Supplementary Material (ESI) for Dalton Transactions. This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hill, Nicholas J.' 'Levason, W.' 'Reid, G.' # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK. ; _publ_section_title ; Arsenic (III) Halide Complexes with Phosphine and Arsine Co-ligands: Synthesis, Spectroscopic and Structural Properties. ; _publ_contact_letter ; This is the CIF file for the structure of [AsCl3(PMe3)] included in our manuscript to be submitted to JCS Dalton Trans. ; _publ_contact_author_phone ' 023 8059 3609 ' _publ_contact_author_fax ' 023 8059 3781 ' _publ_contact_author_email ' gr@soton.ac.uk ' #============================================================================== _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1997). ; #============================================================================== data__ascl3pmeAsCl3+PMe3 _database_code_CSD 170403 _audit_creation_date '2001-07-27' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; [AsCl3(PMe3)] ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SHELX97 (Sheldrick, 1997) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 12.002(6) _cell_length_b 12.297(6) _cell_length_c 12.328(4) _cell_angle_alpha 90 _cell_angle_beta 91.97(4) _cell_angle_gamma 90 _cell_volume 1819(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 9.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 514.72 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H18 As2 Cl6 P2 ' _chemical_formula_moiety '?' _chemical_formula_structural [AsCl3(PMe3)] _chemical_compound_source ? _exptl_crystal_F_000 1008.00 _exptl_absorpt_coefficient_mu 4.709 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.798 _exptl_special_details ; The scan width was (0.89+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.65 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -4 2 4 -2 1 -1 -2 4 _diffrn_reflns_number 3545 _reflns_number_total 3377 _reflns_number_gt 1706 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.12495 _diffrn_reflns_av_sigmaI/netI 0.164 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02151 _diffrn_orient_matrix_UB_12 0.00971 _diffrn_orient_matrix_UB_13 0.07849 _diffrn_orient_matrix_UB_21 -0.07643 _diffrn_orient_matrix_UB_22 -0.02301 _diffrn_orient_matrix_UB_23 0.02031 _diffrn_orient_matrix_UB_31 0.02543 _diffrn_orient_matrix_UB_32 -0.07739 _diffrn_orient_matrix_UB_33 0.00381 #------------------------------------------------------------------------------ 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 24 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 8 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 24 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom As(1) -0.0105(1) 0.4378(1) 0.1579(1) 0.0214(4) 1.000 . Uani d ? As(2) 0.4199(1) 0.4955(1) 0.3434(1) 0.0220(3) 1.000 . Uani d ? Cl(1) -0.0188(3) 0.2654(3) 0.2361(3) 0.039(1) 1.000 . Uani d ? Cl(2) -0.0174(3) 0.6301(3) 0.0654(3) 0.035(1) 1.000 . Uani d ? Cl(3) -0.0510(3) 0.5213(3) 0.3133(2) 0.034(1) 1.000 . Uani d ? Cl(4) 0.2529(3) 0.4290(3) 0.2750(3) 0.034(1) 1.000 . Uani d ? Cl(5) 0.6134(2) 0.5790(3) 0.4448(2) 0.0304(9) 1.000 . Uani d ? Cl(6) 0.4699(3) 0.5770(3) 0.1872(2) 0.033(1) 1.000 . Uani d ? P(1) -0.2025(2) 0.4082(3) 0.1126(2) 0.0189(9) 1.000 . Uani d ? P(2) 0.3169(2) 0.6523(3) 0.3947(3) 0.0185(9) 1.000 . Uani d ? C(1) -0.225(1) 0.281(1) 0.043(1) 0.024(4) 1.000 . Uani d ? C(2) -0.278(1) 0.395(1) 0.233(1) 0.028(4) 1.000 . Uani d ? C(3) -0.263(1) 0.515(1) 0.034(1) 0.042(5) 1.000 . Uani d ? C(4) 0.268(1) 0.723(1) 0.277(1) 0.034(4) 1.000 . Uani d ? C(5) 0.397(1) 0.747(1) 0.479(1) 0.031(4) 1.000 . Uani d ? C(6) 0.1974(9) 0.614(1) 0.471(1) 0.026(4) 1.000 . Uani 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 As(1) 0.0124(6) 0.0339(9) 0.0180(7) -0.0012(6) 0.0024(5) -0.0012(6) As(2) 0.0150(6) 0.0360(9) 0.0152(6) 0.0028(6) 0.0007(5) -0.0017(7) Cl(1) 0.030(2) 0.044(2) 0.044(2) 0.008(2) -0.001(2) 0.017(2) Cl(2) 0.032(2) 0.040(2) 0.034(2) -0.003(2) 0.011(2) -0.009(2) Cl(3) 0.029(2) 0.053(3) 0.020(2) -0.011(2) 0.004(1) -0.013(2) Cl(4) 0.020(2) 0.046(2) 0.035(2) 0.001(2) -0.005(1) -0.013(2) Cl(5) 0.022(2) 0.045(2) 0.025(2) -0.004(2) 0.007(1) 0.002(2) Cl(6) 0.031(2) 0.053(3) 0.017(2) 0.011(2) 0.009(1) 0.005(2) P(1) 0.015(2) 0.028(2) 0.014(2) 0.001(1) 0.001(1) -0.001(1) P(2) 0.015(2) 0.025(2) 0.015(2) 0.002(1) -0.001(1) -0.000(1) C(1) 0.036(8) 0.012(7) 0.024(7) -0.003(6) 0.002(6) -0.011(6) C(2) 0.024(7) 0.037(9) 0.025(7) -0.013(6) 0.015(6) -0.003(6) C(3) 0.015(7) 0.08(1) 0.031(8) -0.001(8) -0.010(6) 0.032(8) C(4) 0.028(8) 0.06(1) 0.019(7) 0.017(7) 0.005(6) -0.002(7) C(5) 0.031(8) 0.039(9) 0.022(7) 0.004(7) -0.002(6) 0.002(7) C(6) 0.009(6) 0.042(9) 0.029(7) 0.006(6) 0.003(5) -0.002(6) #============================================================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1706 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_all 0.0890 _refine_ls_wR_factor_ref 0.0890 _refine_ls_goodness_of_fit_all 2.454 _refine_ls_goodness_of_fit_ref 2.450 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_min -1.44 _refine_diff_density_max 1.74 #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) Cl(1) 2.333(6) . . ? As(1) Cl(2) 2.625(6) . . ? As(1) Cl(3) 2.242(5) . . ? As(1) P(1) 2.380(5) . . ? As(2) Cl(4) 2.298(5) . . ? As(2) Cl(5) 2.795(5) . . ? As(2) Cl(5) 2.809(5) . . ? As(2) Cl(6) 2.270(5) . . ? As(2) P(2) 2.388(5) . . ? P(1) C(1) 1.80(2) . . ? P(1) C(2) 1.78(2) . . ? P(1) C(3) 1.77(2) . . ? P(2) C(4) 1.78(2) . . ? P(2) C(5) 1.81(2) . . ? P(2) C(6) 1.80(2) . . ? C(1) H(1) 0.95(2) . . ? C(1) H(2) 0.95(2) . . ? C(1) H(7) 0.95(2) . . ? C(2) H(3) 0.95(2) . . ? C(2) H(8) 0.95(2) . . ? C(2) H(9) 0.95(2) . . ? C(3) H(4) 0.95(2) . . ? C(3) H(5) 0.95(3) . . ? C(3) H(10) 0.95(2) . . ? C(4) H(6) 0.95(2) . . ? C(4) H(11) 0.95(2) . . ? C(4) H(12) 0.95(2) . . ? C(5) H(13) 0.95(2) . . ? C(5) H(14) 0.95(2) . . ? C(5) H(15) 0.95(2) . . ? C(6) H(16) 0.95(2) . . ? C(6) H(17) 0.95(2) . . ? C(6) H(18) 0.95(2) . . ? #------------------------------------------------------------------------------ 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) As(1) Cl(2) 175.6(2) . . . ? Cl(1) As(1) Cl(3) 92.8(2) . . . ? Cl(1) As(1) P(1) 84.4(2) . . . ? Cl(2) As(1) Cl(3) 87.4(2) . . . ? Cl(2) As(1) P(1) 91.1(2) . . . ? Cl(3) As(1) P(1) 91.9(2) . . . ? Cl(4) As(2) Cl(5) 174.7(2) . . . ? Cl(4) As(2) Cl(5) 94.3(2) . . . ? Cl(4) As(2) Cl(6) 95.6(2) . . . ? Cl(4) As(2) P(2) 86.1(2) . . . ? Cl(5) As(2) Cl(5) 81.2(2) . . . ? Cl(5) As(2) Cl(6) 88.7(2) . . . ? Cl(5) As(2) P(2) 90.8(2) . . . ? Cl(5) As(2) Cl(6) 169.4(2) 3_666 3_666 3_666 ? Cl(5) As(2) P(2) 85.7(2) 3_666 3_666 3_666 ? Cl(6) As(2) P(2) 91.2(2) . . . ? As(2) Cl(5) As(2) 98.8(2) . . . ? As(1) P(1) C(1) 111.7(7) . . . ? As(1) P(1) C(2) 