Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Michael Hill' _publ_contact_author_address ; Department of Chemistry Imperial College London South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email MIKE.HILL@IMPERIAL.AC.UK _publ_section_title ; Configurational Stability of Heteroleptic ( -diketiminato) Heavier Alkaline Earth (Ca, Sr, Ba) Amides ; _publ_requested_category FM loop_ _publ_author_name 'Michael Hill' 'Anthony G. Avent' 'Mark R. Crimmin' 'Peter B. Hitchcock' data_mar104 _database_code_depnum_ccdc_archive 'CCDC 244505' _audit_creation_date 2004-03-01T10:29:10-00:00 _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 'C64 H98 Ca2 N6 O2' _chemical_formula_sum 'C64 H98 Ca2 N6 O2' _chemical_formula_weight 1063.64 _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 11.8176(2) _cell_length_b 15.3722(4) _cell_length_c 17.7226(4) _cell_angle_alpha 90 _cell_angle_beta 99.405(1) _cell_angle_gamma 90 _cell_volume 3176.25(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27656 _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 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.224 _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 0.807 _exptl_absorpt_correction_T_max 0.977 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.749881E-1 _diffrn_orient_matrix_ub_12 0.254642E-1 _diffrn_orient_matrix_ub_13 -0.243713E-1 _diffrn_orient_matrix_ub_21 0.137404E-1 _diffrn_orient_matrix_ub_22 -0.211854E-1 _diffrn_orient_matrix_ub_23 -0.510805E-1 _diffrn_orient_matrix_ub_31 -0.393055E-1 _diffrn_orient_matrix_ub_32 -0.559873E-1 _diffrn_orient_matrix_ub_33 0.82441E-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 0.0848 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_number 48654 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5575 _reflns_number_gt 4454 _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 atom on nitrogen was refined; other H atoms were riding. The C27 isopropyl group is disordered and refined with isotropic C atoms and SADI constraints. 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^)+(0.0393P)^2^+3.1792P] 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 5575 _refine_ls_number_parameters 339 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.412 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' Ca Ca 0.2262 0.3064 '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 Ca Ca 0.01227(4) 0.58567(3) 0.07100(3) 0.02745(14) Uani 1 1 d . . . O O 0.20770(14) 0.57196(11) 0.13816(10) 0.0422(4) Uani 1 1 d . . . N1 N 0.01753(14) 0.74258(11) 0.06987(10) 0.0221(4) Uani 1 1 d . . . N2 N -0.08102(15) 0.61847(11) 0.17804(10) 0.0256(4) Uani 1 1 d . . . N3 N 0.0744(2) 0.43627(14) 0.05790(14) 0.0450(6) Uani 1 1 d . . . H3X H 0.060(3) 0.390(2) 0.0913(19) 0.074(11) Uiso 1 1 d . . . C1 C 0.03926(17) 0.78661(13) 0.13500(12) 0.0222(5) Uani 1 1 d . . . C2 C 0.01703(17) 0.75639(14) 0.20576(12) 0.0235(5) Uani 1 1 d . . . H2 H 0.0525 0.7892 0.2486 0.028 Uiso 1 1 calc R . . C3 C -0.04933(17) 0.68514(14) 0.22414(12) 0.0236(5) Uani 1 1 d . . . C4 C 0.0902(2) 0.87775(15) 0.13619(14) 0.0337(5) Uani 1 1 d . . . H4C H 0.15 0.8792 0.1039 0.051 Uiso 1 1 calc R . . H4B H 0.1235 0.8932 0.1888 0.051 Uiso 1 1 calc R . . H4A H 0.0297 0.9195 0.1167 0.051 Uiso 1 1 calc R . . C5 C -0.0864(2) 0.69270(16) 0.30192(13) 0.0346(6) Uani 1 1 d . . . H5C H -0.1317 0.6415 0.3109 0.052 Uiso 1 1 calc R . . H5B H -0.133 0.7452 0.3033 0.052 Uiso 1 1 calc R . . H5A H -0.0184 0.6963 0.3417 0.052 Uiso 1 1 calc R . . C6 C 0.01945(18) 0.78781(14) -0.00054(12) 0.0248(5) Uani 1 1 d . . . C7 C -0.0752(2) 0.83900(16) -0.03255(14) 0.0330(5) Uani 1 1 d . . . C8 C -0.0737(2) 0.87886(18) -0.10292(15) 0.0403(6) Uani 1 1 d . . . H8 H -0.137 0.9137 -0.1247 0.048 Uiso 1 1 calc R . . C9 C 0.0173(2) 0.86907(19) -0.14178(15) 0.0456(7) Uani 1 1 d . . . H9 H 0.0167 0.8969 -0.1897 0.055 Uiso 1 1 calc R . . C10 C 0.1093(2) 0.81849(18) -0.11037(14) 0.0415(6) Uani 1 1 d . . . H10 H 0.1716 0.8113 -0.1375 0.05 Uiso 1 1 calc R . . C11 C 0.11327(19) 0.77763(15) -0.03987(13) 0.0297(5) Uani 1 1 d . . . C12 C -0.1787(2) 0.85354(19) 0.00752(16) 0.0461(7) Uani 1 1 d . . . H12 H -0.1653 0.8214 0.0572 0.055 Uiso 1 1 calc R . . C13 C -0.2877(2) 0.8173(2) -0.0411(2) 0.0655(10) Uani 1 1 d . . . H13C H -0.3532 0.827 -0.0147 0.098 Uiso 1 1 calc R . . H13B H -0.2784 0.7548 -0.049 0.098 Uiso 1 1 calc R . . H13A H -0.3011 0.847 -0.0907 0.098 Uiso 1 1 calc R . . C14 C -0.1959(3) 0.9500(2) 0.02433(19) 0.0634(9) Uani 1 1 d . . . H14C H -0.2626 0.9565 0.0502 0.095 Uiso 1 1 calc R . . H14B H -0.2086 0.9826 -0.0238 0.095 Uiso 1 1 calc R . . H14A H -0.1274 0.9724 0.0573 0.095 Uiso 1 1 calc R . . C15 C 0.2185(2) 0.72588(16) -0.00623(15) 0.0354(6) Uani 1 1 d . . . H15 H 0.2047 0.7005 0.0434 0.042 Uiso 1 1 calc R . . C16 C 0.3244(2) 0.7846(2) 0.0100(2) 0.0591(8) Uani 1 1 d . . . H16C H 0.3912 0.7498 0.0322 0.089 Uiso 1 1 calc R . . H16B H 0.3112 0.8304 0.0461 0.089 Uiso 1 1 calc R . . H16A H 0.3386 0.8112 -0.0378 0.089 Uiso 1 1 calc R . . C17 C 0.2417(3) 0.6513(2) -0.05816(19) 0.0586(8) Uani 1 1 d . . . H17C H 0.31 0.6193 -0.0343 0.088 Uiso 1 1 calc R . . H17B H 0.2544 0.6746 -0.1076 0.088 Uiso 1 1 calc R . . H17A H 0.1755 0.6119 -0.0661 0.088 Uiso 1 1 calc R . . C18 C -0.15896(19) 0.55558(14) 0.20116(14) 0.0296(5) Uani 1 1 d . A . C19 C -0.27543(19) 0.55968(14) 0.16803(13) 0.0285(5) Uani 1 1 d . . . C20 C -0.3509(2) 0.50021(16) 0.19185(16) 0.0381(6) Uani 1 1 d . . . H20 H -0.43 0.5031 0.1705 0.046 Uiso 1 1 calc R . . C21 C -0.3144(2) 0.43726(17) 0.24549(17) 0.0444(7) Uani 1 1 d . . . H21 H -0.3678 0.3982 0.2618 0.053 Uiso 1 1 calc R . . C22 C -0.2005(3) 0.43165(18) 0.27493(17) 0.0517(8) Uani 1 1 d . A . H22 H -0.175 0.3872 0.311 0.062 Uiso 1 1 calc R . . C23 C -0.1207(2) 