# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'New Journal of Chemistry' _publ_contact_author_name 'Peter C. Junk' _publ_contact_author_address ; School of Chemistry Monash University Box 23 Clayton Victoria AUSTRALIA ; _publ_contact_author_email peter.junk@sci.monash.edu.au loop_ _publ_author_name 'Peter Courtney Junk' 'Marcus L. Cole' _publ_section_title ; N,N'-Bis(2,6-diisopropylphenyl)formamidinate Complexes of the Heavy Alkaline Earths ; data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 247616' _ccdc_chemical_compound_source_recrystallisation THF _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ca(DippForm)2(THF)]' _chemical_melting_point 535 _chemical_formula_moiety 'C54 H78 Ca N4 O' _chemical_formula_sum 'C54 H78 Ca N4 O' _chemical_formula_weight 839.28 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' 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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.174(2) _cell_length_b 14.010(3) _cell_length_c 17.346(4) _cell_angle_alpha 93.49(3) _cell_angle_beta 97.46(3) _cell_angle_gamma 109.51(3) _cell_volume 2522.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.164 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9679 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28677 _diffrn_reflns_av_R_equivalents 0.1398 _diffrn_reflns_av_sigmaI/netI 0.3187 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.90 _reflns_number_total 11710 _reflns_number_gt 4050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0709P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11710 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2771 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 0.54067(8) 0.72887(6) 0.73089(4) 0.0265(2) Uani 1 1 d . G . O1 O 0.6482(3) 0.6359(2) 0.67173(15) 0.0518(9) Uani 1 1 d . . . N1 N 0.6329(3) 0.9040(2) 0.71769(16) 0.0251(7) Uani 1 1 d . . . N2 N 0.4891(3) 0.8019(2) 0.61466(15) 0.0254(8) Uani 1 1 d . . . N3 N 0.3682(3) 0.6349(2) 0.79325(16) 0.0245(7) Uani 1 1 d . . . N4 N 0.5755(3) 0.6656(2) 0.85349(16) 0.0255(7) Uani 1 1 d . . . C1 C 0.7038(4) 1.0039(3) 0.7551(2) 0.0275(9) Uani 1 1 d . A . C2 C 0.6461(4) 1.0535(3) 0.8028(3) 0.0468(12) Uani 1 1 d . . . C3 C 0.7175(4) 1.1483(4) 0.8417(3) 0.0555(14) Uani 1 1 d . A . H3 H 0.6769 1.1832 0.8722 0.067 Uiso 1 1 calc R . . C4 C 0.8456(4) 1.1937(3) 0.8377(2) 0.0409(11) Uani 1 1 d . . . H4 H 0.8939 1.2581 0.8663 0.049 Uiso 1 1 calc R A . C5 C 0.9032(4) 1.1440(3) 0.7914(2) 0.0349(10) Uani 1 1 d . A . H5 H 0.9916 1.1755 0.7878 0.042 Uiso 1 1 calc R . . C6 C 0.8350(4) 1.0492(3) 0.7501(2) 0.0287(9) Uani 1 1 d . . . C7A C 0.5076(16) 0.9946(11) 0.8264(10) 0.032(4) Uani 0.54(2) 1 d P A 1 H7A H 0.4853 0.9212 0.8067 0.038 Uiso 0.54(2) 1 calc PR A 1 C7B C 0.505(2) 1.0189(15) 0.7951(11) 0.038(5) Uani 0.46(2) 1 d P A 2 H7B H 0.4662 0.9704 0.7465 0.046 Uiso 0.46(2) 1 calc PR A 2 C8A C 0.4985(13) 0.9974(13) 0.9126(9) 0.056(4) Uani 0.54(2) 1 d P A 1 H8A1 H 0.5265 1.0684 0.9358 0.084 Uiso 0.54(2) 1 calc PR A 1 H8A2 H 0.5538 0.9634 0.9384 0.084 Uiso 0.54(2) 1 calc PR A 1 H8A3 H 0.4092 0.9622 0.9193 0.084 Uiso 0.54(2) 1 calc PR A 1 C8B C 0.4855(15) 0.9589(15) 0.8669(14) 0.051(6) Uani 0.46(2) 1 d P A 2 H8B1 H 0.5215 0.9042 0.8623 0.077 Uiso 0.46(2) 1 calc PR A 2 H8B2 H 0.3935 0.9293 0.8694 0.077 Uiso 0.46(2) 1 calc PR A 2 H8B3 H 0.5295 1.0049 0.9146 0.077 Uiso 0.46(2) 1 calc PR A 2 C9A C 0.4127(13) 1.0308(16) 0.7794(8) 0.058(4) Uani 0.54(2) 1 d P A 1 H9A1 H 0.3263 0.9950 0.7909 0.088 Uiso 0.54(2) 1 calc PR A 1 H9A2 H 0.4142 1.0169 0.7236 0.088 Uiso 0.54(2) 1 calc PR A 1 H9A3 H 0.4352 1.1043 0.7930 0.088 Uiso 0.54(2) 1 calc PR A 1 C9B C 0.4350(14) 1.0952(14) 0.7988(9) 0.037(4) Uani 0.46(2) 1 d P A 2 H9B1 H 0.4792 1.1482 0.8425 0.055 Uiso 0.46(2) 1 calc PR A 2 H9B2 H 0.3463 1.0601 0.8066 0.055 Uiso 0.46(2) 1 calc PR A 2 H9B3 H 0.4347 1.1263 0.7498 0.055 Uiso 0.46(2) 1 calc PR A 2 C10 C 0.9010(4) 0.9981(4) 0.6989(3) 0.0521(13) Uani 1 1 d . A . H10 H 0.8420 0.9265 0.6816 0.063 Uiso 1 1 calc R . . C11 C 1.0276(5) 0.9941(4) 0.7417(3) 0.0767(17) Uani 1 1 d . . . H11A H 1.0900 1.0634 0.7546 0.115 Uiso 1 1 calc R A . H11B H 1.0616 0.9540 0.7079 0.115 Uiso 1 1 calc R . . H11C H 1.0124 0.9621 0.7899 0.115 Uiso 1 1 calc R . . C12 C 0.9277(5) 1.0526(5) 0.6258(3) 0.091(2) Uani 1 1 d . . . H12A H 0.8479 1.0582 0.5991 0.137 Uiso 1 1 calc R A . H12B H 0.9606 1.0136 0.5905 0.137 Uiso 1 1 calc R . . H12C H 0.9918 1.1209 0.6411 0.137 Uiso 1 1 calc R . . C13 C 0.4215(4) 0.7931(3) 0.5371(2) 0.0348(11) Uani 1 1 d . G . C14 C 0.2865(5) 0.7450(3) 0.5246(3) 0.0477(12) Uani 1 1 d . . . C15 C 0.2199(6) 0.7350(4) 0.4501(3) 0.0778(19) Uani 1 1 d . G . H15 H 0.1291 0.7021 0.4412 0.093 Uiso 1 1 calc R . . C16 C 0.2798(8) 0.7706(4) 0.3890(3) 0.092(3) Uani 1 1 d . . . H16 H 0.2314 0.7649 0.3387 0.110 Uiso 1 1 calc R G . C17 C 0.4132(7) 0.8155(4) 0.4013(3) 0.0706(18) Uani 1 1 d . G . H17 H 0.4552 0.8389 0.3582 0.085 Uiso 1 1 calc R . . C18 C 0.4879(5) 0.8272(3) 0.4754(2) 0.0463(13) Uani 1 1 d . . . C19 C 0.2173(4) 0.7077(4) 0.5910(3) 0.0605(14) Uani 1 1 d . G . H19 H 0.2758 0.6843 0.6278 0.073 Uiso 1 1 calc R . . C20 C 0.0918(5) 0.6174(4) 0.5671(4) 0.112(2) Uani 1 1 d . . . H20A H 0.0291 0.6393 0.5349 0.168 Uiso 1 1 calc R G . H20B H 0.0576 0.5922 0.6141 0.168 Uiso 1 1 calc R . . H20C H 0.1084 0.5629 0.5370 0.168 Uiso 1 1 calc R . . C21 C 0.1935(5) 0.7950(4) 0.6360(3) 0.0751(16) Uani 1 1 d . . . H21A H 0.2755 0.8502 0.6541 0.113 Uiso 1 1 calc R G . H21B H 0.1527 0.7705 0.6811 0.113 Uiso 1 1 calc R . . H21C H 0.1368 0.8203 0.6016 0.113 Uiso 1 1 calc R . . C22 C 0.6329(5) 0.8700(4) 0.4850(2) 0.0543(14) Uani 1 1 d . C . H22 H 0.6744 0.8696 0.5396 0.065 Uiso 1 1 calc R B 1 C23A C 0.6626(8) 0.7956(6) 0.4239(4) 0.058(3) Uani 0.564(8) 1 d P C 1 H23A H 0.6252 0.8019 0.3710 0.086 Uiso 0.564(8) 1 calc PR C 1 H23B H 0.6250 0.7252 0.4358 0.086 Uiso 0.564(8) 1 calc PR C 1 H23C H 0.7558 0.8137 0.4273 0.086 Uiso 0.564(8) 1 calc PR C 1 C23B C 0.7125(10) 0.7945(7) 0.5059(6) 0.047(3) Uani 0.436(8) 1 d P C 2 H23D H 0.7015 0.7465 0.4598 0.070 Uiso 0.436(8) 1 calc PR C 2 H23E H 0.6801 0.7567 0.5490 0.070 Uiso 0.436(8) 1 calc PR C 2 H23F H 0.8040 0.8347 0.5215 0.070 Uiso 0.436(8) 1 calc PR C 2 C24A C 0.6655(8) 0.9743(6) 0.4611(5) 0.049(3) Uani 0.564(8) 1 d P C 1 H24A H 0.6273 0.9708 0.4064 0.074 Uiso 0.564(8) 1 calc PR C 1 H24B H 0.7591 1.0063 0.4669 0.074 Uiso 0.564(8) 1 calc PR C 1 H24C H 0.6315 1.0148 0.4944 0.074 Uiso 0.564(8) 1 calc PR C 1 C24B C 0.7170(12) 0.9413(9) 0.4294(6) 0.051(3) Uani 0.436(8) 1 d P C 2 H24D H 0.6817 0.9948 0.4169 0.077 Uiso 0.436(8) 1 calc PR C 2 H24E H 0.7150 0.9004 0.3810 0.077 Uiso 0.436(8) 1 calc PR C 2 H24F H 0.8060 0.9725 0.4562 0.077 Uiso 0.436(8) 1 calc PR C 2 C25 C 0.5620(3) 0.8931(3) 0.6487(2) 0.0232(9) Uani 1 1 d . G . H25 H 0.5636 0.9516 0.6232 0.028 Uiso 1 1 calc R . . C26 C 0.2353(4) 0.5749(3) 0.7885(2) 0.0339(10) Uani 1 1 d . G . C27 C 0.1900(5) 0.4759(3) 0.7474(2) 0.0493(13) Uani 1 1 d . . . C28 C 0.0635(6) 0.4182(4) 0.7413(3) 0.0825(19) Uani 1 1 d . G . H28 H 0.0325 0.3524 0.7128 0.099 Uiso 1 1 calc R . . C29 C -0.0207(6) 0.4534(5) 0.7757(4) 0.095(2) Uani 1 1 d . . . H29 H -0.1079 0.4107 0.7727 0.114 Uiso 1 1 calc R G . C30 C 0.0224(5) 0.5523(5) 0.8152(3) 0.0698(17) Uani 1 1 d . G . H30 H -0.0365 0.5763 0.8380 0.084 Uiso 1 1 calc R . . C31 C 0.1516(4) 0.6165(3) 0.8217(2) 0.0427(12) Uani 1 1 d . . . C32 C 0.2757(5) 0.4327(3) 0.7088(3) 0.0577(14) Uani 1 1 d . E . H32 H 0.3684 0.4745 0.7265 0.069 Uiso 1 1 calc R D 1 C33A C 0.238(3) 0.4320(14) 0.6222(8) 0.072(5) Uani 0.67(3) 1 d P E 1 H33A H 0.1496 0.3844 0.6055 0.108 Uiso 0.67(3) 1 calc PR E 1 H33B H 0.2965 0.4106 0.5940 0.108 Uiso 0.67(3) 1 calc PR E 1 H33C H 0.2421 0.5007 0.6108 0.108 Uiso 0.67(3) 1 calc PR E 1 C33B C 0.303(3) 0.465(2) 0.6237(18) 0.048(6) Uani 0.33(3) 1 d P E 2 H33D H 0.3397 0.5393 0.6264 0.071 Uiso 0.33(3) 1 calc PR E 2 H33E H 0.2227 0.4398 0.5865 0.071 Uiso 0.33(3) 1 calc PR E 2 H33F H 0.3645 0.4351 0.6062 0.071 Uiso 0.33(3) 1 calc PR E 2 C34A C 0.2441(19) 0.3250(9) 0.7342(10) 0.058(4) Uani 0.67(3) 1 d P E 1 H34A H 0.2420 0.3281 0.7906 0.087 Uiso 0.67(3) 1 calc PR E 1 H34B H 0.3101 0.2972 0.7223 0.087 Uiso 0.67(3) 1 calc PR E 1 H34C H 0.1600 0.2811 0.7059 0.087 Uiso 0.67(3) 1 calc PR E 1 C34B C 0.279(2) 0.3226(18) 0.7027(18) 0.037(5) Uani 0.33(3) 1 d P E 2 H34D H 0.2637 0.2941 0.7522 0.056 Uiso 0.33(3) 1 calc PR E 2 H34E H 0.3632 0.3239 0.6916 0.056 Uiso 0.33(3) 1 calc PR E 2 H34F H 0.2118 0.2803 0.6603 0.056 Uiso 0.33(3) 1 calc PR E 2 C35 C 0.2021(4) 0.7253(3) 0.8626(2) 0.0435(12) Uani 1 1 d . G . H35 H 0.2756 0.7659 0.8375 0.052 Uiso 1 1 calc R . . C36 C 0.1006(5) 0.7766(4) 0.8544(3) 0.0732(17) Uani 1 1 d . . . H36A H 0.0321 0.7432 0.8840 0.110 Uiso 1 1 calc R G . H36B H 0.0641 0.7707 0.7990 0.110 Uiso 1 1 calc R . . H36C H 0.1405 0.8487 0.8748 0.110 Uiso 1 1 calc R . . C37 C 0.2524(5) 0.7282(4) 0.9492(2) 0.0602(14) Uani 1 1 d . . . H37A H 0.1827 0.6871 0.9749 0.090 Uiso 1 1 calc R G . H37B H 0.2842 0.7988 0.9738 0.090 Uiso 1 1 calc R . . H37C H 0.3226 0.7007 0.9544 0.090 Uiso 1 1 calc R . . C38 C 0.6616(3) 0.6447(3) 0.9126(2) 0.0244(9) Uani 1 1 d . G . C39 C 0.7504(4) 0.7280(3) 0.9633(2) 0.0302(10) Uani 1 1 d . . . C40 C 0.8393(4) 