109.6(7) . . . ? As(1) P(1) C(3) 113.2(7) . . . ? C(1) P(1) C(2) 104.6(9) . . . ? C(1) P(1) C(3) 109(1) . . . ? C(2) P(1) C(3) 108(1) . . . ? As(2) P(2) C(4) 109.9(7) . . . ? As(2) P(2) C(5) 113.5(7) . . . ? As(2) P(2) C(6) 110.8(7) . . . ? C(4) P(2) C(5) 108(1) . . . ? C(4) P(2) C(6) 107.7(9) . . . ? C(5) P(2) C(6) 106.7(9) . . . ? P(1) C(1) H(1) 109(2) . . . ? P(1) C(1) H(2) 109(1) . . . ? P(1) C(1) H(7) 109(2) . . . ? H(1) C(1) H(2) 109(2) . . . ? H(1) C(1) H(7) 109(2) . . . ? H(2) C(1) H(7) 109(2) . . . ? P(1) C(2) H(3) 109(2) . . . ? P(1) C(2) H(8) 109(2) . . . ? P(1) C(2) H(9) 109(1) . . . ? H(3) C(2) H(8) 109(2) . . . ? H(3) C(2) H(9) 109(2) . . . ? H(8) C(2) H(9) 109(2) . . . ? P(1) C(3) H(4) 109(2) . . . ? P(1) C(3) H(5) 109(2) . . . ? P(1) C(3) H(10) 109(2) . . . ? H(4) C(3) H(5) 109(2) . . . ? H(4) C(3) H(10) 109(2) . . . ? H(5) C(3) H(10) 109(3) . . . ? P(2) C(4) H(6) 109(2) . . . ? P(2) C(4) H(11) 109(2) . . . ? P(2) C(4) H(12) 109(2) . . . ? H(6) C(4) H(11) 109(2) . . . ? H(6) C(4) H(12) 109(2) . . . ? H(11) C(4) H(12) 109(2) . . . ? P(2) C(5) H(13) 109(2) . . . ? P(2) C(5) H(14) 109(2) . . . ? P(2) C(5) H(15) 109(2) . . . ? H(13) C(5) H(14) 109(2) . . . ? H(13) C(5) H(15) 109(2) . . . ? H(14) C(5) H(15) 109(2) . . . ? P(2) C(6) H(16) 109(2) . . . ? P(2) C(6) H(17) 109(2) . . . ? P(2) C(6) H(18) 109(1) . . . ? H(16) C(6) H(17) 109(2) . . . ? H(16) C(6) H(18) 109(2) . . . ? H(17) C(6) H(18) 109(2) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag As(1) Cl(2) 2.907(6) . 3_565 no As(1) H(10) 3.2577 . 3_565 no As(1) Cl(4) 3.432(5) . . no As(2) H(8) 3.3283 . 1_655 no As(2) Cl(1) 3.556(6) . 4 no Cl(1) H(3) 2.7335 . 4 no Cl(1) H(15) 3.0305 . 2_546 no Cl(1) H(8) 3.4409 . 4 no Cl(1) C(2) 3.50(2) . 4 no Cl(2) H(7) 2.6616 . 3_565 no Cl(2) H(1) 3.0957 . 2_455 no Cl(2) H(12) 3.2246 . 4_465 no Cl(2) C(1) 3.42(2) . 3_565 no Cl(2) P(1) 3.522(7) . 3_565 no Cl(2) H(6) 3.5231 . . no Cl(2) H(10) 3.5586 . 3_565 no Cl(3) H(14) 2.8627 . 4_465 no Cl(3) H(18) 3.1883 . 3_566 no Cl(3) H(16) 3.2109 . . no Cl(3) H(17) 3.2571 . . no Cl(3) H(12) 3.3283 . 4_465 no Cl(3) H(16) 3.3773 . 3_566 no Cl(3) H(13) 3.4930 . 4_465 no Cl(3) C(5) 3.58(2) . 4_465 no Cl(3) H(11) 3.5813 . 4_465 no Cl(4) H(2) 2.9302 . 4 no Cl(4) H(3) 3.2499 . 4 no Cl(4) H(10) 3.3131 . 3_565 no Cl(4) H(4) 3.5388 . 3_565 no Cl(5) H(11) 2.8417 . 4_565 no Cl(5) H(8) 3.1300 . 1_655 no Cl(5) H(17) 3.2199 . 4_565 no Cl(5) H(14) 3.3692 . 4_565 no Cl(5) H(9) 3.4397 . 1_655 no Cl(6) H(4) 2.8628 . 3_565 no Cl(6) H(8) 2.8644 . 1_655 no Cl(6) H(5) 3.1822 . 1_655 no Cl(6) H(1) 3.5054 . 3_565 no C(1) H(10) 3.0210 . 2_445 no C(1) H(5) 3.0438 . 2_445 no C(1) C(3) 3.42(3) . 2_445 no C(1) H(6) 3.4494 . 3_565 no C(2) H(18) 2.8069 . 3_566 no C(2) H(15) 3.3570 . 3_566 no C(3) H(2) 3.0358 . 2_455 no C(3) H(7) 3.2329 . 2_455 no C(3) H(1) 3.4271 . 2_455 no C(4) H(1) 3.3778 . 3_565 no C(4) H(5) 3.5782 . 4_565 no C(5) H(17) 3.1206 . 4_565 no C(6) H(9) 2.9172 . 3_566 no C(6) H(13) 3.2292 . 4_465 no H(1) H(12) 2.9072 . 3_565 no H(1) H(10) 2.9594 . 2_445 no H(1) H(6) 3.0001 . 3_565 no H(1) H(5) 3.0218 . 2_445 no H(2) H(10) 2.5151 . 2_445 no H(2) H(5) 2.9267 . 2_445 no H(2) H(4) 3.1958 . 2_445 no H(3) H(15) 2.8664 . 3_566 no H(3) H(18) 2.9635 . 3_566 no H(4) H(7) 3.4339 . 2_455 no H(5) H(7) 2.6751 . 2_455 no H(5) H(11) 3.2254 . 4_465 no H(5) H(12) 3.2882 . 4_465 no H(6) H(7) 3.0524 . 3_565 no H(7) H(10) 3.1091 . 