0.48929(18) 0.25360(18) 0.0504(8) Uani 1 1 d . . . C24 C -0.31894(19) 0.62984(15) 0.11015(14) 0.0314(5) Uani 1 1 d . . . H24 H -0.2545 0.6455 0.0825 0.038 Uiso 1 1 calc R . . C25 C -0.4197(2) 0.60065(18) 0.05028(16) 0.0440(7) Uani 1 1 d . . . H25C H -0.4432 0.6485 0.0146 0.066 Uiso 1 1 calc R . . H25B H -0.4842 0.584 0.0757 0.066 Uiso 1 1 calc R . . H25A H -0.3965 0.5506 0.0221 0.066 Uiso 1 1 calc R . . C26 C -0.3514(3) 0.71137(18) 0.15037(17) 0.0524(8) Uani 1 1 d . . . H26C H -0.3787 0.756 0.1122 0.079 Uiso 1 1 calc R . . H26B H -0.2841 0.7332 0.1849 0.079 Uiso 1 1 calc R . . H26A H -0.4123 0.6975 0.1799 0.079 Uiso 1 1 calc R . . C30 C 0.1986(3) 0.4405(2) 0.06664(18) 0.0569(8) Uani 1 1 d . . . H30B H 0.2194 0.4695 0.0209 0.068 Uiso 1 1 calc R . . H30A H 0.2288 0.3804 0.0677 0.068 Uiso 1 1 calc R . . C31 C 0.2577(2) 0.48728(19) 0.13649(18) 0.0509(7) Uani 1 1 d . . . H31B H 0.2481 0.4544 0.1831 0.061 Uiso 1 1 calc R . . H31A H 0.3407 0.4924 0.1348 0.061 Uiso 1 1 calc R . . C32 C 0.2658(3) 0.6246(2) 0.19814(19) 0.0663(10) Uani 1 1 d . . . H32C H 0.2658 0.5954 0.2473 0.1 Uiso 1 1 calc R . . H32B H 0.2266 0.6808 0.1983 0.1 Uiso 1 1 calc R . . H32A H 0.345 0.634 0.1902 0.1 Uiso 1 1 calc R . . C27 C -0.0028(4) 0.4849(3) 0.2984(3) 0.0355(12) Uiso 0.615(8) 1 d PD A 1 H27 H 0.0415 0.5357 0.2834 0.043 Uiso 0.615(8) 1 calc PR A 1 C28 C 0.0098(4) 0.4840(3) 0.3857(3) 0.0471(14) Uiso 0.615(8) 1 d PD A 1 H28A H 0.0912 0.481 0.4079 0.071 Uiso 0.615(8) 1 calc PR A 1 H28B H -0.0302 0.4332 0.402 0.071 Uiso 0.615(8) 1 calc PR A 1 H28C H -0.0238 0.5372 0.4031 0.071 Uiso 0.615(8) 1 calc PR A 1 C29 C 0.0523(5) 0.4020(4) 0.2732(3) 0.0543(15) Uiso 0.615(8) 1 d PD A 1 H29A H 0.1308 0.3968 0.3011 0.081 Uiso 0.615(8) 1 calc PR A 1 H29B H 0.0541 0.4048 0.2181 0.081 Uiso 0.615(8) 1 calc PR A 1 H29C H 0.0074 0.3513 0.2842 0.081 Uiso 0.615(8) 1 calc PR A 1 C27A C 0.0177(6) 0.4623(5) 0.2644(4) 0.038(2) Uiso 0.385(8) 1 d PD A 2 H27A H 0.0566 0.5003 0.2307 0.046 Uiso 0.385(8) 1 calc PR A 2 C28A C 0.0609(11) 0.4854(7) 0.3465(6) 0.088(4) Uiso 0.385(8) 1 d PD A 2 H28D H 0.0448 0.5468 0.355 0.132 Uiso 0.385(8) 1 calc PR A 2 H28E H 0.1438 0.4753 0.358 0.132 Uiso 0.385(8) 1 calc PR A 2 H28F H 0.0222 0.4491 0.38 0.132 Uiso 0.385(8) 1 calc PR A 2 C29A C 0.0444(6) 0.3683(5) 0.2494(5) 0.041(2) Uiso 0.385(8) 1 d PD A 2 H29D H 0.0158 0.3542 0.1957 0.061 Uiso 0.385(8) 1 calc PR A 2 H29E H 0.0071 0.3305 0.2825 0.061 Uiso 0.385(8) 1 calc PR A 2 H29F H 0.1275 0.3592 0.2601 0.061 Uiso 0.385(8) 1 calc PR A 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 Ca 0.0317(3) 0.0195(2) 0.0304(3) -0.00559(19) 0.00287(19) 0.00327(19) O 0.0353(10) 0.0440(11) 0.0440(11) -0.0038(8) -0.0032(8) 0.0115(8) N1 0.0237(9) 0.0195(9) 0.0235(10) 0.0002(8) 0.0051(7) 0.0012(7) N2 0.0240(9) 0.0205(9) 0.0319(11) 0.0030(8) 0.0038(8) -0.0030(7) N3 0.0631(16) 0.0276(12) 0.0402(14) -0.0025(10) -0.0032(11) 0.0106(11) C1 0.0189(10) 0.0189(11) 0.0287(12) -0.0012(9) 0.0041(9) 0.0011(8) C2 0.0227(11) 0.0218(11) 0.0254(12) -0.0046(9) 0.0020(9) -0.0013(9) C3 0.0206(11) 0.0232(11) 0.0267(12) 0.0030(9) 0.0032(9) 0.0027(9) C4 0.0389(13) 0.0252(12) 0.0360(14) -0.0009(10) 0.0034(11) -0.0101(10) C5 0.0393(14) 0.0353(14) 0.0321(14) 0.0012(11) 0.0142(11) -0.0012(11) C6 0.0282(12) 0.0215(11) 0.0244(12) -0.0006(9) 0.0033(9) -0.0044(9) C7 0.0327(13) 0.0336(13) 0.0320(13) 0.0042(11) 0.0038(10) 0.0008(10) C8 0.0408(15) 0.0424(15) 0.0353(15) 0.0106(12) -0.0006(11) 0.0029(12) C9 0.0556(17) 0.0538(17) 0.0276(14) 0.0116(12) 0.0075(12) -0.0019(14) C10 0.0426(15) 0.0536(17) 0.0308(14) 0.0028(12) 0.0136(11) -0.0013(13) C11 0.0322(12) 0.0309(13) 0.0271(13) -0.0016(10) 0.0077(10) -0.0023(10) C12 0.0347(14) 0.0564(18) 0.0478(17) 0.0243(14) 0.0089(12) 0.0133(13) C13 0.0372(16) 0.0458(18) 0.114(3) 0.0098(18) 0.0143(17) 0.0017(13) C14 0.0493(18) 0.079(2) 0.061(2) -0.0169(18) 0.0062(15) 0.0171(17) C15 0.0313(13) 0.0400(14) 0.0376(14) 0.0031(11) 0.0139(10) 0.0046(11) C16 0.0415(16) 0.061(2) 0.072(2) -0.0105(17) 0.0014(15) 0.0018(14) C17 0.0576(19) 0.0454(17) 0.074(2) -0.0103(16) 0.0133(16) 0.0130(15) C18 0.0297(12) 0.0246(11) 0.0349(13) 0.0014(10) 0.0068(10) -0.0060(10) C19 0.0291(12) 0.0229(12) 0.0355(13) -0.0064(10) 0.0114(10) -0.0012(9) C20 0.0293(13) 0.0338(14) 0.0541(17) -0.0061(12) 0.0153(12) -0.0061(10) C21 0.0493(17) 0.0328(14) 0.0551(18) -0.0014(12) 0.0208(13) -0.0162(12) C22 0.0585(19) 0.0370(16) 0.0567(19) 0.0175(13) 0.0007(14) -0.0166(13) C23 0.0415(15) 0.0393(15) 0.065(2) 0.0211(14) -0.0063(13) -0.0142(12) C24 0.0242(12) 0.0276(12) 0.0427(14) -0.0035(11) 0.0066(10) 0.0001(10) C25 0.0317(13) 0.0435(16) 0.0539(17) -0.0097(13) -0.0016(12) 0.0016(12) C26 0.0623(19) 0.0341(15) 0.0565(19) -0.0102(13) -0.0032(15) 0.0134(14) C30 0.070(2) 0.0451(17) 0.058(2) -0.0056(14) 0.0179(16) 0.0254(15) C31 0.0355(15) 0.0500(17) 0.066(2) 0.0064(15) 0.0044(13) 0.0180(13) C32 0.0477(18) 0.078(2) 0.064(2) -0.0233(18) -0.0171(15) 0.0117(17) #----------------------------------------------------------------------------# # 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 Ca N3 2.370(2) 3_565 ? Ca N2 2.3983(19) . ? Ca N1 2.4130(17) . ? Ca O 2.4283(17) . ? Ca N3 2.434(2) . ? O C32 1.420(3) . ? O C31 1.432(3) . ? N1 C1 1.326(3) . ? N1 C6 1.432(3) . ? N2 C3 1.326(3) . ? N2 C18 1.440(3) . ? N3 C30 1.452(4) . ? N3 Ca 2.370(2) 3_565 ? C1 C2 1.402(3) . ? C1 C4 1.524(3) . ? C2 C3 1.416(3) . ? C3 C5 1.518(3) . ? C6 C7 1.409(3) . ? C6 C11 1.411(3) . ? C7 C8 1.392(3) . ? C7 C12 1.527(3) . ? C8 C9 1.377(4) . ? C9 C10 1.377(4) . ? C10 C11 1.392(3) . ? C11 C15 1.514(3) . ? C12 C14 1.532(4) . ? C12 C13 1.532(4) . ? C15 C17 1.523(4) . ? C15 C16 1.532(4) . ? C18 C23 1.403(3) . ? C18 C19 1.407(3) . ? C19 C20 1.390(3) . ? C19 C24 1.519(3) . ? C20 C21 1.376(4) . ? C21 C22 1.365(4) . ? C22 C23 1.390(4) . ? C23 C27 1.488(5) . ? C23 C27A 1.667(7) . ? C24 C26 1.522(3) . ? C24 C25 1.527(3) . ? C30 C31 1.501(4) . ? C27 C28 1.529(6) . ? C27 C29 1.531(7) . ? C27A C28A 1.503(10) . ? C27A C29A 1.512(9) . ? 