0.7112(3) 1.0191(2) 0.0440(11) Uani 1 1 d . G . H40 H 0.8997 0.7673 1.0528 0.053 Uiso 1 1 calc R . . C41 C 0.8416(4) 0.6144(4) 1.0266(3) 0.0562(13) Uani 1 1 d . . . H41 H 0.9019 0.6038 1.0661 0.067 Uiso 1 1 calc R G . C42 C 0.7562(4) 0.5332(3) 0.9768(3) 0.0460(12) Uani 1 1 d . G . H42 H 0.7591 0.4668 0.9820 0.055 Uiso 1 1 calc R . . C43 C 0.6654(4) 0.5457(3) 0.9188(2) 0.0301(10) Uani 1 1 d . . . C44 C 0.7499(4) 0.8352(3) 0.9562(2) 0.0354(10) Uani 1 1 d . G . H44 H 0.6628 0.8292 0.9289 0.042 Uiso 1 1 calc R . . C45 C 0.8451(5) 0.8897(4) 0.9075(3) 0.0708(16) Uani 1 1 d . . . H45A H 0.9320 0.8994 0.9338 0.106 Uiso 1 1 calc R G . H45B H 0.8373 0.9562 0.8999 0.106 Uiso 1 1 calc R . . H45C H 0.8288 0.8495 0.8565 0.106 Uiso 1 1 calc R . . C46 C 0.7725(5) 0.8981(4) 1.0361(3) 0.0769(17) Uani 1 1 d . . . H46A H 0.8614 0.9131 1.0615 0.115 Uiso 1 1 calc R G . H46B H 0.7134 0.8591 1.0692 0.115 Uiso 1 1 calc R . . H46C H 0.7572 0.9620 1.0285 0.115 Uiso 1 1 calc R . . C47 C 0.5754(4) 0.4519(3) 0.8661(2) 0.0370(11) Uani 1 1 d . G . H47 H 0.5234 0.4748 0.8248 0.044 Uiso 1 1 calc R . . C48 C 0.6487(5) 0.3954(4) 0.8257(3) 0.0847(19) Uani 1 1 d . . . H48A H 0.6988 0.3705 0.8650 0.127 Uiso 1 1 calc R G . H48B H 0.7069 0.4416 0.7957 0.127 Uiso 1 1 calc R . . H48C H 0.5878 0.3375 0.7902 0.127 Uiso 1 1 calc R . . C49 C 0.4832(4) 0.3786(3) 0.9104(2) 0.0423(11) Uani 1 1 d . . . H49A H 0.4284 0.3187 0.8746 0.063 Uiso 1 1 calc R G . H49B H 0.4295 0.4126 0.9324 0.063 Uiso 1 1 calc R . . H49C H 0.5322 0.3574 0.9528 0.063 Uiso 1 1 calc R . . C50 C 0.4510(4) 0.6197(3) 0.8496(2) 0.0270(9) Uani 1 1 d . G . H50 H 0.4196 0.5752 0.8873 0.032 Uiso 1 1 calc R . . C51 C 0.7554(6) 0.6201(6) 0.7036(3) 0.131(3) Uani 1 1 d . G . H51A H 0.7590 0.6132 0.7602 0.157 Uiso 1 1 calc R F 1 H51B H 0.8350 0.6728 0.6940 0.157 Uiso 1 1 calc R F 1 C52A C 0.7211(16) 0.5034(11) 0.6468(7) 0.073(5) Uani 0.515(12) 1 d P G 1 H52A H 0.7994 0.4853 0.6459 0.088 Uiso 0.515(12) 1 calc PR G 1 H52B H 0.6551 0.4477 0.6663 0.088 Uiso 0.515(12) 1 calc PR G 1 C52B C 0.8175(18) 0.600(2) 0.6423(8) 0.128(10) Uani 0.485(12) 1 d P G 2 H52C H 0.8793 0.5652 0.6588 0.153 Uiso 0.485(12) 1 calc PR G 2 H52D H 0.8605 0.6615 0.6179 0.153 Uiso 0.485(12) 1 calc PR G 2 C53 C 0.6820(11) 0.5202(7) 0.5843(6) 0.177(4) Uani 1 1 d . . . H53A H 0.6047 0.4614 0.5611 0.212 Uiso 1 1 calc R G 1 H53B H 0.7481 0.5259 0.5503 0.212 Uiso 1 1 calc R G 1 C54A C 0.6454(14) 0.6221(11) 0.5845(5) 0.069(5) Uani 0.515(12) 1 d P G 1 H54A H 0.7108 0.6793 0.5660 0.083 Uiso 0.515(12) 1 calc PR G 1 H54B H 0.5592 0.6105 0.5544 0.083 Uiso 0.515(12) 1 calc PR G 1 C54B C 0.5946(13) 0.5408(13) 0.6158(8) 0.085(6) Uani 0.485(12) 1 d P G 2 H54C H 0.5502 0.4832 0.6439 0.102 Uiso 0.485(12) 1 calc PR G 2 H54D H 0.5302 0.5488 0.5742 0.102 Uiso 0.485(12) 1 calc PR G 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 0.0303(5) 0.0226(5) 0.0271(5) 0.0069(3) 0.0053(4) 0.0089(4) O1 0.059(2) 0.070(2) 0.0392(18) -0.0045(16) 0.0021(16) 0.043(2) N1 0.0242(19) 0.0181(19) 0.0262(18) -0.0021(14) -0.0035(15) 0.0021(16) N2 0.032(2) 0.0194(19) 0.0214(18) -0.0008(14) -0.0045(15) 0.0075(17) N3 0.0209(19) 0.0228(19) 0.0245(18) 0.0060(14) -0.0034(15) 0.0025(16) N4 0.0181(19) 0.0274(19) 0.0238(18) 0.0035(14) -0.0004(15) -0.0001(17) C1 0.030(3) 0.023(2) 0.026(2) -0.0011(18) -0.0027(19) 0.008(2) C2 0.026(3) 0.036(3) 0.068(3) -0.024(2) 0.002(2) 0.005(2) C3 0.039(3) 0.047(3) 0.073(3) -0.032(3) -0.003(3) 0.016(3) C4 0.043(3) 0.025(3) 0.044(3) -0.005(2) -0.013(2) 0.005(2) C5 0.026(2) 0.026(3) 0.039(2) 0.006(2) -0.006(2) -0.004(2) C6 0.027(3) 0.021(2) 0.033(2) 0.0073(19) 0.0015(19) 0.002(2) C7A 0.041(7) 0.021(9) 0.026(12) -0.011(7) 0.008(9) 0.003(7) C7B 0.051(10) 0.047(10) 0.015(9) 0.004(7) 0.006(9) 0.013(8) C8A 0.050(8) 0.063(9) 0.055(10) 0.010(7) 0.011(6) 0.017(7) C8B 0.029(8) 0.027(10) 0.09(2) 0.020(10) 0.010(10) 0.004(7) C9A 0.029(7) 0.067(12) 0.063(8) 0.002(8) -0.006(6) 0.001(8) C9B 0.022(7) 0.047(10) 0.044(7) 0.016(6) 0.007(5) 0.012(7) C10 0.036(3) 0.046(3) 0.067(3) -0.015(3) 0.016(3) 0.006(3) C11 0.071(4) 0.086(4) 0.096(4) 0.017(3) 0.030(3) 0.050(4) C12 0.065(4) 0.155(6) 0.047(3) -0.002(4) 0.019(3) 0.029(4) C13 0.055(3) 0.024(2) 0.028(3) -0.0037(19) -0.010(2) 0.024(2) C14 0.054(3) 0.026(3) 0.050(3) -0.003(2) -0.027(3) 0.010(3) C15 0.099(5) 0.045(4) 0.068(4) -0.011(3) -0.053(4) 0.024(3) C16 0.154(7) 0.048(4) 0.054(4) -0.021(3) -0.070(5) 0.046(5) C17 0.154(6) 0.048(4) 0.020(3) -0.002(2) -0.007(3) 0.058(4) C18 0.089(4) 0.034(3) 0.024(3) 0.001(2) -0.002(3) 0.036(3) C19 0.039(3) 0.038(3) 0.085(4) 0.015(3) -0.024(3) 0.000(3) C20 0.051(4) 0.048(4) 0.201(7) 0.018(4) -0.041(4) -0.008(3) C21 0.069(4) 0.067(4) 0.078(4) 0.027(3) 0.012(3) 0.004(3) C22 0.096(4) 0.058(3) 0.035(3) 0.022(2) 0.028(3) 0.052(4) C23A 0.076(7) 0.068(7) 0.042(6) 0.003(4) 0.014(5) 0.041(6) C23B 0.058(7) 0.041(7) 0.040(7) -0.002(5) 0.002(6) 0.019(6) C24A 0.041(6) 0.040(6) 0.061(7) 0.019(5) 0.009(5) 0.005(5) C24B 0.056(9) 0.054(8) 0.036(7) 0.009(6) -0.005(6) 0.014(7) C25 0.028(2) 0.019(2) 0.022(2) 0.0042(17) 0.0055(19) 0.007(2) C26 0.021(2) 0.038(3) 0.032(2) 0.020(2) -0.005(2) -0.004(2) C27 0.040(3) 0.033(3) 0.046(3) 0.013(2) -0.025(2) -0.016(3) C28 0.055(4) 0.060(4) 0.096(5) 0.032(3) -0.035(4) -0.016(4) C29 0.036(4) 0.078(5) 0.126(6) 0.074(4) -0.034(4) -0.033(4) C30 0.024(3) 0.095(5) 0.094(4) 0.068(4) 0.011(3) 0.015(3) C31 0.025(3) 0.055(3) 0.050(3) 0.034(2) 0.003(2) 0.013(3) C32 0.082(4) 0.025(3) 0.051(3) -0.006(2) -0.014(3) 0.010(3) C33A 0.117(14) 0.045(9) 0.057(6) 0.007(6) 0.001(10) 0.037(9) C33B 0.031(13) 0.029(13) 0.066(12) -0.017(10) 0.004(11) -0.007(10) C34A 0.068(9) 0.043(6) 0.055(8) 0.015(6) -0.009(7) 0.014(6) C34B 0.050(12) 0.038(10) 0.030(12) 0.010(9) 0.027(9) 0.015(9) C35 0.037(3) 0.050(3) 0.055(3) 0.026(2) 0.016(2) 0.024(3) C36 0.082(4) 0.113(5) 0.057(3) 0.016(3) 0.013(3) 0.074(4) C37 0.057(3) 0.052(3) 0.061(3) 0.013(3) -0.008(3) 0.011(3) C38 0.015(2) 0.032(3) 0.024(2) 0.0084(19) 0.0046(18) 0.004(2) C39 0.022(2) 0.038(3) 0.029(2) 0.008(2) -0.0004(19) 0.010(2) C40 0.032(3) 0.038(3) 0.047(3) 0.004(2) -0.015(2) 0.000(2) C41 0.029(3) 0.057(4) 0.073(4) 0.028(3) -0.013(3) 0.008(3) C42 0.032(3) 0.039(3) 0.066(3) 0.019(3) 0.000(3) 0.011(3) C43 0.024(2) 0.031(3) 0.034(2) 0.011(2) 0.010(2) 0.003(2) C44 0.022(2) 0.036(3) 0.039(3) -0.004(2) -0.008(2) 0.004(2) C45 0.086(4) 0.052(3) 0.089(4) 0.031(3) 0.034(3) 0.031(3) C46 0.106(5) 0.053(4) 0.068(4) -0.006(3) 0.025(3) 0.020(4) C47 0.041(3) 0.031(3) 0.040(3) 0.011(2) 0.014(2) 0.010(2) C48 0.082(4) 0.043(3) 0.123(5) -0.014(3) 0.069(4) -0.002(3) C49 0.039(3) 0.036(3) 0.044(3) 0.010(2) 0.006(2) 0.002(2) C50 0.029(3) 0.026(2) 0.023(2) 0.0057(17) 0.0044(19) 0.004(2) C51 0.092(5) 0.291(11) 0.067(4) 0.032(5) 0.013(4) 0.138(7) C52A 0.115(12) 0.058(8) 0.054(8) -0.034(6) -0.050(8) 0.069(9) C52B 0.138(17) 0.24(3) 0.105(12) 0.086(15) 0.073(12) 0.17(2) C53 0.211(12) 0.135(9) 0.194(11) -0.050(8) 0.082(10) 0.066(9) C54A 0.114(11) 0.094(11) 0.035(6) 0.030(6) 0.026(6) 0.074(9) C54B 0.102(11) 0.085(12) 0.061(9) -0.037(9) 0.019(8) 0.028(9) _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 O1 2.323(3) . ? Ca1 N1 2.361(3) . ? Ca1 N3 2.374(3) . ? Ca1 N4 2.389(3) . ? Ca1 N2 2.406(3) . ? Ca1 C50 2.735(4) . ? Ca1 C25 2.740(4) . ? O1 C51 1.346(5) . ? O1 C54B 1.494(11) . ? O1 C54A 1.509(9) . ? N1 C25 1.317(4) . ? N1 C1 1.422(4) . ? N2 C25 1.316(4) . ? N2 C13 1.432(4) . ? N3 C50 1.333(4) . ? N3 C26 1.431(5) . ? N4 C50 1.315(4) . ? N4 C38 1.425(4) . ? C1 C2 1.397(5) . ? C1 C6 1.406(5) . ? C2 C3 1.378(6) . ? C2 C7B 1.48(2) . ? C2 C7A 1.612(17) . ? C3 C4 1.371(6) . ? C4 C5 1.382(5) . ? C5 C6 1.386(5) . ? C6 C10 1.515(5) . ? C7A C9A 1.493(18) . ? C7A C8A 1.510(16) . ? C7B C9B 1.52(2) . ? C7B C8B 1.543(17) . ? C10 C12 1.530(6) . ? C10 C11 1.530(6) . ? C13 C18 1.397(6) . ? C13 C14 1.413(6) . ? C14 C15 1.378(6) . ? C14 C19 1.495(6) . ? C15 C16 1.359(8) . ? C16 C17 1.392(8) . ? C17 C18 1.408(6) . ? C18 C22 1.511(6) . ? C19 C21 1.526(6) . ? C19 C20 1.530(6) . ? C22 C24A 1.483(9) . ? C22 C23A 1.582(7) . ? C22 C24B 1.593(12) . ? C22 C23B 1.623(9) . ? C26 C31 1.416(5) . ? C26 C27 1.416(6) . ? C27 C28 1.360(7) . ? C27 C32 1.497(6) . ? C28 C29 1.381(8) . ? C29 C30 1.405(8) . ? C30 C31 1.409(6) . ? C31 C35 1.528(6) . ? C32 C33A 1.506(14) . ? C32 C34A 1.535(12) . ? C32 C34B 1.55(2) . ? C32 C33B 1.61(3) . ? C35 C37 1.527(5) . ? C35 C36 1.528(5) . ? C38 C43 1.412(5) . ? C38 C39 1.412(5) . ? C39 C40 1.383(5) . ? C39 C44 1.516(5) . ? C40 C41 1.380(6) . ? C41 C42 1.376(6) . ? C42 C43 1.395(5) . ? C43 C47 1.519(5) . ? C44 C45 1.484(6) . ? C44 C46 1.540(5) . ? C47 C49 1.517(5) . ? C47 C48 1.518(5) . ? C51 C52B 1.407(11) . ? C51 C52A 1.754(12) . ? C52A C53 1.181(13) . ? C52B C53 1.70(2) . ? C53 C54B 1.282(12) . ? C53 C54A 1.612(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca1 N1 110.82(11) . . ? O1 Ca1 N3 116.29(11) . . ? N1 Ca1 N3 132.88(10) . . ? O1 Ca1 N4 92.06(10) . . ? N1 Ca1 N4 120.69(11) . . ? N3 Ca1 N4 57.78(10) . . ? O1 Ca1 N2 94.90(10) . . ? N1 Ca1 N2 57.33(10) . . ? N3 Ca1 N2 117.80(11) . . ? N4 Ca1 N2 172.98(10) . . ? O1 Ca1 C50 103.97(11) . . ? N1 Ca1 C50 134.74(11) . . ? N3 Ca1 C50 29.17(10) . . ? N4 Ca1 C50 28.73(10) . . ? N2 Ca1 C50 146.95(11) . . ? O1 Ca1 C25 106.25(10) . . ? N1 Ca1 