2_445 no H(7) H(12) 3.5016 . 3_565 no H(8) H(18) 3.1478 . 3_566 no H(8) H(11) 3.4322 . 4_465 no H(8) H(15) 3.5065 . 3_566 no H(9) H(18) 1.9933 . 3_566 no H(9) H(15) 3.1836 . 3_566 no H(9) H(16) 3.2038 . 3_566 no H(9) H(17) 3.3852 . 3_566 no H(13) H(17) 2.3179 . 4_565 no H(13) H(18) 3.4793 . 4_565 no H(14) H(16) 2.9851 . 2_556 no H(14) H(17) 3.1703 . 4_565 no H(15) H(17) 3.5592 . 4_565 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 As(2) Cl(5) As(2) Cl(4) . . . . 177.2(2) no As(2) Cl(5) As(2) Cl(5) . . . . 0.0000(1) no As(2) Cl(5) As(2) Cl(6) . . . . 18(1) no As(2) Cl(5) As(2) P(2) . . . . 91.5(2) no As(2) Cl(5) As(2) Cl(4) . . . . -31(2) no As(2) Cl(5) As(2) Cl(5) . . . . 0.0000(1) no As(2) Cl(5) As(2) Cl(6) . . . . -176.8(2) no As(2) Cl(5) As(2) P(2) . . . . -85.5(2) no Cl(1) As(1) P(1) C(1) . . . . -52.4(7) no Cl(1) As(1) P(1) C(2) . . . . 63.0(8) no Cl(1) As(1) P(1) C(3) . . . . -176.2(9) no Cl(2) As(1) P(1) C(1) . . . . 127.5(7) no Cl(2) As(1) P(1) C(2) . . . . -117.0(8) no Cl(2) As(1) P(1) C(3) . . . . 3.7(9) no Cl(3) As(1) P(1) C(1) . . . . -145.0(7) no Cl(3) As(1) P(1) C(2) . . . . -29.6(8) no Cl(3) As(1) P(1) C(3) . . . . 91.2(9) no Cl(4) As(2) P(2) C(4) . . . . -67.2(8) no Cl(4) As(2) P(2) C(5) . . . . 171.7(8) no Cl(4) As(2) P(2) C(6) . . . . 51.7(7) no Cl(5) As(2) Cl(5) As(2) . . . . 0.0000 no Cl(5) As(2) P(2) C(4) . . . . 117.1(8) no Cl(5) As(2) P(2) C(5) . . . . -4.0(7) no Cl(5) As(2) P(2) C(6) . . . . -124.0(7) no Cl(5) As(2) Cl(5) As(2) . . . . 0.0000(2) no Cl(5) As(2) P(2) C(4) . . . . 161.8(8) no Cl(5) As(2) P(2) C(5) . . . . -77.1(7) no Cl(5) As(2) P(2) C(6) . . . . 42.9(7) no Cl(6) As(2) P(2) C(4) . . . . 28.4(8) no Cl(6) As(2) P(2) C(5) . . . . -92.7(7) no Cl(6) As(2) P(2) C(6) . . . . 147.3(7) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__01njh001 _database_code_CSD 170404 _audit_creation_date '2001-07-27' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; [AsBr3{o-C6H4(AsMe2)2}] ; #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.8794(3) _cell_length_b 16.0455(6) _cell_length_c 11.3094(4) _cell_angle_alpha 90 _cell_angle_beta 110.973(1) _cell_angle_gamma 90 _cell_volume 1673.99(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rhomboid' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.383 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 600.71 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H16 As3 Br3 ' _chemical_formula_moiety 'C10 H16 As3 Br3 ' _chemical_formula_structural [AsBr3{o-C6H4(AsMe2)2}] _chemical_compound_source ? _exptl_crystal_F_000 1120.00 _exptl_absorpt_coefficient_mu 15.343 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute. Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max and min transmission factors: 0.892, 0.494 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 15.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Mercury CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 14643 _reflns_number_total 3929 _reflns_number_gt 2324 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.11669 _diffrn_reflns_av_sigmaI/netI 0.169 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 6.93 _diffrn_reflns_theta_max 88.49 _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 H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 40 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 12 -0.767 1.283 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; As 0 12 -1.011 1.