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 N3 Ca N2 127.60(8) 3_565 . ? N3 Ca N1 98.16(7) 3_565 . ? N2 Ca N1 79.18(6) . . ? N3 Ca O 133.38(8) 3_565 . ? N2 Ca O 98.85(6) . . ? N1 Ca O 93.85(6) . . ? N3 Ca N3 82.15(8) 3_565 . ? N2 Ca N3 117.31(8) . . ? N1 Ca N3 159.05(8) . . ? O Ca N3 71.77(7) . . ? C32 O C31 112.5(2) . . ? C32 O Ca 128.45(16) . . ? C31 O Ca 115.55(15) . . ? C1 N1 C6 118.83(17) . . ? C1 N1 Ca 120.29(14) . . ? C6 N1 Ca 119.78(13) . . ? C3 N2 C18 118.22(19) . . ? C3 N2 Ca 122.00(14) . . ? C18 N2 Ca 118.81(14) . . ? C30 N3 Ca 112.30(18) . 3_565 ? C30 N3 Ca 105.26(17) . . ? Ca N3 Ca 97.85(8) 3_565 . ? N1 C1 C2 124.85(19) . . ? N1 C1 C4 120.07(19) . . ? C2 C1 C4 115.06(19) . . ? C1 C2 C3 130.8(2) . . ? N2 C3 C2 124.6(2) . . ? N2 C3 C5 121.64(19) . . ? C2 C3 C5 113.75(19) . . ? C7 C6 C11 120.0(2) . . ? C7 C6 N1 119.83(19) . . ? C11 C6 N1 120.14(19) . . ? C8 C7 C6 118.7(2) . . ? C8 C7 C12 118.7(2) . . ? C6 C7 C12 122.5(2) . . ? C9 C8 C7 121.7(2) . . ? C8 C9 C10 119.3(2) . . ? C9 C10 C11 121.7(2) . . ? C10 C11 C6 118.6(2) . . ? C10 C11 C15 119.7(2) . . ? C6 C11 C15 121.7(2) . . ? C7 C12 C14 111.9(2) . . ? C7 C12 C13 110.4(2) . . ? C14 C12 C13 109.6(2) . . ? C11 C15 C17 112.0(2) . . ? C11 C15 C16 111.0(2) . . ? C17 C15 C16 109.6(2) . . ? C23 C18 C19 119.8(2) . . ? C23 C18 N2 121.6(2) . . ? C19 C18 N2 118.6(2) . . ? C20 C19 C18 118.4(2) . . ? C20 C19 C24 120.6(2) . . ? C18 C19 C24 120.91(19) . . ? C21 C20 C19 121.9(2) . . ? C22 C21 C20 119.2(2) . . ? C21 C22 C23 121.7(3) . . ? C22 C23 C18 118.9(2) . . ? C22 C23 C27 116.3(3) . . ? C18 C23 C27 124.0(3) . . ? C22 C23 C27A 120.4(3) . . ? C18 C23 C27A 117.4(3) . . ? C19 C24 C26 110.6(2) . . ? C19 C24 C25 113.6(2) . . ? C26 C24 C25 109.9(2) . . ? N3 C30 C31 115.8(2) . . ? O C31 C30 108.3(2) . . ? C23 C27 C28 117.9(4) . . ? C23 C27 C29 106.7(4) . . ? C28 C27 C29 108.2(4) . . ? C28A C27A C29A 110.4(7) . . ? C28A C27A C23 103.0(7) . . ? C29A C27A C23 116.5(5) . . ? #===END data_(3)-dec803 _database_code_depnum_ccdc_archive 'CCDC 252118' _audit_creation_date 2003-12-05T10:53:02-00:00 _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 H67 Ba1 N3 O1 Si2' _chemical_formula_sum 'C39 H67 Ba1 N3 O1 Si2' _chemical_formula_weight 787.48 _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 12.0545(1) _cell_length_b 21.7583(2) _cell_length_c 17.3650(1) _cell_angle_alpha 90 _cell_angle_beta 109.619(1) _cell_angle_gamma 90 _cell_volume 4290.17(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 57485 _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 0.3 _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.012 _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 0.6644 _exptl_absorpt_correction_T_max 0.7319 #----------------------------------------------------------------------------# # 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 -0.26475E-1 _diffrn_orient_matrix_ub_12 -0.77E-5 _diffrn_orient_matrix_ub_13 0.487525E-1 _diffrn_orient_matrix_ub_21 -0.839908E-1 _diffrn_orient_matrix_ub_22 0.5146E-3 _diffrn_orient_matrix_ub_23 -0.368874E-1 _diffrn_orient_matrix_ub_31 -0.9361E-3 _diffrn_orient_matrix_ub_32 -0.459566E-1 _diffrn_orient_matrix_ub_33 -0.4213E-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 0.0359 _diffrn_reflns_av_unetI/netI 0.017 _diffrn_reflns_number 83242 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 9836 _reflns_number_gt 8940 _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^)+(0.0319P)^2^+2.3861P] 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 9836 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.025 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.412 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # 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' Ba Ba -0.3244 2.2819 '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' Si Si 0.0817 0.0704 '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 Ba Ba 0.521604(7) 0.164362(4) 0.311904(5) 0.02221(3) Uani 1 1 d . . . Si1 Si 0.60722(4) 0.30896(2) 0.23386(3) 0.02842(9) Uani 1 1 d . . . Si2 Si 0.51603(4) 0.207777(19) 0.10947(2) 0.02581(9) Uani 1 1 d . . . O1 O 0.62253(13) 0.18104(6) 0.47888(7) 0.0426(3) Uani 1 1 d . . . N1 N 0.54479(10) 0.04524(6) 0.29011(7) 0.0222(2) Uani 1 1 d . . . N2 N 0.31740(11) 0.10608(6) 0.29092(7) 0.0243(3) Uani 1 1 d . . . N3 N 0.54683(12) 0.23942(6) 0.20298(8) 0.0271(3) Uani 1 1 d . . . C1 C 0.52406(13) 0.01307(7) 0.34847(9) 0.0247(3) Uani 1 1 d . . . C2 C 0.43249(14) 0.02647(7) 0.37975(9) 0.0281(3) Uani 1 1 d . . . H2 H 0.4405 0.0076 0.4307 0.034 Uiso 1 1 calc R . . C3 C 0.33046(13) 0.06358(7) 0.34725(9) 0.0269(3) Uani 1 1 d . . . C4 C 0.60081(16) -0.04189(8) 0.38607(11) 0.0368(4) Uani 1 1 d . . . H4A H 0.59 -0.074 0.3446 0.055 Uiso 1 1 calc R . . H4B H 0.5783 -0.0579 0.4315 0.055 Uiso 1 1 calc R . . H4C H 0.6836 -0.0292 0.4064 0.055 Uiso 1 1 calc R . . C5 C 0.23261(15) 0.05118(9) 0.38257(11) 0.0392(4) Uani 1 1 d . . . H5A H 0.2357 0.0821 0.4243 0.059 Uiso 1 1 calc R . . H5B H 0.2432 0.0102 0.4074 0.059 Uiso 1 1 calc R . . H5C H 0.1561 0.0533 0.3388 0.059 Uiso 1 1 calc R . . C6 C 0.62187(13) 0.02204(6) 0.25010(9) 0.0220(3) Uani 1 1 d . . . C7 C 0.57542(14) -0.01549(7) 0.18049(9) 0.0280(3) Uani 1 1 d . . . C8 C 0.64821(16) -0.03252(8) 0.13673(10) 0.0345(4) Uani 1 1 d . . . H8 H 0.6179 -0.0583 0.0902 0.041 Uiso 1 1 calc R . . C9 C 0.76381(16) -0.01277(8) 0.15958(11) 0.0367(4) Uani 1 1 d . . . H9 H 0.8117 -0.0241 0.1282 0.044 Uiso 1 1 calc R . . C10 C 0.80920(15) 0.02342(8) 0.22822(11) 0.0327(3) Uani 1 1 d . . . H10 H 