# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Matthias Westerhausen' _publ_contact_author_email m.we@uni-jena.de _publ_section_title ; Organic Heterobimetallic Complexes of the Alkaline Earth Metals (Ae = Ca, Sr, Ba) with Tetrahedral Metallate Anions of Three-Valent Metals (M = B, Al, Ga, and V) ; # Attachment 'newjchem.cif.txt' #Added by publCIF (CCDC output) (Di 30. Mrz 09:52:04 2010) # start Validation Reply Form _vrf_PLAT761_FO3484 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO3484 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT761_FO3557 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO3557 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_REFLT03_FO3786 ; PROBLEM: Reflection count < 85% complete (theta max?) RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_PLAT022_FO3786 ; PROBLEM: Ratio Unique / Expected Reflections too Low .... 0.80 RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_PLAT029_FO3786 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.80 RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_REFLT03_FO3604 ; PROBLEM: Reflection count < 85% complete (theta max?) RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_PLAT029_FO3604 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.72 RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_PLAT761_FO3520 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO3520 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT761_FO2960 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO2960 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT773_FO2903 ; PROBLEM: Suspect C-C Bond in CIF: C10 -- C11 .. 1.76 Ang. RESPONSE: This distance is part of a disordered thf-molecule. The distance was not fixed by a DFIX command. The distance was free refined. ; _vrf_PLAT761_FO2903 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO2903 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT761_FO2880 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO2880 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT029_FO2934 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94 RESPONSE: The scattering power of the crystal was not strong enough for high order reflexions. ; _vrf_PLAT761_FO2934 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All hydrogen positions were calculated. ; _vrf_PLAT762_FO2934 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All hydrogen positions were calculated. ; loop_ _publ_author_name 'Matthias Westerhausen' 'Jens Langer' 'Sven Krieck' 'Helmar Gorls' 'Gunter Kreisel' 'Wolfgang Seidel' # Attachment '- newjchem.cif' data_FO3484 _database_code_depnum_ccdc_archive 'CCDC 765641' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Ca O6, 2(C24 H20 B), 2(C4 H8 O)' _chemical_formula_sum 'C80 H104 B2 Ca O8' _chemical_formula_weight 1255.33 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' B B 0.0013 0.0007 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 15.5626(4) _cell_length_b 14.6072(5) _cell_length_c 16.9537(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.462(2) _cell_angle_gamma 90.00 _cell_volume 3610.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 25235 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25235 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8234 _reflns_number_gt 6072 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1041P)^2^+11.1504P] 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 8234 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.1095 _refine_ls_wR_factor_ref 0.2985 _refine_ls_wR_factor_gt 0.2809 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.5000 0.0000 0.5000 0.0257(3) Uani 1 2 d S . . O1 O 0.3637(2) 0.0278(2) 0.5253(2) 0.0441(8) Uani 1 1 d . . . O2 O 0.4199(2) -0.0404(3) 0.36091(19) 0.0499(9) Uani 1 1 d . . . O3 O 0.4908(2) 0.1536(2) 0.4586(2) 0.0484(8) Uani 1 1 d . . . C1 C 0.3181(8) 0.1155(8) 0.5221(8) 0.049(3) Uiso 0.423(12) 1 d P A 1 H1A H 0.2765 0.1297 0.4642 0.059 Uiso 0.423(12) 1 calc PR A 1 H1B H 0.3632 0.1657 0.5424 0.059 Uiso 0.423(12) 1 calc PR A 1 C1A C 0.3638(5) 0.0784(6) 0.6055(5) 0.042(2) Uiso 0.577(12) 1 d P A 2 H1AA H 0.3860 0.0384 0.6557 0.050 Uiso 0.577(12) 1 calc PR A 2 H1AB H 0.4016 0.1346 0.6157 0.050 Uiso 0.577(12) 1 calc PR A 2 C2 C 0.2632(4) 0.1005(4) 0.5824(4) 0.0597(14) Uani 1 1 d . . . H2A H 0.3033 0.0930 0.6419 0.072 Uiso 0.423(12) 1 calc PR A 1 H2B H 0.2171 0.1490 0.5773 0.072 Uiso 0.423(12) 1 calc PR A 1 H2C H 0.2446 0.1517 0.5416 0.072 Uiso 0.577(12) 1 d PR A 2 H2D H 0.2474 0.1154 0.6326 0.072 Uiso 0.577(12) 1 d PR A 2 C3 C 0.2205(4) 0.0111(5) 0.5416(5) 0.0707(17) Uani 1 1 d . A . H3A H 0.1745 0.0221 0.4850 0.085 Uiso 0.487(16) 1 calc PR B 1 H3B H 0.1904 -0.0207 0.5765 0.085 Uiso 0.487(16) 1 calc PR B 1 H3C H 0.1536 0.0162 0.5113 0.085 Uiso 0.513(16) 1 d PR B 2 H3D H 0.2333 -0.0390 0.5835 0.085 Uiso 0.513(16) 1 d PR B 2 C4 C 0.3015(9) -0.0456(10) 0.5357(9) 0.069(4) Uiso 0.487(16) 1 d P A 1 H4A H 0.3311 -0.0817 0.5876 0.082 Uiso 0.487(16) 1 calc PR B 1 H4B H 0.2817 -0.0874 0.4866 0.082 Uiso 0.487(16) 1 calc PR B 1 C4A C 0.2755(6) -0.0011(7) 0.4818(6) 0.044(3) Uiso 0.513(16) 1 d P A 2 H4AA H 0.2754 -0.0662 0.4654 0.053 Uiso 0.513(16) 1 calc PR B 2 H4AB H 0.2480 0.0360 0.4302 0.053 Uiso 0.513(16) 1 calc PR B 2 C5 C 0.3717(8) -0.1163(8) 0.3212(7) 0.054(3) Uiso 0.508(15) 1 d P A 1 H5A H 0.3285 -0.1361 0.3491 0.065 Uiso 0.508(15) 1 calc PR A 1 H5B H 0.4141 -0.1674 0.3232 0.065 Uiso 0.508(15) 1 calc PR A 1 C5A C 0.3247(7) -0.0662(7) 0.3226(6) 0.047(3) Uiso 0.492(15) 1 d P A 2 H5AA H 0.2832 -0.0152 0.3237 0.056 Uiso 0.492(15) 1 calc PR A 2 H5AB H 0.3099 -0.1205 0.3505 0.056 Uiso 0.492(15) 1 calc PR A 2 C6 C 0.3190(5) -0.0889(5) 0.2299(3) 0.079(2) Uani 1 1 d . . . H6A H 0.3007 -0.1425 0.1919 0.094 Uiso 0.508(15) 1 calc PR A 1 H6B H 0.2647 -0.0506 0.2243 0.094 Uiso 0.508(15) 1 calc PR A 1 H6C H 0.3270 -0.1553 0.2232 0.094 Uiso 0.492(15) 1 d PR A 2 H6D H 0.2590 -0.0697 0.1888 0.094 Uiso 0.492(15) 1 d PR A 2 C7 C 0.3947(4) -0.0353(5) 0.2168(3) 0.0599(15) Uani 1 1 d . A . H7A H 0.3736 -0.0024 0.1623 0.072 Uiso 0.50 1 calc PR C 1 H7B H 0.4477 -0.0746 0.2202 0.072 Uiso 0.50 1 calc PR C 1 H7C H 0.3852 0.0318 0.2158 0.072 Uiso 0.50 1 d PR C 2 H7D H 0.4082 -0.0551 0.1665 0.072 Uiso 0.50 1 d PR C 2 C8 C 0.4173(6) 0.0314(6) 0.2921(6) 0.0406(19) Uiso 0.50 1 d P A 1 H8A H 0.3687 0.0778 0.2843 0.049 Uiso 0.50 1 calc PR A 1 H8B H 0.4773 0.0621 0.3038 0.049 Uiso 0.50 1 calc PR A 1 C8A C 0.4665(8) -0.0691(8) 0.3018(7) 0.058(3) Uiso 0.50 1 d P A 2 H8AA H 0.4751 -0.1363 0.3022 0.069 Uiso 0.50 1 calc PR A 2 H8AB H 0.5265 -0.0383 0.3144 0.069 Uiso 0.50 1 calc PR A 2 C9 C 0.4045(7) 0.2095(7) 0.4382(7) 0.049(2) Uiso 0.50 1 d P A 1 H9A H 0.3534 0.1815 0.3918 0.059 Uiso 0.50 1 calc PR A 1 H9B H 0.3859 0.2165 0.4881 0.059 Uiso 0.50 1 calc PR A 1 C10 C 0.4325(8) 0.2997(8) 0.4120(8) 0.048(2) Uiso 0.50 1 d P A 1 H10A H 0.4484 0.3440 0.4591 0.058 Uiso 0.50 1 calc PR A 1 H10B H 0.3820 0.3256 0.3637 0.058 Uiso 0.50 1 calc PR A 1 C11 C 0.5159(7) 0.2797(7) 0.3872(7) 0.052(2) Uiso 0.50 1 d P A 1 H11A H 0.4978 0.2553 0.3292 0.062 Uiso 0.50 1 calc PR A 1 H11B H 0.5544 0.3349 0.3922 0.062 Uiso 0.50 1 calc PR A 1 C12 C 0.5638(7) 0.2089(7) 0.4512(7) 0.051(2) Uiso 0.50 1 d P A 1 H12A H 0.6059 0.1719 0.4319 0.061 Uiso 0.50 1 calc PR A 1 H12B H 0.5992 0.2377 0.5058 0.061 Uiso 0.50 1 calc PR A 1 C9A C 0.4237(7) 0.1770(7) 0.3685(7) 0.051(2) Uiso 0.50 1 d P A 2 H9AA H 0.4539 0.1711 0.3261 0.062 Uiso 0.50 1 calc PR A 2 H9AB H 0.3685 0.1375 0.3521 0.062 Uiso 0.50 1 calc PR A 2 C10A C 0.4004(8) 0.2754(8) 0.3794(8) 0.052(2) Uiso 0.50 1 d P A 2 H10C H 0.3799 0.3083 0.3249 0.062 Uiso 0.50 1 calc PR A 2 H10D H 0.3518 0.2793 0.4045 0.062 Uiso 0.50 1 calc PR A 2 C11A C 0.4881(8) 0.3126(8) 0.4372(7) 0.055(3) Uiso 0.50 1 d P A 2 H11C H 0.4771 0.3623 0.4722 0.066 Uiso 0.50 1 calc PR A 2 H11D H 0.5256 0.3370 0.4053 0.066 Uiso 0.50 1 calc PR A 2 C12A C 0.5364(7) 0.2309(7) 0.4922(7) 0.049(2) Uiso 0.50 1 d P A 2 H12C H 0.6007 0.2269 0.4944 0.059 Uiso 0.50 1 calc PR A 2 H12D H 0.5369 0.2391 0.5503 0.059 Uiso 0.50 1 calc PR A 2 B1 B 0.5054(3) 0.5816(3) 0.2576(3) 0.0300(9) Uani 1 1 d . . . C13 C 0.6044(3) 0.5622(3) 0.3331(2) 0.0319(8) Uani 1 1 d . . . C14 C 0.6378(3) 0.6211(3) 0.4032(3) 0.0367(9) Uani 1 1 d . . . H14A H 0.6021 0.6730 0.4060 0.044 Uiso 1 1 calc R . . C15 C 0.7210(3) 0.6067(4) 0.4686(3) 0.0437(11) Uani 1 1 d . . . H15A H 0.7406 0.6484 0.5145 0.052 Uiso 1 1 calc R . . C16 C 0.7743(3) 0.5334(4) 0.4670(3) 0.0462(11) Uani 1 1 d . . . H16A H 0.8318 0.5246 0.5107 0.055 Uiso 1 1 calc R . . C17 C 0.7435(3) 0.4715(4) 0.4007(3) 0.0478(11) Uani 1 1 d . . . H17A H 0.7789 0.4187 0.4001 0.057 Uiso 1 1 calc R . . C18 C 0.6605(3) 0.4870(3) 0.3350(3) 0.0394(10) Uani 1 1 d . . . H18A H 0.6415 0.4445 0.2897 0.047 Uiso 1 1 calc R . . C19 C 0.5123(3) 0.6734(3) 0.2026(2) 0.0299(8) Uani 1 1 d . . . C20 C 0.4449(3) 0.6889(3) 0.1231(3) 0.0389(9) Uani 1 1 d . . . H20A H 0.3964 0.6459 0.1022 0.047 Uiso 1 1 calc R . . C21 C 0.4465(3) 0.7648(3) 0.0739(3) 0.0461(11) Uani 1 1 d . . . H21A H 0.3988 0.7731 0.0211 0.055 Uiso 1 1 calc R . . C22 C 0.5165(4) 0.8278(3) 0.1009(3) 0.0498(12) Uani 1 1 d . . . H22A H 0.5184 0.8790 0.0670 0.060 Uiso 1 1 calc R . . C23 C 0.5841(4) 0.8148(3) 0.1788(3) 0.0474(11) Uani 1 1 d . . . H23A H 0.6327 0.8577 0.1990 0.057 Uiso 1 1 calc R . . C24 C 0.5811(3) 0.7387(3) 0.2281(3) 0.0392(9) Uani 1 1 d . . . H24A H 0.6283 0.7315 0.2813 0.047 Uiso 1 1 calc R . . C25 C 0.4277(3) 0.5983(3) 0.3021(2) 0.0316(8) Uani 1 1 d . . . C26 C 0.4312(3) 0.5514(3) 0.3751(3) 0.0397(10) Uani 1 1 d . . . H26A H 0.4803 0.5099 0.3996 0.048 Uiso 1 1 calc R . . C27 C 0.3658(3) 0.5625(3) 0.4141(3) 0.0459(11) Uani 1 1 d . . . H27A H 0.3709 0.5283 0.4632 0.055 Uiso 1 1 calc R . . C28 C 0.2943(3) 0.6231(3) 0.3811(3) 0.0414(10) Uani 1 1 d . . . H28A H 0.2505 0.6323 0.4077 0.050 Uiso 1 1 calc R . . C29 C 0.2877(3) 0.6703(3) 0.3082(3) 0.0441(11) Uani 1 1 d . . . H29A H 0.2384 0.7118 0.2843 0.053 Uiso 1 1 calc R . . C30 C 0.3524(3) 0.6575(3) 0.2697(3) 0.0398(10) Uani 1 1 d . . . H30A H 0.3453 0.6902 0.2194 0.048 Uiso 1 1 calc R . . C31 C 0.4772(3) 0.4934(3) 0.1937(2) 0.0308(8) Uani 1 1 d . . . C32 C 0.5176(3) 0.4788(3) 0.1329(3) 0.0375(9) Uani 1 1 d . . . H32A H 0.5608 0.5224 0.1283 0.045 Uiso 1 1 calc R . . C33 C 0.4978(3) 0.4037(3) 0.0786(3) 0.0422(10) Uani 1 1 d . . . H33A H 0.5282 0.3962 0.0393 0.051 Uiso 1 1 calc R . . C34 C 0.4333(3) 0.3400(3) 0.0827(3) 0.0454(11) Uani 1 1 d . . . H34A H 0.4176 0.2895 0.0450 0.054 Uiso 1 1 calc R . . C35 C 0.3926(3) 0.3510(3) 0.1418(3) 0.0444(11) Uani 1 1 d . . . H35A H 0.3496 0.3068 0.1460 0.053 Uiso 1 1 calc R . . C36 C 0.4134(3) 0.4266(3) 0.1961(3) 0.0376(9) Uani 1 1 d . . . H36A H 0.3833 0.4327 0.2358 0.045 Uiso 1 1 calc R . . O1T O 0.8335(5) 0.7481(6) 0.2651(5) 0.143(3) Uiso 1 1 d . . . C1T C 0.8457(9) 0.6787(8) 0.3206(8) 0.050(3) Uiso 0.50 1 d P D 1 H1TA H 0.7863 0.6485 0.3128 0.060 Uiso 0.50 1 calc PR D 1 H1TB H 0.8712 0.7022 0.3789 0.060 Uiso 0.50 1 calc PR D 1 C2T C 0.9160(11) 0.6063(11) 0.3039(9) 0.075(4) Uiso 0.50 1 d P D 1 H2TA H 0.9111 0.5436 0.3241 0.090 Uiso 0.50 1 calc PR D 1 H2TB H 0.9805 0.6273 0.3237 0.090 Uiso 0.50 1 calc PR D 1 C3T C 0.8595(6) 0.6215(6) 0.1996(5) 0.0316(16) Uiso 0.50 1 d P D 1 H3TA H 0.9039 0.6295 0.1702 0.038 Uiso 0.50 1 calc PR D 1 H3TB H 0.8211 0.5673 0.1756 0.038 Uiso 0.50 1 calc PR D 1 C4T C 0.8046(8) 0.6990(8) 0.1887(7) 0.061(3) Uiso 0.50 1 d P D 1 H4TA H 0.7394 0.6810 0.1734 0.073 Uiso 0.50 1 calc PR D 1 H4TB H 0.8107 0.7376 0.1429 0.073 Uiso 0.50 1 calc PR D 1 C1TA C 0.8817(13) 0.6669(11) 0.3439(10) 0.082(4) Uiso 0.50 1 d P D 2 H1TC H 0.9460 0.6806 0.3792 0.098 Uiso 0.50 1 calc PR D 2 H1TD H 0.8442 0.6547 0.3793 0.098 Uiso 0.50 1 calc PR D 2 C2TA C 0.8725(14) 0.5904(13) 0.2748(12) 0.098(5) Uiso 0.50 1 d P D 2 H2TC H 0.9058 0.5337 0.2998 0.118 Uiso 0.50 1 calc PR D 2 H2TD H 0.8075 0.5756 0.2426 0.118 Uiso 0.50 1 calc PR D 2 C3TA C 0.9131(9) 0.6348(8) 0.2266(8) 0.060(3) Uiso 0.50 1 d P D 2 H3TC H 0.8943 0.6045 0.1709 0.073 Uiso 0.50 1 calc PR D 2 H3TD H 0.9804 0.6276 0.2532 0.073 Uiso 0.50 1 calc PR D 2 C4TA C 0.8932(11) 0.7270(11) 0.2144(11) 0.090(4) Uiso 0.50 1 d P D 2 H4TC H 0.8604 0.7402 0.1541 0.108 Uiso 0.50 1 calc PR D 2 H4TD H 0.9501 0.7639 0.2343 0.108 Uiso 0.50 1 calc PR D 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 0.0252(5) 0.0250(5) 0.0261(5) -0.0020(4) 0.0080(4) 0.0009(4) O1 0.0372(16) 0.0420(17) 0.060(2) -0.0045(15) 0.0254(15) 0.0002(13) O2 0.0397(17) 0.077(2) 0.0300(16) -0.0141(16) 0.0090(13) -0.0142(16) O3 0.0522(19) 0.0322(16) 0.055(2) 0.0075(14) 0.0111(16) -0.0005(14) C2 0.046(3) 0.073(4) 0.065(3) -0.009(3) 0.025(3) 0.014(3) C3 0.043(3) 0.081(4) 0.096(5) -0.003(4) 0.034(3) 0.000(3) C6 0.106(5) 0.068(4) 0.035(3) -0.005(3) -0.010(3) -0.033(4) C7 0.060(3) 0.087(4) 0.028(2) -0.010(2) 0.009(2) 0.021(3) B1 0.032(2) 0.029(2) 0.029(2) -0.0037(17) 0.0108(17) -0.0021(17) C13 0.0324(19) 0.034(2) 0.032(2) 0.0007(16) 0.0146(16) -0.0031(16) C14 0.036(2) 0.042(2) 0.034(2) -0.0005(18) 0.0134(17) -0.0055(18) C15 0.040(2) 0.061(3) 0.031(2) -0.002(2) 0.0134(18) -0.011(2) C16 0.032(2) 0.069(3) 0.035(2) 0.010(2) 0.0075(18) 0.000(2) C17 0.035(2) 0.057(3) 0.049(3) 0.012(2) 0.012(2) 0.013(2) C18 0.037(2) 0.040(2) 0.039(2) 0.0014(18) 0.0112(18) 0.0034(18) C19 0.0321(19) 0.0282(19) 0.0315(19) 0.0010(15) 0.0136(16) 0.0043(15) C20 0.042(2) 0.037(2) 0.034(2) 0.0022(18) 0.0093(18) 0.0034(18) C21 0.052(3) 0.048(3) 0.037(2) 0.003(2) 0.015(2) 0.011(2) C22 0.068(3) 0.038(2) 0.052(3) 0.009(2) 0.032(3) 0.007(2) C23 0.054(3) 0.038(2) 0.054(3) 0.004(2) 0.023(2) -0.006(2) C24 0.040(2) 0.037(2) 0.040(2) 0.0029(18) 0.0128(18) 0.0003(18) C25 0.0311(19) 0.031(2) 0.032(2) -0.0071(16) 0.0107(16) -0.0051(16) C26 0.038(2) 0.035(2) 0.050(3) 0.0057(19) 0.0218(19) 0.0007(18) C27 0.051(3) 0.039(2) 0.057(3) 0.001(2) 0.030(2) -0.006(2) C28 0.032(2) 0.043(2) 0.055(3) -0.016(2) 0.023(2) -0.0108(18) C29 0.033(2) 0.048(3) 0.051(3) -0.011(2) 0.0145(19) 0.0067(19) C30 0.038(2) 0.045(2) 0.035(2) -0.0013(18) 0.0118(18) 0.0064(19) C31 0.0272(18) 0.031(2) 0.0313(19) 0.0014(16) 0.0073(15) 0.0050(15) C32 0.038(2) 0.036(2) 0.040(2) -0.0009(17) 0.0162(18) -0.0017(17) C33 0.045(2) 0.044(2) 0.040(2) -0.0088(19) 0.0190(19) 0.004(2) C34 0.049(3) 0.040(2) 0.044(3) -0.012(2) 0.013(2) 0.000(2) C35 0.046(3) 0.035(2) 0.053(3) -0.006(2) 0.018(2) -0.0085(19) C36 0.038(2) 0.036(2) 0.042(2) -0.0039(18) 0.0167(18) -0.0022(18) _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 2.325(3) 3_656 ? Ca1 O2 2.325(3) . ? Ca1 O3 2.341(3) . ? Ca1 O3 2.341(3) 3_656 ? Ca1 O1 2.342(3) . ? Ca1 O1 2.342(3) 3_656 ? O1 C4A 1.378(9) . ? O1 C1 1.457(12) . ? O1 C4 1.497(14) . ? O1 C1A 1.547(9) . ? O2 C5 1.376(11) . ? O2 C5A 1.446(10) . ? O2 C8A 1.488(12) . ? O2 C8 1.558(10) . ? O3 C12A 1.349(11) . ? O3 C12 1.434(11) . ? O3 C9 1.505(10) . ? O3 C9A 1.557(11) . ? C1 C2 1.559(13) . ? C1A C2 1.510(9) . ? C2 C3 1.517(9) . ? C3 C4 1.540(14) . ? C3 C4A 1.549(11) . ? C5 C6 1.531(12) . ? C5A C6 1.578(12) . ? C6 C7 1.494(9) . ? C7 C8 1.545(10) . ? C7 C8A 1.564(12) . ? C9 C10 1.503(15) . ? C10 C11 1.526(15) . ? C11 C12 1.496(14) . ? C9A C10A 1.509(15) . ? C10A C11A 1.479(15) . ? C11A C12A 1.540(15) . ? B1 C31 1.641(6) . ? B1 C13 1.647(6) . ? B1 C25 1.652(6) . ? B1 C19 1.659(6) . ? C13 C18 1.397(6) . ? C13 C14 1.412(6) . ? C14 C15 1.394(6) . ? C15 C16 1.360(7) . ? C16 C17 1.391(7) . ? C17 C18 1.398(6) . ? C19 C24 1.385(6) . ? C19 C20 1.406(6) . ? C20 C21 1.392(6) . ? C21 C22 1.377(7) . ? C22 C23 1.384(7) . ? C23 C24 1.401(6) . ? C25 C26 1.400(6) . ? C25 C30 1.405(6) . ? C26 C27 1.402(6) . ? C27 C28 1.378(7) . ? C28 C29 1.387(7) . ? C29 C30 1.390(6) . ? C31 C32 1.398(6) . ? C31 C36 1.403(6) . ? C32 C33 1.396(6) . ? C33 C34 1.388(7) . ? C34 C35 1.369(7) . ? C35 C36 1.400(6) . ? O1T C1T 1.350(13) . ? O1T C4T 1.411(13) . ? O1T C4TA 1.503(17) . ? O1T C1TA 1.747(18) . ? C1T C2T 1.614(19) . ? C2T C3T 1.693(17) . ? C3T C4T 1.391(14) . ? C1TA C2TA 1.59(2) . ? C2TA C3TA 1.36(2) . ? C3TA C4TA 1.38(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 O2 Ca1 O2 180.0 3_656 . ? O2 Ca1 O3 90.91(13) 3_656 . ? O2 Ca1 O3 89.09(13) . . ? O2 Ca1 O3 89.09(13) 3_656 3_656 ? O2 Ca1 O3 90.91(13) . 3_656 ? O3 Ca1 O3 180.00(4) . 3_656 ? O2 Ca1 O1 88.22(12) 3_656 . ? O2 Ca1 O1 91.78(12) . . ? O3 Ca1 O1 85.67(12) . . ? O3 Ca1 O1 94.33(12) 3_656 . ? O2 Ca1 O1 91.78(12) 3_656 3_656 ? O2 Ca1 O1 88.22(12) . 3_656 ? O3 Ca1 O1 94.34(12) . 3_656 ? O3 Ca1 O1 85.66(12) 3_656 3_656 ? O1 Ca1 O1 180.0 . 