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.26679(12) 0.43881(8) 0.09562(12) 0.0317(4) 1.000 . Uani d ? Br(2) 0.03738(12) 0.53715(11) 0.26711(13) 0.0446(4) 1.000 . Uani d ? Br(3) 0.46348(12) 0.62611(8) 0.50362(12) 0.0307(4) 1.000 . Uani d ? As(1) 0.33777(11) 0.51808(8) 0.29510(11) 0.0199(3) 1.000 . Uani d ? As(2) 0.27401(12) 0.64826(8) 0.17498(12) 0.0247(3) 1.000 . Uani d ? As(3) 0.58424(11) 0.53484(8) 0.27543(11) 0.0198(3) 1.000 . Uani d ? C(1) 0.1238(12) 0.6384(9) 0.0132(12) 0.039(4) 1.000 . Uani d ? C(2) 0.2121(13) 0.7376(10) 0.2597(13) 0.062(5) 1.000 . Uani d ? C(3) 0.4458(11) 0.6850(8) 0.1472(13) 0.035(4) 1.000 . Uani d ? C(4) 0.441(1) 0.7587(11) 0.081(2) 0.082(6) 1.000 . Uani d ? C(5) 0.557(2) 0.7910(10) 0.058(2) 0.079(6) 1.000 . Uani d ? C(6) 0.691(1) 0.7463(9) 0.101(2) 0.051(5) 1.000 . Uani d ? C(7) 0.6944(12) 0.6706(8) 0.165(1) 0.042(4) 1.000 . Uani d ? C(8) 0.5719(11) 0.6411(8) 0.1862(11) 0.029(3) 1.000 . Uani d ? C(9) 0.7537(12) 0.5421(9) 0.4238(12) 0.038(4) 1.000 . Uani d ? C(10) 0.6365(12) 0.4519(9) 0.175(1) 0.042(4) 1.000 . Uani d ? H(1) 0.1403 0.5904 -0.0288 0.047 1.000 . Uiso c ? H(2) 0.0329 0.6335 0.0236 0.047 1.000 . Uiso c ? H(3) 0.1233 0.6866 -0.0359 0.047 1.000 . Uiso c ? H(4) 0.2254 0.7211 0.3438 0.075 1.000 . Uiso c ? H(5) 0.1126 0.7494 0.2150 0.075 1.000 . Uiso c ? H(6) 0.2682 0.7861 0.2617 0.075 1.000 . Uiso c ? H(7) 0.3516 0.7883 0.0506 0.098 1.000 . Uiso c ? H(8) 0.5495 0.8425 0.0150 0.094 1.000 . Uiso c ? H(9) 0.7736 0.7664 0.0857 0.061 1.000 . Uiso c ? H(10) 0.7818 0.6393 0.1953 0.050 1.000 . Uiso c ? H(11) 0.5543 0.4390 0.1024 0.050 1.000 . Uiso c ? H(12) 0.7117 0.4731 0.1499 0.050 1.000 . Uiso c ? H(13) 0.6692 0.4029 0.2244 0.050 1.000 . Uiso c ? H(14) 0.8163 0.4968 0.4256 0.046 1.000 . Uiso c ? H(15) 0.7271 0.5400 0.4966 0.046 1.000 . Uiso c ? H(16) 0.8022 0.5931 0.4232 0.046 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 Br(1) 0.0369(7) 0.0255(7) 0.0300(7) -0.0053(5) 0.0088(5) -0.0057(6) Br(2) 0.0223(6) 0.0782(12) 0.0343(8) 0.0010(6) 0.0113(5) 0.0030(8) Br(3) 0.0343(7) 0.0261(8) 0.0281(7) 0.0051(5) 0.0067(5) -0.0037(6) As(1) 0.0195(6) 0.0188(7) 0.0219(7) -0.0011(5) 0.0080(5) -0.0010(5) As(2) 0.0236(6) 0.0185(7) 0.0292(7) 0.0047(5) 0.0061(5) 0.0016(6) As(3) 0.0189(5) 0.0193(7) 0.0213(6) 0.0006(5) 0.0073(5) 0.0009(6) C(1) 0.039(7) 0.046(9) 0.030(7) 0.011(6) 0.009(6) 0.003(7) C(2) 0.062(9) 0.054(10) 0.041(9) 0.035(8) -0.017(7) -0.026(8) C(3) 0.030(6) 0.019(7) 0.059(9) 0.003(5) 0.021(6) 0.006(7) C(4) 0.035(8) 0.060(12) 0.14(2) 0.003(8) 0.013(9) 0.066(12) C(5) 0.084(11) 0.041(11) 0.10(2) 0.002(9) 0.014(10) 0.044(10) C(6) 0.051(8) 0.035(9) 0.064(10) -0.013(7) 0.017(7) 0.025(8) C(7) 0.037(7) 0.024(7) 0.062(10) -0.009(6) 0.014(7) -0.005(7) C(8) 0.035(6) 0.031(7) 0.023(6) -0.008(5) 0.012(5) 0.004(6) C(9) 0.030(6) 0.051(9) 0.033(7) -0.010(6) 0.013(5) -0.010(7) C(10) 0.041(7) 0.034(8) 0.063(10) 0.002(6) 0.033(7) -0.011(7) #============================================================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2324 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_all 0.0780 _refine_ls_wR_factor_ref 0.0780 _refine_ls_goodness_of_fit_all 1.500 _refine_ls_goodness_of_fit_ref 1.500 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.53 _refine_diff_density_max 1.64 #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag BR1 