0.8888 0.0367 0.2439 0.039 Uiso 1 1 calc R . . C11 C 0.74071(13) 0.04089(7) 0.27501(9) 0.0252(3) Uani 1 1 d . . . C12 C 0.44881(16) -0.03822(9) 0.15360(11) 0.0381(4) Uani 1 1 d . . . H12 H 0.4072 -0.0157 0.1861 0.046 Uiso 1 1 calc R . . C13 C 0.4437(2) -0.10707(12) 0.17065(17) 0.0723(8) Uani 1 1 d . . . H13A H 0.3613 -0.1204 0.1536 0.109 Uiso 1 1 calc R . . H13B H 0.4815 -0.1148 0.2293 0.109 Uiso 1 1 calc R . . H13C H 0.485 -0.1301 0.14 0.109 Uiso 1 1 calc R . . C14 C 0.38246(19) -0.02641(10) 0.06334(12) 0.0490(5) Uani 1 1 d . . . H14A H 0.3015 -0.0415 0.0494 0.073 Uiso 1 1 calc R . . H14B H 0.4218 -0.048 0.0302 0.073 Uiso 1 1 calc R . . H14C H 0.3814 0.0178 0.0524 0.073 Uiso 1 1 calc R . . C15 C 0.79537(14) 0.08009(8) 0.35085(10) 0.0306(3) Uani 1 1 d . . . H15 H 0.7348 0.0855 0.378 0.037 Uiso 1 1 calc R . . C16 C 0.90316(17) 0.04899(11) 0.41267(12) 0.0497(5) Uani 1 1 d . . . H16A H 0.9355 0.0757 0.4604 0.075 Uiso 1 1 calc R . . H16B H 0.9632 0.0418 0.3871 0.075 Uiso 1 1 calc R . . H16C H 0.8795 0.0096 0.4299 0.075 Uiso 1 1 calc R . . C17 C 0.82778(18) 0.14406(9) 0.32832(12) 0.0433(4) Uani 1 1 d . . . H17A H 0.8629 0.1682 0.3782 0.065 Uiso 1 1 calc R . . H17B H 0.7567 0.1648 0.293 0.065 Uiso 1 1 calc R . . H17C H 0.8845 0.1401 0.2993 0.065 Uiso 1 1 calc R . . C18 C 0.20785(13) 0.13785(7) 0.25944(9) 0.0271(3) Uani 1 1 d . . . C19 C 0.12531(14) 0.11905(8) 0.18402(10) 0.0319(3) Uani 1 1 d . . . C20 C 0.01885(15) 0.15117(10) 0.15433(12) 0.0422(4) Uani 1 1 d . . . H20 H -0.0386 0.1384 0.1045 0.051 Uiso 1 1 calc R . . C21 C -0.00487(15) 0.20107(10) 0.19576(12) 0.0441(5) Uani 1 1 d . . . H21 H -0.0781 0.2219 0.1747 0.053 Uiso 1 1 calc R . . C22 C 0.07831(15) 0.22031(9) 0.26767(12) 0.0396(4) Uani 1 1 d . . . H22 H 0.0623 0.2551 0.2953 0.047 Uiso 1 1 calc R . . C23 C 0.18588(14) 0.18969(8) 0.30068(10) 0.0318(3) Uani 1 1 d . . . C24 C 0.15221(15) 0.06520(8) 0.13751(11) 0.0358(4) Uani 1 1 d . . . H24 H 0.2397 0.0636 0.1514 0.043 Uiso 1 1 calc R . . C25 C 0.09883(19) 0.07276(11) 0.04454(12) 0.0494(5) Uani 1 1 d . . . H25A H 0.1188 0.0369 0.0176 0.074 Uiso 1 1 calc R . . H25B H 0.1305 0.11 0.0278 0.074 Uiso 1 1 calc R . . H25C H 0.013 0.0762 0.0287 0.074 Uiso 1 1 calc R . . C26 C 0.1143(2) 0.00390(10) 0.16367(14) 0.0530(5) Uani 1 1 d . . . H26A H 0.1329 -0.0295 0.1321 0.079 Uiso 1 1 calc R . . H26B H 0.0293 0.0046 0.1536 0.079 Uiso 1 1 calc R . . H26C H 0.1564 -0.0027 0.222 0.079 Uiso 1 1 calc R . . C27 C 0.27776(16) 0.21485(9) 0.37751(11) 0.0386(4) Uani 1 1 d . . . H27 H 0.3425 0.1839 0.3965 0.046 Uiso 1 1 calc R . . C28 C 0.2295(2) 0.22561(14) 0.44754(14) 0.0671(7) Uani 1 1 d . . . H28A H 0.2921 0.2422 0.495 0.101 Uiso 1 1 calc R . . H28B H 0.2015 0.1866 0.4624 0.101 Uiso 1 1 calc R . . H28C H 0.1642 0.255 0.43 0.101 Uiso 1 1 calc R . . C29 C 0.33106(18) 0.27446(9) 0.35756(14) 0.0499(5) Uani 1 1 d . . . H29A H 0.3902 0.2903 0.4073 0.075 Uiso 1 1 calc R . . H29B H 0.2687 0.3051 0.3362 0.075 Uiso 1 1 calc R . . H29C H 0.3683 0.266 0.3164 0.075 Uiso 1 1 calc R . . C30 C 0.40103(17) 0.14648(9) 0.09709(11) 0.0393(4) Uani 1 1 d . . . H30A H 0.4286 0.117 0.1422 0.059 Uiso 1 1 calc R . . H30B H 0.3871 0.1251 0.045 0.059 Uiso 1 1 calc R . . H30C H 0.3276 0.1655 0.0976 0.059 Uiso 1 1 calc R . . C31 C 0.64537(18) 0.16864(9) 0.09282(11) 0.0403(4) Uani 1 1 d . . . H31A H 0.6804 0.1393 0.1372 0.061 Uiso 1 1 calc R . . H31B H 0.7042 0.1995 0.0921 0.061 Uiso 1 1 calc R . . H31C H 0.6188 0.1467 0.0405 0.061 Uiso 1 1 calc R . . C32 C 0.45670(16) 0.26251(8) 0.02131(10) 0.0364(4) Uani 1 1 d . . . H32A H 0.5141 0.2954 0.0257 0.055 Uiso 1 1 calc R . . H32B H 0.3827 0.2804 0.0225 0.055 Uiso 1 1 calc R . . H32C H 0.4424 0.2403 -0.0302 0.055 Uiso 1 1 calc R . . C33 C 0.7399(2) 0.32748(11) 0.20503(16) 0.0571(6) Uani 1 1 d . . . H33A H 0.7186 0.3263 0.1454 0.086 Uiso 1 1 calc R . . H33B H 0.8018 0.2972 0.2296 0.086 Uiso 1 1 calc R . . H33C H 0.7685 0.3686 0.225 0.086 Uiso 1 1 calc R . . C34 C 0.5020(2) 0.37500(9) 0.19690(14) 0.0550(6) Uani 1 1 d . . . H34A H 0.431 0.3675 0.2111 0.082 Uiso 1 1 calc R . . H34B H 0.4804 0.3788 0.1374 0.082 Uiso 1 1 calc R . . H34C H 0.5397 0.4131 0.2229 0.082 Uiso 1 1 calc R . . C35 C 0.65683(18) 0.31271(9) 0.34889(11) 0.0417(4) Uani 1 1 d . . . H35A H 0.5902 0.3034 0.3673 0.062 Uiso 1 1 calc R . . H35B H 0.6863 0.3541 0.3671 0.062 Uiso 1 1 calc R . . H35C H 0.7197 0.2826 0.3721 0.062 Uiso 1 1 calc R . . C36 C 0.63585(19) 0.23464(10) 0.53102(11) 0.0467(5) Uani 1 1 d . . . H36A H 0.5579 0.2516 0.527 0.056 Uiso 1 1 calc R . . H36B H 0.6816 0.267 0.515 0.056 Uiso 1 1 calc R . . C37 C 0.70095(17) 0.21241(10) 0.61726(10) 0.0415(4) Uani 1 1 d . . . H37A H 0.7873 0.2152 0.6304 0.05 Uiso 1 1 calc R . . H37B H 0.6779 0.2362 0.6581 0.05 Uiso 1 1 calc R . . C38 C 0.6611(2) 0.14619(13) 0.61388(13) 0.0609(6) Uani 1 1 d . . . H38A H 0.5818 0.1431 0.6188 0.073 Uiso 1 1 calc R . . H38B H 0.7173 0.1212 0.6573 0.073 Uiso 1 1 calc R . . C39 C 0.6595(2) 0.12671(10) 0.52971(12) 0.0565(6) Uani 1 1 d . . . H39A H 0.7388 0.1133 0.5314 0.068 Uiso 1 1 calc R . . H39B H 0.6034 0.0925 0.5085 0.068 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 Ba 0.02511(5) 0.01955(5) 0.02230(5) -0.00069(3) 0.00841(4) -0.00229(3) Si1 0.0311(2) 0.0231(2) 0.0299(2) 0.00011(17) 0.00880(17) -0.00561(17) Si2 0.0294(2) 0.0236(2) 0.02302(19) 0.00264(15) 0.00700(16) -0.00161(16) O1 0.0561(8) 0.0416(7) 0.0254(6) -0.0031(5) 0.0076(6) -0.0090(6) N1 0.0221(6) 0.0211(6) 0.0237(6) 0.0008(5) 0.0081(5) 0.0002(5) N2 0.0213(6) 0.0275(6) 0.0252(6) 0.0012(5) 0.0094(5) 0.0007(5) N3 0.0317(7) 0.0233(6) 0.0266(6) 0.0016(5) 0.0100(5) -0.0037(5) C1 0.0254(7) 0.0238(7) 0.0238(7) 0.0020(6) 0.0067(6) -0.0002(6) C2 0.0302(8) 0.0319(8) 0.0235(7) 0.0048(6) 0.0108(6) 0.0007(6) C3 0.0256(7) 0.0318(8) 