Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_category FO loop_ _publ_author_name 'M Lappert ' 'Yanxiang Cheng.' 'David J. Doyle ' 'P. B. Hitchcock' data_(1)-mar1703 _database_code_depnum_ccdc_archive 'CCDC 609658' _audit_creation_date 2003-03-25T10:53:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common "['C6H3iPr2NHCHCPhCHNC6H3iPr2]" _chemical_formula_moiety 'C33 H42 N2' _chemical_formula_sum 'C33 H42 N2' _chemical_formula_weight 466.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 11.2223(2) _cell_length_b 13.0825(3) _cell_length_c 19.4125(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2850.06(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17958 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourrless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0955 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_number 27985 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 2504 _reflns_number_gt 2020 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H on the N atom was refined with occupancy 0.5. 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^)+(0.0573P)^2^+1.2220P] 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_number_reflns 2504 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.228 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.033 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N N 0.21054(14) 0.15393(11) 0.43679(7) 0.0327(4) Uani 1 1 d . . . H1N H 0.228(3) 0.212(2) 0.4144(17) 0.025(9) Uiso 0.5 1 d P . . C1 C 0.21022(15) 0.16325(13) 0.50421(8) 0.0288(4) Uani 1 1 d . . . H1 H 0.1811 0.1074 0.5306 0.035 Uiso 1 1 calc R . . C2 C 0.25 0.25 0.53981(11) 0.0273(5) Uani 1 2 d S . . C3 C 0.25 0.25 0.61630(11) 0.0292(5) Uani 1 2 d S . . C4 C 0.28034(16) 0.16250(15) 0.65330(9) 0.0377(5) Uani 1 1 d . . . H4 H 0.3022 0.1021 0.6292 0.045 Uiso 1 1 calc R . . C5 C 0.27916(19) 0.16230(19) 0.72460(9) 0.0524(6) Uani 1 1 d . . . H5 H 0.2985 0.1016 0.7491 0.063 Uiso 1 1 calc R . . C6 C 0.25 0.25 0.76020(14) 0.0609(9) Uani 1 2 d S . . H6 H 0.25 0.25 0.8091 0.073 Uiso 1 2 calc SR . . C7 C 0.16724(17) 0.06422(13) 0.40296(8) 0.0314(4) Uani 1 1 d . . . C8 C 0.05052(17) 0.06420(14) 0.37802(9) 0.0377(5) Uani 1 1 d . . . C9 C 0.0111(2) -0.02233(16) 0.34277(10) 0.0487(5) Uani 1 1 d . . . H9 H -0.0684 -0.0246 0.3261 0.058 Uiso 1 1 calc R . . C10 C 0.0848(2) -0.10394(17) 0.33179(11) 0.0546(6) Uani 1 1 d . . . H10 H 0.0562 -0.1623 0.3078 0.066 Uiso 1 1 calc R . . C11 C 0.2007(2) -0.10140(16) 0.35550(11) 0.0524(6) Uani 1 1 d . . . H11 H 0.2517 -0.1578 0.3466 0.063 Uiso 1 1 calc R . . C12 C 0.24429(19) -0.01833(14) 0.39196(9) 0.0399(5) Uani 1 1 d . . . C13 C -0.03225(19) 0.15484(16) 0.38889(12) 0.0517(6) Uani 1 1 d . . . H13 H 0.0175 0.2127 0.4064 0.062 Uiso 1 1 calc R . . C14 C -0.0903(3) 0.1904(2) 0.32254(15) 0.0815(9) Uani 1 1 d . . . H14C H -0.1422 0.1363 0.3047 0.122 Uiso 1 1 calc R . . H14B H -0.0285 0.206 0.2885 0.122 Uiso 1 1 calc R . . H14A H -0.1377 0.2519 0.3316 0.122 Uiso 1 1 calc R . . C15 C -0.1235(3) 0.1311(2) 0.44363(15) 0.0846(9) Uani 1 1 d . . . H15C H -0.1703 0.1926 0.4535 0.127 Uiso 1 1 calc R . . H15B H -0.0829 0.1085 0.4857 0.127 Uiso 1 1 calc R . . H15A H -0.1765 0.0768 0.4273 0.127 Uiso 1 1 calc R . . C16 C 0.3724(2) -0.01597(18) 0.41731(12) 0.0553(6) Uani 1 1 d . . . H16 H 0.3736 0.0268 0.46 0.066 Uiso 1 1 calc R . . C17 C 0.4222(2) -0.1199(2) 0.43663(15) 0.0724(8) Uani 1 1 d . . . H17C H 0.3738 -0.1497 0.4735 0.109 Uiso 1 1 calc R . . H17B H 0.5046 -0.1122 0.4526 0.109 Uiso 1 1 calc R . . H17A H 0.4204 -0.1649 0.3963 0.109 Uiso 1 1 calc R . . C18 C 0.4524(2) 0.0360(2) 0.36543(18) 0.0885(10) Uani 1 1 d . . . H18C H 0.4497 -0.0015 0.3217 0.133 Uiso 1 1 calc R . . H18B H 0.5344 0.0368 0.3828 0.133 Uiso 1 1 calc R . . H18A H 0.4252 0.1063 0.3581 0.133 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 N 0.0498(9) 0.0259(8) 0.0225(7) -0.0013(6) 0.0012(6) -0.0015(7) C1 0.0344(9) 0.0276(9) 0.0245(8) 0.0033(7) 0.0011(7) 0.0027(7) C2 0.0301(12) 0.0295(13) 0.0223(11) 0 0 0.0044(10) C3 0.0268(12) 0.0388(14) 0.0220(11) 0 0 -0.0042(11) C4 0.0404(11) 0.0455(11) 0.0273(9) 0.0064(8) -0.0047(7) -0.0026(8) C5 0.0588(14) 0.0692(15) 0.0293(10) 0.0155(10) -0.0089(9) -0.0111(11) C6 0.071(2) 0.094(3) 0.0179(12) 0 0 -0.020(2) C7 0.0453(11) 0.0270(9) 0.0218(8) 0.0004(7) 0.0019(7) -0.0036(8) C8 0.0434(11) 0.0342(10) 0.0354(9) 0.0043(8) 0.0002(8) -0.0039(8) C9 0.0516(13) 0.0463(13) 0.0482(11) -0.0006(10) -0.0101(9) -0.0114(10) C10 0.0714(15) 0.0423(12) 0.0503(12) -0.0150(10) -0.0063(11) -0.0119(12) C11 0.0656(15) 0.0385(12) 0.0531(12) -0.0173(9) -0.0014(10) 0.0058(10) C12 0.0484(11) 0.0354(10) 0.0359(9) -0.0066(8) -0.0006(8) 0.0029(9) C13 0.0444(12) 0.0399(12) 0.0709(14) 0.0062(10) -0.0035(10) -0.0001(9) C14 0.0640(16) 0.088(2) 0.093(2) 0.0381(17) 0.0030(14) 0.0270(15) C15 0.097(2) 0.0702(19) 0.086(2) 0.0082(15) 0.0349(17) 0.0273(16) C16 0.0510(13) 0.0501(14) 0.0648(14) -0.0193(11) -0.0059(10) 0.0097(11) C17 0.0597(15) 0.0751(18) 0.0824(18) 0.0167(14) -0.0016(13) 0.0150(14) C18 0.0511(16) 0.0654(18) 0.149(3) 0.0344(19) -0.0020(17) -0.0009(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N C1 1.314(2) . ? N C7 1.430(2) . ? C1 C2 1.402(2) . ? C2 C1 1.402(2) 2 ? C2 C3 1.485(3) . ? C3 C4 1.394(2) . ? C3 C4 1.394(2) 2 ? C4 C5 1.384(2) . ? C5 C6 1.379(3) . ? C6 C5 1.379(3) 2 ? C7 C8 1.396(3) . ? C7 C12 1.400(3) . ? C8 C9 1.395(3) . ? C8 C13 1.521(3) . ? C9 C10 1.367(3) . ? C10 C11 1.380(3) . ? C11 C12 1.386(3) . ? C12 C16 1.520(3) . ? C13 C15 1.508(3) . ? C13 C14 1.516(3) . ? C16 C18 1.511(4) . ? C16 C17 1.517(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 C1 N C7 122.18(15) . . ? N C1 C2 124.41(16) . . ? C1 C2 C1 120.9(2) . 2 ? C1 C2 C3 119.54(10) . . ? C1 C2 C3 119.54(10) 2 . ? C4 C3 C4 117.9(2) . 2 ? C4 C3 C2 121.03(11) . . ? C4 C3 C2 121.03(11) 2 . ? C5 C4 C3 121.0(2) . . ? C6 C5 C4 120.1(2) . . ? C5 C6 C5 119.8(2) . 2 ? C8 C7 C12 121.77(16) . . ? C8 C7 N 118.56(16) . . ? C12 C7 N 119.56(17) . . ? C9 C8 C7 117.88(18) . . ? C9 C8 C13 120.48(18) . . ? C7 C8 C13 121.64(17) . . ? C10 C9 C8 121.3(2) . . ? C9 C10 C11 119.93(19) . . ? C10 C11 C12 121.5(2) . . ? C11 C12 C7 117.68(19) . . ? C11 C12 C16 121.02(19) . . ? C7 C12 C16 121.28(17) . . ? C15 C13 C14 111.7(2) . . ? C15 C13 C8 110.59(18) . . ? C14 C13 C8 112.6(2) . . ? C18 C16 C17 110.4(2) . . ? C18 C16 C12 110.8(2) . . ? C17 C16 C12 114.2(2) . . ? #===END data_(2)-mar903 _database_code_depnum_ccdc_archive 'CCDC 609659' _audit_creation_date 2003-03-13T15:50:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Li(thf)2{C6H3iPr2NCHCPhCHNC6H3iPr2}]' ; _chemical_formula_moiety 'C41 H57 Li1 N2 O2' _chemical_formula_sum 'C41 H57 Li1 N2 O2' _chemical_formula_weight 616.83 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8630(2) _cell_length_b 19.5833(2) _cell_length_c 20.7986(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7683.00(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40178 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.07 _diffrn_reflns_av_unetI/netI 0.0269 _diffrn_reflns_number 76330 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6731 _reflns_number_gt 5411 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0706P)^2^+5.0881P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6731 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.379 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.039 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 O 0.24046(10) 0.05300(8) 0.69250(7) 0.0565(5) Uani 1 1 d . . . O2 O 0.19195(9) 0.20100(8) 0.70147(8) 0.0525(4) Uani 1 1 d . . . N1 N 0.27880(8) 0.16508(8) 0.56879(7) 0.0287(4) Uani 1 1 d . . . N2 N 0.36349(8) 0.17101(8) 0.68671(7) 0.0300(4) Uani 1 1 d . . . C1 C 0.31662(10) 0.21986(9) 0.55806(9) 0.0273(4) Uani 1 1 d . . . H1 H 0.3138 0.2381 0.5158 0.033 Uiso 1 1 calc R . . C2 C 0.36138(10) 0.25565(9) 0.60132(9) 0.0281(4) Uani 1 1 d . . . C3 C 0.38583(10) 0.22730(9) 0.65958(9) 0.0290(4) Uani 1 1 d . . . H3 H 0.4222 0.2516 0.6813 0.035 Uiso 1 1 calc R . . C4 C 0.38650(10) 0.32385(10) 0.58061(9) 0.0298(4) Uani 1 1 d . . . C5 C 0.34479(12) 0.36403(10) 0.53969(10) 0.0378(5) Uani 1 1 d . . . H5 H 0.3005 0.3467 0.5253 0.045 Uiso 1 1 calc R . . C6 C 0.36604(13) 0.42825(11) 0.51952(11) 0.0444(5) Uani 1 1 d . . . H6 H 0.3372 0.4532 0.4904 0.053 Uiso 1 1 calc R . . C7 C 0.42849(12) 0.45616(11) 0.54123(11) 0.0449(6) Uani 1 1 d . . . H7 H 0.4425 0.5007 0.5283 0.054 Uiso 1 1 calc R . . C8 C 0.47032(12) 0.41831(11) 0.58206(12) 0.0459(6) Uani 1 1 d . . . H8 H 0.5135 0.4372 0.5976 0.055 Uiso 1 1 calc R . . C9 C 0.45057(11) 0.35308(10) 0.60093(11) 0.0380(5) Uani 1 1 d . . . H9 H 0.4811 0.3276 0.6282 0.046 Uiso 1 1 calc R . . C10 C 0.24577(10) 0.13617(9) 0.51317(8) 0.0291(4) Uani 1 1 d . . . C11 C 0.27703(11) 0.07883(10) 0.48393(9) 0.0356(5) Uani 1 1 d . . . C12 C 0.24504(13) 0.05110(11) 0.42957(10) 0.0436(5) Uani 1 1 d . . . H12 H 0.2661 0.0127 0.4092 0.052 Uiso 1 1 calc R . . C13 C 0.18344(12) 0.07812(11) 0.40467(10) 0.0433(5) Uani 1 1 d . . . H13 H 0.1624 0.0585 0.3675 0.052 Uiso 1 1 calc R . . C14 C 0.15256(11) 0.13372(12) 0.43402(10) 0.0403(5) Uani 1 1 d . . . H14 H 0.11 0.1521 0.4168 0.048 Uiso 1 1 calc R . . C15 C 0.18244(10) 0.16368(10) 0.48848(10) 0.0346(5) Uani 1 1 d . . . C16 C 0.34562(13) 0.04941(12) 0.51030(11) 0.0477(6) Uani 1 1 d . . . H16 H 0.3487 0.0627 0.5566 0.057 Uiso 1 1 calc R . . C17 C 0.40924(14) 0.08064(16) 0.47618(15) 0.0688(8) Uani 1 1 d . . . H17A H 0.453 0.0612 0.4938 0.103 Uiso 1 1 calc R . . H17B H 0.4092 0.1302 0.4826 0.103 Uiso 1 1 calc R . . H17C H 0.4065 0.0706 0.4301 0.103 Uiso 1 1 calc R . . C18 C 0.34870(18) -0.02835(14) 0.50713(16) 0.0730(8) Uani 1 1 d . . . H18A H 0.3939 -0.0442 0.5249 0.109 Uiso 1 1 calc R . . H18B H 0.3447 -0.0431 0.4623 0.109 Uiso 1 1 calc R . . H18C H 0.3095 -0.0476 0.5322 0.109 Uiso 1 1 calc R . . C19 C 0.14440(12) 0.22294(12) 0.52060(12) 0.0474(6) Uani 1 1 d . . . H19 H 0.1761 0.2413 0.555 0.057 Uiso 1 1 calc R . . C20 C 0.1281(2) 0.28091(16) 0.47409(19) 0.0896(11) Uani 1 1 d . . . H20A H 0.104 0.3179 0.4972 0.134 Uiso 1 1 calc R . . H20B H 0.0974 0.264 0.4396 0.134 Uiso 1 1 calc R . . H20C H 0.1724 0.2981 0.4556 0.134 Uiso 1 1 calc R . . C21 C 0.07699(16) 0.19840(18) 0.55212(16) 0.0793(9) Uani 1 1 d . . . H21A H 0.0532 0.237 0.573 0.119 Uiso 1 1 calc R . . H21B H 0.0884 0.1636 0.5844 0.119 Uiso 1 1 calc R . . H21C H 0.0456 0.1787 0.5195 0.119 Uiso 1 1 calc R . . C22 C 0.39877(10) 0.14709(10) 0.74294(9) 0.0315(4) Uani 1 1 d . . . C23 C 0.43852(11) 0.08630(10) 0.73829(10) 0.0370(5) Uani 1 1 d . . . C24 C 0.46822(13) 0.05918(12) 0.79398(12) 0.0488(6) Uani 1 1 d . . . H24 H 0.4949 0.0181 0.7913 0.059 Uiso 1 1 calc R . . C25 C 0.45993(13) 0.09014(13) 0.85242(11) 0.0518(6) Uani 1 1 d . . . H25 H 0.4806 0.0707 0.8898 0.062 Uiso 1 1 calc R . . C26 C 0.42154(13) 0.14941(14) 0.85670(11) 0.0529(6) Uani 1 1 d . . . H26 H 0.4158 0.1706 0.8975 0.063 Uiso 1 1 calc R . . C27 C 0.39078(12) 0.17938(12) 0.80265(10) 0.0433(5) Uani 1 1 d . . . C28 C 0.44967(13) 0.05255(12) 0.67346(12) 0.0507(6) Uani 1 1 d . . . H28 H 0.4068 0.0626 0.6468 0.061 Uiso 1 1 calc R . . C29 C 0.4570(2) -0.02492(15) 0.67691(18) 0.0895(11) Uani 1 1 d . . . H29A H 0.4638 -0.0433 0.6335 0.134 Uiso 1 1 calc R . . H29B H 0.4139 -0.0445 0.6958 0.134 Uiso 1 1 calc R . . H29C H 0.4979 -0.0368 0.7037 0.134 Uiso 1 1 calc R . . C30 C 0.51241(18) 0.08382(18) 0.63931(14) 0.0783(9) Uani 1 1 d . . . H30A H 0.5187 0.0617 0.5974 0.118 Uiso 1 1 calc R . . H30B H 0.5552 0.0773 0.6653 0.118 Uiso 1 1 calc R . . H30C H 0.5041 0.1328 0.633 0.118 Uiso 1 1 calc R . . C31 C 0.34943(16) 0.24574(16) 0.81046(12) 0.0704(9) Uani 1 1 d . . . H31 H 0.3259 0.2557 0.7684 0.084 Uiso 1 1 calc R . . C32 C 0.3985(2) 0.30571(17) 0.8257(2) 0.1137(16) Uani 1 1 d . . . H32A H 0.3703 0.3475 0.8301 0.171 Uiso 1 1 calc R . . H32B H 0.4328 0.3113 0.7908 0.171 Uiso 1 1 calc R . . H32C H 0.4237 0.2967 0.866 0.171 Uiso 1 1 calc R . . C33 C 0.2915(2) 0.2380(3) 0.86044(16) 0.1258(19) Uani 1 1 d . . . H33A H 0.2654 0.2811 0.8644 0.189 Uiso 1 1 calc R . . H33B H 0.3127 0.2262 0.902 0.189 Uiso 1 1 calc R . . H33C H 0.2589 0.2017 0.8472 0.189 Uiso 1 1 calc R . . C34 C 0.1961(2) 0.00863(15) 0.65574(14) 0.0829(11) Uani 1 1 d . . . H34A H 0.1508 0.0316 0.6452 0.1 Uiso 1 1 calc R . . H34B H 0.2199 -0.0043 0.6151 0.1 Uiso 1 1 calc R . . C35 C 0.1833(3) -0.05043(19) 0.69415(18) 0.1208(18) Uani 1 1 d . . . H35A H 0.1317 -0.0573 0.6999 0.145 Uiso 1 1 calc R . . H35B H 0.2031 -0.0914 0.6729 0.145 Uiso 1 1 calc R . . C36 C 0.2163(3) -0.0404(2) 0.75455(19) 0.139(2) Uani 1 1 d . . . H36A H 0.2496 -0.0783 0.7633 0.166 Uiso 1 1 calc R . . H36B H 0.18 -0.0399 0.7889 0.166 Uiso 1 1 calc R . . C37 C 0.25375(16) 0.02312(13) 0.75395(12) 0.0604(7) Uani 1 1 d . . . H37A H 0.2364 0.0534 0.7887 0.073 Uiso 1 1 calc R . . H37B H 0.3052 0.0154 0.7601 0.073 Uiso 1 1 calc R . . C38 C 0.13230(16) 0.17768(17) 0.73796(17) 0.0773(9) Uani 1 1 d . . . H38A H 0.1486 0.1515 0.7759 0.093 Uiso 1 1 calc R . . H38B H 0.1022 0.1475 0.7113 0.093 Uiso 1 1 calc R . . C39 C 0.0920(2) 0.2373(2) 0.7585(2) 0.1125(15) Uani 1 1 d . . . H39A H 0.0439 0.2367 0.7395 0.135 Uiso 1 1 calc R . . H39B H 0.0876 0.2383 0.8059 0.135 Uiso 1 1 calc R . . C40 C 0.1313(3) 0.2953(2) 0.7360(4) 0.177(3) Uani 1 1 d . . . H40A H 0.0996 0.3256 0.7109 0.212 Uiso 1 1 calc R . . H40B H 0.1495 0.3215 0.7732 0.212 Uiso 1 1 calc R . . C41 C 0.18912(15) 0.27396(13) 0.69662(13) 0.0580(7) Uani 1 1 d . . . H41A H 0.234 0.2945 0.712 0.07 Uiso 1 1 calc R . . H41B H 0.1814 0.288 0.6515 0.07 Uiso 1 1 calc R . . Li Li 0.26656(17) 0.14186(17) 0.66152(15) 0.0347(7) Uani 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 O1 0.0848(13) 0.0443(9) 0.0404(9) 0.0113(7) -0.0172(8) -0.0270(9) O2 0.0468(9) 0.0535(10) 0.0571(10) -0.0053(8) 0.0195(8) -0.0024(8) N1 0.0306(8) 0.0296(8) 0.0260(8) 0.0013(6) -0.0001(6) -0.0018(7) N2 0.0332(8) 0.0316(8) 0.0253(8) 0.0009(7) -0.0016(7) 0.0025(7) C1 0.0301(10) 0.0289(9) 0.0228(9) 0.0017(7) 0.0022(7) 0.0012(8) C2 0.0287(9) 0.0274(9) 0.0282(9) -0.0003(8) 0.0045(8) 0.0001(8) C3 0.0270(9) 0.0311(10) 0.0290(10) -0.0053(8) -0.0005(8) 0.0010(8) C4 0.0307(10) 0.0300(10) 0.0285(9) -0.0031(8) 0.0075(8) -0.0003(8) C5 0.0445(12) 0.0348(11) 0.0340(11) 0.0021(9) -0.0030(9) -0.0062(9) C6 0.0581(14) 0.0355(11) 0.0396(12) 0.0068(10) 0.0038(10) 0.0010(10) C7 0.0495(13) 0.0300(11) 0.0550(14) 0.0019(10) 0.0201(11) -0.0042(10) C8 0.0322(11) 0.0368(11) 0.0687(15) -0.0068(11) 0.0112(11) -0.0061(9) C9 0.0293(10) 0.0342(11) 0.0504(12) -0.0016(9) 0.0037(9) -0.0001(9) C10 0.0324(10) 0.0304(10) 0.0246(9) 0.0022(8) 0.0031(8) -0.0079(8) C11 0.0442(12) 0.0352(11) 0.0275(10) 0.0010(8) 0.0044(9) -0.0004(9) C12 0.0600(14) 0.0388(11) 0.0319(11) -0.0059(9) 0.0047(10) 0.0000(10) C13 0.0494(13) 0.0493(13) 0.0310(11) -0.0067(10) -0.0008(10) -0.0141(11) C14 0.0329(11) 0.0497(13) 0.0384(11) -0.0016(10) -0.0038(9) -0.0092(10) C15 0.0319(10) 0.0370(11) 0.0349(10) -0.0030(9) 0.0010(8) -0.0079(9) C16 0.0583(14) 0.0487(13) 0.0362(12) -0.0071(10) -0.0026(10) 0.0179(11) C17 0.0465(15) 0.0769(19) 0.083(2) -0.0028(16) -0.0045(14) 0.0120(14) C18 0.089(2) 0.0539(16) 0.0765(19) 0.0040(14) -0.0004(16) 0.0267(15) C19 0.0345(11) 0.0542(14) 0.0533(14) -0.0170(11) -0.0090(10) 0.0053(10) C20 0.108(3) 0.0534(17) 0.108(3) 0.0030(17) 0.015(2) 0.0268(18) C21 0.0662(19) 0.099(2) 0.073(2) -0.0210(18) 0.0253(16) 0.0041(17) C22 0.0291(10) 0.0352(10) 0.0301(10) 0.0036(8) -0.0027(8) 0.0009(8) C23 0.0337(11) 0.0351(11) 0.0421(12) 0.0010(9) -0.0056(9) 0.0005(9) C24 0.0495(13) 0.0401(12) 0.0569(15) 0.0073(11) -0.0113(11) 0.0074(10) C25 0.0552(15) 0.0569(14) 0.0432(13) 0.0169(11) -0.0123(11) 0.0060(12) C26 0.0575(15) 0.0722(17) 0.0291(11) 0.0030(11) -0.0049(10) 0.0125(13) C27 0.0434(12) 0.0565(14) 0.0299(11) -0.0008(10) -0.0044(9) 0.0165(11) C28 0.0493(14) 0.0486(13) 0.0541(14) -0.0146(11) -0.0121(11) 0.0159(11) C29 0.111(3) 0.0530(17) 0.105(3) -0.0286(18) -0.005(2) 0.0158(18) C30 0.092(2) 0.089(2) 0.0542(16) -0.0179(16) 0.0186(16) 0.0083(18) C31 0.082(2) 0.096(2) 0.0329(12) -0.0189(13) -0.0170(12) 0.0546(18) C32 0.162(4) 0.067(2) 0.112(3) -0.040(2) -0.059(3) 0.055(2) C33 0.106(3) 0.220(5) 0.0512(18) -0.027(2) 0.0006(18) 0.101(3) C34 0.131(3) 0.0682(19) 0.0499(16) 0.0054(14) -0.0263(17) -0.0485(19) C35 0.195(5) 0.081(2) 0.086(2) 0.026(2) -0.069(3) -0.073(3) C36 0.214(5) 0.107(3) 0.096(3) 0.056(2) -0.088(3) -0.104(3) C37 0.0780(18) 0.0554(15) 0.0480(14) 0.0185(12) -0.0191(13) -0.0231(14) C38 0.0563(17) 0.088(2) 0.087(2) -0.0036(18) 0.0371(16) -0.0085(16) C39 0.079(2) 0.120(3) 0.138(4) 0.014(3) 0.055(3) 0.028(2) C40 0.173(5) 0.076(3) 0.280(8) 0.014(4) 0.135(5) 0.048(3) C41 0.0615(16) 0.0518(15) 0.0608(16) -0.0071(12) 0.0012(13) 0.0062(12) Li 0.0377(18) 0.0381(18) 0.0282(16) 0.0041(14) 0.0009(13) -0.0047(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 C37 1.428(3) . ? O1 C34 1.428(3) . ? O1 Li 1.920(4) . ? O2 C38 1.432(3) . ? O2 C41 1.433(3) . ? O2 Li 2.003(4) . ? N1 C1 1.307(2) . ? N1 C10 1.431(2) . ? N1 Li 1.995(3) . ? N2 C3 1.308(2) . ? N2 C22 1.425(2) . ? N2 Li 1.986(4) . ? C1 C2 1.419(3) . ? C2 C3 1.410(3) . ? C2 C4 1.481(3) . ? C4 C5 1.401(3) . ? C4 C9 1.402(3) . ? C5 C6 1.385(3) . ? C6 C7 1.375(3) . ? C7 C8 1.376(3) . ? C8 C9 1.387(3) . ? C10 C11 1.407(3) . ? C10 C15 1.407(3) . ? C11 C12 1.392(3) . ? C11 C16 1.519(3) . ? C12 C13 1.378(3) . ? C13 C14 1.378(3) . ? C14 C15 1.394(3) . ? C15 C19 1.519(3) . ? C16 C17 1.522(4) . ? C16 C18 1.525(4) . ? C19 C21 1.509(4) . ? C19 C20 1.523(4) . ? C22 C27 1.402(3) . ? C22 C23 1.410(3) . ? C23 C24 1.392(3) . ? C23 C28 1.516(3) . ? C24 C25 1.367(3) . ? C25 C26 1.371(3) . ? C26 C27 1.395(3) . ? C27 C31 1.524(3) . ? C28 C30 1.510(4) . ? C28 C29 1.525(4) . ? C31 C33 1.516(5) . ? C31 C32 1.528(5) . ? C34 C35 1.426(4) . ? C35 C36 1.415(4) . ? C36 C37 1.431(4) . ? C38 C39 1.456(5) . ? C39 C40 1.435(6) . ? C40 C41 1.426(5) . ? 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 C37 O1 C34 109.44(18) . . ? C37 O1 Li 128.82(17) . . ? C34 O1 Li 121.47(18) . . ? C38 O2 C41 109.0(2) . . ? C38 O2 Li 125.99(19) . . ? C41 O2 Li 124.98(17) . . ? C1 N1 C10 115.11(15) . . ? C1 N1 Li 114.52(15) . . ? C10 N1 Li 129.88(15) . . ? C3 N2 C22 118.74(16) . . ? C3 N2 Li 115.15(16) . . ? C22 N2 Li 123.51(15) . . ? N1 C1 C2 128.44(17) . . ? C3 C2 C1 123.02(17) . . ? C3 C2 C4 120.02(17) . . ? C1 C2 C4 116.83(16) . . ? N2 C3 C2 126.66(17) . . ? C5 C4 C9 115.96(18) . . ? C5 C4 C2 120.24(17) . . ? C9 C4 C2 123.78(18) . . ? C6 C5 C4 122.1(2) . . ? C7 C6 C5 120.6(2) . . ? C6 C7 C8 118.7(2) . . ? C7 C8 C9 121.1(2) . . ? C8 C9 C4 121.5(2) . . ? C11 C10 C15 120.24(17) . . ? C11 C10 N1 118.87(17) . . ? C15 C10 N1 120.88(17) . . ? C12 C11 C10 118.74(19) . . ? C12 C11 C16 120.97(19) . . ? C10 C11 C16 120.26(18) . . ? C13 C12 C11 121.4(2) . . ? C14 C13 C12 119.58(19) . . ? C13 C14 C15 121.4(2) . . ? C14 C15 C10 118.58(19) . . ? C14 C15 C19 119.18(19) . . ? C10 C15 C19 122.20(18) . . ? C11 C16 C17 110.5(2) . . ? C11 C16 C18 113.3(2) . . ? C17 C16 C18 110.5(2) . . ? C21 C19 C15 110.2(2) . . ? C21 C19 C20 110.1(2) . . ? C15 C19 C20 112.7(2) . . ? C27 C22 C23 119.91(18) . . ? C27 C22 N2 121.92(17) . . ? C23 C22 N2 118.01(17) . . ? C24 C23 C22 118.62(19) . . ? C24 C23 C28 121.20(19) . . ? C22 C23 C28 120.17(18) . . ? C25 C24 C23 121.6(2) . . ? C24 C25 C26 119.6(2) . . ? C25 C26 C27 121.6(2) . . ? C26 C27 C22 118.7(2) . . ? C26 C27 C31 119.1(2) . . ? C22 C27 C31 122.27(18) . . ? C30 C28 C23 110.5(2) . . ? C30 C28 C29 110.8(2) . . ? C23 C28 C29 113.8(2) . . ? C33 C31 C27 110.9(3) . . ? C33 C31 C32 111.8(3) . . ? C27 C31 C32 111.6(2) . . ? C35 C34 O1 107.0(2) . . ? C36 C35 C34 108.1(3) . . ? C35 C36 C37 109.3(3) . . ? O1 C37 C36 106.1(2) . . ? O2 C38 C39 108.1(3) . . ? C40 C39 C38 105.6(3) . . ? C41 C40 C39 110.5(3) . . ? C40 C41 O2 106.3(3) . . ? O1 Li N2 114.09(18) . . ? O1 Li N1 124.11(18) . . ? N2 Li N1 94.76(15) . . ? O1 Li O2 101.80(16) . . ? N2 Li O2 111.79(17) . . ? N1 Li O2 110.53(17) . . ? #===END data_(3)-jan704 _database_code_depnum_ccdc_archive 'CCDC 609660' _audit_creation_date 2004-01-20T09:32:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H57 Li1 N4' _chemical_formula_sum 'C39 H57 Li1 N4' _chemical_formula_weight 588.83 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2941(2) _cell_length_b 18.5693(3) _cell_length_c 19.6964(4) _cell_angle_alpha 90 _cell_angle_beta 100.636(1) _cell_angle_gamma 90 _cell_volume 3700.36(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34924 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.449208E-1 _diffrn_orient_matrix_ub_12 0.84152E-2 _diffrn_orient_matrix_ub_13 0.401898E-1 _diffrn_orient_matrix_ub_21 0.88016E-1 _diffrn_orient_matrix_ub_22 0.29576E-2 _diffrn_orient_matrix_ub_23 0.314238E-1 _diffrn_orient_matrix_ub_31 0.22161E-2 _diffrn_orient_matrix_ub_32 0.531085E-1 _diffrn_orient_matrix_ub_33 -0.81182E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_number 49118 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6471 _reflns_number_gt 5094 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0578P)^2^+1.4701P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6471 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.239 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.033 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Li Li 0.0826(3) 0.56908(14) 0.25155(14) 0.0323(6) Uani 1 1 d . . . N1 N 0.25762(12) 0.55855(7) 0.21524(6) 0.0265(3) Uani 1 1 d . . . N2 N 0.05417(12) 0.46283(7) 0.25934(6) 0.0261(3) Uani 1 1 d . . . N3 N -0.04553(15) 0.63351(8) 0.17902(8) 0.0438(4) Uani 1 1 d . . . N4 N -0.00049(15) 0.63325(8) 0.32983(8) 0.0395(4) Uani 1 1 d . . . C1 C 0.26942(15) 0.49988(8) 0.17956(8) 0.0257(3) Uani 1 1 d . . . H1 H 0.3413 0.4993 0.1554 0.031 Uiso 1 1 calc R . . C2 C 0.18958(15) 0.43776(8) 0.17237(8) 0.0258(3) Uani 1 1 d . . . C3 C 0.09704(15) 0.42100(8) 0.21459(7) 0.0259(3) Uani 1 1 d . . . H3 H 0.0615 0.3737 0.2101 0.031 Uiso 1 1 calc R . . C4 C 0.21376(16) 0.38203(8) 0.12232(8) 0.0283(4) Uani 1 1 d . . . C5 C 0.34051(18) 0.36505(9) 0.11104(9) 0.0361(4) Uani 1 1 d . . . H5 H 0.4144 0.3901 0.1363 0.043 Uiso 1 1 calc R . . C6 C 0.3612(2) 0.31280(10) 0.06414(9) 0.0438(5) Uani 1 1 d . . . H6 H 0.4484 0.3029 0.0573 0.053 Uiso 1 1 calc R . . C7 C 0.2566(2) 0.27516(10) 0.02746(9) 0.0488(5) Uani 1 1 d . . . H7 H 0.2711 0.239 -0.0045 0.059 Uiso 1 1 calc R . . C8 C 0.1304(2) 0.29015(10) 0.03731(9) 0.0468(5) Uani 1 1 d . . . H8 H 0.0578 0.2638 0.0125 0.056 Uiso 1 1 calc R . . C9 C 0.10858(19) 0.34369(9) 0.08342(8) 0.0373(4) Uani 1 1 d . . . H9 H 0.0207 0.3544 0.0886 0.045 Uiso 1 1 calc R . . C10 C 0.35627(15) 0.61273(8) 0.21529(8) 0.0289(4) Uani 1 1 d . . . C11 C 0.38274(16) 0.64503(9) 0.15404(9) 0.0349(4) Uani 1 1 d . . . C12 C 0.47415(18) 0.70146(10) 0.16076(11) 0.0459(5) Uani 1 1 d . . . H12 H 0.4926 0.7237 0.1202 0.055 Uiso 1 1 calc R . . C13 C 0.53812(19) 0.72582(10) 0.22393(12) 0.0504(5) Uani 1 1 d . . . H13 H 0.5984 0.7649 0.2268 0.061 Uiso 1 1 calc R . . C14 C 0.51414(17) 0.69300(10) 0.28337(11) 0.0436(5) Uani 1 1 d . . . H14 H 0.5593 0.7095 0.327 0.052 Uiso 1 1 calc R . . C15 C 0.42527(15) 0.63636(9) 0.28046(9) 0.0333(4) Uani 1 1 d . . . C16 C 0.31669(18) 0.62253(10) 0.08134(9) 0.0393(4) Uani 1 1 d . . . H16 H 0.2388 0.5917 0.0853 0.047 Uiso 1 1 calc R . . C17 C 0.4100(2) 0.57828(12) 0.04507(11) 0.0566(6) Uani 1 1 d . . . H17A H 0.3642 0.565 -0.0013 0.085 Uiso 1 1 calc R . . H17B H 0.4372 0.5346 0.0718 0.085 Uiso 1 1 calc R . . H17C H 0.4883 0.6071 0.0416 0.085 Uiso 1 1 calc R . . C18 C 0.2668(2) 0.68696(11) 0.03464(11) 0.0547(5) Uani 1 1 d . . . H18A H 0.2259 0.6695 -0.0113 0.082 Uiso 1 1 calc R . . H18B H 0.3413 0.7185 0.0306 0.082 Uiso 1 1 calc R . . H18C H 0.2014 0.7139 0.0548 0.082 Uiso 1 1 calc R . . C19 C 0.40863(17) 0.59678(9) 0.34586(9) 0.0364(4) Uani 1 1 d . . . H19 H 0.3135 0.5828 0.3408 0.044 Uiso 1 1 calc R . . C20 C 0.4442(2) 0.64133(12) 0.41215(10) 0.0535(5) Uani 1 1 d . . . H20A H 0.3915 0.6856 0.4076 0.08 Uiso 1 1 calc R . . H20B H 0.5384 0.6536 0.4199 0.08 Uiso 1 1 calc R . . H20C H 0.4255 0.6132 0.4514 0.08 Uiso 1 1 calc R . . C21 C 0.49033(19) 0.52745(10) 0.35323(10) 0.0470(5) Uani 1 1 d . . . H21A H 0.4791 0.5023 0.3955 0.071 Uiso 1 1 calc R . . H21B H 0.5839 0.5393 0.3557 0.071 Uiso 1 1 calc R . . H21C H 0.4604 0.4964 0.3132 0.071 Uiso 1 1 calc R . . C22 C -0.01902(16) 0.42844(8) 0.30538(8) 0.0290(4) Uani 1 1 d . . . C23 C -0.15211(17) 0.40942(9) 