AS1 2.463(2) . . ? BR2 AS1 2.886(2) . . ? BR3 AS1 2.830(2) . . ? BR3 AS1 3.345(2) . . ? AS1 AS2 2.448(2) . . ? AS1 AS3 2.537(2) . . ? AS2 C1 1.91(1) . . ? AS2 C2 1.94(2) . . ? AS2 C3 1.926(13) . . ? AS3 C8 1.96(1) . . ? AS3 C9 1.90(2) . . ? AS3 C10 1.93(2) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C1 H3 0.95 . . no C2 H4 0.95 . . no C2 H5 0.95 . . no C2 H6 0.95 . . no C3 C4 1.39(2) . . ? C3 C8 1.36(2) . . ? C4 C5 1.37(2) . . ? C4 H7 0.95 . . no C5 C6 1.42(2) . . ? C5 H8 0.95 . . no C6 C7 1.41(2) . . ? C6 H9 0.95 . . no C7 C8 1.40(2) . . ? C7 H10 0.95 . . no C9 H14 0.95 . . no C9 H15 0.95 . . no C9 H16 0.95 . . no C10 H11 0.95 . . no C10 H12 0.95 . . no C10 H13 0.95 . . 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 AS1 BR3 AS1 96.84(6) . . . ? BR1 AS1 BR2 90.56(6) . . . ? BR1 AS1 BR3 167.30(7) . . . ? BR1 AS1 BR3 99.87(7) . . . ? BR1 AS1 AS2 90.00(7) . . . ? BR1 AS1 AS3 86.67(6) . . . ? BR2 AS1 BR3 98.85(6) . . . ? BR2 AS1 BR3 118.56(6) . . . ? BR2 AS1 AS2 78.37(6) . . . ? BR2 AS1 AS3 163.85(8) . . . ? BR3 AS1 BR3 83.16(6) . . . ? BR3 AS1 AS2 83.62(7) . . . ? BR3 AS1 AS3 81.93(6) . . . ? BR3 AS1 AS2 159.97(7) 3_666 3_666 3_666 ? BR3 AS1 AS3 77.58(5) 3_666 3_666 3_666 ? AS2 AS1 AS3 85.72(6) . . . ? AS1 AS2 C1 114.8(5) . . . ? AS1 AS2 C2 114.9(6) . . . ? AS1 AS2 C3 106.6(4) . . . ? C1 AS2 C2 105.1(6) . . . ? C1 AS2 C3 107.3(7) . . . ? C2 AS2 C3 107.8(7) . . . ? AS1 AS3 C8 104.6(4) . . . ? AS1 AS3 C9 119.9(4) . . . ? AS1 AS3 C10 116.4(4) . . . ? C8 AS3 C9 105.9(6) . . . ? C8 AS3 C10 106.1(7) . . . ? C9 AS3 C10 102.9(7) . . . ? AS2 C1 H1 109.5 . . . no AS2 C1 H2 109.5 . . . no AS2 C1 H3 109.4 . . . no H1 C1 H2 109.5 . . . no H1 C1 H3 109.5 . . . no H2 C1 H3 109.5 . . . no AS2 C2 H4 109.5 . . . no AS2 C2 H5 109.5 . . . no AS2 C2 H6 109.5 . . . no H4 C2 H5 109.5 . . . no H4 C2 H6 109.5 . . . no H5 C2 H6 109.5 . . . no AS2 C3 C4 118.9(11) . . . ? AS2 C3 C8 123.1(11) . . . ? C4 C3 C8 118.0(14) . . . ? C3 C4 C5 123.5(16) . . . ? C3 C4 H7 118.2 . . . no C5 C4 H7 118.2 . . . no C4 C5 C6 119.0(16) . . . ? C4 C5 H8 120.5 . . . no C6 C5 H8 120.4 . . . no C5 C6 C7 117.2(14) . . . ? C5 C6 H9 121.4 . . . no C7 C6 H9 121.4 . . . no C6 C7 C8 121.0(14) . . . ? C6 C7 H10 119.5 . . . no C8 C7 H10 119.5 . . . no AS3 C8 C3 119.9(10) . . . ? AS3 C8 C7 118.9(11) . . . ? C3 C8 C7 121.2(14) . . . ? AS3 C9 H14 109.5 . . . no AS3 C9 H15 109.5 . . . no AS3 C9 H16 109.5 . . . no H14 C9 H15 109.5 . . . no H14 C9 H16 109.5 . . . no H15 C9 H16 109.5 . . . no AS3 C10 H11 109.5 . . . no AS3 C10 H12 109.5 . . . no AS3 C10 H13 109.5 . . . no H11 C10 H12 109.5 . . . no H11 C10 H13 109.5 . . . no H12 C10 H13 109.5 . . . 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 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__01bp005 _database_code_CSD 170405 _audit_creation_date '2001-07-27' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; [AsI3{o-C6H4(AsMe2)2}] ; #============================================================================== _computing_data_collection 'Nonius Kappa CCD Diffractometer Control' _computing_cell_refinement 'Nonius Kappa CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 8.7874(2) _cell_length_b 12.0405(3) _cell_length_c 16.7508(5) _cell_angle_alpha 90 _cell_angle_beta 90.9090(9) _cell_angle_gamma 90 _cell_volume 1772.09(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rhomboid' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.780 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 741.71 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H16 As3 I3 ' _chemical_formula_moiety 'C10 H16 As3 I3 ' _chemical_formula_structural [AsI3{o-C6H4(AsMe2)2}] _chemical_compound_source ? _exptl_crystal_F_000 1336.00 _exptl_absorpt_coefficient_mu 10.833 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute. Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max and min transmission factors: 0.741, 0.673 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Nonius Mercury CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 9514 _reflns_number_total 3757 _reflns_number_gt 2525 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04299 _diffrn_reflns_av_sigmaI/netI 0.111 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.36 _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 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; As 0 12 -0.030 2.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 12 -0.726 1.812 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom I(1) 0.67858(6) 0.11214(5) 0.47339(4) 0.0248(2) 1.000 . Uani d ? I(1) 0.32142(6) -0.11214(5) 0.52661(4) 0.0248(2) 1.000 . Uani d ? I(2) 0.53397(7) 0.03891(5) 0.24409(4) 0.0289(2) 1.000 . Uani d ? I(3) 0.07908(7) 0.11593(5) 0.34357(4) 0.0252(2) 1.000 . Uani d ? As(1) 0.38584(10) 0.10491(7) 0.39849(5) 0.0172(2) 1.000 . Uani d ? As(2) 0.41649(10) 0.29157(7) 0.33846(5) 0.0182(2) 1.000 . Uani d ? As(3) 0.28539(10) 0.21488(7) 0.52088(5) 0.0183(2) 1.000 . Uani d ? C(1) 0.6215(10) 0.3370(8) 0.3169(5) 0.029(3) 1.000 . Uani d ? C(2) 0.3096(11) 0.3126(7) 0.2387(5) 0.029(3) 1.000 . Uani d ? C(3) 0.3328(10) 0.3986(6) 0.4109(5) 0.021(2) 1.000 . Uani d ? C(4) 0.3241(11) 0.5089(8) 0.3881(5) 0.030(3) 1.000 . Uani d ? C(5) 0.2552(11) 0.5870(7) 0.4353(6) 0.028(3) 1.000 . Uani d ? C(6) 0.1918(10) 0.5555(7) 0.5069(6) 0.026(3) 1.000 . Uani d ? C(7) 0.2016(10) 0.4461(7) 0.5313(5) 0.021(2) 1.000 . Uani d ? C(8) 0.2711(10) 0.3672(6) 0.4833(5) 0.020(2) 1.000 . Uani d ? C(9) 0.0878(11) 0.1793(8) 0.5611(6) 0.034(3) 1.000 . Uani d ? C(10) 0.4029(10) 0.2300(7) 0.6185(5) 0.027(3) 1.000 . Uani 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 I(1) 0.0182(3) 0.0266(3) 0.0295(4) -0.0018(3) 0.0005(3) 0.0027(3) I(1) 0.0182(3) 0.0266(3) 0.0295(4) -0.0018(3) 0.0005(3) 0.0027(3) I(2) 0.0367(4) 0.0302(3) 0.0200(3) 0.0052(3) 0.0079(3) -0.0011(3) I(3) 0.0215(4) 0.0297(3) 0.0245(4) -0.0025(3) 0.0012(3) -0.0024(3) As(1) 0.0169(5) 0.0179(4) 0.0168(5) -0.0003(4) 0.0033(4) 0.0010(4) As(2) 0.0232(5) 0.0183(4) 0.0132(5) -0.0035(4) 0.0045(4) 0.0006(4) As(3) 0.0204(5) 0.0218(5) 0.0128(5) -0.0003(4) 0.0040(4) 0.0021(4) C(1) 0.030(6) 0.036(5) 0.021(5) -0.009(5) 0.007(4) -0.002(4) C(2) 0.044(6) 0.026(5) 0.018(5) 0.007(5) 0.006(5) -0.001(4) C(3) 0.027(5) 0.014(4) 0.020(5) -0.003(4) -0.001(4) -0.006(4) C(4) 0.038(6) 0.037(5) 0.015(5) -0.007(5) 0.004(4) -0.006(4) C(5) 0.046(7) 0.011(4) 0.026(6) -0.007(4) -0.019(5) -0.001(4) C(6) 0.028(6) 0.018(5) 0.031(6) 0.006(4) -0.006(4) -0.003(4) C(7) 0.025(5) 0.028(5) 0.010(4) -0.001(4) 0.001(4) 0.004(4) C(8) 0.024(5) 0.017(4) 0.017(5) -0.005(4) 0.003(4) -0.007(4) C(9) 0.031(6) 0.042(6) 0.028(6) -0.008(5) 0.011(5) -0.003(5) C(10) 0.033(6) 0.033(5) 0.014(5) 0.003(4) -0.009(4) 0.003(4) #============================================================================== # REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2525 