C25 28.72(10) . . ? N3 Ca1 C25 129.10(10) . . ? N4 Ca1 C25 148.47(11) . . ? N2 Ca1 C25 28.71(9) . . ? C50 Ca1 C25 149.77(10) . . ? C51 O1 C54B 97.0(6) . . ? C51 O1 C54A 105.2(5) . . ? C54B O1 C54A 50.5(6) . . ? C51 O1 Ca1 126.9(3) . . ? C54B O1 Ca1 129.3(5) . . ? C54A O1 Ca1 123.4(4) . . ? C25 N1 C1 119.0(3) . . ? C25 N1 Ca1 91.8(2) . . ? C1 N1 Ca1 147.4(2) . . ? C25 N2 C13 118.6(3) . . ? C25 N2 Ca1 89.9(2) . . ? C13 N2 Ca1 151.5(3) . . ? C50 N3 C26 117.3(3) . . ? C50 N3 Ca1 90.6(2) . . ? C26 N3 Ca1 149.4(2) . . ? C50 N4 C38 119.3(3) . . ? C50 N4 Ca1 90.4(2) . . ? C38 N4 Ca1 148.9(2) . . ? C2 C1 C6 119.6(4) . . ? C2 C1 N1 119.9(4) . . ? C6 C1 N1 120.3(3) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C7B 118.8(8) . . ? C1 C2 C7B 119.8(9) . . ? C3 C2 C7A 118.3(6) . . ? C1 C2 C7A 121.3(6) . . ? C7B C2 C7A 24.2(5) . . ? C4 C3 C2 121.8(4) . . ? C3 C4 C5 118.9(4) . . ? C4 C5 C6 121.5(4) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C10 119.9(4) . . ? C1 C6 C10 121.3(4) . . ? C9A C7A C8A 113.7(11) . . ? C9A C7A C2 106.9(11) . . ? C8A C7A C2 117.1(11) . . ? C2 C7B C9B 120.9(14) . . ? C2 C7B C8B 99.7(14) . . ? C9B C7B C8B 108.5(15) . . ? C6 C10 C12 110.8(4) . . ? C6 C10 C11 112.8(4) . . ? C12 C10 C11 108.7(4) . . ? C18 C13 C14 121.3(4) . . ? C18 C13 N2 120.9(4) . . ? C14 C13 N2 117.7(4) . . ? C15 C14 C13 118.6(5) . . ? C15 C14 C19 120.8(5) . . ? C13 C14 C19 120.6(4) . . ? C16 C15 C14 122.1(6) . . ? C15 C16 C17 119.1(5) . . ? C16 C17 C18 122.0(5) . . ? C13 C18 C17 116.8(5) . . ? C13 C18 C22 122.9(4) . . ? C17 C18 C22 120.2(5) . . ? C14 C19 C21 110.3(4) . . ? C14 C19 C20 114.2(5) . . ? C21 C19 C20 110.5(4) . . ? C24A C22 C18 105.9(5) . . ? C24A C22 C23A 111.6(6) . . ? C18 C22 C23A 102.1(5) . . ? C24A C22 C24B 39.2(4) . . ? C18 C22 C24B 126.8(6) . . ? C23A C22 C24B 74.3(6) . . ? C24A C22 C23B 135.2(6) . . ? C18 C22 C23B 118.4(5) . . ? C23A C22 C23B 54.2(4) . . ? C24B C22 C23B 102.4(6) . . ? N2 C25 N1 120.5(3) . . ? N2 C25 Ca1 61.40(18) . . ? N1 C25 Ca1 59.45(19) . . ? C31 C26 C27 121.7(4) . . ? C31 C26 N3 120.0(4) . . ? C27 C26 N3 118.3(4) . . ? C28 C27 C26 119.2(5) . . ? C28 C27 C32 118.4(5) . . ? C26 C27 C32 122.4(4) . . ? C27 C28 C29 121.3(6) . . ? C28 C29 C30 120.0(6) . . ? C29 C30 C31 121.1(5) . . ? C30 C31 C26 116.5(5) . . ? C30 C31 C35 122.9(4) . . ? C26 C31 C35 120.6(4) . . ? C27 C32 C33A 105.8(8) . . ? C27 C32 C34A 104.2(10) . . ? C33A C32 C34A 112.8(7) . . ? C27 C32 C34B 130.0(10) . . ? C33A C32 C34B 94.9(11) . . ? C34A C32 C34B 26.8(5) . . ? C27 C32 C33B 117.3(11) . . ? C33A C32 C33B 26.5(7) . . ? C34A C32 C33B 126.3(11) . . ? C34B C32 C33B 101.5(14) . . ? C37 C35 C31 111.3(3) . . ? C37 C35 C36 109.4(3) . . ? C31 C35 C36 112.5(4) . . ? C43 C38 C39 119.8(3) . . ? C43 C38 N4 122.4(3) . . ? C39 C38 N4 117.7(3) . . ? C40 C39 C38 119.4(3) . . ? C40 C39 C44 120.0(4) . . ? C38 C39 C44 120.6(3) . . ? C41 C40 C39 121.1(4) . . ? C42 C41 C40 119.7(4) . . ? C41 C42 C43 121.7(4) . . ? C42 C43 C38 118.3(4) . . ? C42 C43 C47 118.2(4) . . ? C38 C43 C47 123.5(3) . . ? C45 C44 C39 111.2(3) . . ? C45 C44 C46 110.2(4) . . ? C39 C44 C46 113.0(3) . . ? C49 C47 C48 108.9(3) . . ? C49 C47 C43 112.1(3) . . ? C48 C47 C43 111.8(4) . . ? N4 C50 N3 120.7(3) . . ? N4 C50 Ca1 60.87(19) . . ? N3 C50 Ca1 60.23(19) . . ? O1 C51 C52B 108.0(6) . . ? O1 C51 C52A 95.0(5) . . ? C52B C51 C52A 52.5(9) . . ? C53 C52A C51 102.2(9) . . ? C51 C52B C53 95.8(11) . . ? C52A C53 C54B 87.2(12) . . ? C52A C53 C54A 114.5(9) . . ? C54B C53 C54A 51.0(8) . . ? C52A C53 C52B 56.3(10) . . ? C54B C53 C52B 101.2(8) . . ? C54A C53 C52B 82.2(8) . . ? O1 C54A C53 95.3(7) . . ? C53 C54B O1 112.3(11) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.390 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.065 #===END data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 247617' _ccdc_chemical_compound_source_recrystallisation Toluene _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Sr(DippForm)2(THF)2]' _chemical_melting_point 515 _chemical_formula_moiety 'C58 H86 N4 O2 Sr' _chemical_formula_sum 'C58 H86 N4 O2 Sr' _chemical_formula_weight 958.93 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' Sr Sr -1.5307 3.2498 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0689(3) _cell_length_b 12.7964(5) _cell_length_c 19.6889(7) _cell_angle_alpha 84.466(3) _cell_angle_beta 86.449(3) _cell_angle_gamma 64.2010(10) _cell_volume 2724.21(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombohedral plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6828 _exptl_absorpt_correction_T_max 0.9502 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26694 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_sigmaI/netI 0.1572 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.07 _reflns_number_total 12922 _reflns_number_gt 8009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0701P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12922 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.82544(3) 0.79749(3) 0.740539(15) 0.01539(11) Uani 1 1 d . . . O1 O 1.0161(3) 0.6929(2) 0.66696(13) 0.0333(7) Uani 1 1 d . . . O2 O 0.9475(2) 0.9175(2) 0.75280(13) 0.0281(6) Uani 1 1 d . . . N1 N 0.6703(3) 0.9838(3) 0.68041(13) 0.0185(7) Uani 1 1 d . . . N2 N 0.6738(3) 0.8162(3) 0.64567(13) 0.0173(7) Uani 1 1 d . . . N3 N 0.7776(3) 0.6506(3) 0.81995(13) 0.0179(7) Uani 1 1 d . . . N4 N 0.8880(3) 0.7323(2) 0.86815(13) 0.0148(6) Uani 1 1 d . . . C1 C 0.6262(3) 1.1064(3) 0.67171(16) 0.0167(8) Uani 1 1 d . . . C2 C 0.5300(3) 1.1765(3) 0.71512(17) 0.0202(8) Uani 1 1 d . . . C3 C 0.4939(4) 1.2964(3) 0.70855(18) 0.0256(9) Uani 1 1 d . . . H3 H 0.4298 1.3445 0.7376 0.031 Uiso 1 1 calc R . . C4 C 0.5480(4) 1.3471(3) 0.66145(18) 0.0252(9) Uani 1 1 d . . . H4 H 0.5208 1.4291 0.6578 0.030 Uiso 1 1 calc R . . C5 C 0.6425(4) 1.2778(3) 0.61935(18) 0.0255(9) Uani 1 1 d . . . H5 H 0.6803 1.3127 0.5869 0.031 Uiso 1 1 calc R . . C6 C 0.6828(3) 1.1578(3) 0.62401(16) 0.0194(8) Uani 1 1 d . . . C7 C 0.4712(4) 1.1237(4) 0.76934(18) 0.0275(9) Uani 1 1 d . . . H7 H 0.5038 1.0389 0.7627 0.033 Uiso 1 1 calc R . . C8 C 0.5079(4) 1.1353(5) 0.8407(2) 0.0450(13) Uani 1 1 d . . . H8A H 0.5979 1.0992 0.8434 0.068 Uiso 1 1 calc R . . H8B H 0.4740 1.0961 0.8752 0.068 Uiso 1 1 calc R . . H8C H 0.4753 1.2178 0.8489 0.068 Uiso 1 1 calc R . . C9 C 0.3310(4) 1.1773(4) 0.7651(2) 0.0376(11) Uani 1 1 d . . . H9A H 0.2968 1.2609 0.7710 0.056 Uiso 1 1 calc R . . H9B H 0.2979 1.1398 0.8012 0.056 Uiso 1 1 calc R . . H9C H 0.3083 1.1657 0.7205 0.056 Uiso 1 1 calc R . . C10 C 0.7892(4) 1.0839(3) 0.57824(18) 0.0266(9) Uani 1 1 d . . . H10 H 0.8184 1.0009 0.5967 0.032 Uiso 1 1 calc R . . C11 C 0.8984(4) 1.1143(5) 0.5770(2) 0.0472(13) Uani 1 1 d . . . H11A H 0.9651 1.0620 0.5485 0.071 Uiso 1 1 calc R . . H11B H 0.9273 1.1056 0.6236 0.071 Uiso 1 1 calc R . . H11C H 0.8729 1.1950 0.5583 0.071 Uiso 1 1 calc R . . C12 C 0.7453(4) 1.0933(4) 0.5061(2) 0.0443(12) Uani 1 1 d . . . H12A H 0.6747 1.0744 0.5076 0.066 Uiso 1 1 calc R . . H12B H 0.8122 1.0387 0.4786 0.066 Uiso 1 1 calc R . . H12C H 0.7208 1.1729 0.4856 0.066 Uiso 1 1 calc R . . C13 C 0.6271(3) 0.7612(3) 0.60345(17) 0.0206(8) Uani 1 1 d . . . C14 C 0.5366(3) 0.7258(3) 0.63032(18) 0.0227(9) Uani 1 1 d . . . C15 C 0.5007(4) 0.6615(3) 0.5919(2) 0.0310(10) Uani 1 1 d . . . H15 H 0.4409 0.6364 0.6104 0.037 Uiso 1 1 calc R . . C16 C 0.5499(4) 0.6328(4) 0.5268(2) 0.0379(11) Uani 1 1 d . . . H16 H 0.5255 0.5871 0.5014 0.046 Uiso 1 1 calc R . . C17 C 0.6338(4) 0.6712(4) 0.5000(2) 0.0348(11) Uani 1 1 d . . . H17 H 0.6645 0.6547 0.4547 0.042 Uiso 1 1 calc R . . C18 C 0.6761(4) 0.7343(3) 0.53712(18) 0.0262(9) Uani 1 1 d . . . C19 C 0.4771(4) 0.7625(3) 0.70007(18) 0.0260(9) Uani 1 1 d . . . H19 H 0.5418 0.7610 0.7300 0.031 Uiso 1 1 calc R . . C20 C 0.4232(4) 0.6832(4) 0.7353(2) 0.0345(10) Uani 1 1 d . . . H20A H 0.3549 0.6881 0.7087 0.052 Uiso 1 1 calc R . . H20B H 0.3931 0.7076 0.7811 0.052 Uiso 1 1 calc R . . H20C H 0.4870 0.6027 0.7386 0.052 Uiso 1 1 calc R . . C21 C 0.3756(4) 0.8884(4) 0.6927(2) 0.0358(11) Uani 1 1 d . . . H21A H 0.3099 0.8917 0.6645 0.054 Uiso 1 1 calc R . . H21B H 0.4107 0.9399 0.6711 0.054 Uiso 1 1 calc R . . H21C H 0.3417 0.9137 0.7380 0.054 Uiso 1 1 calc R . . C22 C 0.7736(4) 0.7687(4) 0.50504(19) 0.0325(10) Uani 1 1 d . . . H22 H 0.7882 0.8171 0.5372 0.039 Uiso 1 1 calc R . . C23 C 0.8951(4) 0.6607(5) 0.4957(3) 0.0573(15) Uani 1 1 d . . . H23A H 0.9219 0.6174 0.5400 0.086 Uiso 1 1 calc R . . H23B H 0.9579 0.6847 0.4761 0.086 Uiso 1 1 calc R . . H23C H 0.8831 0.6109 0.4649 0.086 Uiso 1 1 calc R . . C24 C 0.7331(5) 0.8420(5) 0.4375(2) 0.0589(15) Uani 1 1 d . . . H24A H 0.7109 0.7994 0.4063 0.088 Uiso 1 1 calc R . . H24B H 0.8008 0.8582 0.4172 0.088 Uiso 1 1 calc R . . H24C H 0.6617 0.9156 0.4456 0.088 Uiso 1 1 calc R . . C25 C 0.6330(3) 0.9304(3) 0.63938(16) 0.0153(8) Uani 1 1 d . . . H25 H 0.5759 0.9748 0.6048 0.018 Uiso 1 1 calc R . . C26 C 0.7204(3) 0.5752(3) 0.83005(17) 0.0184(8) Uani 1 1 d . . . C27 C 0.7546(3) 0.4830(3) 0.78702(17) 0.0190(8) Uani 1 1 d . . . C28 C 0.6975(4) 0.4080(3) 0.79757(18) 0.0250(9) Uani 1 1 d . . . H28 H 0.7202 0.3458 0.7690 0.030 Uiso 1 1 calc R . . C29 C 0.6092(4) 0.4219(3) 0.84830(19) 0.0271(9) Uani 1 1 d . . . H29 H 0.5732 