3_656 ? C4A O1 C1 82.4(6) . . ? C4A O1 C4 43.8(6) . . ? C1 O1 C4 107.9(7) . . ? C4A O1 C1A 108.1(5) . . ? C1 O1 C1A 57.5(6) . . ? C4 O1 C1A 92.3(6) . . ? C4A O1 Ca1 130.2(4) . . ? C1 O1 Ca1 127.4(5) . . ? C4 O1 Ca1 124.2(5) . . ? C1A O1 Ca1 121.4(3) . . ? C5 O2 C5A 43.2(6) . . ? C5 O2 C8A 75.8(7) . . ? C5A O2 C8A 106.7(6) . . ? C5 O2 C8 108.0(6) . . ? C5A O2 C8 94.9(6) . . ? C8A O2 C8 64.9(6) . . ? C5 O2 Ca1 135.1(5) . . ? C5A O2 Ca1 128.6(4) . . ? C8A O2 Ca1 122.7(5) . . ? C8 O2 Ca1 117.0(4) . . ? C12A O3 C12 41.4(6) . . ? C12A O3 C9 86.5(6) . . ? C12 O3 C9 110.2(6) . . ? C12A O3 C9A 107.8(6) . . ? C12 O3 C9A 94.1(6) . . ? C9 O3 C9A 54.3(6) . . ? C12A O3 Ca1 135.0(5) . . ? C12 O3 Ca1 126.8(5) . . ? C9 O3 Ca1 123.0(4) . . ? C9A O3 Ca1 117.0(4) . . ? O1 C1 C2 102.9(8) . . ? C2 C1A O1 101.1(5) . . ? C1A C2 C3 100.5(5) . . ? C1A C2 C1 56.2(6) . . ? C3 C2 C1 94.3(6) . . ? C2 C3 C4 104.8(6) . . ? C2 C3 C4A 98.2(5) . . ? C4 C3 C4A 40.9(6) . . ? O1 C4 C3 101.5(9) . . ? O1 C4A C3 106.8(6) . . ? O2 C5 C6 107.0(8) . . ? O2 C5A C6 101.2(7) . . ? C7 C6 C5 96.7(6) . . ? C7 C6 C5A 105.4(5) . . ? C5 C6 C5A 39.1(5) . . ? C6 C7 C8 99.9(5) . . ? C6 C7 C8A 92.5(6) . . ? C8 C7 C8A 63.5(6) . . ? C7 C8 O2 97.7(6) . . ? O2 C8A C7 99.9(7) . . ? C10 C9 O3 102.4(7) . . ? C9 C10 C11 106.1(8) . . ? C12 C11 C10 100.8(8) . . ? O3 C12 C11 104.1(8) . . ? C10A C9A O3 101.3(8) . . ? C11A C10A C9A 103.0(9) . . ? C10A C11A C12A 105.0(9) . . ? O3 C12A C11A 108.6(8) . . ? C31 B1 C13 109.9(3) . . ? C31 B1 C25 110.3(3) . . ? C13 B1 C25 107.7(3) . . ? C31 B1 C19 108.6(3) . . ? C13 B1 C19 110.5(3) . . ? C25 B1 C19 109.8(3) . . ? C18 C13 C14 114.6(4) . . ? C18 C13 B1 124.1(4) . . ? C14 C13 B1 121.3(4) . . ? C15 C14 C13 123.0(4) . . ? C16 C15 C14 120.4(4) . . ? C15 C16 C17 119.2(4) . . ? C16 C17 C18 120.0(4) . . ? C13 C18 C17 122.8(4) . . ? C24 C19 C20 115.1(4) . . ? C24 C19 B1 125.1(4) . . ? C20 C19 B1 119.7(4) . . ? C21 C20 C19 122.5(4) . . ? C22 C21 C20 120.7(4) . . ? C21 C22 C23 118.3(4) . . ? C22 C23 C24 120.4(5) . . ? C19 C24 C23 122.9(4) . . ? C26 C25 C30 114.5(4) . . ? C26 C25 B1 121.6(4) . . ? C30 C25 B1 123.9(4) . . ? C25 C26 C27 123.5(4) . . ? C28 C27 C26 119.8(4) . . ? C27 C28 C29 118.7(4) . . ? C28 C29 C30 120.7(4) . . ? C29 C30 C25 122.8(4) . . ? C32 C31 C36 114.8(4) . . ? C32 C31 B1 121.3(4) . . ? C36 C31 B1 123.8(4) . . ? C33 C32 C31 123.6(4) . . ? C34 C33 C32 119.4(4) . . ? C35 C34 C33 119.0(4) . . ? C34 C35 C36 120.9(4) . . ? C35 C36 C31 122.2(4) . . ? C1T O1T C4T 100.4(9) . . ? C1T O1T C4TA 106.2(10) . . ? C4T O1T C4TA 55.4(8) . . ? C1T O1T C1TA 16.2(8) . . ? C4T O1T C1TA 105.8(9) . . ? C4TA O1T C1TA 96.4(10) . . ? O1T C1T C2T 108.0(10) . . ? C1T C2T C3T 87.8(9) . . ? C4T C3T C2T 108.4(9) . . ? C3T C4T O1T 107.9(9) . . ? C2TA C1TA O1T 90.6(11) . . ? C3TA C2TA C1TA 99.6(14) . . ? C2TA C3TA C4TA 115.3(14) . . ? C3TA C4TA O1T 105.4(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.828 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.079 #==== END data_FO3557 _database_code_depnum_ccdc_archive 'CCDC 765642' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Ca I O5, C24 H20 B ' _chemical_formula_sum 'C44 H60 B Ca I O5' _chemical_formula_weight 846.71 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' B B 0.0013 0.0007 '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' I I -0.4742 1.8119 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6919(3) _cell_length_b 15.3774(4) _cell_length_c 21.9023(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.797(1) _cell_angle_gamma 90.00 _cell_volume 4265.25(18) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 29850 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29850 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9736 _reflns_number_gt 5951 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0462P)^2^+3.0034P] 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 9736 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 I1 I 0.30953(2) 0.039772(16) 0.090337(13) 0.05076(11) Uani 1 1 d . . . Ca1 Ca 0.29021(5) -0.15897(4) 0.09054(3) 0.02977(16) Uani 1 1 d . . . O1 O 0.2901(2) -0.17251(16) -0.01600(11) 0.0425(6) Uani 1 1 d . . . O2 O 0.10634(18) -0.14126(16) 0.08400(11) 0.0394(6) Uani 1 1 d . . . O3 O 0.47121(18) -0.18864(18) 0.09360(12) 0.0452(7) Uani 1 1 d . . . O4 O 0.2958(2) -0.17489(17) 0.19896(11) 0.0412(6) Uani 1 1 d . . . O5 O 0.2536(2) -0.30967(16) 0.09166(11) 0.0419(6) Uani 1 1 d . . . C1 C 0.2655(4) -0.1105(3) -0.0644(2) 0.0697(15) Uani 1 1 d . . . H1A H 0.1934 -0.1207 -0.0831 0.084 Uiso 1 1 calc R . . H1B H 0.2692 -0.0505 -0.0480 0.084 Uiso 1 1 calc R . . C2 C 0.3423(5) -0.1225(3) -0.1091(2) 0.0730(15) Uani 1 1 d . . . H2A H 0.4026 -0.0823 -0.1011 0.088 Uiso 1 1 calc R . . H2B H 0.3102 -0.1113 -0.1508 0.088 Uiso 1 1 calc R . . C3 C 0.3785(4) -0.2153(3) -0.10322(18) 0.0517(11) Uani 1 1 d . . . H3A H 0.4565 -0.2187 -0.0992 0.062 Uiso 1 1 calc R . . H3B H 0.3523 -0.2498 -0.1393 0.062 Uiso 1 1 calc R . . C4 C 0.3312(3) -0.2478(2) -0.04556(17) 0.0414(9) Uani 1 1 d . . . H4A H 0.2740 -0.2901 -0.0560 0.050 Uiso 1 1 calc R . . H4B H 0.3859 -0.2766 -0.0183 0.050 Uiso 1 1 calc R . . C5 C 0.0353(3) -0.1391(3) 0.03057(19) 0.0561(12) Uani 1 1 d . . . H5A H 0.0329 -0.1964 0.0099 0.067 Uiso 1 1 calc R . . H5B H 0.0576 -0.0946 0.0014 0.067 Uiso 1 1 calc R . . C6 C -0.0705(3) -0.1167(4) 0.0529(2) 0.0709(14) Uani 1 1 d . . . H6A H -0.1143 -0.0851 0.0211 0.085 Uiso 1 1 calc R . . H6B H -0.1086 -0.1699 0.0644 0.085 Uiso 1 1 calc R . . C7 C -0.0465(4) -0.0620(3) 0.1058(2) 0.0652(13) Uani 1 1 d . . . H7A H -0.1022 -0.0668 0.1352 0.078 Uiso 1 1 calc R . . H7B H -0.0401 -0.0004 0.0935 0.078 Uiso 1 1 calc R . . C8 C 0.0571(3) -0.0957(3) 0.13349(19) 0.0510(11) Uani 1 1 d . . . H8A H 0.1024 -0.0471 0.1492 0.061 Uiso 1 1 calc R . . H8B H 0.0456 -0.1360 0.1677 0.061 Uiso 1 1 calc R . . C9 C 0.5346(3) -0.2157(3) 0.1469(2) 0.0575(12) Uani 1 1 d . . . H9A H 0.5678 -0.2729 0.1402 0.069 Uiso 1 1 calc R . . H9B H 0.4919 -0.2195 0.1830 0.069 Uiso 1 1 calc R . . C10 C 0.6173(3) -0.1448(3) 0.1551(2) 0.0632(13) Uani 1 1 d . . . H10A H 0.5879 -0.0910 0.1721 0.076 Uiso 1 1 calc R . . H10B H 0.6791 -0.1641 0.1817 0.076 Uiso 1 1 calc R . . C11 C 0.6451(3) -0.1325(3) 0.0897(2) 0.0551(11) Uani 1 1 d . . . H11A H 0.6754 -0.0741 0.0836 0.066 Uiso 1 1 calc R . . H11B H 0.6962 -0.1771 0.0779 0.066 Uiso 1 1 calc R . . C12 C 0.5406(3) -0.1426(3) 0.0535(2) 0.0494(10) Uani 1 1 d . . . H12A H 0.5108 -0.0850 0.0420 0.059 Uiso 1 1 calc R . . H12B H 0.5494 -0.1766 0.0158 0.059 Uiso 1 1 calc R . . C13 C 0.2736(4) -0.2557(3) 0.23047(18) 0.0574(12) Uani 1 1 d . . . H13A H 0.3145 -0.3043 0.2141 0.069 Uiso 1 1 calc R . . H13B H 0.1975 -0.2700 0.2250 0.069 Uiso 1 1 calc R . . C14 C 0.3055(4) -0.2413(3) 0.29663(19) 0.0613(12) Uani 1 1 d . . . H14A H 0.2554 -0.2698 0.3230 0.074 Uiso 1 1 calc R . . H14B H 0.3773 -0.2642 0.3071 0.074 Uiso 1 1 calc R . . C15 C 0.3028(4) -0.1451(3) 0.3041(2) 0.0674(14) Uani 1 1 d . . . H15A H 0.3538 -0.1261 0.3376 0.081 Uiso 1 1 calc R . . H15B H 0.2313 -0.1253 0.3131 0.081 Uiso 1 1 calc R . . C16 C 0.3327(4) -0.1105(3) 0.24404(19) 0.0610(12) Uani 1 1 d . . . H16A H 0.2985 -0.0536 0.2353 0.073 Uiso 1 1 calc R . . H16B H 0.4102 -0.1031 0.2440 0.073 Uiso 1 1 calc R . . C17 C 0.1473(3) -0.3448(3) 0.0948(2) 0.0531(11) Uani 1 1 d . . . H17A H 0.1059 -0.3374 0.0552 0.064 Uiso 1 1 calc R . . H17B H 0.1098 -0.3155 0.1273 0.064 Uiso 1 1 calc R . . C18 C 0.1636(4) -0.4394(3) 0.1093(4) 0.089(2) Uani 1 1 d . . . H18A H 0.1611 -0.4496 0.1539 0.107 Uiso 1 1 calc R . . H18B H 0.1082 -0.4750 0.0875 0.107 Uiso 1 1 calc R . . C19 C 0.2633(5) -0.4609(3) 0.0899(4) 0.099(2) Uani 1 1 d . . . H19A H 0.2563 -0.4846 0.0478 0.118 Uiso 1 1 calc R . . H19B H 0.2969 -0.5057 0.1172 0.118 Uiso 1 1 calc R . . C20 C 0.3290(4) -0.3814(3) 0.0915(2) 0.0625(13) Uani 1 1 d . . . H20A H 0.3776 -0.3801 0.1288 0.075 Uiso 1 1 calc R . . H20B H 0.3711 -0.3783 0.0551 0.075 Uiso 1 1 calc R . . B1 B 0.2293(3) 0.4544(3) -0.13885(18) 0.0320(8) Uani 1 1 d . . . C21 C 0.1454(3) 0.3938(2) -0.18028(15) 0.0307(8) Uani 1 1 d . . . C22 C 0.0602(3) 0.4269(3) -0.21684(16) 0.0384(8) Uani 1 1 d . . . H22A H 0.0469 0.4877 -0.2158 0.046 Uiso 1 1 calc R . . C23 C -0.0061(3) 0.3748(3) -0.25487(18) 0.0459(10) Uani 1 1 d . . . H23A H -0.0640 0.4001 -0.2782 0.055 Uiso 1 1 calc R . . C24 C 0.0124(3) 0.2866(3) -0.25860(17) 0.0453(10) Uani 1 1 d . . . H24A H -0.0313 0.2511 -0.2852 0.054 Uiso 1 1 calc R . . C25 C 0.0952(3) 0.2504(3) -0.22316(18) 0.0447(10) Uani 1 1 d . . . H25A H 0.1084 0.1897 -0.2249 0.054 Uiso 1 1 calc R . . C26 C 0.1590(3) 0.3033(2) -0.18506(17) 0.0395(9) Uani 1 1 d . . . H26A H 0.2151 0.2769 -0.1608 0.047 Uiso 1 1 calc R . . C27 C 0.1707(3) 0.5474(2) -0.12668(16) 0.0332(8) Uani 1 1 d . . . C28 C 0.1740(3) 0.6177(2) -0.16720(17) 0.0403(9) Uani 1 1 d . . . H28A H 0.2177 0.6133 -0.2007 0.048 Uiso 1 1 calc R . . C29 C 0.1166(3) 0.6936(3) -0.16077(19) 0.0464(10) Uani 1 1 d . . . H29A H 0.1210 0.7393 -0.1896 0.056 Uiso 1 1 calc R . . C30 C 0.0529(3) 0.7024(3) -0.1124(2) 0.0513(11) Uani 1 1 d . . . H30A H 0.0136 0.7542 -0.1076 0.062 Uiso 1 1 calc R . . C31 C 0.0473(3) 0.6351(3) -0.07125(18) 0.0451(10) Uani 1 1 d . . . H31A H 0.0032 0.6403 -0.0380 0.054 Uiso 1 1 calc R . . C32 C 0.1057(3) 0.5596(2) -0.07804(17) 0.0399(9) Uani 1 1 d . . . H32A H 0.1013 0.5145 -0.0486 0.048 Uiso 1 1 calc R . . C33 C 0.3357(3) 0.4701(2) -0.17664(16) 0.0327(8) Uani 1 1 d . . . C34 C 0.3654(3) 0.4176(2) -0.22453(16) 0.0387(9) Uani 1 1 d . . . H34A H 0.3184 0.3733 -0.2395 0.046 Uiso 1 1 calc R . . C35 C 0.4611(3) 0.4274(3) -0.25127(19) 0.0512(11) Uani 1 1 d . . . H35A H 0.4783 0.3899 -0.2836 0.061 Uiso 1 1 calc R . . C36 C 0.5310(3) 0.4916(3) -0.2310(2) 0.0570(12) Uani 1 1 d . . . H36A H 0.5971 0.4975 -0.2485 0.068 Uiso 1 1 calc R . . C37 C 0.5037(3) 0.5472(3) -0.1851(2) 0.0524(11) Uani 1 1 d . . . H37A H 0.5503 0.5926 -0.1716 0.063 Uiso 1 1 calc R . . C38 C 0.4075(3) 0.5365(2) -0.15870(18) 0.0407(9) Uani 1 1 d . . . H38A H 0.3897 0.5755 -0.1274 0.049 Uiso 1 1 calc R . . C39 C 0.2649(3) 0.4053(2) -0.07372(15) 0.0320(8) Uani 1 1 d . . . C40 C 0.1941(3) 0.3540(2) -0.04245(17) 0.0403(9) Uani 1 1 d . . . H40A H 0.1236 0.3484 -0.0594 0.048 Uiso 1 1 calc R . . C41 C 0.2228(3) 0.3108(3) 0.01226(17) 0.0426(9) Uani 1 1 d . . . H41A H 0.1724 0.2762 0.0314 0.051 Uiso 1 1 calc R . . C42 C 0.3236(3) 0.3184(3) 0.03847(17) 0.0458(10) Uani 1 1 d . . . H42A H 0.3435 0.2890 0.0756 0.055 Uiso 1 1 calc R . . C43 C 0.3952(3) 0.3688(3) 0.01053(18) 0.0481(10) Uani 1 1 d . . . H43A H 0.4649 0.3749 0.0286 0.058 Uiso 1 1 calc R . . C44 C 0.3661(3) 0.4115(3) -0.04468(17) 0.0396(9) Uani 1 1 d . . . H44A H 0.4174 0.4460 -0.0631 0.048 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 I1 0.06427(19) 0.03568(15) 0.05120(17) 0.00067(13) -0.00462(13) -0.00648(13) Ca1 0.0262(3) 0.0338(4) 0.0295(3) 0.0017(3) 0.0031(3) 0.0018(3) O1 0.0557(16) 0.0411(15) 0.0317(13) 0.0042(11) 0.0104(12) 0.0111(13) O2 0.0277(13) 0.0511(16) 0.0392(14) -0.0047(12) 0.0014(11) 0.0033(11) O3 0.0267(13) 0.0570(17) 0.0522(16) 0.0181(14) 0.0043(12) 0.0013(12) O4 0.0448(15) 0.0503(16) 0.0286(13) -0.0017(12) 0.0030(11) -0.0053(12) O5 0.0469(15) 0.0347(14) 0.0449(15) 0.0045(12) 0.0081(12) 0.0052(12) C1 0.101(4) 0.062(3) 0.048(3) 0.015(2) 0.018(3) 0.034(3) C2 0.104(4) 0.067(3) 0.052(3) 0.021(2) 0.033(3) 0.014(3) C3 0.061(3) 0.057(3) 0.039(2) -0.0035(19) 0.019(2) 0.002(2) C4 0.046(2) 0.042(2) 0.037(2) -0.0032(17) 0.0047(18) 0.0036(18) C5 0.047(2) 0.078(3) 0.042(2) -0.008(2) -0.009(2) 0.015(2) C6 0.039(2) 0.088(4) 0.084(4) -0.011(3) -0.011(2) 0.017(2) C7 0.051(3) 0.086(4) 0.059(3) -0.003(3) 0.007(2) 0.026(2) C8 0.037(2) 0.071(3) 0.046(2) -0.003(2) 0.0116(19) 0.007(2) C9 0.036(2) 0.084(3) 0.053(3) 0.017(2) 0.004(2) 0.013(2) C10 0.045(3) 0.081(3) 0.062(3) -0.023(3) -0.005(2) 0.022(2) C11 0.036(2) 0.053(3) 0.076(3) 0.006(2) 0.003(2) -0.0065(19) C12 0.033(2) 0.057(3) 0.060(3) 0.005(2) 0.0123(19) -0.0026(18) C13 0.067(3) 0.069(3) 0.036(2) 0.008(2) 0.004(2) -0.026(2) C14 0.072(3) 0.069(3) 0.042(2) 0.000(2) -0.003(2) -0.007(2) C15 0.083(4) 0.083(4) 0.035(2) -0.003(2) 0.002(2) 0.030(3) C16 0.080(3) 0.060(3) 0.042(2) -0.017(2) -0.001(2) -0.003(2) C17 0.051(3) 0.044(2) 0.062(3) -0.005(2) -0.007(2) -0.008(2) C18 0.066(3) 0.038(3) 0.164(6) 0.012(3) 0.013(4) -0.004(2) C19 0.086(4) 0.042(3) 0.165(7) -0.012(3) -0.015(4) 0.007(3) C20 0.072(3) 0.045(2) 0.074(3) 0.011(2) 0.031(3) 0.021(2) B1 0.030(2) 0.032(2) 0.034(2) -0.0003(17) 0.0015(16) 0.0012(17) C21 0.0290(18) 0.037(2) 0.0264(17) -0.0010(15) 0.0057(14) 0.0005(15) C22 0.034(2) 0.045(2) 0.035(2) 0.0014(16) 0.0007(16) 0.0006(17) C23 0.034(2) 0.064(3) 0.039(2) -0.004(2) -0.0046(17) 0.0018(19) C24 0.038(2) 0.062(3) 0.038(2) -0.0140(19) 0.0083(18) -0.016(2) C25 0.049(2) 0.039(2) 0.047(2) -0.0096(18) 0.011(2) -0.0081(18) C26 0.039(2) 0.039(2) 0.041(2) -0.0033(17) 0.0000(17) 0.0026(17) C27 0.0269(17) 0.038(2) 0.0339(18) -0.0060(16) -0.0057(15) -0.0009(15) C28 0.041(2) 0.039(2) 0.039(2) -0.0029(17) -0.0038(17) 0.0067(17) C29 0.053(2) 0.037(2) 0.047(2) -0.0009(18) -0.013(2) 0.0103(18) C30 0.049(2) 0.047(2) 0.056(3) -0.015(2) -0.017(2) 0.019(2) C31 0.037(2) 0.056(3) 0.041(2) -0.0146(19) -0.0051(18) 0.0137(19) C32 0.0319(19) 0.047(2) 0.040(2) -0.0048(17) -0.0029(16) 0.0027(17) C33 0.0300(17) 0.0327(19) 0.0351(19) 0.0089(15) -0.0014(15) 0.0048(15) C34 0.040(2) 0.040(2) 0.037(2) 0.0055(17) 0.0087(17) 0.0020(17) C35 0.047(2) 0.064(3) 0.045(2) 0.005(2) 0.017(2) 0.008(2) C36 0.037(2) 0.075(3) 0.061(3) 0.032(3) 0.016(2) 0.003(2) C37 0.035(2) 0.048(2) 0.073(3) 0.022(2) -0.001(2) -0.0046(19) C38 0.037(2) 0.036(2) 0.048(2) 0.0079(17) -0.0025(17) 0.0000(17) C39 0.0324(19) 0.0316(18) 0.0319(18) -0.0032(15) 0.0022(15) 0.0070(15) C40 0.037(2) 0.044(2) 0.040(2) 0.0014(17) 0.0029(17) 0.0037(17) C41 0.049(2) 0.043(2) 0.037(2) 0.0041(17) 0.0097(18) 0.0029(18) C42 0.055(3) 0.053(2) 0.029(2) 0.0056(18) 0.0044(19) 0.018(2) C43 0.038(2) 0.067(3) 0.038(2) 0.000(2) -0.0034(18) 0.017(2) C44 0.034(2) 0.050(2) 0.035(2) 0.0008(17) 0.0026(16) 0.0040(17) _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 I1 Ca1 3.0660(7) . ? Ca1 O3 2.339(2) . ? Ca1 O1 2.343(2) . ? Ca1 O2 2.344(2) . ? Ca1 O5 2.364(3) . ? Ca1 O4 2.383(2) . ? O1 C4 1.442(4) . ? O1 C1 1.444(5) . ? O2 C5 1.430(5) . ? O2 C8 1.465(5) . ? O3 C9 1.434(5) . ? O3 C12 1.466(5) . ? O4 C16 1.454(5) . ? O4 C13 1.458(5) . ? O5 C17 1.459(5) . ? O5 C20 1.461(5) . ? C1 C2 1.439(6) . ? C2 C3 1.502(6) . ? C3 C4 1.518(5) . ? C5 C6 1.499(6) . ? C6 C7 1.449(7) . ? C7 C8 1.503(6) . ? C9 C10 1.516(7) . ? C10 C11 1.510(6) . ? C11 C12 1.507(6) . ? C13 C14 1.495(6) . ? C14 C15 1.488(7) . ? C15 C16 1.491(6) . ? C17 C18 1.500(6) . ? C18 C19 1.401(8) . ? C19 C20 1.479(7) . ? B1 C21 1.642(5) . ? B1 C27 1.642(5) . ? B1 C33 1.648(5) . ? B1 C39 1.650(5) . ? C21 C22 1.398(5) . ? C21 C26 1.407(5) . ? C22 C23 1.397(5) . ? C23 C24 1.380(6) . ? C24 C25 1.381(6) . ? C25 C26 1.387(5) . ? C27 C32 1.403(5) . ? C27 C28 1.402(5) . ? C28 C29 1.387(5) . ? C29 C30 1.381(6) . ? C30 C31 1.378(6) . ? C31 C32 1.391(5) . ? C33 C34 1.396(5) . ? C33 C38 1.406(5) . ? C34 C35 1.390(5) . ? C35 C36 1.381(6) . ? C36 C37 1.382(6) . ? C37 C38 1.396(5) . ? C39 C44 1.399(5) . ? C39 C40 1.407(5) . ? C40 C41 1.397(5) . ? C41 C42 1.372(6) . ? C42 C43 1.369(6) . ? C43 C44 1.404(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ca1 O1 86.97(9) . . ? O3 Ca1 O2 175.07(10) . . ? O1 Ca1 O2 90.82(9) . . ? O3 Ca1 O5 90.12(9) . . ? O1 Ca1 O5 86.33(9) . . ? O2 Ca1 O5 85.34(9) . . ? O3 Ca1 O4 89.25(9) . . ? O1 Ca1 O4 168.88(9) . . ? O2 Ca1 O4 92.11(9) . . ? O5 Ca1 O4 83.22(9) . . ? O3 Ca1 I1 96.66(7) . . ? O1 Ca1 I1 94.70(7) . . ? O2 Ca1 I1 87.91(7) . . ? O5 Ca1 I1 173.19(7) . . ? O4 Ca1 I1 96.13(7) . . ? C4 O1 C1 105.6(3) . . ? C4 O1 Ca1 122.8(2) . . ? C1 O1 Ca1 131.1(2) . . ? C5 O2 C8 108.5(3) . . ? C5 O2 Ca1 128.6(2) . . ? C8 O2 Ca1 118.8(2) . . ? C9 O3 C12 107.4(3) . . ? C9 O3 Ca1 125.2(2) . . ? C12 O3 Ca1 121.1(2) . . ? C16 O4 C13 108.8(3) . . ? C16 O4 Ca1 126.4(2) . . ? C13 O4 Ca1 124.4(2) . . ? C17 O5 C20 109.2(3) . . ? C17 O5 Ca1 123.2(2) . . ? C20 O5 Ca1 127.6(2) . . ? C2 C1 O1 106.9(4) . . ? C1 C2 C3 106.3(4) . . ? C2 C3 C4 104.5(3) . . ? O1 C4 C3 106.5(3) . . ? O2 C5 C6 105.6(3) . . ? C7 C6 C5 104.4(4) . . ? C6 C7 C8 104.8(4) . . ? O2 C8 C7 105.7(3) . . ? O3 C9 C10 103.6(4) . . ? C11 C10 C9 100.4(4) . . ? C12 C11 C10 103.5(3) . . ? O3 C12 C11 106.2(3) . . ? O4 C13 C14 106.5(3) . . ? C15 C14 C13 104.3(4) . . ? C14 C15 C16 104.4(4) . . ? O4 C16 C15 105.4(4) . . ? O5 C17 C18 104.7(4) . . ? C19 C18 C17 106.2(5) . . ? C18 C19 C20 108.5(4) . . ? O5 C20 C19 104.8(4) . . ? C21 B1 C27 107.4(3) . . ? C21 B1 C33 109.2(3) . . ? C27 B1 C33 110.4(3) . . ? C21 B1 C39 110.4(3) . . ? C27 B1 C39 111.0(3) . . ? C33 B1 C39 108.4(3) . . ? C22 C21 C26 114.3(3) . . ? C22 C21 B1 124.0(3) . . ? C26 C21 B1 121.5(3) . . ? C21 C22 C23 123.0(4) . . ? C24 C23 C22 120.1(4) . . ? C25 C24 C23 119.2(4) . . ? C24 C25 C26 119.6(4) . . ? C25 C26 C21 123.7(4) . . ? C32 C27 C28 114.9(3) . . ? C32 C27 B1 122.4(3) . . ? C28 C27 B1 122.4(3) . . ? C29 C28 C27 123.1(4) . . ? C30 C29 C28 119.9(4) . . ? C31 C30 C29 119.1(4) . . ? C30 C31 C32 120.4(4) . . ? C31 C32 C27 122.5(4) . . ? C34 C33 C38 115.3(3) . . ? C34 C33 B1 124.3(3) . . ? C38 C33 B1 120.2(3) . . ? C35 C34 C33 122.7(4) . . ? C36 C35 C34 120.2(4) . . ? C35 C36 C37 119.3(4) . . ? C36 C37 C38 119.8(4) . . ? C37 C38 C33 122.6(4) . . ? C44 C39 C40 114.4(3) . . ? C44 C39 B1 123.5(3) . . ? C40 C39 B1 122.1(3) . . ? C41 C40 C39 123.1(3) . . ? C42 C41 C40 120.1(4) . . ? C43 C42 C41 119.3(4) . . ? C42 C43 C44 120.4(4) . . ? C39 C44 C43 122.