# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_768276-jul1607 _database_code_depnum_ccdc_archive 'CCDC 768276' #TrackingRef 'bigcif.cif' _audit_creation_date 2007-07-27T11:34:07-00:00 _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 'C46 H64 Ca N6 O2' _chemical_formula_sum 'C46 H64 Ca N6 O2' _chemical_formula_weight 773.11 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 20.9359(3) _cell_length_b 10.5703(2) _cell_length_c 21.4465(4) _cell_angle_alpha 90 _cell_angle_beta 107.570(1) _cell_angle_gamma 90 _cell_volume 4524.67(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18987 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.18 _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 0.9327 _exptl_absorpt_correction_T_max 0.9736 #----------------------------------------------------------------------------# # 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 0.160243E-1 _diffrn_orient_matrix_ub_12 -0.594876E-1 _diffrn_orient_matrix_ub_13 -0.283248E-1 _diffrn_orient_matrix_ub_21 -0.468986E-1 _diffrn_orient_matrix_ub_22 -0.307913E-1 _diffrn_orient_matrix_ub_23 -0.200523E-1 _diffrn_orient_matrix_ub_31 -0.73469E-2 _diffrn_orient_matrix_ub_32 0.668069E-1 _diffrn_orient_matrix_ub_33 -0.344636E-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 0.0322 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_number 31099 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 8671 _reflns_number_gt 7363 _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 lower occupancy site for the disordered C45 atom was 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^)+(0.0569P)^2^+2.7578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8671 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.533 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # 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 0.511255(15) 0.48867(3) 0.212382(14) 0.02294(10) Uani 1 1 d . B . O1 O 0.59792(7) 0.49791(13) 0.15807(7) 0.0457(4) Uani 1 1 d . . . O2 O 0.46730(6) 0.32987(12) 0.12800(6) 0.0357(3) Uani 1 1 d . . . N1 N 0.58936(7) 0.55934(13) 0.31277(7) 0.0292(3) Uani 1 1 d . . . N2 N 0.57541(7) 0.34606(13) 0.29814(7) 0.0315(3) Uani 1 1 d . . . N3 N 0.65426(7) 0.42245(15) 0.39799(6) 0.0309(3) Uani 1 1 d . . . N4 N 0.44858(7) 0.66944(13) 0.15551(7) 0.0284(3) Uani 1 1 d . . . N5 N 0.39672(7) 0.53701(13) 0.20828(7) 0.0292(3) Uani 1 1 d . . . N6 N 0.33638(7) 0.72299(13) 0.15628(7) 0.0290(3) Uani 1 1 d . . . C1 C 0.60462(8) 0.44292(16) 0.33462(8) 0.0266(3) Uani 1 1 d . B . C2 C 0.60877(9) 0.66892(17) 0.35604(8) 0.0329(4) Uani 1 1 d . B . H2 H 0.631 0.6385 0.4016 0.039 Uiso 1 1 calc R . . C3 C 0.54625(10) 0.74272(19) 0.35506(11) 0.0449(5) Uani 1 1 d . . . H3A H 0.5236 0.7715 0.3104 0.067 Uiso 1 1 calc R B . H3B H 0.5588 0.8161 0.3841 0.067 Uiso 1 1 calc R . . H3C H 0.516 0.6882 0.3701 0.067 Uiso 1 1 calc R . . C4 C 0.65726(10) 0.7536(2) 0.33495(11) 0.0466(5) Uani 1 1 d . . . H4A H 0.6977 0.7055 0.3365 0.07 Uiso 1 1 calc R B . H4B H 0.6693 0.8263 0.3645 0.07 Uiso 1 1 calc R . . H4C H 0.636 0.7834 0.2902 0.07 Uiso 1 1 calc R . . C5 C 0.59649(10) 0.21620(17) 0.31631(9) 0.0393(4) Uani 1 1 d . B . H5 H 0.6367 0.2175 0.356 0.047 Uiso 1 1 calc R . . C6 C 0.61527(11) 0.1522(2) 0.26063(11) 0.0524(5) Uani 1 1 d . . . H6A H 0.5775 0.1577 0.2204 0.079 Uiso 1 1 calc R B . H6B H 0.626 0.0632 0.2716 0.079 Uiso 1 1 calc R . . H6C H 0.6544 0.1947 0.2541 0.079 Uiso 1 1 calc R . . C7 C 0.54069(13) 0.1429(2) 0.33196(12) 0.0574(6) Uani 1 1 d . . . H7A H 0.5297 0.1837 0.3685 0.086 Uiso 1 1 calc R B . H7B H 0.5555 0.0559 0.3441 0.086 Uiso 1 1 calc R . . H7C H 0.5009 0.1419 0.2935 0.086 Uiso 1 1 calc R . . C8 C 0.72088(8) 0.45718(17) 0.40375(8) 0.0324(4) Uani 1 1 d . B . C9 C 0.74751(9) 0.42873(19) 0.35351(10) 0.0406(4) Uani 1 1 d . . . H9 H 0.7215 0.3824 0.3166 0.049 Uiso 1 1 calc R B . C10 C 0.81186(11) 0.4674(2) 0.35667(12) 0.0526(5) Uani 1 1 d . B . H10 H 0.8295 0.4477 0.3219 0.063 Uiso 1 1 calc R . . C11 C 0.85004(11) 0.5340(3) 0.40990(13) 0.0605(7) Uani 1 1 d . . . H11 H 0.8941 0.56 0.4122 0.073 Uiso 1 1 calc R B . C12 C 0.82387(11) 0.5628(3) 0.45996(12) 0.0620(7) Uani 1 1 d . B . H12 H 0.8501 0.6095 0.4966 0.074 Uiso 1 1 calc R . . C13 C 0.75998(10) 0.5246(2) 0.45754(10) 0.0475(5) Uani 1 1 d . . . H13 H 0.7428 0.5444 0.4926 0.057 Uiso 1 1 calc R B . C14 C 0.63388(9) 0.37714(17) 0.45062(8) 0.0322(4) Uani 1 1 d . B . C15 C 0.56838(10) 0.39644(19) 0.45168(9) 0.0406(4) Uani 1 1 d . . . H15 H 0.5382 0.4445 0.418 0.049 Uiso 1 1 calc R B . C16 C 0.54695(12) 0.3458(2) 0.50167(11) 0.0524(5) Uani 1 1 d . B . H16 H 0.502 0.3584 0.5016 0.063 Uiso 1 1 calc R . . C17 C 0.59030(13) 0.2775(2) 0.55132(11) 0.0554(6) Uani 1 1 d . . . H17 H 0.5754 0.2431 0.5854 0.067 Uiso 1 1 calc R B . C18 C 0.65560(12) 0.2593(2) 0.55121(10) 0.0528(5) Uani 1 1 d . B . H18 H 0.6857 0.213 0.5857 0.063 Uiso 1 1 calc R . . C19 C 0.67753(10) 0.3080(2) 0.50115(9) 0.0424(5) Uani 1 1 d . . . H19 H 0.7224 0.2943 0.5013 0.051 Uiso 1 1 calc R B . C20 C 0.39539(8) 0.64103(15) 0.17401(8) 0.0252(3) Uani 1 1 d . B . C21 C 0.45088(9) 0.78119(17) 0.11666(9) 0.0338(4) Uani 1 1 d . B . H21 H 0.4054 0.8208 0.102 0.041 Uiso 1 1 calc R . . C22 C 0.47098(11) 0.7419(2) 0.05671(9) 0.0458(5) Uani 1 1 d . . . H22A H 0.5137 0.6962 0.0707 0.069 Uiso 1 1 calc R B . H22B H 0.4759 0.8175 0.032 0.069 Uiso 1 1 calc R . . H22C H 0.4363 0.6869 0.0289 0.069 Uiso 1 1 calc R . . C23 C 0.50090(12) 0.87656(19) 0.15725(11) 0.0490(5) Uani 1 1 d . . . H23A H 0.4855 0.9064 0.1936 0.074 Uiso 1 1 calc R B . H23B H 0.5045 0.9485 0.1297 0.074 Uiso 1 1 calc R . . H23C H 0.5448 0.8361 0.1746 0.074 Uiso 1 1 calc R . . C24 C 0.34559(8) 0.51090(16) 0.24049(9) 0.0306(4) Uani 1 1 d . B . H24 H 0.3196 0.59 0.241 0.037 Uiso 1 1 calc R . . C25 C 0.38117(10) 0.4712(2) 0.31080(10) 0.0456(5) Uani 1 1 d . . . H25A H 0.4063 0.3929 0.3108 0.068 Uiso 1 1 calc R B . H25B H 0.348 0.457 0.3339 0.068 Uiso 1 1 calc R . . H25C H 0.4122 0.5382 0.3329 0.068 Uiso 1 1 calc R . . C26 C 0.29760(9) 0.40777(18) 0.20510(10) 0.0396(4) Uani 1 1 d . . . H26A H 0.2733 0.4365 0.1609 0.059 Uiso 1 1 calc R B . H26B H 0.2656 0.3893 0.2292 0.059 Uiso 1 1 calc R . . H26C H 0.323 0.3311 0.2025 0.059 Uiso 1 1 calc R . . C27 C 0.33810(8) 0.83677(15) 0.19102(8) 0.0272(3) Uani 1 1 d . B . C28 C 0.37899(8) 0.84576(17) 0.25559(9) 0.0328(4) Uani 1 1 d . . . H28 H 0.404 0.7743 0.2764 0.039 Uiso 1 1 calc R B . C29 C 0.38328(10) 0.95852(18) 0.28948(10) 0.0392(4) Uani 1 1 d . B . H29 H 0.412 0.9643 0.3332 0.047 Uiso 1 1 calc R . . C30 C 0.34625(10) 1.06263(18) 0.26049(10) 0.0417(5) Uani 1 1 d . . . H30 H 0.3491 1.1396 0.284 0.05 Uiso 1 1 calc R B . C31 C 0.30500(10) 1.05326(18) 0.19679(10) 0.0404(4) Uani 1 1 d . B . H31 H 0.2789 1.1241 0.1767 0.048 Uiso 1 1 calc R . . C32 C 0.30130(9) 0.94228(17) 0.16192(9) 0.0336(4) Uani 1 1 d . . . H32 H 0.2735 0.9379 0.1178 0.04 Uiso 1 1 calc R B . C33 C 0.27817(8) 0.67955(16) 0.10832(8) 0.0288(4) Uani 1 1 d . B . C34 C 0.21436(9) 0.70732(19) 0.11187(10) 0.0384(4) Uani 1 1 d . . . H34 H 0.2092 0.7594 0.1461 0.046 Uiso 1 1 calc R B . C35 C 0.15831(10) 0.6591(2) 0.06549(12) 0.0531(6) Uani 1 1 d . B . H35 H 0.115 0.6796 0.068 0.064 Uiso 1 1 calc R . . C36 C 0.16445(11) 0.5819(2) 0.01578(11) 0.0553(6) Uani 1 1 d . . . H36 H 0.1258 0.5479 -0.0153 0.066 Uiso 1 1 calc R B . C37 C 0.22734(11) 0.5550(2) 0.01206(10) 0.0514(5) Uani 1 1 d . B . H37 H 0.2322 0.5018 -0.0219 0.062 Uiso 1 1 calc R . . C38 C 0.28385(10) 0.6044(2) 0.05722(9) 0.0417(4) Uani 1 1 d . . . H38 H 0.3269 0.5867 0.0532 0.05 Uiso 1 1 calc R B . C39 C 0.61625(16) 0.4002(3) 0.12163(18) 0.0958(12) Uani 1 1 d . . . H39A H 0.6198 0.3194 0.1458 0.115 Uiso 1 1 calc R . . H39B H 0.5809 0.3905 0.0792 0.115 Uiso 1 1 calc R . . C40 C 0.67585(16) 0.4254(4) 0.1106(3) 0.1228(17) Uani 1 1 d . . . H40A H 0.6684 0.4449 0.0638 0.147 Uiso 1 1 calc R . . H40B H 0.7058 0.3509 0.1223 0.147 Uiso 1 1 calc R . . C41 C 0.70613(13) 0.5335(4) 0.15093(17) 0.0893(10) Uani 1 1 d . . . H41A H 0.7209 0.5976 0.1245 0.107 Uiso 1 1 calc R . . H41B H 0.7453 0.5066 0.1875 0.107 Uiso 1 1 calc R . . C42 C 0.65263(12) 0.5859(3) 0.17624(14) 0.0645(7) Uani 1 1 d . . . H42A H 0.6693 0.595 0.2244 0.077 Uiso 1 1 calc R . . H42B H 0.6381 0.6699 0.1568 0.077 Uiso 1 1 calc R . . C43 C 0.43543(13) 0.3701(2) 0.06187(10) 0.0573(6) Uani 1 1 d . B . H43A H 0.4684 0.3728 0.0371 0.069 Uiso 1 1 calc R A 1 H43B H 0.416 0.4556 0.0614 0.069 Uiso 1 1 calc R A 1 C44 C 0.38207(17) 0.2773(3) 0.03219(14) 0.0942(11) Uani 0.635(11) 1 d P B 1 H44A H 0.3418 0.3207 0.0039 0.113 Uiso 0.635(11) 1 calc PR B 1 H44B H 0.3977 0.2153 0.0054 0.113 Uiso 0.635(11) 1 calc PR B 1 C45 C 0.3675(3) 0.2172(8) 0.08369(19) 0.082(3) Uani 0.635(11) 1 d P B 1 H45A H 0.354 0.1284 0.0721 0.099 Uiso 0.635(11) 1 calc PR B 1 H45B H 0.3305 0.2611 0.0946 0.099 Uiso 0.635(11) 1 calc PR B 1 C46 C 0.43164(12) 0.2221(2) 0.14181(11) 0.0535(6) Uani 0.635(11) 1 d P B 1 H46A H 0.4211 0.2337 0.1834 0.064 Uiso 0.635(11) 1 calc PR B 1 H46B H 0.4582 0.1436 0.1445 0.064 Uiso 0.635(11) 1 calc PR B 1 C44A C 0.38207(17) 0.2773(3) 0.03219(14) 0.0942(11) Uani 0.365(11) 1 d P B 2 H44C H 0.3375 0.3128 0.0294 0.113 Uiso 0.365(11) 1 calc PR B 2 H44D H 0.3827 0.2543 -0.0124 0.113 Uiso 0.365(11) 1 calc PR B 2 C45A C 0.3964(4) 0.1660(7) 0.0754(4) 0.049(2) Uiso 0.365(11) 1 d P B 2 H45C H 0.4258 0.1054 0.0619 0.059 Uiso 0.365(11) 1 calc PR B 2 H45D H 0.3546 0.1225 0.0755 0.059 Uiso 0.365(11) 1 calc PR B 2 C46A C 0.43164(12) 0.2221(2) 0.14181(11) 0.0535(6) Uani 0.365(11) 1 d P B 2 H46C H 0.3989 0.2484 0.1643 0.064 Uiso 0.365(11) 1 calc PR B 2 H46D H 0.463 0.1602 0.1697 0.064 Uiso 0.365(11) 1 calc PR B 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 0.02055(16) 0.02352(18) 0.02305(16) -0.00206(12) 0.00405(12) 0.00116(12) O1 0.0404(7) 0.0498(9) 0.0557(8) -0.0155(7) 0.0275(7) -0.0087(6) O2 0.0357(6) 0.0356(7) 0.0336(6) -0.0089(5) 0.0069(5) -0.0049(5) N1 0.0301(7) 0.0247(7) 0.0269(7) -0.0023(6) -0.0004(6) -0.0021(6) N2 0.0303(7) 0.0242(7) 0.0333(7) 0.0015(6) -0.0008(6) 0.0011(6) N3 0.0243(7) 0.0402(8) 0.0237(7) 0.0044(6) 0.0007(5) -0.0002(6) N4 0.0261(7) 0.0287(7) 0.0308(7) 0.0049(6) 0.0091(6) 0.0041(6) N5 0.0241(7) 0.0258(7) 0.0395(8) 0.0022(6) 0.0124(6) 0.0017(6) N6 0.0232(7) 0.0272(7) 0.0345(7) -0.0035(6) 0.0054(6) 0.0046(6) C1 0.0219(7) 0.0308(9) 0.0237(8) 0.0014(7) 0.0021(6) 0.0002(7) C2 0.0321(9) 0.0307(9) 0.0305(8) -0.0055(7) 0.0012(7) -0.0030(7) C3 0.0408(10) 0.0355(11) 0.0554(12) -0.0105(9) 0.0102(9) 0.0008(9) C4 0.0458(11) 0.0391(11) 0.0537(12) -0.0134(9) 0.0129(9) -0.0143(9) C5 0.0391(10) 0.0268(9) 0.0424(10) 0.0023(8) -0.0022(8) 0.0034(8) C6 0.0522(12) 0.0371(11) 0.0611(13) -0.0057(10) 0.0070(10) 0.0114(10) C7 0.0704(15) 0.0331(11) 0.0665(15) 0.0078(10) 0.0174(12) -0.0085(11) C8 0.0247(8) 0.0361(10) 0.0307(8) 0.0064(7) -0.0001(7) 0.0007(7) C9 0.0325(9) 0.0441(11) 0.0431(10) 0.0004(9) 0.0084(8) 0.0005(8) C10 0.0373(11) 0.0602(14) 0.0634(14) 0.0096(11) 0.0201(10) 0.0024(10) C11 0.0297(10) 0.0752(17) 0.0703(16) 0.0175(13) 0.0056(10) -0.0101(11) C12 0.0417(12) 0.0789(18) 0.0500(13) 0.0063(12) -0.0093(10) -0.0214(12) C13 0.0395(11) 0.0619(14) 0.0326(10) 0.0003(9) -0.0016(8) -0.0101(10) C14 0.0356(9) 0.0309(9) 0.0283(8) 0.0019(7) 0.0068(7) 0.0024(8) C15 0.0399(10) 0.0432(11) 0.0401(10) 0.0076(8) 0.0141(8) 0.0110(9) C16 0.0558(13) 0.0549(13) 0.0571(13) 0.0081(11) 0.0330(11) 0.0114(11) C17 0.0770(16) 0.0528(13) 0.0469(12) 0.0130(10) 0.0345(11) 0.0095(12) C18 0.0660(14) 0.0523(13) 0.0376(10) 0.0157(10) 0.0120(10) 0.0118(11) C19 0.0409(10) 0.0464(11) 0.0364(10) 0.0105(9) 0.0065(8) 0.0092(9) C20 0.0222(7) 0.0240(8) 0.0276(8) -0.0044(6) 0.0050(6) 0.0031(6) C21 0.0369(9) 0.0328(9) 0.0351(9) 0.0097(7) 0.0158(7) 0.0095(8) C22 0.0549(12) 0.0503(12) 0.0376(10) 0.0100(9) 0.0222(9) 0.0103(10) C23 0.0658(14) 0.0325(10) 0.0557(12) 0.0023(9) 0.0289(11) -0.0070(10) C24 0.0267(8) 0.0251(9) 0.0433(10) -0.0006(7) 0.0155(7) -0.0007(7) C25 0.0420(11) 0.0530(12) 0.0443(11) 0.0043(9) 0.0169(9) -0.0109(10) C26 0.0342(9) 0.0301(9) 0.0556(12) -0.0032(8) 0.0154(8) -0.0049(8) C27 0.0252(8) 0.0244(8) 0.0347(8) -0.0006(7) 0.0133(7) 0.0001(7) C28 0.0303(9) 0.0311(9) 0.0368(9) -0.0012(7) 0.0099(7) 0.0017(7) C29 0.0396(10) 0.0378(10) 0.0407(10) -0.0081(8) 0.0128(8) -0.0059(8) C30 0.0488(11) 0.0278(10) 0.0555(12) -0.0091(9) 0.0263(10) -0.0039(9) C31 0.0446(11) 0.0253(9) 0.0551(12) 0.0044(8) 0.0210(9) 0.0039(8) C32 0.0353(9) 0.0290(9) 0.0381(9) 0.0037(7) 0.0139(8) 0.0022(8) C33 0.0269(8) 0.0276(9) 0.0290(8) 0.0029(7) 0.0043(6) 0.0025(7) C34 0.0284(9) 0.0389(10) 0.0467(10) 0.0019(8) 0.0095(8) 0.0036(8) C35 0.0273(9) 0.0582(14) 0.0654(14) 0.0049(11) 0.0011(9) 0.0028(9) C36 0.0409(11) 0.0636(15) 0.0462(12) 0.0023(11) -0.0095(9) -0.0084(11) C37 0.0544(13) 0.0601(14) 0.0334(10) -0.0079(9) 0.0038(9) -0.0058(11) C38 0.0363(10) 0.0499(12) 0.0374(10) -0.0073(9) 0.0086(8) 0.0000(9) C39 0.088(2) 0.101(2) 0.132(3) -0.071(2) 0.084(2) -0.0394(18) C40 0.070(2) 0.111(3) 0.219(5) -0.084(3) 0.090(3) -0.027(2) C41 0.0423(13) 0.130(3) 0.101(2) -0.037(2) 0.0301(15) -0.0211(16) C42 0.0579(14) 0.0698(16) 0.0763(16) -0.0285(14) 0.0364(13) -0.0265(13) C43 0.0681(15) 0.0583(14) 0.0383(11) -0.0031(10) 0.0051(10) -0.0105(12) C44 0.093(2) 0.101(2) 0.0602(17) 0.0005(16) -0.0195(15) -0.043(2) C45 0.058(3) 0.141(6) 0.044(2) -0.026(3) 0.0109(19) -0.060(4) C46 0.0579(13) 0.0426(12) 0.0523(12) -0.0030(10) 0.0052(10) -0.0152(10) C44A 0.093(2) 0.101(2) 0.0602(17) 0.0005(16) -0.0195(15) -0.043(2) C46A 