0.3687 0.8555 0.033 Uiso 1 1 calc R . . C30 C 0.5738(4) 0.5148(3) 0.88869(18) 0.0240(9) Uani 1 1 d . . . H30 H 0.5119 0.5250 0.9230 0.029 Uiso 1 1 calc R . . C31 C 0.6257(3) 0.5934(3) 0.88072(17) 0.0193(8) Uani 1 1 d . . . C32 C 0.8557(3) 0.4621(3) 0.73312(18) 0.0239(9) Uani 1 1 d . . . H32 H 0.8615 0.5376 0.7224 0.029 Uiso 1 1 calc R . . C33 C 0.8312(4) 0.4256(4) 0.6659(2) 0.0401(11) Uani 1 1 d . . . H33A H 0.8324 0.3483 0.6735 0.060 Uiso 1 1 calc R . . H33B H 0.8951 0.4232 0.6320 0.060 Uiso 1 1 calc R . . H33C H 0.7504 0.4820 0.6492 0.060 Uiso 1 1 calc R . . C34 C 0.9790(4) 0.3747(4) 0.7621(2) 0.0368(11) Uani 1 1 d . . . H34A H 0.9948 0.4028 0.8034 0.055 Uiso 1 1 calc R . . H34B H 1.0447 0.3656 0.7281 0.055 Uiso 1 1 calc R . . H34C H 0.9768 0.2993 0.7736 0.055 Uiso 1 1 calc R . . C35 C 0.5812(4) 0.6986(3) 0.92297(17) 0.0227(9) Uani 1 1 d . . . H35 H 0.6562 0.7036 0.9379 0.027 Uiso 1 1 calc R . . C36 C 0.5076(4) 0.8112(4) 0.8808(2) 0.0405(12) Uani 1 1 d . . . H36A H 0.5559 0.8175 0.8401 0.061 Uiso 1 1 calc R . . H36B H 0.4887 0.8773 0.9081 0.061 Uiso 1 1 calc R . . H36C H 0.4308 0.8116 0.8670 0.061 Uiso 1 1 calc R . . C37 C 0.5075(4) 0.6903(4) 0.98774(19) 0.0327(10) Uani 1 1 d . . . H37A H 0.4915 0.7560 1.0148 0.049 Uiso 1 1 calc R . . H37B H 0.5547 0.6171 1.0147 0.049 Uiso 1 1 calc R . . H37C H 0.4292 0.6925 0.9752 0.049 Uiso 1 1 calc R . . C38 C 0.9642(3) 0.7231(3) 0.92301(15) 0.0145(8) Uani 1 1 d . . . C39 C 0.9233(3) 0.8154(3) 0.96635(16) 0.0183(8) Uani 1 1 d . . . C40 C 0.9967(4) 0.8060(3) 1.02081(18) 0.0260(9) Uani 1 1 d . . . H40 H 0.9694 0.8670 1.0506 0.031 Uiso 1 1 calc R . . C41 C 1.1083(4) 0.7100(4) 1.03258(19) 0.0296(10) Uani 1 1 d . . . H41 H 1.1559 0.7046 1.0705 0.036 Uiso 1 1 calc R . . C42 C 1.1495(4) 0.6224(3) 0.98863(17) 0.0241(9) Uani 1 1 d . . . H42 H 1.2266 0.5571 0.9962 0.029 Uiso 1 1 calc R . . C43 C 1.0798(3) 0.6280(3) 0.93307(16) 0.0178(8) Uani 1 1 d . . . C44 C 0.7996(4) 0.9200(3) 0.95635(17) 0.0216(8) Uani 1 1 d . . . H44 H 0.7755 0.9245 0.9081 0.026 Uiso 1 1 calc R . . C45 C 0.8032(4) 1.0356(3) 0.9676(2) 0.0307(10) Uani 1 1 d . . . H45A H 0.8121 1.0395 1.0163 0.046 Uiso 1 1 calc R . . H45B H 0.7266 1.1006 0.9517 0.046 Uiso 1 1 calc R . . H45C H 0.8732 1.0405 0.9419 0.046 Uiso 1 1 calc R . . C46 C 0.7002(4) 0.9052(4) 1.0030(2) 0.0328(10) Uani 1 1 d . . . H46A H 0.6956 0.8332 0.9942 0.049 Uiso 1 1 calc R . . H46B H 0.6205 0.9716 0.9938 0.049 Uiso 1 1 calc R . . H46C H 0.7210 0.9014 1.0508 0.049 Uiso 1 1 calc R . . C47 C 1.1319(3) 0.5301(3) 0.88532(17) 0.0197(8) Uani 1 1 d . . . H47 H 1.0726 0.5503 0.8476 0.024 Uiso 1 1 calc R . . C48 C 1.2559(4) 0.5181(4) 0.8532(2) 0.0310(10) Uani 1 1 d . . . H48A H 1.2461 0.5932 0.8305 0.046 Uiso 1 1 calc R . . H48B H 1.2836 0.4595 0.8196 0.046 Uiso 1 1 calc R . . H48C H 1.3172 0.4940 0.8889 0.046 Uiso 1 1 calc R . . C49 C 1.1466(4) 0.4131(3) 0.92129(19) 0.0292(10) Uani 1 1 d . . . H49A H 1.2067 0.3897 0.9576 0.044 Uiso 1 1 calc R . . H49B H 1.1753 0.3538 0.8881 0.044 Uiso 1 1 calc R . . H49C H 1.0670 0.4210 0.9411 0.044 Uiso 1 1 calc R . . C50 C 0.8435(3) 0.6537(3) 0.87070(16) 0.0141(7) Uani 1 1 d . . . H50 H 0.8589 0.5990 0.9093 0.017 Uiso 1 1 calc R . . C51 C 1.0918(4) 0.5699(4) 0.6778(2) 0.0456(13) Uani 1 1 d . . . H51A H 1.0547 0.5256 0.6569 0.055 Uiso 1 1 calc R . . H51B H 1.1009 0.5458 0.7272 0.055 Uiso 1 1 calc R . . C52 C 1.2116(4) 0.5487(4) 0.6454(2) 0.0485(13) Uani 1 1 d . . . H52A H 1.2545 0.4683 0.6312 0.058 Uiso 1 1 calc R . . H52B H 1.2647 0.5619 0.6767 0.058 Uiso 1 1 calc R . . C53 C 1.1784(4) 0.6363(4) 0.5847(2) 0.0375(11) Uani 1 1 d . . . H53A H 1.1567 0.6063 0.5455 0.045 Uiso 1 1 calc R . . H53B H 1.2471 0.6569 0.5708 0.045 Uiso 1 1 calc R . . C54 C 1.0681(4) 0.7399(4) 0.6103(2) 0.0336(10) Uani 1 1 d . . . H54A H 1.0937 0.7973 0.6258 0.040 Uiso 1 1 calc R . . H54B H 1.0072 0.7786 0.5739 0.040 Uiso 1 1 calc R . . C55 C 1.0712(4) 0.8570(4) 0.7791(2) 0.0336(10) Uani 1 1 d . . . H55A H 1.1329 0.8423 0.7413 0.040 Uiso 1 1 calc R . . H55B H 1.0833 0.7815 0.8033 0.040 Uiso 1 1 calc R . . C56 C 1.0841(4) 0.9354(4) 0.8276(2) 0.0387(11) Uani 1 1 d . . . H56A H 1.0590 0.9190 0.8747 0.046 Uiso 1 1 calc R . . H56B H 1.1696 0.9269 0.8274 0.046 Uiso 1 1 calc R . . C57 C 0.9971(5) 1.0547(4) 0.7983(2) 0.0398(11) Uani 1 1 d . . . H57A H 1.0361 1.0825 0.7595 0.048 Uiso 1 1 calc R . . H57B H 0.9696 1.1118 0.8335 0.048 Uiso 1 1 calc R . . C58 C 0.8913(4) 1.0348(3) 0.7751(2) 0.0320(10) Uani 1 1 d . . . H58A H 0.8316 1.0414 0.8132 0.038 Uiso 1 1 calc R . . H58B H 0.8481 1.0922 0.7371 0.038 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 Sr1 0.01582(19) 0.01549(19) 0.01672(17) 0.00076(12) -0.00265(12) -0.00860(15) O1 0.0298(17) 0.0259(17) 0.0400(16) -0.0034(12) 0.0135(13) -0.0098(14) O2 0.0261(16) 0.0274(16) 0.0389(15) 0.0005(12) -0.0092(12) -0.0186(13) N1 0.0191(17) 0.0164(17) 0.0192(15) -0.0025(12) -0.0028(12) -0.0063(14) N2 0.0170(17) 0.0158(17) 0.0199(15) -0.0018(12) -0.0053(12) -0.0071(14) N3 0.0205(17) 0.0191(17) 0.0200(15) -0.0006(12) -0.0028(12) -0.0139(14) N4 0.0138(16) 0.0136(16) 0.0169(14) -0.0003(11) -0.0031(11) -0.0054(13) C1 0.015(2) 0.0128(19) 0.0185(18) -0.0002(14) -0.0075(14) -0.0020(16) C2 0.019(2) 0.017(2) 0.0221(18) -0.0024(15) -0.0018(15) -0.0057(17) C3 0.025(2) 0.019(2) 0.026(2) -0.0058(16) -0.0001(16) -0.0034(18) C4 0.029(2) 0.011(2) 0.034(2) -0.0011(16) -0.0072(17) -0.0060(18) C5 0.024(2) 0.026(2) 0.027(2) 0.0021(16) -0.0042(16) -0.0111(19) C6 0.017(2) 0.019(2) 0.0180(18) -0.0004(14) -0.0042(14) -0.0036(17) C7 0.025(2) 0.026(2) 0.031(2) -0.0034(17) 0.0068(17) -0.0107(19) C8 0.037(3) 0.071(4) 0.032(2) 0.009(2) -0.001(2) -0.030(3) C9 0.034(3) 0.049(3) 0.034(2) -0.010(2) 0.0043(19) -0.021(2) C10 0.028(2) 0.023(2) 0.025(2) 0.0008(16) 0.0058(16) -0.0081(19) C11 0.030(3) 0.065(4) 0.046(3) -0.010(2) 0.009(2) -0.020(3) C12 0.041(3) 0.057(3) 0.033(2) -0.021(2) 0.008(2) -0.017(3) C13 0.022(2) 0.0112(19) 0.0243(19) 0.0013(14) -0.0108(15) -0.0028(17) C14 0.021(2) 0.019(2) 0.027(2) 0.0029(15) -0.0096(16) -0.0075(18) C15 0.033(3) 0.027(2) 0.040(2) 0.0022(18) -0.0173(19) -0.018(2) C16 0.044(3) 0.033(3) 0.044(3) -0.007(2) -0.019(2) -0.020(2) C17 0.042(3) 0.035(3) 0.027(2) -0.0141(18) -0.0091(19) -0.013(2) C18 0.027(2) 0.025(2) 0.026(2) -0.0064(16) -0.0038(16) -0.0093(19) C19 0.026(2) 0.027(2) 0.028(2) 0.0013(16) -0.0071(16) -0.0142(19) C20 0.039(3) 0.037(3) 0.038(2) 0.0056(19) -0.0101(19) -0.026(2) C21 0.036(3) 0.031(3) 0.042(2) -0.0011(19) 0.005(2) -0.018(2) C22 0.035(3) 0.038(3) 0.027(2) -0.0128(18) 0.0001(18) -0.016(2) C23 0.036(3) 0.060(4) 0.074(4) -0.026(3) 0.007(3) -0.015(3) C24 0.075(4) 0.082(4) 0.035(3) 0.013(3) -0.015(2) -0.050(3) C25 0.0128(19) 0.016(2) 0.0150(17) 0.0024(14) -0.0047(13) -0.0042(16) C26 0.017(2) 0.017(2) 0.0227(19) 0.0063(15) -0.0088(15) -0.0102(17) C27 0.016(2) 0.016(2) 0.0257(19) 0.0008(15) -0.0046(15) -0.0081(17) C28 0.027(2) 0.021(2) 0.033(2) -0.0017(16) -0.0075(17) -0.0144(19) C29 0.027(2) 0.028(2) 0.034(2) 0.0057(17) -0.0049(17) -0.020(2) C30 0.022(2) 0.029(2) 0.026(2) 0.0049(16) -0.0035(16) -0.0164(19) C31 0.018(2) 0.023(2) 0.0199(18) 0.0019(15) -0.0040(15) -0.0120(17) C32 0.025(2) 0.020(2) 0.031(2) -0.0055(16) 0.0025(16) -0.0136(18) C33 0.036(3) 0.050(3) 0.040(2) -0.017(2) 0.004(2) -0.021(2) C34 0.025(2) 0.032(3) 0.052(3) -0.005(2) 0.001(2) -0.011(2) C35 0.022(2) 0.027(2) 0.0217(19) -0.0039(16) 0.0017(15) -0.0128(18) C36 0.050(3) 0.033(3) 0.035(2) -0.0054(19) 0.000(2) -0.014(2) C37 0.026(2) 0.038(3) 0.032(2) -0.0017(18) 0.0036(18) -0.012(2) C38 0.018(2) 0.020(2) 0.0112(16) 0.0026(13) -0.0019(13) -0.0133(17) C39 0.018(2) 0.022(2) 0.0170(18) 0.0007(14) 0.0022(14) -0.0109(17) C40 0.031(2) 0.029(2) 0.0220(19) -0.0093(16) -0.0023(16) -0.014(2) C41 0.025(2) 0.041(3) 0.025(2) -0.0050(18) -0.0102(17) -0.015(2) C42 0.018(2) 0.025(2) 0.026(2) -0.0002(16) -0.0039(16) -0.0067(18) C43 0.017(2) 0.021(2) 0.0168(17) 0.0000(14) 0.0003(14) -0.0098(17) C44 0.028(2) 0.019(2) 0.0204(19) -0.0049(15) -0.0038(15) -0.0117(18) C45 0.030(2) 0.022(2) 0.038(2) -0.0073(17) -0.0014(18) -0.008(2) C46 0.024(2) 0.028(2) 0.046(2) -0.0062(19) 0.0033(19) -0.011(2) C47 0.017(2) 0.021(2) 0.0200(18) 0.0002(15) 0.0005(14) -0.0071(17) C48 0.026(2) 0.032(3) 0.034(2) -0.0033(18) 0.0084(17) -0.012(2) C49 0.032(2) 0.025(2) 0.030(2) -0.0037(17) 0.0018(17) -0.011(2) C50 0.0162(19) 0.0131(19) 0.0145(17) 0.0013(13) 0.0011(14) -0.0084(16) C51 0.049(3) 0.033(3) 0.047(3) 0.005(2) 0.010(2) -0.013(2) C52 0.037(3) 0.045(3) 0.049(3) -0.005(2) 0.006(2) -0.005(2) C53 0.028(3) 0.056(3) 0.031(2) 0.000(2) 0.0051(18) -0.023(2) C54 0.038(3) 0.031(3) 0.033(2) -0.0006(18) 0.0048(19) -0.017(2) C55 0.020(2) 0.044(3) 0.041(2) 0.001(2) -0.0044(18) -0.018(2) C56 0.038(3) 0.063(3) 0.029(2) -0.006(2) -0.0028(19) -0.035(3) C57 0.063(3) 0.045(3) 0.030(2) -0.0040(19) -0.002(2) -0.040(3) C58 0.038(3) 0.025(2) 0.036(2) -0.0032(18) -0.0075(19) -0.015(2) _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 N1 2.537(3) . ? Sr1 O1 2.542(2) . ? Sr1 N3 2.565(3) . ? Sr1 O2 2.583(3) . ? Sr1 N2 2.617(3) . ? Sr1 N4 2.619(3) . ? Sr1 C25 2.956(3) . ? Sr1 C50 2.968(3) . ? O1 C51 1.437(5) . ? O1 C54 1.453(4) . ? O2 C55 1.451(5) . ? O2 C58 1.453(5) . ? N1 C25 1.320(4) . ? N1 C1 1.416(4) . ? N2 C25 1.318(4) . ? N2 