0.28403(9) 0.0340(4) Uani 1 1 d . . . C24 C -0.2203(2) 0.38107(10) 0.33335(10) 0.0455(5) Uani 1 1 d . . . H24 H -0.3104 0.3676 0.3198 0.055 Uiso 1 1 calc R . . C25 C -0.1590(2) 0.37244(10) 0.40107(10) 0.0502(5) Uani 1 1 d . . . H25 H -0.2074 0.3542 0.434 0.06 Uiso 1 1 calc R . . C26 C -0.0277(2) 0.39014(10) 0.42132(9) 0.0436(5) Uani 1 1 d . . . H26 H 0.0139 0.3832 0.4681 0.052 Uiso 1 1 calc R . . C27 C 0.04516(18) 0.41811(8) 0.37445(8) 0.0335(4) Uani 1 1 d . . . C28 C -0.22379(17) 0.41915(10) 0.21016(9) 0.0388(4) Uani 1 1 d . . . H28 H -0.162 0.4442 0.1843 0.047 Uiso 1 1 calc R . . C29 C -0.2602(2) 0.34676(12) 0.17475(11) 0.0552(5) Uani 1 1 d . . . H29A H -0.3062 0.355 0.1272 0.083 Uiso 1 1 calc R . . H29B H -0.3181 0.3201 0.2001 0.083 Uiso 1 1 calc R . . H29C H -0.1796 0.3188 0.1742 0.083 Uiso 1 1 calc R . . C30 C -0.34718(19) 0.46598(12) 0.20518(11) 0.0527(5) Uani 1 1 d . . . H30A H -0.3899 0.4708 0.1566 0.079 Uiso 1 1 calc R . . H30B H -0.3221 0.5137 0.2245 0.079 Uiso 1 1 calc R . . H30C H -0.4087 0.4434 0.2313 0.079 Uiso 1 1 calc R . . C31 C 0.19093(18) 0.43502(9) 0.39550(8) 0.0369(4) Uani 1 1 d . . . H31 H 0.2094 0.478 0.3682 0.044 Uiso 1 1 calc R . . C32 C 0.2339(2) 0.45400(12) 0.47198(10) 0.0541(5) Uani 1 1 d . . . H32A H 0.329 0.464 0.4817 0.081 Uiso 1 1 calc R . . H32B H 0.2147 0.4134 0.5004 0.081 Uiso 1 1 calc R . . H32C H 0.1855 0.4967 0.4828 0.081 Uiso 1 1 calc R . . C33 C 0.2745(2) 0.37278(10) 0.37583(10) 0.0474(5) Uani 1 1 d . . . H33A H 0.3685 0.3844 0.39 0.071 Uiso 1 1 calc R . . H33B H 0.2542 0.3655 0.3257 0.071 Uiso 1 1 calc R . . H33C H 0.2543 0.3287 0.3992 0.071 Uiso 1 1 calc R . . C34 C -0.13795(19) 0.66728(11) 0.21811(10) 0.0476(5) Uani 1 1 d . . . H34A H -0.2069 0.632 0.2245 0.057 Uiso 1 1 calc R . . H34B H -0.1821 0.7086 0.1916 0.057 Uiso 1 1 calc R . . C35 C -0.0673(2) 0.69298(10) 0.28761(11) 0.0481(5) Uani 1 1 d . . . H35A H -0.0011 0.7298 0.2811 0.058 Uiso 1 1 calc R . . H35B H -0.1318 0.7159 0.3124 0.058 Uiso 1 1 calc R . . C36 C 0.0363(2) 0.68882(12) 0.15449(12) 0.0585(6) Uani 1 1 d . . . H36A H 0.0849 0.7156 0.194 0.088 Uiso 1 1 calc R . . H36B H -0.0204 0.722 0.1236 0.088 Uiso 1 1 calc R . . H36C H 0.099 0.6659 0.1295 0.088 Uiso 1 1 calc R . . C37 C -0.1183(3) 0.59375(13) 0.11980(11) 0.0661(6) Uani 1 1 d . . . H37A H -0.173 0.5567 0.1361 0.099 Uiso 1 1 calc R . . H37B H -0.0556 0.5709 0.0946 0.099 Uiso 1 1 calc R . . H37C H -0.175 0.6271 0.089 0.099 Uiso 1 1 calc R . . C38 C -0.0979(2) 0.59286(11) 0.35997(10) 0.0490(5) Uani 1 1 d . . . H38A H -0.0539 0.5531 0.3879 0.074 Uiso 1 1 calc R . . H38B H -0.1658 0.5735 0.3229 0.074 Uiso 1 1 calc R . . H38C H -0.1394 0.6249 0.3893 0.074 Uiso 1 1 calc R . . C39 C 0.1000(2) 0.66209(12) 0.38566(11) 0.0587(6) Uani 1 1 d . . . H39A H 0.1654 0.6894 0.3659 0.088 Uiso 1 1 calc R . . H39B H 0.1439 0.6223 0.4135 0.088 Uiso 1 1 calc R . . H39C H 0.0578 0.6938 0.4149 0.088 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 Li 0.0352(15) 0.0278(14) 0.0356(15) 0.0032(11) 0.0115(12) 0.0024(12) N1 0.0252(7) 0.0248(7) 0.0299(7) -0.0004(5) 0.0061(5) -0.0014(5) N2 0.0285(7) 0.0254(7) 0.0250(7) 0.0017(5) 0.0067(5) -0.0017(6) N3 0.0460(9) 0.0461(9) 0.0427(9) 0.0130(7) 0.0171(7) 0.0118(7) N4 0.0431(9) 0.0320(8) 0.0452(9) -0.0028(7) 0.0128(7) 0.0043(7) C1 0.0245(8) 0.0281(8) 0.0251(8) 0.0018(7) 0.0062(6) 0.0025(7) C2 0.0283(8) 0.0245(8) 0.0244(8) 0.0002(6) 0.0044(6) 0.0002(7) C3 0.0303(8) 0.0232(8) 0.0231(8) 0.0001(6) 0.0022(6) -0.0026(7) C4 0.0392(9) 0.0247(8) 0.0219(8) 0.0024(6) 0.0083(7) -0.0008(7) C5 0.0418(10) 0.0305(9) 0.0368(9) -0.0017(7) 0.0097(8) 0.0028(8) C6 0.0606(12) 0.0349(10) 0.0400(10) 0.0012(8) 0.0200(9) 0.0126(9) C7 0.0889(16) 0.0309(10) 0.0307(10) -0.0033(8) 0.0218(10) 0.0030(10) C8 0.0748(14) 0.0394(10) 0.0260(9) -0.0055(8) 0.0087(9) -0.0184(10) C9 0.0487(11) 0.0384(9) 0.0259(8) -0.0025(7) 0.0099(7) -0.0095(8) C10 0.0225(8) 0.0238(8) 0.0419(9) -0.0017(7) 0.0101(7) 0.0013(6) C11 0.0303(9) 0.0300(9) 0.0475(10) 0.0048(8) 0.0154(8) 0.0028(7) C12 0.0399(10) 0.0397(10) 0.0629(13) 0.0087(9) 0.0224(10) -0.0047(9) C13 0.0371(10) 0.0372(10) 0.0806(15) -0.0018(10) 0.0204(10) -0.0124(9) C14 0.0323(9) 0.0379(10) 0.0607(12) -0.0122(9) 0.0089(9) -0.0071(8) C15 0.0249(8) 0.0302(9) 0.0458(10) -0.0065(7) 0.0093(7) 0.0001(7) C16 0.0424(10) 0.0388(10) 0.0401(10) 0.0076(8) 0.0162(8) 0.0037(8) C17 0.0713(14) 0.0555(13) 0.0507(12) 0.0095(10) 0.0315(11) 0.0158(11) C18 0.0616(13) 0.0523(12) 0.0550(12) 0.0161(10) 0.0236(10) 0.0091(10) C19 0.0314(9) 0.0401(10) 0.0371(9) -0.0094(8) 0.0051(7) -0.0053(8) C20 0.0494(12) 0.0620(13) 0.0470(12) -0.0166(10) 0.0030(9) -0.0100(10) C21 0.0465(11) 0.0474(11) 0.0464(11) 0.0035(9) 0.0064(9) 0.0017(9) C22 0.0393(9) 0.0217(8) 0.0292(8) -0.0007(6) 0.0146(7) -0.0021(7) C23 0.0382(9) 0.0291(9) 0.0381(9) -0.0028(7) 0.0159(8) -0.0059(7) C24 0.0459(11) 0.0442(11) 0.0519(12) -0.0013(9) 0.0234(9) -0.0105(9) C25 0.0688(14) 0.0449(11) 0.0456(11) 0.0049(9) 0.0335(10) -0.0105(10) C26 0.0650(13) 0.0366(10) 0.0329(9) 0.0044(8) 0.0187(9) -0.0055(9) C27 0.0483(10) 0.0251(8) 0.0294(9) 0.0013(7) 0.0129(8) -0.0011(7) C28 0.0322(9) 0.0446(10) 0.0410(10) 0.0008(8) 0.0106(8) -0.0037(8) C29 0.0560(13) 0.0588(13) 0.0505(12) -0.0142(10) 0.0087(10) -0.0043(11) C30 0.0369(10) 0.0574(13) 0.0627(13) -0.0053(10) 0.0061(9) -0.0015(9) C31 0.0482(11) 0.0335(9) 0.0277(9) 0.0059(7) 0.0040(8) -0.0018(8) C32 0.0656(14) 0.0587(13) 0.0342(10) -0.0004(9) -0.0007(9) -0.0040(11) C33 0.0547(12) 0.0456(11) 0.0409(10) 0.0088(9) 0.0066(9) 0.0063(9) C34 0.0403(10) 0.0492(11) 0.0576(12) 0.0159(10) 0.0199(9) 0.0138(9) C35 0.0521(12) 0.0343(10) 0.0626(13) 0.0025(9) 0.0231(10) 0.0113(9) C36 0.0519(12) 0.0649(14) 0.0653(14) 0.0297(11) 0.0275(11) 0.0134(11) C37 0.0931(18) 0.0594(14) 0.0450(12) 0.0103(11) 0.0108(12) 0.0029(13) C38 0.0631(13) 0.0416(11) 0.0487(11) 0.0001(9) 0.0270(10) 0.0004(10) C39 0.0570(13) 0.0567(13) 0.0616(14) -0.0184(11) 0.0088(11) 0.0080(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Li N2 2.005(3) . ? Li N1 2.067(3) . ? Li N3 2.125(3) . ? Li N4 2.240(3) . ? N1 C1 1.3142(19) . ? N1 C10 1.4293(19) . ? N2 C3 1.3108(19) . ? N2 C22 1.4319(19) . ? N3 C37 1.464(3) . ? N3 C36 1.465(3) . ? N3 C34 1.470(2) . ? N4 C38 1.463(2) . ? N4 C39 1.465(3) . ? N4 C35 1.478(2) . ? C1 C2 1.408(2) . ? C2 C3 1.410(2) . ? C2 C4 1.482(2) . ? C4 C5 1.399(2) . ? C4 C9 1.400(2) . ? C5 C6 1.383(2) . ? C6 C7 1.372(3) . ? C7 C8 1.377(3) . ? C8 C9 1.392(2) . ? C10 C15 1.417(2) . ? C10 C11 1.418(2) . ? C11 C12 1.398(2) . ? C11 C16 1.526(3) . ? C12 C13 1.373(3) . ? C13 C14 1.382(3) . ? C14 C15 1.388(2) . ? C15 C19 1.520(2) . ? C16 C17 1.537(3) . ? C16 C18 1.538(3) . ? C19 C21 1.530(3) . ? C19 C20 1.532(2) . ? C22 C23 1.402(2) . ? C22 C27 1.411(2) . ? C23 C24 1.402(2) . ? C23 C28 1.516(2) . ? C24 C25 1.376(3) . ? C25 C26 1.376(3) . ? C26 C27 1.393(2) . ? C27 C31 1.514(2) . ? C28 C30 1.527(3) . ? C28 C29 1.529(3) . ? C31 C32 1.531(2) . ? C31 C33 1.533(3) . ? C34 C35 1.504(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 N2 Li N1 94.72(12) . . ? N2 Li N3 121.61(15) . . ? N1 Li N3 107.05(13) . . ? N2 Li N4 113.03(13) . . ? N1 Li N4 139.18(15) . . ? N3 Li N4 83.96(11) . . ? C1 N1 C10 116.62(12) . . ? C1 N1 Li 115.85(13) . . ? C10 N1 Li 126.71(12) . . ? C3 N2 C22 116.32(12) . . ? C3 N2 Li 117.37(13) . . ? C22 N2 Li 126.07(12) . . ? C37 N3 C36 109.35(16) . . ? C37 N3 C34 110.30(17) . . ? C36 N3 C34 109.90(15) . . ? C37 N3 Li 114.48(15) . . ? C36 N3 Li 107.04(14) . . ? C34 N3 Li 105.63(13) . . ? C38 N4 C39 108.94(16) . . ? C38 N4 C35 109.28(15) . . ? C39 N4 C35 109.81(15) . . ? C38 N4 Li 112.59(13) . . ? C39 N4 Li 113.89(14) . . ? C35 N4 Li 102.08(13) . . ? N1 C1 C2 128.53(14) . . ? C1 C2 C3 124.53(14) . . ? C1 C2 C4 118.18(13) . . ? C3 C2 C4 116.94(13) . . ? N2 C3 C2 127.85(14) . . ? C5 C4 C9 116.62(15) . . ? C5 C4 C2 122.62(15) . . ? C9 C4 C2 120.76(15) . . ? C6 C5 C4 121.82(17) . . ? C7 C6 C5 120.41(18) . . ? C6 C7 C8 119.48(17) . . ? C7 C8 C9 120.41(18) . . ? C8 C9 C4 121.23(18) . . ? C15 C10 C11 119.78(15) . . ? C15 C10 N1 117.13(14) . . ? C11 C10 N1 123.03(15) . . ? C12 C11 C10 117.91(17) . . ? C12 C11 C16 118.00(16) . . ? C10 C11 C16 124.08(15) . . ? C13 C12 C11 122.32(18) . . ? C12 C13 C14 119.46(17) . . ? C13 C14 C15 121.24(18) . . ? C14 C15 C10 119.24(16) . . ? C14 C15 C19 120.52(16) . . ? C10 C15 C19 120.12(14) . . ? C11 C16 C17 111.97(16) . . ? C11 C16 C18 112.95(16) . . ? C17 C16 C18 107.82(15) . . ? C15 C19 C21 109.96(14) . . ? C15 C19 C20 114.49(15) . . ? C21 C19 C20 109.44(16) . . ? C23 C22 C27 120.83(14) . . ? C23 C22 N2 121.44(14) . . ? C27 C22 N2 117.62(14) . . ? C24 C23 C22 118.24(16) . . ? C24 C23 C28 119.51(16) . . ? C22 C23 C28 122.24(14) . . ? C25 C24 C23 121.12(18) . . ? C24 C25 C26 120.22(16) . . ? C25 C26 C27 121.13(17) . . ? C26 C27 C22 118.42(16) . . ? C26 C27 C31 121.57(16) . . ? C22 C27 C31 119.98(14) . . ? C23 C28 C30 112.41(15) . . ? C23 C28 C29 111.59(15) . . ? C30 C28 C29 109.90(16) . . ? C27 C31 C32 114.14(15) . . ? C27 C31 C33 110.40(15) . . ? C32 C31 C33 110.41(15) . . ? N3 C34 C35 111.18(16) . . ? N4 C35 C34 111.75(15) . . ? #===END data_(4)-jul203 _database_code_depnum_ccdc_archive 'CCDC 609661' _audit_creation_date 2003-07-03T16:09:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H41 Al1 Cl2 N2' _chemical_formula_sum 'C33 H41 Al1 Cl2 N2' _chemical_formula_weight 563.56 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0584(1) _cell_length_b 11.9404(1) _cell_length_c 26.9485(3) _cell_angle_alpha 90 _cell_angle_beta 98.394(1) _cell_angle_gamma 90 _cell_volume 3201.88(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24299 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.797134E-1 _diffrn_orient_matrix_ub_12 0.42401E-1 _diffrn_orient_matrix_ub_13 0.168999E-1 _diffrn_orient_matrix_ub_21 0.43721E-2 _diffrn_orient_matrix_ub_22 -0.50365E-1 _diffrn_orient_matrix_ub_23 0.298421E-1 _diffrn_orient_matrix_ub_31 0.610415E-1 _diffrn_orient_matrix_ub_32 -0.517636E-1 _diffrn_orient_matrix_ub_33 -0.151926E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.032 _diffrn_reflns_number 28547 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 5581 _reflns_number_gt 4826 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0347P)^2^+1.5984P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5581 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.044 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.242 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.037 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Al Al 0.51700(4) 0.76500(4) 0.116527(17) 0.02420(12) Uani 1 1 d . . . Cl1 Cl 0.69470(4) 0.82138(4) 0.090759(18) 0.04376(14) Uani 1 1 d . . . Cl2 Cl 0.55205(5) 0.60820(4) 0.152512(16) 0.03919(13) Uani 1 1 d . . . N1 N 0.44797(12) 0.87105(11) 0.15764(4) 0.0227(3) Uani 1 1 d . . . N2 N 0.37023(13) 0.76520(11) 0.06459(5) 0.0236(3) Uani 1 1 d . . . C1 C 0.35400(15) 0.94411(13) 0.13909(6) 0.0240(3) Uani 1 1 d . . . H1 H 0.3347 1.003 0.1606 0.029 Uiso 1 1 calc R . . C2 C 0.28096(15) 0.94229(13) 0.09082(6) 0.0234(3) Uani 1 1 d . . . C3 C 0.28597(15) 0.85160(13) 0.05851(6) 0.0238(3) Uani 1 1 d . . . H3 H 0.222 0.8516 0.0288 0.029 Uiso 1 1 calc R . . C4 C 0.18238(15) 1.03266(14) 0.07445(6) 0.0265(4) Uani 1 1 d . . . C5 C 0.09383(17) 1.07324(16) 0.10545(7) 0.0378(4) Uani 1 1 d . . . H5 H 0.094 1.0415 0.1378 0.045 Uiso 1 1 calc R . . C6 C 0.00581(19) 1.15919(18) 0.08967(7) 0.0466(5) Uani 1 1 d . . . H6 H -0.0534 1.1862 0.1114 0.056 Uiso 1 1 calc R . . C7 C 0.00299(19) 1.20626(16) 0.04266(7) 0.0429(5) Uani 1 1 d . . . H7 H -0.0567 1.2662 0.0322 0.052 Uiso 1 1 calc R . . C8 C 0.08752(19) 1.16540(16) 0.01118(7) 0.0420(5) Uani 1 1 d . . . H8 H 0.085 1.1963 -0.0214 0.05 Uiso 1 1 calc R . . C9 C 0.17623(17) 1.07953(15) 0.02681(6) 0.0338(4) Uani 1 1 d . . . H9 H 0.234 1.052 0.0047 0.041 Uiso 1 1 calc R . . C10 C 0.49121(15) 0.87647(13) 0.21170(5) 0.0243(3) Uani 1 1 d . . . C11 C 0.60278(16) 0.94175(15) 0.23091(6) 0.0306(4) Uani 1 1 d . . . C12 C 0.64115(18) 0.94191(17) 0.28288(6) 0.0378(4) Uani 1 1 d . . . H12 H 0.7169 0.9848 0.297 0.045 Uiso 1 1 calc R . . C13 C 0.57166(19) 0.88136(17) 0.31403(6) 0.0398(4) Uani 1 1 d . . . H13 H 0.5998 0.8826 0.3492 0.048 Uiso 1 1 calc R . . C14 C 0.46110(18) 0.81873(16) 0.29432(6) 0.0344(4) Uani 1 1 d . . . H14 H 0.4135 0.7776 0.3162 0.041 Uiso 1 1 calc R . . C15 C 0.41828(16) 0.81490(14) 0.24298(6) 0.0269(4) Uani 1 1 d . . . C16 C 0.67885(18) 1.01448(17) 0.19850(7) 0.0414(5) Uani 1 1 d . . . H16 H 0.6408 1.0004 0.1627 0.05 Uiso 1 1 calc R . . C17 C 0.8281(2) 0.9848(3) 0.20523(9) 0.0720(8) Uani 1 1 d . . . H17A H 0.874 1.0331 0.1837 0.108 Uiso 1 1 calc R . . H17B H 0.8387 0.9063 0.1959 0.108 Uiso 1 1 calc R . . H17C H 0.8673 0.996 0.2404 0.108 Uiso 1 1 calc R . . C18 C 0.6575(3) 1.1381(2) 0.20958(9) 0.0719(8) Uani 1 1 d . . . H18A H 0.7065 1.1844 0.1883 0.108 Uiso 1 1 calc R . . H18B H 0.6908 1.1535 0.2449 0.108 Uiso 1 1 calc R . . H18C H 0.5614 1.1558 0.2026 0.108 Uiso 1 1 calc R . . C19 C 0.29127(17) 0.74983(15) 0.22283(6) 0.0317(4) Uani 1 1 d . . . H19 H 0.2909 0.7389 0.186 0.038 Uiso 1 1 calc R . . C20 C 0.16599(19) 0.81673(19) 0.22941(9) 0.0515(5) Uani 1 1 d . . . H20A H 0.0857 0.7736 0.2162 0.077 Uiso 1 1 calc R . . H20B H 0.1661 0.8877 0.2112 0.077 Uiso 1 1 calc R . . H20C H 0.1656 0.8319 0.2651 0.077 Uiso 1 1 calc R . . C21 C 0.2866(2) 0.63437(18) 0.24643(8) 0.0503(5) Uani 1 1 d . . . H21A H 0.2035 0.5963 0.2321 0.075 Uiso 1 1 calc R . . H21B H 0.2892 0.6422 0.2828 0.075 Uiso 1 1 calc R . . H21C H 0.3641 0.5903 0.2396 0.075 Uiso 1 1 calc R . . C22 C 0.33557(15) 0.67313(13) 0.02956(6) 0.0254(3) Uani 1 1 d . . . C23 C 0.37940(17) 0.67567(15) -0.01777(6) 0.0301(4) Uani 1 1 d . . . C24 C 0.33888(19) 0.58738(16) -0.05036(7) 0.0388(4) Uani 1 1 d . . . H24 H 0.367 0.5863 -0.0825 0.047 Uiso 1 1 calc R . . C25 C 0.2594(2) 0.50179(17) -0.03725(7) 0.0446(5) Uani 1 1 d . . . H25 H 0.2336 0.4426 -0.0602 0.054 Uiso 1 1 calc R . . C26 C 0.2170(2) 0.50181(16) 0.00939(7) 0.0412(5) Uani 1 1 d . . . H26 H 0.161 0.4429 0.0179 0.049 Uiso 1 1 calc R . . C27 C 0.25512(16) 0.58668(14) 0.04394(6) 0.0304(4) Uani 1 1 d . . . C28 C 0.4635(2) 0.77012(17) -0.03414(7) 0.0406(5) Uani 1 1 d . . . H28 H 0.5152 0.8046 -0.0034 0.049 Uiso 1 1 calc R . . C29 C 0.5635(2) 0.7296(2) -0.06746(9) 0.0572(6) Uani 1 1 d . . . H29A H 0.6159 0.7934 -0.0769 0.086 Uiso 1 1 calc R . . H29B H 0.5149 0.695 -0.0978 0.086 Uiso 1 1 calc R . . H29C H 0.6241 0.6745 -0.0492 0.086 Uiso 1 1 calc R . . C30 C 0.3756(3) 0.8613(2) -0.06230(10) 0.0733(8) Uani 1 1 d . . . H30A H 0.433 0.9213 -0.0721 0.11 Uiso 1 1 calc R . . H30B H 0.3148 0.892 -0.0404 0.11 Uiso 1 1 calc R . . H30C H 0.3229 0.8291 -0.0924 0.11 Uiso 1 1 calc R . . C31 C 0.20674(18) 0.58563(16) 0.09497(6) 0.0350(4) Uani 1 1 d . . . H31 H 0.2711 0.6327 0.1179 0.042 Uiso 1 1 calc R . . C32 C 0.0688(2) 0.6406(2) 0.09223(8) 0.0610(7) Uani 1 1 d . . . H32A H 0.0405 0.6396 0.1255 0.092 Uiso 1 1 calc R . . H32B H 0.0034 0.5993 0.0685 0.092 Uiso 1 1 calc R . . H32C H 0.0739 0.7182 0.0809 0.092 Uiso 1 1 calc R . . C33 C 0.2085(3) 0.46976(19) 0.11816(9) 0.0675(7) Uani 1 1 d . . . H33A H 0.1772 0.4744 0.1509 0.101 Uiso 1 1 calc R . . H33B H 0.3002 0.44 0.1225 0.101 Uiso 1 1 calc R . . H33C H 0.1491 0.42 0.0961 0.101 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 Al 0.0221(2) 0.0286(3) 0.0210(2) -0.00076(19) -0.00018(18) 0.0033(2) Cl1 0.0302(2) 0.0592(3) 0.0441(3) -0.0048(2) 0.01285(19) -0.0038(2) Cl2 0.0434(3) 0.0348(3) 0.0367(2) 0.00634(19) -0.00311(19) 0.0123(2) N1 0.0212(6) 0.0269(7) 0.0190(6) 0.0001(5) -0.0004(5) -0.0004(5) N2 0.0256(7) 0.0237(7) 0.0207(6) -0.0015(5) 0.0003(5) 0.0008(6) C1 0.0225(8) 0.0247(8) 0.0247(8) -0.0010(6) 0.0033(6) -0.0015(6) C2 0.0211(8) 0.0257(9) 0.0229(8) 0.0009(6) 0.0012(6) 0.0001(6) C3 0.0212(8) 0.0280(9) 0.0210(8) 0.0026(6) -0.0010(6) -0.0025(7) C4 0.0219(8) 0.0267(9) 0.0286(8) -0.0041(7) -0.0040(6) 0.0005(7) C5 0.0330(9) 0.0482(11) 0.0298(9) -0.0075(8) -0.0033(7) 0.0106(8) C6 0.0359(10) 0.0568(13) 0.0435(11) -0.0194(10) -0.0063(8) 0.0180(9) C7 0.0353(10) 0.0346(10) 0.0516(12) -0.0084(9) -0.0181(9) 0.0114(8) C8 0.0375(10) 0.0413(11) 0.0433(11) 0.0090(9) -0.0075(8) 0.0052(9) C9 0.0305(9) 0.0357(10) 0.0340(9) 0.0048(8) 0.0008(7) 0.0045(8) C10 0.0237(8) 0.0282(9) 0.0199(8) -0.0028(6) -0.0007(6) 0.0042(7) C11 0.0268(8) 0.0380(10) 0.0262(8) -0.0039(7) 0.0008(7) -0.0019(7) C12 0.0318(9) 0.0517(12) 0.0276(9) -0.0064(8) -0.0039(7) -0.0083(8) C13 0.0445(11) 0.0526(12) 0.0205(8) -0.0026(8) -0.0017(7) -0.0025(9) C14 0.0395(10) 0.0402(11) 0.0239(8) 0.0028(7) 0.0054(7) -0.0015(8) C15 0.0266(8) 0.0295(9) 0.0242(8) -0.0008(7) 0.0020(6) 0.0029(7) C16 0.0387(10) 0.0563(13) 0.0286(9) -0.0050(9) 0.0027(8) -0.0206(9) C17 0.0350(11) 0.135(3) 0.0465(13) -0.0047(14) 0.0081(10) -0.0243(14) C18 0.109(2) 0.0547(15) 0.0540(14) -0.0031(12) 0.0174(14) -0.0351(15) C19 0.0329(9) 0.0362(10) 0.0260(8) -0.0008(7) 0.0048(7) -0.0054(7) C20 0.0318(10) 0.0523(13) 0.0699(15) -0.0043(11) 0.0059(10) -0.0031(9) C21 0.0536(13) 0.0419(12) 0.0544(13) 0.0078(10) 0.0047(10) -0.0117(10) C22 0.0249(8) 0.0256(9) 0.0237(8) -0.0028(6) -0.0034(6) 0.0017(7) C23 0.0308(9) 0.0327(10) 0.0257(8) -0.0027(7) 0.0006(7) 0.0004(7) C24 0.0445(11) 0.0434(11) 0.0289(9) -0.0097(8) 0.0072(8) -0.0054(9) C25 0.0551(12) 0.0401(11) 0.0384(11) -0.0149(9) 0.0064(9) -0.0116(10) C26 0.0467(11) 0.0371(11) 0.0394(10) -0.0059(8) 0.0049(8) -0.0159(9) C27 0.0306(9) 0.0317(10) 0.0279(9) -0.0013(7) 0.0005(7) -0.0015(7) C28 0.0520(12) 0.0453(12) 0.0242(9) -0.0052(8) 0.0048(8) -0.0134(9) C29 0.0428(12) 0.0723(16) 0.0589(14) 0.0001(12) 0.0156(10) -0.0099(11) C30 0.101(2) 0.0573(15) 0.0721(17) 0.0245(13) 0.0476(15) 0.0179(14) C31 0.0370(10) 0.0385(10) 0.0292(9) -0.0014(8) 0.0039(7) -0.0082(8) C32 0.0362(11) 0.103(2) 0.0444(12) 0.0000(12) 0.0081(9) 0.0042(12) C33 0.112(2) 0.0468(14) 0.0498(13) 0.0035(11) 0.0336(13) -0.0140(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Al N2 1.8801(13) . ? Al N1 1.8808(14) . ? Al Cl2 2.1143(7) . ? Al Cl1 2.1195(6) . ? N1 C1 1.329(2) . ? N1 C10 1.4597(19) . ? N2 C3 1.330(2) . ? N2 C22 1.4579(19) . ? C1 C2 1.398(2) . ? C2 C3 1.395(2) . ? C2 C4 1.488(2) . ? C4 C9 1.394(2) . ? C4 C5 1.394(2) . ? C5 C6 1.381(3) . ? C6 C7 1.382(3) . ? C7 C8 1.375(3) . ? C8 C9 1.384(2) . ? C10 C11 1.402(2) . ? C10 C15 1.404(2) . ? C11 C12 1.397(2) . ? C11 C16 1.516(2) . ? C12 C13 1.374(3) . ? C13 C14 1.380(3) . ? C14 C15 1.388(2) . ? C15 C19 1.526(2) . ? C16 C17 1.527(3) . ? C16 C18 1.528(3) . ? C19 C21 1.522(3) . ? C19 C20 1.524(3) . ? C22 C27 1.401(2) . ? C22 C23 1.409(2) . ? C23 C24 1.394(2) . ? C23 C28 1.514(3) . ? C24 C25 1.375(3) . ? C25 C26 1.385(3) . ? C26 C27 1.392(2) . ? C27 C31 1.524(2) . ? C28 C29 1.522(3) . ? C28 C30 1.532(3) . ? C31 C33 1.517(3) . ? C31 C32 1.527(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 N2 Al N1 96.91(6) . . ? N2 Al Cl2 113.75(5) . . ? N1 Al Cl2 112.16(5) . . ? N2 Al Cl1 111.34(5) . . ? N1 Al Cl1 112.37(5) . . ? Cl2 Al Cl1 109.84(3) . . ? C1 N1 C10 115.99(13) . . ? C1 N1 Al 121.59(10) . . ? C10 N1 Al 122.41(10) . . ? C3 N2 C22 114.67(12) . . ? C3 N2 Al 120.64(10) . . ? C22 N2 Al 124.66(10) . . ? N1 C1 C2 126.03(15) . . ? C3 C2 C1 122.07(14) . . ? C3 C2 C4 117.46(13) . . ? C1 C2 C4 120.10(14) . . ? N2 C3 C2 127.28(14) . . ? C9 C4 C5 117.78(15) . . ? C9 C4 C2 120.15(15) . . ? C5 C4 C2 122.06(15) . . ? C6 C5 C4 120.71(18) . . ? C5 C6 C7 120.71(18) . . ? C8 C7 C6 119.29(17) . . ? C7 C8 C9 120.28(18) . . ? C8 C9 C4 121.19(17) . . ? C11 C10 C15 122.00(14) . . ? C11 C10 N1 119.93(14) . . ? C15 C10 N1 118.07(13) . . ? C12 C11 C10 117.38(16) . . ? C12 C11 C16 119.20(15) . . ? C10 C11 C16 123.37(14) . . ? C13 C12 C11 121.40(16) . . ? C12 C13 C14 120.20(16) . . ? C13 C14 C15 121.11(17) . . ? C14 C15 C10 117.89(15) . . ? C14 C15 C19 119.56(15) . . ? C10 C15 C19 122.47(14) . . ? C11 C16 C17 111.64(18) . . ? C11 C16 C18 110.11(17) . . ? C17 C16 C18 111.4(2) . . ? C21 C19 C20 110.47(16) . . ? C21 C19 C15 112.83(15) . . ? C20 C19 C15 110.81(15) . . ? C27 C22 C23 122.41(15) . . ? C27 C22 N2 118.01(14) . . ? C23 C22 N2 119.55(14) . . ? C24 C23 C22 116.90(16) . . ? C24 C23 C28 120.27(15) . . ? C22 C23 C28 122.80(15) . . ? C25 C24 C23 121.84(16) . . ? C24 C25 C26 120.04(17) . . ? C25 C26 C27 121.07(17) . . ? C26 C27 C22 117.73(16) . . ? C26 C27 C31 120.30(16) . . ? C22 C27 C31 121.95(15) . . ? C23 C28 C29 112.40(17) . . ? C23 C28 C30 111.58(17) . . ? C29 C28 C30 108.46(17) . . ? C33 C31 C27 113.16(16) . . ? C33 C31 C32 111.56(19) . . ? C27 C31 C32 111.13(15) . . ? #===END data_(5)-jul603 _database_code_depnum_ccdc_archive 'CCDC 609662' _audit_creation_date 2003-07-07T14:42:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H41 Cl2 Ga1 N2' _chemical_formula_sum 'C33 H41 Cl2 Ga1 N2' _chemical_formula_weight 606.