 0.0312(10) 0.0209(9) 0.0238(10) 0.0160(10) C28 0.081(2) 0.0255(12) 0.082(2) 0.0140(13) 0.0396(19) 0.0011(13) C29 0.0495(13) 0.0473(13) 0.0234(10) 0.0067(9) 0.0156(9) 0.0178(11) C31 0.0242(8) 0.0227(8) 0.0215(8) 0.0078(6) 0.0095(7) 0.0099(7) C32 0.0244(9) 0.0265(9) 0.0269(9) 0.0085(7) 0.0099(7) 0.0098(7) C33 0.0272(9) 0.0373(11) 0.0277(9) 0.0129(8) 0.0064(8) 0.0126(8) C34 0.0371(11) 0.0319(10) 0.0242(9) 0.0122(8) 0.0108(8) 0.0121(8) C35 0.0294(9) 0.0297(9) 0.0277(9) 0.0101(7) 0.0134(8) 0.0079(8) C36 0.0240(9) 0.0265(9) 0.0242(8) 0.0068(7) 0.0093(7) 0.0089(7) C37 0.0229(10) 0.0578(15) 0.0477(13) 0.0224(11) 0.0114(9) 0.0150(10) C38 0.0508(14) 0.0591(15) 0.0338(12) 0.0231(11) 0.0203(11) 0.0140(12) C39 0.0267(11) 0.0506(14) 0.0481(14) 0.0056(11) 0.0068(10) -0.0007(10) _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 In Cl3 2.3870(6) . ? In Cl2 2.4029(6) . ? In Cl1 2.4056(6) . ? In P 2.5281(5) . ? P C21 1.7981(18) . ? P C11 1.7983(18) . ? P C31 1.8007(18) . ? O11 C12 1.362(2) . ? O11 C17 1.436(3) . ? O12 C14 1.367(2) . ? O12 C18 1.428(4) . ? O13 C16 1.350(2) . ? O13 C19 1.428(2) . ? O21 C22 1.360(2) . ? O21 C27 1.441(2) . ? O22 C24 1.369(2) . ? O22 C28 1.428(3) . ? O23 C26 1.347(2) . ? O23 C29 1.428(2) . ? O31 C32 1.362(2) . ? O31 C37 1.433(2) . ? O32 C34 1.363(2) . ? O32 C38 1.433(3) . ? O33 C36 1.363(2) . ? O33 C39 1.421(3) . ? C11 C16 1.405(3) . ? C11 C12 1.407(3) . ? C12 C13 1.391(3) . ? C13 C14 1.392(3) . ? C14 C15 1.384(3) . ? C15 C16 1.395(3) . ? C21 C22 1.400(3) . ? C21 C26 1.411(3) . ? C22 C23 1.391(3) . ? C23 C24 1.389(3) . ? C24 C25 1.393(3) . ? C25 C26 1.385(3) . ? C31 C36 1.398(3) . ? C31 C32 1.410(3) . ? C32 C33 1.382(3) . ? C33 C34 1.394(3) . ? C34 C35 1.390(3) . ? C35 C36 1.395(3) . ? 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 Cl3 In Cl2 105.52(3) . . ? Cl3 In Cl1 105.76(2) . . ? Cl2 In Cl1 105.31(2) . . ? Cl3 In P 114.28(2) . . ? Cl2 In P 111.59(2) . . ? Cl1 In P 113.61(2) . . ? C21 P C11 111.97(8) . . ? C21 P C31 110.23(8) . . ? C11 P C31 111.36(8) . . ? C21 P In 106.41(6) . . ? C11 P In 107.10(6) . . ? C31 P In 109.58(6) . . ? C12 O11 C17 117.50(17) . . ? C14 O12 C18 117.4(2) . . ? C16 O13 C19 119.07(16) . . ? C22 O21 C27 117.32(16) . . ? C24 O22 C28 116.9(2) . . ? C26 O23 C29 119.35(17) . . ? C32 O31 C37 118.34(16) . . ? C34 O32 C38 118.22(18) . . ? C36 O33 C39 118.76(17) . . ? C16 C11 C12 117.87(17) . . ? C16 C11 P 125.85(14) . . ? C12 C11 P 116.26(14) . . ? O11 C12 C13 124.04(18) . . ? O11 C12 C11 114.10(17) . . ? C13 C12 C11 121.86(19) . . ? C12 C13 C14 118.16(19) . . ? O12 C14 C15 123.1(2) . . ? O12 C14 C13 114.9(2) . . ? C15 C14 C13 122.00(19) . . ? C14 C15 C16 119.01(19) . . ? O13 C16 C15 122.13(18) . . ? O13 C16 C11 116.81(17) . . ? C15 C16 C11 121.06(18) . . ? C22 C21 C26 117.68(17) . . ? C22 C21 P 116.46(14) . . ? C26 C21 P 125.75(14) . . ? O21 C22 C23 123.44(17) . . ? O21 C22 C21 114.16(16) . . ? C23 C22 C21 122.40(18) . . ? C24 C23 C22 117.93(18) . . ? O22 C24 C23 124.0(2) . . ? O22 C24 C25 114.2(2) . . ? C23 C24 C25 121.77(18) . . ? C26 C25 C24 119.24(19) . . ? O23 C26 C25 122.61(18) . . ? O23 C26 C21 116.41(16) . . ? C25 C26 C21 120.98(18) . . ? C36 C31 C32 117.82(16) . . ? C36 C31 P 125.94(14) . . ? C32 C31 P 116.11(14) . . ? O31 C32 C33 123.92(18) . . ? O31 C32 C31 114.22(16) . . ? C33 C32 C31 121.81(18) . . ? C32 C33 C34 118.50(18) . . ? O32 C34 C35 123.46(19) . . ? O32 C34 C33 114.81(19) . . ? C35 C34 C33 121.73(18) . . ? C34 C35 C36 118.63(18) . . ? O33 C36 C35 121.43(17) . . ? O33 C36 C31 117.01(16) . . ? C35 C36 C31 121.48(17) . . ? 