C13 1.421(5) . ? N3 C50 1.329(4) . ? N3 C26 1.405(4) . ? N4 C50 1.326(4) . ? N4 C38 1.425(4) . ? C1 C6 1.405(5) . ? C1 C2 1.415(5) . ? C2 C3 1.395(5) . ? C2 C7 1.511(5) . ? C3 C4 1.373(5) . ? C4 C5 1.386(5) . ? C5 C6 1.389(5) . ? C6 C10 1.523(5) . ? C7 C9 1.529(6) . ? C7 C8 1.537(6) . ? C10 C12 1.522(5) . ? C10 C11 1.526(6) . ? C13 C18 1.410(5) . ? C13 C14 1.412(5) . ? C14 C15 1.380(5) . ? C14 C19 1.527(5) . ? C15 C16 1.392(6) . ? C16 C17 1.365(6) . ? C17 C18 1.401(6) . ? C18 C22 1.511(6) . ? C19 C20 1.522(5) . ? C19 C21 1.541(5) . ? C22 C24 1.526(6) . ? C22 C23 1.532(6) . ? C26 C27 1.416(5) . ? C26 C31 1.424(5) . ? C27 C28 1.399(5) . ? C27 C32 1.515(5) . ? C28 C29 1.379(5) . ? C29 C30 1.388(5) . ? C30 C31 1.391(5) . ? C31 C35 1.524(5) . ? C32 C34 1.525(5) . ? C32 C33 1.531(5) . ? C35 C36 1.517(5) . ? C35 C37 1.530(5) . ? C38 C43 1.406(5) . ? C38 C39 1.415(5) . ? C39 C40 1.396(5) . ? C39 C44 1.518(5) . ? C40 C41 1.386(5) . ? C41 C42 1.379(5) . ? C42 C43 1.399(5) . ? C43 C47 1.522(5) . ? C44 C46 1.532(5) . ? C44 C45 1.536(5) . ? C47 C49 1.535(5) . ? C47 C48 1.538(5) . ? C51 C52 1.465(6) . ? C52 C53 1.502(6) . ? C53 C54 1.515(6) . ? C55 C56 1.510(6) . ? C56 C57 1.508(6) . ? C57 C58 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sr1 O1 112.67(9) . . ? N1 Sr1 N3 126.65(10) . . ? O1 Sr1 N3 110.55(9) . . ? N1 Sr1 O2 84.41(9) . . ? O1 Sr1 O2 78.39(9) . . ? N3 Sr1 O2 134.33(8) . . ? N1 Sr1 N2 52.87(9) . . ? O1 Sr1 N2 93.57(9) . . ? N3 Sr1 N2 95.23(9) . . ? O2 Sr1 N2 129.69(9) . . ? N1 Sr1 N4 133.64(9) . . ? O1 Sr1 N4 107.30(9) . . ? N3 Sr1 N4 52.88(9) . . ? O2 Sr1 N4 81.49(9) . . ? N2 Sr1 N4 146.17(9) . . ? N1 Sr1 C25 26.44(9) . . ? O1 Sr1 C25 103.35(9) . . ? N3 Sr1 C25 113.58(9) . . ? O2 Sr1 C25 106.95(9) . . ? N2 Sr1 C25 26.49(9) . . ? N4 Sr1 C25 149.29(9) . . ? N1 Sr1 C50 138.23(9) . . ? O1 Sr1 C50 108.92(9) . . ? N3 Sr1 C50 26.54(9) . . ? O2 Sr1 C50 107.81(9) . . ? N2 Sr1 C50 121.53(9) . . ? N4 Sr1 C50 26.53(9) . . ? C25 Sr1 C50 136.27(9) . . ? C51 O1 C54 108.9(3) . . ? C51 O1 Sr1 121.9(2) . . ? C54 O1 Sr1 129.2(2) . . ? C55 O2 C58 108.9(3) . . ? C55 O2 Sr1 118.1(2) . . ? C58 O2 Sr1 123.1(2) . . ? C25 N1 C1 119.6(3) . . ? C25 N1 Sr1 94.7(2) . . ? C1 N1 Sr1 145.1(2) . . ? C25 N2 C13 119.9(3) . . ? C25 N2 Sr1 91.2(2) . . ? C13 N2 Sr1 148.9(2) . . ? C50 N3 C26 117.5(3) . . ? C50 N3 Sr1 93.9(2) . . ? C26 N3 Sr1 148.6(2) . . ? C50 N4 C38 116.2(3) . . ? C50 N4 Sr1 91.56(19) . . ? C38 N4 Sr1 149.4(2) . . ? C6 C1 C2 120.0(3) . . ? C6 C1 N1 120.7(3) . . ? C2 C1 N1 119.2(3) . . ? C3 C2 C1 118.1(3) . . ? C3 C2 C7 120.4(3) . . ? C1 C2 C7 121.5(3) . . ? C4 C3 C2 122.1(3) . . ? C3 C4 C5 119.5(4) . . ? C4 C5 C6 120.9(4) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C10 119.5(3) . . ? C1 C6 C10 121.0(3) . . ? C2 C7 C9 113.0(3) . . ? C2 C7 C8 110.2(3) . . ? C9 C7 C8 109.9(3) . . ? C12 C10 C6 110.4(3) . . ? C12 C10 C11 110.3(3) . . ? C6 C10 C11 113.1(3) . . ? C18 C13 C14 119.6(3) . . ? C18 C13 N2 121.0(4) . . ? C14 C13 N2 119.2(3) . . ? C15 C14 C13 119.2(4) . . ? C15 C14 C19 121.2(4) . . ? C13 C14 C19 119.6(3) . . ? C14 C15 C16 121.6(4) . . ? C17 C16 C15 119.0(4) . . ? C16 C17 C18 122.0(4) . . ? C17 C18 C13 118.5(4) . . ? C17 C18 C22 118.8(3) . . ? C13 C18 C22 122.7(4) . . ? C20 C19 C14 113.8(3) . . ? C20 C19 C21 109.4(3) . . ? C14 C19 C21 109.7(3) . . ? C18 C22 C24 112.3(4) . . ? C18 C22 C23 110.5(4) . . ? C24 C22 C23 110.8(4) . . ? N2 C25 N1 120.9(3) . . ? N2 C25 Sr1 62.30(17) . . ? N1 C25 Sr1 58.83(17) . . ? N3 C26 C27 119.0(3) . . ? N3 C26 C31 120.9(3) . . ? C27 C26 C31 120.1(3) . . ? C28 C27 C26 118.6(3) . . ? C28 C27 C32 120.6(3) . . ? C26 C27 C32 120.7(3) . . ? C29 C28 C27 121.8(4) . . ? C28 C29 C30 118.9(4) . . ? C29 C30 C31 122.4(3) . . ? C30 C31 C26 118.0(3) . . ? C30 C31 C35 121.8(3) . . ? C26 C31 C35 120.2(3) . . ? C27 C32 C34 109.9(3) . . ? C27 C32 C33 114.3(3) . . ? C34 C32 C33 111.3(3) . . ? C36 C35 C31 111.8(3) . . ? C36 C35 C37 109.6(3) . . ? C31 C35 C37 114.6(3) . . ? C43 C38 C39 119.8(3) . . ? C43 C38 N4 121.9(3) . . ? C39 C38 N4 118.3(3) . . ? C40 C39 C38 118.5(3) . . ? C40 C39 C44 120.3(3) . . ? C38 C39 C44 121.1(3) . . ? C41 C40 C39 121.8(3) . . ? C42 C41 C40 119.3(3) . . ? C41 C42 C43 121.2(3) . . ? C42 C43 C38 119.3(3) . . ? C42 C43 C47 118.7(3) . . ? C38 C43 C47 122.0(3) . . ? C39 C44 C46 111.0(3) . . ? C39 C44 C45 113.1(3) . . ? C46 C44 C45 109.7(3) . . ? C43 C47 C49 112.2(3) . . ? C43 C47 C48 111.3(3) . . ? C49 C47 C48 109.9(3) . . ? N4 C50 N3 120.8(3) . . ? N4 C50 Sr1 61.91(16) . . ? N3 C50 Sr1 59.56(17) . . ? O1 C51 C52 106.2(4) . . ? C51 C52 C53 103.2(4) . . ? C52 C53 C54 103.3(3) . . ? O1 C54 C53 105.5(3) . . ? O2 C55 C56 106.5(3) . . ? C57 C56 C55 102.2(3) . . ? C56 C57 C58 102.7(4) . . ? O2 C58 C57 105.0(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.858 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.116 #===END data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 247618' _ccdc_chemical_compound_source_recrystallisation Toluene _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ba(DippForm)2(THF)2]' _chemical_melting_point '475 decomp.' _chemical_formula_moiety 'C58 H86 Ba N4 O2' _chemical_formula_sum 'C58 H86 Ba N4 O2' _chemical_formula_weight 1008.65 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' 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' Ba Ba -0.3244 2.2819 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9811(4) _cell_length_b 12.8483(4) _cell_length_c 20.3537(9) _cell_angle_alpha 84.4630(10) _cell_angle_beta 86.0010(10) _cell_angle_gamma 63.451(3) _cell_volume 2788.47(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rhombohedral plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8054 _exptl_absorpt_correction_T_max 0.8638 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40603 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.1679 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13111 _reflns_number_gt 7398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0428P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13111 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 Ba1 Ba 0.84220(2) 0.79227(2) 0.739971(12) 0.02987(9) Uani 1 1 d . . . O1 O 1.0611(3) 0.6769(3) 0.67319(16) 0.0647(9) Uani 1 1 d . . . O2 O 0.9615(3) 0.9220(3) 0.76430(17) 0.0658(10) Uani 1 1 d . . . N1 N 0.6824(3) 0.9920(2) 0.67704(14) 0.0336(8) Uani 1 1 d . . . N2 N 0.6742(3) 0.8296(3) 0.64358(14) 0.0314(7) Uani 1 1 d . . . N3 N 0.7827(3) 0.6481(2) 0.82377(14) 0.0289(7) Uani 1 1 d . . . N4 N 0.8879(2) 0.7306(2) 0.87305(14) 0.0236(7) Uani 1 1 d . . . C1 C 0.6246(3) 0.7807(3) 0.60048(19) 0.0358(9) Uani 1 1 d . . . C2 C 0.5354(4) 0.7424(3) 0.6264(2) 0.0392(10) Uani 1 1 d . . . C3 C 0.4954(4) 0.6851(4) 0.5868(2) 0.0626(14) Uani 1 1 d . . . H3 H 0.4383 0.6562 0.6045 0.075 Uiso 1 1 calc R . . C4 C 0.5368(5) 0.6689(6) 0.5221(3) 0.093(2) Uani 1 1 d . . . H4 H 0.5072 0.6304 0.4953 0.111 Uiso 1 1 calc R . . C5 C 0.6201(5) 0.7082(6) 0.4966(3) 0.088(2) Uani 1 1 d . . . H5 H 0.6464 0.6986 0.4516 0.105 Uiso 1 1 calc R . . C6 C 0.6684(4) 0.7628(4) 0.5353(2) 0.0526(12) Uani 1 1 d . B . C7 C 0.4832(4) 0.7671(3) 0.69618(19) 0.0360(9) Uani 1 1 d . . . H7 H 0.5517 0.7628 0.7234 0.043 Uiso 1 1 calc R . . C8 C 0.4372(4) 0.6799(3) 0.7291(2) 0.0491(11) Uani 1 1 d . . . H8A H 0.3604 0.6920 0.7084 0.074 Uiso 1 1 calc R . . H8B H 0.4204 0.6920 0.7763 0.074 Uiso 1 1 calc R . . H8C H 0.5014 0.6001 0.7236 0.074 Uiso 1 1 calc R . . C9 C 0.3779(4) 0.8907(3) 0.6975(2) 0.0472(11) Uani 1 1 d . . . H9A H 0.4080 0.9464 0.6778 0.071 Uiso 1 1 calc R . . H9B H 0.3498 0.9079 0.7433 0.071 Uiso 1 1 calc R . . H9C H 0.3080 0.8971 0.6723 0.071 Uiso 1 1 calc R . . C10 C 0.7672(4) 0.7976(5) 0.5055(2) 0.0621(14) Uani 1 1 d . . . H10 H 0.7824 0.8472 0.5352 0.075 Uiso 1 1 calc R A 1 C11 C 0.8882(5) 0.6901(6) 0.4905(4) 0.130(3) Uani 1 1 d . B . H11A H 0.8716 0.6436 0.4606 0.195 Uiso 1 1 calc R . . H11B H 0.9212 0.6429 0.5317 0.195 Uiso 1 1 calc R . . H11C H 0.9496 0.7147 0.4695 0.195 Uiso 1 1 calc R . . C12A C 0.7320(19) 0.858(3) 0.4401(8) 0.097(7) Uani 0.68(4) 1 d P B 1 H12A H 0.7096 0.8108 0.4132 0.146 Uiso 0.68(4) 1 calc PR B 1 H12B H 0.8024 0.8683 0.4188 0.146 Uiso 0.68(4) 1 calc PR B 1 H12C H 0.6603 0.9339 0.4445 0.146 Uiso 0.68(4) 1 calc PR B 1 C12B C 0.707(2) 0.933(4) 0.4568(15) 0.063(9) Uani 0.32(4) 1 d P B 2 H12D H 0.7765 0.9473 0.4376 0.095 Uiso 0.32(4) 1 calc PR B 2 H12E H 0.6541 0.9956 0.4847 0.095 Uiso 0.32(4) 1 calc PR B 2 H12F H 0.6578 0.9292 0.4214 0.095 Uiso 0.32(4) 1 calc PR B 2 C13 C 0.6369(3) 1.1149(3) 0.67089(18) 0.0340(9) Uani 1 1 d . . . C14 C 0.5387(4) 1.1833(3) 0.71297(19) 0.0386(10) Uani 1 1 d . . . C15 C 0.5015(4) 1.3034(4) 0.7088(2) 0.0507(12) Uani 1 1 d . . . H15 H 0.4360 1.3507 0.7374 0.061 Uiso 1 1 calc R . . C16 C 0.5562(5) 1.3545(4) 0.6650(2) 0.0593(13) Uani 1 1 d . . . H16 H 0.5276 1.4366 0.6624 0.071 Uiso 1 1 calc R . . C17 C 0.6527(5) 1.2870(4) 0.6249(2) 0.0582(13) Uani 1 1 d . . . H17 H 0.6912 1.3229 0.5946 0.070 Uiso 1 1 calc R . . C18 C 0.6953(4) 1.1674(3) 0.6273(2) 0.0442(10) Uani 1 1 d . D . C19 C 0.4772(4) 1.1286(4) 0.7635(2) 0.0468(11) Uani 1 1 d . . . H19 H 0.5092 1.0449 0.7543 0.056 Uiso 1 1 calc R . . C20 C 0.5148(4) 1.1315(5) 0.8338(2) 0.0664(14) Uani 1 1 d . . . H20A H 0.6060 1.0941 0.8359 0.100 Uiso 1 1 calc R . . H20B H 0.4806 1.0896 0.8652 0.100 Uiso 1 1 calc R . . H20C H 0.4817 1.2127 0.8450 0.100 Uiso 1 1 calc R . . C21 C 0.3350(4) 1.1852(4) 0.7594(3) 0.0666(14) Uani 1 1 d . . . H21A H 0.3007 1.2674 0.7689 0.100 Uiso 1 1 calc R . . H21B H 0.3010 1.1445 0.7918 0.100 Uiso 1 1 calc R . . H21C H 0.3122 1.1801 0.7149 0.100 Uiso 1 1 calc R . . C22 C 0.8058(5) 1.0925(4) 0.5827(2) 0.0642(14) Uani 1 1 d . . . H22 H 0.8387 1.0099 0.6018 0.077 Uiso 1 1 calc R C 1 C23A C 0.9076(9) 1.1256(10) 0.5810(5) 0.091(3) Uiso 0.626(9) 1 d P D 1 H23A H 0.9771 1.0738 0.5536 0.137 Uiso 0.626(9) 1 calc PR D 1 H23B H 0.9357 1.1191 0.6260 0.137 Uiso 0.626(9) 1 calc PR D 1 H23C H 0.8784 1.2064 0.5624 0.137 Uiso 0.626(9) 1 calc PR D 1 C23B C 0.9437(14) 1.0504(15) 0.6191(8) 0.082(5) Uiso 0.374(9) 1 d P D 2 H23D H 1.0118 0.9989 0.5908 0.123 Uiso 0.374(9) 1 calc PR D 2 H23E H 0.9435 1.0086 0.6620 0.123 Uiso 0.374(9) 1 calc PR D 2 H23F H 0.9556 1.1193 0.6256 0.123 Uiso 0.374(9) 1 calc PR D 2 C24A C 0.7556(8) 1.0976(8) 0.5122(4) 0.079(3) Uiso 0.626(9) 1 d P D 1 H24A H 0.7311 1.1756 0.4902 0.119 Uiso 0.626(9) 1 calc PR D 1 H24B H 0.6831 1.0809 0.5170 0.119 Uiso 0.626(9) 1 calc PR D 1 H24C H 0.8214 1.0395 0.4858 0.119 Uiso 0.626(9) 1 calc PR D 1 C24B C 0.8278(15) 1.1515(15) 0.5175(8) 0.093(6) Uiso 0.374(9) 1 d P D 2 H24D H 0.8531 1.2113 0.5266 0.140 Uiso 0.374(9) 1 calc PR D 2 H24E H 0.7505 1.1879 0.4928 0.140 Uiso 0.374(9) 1 calc PR D 2 H24F H 0.8937 1.0931 0.4913 0.140 Uiso 0.374(9) 1 calc PR D 2 C25 C 0.6384(3) 0.9428(3) 0.63905(18) 0.0328(9) Uani 1 1 d . . . H25 H 0.5788 0.9905 0.6072 0.039 Uiso 1 1 calc R . . C26 C 0.7280(3) 0.5700(3) 0.83171(18) 0.0295(9) Uani 1 1 d . . . C27 C 0.7684(3) 0.4788(3) 0.7888(2) 0.0370(10) Uani 1 1 d . F . C28 C 0.7132(4) 0.4022(3) 0.7963(2) 0.0461(11) Uani 1 1 d . . . H28 H 0.7404 0.3395 0.7684 0.055 Uiso 1 1 calc R . . C29 C 0.6204(4) 0.4165(4) 0.8433(2) 0.0492(12) Uani 1 1 d . . . H29 H 0.5846 0.3634 0.8479 0.059 Uiso 1 1 calc R . . C30 C 0.5790(4) 0.5070(4) 0.8836(2) 0.0445(11) Uani 1 1 d . . . H30 H 0.5140 0.5160 0.9155 0.053 Uiso 1 1 calc R . . C31 C 0.6302(3) 0.5858(3) 0.87890(19) 0.0324(9) Uani 1 1 d . . . C32 C 0.8713(4) 0.4625(4) 0.7372(3) 0.0481(12) Uani 1 1 d . . . H32 H 0.9093 0.5127 0.7497 0.058 Uiso 1 1 calc R E 1 C33A C 0.8296(12) 0.504(2) 0.6752(12) 0.098(9) Uani 0.52(3) 1 d P F 1 H33A H 0.9006 0.4937 0.6449 0.147 Uiso 0.52(3) 1 calc PR F 1 H33B H 0.7720 0.5877 0.6753 0.147 Uiso 0.52(3) 1 calc PR F 1 H33C H 0.7860 0.4622 0.6606 0.147 Uiso 0.52(3) 1 calc PR F 1 C33B C 0.8408(13) 0.4347(18) 0.6666(7) 0.051(5) Uani 0.48(3) 1 d P F 2 H33D H 0.7557 0.4905 0.6547 0.076 Uiso 0.48(3) 1 calc PR F 2 H33E H 0.8481 0.3553 0.6696 0.076 Uiso 0.48(3) 1 calc PR F 2 H33F H 0.9001 0.4414 0.6328 0.076 Uiso 0.48(3) 1 calc PR F 2 C34A C 0.9821(17) 0.3320(15) 0.7430(10) 0.078(6) Uani 0.52(3) 1 d P F 1 H34A H 0.9514 0.2774 0.7312 0.117 Uiso 0.52(3) 1 calc PR F 1 H34B H 1.0110 0.3119 0.7884 0.117 Uiso 0.52(3) 1 calc PR F 1 H34C H 1.0514 0.3271 0.7129 0.117 Uiso 0.52(3) 1 calc PR F 1 C34B C 0.9914(15) 0.380(2) 0.7598(10) 0.066(5) Uani 0.48(3) 1 d P F 2 H34D H 0.9908 0.3042 0.7716 0.098 Uiso 0.48(3) 1 calc PR F 2 H34E H 1.0113 0.4072 0.7986 0.098 Uiso 0.48(3) 1 calc PR F 2 H34F H 1.0545 0.3712 0.7246 0.098 Uiso 0.48(3) 1 calc PR F 2 C35 C 0.5779(3) 0.6909(4) 0.92118(19) 0.0406(10) Uani 1 1 d . . . H35 H 0.6512 0.6968 0.9380 0.049 Uiso 1 1 calc R . . C36 C 0.5043(4) 0.8043(4) 0.8801(2) 0.0517(11) Uani 1 1 d . . . H36A H 0.4315 0.8020 0.8623 0.078 Uiso 1 1 calc R . . H36B H 0.5576 0.8137 0.8435 0.078 Uiso 1 1 calc R . . H36C H 0.4764 0.8701 0.9079 0.078 Uiso 1 1 calc R . . C37 C 0.4995(4) 0.6805(4) 0.9816(2) 0.0592(13) Uani 1 1 d . . . H37A H 0.4846 0.7423 1.0106 0.089 Uiso 1 1 calc R . . H37B H 0.5442 0.6042 1.0055 0.089 Uiso 1 1 calc R . . H37C H 0.4195 0.6884 0.9674 0.089 Uiso 1 1 calc R . . C38 C 0.9643(3) 0.7207(3) 0.92577(17) 0.0255(8) Uani 1 1 d . . . C39 C 0.9232(3) 0.8131(3) 0.96764(18) 0.0274(8) Uani 1 1 d . . . C40 C 0.9960(3) 0.8035(3) 1.01993(19) 0.0377(10) Uani 1 1 d . . . H40 H 0.9677 0.8654 1.0483 0.045 Uiso 1 1 calc R . . C41 C 1.1077(3) 0.7074(4) 1.0321(2) 0.0396(10) Uani 1 1 d . . . H41 H 1.1548 0.7019 1.0691 0.048 Uiso 1 1 calc R . . C42 C 1.1501(3) 0.6193(3) 0.98991(19) 0.0357(10) Uani 1 1 d . . . H42 H 1.2283 0.5535 0.9976 0.043 Uiso 1 1 calc R . . C43 C 1.0815(3) 0.6238(3) 0.93611(17) 0.0282(8) Uani 1 1 d . . . C44 C 0.7993(3) 0.9196(3) 0.95607(19) 0.0322(9) Uani 1 1 d . . . H44 H 0.7801 0.9255 0.9084 0.039 Uiso 1 1 calc R . . C45 C 0.8010(4) 1.0345(3) 0.9701(2) 0.0511(12) Uani 1 1 d . . . H45A H 0.8076 1.0362 1.0177 0.077 Uiso 1 1 calc R . . H45B H 0.7238 1.1006 0.9548 0.077 Uiso 1 1 calc R . . H45C H 0.8728 1.0399 0.9467 0.077 Uiso 1 1 calc R . . C46 C 0.6939(4) 0.9060(4) 0.9970(2) 0.0540(12) Uani 1 1 d . . . H46A H 0.6902 0.8349 0.9863 0.081 Uiso 1 1 calc R . . H46B H 0.6143 0.9737 0.9869 0.081 Uiso 1 1 calc R . . H46C H 0.7098 0.9006 1.0441 0.081 Uiso 1 1 calc R . . C47 C 1.1372(3) 0.5266(3) 0.88891(19) 0.0319(9) Uani 1 1 d . . . H47 H 1.0805 0.5495 0.8508 0.038 Uiso 1 1 calc R . . C48 C 1.2662(3) 0.5098(4) 0.8616(2) 0.0437(10) Uani 1 1 d . . . H48A H 1.2603 0.5841 0.8409 0.066 Uiso 1 1 calc R . . H48B H 1.2960 0.4515 0.8287 0.066 Uiso 1 1 calc R . . H48C H 1.3248 0.4831 0.8978 0.066 Uiso 1 1 calc R . . C49 C 1.1466(4) 0.4106(3) 0.9215(2) 0.0428(10) Uani 1 1 d . . . H49A H 1.2036 0.3851 0.9583 0.064 Uiso 1 1 calc R . . H49B H 1.1783 0.3517 0.8889 0.064 Uiso 1 1 calc R . . H49C H 1.0638 0.4208 0.9380 0.064 Uiso 1 1 calc R . . C50 C 0.8456(3) 0.6517(3) 0.87338(18) 0.0268(8) Uani 1 1 d . . . H50 H 0.8610 0.5962 0.9102 0.032 Uiso 1 1 calc R . . C51 C 1.1532(5) 0.5612(5) 0.6927(3) 0.0823(17) Uani 1 1 d . . . H51A H 1.2223 0.5638 0.7154 0.099 Uiso 1 1 calc R . . H51B H 1.1156 0.5192 0.7227 0.099 Uiso 1 1 calc R . . C52 C 1.1971(7) 0.5057(5) 0.6321(3) 0.109(2) Uani 1 1 d . . . H52A H 1.1411 0.4739 0.6190 0.130 Uiso 1 1 calc R . . H52B H 1.2824 0.4412 0.6367 0.130 Uiso 1 1 calc R . . C53 C 1.1969(5) 0.6005(5) 0.5818(3) 0.0753(16) Uani 1 1 d . . . H53A H 1.1687 0.5934 0.5386 0.090 Uiso 1 1 calc R . . H53B H 1.2811 0.5972 0.5758 0.090 Uiso 1 1 calc R . . C54 C 1.1049(5) 0.7131(5) 0.6115(2) 0.0703(14) Uani 1 1 d . . . H54A H 1.1467 0.7620 0.6192 0.084 Uiso 1 1 calc R . . H54B H 1.0345 0.7584 0.5818 0.084 Uiso 1 1 calc R . . C55 C 1.0840(4) 0.8562(4) 0.7907(2) 0.0585(13) Uani 1 1 d . . . H55A H 1.1487 0.8371 0.7548 0.070 Uiso 1 1 calc R . . H55B H 1.0914 0.7827 0.8146 0.070 Uiso 1 1 calc R . . C56 C 1.0987(4) 0.9333(5) 0.8372(3) 0.0676(15) Uani 1 1 d . . . H56A H 1.0686 0.9211 0.8825 0.081 Uiso 1 1 calc R . . H56B H 1.1868 0.9194 0.8385 0.081 Uiso 1 1 calc R . . C57 C 1.0180(5) 1.0534(5) 0.8071(3) 0.0731(16) Uani 1 1 d . . . H57A H 1.0621 1.0759 0.7697 0.088 Uiso 1 1 calc R . . H57B H 0.9912 1.1123 0.8401 0.088 Uiso 1 1 calc R . . C58 C 0.9084(5) 1.0399(4) 0.7838(3) 0.0722(15) Uani 1 1 d . . . H58A H 0.8450 1.0518 0.8199 0.087 Uiso 1 1 calc R . . H58B H 0.8689 1.0966 0.7461 0.087 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 Ba1 0.02856(13) 0.02610(14) 0.03673(16) 0.00300(9) -0.00386(9) -0.01432(10) O1 0.0478(19) 0.052(2) 0.076(2) -0.0062(18) 0.0202(16) -0.0085(17) O2 0.054(2) 0.0432(19) 0.116(3) 0.0123(19) -0.0316(18) -0.0343(17) N1 0.0463(19) 0.0226(18) 0.0260(19) -0.0036(14) -0.0067(15) -0.0088(15) N2 0.0344(18) 0.0283(19) 0.0314(19) -0.0028(15) -0.0083(14) -0.0126(15) N3 0.0296(17) 0.0273(17) 0.0357(19) 0.0029(14) -0.0053(14) -0.0184(14) N4 0.0186(15) 0.0214(16) 0.0319(18) -0.0024(13) -0.0027(12) -0.0095(13) C1 0.031(2) 0.033(2) 0.039(3) -0.0091(19) -0.0060(18) -0.0089(18) C2 0.042(2) 0.039(2) 0.040(3) -0.008(2) -0.0137(19) -0.017(2) C3 0.056(3) 0.082(4) 0.063(4) -0.028(3) 0.001(2) -0.038(3) C4 0.076(4) 0.157(6) 0.082(4) -0.070(4) 0.014(3) -0.074(4) C5 0.072(4) 0.153(6) 0.057(4) -0.055(4) 0.004(3) -0.057(4) C6 0.039(3) 0.070(3) 0.042(3) -0.015(2) -0.004(2) -0.015(2) C7 0.041(2) 0.028(2) 0.041(3) -0.0002(19) -0.0093(19) -0.0163(19) C8 0.051(3) 0.035(2) 0.065(3) 0.009(2) -0.021(2) -0.022(2) C9 0.050(3) 0.036(3) 0.056(3) -0.001(2) 0.006(2) -0.020(2) C10 0.053(3) 0.099(4) 0.036(3) -0.022(3) 0.008(2) -0.034(3) C11 0.062(4) 0.159(7) 0.194(8) -0.121(6) 0.050(4) -0.058(4) C12A 0.101(10) 0.15(2) 0.059(8) 0.023(10) -0.013(6) -0.074(14) C12B 0.064(12) 0.076(19) 0.042(13) 0.027(11) -0.016(9) -0.028(12) C13 0.042(2) 0.022(2) 0.029(2) -0.0033(18) -0.0059(18) -0.0047(18) C14 0.047(2) 0.028(2) 0.033(2) -0.0049(19) -0.0031(19) -0.009(2) C15 0.063(3) 0.031(3) 0.040(3) -0.009(2) 0.001(2) -0.004(2) C16 0.096(4) 0.027(3) 0.042(3) -0.002(2) -0.012(3) -0.015(3) C17 0.087(4) 0.038(3) 0.047(3) -0.002(2) 0.009(3) -0.027(3) C18 0.058(3) 0.027(2) 0.037(3) 0.001(2) 0.002(2) -0.011(2) C19 0.038(2) 0.036(3) 0.053(3) -0.009(2) 0.004(2) -0.005(2) C20 0.062(3) 0.094(4) 0.047(3) 0.017(3) -0.004(2) -0.043(3) C21 0.047(3) 0.069(4) 0.077(4) -0.028(3) 0.002(2) -0.016(3) C22 0.086(4) 0.039(3) 0.055(3) 0.003(2) 0.019(3) -0.021(3) C25 0.027(2) 0.033(2) 0.027(2) -0.0008(18) -0.0023(16) -0.0026(18) C26 0.028(2) 0.024(2) 0.039(2) 0.0093(18) -0.0152(17) -0.0148(17) C27 0.031(2) 0.026(2) 0.058(3) 