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0613(1) _cell_length_b 11.9025(2) _cell_length_c 27.0265(5) _cell_angle_alpha 90 _cell_angle_beta 98.114(1) _cell_angle_gamma 90 _cell_volume 3204.15(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30493 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7836 _exptl_absorpt_correction_T_max 0.8479 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.195663E-1 _diffrn_orient_matrix_ub_12 -0.146056E-1 _diffrn_orient_matrix_ub_13 -0.367447E-1 _diffrn_orient_matrix_ub_21 -0.617292E-1 _diffrn_orient_matrix_ub_22 0.662411E-1 _diffrn_orient_matrix_ub_23 -0.3904E-2 _diffrn_orient_matrix_ub_31 0.767201E-1 _diffrn_orient_matrix_ub_32 0.495729E-1 _diffrn_orient_matrix_ub_33 -0.56094E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_unetI/netI 0.0538 _diffrn_reflns_number 32657 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5604 _reflns_number_gt 4320 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0211P)^2^+2.8298P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5604 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.306 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ga Ga 0.51825(3) 0.76557(2) 0.116558(11) 0.02238(9) Uani 1 1 d . . . Cl1 Cl 0.70169(7) 0.82138(7) 0.09100(3) 0.0419(2) Uani 1 1 d . . . Cl2 Cl 0.55165(8) 0.60519(6) 0.15316(3) 0.0381(2) Uani 1 1 d . . . N1 N 0.4482(2) 0.87515(17) 0.15843(8) 0.0197(5) Uani 1 1 d . . . N2 N 0.3699(2) 0.76667(17) 0.06323(8) 0.0215(5) Uani 1 1 d . . . C1 C 0.3526(2) 0.9459(2) 0.13934(10) 0.0221(6) Uani 1 1 d . . . H1 H 0.3309 1.0046 0.1606 0.027 Uiso 1 1 calc R . . C2 C 0.2806(2) 0.9432(2) 0.09125(10) 0.0208(6) Uani 1 1 d . . . C3 C 0.2855(3) 0.8527(2) 0.05852(10) 0.0214(6) Uani 1 1 d . . . H3 H 0.2204 0.853 0.0294 0.026 Uiso 1 1 calc R . . C4 C 0.1806(3) 1.0334(2) 0.07515(10) 0.0228(6) Uani 1 1 d . . . C5 C 0.0915(3) 1.0725(2) 0.10602(11) 0.0337(7) Uani 1 1 d . . . H5 H 0.0919 1.04 0.1381 0.04 Uiso 1 1 calc R . . C6 C 0.0019(3) 1.1584(3) 0.09063(12) 0.0428(8) Uani 1 1 d . . . H6 H -0.0584 1.1842 0.1122 0.051 Uiso 1 1 calc R . . C7 C 0.0001(3) 1.2067(2) 0.04415(13) 0.0395(8) Uani 1 1 d . . . H7 H -0.0599 1.2666 0.0339 0.047 Uiso 1 1 calc R . . C8 C 0.0859(3) 1.1672(2) 0.01286(12) 0.0402(8) Uani 1 1 d . . . H8 H 0.0839 1.199 -0.0195 0.048 Uiso 1 1 calc R . . C9 C 0.1752(3) 1.0815(2) 0.02803(11) 0.0317(7) Uani 1 1 d . . . H9 H 0.2338 1.0552 0.0059 0.038 Uiso 1 1 calc R . . C10 C 0.4910(2) 0.8801(2) 0.21210(9) 0.0216(6) Uani 1 1 d . . . C11 C 0.6025(3) 0.9448(2) 0.23108(10) 0.0276(7) Uani 1 1 d . . . C12 C 0.6403(3) 0.9453(3) 0.28287(11) 0.0362(7) Uani 1 1 d . . . H12 H 0.7157 0.9885 0.2968 0.043 Uiso 1 1 calc R . . C13 C 0.5706(3) 0.8845(3) 0.31398(11) 0.0381(8) Uani 1 1 d . . . H13 H 0.5984 0.8857 0.3491 0.046 Uiso 1 1 calc R . . C14 C 0.4603(3) 0.8218(2) 0.29439(11) 0.0326(7) Uani 1 1 d . . . H14 H 0.4122 0.7809 0.3163 0.039 Uiso 1 1 calc R . . C15 C 0.4182(3) 0.8174(2) 0.24315(10) 0.0242(6) Uani 1 1 d . . . C16 C 0.6788(3) 1.0168(3) 0.19850(11) 0.0387(8) Uani 1 1 d . . . H16 H 0.6413 1.0021 0.1628 0.046 Uiso 1 1 calc R . . C17 C 0.8285(3) 0.9868(4) 0.20548(14) 0.0702(13) Uani 1 1 d . . . H17A H 0.875 1.0349 0.184 0.105 Uiso 1 1 calc R . . H17B H 0.8392 0.9079 0.1964 0.105 Uiso 1 1 calc R . . H17C H 0.867 0.9983 0.2405 0.105 Uiso 1 1 calc R . . C18 C 0.6583(5) 1.1413(3) 0.20909(15) 0.0709(12) Uani 1 1 d . . . H18A H 0.7077 1.1869 0.1876 0.106 Uiso 1 1 calc R . . H18B H 0.6917 1.1573 0.2442 0.106 Uiso 1 1 calc R . . H18C H 0.5625 1.1594 0.2022 0.106 Uiso 1 1 calc R . . C19 C 0.2914(3) 0.7523(2) 0.22313(10) 0.0298(7) Uani 1 1 d . . . H19 H 0.2913 0.7414 0.1864 0.036 Uiso 1 1 calc R . . C20 C 0.1656(3) 0.8182(3) 0.22988(14) 0.0478(9) Uani 1 1 d . . . H20A H 0.086 0.7746 0.2166 0.072 Uiso 1 1 calc R . . H20B H 0.1653 0.8898 0.2119 0.072 Uiso 1 1 calc R . . H20C H 0.1646 0.8328 0.2655 0.072 Uiso 1 1 calc R . . C21 C 0.2868(3) 0.6362(3) 0.24671(13) 0.0480(9) Uani 1 1 d . . . H21A H 0.2039 0.5978 0.2325 0.072 Uiso 1 1 calc R . . H21B H 0.2891 0.644 0.2829 0.072 Uiso 1 1 calc R . . H21C H 0.3644 0.5922 0.2398 0.072 Uiso 1 1 calc R . . C22 C 0.3354(3) 0.6735(2) 0.02876(10) 0.0236(6) Uani 1 1 d . . . C23 C 0.3807(3) 0.6753(2) -0.01816(10) 0.0278(7) Uani 1 1 d . . . C24 C 0.3408(3) 0.5860(2) -0.05035(11) 0.0366(7) Uani 1 1 d . . . H24 H 0.3698 0.5838 -0.0823 0.044 Uiso 1 1 calc R . . C25 C 0.2603(3) 0.5010(3) -0.03684(12) 0.0424(8) Uani 1 1 d . . . H25 H 0.2344 0.4413 -0.0595 0.051 Uiso 1 1 calc R . . C26 C 0.2169(3) 0.5021(2) 0.00947(11) 0.0382(8) Uani 1 1 d . . . H26 H 0.1605 0.4433 0.0181 0.046 Uiso 1 1 calc R . . C27 C 0.2546(3) 0.5880(2) 0.04374(10) 0.0272(7) Uani 1 1 d . . . C28 C 0.4662(3) 0.7696(3) -0.03448(11) 0.0383(7) Uani 1 1 d . . . H28 H 0.5202 0.8016 -0.0038 0.046 Uiso 1 1 calc R . . C29 C 0.5632(3) 0.7296(3) -0.06868(14) 0.0547(9) Uani 1 1 d . . . H29A H 0.6157 0.7934 -0.0781 0.082 Uiso 1 1 calc R . . H29B H 0.5129 0.6961 -0.0988 0.082 Uiso 1 1 calc R . . H29C H 0.6238 0.6733 -0.0513 0.082 Uiso 1 1 calc R . . C30 C 0.3809(4) 0.8646(3) -0.06067(15) 0.0666(12) Uani 1 1 d . . . H30A H 0.4399 0.9239 -0.0702 0.1 Uiso 1 1 calc R . . H30B H 0.3226 0.8955 -0.0379 0.1 Uiso 1 1 calc R . . H30C H 0.3257 0.8351 -0.0906 0.1 Uiso 1 1 calc R . . C31 C 0.2059(3) 0.5877(2) 0.09444(10) 0.0305(7) Uani 1 1 d . . . H31 H 0.2698 0.6354 0.1171 0.037 Uiso 1 1 calc R . . C32 C 0.0684(3) 0.6420(3) 0.09187(13) 0.0562(10) Uani 1 1 d . . . H32A H 0.0401 0.641 0.1251 0.084 Uiso 1 1 calc R . . H32B H 0.0034 0.6001 0.0684 0.084 Uiso 1 1 calc R . . H32C H 0.073 0.7198 0.0804 0.084 Uiso 1 1 calc R . . C33 C 0.2080(4) 0.4720(3) 0.11813(14) 0.0609(11) Uani 1 1 d . . . H33A H 0.1767 0.4773 0.1508 0.091 Uiso 1 1 calc R . . H33B H 0.2998 0.4424 0.1225 0.091 Uiso 1 1 calc R . . H33C H 0.149 0.4214 0.0964 0.091 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 Ga 0.02156(16) 0.02568(17) 0.01908(17) -0.00113(13) -0.00003(11) 0.00360(13) Cl1 0.0281(4) 0.0578(5) 0.0421(5) -0.0057(4) 0.0130(3) -0.0036(4) Cl2 0.0447(5) 0.0325(4) 0.0347(5) 0.0061(3) -0.0028(3) 0.0129(3) N1 0.0190(12) 0.0244(12) 0.0148(12) -0.0011(9) -0.0007(9) -0.0004(9) N2 0.0253(12) 0.0194(11) 0.0186(12) -0.0013(9) -0.0009(9) 0.0020(10) C1 0.0203(14) 0.0216(14) 0.0248(16) -0.0010(11) 0.0041(12) -0.0019(12) C2 0.0183(14) 0.0222(14) 0.0216(16) -0.0001(11) 0.0017(11) -0.0014(11) C3 0.0233(15) 0.0257(14) 0.0143(15) 0.0031(11) -0.0002(11) -0.0023(12) C4 0.0199(14) 0.0228(14) 0.0237(16) -0.0043(11) -0.0038(12) 0.0011(11) C5 0.0334(17) 0.0415(18) 0.0244(17) -0.0059(13) -0.0025(13) 0.0095(14) C6 0.0344(18) 0.050(2) 0.040(2) -0.0176(16) -0.0071(15) 0.0157(16) C7 0.0329(18) 0.0301(17) 0.049(2) -0.0070(15) -0.0167(16) 0.0103(14) C8 0.0387(19) 0.0378(18) 0.040(2) 0.0075(15) -0.0078(15) 0.0053(15) C9 0.0292(16) 0.0337(16) 0.0310(18) 0.0018(13) -0.0001(13) 0.0041(13) C10 0.0203(14) 0.0257(15) 0.0180(15) -0.0018(11) -0.0001(11) 0.0047(11) C11 0.0255(16) 0.0358(16) 0.0212(17) -0.0042(12) 0.0021(12) -0.0036(13) C12 0.0298(17) 0.0482(19) 0.0282(19) -0.0061(14) -0.0042(14) -0.0083(15) C13 0.0438(19) 0.049(2) 0.0190(17) -0.0026(14) -0.0023(14) -0.0004(16) C14 0.0390(18) 0.0376(17) 0.0216(17) 0.0004(13) 0.0052(13) -0.0034(14) C15 0.0246(15) 0.0262(14) 0.0210(16) 0.0000(12) 0.0006(12) 0.0038(12) C16 0.0355(18) 0.056(2) 0.0239(18) -0.0049(15) 0.0015(14) -0.0197(15) C17 0.035(2) 0.136(4) 0.040(2) -0.003(2) 0.0073(17) -0.026(2) C18 0.111(4) 0.051(2) 0.053(3) -0.0046(19) 0.020(2) -0.035(2) C19 0.0319(16) 0.0333(17) 0.0243(16) 0.0009(13) 0.0040(12) -0.0057(13) C20 0.0323(19) 0.048(2) 0.063(2) -0.0027(17) 0.0066(17) -0.0036(16) C21 0.053(2) 0.0362(18) 0.054(2) 0.0071(16) 0.0057(18) -0.0129(16) C22 0.0262(15) 0.0211(14) 0.0214(16) -0.0034(11) -0.0043(12) 0.0019(12) C23 0.0294(16) 0.0296(16) 0.0235(17) -0.0037(12) 0.0011(13) -0.0011(13) C24 0.0429(19) 0.0416(18) 0.0265(18) -0.0118(14) 0.0085(14) -0.0068(15) C25 0.054(2) 0.0373(18) 0.035(2) -0.0176(15) 0.0053(16) -0.0108(16) C26 0.048(2) 0.0332(17) 0.0333(19) -0.0041(14) 0.0040(15) -0.0126(15) C27 0.0291(16) 0.0269(15) 0.0249(17) -0.0023(12) 0.0012(13) -0.0015(13) C28 0.0478(19) 0.0427(18) 0.0249(17) -0.0058(14) 0.0072(14) -0.0123(16) C29 0.042(2) 0.069(2) 0.055(2) -0.0018(19) 0.0144(17) -0.0079(18) C30 0.094(3) 0.050(2) 0.065(3) 0.0211(19) 0.043(2) 0.015(2) C31 0.0339(17) 0.0344(16) 0.0232(17) -0.0009(13) 0.0044(13) -0.0073(13) C32 0.036(2) 0.092(3) 0.041(2) 0.002(2) 0.0088(16) 0.0010(19) C33 0.100(3) 0.041(2) 0.047(2) 0.0044(17) 0.027(2) -0.013(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ga N2 1.923(2) . ? Ga N1 1.924(2) . ? Ga Cl2 2.1544(7) . ? Ga Cl1 2.1644(8) . ? N1 C1 1.327(3) . ? N1 C10 1.455(3) . ? N2 C3 1.325(3) . ? N2 C22 1.458(3) . ? C1 C2 1.396(4) . ? C2 C3 1.399(4) . ? C2 C4 1.492(4) . ? C4 C5 1.388(4) . ? C4 C9 1.391(4) . ? C5 C6 1.388(4) . ? C6 C7 1.379(5) . ? C7 C8 1.374(4) . ? C8 C9 1.382(4) . ? C10 C11 1.398(4) . ? C10 C15 1.404(4) . ? C11 C12 1.397(4) . ? C11 C16 1.513(4) . ? C12 C13 1.374(4) . ? C13 C14 1.379(4) . ? C14 C15 1.391(4) . ? C15 C19 1.525(4) . ? C16 C18 1.528(5) . ? C16 C17 1.534(5) . ? C19 C20 1.522(4) . ? C19 C21 1.525(4) . ? C22 C27 1.397(4) . ? C22 C23 1.407(4) . ? C23 C24 1.396(4) . ? C23 C28 1.517(4) . ? C24 C25 1.376(4) . ? C25 C26 1.382(4) . ? C26 C27 1.397(4) . ? C27 C31 1.519(4) . ? C28 C29 1.512(4) . ? C28 C30 1.531(5) . ? C31 C33 1.518(4) . ? C31 C32 1.520(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 N2 Ga N1 97.26(9) . . ? N2 Ga Cl2 113.86(7) . . ? N1 Ga Cl2 112.14(7) . . ? N2 Ga Cl1 111.42(7) . . ? N1 Ga Cl1 112.28(7) . . ? Cl2 Ga Cl1 109.50(3) . . ? C1 N1 C10 117.2(2) . . ? C1 N1 Ga 120.48(17) . . ? C10 N1 Ga 122.18(16) . . ? C3 N2 C22 115.8(2) . . ? C3 N2 Ga 119.75(17) . . ? C22 N2 Ga 124.26(16) . . ? N1 C1 C2 126.8(2) . . ? C1 C2 C3 123.1(2) . . ? C1 C2 C4 119.7(2) . . ? C3 C2 C4 116.8(2) . . ? N2 C3 C2 127.9(2) . . ? C5 C4 C9 117.8(2) . . ? C5 C4 C2 122.1(2) . . ? C9 C4 C2 120.1(2) . . ? C6 C5 C4 121.0(3) . . ? C7 C6 C5 120.3(3) . . ? C8 C7 C6 119.3(3) . . ? C7 C8 C9 120.6(3) . . ? C8 C9 C4 121.0(3) . . ? C11 C10 C15 122.2(2) . . ? C11 C10 N1 119.8(2) . . ? C15 C10 N1 118.0(2) . . ? C12 C11 C10 117.4(3) . . ? C12 C11 C16 119.5(2) . . ? C10 C11 C16 123.0(2) . . ? C13 C12 C11 121.4(3) . . ? C12 C13 C14 120.1(3) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 C10 117.6(2) . . ? C14 C15 C19 119.6(2) . . ? C10 C15 C19 122.6(2) . . ? C11 C16 C18 110.3(3) . . ? C11 C16 C17 111.5(3) . . ? C18 C16 C17 111.0(3) . . ? C20 C19 C21 110.0(3) . . ? C20 C19 C15 111.3(2) . . ? C21 C19 C15 112.7(2) . . ? C27 C22 C23 123.2(2) . . ? C27 C22 N2 117.7(2) . . ? C23 C22 N2 119.1(2) . . ? C24 C23 C22 116.7(3) . . ? C24 C23 C28 120.5(3) . . ? C22 C23 C28 122.8(2) . . ? C25 C24 C23 121.5(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C27 121.0(3) . . ? C26 C27 C22 117.1(3) . . ? C26 C27 C31 120.3(2) . . ? C22 C27 C31 122.6(2) . . ? C29 C28 C23 112.7(3) . . ? C29 C28 C30 108.5(3) . . ? C23 C28 C30 112.1(3) . . ? C33 C31 C27 113.3(2) . . ? C33 C31 C32 111.3(3) . . ? C27 C31 C32 111.4(2) . . ? #===END data_(6)-oct2103 _database_code_depnum_ccdc_archive 'CCDC 609663' _audit_creation_date 2003-10-27T15:36:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H61 Cl3 In Li N2 O2' _chemical_formula_sum 'C41 H61 Cl3 In Li N2 O2' _chemical_formula_weight 842.03 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3(2) _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 17.7096(2) _cell_length_b 17.7096(2) _cell_length_c 12.2877(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3337.48(6) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36167 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7385 _exptl_absorpt_correction_T_max 0.7933 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.58306E-2 _diffrn_orient_matrix_ub_12 -0.197377E-1 _diffrn_orient_matrix_ub_13 -0.741901E-1 _diffrn_orient_matrix_ub_21 -0.642051E-1 _diffrn_orient_matrix_ub_22 -0.418705E-1 _diffrn_orient_matrix_ub_23 -0.16657E-2 _diffrn_orient_matrix_ub_31 -0.97469E-2 _diffrn_orient_matrix_ub_32 0.459192E-1 _diffrn_orient_matrix_ub_33 -0.334083E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_number 53222 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 25.66 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8192 _reflns_number_gt 7941 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0273P)^2^+1.2303P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 8192 _refine_ls_number_parameters 451 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(13) _refine_diff_density_max 0.497 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.337452(12) 0.989632(11) 0.689169(19) 0.02676(5) Uani 1 1 d . . . Li Li 0.4233(3) 1.1058(3) 0.4536(4) 0.0420(12) Uani 1 1 d . . . Cl1 Cl 0.29566(5) 0.97120(5) 0.49692(5) 0.0492(2) Uani 1 1 d . . . Cl2 Cl 0.43724(5) 0.93740(6) 0.70585(7) 0.0570(2) Uani 1 1 d . . . Cl3 Cl 0.44006(6) 1.14490(5) 0.63938(6) 0.0569(2) Uani 1 1 d . . . O1 O 0.38795(13) 1.17824(13) 0.37738(16) 0.0435(5) Uani 1 1 d . . . O2 O 0.51357(19) 1.09165(19) 0.3852(3) 0.0889(9) Uani 1 1 d . . . N1 N 0.32110(14) 1.03386(14) 0.84902(16) 0.0298(5) Uani 1 1 d . . . N2 N 0.21418(14) 0.86945(14) 0.73155(16) 0.0282(5) Uani 1 1 d . . . C1 C 0.28813(17) 0.97763(18) 0.9311(2) 0.0328(6) Uani 1 1 d . . . H1 H 0.3018 1.0027 1.0018 0.039 Uiso 1 1 calc R . . C2 C 0.23646(18) 0.88733(18) 0.9281(2) 0.0316(6) Uani 1 1 d . . . C3 C 0.19771(16) 0.84039(16) 0.8321(2) 0.0299(5) Uani 1 1 d . . . H3 H 0.1547 0.7808 0.8411 0.036 Uiso 1 1 calc R . . C4 C 0.21417(17) 0.83759(19) 1.0332(2) 0.0398(6) Uani 1 1 d . . . C5 C 0.2117(2) 0.7583(2) 1.0390(3) 0.0544(8) Uani 1 1 d . . . H5 H 0.2235 0.7351 0.9756 0.065 Uiso 1 1 calc R . . C6 C 0.1921(3) 0.7119(3) 1.1366(3) 0.0715(11) Uani 1 1 d . . . H6 H 0.1892 0.6569 1.1387 0.086 Uiso 1 1 calc R . . C7 C 0.1773(2) 0.7448(3) 1.2285(3) 0.0740(12) Uani 1 1 d . . . H7 H 0.165 0.7131 1.2948 0.089 Uiso 1 1 calc R . . C8 C 0.1800(2) 0.8246(3) 1.2262(3) 0.0685(11) Uani 1 1 d . . . H8 H 0.1706 0.848 1.291 0.082 Uiso 1 1 calc R . . C9 C 0.19678(19) 0.8705(2) 1.1279(2) 0.0519(8) Uani 1 1 d . . . H9 H 0.1963 0.9239 1.1254 0.062 Uiso 1 1 calc R . . C10 C 0.36379(16) 1.12395(17) 0.8813(2) 0.0326(6) Uani 1 1 d . . . C11 C 0.44859(18) 1.16326(19) 0.9242(2) 0.0415(7) Uani 1 1 d . . . C12 C 0.4855(2) 1.2502(2) 0.9583(3) 0.0530(8) Uani 1 1 d . . . H12 H 0.5427 1.2786 0.9877 0.064 Uiso 1 1 calc R . . C13 C 0.4423(2) 1.2953(2) 0.9507(3) 0.0539(8) Uani 1 1 d . . . H13 H 0.4689 1.3538 0.9759 0.065 Uiso 1 1 calc R . . C14 C 0.3590(2) 1.2559(2) 0.9060(2) 0.0492(7) Uani 1 1 d . . . H14 H 0.3297 1.2882 0.8992 0.059 Uiso 1 1 calc R . . C15 C 0.31818(18) 1.16955(18) 0.8710(2) 0.0379(6) Uani 1 1 d . . . C16 C 0.4986(2) 1.1144(2) 0.9321(3) 0.0511(8) Uani 1 1 d . . . H16 H 0.4629 1.0566 0.8958 0.061 Uiso 1 1 calc R . . C17 C 0.5856(2) 1.1620(3) 0.8740(3) 0.0637(10) Uani 1 1 d . . . H17A H 0.6156 1.1284 0.8806 0.096 Uiso 1 1 calc R . . H17B H 0.6214 1.2196 0.9068 0.096 Uiso 1 1 calc R . . H17C H 0.576 1.1687 0.7969 0.096 Uiso 1 1 calc R . . C18 C 0.5104(3) 1.0976(4) 1.0501(4) 0.0971(17) Uani 1 1 d . . . H18A H 0.5422 1.0655 1.0537 0.146 Uiso 1 1 calc R . . H18B H 0.4532 1.0631 1.0845 0.146 Uiso 1 1 calc R . . H18C H 0.5436 1.1533 1.0884 0.146 Uiso 1 1 calc R . . C19 C 0.2265(2) 1.1269(2) 0.8241(2) 0.0463(7) Uani 1 1 d . . . H19 H 0.2113 1.0678 0.7969 0.056 Uiso 1 1 calc R . . C20 C 0.1606(2) 1.1152(3) 0.9128(3) 0.0679(10) Uani 1 1 d . . . H20A H 0.1018 1.0871 0.8816 0.102 Uiso 1 1 calc R . . H20B H 0.1752 1.1723 0.9423 0.102 Uiso 1 1 calc R . . H20C H 0.1627 1.0787 0.9713 0.102 Uiso 1 1 calc R . . C21 C 0.2209(3) 1.1784(3) 0.7288(3) 0.0784(12) Uani 1 1 d . . . H21A H 0.1611 1.149 0.7005 0.118 Uiso 1 1 calc R . . H21B H 0.261 1.1821 0.6714 0.118 Uiso 1 1 calc R . . H21C H 0.2368 1.2372 0.7531 0.118 Uiso 1 1 calc R . . C22 C 0.15647(16) 0.81107(16) 0.64998(18) 0.0293(5) Uani 1 1 d . . . C23 C 0.15916(18) 0.73528(17) 0.6235(2) 0.0372(6) Uani 1 1 d . . . C24 C 0.0995(2) 0.67956(19) 0.5456(2) 0.0490(7) Uani 1 1 d . . . H24 H 0.0985 0.6269 0.5275 0.059 Uiso 1 1 calc R . . C25 C 0.0428(2) 0.6990(2) 0.4952(2) 0.0509(8) Uani 1 1 d . . . H25 H 0.003 0.6599 0.4427 0.061 Uiso 1 1 calc R . . C26 C 0.04260(19) 0.7753(2) 0.5198(2) 0.0444(7) Uani 1 1 d . . . H26 H 0.0033 0.7885 0.4832 0.053 Uiso 1 1 calc R . . C27 C 0.09935(17) 0.83281(17) 0.5976(2) 0.0340(6) Uani 1 1 d . . . C28 C 0.2235(2) 0.7125(2) 0.6726(3) 0.0508(7) Uani 1 1 d . . . H28 H 0.2621 0.7604 0.7236 0.061 Uiso 1 1 calc R . . C29 C 0.2814(3) 0.7060(3) 0.5840(4) 0.0827(12) Uani 1 1 d . . . H29A H 0.3229 0.6917 0.6176 0.124 Uiso 1 1 calc R . . H29B H 0.3135 0.762 0.5459 0.124 Uiso 1 1 calc R . . H29C H 0.2448 0.6603 0.5319 0.124 Uiso 1 1 calc R . . C30 C 0.1762(3) 0.6277(2) 0.7384(4) 0.0755(11) Uani 1 1 d . . . H30A H 0.2191 0.6143 0.7697 0.113 Uiso 1 1 calc R . . H30B H 0.1367 0.5799 0.6905 0.113 Uiso 1 1 calc R . . H30C H 0.1427 0.6346 0.797 0.113 Uiso 1 1 calc R . . C31 C 0.09964(19) 0.91620(19) 0.6264(2) 0.0432(7) Uani 1 1 d . . . H31 H 0.161 0.9601 0.6463 0.052 Uiso 1 1 calc R . . C32 C 0.0435(3) 0.9047(3) 0.7264(4) 0.0722(11) Uani 1 1 d . . . H32A H 0.0454 0.9599 0.7424 0.108 Uiso 1 1 calc R . . H32B H 0.066 0.8877 0.7889 0.108 Uiso 1 1 calc R . . H32C H -0.0169 0.8594 0.7119 0.108 Uiso 1 1 calc R . . C33 C 0.0743(3) 0.9546(3) 0.5300(4) 0.0870(14) Uani 1 1 d . . . H33A H 0.0757 1.0083 0.5531 0.13 Uiso 1 1 calc R . . H33B H 0.0153 0.9122 0.5053 0.13 Uiso 1 1 calc R . . H33C H 0.1156 0.9677 0.4701 0.13 Uiso 1 1 calc R . . C34 C 0.3890(2) 1.1883(2) 0.2612(2) 0.0549(8) Uani 1 1 d . . . H34A H 0.4464 1.2009 0.2327 0.066 Uiso 1 1 calc R . . H34B H 0.3814 1.2387 0.2437 0.066 Uiso 1 1 calc R . . C35 C 0.3194(3) 1.1094(3) 0.2063(4) 0.0754(11) Uani 1 1 d . . . H35A H 0.3228 1.1192 0.1276 0.113 Uiso 1 1 calc R . . H35B H 0.2623 1.0974 0.233 0.113 Uiso 1 1 calc R . . H35C H 0.3272 1.0595 0.2223 0.113 Uiso 1 1 calc R . . C36 C 0.3238(3) 1.1915(3) 0.4288(3) 0.0680(10) Uani 1 1 d . . . H36A H 0.3034 1.1555 0.4956 0.082 Uiso 1 1 calc R . . H36B H 0.2732 1.1718 0.3794 0.082 Uiso 1 1 calc R . . C37 C 0.3580(3) 1.2860(3) 0.4584(3) 0.0740(11) Uani 1 1 d . . . H37A H 0.3117 1.2921 0.4936 0.111 Uiso 1 1 calc R . . H37B H 0.3771 1.3218 0.3922 0.111 Uiso 1 1 calc R . . H37C H 0.4074 1.3055 0.5084 0.111 Uiso 1 1 calc R . . C38 C 0.5999(3) 1.1597(4) 0.3646(4) 0.0835(14) Uani 1 1 d . . . H38A H 0.6125 1.1615 0.2858 0.1 Uiso 1 1 calc R . . H38B H 0.6415 1.1478 0.4044 0.1 Uiso 1 1 calc R . . C39 C 0.6116(3) 1.2427(3) 0.3981(5) 0.0985(17) Uani 1 1 d . . . H39A H 0.6718 1.2884 0.3835 0.148 Uiso 1 1 calc R . . H39B H 0.5996 1.2411 0.4762 0.148 Uiso 1 1 calc R . . H39C H 0.5714 1.2551 0.3575 0.148 Uiso 1 1 calc R . . C40 C 0.5059(5) 1.0035(5) 0.3841(9) 0.157(3) Uani 1 1 d . . . H40A H 0.5628 1.0091 0.3653 0.188 Uiso 1 1 calc R . . H40B H 0.4884 0.9764 0.457 0.188 Uiso 1 1 calc R . . C41 C 0.4449(8) 0.9530(7) 0.3090(6) 0.181(4) Uani 1 1 d . . . H41A H 0.4386 0.8948 0.3082 0.272 Uiso 1 1 calc R . . H41B H 0.4632 0.9797 0.2369 0.272 Uiso 1 1 calc R . . H41C H 0.3888 0.9482 0.3279 0.272 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 0.02704(9) 0.03204(13) 0.02156(7) 0.00205(9) 0.00172(6) 0.01504(9) Li 0.047(3) 0.048(3) 0.033(2) 0.013(2) 0.013(2) 0.025(3) Cl1 0.0545(5) 0.0459(4) 0.0217(3) 0.0017(3) -0.0015(3) 0.0060(4) Cl2 0.0501(4) 0.0816(6) 0.0614(5) 0.0132(4) 0.0056(4) 0.0495(4) Cl3 0.0662(5) 0.0375(4) 0.0308(3) 0.0016(3) 0.0002(3) -0.0013(4) O1 0.0437(11) 0.0507(12) 0.0389(11) 0.0104(9) 0.0047(9) 0.0258(10) O2 0.083(2) 0.0764(18) 0.123(2) 0.0208(17) 0.0506(18) 0.0512(17) N1 0.0297(11) 0.0336(12) 0.0255(11) -0.0004(9) -0.0004(9) 0.0154(10) N2 0.0282(11) 0.0336(12) 0.0228(11) 0.0015(9) 0.0004(8) 0.0156(10) C1 0.0303(13) 0.0445(16) 0.0224(13) -0.0017(11) -0.0002(10) 0.0178(12) C2 0.0297(14) 0.0395(15) 0.0246(13) 0.0049(11) 0.0015(10) 0.0164(12) C3 0.0274(12) 0.0303(13) 0.0332(14) 0.0066(10) 0.0038(10) 0.0153(11) C4 0.0285(13) 0.0534(17) 0.0262(13) 0.0108(12) 0.0013(10) 0.0121(12) C5 0.0531(19) 0.061(2) 0.0481(18) 0.0192(15) 0.0023(14) 0.0274(16) C6 0.072(2) 0.081(3) 0.062(2) 0.038(2) 0.0091(19) 0.039(2) C7 0.062(2) 0.100(3) 0.049(2) 0.038(2) 0.0045(17) 0.032(2) C8 0.0499(19) 0.103(3) 0.0277(16) 0.0119(17) 0.0049(14) 0.019(2) C9 0.0432(17) 0.069(2) 0.0273(15) 0.0047(13) 0.0027(12) 0.0163(15) C10 0.0336(13) 0.0336(14) 0.0240(12) -0.0039(10) 0.0030(10) 0.0117(11) C11 0.0369(15) 0.0449(16) 0.0331(14) -0.0078(12) -0.0010(11) 0.0133(13) C12 0.0403(16) 0.0541(19) 0.0478(18) -0.0153(15) -0.0022(13) 0.0110(15) C13 0.0561(19) 0.0388(16) 0.0505(18) -0.0148(14) 0.0057(15) 0.0115(15) C14 0.060(2) 0.0429(17) 0.0439(17) -0.0077(13) 0.0069(14) 0.0252(15) C15 0.0415(15) 0.0417(15) 0.0306(14) -0.0073(11) 0.0029(11) 0.0207(13) C16 0.0357(16) 0.060(2) 0.0538(19) -0.0067(15) -0.0065(13) 0.0207(15) C17 0.0438(18) 0.086(3) 0.060(2) -0.0102(18) -0.0032(16) 0.0315(19) C18 0.083(3) 0.160(5) 0.072(3) 0.039(3) 0.011(2) 0.078(3) C19 0.0516(17) 0.0542(18) 0.0460(16) -0.0157(14) -0.0049(14) 0.0360(15) C20 0.0438(19) 0.086(3) 0.070(2) -0.019(2) 0.0021(16) 0.0294(19) C21 0.092(3) 0.109(3) 0.059(2) -0.004(2) -0.014(2) 0.069(3) C22 0.0286(13) 0.0325(13) 0.0233(12) -0.0006(9) 0.0029(9) 0.0127(11) C23 0.0401(15) 0.0322(14) 0.0372(15) 0.0018(11) 0.0090(12) 0.0166(12) C24 0.0550(18) 0.0366(16) 0.0427(16) -0.0101(13) 0.0068(14) 0.0133(14) C25 0.0472(18) 0.0488(18) 0.0333(15) -0.0095(13) -0.0021(13) 0.0064(14) C26 0.0388(16) 0.0516(18) 0.0321(15) 0.0024(12) -0.0055(12) 0.0144(14) C27 0.0331(13) 0.0397(14) 0.0277(13) 0.0014(11) -0.0001(10) 0.0170(12) C28 0.0537(18) 0.0420(16) 0.066(2) -0.0025(14) 0.0049(15) 0.0306(15) C29 0.073(3) 0.089(3) 0.108(3) -0.006(2) 0.022(2) 0.056(2) C30 0.085(3) 0.052(2) 0.100(3) 0.014(2) -0.001(2) 0.043(2) C31 0.0407(16) 0.0466(17) 0.0487(17) -0.0031(13) -0.0089(13) 0.0268(14) C32 0.055(2) 0.065(2) 0.099(3) -0.017(2) 0.017(2) 0.0315(19) C33 0.116(4) 0.085(3) 0.091(3) -0.011(2) -0.048(3) 0.073(3) C34 0.061(2) 0.059(2) 0.0380(17) 0.0108(14) -0.0030(14) 0.0257(17) C35 0.075(3) 0.072(2) 0.080(3) -0.023(2) -0.016(2) 0.036(2) C36 0.067(2) 0.073(2) 0.071(2) -0.0002(19) 0.0071(19) 0.040(2) C37 0.091(3) 0.062(2) 0.070(2) -0.0072(19) 0.000(2) 0.039(2) C38 0.051(2) 0.132(4) 0.068(3) 0.019(3) 0.0085(18) 0.047(3) C39 0.051(2) 0.084(3) 0.146(5) 0.050(3) -0.005(3) 0.023(2) C40 0.132(6) 0.128(6) 0.231(9) -0.040(6) 0.022(6) 0.080(5) C41 0.317(13) 0.191(9) 0.096(5) -0.027(5) 0.001(6) 0.172(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 2.187(2) . ? In N2 2.218(2) . ? In Cl2 2.3782(7) . ? In Cl1 2.4481(7) . ? In Cl3 2.4982(8) . ? Li O1 1.928(5) . ? Li O2 1.931(5) . ? Li Cl3 2.361(5) . ? Li Cl1 2.385(5) . ? O1 C36 1.418(4) . ? O1 C34 1.438(4) . ? O2 C38 1.418(5) . ? O2 C40 1.498(7) . ? N1 C1 1.330(3) . ? N1 C10 1.438(3) . ? N2 C3 1.314(3) . ? N2 C22 1.436(3) . ? C1 C2 1.390(4) . ? C2 C3 1.408(4) . ? C2 C4 1.501(3) . ? C4 C5 1.385(5) . ? C4 C9 1.403(4) . ? C5 C6 1.396(4) . ? C6 C7 1.355(6) . ? C7 C8 1.390(6) . ? C8 C9 1.403(4) . ? C10 C11 1.404(4) . ? C10 C15 1.405(4) . ? C11 C12 1.403(4) . ? C11 C16 1.518(4) . ? C12 C13 1.357(5) . ? C13 C14 1.390(5) . ? C14 C15 1.393(4) . ? C15 C19 1.520(4) . ? C16 C17 1.515(5) . ? C16 C18 1.516(5) . ? C19 C21 1.517(5) . ? C19 C20 1.533(4) . ? C22 C23 1.405(4) . ? C22 C27 1.406(4) . ? C23 C24 1.402(4) . ? C23 C28 1.512(4) . ? C24 C25 1.362(5) . ? C25 C26 1.387(5) . ? C26 C27 1.391(4) . ? C27 C31 1.516(4) . ? C28 C30 1.533(5) . ? C28 C29 1.539(5) . ? C31 C32 1.529(5) . ? C31 C33 1.540(4) . ? C34 C35 1.484(5) . ? C36 C37 1.513(5) . ? C38 C39 1.438(7) . ? C40 C41 1.361(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_3 _geom_angle_publ_flag N1 In N2 83.67(8) . . ? N1 In Cl2 108.61(6) . . ? N2 In Cl2 99.95(6) . . ? N1 In Cl1 146.01(6) . . ? N2 In Cl1 90.67(5) . . ? Cl2 In Cl1 105.38(3) . . ? N1 In Cl3 88.82(6) . . ? N2 In Cl3 159.86(6) . . ? Cl2 In Cl3 100.15(3) . . ? Cl1 In Cl3 85.15(3) . . ? O1 Li O2 116.1(3) . . ? O1 Li Cl3 108.1(2) . . ? O2 Li Cl3 117.9(3) . . ? O1 Li Cl1 108.2(2) . . ? O2 Li Cl1 113.6(2) . . ? Cl3 Li Cl1 89.69(16) . . ? C36 O1 C34 112.6(3) . . ? C36 O1 Li 116.5(2) . . ? C34 O1 Li 125.2(2) . . ? C38 O2 C40 112.4(4) . . ? C38 O2 Li 125.3(3) . . ? C40 O2 Li 119.3(4) . . ? C1 N1 C10 114.3(2) . . ? C1 N1 In 120.02(18) . . ? C10 N1 In 123.70(15) . . ? C3 N2 C22 115.8(2) . . ? C3 N2 In 121.05(17) . . ? C22 N2 In 122.12(15) . . ? N1 C1 C2 129.1(2) . . ? C1 C2 C3 123.2(2) . . ? C1 C2 C4 118.7(2) . . ? C3 C2 C4 117.8(2) . . ? N2 C3 C2 127.5(2) . . ? C5 C4 C9 118.4(3) . . ? C5 C4 C2 120.3(3) . . ? C9 C4 C2 121.2(3) . . ? C4 C5 C6 120.9(3) . . ? C7 C6 C5 120.5(4) . . ? C6 C7 C8 120.3(3) . . ? C7 C8 C9 119.8(3) . . ? C4 C9 C8 120.1(4) . . ? C11 C10 C15 121.9(2) . . ? C11 C10 N1 119.5(2) . . ? C15 C10 N1 118.6(2) . . ? C12 C11 C10 116.9(3) . . ? C12 C11 C16 121.5(3) . . ? C10 C11 C16 121.7(3) . . ? C13 C12 C11 122.4(3) . . ? C12 C13 C14 120.0(3) . . ? C13 C14 C15 120.8(3) . . ? C14 C15 C10 118.1(3) . . ? C14 C15 C19 120.1(3) . . ? C10 C15 C19 121.8(2) . . ? C17 C16 C18 111.0(3) . . ? C17 C16 C11 111.9(3) . . ? C18 C16 C11 110.6(3) . . ? C21 C19 C15 111.6(3) . . ? C21 C19 C20 110.8(3) . . ? C15 C19 C20 110.4(2) . . ? C23 C22 C27 121.9(2) . . ? C23 C22 N2 119.8(2) . . ? C27 C22 N2 118.3(2) . . ? C24 C23 C22 117.2(3) . . ? C24 C23 C28 119.2(3) . . ? C22 C23 C28 123.6(2) . . ? C25 C24 C23 121.6(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C27 120.7(3) . . ? C26 C27 C22 118.0(3) . . ? C26 C27 C31 121.5(3) . . ? C22 C27 C31 120.5(2) . . ? C23 C28 C30 110.9(3) . . ? C23 C28 C29 110.9(3) . . ? C30 C28 C29 111.0(3) . . ? C27 C31 C32 111.9(3) . . ? C27 C31 C33 113.0(3) . . ? C32 C31 C33 111.3(3) . . ? O1 C34 C35 112.4(3) . . ? O1 C36 C37 112.3(3) . . ? O2 C38 C39 111.1(4) . . ? C41 C40 O2 108.6(8) . . ? #===END data_(8)-feb2104 _database_code_depnum_ccdc_archive 'CCDC 609664' _audit_creation_date 2004-02-25T15:11:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[In(ArNCHCPhCHNAr)(NHAr)2]' ; _chemical_formula_moiety 'C57 H77 In N4' _chemical_formula_sum 'C57 H77 In N4' _chemical_formula_weight 933.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1201(2) _cell_length_b 22.6524(3) _cell_length_c 37.2258(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10220.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 47308 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8793 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.740465E-1 _diffrn_orient_matrix_ub_12 -0.193475E-1 _diffrn_orient_matrix_ub_13 -0.13438E-2 _diffrn_orient_matrix_ub_21 -0.33369E-2 _diffrn_orient_matrix_ub_22 0.13764E-2 _diffrn_orient_matrix_ub_23 -0.26828E-1 _diffrn_orient_matrix_ub_31 0.36242E-1 _diffrn_orient_matrix_ub_32 0.39656E-1 _diffrn_orient_matrix_ub_33 0.2755E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_unetI/netI 0.0333 _diffrn_reflns_number 80123 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 8929 _reflns_number_gt 6952 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atoms on N were refined; others were in riding mode. 