0.0579(13) 0.0426(12) 0.0523(12) -0.0030(10) 0.0052(10) -0.0152(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 Ca N1 2.3962(13) . ? Ca N5 2.4272(13) . ? Ca N4 2.4278(14) . ? Ca O2 2.4359(12) . ? Ca O1 2.4360(13) . ? Ca N2 2.4428(14) . ? O1 C39 1.416(3) . ? O1 C42 1.435(3) . ? O2 C43 1.438(2) . ? O2 C46 1.441(2) . ? N1 C1 1.321(2) . ? N1 C2 1.463(2) . ? N2 C1 1.321(2) . ? N2 C5 1.458(2) . ? N3 C14 1.406(2) . ? N3 C8 1.411(2) . ? N3 C1 1.4564(19) . ? N4 C20 1.325(2) . ? N4 C21 1.455(2) . ? N5 C20 1.318(2) . ? N5 C24 1.465(2) . ? N6 C27 1.409(2) . ? N6 C33 1.413(2) . ? N6 C20 1.462(2) . ? C2 C3 1.519(3) . ? C2 C4 1.521(3) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C7 1.521(3) . ? C5 C6 1.524(3) . ? C5 H5 1 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.387(3) . ? C8 C13 1.392(3) . ? C9 C10 1.390(3) . ? C9 H9 0.95 . ? C10 C11 1.374(4) . ? C10 H10 0.95 . ? C11 C12 1.379(4) . ? C11 H11 0.95 . ? C12 C13 1.383(3) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 C15 1.393(3) . ? C14 C19 1.395(2) . ? C15 C16 1.388(3) . ? C15 H15 0.95 . ? C16 C17 1.377(3) . ? C16 H16 0.95 . ? C17 C18 1.381(3) . ? C17 H17 0.95 . ? C18 C19 1.388(3) . ? C18 H18 0.95 . ? C19 H19 0.95 . ? C21 C23 1.523(3) . ? C21 C22 1.526(2) . ? C21 H21 1 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C26 1.521(2) . ? C24 C25 1.525(3) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C32 1.392(2) . ? C27 C28 1.394(2) . ? C28 C29 1.385(3) . ? C28 H28 0.95 . ? C29 C30 1.381(3) . ? C29 H29 0.95 . ? C30 C31 1.382(3) . ? C30 H30 0.95 . ? C31 C32 1.381(3) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? C33 C38 1.388(3) . ? C33 C34 1.392(2) . ? C34 C35 1.386(3) . ? C34 H34 0.95 . ? C35 C36 1.379(3) . ? C35 H35 0.95 . ? C36 C37 1.373(3) . ? C36 H36 0.95 . ? C37 C38 1.385(3) . ? C37 H37 0.95 . ? C38 H38 0.95 . ? C39 C40 1.364(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 C41 1.458(4) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 C42 1.491(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.478(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.386(5) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 C46 1.532(5) . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C45A H45C 0.99 . ? C45A H45D 0.99 . ? 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 Ca N5 111.45(5) . . ? N1 Ca N4 108.95(5) . . ? N5 Ca N4 55.80(5) . . ? N1 Ca O2 152.20(5) . . ? N5 Ca O2 88.32(5) . . ? N4 Ca O2 98.25(5) . . ? N1 Ca O1 90.71(5) . . ? N5 Ca O1 147.62(5) . . ? N4 Ca O1 95.50(5) . . ? O2 Ca O1 80.87(4) . . ? N1 Ca N2 56.28(5) . . ? N5 Ca N2 118.02(5) . . ? N4 Ca N2 162.72(5) . . ? O2 Ca N2 97.62(5) . . ? O1 Ca N2 93.74(5) . . ? C39 O1 C42 107.17(17) . . ? C39 O1 Ca 126.85(14) . . ? C42 O1 Ca 123.01(12) . . ? C43 O2 C46 108.76(15) . . ? C43 O2 Ca 119.21(12) . . ? C46 O2 Ca 119.68(11) . . ? C1 N1 C2 121.42(13) . . ? C1 N1 Ca 93.14(10) . . ? C2 N1 Ca 143.16(11) . . ? C1 N2 C5 121.50(14) . . ? C1 N2 Ca 91.07(10) . . ? C5 N2 Ca 146.64(11) . . ? C14 N3 C8 123.35(13) . . ? C14 N3 C1 119.73(13) . . ? C8 N3 C1 116.81(13) . . ? C20 N4 C21 122.14(14) . . ? C20 N4 Ca 92.69(10) . . ? C21 N4 Ca 145.13(11) . . ? C20 N5 C24 121.64(14) . . ? C20 N5 Ca 92.88(10) . . ? C24 N5 Ca 142.93(11) . . ? C27 N6 C33 122.73(13) . . ? C27 N6 C20 118.90(13) . . ? C33 N6 C20 118.17(13) . . ? N1 C1 N2 119.51(14) . . ? N1 C1 N3 119.83(14) . . ? N2 C1 N3 120.65(15) . . ? N1 C2 C3 108.95(14) . . ? N1 C2 C4 111.08(15) . . ? C3 C2 C4 110.10(17) . . ? N1 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C4 C2 H2 108.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C7 110.35(16) . . ? N2 C5 C6 109.70(16) . . ? C7 C5 C6 110.12(18) . . ? N2 C5 H5 108.9 . . ? C7 C5 H5 108.9 . . ? C6 C5 H5 108.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.74(17) . . ? C9 C8 N3 119.60(16) . . ? C13 C8 N3 121.60(17) . . ? C8 C9 C10 120.62(19) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.5(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 120.9(2) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 120.0(2) . . ? C12 C13 H13 120 . . ? C8 C13 H13 120 . . ? C15 C14 C19 118.77(17) . . ? C15 C14 N3 120.14(15) . . ? C19 C14 N3 121.04(16) . . ? C16 C15 C14 120.35(18) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.6(2) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 120.56(19) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.21(19) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? N5 C20 N4 118.55(14) . . ? N5 C20 N6 120.89(14) . . ? N4 C20 N6 120.56(14) . . ? N4 C21 C23 110.24(15) . . ? N4 C21 C22 109.09(15) . . ? C23 C21 C22 110.16(16) . . ? N4 C21 H21 109.1 . . ? C23 C21 H21 109.1 . . ? C22 C21 H21 109.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C26 111.50(15) . . ? N5 C24 C25 108.04(14) . . ? C26 C24 C25 110.36(15) . . ? N5 C24 H24 109 . . ? C26 C24 H24 109 . . ? C25 C24 H24 109 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.79(16) . . ? C32 C27 N6 121.63(15) . . ? C28 C27 N6 119.56(15) . . ? C29 C28 C27 120.21(17) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.72(18) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.10(17) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 120.83(18) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 120.33(17) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 118.45(16) . . ? C38 C33 N6 120.01(15) . . ? C34 C33 N6 121.52(16) . . ? C35 C34 C33 120.12(19) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 121.1(2) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C37 C36 C35 118.85(19) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 120.9(2) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 120.61(19) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C40 C39 O1 111.6(2) . . ? C40 C39 H39A 109.3 . . ? O1 C39 H39A 109.3 . . ? C40 C39 H39B 109.3 . . ? O1 C39 H39B 109.3 . . ? H39A C39 H39B 108 . . ? C39 C40 C41 107.9(3) . . ? C39 C40 H40A 110.1 . . ? C41 C40 H40A 110.1 . . ? C39 C40 H40B 110.1 . . ? C41 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C40 C41 C42 105.5(2) . . ? C40 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? C40 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.8 . . ? O1 C42 C41 106.7(2) . . ? O1 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? O1 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? O2 C43 C44 107.1(2) . . ? O2 C43 H43A 110.3 . . ? C44 C43 H43A 110.3 . . ? O2 C43 H43B 110.3 . . ? C44 C43 H43B 110.3 . . ? H43A C43 H43B 108.5 . . ? C45 C44 C43 106.3(3) . . ? C45 C44 H44A 110.5 . . ? C43 C44 H44A 110.5 . . ? C45 C44 H44B 110.5 . . ? C43 C44 H44B 110.5 . . ? H44A C44 H44B 108.7 . . ? C44 C45 C46 106.5(3) . . ? C44 C45 H45A 110.4 . . ? C46 C45 H45A 110.4 . . ? C44 C45 H45B 110.4 . . ? C46 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? O2 C46 C45 103.9(3) . . ? O2 C46 H46A 111 . . ? C45 C46 H46A 111 . . ? O2 C46 H46B 111 . . ? C45 C46 H46B 111 . . ? H46A C46 H46B 109 . . ? H45C C45A H45D 109.1 . . ? data_768277 _database_code_depnum_ccdc_archive 'CCDC 768277' #TrackingRef '768277-80.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 N6 O2 Sr' _chemical_formula_weight 820.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 10.2465(3) _cell_length_b 17.1561(5) _cell_length_c 25.8067(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.401(2) _cell_angle_gamma 90.00 _cell_volume 4532.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51101 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.231 _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 0.7831 _exptl_absorpt_correction_T_max 0.925 _exptl_special_details ; ? ; _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_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35150 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.17 _reflns_number_total 8844 _reflns_number_gt 6576 _reflns_threshold_expression >2sigma(I) _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. C39-42 and C45 modelled as being disordered over 2 sites in a 55:45 ratio. C-C and O-C distances refined subject to distance restraints, and ADPs of all fractional atoms also refined subject to restraints. ; _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^)+(0.0306P)^2^+3.0594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8844 _refine_ls_number_parameters 551 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.76053(2) 0.731287(15) 0.386706(9) 0.02804(8) Uani 1 1 d . A . O1 O 0.9097(2) 0.61782(13) 0.36062(8) 0.0611(7) Uani 1 1 d D . . O2 O 0.9795(2) 0.80046(13) 0.40693(8) 0.0480(5) Uani 1 1 d . . . N1 N 0.5853(2) 0.68165(13) 0.32027(8) 0.0353(5) Uani 1 1 d . . . N2 N 0.7254(2) 0.77296(13) 0.29055(8) 0.0314(5) Uani 1 1 d . . . N3 N 0.5354(2) 0.73919(13) 0.23602(8) 0.0306(5) Uani 1 1 d . . . N4 N 0.7129(2) 0.69882(13) 0.48097(8) 0.0306(5) Uani 1 1 d . . . N5 N 0.6509(2) 0.82073(12) 0.45374(8) 0.0295(5) Uani 1 1 d . . . N6 N 0.5684(2) 0.77205(12) 0.53425(8) 0.0282(5) Uani 1 1 d . . . C1 C 0.6181(3) 0.73063(16) 0.28350(9) 0.0299(6) Uani 1 1 d . A . C2 C 0.4700(3) 0.63142(18) 0.31430(11) 0.0442(8) Uani 1 1 d . A . H2 H 0.4456 0.6258 0.2766 0.053 Uiso 1 1 calc R . . C3 C 0.3557(4) 0.6656(2) 0.34182(16) 0.0735(12) Uani 1 1 d . . . H3A H 0.3324 0.7162 0.3264 0.110 Uiso 1 1 calc R A . H3B H 0.3799 0.6726 0.3787 0.110 Uiso 1 1 calc R . . H3C H 0.2808 0.6303 0.3382 0.110 Uiso 1 1 calc R . . C4 C 0.5060(4) 0.5515(2) 0.33661(15) 0.0678(11) Uani 1 1 d . . . H4A H 0.5318 0.5568 0.3734 0.102 Uiso 1 1 calc R A . H4B H 0.5789 0.5298 0.3179 0.102 Uiso 1 1 calc R . . H4C H 0.4305 0.5166 0.3328 0.102 Uiso 1 1 calc R . . C5 C 0.7620(3) 0.83162(16) 0.25296(10) 0.0365(7) Uani 1 1 d . A . H5 H 0.6866 0.8404 0.2278 0.044 Uiso 1 1 calc R . . C6 C 0.8784(3) 0.8048(2) 0.22342(12) 0.0514(8) Uani 1 1 d . . . H6A H 0.8558 0.7570 0.2043 0.077 Uiso 1 1 calc R A . H6B H 0.9522 0.7944 0.2479 0.077 Uiso 1 1 calc R . . H6C H 0.9027 0.8455 0.1990 0.077 Uiso 1 1 calc R . . C7 C 0.7925(3) 0.90747(18) 0.28149(12) 0.0520(8) Uani 1 1 d . . . H7A H 0.8617 0.8984 0.3082 0.078 Uiso 1 1 calc R A . H7B H 0.7138 0.9263 0.2978 0.078 Uiso 1 1 calc R . . H7C H 0.8218 0.9466 0.2568 0.078 Uiso 1 1 calc R . . C8 C 0.5805(3) 0.70442(16) 0.19053(10) 0.0294(6) Uani 1 1 d . A . C9 C 0.6373(3) 0.63057(16) 0.19327(10) 0.0356(7) Uani 1 1 d . . . H9 H 0.6439 0.6040 0.2256 0.043 Uiso 1 1 calc R A . C10 C 0.6842(3) 0.59560(18) 0.14944(11) 0.0419(7) Uani 1 1 d . A . H10 H 0.7236 0.5456 0.1520 0.050 Uiso 1 1 calc R . . C11 C 0.6741(3) 0.63283(17) 0.10195(11) 0.0391(7) Uani 1 1 d . . . H11 H 0.7046 0.6083 0.0718 0.047 Uiso 1 1 calc R A . C12 C 0.6192(3) 0.70618(17) 0.09901(10) 0.0365(7) Uani 1 1 d . A . H12 H 0.6128 0.7324 0.0666 0.044 Uiso 1 1 calc R . . C13 C 0.5732(3) 0.74215(16) 0.14258(10) 0.0319(6) Uani 1 1 d . . . H13 H 0.5365 0.7929 0.1399 0.038 Uiso 1 1 calc R A . C14 C 0.4333(3) 0.79423(15) 0.23659(10) 0.0302(6) Uani 1 1 d . A . C15 C 0.4306(3) 0.84845(16) 0.27638(11) 0.0370(7) Uani 1 1 d . . . H15 H 0.5002 0.8498 0.3019 0.044 Uiso 1 1 calc R A . C16 C 0.3282(3) 0.90053(17) 0.27961(11) 0.0420(7) Uani 1 1 d . A . H16 H 0.3278 0.9368 0.3074 0.050 Uiso 1 1 calc R . . C17 C 0.2267(3) 0.90026(19) 0.24272(12) 0.0479(8) Uani 1 1 d . . . H17 H 0.1566 0.9363 0.2447 0.057 Uiso 1 1 calc R A . C18 C 0.2289(3) 0.8468(2) 0.20297(13) 0.0503(8) Uani 1 1 d . A . H18 H 0.1598 0.8464 0.1773 0.060 Uiso 1 1 calc R . . C19 C 0.3300(3) 0.79369(17) 0.19975(11) 0.0398(7) Uani 1 1 d . . . H19 H 0.3288 0.7567 0.1723 0.048 Uiso 1 1 calc R A . C20 C 0.6466(2) 0.76410(15) 0.48833(9) 0.0266(6) Uani 1 1 d . A . C21 C 0.7229(3) 0.63859(16) 0.52105(10) 0.0347(6) Uani 1 1 d . A . H21 H 0.6859 0.6591 0.5536 0.042 Uiso 1 1 calc R . . C22 C 0.8672(3) 0.6195(2) 0.53139(13) 0.0523(9) Uani 1 1 d . . . H22A H 0.9137 0.6664 0.5435 0.078 Uiso 1 1 calc R A . H22B H 0.9048 0.6010 0.4993 0.078 Uiso 1 1 calc R . . H22C H 0.8759 0.5788 0.5580 0.078 Uiso 1 1 calc R . . C23 C 0.6470(3) 0.56622(18) 0.50377(13) 0.0535(9) Uani 1 1 d . . . H23A H 0.6818 0.5463 0.4715 0.080 Uiso 1 1 calc R A . H23B H 0.5546 0.5796 0.4979 0.080 Uiso 1 1 calc R . . H23C H 0.6558 0.5262 0.5308 0.080 Uiso 1 1 calc R . . C24 C 0.5751(3) 0.89226(15) 0.45895(10) 0.0325(6) Uani 1 1 d . A . H24 H 0.5137 0.8857 0.4877 0.039 Uiso 1 1 calc R . . C25 C 0.4972(3) 0.90880(19) 0.40908(12) 0.0529(9) Uani 1 1 d . . . H25A H 0.4395 0.8646 0.4008 0.079 Uiso 1 1 calc R A . H25B H 0.5570 0.9166 0.3809 0.079 Uiso 1 1 calc R . . H25C H 0.4446 0.9559 0.4133 0.079 Uiso 1 1 calc R . . C26 C 0.6662(3) 0.96076(17) 0.47146(13) 0.0483(8) Uani 1 1 d . . . H26A H 0.7306 0.9651 0.4446 0.072 Uiso 1 1 calc R A . H26B H 0.7112 0.9522 0.5052 0.072 Uiso 1 1 calc R . . H26C H 0.6150 1.0090 0.4726 0.072 Uiso 1 1 calc R . . C27 C 0.4544(3) 0.72584(15) 0.53546(10) 0.0297(6) Uani 1 1 d . A . C28 C 0.3744(3) 0.71916(17) 0.49092(11) 0.0376(7) Uani 1 1 d . . . H28 H 0.3930 0.7488 0.4610 0.045 Uiso 1 1 calc R A . C29 C 0.2673(3) 0.66930(18) 0.48974(13) 0.0447(8) Uani 1 1 d . A . H29 H 0.2137 0.6649 0.4589 0.054 Uiso 1 1 calc R . . C30 C 0.2381(3) 0.62628(18) 0.53287(13) 0.0463(8) Uani 1 1 d . . . H30 H 0.1653 0.5920 0.5318 0.056 Uiso 1 1 calc R A . C31 C 0.3160(3) 0.63357(18) 0.57762(13) 0.0451(8) Uani 1 1 d . A . H31 H 0.2956 0.6048 0.6077 0.054 Uiso 1 1 calc R . . C32 C 0.4236(3) 0.68245(17) 0.57911(11) 0.0378(7) Uani 1 1 d . . . H32 H 0.4768 0.6865 0.6100 0.045 Uiso 1 1 calc R A . C33 C 0.6179(3) 0.81579(14) 0.57671(9) 0.0278(6) Uani 1 1 d . A . C34 C 0.5373(3) 0.84178(17) 0.61527(11) 0.0392(7) Uani 1 1 d . . . H34 H 0.4468 0.8297 0.6134 0.047 Uiso 1 1 calc R A . C35 C 0.5894(3) 0.88537(18) 0.65644(11) 0.0471(8) Uani 1 1 d . A . H35 H 0.5339 0.9020 0.6829 0.057 Uiso 1 1 calc R . . C36 C 0.7192(3) 0.90500(17) 0.65980(11) 0.0443(8) Uani 1 1 d . . . H36 H 0.7534 0.9347 0.6883 0.053 Uiso 1 1 calc R A . C37 C 0.7997(3) 0.88112(16) 0.62119(11) 0.0371(7) Uani 1 1 d . A . H37 H 0.8892 0.8956 0.6226 0.045 Uiso 1 1 calc R . . C38 C 0.7499(3) 0.83606(15) 0.58042(10) 0.0324(6) Uani 1 1 d . . . H38 H 0.8065 0.8187 0.5546 0.039 Uiso 1 1 calc R A . C39 C 0.9880(9) 0.5600(6) 0.3839(4) 0.061(3) Uani 0.55 1 d PDU A 1 H39A H 0.9383 0.5321 0.4102 0.073 Uiso 0.55 1 calc PR A 1 H39B H 1.0655 0.5841 0.4016 0.073 Uiso 0.55 1 calc PR A 1 C40 C 1.0293(10) 0.5055(6) 0.3449(4) 0.073(3) Uani 0.55 1 d PDU A 1 H40A H 1.1239 0.4942 0.3495 0.088 Uiso 0.55 1 calc PR A 1 H40B H 0.9800 0.4560 0.3467 0.088 Uiso 0.55 1 calc PR A 1 C41 C 1.0009(10) 0.5449(5) 0.2969(3) 0.058(2) Uani 0.55 1 d PDU A 1 H41A H 1.0805 0.5478 0.2765 0.070 Uiso 0.55 1 calc PR A 1 H41B H 0.9331 0.5160 0.2763 0.070 Uiso 0.55 1 calc PR A 1 C42 C 0.9562(7) 0.6205(4) 0.3077(3) 0.0516(18) Uani 0.55 1 d PDU A 1 H42A H 0.8844 0.6355 0.2828 0.062 Uiso 0.55 1 calc PR A 1 H42B H 1.0280 0.6588 0.3052 0.062 Uiso 0.55 1 calc PR A 1 C43 C 1.0854(3) 0.8268(2) 0.37726(13) 0.0538(9) Uani 1 1 d . A . H43A H 1.0627 0.8231 0.3397 0.065 Uiso 1 1 calc R . . H43B H 1.1646 0.7953 0.3851 0.065 Uiso 1 1 calc R . . C44 C 1.1073(4) 0.9099(2) 0.39293(16) 0.0780(12) Uani 1 1 d D . . H44A H 1.0426 0.9453 0.3758 0.094 Uiso 1 1 calc R A 1 H44B H 1.1968 0.9277 0.3859 0.094 Uiso 1 1 calc R A 1 C45 C 1.0863(10) 0.9018(7) 0.4518(4) 0.080(4) Uani 0.55 1 d PDU A 1 H45A H 1.1698 0.8900 0.4709 0.097 Uiso 0.55 1 calc PR A 1 H45B H 1.0500 0.9506 0.4659 0.097 Uiso 0.55 1 calc PR A 1 C46 C 0.9952(4) 0.8385(2) 0.45644(12) 0.0636(10) Uani 1 1 d D A . H46A H 1.0286 0.8010 0.4830 0.076 Uiso 1 1 calc R B 1 H46B H 0.9100 0.8587 0.4673 0.076 Uiso 1 1 calc R B 1 C39A C 0.9338(14) 0.5441(6) 0.3820(5) 0.072(4) Uani 0.45 1 d PDU A 2 H39C H 0.8576 0.5266 0.4013 0.086 Uiso 0.45 1 calc PR A 2 H39D H 1.0109 0.5461 0.4064 0.086 Uiso 0.45 1 calc PR A 2 C40A C 0.9570(11) 0.4915(6) 0.3405(4) 0.060(3) Uani 0.45 1 d PDU A 2 H40C H 1.0450 0.4683 0.3458 0.072 Uiso 0.45 1 calc PR A 2 H40D H 0.8922 0.4487 0.3408 0.072 Uiso 0.45 1 calc PR A 2 C41A C 0.9483(15) 0.5288(8) 0.2932(6) 0.102(6) Uani 0.45 1 d PDU A 2 H41C H 1.0354 0.5420 0.2805 0.122 Uiso 0.45 1 calc PR A 2 H41D H 0.8988 0.4978 0.2667 0.122 Uiso 0.45 1 calc PR A 2 C42A C 0.8832(13) 0.5916(8) 0.3070(4) 0.095(4) Uani 0.45 1 d PDU A 2 H42C H 0.7885 0.5808 0.3022 0.114 Uiso 0.45 1 calc PR A 2 H42D H 0.9043 0.6348 0.2833 0.114 Uiso 0.45 1 calc PR A 2 C45A C 1.0385(10) 0.9244(6) 0.4415(4) 0.060(3) Uani 0.45 1 d PDU A 2 H45C H 0.9620 0.9590 0.4354 0.072 Uiso 0.45 1 calc PR A 2 H45D H 1.0977 0.9475 0.4687 0.072 Uiso 0.45 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 Sr1 0.03432(14) 0.02900(14) 0.02089(13) -0.00101(11) 0.00226(10) 0.00339(12) O1 0.0853(18) 0.0545(15) 0.0433(13) -0.0065(11) 0.0004(12) 0.0386(13) O2 0.0410(12) 0.0667(15) 0.0368(11) -0.0042(10) 0.0069(10) -0.0127(11) N1 0.0452(14) 0.0338(13) 0.0266(12) 0.0006(10) -0.0021(11) -0.0056(11) N2 0.0369(13) 0.0351(13) 0.0221(11) 0.0013(10) 0.0002(10) -0.0005(11) N3 0.0367(13) 0.0338(13) 0.0212(11) -0.0050(9) -0.0021(10) 0.0076(10) N4 0.0386(13) 0.0291(12) 0.0242(11) 0.0026(9) 0.0024(10) 0.0031(10) N5 0.0378(13) 0.0254(12) 0.0256(11) 0.0001(9) 0.0057(10) 0.0034(10) N6 0.0320(12) 0.0294(12) 0.0236(11) -0.0028(9) 0.0045(9) -0.0022(10) C1 0.0376(15) 0.0311(14) 0.0208(13) -0.0051(12) -0.0009(11) 0.0072(13) C2 0.055(2) 0.0455(19) 0.0321(16) -0.0048(13) 0.0014(15) -0.0142(15) C3 0.062(2) 0.076(3) 0.085(3) -0.010(2) 0.027(2) -0.020(2) C4 0.091(3) 0.045(2) 0.068(2) 0.0041(18) 0.003(2) -0.022(2) C5 0.0418(17) 0.0406(17) 0.0269(14) 0.0051(12) -0.0003(13) -0.0037(14) C6 0.0501(19) 0.066(2) 0.0390(17) 0.0025(16) 0.0102(15) -0.0085(17) C7 0.067(2) 0.0431(19) 0.0460(18) 0.0034(15) 0.0004(17) -0.0105(17) C8 0.0314(14) 0.0319(15) 0.0248(13) -0.0049(11) 0.0004(12) -0.0006(12) C9 0.0468(17) 0.0329(16) 0.0269(14) -0.0003(12) -0.0016(13) 0.0053(13) C10 0.0508(18) 0.0366(17) 0.0383(16) -0.0039(13) 0.0023(15) 0.0115(14) C11 0.0448(17) 0.0424(18) 0.0306(15) -0.0091(13) 0.0075(13) 0.0007(14) C12 0.0468(17) 0.0371(17) 0.0258(14) -0.0014(12) 0.0034(13) -0.0050(14) C13 0.0400(16) 0.0279(15) 0.0276(14) 0.0006(11) -0.0004(12) 0.0004(12) C14 0.0335(15) 0.0290(14) 0.0282(14) -0.0015(11) 0.0030(12) 0.0006(12) C15 0.0420(17) 0.0364(17) 0.0322(15) -0.0069(12) -0.0032(13) 0.0066(13) C16 0.0496(19) 0.0368(17) 0.0398(17) -0.0067(13) 0.0048(15) 0.0078(14) C17 0.0429(18) 0.048(2) 0.0525(19) -0.0055(16) 0.0029(16) 0.0168(15) C18 0.0355(17) 0.063(2) 0.052(2) -0.0083(17) -0.0089(16) 0.0099(16) C19 0.0377(16) 0.0423(18) 0.0392(16) -0.0109(13) -0.0018(14) 0.0005(13) C20 0.0310(14) 0.0298(14) 0.0192(12) -0.0046(11) 0.0020(11) -0.0041(12) C21 0.0445(17) 0.0314(16) 0.0283(14) 0.0058(12) 0.0031(13) 0.0032(13) C22 0.053(2) 0.056(2) 0.0480(19) 0.0114(16) -0.0002(16) 0.0153(17) C23 0.065(2) 0.0338(18) 0.061(2) 0.0037(15) 0.0015(18) -0.0011(16) C24 0.0412(16) 0.0276(15) 0.0290(14) 0.0008(11) 0.0057(13) 0.0061(12) C25 0.070(2) 0.0413(19) 0.0464(19) 0.0006(15) -0.0121(18) 0.0141(17) C26 0.061(2) 0.0298(17) 0.0538(19) -0.0013(14) 0.0030(17) 0.0021(15) C27 0.0306(14) 0.0296(15) 0.0293(14) -0.0034(12) 0.0055(12) 0.0000(12) C28 0.0391(16) 0.0389(18) 0.0349(16) -0.0024(12) 0.0016(13) -0.0035(13) C29 0.0394(17) 0.0448(19) 0.0496(19) -0.0114(15) -0.0022(15) -0.0026(15) C30 0.0349(17) 0.0372(18) 0.068(2) -0.0099(16) 0.0124(17) -0.0058(14) C31 0.0441(18) 0.0388(18) 0.0535(19) 0.0058(15) 0.0140(16) -0.0040(15) C32 0.0389(16) 0.0393(18) 0.0356(16) 0.0023(13) 0.0054(13) 0.0008(13) C33 0.0379(15) 0.0243(14) 0.0212(13) -0.0002(10) 0.0012(12) 0.0028(12) C34 0.0438(17) 0.0393(17) 0.0350(16) -0.0057(13) 0.0086(14) 0.0037(14) C35 0.067(2) 0.0419(19) 0.0333(16) -0.0131(14) 0.0099(16) 0.0081(16) C36 0.066(2) 0.0324(17) 0.0333(16) -0.0101(13) -0.0109(16) 0.0021(15) C37 0.0439(17) 0.0273(15) 0.0396(16) -0.0014(12) -0.0064(14) 0.0003(13) C38 0.0376(16) 0.0322(16) 0.0273(14) -0.0005(11) 0.0013(12) 0.0015(12) C39 0.064(5) 0.067(6) 0.049(4) -0.006(4) -0.010(4) 0.027(4) C40 0.088(6) 0.068(6) 0.065(5) 0.002(4) 0.015(5) 0.038(5) C41 0.075(5) 0.055(5) 0.045(4) -0.012(3) 0.007(4) 0.015(4) C42 0.055(4) 0.052(4) 0.050(4) 0.010(3) 0.022(3) 0.015(3) C43 0.0413(18) 0.076(3) 0.0455(19) -0.0019(17) 0.0123(16) 0.0023(17) C44 0.078(3) 0.067(3) 0.090(3) -0.003(2) 0.013(2) -0.018(2) C45 0.071(6) 0.092(7) 0.079(6) -0.032(5) 0.011(5) -0.023(5) C46 0.055(2) 0.100(3) 0.0350(18) -0.0088(18) 0.0010(17) -0.013(2) C39A 0.100(9) 0.056(6) 0.061(6) 0.019(5) 0.020(6) 0.018(6) C40A 0.087(7) 0.034(4) 0.060(5) -0.005(4) 0.016(6) 0.003(5) C41A 0.133(10) 0.084(8) 0.085(8) -0.032(6) -0.038(7) -0.001(7) C42A 0.099(7) 0.115(8) 0.070(6) -0.018(6) -0.013(6) 0.054(6) C45A 0.045(6) 0.064(6) 0.073(6) -0.030(5) 0.012(5) -0.009(4) _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 Sr1 N4 2.562(2) . ? Sr1 O2 2.572(2) . ? Sr1 N1 2.575(2) . ? Sr1 O1 2.582(2) . ? Sr1 N2 2.593(2) . ? Sr1 N5 2.602(2) . ? Sr1 C20 2.969(2) . ? Sr1 C1 2.983(2) . ? O1 C39 1.395(8) . ? O1 C39A 1.397(10) . ? O1 C42 1.467(6) . ? O1 C42A 1.469(9) . ? O2 C43 1.427(4) . ? O2 C46 1.438(4) . ? N1 C1 1.322(3) . ? N1 C2 1.465(4) . ? N2 C1 1.324(3) . ? N2 C5 1.458(3) . ? N3 C14 1.410(3) . ? N3 C8 1.412(3) . ? N3 C1 1.467(3) . ? N4 C20 1.328(3) . ? N4 C21 1.463(3) . ? N5 C20 1.321(3) . ? N5 C24 1.462(3) . ? N6 C33 1.405(3) . ? N6 C27 1.413(3) . ? N6 C20 1.464(3) . ? C2 C3 1.514(5) . ? C2 C4 1.526(5) . ? C5 C6 1.514(4) . ? C5 C7 1.521(4) . ? C8 C9 1.395(4) . ? C8 C13 1.396(4) . ? C9 C10 1.384(4) . ? C10 C11 1.382(4) . ? C11 C12 1.379(4) . ? C12 C13 1.382(4) . ? C14 C15 1.387(4) . ? C14 C19 1.393(4) . ? C15 C16 1.383(4) . ? C16 C17 1.381(4) . ? C17 C18 1.377(4) . ? C18 C19 1.385(4) . ? C21 C23 1.522(4) . ? C21 C22 1.527(4) . ? C24 C25 1.513(4) . ? C24 C26 1.527(4) . ? C27 C28 1.388(4) . ? C27 C32 1.398(4) . ? C28 C29 1.391(4) . ? C29 C30 1.379(4) . ? C30 C31 1.382(4) . ? C31 C32 1.384(4) . ? C33 C34 1.392(4) . ? C33 C38 1.396(4) . ? C34 C35 1.387(4) . ? C35 C36 1.371(4) . ? C36 C37 1.382(4) . ? C37 C38 1.386(4) . ? C39 C40 1.449(9) . ? C40 C41 1.433(9) . ? C41 C42 1.406(8) . ? C43 C44 1.496(5) . ? C44 C45A 1.484(10) . ? C44 C45 1.551(10) . ? C45 C46 1.440(11) . ? C46 C45A 1.591(11) . ? C39A C40A 1.428(11) . ? C40A C41A 1.379(12) . ? C41A C42A 1.324(12) . ? 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 Sr1 O2 96.13(7) . . ? N4 Sr1 N1 113.89(7) . . ? O2 Sr1 N1 149.96(7) . . ? N4 Sr1 O1 102.83(7) . . ? O2 Sr1 O1 83.10(8) . . ? N1 Sr1 O1 88.92(8) . . ? N4 Sr1 N2 160.76(7) . . ? O2 Sr1 N2 98.74(7) . . ? N1 Sr1 N2 52.34(7) . . ? O1 Sr1 N2 91.05(7) . . ? N4 Sr1 N5 52.58(7) . . ? O2 Sr1 N5 89.43(7) . . ? N1 Sr1 N5 109.22(7) . . ? O1 Sr1 N5 153.47(7) . . ? N2 Sr1 N5 115.28(7) . . ? N4 Sr1 C20 26.49(7) . . ? O2 Sr1 C20 96.04(6) . . ? N1 Sr1 C20 111.21(7) . . ? O1 Sr1 C20 129.22(7) . . ? N2 Sr1 C20 138.51(7) . . ? N5 Sr1 C20 26.40(7) . . ? N4 Sr1 C1 137.84(7) . . ? O2 Sr1 C1 124.96(7) . . ? N1 Sr1 C1 26.21(7) . . ? O1 Sr1 C1 92.13(7) . . ? N2 Sr1 C1 26.30(7) . . ? N5 Sr1 C1 112.78(7) . . ? C20 Sr1 C1 126.41(7) . . ? C39 O1 C39A 25.6(7) . . ? C39 O1 C42 102.7(5) . . ? C39A O1 C42 109.7(6) . . ? C39 O1 C42A 105.6(6) . . ? C39A O1 C42A 96.8(8) . . ? C42 O1 C42A 35.6(5) . . ? C39 O1 Sr1 139.4(4) . . ? C39A O1 Sr1 132.5(6) . . ? C42 O1 Sr1 116.0(3) . . ? C42A O1 Sr1 112.8(4) . . ? C43 O2 C46 105.9(2) . . ? C43 O2 Sr1 135.51(18) . . ? C46 O2 Sr1 117.02(18) . . ? C1 N1 C2 121.8(2) . . ? C1 N1 Sr1 94.39(16) . . ? C2 N1 Sr1 143.25(17) . . ? C1 N2 C5 121.5(2) . . ? C1 N2 Sr1 93.52(15) . . ? C5 N2 Sr1 142.92(17) . . ? C14 N3 C8 124.1(2) . . ? C14 N3 C1 117.5(2) . . ? C8 N3 C1 117.0(2) . . ? C20 N4 C21 121.1(2) . . ? C20 N4 Sr1 94.09(15) . . ? C21 N4 Sr1 144.53(17) . . ? C20 N5 C24 121.5(2) . . ? C20 N5 Sr1 92.47(15) . . ? C24 N5 Sr1 143.34(16) . . ? C33 N6 C27 123.6(2) . . ? C33 N6 C20 119.3(2) . . ? C27 N6 C20 116.5(2) . . ? N1 C1 N2 119.0(2) . . ? N1 C1 N3 120.5(2) . . ? N2 C1 N3 120.4(2) . . ? N1 C1 Sr1 59.40(13) . . ? N2 C1 Sr1 60.18(13) . . ? N3 C1 Sr1 171.44(17) . . ? N1 C2 C3 111.0(3) . . ? N1 C2 C4 107.9(3) . . ? C3 C2 C4 110.6(3) . . ? N2 C5 C6 110.8(2) . . ? N2 C5 C7 108.8(2) . . ? C6 C5 C7 110.7(3) . . ? C9 C8 C13 118.2(2) . . ? C9 C8 N3 119.5(2) . . ? C13 C8 N3 122.3(2) . . ? C10 C9 C8 120.7(3) . . ? C11 C10 C9 120.6(3) . . ? C12 C11 C10 119.0(3) . . ? C11 C12 C13 121.0(3) . . ? C12 C13 C8 120.4(3) . . ? C15 C14 C19 118.2(3) . . ? C15 C14 N3 119.6(2) . . ? C19 C14 N3 122.1(2) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 C15 120.5(3) . . ? C18 C17 C16 118.7(3) . . ? C17 C18 C19 121.2(3) . . ? C18 C19 C14 120.2(3) . . ? N5 C20 N4 119.5(2) . . ? N5 C20 N6 120.9(2) . . ? N4 C20 N6 119.7(2) . . ? N5 C20 Sr1 61.12(13) . . ? N4 C20 Sr1 59.42(12) . . ? N6 C20 Sr1 168.90(16) . . ? N4 C21 C23 110.4(2) . . ? N4 C21 C22 108.3(2) . . ? C23 C21 C22 110.8(3) . . ? N5 C24 C25 110.0(2) . . ? N5 C24 C26 110.1(2) . . ? C25 C24 C26 109.4(2) . . ? C28 C27 C32 118.5(3) . . ? C28 C27 N6 119.2(2) . . ? C32 C27 N6 122.1(2) . . ? C27 C28 C29 120.5(3) . . ? C30 C29 C28 120.6(3) . . ? C29 C30 C31 119.3(3) . . ? C30 C31 C32 120.6(3) . . ? C31 C32 C27 120.5(3) . . ? C34 C33 C38 118.2(2) . . ? C34 C33 N6 121.6(2) . . ? C38 C33 N6 120.2(2) . . ? C35 C34 C33 120.0(3) . . ? C36 C35 C34 121.5(3) . . ? C35 C36 C37 119.2(3) . . ? C36 C37 C38 120.1(3) . . ? C37 C38 C33 121.0(3) . . ? O1 C39 C40 109.9(7) . . ? C41 C40 C39 104.0(7) . . ? C42 C41 C40 108.6(7) . . ? C41 C42 O1 106.1(6) . . ? O2 C43 C44 105.4(3) . . ? C45A C44 C43 108.5(5) . . ? C45A C44 C45 25.4(5) . . ? C43 C44 C45 98.9(5) . . ? C46 C45 C44 105.4(6) . . ? O2 C46 C45 108.5(4) . . ? O2 C46 C45A 103.1(5) . . ? C45 C46 C45A 24.9(6) . . ? O1 C39A C40A 107.9(9) . . ? C41A C40A C39A 111.3(10) . . ? C42A C41A C40A 98.9(13) . . ? C41A C42A O1 115.2(9) . . ? C44 C45A C46 101.3(6) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.17 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.277 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.056 data_768278-k08msh7 _database_code_depnum_ccdc_archive 'CCDC 768278' #TrackingRef '768277-80.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H48 Ca0.50 N3 O Si2' _chemical_formula_weight 458.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.2500(5) _cell_length_b 26.3080(9) _cell_length_c 10.1110(5) _cell_angle_alpha 90.00 _cell_angle_beta 132.16(2) _cell_angle_gamma 90.00 _cell_volume 2809.