0.003(2) -0.0090(19) -0.0164(18) C28 0.040(2) 0.025(2) 0.078(3) 0.000(2) -0.015(2) -0.018(2) C29 0.044(3) 0.038(3) 0.078(4) 0.025(3) -0.025(2) -0.032(2) C30 0.033(2) 0.055(3) 0.052(3) 0.018(2) -0.0125(19) -0.028(2) C31 0.025(2) 0.034(2) 0.041(2) 0.0128(19) -0.0118(17) -0.0162(18) C32 0.038(3) 0.032(3) 0.082(4) -0.018(3) 0.007(2) -0.022(2) C33A 0.046(6) 0.075(14) 0.125(15) 0.048(13) 0.008(8) 0.004(8) C33B 0.041(6) 0.050(9) 0.060(8) -0.033(7) 0.005(5) -0.015(7) C34A 0.057(9) 0.041(10) 0.086(12) -0.004(8) 0.008(7) 0.020(7) C34B 0.032(6) 0.053(12) 0.101(12) -0.013(8) 0.006(7) -0.009(7) C35 0.031(2) 0.057(3) 0.039(3) 0.006(2) -0.0045(18) -0.026(2) C36 0.055(3) 0.048(3) 0.046(3) -0.004(2) -0.002(2) -0.017(2) C37 0.037(3) 0.071(4) 0.058(3) 0.012(3) 0.004(2) -0.018(2) C38 0.0222(18) 0.030(2) 0.030(2) 0.0004(17) 0.0002(15) -0.0173(17) C39 0.0229(19) 0.027(2) 0.034(2) -0.0030(17) -0.0024(16) -0.0124(16) C40 0.040(2) 0.039(2) 0.043(3) -0.014(2) 0.0023(19) -0.024(2) C41 0.035(2) 0.048(3) 0.039(3) -0.009(2) -0.0117(18) -0.019(2) C42 0.0217(19) 0.042(2) 0.045(3) 0.000(2) -0.0076(17) -0.0157(18) C43 0.0242(19) 0.033(2) 0.033(2) -0.0038(17) 0.0017(16) -0.0180(17) C44 0.031(2) 0.028(2) 0.038(2) -0.0105(18) -0.0010(17) -0.0125(17) C45 0.040(2) 0.036(3) 0.075(3) -0.015(2) 0.006(2) -0.014(2) C46 0.031(2) 0.047(3) 0.082(4) -0.008(2) 0.005(2) -0.016(2) C47 0.0231(19) 0.030(2) 0.040(2) -0.0037(18) 0.0014(16) -0.0094(17) C48 0.032(2) 0.040(3) 0.056(3) -0.010(2) 0.0084(19) -0.0130(19) C49 0.039(2) 0.034(2) 0.054(3) -0.005(2) 0.003(2) -0.014(2) C50 0.0199(18) 0.027(2) 0.033(2) 0.0015(17) -0.0012(16) -0.0107(16) C51 0.064(4) 0.065(4) 0.101(5) -0.008(3) 0.004(3) -0.015(3) C52 0.141(6) 0.072(4) 0.069(4) -0.010(4) -0.031(4) -0.003(4) C53 0.063(3) 0.089(4) 0.071(4) -0.034(4) 0.014(3) -0.028(3) C54 0.071(3) 0.071(4) 0.065(4) -0.012(3) 0.009(3) -0.027(3) C55 0.040(3) 0.061(3) 0.084(4) 0.001(3) -0.010(2) -0.031(2) C56 0.054(3) 0.107(5) 0.062(3) -0.009(3) 0.003(3) -0.054(3) C57 0.102(4) 0.081(4) 0.066(4) -0.021(3) 0.007(3) -0.066(4) C58 0.074(4) 0.054(3) 0.092(4) 0.000(3) -0.013(3) -0.031(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 Ba1 N1 2.685(3) . ? Ba1 N3 2.693(3) . ? Ba1 O1 2.709(3) . ? Ba1 O2 2.730(3) . ? Ba1 N2 2.763(3) . ? Ba1 N4 2.769(3) . ? Ba1 C25 3.104(4) . ? Ba1 C50 3.105(4) . ? O1 C51 1.438(6) . ? O1 C54 1.442(6) . ? O2 C55 1.439(5) . ? O2 C58 1.442(5) . ? N1 C25 1.313(4) . ? N1 C13 1.417(4) . ? N2 C25 1.315(4) . ? N2 C1 1.425(4) . ? N3 C50 1.318(4) . ? N3 C26 1.416(4) . ? N4 C50 1.320(4) . ? N4 C38 1.419(4) . ? C1 C6 1.394(6) . ? C1 C2 1.415(5) . ? C2 C3 1.382(5) . ? C2 C7 1.514(5) . ? C3 C4 1.376(7) . ? C4 C5 1.360(7) . ? C5 C6 1.406(6) . ? C6 C10 1.512(6) . ? C7 C9 1.525(5) . ? C7 C8 1.538(5) . ? C10 C12A 1.461(13) . ? C10 C11 1.527(7) . ? C10 C12B 1.78(3) . ? C13 C18 1.397(5) . ? C13 C14 1.404(5) . ? C14 C15 1.397(5) . ? C14 C19 1.520(6) . ? C15 C16 1.359(6) . ? C16 C17 1.366(6) . ? C17 C18 1.382(5) . ? C18 C22 1.538(6) . ? C19 C21 1.529(6) . ? C19 C20 1.538(6) . ? C22 C23A 1.457(10) . ? C22 C24B 1.530(17) . ? C22 C24A 1.578(9) . ? C22 C23B 1.692(15) . ? C26 C27 1.414(5) . ? C26 C31 1.415(5) . ? C27 C28 1.403(5) . ? C27 C32 1.517(6) . ? C28 C29 1.374(6) . ? C29 C30 1.372(6) . ? C30 C31 1.393(5) . ? C31 C35 1.533(5) . ? C32 C33A 1.360(19) . ? C32 C34B 1.429(17) . ? C32 C34A 1.606(15) . ? C32 C33B 1.617(13) . ? C35 C36 1.523(6) . ? C35 C37 1.527(5) . ? C38 C39 1.412(5) . ? C38 C43 1.412(5) . ? C39 C40 1.384(5) . ? C39 C44 1.517(5) . ? C40 C41 1.374(5) . ? C41 C42 1.375(5) . ? C42 C43 1.396(5) . ? C43 C47 1.525(5) . ? C44 C46 1.530(5) . ? C44 C45 1.540(5) . ? C47 C49 1.530(5) . ? C47 C48 1.534(5) . ? C51 C52 1.431(7) . ? C52 C53 1.514(8) . ? C53 C54 1.525(7) . ? C55 C56 1.507(6) . ? C56 C57 1.503(7) . ? C57 C58 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ba1 N3 126.67(9) . . ? N1 Ba1 O1 114.49(10) . . ? N3 Ba1 O1 112.26(9) . . ? N1 Ba1 O2 83.41(9) . . ? N3 Ba1 O2 129.19(9) . . ? O1 Ba1 O2 80.05(10) . . ? N1 Ba1 N2 49.94(9) . . ? N3 Ba1 N2 97.70(9) . . ? O1 Ba1 N2 100.61(9) . . ? O2 Ba1 N2 129.51(9) . . ? N1 Ba1 N4 131.10(8) . . ? N3 Ba1 N4 49.80(8) . . ? O1 Ba1 N4 107.07(9) . . ? O2 Ba1 N4 79.40(9) . . ? N2 Ba1 N4 143.42(8) . . ? N1 Ba1 C25 24.90(9) . . ? N3 Ba1 C25 114.32(9) . . ? O1 Ba1 C25 108.72(10) . . ? O2 Ba1 C25 106.42(9) . . ? N2 Ba1 C25 25.05(9) . . ? N4 Ba1 C25 144.21(8) . . ? N1 Ba1 C50 136.73(9) . . ? N3 Ba1 C50 25.00(8) . . ? O1 Ba1 C50 108.78(9) . . ? O2 Ba1 C50 104.40(9) . . ? N2 Ba1 C50 122.12(9) . . ? N4 Ba1 C50 25.14(8) . . ? C25 Ba1 C50 134.61(9) . . ? C51 O1 C54 107.3(4) . . ? C51 O1 Ba1 124.2(3) . . ? C54 O1 Ba1 128.4(3) . . ? C55 O2 C58 109.8(3) . . ? C55 O2 Ba1 115.0(2) . . ? C58 O2 Ba1 128.7(3) . . ? C25 N1 C13 119.2(3) . . ? C25 N1 Ba1 95.7(2) . . ? C13 N1 Ba1 145.0(2) . . ? C25 N2 C1 119.8(3) . . ? C25 N2 Ba1 92.1(2) . . ? C1 N2 Ba1 147.9(2) . . ? C50 N3 C26 117.6(3) . . ? C50 N3 Ba1 95.3(2) . . ? C26 N3 Ba1 146.6(2) . . ? C50 N4 C38 117.2(3) . . ? C50 N4 Ba1 91.8(2) . . ? C38 N4 Ba1 145.8(2) . . ? C6 C1 C2 120.0(3) . . ? C6 C1 N2 121.3(4) . . ? C2 C1 N2 118.6(3) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 C7 121.1(4) . . ? C1 C2 C7 119.9(3) . . ? C4 C3 C2 121.2(5) . . ? C5 C4 C3 119.7(4) . . ? C4 C5 C6 121.8(5) . . ? C1 C6 C5 118.2(4) . . ? C1 C6 C10 122.4(4) . . ? C5 C6 C10 119.3(4) . . ? C2 C7 C9 110.3(3) . . ? C2 C7 C8 114.3(3) . . ? C9 C7 C8 109.5(3) . . ? C12A C10 C6 110.7(6) . . ? C12A C10 C11 102.4(14) . . ? C6 C10 C11 110.9(5) . . ? C12A C10 C12B 32.7(7) . . ? C6 C10 C12B 114.2(9) . . ? C11 C10 C12B 125.4(11) . . ? C18 C13 C14 119.8(3) . . ? C18 C13 N1 120.7(3) . . ? C14 C13 N1 119.3(3) . . ? C15 C14 C13 118.0(4) . . ? C15 C14 C19 120.5(4) . . ? C13 C14 C19 121.4(3) . . ? C16 C15 C14 121.9(4) . . ? C15 C16 C17 119.6(4) . . ? C16 C17 C18 121.4(4) . . ? C17 C18 C13 119.3(4) . . ? C17 C18 C22 120.6(4) . . ? C13 C18 C22 120.1(3) . . ? C14 C19 C21 113.2(4) . . ? C14 C19 C20 110.7(3) . . ? C21 C19 C20 110.2(4) . . ? C23A C22 C24B 63.9(7) . . ? C23A C22 C18 112.2(5) . . ? C24B C22 C18 117.2(7) . . ? C23A C22 C24A 113.5(6) . . ? C24B C22 C24A 51.1(6) . . ? C18 C22 C24A 108.6(5) . . ? C23A C22 C23B 40.7(6) . . ? C24B C22 C23B 100.7(8) . . ? C18 C22 C23B 111.3(6) . . ? C24A C22 C23B 139.0(7) . . ? N1 C25 N2 122.2(3) . . ? N1 C25 Ba1 59.40(18) . . ? N2 C25 Ba1 62.84(18) . . ? C27 C26 N3 118.5(3) . . ? C27 C26 C31 120.2(3) . . ? N3 C26 C31 121.2(3) . . ? C28 C27 C26 118.5(4) . . ? C28 C27 C32 120.8(4) . . ? C26 C27 C32 120.7(3) . . ? C29 C28 C27 120.9(4) . . ? C30 C29 C28 120.5(4) . . ? C29 C30 C31 121.4(4) . . ? C30 C31 C26 118.5(4) . . ? C30 C31 C35 121.0(4) . . ? C26 C31 C35 120.5(3) . . ? C33A C32 C34B 131.1(10) . . ? C33A C32 C27 114.0(6) . . ? C34B C32 C27 112.4(9) . . ? C33A C32 C34A 115.3(10) . . ? C34B C32 C34A 29.2(7) . . ? C27 C32 C34A 111.6(8) . . ? C33A C32 C33B 32.9(9) . . ? C34B C32 C33B 112.6(8) . . ? C27 C32 C33B 112.5(5) . . ? C34A C32 C33B 87.8(7) . . ? C36 C35 C37 109.9(4) . . ? C36 C35 C31 111.5(3) . . ? C37 C35 C31 114.6(3) . . ? C39 C38 C43 119.2(3) . . ? C39 C38 N4 118.5(3) . . ? C43 C38 N4 122.2(3) . . ? C40 C39 C38 119.0(3) . . ? C40 C39 C44 121.0(3) . . ? C38 C39 C44 120.0(3) . . ? C41 C40 C39 122.2(3) . . ? C40 C41 C42 118.8(3) . . ? C41 C42 C43 121.8(3) . . ? C42 C43 C38 118.8(3) . . ? C42 C43 C47 119.2(3) . . ? C38 C43 C47 121.9(3) . . ? C39 C44 C46 111.0(3) . . ? C39 C44 C45 113.4(3) . . ? C46 C44 C45 109.6(3) . . ? C43 C47 C49 112.0(3) . . ? C43 C47 C48 111.7(3) . . ? C49 C47 C48 109.4(3) . . ? N3 C50 N4 121.5(3) . . ? N3 C50 Ba1 59.71(18) . . ? N4 C50 Ba1 63.06(19) . . ? C52 C51 O1 104.6(5) . . ? C51 C52 C53 105.2(5) . . ? C52 C53 C54 103.8(4) . . ? O1 C54 C53 105.4(4) . . ? O2 C55 C56 105.8(4) . . ? C57 C56 C55 102.2(4) . . ? C56 C57 C58 102.5(4) . . ? O2 C58 C57 104.5(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.948 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.108 #===END data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 247619' _ccdc_chemical_compound_source_recrystallisation 'Diethyl ether' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common DippN(4-HC6F4)C(H)NDipp _chemical_melting_point 451 _chemical_formula_moiety 'C31 H36 F4 N2' _chemical_formula_sum 'C31 H36 F4 N2' _chemical_formula_weight 512.62 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' F F 0.0171 0.0103 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4525(4) _cell_length_b 11.4180(5) _cell_length_c 14.3724(7) _cell_angle_alpha 110.256(3) _cell_angle_beta 91.904(2) _cell_angle_gamma 106.1040(10) _cell_volume 1383.70(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9734 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20737 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.79 _reflns_number_total 6442 _reflns_number_gt 4552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.1055P)^2^+0.1303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6442 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 F1 F 0.25058(10) 0.02346(9) 0.10983(7) 0.0267(2) Uani 1 1 d . . . F2 F 0.30495(12) -0.16395(10) -0.04086(7) 0.0323(3) Uani 1 1 d . . . F3 F 0.75015(11) -0.11064(10) 0.14956(8) 0.0320(3) Uani 1 1 d . . . F4 F 0.70078(10) 0.07974(9) 0.30021(7) 0.0254(2) Uani 