0.0259(7) -0.0012(6) 0.0119(6) -0.0021(6) C4 0.0396(9) 0.0350(9) 0.0393(9) 0.0154(7) 0.0178(8) 0.0107(7) C5 0.0339(9) 0.0503(11) 0.0406(9) 0.0115(8) 0.0221(8) 0.0029(8) C6 0.0258(7) 0.0172(6) 0.0244(7) 0.0036(5) 0.0103(6) 0.0029(5) C7 0.0342(8) 0.0208(7) 0.0289(7) 0.0004(6) 0.0105(6) -0.0004(6) C8 0.0472(10) 0.0273(8) 0.0314(8) -0.0057(6) 0.0164(7) 0.0011(7) C9 0.0438(10) 0.0360(9) 0.0387(9) -0.0005(7) 0.0249(8) 0.0071(7) C10 0.0299(8) 0.0342(9) 0.0378(9) 0.0031(7) 0.0164(7) 0.0033(7) C11 0.0262(7) 0.0232(7) 0.0266(7) 0.0029(6) 0.0093(6) 0.0024(6) C12 0.0370(9) 0.0384(10) 0.0364(9) -0.0091(7) 0.0089(7) -0.0101(7) C13 0.0646(15) 0.0574(15) 0.0748(16) 0.0200(12) -0.0034(12) -0.0322(12) C14 0.0489(11) 0.0407(10) 0.0444(11) -0.0067(8) -0.0014(9) -0.0036(9) C15 0.0236(7) 0.0383(9) 0.0278(7) -0.0014(7) 0.0060(6) 0.0004(6) C16 0.0329(9) 0.0695(14) 0.0380(10) 0.0038(9) 0.0002(8) 0.0074(9) C17 0.0461(10) 0.0404(10) 0.0402(10) -0.0098(8) 0.0101(8) -0.0145(8) C18 0.0209(7) 0.0322(8) 0.0310(8) 0.0048(6) 0.0122(6) 0.0007(6) C19 0.0235(7) 0.0380(9) 0.0342(8) 0.0035(7) 0.0100(6) -0.0040(6) C20 0.0222(8) 0.0549(11) 0.0446(10) 0.0037(9) 0.0047(7) -0.0020(8) C21 0.0231(8) 0.0528(12) 0.0566(12) 0.0077(9) 0.0136(8) 0.0086(8) C22 0.0309(9) 0.0436(10) 0.0496(10) 0.0036(8) 0.0207(8) 0.0092(7) C23 0.0271(8) 0.0372(9) 0.0341(8) 0.0027(7) 0.0144(7) 0.0039(7) C24 0.0295(8) 0.0406(10) 0.0349(9) -0.0038(7) 0.0078(7) -0.0079(7) C25 0.0473(11) 0.0578(13) 0.0369(10) -0.0068(9) 0.0061(8) -0.0099(9) C26 0.0626(13) 0.0439(11) 0.0537(12) -0.0061(9) 0.0213(10) -0.0165(10) C27 0.0359(9) 0.0456(10) 0.0355(9) -0.0074(8) 0.0136(7) 0.0107(8) C28 0.0686(15) 0.0941(19) 0.0461(12) -0.0154(12) 0.0290(11) 0.0206(13) C29 0.0384(10) 0.0414(11) 0.0624(13) -0.0114(9) 0.0072(9) 0.0057(8) C30 0.0456(10) 0.0331(9) 0.0335(9) -0.0015(7) 0.0057(8) -0.0123(8) C31 0.0449(10) 0.0448(11) 0.0326(9) 0.0015(7) 0.0146(8) 0.0105(8) C32 0.0385(9) 0.0383(9) 0.0312(8) 0.0101(7) 0.0102(7) 0.0036(7) C33 0.0589(13) 0.0583(14) 0.0650(14) -0.0165(11) 0.0351(12) -0.0291(11) C34 0.0577(12) 0.0257(9) 0.0646(14) -0.0017(9) -0.0019(10) 0.0001(9) C35 0.0508(11) 0.0359(9) 0.0340(9) -0.0055(7) 0.0085(8) -0.0100(8) C36 0.0515(11) 0.0493(11) 0.0315(9) -0.0090(8) 0.0036(8) 0.0050(9) C37 0.0388(9) 0.0585(12) 0.0265(8) -0.0079(8) 0.0099(7) -0.0027(8) C38 0.0645(14) 0.0818(16) 0.0333(10) 0.0065(10) 0.0121(10) -0.0306(13) C39 0.0819(16) 0.0438(12) 0.0336(10) 0.0036(8) 0.0059(10) -0.0182(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 Ba N3 2.5931(13) . ? Ba N1 2.6477(12) . ? Ba N2 2.6829(12) . ? Ba O1 2.7659(12) . ? Si1 N3 1.6866(13) . ? Si1 C33 1.873(2) . ? Si1 C34 1.881(2) . ? Si1 C35 1.8848(18) . ? Si2 N3 1.6863(13) . ? Si2 C32 1.8811(17) . ? Si2 C31 1.8822(19) . ? Si2 C30 1.8833(18) . ? O1 C36 1.452(2) . ? O1 C39 1.453(2) . ? N1 C1 1.3228(19) . ? N1 C6 1.4264(18) . ? N2 C3 1.317(2) . ? N2 C18 1.4269(19) . ? C1 C2 1.415(2) . ? C1 C4 1.519(2) . ? C2 C3 1.420(2) . ? C3 C5 1.525(2) . ? C6 C7 1.410(2) . ? C6 C11 1.411(2) . ? C7 C8 1.390(2) . ? C7 C12 1.521(2) . ? C8 C9 1.383(3) . ? C9 C10 1.379(2) . ? C10 C11 1.392(2) . ? C11 C15 1.521(2) . ? C12 C14 1.523(3) . ? C12 C13 1.532(3) . ? C15 C17 1.532(3) . ? C15 C16 1.537(2) . ? C18 C23 1.408(2) . ? C18 C19 1.413(2) . ? C19 C20 1.399(2) . ? C19 C24 1.518(2) . ? C20 C21 1.384(3) . ? C21 C22 1.378(3) . ? C22 C23 1.398(2) . ? C23 C27 1.521(2) . ? C24 C26 1.527(3) . ? C24 C25 1.533(3) . ? C27 C28 1.532(3) . ? C27 C29 1.538(3) . ? C36 C37 1.518(3) . ? C37 C38 1.514(3) . ? C38 C39 1.516(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 N3 Ba N1 117.93(4) . . ? N3 Ba N2 121.71(4) . . ? N1 Ba N2 69.75(4) . . ? N3 Ba O1 124.34(4) . . ? N1 Ba O1 104.35(4) . . ? N2 Ba O1 105.36(4) . . ? N3 Si1 C33 115.09(9) . . ? N3 Si1 C34 114.03(8) . . ? C33 Si1 C34 106.43(12) . . ? N3 Si1 C35 108.98(7) . . ? C33 Si1 C35 106.17(10) . . ? C34 Si1 C35 105.44(10) . . ? N3 Si2 C32 115.20(8) . . ? N3 Si2 C31 114.00(8) . . ? C32 Si2 C31 105.64(8) . . ? N3 Si2 C30 108.35(8) . . ? C32 Si2 C30 106.94(8) . . ? C31 Si2 C30 106.14(9) . . ? C36 O1 C39 109.12(14) . . ? C36 O1 Ba 132.59(11) . . ? C39 O1 Ba 117.86(11) . . ? C1 N1 C6 120.50(12) . . ? C1 N1 Ba 110.63(10) . . ? C6 N1 Ba 122.23(9) . . ? C3 N2 C18 119.30(12) . . ? C3 N2 Ba 110.84(9) . . ? C18 N2 Ba 120.79(9) . . ? Si2 N3 Si1 127.19(8) . . ? Si2 N3 Ba 113.79(6) . . ? Si1 N3 Ba 118.48(6) . . ? N1 C1 C2 123.89(14) . . ? N1 C1 C4 120.10(14) . . ? C2 C1 C4 116.01(13) . . ? C1 C2 C3 130.39(14) . . ? N2 C3 C2 124.48(14) . . ? N2 C3 C5 120.49(14) . . ? C2 C3 C5 115.03(14) . . ? C7 C6 C11 120.09(14) . . ? C7 C6 N1 119.12(13) . . ? C11 C6 N1 120.54(13) . . ? C8 C7 C6 118.77(15) . . ? C8 C7 C12 119.87(15) . . ? C6 C7 C12 121.35(14) . . ? C9 C8 C7 121.36(15) . . ? C10 C9 C8 119.64(15) . . ? C9 C10 C11 121.31(16) . . ? C10 C11 C6 118.80(14) . . ? C10 C11 C15 119.30(14) . . ? C6 C11 C15 121.90(13) . . ? C7 C12 C14 112.78(16) . . ? C7 C12 C13 111.10(17) . . ? C14 C12 C13 108.80(16) . . ? C11 C15 C17 111.22(13) . . ? C11 C15 C16 112.13(15) . . ? C17 C15 C16 110.50(15) . . ? C23 C18 C19 120.60(14) . . ? C23 C18 N2 120.09(14) . . ? C19 C18 N2 119.19(14) . . ? C20 C19 C18 118.04(16) . . ? C20 C19 C24 121.52(16) . . ? C18 C19 C24 120.44(14) . . ? C21 C20 C19 121.63(17) . . ? C22 C21 C20 119.65(17) . . ? C21 C22 C23 121.28(18) . . ? C22 C23 C18 118.70(16) . . ? C22 C23 C27 119.34(16) . . ? C18 C23 C27 121.90(14) . . ? C19 C24 C26 112.14(15) . . ? C19 C24 C25 112.85(16) . . ? C26 C24 C25 110.19(16) . . ? C23 C27 C28 113.12(17) . . ? C23 C27 C29 110.01(16) . . ? C28 C27 C29 110.40(18) . . ? O1 C36 C37 105.76(16) . . ? C38 C37 C36 102.29(16) . . ? C37 C38 C39 101.80(16) . . ? O1 C39 C38 105.07(19) . . ? #===END data_(11)-jul2604 _database_code_depnum_ccdc_archive 'CCDC 