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^)+(0.0348P)^2^+9.7621P] 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_number_reflns 8929 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.086 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.309 _refine_diff_density_min -0.5 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.366739(14) 0.254394(7) 0.118614(5) 0.02585(7) Uani 1 1 d . . . N1 N 0.38912(17) 0.34927(9) 0.11849(5) 0.0287(5) Uani 1 1 d . . . N2 N 0.28106(16) 0.26519(9) 0.16875(5) 0.0275(5) Uani 1 1 d . . . N3 N 0.5226(2) 0.21660(11) 0.11389(7) 0.0360(6) Uani 1 1 d . . . H3X H 0.521(2) 0.2047(13) 0.0955(8) 0.034(9) Uiso 1 1 d . . . N4 N 0.2433(2) 0.22672(10) 0.08375(6) 0.0323(5) Uani 1 1 d . . . H4X H 0.190(2) 0.2241(12) 0.0960(7) 0.029(8) Uiso 1 1 d . . . C1 C 0.3891(2) 0.38022(11) 0.14851(7) 0.0296(6) Uani 1 1 d . . . H1 H 0.4149 0.4197 0.1465 0.036 Uiso 1 1 calc R . . C2 C 0.3561(2) 0.36261(11) 0.18309(7) 0.0304(6) Uani 1 1 d . . . C3 C 0.2968(2) 0.31110(11) 0.19018(7) 0.0294(6) Uani 1 1 d . . . H3 H 0.2637 0.3087 0.2133 0.035 Uiso 1 1 calc R . . C4 C 0.3754(2) 0.40592(11) 0.21271(7) 0.0328(6) Uani 1 1 d . . . C5 C 0.4745(2) 0.43677(12) 0.21470(8) 0.0409(7) Uani 1 1 d . . . H5 H 0.5303 0.4294 0.1974 0.049 Uiso 1 1 calc R . . C6 C 0.4934(3) 0.47814(13) 0.24154(8) 0.0488(8) Uani 1 1 d . . . H6 H 0.5612 0.4992 0.2421 0.059 Uiso 1 1 calc R . . C7 C 0.4152(3) 0.48878(14) 0.26729(9) 0.0503(8) Uani 1 1 d . . . H7 H 0.4284 0.517 0.2857 0.06 Uiso 1 1 calc R . . C8 C 0.3167(3) 0.45800(14) 0.26619(8) 0.0502(8) Uani 1 1 d . . . H8 H 0.2626 0.4646 0.2842 0.06 Uiso 1 1 calc R . . C9 C 0.2964(2) 0.41744(13) 0.23889(8) 0.0421(7) Uani 1 1 d . . . H9 H 0.2276 0.3973 0.2381 0.051 Uiso 1 1 calc R . . C10 C 0.4077(2) 0.38023(11) 0.08500(7) 0.0305(6) Uani 1 1 d . . . C11 C 0.5158(2) 0.38658(11) 0.07206(7) 0.0369(6) Uani 1 1 d . . . C12 C 0.5301(3) 0.41324(12) 0.03852(8) 0.0455(7) Uani 1 1 d . . . H12 H 0.6024 0.4182 0.0292 0.055 Uiso 1 1 calc R . . C13 C 0.4410(3) 0.43249(12) 0.01884(8) 0.0443(8) Uani 1 1 d . . . H13 H 0.4522 0.45 -0.0041 0.053 Uiso 1 1 calc R . . C14 C 0.3352(3) 0.42649(11) 0.03219(7) 0.0399(7) Uani 1 1 d . . . H14 H 0.2745 0.4404 0.0184 0.048 Uiso 1 1 calc R . . C15 C 0.3159(2) 0.40038(11) 0.06547(7) 0.0324(6) Uani 1 1 d . . . C16 C 0.6154(2) 0.36756(14) 0.09405(8) 0.0459(7) Uani 1 1 d . . . H16 H 0.5882 0.3421 0.1141 0.055 Uiso 1 1 calc R . . C17 C 0.6971(3) 0.33098(18) 0.07176(10) 0.0709(11) Uani 1 1 d . . . H17C H 0.6602 0.2954 0.0628 0.106 Uiso 1 1 calc R . . H17B H 0.7599 0.3196 0.0868 0.106 Uiso 1 1 calc R . . H17A H 0.7233 0.3545 0.0514 0.106 Uiso 1 1 calc R . . C18 C 0.6722(3) 0.42131(17) 0.11068(11) 0.0737(11) Uani 1 1 d . . . H18C H 0.6971 0.4479 0.0916 0.111 Uiso 1 1 calc R . . H18B H 0.736 0.4083 0.1248 0.111 Uiso 1 1 calc R . . H18A H 0.6202 0.4422 0.1263 0.111 Uiso 1 1 calc R . . C19 C 0.1997(2) 0.39443(12) 0.08048(7) 0.0384(6) Uani 1 1 d . . . H19 H 0.1951 0.3558 0.0934 0.046 Uiso 1 1 calc R . . C20 C 0.1734(3) 0.44406(14) 0.10782(8) 0.0491(8) Uani 1 1 d . . . H20C H 0.226 0.4422 0.1278 0.074 Uiso 1 1 calc R . . H20B H 0.0983 0.4388 0.1171 0.074 Uiso 1 1 calc R . . H20A H 0.1792 0.4825 0.0959 0.074 Uiso 1 1 calc R . . C21 C 0.1108(3) 0.39472(15) 0.05165(9) 0.0534(8) Uani 1 1 d . . . H21C H 0.1139 0.432 0.0383 0.08 Uiso 1 1 calc R . . H21B H 0.0381 0.3906 0.0629 0.08 Uiso 1 1 calc R . . H21A H 0.123 0.3617 0.0351 0.08 Uiso 1 1 calc R . . C22 C 0.1926(2) 0.22477(11) 0.17732(6) 0.0284(6) Uani 1 1 d . . . C23 C 0.2165(2) 0.16625(11) 0.18684(6) 0.0301(6) Uani 1 1 d . . . C24 C 0.1285(2) 0.12862(12) 0.19428(7) 0.0377(7) Uani 1 1 d . . . H24 H 0.1428 0.0891 0.2013 0.045 Uiso 1 1 calc R . . C25 C 0.0210(2) 0.14783(13) 0.19160(7) 0.0413(7) Uani 1 1 d . . . H25 H -0.0379 0.1217 0.1971 0.05 Uiso 1 1 calc R . . C26 C -0.0015(2) 0.20455(13) 0.18101(7) 0.0402(7) Uani 1 1 d . . . H26 H -0.0762 0.2168 0.1788 0.048 Uiso 1 1 calc R . . C27 C 0.0827(2) 0.24472(12) 0.17332(7) 0.0335(6) Uani 1 1 d . . . C28 C 0.3339(2) 0.14275(12) 0.18821(7) 0.0355(6) Uani 1 1 d . . . H28 H 0.3848 0.1759 0.1818 0.043 Uiso 1 1 calc R . . C29 C 0.3515(3) 0.09302(14) 0.16092(9) 0.0517(8) Uani 1 1 d . . . H29C H 0.3012 0.0603 0.1663 0.078 Uiso 1 1 calc R . . H29B H 0.4279 0.0791 0.1623 0.078 Uiso 1 1 calc R . . H29A H 0.3367 0.1078 0.1367 0.078 Uiso 1 1 calc R . . C30 C 0.3643(3) 0.12147(16) 0.22597(8) 0.0519(8) Uani 1 1 d . . . H30C H 0.3577 0.1543 0.243 0.078 Uiso 1 1 calc R . . H30B H 0.4404 0.1069 0.226 0.078 Uiso 1 1 calc R . . H30A H 0.3143 0.0896 0.2331 0.078 Uiso 1 1 calc R . . C31 C 0.0541(2) 0.30628(13) 0.15998(8) 0.0393(7) Uani 1 1 d . . . H31 H 0.1242 0.3254 0.1518 0.047 Uiso 1 1 calc R . . C32 C 0.0048(3) 0.34497(14) 0.18969(9) 0.0525(8) Uani 1 1 d . . . H32C H -0.0631 0.3267 0.1987 0.079 Uiso 1 1 calc R . . H32B H -0.012 0.3842 0.18 0.079 Uiso 1 1 calc R . . H32A H 0.0579 0.3488 0.2094 0.079 Uiso 1 1 calc R . . C33 C -0.0244(3) 0.30457(16) 0.12781(8) 0.0530(8) Uani 1 1 d . . . H33C H 0.01 0.2825 0.1081 0.08 Uiso 1 1 calc R . . H33B H -0.0402 0.345 0.1199 0.08 Uiso 1 1 calc R . . H33A H -0.0934 0.2851 0.1348 0.08 Uiso 1 1 calc R . . C34 C 0.5827(2) 0.17902(12) 0.13646(7) 0.0336(6) Uani 1 1 d . . . C35 C 0.6201(2) 0.12360(13) 0.12402(8) 0.0378(6) Uani 1 1 d . . . C36 C 0.6848(2) 0.08842(13) 0.14655(8) 0.0453(7) Uani 1 1 d . . . H36 H 0.7121 0.0517 0.138 0.054 Uiso 1 1 calc R . . C37 C 0.7096(2) 0.10621(14) 0.18103(8) 0.0477(8) Uani 1 1 d . . . H37 H 0.7527 0.0816 0.1962 0.057 Uiso 1 1 calc R . . C38 C 0.6716(2) 0.15953(14) 0.19329(8) 0.0446(7) Uani 1 1 d . . . H38 H 0.6878 0.171 0.2173 0.053 Uiso 1 1 calc R . . C39 C 0.6104(2) 0.19730(13) 0.17181(7) 0.0365(6) Uani 1 1 d . . . C40 C 0.5951(3) 0.10240(14) 0.08614(8) 0.0464(7) Uani 1 1 d . . . H40 H 0.5242 0.1213 0.0786 0.056 Uiso 1 1 calc R . . C41 C 0.5803(4) 0.03614(17) 0.08257(11) 0.0790(12) Uani 1 1 d . . . H41C H 0.5581 0.0266 0.0579 0.119 Uiso 1 1 calc R . . H41B H 0.5232 0.0228 0.0993 0.119 Uiso 1 1 calc R . . H41A H 0.6501 0.0163 0.0881 0.119 Uiso 1 1 calc R . . C42 C 0.6833(3) 0.12318(19) 0.06027(9) 0.0726(11) Uani 1 1 d . . . H42C H 0.6866 0.1664 0.0605 0.109 Uiso 1 1 calc R . . H42B H 0.6656 0.1095 0.036 0.109 Uiso 1 1 calc R . . H42A H 0.755 0.1071 0.0676 0.109 Uiso 1 1 calc R . . C43 C 0.5826(2) 0.25868(13) 0.18552(8) 0.0411(7) Uani 1 1 d . . . H43 H 0.5229 0.2753 0.17 0.049 Uiso 1 1 calc R . . C44 C 0.6843(3) 0.29884(15) 0.18213(10) 0.0609(9) Uani 1 1 d . . . H44C H 0.7449 0.2826 0.1965 0.091 Uiso 1 1 calc R . . H44B H 0.666 0.3385 0.1909 0.091 Uiso 1 1 calc R . . H44A H 0.7068 0.3011 0.1569 0.091 Uiso 1 1 calc R . . C45 C 0.5425(3) 0.26026(15) 0.22458(8) 0.0561(9) Uani 1 1 d . . . H45C H 0.4759 0.2361 0.2269 0.084 Uiso 1 1 calc R . . H45B H 0.5257 0.3011 0.2314 0.084 Uiso 1 1 calc R . . H45A H 0.6003 0.2447 0.2404 0.084 Uiso 1 1 calc R . . C46 C 0.2619(2) 0.17684(11) 0.06201(6) 0.0303(6) Uani 1 1 d . . . C47 C 0.1996(2) 0.12426(11) 0.06591(7) 0.0342(6) Uani 1 1 d . . . C48 C 0.2246(2) 0.07642(12) 0.04419(7) 0.0411(7) Uani 1 1 d . . . H48 H 0.1827 0.0412 0.0465 0.049 Uiso 1 1 calc R . . C49 C 0.3093(3) 0.07877(13) 0.01914(8) 0.0436(7) Uani 1 1 d . . . H49 H 0.3271 0.0449 0.0052 0.052 Uiso 1 1 calc R . . C50 C 0.3672(2) 0.13043(12) 0.01464(7) 0.0388(7) Uani 1 1 d . . . H50 H 0.4243 0.132 -0.0028 0.047 Uiso 1 1 calc R . . C51 C 0.3444(2) 0.18047(12) 0.03509(7) 0.0330(6) Uani 1 1 d . . . C52 C 0.1044(2) 0.12141(12) 0.09239(7) 0.0386(7) Uani 1 1 d . . . H52 H 0.1278 0.1431 0.1145 0.046 Uiso 1 1 calc R . . C53 C 0.0027(2) 0.15345(15) 0.07722(9) 0.0527(8) Uani 1 1 d . . . H53C H 0.0212 0.1949 0.0726 0.079 Uiso 1 1 calc R . . H53B H -0.0577 0.1514 0.0947 0.079 Uiso 1 1 calc R . . H53A H -0.0202 0.1345 0.0548 0.079 Uiso 1 1 calc R . . C54 C 0.0717(3) 0.05910(14) 0.10390(9) 0.0588(9) Uani 1 1 d . . . H54C H 0.0487 0.0364 0.0828 0.088 Uiso 1 1 calc R . . H54B H 0.0105 0.0613 0.121 0.088 Uiso 1 1 calc R . . H54A H 0.1349 0.0397 0.1153 0.088 Uiso 1 1 calc R . . C55 C 0.3974(2) 0.23955(12) 0.02619(7) 0.0363(6) Uani 1 1 d . . . H55 H 0.4103 0.261 0.0493 0.044 Uiso 1 1 calc R . . C56 C 0.5068(3) 0.23584(15) 0.00657(9) 0.0531(8) Uani 1 1 d . . . H56C H 0.56 0.2141 0.0213 0.08 Uiso 1 1 calc R . . H56B H 0.5347 0.2758 0.0021 0.08 Uiso 1 1 calc R . . H56A H 0.4964 0.2153 -0.0163 0.08 Uiso 1 1 calc R . . C57 C 0.3157(3) 0.27630(13) 0.00374(9) 0.0481(8) Uani 1 1 d . . . H57C H 0.2983 0.2551 -0.0185 0.072 Uiso 1 1 calc R . . H57B H 0.349 0.3145 -0.0021 0.072 Uiso 1 1 calc R . . H57A H 0.2479 0.2826 0.0175 0.072 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 0.02499(11) 0.02735(10) 0.02521(11) -0.00058(7) 0.00066(7) -0.00061(7) N1 0.0265(12) 0.0291(11) 0.0306(12) 0.0002(9) 0.0026(9) -0.0021(9) N2 0.0241(11) 0.0314(11) 0.0269(11) -0.0003(9) -0.0003(8) -0.0015(9) N3 0.0349(14) 0.0480(15) 0.0252(14) 0.0004(11) 0.0000(10) 0.0120(11) N4 0.0259(13) 0.0375(13) 0.0336(13) -0.0062(10) 0.0015(10) 0.0002(10) C1 0.0252(14) 0.0279(13) 0.0358(15) -0.0016(11) 0.0009(11) -0.0002(10) C2 0.0275(14) 0.0324(14) 0.0311(14) -0.0034(11) -0.0019(10) 0.0015(11) C3 0.0249(14) 0.0374(14) 0.0260(13) -0.0018(11) -0.0032(10) 0.0036(11) C4 0.0348(16) 0.0315(14) 0.0320(15) -0.0032(11) -0.0031(11) 0.0015(12) C5 0.0349(16) 0.0428(16) 0.0448(17) -0.0118(13) 0.0018(13) -0.0037(13) C6 0.0411(18) 0.0460(18) 0.059(2) -0.0167(15) -0.0051(15) -0.0052(14) C7 0.051(2) 0.0478(18) 0.0518(19) -0.0212(15) -0.0077(15) 0.0014(16) C8 0.051(2) 0.0546(19) 0.0455(18) -0.0190(15) 0.0069(14) 0.0018(16) C9 0.0334(16) 0.0476(17) 0.0453(17) -0.0123(14) -0.0001(13) -0.0008(13) C10 0.0388(16) 0.0242(13) 0.0285(14) -0.0027(10) 0.0032(11) -0.0036(11) C11 0.0402(17) 0.0306(14) 0.0398(16) -0.0009(12) 0.0071(12) -0.0046(12) C12 0.051(2) 0.0410(17) 0.0447(18) 0.0021(13) 0.0147(15) -0.0081(14) C13 0.070(2) 0.0309(15) 0.0321(16) 0.0006(12) 0.0111(15) -0.0080(15) C14 0.058(2) 0.0277(14) 0.0337(16) 0.0012(12) -0.0046(14) 0.0001(13) C15 0.0403(16) 0.0253(13) 0.0315(14) -0.0011(11) -0.0001(12) -0.0017(12) C16 0.0336(17) 0.0537(18) 0.0503(19) 0.0059(14) 0.0045(13) -0.0068(14) C17 0.046(2) 0.095(3) 0.072(3) 0.006(2) 0.0102(18) 0.016(2) C18 0.060(2) 0.072(3) 0.088(3) 0.003(2) -0.015(2) -0.023(2) C19 0.0389(17) 0.0368(15) 0.0395(16) 0.0054(12) -0.0052(12) 0.0013(13) C20 0.0446(18) 0.0562(19) 0.0465(18) -0.0036(15) -0.0003(14) 0.0075(15) C21 0.048(2) 0.061(2) 0.051(2) -0.0043(16) -0.0091(15) 0.0025(16) C22 0.0268(14) 0.0370(14) 0.0214(13) -0.0040(11) 0.0029(10) -0.0034(11) C23 0.0302(15) 0.0361(14) 0.0241(13) 0.0008(11) 0.0022(10) -0.0019(11) C24 0.0400(17) 0.0375(15) 0.0356(16) 0.0030(12) 0.0053(12) -0.0073(13) C25 0.0308(16) 0.0525(18) 0.0405(17) -0.0008(14) 0.0092(12) -0.0111(14) C26 0.0257(15) 0.0533(18) 0.0417(17) -0.0004(13) 0.0048(12) -0.0032(13) C27 0.0265(14) 0.0432(15) 0.0308(14) -0.0051(12) 0.0031(11) 0.0000(12) C28 0.0338(16) 0.0353(14) 0.0374(16) 0.0074(12) 0.0042(12) 0.0004(12) C29 0.0445(19) 0.0485(18) 0.062(2) -0.0097(16) 0.0105(15) 0.0024(15) C30 0.0403(18) 0.069(2) 0.0464(19) 0.0149(16) 0.0010(14) 0.0092(16) C31 0.0275(15) 0.0470(17) 0.0433(17) 0.0032(13) 0.0000(12) 0.0043(13) C32 0.052(2) 0.0520(19) 0.054(2) -0.0053(15) 0.0025(15) 0.0120(16) C33 0.0420(19) 0.065(2) 0.052(2) 0.0052(16) -0.0053(14) 0.0089(16) C34 0.0237(14) 0.0407(15) 0.0362(15) 0.0072(12) 0.0014(11) 0.0012(12) C35 0.0292(16) 0.0431(16) 0.0411(16) 0.0054(13) 0.0014(12) 0.0013(12) C36 0.0379(17) 0.0415(17) 0.057(2) 0.0097(14) -0.0007(14) 0.0045(14) C37 0.0364(17) 0.0531(19) 0.054(2) 0.0165(15) -0.0084(14) 0.0034(15) C38 0.0365(17) 0.0589(19) 0.0383(17) 0.0079(14) -0.0072(13) 0.0011(14) C39 0.0258(15) 0.0461(16) 0.0375(16) 0.0045(13) 0.0021(11) 0.0010(12) C40 0.0410(18) 0.0493(18) 0.0489(18) -0.0051(14) -0.0047(14) 0.0108(14) C41 0.086(3) 0.065(2) 0.086(3) -0.015(2) -0.011(2) -0.008(2) C42 0.077(3) 0.095(3) 0.047(2) -0.0038(19) 0.0099(19) -0.007(2) C43 0.0335(16) 0.0504(17) 0.0395(16) 0.0013(13) -0.0058(12) 0.0005(14) C44 0.046(2) 0.059(2) 0.077(2) -0.0025(18) 0.0013(17) -0.0044(17) C45 0.057(2) 0.070(2) 0.0412(18) -0.0087(16) -0.0025(15) 0.0020(17) C46 0.0297(14) 0.0340(14) 0.0271(13) -0.0017(11) -0.0061(11) 0.0018(11) C47 0.0385(16) 0.0338(14) 0.0305(14) 0.0021(11) -0.0073(12) -0.0018(12) C48 0.0521(19) 0.0311(15) 0.0402(16) -0.0024(12) -0.0039(14) -0.0035(13) C49 0.057(2) 0.0363(16) 0.0380(17) -0.0091(12) -0.0030(14) 0.0059(14) C50 0.0400(17) 0.0442(16) 0.0323(15) -0.0033(12) 0.0018(12) 0.0042(13) C51 0.0322(15) 0.0376(15) 0.0291(14) -0.0009(11) -0.0038(11) 0.0043(12) C52 0.0423(17) 0.0385(15) 0.0351(15) -0.0032(12) -0.0015(12) -0.0086(13) C53 0.0381(18) 0.069(2) 0.0510(19) -0.0100(16) -0.0034(14) -0.0041(16) C54 0.065(2) 0.0507(19) 0.061(2) -0.0014(16) 0.0151(17) -0.0161(17) C55 0.0349(15) 0.0417(16) 0.0324(15) -0.0026(12) 0.0013(12) -0.0026(12) C56 0.0448(19) 0.058(2) 0.057(2) 0.0050(16) 0.0136(15) 0.0016(15) C57 0.0472(19) 0.0354(16) 0.062(2) 0.0033(14) -0.0105(15) 0.0002(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N4 2.078(2) . ? In N3 2.081(2) . ? In N2 2.150(2) . ? In N1 2.166(2) . ? N1 C1 1.319(3) . ? N1 C10 1.448(3) . ? N2 C3 1.325(3) . ? N2 C22 1.446(3) . ? N3 C34 1.400(3) . ? N4 C46 1.408(3) . ? C1 C2 1.405(4) . ? C2 C3 1.396(4) . ? C2 C4 1.494(4) . ? C4 C5 1.391(4) . ? C4 C9 1.391(4) . ? C5 C6 1.389(4) . ? C6 C7 1.370(4) . ? C7 C8 1.382(4) . ? C8 C9 1.392(4) . ? C10 C11 1.404(4) . ? C10 C15 1.405(4) . ? C11 C12 1.398(4) . ? C11 C16 1.520(4) . ? C12 C13 1.376(4) . ? C13 C14 1.382(4) . ? C14 C15 1.393(4) . ? C15 C19 1.522(4) . ? C16 C18 1.530(5) . ? C16 C17 1.535(4) . ? C19 C21 1.521(4) . ? C19 C20 1.550(4) . ? C22 C23 1.402(4) . ? C22 C27 1.414(4) . ? C23 C24 1.393(4) . ? C23 C28 1.520(4) . ? C24 C25 1.377(4) . ? C25 C26 1.371(4) . ? C26 C27 1.398(4) . ? C27 C31 1.520(4) . ? C28 C30 1.531(4) . ? C28 C29 1.532(4) . ? C31 C33 1.530(4) . ? C31 C32 1.533(4) . ? C34 C35 1.413(4) . ? C34 C39 1.420(4) . ? C35 C36 1.397(4) . ? C35 C40 1.520(4) . ? C36 C37 1.378(4) . ? C37 C38 1.371(4) . ? C38 C39 1.386(4) . ? C39 C43 1.519(4) . ? C40 C42 1.514(5) . ? C40 C41 1.517(5) . ? C43 C45 1.533(4) . ? C43 C44 1.537(4) . ? C46 C47 1.417(4) . ? C46 C51 1.418(4) . ? C47 C48 1.386(4) . ? C47 C52 1.519(4) . ? C48 C49 1.388(4) . ? C49 C50 1.375(4) . ? C50 C51 1.393(4) . ? C51 C55 1.521(4) . ? C52 C54 1.527(4) . ? C52 C53 1.538(4) . ? C55 C56 1.515(4) . ? C55 C57 1.540(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 N4 In N3 118.47(10) . . ? N4 In N2 103.22(9) . . ? N3 In N2 123.96(9) . . ? N4 In N1 112.84(8) . . ? N3 In N1 107.12(9) . . ? N2 In N1 87.10(7) . . ? C1 N1 C10 118.2(2) . . ? C1 N1 In 121.70(17) . . ? C10 N1 In 120.11(15) . . ? C3 N2 C22 118.1(2) . . ? C3 N2 In 122.85(17) . . ? C22 N2 In 118.55(15) . . ? C34 N3 In 132.16(18) . . ? C46 N4 In 119.05(17) . . ? N1 C1 C2 128.7(2) . . ? C3 C2 C1 123.9(2) . . ? C3 C2 C4 119.3(2) . . ? C1 C2 C4 116.4(2) . . ? N2 C3 C2 128.1(2) . . ? C5 C4 C9 117.6(2) . . ? C5 C4 C2 120.3(2) . . ? C9 C4 C2 122.2(2) . . ? C6 C5 C4 121.3(3) . . ? C7 C6 C5 120.5(3) . . ? C6 C7 C8 119.2(3) . . ? C7 C8 C9 120.5(3) . . ? C4 C9 C8 120.9(3) . . ? C11 C10 C15 121.9(2) . . ? C11 C10 N1 119.3(2) . . ? C15 C10 N1 118.7(2) . . ? C12 C11 C10 117.8(3) . . ? C12 C11 C16 120.4(3) . . ? C10 C11 C16 121.8(2) . . ? C13 C12 C11 121.0(3) . . ? C12 C13 C14 120.4(3) . . ? C13 C14 C15 121.1(3) . . ? C14 C15 C10 117.8(3) . . ? C14 C15 C19 121.3(2) . . ? C10 C15 C19 120.9(2) . . ? C11 C16 C18 110.5(3) . . ? C11 C16 C17 112.0(3) . . ? C18 C16 C17 111.0(3) . . ? C21 C19 C15 113.4(2) . . ? C21 C19 C20 108.3(2) . . ? C15 C19 C20 111.5(2) . . ? C23 C22 C27 121.6(2) . . ? C23 C22 N2 120.1(2) . . ? C27 C22 N2 118.2(2) . . ? C24 C23 C22 118.1(2) . . ? C24 C23 C28 119.7(2) . . ? C22 C23 C28 122.2(2) . . ? C25 C24 C23 121.1(3) . . ? C26 C25 C24 120.3(3) . . ? C25 C26 C27 121.6(3) . . ? C26 C27 C22 117.3(2) . . ? C26 C27 C31 119.8(2) . . ? C22 C27 C31 122.9(2) . . ? C23 C28 C30 111.5(2) . . ? C23 C28 C29 111.5(2) . . ? C30 C28 C29 110.1(3) . . ? C27 C31 C33 112.0(2) . . ? C27 C31 C32 112.2(2) . . ? C33 C31 C32 109.7(2) . . ? N3 C34 C35 120.7(2) . . ? N3 C34 C39 120.1(3) . . ? C35 C34 C39 119.1(2) . . ? C36 C35 C34 119.3(3) . . ? C36 C35 C40 119.3(3) . . ? C34 C35 C40 121.4(2) . . ? C37 C36 C35 121.0(3) . . ? C38 C37 C36 119.6(3) . . ? C37 C38 C39 122.1(3) . . ? C38 C39 C34 118.8(3) . . ? C38 C39 C43 119.3(3) . . ? C34 C39 C43 121.7(2) . . ? C42 C40 C41 109.6(3) . . ? C42 C40 C35 110.5(3) . . ? C41 C40 C35 114.7(3) . . ? C39 C43 C45 114.2(2) . . ? C39 C43 C44 109.7(2) . . ? C45 C43 C44 108.6(3) . . ? N4 C46 C47 122.0(2) . . ? N4 C46 C51 118.2(2) . . ? C47 C46 C51 119.8(2) . . ? C48 C47 C46 118.8(3) . . ? C48 C47 C52 120.7(2) . . ? C46 C47 C52 120.5(2) . . ? C47 C48 C49 121.6(3) . . ? C50 C49 C48 119.5(3) . . ? C49 C50 C51 121.6(3) . . ? C50 C51 C46 118.6(2) . . ? C50 C51 C55 120.8(2) . . ? C46 C51 C55 120.2(2) . . ? C47 C52 C54 114.8(2) . . ? C47 C52 C53 110.5(2) . . ? C54 C52 C53 109.3(3) . . ? C56 C55 C51 115.2(2) . . ? C56 C55 C57 109.3(2) . . ? C51 C55 C57 108.8(2) . . ? #===END data_(10)-dec2403 _database_code_depnum_ccdc_archive 'CCDC 609665' _audit_creation_date 2003-12-22T08:27:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[{InCl(OH)(ArNCHCPhCHNAr)}2].(thf)' ; _chemical_formula_moiety '(C66 H84 Cl2 In2 N4 O2) (C4 H8 O1)' _chemical_formula_sum 'C70 H92 Cl2 In2 N4 O3' _chemical_formula_weight 1338.02 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3394(2) _cell_length_b 14.4401(2) _cell_length_c 17.9795(3) _cell_angle_alpha 83.201(1) _cell_angle_beta 70.719(1) _cell_angle_gamma 71.788(1) _cell_volume 3337.55(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28899 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7607 _exptl_absorpt_correction_T_max 0.8358 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.682793E-1 _diffrn_orient_matrix_ub_12 0.425036E-1 _diffrn_orient_matrix_ub_13 0.31801E-1 _diffrn_orient_matrix_ub_21 0.360045E-1 _diffrn_orient_matrix_ub_22 0.310128E-1 _diffrn_orient_matrix_ub_23 0.243928E-1 _diffrn_orient_matrix_ub_31 0.28212E-2 _diffrn_orient_matrix_ub_32 0.504788E-1 _diffrn_orient_matrix_ub_33 -0.432054E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_number 49840 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 15237 _reflns_number_gt 13503 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The hydroxyl hydrogens were located on a difference map and refined; other hydrogens were in riding mode. 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^)+(0.0289P)^2^+2.6200P] 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_number_reflns 15237 _refine_ls_number_parameters 738 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.068 _refine_ls_wR_factor_gt 0.064 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.813 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.118586(9) 0.003768(8) -0.001135(7) 0.01801(4) Uani 1 1 d . . . Cl Cl 0.20961(4) 0.03196(4) -0.13365(3) 0.03367(11) Uani 1 1 d . . . O1 O 0.03461(10) -0.09148(10) -0.00182(9) 0.0270(3) Uani 1 1 d . . . H1X H 0.056(2) -0.144(2) -0.0081(17) 0.050(9) Uiso 1 1 d . . . N1 N 0.22896(12) -0.10647(11) 0.04667(9) 0.0215(3) Uani 1 1 d . . . N2 N 0.12500(11) 0.10477(11) 0.07462(9) 0.0199(3) Uani 1 1 d . . . C1 C 0.28855(14) -0.08534(14) 0.08033(11) 0.0227(4) Uani 1 1 d . . . H1 H 0.34 -0.1392 0.0924 0.027 Uiso 1 1 calc R . . C2 C 0.28551(14) 0.00671(13) 0.10057(10) 0.0218(4) Uani 1 1 d . . . C3 C 0.20433(14) 0.09159(13) 0.10149(11) 0.0214(3) Uani 1 1 d . . . H3 H 0.2061 0.1469 0.1242 0.026 Uiso 1 1 calc R . . C4 C 0.36666(14) 0.01156(14) 0.13356(11) 0.0244(4) Uani 1 1 d . . . C5 C 0.46978(15) -0.04257(15) 0.10001(12) 0.0291(4) Uani 1 1 d . . . H5 H 0.4882 -0.0813 0.0553 0.035 Uiso 1 1 calc R . . C6 C 0.54549(17) -0.04005(17) 0.13159(14) 0.0372(5) Uani 1 1 d . . . H6 H 0.615 -0.0778 0.1087 0.045 Uiso 1 1 calc R . . C7 C 0.52015(17) 0.01686(18) 0.19584(14) 0.0386(5) Uani 1 1 d . . . H7 H 0.572 0.0183 0.2172 0.046 Uiso 1 1 calc R . . C8 C 0.41883(18) 0.07180(18) 0.22905(13) 0.0366(5) Uani 1 1 d . . . H8 H 0.4013 0.1117 0.2729 0.044 Uiso 1 1 calc R . . C9 C 0.34266(16) 0.06873(16) 0.19837(12) 0.0306(4) Uani 1 1 d . . . H9 H 0.2732 0.1062 0.2219 0.037 Uiso 1 1 calc R . . C10 C 0.23747(15) -0.20887(13) 0.04446(12) 0.0260(4) Uani 1 1 d . . . C11 C 0.30798(18) -0.26372(15) -0.02083(13) 0.0354(5) Uani 1 1 d . . . C12 C 0.3098(2) -0.36111(18) -0.02203(18) 0.0558(7) Uani 1 1 d . . . H12 H 0.3562 -0.4003 -0.0656 0.067 Uiso 1 1 calc R . . C13 C 0.2451(3) -0.40106(19) 0.0390(2) 0.0631(8) Uani 1 1 d . . . H13 H 0.2468 -0.4669 0.0365 0.076 Uiso 1 1 calc R . . C14 C 0.1790(2) -0.34692(18) 0.10283(17) 0.0491(6) Uani 1 1 d . . . H14 H 0.1363 -0.3762 0.1447 0.059 Uiso 1 1 calc R . . C15 C 0.17274(17) -0.24885(15) 0.10807(14) 0.0338(5) Uani 1 1 d . . . C16 C 0.38487(19) -0.22365(16) -0.08555(13) 0.0395(5) Uani 1 1 d . . . H16 H 0.3576 -0.1509 -0.0849 0.047 Uiso 1 1 calc R . . C17 C 0.4014(3) -0.2568(2) -0.16749(16) 0.0637(8) Uani 1 1 d . . . H17C H 0.4277 -0.328 -0.1695 0.096 Uiso 1 1 calc R . . H17B H 0.4515 -0.2284 -0.2066 0.096 Uiso 1 1 calc R . . H17A H 0.3356 -0.2351 -0.1791 0.096 Uiso 1 1 calc R . . C18 C 0.4889(2) -0.2523(2) -0.06940(16) 0.0547(7) Uani 1 1 d . . . H18C H 0.4794 -0.2258 -0.0188 0.082 Uiso 1 1 calc R . . H18B H 0.5379 -0.2258 -0.1115 0.082 Uiso 1 1 calc R . . H18A H 0.5161 -0.3235 -0.0676 0.082 Uiso 1 1 calc R . . C19 C 0.10285(18) -0.19130(18) 0.18129(14) 0.0407(5) Uani 1 1 d . . . H19 H 0.0976 -0.1209 0.1686 0.049 Uiso 1 1 calc R . . C20 C 0.1496(2) -0.2209(3) 0.2480(2) 0.0857(12) Uani 1 1 d . . . H20C H 0.1584 -0.2904 0.2602 0.129 Uiso 1 1 calc R . . H20B H 0.1036 -0.1828 0.2948 0.129 Uiso 1 1 calc R . . H20A H 0.2169 -0.2085 0.2321 0.129 Uiso 1 1 calc R . . C21 C -0.0057(2) -0.2009(3) 0.20877(18) 0.0617(8) Uani 1 1 d . . . H21C H -0.0377 -0.1775 0.1669 0.093 Uiso 1 1 calc R . . H21B H -0.0467 -0.1618 0.256 0.093 Uiso 1 1 calc R . . H21A H -0.0029 -0.2694 0.2212 0.093 Uiso 1 1 calc R . . C22 C 0.04530(14) 0.19678(13) 0.09464(11) 0.0229(4) Uani 1 1 d . . . C23 C 0.05408(17) 0.27848(14) 0.04524(12) 0.0307(4) Uani 1 1 d . . . C24 C -0.0243(2) 0.36554(17) 0.06736(16) 0.0460(6) Uani 1 1 d . . . H24 H -0.0207 0.4221 0.035 0.055 Uiso 1 1 calc R . . C25 C -0.1067(2) 0.37146(18) 0.13491(17) 0.0511(7) Uani 1 1 d . . . H25 H -0.1581 0.4322 0.1494 0.061 Uiso 1 1 calc R . . C26 C -0.11515(18) 0.28963(17) 0.18187(15) 0.0424(5) Uani 1 1 d . . . H26 H -0.1732 0.2944 0.2278 0.051 Uiso 1 1 calc R . . C27 C -0.03949(15) 0.20007(15) 0.16264(12) 0.0287(4) Uani 1 1 d . . . C28 C 0.1463(2) 0.27382(16) -0.02841(12) 0.0379(5) Uani 1 1 d . . . H28 H 0.1776 0.2041 -0.0445 0.045 Uiso 1 1 calc R . . C29 C 0.1175(3) 0.3325(2) -0.09788(16) 0.0643(9) Uani 1 1 d . . . H29C H 0.0688 0.3078 -0.1113 0.096 Uiso 1 1 calc R . . H29B H 0.1799 0.3262 -0.1434 0.096 Uiso 1 1 calc R . . H29A H 0.0853 0.4013 -0.0837 0.096 Uiso 1 1 calc R . . C30 C 0.2289(3) 0.3064(3) -0.01180(16) 0.0665(9) Uani 1 1 d . . . H30C H 0.1998 0.3738 0.0064 0.1 Uiso 1 1 calc R . . H30B H 0.2873 0.3024 -0.0601 0.1 Uiso 1 1 calc R . . H30A H 0.2528 0.2639 0.029 0.1 Uiso 1 1 calc R . . C31 C -0.04787(17) 0.10944(16) 0.21369(13) 0.0351(5) Uani 1 1 d . . . H31 H -0.0178 0.0524 0.1778 0.042 Uiso 1 1 calc R . . C32 C 0.0151(2) 0.0919(2) 0.27105(14) 0.0482(6) Uani 1 1 d . . . H32C H 0.088 0.0836 0.2412 0.072 Uiso 1 1 calc R . . H32B H 0.0084 0.033 0.3028 0.072 Uiso 1 1 calc R . . H32A H -0.0107 0.1479 0.3057 0.072 Uiso 1 1 calc R . . C33 C -0.1590(2) 0.1113(2) 0.26009(15) 0.0506(6) Uani 1 1 d . . . H33C H -0.1911 0.1673 0.2952 0.076 Uiso 1 1 calc R . . H33B H -0.1589 0.0509 0.2914 0.076 Uiso 1 1 calc R . . H33A H -0.1981 0.1168 0.2234 0.076 Uiso 1 1 calc R . . In1B In 0.468216(9) 0.454396(8) 0.431017(7) 0.01750(4) Uani 1 1 d . . 1 Cl1B Cl 0.62175(4) 0.37977(4) 0.33080(3) 0.03734(12) Uani 1 1 d . A 1 O1B O 0.49278(12) 0.57968(11) 0.46309(9) 0.0289(3) Uani 1 1 d . . 