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 48724 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21929 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3278 _reflns_number_gt 2833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+11.3026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0056(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3278 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.0000 0.0000 0.5000 0.0234(3) Uani 1 4 d S . . Si1 Si -0.07958(9) 0.19404(3) 0.29606(12) 0.0372(3) Uani 1 1 d . A . O1 O 0.1371(3) 0.0000 0.8264(4) 0.0476(9) Uani 1 2 d S . . N1 N 0.0861(2) 0.08122(9) 0.5141(4) 0.0307(5) Uani 1 1 d . . . N2 N 0.0000 0.16308(11) 0.5000 0.0295(7) Uani 1 2 d S . . C1 C 0.0000 0.10778(14) 0.5000 0.0271(8) Uani 1 2 d S . . C2 C 0.0310(5) 0.2284(2) 0.2871(7) 0.093(2) Uani 1 1 d . . . H2A H 0.0716 0.2564 0.3733 0.140 Uiso 1 1 calc R A . H2B H -0.0165 0.2420 0.1668 0.140 Uiso 1 1 calc R . . H2C H 0.0959 0.2048 0.3165 0.140 Uiso 1 1 calc R . . C3 C -0.1679(4) 0.14730(15) 0.1114(5) 0.0601(11) Uani 1 1 d . . . H3A H -0.1342 0.1132 0.1595 0.090 Uiso 1 1 calc R A . H3B H -0.1586 0.1558 0.0263 0.090 Uiso 1 1 calc R . . H3C H -0.2577 0.1482 0.0507 0.090 Uiso 1 1 calc R . . C4 C -0.1907(7) 0.2418(2) 0.2584(8) 0.113(3) Uani 1 1 d . . . H4A H -0.2585 0.2246 0.2429 0.169 Uiso 1 1 calc R A . H4B H -0.2274 0.2616 0.1510 0.169 Uiso 1 1 calc R . . H4C H -0.1452 0.2647 0.3614 0.169 Uiso 1 1 calc R . . C5 C 0.1904(3) 0.10605(11) 0.5438(4) 0.0311(6) Uani 1 1 d . A . H5 H 0.1845 0.1436 0.5525 0.037 Uiso 1 1 calc R . . C6 C 0.1855(3) 0.09527(16) 0.3913(5) 0.0503(9) Uani 1 1 d . . . H6A H 0.1050 0.1085 0.2786 0.060 Uiso 1 1 calc R A . H6B H 0.1874 0.0581 0.3783 0.060 Uiso 1 1 calc R . . C7 C 0.2972(4) 0.12003(18) 0.4243(6) 0.0599(11) Uani 1 1 d . A . H7A H 0.2923 0.1116 0.3244 0.072 Uiso 1 1 calc R . . H7B H 0.2914 0.1574 0.4277 0.072 Uiso 1 1 calc R . . C8 C 0.4217(4) 0.10229(18) 0.5961(6) 0.0659(12) Uani 1 1 d . . . H8A H 0.4913 0.1207 0.6171 0.079 Uiso 1 1 calc R A . H8B H 0.4320 0.0655 0.5877 0.079 Uiso 1 1 calc R . . C9 C 0.4292(3) 0.1115(2) 0.7507(6) 0.0652(12) Uani 1 1 d . A . H9A H 0.4297 0.1486 0.7684 0.078 Uiso 1 1 calc R . . H9B H 0.5092 0.0972 0.8610 0.078 Uiso 1 1 calc R . . C10 C 0.3173(3) 0.08723(17) 0.7169(5) 0.0545(10) Uani 1 1 d . . . H10A H 0.3218 0.0498 0.7111 0.065 Uiso 1 1 calc R A . H10B H 0.3230 0.0952 0.8179 0.065 Uiso 1 1 calc R . . C11 C 0.0836(6) -0.0085(7) 0.9063(8) 0.045(4) Uani 0.50 1 d P A -1 H11A H 0.0727 -0.0453 0.9133 0.054 Uiso 0.50 1 calc PR A -1 H11B H 0.0006 0.0086 0.8365 0.054 Uiso 0.50 1 calc PR A -1 C12 C 0.1782(8) 0.0141(3) 1.0881(10) 0.059(2) Uani 0.50 1 d P A -1 H12A H 0.1656 0.0033 1.1689 0.071 Uiso 0.50 1 calc PR A -1 H12B H 0.1821 0.0516 1.0860 0.071 Uiso 0.50 1 calc PR A -1 C13 C 0.3008(7) -0.0142(3) 1.1328(9) 0.052(2) Uani 0.50 1 d P A -1 H13A H 0.3816 0.0026 1.2330 0.062 Uiso 0.50 1 calc PR A -1 H13B H 0.3054 -0.0506 1.1607 0.062 Uiso 0.50 1 calc PR A -1 C14 C 0.2711(5) -0.0072(9) 0.9692(8) 0.041(4) Uani 0.50 1 d P A -1 H14A H 0.2986 -0.0374 0.9441 0.049 Uiso 0.50 1 calc PR A -1 H14B H 0.3169 0.0228 0.9779 0.049 Uiso 0.50 1 calc PR A -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 Ca1 0.0240(5) 0.0180(5) 0.0322(6) 0.000 0.0205(5) 0.000 Si1 0.0445(5) 0.0234(4) 0.0435(5) 0.0044(3) 0.0295(4) 0.0038(3) O1 0.0331(17) 0.078(3) 0.0309(17) 0.000 0.0211(15) 0.000 N1 0.0297(12) 0.0214(11) 0.0525(15) 0.0012(10) 0.0323(12) -0.0001(9) N2 0.0361(18) 0.0145(14) 0.044(2) 0.000 0.0295(17) 0.000 C1 0.0293(19) 0.0188(17) 0.039(2) 0.000 0.0252(18) 0.000 C2 0.086(3) 0.098(4) 0.065(3) 0.022(3) 0.038(3) -0.039(3) C3 0.066(3) 0.044(2) 0.047(2) 0.0016(17) 0.028(2) -0.0027(18) C4 0.167(6) 0.109(4) 0.084(4) 0.058(3) 0.093(4) 0.106(4) C5 0.0296(14) 0.0236(13) 0.0502(18) 0.0025(12) 0.0308(14) -0.0002(11) C6 0.0453(19) 0.063(2) 0.061(2) -0.0136(19) 0.0434(19) -0.0168(17) C7 0.051(2) 0.082(3) 0.072(3) -0.003(2) 0.052(2) -0.014(2) C8 0.050(2) 0.073(3) 0.102(3) 0.008(3) 0.063(3) 0.001(2) C9 0.0292(17) 0.099(3) 0.063(3) 0.015(2) 0.0292(18) -0.0018(19) C10 0.0348(17) 0.072(3) 0.064(2) 0.023(2) 0.0360(18) 0.0077(17) C11 0.037(3) 0.060(13) 0.047(3) -0.010(4) 0.032(3) -0.004(4) C12 0.091(5) 0.057(6) 0.060(4) -0.021(3) 0.063(4) -0.025(4) C13 0.044(3) 0.056(6) 0.040(3) 0.012(3) 0.022(3) 0.004(3) C14 0.033(2) 0.043(13) 0.044(3) -0.008(4) 0.025(2) 0.000(3) _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 Ca1 N1 2.420(2) 5_556 ? Ca1 N1 2.420(2) 6 ? Ca1 N1 2.420(2) . ? Ca1 N1 2.420(2) 2_556 ? Ca1 O1 2.460(3) 5_556 ? Ca1 O1 2.460(3) . ? Ca1 C1 2.835(4) . ? Ca1 C1 2.835(4) 5_556 ? Si1 N2 1.7499(17) . ? Si1 C4 1.851(4) . ? Si1 C3 1.851(4) . ? Si1 C2 1.871(5) . ? O1 C14 1.437(7) 6 ? O1 C14 1.437(7) . ? O1 C11 1.453(7) . ? O1 C11 1.453(7) 6 ? N1 C1 1.334(3) . ? N1 C5 1.459(3) . ? N2 C1 1.455(5) . ? N2 Si1 1.7499(17) 2_556 ? C1 N1 1.334(3) 2_556 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.522(4) . ? C5 C10 1.526(5) . ? C5 H5 1.0000 . ? C6 C7 1.535(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.498(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.513(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.529(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.491(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.657(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.418(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ca1 N1 55.99(10) 5_556 6 ? N1 Ca1 N1 180.00(5) 5_556 . ? N1 Ca1 N1 124.01(10) 6 . ? N1 Ca1 N1 124.01(10) 5_556 2_556 ? N1 Ca1 N1 180.00(16) 6 2_556 ? N1 Ca1 N1 55.99(10) . 2_556 ? N1 Ca1 O1 90.35(7) 5_556 5_556 ? N1 Ca1 O1 89.65(7) 6 5_556 ? N1 Ca1 O1 89.65(7) . 5_556 ? N1 Ca1 O1 90.35(7) 2_556 5_556 ? N1 Ca1 O1 89.65(7) 5_556 . ? N1 Ca1 O1 90.35(7) 6 . ? N1 Ca1 O1 90.35(7) . . ? N1 Ca1 O1 89.65(7) 2_556 . ? O1 Ca1 O1 180.00(15) 5_556 . ? N1 Ca1 C1 152.01(5) 5_556 . ? N1 Ca1 C1 152.01(5) 6 . ? N1 Ca1 C1 27.99(5) . . ? N1 Ca1 C1 27.99(5) 2_556 . ? O1 Ca1 C1 90.0 5_556 . ? O1 Ca1 C1 90.0 . . ? N1 Ca1 C1 27.99(5) 5_556 5_556 ? N1 Ca1 C1 27.99(5) 6 5_556 ? N1 Ca1 C1 152.01(5) . 5_556 ? N1 Ca1 C1 152.01(5) 2_556 5_556 ? O1 Ca1 C1 90.0 5_556 5_556 ? O1 Ca1 C1 90.0 . 5_556 ? C1 Ca1 C1 180.0 . 5_556 ? N2 Si1 C4 110.30(17) . . ? N2 Si1 C3 110.08(16) . . ? C4 Si1 C3 109.6(3) . . ? N2 Si1 C2 112.41(17) . . ? C4 Si1 C2 107.1(3) . . ? C3 Si1 C2 107.3(2) . . ? C14 O1 C14 15.2(18) 6 . ? C14 O1 C11 107.5(4) 6 . ? C14 O1 C11 105.1(4) . . ? C14 O1 C11 105.1(4) 6 6 ? C14 O1 C11 107.5(4) . 6 ? C11 O1 C11 17.7(14) . 6 ? C14 O1 Ca1 132.2(3) 6 . ? C14 O1 Ca1 132.2(3) . . ? C11 O1 Ca1 120.4(3) . . ? C11 O1 Ca1 120.4(3) 6 . ? C1 N1 C5 121.7(2) . . ? C1 N1 Ca1 93.60(17) . . ? C5 N1 Ca1 144.46(17) . . ? C1 N2 Si1 117.74(9) . . ? C1 N2 Si1 117.74(9) . 2_556 ? Si1 N2 Si1 124.52(18) . 2_556 ? N1 C1 N1 116.8(3) 2_556 . ? N1 C1 N2 121.59(16) 2_556 . ? N1 C1 N2 121.59(16) . . ? N1 C1 Ca1 58.41(16) 2_556 . ? N1 C1 Ca1 58.41(16) . . ? N2 C1 Ca1 180.0 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 111.1(3) . . ? N1 C5 C10 110.5(2) . . ? C6 C5 C10 108.4(3) . . ? N1 C5 H5 108.9 . . ? C6 C5 H5 108.9 . . ? C10 C5 H5 108.9 . . ? C5 C6 C7 111.4(3) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.6(3) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 110.8(3) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 111.2(4) . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C5 C10 C9 112.0(3) . . ? C5 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C5 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O1 C11 C12 104.3(7) . . ? O1 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? O1 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? C11 C12 C13 94.2(6) . . ? C11 C12 H12A 112.9 . . ? C13 C12 H12A 112.9 . . ? C11 C12 H12B 112.9 . . ? C13 C12 H12B 112.9 . . ? H12A C12 H12B 110.3 . . ? C14 C13 C12 100.9(7) . . ? C14 C13 H13A 111.6 . . ? C12 C13 H13A 111.6 . . ? C14 C13 H13B 111.6 . . ? C12 C13 H13B 111.6 . . ? H13A C13 H13B 109.4 . . ? C13 C14 O1 110.2(5) . . ? C13 C14 H14A 109.6 . . ? O1 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? O1 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? 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 N1 Ca1 O1 C14 128.2(12) 5_556 . . 6 ? N1 Ca1 O1 C14 72.3(12) 6 . . 6 ? N1 Ca1 O1 C14 -51.8(12) . . . 6 ? N1 Ca1 O1 C14 -107.7(12) 2_556 . . 6 ? O1 Ca1 O1 C14 -169.7(14) 5_556 . . 6 ? C1 Ca1 O1 C14 -79.7(12) . . . 6 ? C1 Ca1 O1 C14 100.3(12) 5_556 . . 6 ? N1 Ca1 O1 C14 107.7(12) 5_556 . . . ? N1 Ca1 O1 C14 51.8(12) 6 . . . ? N1 Ca1 O1 C14 -72.3(12) . . . . ? N1 Ca1 O1 C14 -128.2(12) 2_556 . . . ? O1 Ca1 O1 C14 169.7(14) 5_556 . . . ? C1 Ca1 O1 C14 -100.3(12) . . . . ? C1 Ca1 O1 C14 79.7(12) 5_556 . . . ? N1 Ca1 O1 C11 -51.7(8) 5_556 . . . ? N1 Ca1 O1 C11 -107.7(8) 6 . . . ? N1 Ca1 O1 C11 128.3(8) . . . . ? N1 Ca1 O1 C11 72.3(8) 2_556 . . . ? O1 Ca1 O1 C11 10.3(11) 5_556 . . . ? C1 Ca1 O1 C11 100.3(8) . . . . ? C1 Ca1 O1 C11 -79.7(8) 5_556 . . . ? N1 Ca1 O1 C11 -72.3(8) 5_556 . . 6 ? N1 Ca1 O1 C11 -128.3(8) 6 . . 6 ? N1 Ca1 O1 C11 107.7(8) . . . 6 ? N1 Ca1 O1 C11 51.7(8) 2_556 . . 6 ? O1 Ca1 O1 C11 -10.3(11) 5_556 . . 6 ? C1 Ca1 O1 C11 79.7(8) . . . 6 ? C1 Ca1 O1 C11 -100.3(8) 5_556 . . 6 ? N1 Ca1 N1 C1 -2(18) 5_556 . . . ? N1 Ca1 N1 C1 180.0 6 . . . ? N1 Ca1 N1 C1 0.0 2_556 . . . ? O1 Ca1 N1 C1 90.66(14) 5_556 . . . ? O1 Ca1 N1 C1 -89.34(14) . . . . ? C1 Ca1 N1 C1 180.0 5_556 . . . ? N1 Ca1 N1 C5 171(18) 5_556 . . . ? N1 Ca1 N1 C5 -6.9(4) 6 . . . ? N1 Ca1 N1 C5 173.1(4) 2_556 . . . ? O1 Ca1 N1 C5 -96.2(3) 5_556 . . . ? O1 Ca1 N1 C5 83.8(3) . . . . ? C1 Ca1 N1 C5 173.1(4) . . . . ? C1 Ca1 N1 C5 -6.9(4) 5_556 . . . ? C4 Si1 N2 C1 128.6(3) . . . . ? C3 Si1 N2 C1 7.58(17) . . . . ? C2 Si1 N2 C1 -111.9(2) . . . . ? C4 Si1 N2 Si1 -51.4(3) . . . 2_556 ? C3 Si1 N2 Si1 -172.42(17) . . . 2_556 ? C2 Si1 N2 Si1 68.1(2) . . . 2_556 ? C5 N1 C1 N1 -175.3(3) . . . 2_556 ? Ca1 N1 C1 N1 0.0 . . . 2_556 ? C5 N1 C1 N2 4.7(3) . . . . ? Ca1 N1 C1 N2 180.0 . . . . ? C5 N1 C1 Ca1 -175.3(3) . . . . ? Si1 N2 C1 N1 -93.94(14) . . . 2_556 ? Si1 N2 C1 N1 86.06(14) 2_556 . . 2_556 ? Si1 N2 C1 N1 86.06(14) . . . . ? Si1 N2 C1 N1 -93.94(14) 2_556 . . . ? Si1 N2 C1 Ca1 81(100) . . . . ? Si1 N2 C1 Ca1 -99(100) 2_556 . . . ? N1 Ca1 C1 N1 0.0 5_556 . . 2_556 ? N1 Ca1 C1 N1 180.0 6 . . 2_556 ? N1 Ca1 C1 N1 180.0 . . . 2_556 ? O1 Ca1 C1 N1 90.74(15) 5_556 . . 2_556 ? O1 Ca1 C1 N1 -89.26(15) . . . 2_556 ? C1 Ca1 C1 N1 -50(54) 5_556 . . 2_556 ? N1 Ca1 C1 N1 180.0 5_556 . . . ? N1 Ca1 C1 N1 0.0 6 . . . ? N1 Ca1 C1 N1 180.0 2_556 . . . ? O1 Ca1 C1 N1 -89.26(15) 5_556 . . . ? O1 Ca1 C1 N1 90.74(15) . . . . ? C1 Ca1 C1 N1 130(54) 5_556 . . . ? N1 Ca1 C1 N2 -175(100) 5_556 . . . ? N1 Ca1 C1 N2 5(77) 6 . . . ? N1 Ca1 C1 N2 5(77) . . . . ? N1 Ca1 C1 N2 -175(100) 2_556 . . . ? O1 Ca1 C1 N2 -84(77) 5_556 . . . ? O1 Ca1 C1 N2 96(100) . . . . ? C1 Ca1 C1 N2 0(100) 5_556 . . . ? C1 N1 C5 C6 -119.1(3) . . . . ? Ca1 N1 C5 C6 69.0(4) . . . . ? C1 N1 C5 C10 120.6(3) . . . . ? Ca1 N1 C5 C10 -51.4(5) . . . . ? N1 C5 C6 C7 -178.4(3) . . . . ? C10 C5 C6 C7 -56.8(4) . . . . ? C5 C6 C7 C8 57.6(5) . . . . ? C6 C7 C8 C9 -55.4(5) . . . . ? C7 C8 C9 C10 54.7(5) . . . . ? N1 C5 C10 C9 178.7(3) . . . . ? C6 C5 C10 C9 56.8(4) . . . . ? C8 C9 C10 C5 -56.5(5) . . . . ? C14 O1 C11 C12 21.9(14) 6 . . . ? C14 O1 C11 C12 37.5(14) . . . . ? C11 O1 C11 C12 -62.9(9) 6 . . . ? Ca1 O1 C11 C12 -158.1(5) . . . . ? O1 C11 C12 C13 -47.9(9) . . . . ? C11 C12 C13 C14 43.0(11) . . . . ? C12 C13 C14 O1 -23.6(15) . . . . ? C14 O1 C14 C13 95.1(13) 6 . . . ? C11 O1 C14 C13 -6.2(17) . . . . ? C11 O1 C14 C13 12.1(18) 6 . . . ? Ca1 O1 C14 C13 -167.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.480 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.081 data_768279-k07msh6 _database_code_depnum_ccdc_archive 'CCDC 768279' #TrackingRef '768277-80.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 Ca F2 N6 O2' _chemical_formula_weight 656.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3450(2) _cell_length_b 12.1410(3) _cell_length_c 18.4510(4) _cell_angle_alpha 87.950(1) _cell_angle_beta 82.074(1) _cell_angle_gamma 77.667(1) _cell_volume 1808.77(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 83464 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.221 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31965 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _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 3.58 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8218 _reflns_number_gt 6456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H3 and H6 located and refined at 0.90 \%A from the parent nitrogen atoms. C32/33 disordered over 2 sites in a 60:40 ratio. C-C distances involving the disordered fractional carbons refined subject to distance restraints. ; _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^)+(0.1000P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8218 _refine_ls_number_parameters 441 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.47012(4) 0.37683(3) 0.766988(19) 0.02904(14) Uani 1 1 d . . . F1 F 0.12071(15) 0.49778(10) 0.89297(6) 0.0416(3) Uani 1 1 d . . . F2 F 0.86269(17) 0.19198(12) 0.80296(8) 0.0571(4) Uani 1 1 d . . . O1 O 0.66500(17) 0.42606(12) 0.83783(7) 0.0379(3) Uani 1 1 d . . . O2 O 0.37407(19) 0.28154(12) 0.87380(8) 0.0444(4) Uani 1 1 d . B . N1 N 0.31246(19) 0.57084(12) 0.78031(8) 0.0305(3) Uani 1 1 d . . . N2 N 0.51059(18) 0.52971(13) 0.68233(8) 0.0305(3) Uani 1 1 d . . . N3 N 0.3406(2) 0.71361(14) 0.68909(10) 0.0374(4) Uani 1 1 d D . . N4 N 0.60918(19) 0.18691(13) 0.72677(8) 0.0313(3) Uani 1 1 d . . . N5 N 0.37368(19) 0.26949(13) 0.68032(8) 0.0299(3) Uani 1 1 d . . . N6 N 0.5338(2) 0.10006(15) 0.62564(9) 0.0375(4) Uani 1 1 d D . . C1 C 0.2601(2) 0.63862(15) 0.84099(10) 0.0311(4) Uani 1 1 d . . . C2 C 0.3026(2) 0.74194(17) 0.85432(12) 0.0384(5) Uani 1 1 d . . . H2 H 0.3681 0.7747 0.8169 0.046 Uiso 1 1 calc R . . C3 C 0.2506(3) 0.79678(19) 0.92101(14) 0.0486(6) Uani 1 1 d . . . H3A H 0.2835 0.8654 0.9282 0.058 Uiso 1 1 calc R . . C4 C 0.1533(3) 0.7549(2) 0.97698(13) 0.0501(6) Uani 1 1 d . . . H4 H 0.1177 0.7945 