252119' _audit_creation_date 2004-07-29T14:46:38-00:00 _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 '(C45 H67 Ca1 N3 O1), 0.5(C6 H14)' _chemical_formula_sum 'C48 H74 Ca N3 O' _chemical_formula_weight 749.18 _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 9.3762(2) _cell_length_b 12.6466(3) _cell_length_c 19.4777(5) _cell_angle_alpha 81.148(1) _cell_angle_beta 87.652(1) _cell_angle_gamma 83.765(1) _cell_volume 2267.91(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24049 _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 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.175 _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 0.8779 _exptl_absorpt_correction_T_max 0.9966 #----------------------------------------------------------------------------# # 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 0.34094E-1 _diffrn_orient_matrix_ub_12 -0.90252E-2 _diffrn_orient_matrix_ub_13 0.487382E-1 _diffrn_orient_matrix_ub_21 -0.101709 _diffrn_orient_matrix_ub_22 0.32251E-2 _diffrn_orient_matrix_ub_23 0.177906E-1 _diffrn_orient_matrix_ub_31 0.32422E-2 _diffrn_orient_matrix_ub_32 -0.79886E-1 _diffrn_orient_matrix_ub_33 0.30875E-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 0.0401 _diffrn_reflns_av_unetI/netI 0.03 _diffrn_reflns_number 31384 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 7917 _reflns_number_gt 6892 _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 molecule of haxane solvate is disordered about an inversion centre and was included with isotropic C atoms and H atoms omitted. The thf group has two disordered C atoms that were left isotropic. 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^)+(0.0844P)^2^+2.0079P] 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 7917 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.938 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # 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' Ca Ca 0.2262 0.3064 '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 Ca Ca 0.12413(4) 0.85062(3) 0.25714(2) 0.02448(14) Uani 1 1 d . A . O O -0.09797(17) 0.84857(15) 0.21005(9) 0.0398(4) Uani 1 1 d . . . N1 N 0.06367(18) 0.99462(14) 0.32207(9) 0.0263(4) Uani 1 1 d . . . N2 N 0.09568(19) 0.75091(14) 0.36742(9) 0.0267(4) Uani 1 1 d . . . N3 N 0.27891(19) 0.74694(15) 0.19580(9) 0.0305(4) Uani 1 1 d . . . H3 H 0.3015 0.6847 0.2221 0.037 Uiso 1 1 calc R A . C1 C -0.0251(2) 0.98596(17) 0.37698(11) 0.0279(5) Uani 1 1 d . A . C2 C -0.0626(2) 0.88780(18) 0.41438(11) 0.0294(5) Uani 1 1 d . . . H2 H -0.1437 0.8947 0.4448 0.035 Uiso 1 1 calc R A . C3 C -0.0003(2) 0.78131(18) 0.41437(11) 0.0277(5) Uani 1 1 d . A . C4 C -0.0919(3) 1.0857(2) 0.40575(13) 0.0381(6) Uani 1 1 d . . . H4A H -0.0464 1.1486 0.383 0.057 Uiso 1 1 calc R A . H4B H -0.0773 1.0763 0.4559 0.057 Uiso 1 1 calc R . . H4C H -0.1949 1.0964 0.3968 0.057 Uiso 1 1 calc R . . C5 C -0.0488(3) 0.7005(2) 0.47411(12) 0.0383(6) Uani 1 1 d . . . H5A H -0.1298 0.6669 0.4597 0.057 Uiso 1 1 calc R A . H5B H -0.0786 0.7373 0.5139 0.057 Uiso 1 1 calc R . . H5C H 0.0307 0.645 0.4874 0.057 Uiso 1 1 calc R . . C6 C 0.1053(2) 1.09745(17) 0.29171(12) 0.0292(5) Uani 1 1 d . A . C7 C 0.0161(3) 1.16913(18) 0.24510(13) 0.0350(5) Uani 1 1 d . . . C8 C 0.0692(3) 1.2622(2) 0.21116(15) 0.0452(6) Uani 1 1 d . A . H8 H 0.0103 1.3104 0.1791 0.054 Uiso 1 1 calc R . . C9 C 0.2048(3) 1.2863(2) 0.22283(16) 0.0494(7) Uani 1 1 d . . . H9 H 0.2388 1.3506 0.1992 0.059 Uiso 1 1 calc R A . C10 C 0.2915(3) 1.21664(19) 0.26906(15) 0.0424(6) Uani 1 1 d . A . H10 H 0.3848 1.2339 0.2772 0.051 Uiso 1 1 calc R . . C11 C 0.2445(2) 1.12170(18) 0.30389(13) 0.0330(5) Uani 1 1 d . . . C12 C -0.1350(3) 1.1479(2) 0.22948(15) 0.0433(6) Uani 1 1 d . A . H12 H -0.1605 1.0838 0.2627 0.052 Uiso 1 1 calc R . . C13 C -0.1410(4) 1.1210(3) 0.15555(17) 0.0647(9) Uani 1 1 d . . . H13A H -0.239 1.1076 0.1464 0.097 Uiso 1 1 calc R A . H13B H -0.0751 1.0567 0.151 0.097 Uiso 1 1 calc R . . H13C H -0.1128 1.1817 0.122 0.097 Uiso 1 1 calc R . . C14 C -0.2449(3) 1.2430(3) 0.2402(2) 0.0698(10) Uani 1 1 d . . . H14A H -0.3408 1.2268 0.2297 0.105 Uiso 1 1 calc R A . H14B H -0.2205 1.3075 0.2092 0.105 Uiso 1 1 calc R . . H14C H -0.2437 1.2555 0.2886 0.105 Uiso 1 1 calc R . . C15 C 0.3414(3) 1.0454(2) 0.35435(14) 0.0407(6) Uani 1 1 d . A . H15 H 0.3165 0.971 0.3526 0.049 Uiso 1 1 calc R . . C16 C 0.3149(4) 1.0658(4) 0.42688(18) 0.0927(14) Uani 1 1 d . . . H16A H 0.3791 1.0152 0.4578 0.139 Uiso 1 1 calc R A . H16B H 0.215 1.0559 0.4407 0.139 Uiso 1 1 calc R . . H16C H 0.3332 1.1396 0.4302 0.139 Uiso 1 1 calc R . . C17 C 0.5008(3) 1.0466(4) 0.3349(2) 0.0790(11) Uani 1 1 d . . . H17A H 0.5171 1.0323 0.2871 0.118 Uiso 1 1 calc R A . H17B H 0.5567 0.991 0.3665 0.118 Uiso 1 1 calc R . . H17C H 0.5307 1.1172 0.3388 0.118 Uiso 1 1 calc R . . C18 C 0.1688(2) 0.64418(17) 0.37815(11) 0.0280(5) Uani 1 1 d . A . C19 C 0.1079(2) 0.55675(18) 0.35841(12) 0.0324(5) Uani 1 1 d . . . C20 C 0.1879(3) 0.45603(19) 0.36626(13) 0.0393(6) Uani 1 1 d . A . H20 H 0.1481 0.3965 0.353 0.047 Uiso 1 1 calc R . . C21 C 0.3237(3) 0.4416(2) 0.39296(14) 0.0434(6) Uani 1 1 d . . . H21 H 0.3761 0.3723 0.3986 0.052 Uiso 1 1 calc R A . C22 C 0.3839(3) 0.5277(2) 0.41157(14) 0.0408(6) Uani 1 1 d . A . H22 H 0.4778 0.517 0.4297 0.049 Uiso 1 1 calc R . . C23 C 0.3091(2) 0.63006(18) 0.40423(12) 0.0333(5) Uani 1 1 d . . . C24 C -0.0385(3) 0.56912(19) 0.32608(13) 0.0373(6) Uani 1 1 d . A . H24 H -0.0838 0.6436 0.3292 0.045 Uiso 1 1 calc R . . C25 C -0.0227(3) 0.5573(2) 0.24912(14) 0.0460(6) Uani 1 1 d . . . H25A H -0.1179 0.5657 0.2288 0.069 Uiso 1 1 calc R A . H25B H 0.0255 0.486 0.2444 0.069 Uiso 1 1 calc R . . H25C H 0.0344 0.6127 0.2248 0.069 Uiso 1 1 calc R . . C26 C -0.1387(3) 0.4898(2) 0.36389(17) 0.0531(7) Uani 