1 H1Y H 0.494(2) 0.620(2) 0.4416(17) 0.044(9) Uiso 1 1 d . B 1 N1B N 0.36532(11) 0.54232(10) 0.36742(9) 0.0192(3) Uani 1 1 d . C 1 N2B N 0.36657(11) 0.36201(11) 0.46393(9) 0.0198(3) Uani 1 1 d . C 1 C1B C 0.31175(14) 0.50563(13) 0.33820(10) 0.0205(3) Uani 1 1 d . C 1 H1B H 0.283 0.5454 0.3005 0.025 Uiso 1 1 calc R C 1 C2B C 0.29193(14) 0.41480(13) 0.35595(10) 0.0209(3) Uani 1 1 d . C 1 C3B C 0.31085(14) 0.35549(13) 0.41997(11) 0.0211(3) Uani 1 1 d . C 1 H3B H 0.2798 0.304 0.4336 0.025 Uiso 1 1 calc R C 1 C4B C 0.23441(15) 0.38799(13) 0.31042(11) 0.0236(4) Uani 1 1 d . C 1 C5B C 0.2581(2) 0.40618(18) 0.22978(13) 0.0402(5) Uani 1 1 d . C 1 H5B H 0.3128 0.4337 0.2036 0.048 Uiso 1 1 calc R C 1 C6B C 0.2026(2) 0.3847(2) 0.18661(15) 0.0525(7) Uani 1 1 d . C 1 H6B H 0.2186 0.3994 0.1317 0.063 Uiso 1 1 calc R C 1 C7B C 0.1249(2) 0.34224(17) 0.22288(15) 0.0426(6) Uani 1 1 d . C 1 H7B H 0.0876 0.3272 0.1933 0.051 Uiso 1 1 calc R C 1 C8B C 0.10189(17) 0.32195(17) 0.30252(14) 0.0374(5) Uani 1 1 d . C 1 H8B H 0.0491 0.2918 0.3279 0.045 Uiso 1 1 calc R C 1 C9B C 0.15514(15) 0.34510(15) 0.34615(13) 0.0305(4) Uani 1 1 d . C 1 H9B H 0.1374 0.3316 0.4012 0.037 Uiso 1 1 calc R C 1 C10B C 0.35508(14) 0.64519(13) 0.35185(11) 0.0220(4) Uani 1 1 d . C 1 C11B C 0.41967(16) 0.67540(15) 0.28260(12) 0.0304(4) Uani 1 1 d . C 1 C12B C 0.4064(2) 0.77560(17) 0.27140(14) 0.0420(6) Uani 1 1 d . C 1 H12B H 0.4497 0.7984 0.2254 0.05 Uiso 1 1 calc R C 1 C13B C 0.3325(2) 0.84180(17) 0.32510(15) 0.0499(7) Uani 1 1 d . C 1 H13B H 0.3245 0.9095 0.3156 0.06 Uiso 1 1 calc R C 1 C14B C 0.2697(2) 0.81026(16) 0.39313(14) 0.0440(6) Uani 1 1 d . C 1 H14B H 0.2186 0.8567 0.43 0.053 Uiso 1 1 calc R C 1 C15B C 0.28038(17) 0.71115(14) 0.40825(12) 0.0290(4) Uani 1 1 d . C 1 C16B C 0.50095(18) 0.60484(19) 0.22151(14) 0.0455(6) Uani 1 1 d . C 1 H16B H 0.4981 0.5374 0.2401 0.055 Uiso 1 1 calc R C 1 C17B C 0.6087(2) 0.6104(3) 0.2130(2) 0.0854(13) Uani 1 1 d . C 1 H17F H 0.6126 0.6766 0.1966 0.128 Uiso 1 1 calc R C 1 H17E H 0.6604 0.5641 0.1733 0.128 Uiso 1 1 calc R C 1 H17D H 0.6222 0.5941 0.2637 0.128 Uiso 1 1 calc R C 1 C18B C 0.4792(3) 0.6234(3) 0.14233(16) 0.0779(11) Uani 1 1 d . C 1 H18F H 0.4115 0.6154 0.1489 0.117 Uiso 1 1 calc R C 1 H18E H 0.5327 0.5767 0.1037 0.117 Uiso 1 1 calc R C 1 H18D H 0.4795 0.6899 0.1236 0.117 Uiso 1 1 calc R C 1 C19B C 0.21138(17) 0.67655(15) 0.48325(13) 0.0348(5) Uani 1 1 d . C 1 H19B H 0.2507 0.6091 0.4952 0.042 Uiso 1 1 calc R C 1 C20B C 0.1131(2) 0.6692(2) 0.47120(16) 0.0510(6) Uani 1 1 d . C 1 H20F H 0.0742 0.7335 0.4562 0.076 Uiso 1 1 calc R C 1 H20E H 0.0704 0.6467 0.5203 0.076 Uiso 1 1 calc R C 1 H20D H 0.1318 0.6229 0.4294 0.076 Uiso 1 1 calc R C 1 C21B C 0.1851(2) 0.73821(19) 0.55457(14) 0.0470(6) Uani 1 1 d . C 1 H21F H 0.2489 0.7364 0.5645 0.07 Uiso 1 1 calc R C 1 H21E H 0.1409 0.7122 0.6008 0.07 Uiso 1 1 calc R C 1 H21D H 0.1486 0.8057 0.5443 0.07 Uiso 1 1 calc R C 1 C22B C 0.35818(15) 0.29958(13) 0.53387(11) 0.0225(4) Uani 1 1 d . C 1 C23B C 0.43692(16) 0.21110(14) 0.53166(12) 0.0269(4) Uani 1 1 d . C 1 C24B C 0.42628(19) 0.15321(16) 0.60030(13) 0.0385(5) Uani 1 1 d . C 1 H24B H 0.4786 0.0938 0.6014 0.046 Uiso 1 1 calc R C 1 C25B C 0.3415(2) 0.18040(18) 0.66652(14) 0.0450(6) Uani 1 1 d . C 1 H25B H 0.3357 0.1393 0.7121 0.054 Uiso 1 1 calc R C 1 C26B C 0.26532(19) 0.26694(17) 0.66680(13) 0.0393(5) Uani 1 1 d . C 1 H26B H 0.2069 0.2844 0.7125 0.047 Uiso 1 1 calc R C 1 C27B C 0.27285(16) 0.32946(14) 0.60065(12) 0.0290(4) Uani 1 1 d . C 1 C28B C 0.52655(16) 0.17880(14) 0.45742(13) 0.0317(4) Uani 1 1 d . C 1 H28B H 0.5472 0.238 0.4325 0.038 Uiso 1 1 calc R C 1 C29B C 0.6219(2) 0.1047(2) 0.47158(17) 0.0523(7) Uani 1 1 d . C 1 H29F H 0.6462 0.1329 0.5059 0.078 Uiso 1 1 calc R C 1 H29E H 0.6765 0.0878 0.4211 0.078 Uiso 1 1 calc R C 1 H29D H 0.6041 0.0459 0.4968 0.078 Uiso 1 1 calc R C 1 C30B C 0.4959(2) 0.13687(19) 0.39760(16) 0.0498(6) Uani 1 1 d . C 1 H30F H 0.4724 0.0801 0.421 0.075 Uiso 1 1 calc R C 1 H30E H 0.5557 0.1171 0.3504 0.075 Uiso 1 1 calc R C 1 H30D H 0.44 0.1866 0.3831 0.075 Uiso 1 1 calc R C 1 C31B C 0.18838(16) 0.42588(15) 0.60404(13) 0.0339(5) Uani 1 1 d . C 1 H31B H 0.2134 0.4652 0.5561 0.041 Uiso 1 1 calc R C 1 C32B C 0.0891(2) 0.4093(2) 0.60119(19) 0.0548(7) Uani 1 1 d . C 1 H32F H 0.1034 0.3765 0.5522 0.082 Uiso 1 1 calc R C 1 H32E H 0.0363 0.4723 0.6031 0.082 Uiso 1 1 calc R C 1 H32D H 0.0642 0.3686 0.6464 0.082 Uiso 1 1 calc R C 1 C33B C 0.1670(2) 0.4848(2) 0.67577(17) 0.0533(7) Uani 1 1 d . C 1 H33F H 0.1444 0.4472 0.7238 0.08 Uiso 1 1 calc R C 1 H33E H 0.1127 0.546 0.6755 0.08 Uiso 1 1 calc R C 1 H33D H 0.2302 0.499 0.6741 0.08 Uiso 1 1 calc R C 1 O1C O 0.7897(3) -0.1610(2) 0.51762(18) 0.1061(10) Uani 1 1 d . D 1 C1C C 0.8444(3) -0.1310(3) 0.4471(2) 0.0812(11) Uani 1 1 d . D 1 H1C1 H 0.7972 -0.0956 0.4167 0.097 Uiso 1 1 calc R D 1 H1C2 H 0.8948 -0.1882 0.4165 0.097 Uiso 1 1 calc R D 1 C2C C 0.9009(3) -0.0645(2) 0.4603(2) 0.0872(13) Uani 1 1 d . D 1 H2C1 H 0.8693 0.0042 0.4472 0.105 Uiso 1 1 calc R D 1 H2C2 H 0.9749 -0.0848 0.4288 0.105 Uiso 1 1 calc R D 1 C3C C 0.8865(3) -0.0791(2) 0.5495(2) 0.0772(11) Uani 1 1 d . D 1 H3C1 H 0.9423 -0.134 0.5606 0.093 Uiso 1 1 calc R D 1 H3C2 H 0.8815 -0.0192 0.574 0.093 Uiso 1 1 calc R D 1 C4C C 0.7849(3) -0.1020(2) 0.57485(18) 0.0616(8) Uani 1 1 d . D 1 H4C1 H 0.7742 -0.1363 0.6267 0.074 Uiso 1 1 calc R D 1 H4C2 H 0.7272 -0.0413 0.5793 0.074 Uiso 1 1 calc R D 1 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 0.01491(6) 0.02065(6) 0.02099(6) -0.00152(5) -0.00764(5) -0.00604(5) Cl 0.0282(2) 0.0501(3) 0.0230(2) 0.0010(2) -0.00563(19) -0.0147(2) O1 0.0198(7) 0.0188(7) 0.0471(9) -0.0041(6) -0.0162(6) -0.0046(5) N1 0.0204(7) 0.0199(7) 0.0265(8) 0.0005(6) -0.0101(6) -0.0063(6) N2 0.0183(7) 0.0219(7) 0.0207(7) -0.0009(6) -0.0079(6) -0.0054(6) C1 0.0182(8) 0.0267(9) 0.0245(9) 0.0027(7) -0.0094(7) -0.0066(7) C2 0.0206(8) 0.0262(9) 0.0224(9) 0.0018(7) -0.0099(7) -0.0096(7) C3 0.0209(9) 0.0232(9) 0.0241(9) 0.0005(7) -0.0090(7) -0.0101(7) C4 0.0233(9) 0.0298(9) 0.0269(9) 0.0065(8) -0.0131(8) -0.0139(8) C5 0.0247(10) 0.0324(10) 0.0351(11) 0.0032(8) -0.0136(8) -0.0118(8) C6 0.0251(10) 0.0424(12) 0.0504(13) 0.0069(10) -0.0192(10) -0.0133(9) C7 0.0330(11) 0.0531(14) 0.0442(13) 0.0106(11) -0.0252(10) -0.0223(10) C8 0.0396(12) 0.0514(13) 0.0314(11) 0.0011(10) -0.0186(10) -0.0229(10) C9 0.0268(10) 0.0427(12) 0.0283(10) 0.0003(9) -0.0118(8) -0.0153(9) C10 0.0266(9) 0.0212(9) 0.0351(10) 0.0019(8) -0.0165(8) -0.0072(7) C11 0.0419(12) 0.0251(10) 0.0392(12) -0.0017(9) -0.0146(10) -0.0074(9) C12 0.0745(19) 0.0269(12) 0.0585(17) -0.0105(11) -0.0107(15) -0.0116(12) C13 0.084(2) 0.0255(12) 0.081(2) -0.0023(13) -0.0195(18) -0.0240(13) C14 0.0506(15) 0.0320(12) 0.0670(17) 0.0108(12) -0.0167(13) -0.0210(11) C15 0.0316(11) 0.0287(10) 0.0445(12) 0.0063(9) -0.0162(10) -0.0115(9) C16 0.0469(13) 0.0302(11) 0.0334(11) -0.0030(9) -0.0078(10) -0.0041(10) C17 0.085(2) 0.0635(18) 0.0391(14) -0.0059(13) -0.0199(15) -0.0147(17) C18 0.0477(15) 0.0680(18) 0.0426(14) 0.0061(13) -0.0085(12) -0.0171(13) C19 0.0360(12) 0.0380(12) 0.0447(13) 0.0094(10) -0.0086(10) -0.0141(10) C20 0.0460(17) 0.151(4) 0.0581(19) -0.028(2) -0.0234(15) -0.008(2) C21 0.0368(14) 0.084(2) 0.0588(17) 0.0111(16) -0.0126(13) -0.0169(14) C22 0.0243(9) 0.0219(9) 0.0259(9) -0.0054(7) -0.0129(8) -0.0042(7) C23 0.0398(11) 0.0251(9) 0.0307(10) -0.0021(8) -0.0171(9) -0.0073(8) C24 0.0614(16) 0.0248(11) 0.0498(14) -0.0021(10) -0.0245(13) -0.0017(10) C25 0.0472(15) 0.0295(12) 0.0688(18) -0.0168(12) -0.0221(14) 0.0098(10) C26 0.0285(11) 0.0414(13) 0.0507(14) -0.0195(11) -0.0042(10) -0.0030(9) C27 0.0254(10) 0.0306(10) 0.0308(10) -0.0103(8) -0.0074(8) -0.0072(8) C28 0.0595(15) 0.0283(10) 0.0269(10) 0.0016(8) -0.0111(10) -0.0177(10) C29 0.107(3) 0.0573(17) 0.0354(14) 0.0074(12) -0.0291(16) -0.0290(17) C30 0.083(2) 0.098(2) 0.0377(14) 0.0129(15) -0.0149(15) -0.062(2) C31 0.0349(11) 0.0374(11) 0.0301(10) -0.0070(9) 0.0008(9) -0.0158(9) C32 0.0447(14) 0.0636(16) 0.0341(12) 0.0070(11) -0.0067(11) -0.0214(12) C33 0.0462(14) 0.0636(17) 0.0436(14) -0.0139(12) 0.0027(11) -0.0313(13) In1B 0.01827(6) 0.01780(6) 0.01909(6) 0.00081(4) -0.00901(5) -0.00594(5) Cl1B 0.0261(2) 0.0384(3) 0.0351(3) -0.0032(2) 0.0002(2) -0.0018(2) O1B 0.0475(9) 0.0217(7) 0.0315(8) 0.0105(6) -0.0269(7) -0.0179(7) N1B 0.0203(7) 0.0184(7) 0.0209(7) 0.0029(6) -0.0088(6) -0.0070(6) N2B 0.0225(7) 0.0195(7) 0.0212(7) 0.0041(6) -0.0108(6) -0.0087(6) C1B 0.0230(9) 0.0212(8) 0.0182(8) 0.0019(7) -0.0092(7) -0.0055(7) C2B 0.0217(8) 0.0223(8) 0.0220(8) -0.0001(7) -0.0102(7) -0.0077(7) C3B 0.0213(8) 0.0206(8) 0.0252(9) 0.0005(7) -0.0091(7) -0.0095(7) C4B 0.0277(9) 0.0209(8) 0.0272(9) 0.0008(7) -0.0151(8) -0.0072(7) C5B 0.0600(15) 0.0475(13) 0.0293(11) 0.0055(10) -0.0215(11) -0.0321(12) C6B 0.087(2) 0.0600(16) 0.0364(13) 0.0089(11) -0.0386(14) -0.0409(16) C7B 0.0564(15) 0.0364(12) 0.0539(14) -0.0037(10) -0.0397(13) -0.0145(11) C8B 0.0330(11) 0.0381(12) 0.0514(14) -0.0028(10) -0.0219(10) -0.0146(9) C9B 0.0279(10) 0.0362(11) 0.0332(11) -0.0012(9) -0.0137(9) -0.0125(9) C10B 0.0261(9) 0.0203(8) 0.0255(9) 0.0059(7) -0.0155(8) -0.0093(7) C11B 0.0317(10) 0.0338(10) 0.0303(10) 0.0116(8) -0.0144(9) -0.0150(9) C12B 0.0588(15) 0.0396(12) 0.0409(13) 0.0225(10) -0.0252(12) -0.0309(12) C13B 0.092(2) 0.0239(11) 0.0492(14) 0.0123(10) -0.0364(15) -0.0272(12) C14B 0.0740(18) 0.0215(10) 0.0383(12) 0.0004(9) -0.0248(12) -0.0087(11) C15B 0.0387(11) 0.0219(9) 0.0294(10) 0.0023(8) -0.0174(9) -0.0067(8) C16B 0.0365(12) 0.0469(13) 0.0362(12) 0.0184(10) -0.0029(10) -0.0050(10) C17B 0.0350(15) 0.097(3) 0.098(3) 0.046(2) -0.0043(16) -0.0177(16) C18B 0.094(3) 0.070(2) 0.0326(14) -0.0025(14) -0.0118(15) 0.0179(18) C19B 0.0384(12) 0.0244(10) 0.0326(11) -0.0011(8) -0.0063(9) -0.0015(9) C20B 0.0442(14) 0.0569(16) 0.0483(15) -0.0144(12) -0.0044(12) -0.0155(12) C21B 0.0514(15) 0.0476(14) 0.0346(12) -0.0086(10) -0.0105(11) -0.0048(12) C22B 0.0294(9) 0.0215(8) 0.0232(9) 0.0058(7) -0.0140(8) -0.0125(7) C23B 0.0320(10) 0.0213(9) 0.0310(10) 0.0051(8) -0.0152(8) -0.0091(8) C24B 0.0462(13) 0.0280(10) 0.0384(12) 0.0115(9) -0.0190(10) -0.0051(9) C25B 0.0619(16) 0.0386(12) 0.0308(11) 0.0168(10) -0.0173(11) -0.0129(11) C26B 0.0487(13) 0.0386(12) 0.0252(10) 0.0078(9) -0.0061(10) -0.0140(10) C27B 0.0342(11) 0.0271(10) 0.0268(10) 0.0031(8) -0.0108(8) -0.0104(8) C28B 0.0336(11) 0.0216(9) 0.0377(11) 0.0047(8) -0.0114(9) -0.0066(8) C29B 0.0387(13) 0.0508(15) 0.0574(16) 0.0058(13) -0.0142(12) -0.0028(11) C30B 0.0527(15) 0.0435(14) 0.0472(14) -0.0163(11) -0.0135(12) -0.0024(12) C31B 0.0318(11) 0.0309(10) 0.0313(11) 0.0043(8) -0.0040(9) -0.0066(9) C32B 0.0429(14) 0.0528(16) 0.0691(19) -0.0039(14) -0.0236(14) -0.0069(12) C33B 0.0524(16) 0.0439(14) 0.0592(17) -0.0128(12) -0.0182(13) -0.0030(12) O1C 0.142(3) 0.111(2) 0.0824(19) -0.0054(17) -0.0238(19) -0.071(2) C1C 0.102(3) 0.060(2) 0.081(3) 0.0031(18) -0.038(2) -0.014(2) C2C 0.067(2) 0.0506(18) 0.100(3) 0.0271(18) 0.014(2) -0.0087(16) C3C 0.071(2) 0.0493(17) 0.119(3) -0.0200(19) -0.056(2) 0.0074(15) C4C 0.070(2) 0.0518(16) 0.0537(17) -0.0017(13) -0.0152(15) -0.0082(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 2.0954(13) . ? In N2 2.1512(15) . ? In O1 2.1523(13) 2 ? In N1 2.1857(15) . ? In Cl 2.3653(5) . ? O1 In 2.1523(13) 2 ? N1 C1 1.318(2) . ? N1 C10 1.449(2) . ? N2 C3 1.330(2) . ? N2 C22 1.447(2) . ? C1 C2 1.403(3) . ? C2 C3 1.399(3) . ? C2 C4 1.492(2) . ? C4 C9 1.394(3) . ? C4 C5 1.401(3) . ? C5 C6 1.392(3) . ? C6 C7 1.379(3) . ? C7 C8 1.384(3) . ? C8 C9 1.390(3) . ? C10 C11 1.401(3) . ? C10 C15 1.407(3) . ? C11 C12 1.401(3) . ? C11 C16 1.515(3) . ? C12 C13 1.382(4) . ? C13 C14 1.362(4) . ? C14 C15 1.403(3) . ? C15 C19 1.515(3) . ? C16 C17 1.523(3) . ? C16 C18 1.535(4) . ? C19 C21 1.516(3) . ? C19 C20 1.517(4) . ? C22 C23 1.403(3) . ? C22 C27 1.404(3) . ? C23 C24 1.393(3) . ? C23 C28 1.522(3) . ? C24 C25 1.376(4) . ? C25 C26 1.382(4) . ? C26 C27 1.396(3) . ? C27 C31 1.520(3) . ? C28 C29 1.523(3) . ? C28 C30 1.526(4) . ? C31 C33 1.528(3) . ? C31 C32 1.534(3) . ? In1B O1B 2.1188(14) 2_666 ? In1B O1B 2.1234(14) . ? In1B N1B 2.1669(14) . ? In1B N2B 2.1710(14) . ? In1B Cl1B 2.3689(5) . ? O1B In1B 2.1188(14) 2_666 ? N1B C1B 1.317(2) . ? N1B C10B 1.449(2) . ? N2B C3B 1.324(2) . ? N2B C22B 1.452(2) . ? C1B C2B 1.406(2) . ? C2B C3B 1.400(2) . ? C2B C4B 1.490(2) . ? C4B C5B 1.388(3) . ? C4B C9B 1.397(3) . ? C5B C6B 1.397(3) . ? C6B C7B 1.376(4) . ? C7B C8B 1.376(3) . ? C8B C9B 1.388(3) . ? C10B C15B 1.399(3) . ? C10B C11B 1.400(3) . ? C11B C12B 1.398(3) . ? C11B C16B 1.510(3) . ? C12B C13B 1.370(4) . ? C13B C14B 1.383(4) . ? C14B C15B 1.394(3) . ? C15B C19B 1.522(3) . ? C16B C17B 1.528(4) . ? C16B C18B 1.532(4) . ? C19B C21B 1.523(3) . ? C19B C20B 1.531(3) . ? C22B C27B 1.396(3) . ? C22B C23B 1.410(3) . ? C23B C24B 1.399(3) . ? C23B C28B 1.514(3) . ? C24B C25B 1.380(3) . ? C25B C26B 1.378(3) . ? C26B C27B 1.401(3) . ? C27B C31B 1.525(3) . ? C28B C29B 1.526(3) . ? C28B C30B 1.533(3) . ? C31B C33B 1.522(3) . ? C31B C32B 1.533(3) . ? O1C C1C 1.355(5) . ? O1C C4C 1.383(4) . ? C1C C2C 1.516(5) . ? C2C C3C 1.545(5) . ? C3C C4C 1.505(5) . ? 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 N2 140.69(6) . . ? O1 In O1 72.61(6) . 2 ? N2 In O1 90.25(5) . 2 ? O1 In N1 93.68(5) . . ? N2 In N1 86.34(6) . . ? O1 In N1 153.35(6) 2 . ? O1 In Cl 107.46(4) . . ? N2 In Cl 110.19(4) . . ? O1 In Cl 99.55(4) 2 . ? N1 In Cl 106.43(4) . . ? In O1 In 107.39(6) . 2 ? C1 N1 C10 116.37(15) . . ? C1 N1 In 123.45(12) . . ? C10 N1 In 120.16(11) . . ? C3 N2 C22 115.15(15) . . ? C3 N2 In 123.44(12) . . ? C22 N2 In 121.22(11) . . ? N1 C1 C2 128.12(17) . . ? C3 C2 C1 124.11(16) . . ? C3 C2 C4 117.80(16) . . ? C1 C2 C4 117.54(16) . . ? N2 C3 C2 128.33(17) . . ? C9 C4 C5 118.14(17) . . ? C9 C4 C2 121.58(17) . . ? C5 C4 C2 120.28(18) . . ? C6 C5 C4 120.6(2) . . ? C7 C6 C5 120.4(2) . . ? C6 C7 C8 119.74(19) . . ? C7 C8 C9 120.1(2) . . ? C8 C9 C4 121.0(2) . . ? C11 C10 C15 122.58(18) . . ? C11 C10 N1 119.25(18) . . ? C15 C10 N1 118.16(18) . . ? C12 C11 C10 117.1(2) . . ? C12 C11 C16 120.1(2) . . ? C10 C11 C16 122.63(19) . . ? C13 C12 C11 121.1(3) . . ? C14 C13 C12 120.7(2) . . ? C13 C14 C15 121.4(2) . . ? C14 C15 C10 117.1(2) . . ? C14 C15 C19 120.7(2) . . ? C10 C15 C19 122.21(19) . . ? C11 C16 C17 113.3(2) . . ? C11 C16 C18 110.25(19) . . ? C17 C16 C18 109.4(2) . . ? C15 C19 C21 113.7(2) . . ? C15 C19 C20 110.5(2) . . ? C21 C19 C20 109.4(2) . . ? C23 C22 C27 122.44(18) . . ? C23 C22 N2 119.38(17) . . ? C27 C22 N2 118.18(16) . . ? C24 C23 C22 117.2(2) . . ? C24 C23 C28 120.9(2) . . ? C22 C23 C28 121.88(18) . . ? C25 C24 C23 121.6(2) . . ? C24 C25 C26 120.4(2) . . ? C25 C26 C27 120.8(2) . . ? C26 C27 C22 117.6(2) . . ? C26 C27 C31 121.4(2) . . ? C22 C27 C31 121.04(18) . . ? C23 C28 C29 113.4(2) . . ? C23 C28 C30 111.35(19) . . ? C29 C28 C30 109.6(2) . . ? C27 C31 C33 113.6(2) . . ? C27 C31 C32 111.51(18) . . ? C33 C31 C32 109.10(19) . . ? O1B In1B O1B 72.28(6) 2_666 . ? O1B In1B N1B 149.70(6) 2_666 . ? O1B In1B N1B 91.85(5) . . ? O1B In1B N2B 92.29(5) 2_666 . ? O1B In1B N2B 144.00(6) . . ? N1B In1B N2B 85.75(5) . . ? O1B In1B Cl1B 104.80(5) 2_666 . ? O1B In1B Cl1B 105.41(5) . . ? N1B In1B Cl1B 104.26(4) . . ? N2B In1B Cl1B 109.99(4) . . ? In1B O1B In1B 107.72(6) 2_666 . ? C1B N1B C10B 116.05(14) . . ? C1B N1B In1B 122.66(12) . . ? C10B N1B In1B 121.24(11) . . ? C3B N2B C22B 115.06(14) . . ? C3B N2B In1B 122.42(12) . . ? C22B N2B In1B 122.47(11) . . ? N1B C1B C2B 127.90(16) . . ? C3B C2B C1B 123.55(16) . . ? C3B C2B C4B 118.74(16) . . ? C1B C2B C4B 117.14(15) . . ? N2B C3B C2B 128.23(16) . . ? C5B C4B C9B 117.52(18) . . ? C5B C4B C2B 120.21(18) . . ? C9B C4B C2B 122.27(17) . . ? C4B C5B C6B 121.0(2) . . ? C7B C6B C5B 120.6(2) . . ? C6B C7B C8B 119.1(2) . . ? C7B C8B C9B 120.6(2) . . ? C8B C9B C4B 121.1(2) . . ? C15B C10B C11B 122.31(17) . . ? C15B C10B N1B 117.76(16) . . ? C11B C10B N1B 119.92(17) . . ? C12B C11B C10B 117.1(2) . . ? C12B C11B C16B 120.1(2) . . ? C10B C11B C16B 122.78(18) . . ? C13B C12B C11B 121.7(2) . . ? C12B C13B C14B 120.2(2) . . ? C13B C14B C15B 120.8(2) . . ? C14B C15B C10B 117.9(2) . . ? C14B C15B C19B 120.7(2) . . ? C10B C15B C19B 121.37(17) . . ? C11B C16B C17B 110.6(3) . . ? C11B C16B C18B 110.9(2) . . ? C17B C16B C18B 111.3(3) . . ? C15B C19B C21B 113.39(19) . . ? C15B C19B C20B 111.32(19) . . ? C21B C19B C20B 110.8(2) . . ? C27B C22B C23B 122.57(17) . . ? C27B C22B N2B 118.82(16) . . ? C23B C22B N2B 118.61(17) . . ? C24B C23B C22B 116.89(19) . . ? C24B C23B C28B 121.69(18) . . ? C22B C23B C28B 121.39(16) . . ? C25B C24B C23B 121.5(2) . . ? C26B C25B C24B 120.32(19) . . ? C25B C26B C27B 120.9(2) . . ? C22B C27B C26B 117.74(19) . . ? C22B C27B C31B 122.91(17) . . ? C26B C27B C31B 119.35(19) . . ? C23B C28B C29B 114.22(18) . . ? C23B C28B C30B 111.92(19) . . ? C29B C28B C30B 108.5(2) . . ? C33B C31B C27B 112.15(19) . . ? C33B C31B C32B 110.9(2) . . ? C27B C31B C32B 111.09(19) . . ? C1C O1C C4C 107.7(3) . . ? O1C C1C C2C 109.5(3) . . ? C1C C2C C3C 101.9(3) . . ? C4C C3C C2C 98.4(3) . . ? O1C C4C C3C 106.6(3) . . ? #===END data_(11a)-mar3504 _database_code_depnum_ccdc_archive 'CCDC 609666' _audit_creation_date 2004-03-31T10:03:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H82 Cl2 In2 N4, C4 H8 O1' _chemical_formula_sum 'C70 H90 Cl2 In2 N4 O' _chemical_formula_weight 1304 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9262(3) _cell_length_b 14.4149(2) _cell_length_c 17.9008(4) _cell_angle_alpha 83.762(1) _cell_angle_beta 72.690(1) _cell_angle_gamma 72.979(1) _cell_volume 3279.55(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31620 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7929 _exptl_absorpt_correction_T_max 0.8455 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.693174E-1 _diffrn_orient_matrix_ub_12 0.98907E-2 _diffrn_orient_matrix_ub_13 -0.304665E-1 _diffrn_orient_matrix_ub_21 0.225582E-1 _diffrn_orient_matrix_ub_22 -0.99371E-2 _diffrn_orient_matrix_ub_23 0.490319E-1 _diffrn_orient_matrix_ub_31 0.283516E-1 _diffrn_orient_matrix_ub_32 -0.712034E-1 _diffrn_orient_matrix_ub_33 -0.96654E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_unetI/netI 0.035 _diffrn_reflns_number 45757 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 11549 _reflns_number_gt 9867 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0291P)^2^+3.9707P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 11549 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.084 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.527964(14) 0.036939(13) 0.055789(11) 0.02091(6) Uani 1 1 d . . . Cl Cl 0.38297(6) 0.11702(6) 0.16025(5) 0.03856(19) Uani 1 1 d . . . N1 N 0.62685(18) 0.13422(15) 0.02796(13) 0.0226(5) Uani 1 1 d . . . N2 N 0.62797(17) -0.04871(15) 0.12451(13) 0.0219(5) Uani 1 1 d . . . C1 C 0.6820(2) 0.14075(19) 0.07483(16) 0.0241(6) Uani 1 1 d . . . H1 H 0.7142 0.1922 0.0627 0.029 Uiso 1 1 calc R . . C2 C 0.6994(2) 0.08266(19) 0.13958(16) 0.0243(6) Uani 1 1 d . . . C3 C 0.6798(2) -0.00853(19) 0.15630(16) 0.0235(6) Uani 1 1 d . . . H3 H 0.7076 -0.0464 0.1958 0.028 Uiso 1 1 calc R . . C4 C 0.7565(2) 0.1113(2) 0.18792(17) 0.0282(6) Uani 1 1 d . . . C5 C 0.8420(2) 0.1484(2) 0.15425(19) 0.0353(7) Uani 1 1 d . . . H5 H 0.8646 0.1566 0.099 0.042 Uiso 1 1 calc R . . C6 C 0.8947(3) 0.1735(2) 0.2004(2) 0.0425(8) Uani 1 1 d . . . H6 H 0.9522 0.1995 0.1765 0.051 Uiso 1 1 calc R . . C7 C 0.8646(3) 0.1610(2) 0.2802(2) 0.0493(10) Uani 1 1 d . . . H7 H 0.9018 0.1766 0.3115 0.059 Uiso 1 1 calc R . . C8 C 0.7792(4) 0.1253(3) 0.3144(2) 0.0600(11) Uani 1 1 d . . . H8 H 0.7572 0.1172 0.3697 0.072 Uiso 1 1 calc R . . C9 C 0.7252(3) 0.1013(3) 0.26891(19) 0.0476(9) Uani 1 1 d . . . H9 H 0.6661 0.0777 0.2935 0.057 Uiso 1 1 calc R . . C10 C 0.6377(2) 0.1975(2) -0.04100(17) 0.0266(6) Uani 1 1 d . . . C11 C 0.5625(2) 0.2882(2) -0.0383(2) 0.0359(7) Uani 1 1 d . . . C12 C 0.5761(3) 0.3483(3) -0.1045(2) 0.0477(9) Uani 1 1 d . . . H12 H 0.5265 0.4096 -0.1051 0.057 Uiso 1 1 calc R . . C13 C 0.6606(3) 0.3203(3) -0.1697(2) 0.0505(10) Uani 1 1 d . . . H13 H 0.6683 0.3628 -0.2142 0.061 Uiso 1 1 calc R . . C14 C 0.7338(3) 0.2315(2) -0.17090(19) 0.0432(8) Uani 1 1 d . . . H14 H 0.7918 0.2137 -0.2159 0.052 Uiso 1 1 calc R . . C15 C 0.7230(2) 0.1672(2) -0.10584(18) 0.0318(7) Uani 1 1 d . . . C16 C 0.4732(3) 0.3214(2) 0.0354(2) 0.0467(9) Uani 1 1 d . . . H16 H 0.4467 0.264 0.0578 0.056 Uiso 1 1 calc R . . C17 C 0.5072(3) 0.3562(3) 0.0990(3) 0.0628(11) Uani 1 1 d . . . H17A H 0.5671 0.3064 0.1095 0.094 Uiso 1 1 calc R . . H17B H 0.4491 0.3681 0.1471 0.094 Uiso 1 1 calc R . . H17C H 0.5271 0.4164 0.0812 0.094 Uiso 1 1 calc R . . C18 C 0.3807(3) 0.4022(3) 0.0241(3) 0.0648(11) Uani 1 1 d . . . H18A H 0.328 0.4175 0.0747 0.097 Uiso 1 1 calc R . . H18B H 0.3503 0.3815 -0.0119 0.097 Uiso 1 1 calc R . . H18C H 0.4037 0.4599 0.0023 0.097 Uiso 1 1 calc R . . C19 C 0.8067(3) 0.0708(2) -0.10713(19) 0.0379(8) Uani 1 1 d . . . H19 H 0.7775 0.0296 -0.0625 0.046 Uiso 1 1 calc R . . C20 C 0.8348(3) 0.0153(3) -0.1818(2) 0.0539(10) Uani 1 1 d . . . H20A H 0.8883 -0.0458 -0.1793 0.081 Uiso 1 1 calc R . . H20B H 0.862 0.0545 -0.2269 0.081 Uiso 1 1 calc R . . H20C H 0.7723 0.0016 -0.187 0.081 Uiso 1 1 calc R . . C21 C 0.9048(3) 0.0853(3) -0.0940(2) 0.0531(10) Uani 1 1 d . . . H21A H 0.9568 0.0223 -0.0948 0.08 Uiso 1 1 calc R . . H21B H 0.8867 0.1151 -0.0432 0.08 Uiso 1 1 calc R . . H21C H 0.9338 0.1278 -0.1357 0.08 Uiso 1 1 calc R . . C22 C 0.6397(2) -0.15100(19) 0.14160(16) 0.0247(6) Uani 1 1 d . . . C23 C 0.5783(2) -0.1817(2) 0.21146(18) 0.0336(7) Uani 1 1 d . . . C24 C 0.5934(3) -0.2811(2) 0.2251(2) 0.0444(9) Uani 1 1 d . . . H24 H 0.5511 -0.3038 0.2713 0.053 Uiso 1 1 calc R . . C25 C 0.6682(3) -0.3472(2) 0.1732(2) 0.0498(10) Uani 1 1 d . . . H25 H 0.6781 -0.4148 0.1843 0.06 Uiso 1 1 calc R . . C26 C 0.7286(3) -0.3153(2) 0.1052(2) 0.0446(9) Uani 1 1 d . . . H26 H 0.7802 -0.3615 0.0698 0.053 Uiso 1 1 calc R . . C27 C 0.7159(2) -0.2169(2) 0.08735(17) 0.0303(7) Uani 1 1 d . . . C28 C 0.4992(3) -0.1103(3) 0.2723(2) 0.0459(9) Uani 1 1 d . . . H28 H 0.4992 -0.0431 0.2515 0.055 Uiso 1 1 calc R . . C29 C 0.5304(4) -0.1242(3) 0.3493(2) 0.0756(14) Uani 1 1 d . . . H29A H 0.4789 -0.0774 0.3875 0.113 Uiso 1 1 calc R . . H29B H 0.5995 -0.1136 0.3394 0.113 Uiso 1 1 calc R . . H29C H 0.5325 -0.1903 0.3701 0.113 Uiso 1 1 calc R . . C30 C 0.3904(3) -0.1210(4) 0.2861(3) 0.0817(15) Uani 1 1 d . . . H30A H 0.3406 -0.0744 0.3251 0.122 Uiso 1 1 calc R . . H30B H 0.3892 -0.187 0.3052 0.122 Uiso 1 1 calc R . . H30C H 0.371 -0.1084 0.2369 0.122 Uiso 1 1 calc R . . C31 C 0.7854(3) -0.1823(2) 0.01338(18) 0.0370(8) Uani 1 1 d . . . H31 H 0.7443 -0.1173 -0.0016 0.044 Uiso 1 1 calc R . . C32 C 0.8165(3) -0.2483(3) -0.0560(2) 0.0468(9) Uani 1 1 d . . . H32A H 0.8608 -0.2221 -0.1016 0.07 Uiso 1 1 calc R . . H32B H 0.7534 -0.2516 -0.0681 0.07 Uiso 1 1 calc R . . H32C H 0.8551 -0.3135 -0.0428 0.07 Uiso 1 1 calc R . . C33 C 0.8827(3) -0.1679(3) 0.0285(2) 0.0542(10) Uani 1 1 d . . . H33A H 0.9259 -0.1456 -0.0199 0.081 Uiso 1 1 calc R . . H33B H 0.9231 -0.2296 0.0463 0.081 Uiso 1 1 calc R . . H33C H 0.8613 -0.1194 0.0689 0.081 Uiso 1 1 calc R . . In1B In 0.097658(15) 0.502111(13) 0.501068(11) 0.02200(6) Uani 1 1 d . . 