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.091 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.075 #==== END data_FO3786 _database_code_depnum_ccdc_archive 'CCDC 765643' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H33 Al N, C14 H32 Li N2 O2' _chemical_formula_sum 'C41 H65 Al Li N3 O2' _chemical_formula_weight 665.88 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.0743(5) _cell_length_b 16.2193(4) _cell_length_c 30.1905(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.514(3) _cell_angle_gamma 90.00 _cell_volume 8322.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 14979 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-can' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14979 _diffrn_reflns_av_R_equivalents 0.0969 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7658 _reflns_number_gt 3932 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0861P)^2^+17.6800P] 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 7658 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1780 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.2456 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Al1 Al 0.74535(7) 0.10518(7) 0.11396(4) 0.0354(3) Uani 1 1 d . . . Li1 Li 0.7307(5) -0.3655(5) 0.1439(3) 0.058(2) Uani 1 1 d . . . O1 O 0.7002(2) -0.2766(2) 0.10320(10) 0.0686(10) Uani 1 1 d . . . O2 O 0.62895(19) -0.4071(2) 0.15710(10) 0.0663(9) Uani 1 1 d . . . N1 N 0.65435(17) 0.15629(19) 0.08566(10) 0.0346(7) Uani 1 1 d . . . N2 N 0.8244(2) -0.3270(2) 0.18878(12) 0.0574(10) Uani 1 1 d . . . N3 N 0.8034(2) -0.4582(3) 0.12356(13) 0.0636(11) Uani 1 1 d . . . C1 C 0.6112(2) 0.1219(3) 0.04430(13) 0.0410(10) Uani 1 1 d . . . C2 C 0.5215(2) 0.1304(3) 0.04428(17) 0.0601(13) Uani 1 1 d . . . H2A H 0.4964 0.1140 0.0146 0.072 Uiso 1 1 calc R . . H2B H 0.5033 0.0914 0.0664 0.072 Uiso 1 1 calc R . . C3 C 0.4937(3) 0.2158(3) 0.05478(18) 0.0724(16) Uani 1 1 d . . . H3A H 0.5056 0.2547 0.0311 0.087 Uiso 1 1 calc R . . H3B H 0.4361 0.2156 0.0566 0.087 Uiso 1 1 calc R . . C4 C 0.5359(2) 0.2416(3) 0.09880(16) 0.0565(13) Uani 1 1 d . . . H4A H 0.5186 0.2056 0.1225 0.068 Uiso 1 1 calc R . . H4B H 0.5203 0.2988 0.1053 0.068 Uiso 1 1 calc R . . C5 C 0.6266(2) 0.2376(2) 0.10034(12) 0.0385(9) Uani 1 1 d . . . C6 C 0.6366(3) 0.1605(3) 0.00165(14) 0.0693(15) Uani 1 1 d . . . H6A H 0.6193 0.2181 -0.0004 0.104 Uiso 1 1 calc R . . H6B H 0.6127 0.1299 -0.0242 0.104 Uiso 1 1 calc R . . H6C H 0.6940 0.1581 0.0022 0.104 Uiso 1 1 calc R . . C7 C 0.6258(3) 0.0301(3) 0.04158(15) 0.0553(12) Uani 1 1 d . . . H7A H 0.6188 0.0045 0.0703 0.083 Uiso 1 1 calc R . . H7B H 0.6797 0.0205 0.0341 0.083 Uiso 1 1 calc R . . H7C H 0.5885 0.0059 0.0185 0.083 Uiso 1 1 calc R . . C8 C 0.6570(3) 0.3106(3) 0.07442(16) 0.0617(13) Uani 1 1 d . . . H8A H 0.6334 0.3088 0.0435 0.093 Uiso 1 1 calc R . . H8B H 0.7144 0.3072 0.0750 0.093 Uiso 1 1 calc R . . H8C H 0.6426 0.3624 0.0882 0.093 Uiso 1 1 calc R . . C9 C 0.6557(3) 0.2519(3) 0.14958(13) 0.0510(11) Uani 1 1 d . . . H9A H 0.6435 0.2034 0.1670 0.076 Uiso 1 1 calc R . . H9B H 0.6294 0.3004 0.1606 0.076 Uiso 1 1 calc R . . H9C H 0.7127 0.2610 0.1524 0.076 Uiso 1 1 calc R . . C10 C 0.8296(2) 0.1834(2) 0.14133(13) 0.0379(9) Uani 1 1 d . . . C11 C 0.8705(2) 0.2381(3) 0.11629(15) 0.0522(11) Uani 1 1 d . . . H11A H 0.8573 0.2404 0.0850 0.063 Uiso 1 1 calc R . . C12 C 0.9302(3) 0.2900(3) 0.1353(2) 0.0660(14) Uani 1 1 d . . . H12A H 0.9557 0.3270 0.1170 0.079 Uiso 1 1 calc R . . C13 C 0.9522(3) 0.2875(3) 0.1806(2) 0.0667(15) Uani 1 1 d . . . H13A H 0.9934 0.3216 0.1935 0.080 Uiso 1 1 calc R . . C14 C 0.9135(3) 0.2353(3) 0.20630(17) 0.0607(13) Uani 1 1 d . . . H14A H 0.9273 0.2332 0.2375 0.073 Uiso 1 1 calc R . . C15 C 0.8539(2) 0.1850(3) 0.18692(14) 0.0471(11) Uani 1 1 d . . . H15A H 0.8279 0.1495 0.2058 0.057 Uiso 1 1 calc R . . C16 C 0.8089(2) 0.0354(3) 0.07535(13) 0.0382(9) Uani 1 1 d . . . C17 C 0.8465(2) 0.0664(3) 0.03996(14) 0.0485(11) Uani 1 1 d . . . H17A H 0.8400 0.1231 0.0327 0.058 Uiso 1 1 calc R . . C18 C 0.8932(3) 0.0186(3) 0.01473(16) 0.0601(13) Uani 1 1 d . . . H18A H 0.9165 0.0425 -0.0096 0.072 Uiso 1 1 calc R . . C19 C 0.9058(3) -0.0638(3) 0.02498(16) 0.0550(12) Uani 1 1 d . . . H19A H 0.9385 -0.0968 0.0083 0.066 Uiso 1 1 calc R . . C20 C 0.8703(2) -0.0966(3) 0.05959(16) 0.0536(12) Uani 1 1 d . . . H20A H 0.8781 -0.1531 0.0671 0.064 Uiso 1 1 calc R . . C21 C 0.8232(2) -0.0485(3) 0.08367(14) 0.0442(10) Uani 1 1 d . . . H21A H 0.7990 -0.0736 0.1073 0.053 Uiso 1 1 calc R . . C22 C 0.7125(2) 0.0310(3) 0.16264(13) 0.0412(10) Uani 1 1 d . . . C23 C 0.7655(3) -0.0152(3) 0.19141(14) 0.0519(11) Uani 1 1 d . . . H23A H 0.8202 -0.0105 0.1885 0.062 Uiso 1 1 calc R . . C24 C 0.7409(4) -0.0674(3) 0.22395(15) 0.0682(15) Uani 1 1 d . . . H24A H 0.7784 -0.0980 0.2426 0.082 Uiso 1 1 calc R . . C25 C 0.6612(4) -0.0745(3) 0.22888(18) 0.0749(17) Uani 1 1 d . . . H25A H 0.6440 -0.1099 0.2511 0.090 Uiso 1 1 calc R . . C26 C 0.6071(4) -0.0304(3) 0.20173(18) 0.0683(15) Uani 1 1 d . . . H26A H 0.5525 -0.0351 0.2050 0.082 Uiso 1 1 calc R . . C27 C 0.6330(3) 0.0207(3) 0.16957(15) 0.0494(11) Uani 1 1 d . . . H27A H 0.5948 0.0506 0.1511 0.059 Uiso 1 1 calc R . . C28 C 0.7121(3) -0.2698(3) 0.05705(16) 0.0669(14) Uani 1 1 d . . . H28A H 0.6952 -0.3210 0.0411 0.080 Uiso 1 1 calc R . . H28B H 0.7684 -0.2603 0.0535 0.080 Uiso 1 1 calc R . . C29 C 0.6638(3) -0.1985(4) 0.03902(18) 0.0835(19) Uani 1 1 d . . . H29A H 0.6412 -0.2092 0.0081 0.100 Uiso 1 1 calc R . . H29B H 0.6956 -0.1474 0.0396 0.100 Uiso 1 1 calc R . . C30 C 0.6002(3) -0.1925(4) 0.07014(19) 0.0783(17) Uani 1 1 d . . . H30A H 0.5774 -0.1364 0.0702 0.094 Uiso 1 1 calc R . . H30B H 0.5576 -0.2330 0.0624 0.094 Uiso 1 1 calc R . . C31 C 0.6450(3) -0.2125(3) 0.11376(18) 0.0700(14) Uani 1 1 d . . . H31A H 0.6734 -0.1634 0.1264 0.084 Uiso 1 1 calc R . . H31B H 0.6094 -0.2329 0.1353 0.084 Uiso 1 1 calc R . . C32 C 0.6016(3) -0.4303(4) 0.19764(18) 0.0876(19) Uani 1 1 d . . . H32A H 0.5848 -0.3812 0.2138 0.105 Uiso 1 1 calc R . . H32B H 0.6435 -0.4590 0.2167 0.105 Uiso 1 1 calc R . . C33 C 0.5349(5) -0.4856(6) 0.1866(3) 0.149(4) Uani 1 1 d . . . H33A H 0.5485 -0.5423 0.1966 0.178 Uiso 1 1 calc R . . H33B H 0.4888 -0.4671 0.2015 0.178 Uiso 1 1 calc R . . C34 C 0.5166(4) -0.4838(5) 0.1388(3) 0.117(3) Uani 1 1 d . . . H34A H 0.5256 -0.5386 0.1258 0.141 Uiso 1 1 calc R . . H34B H 0.4609 -0.4681 0.1310 0.141 Uiso 1 1 calc R . . C35 C 0.5680(4) -0.4238(5) 0.1224(2) 0.106(2) Uani 1 1 d . . . H35A H 0.5385 -0.3727 0.1140 0.127 Uiso 1 1 calc R . . H35B H 0.5909 -0.4453 0.0958 0.127 Uiso 1 1 calc R . . C36 C 0.8833(3) -0.3948(4) 0.18734(18) 0.0737(15) Uani 1 1 d . . . H36A H 0.8711 -0.4390 0.2082 0.088 Uiso 1 1 calc R . . H36B H 0.9364 -0.3732 0.1972 0.088 Uiso 1 1 calc R . . C37 C 0.8834(3) -0.4304(4) 0.14116(19) 0.0722(15) Uani 1 1 d . . . H37A H 0.9021 -0.3881 0.1210 0.087 Uiso 1 1 calc R . . H37B H 0.9201 -0.4777 0.1419 0.087 Uiso 1 1 calc R . . C38 C 0.8046(4) -0.4783(4) 0.07598(19) 0.103(2) Uani 1 1 d . . . H38A H 0.8423 -0.5228 0.0726 0.154 Uiso 1 1 calc R . . H38B H 0.8202 -0.4293 0.0599 0.154 Uiso 1 1 calc R . . H38C H 0.7520 -0.4959 0.0638 0.154 Uiso 1 1 calc R . . C39 C 0.7811(4) -0.5323(3) 0.1475(2) 0.0847(18) Uani 1 1 d . . . H39A H 0.8192 -0.5764 0.1436 0.127 Uiso 1 1 calc R . . H39B H 0.7285 -0.5503 0.1355 0.127 Uiso 1 1 calc R . . H39C H 0.7809 -0.5195 0.1792 0.127 Uiso 1 1 calc R . . C40 C 0.8561(3) -0.2508(3) 0.17136(17) 0.0674(14) Uani 1 1 d . . . H40A H 0.9054 -0.2364 0.1890 0.101 Uiso 1 1 calc R . . H40B H 0.8179 -0.2061 0.1732 0.101 Uiso 1 1 calc R . . H40C H 0.8660 -0.2590 0.1402 0.101 Uiso 1 1 calc R . . C41 C 0.8114(4) -0.3131(4) 0.23511(16) 0.0860(19) Uani 1 1 d . . . H41A H 0.8607 -0.2955 0.2517 0.129 Uiso 1 1 calc R . . H41B H 0.7932 -0.3643 0.2480 0.129 Uiso 1 1 calc R . . H41C H 0.7715 -0.2701 0.2368 0.129 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 Al1 0.0314(6) 0.0390(7) 0.0356(6) 0.0003(5) 0.0031(5) 0.0022(5) Li1 0.057(5) 0.063(5) 0.055(4) -0.005(4) 0.006(4) 0.002(4) O1 0.077(2) 0.080(2) 0.0503(19) 0.0086(17) 0.0131(17) 0.023(2) O2 0.061(2) 0.081(2) 0.056(2) 0.0016(18) 0.0000(17) -0.0063(18) N1 0.0305(16) 0.0401(19) 0.0326(16) -0.0055(14) 0.0003(13) 0.0061(15) N2 0.075(3) 0.058(3) 0.040(2) -0.0056(18) 0.0123(19) -0.011(2) N3 0.064(3) 0.066(3) 0.061(2) -0.017(2) 0.007(2) -0.002(2) C1 0.041(2) 0.040(2) 0.040(2) -0.0087(18) -0.0069(18) 0.0048(19) C2 0.042(2) 0.061(3) 0.074(3) -0.028(3) -0.013(2) 0.013(2) C3 0.047(3) 0.077(4) 0.088(4) -0.036(3) -0.022(3) 0.020(3) C4 0.047(3) 0.051(3) 0.071(3) -0.024(2) 0.002(2) 0.014(2) C5 0.039(2) 0.040(2) 0.036(2) -0.0078(17) -0.0037(17) 0.0079(19) C6 0.089(4) 0.084(4) 0.035(2) -0.010(2) 0.004(2) 0.005(3) C7 0.051(3) 0.051(3) 0.061(3) -0.021(2) -0.009(2) 0.008(2) C8 0.085(4) 0.042(3) 0.058(3) 0.003(2) 0.007(3) 0.003(3) C9 0.057(3) 0.052(3) 0.043(2) -0.016(2) 0.001(2) 0.014(2) C10 0.0258(19) 0.047(3) 0.041(2) -0.0021(18) 0.0018(17) 0.0031(18) C11 0.046(2) 0.057(3) 0.054(3) 0.000(2) 0.011(2) -0.004(2) C12 0.045(3) 0.055(3) 0.100(4) -0.003(3) 0.020(3) -0.007(2) C13 0.039(3) 0.059(3) 0.100(4) -0.022(3) -0.008(3) -0.007(2) C14 0.051(3) 0.065(3) 0.062(3) -0.010(3) -0.013(2) 0.000(3) C15 0.040(2) 0.053(3) 0.048(2) -0.003(2) -0.001(2) -0.002(2) C16 0.033(2) 0.040(2) 0.041(2) 0.0007(18) -0.0021(17) 0.0036(18) C17 0.050(3) 0.046(3) 0.052(3) 0.002(2) 0.015(2) 0.007(2) C18 0.049(3) 0.078(4) 0.057(3) -0.006(3) 0.022(2) 0.007(3) C19 0.044(3) 0.057(3) 0.065(3) -0.015(2) 0.017(2) 0.012(2) C20 0.042(2) 0.043(3) 0.075(3) -0.004(2) 0.005(2) 0.012(2) C21 0.033(2) 0.045(3) 0.055(3) -0.003(2) 0.0059(19) 0.0089(19) C22 0.045(2) 0.040(2) 0.039(2) -0.0001(18) 0.0059(19) -0.0030(19) C23 0.065(3) 0.048(3) 0.043(2) -0.001(2) 0.005(2) 0.000(2) C24 0.116(5) 0.044(3) 0.043(3) 0.004(2) 0.000(3) 0.007(3) C25 0.120(5) 0.056(3) 0.053(3) -0.002(3) 0.031(3) -0.029(3) C26 0.085(4) 0.056(3) 0.068(3) -0.003(3) 0.027(3) -0.028(3) C27 0.053(3) 0.042(3) 0.054(3) -0.004(2) 0.013(2) -0.006(2) C28 0.069(3) 0.081(4) 0.052(3) 0.002(3) 0.008(3) -0.002(3) C29 0.064(3) 0.120(5) 0.064(3) 0.024(3) -0.012(3) -0.011(3) C30 0.062(3) 0.089(4) 0.085(4) 0.031(3) 0.011(3) 0.008(3) C31 0.065(3) 0.071(4) 0.075(4) 0.005(3) 0.015(3) 0.011(3) C32 0.072(4) 0.131(6) 0.061(3) -0.005(3) 0.011(3) -0.019(4) C33 0.117(7) 0.205(10) 0.126(7) 0.014(7) 0.022(6) -0.063(7) C34 0.088(5) 0.130(7) 0.130(7) -0.021(5) -0.012(5) -0.037(5) C35 0.085(4) 0.146(7) 0.080(4) 0.006(4) -0.025(4) -0.038(5) C36 0.068(3) 0.072(4) 0.078(4) -0.005(3) -0.009(3) -0.003(3) C37 0.057(3) 0.072(4) 0.087(4) -0.012(3) 0.008(3) 0.009(3) C38 0.126(6) 0.116(6) 0.065(4) -0.034(4) 0.006(4) 0.029(5) C39 0.088(4) 0.055(4) 0.111(5) -0.001(3) 0.006(4) 0.000(3) C40 0.078(4) 0.061(3) 0.064(3) -0.003(3) 0.011(3) -0.015(3) C41 0.122(5) 0.093(4) 0.045(3) -0.009(3) 0.020(3) -0.027(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 Al1 N1 1.891(3) . ? Al1 C16 2.015(4) . ? Al1 C22 2.020(4) . ? Al1 C10 2.034(4) . ? Li1 O1 1.932(9) . ? Li1 O2 1.940(9) . ? Li1 N3 2.080(9) . ? Li1 N2 2.092(9) . ? O1 C28 1.431(5) . ? O1 C31 1.459(6) . ? O2 C32 1.403(6) . ? O2 C35 1.430(6) . ? N1 C5 1.483(5) . ? N1 C1 1.496(4) . ? N2 C41 1.455(6) . ? N2 C40 1.466(6) . ? N2 C36 1.493(6) . ? N3 C39 1.469(7) . ? N3 C38 1.475(6) . ? N3 C37 1.487(6) . ? C1 C7 1.513(6) . ? C1 C6 1.531(6) . ? C1 C2 1.538(6) . ? C2 C3 1.507(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.547(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.537(6) . ? C5 C9 1.539(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.396(6) . ? C10 C15 1.399(5) . ? C11 C12 1.401(6) . ? C11 H11A 0.9500 . ? C12 C13 1.383(7) . ? C12 H12A 0.9500 . ? C13 C14 1.362(7) . ? C13 H13A 0.9500 . ? C14 C15 1.388(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.393(5) . ? C16 C21 1.400(6) . ? C17 C18 1.391(6) . ? C17 H17A 0.9500 . ? C18 C19 1.384(7) . ? C18 H18A 0.9500 . ? C19 C20 1.366(6) . ? C19 H19A 0.9500 . ? C20 C21 1.378(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.403(6) . ? C22 C23 1.408(6) . ? C23 C24 1.392(6) . ? C23 H23A 0.9500 . ? C24 C25 1.388(8) . ? C24 H24A 0.9500 . ? C25 C26 1.375(8) . ? C25 H25A 0.9500 . ? C26 C27 1.381(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.492(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.507(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.494(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.463(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.448(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.429(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.509(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? 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 Al1 C16 116.71(15) . . ? N1 Al1 C22 108.44(16) . . ? C16 Al1 C22 106.78(17) . . ? N1 Al1 C10 115.38(16) . . ? C16 Al1 C10 100.74(16) . . ? C22 Al1 C10 108.13(17) . . ? O1 Li1 O2 101.5(4) . . ? O1 Li1 N3 119.0(4) . . ? O2 Li1 N3 112.4(4) . . ? O1 Li1 N2 109.4(4) . . ? O2 Li1 N2 127.9(4) . . ? N3 Li1 N2 88.0(3) . . ? C28 O1 C31 108.2(4) . . ? C28 O1 Li1 128.4(4) . . ? C31 O1 Li1 122.2(4) . . ? C32 O2 C35 107.9(4) . . ? C32 O2 Li1 130.8(4) . . ? C35 O2 Li1 121.2(4) . . ? C5 N1 C1 115.8(3) . . ? C5 N1 Al1 121.8(2) . . ? C1 N1 Al1 122.1(2) . . ? C41 N2 C40 108.0(4) . . ? C41 N2 C36 108.0(4) . . ? C40 N2 C36 109.7(4) . . ? C41 N2 Li1 119.4(4) . . ? C40 N2 Li1 107.7(4) . . ? C36 N2 Li1 103.7(4) . . ? C39 N3 C38 109.1(5) . . ? C39 N3 C37 110.2(4) . . ? C38 N3 C37 108.5(4) . . ? C39 N3 Li1 104.9(4) . . ? C38 N3 Li1 120.7(4) . . ? C37 N3 Li1 103.2(4) . . ? N1 C1 C7 110.0(3) . . ? N1 C1 C6 113.1(3) . . ? C7 C1 C6 107.1(4) . . ? N1 C1 C2 112.2(3) . . ? C7 C1 C2 105.0(4) . . ? C6 C1 C2 109.0(4) . . ? C3 C2 C1 114.6(4) . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 107.9(4) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C3 C4 C5 114.0(4) . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C8 113.6(3) . . ? N1 C5 C9 109.9(3) . . ? C8 C5 C9 106.4(3) . . ? N1 C5 C4 112.1(3) . . ? C8 C5 C4 109.7(4) . . ? C9 C5 C4 104.6(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 113.9(4) . . ? C11 C10 Al1 123.2(3) . . ? C15 C10 Al1 122.8(3) . . ? C12 C11 C10 122.7(4) . . ? C12 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C14 C13 C12 118.7(5) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C10 124.1(4) . . ? C14 C15 H15A 117.9 . . ? C10 C15 H15A 117.9 . . ? C17 C16 C21 113.7(4) . . ? C17 C16 Al1 123.7(3) . . ? C21 C16 Al1 122.4(3) . . ? C16 C17 C18 123.4(4) . . ? C16 C17 H17A 118.3 . . ? C18 C17 H17A 118.3 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C20 C19 C18 118.4(4) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C16 123.8(4) . . ? C20 C21 H21A 118.1 . . ? C16 C21 H21A 118.1 . . ? C27 C22 C23 114.7(4) . . ? C27 C22 Al1 121.3(3) . . ? C23 C22 Al1 124.0(3) . . ? C24 C23 C22 122.6(5) . . ? C24 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C26 C25 C24 120.2(5) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C27 119.3(5) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? C26 C27 C22 123.8(5) . . ? C26 C27 H27A 118.1 . . ? C22 C27 H27A 118.1 . . ? O1 C28 C29 106.9(4) . . ? O1 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? O1 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.6 . . ? C28 C29 C30 103.2(4) . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29B 111.1 . . ? C30 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? C31 C30 C29 101.3(4) . . ? C31 C30 H30A 111.5 . . ? C29 C30 H30A 111.5 . . ? C31 C30 H30B 111.5 . . ? C29 C30 H30B 111.5 . . ? H30A C30 H30B 109.3 . . ? O1 C31 C30 104.4(4) . . ? O1 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? O1 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? O2 C32 C33 106.4(5) . . ? O2 C32 H32A 110.4 . . ? C33 C32 H32A 110.4 . . ? O2 C32 H32B 110.4 . . ? C33 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C34 C33 C32 107.7(6) . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C35 C34 C33 106.1(6) . . ? C35 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? C35 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C34 C35 O2 107.7(5) . . ? C34 C35 H35A 110.2 . . ? O2 C35 H35A 110.2 . . ? C34 C35 H35B 110.2 . . ? O2 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? N2 C36 C37 111.6(4) . . ? N2 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? N2 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? N3 C37 C36 111.4(4) . . ? N3 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? N3 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 H39A 109.5 . . ? N3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C40 H40A 109.5 . . ? N2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N2 C41 H41A 109.5 . . ? N2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 0.270 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.050 #==== END data_FO3604 _database_code_depnum_ccdc_archive 'CCDC 765644' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H38 Al N2), C12 H26 K O3, C8 H16 K O2' _chemical_formula_sum 'C52 H59 Al K N2 O2.50' _chemical_formula_weight 818.09 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8940(4) _cell_length_b 12.2427(5) _cell_length_c 34.7637(13) _cell_angle_alpha 94.365(2) _cell_angle_beta 91.070(2) _cell_angle_gamma 104.162(2) _cell_volume 4479.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 19265 _cell_measurement_theta_min 1.18 _cell_measurement_theta_max 27.63 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19265 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.63 _reflns_number_total 14916 _reflns_number_gt 9481 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1030P)^2^+8.7760P] 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 14916 _refine_ls_number_parameters 1042 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2594 _refine_ls_wR_factor_gt 0.2264 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _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 K1A K 0.24757(10) -0.07286(10) 0.87170(3) 0.0480(3) Uani 1 1 d . A . Al1A Al 0.61116(11) 0.29128(12) 0.86961(3) 0.0336(3) Uani 1 1 d . . . O1A O 0.0509(3) -0.0560(4) 0.82456(11) 0.0665(11) Uani 1 1 d . . . O2A O 0.3088(4) -0.1593(4) 0.93783(14) 0.0901(15) Uani 1 1 d . . . O3A O 0.1158(6) -0.2985(4) 0.85467(16) 0.1057(17) Uani 1 1 d . . . N1A N 0.6145(3) 0.1360(3) 0.87237(9) 0.0355(9) Uani 1 1 d . A . N2A N 0.4302(3) 0.2637(3) 0.86682(9) 0.0369(9) Uani 1 1 d . A . C1A C 0.4946(5) -0.1533(5) 0.82985(15) 0.0548(14) Uani 1 1 d . . . H1AA H 0.5103 -0.2286 0.8341 0.066 Uiso 1 1 calc R A . C2A C 0.4199(5) -0.1416(5) 0.79860(16) 0.0559(14) Uani 1 1 d . A . H2AA H 0.3829 -0.2084 0.7800 0.067 Uiso 1 1 calc R . . C3A C 0.4084(5) -0.0344(5) 0.79052(14) 0.0513(14) Uani 1 1 d . . . H3AA H 0.3622 -0.0264 0.7662 0.062 Uiso 1 1 calc R A . C4A C 0.4692(4) 0.0622(5) 0.81330(12) 0.0434(12) Uani 1 1 d . A . H4AA H 0.4676 0.1387 0.8053 0.052 Uiso 1 1 calc R . . C5A C 0.5440(4) 0.0515(4) 0.84553(12) 0.0394(11) Uani 1 1 d . . . C6A C 0.5585(4) -0.0559(4) 0.85349(13) 0.0430(12) Uani 1 1 d . A . C7A C 0.6420(4) -0.0381(5) 0.88708(13) 0.0438(12) Uani 1 1 d . . . C8A C 0.6929(5) -0.1118(5) 0.90803(16) 0.0591(15) Uani 1 1 d . A . H8AA H 0.6748 -0.1903 0.9001 0.071 Uiso 1 1 calc R . . C9A C 0.7691(5) -0.0679(6) 0.94011(16) 0.0614(16) Uani 1 1 d . . . H9AA H 0.8045 -0.1163 0.9546 0.074 Uiso 1 1 calc R A . C10A C 0.7954(5) 0.0477(6) 0.95173(14) 0.0590(16) Uani 1 1 d . A . H10A H 0.8477 0.0762 0.9742 0.071 Uiso 1 1 calc R . . C11A C 0.7470(4) 0.1219(5) 0.93124(13) 0.0468(12) Uani 1 1 d . . . H11A H 0.7644 0.2000 0.9397 0.056 Uiso 1 1 calc R A . C12A C 0.6718(4) 0.0785(4) 0.89771(12) 0.0400(11) Uani 1 1 d . A . C13A C 0.3539(4) 0.2055(4) 0.89426(12) 0.0370(11) Uani 1 1 d . . . C14A C 0.3895(4) 0.1596(4) 0.92694(12) 0.0443(12) Uani 1 1 d . A . H14A H 0.4810 0.1737 0.9350 0.053 Uiso 1 1 calc R . . C15A C 0.2961(5) 0.1049(5) 0.95037(13) 0.0485(13) Uani 1 1 d . . . H15A H 0.3207 0.0794 0.9754 0.058 Uiso 1 1 calc R A . C16A C 0.1674(5) 0.0969(5) 0.94127(13) 0.0484(13) Uani 1 1 d . A . H16A H 0.1021 0.0636 0.9598 0.058 Uiso 1 1 calc R . . C17A C 0.1304(4) 0.1406(4) 0.90933(13) 0.0444(12) Uani 1 1 d . . . H17A H 0.0394 0.1397 0.9046 0.053 Uiso 1 1 calc R A . C18A C 0.2237(4) 0.1967(4) 0.88536(12) 0.0373(11) Uani 1 1 d . A . C19A C 0.2193(4) 0.2519(4) 0.85060(12) 0.0395(11) Uani 1 1 d . . . C20A C 0.1218(4) 0.2715(5) 0.82773(13) 0.0474(13) Uani 1 1 d . A . H20A H 0.0366 0.2488 0.8353 0.057 Uiso 1 1 calc R . . C21A C 0.1489(4) 0.3235(5) 0.79449(14) 0.0535(14) Uani 1 1 d . . . H21A H 0.0823 0.3371 0.7790 0.064 Uiso 1 1 calc R A . C22A C 0.2737(4) 0.3568(5) 0.78320(13) 0.0501(13) Uani 1 1 d . A . H22A H 0.2908 0.3914 0.7597 0.060 Uiso 1 1 calc R . . C23A C 0.3739(4) 0.3407(4) 0.80555(12) 0.0431(12) Uani 1 1 d . . . H23A H 0.4586 0.3642 0.7977 0.052 Uiso 1 1 calc R A . C24A C 0.3468(4) 0.2890(4) 0.83994(12) 0.0366(11) Uani 1 1 d . A . C25A C 0.6930(4) 0.3608(4) 0.82238(11) 0.0331(10) Uani 1 1 d . . . C26A C 0.6945(4) 0.4749(4) 0.81825(12) 0.0387(11) Uani 1 1 d . . . C27A C 0.7618(4) 0.5341(4) 0.78923(14) 0.0465(12) Uani 1 1 d . . . H27A H 0.7612 0.6110 0.7874 0.056 Uiso 1 1 calc R . . C28A C 0.8292(4) 0.4829(5) 0.76320(13) 0.0446(12) Uani 1 1 d . . . C29A C 0.8282(4) 0.3722(4) 0.76664(12) 0.0403(12) Uani 1 1 d . . . H29A H 0.8739 0.3361 0.7489 0.048 Uiso 1 1 calc R . . C30A C 0.7629(4) 0.3102(4) 0.79515(11) 0.0345(10) Uani 1 1 d . . . C31A C 0.6261(5) 0.5408(5) 0.84537(14) 0.0523(13) Uani 1 1 d . . . H31A H 0.5829 0.4917 0.8645 0.078 Uiso 1 1 calc R . . H31B H 0.5637 0.5678 0.8305 0.078 Uiso 1 1 calc R . . H31C H 0.6876 0.6056 0.8586 0.078 Uiso 1 1 calc R . . C32A C 0.9069(6) 0.5513(6) 0.73285(17) 0.0739(18) Uani 1 1 d . . . H32A H 0.9483 0.5024 0.7169 0.111 Uiso 1 1 calc R . . H32B H 0.9714 0.6143 0.7458 0.111 Uiso 1 1 calc R . . H32C H 0.8507 0.5810 0.7164 0.111 Uiso 1 1 calc R . . C33A C 0.7722(4) 0.1904(4) 0.79491(13) 0.0407(11) Uani 1 1 d . . . H33A H 0.8259 0.1743 0.7740 0.061 Uiso 1 1 calc R . . H33B H 0.6874 0.1395 0.7909 0.061 Uiso 1 1 calc R . . H33C H 0.8094 0.1786 0.8197 0.061 Uiso 1 1 calc R . . C34A C 0.6935(4) 0.3947(4) 0.91586(11) 0.0386(11) Uani 1 1 d . . . C35A C 0.6342(5) 0.4624(4) 0.94068(12) 0.0434(12) Uani 1 1 d . . . C36A C 0.7043(5) 0.5457(5) 0.96721(13) 0.0500(13) Uani 1 1 d . . . H36A H 0.6613 0.5911 0.9825 0.060 Uiso 1 1 calc R . . C37A C 0.8346(5) 0.5655(5) 0.97222(14) 0.0553(14) Uani 1 1 d . . . C38A C 0.8932(5) 0.4993(5) 0.94860(14) 0.0524(14) Uani 1 1 d . . . H38A H 0.9822 0.5094 0.9517 0.063 Uiso 1 1 calc R . . C39A C 0.8271(4) 0.4186(4) 0.92054(12) 0.0416(11) Uani 1 1 d . . . C40A C 0.4918(5) 0.4504(5) 0.93912(15) 0.0530(14) Uani 1 1 d . . . H40A H 0.4707 0.5051 0.9583 0.080 Uiso 1 1 calc R . . H40B H 0.4480 0.3736 0.9447 0.080 Uiso 1 1 calc R . . H40C H 0.4650 0.4648 0.9133 0.080 Uiso 1 1 calc R . . C41A C 0.9065(6) 0.6573(6) 1.00162(18) 0.082(2) Uani 1 1 d . . . H41A H 0.8468 0.6931 1.0153 0.123 Uiso 1 1 calc R . . H41B H 0.9666 0.7142 0.9884 0.123 Uiso 1 1 calc R . . H41C H 0.9527 0.6243 1.0202 0.123 Uiso 1 1 calc R . . C42A C 0.9048(4) 0.3594(4) 0.89421(13) 0.0452(12) Uani 1 1 d . . . H42A H 0.9950 0.3888 0.9013 0.068 Uiso 1 1 calc R . . H42B H 0.8894 0.3733 0.8674 0.068 Uiso 1 1 calc R . . H42C H 0.8802 0.2779 0.8970 0.068 Uiso 1 1 calc R . . C43A C 0.0664(11) -0.0401(13) 0.7849(3) 0.060(3) Uiso 0.50 1 d P A 1 H43A H 0.1275 -0.0805 0.7738 0.071 Uiso 0.50 1 calc PR A 1 H43B H 0.0947 0.0411 0.7806 0.071 Uiso 0.50 1 calc PR A 1 C43C C 0.0436(13) -0.1084(15) 0.7856(4) 0.078(4) Uiso 0.50 1 d P A 2 H43C H 0.0417 -0.1895 0.7859 0.093 Uiso 0.50 1 calc PR A 2 H43D H 0.1178 -0.0712 0.7712 0.093 Uiso 0.50 1 calc PR A 2 C44A C -0.0745(6) -0.0943(9) 0.7675(2) 0.111(3) Uani 1 1 d . . . H44A H -0.0964 -0.0481 0.7475 0.133 Uiso 0.50 1 calc PR A 1 H44B H -0.0818 -0.1719 0.7557 0.133 Uiso 0.50 1 calc PR A 1 H44C H -0.0600 -0.0217 0.7555 0.133 Uiso 0.50 1 calc PR A 2 H44D H -0.1099 -0.1570 0.7476 0.133 Uiso 0.50 1 calc PR A 2 C45A C -0.1584(6) -0.0961(6) 0.79983(19) 0.0759(18) Uani 1 1 d . A . H45A H -0.1974 -0.1744 0.8060 0.091 Uiso 1 1 calc R . . H45B H -0.2260 -0.0575 0.7945 0.091 Uiso 1 1 calc R . . C46A C -0.0691(6) -0.0327(7) 0.8316(2) 0.089(2) Uani 1 1 d . A . H46A H -0.0626 0.0494 0.8318 0.106 Uiso 1 1 calc R . . H46B H -0.0993 -0.0580 0.8570 0.106 Uiso 1 1 calc R . . C47A C 0.4181(6) -0.1354(7) 0.9624(2) 0.081(2) Uani 1 1 d . A . H47A H 0.4070 -0.0881 0.9859 0.098 Uiso 1 1 calc R . . H47B H 0.4930 -0.0948 0.9490 0.098 Uiso 1 1 calc R . . C48A C 0.4339(7) -0.2431(7) 0.9725(2) 0.097(2) Uani 1 1 d . . . H48A H 0.4783 -0.2355 0.9980 0.116 Uiso 1 1 calc R A . H48B H 0.4834 -0.2750 0.9530 0.116 Uiso 1 1 calc R . . C49A C 0.3035(7) -0.3161(7) 0.9734(2) 0.087(2) Uani 1 1 d . A . H49A H 0.2800 -0.3312 1.0002 0.104 Uiso 1 1 calc R . . H49B H 0.2955 -0.3890 0.9579 0.104 Uiso 1 1 calc R . . C50A C 0.2219(7) -0.2478(7) 0.9559(2) 0.089(2) Uani 1 1 d . A . H50A H 0.1598 -0.2955 0.9366 0.107 Uiso 1 1 calc R . . H50B H 0.1754 -0.2152 0.9762 0.107 Uiso 1 1 calc R . . C51A C -0.0553(9) -0.2584(9) 0.8915(3) 0.148(4) Uani 1 1 d . . . H51A H -0.1379 -0.2948 0.9012 0.222 Uiso 1 1 calc R A . H51B H -0.0653 -0.2005 0.8745 0.222 Uiso 1 1 calc R . . H51C H 0.0029 -0.2231 0.9132 0.222 Uiso 1 1 calc R . . C52A C -0.0030(8) -0.3450(9) 0.8693(3) 0.127(3) Uani 1 1 d . A . H52A H 0.0047 -0.4043 0.8864 0.152 Uiso 1 1 calc R . . H52B H -0.0629 -0.3813 0.8476 0.152 Uiso 1 1 calc R . . C53A C 0.1691(12) -0.3820(8) 0.8335(3) 0.149(5) Uani 1 1 d . A . H53A H 0.2196 -0.3492 0.8119 0.179 Uiso 1 1 calc R . . H53B H 0.1018 -0.4484 0.8232 0.179 Uiso 1 1 calc R . . C54A C 0.2530(9) -0.4140(10) 0.8643(3) 0.151(4) Uani 1 1 d . . . H54A H 0.2981 -0.4674 0.8525 0.227 Uiso 1 1 calc R A . H54B H 0.2002 -0.4492 0.8847 0.227 Uiso 1 1 calc R . . H54C H 0.3145 -0.3459 0.8754 0.227 Uiso 1 1 calc R . . K1B K 0.20780(10) 0.22558(10) 0.61285(3) 0.0531(3) Uani 1 1 d . B . Al1B Al -0.16038(12) -0.12197(13) 0.61131(4) 0.0403(4) Uani 1 1 d . . . O1B O 0.4267(4) 0.2538(4) 0.65344(12) 0.0762(13) Uani 1 1 d . . . O2B O 0.2403(5) 0.4413(4) 0.60344(15) 0.1004(16) Uani 1 1 d . B . N1B N 0.0184(3) -0.1103(3) 0.61492(10) 0.0382(9) Uani 1 1 d . . . N2B N -0.1471(3) 0.0383(4) 0.61192(10) 0.0444(10) Uani 1 1 d . . . C1B C 0.0966(4) -0.1379(4) 0.64291(11) 0.0382(11) Uani 1 1 d . . . C2B C 0.0618(4) -0.1989(5) 0.67498(13) 0.0501(13) Uani 1 1 d . . . H2BA H -0.0248 -0.2285 0.6801 0.060 Uiso 1 1 calc R . . C3B C 0.1576(5) -0.2151(5) 0.69926(14) 0.0598(16) Uani 1 1 d . . . H3BA H 0.1356 -0.2578 0.7209 0.072 Uiso 1 1 calc R . . C4B C 0.2855(5) -0.1701(5) 0.69254(14) 0.0559(15) Uani 1 1 d . . . H4BA H 0.3486 -0.1810 0.7100 0.067 Uiso 1 1 calc R . . C5B C 0.3207(4) -0.1108(5) 0.66118(13) 0.0484(13) Uani 1 1 d . . . H5BA H 0.4078 -0.0826 0.6563 0.058 Uiso 1 1 calc R . . C6B C 0.2260(4) -0.0920(4) 0.63626(12) 0.0379(11) Uani 1 1 d . . . C7B C 0.2293(4) -0.0350(4) 0.60204(12) 0.0395(11) Uani 1 1 d . . . C8B C 0.3272(5) 0.0266(4) 0.58071(13) 0.0441(12) Uani 1 1 d . . . H8BA H 0.4133 0.0354 0.5886 0.053 Uiso 1 1 calc R . . C9B C 0.2968(5) 0.0743(5) 0.54811(14) 0.0526(13) Uani 1 1 d . . . H9BA H 0.3624 0.1155 0.5334 0.063 Uiso 1 1 calc R . . C10B C 0.1700(5) 0.0623(5) 0.53662(14) 0.0548(14) Uani 1 1 d . . . H10B H 0.1511 0.0957 0.5142 0.066 Uiso 1 1 calc R . . C11B C 0.0718(5) 0.0032(4) 0.55706(13) 0.0468(12) Uani 1 1 d . . . H11B H -0.0138 -0.0038 0.5490 0.056 Uiso 1 1 calc R . . C12B C 0.1016(4) -0.0468(4) 0.59029(12) 0.0392(11) Uani 1 1 d . . . C13B C -0.0745(4) 0.1161(4) 0.64034(12) 0.0396(11) Uani 1 1 d . . . C14B C -0.0094(4) 0.0933(5) 0.67314(12) 0.0422(11) Uani 1 1 d . . . H14B H -0.0118 0.0179 0.6785 0.051 Uiso 1 1 calc R . . C15B C 0.0582(4) 0.1848(5) 0.69727(13) 0.0496(13) Uani 1 1 d . . . H15B H 0.1033 0.1713 0.7193 0.060 Uiso 1 1 calc R . . C16B C 0.0615(5) 0.2966(5) 0.68994(14) 0.0499(13) Uani 1 1 d . . . H16B H 0.1081 0.3574 0.7071 0.060 Uiso 1 1 calc R . . C17B C -0.0024(4) 0.3184(5) 0.65808(14) 0.0492(13) Uani 1 1 d . . . H17B H -0.0004 0.3942 0.6532 0.059 Uiso 1 1 calc R . . C18B C -0.0703(4) 0.2285(4) 0.63284(13) 0.0420(12) Uani 1 1 d . . . C19B C -0.1412(5) 0.2221(5) 0.59709(14) 0.0477(13) Uani 1 1 d . . . C20B C -0.1668(5) 0.3040(5) 0.57429(15) 0.0588(15) Uani 1 1 d . . . H20B H -0.1394 0.3821 0.5827 0.071 Uiso 1 1 calc R . . C21B C -0.2325(6) 0.2691(6) 0.53943(17) 0.0726(18) Uani 1 1 d . . . H21B H -0.2496 0.3234 0.5234 0.087 Uiso 1 1 calc R . . C22B C -0.2739(7) 0.1544(6) 0.52773(17) 0.080(2) Uani 1 1 d . . . H22B H -0.3197 0.1322 0.5037 0.096 Uiso 1 1 calc R . . C23B C -0.2513(6) 0.0724(5) 0.54945(15) 0.0667(17) Uani 1 1 d . . . H23B H -0.2799 -0.0052 0.5406 0.080 Uiso 1 1 calc R . . C24B C -0.1845(5) 0.1057(5) 0.58530(13) 0.0488(13) Uani 1 1 d . . . C25B C -0.2527(4) -0.1999(5) 0.65555(13) 0.0431(12) Uani 1 1 d . . . C26B C -0.3178(4) -0.1506(5) 0.68492(14) 0.0463(13) Uani 1 1 d . . . C27B C -0.3918(4) -0.2183(5) 0.71066(14) 0.0526(14) Uani 1 1 d . . . H27B H -0.4319 -0.1832 0.7304 0.063 Uiso 1 1 calc R . . C28B C -0.4091(5) -0.3338(5) 0.70866(16) 0.0547(14) Uani 1 1 d . . . C29B C -0.3470(5) -0.3824(5) 0.68035(16) 0.0589(14) Uani 1 1 d . . . H29B H -0.3574 -0.4620 0.6784 0.071 Uiso 1 1 calc R . . C30B C -0.2695(4) -0.3181(5) 0.65456(14) 0.0481(13) Uani 1 1 d . . . C31B C -0.3138(5) -0.0266(5) 0.68912(16) 0.0567(15) Uani 1 1 d . . . H31D H -0.3643 -0.0110 0.7109 0.085 Uiso 1 1 calc R . . H31E H -0.3486 -0.0053 0.6654 0.085 Uiso 1 1 calc R . . H31F H -0.2259 0.0172 0.6937 0.085 Uiso 1 1 calc R . . C32B C -0.4968(6) -0.4039(6) 0.73562(19) 0.0764(19) Uani 1 1 d . . . H32D H -0.5310 -0.3540 0.7535 0.115 Uiso 1 1 calc R . . H32E H -0.4498 -0.4468 0.7503 0.115 Uiso 1 1 calc R . . H32F H -0.5666 -0.4564 0.7206 0.115 Uiso 1 1 calc R . . C33B C -0.2056(5) -0.3825(5) 0.62539(15) 0.0571(14) Uani 1 1 d . . . H33D H -0.1532 -0.3294 0.6090 0.086 Uiso 1 1 calc R . . H33E H -0.2702 -0.4377 0.6093 0.086 Uiso 1 1 calc R . . H33F H -0.1520 -0.4219 0.6390 0.086 Uiso 1 1 calc R . . C34B C -0.2483(4) -0.2068(4) 0.56224(13) 0.0450(12) Uani 1 1 d . . . C35B C -0.3793(5) -0.2114(5) 0.55725(14) 0.0520(14) Uani 1 1 d . . . C36B C -0.4521(5) -0.2732(5) 0.52566(15) 0.0539(14) Uani 1 1 d . . . H36B H -0.5396 -0.2750 0.5237 0.065 Uiso 1 1 calc R . . C37B C -0.4012(5) -0.3316(5) 0.49743(14) 0.0519(13) Uani 1 1 d . . . C38B C -0.2753(5) -0.3307(4) 0.50235(13) 0.0496(13) Uani 1 1 d . . . H38B H -0.2389 -0.3723 0.4836 0.059 Uiso 1 1 calc R . . C39B C -0.1981(4) -0.2715(4) 0.53371(13) 0.0445(12) Uani 1 1 d . . . C40B C -0.4463(5) -0.1527(6) 0.58705(17) 0.0709(19) Uani 1 1 d . . . H40D H -0.5357 -0.1653 0.5790 0.106 Uiso 1 1 calc R . . H40E H -0.4064 -0.0714 0.5894 0.106 Uiso 1 1 calc R . . H40F H -0.4402 -0.1834 0.6120 0.106 Uiso 1 1 calc R . . C41B C -0.4799(5) -0.3947(5) 0.46274(15) 0.0663(16) Uani 1 1 d . . . H41D H -0.4270 -0.4303 0.4459 0.099 Uiso 1 1 calc R . . H41E H -0.5135 -0.3416 0.4484 0.099 Uiso 1 1 calc R . . H41F H -0.5504 -0.4529 0.4713 0.099 Uiso 1 1 calc R . . C42B C -0.0630(5) -0.2805(5) 0.53507(14) 0.0544(14) Uani 1 1 d . . . H42D H -0.0492 -0.3299 0.5129 0.082 Uiso 1 1 calc R . . H42E H -0.0457 -0.3123 0.5590 0.082 Uiso 1 1 calc R . . H42F H -0.0061 -0.2053 0.5342 0.082 Uiso 1 1 calc R . . C43B C 0.4147(6) 0.2266(8) 0.6918(2) 0.097(3) Uani 1 1 d . . . H43X H 0.3662 0.1471 0.6926 0.117 Uiso 1 1 calc R . . H43Y H 0.3682 0.2759 0.7061 0.117 Uiso 1 1 calc R . . C44B C 0.5407(6) 0.2422(8) 0.7099(2) 0.097(3) Uani 1 1 d . . . H44X H 0.5477 0.1728 0.7217 0.117 Uiso 1 1 calc R . . H44Y H 0.5573 0.3056 0.7303 0.117 Uiso 1 1 calc R . . C45B C 0.6319(6) 0.2673(6) 0.6789(2) 0.0764(19) Uani 1 1 d . . . H45C H 0.6842 0.2114 0.6767 0.092 Uiso 1 1 calc R . . H45D H 0.6887 0.3439 0.6840 0.092 Uiso 1 1 calc R . . C46B C 0.5529(6) 0.2598(8) 0.6431(2) 0.100(3) Uani 1 1 d . . . H46C H 0.5850 0.3272 0.6287 0.120 Uiso 1 1 calc R . . H46D H 0.5565 0.1918 0.6263 0.120 Uiso 1 1 calc R . . C47B C 0.1791(9) 0.5182(8) 0.5868(3) 0.111(3) Uiso 1 1 d . . . H47C H 0.1456 0.4884 0.5604 0.133 Uiso 0.516(11) 1 calc PR B 1 H47D H 0.1079 0.5294 0.6026 0.133 Uiso 0.516(11) 1 calc PR B 1 H47E H 0.2133 0.5374 0.5613 0.133 Uiso 0.484(11) 1 calc PR B 2 H47F H 0.0866 0.4858 0.5836 0.133 Uiso 0.484(11) 1 calc PR B 2 C48B C 0.2720(15) 0.6215(14) 0.5857(5) 0.097(5) Uiso 0.516(11) 1 d P B 1 H48C H 0.2357 0.6865 0.5929 0.116 Uiso 0.516(11) 1 calc PR B 1 H48D H 0.3061 0.6292 0.5596 0.116 Uiso 0.516(11) 1 calc PR B 1 C49B C 0.3726(13) 0.6156(12) 0.6143(4) 0.080(4) Uiso 0.516(11) 1 d P B 1 H49C H 0.4549 0.6255 0.6017 0.096 Uiso 0.516(11) 1 calc PR B 1 H49D H 0.3808 0.6766 0.6353 0.096 Uiso 0.516(11) 1 calc PR B 1 C48C C 0.2069(15) 0.6128(14) 0.6133(4) 0.086(5) Uiso 0.484(11) 1 d P B 2 H48E H 0.1283 0.6258 