1 1 d . . . N1 N 0.44953(14) 0.16415(12) 0.29207(9) 0.0188(3) Uani 1 1 d . . . N2 N 0.43495(14) 0.28872(12) 0.19527(10) 0.0201(3) Uani 1 1 d . . . C1 C 0.44579(17) 0.15764(15) 0.39144(12) 0.0200(3) Uani 1 1 d . . . C2 C 0.31926(18) 0.07315(16) 0.40881(12) 0.0233(3) Uani 1 1 d . . . C3 C 0.31718(19) 0.06636(17) 0.50327(13) 0.0287(4) Uani 1 1 d . . . H3 H 0.2344 0.0072 0.5158 0.034 Uiso 1 1 calc R . . C4 C 0.4346(2) 0.14501(18) 0.57975(14) 0.0305(4) Uani 1 1 d . . . H4 H 0.4321 0.1389 0.6440 0.037 Uiso 1 1 calc R . . C5 C 0.5544(2) 0.23169(17) 0.56258(13) 0.0272(4) Uani 1 1 d . . . H5 H 0.6318 0.2879 0.6164 0.033 Uiso 1 1 calc R . . C6 C 0.56535(18) 0.23924(15) 0.46810(12) 0.0217(3) Uani 1 1 d . . . C7 C 0.18103(19) -0.00158(18) 0.33059(14) 0.0300(4) Uani 1 1 d . . . H7 H 0.2080 0.0038 0.2652 0.036 Uiso 1 1 calc R . . C8 C 0.1227(3) -0.1450(2) 0.3161(2) 0.0752(10) Uani 1 1 d . . . H8A H 0.0891 -0.1530 0.3781 0.113 Uiso 1 1 calc R . . H8B H 0.2020 -0.1854 0.2995 0.113 Uiso 1 1 calc R . . H8C H 0.0390 -0.1896 0.2615 0.113 Uiso 1 1 calc R . . C9 C 0.0609(3) 0.0634(3) 0.3589(2) 0.0637(8) Uani 1 1 d . . . H9A H 0.0255 0.0518 0.4194 0.096 Uiso 1 1 calc R . . H9B H -0.0222 0.0233 0.3039 0.096 Uiso 1 1 calc R . . H9C H 0.1017 0.1573 0.3718 0.096 Uiso 1 1 calc R . . C10 C 0.70217(18) 0.33632(15) 0.45427(12) 0.0220(3) Uani 1 1 d . . . H10 H 0.6990 0.3207 0.3812 0.026 Uiso 1 1 calc R . . C11 C 0.84733(19) 0.32008(17) 0.49116(14) 0.0288(4) Uani 1 1 d . . . H11A H 0.8587 0.3465 0.5642 0.043 Uiso 1 1 calc R . . H11B H 0.9318 0.3754 0.4724 0.043 Uiso 1 1 calc R . . H11C H 0.8441 0.2280 0.4604 0.043 Uiso 1 1 calc R . . C12 C 0.7023(2) 0.47804(16) 0.51058(14) 0.0292(4) Uani 1 1 d . . . H12A H 0.6135 0.4911 0.4840 0.044 Uiso 1 1 calc R . . H12B H 0.7915 0.5393 0.5016 0.044 Uiso 1 1 calc R . . H12C H 0.7018 0.4940 0.5821 0.044 Uiso 1 1 calc R . . C13 C 0.40115(18) 0.40004(15) 0.18816(11) 0.0207(3) Uani 1 1 d . . . C14 C 0.51847(19) 0.50163(16) 0.18015(12) 0.0242(4) Uani 1 1 d . . . C15 C 0.4858(2) 0.60781(17) 0.16831(13) 0.0289(4) Uani 1 1 d . . . H15 H 0.5641 0.6772 0.1629 0.035 Uiso 1 1 calc R . . C16 C 0.3425(2) 0.61424(17) 0.16421(14) 0.0317(4) Uani 1 1 d . . . H16 H 0.3227 0.6881 0.1571 0.038 Uiso 1 1 calc R . . C17 C 0.2272(2) 0.51216(17) 0.17045(13) 0.0283(4) Uani 1 1 d . . . H17 H 0.1286 0.5170 0.1673 0.034 Uiso 1 1 calc R . . C18 C 0.25287(18) 0.40246(15) 0.18122(12) 0.0228(3) Uani 1 1 d . . . C19 C 0.6781(2) 0.49894(17) 0.18846(14) 0.0307(4) Uani 1 1 d . . . H19 H 0.6749 0.4062 0.1751 0.037 Uiso 1 1 calc R . . C20 C 0.7643(3) 0.5422(3) 0.11288(18) 0.0537(6) Uani 1 1 d . . . H20A H 0.7092 0.4906 0.0454 0.081 Uiso 1 1 calc R . . H20B H 0.8619 0.5287 0.1163 0.081 Uiso 1 1 calc R . . H20C H 0.7774 0.6355 0.1280 0.081 Uiso 1 1 calc R . . C21 C 0.7577(3) 0.5813(3) 0.29379(17) 0.0504(6) Uani 1 1 d . . . H21A H 0.8584 0.5743 0.2992 0.076 Uiso 1 1 calc R . . H21B H 0.7028 0.5498 0.3415 0.076 Uiso 1 1 calc R . . H21C H 0.7635 0.6732 0.3089 0.076 Uiso 1 1 calc R . . C22 C 0.12168(19) 0.28625(16) 0.17634(13) 0.0276(4) Uani 1 1 d . . . H22 H 0.1598 0.2333 0.2079 0.033 Uiso 1 1 calc R . . C23 C 0.0608(2) 0.1991(2) 0.06677(15) 0.0405(5) Uani 1 1 d . . . H23A H 0.0205 0.2478 0.0342 0.061 Uiso 1 1 calc R . . H23B H -0.0182 0.1207 0.0636 0.061 Uiso 1 1 calc R . . H23C H 0.1412 0.1729 0.0323 0.061 Uiso 1 1 calc R . . C24 C -0.0026(2) 0.3253(2) 0.23230(15) 0.0375(5) Uani 1 1 d . . . H24A H 0.0387 0.3839 0.3016 0.056 Uiso 1 1 calc R . . H24B H -0.0781 0.2464 0.2320 0.056 Uiso 1 1 calc R . . H24C H -0.0483 0.3706 0.1992 0.056 Uiso 1 1 calc R . . C25 C 0.42554(16) 0.27053(14) 0.27696(11) 0.0186(3) Uani 1 1 d . . . H25 H 0.4005 0.3338 0.3312 0.022 Uiso 1 1 calc R . . C26 C 0.47481(17) 0.06085(14) 0.21137(11) 0.0182(3) Uani 1 1 d . . . C27 C 0.37608(17) -0.00601(14) 0.12183(12) 0.0204(3) Uani 1 1 d . . . C28 C 0.40399(19) -0.10510(15) 0.04352(12) 0.0232(3) Uani 1 1 d . . . C29 C 0.52850(19) -0.14329(15) 0.04996(12) 0.0250(4) Uani 1 1 d . . . H29 H 0.5469 -0.2112 -0.0041 0.030 Uiso 1 1 calc R . . C30 C 0.62527(18) -0.07875(15) 0.13827(13) 0.0230(3) Uani 1 1 d . . . C31 C 0.59937(17) 0.02010(14) 0.21714(12) 0.0191(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0226(5) 0.0262(5) 0.0264(5) 0.0029(4) -0.0043(4) 0.0100(4) F2 0.0354(6) 0.0288(5) 0.0216(5) -0.0021(4) -0.0059(4) 0.0088(4) F3 0.0282(6) 0.0327(5) 0.0356(6) 0.0059(4) 0.0051(4) 0.0188(4) F4 0.0222(5) 0.0270(5) 0.0224(5) 0.0028(4) -0.0024(4) 0.0094(4) N1 0.0204(7) 0.0180(6) 0.0170(6) 0.0038(5) 0.0021(5) 0.0077(5) N2 0.0204(7) 0.0160(6) 0.0203(7) 0.0028(5) 0.0004(5) 0.0054(5) C1 0.0207(8) 0.0211(7) 0.0182(7) 0.0047(6) 0.0033(6) 0.0096(6) C2 0.0200(8) 0.0242(8) 0.0234(8) 0.0061(6) 0.0036(6) 0.0065(6) C3 0.0239(9) 0.0313(9) 0.0297(9) 0.0122(7) 0.0085(7) 0.0051(7) C4 0.0336(10) 0.0354(9) 0.0234(9) 0.0116(7) 0.0067(7) 0.0109(8) C5 0.0264(9) 0.0311(9) 0.0196(8) 0.0055(7) 0.0005(6) 0.0075(7) C6 0.0200(8) 0.0210(7) 0.0206(8) 0.0029(6) 0.0015(6) 0.0072(6) C7 0.0199(8) 0.0349(9) 0.0303(9) 0.0111(8) 0.0030(7) 0.0026(7) C8 0.0697(18) 0.0327(12) 0.094(2) 0.0088(13) -0.0460(16) -0.0028(12) C9 0.0380(13) 0.0834(18) 0.0652(17) 0.0129(14) -0.0082(11) 0.0323(13) C10 0.0205(8) 0.0222(8) 0.0198(8) 0.0039(6) 0.0015(6) 0.0064(6) C11 0.0211(8) 0.0281(9) 0.0318(9) 0.0055(7) 0.0004(7) 0.0070(7) C12 0.0254(9) 0.0238(8) 0.0324(9) 0.0042(7) 0.0007(7) 0.0070(7) C13 0.0250(8) 0.0202(7) 0.0148(7) 0.0028(6) 0.0004(6) 0.0089(6) C14 0.0249(8) 0.0230(8) 0.0211(8) 0.0047(6) 0.0015(6) 0.0067(6) C15 0.0313(9) 0.0251(8) 0.0305(9) 0.0126(7) 0.0037(7) 0.0063(7) C16 0.0395(10) 0.0293(9) 0.0329(10) 0.0162(8) 0.0028(8) 0.0149(8) C17 0.0277(9) 0.0325(9) 0.0279(9) 0.0112(7) 0.0011(7) 0.0147(7) C18 0.0235(8) 0.0248(8) 0.0186(8) 0.0055(6) 0.0008(6) 0.0087(6) C19 0.0251(9) 0.0253(8) 0.0392(10) 0.0098(8) 0.0043(7) 0.0069(7) C20 0.0330(12) 0.0833(18) 0.0452(13) 0.0241(12) 0.0123(9) 0.0173(11) C21 0.0357(12) 0.0752(16) 0.0402(12) 0.0190(11) -0.0017(9) 0.0206(11) C22 0.0218(8) 0.0278(8) 0.0325(9) 0.0099(7) 0.0003(7) 0.0086(7) C23 0.0297(10) 0.0353(10) 0.0399(11) -0.0016(8) 0.0008(8) 0.0051(8) C24 0.0293(10) 0.0400(11) 0.0376(11) 0.0093(9) 0.0070(8) 0.0082(8) C25 0.0158(7) 0.0171(7) 0.0191(8) 0.0020(6) -0.0004(6) 0.0053(6) C26 0.0202(8) 0.0163(7) 0.0171(7) 0.0055(6) 0.0034(6) 0.0049(6) C27 0.0204(8) 0.0188(7) 0.0216(8) 0.0073(6) 0.0014(6) 0.0061(6) C28 0.0283(9) 0.0186(7) 0.0181(8) 0.0042(6) 0.0001(6) 0.0041(6) C29 0.0319(9) 0.0192(8) 0.0235(8) 0.0056(6) 0.0067(7) 0.0100(7) C30 0.0256(8) 0.0213(8) 0.0265(8) 0.0099(7) 0.0078(7) 0.0123(7) C31 0.0190(8) 0.0172(7) 0.0191(7) 0.0063(6) 0.0005(6) 0.0031(6) _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 F1 C27 1.3410(17) . ? F2 C28 1.3454(18) . ? F3 C30 1.3486(18) . ? F4 C31 1.3442(17) . ? N1 C25 1.3806(19) . ? N1 C26 1.4216(19) . ? N1 C1 1.457(2) . ? N2 C25 1.263(2) . ? N2 C13 1.4287(19) . ? C1 C2 1.404(2) . ? C1 C6 1.408(2) . ? C2 C3 1.387(2) . ? C2 C7 1.523(2) . ? C3 C4 1.389(2) . ? C4 C5 1.375(3) . ? C5 C6 1.395(2) . ? C6 C10 1.522(2) . ? C7 C8 1.512(3) . ? C7 C9 1.515(3) . ? C10 C11 1.536(2) . ? C10 C12 1.538(2) . ? C13 C14 1.406(2) . ? C13 C18 1.410(2) . ? C14 C15 1.393(2) . ? C14 C19 1.519(2) . ? C15 C16 1.377(3) . ? C16 C17 1.389(3) . ? C17 C18 1.397(2) . ? C18 C22 1.523(2) . ? C19 C21 1.513(3) . ? C19 C20 1.515(3) . ? C22 C24 1.527(2) . ? C22 C23 1.529(3) . ? C26 C31 1.391(2) . ? C26 C27 1.398(2) . ? C27 C28 1.386(2) . ? C28 C29 1.375(2) . ? C29 C30 1.375(2) . ? C30 C31 1.380(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 N1 C26 120.56(13) . . ? C25 N1 C1 119.19(12) . . ? C26 N1 C1 120.24(12) . . ? C25 N2 C13 118.26(13) . . ? C2 C1 C6 121.83(15) . . ? C2 C1 N1 118.54(13) . . ? C6 C1 N1 119.58(14) . . ? C3 C2 C1 118.22(15) . . ? C3 C2 C7 119.44(15) . . ? C1 C2 C7 122.15(15) . . ? C4 C3 C2 120.85(16) . . ? C5 C4 C3 120.04(16) . . ? C4 C5 C6 121.65(16) . . ? C5 C6 C1 117.29(15) . . ? C5 C6 C10 118.78(14) . . ? C1 C6 C10 123.91(14) . . ? C8 C7 C9 110.2(2) . . ? C8 C7 C2 112.99(16) . . ? C9 C7 C2 109.69(16) . . ? C6 C10 C11 112.07(13) . . ? C6 C10 C12 110.49(13) . . ? C11 C10 C12 108.96(13) . . ? C14 C13 C18 121.26(14) . . ? C14 C13 N2 117.84(14) . . ? C18 C13 N2 120.70(14) . . ? C15 C14 C13 118.41(15) . . ? C15 C14 C19 120.54(15) . . ? C13 C14 C19 121.00(14) . . ? C16 C15 C14 121.40(17) . . ? C15 C16 C17 119.64(15) . . ? C16 C17 C18 121.55(16) . . ? C17 C18 C13 117.69(16) . . ? C17 C18 C22 119.76(15) . . ? C13 C18 C22 122.35(14) . . ? C21 C19 C20 110.48(18) . . ? C21 C19 C14 110.31(16) . . ? C20 C19 C14 113.11(16) . . ? C18 C22 C24 113.86(14) . . ? C18 C22 C23 109.48(16) . . ? C24 C22 C23 110.38(15) . . ? N2 C25 N1 123.85(13) . . ? C31 C26 C27 116.05(13) . . ? C31 C26 N1 121.81(13) . . ? C27 C26 N1 122.14(13) . . ? F1 C27 C28 118.12(13) . . ? F1 C27 C26 120.67(13) . . ? C28 C27 C26 121.20(14) . . ? F2 C28 C29 120.05(14) . . ? F2 C28 C27 117.90(14) . . ? C29 C28 C27 122.05(15) . . ? C28 C29 C30 117.00(14) . . ? F3 C30 C29 120.18(14) . . ? F3 C30 C31 118.00(14) . . ? C29 C30 C31 121.82(15) . . ? F4 C31 C30 118.08(13) . . ? F4 C31 C26 120.03(13) . . ? C30 C31 C26 121.86(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.342 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.056 #===END