1 Cl1B Cl 0.19949(6) 0.53743(6) 0.37329(4) 0.03557(18) Uani 1 1 d . A 1 N1B N 0.21303(18) 0.39248(16) 0.54580(14) 0.0261(5) Uani 1 1 d . B 1 N2B N 0.11179(17) 0.60563(16) 0.57268(13) 0.0235(5) Uani 1 1 d . B 1 C1B C 0.2769(2) 0.4159(2) 0.57750(16) 0.0260(6) Uani 1 1 d . B 1 H1B H 0.3306 0.363 0.5886 0.031 Uiso 1 1 calc R B 1 C2B C 0.2769(2) 0.5074(2) 0.59710(16) 0.0258(6) Uani 1 1 d . B 1 C3B C 0.1947(2) 0.5913(2) 0.59845(16) 0.0259(6) Uani 1 1 d . B 1 H3B H 0.1991 0.6459 0.6212 0.031 Uiso 1 1 calc R B 1 C4B C 0.3626(2) 0.5120(2) 0.62971(16) 0.0276(6) Uani 1 1 d . B 1 C5B C 0.3431(2) 0.5690(2) 0.69352(17) 0.0342(7) Uani 1 1 d . B 1 H5B H 0.2737 0.6063 0.717 0.041 Uiso 1 1 calc R B 1 C6B C 0.4231(3) 0.5722(3) 0.72310(19) 0.0396(8) Uani 1 1 d . B 1 H6B H 0.4084 0.6118 0.7665 0.048 Uiso 1 1 calc R B 1 C7B C 0.5248(3) 0.5181(3) 0.6898(2) 0.0419(8) Uani 1 1 d . B 1 H7B H 0.5797 0.5203 0.7102 0.05 Uiso 1 1 calc R B 1 C8B C 0.5451(3) 0.4613(2) 0.6273(2) 0.0404(8) Uani 1 1 d . B 1 H8B H 0.6146 0.4235 0.6047 0.048 Uiso 1 1 calc R B 1 C9B C 0.4656(2) 0.4582(2) 0.59669(18) 0.0331(7) Uani 1 1 d . B 1 H9B H 0.4814 0.4192 0.5528 0.04 Uiso 1 1 calc R B 1 C10B C 0.2219(2) 0.2897(2) 0.54597(18) 0.0304(7) Uani 1 1 d . B 1 C11B C 0.2936(3) 0.2335(2) 0.4836(2) 0.0419(8) Uani 1 1 d . B 1 C12B C 0.2984(4) 0.1353(3) 0.4869(2) 0.0591(11) Uani 1 1 d . B 1 H12B H 0.3459 0.0949 0.4455 0.071 Uiso 1 1 calc R B 1 C13B C 0.2364(3) 0.0957(3) 0.5481(3) 0.0617(11) Uani 1 1 d . B 1 H13B H 0.24 0.0289 0.5477 0.074 Uiso 1 1 calc R B 1 C14B C 0.1688(3) 0.1509(2) 0.6104(3) 0.0529(10) Uani 1 1 d . B 1 H14B H 0.128 0.1214 0.6532 0.063 Uiso 1 1 calc R B 1 C15B C 0.1596(3) 0.2499(2) 0.6114(2) 0.0385(8) Uani 1 1 d . B 1 C16B C 0.3708(3) 0.2737(3) 0.4187(2) 0.0494(9) Uani 1 1 d . B 1 H16B H 0.3426 0.3459 0.4167 0.059 Uiso 1 1 calc R B 1 C17B C 0.4782(3) 0.2493(3) 0.4360(2) 0.0562(10) Uani 1 1 d . B 1 H17D H 0.5266 0.276 0.3938 0.084 Uiso 1 1 calc R B 1 H17E H 0.5065 0.1787 0.4394 0.084 Uiso 1 1 calc R B 1 H17F H 0.4694 0.2777 0.4857 0.084 Uiso 1 1 calc R B 1 C18B C 0.3879(4) 0.2357(3) 0.3386(2) 0.0719(13) Uani 1 1 d . B 1 H18D H 0.4379 0.2643 0.2994 0.108 Uiso 1 1 calc R B 1 H18E H 0.3213 0.2534 0.3255 0.108 Uiso 1 1 calc R B 1 H18F H 0.4157 0.1649 0.3393 0.108 Uiso 1 1 calc R B 1 C19B C 0.0911(3) 0.3100(3) 0.6831(2) 0.0489(9) Uani 1 1 d . B 1 H19B H 0.0779 0.3799 0.6663 0.059 Uiso 1 1 calc R B 1 C20B C -0.0134(3) 0.2897(4) 0.7183(3) 0.0699(12) Uani 1 1 d . B 1 H20D H -0.051 0.3003 0.6784 0.105 Uiso 1 1 calc R B 1 H20E H -0.0543 0.3334 0.7618 0.105 Uiso 1 1 calc R B 1 H20F H -0.0029 0.2223 0.7376 0.105 Uiso 1 1 calc R B 1 C21B C 0.1478(4) 0.2948(5) 0.7457(3) 0.104(2) Uani 1 1 d . B 1 H21D H 0.2158 0.3082 0.7233 0.156 Uiso 1 1 calc R B 1 H21E H 0.1582 0.2275 0.7655 0.156 Uiso 1 1 calc R B 1 H21F H 0.1059 0.3389 0.7888 0.156 Uiso 1 1 calc R B 1 C22B C 0.0329(2) 0.6971(2) 0.59372(16) 0.0263(6) Uani 1 1 d . B 1 C23B C 0.0430(3) 0.7791(2) 0.54590(18) 0.0353(7) Uani 1 1 d . B 1 C24B C -0.0336(3) 0.8663(2) 0.5703(2) 0.0501(10) Uani 1 1 d . B 1 H24B H -0.0301 0.9238 0.5394 0.06 Uiso 1 1 calc R B 1 C25B C -0.1137(3) 0.8704(3) 0.6383(2) 0.0513(10) Uani 1 1 d . B 1 H25B H -0.1639 0.9307 0.6538 0.062 Uiso 1 1 calc R B 1 C26B C -0.1219(3) 0.7886(3) 0.6836(2) 0.0445(9) Uani 1 1 d . B 1 H26B H -0.178 0.793 0.7301 0.053 Uiso 1 1 calc R B 1 C27B C -0.0489(2) 0.6988(2) 0.66262(18) 0.0331(7) Uani 1 1 d . B 1 C28B C 0.1348(3) 0.7762(2) 0.47304(19) 0.0424(8) Uani 1 1 d . B 1 H28B H 0.1626 0.708 0.4545 0.051 Uiso 1 1 calc R B 1 C29B C 0.1047(4) 0.8410(3) 0.4060(2) 0.0654(12) Uani 1 1 d . B 1 H29D H 0.1667 0.8356 0.361 0.098 Uiso 1 1 calc R B 1 H29E H 0.076 0.9085 0.4226 0.098 Uiso 1 1 calc R B 1 H29F H 0.0519 0.8205 0.391 0.098 Uiso 1 1 calc R B 1 C30B C 0.2239(4) 0.8038(4) 0.4906(2) 0.0685(12) Uani 1 1 d . B 1 H30D H 0.2814 0.8005 0.4425 0.103 Uiso 1 1 calc R B 1 H30E H 0.2488 0.7586 0.5301 0.103 Uiso 1 1 calc R B 1 H30F H 0.1984 0.87 0.5103 0.103 Uiso 1 1 calc R B 1 C31B C -0.0556(3) 0.6083(2) 0.71399(18) 0.0394(8) Uani 1 1 d . B 1 H31B H -0.0274 0.5517 0.6786 0.047 Uiso 1 1 calc R B 1 C32B C -0.1663(3) 0.6079(3) 0.7608(2) 0.0541(10) Uani 1 1 d . B 1 H32D H -0.1645 0.5476 0.7921 0.081 Uiso 1 1 calc R B 1 H32E H -0.2088 0.6126 0.7249 0.081 Uiso 1 1 calc R B 1 H32F H -0.197 0.6634 0.7956 0.081 Uiso 1 1 calc R B 1 C33B C 0.0131(3) 0.5917(3) 0.7700(2) 0.0502(9) Uani 1 1 d . B 1 H33D H 0.0075 0.5328 0.802 0.075 Uiso 1 1 calc R B 1 H33E H -0.0105 0.6475 0.8042 0.075 Uiso 1 1 calc R B 1 H33F H 0.0861 0.5843 0.7396 0.075 Uiso 1 1 calc R B 1 O1A O 0.7872(3) 0.3333(3) 0.0201(2) 0.0981(12) Uani 1 1 d . C 2 C1A C 0.8389(4) 0.3650(3) -0.0492(3) 0.0709(13) Uani 1 1 d . C 2 H1A1 H 0.7886 0.4004 -0.0785 0.085 Uiso 1 1 calc R C 2 H1A2 H 0.8879 0.3088 -0.0804 0.085 Uiso 1 1 calc R C 2 C2A C 0.8989(4) 0.4311(3) -0.0372(3) 0.0761(15) Uani 1 1 d . C 2 H2A1 H 0.8678 0.4992 -0.0515 0.091 Uiso 1 1 calc R C 2 H2A2 H 0.9732 0.4104 -0.068 0.091 Uiso 1 1 calc R C 2 C3A C 0.8868(4) 0.4181(3) 0.0521(3) 0.0787(16) Uani 1 1 d . C 2 H3A1 H 0.9441 0.3648 0.0641 0.094 Uiso 1 1 calc R C 2 H3A2 H 0.8823 0.4787 0.0758 0.094 Uiso 1 1 calc R C 2 C4A C 0.7839(3) 0.3929(3) 0.0770(2) 0.0565(10) Uani 1 1 d . C 2 H4A1 H 0.7748 0.3587 0.1286 0.068 Uiso 1 1 calc R C 2 H4A2 H 0.725 0.4524 0.0809 0.068 Uiso 1 1 calc R C 2 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 0.02063(11) 0.02025(11) 0.02240(11) -0.00025(8) -0.00637(8) -0.00618(8) Cl 0.0297(4) 0.0400(4) 0.0345(4) -0.0064(3) 0.0022(3) -0.0018(3) N1 0.0250(13) 0.0183(11) 0.0253(12) 0.0013(9) -0.0085(10) -0.0061(9) N2 0.0251(13) 0.0195(12) 0.0216(12) 0.0011(9) -0.0067(10) -0.0074(10) C1 0.0224(15) 0.0190(14) 0.0291(16) -0.0023(11) -0.0039(12) -0.0056(11) C2 0.0236(15) 0.0247(15) 0.0246(15) -0.0031(11) -0.0063(12) -0.0062(12) C3 0.0230(15) 0.0254(15) 0.0196(14) -0.0005(11) -0.0049(12) -0.0040(12) C4 0.0340(17) 0.0223(15) 0.0314(17) -0.0030(12) -0.0141(14) -0.0065(12) C5 0.0349(18) 0.0387(18) 0.0361(18) -0.0028(14) -0.0130(15) -0.0119(14) C6 0.0361(19) 0.045(2) 0.055(2) -0.0073(16) -0.0215(17) -0.0121(15) C7 0.067(3) 0.041(2) 0.059(2) -0.0046(17) -0.041(2) -0.0175(18) C8 0.102(3) 0.067(3) 0.033(2) 0.0056(18) -0.031(2) -0.045(3) C9 0.070(3) 0.057(2) 0.0322(19) 0.0029(16) -0.0176(18) -0.039(2) C10 0.0306(16) 0.0258(15) 0.0300(16) 0.0075(12) -0.0147(13) -0.0144(12) C11 0.0337(18) 0.0280(17) 0.051(2) 0.0116(14) -0.0199(16) -0.0124(14) C12 0.047(2) 0.0341(19) 0.065(3) 0.0173(17) -0.026(2) -0.0116(16) C13 0.070(3) 0.041(2) 0.049(2) 0.0232(17) -0.030(2) -0.0239(19) C14 0.057(2) 0.044(2) 0.0303(18) 0.0083(14) -0.0104(16) -0.0228(17) C15 0.0406(19) 0.0274(16) 0.0323(17) 0.0056(12) -0.0142(14) -0.0151(14) C16 0.0317(19) 0.0283(18) 0.070(3) 0.0124(16) -0.0089(17) -0.0035(14) C17 0.056(3) 0.051(2) 0.074(3) -0.020(2) -0.012(2) -0.0027(19) C18 0.055(3) 0.056(3) 0.076(3) 0.001(2) -0.019(2) -0.005(2) C19 0.042(2) 0.0326(17) 0.0326(18) 0.0013(13) -0.0003(15) -0.0106(14) C20 0.051(2) 0.052(2) 0.055(2) -0.0161(18) -0.0080(19) -0.0095(18) C21 0.051(2) 0.050(2) 0.056(2) -0.0056(18) -0.0214(19) -0.0030(18) C22 0.0300(16) 0.0223(14) 0.0272(15) 0.0039(11) -0.0129(13) -0.0118(12) C23 0.0358(18) 0.0343(17) 0.0313(17) 0.0069(13) -0.0098(14) -0.0131(14) C24 0.059(2) 0.041(2) 0.040(2) 0.0178(16) -0.0160(18) -0.0289(18) C25 0.089(3) 0.0237(17) 0.046(2) 0.0086(15) -0.029(2) -0.0220(18) C26 0.073(3) 0.0225(17) 0.0362(19) -0.0026(14) -0.0179(18) -0.0067(16) C27 0.0387(18) 0.0222(15) 0.0303(16) -0.0010(12) -0.0137(14) -0.0049(13) C28 0.039(2) 0.050(2) 0.038(2) 0.0150(16) -0.0027(16) -0.0099(16) C29 0.082(3) 0.084(3) 0.039(2) -0.014(2) -0.013(2) 0.011(3) C30 0.045(3) 0.099(4) 0.088(4) 0.020(3) -0.007(2) -0.020(2) C31 0.0395(19) 0.0280(17) 0.0339(18) -0.0007(13) -0.0041(15) -0.0010(14) C32 0.046(2) 0.048(2) 0.037(2) -0.0089(16) -0.0073(16) -0.0022(17) C33 0.048(2) 0.051(2) 0.059(2) -0.0156(18) -0.0022(19) -0.0161(18) In1B 0.01995(11) 0.02337(11) 0.02344(11) -0.00384(8) -0.00597(8) -0.00600(8) Cl1B 0.0326(4) 0.0496(5) 0.0253(4) -0.0021(3) -0.0028(3) -0.0173(3) N1B 0.0255(13) 0.0219(12) 0.0310(13) -0.0011(10) -0.0082(11) -0.0064(10) N2B 0.0225(13) 0.0239(12) 0.0233(12) -0.0045(9) -0.0059(10) -0.0045(10) C1B 0.0210(15) 0.0288(16) 0.0259(15) 0.0031(12) -0.0052(12) -0.0063(12) C2B 0.0230(15) 0.0329(16) 0.0248(15) 0.0002(12) -0.0083(12) -0.0113(12) C3B 0.0318(17) 0.0280(15) 0.0196(14) -0.0014(11) -0.0071(12) -0.0105(13) C4B 0.0270(16) 0.0333(16) 0.0251(15) 0.0061(12) -0.0077(13) -0.0142(13) C5B 0.0300(17) 0.0478(19) 0.0285(17) 0.0003(14) -0.0100(14) -0.0149(14) C6B 0.042(2) 0.054(2) 0.0322(18) 0.0022(15) -0.0152(15) -0.0229(17) C7B 0.036(2) 0.059(2) 0.043(2) 0.0091(17) -0.0219(16) -0.0233(17) C8B 0.0282(18) 0.046(2) 0.049(2) 0.0066(16) -0.0140(15) -0.0127(15) C9B 0.0306(17) 0.0358(17) 0.0338(17) 0.0040(13) -0.0092(14) -0.0123(14) C10B 0.0302(17) 0.0228(15) 0.0416(18) 0.0013(13) -0.0167(14) -0.0063(12) C11B 0.052(2) 0.0303(18) 0.043(2) -0.0034(14) -0.0174(17) -0.0059(15) C12B 0.083(3) 0.031(2) 0.059(3) -0.0086(17) -0.017(2) -0.0074(19) C13B 0.076(3) 0.0257(19) 0.087(3) 0.0004(19) -0.026(3) -0.0170(19) C14B 0.051(2) 0.033(2) 0.076(3) 0.0124(18) -0.018(2) -0.0197(17) C15B 0.0342(18) 0.0338(18) 0.050(2) 0.0041(15) -0.0153(16) -0.0121(14) C16B 0.062(3) 0.0366(19) 0.037(2) -0.0030(15) -0.0049(18) -0.0035(17) C17B 0.054(2) 0.066(3) 0.046(2) -0.0033(19) -0.0093(19) -0.018(2) C18B 0.081(3) 0.081(3) 0.047(2) -0.012(2) -0.018(2) -0.010(3) C19B 0.042(2) 0.040(2) 0.053(2) 0.0085(16) 0.0021(17) -0.0139(16) C20B 0.045(2) 0.092(3) 0.064(3) 0.006(2) -0.006(2) -0.017(2) C21B 0.055(3) 0.195(6) 0.060(3) -0.046(4) -0.010(2) -0.022(4) C22B 0.0291(16) 0.0242(15) 0.0279(16) -0.0088(12) -0.0120(13) -0.0038(12) C23B 0.050(2) 0.0259(16) 0.0328(17) -0.0066(13) -0.0186(15) -0.0058(14) C24B 0.073(3) 0.0285(18) 0.047(2) -0.0043(15) -0.023(2) -0.0019(17) C25B 0.051(2) 0.037(2) 0.058(2) -0.0188(18) -0.018(2) 0.0084(17) C26B 0.0347(19) 0.047(2) 0.047(2) -0.0226(17) -0.0051(16) -0.0024(16) C27B 0.0329(17) 0.0339(17) 0.0331(17) -0.0141(13) -0.0081(14) -0.0065(13) C28B 0.069(2) 0.0294(17) 0.0308(18) -0.0015(13) -0.0117(17) -0.0179(16) C29B 0.099(4) 0.061(3) 0.045(2) 0.0085(19) -0.029(2) -0.030(2) C30B 0.080(3) 0.094(3) 0.045(2) 0.012(2) -0.015(2) -0.051(3) C31B 0.043(2) 0.0410(19) 0.0294(17) -0.0112(14) 0.0041(15) -0.0147(15) C32B 0.052(2) 0.066(3) 0.045(2) -0.0155(18) 0.0018(18) -0.027(2) C33B 0.051(2) 0.063(2) 0.0325(19) 0.0035(17) -0.0071(17) -0.0168(19) O1A 0.127(3) 0.099(3) 0.085(3) -0.013(2) -0.015(2) -0.067(2) C1A 0.089(4) 0.054(3) 0.077(3) 0.003(2) -0.035(3) -0.019(2) C2A 0.061(3) 0.045(2) 0.087(3) 0.019(2) 0.017(2) -0.008(2) C3A 0.063(3) 0.059(3) 0.126(4) -0.040(3) -0.063(3) 0.016(2) C4A 0.066(3) 0.047(2) 0.047(2) -0.0066(17) -0.005(2) -0.0093(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 2.159(2) . ? In N1 2.164(2) . ? In Cl 2.4009(7) . ? In In 2.7575(4) 2_655 ? N1 C1 1.321(4) . ? N1 C10 1.450(3) . ? N2 C3 1.320(3) . ? N2 C22 1.444(3) . ? C1 C2 1.393(4) . ? C2 C3 1.402(4) . ? C2 C4 1.494(4) . ? C4 C9 1.389(4) . ? C4 C5 1.394(4) . ? C5 C6 1.390(4) . ? C6 C7 1.371(5) . ? C7 C8 1.382(5) . ? C8 C9 1.388(5) . ? C10 C15 1.391(4) . ? C10 C11 1.410(4) . ? C11 C12 1.390(5) . ? C11 C16 1.526(5) . ? C12 C13 1.384(5) . ? C13 C14 1.382(5) . ? C14 C15 1.408(4) . ? C15 C19 1.527(4) . ? C16 C18 1.510(5) . ? C16 C17 1.535(6) . ? C19 C20 1.521(5) . ? C19 C21 1.527(5) . ? C22 C23 1.398(4) . ? C22 C27 1.403(4) . ? C23 C24 1.391(4) . ? C23 C28 1.525(5) . ? C24 C25 1.375(5) . ? C25 C26 1.378(5) . ? C26 C27 1.390(4) . ? C27 C31 1.522(4) . ? C28 C30 1.512(5) . ? C28 C29 1.541(5) . ? C31 C32 1.527(4) . ? C31 C33 1.532(5) . ? In1B N2B 2.156(2) . ? In1B N1B 2.174(2) . ? In1B Cl1B 2.3962(7) . ? In1B In1B 2.7501(4) 2_566 ? N1B C1B 1.320(4) . ? N1B C10B 1.449(4) . ? N2B C3B 1.321(4) . ? N2B C22B 1.449(3) . ? C1B C2B 1.401(4) . ? C2B C3B 1.398(4) . ? C2B C4B 1.495(4) . ? C4B C5B 1.394(4) . ? C4B C9B 1.398(4) . ? C5B C6B 1.383(4) . ? C6B C7B 1.386(5) . ? C7B C8B 1.370(5) . ? C8B C9B 1.387(4) . ? C10B C11B 1.400(5) . ? C10B C15B 1.413(4) . ? C11B C12B 1.393(5) . ? C11B C16B 1.523(5) . ? C12B C13B 1.364(6) . ? C13B C14B 1.376(6) . ? C14B C15B 1.395(5) . ? C15B C19B 1.528(5) . ? C16B C18B 1.516(5) . ? C16B C17B 1.550(5) . ? C19B C20B 1.504(5) . ? C19B C21B 1.516(6) . ? C22B C23B 1.398(4) . ? C22B C27B 1.405(4) . ? C23B C24B 1.402(5) . ? C23B C28B 1.525(5) . ? C24B C25B 1.377(5) . ? C25B C26B 1.370(5) . ? C26B C27B 1.400(4) . ? C27B C31B 1.522(4) . ? C28B C29B 1.522(5) . ? C28B C30B 1.531(5) . ? C31B C32B 1.521(5) . ? C31B C33B 1.538(5) . ? O1A C1A 1.343(6) . ? O1A C4A 1.383(5) . ? C1A C2A 1.506(6) . ? C2A C3A 1.553(7) . ? C3A C4A 1.508(6) . ? 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 N2 In N1 87.55(8) . . ? N2 In Cl 98.85(6) . . ? N1 In Cl 103.01(6) . . ? N2 In In 124.44(6) . 2_655 ? N1 In In 123.23(6) . 2_655 ? Cl In In 114.31(2) . 2_655 ? C1 N1 C10 114.6(2) . . ? C1 N1 In 121.11(18) . . ? C10 N1 In 124.24(17) . . ? C3 N2 C22 115.6(2) . . ? C3 N2 In 121.00(18) . . ? C22 N2 In 123.32(17) . . ? N1 C1 C2 129.0(3) . . ? C1 C2 C3 123.9(3) . . ? C1 C2 C4 118.5(2) . . ? C3 C2 C4 116.9(2) . . ? N2 C3 C2 128.6(3) . . ? C9 C4 C5 117.9(3) . . ? C9 C4 C2 120.2(3) . . ? C5 C4 C2 122.0(3) . . ? C6 C5 C4 120.9(3) . . ? C7 C6 C5 120.7(3) . . ? C6 C7 C8 119.0(3) . . ? C7 C8 C9 120.8(3) . . ? C8 C9 C4 120.8(3) . . ? C15 C10 C11 123.1(3) . . ? C15 C10 N1 118.6(2) . . ? C11 C10 N1 118.3(3) . . ? C12 C11 C10 117.1(3) . . ? C12 C11 C16 121.2(3) . . ? C10 C11 C16 121.7(3) . . ? C13 C12 C11 121.1(3) . . ? C14 C13 C12 120.9(3) . . ? C13 C14 C15 120.4(3) . . ? C10 C15 C14 117.4(3) . . ? C10 C15 C19 122.9(3) . . ? C14 C15 C19 119.6(3) . . ? C18 C16 C11 116.1(3) . . ? C18 C16 C17 105.4(3) . . ? C11 C16 C17 113.5(3) . . ? C20 C19 C21 110.3(3) . . ? C20 C19 C15 112.9(3) . . ? C21 C19 C15 111.3(3) . . ? C23 C22 C27 122.0(3) . . ? C23 C22 N2 120.1(3) . . ? C27 C22 N2 117.9(2) . . ? C24 C23 C22 117.6(3) . . ? C24 C23 C28 120.3(3) . . ? C22 C23 C28 122.1(3) . . ? C25 C24 C23 121.5(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C27 121.5(3) . . ? C26 C27 C22 117.5(3) . . ? C26 C27 C31 121.1(3) . . ? C22 C27 C31 121.3(3) . . ? C30 C28 C23 110.6(3) . . ? C30 C28 C29 111.0(3) . . ? C23 C28 C29 110.8(3) . . ? C27 C31 C32 113.4(3) . . ? C27 C31 C33 111.2(3) . . ? C32 C31 C33 110.5(3) . . ? N2B In1B N1B 87.98(8) . . ? N2B In1B Cl1B 102.72(6) . . ? N1B In1B Cl1B 102.11(7) . . ? N2B In1B In1B 119.52(6) . 2_566 ? N1B In1B In1B 128.74(6) . 2_566 ? Cl1B In1B In1B 111.21(2) . 2_566 ? C1B N1B C10B 115.7(2) . . ? C1B N1B In1B 121.80(18) . . ? C10B N1B In1B 122.42(18) . . ? C3B N2B C22B 115.3(2) . . ? C3B N2B In1B 122.16(18) . . ? C22B N2B In1B 122.48(17) . . ? N1B C1B C2B 129.4(3) . . ? C3B C2B C1B 123.8(3) . . ? C3B C2B C4B 118.1(3) . . ? C1B C2B C4B 117.4(3) . . ? N2B C3B C2B 129.4(3) . . ? C5B C4B C9B 117.8(3) . . ? C5B C4B C2B 121.8(3) . . ? C9B C4B C2B 120.4(3) . . ? C6B C5B C4B 121.0(3) . . ? C5B C6B C7B 120.4(3) . . ? C8B C7B C6B 119.3(3) . . ? C7B C8B C9B 120.8(3) . . ? C8B C9B C4B 120.7(3) . . ? C11B C10B C15B 122.6(3) . . ? C11B C10B N1B 119.5(3) . . ? C15B C10B N1B 117.9(3) . . ? C12B C11B C10B 116.9(3) . . ? C12B C11B C16B 120.3(3) . . ? C10B C11B C16B 122.5(3) . . ? C13B C12B C11B 121.6(4) . . ? C12B C13B C14B 121.1(3) . . ? C13B C14B C15B 120.7(4) . . ? C14B C15B C10B 117.0(3) . . ? C14B C15B C19B 121.0(3) . . ? C10B C15B C19B 121.8(3) . . ? C18B C16B C11B 113.3(3) . . ? C18B C16B C17B 108.3(3) . . ? C11B C16B C17B 110.6(3) . . ? C20B C19B C21B 108.9(4) . . ? C20B C19B C15B 114.1(3) . . ? C21B C19B C15B 110.6(3) . . ? C23B C22B C27B 123.4(3) . . ? C23B C22B N2B 118.8(3) . . ? C27B C22B N2B 117.8(2) . . ? C22B C23B C24B 116.5(3) . . ? C22B C23B C28B 122.4(3) . . ? C24B C23B C28B 121.0(3) . . ? C25B C24B C23B 121.4(3) . . ? C26B C25B C24B 120.8(3) . . ? C25B C26B C27B 121.1(3) . . ? C26B C27B C22B 116.9(3) . . ? C26B C27B C31B 121.3(3) . . ? C22B C27B C31B 121.7(3) . . ? C29B C28B C23B 113.5(3) . . ? C29B C28B C30B 108.5(3) . . ? C23B C28B C30B 112.0(3) . . ? C32B C31B C27B 114.2(3) . . ? C32B C31B C33B 109.2(3) . . ? C27B C31B C33B 111.4(3) . . ? C1A O1A C4A 107.6(3) . . ? O1A C1A C2A 110.3(4) . . ? C1A C2A C3A 101.8(3) . . ? C4A C3A C2A 98.4(3) . . ? O1A C4A C3A 106.3(3) . . ? #===END data_(12)-apr1704 _database_code_depnum_ccdc_archive 'CCDC 609667' _audit_creation_date 2004-04-16T11:35:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H82 Cl2 In2 N4 S1' _chemical_formula_sum 'C66 H82 Cl2 In2 N4 S1' _chemical_formula_weight 1263.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6868(2) _cell_length_b 12.9207(2) _cell_length_c 26.4950(4) _cell_angle_alpha 90 _cell_angle_beta 101.491(1) _cell_angle_gamma 90 _cell_volume 6268.90(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39713 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7016 _exptl_absorpt_correction_T_max 0.7739 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.138155E-1 _diffrn_orient_matrix_ub_12 0.727062E-1 _diffrn_orient_matrix_ub_13 -0.106706E-1 _diffrn_orient_matrix_ub_21 -0.26624E-2 _diffrn_orient_matrix_ub_22 0.175209E-1 _diffrn_orient_matrix_ub_23 0.36343E-1 _diffrn_orient_matrix_ub_31 0.527646E-1 _diffrn_orient_matrix_ub_32 0.199209E-1 _diffrn_orient_matrix_ub_33 0.69804E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_number 47347 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 11596 _reflns_number_gt 9635 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0220P)^2^+10.7049P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 11596 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.408 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 In1 In 0.244096(11) 0.557980(16) 0.306366(8) 0.01869(6) Uani 1 1 d . . . In2 In 0.220771(11) 0.793984(17) 0.376225(8) 0.02180(7) Uani 1 1 d . . . Cl1 Cl 0.11627(4) 0.56941(7) 0.28882(4) 0.0393(2) Uani 1 1 d . . . Cl2 Cl 0.18090(5) 0.87548(8) 0.29609(3) 0.0401(2) Uani 1 1 d . . . S S 0.30397(5) 0.65553(7) 0.37818(3) 0.0312(2) Uani 1 1 d . . . N1 N 0.27837(13) 0.39915(18) 0.31384(9) 0.0180(5) Uani 1 1 d . . . N2 N 0.28206(13) 0.56148(18) 0.23524(9) 0.0190(5) Uani 1 1 d . . . N3 N 0.12958(13) 0.79829(19) 0.41387(9) 0.0199(5) Uani 1 1 d . . . N4 N 0.27574(13) 0.90047(19) 0.43307(9) 0.0186(5) Uani 1 1 d . . . C1 C 0.28628(15) 0.3419(2) 0.27439(11) 0.0181(6) Uani 1 1 d . . . H1 H 0.2924 0.2698 0.2809 0.022 Uiso 1 1 calc R . . C2 C 0.28691(16) 0.3736(2) 0.22382(11) 0.0199(7) Uani 1 1 d . . . C3 C 0.29034(15) 0.4772(2) 0.20882(11) 0.0191(6) Uani 1 1 d . . . H3 H 0.2999 0.4882 0.1753 0.023 Uiso 1 1 calc R . . C4 C 0.29214(17) 0.2910(2) 0.18531(12) 0.0246(7) Uani 1 1 d . . . C5 C 0.2532(2) 0.1997(3) 0.18495(14) 0.0362(9) Uani 1 1 d . . . H5 H 0.2222 0.1904 0.209 0.043 Uiso 1 1 calc R . . C6 C 0.2588(3) 0.1212(3) 0.14982(17) 0.0528(12) Uani 1 1 d . . . H6 H 0.232 0.0589 0.1504 0.063 Uiso 1 1 calc R . . C7 C 0.3027(3) 0.1337(4) 0.11441(16) 0.0555(13) Uani 1 1 d . . . H7 H 0.3059 0.0805 0.0902 0.067 Uiso 1 1 calc R . . C8 C 0.3420(2) 0.2232(3) 0.11427(14) 0.0495(11) Uani 1 1 d . . . H8 H 0.3726 0.2317 0.0899 0.059 Uiso 1 1 calc R . . C9 C 0.33752(19) 0.3017(3) 0.14937(12) 0.0346(8) Uani 1 1 d . . . H9 H 0.3654 0.3631 0.149 0.041 Uiso 1 1 calc R . . C10 C 0.28826(16) 0.3518(2) 0.36436(11) 0.0195(6) Uani 1 1 d . . . C11 C 0.35268(17) 0.3730(2) 0.39999(12) 0.0226(7) Uani 1 1 d . . . C12 C 0.35967(19) 0.3314(3) 0.44949(12) 0.0317(8) Uani 1 1 d . . . H12 H 0.4026 0.3447 0.4746 0.038 Uiso 1 1 calc R . . C13 C 0.3049(2) 0.2713(3) 0.46228(13) 0.0351(9) Uani 1 1 d . . . H13 H 0.3103 0.2443 0.4962 0.042 Uiso 1 1 calc R . . C14 C 0.24263(19) 0.2502(3) 0.42657(13) 0.0308(8) Uani 1 1 d . . . H14 H 0.2059 0.2077 0.436 0.037 Uiso 1 1 calc R . . C15 C 0.23225(17) 0.2900(2) 0.37672(12) 0.0234(7) Uani 1 1 d . . . C16 C 0.41406(17) 0.4354(3) 0.38484(12) 0.0265(7) Uani 1 1 d . . . H16 H 0.3906 0.4893 0.3599 0.032 Uiso 1 1 calc R . . C17 C 0.46080(18) 0.3681(3) 0.35655(14) 0.0348(8) Uani 1 1 d . . . H17A H 0.4996 0.4104 0.347 0.052 Uiso 1 1 calc R . . H17B H 0.4301 0.3392 0.3254 0.052 Uiso 1 1 calc R . . H17C H 0.4826 0.3116 0.3791 0.052 Uiso 1 1 calc R . . C18 C 0.46210(19) 0.4925(3) 0.42971(14) 0.0401(9) Uani 1 1 d . . . H18A H 0.5 0.5313 0.4171 0.06 Uiso 1 1 calc R . . H18B H 0.4851 0.4423 0.4557 0.06 Uiso 1 1 calc R . . H18C H 0.432 0.5405 0.4452 0.06 Uiso 1 1 calc R . . C19 C 0.16153(17) 0.2674(3) 0.33904(13) 0.0275(7) Uani 1 1 d . . . H19 H 0.1633 0.3045 0.3062 0.033 Uiso 1 1 calc R . . C20 C 0.09552(19) 0.3077(3) 0.35895(15) 0.0437(10) Uani 1 1 d . . . H20A H 0.0508 0.2925 0.3337 0.066 Uiso 1 1 calc R . . H20B H 0.1001 0.3827 0.3642 0.066 Uiso 1 1 calc R . . H20C H 0.0933 0.2739 0.3917 0.066 Uiso 1 1 calc R . . C21 C 0.1547(2) 0.1517(3) 0.32711(17) 0.0541(11) Uani 1 1 d . . . H21A H 0.1089 0.1385 0.3025 0.081 Uiso 1 1 calc R . . H21B H 0.1546 0.1131 0.359 0.081 Uiso 1 1 calc R . . H21C H 0.196 0.1292 0.3122 0.081 Uiso 1 1 calc R . . C22 C 0.30121(16) 0.6597(2) 0.21529(11) 0.0204(7) Uani 1 1 d . . . C23 C 0.37327(17) 0.6940(2) 0.23089(12) 0.0233(7) Uani 1 1 d . . . C24 C 0.39114(19) 0.7899(3) 0.21272(13) 0.0314(8) Uani 1 1 d . . . H24 H 0.4399 0.8147 0.2221 0.038 Uiso 1 1 calc R . . C25 C 0.3393(2) 0.8493(3) 0.18149(13) 0.0347(8) Uani 1 1 d . . . H25 H 0.3524 0.9148 0.1698 0.042 Uiso 1 1 calc R . . C26 C 0.2687(2) 0.8145(3) 0.16711(13) 0.0317(8) Uani 1 1 d . . . H26 H 0.2334 0.8568 0.1458 0.038 Uiso 1 1 calc R . . C27 C 0.24785(17) 0.7182(2) 0.18331(11) 0.0235(7) Uani 1 1 d . . . C28 C 0.43193(17) 0.6280(3) 0.26467(13) 0.0320(8) Uani 1 1 d . . . H28 H 0.4059 0.5735 0.2809 0.038 Uiso 1 1 calc R . . C29 C 0.4790(2) 0.6873(4) 0.30788(17) 0.0607(13) Uani 1 1 d . . . H29A H 0.5149 0.6405 0.3281 0.091 Uiso 1 1 calc R . . H29B H 0.4482 0.717 0.3301 0.091 Uiso 1 1 calc R . . H29C H 0.5043 0.7431 0.2935 0.091 Uiso 1 1 calc R . . C30 C 0.4778(3) 0.5722(4) 0.23162(18) 0.0687(15) Uani 1 1 d . . . H30A H 0.4457 0.534 0.2041 0.103 Uiso 1 1 calc R . . H30B H 0.5111 0.5237 0.2531 0.103 Uiso 1 1 calc R . . H30C H 0.5063 0.6229 0.2164 0.103 Uiso 1 1 calc R . . C31 C 0.17120(18) 0.6763(3) 0.16383(13) 0.0335(8) Uani 1 1 d . . . H31 H 0.1619 0.6225 0.1889 0.04 Uiso 1 1 calc R . . C32 C 0.1117(2) 0.7581(4) 0.16055(15) 0.0496(11) Uani 1 1 d . . . H32A H 0.0638 0.7261 0.1481 0.074 Uiso 1 1 calc R . . H32B H 0.1197 0.8128 0.1367 0.074 Uiso 1 1 calc R . . H32C H 0.1132 0.7879 0.1948 0.074 Uiso 1 1 calc R . . C33 C 0.1661(2) 0.6229(3) 0.11179(15) 0.0435(10) Uani 1 1 d . . . H33A H 0.1165 0.5959 0.1 0.065 Uiso 1 1 calc R . . H33B H 0.2011 0.5657 0.1154 0.065 Uiso 1 1 calc R . . H33C H 0.1772 0.6728 0.0866 0.065 Uiso 1 1 calc R . . C34 C 0.11773(16) 0.8801(2) 0.44070(11) 0.0206(7) Uani 1 1 d . . . H34 H 0.0709 0.8832 0.4495 0.025 Uiso 1 1 calc R . . C35 C 0.16441(16) 0.9638(2) 0.45821(11) 0.0187(6) Uani 1 1 d . . . C36 C 0.23945(16) 0.9648(2) 0.45758(11) 0.0184(6) Uani 1 1 d . . . H36 H 0.2674 1.0179 0.4771 0.022 Uiso 1 1 calc R . . C37 C 0.13341(16) 1.0535(2) 0.48222(11) 0.0204(7) Uani 1 1 d . . . C38 C 0.17197(17) 1.1042(2) 0.52556(12) 0.0253(7) Uani 1 1 d . . . H38 H 0.2185 1.0789 0.542 0.03 Uiso 1 1 calc R . . C39 C 0.14360(19) 1.1912(3) 0.54513(13) 0.0337(8) Uani 1 1 d . . . H39 H 0.1711 1.2253 0.5744 0.04 Uiso 1 1 calc R . . C40 C 0.0757(2) 1.2285(3) 0.52240(14) 0.0363(9) Uani 1 1 d . . . H40 H 0.0563 1.2882 0.5358 0.044 Uiso 1 1 calc R . . C41 C 0.03623(19) 1.1781(3) 0.47999(15) 0.0365(9) Uani 1 1 d . . . H41 H -0.0109 1.2028 0.4644 0.044 Uiso 1 1 calc R . . C42 C 0.06469(17) 1.0915(2) 0.45980(13) 0.0274(7) Uani 1 1 d . . . H42 H 0.037 1.0579 0.4304 0.033 Uiso 1 1 calc R . . C43 C 0.07364(16) 0.7195(2) 0.40335(12) 0.0217(7) Uani 1 1 d . . . C44 C 0.08517(17) 0.6259(2) 0.43051(12) 0.0254(7) Uani 1 1 d . . . C45 C 0.03156(18) 0.5496(3) 0.41902(14) 0.0334(8) Uani 1 1 d . . . H45 H 0.0379 0.4856 0.437 0.04 Uiso 1 1 calc R . . C46 C -0.0308(2) 0.5660(3) 0.38176(15) 0.0394(9) Uani 1 1 d . . . H46 H -0.067 0.5135 0.3744 0.047 Uiso 1 1 calc R . . C47 C -0.04031(18) 0.6583(3) 0.35539(14) 0.0354(9) Uani 1 1 d . . . H47 H -0.0833 0.6684 0.3299 0.042 Uiso 1 1 calc R . . C48 C 0.01119(17) 0.7372(3) 0.36502(13) 0.0279(8) Uani 1 1 d . . . C49 C 0.15207(18) 0.6063(3) 0.47235(13) 0.0293(8) Uani 1 1 d . . . H49 H 0.1888 0.6609 0.4691 0.035 Uiso 1 1 calc R . . C50 C 0.1335(3) 0.6176(5) 0.52503(16) 0.0748(17) Uani 1 1 d . . . H50A H 0.1774 0.6051 0.5515 0.112 Uiso 1 1 calc R . . H50B H 0.0957 0.5672 0.5288 0.112 Uiso 1 1 calc R . . H50C H 0.1155 0.6878 0.5289 0.112 Uiso 1 1 calc R . . C51 C 0.1878(2) 0.5020(3) 0.46775(16) 0.0482(10) Uani 1 1 d . . . H51A H 0.2307 0.4946 0.4956 0.072 Uiso 1 1 calc R . . H51B H 0.2029 0.4977 0.4345 0.072 Uiso 1 1 calc R . . H51C H 0.1528 0.4466 0.4702 0.072 Uiso 1 1 calc R . . C52 C -0.00097(18) 0.8367(3) 0.33416(13) 0.0315(8) Uani 1 1 d . . . H52 H 0.0445 0.8791 0.3433 0.038 Uiso 1 1 calc R . . C53 C -0.0146(2) 0.8155(3) 0.27643(14) 0.0468(10) Uani 1 1 d . . . H53A H -0.0218 0.8811 0.2576 0.07 Uiso 1 1 calc R . . H53B H -0.0583 0.7723 0.2666 0.07 Uiso 1 1 calc R . . H53C H 0.0276 0.7793 0.268 0.07 Uiso 1 1 calc R . . C54 C -0.0639(2) 0.9003(3) 0.34726(16) 0.0460(10) Uani 1 1 d . . . H54A H -0.0699 0.964 0.3268 0.069 Uiso 1 1 calc R . . H54B H -0.0531 0.9179 0.384 0.069 Uiso 1 1 calc R . . H54C H -0.1091 0.8598 0.3394 0.069 Uiso 1 1 calc R . . C55 C 0.35393(16) 0.8982(2) 0.44667(12) 0.0202(7) Uani 1 1 d . . . C56 C 0.39513(17) 0.9371(2) 0.41191(12) 0.0241(7) Uani 1 1 d . . . C57 C 0.47075(18) 0.9248(3) 0.42440(14) 0.0324(8) Uani 1 1 d . . . H57 H 0.4997 0.9508 0.4015 0.039 Uiso 1 1 calc R . . C58 C 0.50456(18) 0.8761(3) 0.46893(14) 0.0364(9) Uani 1 1 d . . . H58 H 0.5561 0.8682 0.4765 0.044 Uiso 1 1 calc R . . C59 C 0.46302(18) 0.8389(3) 0.50261(14) 0.0340(8) Uani 1 1 d . . . H59 H 0.4866 0.8055 0.5334 0.041 Uiso 1 1 calc R . . C60 C 0.38737(17) 0.8490(3) 0.49253(12) 0.0260(7) Uani 1 1 d . . . C61 C 0.36018(18) 0.9935(3) 0.36320(13) 0.0293(8) Uani 1 1 d . . . H61 H 0.3064 0.9962 0.3619 0.035 Uiso 1 1 calc R . . C62 C 0.3726(2) 0.9365(3) 0.31504(14) 0.0415(9) Uani 1 1 d . . . H62A H 0.3491 0.9748 0.2843 0.062 Uiso 1 1 calc R . . H62B H 0.3514 0.8669 0.3142 0.062 Uiso 1 1 calc R . . H62C H 0.4251 0.9312 0.3158 0.062 Uiso 1 1 calc R . . C63 C 0.3877(2) 1.1041(3) 0.36354(15) 0.0403(9) Uani 1 1 d . . . H63A H 0.3642 1.1389 0.3317 0.06 Uiso 1 1 calc R . . H63B H 0.4408 1.1037 0.366 0.06 Uiso 1 1 calc R . . H63C H 0.3761 1.141 0.3932 0.06 Uiso 1 1 calc R . . C64 C 0.34410(18) 0.8057(3) 0.53087(13) 0.0306(8) Uani 1 1 d . . . H64 H 0.2912 0.8198 0.5169 0.037 Uiso 1 1 calc R . . C65 C 0.3652(2) 0.8617(3) 0.58289(14) 0.0440(10) Uani 1 1 d . . . H65A H 0.3368 0.8334 0.607 0.066 Uiso 1 1 calc R . . H65B H 0.355 0.9358 0.578 0.066 Uiso 1 1 calc R . . H65C H 0.4174 0.8517 0.5968 0.066 Uiso 1 1 calc R . . C66 C 0.3535(2) 0.6886(3) 0.53701(14) 0.0412(9) Uani 1 1 d . . . H66A H 0.3248 0.6635 0.5617 0.062 Uiso 1 1 calc R . . H66B H 0.4051 0.6723 0.5496 0.062 Uiso 1 