1.0218 0.060 Uiso 1 1 calc R . . C5 C 0.1080(3) 0.65343(19) 0.96646(11) 0.0418(5) Uani 1 1 d . . . H5 H 0.0410 0.6222 1.0041 0.050 Uiso 1 1 calc R . . C6 C 0.1621(2) 0.59893(16) 0.90062(11) 0.0341(4) Uani 1 1 d . . . C7 C 0.3898(2) 0.60539(15) 0.71654(10) 0.0304(4) Uani 1 1 d . . . C8 C 0.1681(2) 0.77782(16) 0.69902(12) 0.0376(4) Uani 1 1 d . . . H8 H 0.1210 0.7708 0.7514 0.045 Uiso 1 1 calc R . . C9 C 0.0622(3) 0.7332(2) 0.65184(15) 0.0513(6) Uani 1 1 d . . . H9A H 0.1048 0.7411 0.6001 0.077 Uiso 1 1 calc R . . H9B H -0.0521 0.7761 0.6614 0.077 Uiso 1 1 calc R . . H9C H 0.0652 0.6534 0.6634 0.077 Uiso 1 1 calc R . . C10 C 0.1704(3) 0.90113(18) 0.68291(14) 0.0492(5) Uani 1 1 d . . . H10A H 0.2315 0.9287 0.7176 0.074 Uiso 1 1 calc R . . H10B H 0.0566 0.9454 0.6878 0.074 Uiso 1 1 calc R . . H10C H 0.2244 0.9089 0.6329 0.074 Uiso 1 1 calc R . . C11 C 0.5846(2) 0.54902(16) 0.60791(10) 0.0343(4) Uani 1 1 d . . . H11 H 0.4961 0.5906 0.5797 0.041 Uiso 1 1 calc R . . C12 C 0.7183(3) 0.61856(19) 0.60697(12) 0.0425(5) Uani 1 1 d . . . H12A H 0.6712 0.6893 0.6333 0.064 Uiso 1 1 calc R . . H12B H 0.7589 0.6353 0.5562 0.064 Uiso 1 1 calc R . . H12C H 0.8103 0.5756 0.6308 0.064 Uiso 1 1 calc R . . C13 C 0.6595(3) 0.43542(19) 0.57208(11) 0.0444(5) Uani 1 1 d . . . H13A H 0.7434 0.3928 0.6005 0.067 Uiso 1 1 calc R . . H13B H 0.7110 0.4471 0.5222 0.067 Uiso 1 1 calc R . . H13C H 0.5723 0.3931 0.5705 0.067 Uiso 1 1 calc R . . C14 C 0.6259(3) 0.49601(18) 0.90242(11) 0.0387(5) Uani 1 1 d . . . H14A H 0.6624 0.4518 0.9455 0.046 Uiso 1 1 calc R . . H14B H 0.5051 0.5262 0.9125 0.046 Uiso 1 1 calc R . . C15 C 0.7181(3) 0.59232(18) 0.88647(12) 0.0438(5) Uani 1 1 d . . . H15A H 0.6401 0.6664 0.8913 0.053 Uiso 1 1 calc R . . H15B H 0.8012 0.5894 0.9203 0.053 Uiso 1 1 calc R . . C16 C 0.8017(3) 0.57277(19) 0.80784(12) 0.0447(5) Uani 1 1 d . . . H16A H 0.7327 0.6170 0.7729 0.054 Uiso 1 1 calc R . . H16B H 0.9117 0.5928 0.8011 0.054 Uiso 1 1 calc R . . C17 C 0.8169(3) 0.44793(18) 0.79842(12) 0.0411(5) Uani 1 1 d . . . H17A H 0.8273 0.4286 0.7461 0.049 Uiso 1 1 calc R . . H17B H 0.9142 0.4041 0.8195 0.049 Uiso 1 1 calc R . . C18 C 0.6800(2) 0.09121(16) 0.76284(10) 0.0318(4) Uani 1 1 d . . . C19 C 0.6287(3) -0.01292(17) 0.76880(12) 0.0418(5) Uani 1 1 d . . . H19 H 0.5390 -0.0215 0.7444 0.050 Uiso 1 1 calc R . . C20 C 0.7045(3) -0.1026(2) 0.80891(13) 0.0511(6) Uani 1 1 d . . . H20 H 0.6662 -0.1711 0.8108 0.061 Uiso 1 1 calc R . . C21 C 0.8336(3) -0.0954(2) 0.84614(13) 0.0520(6) Uani 1 1 d . . . H21 H 0.8860 -0.1581 0.8728 0.062 Uiso 1 1 calc R . . C22 C 0.8852(3) 0.0064(2) 0.84350(12) 0.0471(5) Uani 1 1 d . . . H22 H 0.9721 0.0149 0.8697 0.056 Uiso 1 1 calc R . . C23 C 0.8098(2) 0.09459(17) 0.80289(11) 0.0370(4) Uani 1 1 d . . . C24 C 0.5024(2) 0.18530(15) 0.67744(10) 0.0308(4) Uani 1 1 d . . . C25 C 0.7003(3) 0.04294(19) 0.59507(12) 0.0446(5) Uani 1 1 d . . . H25 H 0.7685 0.0225 0.6360 0.054 Uiso 1 1 calc R . . C26 C 0.7813(4) 0.1215(3) 0.5416(2) 0.0883(11) Uani 1 1 d . . . H26A H 0.7185 0.1395 0.5001 0.132 Uiso 1 1 calc R . . H26B H 0.8954 0.0839 0.5240 0.132 Uiso 1 1 calc R . . H26C H 0.7815 0.1912 0.5668 0.132 Uiso 1 1 calc R . . C27 C 0.6925(3) -0.0630(2) 0.55811(18) 0.0667(7) Uani 1 1 d . . . H27A H 0.6403 -0.1113 0.5933 0.100 Uiso 1 1 calc R . . H27B H 0.8047 -0.1028 0.5394 0.100 Uiso 1 1 calc R . . H27C H 0.6272 -0.0442 0.5174 0.100 Uiso 1 1 calc R . . C28 C 0.2649(2) 0.28714(16) 0.62354(11) 0.0340(4) Uani 1 1 d . . . H28 H 0.3333 0.2678 0.5750 0.041 Uiso 1 1 calc R . . C29 C 0.1803(3) 0.41027(17) 0.62305(12) 0.0385(5) Uani 1 1 d . . . H29A H 0.1120 0.4298 0.6703 0.058 Uiso 1 1 calc R . . H29B H 0.1100 0.4242 0.5839 0.058 Uiso 1 1 calc R . . H29C H 0.2640 0.4566 0.6147 0.058 Uiso 1 1 calc R . . C30 C 0.1350(3) 0.21336(19) 0.63639(14) 0.0480(5) Uani 1 1 d . . . H30A H 0.1909 0.1339 0.6387 0.072 Uiso 1 1 calc R . . H30B H 0.0679 0.2246 0.5961 0.072 Uiso 1 1 calc R . . H30C H 0.0634 0.2345 0.6826 0.072 Uiso 1 1 calc R . . C31 C 0.2557(3) 0.2115(2) 0.87240(14) 0.0574(6) Uani 1 1 d D . . H31A H 0.2792 0.1673 0.8267 0.069 Uiso 1 1 calc R A 1 H31B H 0.1420 0.2580 0.8757 0.069 Uiso 1 1 calc R A 1 C32 C 0.2743(8) 0.1334(7) 0.9388(4) 0.075(3) Uani 0.60 1 d PD B 1 H32A H 0.2619 0.0569 0.9274 0.090 Uiso 0.60 1 calc PR B 1 H32B H 0.1909 0.1633 0.9809 0.090 Uiso 0.60 1 calc PR B 1 C33 C 0.4493(6) 0.1315(4) 0.9554(3) 0.0507(14) Uani 0.60 1 d PD B 1 H33A H 0.4601 0.1148 1.0076 0.061 Uiso 0.60 1 calc PR B 1 H33B H 0.5333 0.0765 0.9244 0.061 Uiso 0.60 1 calc PR B 1 C34 C 0.4618(4) 0.2505(2) 0.93572(14) 0.0671(8) Uani 1 1 d D . . H34A H 0.4116 0.3012 0.9774 0.081 Uiso 1 1 calc R B 1 H34B H 0.5791 0.2557 0.9231 0.081 Uiso 1 1 calc R B 1 H6 H 0.464(2) 0.1170(18) 0.5922(10) 0.041(6) Uiso 1 1 d D . . H3 H 0.393(2) 0.7214(18) 0.6442(7) 0.037(6) Uiso 1 1 d D . . C33A C 0.3781(15) 0.1655(8) 0.9766(5) 0.071(3) Uani 0.40 1 d PD B 2 H33C H 0.2869 0.2022 1.0137 0.086 Uiso 0.40 1 calc PR B 2 H33D H 0.4576 0.1092 1.0012 0.086 Uiso 0.40 1 calc PR B 2 C32A C 0.3115(13) 0.1104(8) 0.9170(5) 0.059(3) Uani 0.40 1 d PD B 2 H32C H 0.3992 0.0540 0.8890 0.071 Uiso 0.40 1 calc PR B 2 H32D H 0.2186 0.0748 0.9374 0.071 Uiso 0.40 1 calc PR B 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 Ca1 0.0333(2) 0.0249(2) 0.0287(2) 0.00186(14) -0.00634(15) -0.00460(15) F1 0.0431(7) 0.0373(6) 0.0433(6) 0.0042(5) 0.0007(5) -0.0108(5) F2 0.0573(8) 0.0513(8) 0.0688(9) 0.0040(7) -0.0265(7) -0.0144(7) O1 0.0337(7) 0.0407(8) 0.0403(7) -0.0027(6) -0.0073(6) -0.0081(6) O2 0.0490(9) 0.0409(8) 0.0408(8) 0.0087(6) -0.0015(7) -0.0085(7) N1 0.0283(8) 0.0257(8) 0.0361(8) 0.0018(6) -0.0022(6) -0.0040(6) N2 0.0271(8) 0.0308(8) 0.0331(8) 0.0043(6) -0.0045(6) -0.0051(6) N3 0.0301(9) 0.0322(8) 0.0461(10) 0.0120(7) -0.0013(7) -0.0025(7) N4 0.0292(8) 0.0280(8) 0.0355(8) -0.0014(6) -0.0086(6) -0.0004(6) N5 0.0290(8) 0.0282(8) 0.0317(8) 0.0001(6) -0.0061(6) -0.0027(6) N6 0.0315(9) 0.0399(9) 0.0387(9) -0.0110(7) -0.0101(7) 0.0026(7) C1 0.0238(9) 0.0311(9) 0.0371(10) 0.0022(8) -0.0104(7) 0.0007(7) C2 0.0335(10) 0.0329(10) 0.0504(12) 0.0009(9) -0.0149(9) -0.0053(8) C3 0.0486(13) 0.0352(11) 0.0655(15) -0.0099(10) -0.0262(11) -0.0032(9) C4 0.0483(13) 0.0539(14) 0.0443(12) -0.0140(10) -0.0143(10) 0.0049(11) C5 0.0345(11) 0.0491(12) 0.0373(11) -0.0011(9) -0.0077(8) 0.0028(9) C6 0.0293(9) 0.0340(10) 0.0372(10) 0.0010(8) -0.0086(8) -0.0003(8) C7 0.0277(9) 0.0262(9) 0.0389(10) 0.0036(7) -0.0077(8) -0.0079(7) C8 0.0326(10) 0.0328(10) 0.0440(11) 0.0083(8) -0.0070(8) 0.0004(8) C9 0.0410(12) 0.0429(12) 0.0720(16) 0.0057(11) -0.0196(11) -0.0064(10) C10 0.0498(13) 0.0317(11) 0.0645(14) 0.0064(10) -0.0143(11) -0.0018(9) C11 0.0318(10) 0.0381(10) 0.0328(10) 0.0044(8) -0.0040(8) -0.0081(8) C12 0.0363(11) 0.0471(12) 0.0446(11) 0.0062(9) 0.0004(9) -0.0148(9) C13 0.0469(12) 0.0480(12) 0.0366(11) -0.0017(9) 0.0014(9) -0.0107(10) C14 0.0356(11) 0.0464(12) 0.0330(10) -0.0002(8) -0.0098(8) -0.0030(9) C15 0.0418(12) 0.0411(11) 0.0480(12) -0.0048(9) -0.0122(9) -0.0034(9) C16 0.0449(12) 0.0448(12) 0.0467(12) 0.0025(10) -0.0120(10) -0.0114(10) C17 0.0325(10) 0.0475(12) 0.0432(11) -0.0032(9) -0.0055(9) -0.0076(9) C18 0.0288(9) 0.0323(10) 0.0305(9) -0.0025(7) -0.0008(7) 0.0003(7) C19 0.0384(11) 0.0355(11) 0.0507(12) 0.0019(9) -0.0077(9) -0.0049(9) C20 0.0541(14) 0.0376(12) 0.0570(14) 0.0057(10) -0.0049(11) -0.0020(10) C21 0.0567(14) 0.0434(12) 0.0467(12) 0.0116(10) -0.0069(11) 0.0081(10) C22 0.0435(12) 0.0519(13) 0.0415(12) -0.0009(10) -0.0143(10) 0.0050(10) C23 0.0355(10) 0.0350(10) 0.0393(10) -0.0034(8) -0.0084(8) -0.0022(8) C24 0.0308(9) 0.0299(9) 0.0311(9) -0.0003(7) -0.0040(7) -0.0055(7) C25 0.0356(11) 0.0507(13) 0.0425(11) -0.0143(10) -0.0086(9) 0.0065(9) C26 0.070(2) 0.0622(18) 0.116(3) -0.0213(18) 0.0429(19) -0.0076(16) C27 0.0557(15) 0.0412(13) 0.096(2) -0.0234(13) -0.0041(14) 0.0066(11) C28 0.0293(10) 0.0350(10) 0.0371(10) -0.0021(8) -0.0066(8) -0.0038(8) C29 0.0339(10) 0.0360(10) 0.0447(11) 0.0023(9) -0.0127(9) -0.0013(8) C30 0.0375(12) 0.0409(12) 0.0682(15) -0.0031(11) -0.0157(11) -0.0083(9) C31 0.0521(14) 0.0639(16) 0.0583(15) 0.0119(12) -0.0030(12) -0.0218(12) C32 0.053(4) 0.069(5) 0.099(6) 0.043(4) -0.008(4) -0.009(3) C33 0.049(3) 0.046(3) 0.047(3) 0.012(2) 0.008(2) 0.000(2) C34 0.108(2) 0.0645(17) 0.0367(12) 0.0148(11) -0.0175(13) -0.0327(16) C33A 0.105(8) 0.067(6) 0.059(6) 0.026(4) -0.035(5) -0.045(6) C32A 0.062(6) 0.040(4) 0.066(5) -0.004(3) 0.030(4) -0.014(4) _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 Ca1 O2 2.3796(14) . ? Ca1 O1 2.4018(13) . ? Ca1 N5 2.4198(15) . ? Ca1 N2 2.4319(15) . ? Ca1 N4 2.4404(16) . ? Ca1 N1 2.4430(15) . ? Ca1 C24 2.8449(18) . ? Ca1 C7 2.8652(18) . ? Ca1 F1 3.5507(12) . ? Ca1 F2 3.6826(14) . ? F1 C6 1.362(2) . ? F2 C23 1.348(2) . ? O1 C17 1.443(2) . ? O1 C14 1.447(2) . ? O2 C31 1.438(3) . ? O2 C34 1.437(3) . ? N1 C7 1.360(2) . ? N1 C1 1.378(2) . ? N2 C7 1.315(2) . ? N2 C11 1.459(2) . ? N3 C7 1.389(2) . ? N3 C8 1.474(3) . ? N3 H3 0.893(9) . ? N4 C24 1.362(2) . ? N4 C18 1.379(2) . ? N5 C24 1.312(2) . ? N5 C28 1.460(2) . ? N6 C24 1.393(2) . ? N6 C25 1.460(3) . ? N6 H6 0.897(9) . ? C1 C2 1.413(3) . ? C1 C6 1.412(3) . ? C2 C3 1.391(3) . ? C2 H2 0.9500 . ? C3 C4 1.376(4) . ? C3 H3A 0.9500 . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C8 C9 1.511(3) . ? C8 C10 1.520(3) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.521(3) . ? C11 C12 1.534(3) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.531(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.508(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.401(3) . ? C18 C19 1.415(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.375(4) . ? C20 H20 0.9500 . ? C21 C22 1.390(3) . ? C21 H21 0.9500 . ? C22 C23 1.374(3) . ? C22 H22 0.9500 . ? C25 C27 1.495(3) . ? C25 C26 1.537(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.511(3) . ? C28 C30 1.537(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32A 1.480(10) . ? C31 C32 1.527(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.528(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.497(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C33A 1.493(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C33A C32A 1.531(5) . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca1 O1 86.36(5) . . ? O2 Ca1 N5 96.43(5) . . ? O1 Ca1 N5 156.57(5) . . ? O2 Ca1 N2 160.00(6) . . ? O1 Ca1 N2 89.32(5) . . ? N5 Ca1 N2 95.27(5) . . ? O2 Ca1 N4 83.59(5) . . ? O1 Ca1 N4 101.76(5) . . ? N5 Ca1 N4 55.75(5) . . ? N2 Ca1 N4 116.41(5) . . ? O2 Ca1 N1 104.88(5) . . ? O1 Ca1 N1 88.31(5) . . ? N5 Ca1 N1 113.17(5) . . ? N2 Ca1 N1 55.42(5) . . ? N4 Ca1 N1 167.36(5) . . ? O2 Ca1 C24 92.46(5) . . ? O1 Ca1 C24 129.55(5) . . ? N5 Ca1 C24 27.36(5) . . ? N2 Ca1 C24 105.25(5) . . ? N4 Ca1 C24 28.58(5) . . ? N1 Ca1 C24 139.69(5) . . ? O2 Ca1 C7 133.15(6) . . ? O1 Ca1 C7 89.91(5) . . ? N5 Ca1 C7 104.56(5) . . ? N2 Ca1 C7 27.20(5) . . ? N4 Ca1 C7 142.47(5) . . ? N1 Ca1 C7 28.27(5) . . ? C24 Ca1 C7 124.11(5) . . ? O2 Ca1 F1 56.64(4) . . ? O1 Ca1 F1 93.86(4) . . ? N5 Ca1 F1 107.14(4) . . ? N2 Ca1 F1 104.29(4) . . ? N4 Ca1 F1 136.21(4) . . ? N1 Ca1 F1 49.14(4) . . ? C24 Ca1 F1 126.70(4) . . ? C7 Ca1 F1 77.12(4) . . ? O2 Ca1 F2 80.24(4) . . ? O1 Ca1 F2 54.46(4) . . ? N5 Ca1 F2 102.96(4) . . ? N2 Ca1 F2 112.76(4) . . ? N4 Ca1 F2 47.34(4) . . ? N1 Ca1 F2 142.40(4) . . ? C24 Ca1 F2 75.61(4) . . ? C7 Ca1 F2 132.43(4) . . ? F1 Ca1 F2 129.11(3) . . ? C6 F1 Ca1 97.50(10) . . ? C23 F2 Ca1 96.04(10) . . ? C17 O1 C14 107.08(14) . . ? C17 O1 Ca1 117.24(11) . . ? C14 O1 Ca1 126.38(11) . . ? C31 O2 C34 109.15(17) . . ? C31 O2 Ca1 121.54(13) . . ? C34 O2 Ca1 125.47(15) . . ? C7 N1 C1 123.25(15) . . ? C7 N1 Ca1 93.39(11) . . ? C1 N1 Ca1 131.29(12) . . ? C7 N2 C11 121.38(15) . . ? C7 N2 Ca1 95.08(11) . . ? C11 N2 Ca1 140.82(12) . . ? C7 N3 C8 123.67(16) . . ? C7 N3 H3 111.4(14) . . ? C8 N3 H3 112.9(15) . . ? C24 N4 C18 122.52(16) . . ? C24 N4 Ca1 92.44(11) . . ? C18 N4 Ca1 133.43(12) . . ? C24 N5 C28 121.56(16) . . ? C24 N5 Ca1 94.68(11) . . ? C28 N5 Ca1 139.74(12) . . ? C24 N6 C25 123.28(16) . . ? C24 N6 H6 110.4(14) . . ? C25 N6 H6 113.5(15) . . ? N1 C1 C2 127.88(18) . . ? N1 C1 C6 118.04(16) . . ? C2 C1 C6 113.90(18) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 122.2(2) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 118.5(2) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 118.9(2) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? F1 C6 C5 117.45(18) . . ? F1 C6 C1 117.45(17) . . ? C5 C6 C1 125.08(19) . . ? N2 C7 N1 115.90(15) . . ? N2 C7 N3 122.66(17) . . ? N1 C7 N3 121.43(17) . . ? N2 C7 Ca1 57.72(9) . . ? N1 C7 Ca1 58.34(9) . . ? N3 C7 Ca1 175.12(13) . . ? N3 C8 C9 111.96(18) . . ? N3 C8 C10 107.93(17) . . ? C9 C8 C10 112.02(18) . . ? N3 C8 H8 108.3 . . ? C9 C8 H8 108.3 . . ? C10 C8 H8 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C13 108.60(16) . . ? N2 C11 C12 111.61(16) . . ? C13 C11 C12 109.92(17) . . ? N2 C11 H11 108.9 . . ? C13 C11 H11 108.9 . . ? C12 C11 H11 108.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 C15 106.52(16) . . ? O1 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O1 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C16 C15 C14 104.41(17) . . ? C16 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? C16 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C17 C16 C15 102.73(18) . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? O1 C17 C16 103.92(17) . . ? O1 C17 H17A 111.0 . . ? C16 C17 H17A 111.0 . . ? O1 C17 H17B 111.0 . . ? C16 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? N4 C18 C23 119.47(17) . . ? N4 C18 C19 126.85(17) . . ? C23 C18 C19 113.53(18) . . ? C20 C19 C18 122.3(2) . . ? C20 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C21 C20 C19 121.8(2) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 117.9(2) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? F2 C23 C22 117.41(18) . . ? F2 C23 C18 117.83(17) . . ? C22 C23 C18 124.7(2) . . ? N5 C24 N4 116.39(16) . . ? N5 C24 N6 122.76(16) . . ? N4 C24 N6 120.82(17) . . ? N5 C24 Ca1 57.97(9) . . ? N4 C24 Ca1 58.99(9) . . ? N6 C24 Ca1 170.93(13) . . ? N6 C25 C27 109.55(19) . . ? N6 C25 C26 110.4(2) . . ? C27 C25 C26 111.2(2) . . ? N6 C25 H25 108.6 . . ? C27 C25 H25 108.6 . . ? C26 C25 H25 108.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 C29 108.38(15) . . ? N5 C28 C30 111.71(16) . . ? C29 C28 C30 110.04(16) . . ? N5 C28 H28 108.9 . . ? C29 C28 H28 108.9 . . ? C30 C28 H28 108.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C31 C32A 106.3(4) . . ? O2 C31 C32 105.6(3) . . ? C32A C31 C32 19.9(4) . . ? O2 C31 H31A 110.6 . . ? C32A C31 H31A 92.4 . . ? C32 C31 H31A 110.6 . . ? O2 C31 H31B 110.6 . . ? C32A C31 H31B 126.4 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.8 . . ? C31 C32 C33 104.1(5) . . ? C31 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? C31 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 109.0 . . ? C34 C33 C32 100.2(5) . . ? C34 C33 H33A 111.7 . . ? C32 C33 H33A 111.7 . . ? C34 C33 H33B 111.7 . . ? C32 C33 H33B 111.7 . . ? H33A C33 H33B 109.5 . . ? O2 C34 C33 106.8(3) . . ? O2 C34 C33A 104.8(4) . . ? C33 C34 C33A 27.9(4) . . ? O2 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? C33A C34 H34A 85.8 . . ? O2 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? C33A C34 H34B 133.4 . . ? H34A C34 H34B 108.6 . . ? C34 C33A C32A 103.7(6) . . ? C34 C33A H33C 111.0 . . ? C32A C33A H33C 111.0 . . ? C34 C33A H33D 111.0 . . ? C32A C33A H33D 111.0 . . ? H33C C33A H33D 109.0 . . ? C31 C32A C33A 99.4(7) . . ? C31 C32A H32C 111.9 . . ? C33A C32A H32C 111.9 . . ? C31 C32A H32D 111.9 . . ? C33A C32A H32D 111.9 . . ? H32C C32A H32D 109.6 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.080 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.053 data_768280-k08msh11 _database_code_depnum_ccdc_archive 'CCDC 768280' #TrackingRef '768277-80.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H76 Ca2 F4 N12' _chemical_formula_weight 1025.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7164(2) _cell_length_b 14.7870(2) _cell_length_c 18.3215(3) _cell_angle_alpha 85.925(1) _cell_angle_beta 80.722(1) _cell_angle_gamma 79.709(1) _cell_volume 2816.54(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 70496 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51547 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.53 _reflns_number_total 12871 _reflns_number_gt 9679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Asymmetric consists of 2 crystallographically independent dimmer halves. The fluorine atoms on the non-ligated aromatic rings exhibited disorder for F21, F2A (65% occupancy) and F22, F2B (35% occupancy). The associated partial hydrogen atoms were not included in the refinement. Efforts (FLAT instruction in SHELXL) to maintain planarity between the aromatic rings and the minor fluorine fragments above proved largely ineffective, perhaps a function of minimal electron density in the areas of the electron density map. ; _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^)+(0.0636P)^2^+1.3456P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12871 _refine_ls_number_parameters 666 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.00371(3) 1.47410(3) 0.90404(2) 0.02550(10) Uani 1 1 d . . . Ca2 Ca 0.55497(3) 0.97080(3) 0.403618(19) 0.02531(10) Uani 1 1 d . . . F1 F 0.12734(12) 1.31668(8) 0.91187(7) 0.0423(3) Uani 1 1 d . . . F21 F 0.0078(2) 1.59507(14) 0.68342(11) 0.0493(5) Uani 0.65 1 d PD A 1 F22 F 0.1799(4) 1.2973(2) 0.7568(2) 0.0472(9) Uani 0.35 1 d PD A 2 F1A F 0.48455(13) 0.81947(8) 0.42353(8) 0.0456(3) Uani 1 1 d . . . F2A F 0.54282(19) 0.78696(12) 0.26524(10) 0.0401(4) Uani 0.65 1 d PD B 1 F2B F 0.5952(4) 1.0886(3) 0.1888(3) 0.0599(11) Uani 0.35 1 d PD B 2 N1 N -0.01313(16) 1.44144(12) 0.78190(9) 0.0335(4) Uani 1 1 d . . . N2 N -0.18197(15) 1.53319(12) 0.84552(9) 0.0312(4) Uani 1 1 d . . . N3 N -0.20024(17) 1.49123(13) 0.72543(10) 0.0384(4) Uani 1 1 d . . . H31 H -0.2546 1.5413 0.7163 0.046 Uiso 1 1 calc R . . N4 N 0.20832(14) 1.52044(11) 0.89929(8) 0.0271(3) Uani 1 1 d . . . N5 N 0.24217(17) 1.66244(12) 0.93723(10) 0.0358(4) Uani 1 1 d . . . H51 H 0.3070 1.6639 0.9012 0.043 Uiso 1 1 calc R . . N6 N -0.04579(14) 1.39334(10) 1.02394(8) 0.0254(3) Uani 1 1 d . . . N1A N 0.65759(15) 0.93297(12) 0.28175(9) 0.0309(4) Uani 1 1 d . . . N2A N 0.74171(15) 1.03055(12) 0.34262(9) 0.0310(4) Uani 1 1 d . . . N3A N 0.84307(17) 0.99147(13) 0.22116(10) 0.0382(4) Uani 1 1 d . . . H3A1 H 0.8729 1.0434 0.2113 0.046 Uiso 1 1 calc R . . N4A N 0.32988(14) 1.02182(11) 0.39940(8) 0.0270(3) Uani 1 1 d . . . N5A N 0.20298(16) 1.15912(12) 0.44536(10) 0.0352(4) Uani 1 1 d . . . H5A H 0.1518 1.1593 0.4123 0.042 Uiso 1 1 calc R . . N6A N 0.58775(14) 0.89373(10) 0.52455(8) 0.0256(3) Uani 1 1 d . . . C1 C 0.12642(19) 1.27141(14) 0.98027(12) 0.0354(5) Uani 1 1 d . . . C2 C 0.2144(2) 1.19234(15) 0.98685(17) 0.0494(6) Uani 1 1 d . . . H2 H 0.2768 1.1711 0.9460 0.059 Uiso 1 1 calc R . . C3 C 0.2092(3) 1.14510(17) 1.05410(19) 0.0609(8) Uani 1 1 d . . . H3 H 0.2680 1.0899 1.0604 0.073 Uiso 1 1 calc R . . C4 C 0.1178(3) 1.17833(17) 1.11288(16) 0.0580(7) Uani 1 1 d . . . H4 H 0.1139 1.1452 1.1593 0.070 Uiso 1 1 calc R . . C5 C 0.0315(2) 1.25943(15) 1.10492(13) 0.0430(5) Uani 1 1 d . . . H5 H -0.0295 1.2814 1.1461 0.052 Uiso 1 1 calc R . . C6 C 0.03381(18) 1.30894(13) 1.03701(11) 0.0298(4) Uani 1 1 d . . . C7 C -0.13358(19) 1.49061(14) 0.78438(11) 0.0317(4) Uani 1 1 d . . . C8 C 0.07506(19) 1.43864(14) 0.71766(11) 0.0321(4) Uani 1 1 d D A . C9 C 0.0836(2) 1.51210(16) 0.66570(13) 0.0419(5) Uani 1 1 d D . . C10 C 0.1748(2) 1.50831(19) 0.60336(13) 0.0486(6) Uani 1 1 d D A . H10 H 0.1745 1.5594 0.5688 0.058 Uiso 1 1 calc R . . C11 C 0.2666(2) 1.43071(18) 0.59093(13) 0.0454(5) Uani 1 1 d . . . H11 H 0.3295 1.4275 0.5478 0.054 Uiso 1 1 calc R A . C12 C 0.2657(2) 1.35785(17) 0.64212(12) 0.0431(5) Uani 1 1 d D A . H12 H 0.3298 1.3046 0.6350 0.052 Uiso 1 1 calc R . . C13 C 0.1717(2) 1.36177(15) 0.70399(11) 0.0366(5) Uani 1 1 d D . . C14 C -0.31629(19) 1.57829(16) 0.85728(12) 0.0383(5) Uani 1 1 d . . . H14 H -0.3696 1.5384 0.8388 0.046 Uiso 1 1 calc R . . C15 C -0.3352(3) 1.67212(17) 0.81663(15) 0.0541(6) Uani 1 1 d . . . H15A H -0.2880 1.7131 0.8368 0.081 Uiso 1 1 calc R . . H15B H -0.4267 1.6984 0.8231 0.081 Uiso 1 1 calc R . . H15C H -0.3029 1.6652 0.7638 0.081 Uiso 1 1 calc R . . C16 C -0.3583(2) 1.5883(2) 0.93986(13) 0.0517(6) Uani 1 1 d . . . H16A H -0.3445 1.5276 0.9654 0.078 Uiso 1 1 calc R . . H16B H -0.4496 1.6151 0.9493 0.078 Uiso 1 1 calc R . . H16C H -0.3081 1.6286 0.9582 0.078 Uiso 1 1 calc R . . C17 C 0.16912(17) 1.59539(13) 0.93549(10) 0.0259(4) Uani 1 1 d . . . C18 C 0.34119(18) 1.50067(14) 0.86111(11) 0.0322(4) Uani 1 1 d . . . H18 H 0.3985 1.5238 0.8909 0.039 Uiso 1 1 calc R . . C19 C 0.3533(2) 1.54830(17) 0.78471(12) 0.0434(5) Uani 1 1 d . . . H19A H 0.2969 1.5264 0.7552 0.065 Uiso 1 1 calc R . . H19B H 0.4424 1.5343 0.7601 0.065 Uiso 1 1 calc R . . H19C H 0.3284 1.6149 0.7894 0.065 Uiso 1 1 calc R . . C20 C 0.3821(2) 1.39729(15) 0.85489(13) 0.0396(5) Uani 1 1 d . . . H20A H 0.3709 1.3671 0.9043 0.059 Uiso 1 1 calc R . . H20B H 0.4726 1.3838 0.8326 0.059 Uiso 1 1 calc R . . H20C H 0.3293 1.3744 0.8237 0.059 Uiso 1 1 calc R . . C21 C 0.2227(2) 1.73170(14) 0.99308(13) 0.0382(5) Uani 1 1 d . . . H21 H 0.1284 1.7527 1.0071 0.046 Uiso 1 1 calc R . . C22 C 0.2822(3) 1.81312(17) 0.95773(18) 0.0620(7) Uani 1 1 d . . . H22A H 0.3751 1.7941 0.9449 0.093 Uiso 1 1 calc R . . H22B H 0.2646 1.8626 0.9927 0.093 Uiso 1 1 calc R . . H22C H 0.2452 1.8352 0.9128 0.093 Uiso 1 1 calc R . . C23 C 0.2780(3) 1.69349(18) 1.06216(13) 0.0504(6) Uani 1 1 d . . . H23A H 0.2373 1.6413 1.0834 0.076 Uiso 1 1 calc R . . H23B H 0.2618 1.7415 1.0984 0.076 Uiso 1 1 calc R . . H23C H 0.3707 1.6730 1.0494 0.076 Uiso 1 1 calc R . . C24 C -0.1860(2) 1.41374(16) 0.67732(12) 0.0413(5) Uani 1 1 d . . . H24 H -0.0935 1.3844 0.6693 0.050 Uiso 1 1 calc R . . C25 C -0.2230(4) 1.4479(2) 0.60420(15) 0.0820(11) Uani 1 1 d . . . H25A H -0.3121 1.4798 0.6111 0.123 Uiso 1 1 calc R . . H25B H -0.2145 1.3957 0.5725 0.123 Uiso 1 1 calc R . . H25C H -0.1667 1.4905 0.5808 0.123 Uiso 1 1 calc R . . C26 C -0.2633(4) 1.3425(2) 0.71215(17) 0.0787(10) Uani 1 1 d . . . H26A H -0.2373 1.3211 0.7602 0.118 Uiso 1 1 calc R . . H26B H -0.2485 1.2904 0.6798 0.118 Uiso 1 1 calc R . . H26C H -0.3546 1.3694 0.7192 0.118 Uiso 1 1 calc R . . C30 C 0.5500(2) 0.75902(16) 0.60956(14) 0.0465(6) Uani 1 1 d . . . H30 H 0.5879 0.7811 0.6467 0.056 Uiso 1 1 calc R . . C1A C 0.48685(19) 0.77257(14) 0.49088(13) 0.0381(5) Uani 1 1 d . . . C2A C 0.4363(2) 0.69224(17) 0.50353(19) 0.0569(7) Uani 1 1 d . . . H2A H 0.3968 0.6702 0.4671 0.068 Uiso 1 1 calc R . . C3A C 0.4448(3) 0.64478(18) 0.5708(2) 0.0691(9) Uani 1 1 d . . . H3A H 0.4112 0.5892 0.5811 0.083 Uiso 1 1 calc R . . C4A C 0.5019(3) 0.67807(18) 0.62298(18) 0.0635(8) Uani 1 1 d . . . H4A H 0.5082 0.6448 0.6689 0.076 Uiso 1 1 calc R . . C5A C 0.54400(18) 0.80989(13) 0.54163(11) 0.0309(4) Uani 1 1 d . . . C7A C 0.74820(18) 0.98704(14) 0.28161(11) 0.0300(4) Uani 1 1 d . . . C8A C 0.59949(17) 0.93015(14) 0.21980(10) 0.0294(4) Uani 1 1 d D B . C9A C 0.5430(2) 0.85430(15) 0.21064(12) 0.0369(5) Uani 1 1 d D . . C10A C 0.4739(2) 0.84963(16) 0.15418(13) 0.0448(5) Uani 1 1 d D B . H10A H 0.4363 0.7968 0.1509 0.054 Uiso 1 1 calc R . . C11A C 0.4593(2) 0.92121(18) 0.10260(13) 0.0465(6) Uani 1 1 d . . . H11A H 0.4124 0.9184 0.0633 0.056 Uiso 1 1 calc R B . C12A C 0.5138(2) 0.99694(19) 0.10889(14) 0.0528(6) Uani 1 1 d D B . H12A H 0.5048 1.0468 0.0734 0.063 Uiso 1 1 calc R . . C13A C 0.5815(2) 1.00163(17) 0.16620(13) 0.0459(5) Uani 1 1 d D . . C14A C 0.84446(19) 1.07953(15) 0.35271(12) 0.0364(5) Uani 1 1 d . . . H14A H 0.9286 1.0424 0.3320 0.044 Uiso 1 1 calc R . . C15A C 0.8315(3) 1.17410(18) 0.31304(15) 0.0538(6) Uani 1 1 d . . . H15D H 0.8338 1.1673 0.2600 0.081 Uiso 1 1 calc R . . H15E H 0.9025 1.2043 0.3204 0.081 Uiso 1 1 calc R . . H15F H 0.7498 1.2115 0.3332 0.081 Uiso 1 1 calc R . . C16A C 0.8416(2) 1.08763(19) 0.43526(13) 0.0463(6) Uani 1 1 d . . . H16D H 0.7581 1.1215 0.4567 0.070 Uiso 1 1 calc R . . H16E H 0.9097 1.1206 0.4431 0.070 Uiso 1 1 calc R . . H16F H 0.8552 1.0260 0.4592 0.070 Uiso 1 1 calc R . . C17A C 0.31232(17) 1.09484(13) 0.43841(10) 0.0258(4) Uani 1 1 d . . . C18A C 0.22513(18) 1.00312(14) 0.36294(11) 0.0319(4) Uani 1 1 d . . . H18A H 0.1416 1.0247 0.3948 0.038 Uiso 1 1 calc R . . C19A C 0.2260(2) 1.05478(17) 0.28815(12) 0.0433(5) Uani 1 1 d . . . H19D H 0.2146 1.1210 0.2951 0.065 Uiso 1 1 calc R . . H19E H 0.1559 1.0416 0.2645 0.065 Uiso 1 1 calc R . . H19F H 0.3081 1.0350 0.2567 0.065 Uiso 1 1 calc R . . C20A C 0.2387(2) 0.90012(15) 0.35408(12) 0.0387(5) Uani 1 1 d . . . H20D H 0.3199 0.8783 0.3225 0.058 Uiso 1 1 calc R . . H20E H 0.1671 0.8877 0.3313 0.058 Uiso 1 1 calc R . . H20F H 0.2377 0.8680 0.4028 0.058 Uiso 1 1 calc R . . C21A C 0.16176(19) 1.22798(14) 0.50225(12) 0.0351(4) Uani 1 1 d . . . H21A H 0.2399 1.2461 0.5165 0.042 Uiso 1 1 calc R . . C22A C 0.0842(3) 1.31233(17) 0.46861(17) 0.0592(7) Uani 1 1 d . . . H22D H 0.1363 1.3354 0.4247 0.089 Uiso 1 1 calc R . . H22E H 0.0591 1.3603 0.5050 0.089 Uiso 1 1 calc R . . H22F H 0.0071 1.2957 0.4545 0.089 Uiso 1 1 calc R . . C23A C 0.0862(3) 1.19017(18) 0.57036(13) 0.0499(6) Uani 1 1 d . . . H23D H 0.0090 1.1724 0.5574 0.075 Uiso 1 1 calc R . . H23E H 0.0614 1.2373 0.6074 0.075 Uiso 1 1 calc R . . H23F H 0.1390 1.1361 0.5907 0.075 Uiso 1 1 calc R . . C24A C 0.8969(2) 0.91526(16) 0.17258(11) 0.0369(5) Uani 1 1 d . . . H24A H 0.8260 0.8822 0.1662 0.044 Uiso 1 1 calc R . . C25A C 0.9503(3) 0.95267(19) 0.09774(14) 0.0588(7) Uani 1 1 d . . . H25D H 0.8808 0.9909 0.0752 0.088 Uiso 1 1 calc R . . H25E H 0.9900 0.9015 0.0659 0.088 Uiso 1 1 calc R . . H25F H 1.0150 0.9899 0.1033 0.088 Uiso 1 1 calc R . . C26A C 0.9985(3) 0.8471(2) 0.20619(15) 0.0589(7) Uani 1 1 d . . . H26D H 1.0729 0.8765 0.2082 0.088 Uiso 1 1 calc R . . H26E H 1.0251 0.7933 0.1756 0.088 Uiso 1 1 calc R . . H26F H 0.9629 0.8278 0.2564 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 Ca1 0.02409(19) 0.0306(2) 0.02367(19) -0.00061(14) -0.00546(14) -0.00823(14) Ca2 0.01995(18) 0.0332(2) 0.02246(18) -0.00253(14) -0.00252(13) -0.00378(14) F1 0.0407(7) 0.0364(6) 0.0440(7) -0.0050(5) 0.0072(5) -0.0019(5) F21 0.0480(12) 0.0421(11) 0.0482(12) 0.0048(9) 0.0008(9) 0.0084(9) F22 0.048(2) 0.0379(19) 0.049(2) -0.0034(17) 0.0021(17) 0.0043(16) F1A 0.0485(8) 0.0367(7) 0.0587(8) -0.0118(6) -0.0264(6) -0.0054(6) F2A 0.0499(11) 0.0338(9) 0.0418(10) 0.0003(8) -0.0155(9) -0.0142(8) F2B 0.066(3) 0.053(2) 0.072(3) 0.021(2) -0.032(2) -0.030(2) N1 0.0305(9) 0.0410(9) 0.0278(8) -0.0075(7) -0.0064(7) 0.0012(7) N2 0.0241(8) 0.0401(9) 0.0302(8) -0.0079(7) -0.0066(6) -0.0032(7) N3 0.0364(9) 0.0435(10) 0.0367(9) -0.0125(8) -0.0158(8) 