1 1 d . . . H26A H -0.2316 0.5014 0.3412 0.08 Uiso 1 1 calc R A . H26B H -0.1525 0.5013 0.4124 0.08 Uiso 1 1 calc R . . H26C H -0.096 0.4159 0.3622 0.08 Uiso 1 1 calc R . . C27 C 0.3767(3) 0.7235(2) 0.42527(15) 0.0435(6) Uani 1 1 d . A . H27 H 0.3328 0.7911 0.3971 0.052 Uiso 1 1 calc R . . C28 C 0.5394(3) 0.7172(3) 0.41218(19) 0.0674(9) Uani 1 1 d . . . H28A H 0.5763 0.7797 0.4267 0.101 Uiso 1 1 calc R A . H28B H 0.5609 0.7168 0.3625 0.101 Uiso 1 1 calc R . . H28C H 0.5852 0.6512 0.4389 0.101 Uiso 1 1 calc R . . C29 C 0.3438(3) 0.7318(3) 0.50198(18) 0.0619(9) Uani 1 1 d . . . H29A H 0.3878 0.7929 0.5145 0.093 Uiso 1 1 calc R A . H29B H 0.3829 0.6654 0.5308 0.093 Uiso 1 1 calc R . . H29C H 0.2397 0.7426 0.5098 0.093 Uiso 1 1 calc R . . C30 C 0.3499(2) 0.74600(18) 0.13280(11) 0.0277(5) Uani 1 1 d . A . C31 C 0.3404(2) 0.84238(18) 0.08333(12) 0.0308(5) Uani 1 1 d . . . C32 C 0.4150(3) 0.8442(2) 0.01991(12) 0.0385(6) Uani 1 1 d . A . H32 H 0.409 0.9091 -0.0122 0.046 Uiso 1 1 calc R . . C33 C 0.4975(3) 0.7546(2) 0.00226(13) 0.0451(6) Uani 1 1 d . . . H33 H 0.5493 0.7579 -0.0408 0.054 Uiso 1 1 calc R A . C34 C 0.5032(3) 0.6599(2) 0.04862(13) 0.0401(6) Uani 1 1 d . A . H34 H 0.5577 0.5976 0.0361 0.048 Uiso 1 1 calc R . . C35 C 0.4319(2) 0.65240(19) 0.11297(12) 0.0316(5) Uani 1 1 d . . . C36 C 0.2478(3) 0.94066(19) 0.10072(12) 0.0373(5) Uani 1 1 d . A . H36 H 0.1601 0.9147 0.1258 0.045 Uiso 1 1 calc R . . C37 C 0.1965(3) 1.0210(2) 0.03725(16) 0.0570(8) Uani 1 1 d . . . H37A H 0.1366 1.0818 0.0527 0.085 Uiso 1 1 calc R A . H37B H 0.1402 0.9855 0.008 0.085 Uiso 1 1 calc R . . H37C H 0.2797 1.0472 0.0105 0.085 Uiso 1 1 calc R . . C38 C 0.3218(3) 0.9989(2) 0.15029(15) 0.0497(7) Uani 1 1 d . . . H38A H 0.2586 1.0619 0.1603 0.075 Uiso 1 1 calc R A . H38B H 0.4117 1.022 0.1287 0.075 Uiso 1 1 calc R . . H38C H 0.3424 0.95 0.1937 0.075 Uiso 1 1 calc R . . C39 C 0.4379(3) 0.54595(19) 0.16201(13) 0.0362(5) Uani 1 1 d . A . H39 H 0.3393 0.5395 0.1828 0.043 Uiso 1 1 calc R . . C40 C 0.5391(3) 0.5418(2) 0.22195(15) 0.0513(7) Uani 1 1 d . . . H40A H 0.539 0.4722 0.252 0.077 Uiso 1 1 calc R A . H40B H 0.5068 0.5997 0.2489 0.077 Uiso 1 1 calc R . . H40C H 0.6365 0.5509 0.2034 0.077 Uiso 1 1 calc R . . C41 C 0.4789(3) 0.4472(2) 0.12606(17) 0.0527(7) Uani 1 1 d . . . H41A H 0.4804 0.3819 0.1605 0.079 Uiso 1 1 calc R A . H41B H 0.5741 0.4517 0.1039 0.079 Uiso 1 1 calc R . . H41C H 0.4083 0.4446 0.0908 0.079 Uiso 1 1 calc R . . C42 C -0.1245(3) 0.8242(2) 0.14144(14) 0.0484(7) Uani 0.530(10) 1 d P A 1 H42A H -0.0819 0.751 0.1352 0.058 Uiso 0.530(10) 1 calc PR A 1 H42B H -0.0882 0.8775 0.1041 0.058 Uiso 0.530(10) 1 calc PR A 1 C43 C -0.2981(7) 0.8331(7) 0.1446(3) 0.0549(18) Uiso 0.530(10) 1 d P A 1 H43A H -0.3408 0.9083 0.1319 0.066 Uiso 0.530(10) 1 calc PR A 1 H43B H -0.3356 0.7872 0.1141 0.066 Uiso 0.530(10) 1 calc PR A 1 C44 C -0.3248(5) 0.7912(5) 0.2217(3) 0.0382(16) Uiso 0.530(10) 1 d P A 1 H44A H -0.4264 0.806 0.2365 0.046 Uiso 0.530(10) 1 calc PR A 1 H44B H -0.293 0.7135 0.2338 0.046 Uiso 0.530(10) 1 calc PR A 1 C45 C -0.2333(3) 0.8570(3) 0.24854(16) 0.0540(7) Uani 0.530(10) 1 d P A 1 H45A H -0.2182 0.8321 0.2987 0.065 Uiso 0.530(10) 1 calc PR A 1 H45B H -0.2767 0.9327 0.2426 0.065 Uiso 0.530(10) 1 calc PR A 1 C42A C -0.1245(3) 0.8242(2) 0.14144(14) 0.0484(7) Uani 0.470(10) 1 d P A 2 H42C H -0.1193 0.8894 0.1065 0.058 Uiso 0.470(10) 1 calc PR A 2 H42D H -0.0501 0.768 0.1291 0.058 Uiso 0.470(10) 1 calc PR A 2 C43A C -0.2649(6) 0.7868(6) 0.1408(3) 0.0371(16) Uiso 0.470(10) 1 d P A 2 H43C H -0.2616 0.7079 0.1545 0.044 Uiso 0.470(10) 1 calc PR A 2 H43D H -0.31 0.808 0.095 0.044 Uiso 0.470(10) 1 calc PR A 2 C44A C -0.3445(10) 0.8515(10) 0.1993(5) 0.080(3) Uiso 0.470(10) 1 d P A 2 H44C H -0.384 0.9245 0.1783 0.096 Uiso 0.470(10) 1 calc PR A 2 H44D H -0.4236 0.8127 0.2225 0.096 Uiso 0.470(10) 1 calc PR A 2 C45A C -0.2333(3) 0.8570(3) 0.24854(16) 0.0540(7) Uani 0.470(10) 1 d P A 2 H45C H -0.248 0.9261 0.2672 0.065 Uiso 0.470(10) 1 calc PR A 2 H45D H -0.235 0.7973 0.2878 0.065 Uiso 0.470(10) 1 calc PR A 2 C1S C 0.0873(8) 0.6780(7) 0.0069(4) 0.160(3) Uiso 1 1 d . B 2 C2S C 0.0663(11) 0.5680(9) 0.0506(5) 0.199(4) Uiso 1 1 d . . 2 C3S C -0.0767(12) 0.5315(9) 0.0482(6) 0.110(3) Uiso 0.5 1 d P . 2 C4S C -0.1252(13) 0.5146(10) -0.0198(7) 0.124(4) Uiso 0.5 1 d P . 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 Ca 0.0246(2) 0.0248(2) 0.0235(2) -0.00377(17) 0.00078(16) -0.00030(16) O 0.0286(8) 0.0565(11) 0.0349(9) -0.0071(8) -0.0042(7) -0.0054(7) N1 0.0271(9) 0.0225(9) 0.0284(9) -0.0031(7) 0.0011(7) -0.0012(7) N2 0.0291(9) 0.0240(9) 0.0261(9) -0.0018(7) -0.0014(7) -0.0014(7) N3 0.0335(10) 0.0286(10) 0.0267(10) -0.0011(8) 0.0045(8) 0.0020(8) C1 0.0250(11) 0.0291(11) 0.0297(11) -0.0076(9) -0.0036(9) 0.0014(9) C2 0.0267(11) 0.0350(12) 0.0262(11) -0.0057(9) 0.0036(9) -0.0014(9) C3 0.0271(11) 0.0327(12) 0.0234(11) -0.0019(9) -0.0032(8) -0.0055(9) C4 0.0389(13) 0.0355(13) 0.0407(14) -0.0135(11) 0.0065(11) 0.0008(10) C5 0.0431(14) 0.0384(13) 0.0308(12) 0.0017(10) 0.0036(10) -0.0047(11) C6 0.0329(12) 0.0225(11) 0.0326(12) -0.0089(9) 0.0051(9) 0.0002(9) C7 0.0359(12) 0.0246(11) 0.0426(14) -0.0023(10) 0.0013(10) 0.0001(9) C8 0.0470(15) 0.0273(12) 0.0569(17) 0.0050(11) 0.0000(12) -0.0012(11) C9 0.0500(16) 0.0261(13) 0.0692(19) 0.0030(12) 0.0080(14) -0.0085(11) C10 0.0366(13) 0.0308(13) 0.0614(17) -0.0105(12) 0.0058(12) -0.0084(10) C11 0.0337(12) 0.0269(11) 0.0397(13) -0.0116(10) 0.0037(10) -0.0022(9) C12 0.0383(14) 0.0315(13) 0.0560(16) 0.0085(11) -0.0099(12) -0.0030(10) C13 0.074(2) 0.063(2) 0.0568(19) 0.0107(15) -0.0217(16) -0.0234(17) C14 0.0414(16) 0.0465(17) 0.112(3) 0.0116(18) -0.0076(17) 0.0065(13) C15 0.0339(13) 0.0355(13) 0.0536(16) -0.0066(11) -0.0034(11) -0.0061(10) C16 