1 calc R . . H66C H 0.3364 0.655 0.5036 0.062 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 In1 0.02247(12) 0.01632(11) 0.01794(11) -0.00087(9) 0.00561(8) 0.00192(9) In2 0.02090(12) 0.02084(12) 0.02355(12) -0.00512(9) 0.00418(9) 0.00167(9) Cl1 0.0232(4) 0.0466(5) 0.0489(5) 0.0020(4) 0.0093(4) 0.0059(4) Cl2 0.0432(5) 0.0473(6) 0.0265(4) 0.0042(4) -0.0008(4) -0.0039(4) S 0.0296(4) 0.0293(5) 0.0309(5) -0.0132(4) -0.0028(4) 0.0096(4) N1 0.0200(13) 0.0155(12) 0.0181(13) 0.0014(11) 0.0027(10) 0.0025(11) N2 0.0231(13) 0.0173(13) 0.0165(13) 0.0009(11) 0.0039(10) 0.0004(11) N3 0.0164(12) 0.0176(13) 0.0252(14) -0.0034(11) 0.0026(10) 0.0026(11) N4 0.0182(12) 0.0178(13) 0.0196(13) -0.0011(11) 0.0029(10) 0.0009(11) C1 0.0190(15) 0.0129(14) 0.0206(16) -0.0017(13) -0.0002(12) 0.0017(12) C2 0.0218(15) 0.0177(15) 0.0193(16) -0.0021(13) 0.0018(12) 0.0031(13) C3 0.0179(15) 0.0239(16) 0.0154(15) 0.0012(13) 0.0029(12) 0.0032(13) C4 0.0275(17) 0.0238(17) 0.0189(16) -0.0023(14) -0.0041(13) 0.0114(14) C5 0.045(2) 0.0245(18) 0.035(2) -0.0080(16) -0.0021(17) 0.0079(17) C6 0.067(3) 0.027(2) 0.053(3) -0.0162(19) -0.014(2) 0.010(2) C7 0.073(3) 0.050(3) 0.034(2) -0.024(2) -0.013(2) 0.034(2) C8 0.063(3) 0.058(3) 0.024(2) -0.0061(19) -0.0003(18) 0.032(2) C9 0.040(2) 0.041(2) 0.0221(18) -0.0017(16) 0.0033(15) 0.0168(17) C10 0.0266(16) 0.0159(15) 0.0162(15) 0.0015(12) 0.0047(13) 0.0077(13) C11 0.0252(16) 0.0219(16) 0.0214(16) -0.0014(13) 0.0062(13) 0.0084(14) C12 0.0338(19) 0.037(2) 0.0217(17) 0.0001(15) -0.0021(15) 0.0152(16) C13 0.046(2) 0.040(2) 0.0204(17) 0.0094(16) 0.0093(16) 0.0127(18) C14 0.039(2) 0.0290(18) 0.0261(18) 0.0080(15) 0.0103(15) 0.0079(16) C15 0.0308(17) 0.0160(15) 0.0241(17) 0.0027(13) 0.0071(14) 0.0046(14) C16 0.0249(16) 0.0267(18) 0.0259(17) -0.0044(14) 0.0004(14) 0.0054(14) C17 0.0278(18) 0.040(2) 0.037(2) -0.0046(17) 0.0068(16) 0.0039(16) C18 0.0312(19) 0.046(2) 0.038(2) -0.0076(18) -0.0055(16) 0.0015(18) C19 0.0283(17) 0.0284(18) 0.0257(17) 0.0054(15) 0.0050(14) -0.0039(15) C20 0.0304(19) 0.062(3) 0.039(2) 0.008(2) 0.0081(17) -0.0044(19) C21 0.065(3) 0.035(2) 0.054(3) -0.001(2) -0.008(2) -0.007(2) C22 0.0252(16) 0.0185(15) 0.0196(15) -0.0009(13) 0.0092(13) -0.0002(13) C23 0.0256(16) 0.0256(17) 0.0209(16) -0.0042(14) 0.0098(13) -0.0002(14) C24 0.0360(19) 0.0327(19) 0.0276(18) -0.0039(16) 0.0110(15) -0.0144(16) C25 0.053(2) 0.0239(18) 0.0298(19) 0.0023(15) 0.0149(17) -0.0068(17) C26 0.044(2) 0.0237(18) 0.0291(19) 0.0063(15) 0.0107(16) 0.0086(16) C27 0.0271(17) 0.0248(17) 0.0195(16) 0.0018(13) 0.0064(13) 0.0026(14) C28 0.0214(16) 0.041(2) 0.0346(19) 0.0058(16) 0.0069(15) 0.0014(16) C29 0.044(2) 0.067(3) 0.059(3) 0.003(2) -0.019(2) -0.002(2) C30 0.058(3) 0.087(4) 0.064(3) 0.010(3) 0.020(2) 0.040(3) C31 0.0257(17) 0.039(2) 0.035(2) 0.0144(17) 0.0039(15) 0.0016(16) C32 0.033(2) 0.075(3) 0.039(2) 0.000(2) 0.0034(17) 0.017(2) C33 0.036(2) 0.037(2) 0.052(2) -0.0052(19) -0.0037(18) 0.0004(18) C34 0.0168(15) 0.0226(16) 0.0220(16) 0.0024(13) 0.0033(12) 0.0036(13) C35 0.0200(15) 0.0171(15) 0.0186(15) -0.0009(12) 0.0031(12) 0.0029(13) C36 0.0223(15) 0.0154(15) 0.0166(15) 0.0008(12) 0.0019(12) 0.0002(13) C37 0.0236(16) 0.0179(15) 0.0220(16) 0.0002(13) 0.0103(13) -0.0012(13) C38 0.0249(17) 0.0243(17) 0.0277(17) -0.0014(14) 0.0074(14) -0.0002(14) C39 0.040(2) 0.0317(19) 0.0324(19) -0.0141(16) 0.0145(16) -0.0050(17) C40 0.044(2) 0.0266(19) 0.043(2) -0.0112(17) 0.0217(18) 0.0020(17) C41 0.0306(19) 0.032(2) 0.050(2) -0.0013(18) 0.0150(17) 0.0112(16) C42 0.0273(17) 0.0242(17) 0.0308(18) -0.0060(15) 0.0063(14) 0.0011(15) C43 0.0200(15) 0.0208(16) 0.0248(17) -0.0067(13) 0.0056(13) 0.0006(13) C44 0.0266(17) 0.0202(16) 0.0308(18) -0.0051(14) 0.0090(14) 0.0017(14) C45 0.0342(19) 0.0219(18) 0.045(2) -0.0028(16) 0.0096(17) -0.0038(16) C46 0.034(2) 0.030(2) 0.052(2) -0.0124(18) 0.0039(17) -0.0097(17) C47 0.0233(17) 0.040(2) 0.040(2) -0.0099(18) -0.0022(15) -0.0066(16) C48 0.0228(16) 0.0295(18) 0.0301(18) -0.0068(15) 0.0025(14) 0.0023(15) C49 0.0316(18) 0.0204(17) 0.0347(19) 0.0020(15) 0.0033(15) 0.0020(15) C50 0.062(3) 0.123(5) 0.034(2) -0.022(3) -0.002(2) 0.037(3) C51 0.050(2) 0.036(2) 0.055(3) 0.000(2) -0.001(2) 0.0152(19) C52 0.0257(17) 0.036(2) 0.0299(18) -0.0004(16) -0.0019(14) 0.0051(15) C53 0.045(2) 0.055(3) 0.035(2) -0.0005(19) -0.0044(18) 0.010(2) C54 0.041(2) 0.043(2) 0.053(3) 0.005(2) 0.0067(19) 0.0144(19) C55 0.0198(15) 0.0162(15) 0.0246(16) -0.0068(13) 0.0041(13) -0.0009(13) C56 0.0232(16) 0.0216(16) 0.0279(17) -0.0029(14) 0.0058(14) 0.0014(14) C57 0.0267(18) 0.036(2) 0.038(2) 0.0020(16) 0.0136(16) 0.0018(16) C58 0.0203(17) 0.045(2) 0.044(2) 0.0017(18) 0.0050(16) 0.0051(16) C59 0.0256(17) 0.041(2) 0.0339(19) 0.0055(17) 0.0021(15) 0.0087(16) C60 0.0246(16) 0.0263(17) 0.0268(17) 0.0023(14) 0.0041(14) 0.0039(14) C61 0.0267(17) 0.0307(19) 0.0324(19) 0.0026(15) 0.0103(15) 0.0020(15) C62 0.051(2) 0.043(2) 0.033(2) 0.0006(18) 0.0126(18) -0.0023(19) C63 0.047(2) 0.0283(19) 0.049(2) 0.0054(18) 0.0184(19) 0.0051(18) C64 0.0233(16) 0.040(2) 0.0279(18) 0.0097(16) 0.0050(14) 0.0028(16) C65 0.054(2) 0.048(2) 0.035(2) 0.0014(18) 0.0189(19) -0.001(2) C66 0.044(2) 0.041(2) 0.037(2) 0.0080(18) 0.0026(17) -0.0033(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 In1 N2 2.142(2) . ? In1 N1 2.147(2) . ? In1 Cl1 2.3454(8) . ? In1 S 2.3691(8) . ? In2 N3 2.140(2) . ? In2 N4 2.145(2) . ? In2 Cl2 2.3540(9) . ? In2 S 2.3640(8) . ? N1 C1 1.313(4) . ? N1 C10 1.450(4) . ? N2 C3 1.320(4) . ? N2 C22 1.447(4) . ? N3 C34 1.317(4) . ? N3 C43 1.446(4) . ? N4 C36 1.322(4) . ? N4 C55 1.434(4) . ? C1 C2 1.403(4) . ? C2 C3 1.402(4) . ? C2 C4 1.493(4) . ? C4 C5 1.385(5) . ? C4 C9 1.402(5) . ? C5 C6 1.394(5) . ? C6 C7 1.375(6) . ? C7 C8 1.370(6) . ? C8 C9 1.390(5) . ? C10 C11 1.401(4) . ? C10 C15 1.406(4) . ? C11 C12 1.399(4) . ? C11 C16 1.520(4) . ? C12 C13 1.379(5) . ? C13 C14 1.373(5) . ? C14 C15 1.394(4) . ? C15 C19 1.517(4) . ? C16 C18 1.529(4) . ? C16 C17 1.530(4) . ? C19 C20 1.527(5) . ? C19 C21 1.528(5) . ? C22 C27 1.395(4) . ? C22 C23 1.399(4) . ? C23 C24 1.394(4) . ? C23 C28 1.529(4) . ? C24 C25 1.376(5) . ? C25 C26 1.374(5) . ? C26 C27 1.397(4) . ? C27 C31 1.522(4) . ? C28 C29 1.507(5) . ? C28 C30 1.524(5) . ? C31 C32 1.524(5) . ? C31 C33 1.528(5) . ? C34 C35 1.408(4) . ? C35 C36 1.406(4) . ? C35 C37 1.494(4) . ? C37 C38 1.392(4) . ? C37 C42 1.393(4) . ? C38 C39 1.386(4) . ? C39 C40 1.379(5) . ? C40 C41 1.379(5) . ? C41 C42 1.391(5) . ? C43 C44 1.402(4) . ? C43 C48 1.405(4) . ? C44 C45 1.395(5) . ? C44 C49 1.518(4) . ? C45 C46 1.385(5) . ? C46 C47 1.376(5) . ? C47 C48 1.390(5) . ? C48 C52 1.516(5) . ? C49 C50 1.511(5) . ? C49 C51 1.519(5) . ? C52 C53 1.525(5) . ? C52 C54 1.531(5) . ? C55 C60 1.403(4) . ? C55 C56 1.406(4) . ? C56 C57 1.395(4) . ? C56 C61 1.513(4) . ? C57 C58 1.375(5) . ? C58 C59 1.381(5) . ? C59 C60 1.391(4) . ? C60 C64 1.525(4) . ? C61 C63 1.518(5) . ? C61 C62 1.531(5) . ? C64 C66 1.527(5) . ? C64 C65 1.537(5) . ? 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 N2 In1 N1 87.50(9) . . ? N2 In1 Cl1 109.08(7) . . ? N1 In1 Cl1 110.59(7) . . ? N2 In1 S 120.60(7) . . ? N1 In1 S 110.48(7) . . ? Cl1 In1 S 115.16(3) . . ? N3 In2 N4 88.31(9) . . ? N3 In2 Cl2 105.69(7) . . ? N4 In2 Cl2 111.57(7) . . ? N3 In2 S 126.22(7) . . ? N4 In2 S 104.43(7) . . ? Cl2 In2 S 116.54(3) . . ? In2 S In1 100.47(3) . . ? C1 N1 C10 118.9(2) . . ? C1 N1 In1 122.95(19) . . ? C10 N1 In1 118.01(18) . . ? C3 N2 C22 117.8(2) . . ? C3 N2 In1 122.9(2) . . ? C22 N2 In1 119.28(18) . . ? C34 N3 C43 118.5(2) . . ? C34 N3 In2 120.5(2) . . ? C43 N3 In2 120.27(18) . . ? C36 N4 C55 119.1(2) . . ? C36 N4 In2 121.83(19) . . ? C55 N4 In2 119.01(18) . . ? N1 C1 C2 128.3(3) . . ? C3 C2 C1 124.0(3) . . ? C3 C2 C4 118.4(3) . . ? C1 C2 C4 117.3(3) . . ? N2 C3 C2 128.4(3) . . ? C5 C4 C9 117.8(3) . . ? C5 C4 C2 120.5(3) . . ? C9 C4 C2 121.6(3) . . ? C4 C5 C6 121.0(4) . . ? C7 C6 C5 120.3(4) . . ? C8 C7 C6 119.6(4) . . ? C7 C8 C9 120.7(4) . . ? C8 C9 C4 120.5(4) . . ? C11 C10 C15 122.3(3) . . ? C11 C10 N1 118.3(3) . . ? C15 C10 N1 119.4(3) . . ? C12 C11 C10 117.6(3) . . ? C12 C11 C16 121.1(3) . . ? C10 C11 C16 121.2(3) . . ? C13 C12 C11 120.7(3) . . ? C14 C13 C12 120.7(3) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 C10 117.4(3) . . ? C14 C15 C19 119.4(3) . . ? C10 C15 C19 123.2(3) . . ? C11 C16 C18 114.1(3) . . ? C11 C16 C17 111.3(3) . . ? C18 C16 C17 110.5(3) . . ? C15 C19 C20 111.4(3) . . ? C15 C19 C21 110.5(3) . . ? C20 C19 C21 111.4(3) . . ? C27 C22 C23 122.5(3) . . ? C27 C22 N2 119.9(3) . . ? C23 C22 N2 117.6(3) . . ? C24 C23 C22 117.5(3) . . ? C24 C23 C28 120.3(3) . . ? C22 C23 C28 122.1(3) . . ? C25 C24 C23 121.0(3) . . ? C26 C25 C24 120.5(3) . . ? C25 C26 C27 121.1(3) . . ? C22 C27 C26 117.4(3) . . ? C22 C27 C31 121.6(3) . . ? C26 C27 C31 121.0(3) . . ? C29 C28 C30 111.6(3) . . ? C29 C28 C23 113.7(3) . . ? C30 C28 C23 110.3(3) . . ? C27 C31 C32 113.5(3) . . ? C27 C31 C33 110.6(3) . . ? C32 C31 C33 110.4(3) . . ? N3 C34 C35 129.4(3) . . ? C36 C35 C34 123.9(3) . . ? C36 C35 C37 118.0(3) . . ? C34 C35 C37 117.9(3) . . ? N4 C36 C35 127.6(3) . . ? C38 C37 C42 117.9(3) . . ? C38 C37 C35 122.4(3) . . ? C42 C37 C35 119.7(3) . . ? C39 C38 C37 121.1(3) . . ? C40 C39 C38 120.5(3) . . ? C41 C40 C39 119.1(3) . . ? C40 C41 C42 120.7(3) . . ? C41 C42 C37 120.7(3) . . ? C44 C43 C48 122.2(3) . . ? C44 C43 N3 118.5(3) . . ? C48 C43 N3 119.3(3) . . ? C45 C44 C43 117.8(3) . . ? C45 C44 C49 119.5(3) . . ? C43 C44 C49 122.6(3) . . ? C46 C45 C44 120.9(3) . . ? C47 C46 C45 120.0(3) . . ? C46 C47 C48 121.8(3) . . ? C47 C48 C43 117.3(3) . . ? C47 C48 C52 119.9(3) . . ? C43 C48 C52 122.8(3) . . ? C50 C49 C44 110.6(3) . . ? C50 C49 C51 110.2(3) . . ? C44 C49 C51 113.6(3) . . ? C48 C52 C53 111.5(3) . . ? C48 C52 C54 111.9(3) . . ? C53 C52 C54 110.0(3) . . ? C60 C55 C56 121.4(3) . . ? C60 C55 N4 118.9(3) . . ? C56 C55 N4 119.5(3) . . ? C57 C56 C55 117.7(3) . . ? C57 C56 C61 120.1(3) . . ? C55 C56 C61 122.1(3) . . ? C58 C57 C56 121.8(3) . . ? C57 C58 C59 119.5(3) . . ? C58 C59 C60 121.6(3) . . ? C59 C60 C55 118.0(3) . . ? C59 C60 C64 119.4(3) . . ? C55 C60 C64 122.6(3) . . ? C56 C61 C63 111.1(3) . . ? C56 C61 C62 111.6(3) . . ? C63 C61 C62 110.5(3) . . ? C60 C64 C66 111.7(3) . . ? C60 C64 C65 110.4(3) . . ? C66 C64 C65 111.6(3) . . ? #===END data_(14)-apr304 _database_code_depnum_ccdc_archive 'CCDC 609668' _audit_creation_date 2004-04-01T14:36:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H44 Cl6 In2 N4 O2 Sn2, 1.5(C4 H8 O1)' _chemical_formula_sum 'C22 H56 Cl6 In2 N4 O3.5 Sn2' _chemical_formula_weight 1112.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 23.5091(9) _cell_length_b 23.5091(9) _cell_length_c 28.5786(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 15794.8(9) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15555 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8704 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7457 _exptl_absorpt_correction_T_max 0.8673 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.30992E-2 _diffrn_orient_matrix_ub_12 0.20666E-2 _diffrn_orient_matrix_ub_13 -0.348568E-1 _diffrn_orient_matrix_ub_21 -0.75178E-2 _diffrn_orient_matrix_ub_22 0.417871E-1 _diffrn_orient_matrix_ub_23 0.21288E-2 _diffrn_orient_matrix_ub_31 0.417522E-1 _diffrn_orient_matrix_ub_32 0.76775E-2 _diffrn_orient_matrix_ub_33 -0.22041E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1094 _diffrn_reflns_av_unetI/netI 0.0796 _diffrn_reflns_number 34624 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 6811 _reflns_number_gt 4602 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0145P)^2^+176.7050P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6811 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.652 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.143 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn1 Sn 0.28463(2) 0.55373(2) 0.026520(17) 0.02422(14) Uani 1 1 d . . . Sn2 Sn 0.17281(2) 0.62783(3) 0.030004(18) 0.03050(16) Uani 1 1 d . . . In1 In 0.30579(3) 0.70728(2) 0.045175(18) 0.02874(16) Uani 1 1 d . . . In2 In 0.15007(2) 0.47283(2) 0.038220(18) 0.02626(15) Uani 1 1 d . . . Cl1 Cl 0.30118(10) 0.69606(10) 0.13031(7) 0.0411(6) Uani 1 1 d . . . Cl2 Cl 0.38870(10) 0.63954(9) 0.03942(8) 0.0429(6) Uani 1 1 d . . . Cl3 Cl 0.20909(9) 0.75620(9) 0.04354(7) 0.0404(5) Uani 1 1 d . . . Cl4 Cl 0.15427(10) 0.47554(9) 0.12392(7) 0.0377(5) Uani 1 1 d . . . Cl5 Cl 0.24443(9) 0.42181(10) 0.03462(8) 0.0418(6) Uani 1 1 d . . . Cl6 Cl 0.06657(9) 0.54102(9) 0.03931(7) 0.0389(5) Uani 1 1 d . . . O1 O 0.2586(2) 0.6367(2) 0.02193(16) 0.0252(12) Uani 1 1 d . . . O2 O 0.1984(2) 0.5453(2) 0.02042(16) 0.0263(12) Uani 1 1 d . . . O3 O 0.5496(4) 0.6333(4) -0.0769(3) 0.085(3) Uani 1 1 d . . . O4 O 0 0.75 0.0263(3) 0.063(3) Uani 1 2 d S . . N1 N 0.3592(3) 0.7894(3) 0.0534(2) 0.0382(19) Uani 1 1 d . . . N2 N 0.3195(3) 0.7359(3) -0.0339(2) 0.0302(16) Uani 1 1 d . . . N3 N 0.0959(3) 0.3899(3) 0.0424(2) 0.0383(18) Uani 1 1 d . . . N4 N 0.1318(3) 0.4528(3) -0.0413(2) 0.0339(17) Uani 1 1 d . . . C1 C 0.3712(5) 0.8110(5) 0.0069(3) 0.073(4) Uani 1 1 d . . . H1A H 0.3566 0.8505 0.0057 0.088 Uiso 1 1 calc R . . H1B H 0.4131 0.8134 0.004 0.088 Uiso 1 1 calc R . . C2 C 0.3525(9) 0.7853(7) -0.0309(4) 0.184(11) Uani 1 1 d . . . H2A H 0.3869 0.7774 -0.0498 0.22 Uiso 1 1 calc R . . H2B H 0.331 0.8146 -0.0483 0.22 Uiso 1 1 calc R . . C3 C 0.4131(5) 0.7778(5) 0.0786(4) 0.067(3) Uani 1 1 d . . . H3A H 0.4046 0.7632 0.11 0.101 Uiso 1 1 calc R . . H3B H 0.4351 0.8131 0.0813 0.101 Uiso 1 1 calc R . . H3C H 0.4353 0.7495 0.0613 0.101 Uiso 1 1 calc R . . C4 C 0.3282(4) 0.8333(4) 0.0811(4) 0.061(3) Uani 1 1 d . . . H4A H 0.3193 0.818 0.1122 0.092 Uiso 1 1 calc R . . H4B H 0.2928 0.8434 0.065 0.092 Uiso 1 1 calc R . . H4C H 0.3521 0.8672 0.0844 0.092 Uiso 1 1 calc R . . C5 C 0.2667(5) 0.7488(6) -0.0594(3) 0.096(5) Uani 1 1 d . . . H5A H 0.2433 0.7144 -0.0615 0.143 Uiso 1 1 calc R . . H5B H 0.276 0.7622 -0.091 0.143 Uiso 1 1 calc R . . H5C H 0.2456 0.7785 -0.0427 0.143 Uiso 1 1 calc R . . C6 C 0.3474(6) 0.6928(5) -0.0622(3) 0.096(5) Uani 1 1 d . . . H6A H 0.3235 0.6588 -0.0636 0.143 Uiso 1 1 calc R . . H6B H 0.3842 0.6832 -0.0482 0.143 Uiso 1 1 calc R . . H6C H 0.3534 0.7075 -0.0939 0.143 Uiso 1 1 calc R . . C7 C 0.0858(7) 0.3714(6) -0.0060(4) 0.117(6) Uani 1 1 d . . . H7A H 0.1069 0.3354 -0.0102 0.14 Uiso 1 1 calc R . . H7B H 0.0449 0.3619 -0.0083 0.14 Uiso 1 1 calc R . . C8 C 0.0974(7) 0.4024(6) -0.0412(4) 0.121(7) Uani 1 1 d . . . H8A H 0.0603 0.414 -0.0544 0.146 Uiso 1 1 calc R . . H8B H 0.115 0.3766 -0.0645 0.146 Uiso 1 1 calc R . . C9 C 0.0415(4) 0.4001(4) 0.0662(4) 0.067(3) Uani 1 1 d . . . H9A H 0.0207 0.4303 0.0499 0.101 Uiso 1 1 calc R . . H9B H 0.0487 0.4118 0.0986 0.101 Uiso 1 1 calc R . . H9C H 0.0189 0.3651 0.0661 0.101 Uiso 1 1 calc R . . C10 C 0.1256(5) 0.3446(4) 0.0687(4) 0.067(3) Uani 1 1 d . . . H10A H 0.1621 0.3364 0.0536 0.101 Uiso 1 1 calc R . . H10B H 0.1021 0.3102 0.069 0.101 Uiso 1 1 calc R . . H10C H 0.1323 0.3573 0.1009 0.101 Uiso 1 1 calc R . . C11 C 0.1013(6) 0.4983(6) -0.0656(4) 0.100(5) Uani 1 1 d . . . H11A H 0.1244 0.5331 -0.0652 0.15 Uiso 1 1 calc R . . H11B H 0.065 0.5055 -0.0498 0.15 Uiso 1 1 calc R . . H11C H 0.0942 0.4869 -0.098 0.15 Uiso 1 1 calc R . . C12 C 0.1843(4) 0.4426(6) -0.0683(3) 0.084(4) Uani 1 1 d . . . H12A H 0.208 0.4768 -0.0678 0.125 Uiso 1 1 calc R . . H12B H 0.1743 0.4333 -0.1008 0.125 Uiso 1 1 calc R . . H12C H 0.2053 0.4108 -0.0545 0.125 Uiso 1 1 calc R . . C13 C 0.3030(4) 0.5378(3) 0.0969(2) 0.030(2) Uani 1 1 d . . . H13A H 0.344 0.5413 0.1021 0.045 Uiso 1 1 calc R . . H13B H 0.2906 0.4993 0.1051 0.045 Uiso 1 1 calc R . . H13C H 0.2829 0.5655 0.1166 0.045 Uiso 1 1 calc R . . C14 C 0.3244(3) 0.5282(4) -0.0362(2) 0.032(2) Uani 1 1 d . . . H14A H 0.3657 0.5324 -0.0331 0.049 Uiso 1 1 calc R . . H14B H 0.3108 0.5521 -0.062 0.049 Uiso 1 1 calc R . . H14C H 0.315 0.4884 -0.0427 0.049 Uiso 1 1 calc R . . C15 C 0.1556(4) 0.6370(4) 0.1018(3) 0.037(2) Uani 1 1 d . . . H15A H 0.1146 0.633 0.1072 0.056 Uiso 1 1 calc R . . H15B H 0.1682 0.6746 0.1123 0.056 Uiso 1 1 calc R . . H15C H 0.176 0.6075 0.1194 0.056 Uiso 1 1 calc R . . C16 C 0.1308(4) 0.6562(4) -0.0311(3) 0.035(2) Uani 1 1 d . . . H16A H 0.0896 0.6519 -0.0271 0.052 Uiso 1 1 calc R . . H16B H 0.1434 0.6335 -0.0579 0.052 Uiso 1 1 calc R . . H16C H 0.1399 0.6963 -0.0366 0.052 Uiso 1 1 calc R . . C17 C 0.5016(4) 0.6229(5) -0.0482(4) 0.067(3) Uani 1 1 d . . . H17A H 0.4663 0.6244 -0.0671 0.081 Uiso 1 1 calc R . . H17B H 0.499 0.6521 -0.0233 0.081 Uiso 1 1 calc R . . C18 C 0.5081(5) 0.5668(5) -0.0274(4) 0.076(4) Uani 1 1 d . . . H18A H 0.5106 0.5697 0.0071 0.091 Uiso 1 1 calc R . . H18B H 0.4752 0.5423 -0.0355 0.091 Uiso 1 1 calc R . . C19 C 0.5600(5) 0.5434(5) -0.0464(5) 0.080(4) Uani 1 1 d . . . H19A H 0.5534 0.5042 -0.0578 0.096 Uiso 1 1 calc R . . H19B H 0.5899 0.5423 -0.022 0.096 Uiso 1 1 calc R . . C20 C 0.5774(6) 0.5801(6) -0.0847(4) 0.083(4) Uani 1 1 d . . . H20A H 0.6193 0.585 -0.0848 0.099 Uiso 1 1 calc R . . H20B H 0.5657 0.5636 -0.1151 0.099 Uiso 1 1 calc R . . C21 C -0.0371(5) 0.7824(5) 0.0555(4) 0.064(3) Uani 1 1 d . . . H21A H -0.0761 0.7664 0.0548 0.077 Uiso 1 1 calc R . . H21B H -0.0386 0.8224 0.0449 0.077 Uiso 1 1 calc R . . C22 C -0.0129(5) 0.7788(5) 0.1042(4) 0.077(4) Uani 1 1 d . . . H22A H 0.0162 0.8086 0.1096 0.093 Uiso 1 1 calc R . . H22B H -0.043 0.7821 0.1282 0.093 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 Sn1 0.0218(3) 0.0283(3) 0.0226(3) 0.0007(2) 0.0015(2) 0.0064(3) Sn2 0.0302(4) 0.0369(4) 0.0244(3) 0.0019(2) 0.0031(2) 0.0160(3) In1 0.0387(4) 0.0218(3) 0.0257(3) -0.0023(2) 0.0036(3) -0.0039(3) In2 0.0227(3) 0.0277(3) 0.0284(3) -0.0025(2) 0.0027(2) -0.0044(3) Cl1 0.0528(15) 0.0424(14) 0.0279(11) -0.0025(9) 0.0028(10) -0.0042(12) Cl2 0.0481(15) 0.0361(13) 0.0446(13) 0.0020(10) 0.0058(10) 0.0154(11) Cl3 0.0351(13) 0.0382(14) 0.0479(13) 0.0003(10) 0.0044(10) 0.0070(10) Cl4 0.0447(14) 0.0389(13) 0.0295(11) 0.0039(10) 0.0035(9) -0.0039(11) Cl5 0.0280(13) 0.0418(14) 0.0554(14) -0.0124(11) 0.0010(10) 0.0067(10) Cl6 0.0281(12) 0.0396(14) 0.0490(13) -0.0016(10) -0.0015(10) 0.0083(10) O1 0.032(3) 0.020(3) 0.024(3) 0.004(2) 0.003(2) -0.002(2) O2 0.026(3) 0.030(3) 0.023(3) 0.000(2) -0.001(2) 0.002(3) O3 0.098(7) 0.062(6) 0.094(6) 0.020(5) -0.008(5) -0.014(5) O4 0.057(7) 0.075(8) 0.057(6) 0 0 0.009(6) N1 0.050(5) 0.028(4) 0.036(4) -0.005(3) 0.000(4) -0.005(4) N2 0.038(4) 0.025(4) 0.028(4) -0.002(3) 0.004(3) -0.004(3) N3 0.036(5) 0.033(5) 0.046(4) -0.001(3) -0.005(3) -0.008(4) N4 0.027(4) 0.044(5) 0.031(4) -0.006(3) 0.001(3) -0.010(3) C1 0.104(10) 0.066(8) 0.050(7) 0.005(6) 0.007(6) -0.054(7) C2 0.35(3) 0.156(15) 0.046(8) 0.016(8) -0.014(11) -0.216(18) C3 0.060(8) 0.048(7) 0.094(9) -0.006(6) -0.026(6) -0.001(6) C4 0.056(7) 0.033(6) 0.094(8) -0.021(6) 0.007(6) -0.003(5) C5 0.078(9) 0.173(15) 0.037(6) 0.038(7) 0.006(6) 0.052(9) C6 0.151(13) 0.097(10) 0.038(6) 0.021(6) 0.038(7) 0.082(10) C7 0.188(17) 0.100(12) 0.061(9) -0.004(8) -0.019(9) -0.104(12) C8 0.183(16) 0.136(13) 0.045(8) -0.016(8) 0.008(8) -0.124(13) C9 0.015(6) 0.042(7) 0.145(11) 0.009(6) 0.013(6) -0.009(5) C10 0.062(8) 0.039(7) 0.100(9) 0.014(6) 0.006(6) -0.003(6) C11 0.155(14) 0.103(11) 0.042(7) -0.008(6) -0.036(7) 0.062(10) C12 0.042(7) 0.177(14) 0.033(6) -0.029(7) 0.013(5) 0.000(8) C13 0.035(5) 0.027(5) 0.027(4) -0.008(3) -0.001(4) -0.008(4) C14 0.035(5) 0.040(5) 0.022(4) -0.004(4) -0.002(4) 0.002(4) C15 0.031(5) 0.037(6) 0.043(5) 0.000(4) 0.002(4) 0.004(4) C16 0.035(5) 0.034(5) 0.036(5) 0.006(4) -0.001(4) 0.006(4) C17 0.033(7) 0.083(10) 0.086(8) 0.005(7) -0.018(6) -0.002(6) C18 0.077(9) 0.057(8) 0.094(9) 0.007(7) 0.017(7) -0.004(7) C19 0.068(9) 0.069(9) 0.104(10) -0.011(8) 0.015(7) 0.004(7) C20 0.106(11) 0.075(10) 0.067(8) -0.014(7) 0.021(7) -0.002(9) C21 0.053(7) 0.057(8) 0.082(8) 0.013(6) -0.001(6) 0.015(6) C22 0.085(10) 0.083(10) 0.064(8) -0.013(6) 0.002(7) 0.036(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn1 O2 2.044(5) . ? Sn1 O1 2.048(5) . ? Sn1 C13 2.092(7) . ? Sn1 C14 2.108(7) . ? Sn2 O1 2.040(5) . ? Sn2 O2 2.049(5) . ? Sn2 C15 2.103(8) . ? Sn2 C16 2.114(7) . ? In1 O1 2.104(5) . ? In1 N1 2.315(7) . ? In1 N2 2.381(6) . ? In1 Cl1 2.450(2) . ? In1 Cl2 2.522(2) . ? In1 Cl3 2.548(2) . ? In2 O2 2.111(5) . ? In2 N3 2.331(7) . ? In2 N4 2.359(6) . ? In2 Cl4 2.4520(19) . ? In2 Cl5 2.524(2) . ? In2 Cl6 2.535(2) . ? O3 C17 1.419(13) . ? O3 C20 1.430(13) . ? O4 C21 1.427(11) . ? N1 C1 1.450(11) . ? N1 C3 1.485(12) . ? N1 C4 1.490(11) . ? N2 C2 1.398(12) . ? N2 C6 1.453(11) . ? N2 C5 1.471(12) . ? N3 C9 1.468(11) . ? N3 C7 1.470(12) . ? N3 C10 1.478(12) . ? N4 C8 1.433(13) . ? N4 C11 1.465(12) . ? N4 C12 1.475(11) . ? C1 C2 1.312(14) . ? C7 C8 1.272(15) . ? C17 C18 1.455(14) . ? C18 C19 1.444(15) . ? C19 C20 1.454(15) . ? C21 C22 1.505(14) . ? C22 C22 1.48(2) 6_464 ? 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 O2 Sn1 O1 77.9(2) . . ? O2 Sn1 C13 105.6(3) . . ? O1 Sn1 C13 107.1(3) . . ? O2 Sn1 C14 109.8(3) . . ? O1 Sn1 C14 110.4(3) . . ? C13 Sn1 C14 132.5(3) . . ? O1 Sn2 O2 77.9(2) . . ? O1 Sn2 C15 106.9(3) . . ? O2 Sn2 C15 106.5(3) . . ? O1 Sn2 C16 109.6(3) . . ? O2 Sn2 C16 109.0(3) . . ? C15 Sn2 C16 133.2(3) . . ? O1 In1 N1 167.4(2) . . ? O1 In1 N2 89.7(2) . . ? N1 In1 N2 77.7(2) . . ? O1 In1 Cl1 101.85(13) . . ? N1 In1 Cl1 90.76(17) . . ? N2 In1 Cl1 168.38(17) . . ? O1 In1 Cl2 83.64(15) . . ? N1 In1 Cl2 96.58(19) . . ? N2 In1 Cl2 90.68(17) . . ? Cl1 In1 Cl2 91.78(8) . . ? O1 In1 Cl3 83.08(15) . . ? N1 In1 Cl3 96.24(19) . . ? N2 In1 Cl3 88.63(17) . . ? Cl1 In1 Cl3 91.56(8) . . ? Cl2 In1 Cl3 166.70(8) . . ? O2 In2 N3 169.0(2) . . ? O2 In2 N4 91.6(2) . . ? N3 In2 N4 77.5(2) . . ? O2 In2 Cl4 101.43(13) . . ? N3 In2 Cl4 89.55(18) . . ? N4 In2 Cl4 166.96(17) . . ? O2 In2 Cl5 84.31(15) . . ? N3 In2 Cl5 94.87(19) . . ? N4 In2 Cl5 91.45(18) . . ? Cl4 In2 Cl5 91.02(8) . . ? O2 In2 Cl6 84.78(15) . . ? N3 In2 Cl6 96.03(19) . . ? N4 In2 Cl6 89.87(18) . . ? Cl4 In2 Cl6 90.14(7) . . ? Cl5 In2 Cl6 169.04(8) . . ? Sn2 O1 Sn1 101.0(2) . . ? Sn2 O1 In1 124.5(2) . . ? Sn1 O1 In1 124.9(2) . . ? Sn1 O2 Sn2 100.9(2) . . ? Sn1 O2 In2 126.2(2) . . ? Sn2 O2 In2 125.0(2) . . ? C17 O3 C20 107.6(9) . . ? C21 O4 C21 108.4(11) . 6_464 ? C1 N1 C3 110.1(9) . . ? C1 N1 C4 110.0(8) . . ? C3 N1 C4 106.6(7) . . ? C1 N1 In1 107.7(5) . . ? C3 N1 In1 111.0(6) . . ? C4 N1 In1 111.5(5) . . ? C2 N2 C6 111.3(12) . . ? C2 N2 C5 109.2(12) . . ? C6 N2 C5 104.5(9) . . ? C2 N2 In1 104.5(6) . . ? C6 N2 In1 113.1(5) . . ? C5 N2 In1 114.4(6) . . ? C9 N3 C7 110.1(10) . . ? C9 N3 C10 107.1(8) . . ? C7 N3 C10 110.0(9) . . ? C9 N3 In2 111.3(6) . . ? C7 N3 In2 106.7(6) . . ? C10 N3 In2 111.7(6) . . ? C8 N4 C11 109.2(10) . . ? C8 N4 C12 109.8(10) . . ? C11 N4 C12 106.2(9) . . ? C8 N4 In2 105.5(6) . . ? C11 N4 In2 113.5(6) . . ? C12 N4 In2 112.7(5) . . ? C2 C1 N1 121.8(9) . . ? C1 C2 N2 128.3(10) . . ? C8 C7 N3 122.7(10) . . ? C7 C8 N4 126.5(10) . . ? O3 C17 C18 108.0(9) . . ? C19 C18 C17 106.2(10) . . ? C18 C19 C20 107.3(11) . . ? O3 C20 C19 105.8(9) . . ? O4 C21 C22 106.2(9) . . ? C22 C22 C21 101.9(7) 6_464 . ? #===END data_(11b)-nov2603 _database_code_depnum_ccdc_archive 'CCDC 609669' _audit_creation_date 2003-11-28T08:45:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H82 Cl2 In2 N4' _chemical_formula_sum 'C66 H82 Cl2 In2 N4' _chemical_formula_weight 1231.