0.0031(8) N4 0.0226(8) 0.0326(8) 0.0266(8) -0.0041(6) -0.0013(6) -0.0070(6) N5 0.0329(9) 0.0378(9) 0.0390(9) -0.0082(7) 0.0038(7) -0.0177(7) N6 0.0231(8) 0.0248(7) 0.0279(8) -0.0004(6) -0.0031(6) -0.0040(6) N1A 0.0289(8) 0.0401(9) 0.0258(8) -0.0073(7) -0.0009(6) -0.0117(7) N2A 0.0234(8) 0.0400(9) 0.0305(8) -0.0090(7) -0.0002(6) -0.0086(7) N3A 0.0351(9) 0.0448(10) 0.0362(9) -0.0135(8) 0.0077(7) -0.0182(8) N4A 0.0215(7) 0.0344(8) 0.0261(8) -0.0033(6) -0.0049(6) -0.0053(6) N5A 0.0288(9) 0.0396(9) 0.0366(9) -0.0085(7) -0.0129(7) 0.0055(7) N6A 0.0242(8) 0.0264(8) 0.0272(8) -0.0004(6) -0.0050(6) -0.0059(6) C1 0.0281(10) 0.0297(10) 0.0499(12) -0.0033(9) -0.0082(9) -0.0059(8) C2 0.0303(11) 0.0323(11) 0.0862(19) -0.0113(12) -0.0126(11) 0.0001(9) C3 0.0521(16) 0.0354(13) 0.099(2) 0.0020(14) -0.0392(16) 0.0043(11) C4 0.0767(19) 0.0392(13) 0.0647(17) 0.0166(12) -0.0389(15) -0.0099(13) C5 0.0508(14) 0.0384(12) 0.0436(12) 0.0074(10) -0.0204(10) -0.0098(10) C6 0.0268(9) 0.0263(9) 0.0397(11) -0.0007(8) -0.0123(8) -0.0069(7) C7 0.0289(10) 0.0358(10) 0.0316(10) -0.0023(8) -0.0082(8) -0.0049(8) C8 0.0273(10) 0.0403(11) 0.0310(10) -0.0071(8) -0.0098(8) -0.0049(8) C9 0.0356(11) 0.0441(12) 0.0409(12) -0.0012(10) -0.0008(9) 0.0023(9) C10 0.0383(12) 0.0622(15) 0.0412(13) 0.0038(11) -0.0018(10) -0.0039(11) C11 0.0343(12) 0.0635(15) 0.0354(12) -0.0074(11) 0.0022(9) -0.0053(10) C12 0.0336(11) 0.0525(14) 0.0398(12) -0.0148(10) -0.0010(9) 0.0029(10) C13 0.0356(11) 0.0412(11) 0.0330(11) -0.0101(9) -0.0038(8) -0.0044(9) C14 0.0269(10) 0.0485(12) 0.0402(12) -0.0155(10) -0.0081(8) -0.0005(9) C15 0.0470(14) 0.0512(14) 0.0625(16) -0.0147(12) -0.0195(12) 0.0105(11) C16 0.0316(12) 0.0790(18) 0.0425(13) -0.0235(12) -0.0024(10) 0.0009(11) C17 0.0259(9) 0.0293(9) 0.0235(9) 0.0022(7) -0.0041(7) -0.0085(7) C18 0.0236(9) 0.0419(11) 0.0309(10) -0.0065(8) 0.0016(7) -0.0087(8) C19 0.0397(12) 0.0550(14) 0.0336(11) 0.0001(10) 0.0036(9) -0.0120(10) C20 0.0302(11) 0.0439(12) 0.0413(12) -0.0094(10) 0.0036(9) -0.0025(9) C21 0.0297(10) 0.0349(11) 0.0527(13) -0.0144(10) -0.0031(9) -0.0104(8) C22 0.0718(19) 0.0384(13) 0.083(2) -0.0046(13) -0.0159(15) -0.0234(13) C23 0.0514(14) 0.0560(15) 0.0461(14) -0.0167(11) -0.0015(11) -0.0150(12) C24 0.0338(11) 0.0536(13) 0.0380(12) -0.0191(10) -0.0077(9) -0.0027(10) C25 0.156(4) 0.0691(19) 0.0394(15) -0.0029(13) -0.0369(18) -0.049(2) C26 0.137(3) 0.0471(16) 0.0530(17) -0.0071(13) 0.0007(18) -0.0311(18) C30 0.0476(13) 0.0407(12) 0.0453(13) 0.0072(10) 0.0067(10) -0.0073(10) C1A 0.0267(10) 0.0290(10) 0.0579(14) -0.0039(9) -0.0050(9) -0.0034(8) C2A 0.0294(12) 0.0391(13) 0.105(2) -0.0210(14) -0.0066(13) -0.0098(10) C3A 0.0454(15) 0.0351(13) 0.118(3) 0.0115(16) 0.0167(16) -0.0137(11) C4A 0.0602(17) 0.0446(14) 0.077(2) 0.0165(14) 0.0150(15) -0.0146(13) C5A 0.0224(9) 0.0260(9) 0.0417(11) -0.0014(8) 0.0021(8) -0.0032(7) C7A 0.0241(9) 0.0368(10) 0.0294(10) -0.0055(8) -0.0001(7) -0.0074(8) C8A 0.0223(9) 0.0379(10) 0.0272(9) -0.0076(8) 0.0010(7) -0.0045(8) C9A 0.0401(12) 0.0378(11) 0.0346(11) -0.0080(9) -0.0083(9) -0.0062(9) C10A 0.0438(13) 0.0460(13) 0.0500(14) -0.0164(11) -0.0174(10) -0.0070(10) C11A 0.0381(12) 0.0666(16) 0.0370(12) -0.0111(11) -0.0143(9) -0.0033(11) C12A 0.0492(14) 0.0664(17) 0.0456(14) 0.0134(12) -0.0168(11) -0.0149(12) C13A 0.0472(13) 0.0481(13) 0.0474(13) 0.0036(10) -0.0158(11) -0.0163(11) C14A 0.0251(10) 0.0460(12) 0.0398(11) -0.0155(9) 0.0027(8) -0.0120(9) C15A 0.0518(15) 0.0532(15) 0.0605(16) -0.0141(12) 0.0021(12) -0.0248(12) C16A 0.0319(11) 0.0675(16) 0.0446(13) -0.0238(11) -0.0027(9) -0.0160(11) C17A 0.0234(9) 0.0296(9) 0.0233(9) 0.0014(7) -0.0027(7) -0.0035(7) C18A 0.0213(9) 0.0450(11) 0.0311(10) -0.0083(8) -0.0069(7) -0.0048(8) C19A 0.0379(12) 0.0598(14) 0.0360(12) 0.0021(10) -0.0144(9) -0.0121(10) C20A 0.0322(11) 0.0471(12) 0.0413(12) -0.0110(10) -0.0117(9) -0.0100(9) C21A 0.0288(10) 0.0329(10) 0.0432(12) -0.0093(9) -0.0091(8) 0.0020(8) C22A 0.0623(17) 0.0376(13) 0.0723(18) -0.0047(12) -0.0160(14) 0.0119(12) C23A 0.0530(14) 0.0507(14) 0.0439(13) -0.0117(11) 0.0000(11) -0.0063(11) C24A 0.0297(10) 0.0492(12) 0.0330(11) -0.0149(9) 0.0026(8) -0.0111(9) C25A 0.0754(19) 0.0577(16) 0.0373(13) -0.0110(11) 0.0156(12) -0.0134(14) C26A 0.0607(17) 0.0614(17) 0.0526(15) -0.0125(13) -0.0090(13) -0.0009(13) _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 Ca1 N1 2.3639(16) . ? Ca1 N4 2.3982(16) . ? Ca1 N2 2.4096(16) . ? Ca1 N6 2.4518(16) . ? Ca1 F1 2.4711(13) . ? Ca1 N6 2.5811(16) 2_587 ? Ca1 C7 2.805(2) . ? Ca1 C17 2.8815(19) . ? Ca1 Ca1 3.6371(7) 2_587 ? Ca2 N1A 2.3820(16) . ? Ca2 N4A 2.4074(15) . ? Ca2 N2A 2.4091(16) . ? Ca2 N6A 2.4659(16) . ? Ca2 F1A 2.4716(13) . ? Ca2 N6A 2.5913(15) 2_676 ? Ca2 C7A 2.8198(19) . ? Ca2 C17A 2.9086(18) . ? Ca2 Ca2 3.6517(7) 2_676 ? F1 C1 1.378(3) . ? F21 C9 1.373(3) . ? F22 C13 1.311(4) . ? F1A C1A 1.373(3) . ? F2A C9A 1.360(3) . ? F2B C13A 1.418(5) . ? N1 C7 1.359(3) . ? N1 C8 1.384(3) . ? N2 C7 1.310(3) . ? N2 C14 1.463(3) . ? N3 C7 1.386(2) . ? N3 C24 1.466(3) . ? N4 C17 1.301(2) . ? N4 C18 1.470(2) . ? N5 C17 1.373(2) . ? N5 C21 1.464(3) . ? N6 C17 1.396(2) 2_587 ? N6 C6 1.409(2) . ? N6 Ca1 2.5811(15) 2_587 ? N1A C7A 1.363(2) . ? N1A C8A 1.386(2) . ? N2A C7A 1.315(2) . ? N2A C14A 1.463(2) . ? N3A C7A 1.384(2) . ? N3A C24A 1.463(3) . ? N4A C17A 1.306(2) . ? N4A C18A 1.470(2) . ? N5A C17A 1.365(2) . ? N5A C21A 1.470(3) . ? N6A C17A 1.397(2) 2_676 ? N6A C5A 1.400(2) . ? N6A Ca2 2.5913(15) 2_676 ? C1 C2 1.376(3) . ? C1 C6 1.388(3) . ? C2 C3 1.371(4) . ? C3 C4 1.387(4) . ? C4 C5 1.391(3) . ? C5 C6 1.397(3) . ? C8 C9 1.398(3) . ? C8 C13 1.401(3) . ? C9 C10 1.376(3) . ? C10 C11 1.378(3) . ? C11 C12 1.378(3) . ? C12 C13 1.387(3) . ? C14 C16 1.517(3) . ? C14 C15 1.524(3) . ? C17 N6 1.396(2) 2_587 ? C18 C19 1.519(3) . ? C18 C20 1.520(3) . ? C21 C23 1.514(3) . ? C21 C22 1.518(3) . ? C24 C25 1.487(4) . ? C24 C26 1.500(4) . ? C30 C4A 1.377(4) . ? C30 C5A 1.412(3) . ? C1A C2A 1.382(3) . ? C1A C5A 1.386(3) . ? C2A C3A 1.383(4) . ? C3A C4A 1.375(5) . ? C8A C9A 1.398(3) . ? C8A C13A 1.400(3) . ? C9A C10A 1.378(3) . ? C10A C11A 1.373(4) . ? C11A C12A 1.372(4) . ? C12A C13A 1.381(3) . ? C14A C16A 1.521(3) . ? C14A C15A 1.524(4) . ? C17A N6A 1.397(2) 2_676 ? C18A C19A 1.520(3) . ? C18A C20A 1.522(3) . ? C21A C23A 1.504(3) . ? C21A C22A 1.520(3) . ? C24A C25A 1.505(3) . ? C24A C26A 1.521(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 N1 Ca1 N4 106.79(6) . . ? N1 Ca1 N2 56.71(6) . . ? N4 Ca1 N2 133.55(6) . . ? N1 Ca1 N6 132.52(6) . . ? N4 Ca1 N6 107.89(5) . . ? N2 Ca1 N6 113.83(6) . . ? N1 Ca1 F1 86.00(5) . . ? N4 Ca1 F1 84.18(5) . . ? N2 Ca1 F1 130.64(5) . . ? N6 Ca1 F1 66.54(5) . . ? N1 Ca1 N6 139.52(6) . 2_587 ? N4 Ca1 N6 54.98(5) . 2_587 ? N2 Ca1 N6 106.77(5) . 2_587 ? N6 Ca1 N6 87.48(5) . 2_587 ? F1 Ca1 N6 122.27(5) . 2_587 ? N1 Ca1 C7 28.92(6) . . ? N4 Ca1 C7 124.56(6) . . ? N2 Ca1 C7 27.80(5) . . ? N6 Ca1 C7 127.08(6) . . ? F1 Ca1 C7 109.38(5) . . ? N6 Ca1 C7 126.72(5) 2_587 . ? N1 Ca1 C17 122.38(6) . . ? N4 Ca1 C17 26.57(5) . . ? N2 Ca1 C17 120.57(6) . . ? N6 Ca1 C17 102.71(5) . . ? F1 Ca1 C17 106.06(5) . . ? N6 Ca1 C17 28.95(5) 2_587 . ? C7 Ca1 C17 126.97(6) . . ? N1 Ca1 Ca1 174.49(5) . 2_587 ? N4 Ca1 Ca1 78.46(4) . 2_587 ? N2 Ca1 Ca1 118.50(4) . 2_587 ? N6 Ca1 Ca1 45.15(4) . 2_587 ? F1 Ca1 Ca1 96.35(3) . 2_587 ? N6 Ca1 Ca1 42.33(3) 2_587 2_587 ? C7 Ca1 Ca1 146.17(4) . 2_587 ? C17 Ca1 Ca1 61.80(4) . 2_587 ? N1A Ca2 N4A 108.03(6) . . ? N1A Ca2 N2A 56.58(5) . . ? N4A Ca2 N2A 131.47(6) . . ? N1A Ca2 N6A 130.61(6) . . ? N4A Ca2 N6A 110.52(5) . . ? N2A Ca2 N6A 112.27(6) . . ? N1A Ca2 F1A 90.78(5) . . ? N4A Ca2 F1A 81.63(5) . . ? N2A Ca2 F1A 137.07(5) . . ? N6A Ca2 F1A 66.03(5) . . ? N1A Ca2 N6A 140.77(6) . 2_676 ? N4A Ca2 N6A 54.79(5) . 2_676 ? N2A Ca2 N6A 105.45(5) . 2_676 ? N6A Ca2 N6A 87.58(5) . 2_676 ? F1A Ca2 N6A 117.06(5) . 2_676 ? N1A Ca2 C7A 28.85(5) . . ? N4A Ca2 C7A 123.47(6) . . ? N2A Ca2 C7A 27.73(5) . . ? N6A Ca2 C7A 125.86(6) . . ? F1A Ca2 C7A 115.68(5) . . ? N6A Ca2 C7A 125.64(5) 2_676 . ? N1A Ca2 C17A 124.82(6) . . ? N4A Ca2 C17A 26.34(5) . . ? N2A Ca2 C17A 119.79(6) . . ? N6A Ca2 C17A 102.91(5) . . ? F1A Ca2 C17A 101.24(5) . . ? N6A Ca2 C17A 28.69(5) 2_676 . ? C7A Ca2 C17A 126.97(6) . . ? N1A Ca2 Ca2 171.57(4) . 2_676 ? N4A Ca2 Ca2 80.07(4) . 2_676 ? N2A Ca2 Ca2 116.42(4) . 2_676 ? N6A Ca2 Ca2 45.15(4) . 2_676 ? F1A Ca2 Ca2 92.78(4) . 2_676 ? N6A Ca2 Ca2 42.43(3) 2_676 2_676 ? C7A Ca2 Ca2 144.01(4) . 2_676 ? C17A Ca2 Ca2 61.86(4) . 2_676 ? C1 F1 Ca1 118.49(11) . . ? C1A F1A Ca2 120.14(11) . . ? C7 N1 C8 121.41(17) . . ? C7 N1 Ca1 93.85(12) . . ? C8 N1 Ca1 130.94(13) . . ? C7 N2 C14 120.36(16) . . ? C7 N2 Ca1 93.12(12) . . ? C14 N2 Ca1 145.24(13) . . ? C7 N3 C24 124.14(18) . . ? C17 N4 C18 119.82(16) . . ? C17 N4 Ca1 97.91(11) . . ? C18 N4 Ca1 141.07(12) . . ? C17 N5 C21 126.41(17) . . ? C17 N6 C6 115.58(15) 2_587 . ? C17 N6 Ca1 122.37(11) 2_587 . ? C6 N6 Ca1 116.97(12) . . ? C17 N6 Ca1 87.55(10) 2_587 2_587 ? C6 N6 Ca1 113.19(11) . 2_587 ? Ca1 N6 Ca1 92.52(5) . 2_587 ? C7A N1A C8A 120.99(17) . . ? C7A N1A Ca2 93.70(11) . . ? C8A N1A Ca2 127.31(12) . . ? C7A N2A C14A 120.47(16) . . ? C7A N2A Ca2 93.78(12) . . ? C14A N2A Ca2 144.92(12) . . ? C7A N3A C24A 124.15(18) . . ? C17A N4A C18A 119.53(16) . . ? C17A N4A Ca2 98.77(11) . . ? C18A N4A Ca2 141.19(12) . . ? C17A N5A C21A 126.86(16) . . ? C17A N6A C5A 114.27(15) 2_676 . ? C17A N6A Ca2 122.93(11) 2_676 . ? C5A N6A Ca2 117.40(12) . . ? C17A N6A Ca2 88.37(10) 2_676 2_676 ? C5A N6A Ca2 113.24(11) . 2_676 ? Ca2 N6A Ca2 92.42(5) . 2_676 ? C2 C1 F1 118.2(2) . . ? C2 C1 C6 125.2(2) . . ? F1 C1 C6 116.61(17) . . ? C3 C2 C1 118.0(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C5 121.1(2) . . ? C4 C5 C6 120.7(2) . . ? C1 C6 C5 115.36(19) . . ? C1 C6 N6 119.49(18) . . ? C5 C6 N6 125.10(19) . . ? N2 C7 N1 116.28(17) . . ? N2 C7 N3 123.45(18) . . ? N1 C7 N3 120.23(18) . . ? N2 C7 Ca1 59.08(10) . . ? N1 C7 Ca1 57.24(10) . . ? N3 C7 Ca1 175.46(15) . . ? N1 C8 C9 124.44(19) . . ? N1 C8 C13 120.43(19) . . ? C9 C8 C13 114.88(19) . . ? F21 C9 C10 118.8(2) . . ? F21 C9 C8 117.39(19) . . ? C10 C9 C8 123.2(2) . . ? C9 C10 C11 120.2(2) . . ? C12 C11 C10 118.8(2) . . ? C11 C12 C13 120.4(2) . . ? F22 C13 C12 120.1(2) . . ? F22 C13 C8 117.0(2) . . ? C12 C13 C8 122.4(2) . . ? N2 C14 C16 108.06(17) . . ? N2 C14 C15 111.77(19) . . ? C16 C14 C15 110.3(2) . . ? N4 C17 N5 124.13(17) . . ? N4 C17 N6 117.30(16) . 2_587 ? N5 C17 N6 118.56(16) . 2_587 ? N4 C17 Ca1 55.52(9) . . ? N5 C17 Ca1 168.29(13) . . ? N6 C17 Ca1 63.50(9) 2_587 . ? N4 C18 C19 110.68(17) . . ? N4 C18 C20 109.40(16) . . ? C19 C18 C20 110.15(17) . . ? N5 C21 C23 111.95(18) . . ? N5 C21 C22 107.7(2) . . ? C23 C21 C22 111.9(2) . . ? N3 C24 C25 109.8(2) . . ? N3 C24 C26 111.5(2) . . ? C25 C24 C26 110.9(2) . . ? C4A C30 C5A 121.2(3) . . ? F1A C1A C2A 119.5(2) . . ? F1A C1A C5A 116.00(18) . . ? C2A C1A C5A 124.4(2) . . ? C1A C2A C3A 118.1(3) . . ? C4A C3A C2A 120.0(2) . . ? C3A C4A C30 120.9(3) . . ? C1A C5A N6A 120.03(18) . . ? C1A C5A C30 115.33(19) . . ? N6A C5A C30 124.6(2) . . ? N2A C7A N1A 115.93(17) . . ? N2A C7A N3A 123.35(18) . . ? N1A C7A N3A 120.67(17) . . ? N2A C7A Ca2 58.49(10) . . ? N1A C7A Ca2 57.46(9) . . ? N3A C7A Ca2 177.76(14) . . ? N1A C8A C9A 119.75(18) . . ? N1A C8A C13A 125.46(19) . . ? C9A C8A C13A 114.56(18) . . ? F2A C9A C10A 118.1(2) . . ? F2A C9A C8A 118.01(18) . . ? C10A C9A C8A 123.4(2) . . ? C11A C10A C9A 120.1(2) . . ? C12A C11A C10A 118.8(2) . . ? C11A C12A C13A 120.8(2) . . ? C12A C13A C8A 122.4(2) . . ? C12A C13A F2B 119.7(3) . . ? C8A C13A F2B 114.2(2) . . ? N2A C14A C16A 108.32(17) . . ? N2A C14A C15A 111.86(19) . . ? C16A C14A C15A 110.84(19) . . ? N4A C17A N5A 124.08(17) . . ? N4A C17A N6A 117.07(16) . 2_676 ? N5A C17A N6A 118.85(16) . 2_676 ? N4A C17A Ca2 54.88(9) . . ? N5A C17A Ca2 171.96(13) . . ? N6A C17A Ca2 62.94(9) 2_676 . ? N4A C18A C19A 110.37(17) . . ? N4A C18A C20A 109.71(16) . . ? C19A C18A C20A 110.64(17) . . ? N5A C21A C23A 111.49(18) . . ? N5A C21A C22A 108.18(19) . . ? C23A C21A C22A 111.6(2) . . ? N3A C24A C25A 109.48(19) . . ? N3A C24A C26A 111.29(18) . . ? C25A C24A C26A 111.4(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.765 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.054 #===end data_h07msh4 _database_code_depnum_ccdc_archive 'CCDC 768281' #TrackingRef 'bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H80 N4 O2 P2 Sr' _chemical_formula_sum 'C58 H80 N4 O2 P2 Sr' _chemical_formula_weight 1014.