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_all 0.0480 _refine_ls_wR_factor_ref 0.0460 _refine_ls_goodness_of_fit_all 1.160 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.42 _refine_diff_density_max 1.32 #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 AS1 2.8456(11) . . ? I1 AS1 3.4344(11) . . ? I2 AS1 2.8376(11) . . ? I3 AS1 3.0202(11) . . ? AS1 AS2 2.6067(12) . . ? AS1 AS3 2.4785(12) . . ? AS2 C1 1.928(9) . . ? AS2 C2 1.922(9) . . ? AS2 C3 1.944(8) . . ? AS3 C8 1.926(8) . . ? AS3 C9 1.922(10) . . ? AS3 C10 1.924(10) . . ? C1 H1 0.948(9) . . ? C1 H2 0.949(10) . . ? C1 H3 0.953(10) . . ? C2 H4 0.952(10) . . ? C2 H5 0.952(10) . . ? C2 H6 0.945(11) . . ? C3 C4 1.393(12) . . ? C3 C8 1.386(12) . . ? C4 C5 1.380(12) . . ? C4 H7 0.950(9) . . ? C5 C6 1.38(1) . . ? C5 H8 0.953(9) . . ? C6 C7 1.373(13) . . ? C6 H9 0.951(9) . . ? C7 C8 1.384(12) . . ? C7 H10 0.948(9) . . ? C9 H11 0.951(10) . . ? C9 H12 0.948(10) . . ? C9 H13 0.950(9) . . ? C10 H14 0.949(10) . . ? C10 H15 0.952(10) . . ? C10 H16 0.948(10) . . ? #------------------------------------------------------------------------------ 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 AS1 I1 AS1 95.48(3) . . . ? I1 AS1 I1 84.52(3) . . . ? I1 AS1 I2 171.52(4) . . . ? I1 AS1 I3 89.24(3) . . . ? I1 AS1 AS2 87.29(4) . . . ? I1 AS1 AS3 92.74(4) . . . ? I1 AS1 I2 94.19(3) 3_656 3_656 3_656 ? I1 AS1 I3 114.36(3) 3_656 3_656 3_656 ? I1 AS1 AS2 80.44(3) 3_656 3_656 3_656 ? I1 AS1 AS3 164.49(4) 3_656 3_656 3_656 ? I2 AS1 I3 98.91(3) . . . ? I2 AS1 AS2 84.23(4) . . . ? I2 AS1 AS3 86.27(4) . . . ? I3 AS1 AS2 164.40(4) . . . ? I3 AS1 AS3 80.79(3) . . . ? AS2 AS1 AS3 84.19(4) . . . ? AS1 AS2 C1 122.1(3) . . . ? AS1 AS2 C2 118.8(3) . . . ? AS1 AS2 C3 104.2(3) . . . ? C1 AS2 C2 101.5(4) . . . ? C1 AS2 C3 102.7(4) . . . ? C2 AS2 C3 105.5(4) . . . ? AS1 AS3 C8 107.8(3) . . . ? AS1 AS3 C9 114.7(3) . . . ? AS1 AS3 C10 116.3(3) . . . ? C8 AS3 C9 105.9(4) . . . ? C8 AS3 C10 107.2(4) . . . ? C9 AS3 C10 104.2(4) . . . ? AS2 C1 H1 109.6(7) . . . ? AS2 C1 H2 109.6(7) . . . ? AS2 C1 H3 109.4(7) . . . ? H1 C1 H2 109.7(9) . . . ? H1 C1 H3 109.3(10) . . . ? H2 C1 H3 109.3(9) . . . ? AS2 C2 H4 109.3(7) . . . ? AS2 C2 H5 109.2(8) . . . ? AS2 C2 H6 109.7(7) . . . ? H4 C2 H5 109.1(10) . . . ? H4 C2 H6 109.8(10) . . . ? H5 C2 H6 109.7(10) . . . ? AS2 C3 C4 118.8(6) . . . ? AS2 C3 C8 121.1(6) . . . ? C4 C3 C8 120.0(8) . . . ? C3 C4 C5 120.1(8) . . . ? C3 C4 H7 119.8(8) . . . ? C4 C5 C6 119.7(8) . . . ? C4 C5 H8 120.1(10) . . . ? C6 C5 H8 120.2(9) . . . ? C5 C6 C7 119.9(8) . . . ? C5 C6 H9 119.9(10) . . . ? C7 C6 H9 120.2(10) . . . ? C6 C7 C8 121.2(9) . . . ? C6 C7 H10 119.4(10) . . . ? C8 C7 H10 119.5(9) . . . ? AS3 C8 C3 121.8(6) . . . ? AS3 C8 C7 119.0(7) . . . ? C3 C8 C7 119.0(8) . . . ? AS3 C9 H11 109.3(7) . . . ? AS3 C9 H12 109.5(8) . . . ? AS3 C9 H13 109.4(7) . . . ? H11 C9 H12 109.6(9) . . . ? H11 C9 H13 109.4(10) . . . ? H12 C9 H13 109.7(9) . . . ? AS3 C10 H14 109.4(8) . . . ? AS3 C10 H15 109.2(7) . . . ? AS3 C10 H16 109.5(7) . . . ? H14 C10 H15 109.4(9) . . . ? H14 C10 H16 109.8(9) . . . ? H15 C10 H16 109.5(10) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #============================================================================== # End of CIF #==============================================================================