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 In P C21 134.44(6) . . . . ? Cl2 In P C21 14.82(7) . . . . ? Cl1 In P C21 -104.06(6) . . . . ? Cl3 In P C11 -105.64(7) . . . . ? Cl2 In P C11 134.73(6) . . . . ? Cl1 In P C11 15.85(7) . . . . ? Cl3 In P C31 15.28(7) . . . . ? Cl2 In P C31 -104.35(7) . . . . ? Cl1 In P C31 136.77(7) . . . . ? C21 P C11 C16 -15.35(19) . . . . ? C31 P C11 C16 108.57(17) . . . . ? In P C11 C16 -131.64(15) . . . . ? C21 P C11 C12 162.64(14) . . . . ? C31 P C11 C12 -73.43(16) . . . . ? In P C11 C12 46.36(15) . . . . ? C17 O11 C12 C13 6.5(3) . . . . ? C17 O11 C12 C11 -173.79(18) . . . . ? C16 C11 C12 O11 -178.14(16) . . . . ? P C11 C12 O11 3.7(2) . . . . ? C16 C11 C12 C13 1.6(3) . . . . ? P C11 C12 C13 -176.60(16) . . . . ? O11 C12 C13 C14 178.81(19) . . . . ? C11 C12 C13 C14 -0.9(3) . . . . ? C18 O12 C14 C15 5.6(4) . . . . ? C18 O12 C14 C13 -173.9(2) . . . . ? C12 C13 C14 O12 178.4(2) . . . . ? C12 C13 C14 C15 -1.1(3) . . . . ? O12 C14 C15 C16 -177.2(2) . . . . ? C13 C14 C15 C16 2.2(3) . . . . ? C19 O13 C16 C15 -10.2(3) . . . . ? C19 O13 C16 C11 169.39(17) . . . . ? C14 C15 C16 O13 178.08(18) . . . . ? C14 C15 C16 C11 -1.5(3) . . . . ? C12 C11 C16 O13 -179.94(16) . . . . ? P C11 C16 O13 -2.0(2) . . . . ? C12 C11 C16 C15 -0.4(3) . . . . ? P C11 C16 C15 177.59(15) . . . . ? C11 P C21 C22 -69.05(16) . . . . ? C31 P C21 C22 166.40(14) . . . . ? In P C21 C22 47.66(15) . . . . ? C11 P C21 C26 114.82(17) . . . . ? C31 P C21 C26 -9.73(19) . . . . ? In P C21 C26 -128.47(15) . . . . ? C27 O21 C22 C23 10.9(3) . . . . ? C27 O21 C22 C21 -169.48(18) . . . . ? C26 C21 C22 O21 -179.44(16) . . . . ? P C21 C22 O21 4.1(2) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? P C21 C22 C23 -176.25(16) . . . . ? O21 C22 C23 C24 179.45(19) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C28 O22 C24 C23 -2.8(4) . . . . ? C28 O22 C24 C25 176.8(2) . . . . ? C22 C23 C24 O22 179.6(2) . . . . ? C22 C23 C24 C25 0.0(3) . . . . ? O22 C24 C25 C26 -179.52(19) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C29 O23 C26 C25 -11.7(3) . . . . ? C29 O23 C26 C21 168.18(18) . . . . ? C24 C25 C26 O23 179.93(19) . . . . ? C24 C25 C26 C21 0.0(3) . . . . ? C22 C21 C26 O23 179.94(17) . . . . ? P C21 C26 O23 -4.0(3) . . . . ? C22 C21 C26 C25 -0.1(3) . . . . ? P C21 C26 C25 175.96(15) . . . . ? C21 P C31 C36 107.50(17) . . . . ? C11 P C31 C36 -17.4(2) . . . . ? In P C31 C36 -135.72(15) . . . . ? C21 P C31 C32 -68.08(16) . . . . ? C11 P C31 C32 167.01(14) . . . . ? In P C31 C32 48.70(16) . . . . ? C37 O31 C32 C33 10.2(3) . . . . ? C37 O31 C32 C31 -172.46(19) . . . . ? C36 C31 C32 O31 -177.82(17) . . . . ? P C31 C32 O31 -1.9(2) . . . . ? C36 C31 C32 C33 -0.4(3) . . . . ? P C31 C32 C33 175.56(16) . . . . ? O31 C32 C33 C34 176.33(19) . . . . ? C31 C32 C33 C34 -0.8(3) . . . . ? C38 O32 C34 C35 -5.6(3) . . . . ? C38 O32 C34 C33 174.2(2) . . . . ? C32 C33 C34 O32 -177.9(2) . . . . ? C32 C33 C34 C35 1.9(3) . . . . ? O32 C34 C35 C36 178.0(2) . . . . ? C33 C34 C35 C36 -1.7(3) . . . . ? C39 O33 C36 C35 -31.0(3) . . . . ? C39 O33 C36 C31 152.3(2) . . . . ? C34 C35 C36 O33 -176.10(19) . . . . ? C34 C35 C36 C31 0.4(3) . . . . ? C32 C31 C36 O33 177.26(17) . . . . ? P C31 C36 O33 1.8(3) . . . . ? C32 C31 C36 C35 0.6(3) . . . . ? P C31 C36 C35 -174.89(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.383 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.081 #===END