0.6245 0.103 Uiso 0.484(11) 1 calc PR B 2 H48F H 0.2502 0.6809 0.6007 0.103 Uiso 0.484(11) 1 calc PR B 2 C49C C 0.2921(14) 0.5878(14) 0.6441(4) 0.086(5) Uiso 0.484(11) 1 d P B 2 H49E H 0.3607 0.6559 0.6520 0.103 Uiso 0.484(11) 1 calc PR B 2 H49F H 0.2434 0.5641 0.6671 0.103 Uiso 0.484(11) 1 calc PR B 2 C50B C 0.3387(9) 0.5077(8) 0.6296(3) 0.117(3) Uiso 1 1 d . . . H50C H 0.3074 0.5144 0.6560 0.141 Uiso 0.516(11) 1 calc PR B 1 H50D H 0.4122 0.4736 0.6304 0.141 Uiso 0.516(11) 1 calc PR B 1 H50E H 0.3590 0.4620 0.6500 0.141 Uiso 0.484(11) 1 calc PR B 2 H50F H 0.4166 0.5383 0.6158 0.141 Uiso 0.484(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 K1A 0.0450(6) 0.0528(8) 0.0500(6) 0.0089(5) 0.0033(4) 0.0177(5) Al1A 0.0267(6) 0.0434(9) 0.0337(6) 0.0039(6) 0.0009(5) 0.0141(6) O1A 0.054(2) 0.082(3) 0.067(2) 0.006(2) -0.0064(18) 0.023(2) O2A 0.076(3) 0.093(4) 0.100(3) 0.045(3) -0.016(2) 0.010(3) O3A 0.125(5) 0.069(4) 0.125(4) 0.017(3) 0.032(3) 0.024(3) N1A 0.0332(19) 0.039(2) 0.0356(17) 0.0068(16) 0.0023(14) 0.0108(17) N2A 0.0281(18) 0.051(3) 0.0345(17) 0.0081(17) 0.0016(14) 0.0138(17) C1A 0.057(3) 0.044(4) 0.067(3) 0.004(3) 0.019(3) 0.018(3) C2A 0.055(3) 0.047(4) 0.062(3) -0.008(3) 0.017(3) 0.008(3) C3A 0.044(3) 0.058(4) 0.046(3) -0.011(3) 0.002(2) 0.006(3) C4A 0.038(2) 0.052(3) 0.041(2) 0.004(2) 0.0047(19) 0.013(2) C5A 0.030(2) 0.048(3) 0.043(2) 0.007(2) 0.0122(18) 0.012(2) C6A 0.039(3) 0.042(3) 0.052(3) 0.009(2) 0.016(2) 0.015(2) C7A 0.041(3) 0.048(4) 0.051(3) 0.013(2) 0.018(2) 0.023(2) C8A 0.063(4) 0.053(4) 0.073(4) 0.023(3) 0.021(3) 0.031(3) C9A 0.060(3) 0.080(5) 0.062(3) 0.029(3) 0.013(3) 0.044(3) C10A 0.046(3) 0.092(5) 0.049(3) 0.021(3) 0.005(2) 0.033(3) C11A 0.040(3) 0.062(4) 0.044(2) 0.012(2) 0.0052(19) 0.020(2) C12A 0.033(2) 0.053(4) 0.041(2) 0.014(2) 0.0108(18) 0.020(2) C13A 0.032(2) 0.042(3) 0.038(2) 0.004(2) 0.0055(17) 0.012(2) C14A 0.038(3) 0.056(4) 0.042(2) 0.007(2) 0.0057(19) 0.018(2) C15A 0.048(3) 0.061(4) 0.042(2) 0.010(2) 0.009(2) 0.022(3) C16A 0.043(3) 0.056(4) 0.046(3) 0.006(2) 0.017(2) 0.010(2) C17A 0.034(2) 0.049(3) 0.050(3) -0.002(2) 0.0121(19) 0.010(2) C18A 0.031(2) 0.042(3) 0.043(2) 0.001(2) 0.0055(18) 0.016(2) C19A 0.029(2) 0.051(3) 0.039(2) -0.002(2) 0.0028(17) 0.013(2) C20A 0.028(2) 0.068(4) 0.046(3) -0.001(2) -0.0004(19) 0.015(2) C21A 0.034(3) 0.078(4) 0.052(3) 0.004(3) -0.008(2) 0.024(3) C22A 0.038(3) 0.072(4) 0.046(2) 0.017(2) 0.001(2) 0.020(3) C23A 0.032(2) 0.060(4) 0.042(2) 0.009(2) 0.0032(18) 0.017(2) C24A 0.027(2) 0.047(3) 0.038(2) 0.001(2) -0.0001(17) 0.013(2) C25A 0.022(2) 0.039(3) 0.038(2) 0.0022(19) -0.0020(16) 0.0083(19) C26A 0.032(2) 0.043(3) 0.043(2) 0.003(2) -0.0027(18) 0.011(2) C27A 0.048(3) 0.037(3) 0.058(3) 0.011(2) 0.002(2) 0.014(2) C28A 0.038(3) 0.047(4) 0.051(3) 0.017(2) 0.001(2) 0.011(2) C29A 0.028(2) 0.056(4) 0.038(2) 0.002(2) 0.0020(17) 0.013(2) C30A 0.023(2) 0.047(3) 0.033(2) 0.0035(19) -0.0041(16) 0.0095(19) C31A 0.062(3) 0.048(4) 0.055(3) 0.007(2) 0.002(2) 0.027(3) C32A 0.071(4) 0.076(5) 0.074(4) 0.031(3) 0.025(3) 0.008(3) C33A 0.035(2) 0.043(3) 0.048(2) 0.004(2) 0.0074(19) 0.017(2) C34A 0.038(2) 0.046(3) 0.033(2) 0.002(2) -0.0002(17) 0.013(2) C35A 0.050(3) 0.048(3) 0.036(2) 0.001(2) 0.0087(19) 0.020(2) C36A 0.060(3) 0.055(4) 0.042(2) 0.000(2) 0.008(2) 0.030(3) C37A 0.061(3) 0.056(4) 0.049(3) -0.011(3) -0.006(2) 0.019(3) C38A 0.043(3) 0.059(4) 0.053(3) -0.006(3) -0.005(2) 0.013(3) C39A 0.043(3) 0.042(3) 0.041(2) -0.003(2) -0.0037(19) 0.016(2) C40A 0.048(3) 0.059(4) 0.057(3) -0.005(3) 0.014(2) 0.024(3) C41A 0.082(4) 0.083(5) 0.077(4) -0.035(4) -0.019(3) 0.027(4) C42A 0.035(2) 0.051(3) 0.050(3) -0.005(2) -0.0043(19) 0.015(2) C44A 0.062(4) 0.209(10) 0.072(4) -0.012(5) -0.014(3) 0.061(5) C45A 0.060(4) 0.078(5) 0.091(4) 0.002(4) -0.004(3) 0.021(3) C46A 0.055(4) 0.107(6) 0.099(5) -0.005(4) 0.001(3) 0.014(4) C47A 0.072(4) 0.095(6) 0.090(5) 0.033(4) 0.008(3) 0.036(4) C48A 0.093(5) 0.085(6) 0.112(6) 0.011(5) -0.033(4) 0.023(4) C49A 0.086(5) 0.082(5) 0.095(5) 0.039(4) 0.003(4) 0.015(4) C50A 0.079(5) 0.100(6) 0.083(4) 0.012(4) -0.002(4) 0.012(4) C51A 0.121(8) 0.132(9) 0.221(12) 0.064(8) 0.080(8) 0.067(7) C52A 0.088(6) 0.130(9) 0.142(8) 0.027(7) -0.001(6) -0.017(6) C53A 0.194(11) 0.072(7) 0.148(9) -0.018(6) 0.059(9) -0.025(7) C54A 0.101(7) 0.194(13) 0.152(9) 0.039(9) -0.019(6) 0.018(7) K1B 0.0435(6) 0.0474(8) 0.0678(7) -0.0018(6) -0.0012(5) 0.0125(5) Al1B 0.0323(7) 0.0466(10) 0.0436(7) -0.0031(6) -0.0071(5) 0.0157(7) O1B 0.049(2) 0.103(4) 0.076(3) -0.001(2) -0.0079(19) 0.020(2) O2B 0.118(4) 0.054(3) 0.116(4) 0.006(3) -0.039(3) -0.001(3) N1B 0.0333(19) 0.045(3) 0.0388(18) 0.0040(17) -0.0034(15) 0.0149(18) N2B 0.041(2) 0.050(3) 0.044(2) -0.0024(19) -0.0124(16) 0.0180(19) C1B 0.033(2) 0.051(3) 0.034(2) 0.002(2) 0.0001(17) 0.019(2) C2B 0.036(3) 0.078(4) 0.044(2) 0.014(2) 0.0069(19) 0.027(3) C3B 0.050(3) 0.094(5) 0.047(3) 0.026(3) 0.006(2) 0.035(3) C4B 0.042(3) 0.086(5) 0.049(3) 0.013(3) -0.007(2) 0.033(3) C5B 0.034(2) 0.070(4) 0.047(3) 0.005(2) -0.0023(19) 0.024(2) C6B 0.031(2) 0.049(3) 0.038(2) -0.002(2) 0.0015(17) 0.019(2) C7B 0.040(3) 0.043(3) 0.040(2) 0.000(2) 0.0021(19) 0.020(2) C8B 0.040(3) 0.039(3) 0.054(3) -0.002(2) 0.006(2) 0.012(2) C9B 0.057(3) 0.051(4) 0.049(3) 0.010(2) 0.009(2) 0.009(3) C10B 0.074(4) 0.051(4) 0.043(3) 0.009(2) 0.000(2) 0.021(3) C11B 0.046(3) 0.051(4) 0.043(2) 0.003(2) -0.005(2) 0.012(2) C12B 0.039(2) 0.041(3) 0.039(2) 0.000(2) -0.0004(18) 0.014(2) C13B 0.033(2) 0.042(3) 0.044(2) -0.002(2) -0.0010(18) 0.012(2) C14B 0.036(2) 0.049(3) 0.043(2) 0.002(2) -0.0029(19) 0.014(2) C15B 0.040(3) 0.065(4) 0.041(2) -0.001(2) -0.002(2) 0.011(3) C16B 0.042(3) 0.053(4) 0.050(3) -0.007(3) 0.000(2) 0.009(3) C17B 0.045(3) 0.051(4) 0.053(3) -0.005(2) 0.002(2) 0.017(3) C18B 0.036(2) 0.046(3) 0.047(2) -0.003(2) -0.0001(19) 0.017(2) C19B 0.049(3) 0.051(4) 0.050(3) 0.000(2) -0.005(2) 0.028(3) C20B 0.062(3) 0.055(4) 0.066(3) 0.002(3) -0.010(3) 0.030(3) C21B 0.090(4) 0.074(5) 0.066(3) 0.006(3) -0.023(3) 0.046(4) C22B 0.108(5) 0.074(5) 0.067(4) -0.014(3) -0.046(3) 0.049(4) C23B 0.083(4) 0.059(4) 0.064(3) -0.012(3) -0.036(3) 0.036(3) C24B 0.052(3) 0.052(4) 0.048(3) -0.005(2) -0.011(2) 0.028(3) C25B 0.027(2) 0.050(4) 0.052(3) -0.004(2) -0.0035(19) 0.013(2) C26B 0.030(2) 0.054(4) 0.052(3) -0.008(2) -0.007(2) 0.011(2) C27B 0.033(3) 0.072(5) 0.055(3) 0.000(3) 0.002(2) 0.018(3) C28B 0.038(3) 0.061(4) 0.069(3) 0.011(3) 0.008(2) 0.016(3) C29B 0.050(3) 0.055(4) 0.078(4) 0.014(3) 0.009(3) 0.021(3) C30B 0.039(3) 0.056(4) 0.055(3) 0.001(2) 0.001(2) 0.023(3) C31B 0.037(3) 0.061(4) 0.069(3) -0.017(3) 0.002(2) 0.014(3) C32B 0.060(4) 0.087(5) 0.090(4) 0.034(4) 0.022(3) 0.026(4) C33B 0.059(3) 0.052(4) 0.063(3) 0.003(3) 0.005(3) 0.022(3) C34B 0.042(3) 0.043(3) 0.052(3) -0.002(2) -0.007(2) 0.017(2) C35B 0.050(3) 0.054(4) 0.055(3) -0.007(3) -0.013(2) 0.023(3) C36B 0.041(3) 0.058(4) 0.063(3) 0.002(3) -0.014(2) 0.013(3) C37B 0.056(3) 0.047(4) 0.048(3) 0.001(2) -0.010(2) 0.006(3) C38B 0.056(3) 0.046(4) 0.045(3) -0.001(2) 0.000(2) 0.009(3) C39B 0.048(3) 0.039(3) 0.048(3) 0.002(2) -0.001(2) 0.013(2) C40B 0.049(3) 0.075(5) 0.090(4) -0.032(4) -0.026(3) 0.030(3) C41B 0.060(3) 0.074(5) 0.059(3) -0.005(3) -0.014(3) 0.009(3) C42B 0.050(3) 0.060(4) 0.054(3) -0.005(3) 0.002(2) 0.019(3) C43B 0.059(4) 0.143(8) 0.083(5) 0.006(5) -0.005(3) 0.014(4) C44B 0.068(4) 0.154(8) 0.083(4) 0.001(5) -0.004(4) 0.055(5) C45B 0.058(4) 0.067(5) 0.108(5) 0.006(4) -0.010(4) 0.025(3) C46B 0.057(4) 0.151(8) 0.078(4) -0.030(5) -0.003(3) 0.008(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 K1A O1A 2.731(4) . ? K1A O2A 2.740(4) . ? K1A O3A 2.797(6) . ? K1A C15A 3.313(5) . ? K1A C14A 3.329(5) . ? K1A C16A 3.336(5) . ? K1A C13A 3.346(5) . ? K1A C3A 3.352(5) . ? K1A C2A 3.364(5) . ? K1A C17A 3.368(5) . ? K1A C18A 3.372(5) . ? K1A C4A 3.380(5) . ? Al1A N2A 1.916(4) . ? Al1A N1A 1.920(4) . ? Al1A C34A 2.019(4) . ? Al1A C25A 2.027(4) . ? O1A C43A 1.413(11) . ? O1A C46A 1.426(7) . ? O1A C43C 1.446(14) . ? O2A C47A 1.410(7) . ? O2A C50A 1.446(8) . ? O3A C52A 1.402(9) . ? O3A C53A 1.454(11) . ? N1A C12A 1.397(5) . ? N1A C5A 1.403(6) . ? N2A C24A 1.395(5) . ? N2A C13A 1.397(5) . ? C1A C2A 1.382(8) . ? C1A C6A 1.416(7) . ? C1A H1AA 1.0000 . ? C2A C3A 1.397(8) . ? C2A H2AA 1.0000 . ? C3A C4A 1.385(7) . ? C3A H3AA 1.0000 . ? C4A C5A 1.406(6) . ? C4A H4AA 1.0000 . ? C5A C6A 1.409(7) . ? C6A C7A 1.436(7) . ? C7A C12A 1.403(7) . ? C7A C8A 1.408(7) . ? C8A C9A 1.371(8) . ? C8A H8AA 0.9500 . ? C9A C10A 1.399(8) . ? C9A H9AA 0.9500 . ? C10A C11A 1.388(7) . ? C10A H10A 0.9500 . ? C11A C12A 1.404(6) . ? C11A H11A 0.9500 . ? C13A C14A 1.394(6) . ? C13A C18A 1.422(6) . ? C14A C15A 1.389(7) . ? C14A H14A 1.0000 . ? C15A C16A 1.410(7) . ? C15A H15A 1.0000 . ? C16A C17A 1.364(7) . ? C16A H16A 1.0000 . ? C17A C18A 1.406(6) . ? C17A H17A 1.0000 . ? C18A C19A 1.434(6) . ? C19A C20A 1.393(6) . ? C19A C24A 1.417(6) . ? C20A C21A 1.364(7) . ? C20A H20A 0.9500 . ? C21A C22A 1.394(7) . ? C21A H21A 0.9500 . ? C22A C23A 1.389(6) . ? C22A H22A 0.9500 . ? C23A C24A 1.398(6) . ? C23A H23A 0.9500 . ? C25A C26A 1.412(7) . ? C25A C30A 1.424(6) . ? C26A C27A 1.400(6) . ? C26A C31A 1.516(6) . ? C27A C28A 1.384(7) . ? C27A H27A 0.9500 . ? C28A C29A 1.366(7) . ? C28A C32A 1.534(7) . ? C29A C30A 1.393(6) . ? C29A H29A 0.9500 . ? C30A C33A 1.495(7) . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A C39A 1.416(6) . ? C34A C35A 1.422(6) . ? C35A C36A 1.387(7) . ? C35A C40A 1.522(7) . ? C36A C37A 1.386(7) . ? C36A H36A 0.9500 . ? C37A C38A 1.382(7) . ? C37A C41A 1.512(7) . ? C38A C39A 1.388(6) . ? C38A H38A 0.9500 . ? C39A C42A 1.519(6) . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 0.9800 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A C44A 1.603(13) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C43C C44A 1.475(14) . ? C43C H43C 0.9900 . ? C43C H43D 0.9900 . ? C44A C45A 1.460(9) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C45A C46A 1.494(9) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A C48A 1.438(10) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A C49A 1.485(10) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C50A 1.509(9) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C51A C52A 1.493(12) . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A C54A 1.528(14) . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C54A H54A 0.9800 . ? C54A H54B 0.9800 . ? C54A H54C 0.9800 . ? K1B O2B 2.625(5) . ? K1B O1B 2.682(4) . ? K1B C9B 3.124(5) . ? K1B C18B 3.129(4) . ? K1B C10B 3.152(5) . ? K1B C8B 3.172(5) . ? K1B C17B 3.185(5) . ? K1B C13B 3.234(5) . ? K1B C11B 3.238(5) . ? K1B C7B 3.249(5) . ? K1B C12B 3.280(5) . ? K1B C16B 3.311(5) . ? Al1B N1B 1.918(4) . ? Al1B N2B 1.931(5) . ? Al1B C34B 2.022(5) . ? Al1B C25B 2.025(5) . ? O1B C43B 1.400(8) . ? O1B C46B 1.413(7) . ? O2B C47B 1.428(10) . ? O2B C50B 1.437(10) . ? N1B C12B 1.395(6) . ? N1B C1B 1.395(5) . ? N2B C13B 1.403(6) . ? N2B C24B 1.403(6) . ? C1B C2B 1.396(6) . ? C1B C6B 1.415(6) . ? C2B C3B 1.390(6) . ? C2B H2BA 0.9500 . ? C3B C4B 1.398(7) . ? C3B H3BA 0.9500 . ? C4B C5B 1.365(7) . ? C4B H4BA 0.9500 . ? C5B C6B 1.407(6) . ? C5B H5BA 0.9500 . ? C6B C7B 1.422(6) . ? C7B C8B 1.406(7) . ? C7B C12B 1.412(6) . ? C8B C9B 1.384(7) . ? C8B H8BA 0.9500 . ? C9B C10B 1.400(7) . ? C9B H9BA 0.9500 . ? C10B C11B 1.378(7) . ? C10B H10B 0.9500 . ? C11B C12B 1.416(6) . ? C11B H11B 0.9500 . ? C13B C18B 1.410(7) . ? C13B C14B 1.413(6) . ? C14B C15B 1.390(7) . ? C14B H14B 0.9500 . ? C15B C16B 1.403(8) . ? C15B H15B 0.9500 . ? C16B C17B 1.375(7) . ? C16B H16B 0.9500 . ? C17B C18B 1.400(7) . ? C17B H17B 0.9500 . ? C18B C19B 1.438(6) . ? C19B C20B 1.400(7) . ? C19B C24B 1.413(7) . ? C20B C21B 1.380(7) . ? C20B H20B 0.9500 . ? C21B C22B 1.392(9) . ? C21B H21B 0.9500 . ? C22B C23B 1.366(8) . ? C22B H22B 0.9500 . ? C23B C24B 1.412(6) . ? C23B H23B 0.9500 . ? C25B C30B 1.411(7) . ? C25B C26B 1.433(6) . ? C26B C27B 1.396(7) . ? C26B C31B 1.504(8) . ? C27B C28B 1.375(8) . ? C27B H27B 0.9500 . ? C28B C29B 1.384(7) . ? C28B C32B 1.511(8) . ? C29B C30B 1.395(7) . ? C29B H29B 0.9500 . ? C30B C33B 1.519(7) . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B C35B 1.421(6) . ? C34B C39B 1.422(6) . ? C35B C36B 1.398(7) . ? C35B C40B 1.515(7) . ? C36B C37B 1.374(7) . ? C36B H36B 0.9500 . ? C37B C38B 1.375(7) . ? C37B C41B 1.511(7) . ? C38B C39B 1.403(6) . ? C38B H38B 0.9500 . ? C39B C42B 1.503(7) . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B C44B 1.462(8) . ? C43B H43X 0.9900 . ? C43B H43Y 0.9900 . ? C44B C45B 1.478(9) . ? C44B H44X 0.9900 . ? C44B H44Y 0.9900 . ? C45B C46B 1.483(9) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B C48C 1.392(16) . ? C47B C48B 1.416(17) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C47B H47E 0.9900 . ? C47B H47F 0.9900 . ? C48B C49B 1.483(18) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49B C50B 1.430(15) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C48C C49C 1.501(19) . ? C48C H48E 0.9900 . ? C48C H48F 0.9900 . ? C49C C50B 1.285(15) . ? C49C H49E 0.9900 . ? C49C H49F 0.9900 . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? C50B H50E 0.9900 . ? C50B H50F 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 O1A K1A O2A 144.08(14) . . ? O1A K1A O3A 77.18(16) . . ? O2A K1A O3A 81.08(16) . . ? O1A K1A C15A 114.12(13) . . ? O2A K1A C15A 64.53(15) . . ? O3A K1A C15A 134.69(15) . . ? O1A K1A C14A 116.16(13) . . ? O2A K1A C14A 77.73(14) . . ? O3A K1A C14A 157.05(15) . . ? C15A K1A C14A 24.14(11) . . ? O1A K1A C16A 91.49(12) . . ? O2A K1A C16A 77.02(15) . . ? O3A K1A C16A 123.29(15) . . ? C15A K1A C16A 24.48(12) . . ? C14A K1A C16A 42.70(12) . . ? O1A K1A C13A 95.37(12) . . ? O2A K1A C13A 101.82(13) . . ? O3A K1A C13A 169.76(15) . . ? C15A K1A C13A 42.21(12) . . ? C14A K1A C13A 24.11(10) . . ? C16A K1A C13A 49.07(11) . . ? O1A K1A C3A 82.66(12) . . ? O2A K1A C3A 129.08(15) . . ? O3A K1A C3A 98.74(15) . . ? C15A K1A C3A 125.52(13) . . ? C14A K1A C3A 101.39(12) . . ? C16A K1A C3A 135.17(14) . . ? C13A K1A C3A 87.10(12) . . ? O1A K1A C2A 94.24(13) . . ? O2A K1A C2A 110.20(16) . . ? O3A K1A C2A 80.91(15) . . ? C15A K1A C2A 137.02(13) . . ? C14A K1A C2A 114.69(13) . . ? C16A K1A C2A 155.80(14) . . ? C13A K1A C2A 106.91(13) . . ? C3A K1A C2A 24.01(13) . . ? O1A K1A C17A 71.72(12) . . ? O2A K1A C17A 100.47(14) . . ? O3A K1A C17A 127.19(15) . . ? C15A K1A C17A 42.51(12) . . ? C14A K1A C17A 49.92(11) . . ? C16A K1A C17A 23.47(11) . . ? C13A K1A C17A 42.78(11) . . ? C3A K1A C17A 117.80(14) . . ? C2A K1A C17A 141.76(14) . . ? O1A K1A C18A 73.47(12) . . ? O2A K1A C18A 113.68(14) . . ? O3A K1A C18A 145.63(15) . . ? C15A K1A C18A 49.20(12) . . ? C14A K1A C18A 42.73(11) . . ? C16A K1A C18A 41.64(12) . . ? C13A K1A C18A 24.44(10) . . ? C3A K1A C18A 94.89(13) . . ? C2A K1A C18A 118.43(13) . . ? C17A K1A C18A 24.08(11) . . ? O1A K1A C4A 93.29(12) . . ? O2A K1A C4A 122.53(13) . . ? O3A K1A C4A 121.93(14) . . ? C15A K1A C4A 101.79(12) . . ? C14A K1A C4A 77.66(12) . . ? C16A K1A C4A 113.97(13) . . ? C13A K1A C4A 64.92(11) . . ? C3A K1A C4A 23.74(12) . . ? C2A K1A C4A 42.26(13) . . ? C17A K1A C4A 101.72(13) . . ? C18A K1A C4A 77.64(12) . . ? N2A Al1A N1A 95.63(17) . . ? N2A Al1A C34A 113.71(17) . . ? N1A Al1A C34A 114.30(18) . . ? N2A Al1A C25A 112.65(16) . . ? N1A Al1A C25A 113.95(17) . . ? C34A Al1A C25A 106.61(19) . . ? C43A O1A C46A 103.3(6) . . ? C43A O1A C43C 33.1(7) . . ? C46A O1A C43C 107.0(7) . . ? C43A O1A K1A 121.7(5) . . ? C46A O1A K1A 133.3(4) . . ? C43C O1A K1A 117.3(6) . . ? C47A O2A C50A 103.2(5) . . ? C47A O2A K1A 133.7(4) . . ? C50A O2A K1A 123.2(4) . . ? C52A O3A C53A 113.2(7) . . ? C52A O3A K1A 123.0(5) . . ? C53A O3A K1A 123.5(5) . . ? C12A N1A C5A 104.9(4) . . ? C12A N1A Al1A 134.3(3) . . ? C5A N1A Al1A 120.7(3) . . ? C24A N2A C13A 105.6(3) . . ? C24A N2A Al1A 132.2(3) . . ? C13A N2A Al1A 122.2(3) . . ? C2A C1A C6A 119.3(5) . . ? C2A C1A K1A 76.8(3) . . ? C6A C1A K1A 78.7(3) . . ? C2A C1A H1AA 120.2 . . ? C6A C1A H1AA 120.2 . . ? K1A C1A H1AA 120.2 . . ? C1A C2A C3A 120.0(5) . . ? C1A C2A K1A 79.6(3) . . ? C3A C2A K1A 77.5(3) . . ? C1A C2A H2AA 119.8 . . ? C3A C2A H2AA 119.8 . . ? K1A C2A H2AA 119.8 . . ? C4A C3A C2A 121.8(5) . . ? C4A C3A K1A 79.3(3) . . ? C2A C3A K1A 78.5(3) . . ? C4A C3A H3AA 118.9 . . ? C2A C3A H3AA 118.9 . . ? K1A C3A H3AA 118.9 . . ? C3A C4A C5A 118.8(5) . . ? C3A C4A K1A 77.0(3) . . ? C5A C4A K1A 78.4(3) . . ? C3A C4A H4AA 120.4 . . ? C5A C4A H4AA 120.4 . . ? K1A C4A H4AA 120.4 . . ? N1A C5A C4A 129.1(5) . . ? N1A C5A C6A 111.0(4) . . ? C4A C5A C6A 119.8(5) . . ? N1A C5A K1A 115.2(2) . . ? C4A C5A K1A 77.7(3) . . ? C6A C5A K1A 79.1(3) . . ? C5A C6A C1A 120.1(5) . . ? C5A C6A C7A 106.3(4) . . ? C1A C6A C7A 133.5(5) . . ? C5A C6A K1A 77.0(2) . . ? C1A C6A K1A 77.3(3) . . ? C7A C6A K1A 115.2(3) . . ? C12A C7A C8A 121.2(5) . . ? C12A C7A C6A 106.0(4) . . ? C8A C7A C6A 132.8(5) . . ? C9A C8A C7A 118.6(6) . . ? C9A C8A H8AA 120.7 . . ? C7A C8A H8AA 120.7 . . ? C8A C9A C10A 120.6(5) . . ? C8A C9A H9AA 119.7 . . ? C10A C9A H9AA 119.7 . . ? C11A C10A C9A 121.7(5) . . ? C11A C10A H10A 119.1 . . ? C9A C10A H10A 119.1 . . ? C10A C11A C12A 118.3(5) . . ? C10A C11A H11A 120.9 . . ? C12A C11A H11A 120.9 . . ? N1A C12A C7A 111.7(4) . . ? N1A C12A C11A 128.6(5) . . ? C7A C12A C11A 119.6(5) . . ? C14A C13A N2A 129.1(4) . . ? C14A C13A C18A 120.2(4) . . ? N2A C13A C18A 110.7(4) . . ? C14A C13A K1A 77.3(3) . . ? N2A C13A K1A 114.8(3) . . ? C18A C13A K1A 78.8(3) . . ? C15A C14A C13A 119.0(4) . . ? C15A C14A K1A 77.3(3) . . ? C13A C14A K1A 78.6(3) . . ? C15A C14A H14A 120.3 . . ? C13A C14A H14A 120.3 . . ? K1A C14A H14A 120.3 . . ? C14A C15A C16A 120.2(4) . . ? C14A C15A K1A 78.6(3) . . ? C16A C15A K1A 78.7(3) . . ? C14A C15A H15A 119.7 . . ? C16A C15A H15A 119.7 . . ? K1A C15A H15A 119.7 . . ? C17A C16A C15A 121.7(4) . . ? C17A C16A K1A 79.6(3) . . ? C15A C16A K1A 76.8(3) . . ? C17A C16A H16A 119.1 . . ? C15A C16A H16A 119.1 . . ? K1A C16A H16A 119.1 . . ? C16A C17A C18A 118.8(4) . . ? C16A C17A K1A 77.0(3) . . ? C18A C17A K1A 78.1(3) . . ? C16A C17A H17A 120.4 . . ? C18A C17A H17A 120.4 . . ? K1A C17A H17A 120.4 . . ? C17A C18A C13A 120.0(4) . . ? C17A C18A C19A 133.6(4) . . ? C13A C18A C19A 106.4(4) . . ? C17A C18A K1A 77.8(3) . . ? C13A C18A K1A 76.7(3) . . ? C19A C18A K1A 114.7(3) . . ? C20A C19A C24A 120.0(4) . . ? C20A C19A C18A 134.1(4) . . ? C24A C19A C18A 105.9(4) . . ? C21A C20A C19A 120.0(4) . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C20A C21A C22A 120.3(4) . . ? C20A C21A H21A 119.9 . . ? C22A C21A H21A 119.9 . . ? C23A C22A C21A 121.6(4) . . ? C23A C22A H22A 119.2 . . ? C21A C22A H22A 119.2 . . ? C22A C23A C24A 118.3(4) . . ? C22A C23A H23A 120.8 . . ? C24A C23A H23A 120.8 . . ? N2A C24A C23A 128.8(4) . . ? N2A C24A C19A 111.4(4) . . ? C23A C24A C19A 119.8(4) . . ? C26A C25A C30A 115.9(4) . . ? C26A C25A Al1A 117.4(3) . . ? C30A C25A Al1A 126.2(3) . . ? C27A C26A C25A 121.6(4) . . ? C27A C26A C31A 116.3(5) . . ? C25A C26A C31A 122.1(4) . . ? C28A C27A C26A 121.3(5) . . ? C28A C27A H27A 119.4 . . ? C26A C27A H27A 119.4 . . ? C29A C28A C27A 117.9(4) . . ? C29A C28A C32A 121.9(5) . . ? C27A C28A C32A 120.1(5) . . ? C28A C29A C30A 122.7(4) . . ? C28A C29A H29A 118.7 . . ? C30A C29A H29A 118.7 . . ? C29A C30A C25A 120.6(4) . . ? C29A C30A C33A 115.8(4) . . ? C25A C30A C33A 123.6(4) . . ? C26A C31A H31A 109.5 . . ? C26A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C26A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C28A C32A H32A 109.5 . . ? C28A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C28A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30A C33A H33A 109.5 . . ? C30A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C30A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C39A C34A C35A 115.2(4) . . ? C39A C34A Al1A 117.6(3) . . ? C35A C34A Al1A 126.2(3) . . ? C36A C35A C34A 121.4(4) . . ? C36A C35A C40A 116.1(4) . . ? C34A C35A C40A 122.5(4) . . ? C37A C36A C35A 122.6(4) . . ? C37A C36A H36A 118.7 . . ? C35A C36A H36A 118.7 . . ? C38A C37A C36A 116.6(5) . . ? C38A C37A C41A 123.0(5) . . ? C36A C37A C41A 120.4(5) . . ? C37A C38A C39A 122.5(5) . . ? C37A C38A H38A 118.7 . . ? C39A C38A H38A 118.7 . . ? C38A C39A C34A 121.6(4) . . ? C38A C39A C42A 117.0(4) . . ? C34A C39A C42A 121.4(4) . . ? C35A C40A H40A 109.5 . . ? C35A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C35A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? C37A C41A H41A 109.5 . . ? C37A C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? C37A C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C39A C42A H42A 109.5 . . ? C39A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C39A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? O1A C43A C44A 101.5(8) . . ? O1A C43A H43A 111.5 . . ? C44A C43A H43A 111.5 . . ? O1A C43A H43B 111.5 . . ? C44A C43A H43B 111.5 . . ? H43A C43A H43B 109.3 . . ? O1A C43C C44A 106.3(9) . . ? O1A C43C H43C 110.5 . . ? C44A C43C H43C 110.5 . . ? O1A C43C H43D 110.5 . . ? C44A C43C H43D 110.5 . . ? H43C C43C H43D 108.7 . . ? C45A C44A C43C 103.3(7) . . ? C45A C44A C43A 106.3(6) . . ? C43C C44A C43A 30.3(7) . . ? C45A C44A H44A 110.5 . . ? C43C C44A H44A 135.8 . . ? C43A C44A H44A 110.5 . . ? C45A C44A H44B 110.5 . . ? C43C C44A H44B 84.1 . . ? C43A C44A H44B 110.5 . . ? H44A C44A H44B 108.7 . . ? C45A C44A H44C 111.1 . . ? C43C C44A H44C 111.1 . . ? C43A C44A H44C 82.4 . . ? H44A C44A H44C 29.8 . . ? H44B C44A H44C 130.3 . . ? C45A C44A H44D 111.1 . . ? C43C C44A H44D 111.1 . . ? C43A C44A H44D 132.7 . . ? H44A C44A H44D 82.5 . . ? H44B C44A H44D 28.5 . . ? H44C C44A H44D 109.1 . . ? C44A C45A C46A 101.9(5) . . ? C44A C45A H45A 111.4 . . ? C46A C45A H45A 111.4 . . ? C44A C45A H45B 111.4 . . ? C46A C45A H45B 111.4 . . ? H45A C45A H45B 109.2 . . ? O1A C46A C45A 106.7(5) . . ? O1A C46A H46A 110.4 . . ? C45A C46A H46A 110.4 . . ? O1A C46A H46B 110.4 . . ? C45A C46A H46B 110.4 . . ? H46A C46A H46B 108.6 . . ? O2A C47A C48A 106.0(6) . . ? O2A C47A H47A 110.5 . . ? C48A C47A H47A 110.5 . . ? O2A C47A H47B 110.5 . . ? C48A C47A H47B 110.5 . . ? H47A C47A H47B 108.7 . . ? C47A C48A C49A 105.2(6) . . ? C47A C48A H48A 110.7 . . ? C49A C48A H48A 110.7 . . ? C47A C48A H48B 110.7 . . ? C49A C48A H48B 110.7 . . ? H48A C48A H48B 108.8 . . ? C48A C49A C50A 103.8(6) . . ? C48A C49A H49A 111.0 . . ? C50A C49A H49A 111.0 . . ? C48A C49A H49B 111.0 . . ? C50A C49A H49B 111.0 . . ? H49A C49A H49B 109.0 . . ? O2A C50A C49A 105.4(6) . . ? O2A C50A H50A 110.7 . . ? C49A C50A H50A 110.7 . . ? O2A C50A H50B 110.7 . . ? C49A C50A H50B 110.7 . . ? H50A C50A H50B 108.8 . . ? C52A C51A H51A 109.5 . . ? C52A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C52A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? O3A C52A C51A 112.4(8) . . ? O3A C52A H52A 109.1 . . ? C51A C52A H52A 109.1 . . ? O3A C52A H52B 109.1 . . ? C51A C52A H52B 109.1 . . ? H52A C52A H52B 107.8 . . ? O3A C53A C54A 102.8(8) . . ? O3A C53A H53A 111.2 . . ? C54A C53A H53A 111.2 . . ? O3A C53A H53B 111.2 . . ? C54A C53A H53B 111.2 . . ? H53A C53A H53B 109.1 . . ? C53A C54A H54A 109.5 . . ? C53A C54A H54B 109.5 . . ? H54A C54A H54B 109.5 . . ? C53A C54A H54C 109.5 . . ? H54A C54A H54C 109.5 . . ? H54B C54A H54C 109.5 . . ? O2B K1B O1B 94.44(15) . . ? O2B K1B C9B 118.02(16) . . ? O1B K1B C9B 91.19(14) . . ? O2B K1B C18B 85.88(16) . . ? O1B K1B C18B 135.33(13) . . ? C9B K1B C18B 127.76(14) . . ? O2B K1B C10B 115.96(15) . . ? O1B K1B C10B 116.70(14) . . ? C9B K1B C10B 25.78(13) . . ? C18B K1B C10B 102.74(14) . . ? O2B K1B C8B 136.70(16) . . ? O1B K1B C8B 74.31(13) . . ? C9B K1B C8B 25.39(12) . . ? C18B K1B C8B 131.45(14) . . ? C10B K1B C8B 44.94(13) . . ? O2B K1B C17B 70.80(17) . . ? O1B K1B C17B 114.12(13) . . ? C9B K1B C17B 153.18(14) . . ? C18B K1B C17B 25.59(12) . . ? C10B K1B C17B 127.66(14) . . ? C8B K1B C17B 152.09(14) . . ? O2B K1B C13B 111.34(16) . . ? O1B K1B C13B 127.24(13) . . ? C9B K1B C13B 113.13(13) . . ? C18B K1B C13B 25.55(13) . . ? C10B K1B C13B 92.79(13) . . ? C8B K1B C13B 108.38(13) . . ? C17B K1B C13B 44.59(13) . . ? O2B K1B C11B 130.89(14) . . ? O1B K1B C11B 125.38(14) . . ? C9B K1B C11B 44.79(13) . . ? C18B K1B C11B 83.80(13) . . ? C10B K1B C11B 24.87(13) . . ? C8B K1B C11B 52.31(13) . . ? C17B K1B C11B 109.32(13) . . ? C13B K1B C11B 69.12(12) . . ? O2B K1B C7B 161.68(16) . . ? O1B K1B C7B 82.56(13) . . ? C9B K1B C7B 44.34(13) . . ? C18B K1B C7B 108.98(13) . . ? C10B K1B C7B 51.50(13) . . ? C8B K1B C7B 25.27(12) . . ? C17B K1B C7B 126.90(14) . . ? C13B K1B C7B 84.31(12) . . ? C11B K1B C7B 44.40(12) . . ? O2B K1B C12B 155.83(13) . . ? O1B K1B C12B 106.72(13) . . ? C9B K1B C12B 51.56(13) . . ? C18B K1B C12B 87.06(13) . . ? C10B K1B C12B 43.79(13) . . ? C8B K1B C12B 44.41(12) . . ? C17B K1B C12B 109.31(13) . . ? C13B K1B C12B 64.72(12) . . ? C11B K1B C12B 25.09(11) . . ? C7B K1B C12B 24.97(11) . . ? O2B K1B C16B 81.62(17) . . ? O1B K1B C16B 92.14(13) . . ? C9B K1B C16B 159.75(15) . . ? C18B K1B C16B 43.61(12) . . ? C10B K1B C16B 143.14(14) . . ? C8B K1B C16B 139.11(14) . . ? C17B K1B C16B 24.34(12) . . ? C13B K1B C16B 50.42(12) . . ? C11B K1B C16B 119.33(13) . . ? C7B K1B C16B 116.47(14) . . ? C12B K1B C16B 108.50(13) . . ? N1B Al1B N2B 96.13(17) . . ? N1B Al1B C34B 114.46(18) . . ? N2B Al1B C34B 111.89(19) . . ? N1B Al1B C25B 112.27(17) . . ? N2B Al1B C25B 115.82(19) . . ? C34B Al1B C25B 106.4(2) . . ? C43B O1B C46B 108.3(5) . . ? C43B O1B K1B 115.3(3) . . ? C46B O1B K1B 133.7(4) . . ? C47B O2B C50B 107.0(6) . . ? C47B O2B K1B 141.4(5) . . ? C50B O2B K1B 110.2(5) . . ? C12B N1B C1B 104.7(3) . . ? C12B N1B Al1B 121.5(3) . . ? C1B N1B Al1B 132.8(3) . . ? C13B N2B C24B 104.4(4) . . ? C13B N2B Al1B 122.1(3) . . ? C24B N2B Al1B 133.0(3) . . ? N1B C1B C2B 128.5(4) . . ? N1B C1B C6B 111.3(4) . . ? C2B C1B C6B 120.2(4) . . ? C3B C2B C1B 118.2(5) . . ? C3B C2B H2BA 120.9 . . ? C1B C2B H2BA 120.9 . . ? C2B C3B C4B 121.6(5) . . ? C2B C3B H3BA 119.2 . . ? C4B C3B H3BA 119.2 . . ? C5B C4B C3B 120.9(4) . . ? C5B C4B H4BA 119.6 . . ? C3B C4B H4BA 119.6 . . ? C4B C5B C6B 118.9(4) . . ? C4B C5B H5BA 120.5 . . ? C6B C5B H5BA 120.5 . . ? C5B C6B C1B 120.3(4) . . ? C5B C6B C7B 133.4(4) . . ? C1B C6B C7B 106.3(4) . . ? C8B C7B C12B 120.0(4) . . ? C8B C7B C6B 134.0(4) . . ? C12B C7B C6B 106.0(4) . . ? C8B C7B K1B 74.3(3) . . ? C12B C7B K1B 78.7(3) . . ? C6B C7B K1B 116.4(3) . . ? C9B C8B C7B 119.3(4) . . ? C9B C8B K1B 75.3(3) . . ? C7B C8B K1B 80.4(3) . . ? C9B C8B H8BA 120.4 . . ? C7B C8B H8BA 120.4 . . ? K1B C8B H8BA 114.5 . . ? C8B C9B C10B 120.5(5) . . ? C8B C9B K1B 79.3(3) . . ? C10B C9B K1B 78.3(3) . . ? C8B C9B H9BA 119.8 . . ? C10B C9B H9BA 119.8 . . ? K1B C9B H9BA 113.1 . . ? C11B C10B C9B 121.6(5) . . ? C11B C10B K1B 81.0(3) . . ? C9B C10B K1B 76.0(3) . . ? C11B C10B H10B 119.2 . . ? C9B C10B H10B 119.2 . . ? K1B C10B H10B 114.1 . . ? C10B C11B C12B 118.5(4) . . ? C10B C11B K1B 74.1(3) . . ? C12B C11B K1B 79.1(3) . . ? C10B C11B H11B 120.8 . . ? C12B C11B H11B 120.8 . . ? K1B C11B H11B 116.9 . . ? N1B C12B C7B 111.7(4) . . ? N1B C12B C11B 128.1(4) . . ? C7B C12B C11B 120.1(4) . . ? N1B C12B K1B 118.6(3) . . ? C7B C12B K1B 76.3(3) . . ? C11B C12B K1B 75.8(3) . . ? N2B C13B C18B 111.7(4) . . ? N2B C13B C14B 128.0(5) . . ? C18B C13B C14B 120.4(4) . . ? N2B C13B K1B 112.2(3) . . ? C18B C13B K1B 73.1(3) . . ? C14B C13B K1B 83.7(3) . . ? C15B C14B C13B 117.8(5) . . ? C15B C14B K1B 78.6(3) . . ? C13B C14B K1B 71.8(3) . . ? C15B C14B H14B 121.1 . . ? C13B C14B H14B 121.1 . . ? K1B C14B H14B 119.5 . . ? C14B C15B C16B 121.8(5) . . ? C14B C15B K1B 77.7(3) . . ? C16B C15B K1B 74.6(3) . . ? C14B C15B H15B 119.1 . . ? C16B C15B H15B 119.1 . . ? K1B C15B H15B 119.5 . . ? C17B C16B C15B 120.2(5) . . ? C17B C16B K1B 72.7(3) . . ? C15B C16B K1B 81.3(3) . . ? C17B C16B H16B 119.9 . . ? C15B C16B H16B 119.9 . . ? K1B C16B H16B 116.8 . . ? C16B C17B C18B 119.6(5) . . ? C16B C17B K1B 83.0(3) . . ? C18B C17B K1B 75.0(3) . . ? C16B C17B H17B 120.2 . . ? C18B C17B H17B 120.2 . . ? K1B C17B H17B 112.3 . . ? C17B C18B C13B 120.2(4) . . ? C17B C18B C19B 133.6(5) . . ? C13B C18B C19B 106.2(4) . . ? C17B C18B K1B 79.4(3) . . ? C13B C18B K1B 81.4(3) . . ? C19B C18B K1B 107.7(3) . . ? C20B C19B C24B 121.0(5) . . ? C20B C19B C18B 133.2(5) . . ? C24B C19B C18B 105.8(4) . . ? C21B C20B C19B 118.7(6) . . ? C21B C20B H20B 120.7 . . ? C19B C20B H20B 120.7 . . ? C20B C21B C22B 120.2(6) . . ? C20B C21B H21B 119.9 . . ? C22B C21B H21B 119.9 . . ? C23B C22B C21B 122.5(5) . . ? C23B C22B H22B 118.7 . . ? C21B C22B H22B 118.7 . . ? C22B C23B C24B 118.5(6) . . ? C22B C23B H23B 120.7 . . ? C24B C23B H23B 120.7 . . ? N2B C24B C23B 129.0(5) . . ? N2B C24B C19B 111.8(4) . . ? C23B C24B C19B 119.1(5) . . ? C30B C25B C26B 116.0(5) . . ? C30B C25B Al1B 116.7(3) . . ? C26B C25B Al1B 126.7(4) . . ? C27B C26B C25B 120.4(5) . . ? C27B C26B C31B 116.8(5) . . ? C25B C26B C31B 122.8(5) . . ? C28B C27B C26B 122.7(5) . . ? C28B C27B H27B 118.6 . . ? C26B C27B H27B 118.6 . . ? C27B C28B C29B 117.5(5) . . ? C27B C28B C32B 120.6(5) . . ? C29B C28B C32B 121.9(6) . . ? C28B C29B C30B 122.0(6) . . ? C28B C29B H29B 119.0 . . ? C30B C29B H29B 119.0 . . ? C29B C30B C25B 121.5(5) . . ? C29B C30B C33B 116.3(5) . . ? C25B C30B C33B 122.2(5) . . ? C26B C31B H31D 109.5 . . ? C26B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C26B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C28B C32B H32D 109.5 . . ? C28B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C28B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C30B C33B H33D 109.5 . . ? C30B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C30B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C35B C34B C39B 115.6(4) . . ? C35B C34B Al1B 116.4(3) . . ? C39B C34B Al1B 127.8(3) . . ? C36B C35B C34B 121.6(5) . . ? C36B C35B C40B 117.5(4) . . ? C34B C35B C40B 120.8(4) . . ? C37B C36B C35B 122.2(5) . . ? C37B C36B H36B 118.9 . . ? C35B C36B H36B 118.9 . . ? C36B C37B C38B 116.9(4) . . ? C36B C37B C41B 121.6(5) . . ? C38B C37B C41B 121.5(5) . . ? C37B C38B C39B 123.3(5) . . ? C37B C38B H38B 118.3 . . ? C39B C38B H38B 118.3 . . ? C38B C39B C34B 120.3(4) . . ? C38B C39B C42B 116.7(4) . . ? C34B C39B C42B 123.1(4) . . ? C35B C40B H40D 109.5 . . ? C35B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C35B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C37B C41B H41D 109.5 . . ? C37B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C37B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C39B C42B H42D 109.5 . . ? C39B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C39B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? O1B C43B C44B 109.3(6) . . ? O1B C43B K1B 43.6(3) . . ? C44B C43B K1B 152.8(5) . . ? O1B C43B H43X 109.8 . . ? C44B C43B H43X 109.8 . . ? K1B C43B H43X 84.1 . . ? O1B C43B H43Y 109.8 . . ? C44B C43B H43Y 109.8 . . ? K1B C43B H43Y 86.3 . . ? H43X C43B H43Y 108.3 . . ? C43B C44B C45B 106.5(6) . . ? C43B C44B H44X 110.4 . . ? C45B C44B H44X 110.4 . . ? C43B C44B H44Y 110.4 . . ? C45B C44B H44Y 110.4 . . ? H44X C44B H44Y 108.6 . . ? C44B C45B C46B 105.1(5) . . ? C44B C45B H45C 110.7 . . ? C46B C45B H45C 110.7 . . ? C44B C45B H45D 110.7 . . ? C46B C45B H45D 110.7 . . ? H45C C45B H45D 108.8 . . ? O1B C46B C45B 108.5(5) . . ? O1B C46B H46C 110.0 . . ? C45B C46B H46C 110.0 . . ? O1B C46B H46D 110.0 . . ? C45B C46B H46D 110.0 . . ? H46C C46B H46D 108.4 . . ? C48C C47B C48B 50.5(9) . . ? C48C C47B O2B 103.7(9) . . ? C48B C47B O2B 106.7(9) . . ? C48C C47B H47C 145.1 . . ? C48B C47B H47C 110.4 . . ? O2B C47B H47C 110.4 . . ? C48C C47B H47D 64.5 . . ? C48B C47B H47D 110.4 . . ? O2B C47B H47D 110.4 . . ? H47C C47B H47D 108.6 . . ? C48C C47B H47E 111.0 . . ? C48B C47B H47E 63.0 . . ? O2B C47B H47E 111.0 . . ? H47C C47B H47E 49.4 . . ? H47D C47B H47E 138.1 . . ? C48C C47B H47F 111.0 . . ? C48B C47B H47F 141.5 . . ? O2B C47B H47F 111.0 . . ? H47C C47B H47F 63.4 . . ? H47D C47B H47F 48.2 . . ? H47E C47B H47F 109.0 . . ? C47B C48B C49B 105.1(12) . . ? C47B C48B H48C 110.7 . . ? C49B C48B H48C 110.7 . . ? C47B C48B H48D 110.7 . . ? C49B C48B H48D 110.7 . . ? H48C C48B H48D 108.8 . . ? C50B C49B C48B 108.4(12) . . ? C50B C49B H49C 110.0 . . ? C48B C49B H49C 110.0 . . ? C50B C49B H49D 110.0 . . ? C48B C49B H49D 110.0 . . ? H49C C49B H49D 108.4 . . ? C47B C48C C49C 106.1(12) . . ? C47B C48C H48E 110.5 . . ? C49C C48C H48E 110.5 . . ? C47B C48C H48F 110.5 . . ? C49C C48C H48F 110.5 . . ? H48E C48C H48F 108.7 . . ? C50B C49C C48C 106.9(12) . . ? C50B C49C H49E 110.4 . . ? C48C C49C H49E 110.4 . . ? C50B C49C H49F 110.3 . . ? C48C C49C H49F 110.4 . . ? H49E C49C H49F 108.6 . . ? C49C C50B C49B 60.8(9) . . ? C49C C50B O2B 104.2(10) . . ? C49B C50B O2B 104.3(8) . . ? C49C C50B K1B 130.9(9) . . ? C49B C50B K1B 147.5(7) . . ? O2B C50B K1B 46.4(4) . . ? C49C C50B H50C 54.0 . . ? C49B C50B H50C 110.9 . . ? O2B C50B H50C 110.9 . . ? K1B C50B H50C 95.5 . . ? C49C C50B H50D 144.8 . . ? C49B C50B H50D 110.9 . . ? O2B C50B H50D 110.9 . . ? K1B C50B H50D 76.0 . . ? H50C C50B H50D 108.9 . . ? C49C C50B H50E 110.9 . . ? C49B C50B H50E 144.7 . . ? O2B C50B H50E 110.9 . . ? K1B C50B H50E 65.8 . . ? H50C C50B H50E 58.4 . . ? H50D C50B H50E 54.1 . . ? C49C C50B H50F 110.9 . . ? C49B C50B H50F 53.9 . . ? O2B C50B H50F 110.9 . . ? K1B C50B H50F 116.3 . . ? H50C C50B H50F 138.0 . . ? H50D C50B H50F 58.4 . . ? H50E C50B H50F 108.9 . . ? _diffrn_measured_fraction_theta_max 0.716 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.716 _refine_diff_density_max 0.731 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.066 #==== END data_FO3520 _database_code_depnum_ccdc_archive 'CCDC 765645' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H56 O7 Sr, 2(C24 H20 Al), C4 H8 O' _chemical_formula_sum 'C80 H104 Al2 O8 Sr' _chemical_formula_weight 1335.21 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' Al Al 0.0645 0.0514 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.4995(4) _cell_length_b 18.2740(3) _cell_length_c 18.9071(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.464(1) _cell_angle_gamma 90.00 _cell_volume 7428.