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3372(5) _cell_length_b 12.3604(6) _cell_length_c 12.9731(4) _cell_angle_alpha 92.242(2) _cell_angle_beta 118.216(2) _cell_angle_gamma 111.648(2) _cell_volume 1564.23(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9593 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9269 _exptl_absorpt_correction_T_max 0.9918 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.540542E-1 _diffrn_orient_matrix_ub_12 -0.744031E-1 _diffrn_orient_matrix_ub_13 0.141028E-1 _diffrn_orient_matrix_ub_21 -0.869569E-1 _diffrn_orient_matrix_ub_22 0.13008E-2 _diffrn_orient_matrix_ub_23 -0.625219E-1 _diffrn_orient_matrix_ub_31 -0.00304 _diffrn_orient_matrix_ub_32 -0.509072E-1 _diffrn_orient_matrix_ub_33 -0.640506E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.0472 _diffrn_reflns_number 15514 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 4345 _reflns_number_gt 3773 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0368P)^2^+2.0445P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4345 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.865 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' 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 0.62024(3) 0.60662(3) 0.57883(2) 0.02631(12) Uani 1 1 d . . . Cl Cl 0.56241(12) 0.74759(11) 0.64806(10) 0.0412(3) Uani 1 1 d . . . N1 N 0.7948(3) 0.6142(3) 0.7457(3) 0.0260(8) Uani 1 1 d . . . N2 N 0.7660(3) 0.7140(3) 0.5308(3) 0.0241(8) Uani 1 1 d . . . C1 C 0.9228(4) 0.6643(4) 0.7715(4) 0.0264(9) Uani 1 1 d . . . H1 H 0.9883 0.6596 0.8468 0.032 Uiso 1 1 calc R . . C2 C 0.9756(4) 0.7225(4) 0.7046(4) 0.0289(10) Uani 1 1 d . . . C3 C 0.8991(4) 0.7468(4) 0.5958(4) 0.0267(10) Uani 1 1 d . . . H3 H 0.9504 0.7938 0.564 0.032 Uiso 1 1 calc R . . C4 C 1.1245(4) 0.7636(4) 0.7536(4) 0.0329(11) Uani 1 1 d . . . C5 C 1.1719(5) 0.7446(5) 0.6796(5) 0.0431(12) Uani 1 1 d . . . H5 H 1.1086 0.7059 0.5957 0.052 Uiso 1 1 calc R . . C6 C 1.3124(6) 0.7819(5) 0.7276(6) 0.0591(16) Uani 1 1 d . . . H6 H 1.3438 0.7689 0.6761 0.071 Uiso 1 1 calc R . . C7 C 1.4044(6) 0.8371(6) 0.8487(7) 0.0675(18) Uani 1 1 d . . . H7 H 1.4993 0.8616 0.8809 0.081 Uiso 1 1 calc R . . C8 C 1.3604(5) 0.8573(5) 0.9236(5) 0.0597(16) Uani 1 1 d . . . H8 H 1.4246 0.8951 1.0075 0.072 Uiso 1 1 calc R . . C9 C 1.2216(5) 0.8222(5) 0.8765(4) 0.0461(13) Uani 1 1 d . . . H9 H 1.1921 0.8382 0.9286 0.055 Uiso 1 1 calc R . . C10 C 0.7801(4) 0.5631(4) 0.8396(3) 0.0266(10) Uani 1 1 d . . . C11 C 0.8107(4) 0.6414(4) 0.9417(4) 0.0318(10) Uani 1 1 d . . . C12 C 0.8014(5) 0.5888(5) 1.0326(4) 0.0400(12) Uani 1 1 d . . . H12 H 0.8223 0.6383 1.1035 0.048 Uiso 1 1 calc R . . C13 C 0.7629(5) 0.4679(5) 1.0219(4) 0.0441(12) Uani 1 1 d . . . H13 H 0.7569 0.435 1.085 0.053 Uiso 1 1 calc R . . C14 C 0.7328(5) 0.3936(5) 0.9208(4) 0.0409(12) Uani 1 1 d . . . H14 H 0.7066 0.31 0.9152 0.049 Uiso 1 1 calc R . . C15 C 0.7403(4) 0.4396(4) 0.8264(4) 0.0317(10) Uani 1 1 d . . . C16 C 0.8576(5) 0.7752(4) 0.9585(4) 0.0377(11) Uani 1 1 d . . . H16 H 0.8437 0.7931 0.8798 0.045 Uiso 1 1 calc R . . C17 C 0.7756(5) 0.8204(5) 0.9927(5) 0.0494(13) Uani 1 1 d . . . H17A H 0.8091 0.9075 1.002 0.074 Uiso 1 1 calc R . . H17B H 0.7868 0.803 1.0693 0.074 Uiso 1 1 calc R . . H17C H 0.6784 0.7794 0.9288 0.074 Uiso 1 1 calc R . . C18 C 1.0108(5) 0.8445(5) 1.0546(5) 0.0520(13) Uani 1 1 d . . . H18A H 1.0393 0.9312 1.0636 0.078 Uiso 1 1 calc R . . H18B H 1.0634 0.8198 1.0293 0.078 Uiso 1 1 calc R . . H18C H 1.0276 0.8266 1.1323 0.078 Uiso 1 1 calc R . . C19 C 0.7173(5) 0.3597(4) 0.7189(4) 0.0404(11) Uani 1 1 d . . . H19 H 0.6745 0.3895 0.6464 0.048 Uiso 1 1 calc R . . C20 C 0.8535(6) 0.3695(5) 0.7368(6) 0.0606(15) Uani 1 1 d . . . H20A H 0.8353 0.3175 0.6659 0.091 Uiso 1 1 calc R . . H20B H 0.9001 0.344 0.8094 0.091 Uiso 1 1 calc R . . H20C H 0.912 0.4533 0.7466 0.091 Uiso 1 1 calc R . . C21 C 0.6222(5) 0.2285(5) 0.6897(5) 0.0566(14) Uani 1 1 d . . . H21A H 0.6117 0.183 0.6193 0.085 Uiso 1 1 calc R . . H21B H 0.5325 0.2208 0.6713 0.085 Uiso 1 1 calc R . . H21C H 0.6606 0.1966 0.7594 0.085 Uiso 1 1 calc R . . C22 C 0.7253(4) 0.7628(4) 0.4259(4) 0.0257(9) Uani 1 1 d . . . C23 C 0.7450(4) 0.8824(4) 0.4412(4) 0.0273(10) Uani 1 1 d . . . C24 C 0.7130(4) 0.9284(4) 0.3389(4) 0.0347(11) Uani 1 1 d . . . H24 H 0.7267 1.0099 0.3465 0.042 Uiso 1 1 calc R . . C25 C 0.6621(4) 0.8566(5) 0.2280(4) 0.0388(12) Uani 1 1 d . . . H25 H 0.6405 0.889 0.1596 0.047 Uiso 1 1 calc R . . C26 C 0.6420(4) 0.7390(5) 0.2142(4) 0.0382(11) Uani 1 1 d . . . H26 H 0.6056 0.6911 0.1363 0.046 Uiso 1 1 calc R . . C27 C 0.6739(4) 0.6884(4) 0.3127(4) 0.0317(10) Uani 1 1 d . . . C28 C 0.8052(4) 0.9648(4) 0.5644(4) 0.0343(10) Uani 1 1 d . . . H28 H 0.8092 0.9139 0.623 0.041 Uiso 1 1 calc R . . C29 C 0.7162(5) 1.0260(5) 0.5599(5) 0.0513(13) Uani 1 1 d . . . H29A H 0.6231 0.9645 0.5304 0.077 Uiso 1 1 calc R . . H29B H 0.7133 1.0787 0.5051 0.077 Uiso 1 1 calc R . . H29C H 0.7551 1.0741 0.6413 0.077 Uiso 1 1 calc R . . C30 C 0.9499(5) 1.0591(5) 0.6112(5) 0.0615(16) Uani 1 1 d . . . H30A H 0.9864 1.1101 0.6905 0.092 Uiso 1 1 calc R . . H30B H 0.949 1.109 0.5542 0.092 Uiso 1 1 calc R . . H30C H 1.0079 1.0191 0.6192 0.092 Uiso 1 1 calc R . . C31 C 0.6660(5) 0.5629(4) 0.3015(4) 0.0445(12) Uani 1 1 d . . . H31 H 0.6415 0.5281 0.3601 0.053 Uiso 1 1 calc R . . C32 C 0.5601(5) 0.4773(5) 0.1773(5) 0.0562(14) Uani 1 1 d . . . H32A H 0.5609 0.3984 0.1778 0.084 Uiso 1 1 calc R . . H32B H 0.5814 0.5092 0.1178 0.084 Uiso 1 1 calc R . . H32C H 0.4692 0.4689 0.1558 0.084 Uiso 1 1 calc R . . C33 C 0.8084(5) 0.5669(5) 0.3370(4) 0.0478(13) Uani 1 1 d . . . H33A H 0.8004 0.4848 0.3295 0.072 Uiso 1 1 calc R . . H33B H 0.8768 0.615 0.4209 0.072 Uiso 1 1 calc R . . H33C H 0.8367 0.6035 0.2829 0.072 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 0.02496(18) 0.0353(2) 0.02567(17) 0.01356(13) 0.01546(13) 0.01652(14) Cl 0.0430(7) 0.0505(8) 0.0480(7) 0.0152(6) 0.0302(6) 0.0290(6) N1 0.0261(19) 0.031(2) 0.0272(18) 0.0127(15) 0.0174(15) 0.0138(17) N2 0.027(2) 0.030(2) 0.0260(18) 0.0141(15) 0.0183(16) 0.0171(17) C1 0.028(2) 0.026(2) 0.028(2) 0.0112(18) 0.0140(19) 0.016(2) C2 0.027(2) 0.032(3) 0.035(2) 0.015(2) 0.019(2) 0.017(2) C3 0.035(3) 0.026(3) 0.035(2) 0.0164(19) 0.026(2) 0.017(2) C4 0.027(2) 0.029(3) 0.051(3) 0.024(2) 0.023(2) 0.016(2) C5 0.039(3) 0.041(3) 0.068(3) 0.026(3) 0.034(3) 0.026(2) C6 0.055(4) 0.048(4) 0.115(5) 0.043(4) 0.062(4) 0.036(3) C7 0.028(3) 0.058(4) 0.118(6) 0.046(4) 0.033(4) 0.025(3) C8 0.030(3) 0.057(4) 0.076(4) 0.033(3) 0.017(3) 0.017(3) C9 0.035(3) 0.049(3) 0.052(3) 0.031(3) 0.020(2) 0.019(3) C10 0.023(2) 0.037(3) 0.026(2) 0.0156(19) 0.0128(18) 0.018(2) C11 0.026(2) 0.038(3) 0.028(2) 0.013(2) 0.0131(19) 0.013(2) C12 0.042(3) 0.048(3) 0.030(2) 0.012(2) 0.020(2) 0.017(2) C13 0.046(3) 0.054(4) 0.036(3) 0.024(2) 0.024(2) 0.021(3) C14 0.041(3) 0.036(3) 0.046(3) 0.021(2) 0.023(2) 0.017(2) C15 0.029(2) 0.032(3) 0.035(2) 0.017(2) 0.016(2) 0.015(2) C16 0.042(3) 0.042(3) 0.030(2) 0.009(2) 0.021(2) 0.018(2) C17 0.051(3) 0.046(3) 0.052(3) 0.009(2) 0.028(3) 0.021(3) C18 0.051(3) 0.042(3) 0.054(3) 0.008(3) 0.029(3) 0.011(3) C19 0.044(3) 0.038(3) 0.044(3) 0.015(2) 0.022(2) 0.022(2) C20 0.057(3) 0.037(3) 0.100(5) 0.014(3) 0.052(3) 0.017(3) C21 0.041(3) 0.052(4) 0.072(4) 0.009(3) 0.024(3) 0.023(3) C22 0.026(2) 0.029(3) 0.030(2) 0.0155(19) 0.0179(19) 0.015(2) C23 0.022(2) 0.034(3) 0.033(2) 0.0149(19) 0.0168(19) 0.016(2) C24 0.033(3) 0.035(3) 0.044(3) 0.019(2) 0.022(2) 0.019(2) C25 0.033(3) 0.053(4) 0.033(3) 0.025(2) 0.017(2) 0.021(2) C26 0.036(3) 0.046(3) 0.026(2) 0.011(2) 0.015(2) 0.014(2) C27 0.036(3) 0.034(3) 0.032(2) 0.013(2) 0.023(2) 0.015(2) C28 0.039(3) 0.030(3) 0.040(3) 0.008(2) 0.024(2) 0.017(2) C29 0.058(3) 0.043(3) 0.062(3) 0.008(3) 0.034(3) 0.029(3) C30 0.046(3) 0.066(4) 0.048(3) -0.009(3) 0.024(3) 0.003(3) C31 0.065(3) 0.041(3) 0.038(3) 0.015(2) 0.036(3) 0.021(3) C32 0.055(3) 0.050(4) 0.060(3) 0.004(3) 0.033(3) 0.016(3) C33 0.052(3) 0.048(3) 0.042(3) 0.009(2) 0.019(2) 0.030(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 2.179(3) . ? In N1 2.182(3) . ? In Cl 2.3983(11) . ? In In 2.8290(6) 2_666 ? N1 C1 1.324(5) . ? N1 C10 1.449(5) . ? N2 C3 1.321(5) . ? N2 C22 1.452(5) . ? C1 C2 1.390(6) . ? C2 C3 1.399(6) . ? C2 C4 1.489(6) . ? C4 C5 1.392(6) . ? C4 C9 1.402(7) . ? C5 C6 1.405(7) . ? C6 C7 1.371(8) . ? C7 C8 1.371(8) . ? C8 C9 1.392(7) . ? C10 C15 1.396(6) . ? C10 C11 1.411(6) . ? C11 C12 1.399(6) . ? C11 C16 1.505(6) . ? C12 C13 1.369(7) . ? C13 C14 1.376(7) . ? C14 C15 1.399(6) . ? C15 C19 1.521(6) . ? C16 C17 1.534(6) . ? C16 C18 1.534(7) . ? C19 C21 1.509(7) . ? C19 C20 1.540(7) . ? C22 C23 1.397(6) . ? C22 C27 1.410(6) . ? C23 C24 1.403(6) . ? C23 C28 1.528(6) . ? C24 C25 1.374(6) . ? C25 C26 1.370(7) . ? C26 C27 1.395(6) . ? C27 C31 1.515(7) . ? C28 C30 1.516(7) . ? C28 C29 1.530(6) . ? C31 C32 1.509(7) . ? C31 C33 1.571(7) . ? 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 N2 In N1 87.39(12) . . ? N2 In Cl 104.57(9) . . ? N1 In Cl 102.40(9) . . ? N2 In In 124.05(9) . 2_666 ? N1 In In 124.75(9) . 2_666 ? Cl In In 109.80(3) . 2_666 ? C1 N1 C10 113.5(3) . . ? C1 N1 In 124.3(3) . . ? C10 N1 In 122.3(2) . . ? C3 N2 C22 113.3(3) . . ? C3 N2 In 124.4(2) . . ? C22 N2 In 122.2(2) . . ? N1 C1 C2 129.6(4) . . ? C1 C2 C3 124.5(4) . . ? C1 C2 C4 117.5(4) . . ? C3 C2 C4 117.9(4) . . ? N2 C3 C2 129.4(4) . . ? C5 C4 C9 117.8(4) . . ? C5 C4 C2 121.3(4) . . ? C9 C4 C2 120.9(4) . . ? C4 C5 C6 120.6(5) . . ? C7 C6 C5 120.0(5) . . ? C8 C7 C6 120.5(5) . . ? C7 C8 C9 119.9(5) . . ? C8 C9 C4 121.1(5) . . ? C15 C10 C11 123.2(4) . . ? C15 C10 N1 118.4(4) . . ? C11 C10 N1 118.3(4) . . ? C12 C11 C10 116.2(4) . . ? C12 C11 C16 120.1(4) . . ? C10 C11 C16 123.6(4) . . ? C13 C12 C11 121.7(4) . . ? C12 C13 C14 120.8(4) . . ? C13 C14 C15 120.8(5) . . ? C10 C15 C14 117.3(4) . . ? C10 C15 C19 121.6(4) . . ? C14 C15 C19 121.0(4) . . ? C11 C16 C17 112.4(4) . . ? C11 C16 C18 110.8(4) . . ? C17 C16 C18 109.7(4) . . ? C21 C19 C15 114.2(4) . . ? C21 C19 C20 108.9(4) . . ? C15 C19 C20 111.5(4) . . ? C23 C22 C27 122.4(4) . . ? C23 C22 N2 119.4(3) . . ? C27 C22 N2 118.1(4) . . ? C24 C23 C22 117.6(4) . . ? C24 C23 C28 119.7(4) . . ? C22 C23 C28 122.7(4) . . ? C25 C24 C23 120.5(4) . . ? C24 C25 C26 121.2(4) . . ? C25 C26 C27 121.2(4) . . ? C26 C27 C22 117.1(4) . . ? C26 C27 C31 121.7(4) . . ? C22 C27 C31 121.0(4) . . ? C30 C28 C23 111.1(4) . . ? C30 C28 C29 109.9(4) . . ? C23 C28 C29 111.9(4) . . ? C32 C31 C27 114.5(4) . . ? C32 C31 C33 108.1(4) . . ? C27 C31 C33 111.2(4) . . ? #===END data_(11c)-jan504 _database_code_depnum_ccdc_archive 'CCDC 609670' _audit_creation_date 2004-01-15T14:47:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C66 H82 Cl2 In2 N4)(C6 H14)' _chemical_formula_sum 'C72 H96 Cl2 In2 N4' _chemical_formula_weight 1318.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3062(2) _cell_length_b 13.9612(2) _cell_length_c 18.5787(2) _cell_angle_alpha 90 _cell_angle_beta 95.975(1) _cell_angle_gamma 90 _cell_volume 3432.62(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 38413 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7465 _exptl_absorpt_correction_T_max 0.7927 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.721845E-1 _diffrn_orient_matrix_ub_12 0.153174E-1 _diffrn_orient_matrix_ub_13 -0.163738E-1 _diffrn_orient_matrix_ub_21 -0.10015E-1 _diffrn_orient_matrix_ub_22 0.220397E-1 _diffrn_orient_matrix_ub_23 0.499677E-1 _diffrn_orient_matrix_ub_31 0.199735E-1 _diffrn_orient_matrix_ub_32 0.664083E-1 _diffrn_orient_matrix_ub_33 -0.128066E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0188 _diffrn_reflns_number 51839 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 7826 _reflns_number_gt 6811 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The hexane solvate molecule was poorly defined and was refined with SADI constraints and isotropic C atoms. 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^)+(0.0457P)^2^+3.7956P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7826 _refine_ls_number_parameters 346 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.011 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.073657(12) 0.957320(11) 0.046684(8) 0.02534(7) Uani 1 1 d . . . Cl Cl 0.00373(6) 0.86893(5) 0.14047(4) 0.04509(16) Uani 1 1 d . . . N1 N 0.19970(16) 1.02835(14) 0.10801(11) 0.0299(4) Uani 1 1 d . . . N2 N 0.18453(16) 0.85743(15) 0.01414(11) 0.0323(4) Uani 1 1 d . . . C1 C 0.27728(19) 0.97805(18) 0.13731(13) 0.0320(5) Uani 1 1 d . . . H1 H 0.3198 1.0093 0.1744 0.038 Uiso 1 1 calc R . . C2 C 0.30512(18) 0.88432(18) 0.12076(13) 0.0320(5) Uani 1 1 d . . . C3 C 0.26474(19) 0.83552(18) 0.05879(14) 0.0331(5) Uani 1 1 d . . . H3 H 0.2997 0.7791 0.0473 0.04 Uiso 1 1 calc R . . C4 C 0.39089(19) 0.8382(2) 0.16612(14) 0.0366(5) Uani 1 1 d . . . C5 C 0.3885(3) 0.7396(3) 0.1801(2) 0.0578(8) Uani 1 1 d . . . H5 H 0.3316 0.7028 0.1614 0.069 Uiso 1 1 calc R . . C6 C 0.4686(3) 0.6950(3) 0.2212(2) 0.0736(11) Uani 1 1 d . . . H6 H 0.4666 0.6279 0.2293 0.088 Uiso 1 1 calc R . . C7 C 0.5508(3) 0.7472(3) 0.2504(2) 0.0644(10) Uani 1 1 d . . . H7 H 0.605 0.7166 0.2789 0.077 Uiso 1 1 calc R . . C8 C 0.5534(3) 0.8425(4) 0.2378(2) 0.0763(12) Uani 1 1 d . . . H8 H 0.6097 0.8789 0.2581 0.092 Uiso 1 1 calc R . . C9 C 0.4749(3) 0.8881(3) 0.1957(2) 0.0618(9) Uani 1 1 d . . . H9 H 0.4792 0.955 0.187 0.074 Uiso 1 1 calc R . . C10 C 0.19640(19) 1.12870(17) 0.12716(14) 0.0341(5) Uani 1 1 d . . . C11 C 0.2311(2) 1.1957(2) 0.07930(15) 0.0436(6) Uani 1 1 d . . . C12 C 0.2263(3) 1.2921(2) 0.09834(19) 0.0567(9) Uani 1 1 d . . . H12 H 0.2496 1.3393 0.0672 0.068 Uiso 1 1 calc R . . C13 C 0.1889(3) 1.3203(2) 0.16078(19) 0.0576(9) Uani 1 1 d . . . H13 H 0.1846 1.3866 0.1717 0.069 Uiso 1 1 calc R . . C14 C 0.1573(3) 1.2533(2) 0.20809(19) 0.0531(8) Uani 1 1 d . . . H14 H 0.1322 1.274 0.2515 0.064 Uiso 1 1 calc R . . C15 C 0.1618(2) 1.1549(2) 0.19297(16) 0.0433(6) Uani 1 1 d . . . C16 C 0.2787(3) 1.1637(2) 0.01223(18) 0.0595(9) Uani 1 1 d . . . H16 H 0.2484 1.1003 -0.0027 0.071 Uiso 1 1 calc R . . C17 C 0.2605(4) 1.2300(3) -0.0521(2) 0.0794(13) Uani 1 1 d . . . H17A H 0.1876 1.2392 -0.0641 0.119 Uiso 1 1 calc R . . H17B H 0.2894 1.2019 -0.0936 0.119 Uiso 1 1 calc R . . H17C H 0.2926 1.292 -0.0402 0.119 Uiso 1 1 calc R . . C18 C 0.3919(4) 1.1481(4) 0.0305(3) 0.0875(14) Uani 1 1 d . . . H18A H 0.4034 1.1048 0.072 0.131 Uiso 1 1 calc R . . H18B H 0.4248 1.2097 0.0424 0.131 Uiso 1 1 calc R . . H18C H 0.4201 1.1198 -0.0113 0.131 Uiso 1 1 calc R . . C19 C 0.1342(3) 1.0812(2) 0.24824(17) 0.0507(7) Uani 1 1 d . . . H19 H 0.1303 1.0172 0.2238 0.061 Uiso 1 1 calc R . . C20 C 0.2167(4) 1.0753(3) 0.3119(2) 0.0719(11) Uani 1 1 d . . . H20A H 0.282 1.0624 0.2938 0.108 Uiso 1 1 calc R . . H20B H 0.2008 1.0235 0.3445 0.108 Uiso 1 1 calc R . . H20C H 0.2203 1.1362 0.3383 0.108 Uiso 1 1 calc R . . C21 C 0.0328(4) 1.1007(4) 0.2745(3) 0.0882(14) Uani 1 1 d . . . H21A H 0.0185 1.0518 0.3098 0.132 Uiso 1 1 calc R . . H21B H -0.0197 1.099 0.2334 0.132 Uiso 1 1 calc R . . H21C H 0.0336 1.164 0.2972 0.132 Uiso 1 1 calc R . . C22 C 0.1674(2) 0.8002(2) -0.05101(14) 0.0388(6) Uani 1 1 d . . . C23 C 0.1971(3) 0.8376(2) -0.11538(16) 0.0487(7) Uani 1 1 d . . . C24 C 0.1806(3) 0.7801(3) -0.17706(19) 0.0675(10) Uani 1 1 d . . . H24 H 0.2007 0.8028 -0.2216 0.081 Uiso 1 1 calc R . . C25 C 0.1359(4) 0.6916(3) -0.1747(2) 0.0731(12) Uani 1 1 d . . . H25 H 0.1244 0.6544 -0.2176 0.088 Uiso 1 1 calc R . . C26 C 0.1080(3) 0.6571(3) -0.1109(2) 0.0676(10) Uani 1 1 d . . . H26 H 0.0771 0.5958 -0.1101 0.081 Uiso 1 1 calc R . . C27 C 0.1240(3) 0.7097(2) -0.04682(18) 0.0510(7) Uani 1 1 d . . . C28 C 0.2478(3) 0.9344(3) -0.11715(19) 0.0620(9) Uani 1 1 d . . . H28 H 0.2208 0.9751 -0.0792 0.074 Uiso 1 1 calc R . . C29 C 0.2283(4) 0.9877(4) -0.1888(2) 0.0846(14) Uani 1 1 d . . . H29A H 0.2631 1.0497 -0.1852 0.127 Uiso 1 1 calc R . . H29B H 0.1555 0.9982 -0.2001 0.127 Uiso 1 1 calc R . . H29C H 0.2537 0.9496 -0.2274 0.127 Uiso 1 1 calc R . . C30 C 0.3608(4) 0.9242(4) -0.0970(2) 0.0856(13) Uani 1 1 d . . . H30A H 0.3732 0.8905 -0.0507 0.128 Uiso 1 1 calc R . . H30B H 0.3919 0.9878 -0.0928 0.128 Uiso 1 1 calc R . . H30C H 0.3903 0.8876 -0.1346 0.128 Uiso 1 1 calc R . . C31 C 0.0979(3) 0.6663(2) 0.0245(2) 0.0620(9) Uani 1 1 d . . . H31 H 0.1074 0.7176 0.0621 0.074 Uiso 1 1 calc R . . C32 C 0.1695(4) 0.5829(3) 0.0497(3) 0.0863(14) Uani 1 1 d . . . H32A H 0.2397 0.6051 0.0528 0.13 Uiso 1 1 calc R . . H32B H 0.16 0.5301 0.0148 0.13 Uiso 1 1 calc R . . H32C H 0.1541 0.5606 0.0973 0.13 Uiso 1 1 calc R . . C33 C -0.0107(4) 0.6372(4) 0.0185(3) 0.0857(13) Uani 1 1 d . . . H33A H -0.0263 0.6096 0.0646 0.129 Uiso 1 1 calc R . . H33B H -0.0236 0.5894 -0.02 0.129 Uiso 1 1 calc R . . H33C H -0.0535 0.6934 0.0071 0.129 Uiso 1 1 calc R . . C34 C 0.5910(11) 0.3719(10) 0.0886(7) 0.255(6) Uiso 1 1 d D . . H34A H 0.6075 0.3576 0.1402 0.382 Uiso 1 1 calc R . . H34B H 0.6536 0.3804 0.0658 0.382 Uiso 1 1 calc R . . H34C H 0.5521 0.3187 0.0652 0.382 Uiso 1 1 calc R . . C35 C 0.5279(15) 0.4644(15) 0.0803(7) 0.344(10) Uiso 1 1 d D . . H35A H 0.4606 0.4596 0.0982 0.413 Uiso 1 1 calc R . . H35B H 0.5643 0.5226 0.0988 0.413 Uiso 1 1 calc R . . C36 C 0.5272(14) 0.4493(8) -0.0002(6) 0.305(9) Uiso 1 1 d D . . H36A H 0.4842 0.3959 -0.0205 0.366 Uiso 1 1 calc R . . H36B H 0.5945 0.4496 -0.0184 0.366 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 0.02781(10) 0.02315(9) 0.02391(10) -0.00032(5) -0.00276(6) 0.00033(6) Cl 0.0536(4) 0.0444(4) 0.0376(3) 0.0100(3) 0.0060(3) -0.0092(3) N1 0.0327(10) 0.0242(9) 0.0315(10) 0.0004(8) -0.0021(8) -0.0023(8) N2 0.0379(11) 0.0287(10) 0.0292(10) -0.0039(8) -0.0016(8) 0.0046(8) C1 0.0322(12) 0.0333(12) 0.0291(12) 0.0003(9) -0.0035(9) -0.0047(10) C2 0.0308(11) 0.0327(12) 0.0315(12) 0.0035(10) -0.0011(9) 0.0009(10) C3 0.0351(12) 0.0293(12) 0.0348(12) 0.0013(10) 0.0031(10) 0.0058(10) C4 0.0312(12) 0.0424(14) 0.0355(13) 0.0072(11) -0.0001(10) 0.0042(11) C5 0.0563(19) 0.0534(19) 0.061(2) 0.0078(16) -0.0048(16) 0.0072(15) C6 0.084(3) 0.059(2) 0.075(3) 0.0169(19) -0.005(2) 0.022(2) C7 0.0460(18) 0.076(3) 0.067(2) 0.0218(19) -0.0123(16) 0.0165(17) C8 0.0455(19) 0.094(3) 0.084(3) 0.016(2) -0.0180(18) -0.0033(19) C9 0.0482(18) 0.063(2) 0.071(2) 0.0181(18) -0.0084(16) -0.0022(16) C10 0.0362(12) 0.0248(11) 0.0383(13) -0.0035(10) -0.0103(10) -0.0031(10) C11 0.0546(17) 0.0340(14) 0.0385(14) 0.0042(11) -0.0131(12) -0.0100(12) C12 0.077(2) 0.0317(14) 0.0546(19) 0.0092(13) -0.0233(16) -0.0113(15) C13 0.074(2) 0.0273(14) 0.065(2) -0.0093(13) -0.0247(17) 0.0016(14) C14 0.0612(19) 0.0374(15) 0.0579(19) -0.0179(14) -0.0070(15) 0.0018(14) C15 0.0479(15) 0.0324(13) 0.0471(16) -0.0101(11) -0.0069(12) -0.0022(11) C16 0.088(3) 0.0451(17) 0.0449(17) 0.0042(14) 0.0042(17) -0.0228(17) C17 0.093(3) 0.090(3) 0.053(2) 0.020(2) 0.000(2) -0.024(2) C18 0.090(3) 0.092(3) 0.085(3) 0.017(3) 0.030(3) 0.015(3) C19 0.067(2) 0.0430(16) 0.0419(16) -0.0123(13) 0.0070(14) -0.0058(15) C20 0.101(3) 0.062(2) 0.0486(19) 0.0082(17) -0.014(2) -0.015(2) C21 0.093(3) 0.083(3) 0.095(3) 0.011(3) 0.039(3) 0.011(3) C22 0.0417(14) 0.0372(14) 0.0358(13) -0.0102(11) -0.0035(11) 0.0107(11) C23 0.0599(18) 0.0482(17) 0.0383(15) -0.0058(13) 0.0058(13) 0.0141(14) C24 0.097(3) 0.068(2) 0.0376(17) -0.0093(16) 0.0062(17) 0.022(2) C25 0.102(3) 0.064(2) 0.050(2) -0.0270(18) -0.010(2) 0.017(2) C26 0.085(3) 0.0483(19) 0.067(2) -0.0270(17) -0.005(2) -0.0002(18) C27 0.0633(19) 0.0385(15) 0.0495(17) -0.0132(13) -0.0026(14) 0.0042(14) C28 0.085(3) 0.060(2) 0.0444(18) -0.0046(15) 0.0265(18) 0.0007(19) C29 0.110(4) 0.079(3) 0.071(3) 0.020(2) 0.035(3) 0.015(3) C30 0.098(3) 0.099(3) 0.061(2) 0.007(2) 0.012(2) -0.027(3) C31 0.080(2) 0.0394(17) 0.066(2) -0.0111(15) 0.0043(19) -0.0111(17) C32 0.092(3) 0.061(2) 0.099(3) 0.019(2) -0.026(3) -0.015(2) C33 0.081(3) 0.082(3) 0.094(3) -0.008(3) 0.003(2) -0.009(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 2.162(2) . ? In N1 2.167(2) . ? In Cl 2.4004(7) . ? In In 2.7502(3) 3_575 ? N1 C1 1.318(3) . ? N1 C10 1.447(3) . ? N2 C3 1.318(3) . ? N2 C22 1.448(3) . ? C1 C2 1.403(4) . ? C2 C3 1.396(4) . ? C2 C4 1.492(3) . ? C4 C9 1.381(4) . ? C4 C5 1.403(4) . ? C5 C6 1.392(5) . ? C6 C7 1.378(6) . ? C7 C8 1.351(6) . ? C8 C9 1.393(5) . ? C10 C15 1.399(4) . ? C10 C11 1.401(4) . ? C11 C12 1.395(4) . ? C11 C16 1.522(5) . ? C12 C13 1.367(5) . ? C13 C14 1.379(5) . ? C14 C15 1.405(4) . ? C15 C19 1.525(4) . ? C16 C17 1.512(5) . ? C16 C18 1.524(6) . ? C19 C21 1.507(5) . ? C19 C20 1.530(5) . ? C22 C27 1.395(4) . ? C22 C23 1.399(4) . ? C23 C24 1.397(4) . ? C23 C28 1.513(5) . ? C24 C25 1.373(6) . ? C25 C26 1.367(6) . ? C26 C27 1.396(4) . ? C27 C31 1.529(5) . ? C28 C30 1.518(7) . ? C28 C29 1.524(5) . ? C31 C33 1.494(6) . ? C31 C32 1.546(6) . ? C34 C35 1.540(16) . ? C35 C36 1.508(17) . ? C36 C36 1.589(18) 3_665 ? 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 N2 In N1 85.92(8) . . ? N2 In Cl 101.47(6) . . ? N1 In Cl 101.01(6) . . ? N2 In In 124.44(5) . 3_575 ? N1 In In 126.52(5) . 3_575 ? Cl In In 112.08(2) . 3_575 ? C1 N1 C10 117.2(2) . . ? C1 N1 In 120.21(16) . . ? C10 N1 In 122.05(15) . . ? C3 N2 C22 116.4(2) . . ? C3 N2 In 120.35(16) . . ? C22 N2 In 122.50(16) . . ? N1 C1 C2 128.3(2) . . ? C3 C2 C1 123.2(2) . . ? C3 C2 C4 117.5(2) . . ? C1 C2 C4 118.8(2) . . ? N2 C3 C2 128.5(2) . . ? C9 C4 C5 117.1(3) . . ? C9 C4 C2 123.1(3) . . ? C5 C4 C2 119.8(3) . . ? C6 C5 C4 120.6(4) . . ? C7 C6 C5 120.7(4) . . ? C8 C7 C6 119.1(3) . . ? C7 C8 C9 121.1(4) . . ? C4 C9 C8 121.4(4) . . ? C15 C10 C11 122.7(2) . . ? C15 C10 N1 119.2(2) . . ? C11 C10 N1 118.0(2) . . ? C12 C11 C10 117.1(3) . . ? C12 C11 C16 121.7(3) . . ? C10 C11 C16 121.1(3) . . ? C13 C12 C11 121.6(3) . . ? C12 C13 C14 120.5(3) . . ? C13 C14 C15 120.9(3) . . ? C10 C15 C14 117.0(3) . . ? C10 C15 C19 122.4(2) . . ? C14 C15 C19 120.5(3) . . ? C17 C16 C11 114.9(3) . . ? C17 C16 C18 109.7(3) . . ? C11 C16 C18 110.2(3) . . ? C21 C19 C15 112.4(3) . . ? C21 C19 C20 110.7(3) . . ? C15 C19 C20 110.7(3) . . ? C27 C22 C23 122.7(3) . . ? C27 C22 N2 118.9(3) . . ? C23 C22 N2 118.4(3) . . ? C24 C23 C22 116.9(3) . . ? C24 C23 C28 121.8(3) . . ? C22 C23 C28 121.2(3) . . ? C25 C24 C23 121.5(4) . . ? C26 C25 C24 120.1(3) . . ? C25 C26 C27 121.5(4) . . ? C22 C27 C26 117.1(3) . . ? C22 C27 C31 122.7(3) . . ? C26 C27 C31 120.1(3) . . ? C23 C28 C30 110.0(3) . . ? C23 C28 C29 114.8(4) . . ? C30 C28 C29 109.6(3) . . ? C33 C31 C27 110.4(3) . . ? C33 C31 C32 112.2(3) . . ? C27 C31 C32 111.9(4) . . ? C36 C35 C34 86.0(12) . . ? C35 C36 C36 80.1(12) . 3_665 ? 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 N2 In N1 C1 -33.33(19) . . . . ? Cl In N1 C1 67.57(19) . . . . ? In In N1 C1 -164.07(16) 3_575 . . . ? N2 In N1 C10 155.6(2) . . . . ? Cl In N1 C10 -103.48(19) . . . . ? In In N1 C10 24.9(2) 3_575 . . . ? N1 In N2 C3 33.2(2) . . . . ? Cl In N2 C3 -67.3(2) . . . . ? In In N2 C3 165.58(17) 3_575 . . . ? N1 In N2 C22 -157.2(2) . . . . ? Cl In N2 C22 102.4(2) . . . . ? In In N2 C22 -24.8(2) 3_575 . . . ? C10 N1 C1 C2 -170.9(3) . . . . ? In N1 C1 C2 17.7(4) . . . . ? N1 C1 C2 C3 13.7(4) . . . . ? N1 C1 C2 C4 -174.2(2) . . . . ? C22 N2 C3 C2 172.5(3) . . . . ? In N2 C3 C2 -17.2(4) . . . . ? C1 C2 C3 N2 -14.0(4) . . . . ? C4 C2 C3 N2 173.8(3) . . . . ? C3 C2 C4 C9 137.5(3) . . . . ? C1 C2 C4 C9 -35.1(4) . . . . ? C3 C2 C4 C5 -42.3(4) . . . . ? C1 C2 C4 C5 145.2(3) . . . . ? C9 C4 C5 C6 -0.9(5) . . . . ? C2 C4 C5 C6 178.8(3) . . . . ? C4 C5 C6 C7 1.5(6) . . . . ? C5 C6 C7 C8 -0.8(7) . . . . ? C6 C7 C8 C9 -0.5(7) . . . . ? C5 C4 C9 C8 -0.4(6) . . . . ? C2 C4 C9 C8 179.9(3) . . . . ? C7 C8 C9 C4 1.1(7) . . . . ? C1 N1 C10 C15 -80.4(3) . . . . ? In N1 C10 C15 91.0(3) . . . . ? C1 N1 C10 C11 97.8(3) . . . . ? In N1 C10 C11 -90.8(3) . . . . ? C15 C10 C11 C12 -2.6(4) . . . . ? N1 C10 C11 C12 179.3(3) . . . . ? C15 C10 C11 C16 173.3(3) . . . . ? N1 C10 C11 C16 -4.8(4) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? C16 C11 C12 C13 -176.1(3) . . . . ? C11 C12 C13 C14 1.9(5) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C11 C10 C15 C14 3.6(4) . . . . ? N1 C10 C15 C14 -178.2(3) . . . . ? C11 C10 C15 C19 -173.6(3) . . . . ? N1 C10 C15 C19 4.5(4) . . . . ? C13 C14 C15 C10 -2.0(5) . . . . ? C13 C14 C15 C19 175.3(3) . . . . ? C12 C11 C16 C17 -36.6(5) . . . . ? C10 C11 C16 C17 147.7(3) . . . . ? C12 C11 C16 C18 87.9(4) . . . . ? C10 C11 C16 C18 -87.8(4) . . . . ? C10 C15 C19 C21 -131.1(4) . . . . ? C14 C15 C19 C21 51.8(4) . . . . ? C10 C15 C19 C20 104.5(3) . . . . ? C14 C15 C19 C20 -72.7(4) . . . . ? C3 N2 C22 C27 79.2(3) . . . . ? In N2 C22 C27 -90.8(3) . . . . ? C3 N2 C22 C23 -99.6(3) . . . . ? In N2 C22 C23 90.4(3) . . . . ? C27 C22 C23 C24 0.5(5) . . . . ? N2 C22 C23 C24 179.3(3) . . . . ? C27 C22 C23 C28 -177.5(3) . . . . ? N2 C22 C23 C28 1.2(4) . . . . ? C22 C23 C24 C25 0.9(5) . . . . ? C28 C23 C24 C25 179.0(4) . . . . ? C23 C24 C25 C26 -1.2(6) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C23 C22 C27 C26 -1.7(5) . . . . ? N2 C22 C27 C26 179.5(3) . . . . ? C23 C22 C27 C31 175.9(3) . . . . ? N2 C22 C27 C31 -2.8(5) . . . . ? C25 C26 C27 C22 1.5(6) . . . . ? C25 C26 C27 C31 -176.2(4) . . . . ? C24 C23 C28 C30 -92.4(4) . . . . ? C22 C23 C28 C30 85.5(4) . . . . ? C24 C23 C28 C29 31.7(5) . . . . ? C22 C23 C28 C29 -150.3(3) . . . . ? C22 C27 C31 C33 125.4(4) . . . . ? C26 C27 C31 C33 -57.0(5) . . . . ? C22 C27 C31 C32 -108.8(4) . . . . ? C26 C27 C31 C32 68.7(5) . . . . ? C34 C35 C36 C36 -174.5(17) . . . 3_665 ? #===END