0.071(2) 0.153(4) 0.045(2) -0.013(2) -0.0049(17) 0.028(3) C17 0.0437(18) 0.113(3) 0.070(2) -0.003(2) 0.0018(16) 0.0203(19) C18 0.0323(11) 0.0257(11) 0.0238(11) 0.0013(8) 0.0003(9) -0.0006(9) C19 0.0355(12) 0.0286(12) 0.0320(12) -0.0010(9) -0.0038(10) -0.0023(9) C20 0.0486(15) 0.0260(12) 0.0427(14) -0.0037(10) -0.0081(11) -0.0013(10) C21 0.0479(15) 0.0279(12) 0.0509(16) -0.0007(11) -0.0092(12) 0.0079(11) C22 0.0373(13) 0.0375(13) 0.0439(14) 0.0032(11) -0.0105(11) 0.0026(10) C23 0.0363(12) 0.0312(12) 0.0308(12) 0.0012(9) -0.0059(10) -0.0030(10) C24 0.0388(13) 0.0261(12) 0.0467(14) -0.0030(10) -0.0095(11) -0.0024(10) C25 0.0485(15) 0.0411(14) 0.0486(16) -0.0051(12) -0.0173(12) -0.0018(12) C26 0.0431(15) 0.0498(16) 0.0657(19) 0.0003(14) -0.0084(13) -0.0127(13) C27 0.0415(14) 0.0324(13) 0.0553(16) 0.0022(11) -0.0194(12) -0.0042(11) C28 0.0565(19) 0.080(2) 0.071(2) -0.0131(18) 0.0015(16) -0.0329(17) C29 0.0514(17) 0.064(2) 0.080(2) -0.0409(18) -0.0057(16) -0.0023(15) C30 0.0246(10) 0.0326(12) 0.0276(11) -0.0078(9) 0.0000(8) -0.0056(9) C31 0.0307(11) 0.0352(12) 0.0273(11) -0.0055(9) -0.0009(9) -0.0053(9) C32 0.0467(14) 0.0415(14) 0.0274(12) -0.0021(10) 0.0012(10) -0.0096(11) C33 0.0561(16) 0.0533(16) 0.0272(13) -0.0120(11) 0.0129(11) -0.0088(13) C34 0.0452(14) 0.0411(14) 0.0360(13) -0.0163(11) 0.0092(11) -0.0023(11) C35 0.0304(11) 0.0347(12) 0.0311(12) -0.0093(10) 0.0013(9) -0.0039(9) C36 0.0394(13) 0.0359(13) 0.0325(13) 0.0040(10) 0.0043(10) -0.0006(10) C37 0.0576(18) 0.0507(17) 0.0511(17) 0.0157(13) 0.0052(14) 0.0103(14) C38 0.0602(17) 0.0390(14) 0.0511(17) -0.0134(12) 0.0114(13) -0.0058(12) C39 0.0339(12) 0.0335(12) 0.0408(14) -0.0081(10) 0.0079(10) -0.0019(10) C40 0.0528(16) 0.0481(16) 0.0492(17) 0.0001(13) -0.0063(13) 0.0032(13) C41 0.0577(17) 0.0374(15) 0.0626(19) -0.0138(13) 0.0128(14) 0.0006(12) C42 0.0578(17) 0.0543(17) 0.0346(14) -0.0026(12) -0.0147(12) -0.0128(13) C45 0.0297(13) 0.076(2) 0.0545(17) -0.0069(15) 0.0037(12) -0.0033(13) C42A 0.0578(17) 0.0543(17) 0.0346(14) -0.0026(12) -0.0147(12) -0.0128(13) C45A 0.0297(13) 0.076(2) 0.0545(17) -0.0069(15) 0.0037(12) -0.0033(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 Ca N3 2.2758(18) . ? Ca O 2.3139(16) . ? Ca N2 2.3384(18) . ? Ca N1 2.3798(18) . ? O C45 1.449(3) . ? O C42 1.454(3) . ? N1 C1 1.326(3) . ? N1 C6 1.431(3) . ? N2 C3 1.327(3) . ? N2 C18 1.435(3) . ? N3 C30 1.373(3) . ? C1 C2 1.411(3) . ? C1 C4 1.521(3) . ? C2 C3 1.408(3) . ? C3 C5 1.516(3) . ? C6 C7 1.411(3) . ? C6 C11 1.410(3) . ? C7 C8 1.390(3) . ? C7 C12 1.522(3) . ? C8 C9 1.375(4) . ? C9 C10 1.381(4) . ? C10 C11 1.391(3) . ? C11 C15 1.521(3) . ? C12 C14 1.530(4) . ? C12 C13 1.534(4) . ? C15 C16 1.481(4) . ? C15 C17 1.527(4) . ? C18 C19 1.408(3) . ? C18 C23 1.412(3) . ? C19 C20 1.397(3) . ? C19 C24 1.516(3) . ? C20 C21 1.378(4) . ? C21 C22 1.381(4) . ? C22 C23 1.393(3) . ? C23 C27 1.517(3) . ? C24 C25 1.529(4) . ? C24 C26 1.534(4) . ? C27 C29 1.530(4) . ? C27 C28 1.532(4) . ? C30 C31 1.430(3) . ? C30 C35 1.436(3) . ? C31 C32 1.393(3) . ? C31 C36 1.511(3) . ? C32 C33 1.382(4) . ? C33 C34 1.382(4) . ? C34 C35 1.391(3) . ? C35 C39 1.523(3) . ? C36 C38 1.530(4) . ? C36 C37 1.533(3) . ? C39 C40 1.526(4) . ? C39 C41 1.530(3) . ? C42 C43 1.618(7) . ? C43 C44 1.534(8) . ? C44 C45 1.425(6) . ? C43A C44A 1.614(12) . ? C1S C2S 1.542(11) . ? C2S C4S 1.341(13) 2_565 ? C2S C3S 1.470(13) . ? C3S C4S 1.471(15) . ? C4S C2S 1.341(13) 2_565 ? 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 N3 Ca O 105.00(7) . . ? N3 Ca N2 106.61(6) . . ? O Ca N2 101.73(6) . . ? N3 Ca N1 153.36(7) . . ? O Ca N1 98.20(6) . . ? N2 Ca N1 80.80(6) . . ? C45 O C42 108.7(2) . . ? C45 O Ca 124.44(15) . . ? C42 O Ca 126.36(15) . . ? C1 N1 C6 120.40(17) . . ? C1 N1 Ca 122.10(14) . . ? C6 N1 Ca 116.47(13) . . ? C3 N2 C18 119.74(18) . . ? C3 N2 Ca 123.06(14) . . ? C18 N2 Ca 116.25(13) . . ? C30 N3 Ca 143.00(15) . . ? N1 C1 C2 124.77(19) . . ? N1 C1 C4 120.6(2) . . ? C2 C1 C4 114.60(19) . . ? C3 C2 C1 131.1(2) . . ? N2 C3 C2 124.4(2) . . ? N2 C3 C5 120.7(2) . . ? C2 C3 C5 114.9(2) . . ? C7 C6 C11 120.0(2) . . ? C7 C6 N1 121.4(2) . . ? C11 C6 N1 118.31(19) . . ? C8 C7 C6 118.7(2) . . ? C8 C7 C12 118.6(2) . . ? C6 C7 C12 122.7(2) . . ? C9 C8 C7 121.6(2) . . ? C8 C9 C10 119.7(2) . . ? C9 C10 C11 121.2(2) . . ? C10 C11 C6 118.9(2) . . ? C10 C11 C15 120.6(2) . . ? C6 C11 C15 120.5(2) . . ? C7 C12 C14 111.5(2) . . ? C7 C12 C13 110.6(2) . . ? C14 C12 C13 110.9(3) . . ? C16 C15 C11 111.8(2) . . ? C16 C15 C17 110.2(3) . . ? C11 C15 C17 113.4(2) . . ? C19 C18 C23 120.3(2) . . ? C19 C18 N2 121.32(19) . . ? C23 C18 N2 118.18(19) . . ? C20 C19 C18 118.7(2) . . ? C20 C19 C24 118.9(2) . . ? C18 C19 C24 122.4(2) . . ? C21 C20 C19 121.1(2) . . ? C20 C21 C22 120.1(2) . . ? C21 C22 C23 121.1(2) . . ? C22 C23 C18 118.7(2) . . ? C22 C23 C27 120.3(2) . . ? C18 C23 C27 121.0(2) . . ? C19 C24 C25 110.2(2) . . ? C19 C24 C26 112.8(2) . . ? C25 C24 C26 110.4(2) . . ? C23 C27 C29 110.7(2) . . ? C23 C27 C28 113.5(2) . . ? C29 C27 C28 109.1(2) . . ? N3 C30 C31 118.83(19) . . ? N3 C30 C35 123.5(2) . . ? C31 C30 C35 117.6(2) . . ? C32 C31 C30 119.8(2) . . ? C32 C31 C36 121.1(2) . . ? C30 C31 C36 119.1(2) . . ? C33 C32 C31 122.0(2) . . ? C34 C33 C32 118.6(2) . . ? C33 C34 C35 122.4(2) . . ? C34 C35 C30 119.4(2) . . ? C34 C35 C39 120.9(2) . . ? C30 C35 C39 119.7(2) . . ? C31 C36 C38 111.9(2) . . ? C31 C36 C37 114.4(2) . . ? C38 C36 C37 109.5(2) . . ? C35 C39 C40 112.5(2) . . ? C35 C39 C41 113.9(2) . . ? C40 C39 C41 108.6(2) . . ? O C42 C43 99.8(3) . . ? C44 C43 C42 100.5(4) . . ? C45 C44 C43 96.7(4) . . ? C44 C45 O 107.1(3) . . ? C4S C2S C3S 90.7(9) 2_565 . ? C4S C2S C1S 112.4(10) 2_565 . ? C3S C2S C1S 115.7(9) . . ? C2S C3S C4S 117.4(10) . . ? C2S C4S C3S 121.1(11) 2_565 . ? #===END