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 13.1977(2) _cell_length_b 16.0704(3) _cell_length_c 13.9234(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.2530(10) _cell_angle_gamma 90.00 _cell_volume 2713.17(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25438 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'square plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7344 _exptl_absorpt_correction_T_max 0.8982 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '164 2.0 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36348 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.63 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6172 _reflns_number_gt 4948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0344P)^2^+1.0772P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6172 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0747 _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 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr Sr 0.0000 0.0000 0.0000 0.02325(7) Uani 1 2 d S . . O O 0.02687(12) 0.15633(8) 0.02736(12) 0.0375(3) Uani 1 1 d . B . C1 C -0.05394(19) 0.22001(13) -0.01993(18) 0.0400(5) Uani 1 1 d . . . H1A H -0.0520 0.2629 0.0318 0.048 Uiso 0.50 1 calc PR A 1 H1B H -0.1291 0.1962 -0.0516 0.048 Uiso 0.50 1 calc PR A 1 H1C H -0.0719 0.2486 0.0343 0.048 Uiso 0.50 1 calc PR A 2 H1D H -0.1224 0.1947 -0.0710 0.048 Uiso 0.50 1 calc PR A 2 C2 C -0.0186(10) 0.2565(6) -0.1040(8) 0.0411(18) Uani 0.50 1 d P B 1 H2A H -0.0563 0.2276 -0.1716 0.049 Uiso 0.50 1 calc PR B 1 H2B H -0.0358 0.3166 -0.1139 0.049 Uiso 0.50 1 calc PR B 1 C2A C -0.0100(10) 0.2802(6) -0.0729(9) 0.059(3) Uani 0.50 1 d P B 2 H2C H 0.0005 0.3354 -0.0387 0.071 Uiso 0.50 1 calc PR B 2 H2D H -0.0602 0.2863 -0.1473 0.071 Uiso 0.50 1 calc PR B 2 C3 C 0.1033(2) 0.24219(15) -0.0623(2) 0.0467(6) Uani 1 1 d . . . H3A H 0.1434 0.2958 -0.0456 0.056 Uiso 0.50 1 calc PR B 1 H3B H 0.1237 0.2123 -0.1142 0.056 Uiso 0.50 1 calc PR B 1 H3C H 0.0956 0.2074 -0.1234 0.056 Uiso 0.50 1 calc PR B 2 H3D H 0.1592 0.2860 -0.0529 0.056 Uiso 0.50 1 calc PR B 2 C4 C 0.13127(18) 0.19033(13) 0.03559(18) 0.0398(5) Uani 1 1 d . B . H4A H 0.1836 0.1453 0.0384 0.048 Uiso 1 1 calc R . . H4B H 0.1643 0.2252 0.0990 0.048 Uiso 1 1 calc R . . C5 C -0.24334(14) 0.02537(11) -0.11581(14) 0.0237(3) Uani 1 1 d . . . N1 N -0.17678(12) 0.01259(10) -0.16534(12) 0.0276(3) Uani 1 1 d . . . C11 C -0.21200(14) -0.00160(11) -0.27678(13) 0.0247(3) Uani 1 1 d . . . H11 H -0.2877 0.0216 -0.3145 0.030 Uiso 1 1 calc R . . C12 C -0.21252(16) -0.09519(12) -0.29953(15) 0.0298(4) Uani 1 1 d . . . H12A H -0.1393 -0.1189 -0.2566 0.036 Uiso 1 1 calc R . . H12B H -0.2679 -0.1231 -0.2791 0.036 Uiso 1 1 calc R . . C13 C -0.23911(17) -0.11248(13) -0.41442(16) 0.0370(5) Uani 1 1 d . . . H13A H -0.3151 -0.0935 -0.4570 0.044 Uiso 1 1 calc R . . H13B H -0.2358 -0.1732 -0.4251 0.044 Uiso 1 1 calc R . . C14 C -0.15857(19) -0.06828(14) -0.45085(17) 0.0404(5) Uani 1 1 d . . . H14A H -0.1806 -0.0777 -0.5267 0.048 Uiso 1 1 calc R . . H14B H -0.0837 -0.0916 -0.4138 0.048 Uiso 1 1 calc R . . C15 C -0.15671(19) 0.02477(14) -0.42943(16) 0.0380(5) Uani 1 1 d . . . H15A H -0.1001 0.0518 -0.4489 0.046 Uiso 1 1 calc R . . H15B H -0.2292 0.0492 -0.4731 0.046 Uiso 1 1 calc R . . C16 C -0.13143(16) 0.04174(13) -0.31473(15) 0.0307(4) Uani 1 1 d . . . H16A H -0.1343 0.1025 -0.3042 0.037 Uiso 1 1 calc R . . H16B H -0.0556 0.0226 -0.2720 0.037 Uiso 1 1 calc R . . N2 N -0.19677(12) 0.02560(11) -0.01188(12) 0.0292(3) Uani 1 1 d . . . C21 C -0.25215(15) 0.04073(12) 0.05854(14) 0.0271(4) Uani 1 1 d . . . H21 H -0.3291 0.0603 0.0174 0.032 Uiso 1 1 calc R . . C22 C -0.25541(18) -0.03966(13) 0.11604(17) 0.0367(4) Uani 1 1 d . . . H22A H -0.3011 -0.0813 0.0648 0.044 Uiso 1 1 calc R . . H22B H -0.1798 -0.0623 0.1500 0.044 Uiso 1 1 calc R . . C23 C -0.3026(2) -0.02572(15) 0.19881(19) 0.0435(5) Uani 1 1 d . . . H23A H -0.3810 -0.0091 0.1641 0.052 Uiso 1 1 calc R . . H23B H -0.2994 -0.0785 0.2366 0.052 Uiso 1 1 calc R . . C24 C -0.2397(2) 0.04085(16) 0.27633(17) 0.0462(5) Uani 1 1 d . . . H24A H -0.2755 0.0508 0.3258 0.055 Uiso 1 1 calc R . . H24B H -0.1634 0.0215 0.3169 0.055 Uiso 1 1 calc R . . C25 C -0.2367(2) 0.12119(15) 0.22080(18) 0.0446(5) Uani 1 1 d . . . H25A H -0.1910 0.1625 0.2725 0.053 Uiso 1 1 calc R . . H25B H -0.3123 0.1439 0.1870 0.053 Uiso 1 1 calc R . . C26 C -0.18925(18) 0.10726(13) 0.13818(16) 0.0346(4) Uani 1 1 d . . . H26A H -0.1110 0.0903 0.1732 0.041 Uiso 1 1 calc R . . H26B H -0.1917 0.1603 0.1011 0.041 Uiso 1 1 calc R . . P P -0.39759(4) 0.04546(3) -0.17959(4) 0.02368(11) Uani 1 1 d . . . C31 C -0.41260(15) 0.13243(11) -0.26904(14) 0.0262(4) Uani 1 1 d . . . C32 C -0.32379(16) 0.18024(12) -0.26816(15) 0.0312(4) Uani 1 1 d . . . H32 H -0.2506 0.1619 -0.2287 0.037 Uiso 1 1 calc R . . C33 C -0.34082(18) 0.25414(12) -0.32407(17) 0.0376(5) Uani 1 1 d . . . H33 H -0.2794 0.2857 -0.3228 0.045 Uiso 1 1 calc R . . C34 C -0.44672(19) 0.28198(13) -0.38161(17) 0.0406(5) Uani 1 1 d . . . H34 H -0.4582 0.3329 -0.4190 0.049 Uiso 1 1 calc R . . C35 C -0.53581(18) 0.23530(13) -0.38443(16) 0.0375(5) Uani 1 1 d . . . H35 H -0.6087 0.2538 -0.4247 0.045 Uiso 1 1 calc R . . C36 C -0.51899(16) 0.16125(12) -0.32841(15) 0.0307(4) Uani 1 1 d . . . H36 H -0.5808 0.1298 -0.3306 0.037 Uiso 1 1 calc R . . C37 C -0.45111(14) -0.04627(11) -0.26225(14) 0.0256(4) Uani 1 1 d . . . C38 C -0.49925(15) -0.04641(12) -0.37096(14) 0.0281(4) Uani 1 1 d . . . H38 H -0.5029 0.0038 -0.4081 0.034 Uiso 1 1 calc R . . C39 C -0.54228(16) -0.11944(12) -0.42602(16) 0.0341(4) Uani 1 1 d . . . H39 H -0.5747 -0.1188 -0.5003 0.041 Uiso 1 1 calc R . . C40 C -0.53772(18) -0.19298(13) -0.37240(18) 0.0394(5) Uani 1 1 d . . . H40 H -0.5666 -0.2429 -0.4098 0.047 Uiso 1 1 calc R . . C41 C -0.49122(19) -0.19353(13) -0.26464(18) 0.0410(5) Uani 1 1 d . . . H41 H -0.4878 -0.2439 -0.2278 0.049 Uiso 1 1 calc R . . C42 C -0.44915(17) -0.12032(12) -0.20953(16) 0.0335(4) Uani 1 1 d . . . H42 H -0.4188 -0.1210 -0.1353 0.040 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 Sr 0.01832(11) 0.02654(12) 0.02330(12) 0.00118(9) 0.00650(8) -0.00042(9) O 0.0364(8) 0.0290(7) 0.0434(8) 0.0074(6) 0.0118(6) -0.0035(6) C1 0.0436(12) 0.0332(11) 0.0441(12) 0.0037(9) 0.0183(10) 0.0039(9) C2 0.045(3) 0.042(5) 0.037(4) 0.007(2) 0.016(3) -0.004(3) C2A 0.054(5) 0.055(6) 0.079(8) 0.037(4) 0.038(6) 0.022(5) C3 0.0472(13) 0.0422(12) 0.0540(14) 0.0128(10) 0.0237(11) 0.0008(10) C4 0.0355(11) 0.0332(10) 0.0467(12) 0.0064(9) 0.0121(9) -0.0039(8) C5 0.0197(8) 0.0260(8) 0.0244(9) -0.0001(6) 0.0077(7) -0.0011(6) N1 0.0210(7) 0.0414(9) 0.0205(7) -0.0010(6) 0.0083(6) 0.0009(6) C11 0.0213(8) 0.0314(9) 0.0207(8) -0.0008(7) 0.0073(6) 0.0014(7) C12 0.0279(9) 0.0315(10) 0.0311(10) 0.0001(7) 0.0129(8) 0.0031(7) C13 0.0349(11) 0.0399(11) 0.0358(11) -0.0097(8) 0.0134(9) 0.0013(8) C14 0.0426(12) 0.0524(13) 0.0302(10) -0.0079(9) 0.0187(9) 0.0059(10) C15 0.0414(11) 0.0482(12) 0.0309(10) 0.0012(9) 0.0212(9) 0.0007(9) C16 0.0304(10) 0.0377(10) 0.0269(10) -0.0020(8) 0.0144(8) -0.0019(8) N2 0.0219(7) 0.0452(9) 0.0212(7) 0.0003(6) 0.0092(6) 0.0024(6) C21 0.0218(9) 0.0381(10) 0.0230(9) -0.0010(7) 0.0107(7) 0.0012(7) C22 0.0431(12) 0.0361(11) 0.0398(11) -0.0015(9) 0.0261(10) -0.0031(9) C23 0.0528(14) 0.0450(12) 0.0462(13) 0.0071(10) 0.0338(11) -0.0011(10) C24 0.0497(13) 0.0665(15) 0.0294(11) 0.0035(10) 0.0231(10) 0.0020(11) C25 0.0550(14) 0.0488(13) 0.0385(12) -0.0115(10) 0.0276(11) -0.0071(10) C26 0.0385(11) 0.0380(11) 0.0318(10) -0.0026(8) 0.0188(9) -0.0051(8) P 0.0196(2) 0.0278(2) 0.0227(2) -0.00079(17) 0.00739(17) 0.00034(16) C31 0.0284(9) 0.0253(9) 0.0247(9) -0.0048(7) 0.0103(7) 0.0008(7) C32 0.0311(10) 0.0286(9) 0.0331(10) -0.0029(7) 0.0119(8) -0.0008(7) C33 0.0434(12) 0.0279(10) 0.0443(12) -0.0010(8) 0.0203(10) -0.0055(8) C34 0.0537(13) 0.0271(10) 0.0414(12) 0.0041(8) 0.0193(10) 0.0052(9) C35 0.0379(11) 0.0355(11) 0.0361(11) 0.0020(8) 0.0113(9) 0.0105(8) C36 0.0290(9) 0.0314(9) 0.0301(10) -0.0015(8) 0.0098(8) 0.0034(7) C37 0.0195(8) 0.0288(9) 0.0274(9) -0.0011(7) 0.0081(7) -0.0005(6) C38 0.0272(9) 0.0284(9) 0.0272(9) -0.0020(7) 0.0092(8) -0.0006(7) C39 0.0326(10) 0.0370(10) 0.0308(10) -0.0076(8) 0.0106(8) -0.0044(8) C40 0.0401(12) 0.0320(10) 0.0457(12) -0.0090(9) 0.0164(10) -0.0086(8) C41 0.0466(13) 0.0290(10) 0.0472(13) 0.0038(9) 0.0184(10) -0.0044(9) C42 0.0339(10) 0.0329(10) 0.0322(10) 0.0033(8) 0.0113(8) -0.0023(8) _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 Sr O 2.5447(14) . ? Sr O 2.5447(14) 3 ? Sr N1 2.5579(15) . ? Sr N1 2.5579(15) 3 ? Sr N2 2.5693(15) . ? Sr N2 2.5693(15) 3 ? Sr C5 2.9986(17) . ? Sr C5 2.9986(17) 3 ? O C1 1.437(2) . ? O C4 1.444(2) . ? C1 C2A 1.468(13) . ? C1 C2 1.536(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.497(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2A C3 1.568(12) . ? C2A H2C 0.9900 . ? C2A H2D 0.9900 . ? C3 C4 1.513(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.330(2) . ? C5 N2 1.330(2) . ? C5 P 1.8999(18) . ? N1 C11 1.451(2) . ? C11 C16 1.529(3) . ? C11 C12 1.536(3) . ? C11 H11 1.0000 . ? C12 C13 1.522(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.522(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.522(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N2 C21 1.456(2) . ? C21 C26 1.528(3) . ? C21 C22 1.529(3) . ? C21 H21 1.0000 . ? C22 C23 1.527(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.514(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.513(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? P C31 1.8300(19) . ? P C37 1.8315(18) . ? C31 C32 1.398(3) . ? C31 C36 1.398(3) . ? C32 C33 1.389(3) . ? C32 H32 0.9500 . ? C33 C34 1.382(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.392(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 C42 1.393(3) . ? C38 C39 1.394(3) . ? C38 H38 0.9500 . ? C39 C40 1.386(3) . ? C39 H39 0.9500 . ? C40 C41 1.379(3) . ? C40 H40 0.9500 . ? C41 C42 1.395(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? 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 O Sr O 180.0 . 3 ? O Sr N1 94.61(5) . . ? O Sr N1 85.39(5) 3 . ? O Sr N1 85.39(5) . 3 ? O Sr N1 94.61(5) 3 3 ? N1 Sr N1 180.00(7) . 3 ? O Sr N2 85.94(5) . . ? O Sr N2 94.06(5) 3 . ? N1 Sr N2 52.40(5) . . ? N1 Sr N2 127.60(5) 3 . ? O Sr N2 94.06(5) . 3 ? O Sr N2 85.94(5) 3 3 ? N1 Sr N2 127.60(5) . 3 ? N1 Sr N2 52.40(5) 3 3 ? N2 Sr N2 180.0 . 3 ? O Sr C5 90.15(5) . . ? O Sr C5 89.85(5) 3 . ? N1 Sr C5 26.18(5) . . ? N1 Sr C5 153.82(5) 3 . ? N2 Sr C5 26.22(5) . . ? N2 Sr C5 153.78(5) 3 . ? O Sr C5 89.85(5) . 3 ? O Sr C5 90.15(5) 3 3 ? N1 Sr C5 153.82(5) . 3 ? N1 Sr C5 26.18(5) 3 3 ? N2 Sr C5 153.78(5) . 3 ? N2 Sr C5 26.22(5) 3 3 ? C5 Sr C5 180.00(7) . 3 ? C1 O C4 106.21(15) . . ? C1 O Sr 126.89(12) . . ? C4 O Sr 117.24(12) . . ? O C1 C2A 109.3(5) . . ? O C1 C2 103.1(5) . . ? O C1 H1A 111.1 . . ? C2A C1 H1A 90.3 . . ? C2 C1 H1A 111.1 . . ? O C1 H1B 111.1 . . ? C2A C1 H1B 123.8 . . ? C2 C1 H1B 111.1 . . ? H1A C1 H1B 109.1 . . ? O C1 H1C 109.8 . . ? C2A C1 H1C 109.8 . . ? C2 C1 H1C 129.8 . . ? H1B C1 H1C 91.1 . . ? O C1 H1D 109.8 . . ? C2A C1 H1D 109.8 . . ? C2 C1 H1D 94.3 . . ? H1A C1 H1D 124.3 . . ? H1C C1 H1D 108.3 . . ? C3 C2 C1 104.4(7) . . ? C3 C2 H2A 110.9 . . ? C1 C2 H2A 110.9 . . ? C3 C2 H2B 110.9 . . ? C1 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? C1 C2A C3 104.3(7) . . ? C1 C2A H2C 110.9 . . ? C3 C2A H2C 110.9 . . ? C1 C2A H2D 110.9 . . ? C3 C2A H2D 110.9 . . ? H2C C2A H2D 108.9 . . ? C2 C3 C4 106.0(5) . . ? C4 C3 C2A 100.6(5) . . ? C2 C3 H3A 110.5 . . ? C4 C3 H3A 110.5 . . ? C2A C3 H3A 94.8 . . ? C2 C3 H3B 110.5 . . ? C4 C3 H3B 110.5 . . ? C2A C3 H3B 130.1 . . ? H3A C3 H3B 108.7 . . ? C2 C3 H3C 91.3 . . ? C4 C3 H3C 111.6 . . ? C2A C3 H3C 111.6 . . ? H3A C3 H3C 123.9 . . ? C2 C3 H3D 125.0 . . ? C4 C3 H3D 111.6 . . ? C2A C3 H3D 111.6 . . ? H3B C3 H3D 92.2 . . ? H3C C3 H3D 109.4 . . ? O C4 C3 104.55(17) . . ? O C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? O C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? N1 C5 N2 116.65(15) . . ? N1 C5 P 126.10(13) . . ? N2 C5 P 117.24(13) . . ? N1 C5 Sr 58.08(9) . . ? N2 C5 Sr 58.57(9) . . ? P C5 Sr 175.52(9) . . ? C5 N1 C11 125.49(15) . . ? C5 N1 Sr 95.74(11) . . ? C11 N1 Sr 138.00(11) . . ? N1 C11 C16 108.97(14) . . ? N1 C11 C12 110.35(15) . . ? C16 C11 C12 108.76(15) . . ? N1 C11 H11 109.6 . . ? C16 C11 H11 109.6 . . ? C12 C11 H11 109.6 . . ? C13 C12 C11 112.08(16) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 111.31(17) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 110.63(17) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.19(17) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 112.76(16) . . ? C15 C16 H16A 109.0 . . ? C11 C16 H16A 109.0 . . ? C15 C16 H16B 109.0 . . ? C11 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C5 N2 C21 126.42(15) . . ? C5 N2 Sr 95.21(11) . . ? C21 N2 Sr 138.30(11) . . ? N2 C21 C26 109.40(15) . . ? N2 C21 C22 109.68(16) . . ? C26 C21 C22 109.31(16) . . ? N2 C21 H21 109.5 . . ? C26 C21 H21 109.5 . . ? C22 C21 H21 109.5 . . ? C23 C22 C21 112.04(17) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 111.69(18) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 110.87(18) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.17(19) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 112.47(17) . . ? C25 C26 H26A 109.1 . . ? C21 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C21 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C31 P C37 106.01(8) . . ? C31 P C5 104.83(8) . . ? C37 P C5 103.49(8) . . ? C32 C31 C36 117.79(17) . . ? C32 C31 P 123.29(14) . . ? C36 C31 P 117.99(15) . . ? C33 C32 C31 121.04(18) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.67(19) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.16(19) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 121.04(19) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C38 C37 C42 118.51(17) . . ? C38 C37 P 125.61(14) . . ? C42 C37 P 115.73(14) . . ? C37 C38 C39 120.77(18) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 119.99(19) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 119.83(19) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.19(19) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.68(19) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.355 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.052 #===end