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 52349 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52349 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16953 _reflns_number_gt 10094 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0960P)^2^+6.4799P] 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 16953 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2034 _refine_ls_wR_factor_gt 0.1663 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.745473(16) -0.028495(19) 0.249311(18) 0.03538(11) Uani 1 1 d . A . O1 O 0.65854(15) -0.0144(2) 0.15569(19) 0.0708(10) Uani 1 1 d . . . O2 O 0.69998(13) -0.15779(16) 0.24842(16) 0.0497(7) Uani 1 1 d . . . O3 O 0.80277(14) -0.00184(17) 0.13422(14) 0.0506(7) Uani 1 1 d . . . O4 O 0.80532(15) -0.00945(17) 0.36645(15) 0.0541(8) Uani 1 1 d . . . O5 O 0.84073(12) -0.11225(15) 0.24213(15) 0.0458(7) Uani 1 1 d . . . O6 O 0.74004(13) 0.11076(16) 0.25176(18) 0.0559(8) Uani 1 1 d . . . O7 O 0.65630(16) -0.02062(18) 0.33984(18) 0.0641(9) Uani 1 1 d . . . C49 C 0.5914(5) -0.0220(8) 0.1691(7) 0.068(4) Uiso 0.477(17) 1 d P A 1 H49A H 0.5815 -0.0738 0.1796 0.082 Uiso 0.477(17) 1 calc PR A 1 H49B H 0.5798 0.0080 0.2105 0.082 Uiso 0.477(17) 1 calc PR A 1 C49A C 0.6025(4) -0.0577(5) 0.1386(5) 0.046(3) Uiso 0.523(17) 1 d P A 2 H49C H 0.5856 -0.0817 0.1813 0.055 Uiso 0.523(17) 1 calc PR A 2 H49D H 0.6112 -0.0954 0.1024 0.055 Uiso 0.523(17) 1 calc PR A 2 C50 C 0.5583(3) 0.0006(4) 0.1103(4) 0.0863(19) Uani 1 1 d . . . H50A H 0.5182 0.0232 0.1238 0.104 Uiso 0.477(17) 1 calc PR A 1 H50B H 0.5500 -0.0407 0.0777 0.104 Uiso 0.477(17) 1 calc PR A 1 H50C H 0.5292 -0.0202 0.0747 0.104 Uiso 0.523(17) 1 calc PR A 2 H50D H 0.5339 0.0228 0.1490 0.104 Uiso 0.523(17) 1 calc PR A 2 C51 C 0.6014(3) 0.0567(4) 0.0768(4) 0.098(2) Uani 1 1 d . A . H51A H 0.5950 0.0584 0.0249 0.118 Uiso 1 1 calc R . . H51B H 0.5937 0.1061 0.0965 0.118 Uiso 1 1 calc R . . C52 C 0.6645(3) 0.0319(4) 0.0942(3) 0.0832(19) Uani 1 1 d . A . H52A H 0.6824 0.0041 0.0543 0.100 Uiso 1 1 calc R . . H52B H 0.6919 0.0741 0.1048 0.100 Uiso 1 1 calc R . . C53 C 0.6888(2) -0.2045(3) 0.3087(3) 0.0614(12) Uani 1 1 d . A . H53A H 0.6802 -0.1750 0.3514 0.074 Uiso 1 1 calc R . . H53B H 0.7252 -0.2362 0.3183 0.074 Uiso 1 1 calc R . . C54 C 0.6322(3) -0.2502(3) 0.2879(4) 0.0828(17) Uani 1 1 d . . . H54A H 0.6377 -0.3017 0.3031 0.099 Uiso 1 1 calc R A . H54B H 0.5941 -0.2305 0.3100 0.099 Uiso 1 1 calc R . . C55 C 0.6280(3) -0.2452(4) 0.2102(3) 0.0866(19) Uani 1 1 d . A . H55A H 0.5893 -0.2199 0.1956 0.104 Uiso 1 1 calc R . . H55B H 0.6284 -0.2946 0.1887 0.104 Uiso 1 1 calc R . . C56 C 0.6839(3) -0.2023(3) 0.1879(3) 0.0685(14) Uani 1 1 d . A . H56A H 0.7187 -0.2354 0.1757 0.082 Uiso 1 1 calc R . . H56B H 0.6740 -0.1712 0.1464 0.082 Uiso 1 1 calc R . . C57 C 0.8084(3) -0.0601(3) 0.0824(3) 0.0653(13) Uani 1 1 d . A . H57A H 0.7685 -0.0867 0.0771 0.078 Uiso 1 1 calc R . . H57B H 0.8411 -0.0953 0.0969 0.078 Uiso 1 1 calc R . . C58 C 0.8255(3) -0.0230(3) 0.0143(3) 0.0715(15) Uani 1 1 d . . . H58A H 0.7881 -0.0053 -0.0114 0.086 Uiso 1 1 calc R A . H58B H 0.8493 -0.0562 -0.0168 0.086 Uiso 1 1 calc R . . C59 C 0.8650(3) 0.0397(3) 0.0403(3) 0.0734(16) Uani 1 1 d . A . H59A H 0.9084 0.0237 0.0491 0.088 Uiso 1 1 calc R . . H59B H 0.8651 0.0803 0.0057 0.088 Uiso 1 1 calc R . . C60 C 0.8345(2) 0.0626(3) 0.1080(3) 0.0599(12) Uani 1 1 d . A . H60A H 0.8661 0.0797 0.1427 0.072 Uiso 1 1 calc R . . H60B H 0.8045 0.1027 0.0992 0.072 Uiso 1 1 calc R . . C61 C 0.8135(4) -0.0728(3) 0.4105(3) 0.094(2) Uani 1 1 d . A . H61A H 0.8334 -0.1130 0.3838 0.112 Uiso 1 1 calc R . . H61B H 0.7730 -0.0902 0.4284 0.112 Uiso 1 1 calc R . . C62 C 0.8542(5) -0.0484(4) 0.4698(4) 0.129(3) Uani 1 1 d . . . H62A H 0.8420 -0.0727 0.5144 0.155 Uiso 1 1 calc R A . H62B H 0.8982 -0.0604 0.4600 0.155 Uiso 1 1 calc R . . C63 C 0.8460(4) 0.0290(4) 0.4751(3) 0.093(2) Uani 1 1 d . A . H63A H 0.8845 0.0528 0.4926 0.112 Uiso 1 1 calc R . . H63B H 0.8116 0.0409 0.5077 0.112 Uiso 1 1 calc R . . C64 C 0.8310(3) 0.0535(3) 0.4022(2) 0.0598(12) Uani 1 1 d . A . H64A H 0.8004 0.0939 0.4030 0.072 Uiso 1 1 calc R . . H64B H 0.8689 0.0707 0.3780 0.072 Uiso 1 1 calc R . . C65 C 0.8475(2) -0.1899(2) 0.2304(3) 0.0572(12) Uani 1 1 d . A . H65A H 0.8236 -0.2052 0.1880 0.069 Uiso 1 1 calc R . . H65B H 0.8323 -0.2177 0.2718 0.069 Uiso 1 1 calc R . . C66 C 0.9155(2) -0.2032(3) 0.2201(3) 0.0722(15) Uani 1 1 d . . . H66A H 0.9261 -0.2025 0.1692 0.087 Uiso 1 1 calc R A . H66B H 0.9282 -0.2508 0.2405 0.087 Uiso 1 1 calc R . . C67 C 0.9462(2) -0.1411(3) 0.2584(3) 0.0667(14) Uani 1 1 d . A . H67A H 0.9880 -0.1308 0.2393 0.080 Uiso 1 1 calc R . . H67B H 0.9498 -0.1513 0.3097 0.080 Uiso 1 1 calc R . . C68 C 0.9022(2) -0.0792(3) 0.2441(3) 0.0631(13) Uani 1 1 d . A . H68A H 0.9050 -0.0420 0.2821 0.076 Uiso 1 1 calc R . . H68B H 0.9117 -0.0555 0.1983 0.076 Uiso 1 1 calc R . . C69 C 0.7875(2) 0.1666(3) 0.2549(3) 0.0556(11) Uani 1 1 d . A . H69A H 0.7970 0.1850 0.2070 0.067 Uiso 1 1 calc R . . H69B H 0.8261 0.1472 0.2767 0.067 Uiso 1 1 calc R . . C70 C 0.7600(2) 0.2265(3) 0.3000(3) 0.0664(13) Uani 1 1 d . . . H70A H 0.7719 0.2201 0.3503 0.080 Uiso 1 1 calc R A . H70B H 0.7738 0.2753 0.2839 0.080 Uiso 1 1 calc R . . C71 C 0.6908(3) 0.2173(4) 0.2897(4) 0.094(2) Uani 1 1 d . A . H71A H 0.6697 0.2151 0.3360 0.113 Uiso 1 1 calc R . . H71B H 0.6735 0.2590 0.2624 0.113 Uiso 1 1 calc R . . C72 C 0.6821(3) 0.1505(3) 0.2518(5) 0.100(2) Uani 1 1 d . A . H72A H 0.6687 0.1610 0.2026 0.120 Uiso 1 1 calc R . . H72B H 0.6494 0.1208 0.2746 0.120 Uiso 1 1 calc R . . C73 C 0.6520(3) 0.0247(4) 0.3994(4) 0.096(2) Uani 1 1 d . A . H73A H 0.6287 0.0699 0.3878 0.116 Uiso 1 1 calc R . . H73B H 0.6939 0.0383 0.4170 0.116 Uiso 1 1 calc R . . C74 C 0.6179(4) -0.0197(4) 0.4537(3) 0.100(2) Uani 1 1 d . . . H74A H 0.6473 -0.0482 0.4833 0.120 Uiso 1 1 calc R A . H74B H 0.5928 0.0123 0.4847 0.120 Uiso 1 1 calc R . . C75 C 0.5778(3) -0.0684(4) 0.4122(3) 0.0889(19) Uani 1 1 d . A . H75A H 0.5333 -0.0577 0.4206 0.107 Uiso 1 1 calc R . . H75B H 0.5861 -0.1203 0.4238 0.107 Uiso 1 1 calc R . . C76 C 0.5953(3) -0.0514(4) 0.3371(3) 0.0777(16) Uani 1 1 d . A . H76A H 0.5951 -0.0966 0.3082 0.093 Uiso 1 1 calc R . . H76B H 0.5655 -0.0162 0.3159 0.093 Uiso 1 1 calc R . . Al1 Al 0.53319(5) 0.24117(7) 0.46638(6) 0.0438(3) Uani 1 1 d . . . C1 C 0.59563(18) 0.3149(2) 0.4326(2) 0.0423(9) Uani 1 1 d . . . C2 C 0.65793(19) 0.3152(2) 0.4556(2) 0.0498(10) Uani 1 1 d . . . H2A H 0.6709 0.2794 0.4890 0.060 Uiso 1 1 calc R . . C3 C 0.7013(2) 0.3655(3) 0.4319(3) 0.0567(11) Uani 1 1 d . . . H3A H 0.7431 0.3631 0.4485 0.068 Uiso 1 1 calc R . . C4 C 0.6842(2) 0.4182(3) 0.3849(3) 0.0609(12) Uani 1 1 d . . . H4A H 0.7138 0.4529 0.3689 0.073 Uiso 1 1 calc R . . C5 C 0.6242(2) 0.4210(3) 0.3611(2) 0.0586(12) Uani 1 1 d . . . H5A H 0.6119 0.4580 0.3285 0.070 Uiso 1 1 calc R . . C6 C 0.5809(2) 0.3696(3) 0.3843(2) 0.0512(11) Uani 1 1 d . . . H6A H 0.5396 0.3721 0.3664 0.061 Uiso 1 1 calc R . . C7 C 0.56935(19) 0.1901(2) 0.5509(2) 0.0454(9) Uani 1 1 d . . . C8 C 0.5443(2) 0.1952(3) 0.6188(2) 0.0600(12) Uani 1 1 d . . . H8A H 0.5070 0.2223 0.6251 0.072 Uiso 1 1 calc R . . C9 C 0.5720(3) 0.1620(3) 0.6777(3) 0.0737(15) Uani 1 1 d . . . H9A H 0.5540 0.1677 0.7231 0.088 Uiso 1 1 calc R . . C10 C 0.6243(3) 0.1220(3) 0.6704(3) 0.0700(15) Uani 1 1 d . . . H10A H 0.6425 0.0989 0.7106 0.084 Uiso 1 1 calc R . . C11 C 0.6510(2) 0.1145(3) 0.6061(3) 0.0633(13) Uani 1 1 d . . . H11A H 0.6880 0.0865 0.6010 0.076 Uiso 1 1 calc R . . C12 C 0.6235(2) 0.1485(3) 0.5471(2) 0.0531(11) Uani 1 1 d . . . H12A H 0.6427 0.1430 0.5024 0.064 Uiso 1 1 calc R . . C13 C 0.45312(19) 0.2904(3) 0.4961(2) 0.0493(10) Uani 1 1 d . . . C14 C 0.4525(3) 0.3546(3) 0.5343(3) 0.0774(16) Uani 1 1 d . . . H14A H 0.4911 0.3771 0.5459 0.093 Uiso 1 1 calc R . . C15 C 0.3976(3) 0.3881(4) 0.5570(4) 0.0893(19) Uani 1 1 d . . . H15A H 0.3997 0.4326 0.5829 0.107 Uiso 1 1 calc R . . C16 C 0.3417(3) 0.3577(4) 0.5422(3) 0.0761(17) Uani 1 1 d . . . H16A H 0.3043 0.3801 0.5574 0.091 Uiso 1 1 calc R . . C17 C 0.3405(2) 0.2937(4) 0.5049(3) 0.0781(17) Uani 1 1 d . . . H17A H 0.3016 0.2712 0.4944 0.094 Uiso 1 1 calc R . . C18 C 0.3947(2) 0.2612(3) 0.4822(3) 0.0612(12) Uani 1 1 d . . . H18A H 0.3920 0.2169 0.4560 0.073 Uiso 1 1 calc R . . C19 C 0.51186(17) 0.1716(2) 0.3884(2) 0.0436(9) Uani 1 1 d . . . C20 C 0.52361(18) 0.1855(3) 0.3161(2) 0.0476(10) Uani 1 1 d . . . H20A H 0.5481 0.2269 0.3043 0.057 Uiso 1 1 calc R . . C21 C 0.5013(2) 0.1419(3) 0.2616(2) 0.0589(12) Uani 1 1 d . . . H21A H 0.5105 0.1537 0.2139 0.071 Uiso 1 1 calc R . . C22 C 0.4660(2) 0.0818(3) 0.2769(3) 0.0690(15) Uani 1 1 d . . . H22A H 0.4500 0.0521 0.2397 0.083 Uiso 1 1 calc R . . C23 C 0.4538(2) 0.0644(3) 0.3454(3) 0.0704(15) Uani 1 1 d . . . H23A H 0.4300 0.0221 0.3561 0.084 Uiso 1 1 calc R . . C24 C 0.4762(2) 0.1087(3) 0.3998(3) 0.0611(12) Uani 1 1 d . . . H24A H 0.4667 0.0956 0.4471 0.073 Uiso 1 1 calc R . . Al2 Al 0.97060(5) 0.24986(7) 0.46240(6) 0.0413(3) Uani 1 1 d . . . C25 C 0.90641(19) 0.2215(2) 0.5338(2) 0.0429(9) Uani 1 1 d . . . C26 C 0.8428(2) 0.2335(3) 0.5256(2) 0.0529(11) Uani 1 1 d . . . H26A H 0.8287 0.2595 0.4851 0.064 Uiso 1 1 calc R . . C27 C 0.7992(2) 0.2095(3) 0.5734(3) 0.0636(13) Uani 1 1 d . . . H27A H 0.7563 0.2197 0.5656 0.076 Uiso 1 1 calc R . . C28 C 0.8179(2) 0.1703(3) 0.6335(3) 0.0609(12) Uani 1 1 d . . . H28A H 0.7881 0.1528 0.6662 0.073 Uiso 1 1 calc R . . C29 C 0.8798(2) 0.1576(3) 0.6439(3) 0.0673(14) Uani 1 1 d . . . H29A H 0.8936 0.1316 0.6846 0.081 Uiso 1 1 calc R . . C30 C 0.9231(2) 0.1828(3) 0.5949(2) 0.0582(12) Uani 1 1 d . . . H30A H 0.9660 0.1733 0.6035 0.070 Uiso 1 1 calc R . . C31 C 0.94679(18) 0.3422(2) 0.4126(2) 0.0430(9) Uani 1 1 d . . . C32 C 0.9799(2) 0.4078(2) 0.4211(2) 0.0475(10) Uani 1 1 d . . . H32A H 1.0168 0.4073 0.4491 0.057 Uiso 1 1 calc R . . C33 C 0.9612(2) 0.4734(3) 0.3905(3) 0.0575(12) Uani 1 1 d . . . H33A H 0.9851 0.5166 0.3976 0.069 Uiso 1 1 calc R . . C34 C 0.9077(3) 0.4752(3) 0.3498(3) 0.0646(13) Uani 1 1 d . . . H34A H 0.8946 0.5199 0.3288 0.077 Uiso 1 1 calc R . . C35 C 0.8737(2) 0.4134(3) 0.3394(2) 0.0616(13) Uani 1 1 d . . . H35A H 0.8369 0.4149 0.3114 0.074 Uiso 1 1 calc R . . C36 C 0.8931(2) 0.3478(3) 0.3702(2) 0.0556(11) Uani 1 1 d . . . H36A H 0.8689 0.3051 0.3622 0.067 Uiso 1 1 calc R . . C37 C 1.0524(2) 0.2653(2) 0.5121(2) 0.0474(10) Uani 1 1 d . . . C38 C 1.1085(2) 0.2435(3) 0.4826(3) 0.0620(12) Uani 1 1 d . . . H38A H 1.1074 0.2188 0.4385 0.074 Uiso 1 1 calc R . . C39 C 1.1657(3) 0.2559(4) 0.5141(4) 0.0849(19) Uani 1 1 d . . . H39A H 1.2026 0.2395 0.4918 0.102 Uiso 1 1 calc R . . C40 C 1.1692(3) 0.2917(4) 0.5773(4) 0.086(2) Uani 1 1 d . . . H40A H 1.2085 0.3011 0.5987 0.103 Uiso 1 1 calc R . . C41 C 1.1152(3) 0.3141(3) 0.6101(3) 0.0799(18) Uani 1 1 d . . . H41A H 1.1172 0.3383 0.6546 0.096 Uiso 1 1 calc R . . C42 C 1.0573(2) 0.3009(3) 0.5773(3) 0.0627(13) Uani 1 1 d . . . H42A H 1.0204 0.3167 0.6001 0.075 Uiso 1 1 calc R . . C43 C 0.9805(2) 0.1669(3) 0.3933(2) 0.0550(12) Uani 1 1 d . . . C44 C 0.9697(2) 0.1712(3) 0.3208(3) 0.0698(15) Uani 1 1 d . . . H44A H 0.9532 0.2151 0.3011 0.084 Uiso 1 1 calc R . . C45 C 0.9831(3) 0.1104(5) 0.2750(3) 0.088(2) Uani 1 1 d . . . H45A H 0.9755 0.1136 0.2256 0.106 Uiso 1 1 calc R . . C46 C 1.0072(3) 0.0470(4) 0.3044(5) 0.090(2) Uani 1 1 d . . . H46A H 1.0170 0.0070 0.2744 0.108 Uiso 1 1 calc R . . C47 C 1.0172(3) 0.0406(4) 0.3748(4) 0.088(2) Uani 1 1 d . . . H47A H 1.0326 -0.0039 0.3941 0.106 Uiso 1 1 calc R . . C48 C 1.0049(2) 0.0998(3) 0.4185(3) 0.0695(14) Uani 1 1 d . . . H48A H 1.0132 0.0951 0.4677 0.083 Uiso 1 1 calc R . . O1T O 0.7859(3) -0.3573(4) 0.2418(3) 0.1320(19) Uiso 1 1 d . . . C1T C 0.7536(4) -0.4184(5) 0.2743(5) 0.126(3) Uiso 1 1 d . . . H1TA H 0.7142 -0.4022 0.2960 0.151 Uiso 1 1 calc R . . H1TB H 0.7799 -0.4421 0.3110 0.151 Uiso 1 1 calc R . . C2T C 0.7418(5) -0.4681(5) 0.2150(5) 0.127(3) Uiso 1 1 d . . . H2TA H 0.7054 -0.4523 0.1864 0.152 Uiso 1 1 calc R . . H2TB H 0.7354 -0.5190 0.2313 0.152 Uiso 1 1 calc R . . C3T C 0.8015(6) -0.4601(7) 0.1750(8) 0.185(5) Uiso 1 1 d . . . H3TA H 0.8348 -0.4904 0.1965 0.222 Uiso 1 1 calc R . . H3TB H 0.7958 -0.4748 0.1249 0.222 Uiso 1 1 calc R . . C4T C 0.8166(4) -0.3818(4) 0.1805(4) 0.101(2) Uiso 1 1 d . . . H4TA H 0.8621 -0.3745 0.1851 0.121 Uiso 1 1 calc R . . H4TB H 0.8015 -0.3550 0.1383 0.121 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 0.03383(19) 0.03547(19) 0.03691(18) 0.00390(16) 0.00477(13) 0.00020(15) O1 0.0476(18) 0.095(3) 0.070(2) 0.040(2) -0.0130(15) -0.0152(18) O2 0.0445(16) 0.0440(17) 0.0605(18) 0.0003(14) -0.0018(13) -0.0097(13) O3 0.0576(18) 0.0533(18) 0.0410(15) 0.0079(13) 0.0125(13) 0.0006(15) O4 0.071(2) 0.0491(18) 0.0423(16) -0.0001(14) -0.0080(14) -0.0024(15) O5 0.0346(14) 0.0393(15) 0.0634(18) -0.0012(13) 0.0027(12) 0.0034(12) O6 0.0446(17) 0.0354(15) 0.088(2) 0.0024(15) 0.0050(15) 0.0025(13) O7 0.063(2) 0.059(2) 0.071(2) -0.0076(17) 0.0330(17) -0.0078(16) C50 0.055(3) 0.113(5) 0.092(4) 0.040(4) -0.006(3) -0.005(3) C51 0.060(3) 0.123(6) 0.112(5) 0.068(4) -0.018(3) -0.011(3) C52 0.057(3) 0.112(5) 0.080(4) 0.051(4) -0.004(3) -0.008(3) C53 0.054(3) 0.058(3) 0.072(3) 0.016(3) -0.005(2) -0.007(2) C54 0.073(4) 0.072(4) 0.103(5) 0.009(3) 0.010(3) -0.031(3) C55 0.080(4) 0.084(4) 0.095(4) 0.007(3) -0.016(3) -0.044(3) C56 0.070(3) 0.068(3) 0.067(3) -0.014(3) 0.001(2) -0.021(3) C57 0.088(4) 0.056(3) 0.051(3) -0.003(2) 0.010(2) 0.001(3) C58 0.094(4) 0.077(4) 0.043(2) 0.002(3) 0.017(2) -0.001(3) C59 0.076(4) 0.078(4) 0.067(3) 0.015(3) 0.035(3) 0.008(3) C60 0.063(3) 0.059(3) 0.058(3) 0.011(2) 0.017(2) -0.004(2) C61 0.155(7) 0.066(4) 0.060(3) 0.009(3) -0.026(4) -0.009(4) C62 0.213(10) 0.090(5) 0.082(5) 0.011(4) -0.070(6) 0.001(6) C63 0.140(6) 0.077(4) 0.062(3) 0.003(3) -0.027(4) -0.026(4) C64 0.072(3) 0.058(3) 0.050(3) 0.002(2) -0.014(2) -0.017(2) C65 0.049(3) 0.041(2) 0.081(3) -0.003(2) 0.007(2) 0.003(2) C66 0.053(3) 0.053(3) 0.112(4) 0.002(3) 0.018(3) 0.012(2) C67 0.039(2) 0.078(4) 0.083(3) 0.000(3) -0.006(2) 0.011(2) C68 0.035(2) 0.058(3) 0.096(4) -0.012(3) 0.002(2) -0.005(2) C69 0.051(3) 0.050(3) 0.066(3) 0.005(2) 0.004(2) -0.002(2) C70 0.070(3) 0.058(3) 0.071(3) -0.011(3) -0.004(3) -0.001(3) C71 0.061(3) 0.084(4) 0.138(6) -0.053(4) -0.009(3) 0.020(3) C72 0.046(3) 0.061(4) 0.193(8) -0.022(4) -0.007(4) 0.011(3) C73 0.090(5) 0.089(5) 0.111(5) -0.026(4) 0.047(4) -0.021(4) C74 0.121(6) 0.116(6) 0.065(4) -0.021(4) 0.030(4) -0.040(5) C75 0.095(5) 0.097(5) 0.075(4) 0.001(3) 0.037(3) -0.024(4) C76 0.056(3) 0.103(5) 0.074(3) 0.006(3) 0.019(3) 0.002(3) Al1 0.0349(6) 0.0507(7) 0.0459(6) -0.0063(6) 0.0006(5) 0.0009(5) C1 0.039(2) 0.048(2) 0.040(2) -0.0087(18) 0.0011(16) 0.0059(18) C2 0.043(2) 0.045(2) 0.061(3) 0.001(2) -0.0023(19) 0.0023(19) C3 0.042(2) 0.055(3) 0.073(3) -0.006(2) 0.001(2) 0.001(2) C4 0.063(3) 0.054(3) 0.066(3) -0.012(2) 0.018(2) -0.008(2) C5 0.077(3) 0.049(3) 0.049(2) 0.007(2) 0.005(2) 0.005(2) C6 0.052(3) 0.055(3) 0.047(2) -0.013(2) -0.0046(19) 0.010(2) C7 0.043(2) 0.048(2) 0.045(2) -0.0021(19) 0.0025(17) -0.0039(19) C8 0.060(3) 0.069(3) 0.052(3) -0.005(2) 0.007(2) 0.001(2) C9 0.097(4) 0.083(4) 0.041(3) -0.004(3) 0.009(3) -0.004(3) C10 0.090(4) 0.063(3) 0.057(3) 0.006(3) -0.017(3) -0.007(3) C11 0.063(3) 0.057(3) 0.070(3) 0.008(3) -0.007(2) -0.001(2) C12 0.058(3) 0.050(3) 0.051(2) 0.001(2) 0.005(2) -0.003(2) C13 0.040(2) 0.059(3) 0.048(2) -0.004(2) 0.0010(17) 0.003(2) C14 0.052(3) 0.079(4) 0.101(4) -0.029(3) 0.006(3) 0.007(3) C15 0.085(5) 0.086(4) 0.097(4) -0.023(4) 0.016(3) 0.017(4) C16 0.054(3) 0.111(5) 0.064(3) 0.015(3) 0.017(2) 0.028(3) C17 0.042(3) 0.115(5) 0.077(4) 0.010(4) 0.004(2) 0.002(3) C18 0.044(3) 0.077(3) 0.063(3) -0.004(3) 0.005(2) -0.002(2) C19 0.0299(19) 0.051(2) 0.050(2) -0.0038(19) 0.0026(16) 0.0050(17) C20 0.036(2) 0.055(3) 0.051(2) -0.003(2) 0.0017(17) 0.0061(19) C21 0.052(3) 0.074(3) 0.051(3) -0.016(2) -0.004(2) 0.013(2) C22 0.049(3) 0.070(3) 0.087(4) -0.042(3) -0.006(3) -0.004(3) C23 0.056(3) 0.061(3) 0.094(4) -0.017(3) 0.012(3) -0.015(2) C24 0.063(3) 0.057(3) 0.063(3) -0.009(2) 0.019(2) -0.010(2) Al2 0.0368(6) 0.0423(7) 0.0447(6) -0.0064(5) 0.0019(5) -0.0012(5) C25 0.044(2) 0.040(2) 0.044(2) -0.0017(18) 0.0014(17) 0.0017(18) C26 0.044(2) 0.055(3) 0.059(3) 0.012(2) 0.0022(19) 0.003(2) C27 0.044(3) 0.067(3) 0.080(3) 0.007(3) 0.011(2) 0.000(2) C28 0.061(3) 0.065(3) 0.057(3) -0.003(2) 0.016(2) -0.009(2) C29 0.071(3) 0.082(4) 0.048(3) 0.017(3) -0.003(2) -0.010(3) C30 0.051(3) 0.068(3) 0.055(3) 0.009(2) -0.004(2) 0.000(2) C31 0.038(2) 0.054(3) 0.0372(19) -0.0028(18) 0.0055(16) 0.0003(18) C32 0.041(2) 0.051(3) 0.051(2) -0.003(2) 0.0099(17) 0.0004(19) C33 0.061(3) 0.051(3) 0.061(3) 0.004(2) 0.015(2) -0.002(2) C34 0.072(3) 0.065(3) 0.057(3) 0.016(3) 0.015(2) 0.017(3) C35 0.057(3) 0.079(4) 0.049(3) 0.012(3) -0.002(2) 0.008(3) C36 0.047(2) 0.071(3) 0.049(2) -0.001(2) -0.0023(19) -0.005(2) C37 0.044(2) 0.043(2) 0.056(2) 0.001(2) -0.0043(19) -0.0026(18) C38 0.046(3) 0.062(3) 0.078(3) 0.004(3) -0.003(2) 0.000(2) C39 0.044(3) 0.076(4) 0.134(6) 0.024(4) -0.018(3) -0.007(3) C40 0.055(3) 0.073(4) 0.127(6) 0.044(4) -0.039(4) -0.021(3) C41 0.106(5) 0.062(3) 0.071(3) 0.009(3) -0.042(3) -0.026(3) C42 0.065(3) 0.059(3) 0.064(3) -0.004(2) -0.016(2) -0.007(2) C43 0.039(2) 0.064(3) 0.062(3) -0.018(2) 0.0107(19) -0.018(2) C44 0.061(3) 0.089(4) 0.060(3) -0.018(3) 0.014(2) -0.034(3) C45 0.072(4) 0.125(6) 0.068(3) -0.039(4) 0.026(3) -0.052(4) C46 0.061(4) 0.085(5) 0.125(6) -0.046(4) 0.035(4) -0.023(3) C47 0.070(4) 0.076(4) 0.118(6) -0.042(4) 0.014(4) -0.003(3) C48 0.057(3) 0.057(3) 0.094(4) -0.023(3) 0.004(3) 0.003(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 O6 2.548(3) . ? Sr1 O2 2.557(3) . ? Sr1 O3 2.556(3) . ? Sr1 O5 2.561(3) . ? Sr1 O4 2.576(3) . ? Sr1 O1 2.577(3) . ? Sr1 O7 2.584(3) . ? O1 C52 1.444(6) . ? O1 C49A 1.476(9) . ? O1 C49 1.473(12) . ? O2 C56 1.443(6) . ? O2 C53 1.445(5) . ? O3 C60 1.451(6) . ? O3 C57 1.453(6) . ? O4 C61 1.437(6) . ? O4 C64 1.441(5) . ? O5 C65 1.443(5) . ? O5 C68 1.454(5) . ? O6 C69 1.443(5) . ? O6 C72 1.443(6) . ? O7 C73 1.401(7) . ? O7 C76 1.428(7) . ? C49 C50 1.380(12) . ? C49A C50 1.523(10) . ? C50 C51 1.523(8) . ? C51 C52 1.467(8) . ? C53 C54 1.524(7) . ? C54 C55 1.474(9) . ? C55 C56 1.499(7) . ? C57 C58 1.502(7) . ? C58 C59 1.508(8) . ? C59 C60 1.502(7) . ? C61 C62 1.485(9) . ? C62 C63 1.430(9) . ? C63 C64 1.483(7) . ? C65 C66 1.497(7) . ? C66 C67 1.497(8) . ? C67 C68 1.498(7) . ? C69 C70 1.511(7) . ? C70 C71 1.508(8) . ? C71 C72 1.427(8) . ? C73 C74 1.506(9) . ? C74 C75 1.462(9) . ? C75 C76 1.505(7) . ? Al1 C19 1.998(4) . ? Al1 C7 2.003(4) . ? Al1 C1 2.010(4) . ? Al1 C13 2.025(4) . ? C1 C6 1.387(6) . ? C1 C2 1.405(6) . ? C2 C3 1.386(6) . ? C3 C4 1.359(7) . ? C4 C5 1.363(7) . ? C5 C6 1.397(7) . ? C7 C12 1.391(6) . ? C7 C8 1.400(6) . ? C8 C9 1.398(7) . ? C9 C10 1.349(8) . ? C10 C11 1.356(7) . ? C11 C12 1.404(7) . ? C13 C14 1.379(7) . ? C13 C18 1.387(6) . ? C14 C15 1.400(8) . ? C15 C16 1.351(9) . ? C16 C17 1.366(9) . ? C17 C18 1.380(7) . ? C19 C24 1.399(6) . ? C19 C20 1.415(6) . ? C20 C21 1.384(6) . ? C21 C22 1.368(8) . ? C22 C23 1.360(8) . ? C23 C24 1.392(7) . ? Al2 C31 1.998(5) . ? Al2 C25 2.006(4) . ? Al2 C37 2.008(4) . ? Al2 C43 2.013(5) . ? C25 C26 1.392(6) . ? C25 C30 1.399(6) . ? C26 C27 1.379(6) . ? C27 C28 1.399(7) . ? C28 C29 1.365(7) . ? C29 C30 1.397(7) . ? C31 C36 1.403(6) . ? C31 C32 1.403(6) . ? C32 C33 1.389(6) . ? C33 C34 1.380(7) . ? C34 C35 1.358(8) . ? C35 C36 1.396(7) . ? C37 C38 1.390(7) . ? C37 C42 1.396(6) . ? C38 C39 1.381(7) . ? C39 C40 1.364(10) . ? C40 C41 1.382(9) . ? C41 C42 1.407(7) . ? C43 C44 1.391(7) . ? C43 C48 1.414(7) . ? C44 C45 1.439(8) . ? C45 C46 1.384(10) . ? C46 C47 1.350(10) . ? C47 C48 1.389(7) . ? O1T C4T 1.410(9) . ? O1T C1T 1.454(10) . ? C1T C2T 1.464(12) . ? C2T C3T 1.503(14) . ? C3T C4T 1.472(13) . ? 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 O6 Sr1 O2 154.87(9) . . ? O6 Sr1 O3 81.24(10) . . ? O2 Sr1 O3 110.94(10) . . ? O6 Sr1 O5 129.39(9) . . ? O2 Sr1 O5 75.73(9) . . ? O3 Sr1 O5 71.19(10) . . ? O6 Sr1 O4 82.65(10) . . ? O2 Sr1 O4 108.59(10) . . ? O3 Sr1 O4 117.74(10) . . ? O5 Sr1 O4 74.47(10) . . ? O6 Sr1 O1 83.09(12) . . ? O2 Sr1 O1 79.19(11) . . ? O3 Sr1 O1 75.41(10) . . ? O5 Sr1 O1 126.81(12) . . ? O4 Sr1 O1 158.69(12) . . ? O6 Sr1 O7 84.15(10) . . ? O2 Sr1 O7 76.71(10) . . ? O3 Sr1 O7 156.70(11) . . ? O5 Sr1 O7 131.77(11) . . ? O4 Sr1 O7 77.94(11) . . ? O1 Sr1 O7 84.93(12) . . ? C52 O1 C49A 102.5(5) . . ? C52 O1 C49 106.7(5) . . ? C49A O1 C49 35.7(5) . . ? C52 O1 Sr1 122.9(3) . . ? C49A O1 Sr1 133.1(4) . . ? C49 O1 Sr1 125.3(5) . . ? C56 O2 C53 104.6(4) . . ? C56 O2 Sr1 127.9(3) . . ? C53 O2 Sr1 127.4(3) . . ? C60 O3 C57 108.8(3) . . ? C60 O3 Sr1 132.6(3) . . ? C57 O3 Sr1 118.6(3) . . ? C61 O4 C64 109.1(4) . . ? C61 O4 Sr1 116.6(3) . . ? C64 O4 Sr1 134.2(3) . . ? C65 O5 C68 108.7(3) . . ? C65 O5 Sr1 132.6(2) . . ? C68 O5 Sr1 118.5(2) . . ? C69 O6 C72 104.8(4) . . ? C69 O6 Sr1 132.4(3) . . ? C72 O6 Sr1 122.8(3) . . ? C73 O7 C76 101.3(4) . . ? C73 O7 Sr1 128.3(3) . . ? C76 O7 Sr1 129.8(3) . . ? C50 C49 O1 109.5(8) . . ? O1 C49A C50 102.0(6) . . ? C49 C50 C51 103.0(7) . . ? C49 C50 C49A 35.8(6) . . ? C51 C50 C49A 103.7(5) . . ? C52 C51 C50 105.3(5) . . ? O1 C52 C51 105.9(4) . . ? O2 C53 C54 105.0(4) . . ? C55 C54 C53 105.3(4) . . ? C54 C55 C56 105.7(4) . . ? O2 C56 C55 105.0(4) . . ? O3 C57 C58 105.7(4) . . ? C57 C58 C59 101.8(4) . . ? C60 C59 C58 103.9(4) . . ? O3 C60 C59 106.0(4) . . ? O4 C61 C62 105.3(5) . . ? C63 C62 C61 106.1(6) . . ? C62 C63 C64 105.0(5) . . ? O4 C64 C63 106.0(4) . . ? O5 C65 C66 106.2(4) . . ? C65 C66 C67 103.9(4) . . ? C66 C67 C68 102.2(4) . . ? O5 C68 C67 105.2(4) . . ? O6 C69 C70 104.8(4) . . ? C71 C70 C69 103.7(4) . . ? C72 C71 C70 106.6(5) . . ? C71 C72 O6 108.7(5) . . ? O7 C73 C74 105.4(5) . . ? C75 C74 C73 104.4(5) . . ? C74 C75 C76 103.4(5) . . ? O7 C76 C75 106.4(5) . . ? C19 Al1 C7 112.18(18) . . ? C19 Al1 C1 109.99(17) . . ? C7 Al1 C1 108.09(17) . . ? C19 Al1 C13 107.26(17) . . ? C7 Al1 C13 108.12(18) . . ? C1 Al1 C13 111.21(18) . . ? C6 C1 C2 114.4(4) . . ? C6 C1 Al1 122.9(3) . . ? C2 C1 Al1 122.8(3) . . ? C3 C2 C1 122.9(4) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 119.6(5) . . ? C4 C5 C6 120.1(5) . . ? C1 C6 C5 122.9(4) . . ? C12 C7 C8 114.3(4) . . ? C12 C7 Al1 122.2(3) . . ? C8 C7 Al1 123.4(3) . . ? C7 C8 C9 122.5(5) . . ? C10 C9 C8 120.3(5) . . ? C9 C10 C11 120.4(5) . . ? C10 C11 C12 119.2(5) . . ? C7 C12 C11 123.3(4) . . ? C14 C13 C18 114.4(4) . . ? C14 C13 Al1 122.4(3) . . ? C18 C13 Al1 123.2(4) . . ? C13 C14 C15 123.0(5) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C17 118.3(5) . . ? C16 C17 C18 121.0(5) . . ? C17 C18 C13 122.8(5) . . ? C24 C19 C20 113.5(4) . . ? C24 C19 Al1 122.1(3) . . ? C20 C19 Al1 123.9(3) . . ? C21 C20 C19 123.5(4) . . ? C22 C21 C20 119.6(5) . . ? C23 C22 C21 120.0(5) . . ? C22 C23 C24 120.0(5) . . ? C23 C24 C19 123.4(5) . . ? C31 Al2 C25 111.13(17) . . ? C31 Al2 C37 108.79(18) . . ? C25 Al2 C37 109.06(18) . . ? C31 Al2 C43 111.0(2) . . ? C25 Al2 C43 108.56(18) . . ? C37 Al2 C43 108.25(19) . . ? C26 C25 C30 114.6(4) . . ? C26 C25 Al2 124.4(3) . . ? C30 C25 Al2 120.8(3) . . ? C27 C26 C25 123.4(4) . . ? C26 C27 C28 120.1(4) . . ? C29 C28 C27 118.5(4) . . ? C28 C29 C30 120.2(5) . . ? C25 C30 C29 123.1(4) . . ? C36 C31 C32 114.8(4) . . ? C36 C31 Al2 122.5(3) . . ? C32 C31 Al2 122.6(3) . . ? C33 C32 C31 123.0(4) . . ? C34 C33 C32 119.4(5) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 119.7(5) . . ? C35 C36 C31 122.8(5) . . ? C38 C37 C42 115.4(4) . . ? C38 C37 Al2 122.1(3) . . ? C42 C37 Al2 122.5(3) . . ? C39 C38 C37 123.5(6) . . ? C40 C39 C38 119.9(6) . . ? C39 C40 C41 119.7(5) . . ? C40 C41 C42 119.6(6) . . ? C37 C42 C41 121.9(5) . . ? C44 C43 C48 116.1(5) . . ? C44 C43 Al2 125.4(4) . . ? C48 C43 Al2 118.4(4) . . ? C43 C44 C45 121.0(6) . . ? C46 C45 C44 118.8(6) . . ? C47 C46 C45 121.6(6) . . ? C46 C47 C48 119.2(7) . . ? C47 C48 C43 123.2(6) . . ? C4T O1T C1T 109.4(7) . . ? O1T C1T C2T 103.5(8) . . ? C1T C2T C3T 100.5(9) . . ? C4T C3T C2T 104.3(10) . . ? O1T C4T C3T 105.2(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.056 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.072 #==== END data_FO3506 _database_code_depnum_ccdc_archive 'CCDC 765646' #TrackingRef 'newjchem.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H40 Ca O8), 4(C18 H23 Ga N), C7 H8' _chemical_formula_sum 'C55.50 H90 Ca Ga2 N2 O8' _chemical_formula_weight 1092.82 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' 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.6288(2) _cell_length_b 21.8473(3) _cell_length_c 37.9734(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12136.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 71173 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4664 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71173 _diffrn_reflns_av_R_equivalents 0.1318 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13866 _reflns_number_gt 7444 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1331P)^2^+13.7936P] 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 13866 _refine_ls_number_parameters 617 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1634 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2589 _refine_ls_wR_factor_gt 0.2136 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.48956(6) -0.27613(4) 0.12137(3) 0.0241(2) Uani 1 1 d . . . O1 O 0.6158(3) -0.20197(16) 0.11392(10) 0.0382(9) Uani 1 1 d . . . O2 O 0.5315(3) -0.22070(17) 0.17488(9) 0.0395(9) Uani 1 1 d . . . O3 O 0.6293(2) -0.33650(16) 0.13627(10) 0.0386(9) Uani 1 1 d . . . O4 O 0.4701(2) -0.35320(17) 0.16877(10) 0.0383(9) Uani 1 1 d . . . O5 O 0.3389(2) -0.32223(16) 0.10859(10) 0.0397(9) Uani 1 1 d . . . O6 O 0.3560(3) -0.20985(18) 0.13575(11) 0.0463(10) Uani 1 1 d . . . O7 O 0.5176(3) -0.34258(17) 0.07098(10) 0.0398(9) Uani 1 1 d . . . O8 O 0.4604(2) -0.22597(15) 0.06562(9) 0.0346(8) Uani 1 1 d . . . C1 C 0.6616(4) -0.1862(3) 0.08206(16) 0.0505(16) Uani 1 1 d . . . H1A H 0.7278 -0.1865 0.0860 0.076 Uiso 1 1 calc R . . H1B H 0.6424 -0.1453 0.0745 0.076 Uiso 1 1 calc R . . H1C H 0.6461 -0.2160 0.0637 0.076 Uiso 1 1 calc R . . C2 C 0.6352(5) -0.1627(3) 0.14199(18) 0.067(2) Uani 1 1 d . . . H2A H 0.6012 -0.1240 0.1385 0.081 Uiso 1 1 calc R . . H2B H 0.7013 -0.1528 0.1416 0.081 Uiso 1 1 calc R . . C3 C 0.6131(5) -0.1865(3) 0.17511(18) 0.065(2) Uani 1 1 d . . . H3A H 0.6069 -0.1524 0.1921 0.077 Uiso 1 1 calc R . . H3B H 0.6638 -0.2130 0.1833 0.077 Uiso 1 1 calc R . . C4 C 0.4918(5) -0.2292(3) 0.20957(17) 0.0607(19) Uani 1 1 d . . . H4A H 0.4881 -0.1897 0.2216 0.091 Uiso 1 1 calc R . . H4B H 0.5302 -0.2572 0.2233 0.091 Uiso 1 1 calc R . . H4C H 0.4303 -0.2466 0.2072 0.091 Uiso 1 1 calc R . . C5 C 0.7188(4) -0.3331(3) 0.12054(19) 0.0571(17) Uani 1 1 d . . . H5A H 0.7462 -0.3740 0.1200 0.086 Uiso 1 1 calc R . . H5B H 0.7575 -0.3056 0.1345 0.086 Uiso 1 1 calc R . . H5C H 0.7135 -0.3173 0.0965 0.086 Uiso 1 1 calc R . . C6 C 0.6320(4) -0.3609(3) 0.17101(16) 0.0443(15) Uani 1 1 d . . . H6A H 0.6406 -0.3275 0.1883 0.053 Uiso 1 1 calc R . . H6B H 0.6837 -0.3898 0.1733 0.053 Uiso 1 1 calc R . . C7 C 0.5444(4) -0.3930(3) 0.17782(16) 0.0461(15) Uani 1 1 d . . . H7A H 0.5413 -0.4308 0.1635 0.055 Uiso 1 1 calc R . . H7B H 0.5404 -0.4044 0.2030 0.055 Uiso 1 1 calc R . . C8 C 0.3863(5) -0.3741(3) 0.18406(17) 0.0574(18) Uani 1 1 d . . . H8A H 0.3918 -0.3741 0.2098 0.086 Uiso 1 1 calc R . . H8B H 0.3732 -0.4157 0.1758 0.086 Uiso 1 1 calc R . . H8C H 0.3364 -0.3468 0.1770 0.086 Uiso 1 1 calc R . . C9 C 0.3206(5) -0.3852(3) 0.09911(19) 0.0589(18) Uani 1 1 d . . . H9A H 0.2766 -0.4028 0.1157 0.088 Uiso 1 1 calc R . . H9B H 0.3776 -0.4087 0.1000 0.088 Uiso 1 1 calc R . . H9C H 0.2954 -0.3868 0.0752 0.088 Uiso 1 1 calc R . . C10 C 0.2582(4) -0.2886(3) 0.1141(2) 0.065(2) Uani 1 1 d . . . H10C H 0.2276 -0.3040 0.1356 0.078 Uiso 1 1 calc R . . H10D H 0.2164 -0.2956 0.0940 0.078 Uiso 1 1 calc R . . C11 C 0.2738(4) -0.2247(3) 0.1178(2) 0.069(2) Uani 1 1 d . . . H11C H 0.2217 -0.2064 0.1307 0.083 Uiso 1 1 calc R . . H11D H 0.2755 -0.2059 0.0940 0.083 Uiso 1 1 calc R . . C12 C 0.3582(5) -0.1478(3) 0.1483(2) 0.0616(19) Uani 1 1 d . . . H12A H 0.3145 -0.1431 0.1677 0.092 Uiso 1 1 calc R . . H12B H 0.3416 -0.1199 0.1291 0.092 Uiso 1 1 calc R . . H12C H 0.4198 -0.1380 0.1567 0.092 Uiso 1 1 calc R . . C13 C 0.5594(5) -0.4017(2) 0.06958(18) 0.0500(16) Uani 1 1 d . . . H13E H 0.5215 -0.4292 0.0553 0.075 Uiso 1 1 calc R . . H13F H 0.5650 -0.4182 0.0935 0.075 Uiso 1 1 calc R . . H13G H 0.6202 -0.3982 0.0589 0.075 Uiso 1 1 calc R . . C14 C 0.5045(5) -0.3179(3) 0.03644(16) 0.0516(17) Uani 1 1 d . . . H14G H 0.5651 -0.3089 0.0260 0.062 Uiso 1 1 calc R . . H14H H 0.4748 -0.3494 0.0216 0.062 Uiso 1 1 calc R . . C15 C 0.4512(6) -0.2642(3) 0.03557(17) 0.066(2) Uani 1 1 d . . . H15E H 0.3861 -0.2760 0.0331 0.079 Uiso 1 1 calc R . . H15F H 0.4681 -0.2404 0.0144 0.079 Uiso 1 1 calc R . . C16 C 0.4429(5) -0.1631(3) 0.05806(16) 0.0478(15) Uani 1 1 d . . . H16G H 0.4821 -0.1497 0.0386 0.072 Uiso 1 1 calc R . . H16H H 0.4559 -0.1384 0.0790 0.072 Uiso 1 1 calc R . . H16I H 0.3786 -0.1580 0.0514 0.072 Uiso 1 1 calc R . . Ga1A Ga 0.47771(4) 0.02216(3) 0.199329(17) 0.0410(2) Uani 1 1 d . . . N1A N 0.5341(3) 0.0027(2) 0.15233(12) 0.0383(11) Uani 1 1 d . . . C1A C 0.4966(4) -0.0002(2) 0.11896(15) 0.0356(12) Uani 1 1 d . . . C2A C 0.4043(4) 0.0038(3) 0.10908(15) 0.0409(14) Uani 1 1 d . . . H2AA H 0.3579 0.0116 0.1260 0.049 Uiso 1 1 calc R . . C3A C 0.3829(4) -0.0040(2) 0.07368(16) 0.0424(14) Uani 1 1 d . . . H3AA H 0.3205 -0.0032 0.0667 0.051 Uiso 1 1 calc R . . C4A C 0.4490(4) -0.0127(2) 0.04834(15) 0.0425(14) Uani 1 1 d . . . H4AA H 0.4310 -0.0178 0.0245 0.051 Uiso 1 1 calc R . . C5A C 0.5422(4) -0.0142(2) 0.05694(15) 0.0409(14) Uani 1 1 d . . . H5AA H 0.5879 -0.0192 0.0394 0.049 Uiso 1 1 calc R . . C6A C 0.5652(4) -0.0078(2) 0.09316(14) 0.0348(12) Uani 1 1 d . . . C7A C 0.6503(4) -0.0106(2) 0.11156(14) 0.0346(12) Uani 1 1 d . . . C8A C 0.7411(4) -0.0196(2) 0.10153(16) 0.0409(14) Uani 1 1 d . . . H8AA H 0.7568 -0.0226 0.0773 0.049 Uiso 1 1 calc R . . C9A C 0.8071(4) -0.0241(3) 0.12678(18) 0.0494(16) Uani 1 1 d . . . H9AA H 0.8686 -0.0316 0.1200 0.059 Uiso 1 1 calc R . . C10A C 0.7851(4) -0.0176(3) 0.16283(17) 0.0463(15) Uani 1 1 d . . . H10A H 0.8319 -0.0208 0.1801 0.056 Uiso 1 1 calc R . . C11A C 0.6963(4) -0.0066(3) 0.17316(16) 0.0436(14) Uani 1 1 d . . . H11A H 0.6822 -0.0006 0.1973 0.052 Uiso 1 1 calc R . . C12A C 0.6279(4) -0.0044(2) 0.14801(15) 0.0365(13) Uani 1 1 d . . . C13A C 0.5371(5) 0.1019(3) 0.21183(19) 0.0591(18) Uani 1 1 d . . . H13A H 0.5016 0.1221 0.2307 0.071 Uiso 1 1 calc R . . H13B H 0.5995 0.0940 0.2209 0.071 Uiso 1 1 calc R . . C14A C 0.5428(8) 0.1446(4) 0.1797(3) 0.103(3) Uani 1 1 d . . . H14A H 0.5618 0.1855 0.1874 0.155 Uiso 1 1 calc R . . H14B H 0.4827 0.1472 0.1684 0.155 Uiso 1 1 calc R . . H14C H 0.5875 0.1284 0.1629 0.155 Uiso 1 1 calc R . . C15A C 0.3417(4) 0.0309(3) 0.19590(16) 0.0564(17) Uani 1 1 d . . . H15A H 0.3265 0.0670 0.1813 0.068 Uiso 1 1 calc R . . H15B H 0.3155 -0.0058 0.1844 0.068 Uiso 1 1 calc R . . C16A C 0.2993(5) 0.0385(4) 0.23315(19) 0.075(2) Uani 1 1 d . . . H16A H 0.2348 0.0499 0.2309 0.113 Uiso 1 1 calc R . . H16B H 0.3321 0.0706 0.2460 0.113 Uiso 1 1 calc R . . H16C H 0.3042 -0.0002 0.2461 0.113 Uiso 1 1 calc R . . C17A C 0.5091(5) -0.0497(3) 0.23021(18) 0.0543(17) Uani 1 1 d . . . H17A H 0.4604 -0.0808 0.2278 0.065 Uiso 1 1 calc R . . H17B H 0.5667 -0.0682 0.2215 0.065 Uiso 1 1 calc R . . C18A C 0.5206(6) -0.0345(4) 0.2692(2) 0.072(2) Uani 1 1 d . . . H18A H 0.5264 -0.0725 0.2827 0.109 Uiso 1 1 calc R . . H18B H 0.4671 -0.0117 0.2775 0.109 Uiso 1 1 calc R . . H18C H 0.5756 -0.0095 0.2725 0.109 Uiso 1 1 calc R . . Ga1B Ga 0.52505(5) -0.36737(3) -0.079469(17) 0.0421(2) Uani 1 1 d . A . N1B N 0.6120(3) -0.3232(2) -0.04612(12) 0.0373(11) Uani 1 1 d . . . C1B C 0.6774(4) -0.3478(3) -0.02386(15) 0.0374(13) Uani 1 1 d . . . C2B C 0.6971(4) -0.4101(3) -0.01743(16) 0.0459(15) Uani 1 1 d . . . H2BA H 0.6661 -0.4416 -0.0299 0.055 Uiso 1 1 calc R . . C3B C 0.7622(4) -0.4238(3) 0.00733(17) 0.0504(16) Uani 1 1 d . . . H3BA H 0.7759 -0.4656 0.0119 0.060 Uiso 1 1 calc R . . C4B C 0.8084(4) -0.3796(3) 0.02578(17) 0.0546(18) Uani 1 1 d . . . H4BA H 0.8534 -0.3914 0.0425 0.066 Uiso 1 1 calc R . . C5B C 0.7904(4) -0.3178(3) 0.02032(16) 0.0457(15) Uani 1 1 d . . . H5BA H 0.8215 -0.2871 0.0334 0.055 Uiso 1 1 calc R . . C6B C 0.7242(4) -0.3022(3) -0.00527(15) 0.0395(14) Uani 1 1 d . . . C7B C 0.6849(4) -0.2448(3) -0.01635(15) 0.0380(13) Uani 1 1 d . . . C8B C 0.7002(4) -0.1830(3) -0.00710(16) 0.0465(15) Uani 1 1 d . . . H8BA H 0.7475 -0.1721 0.0089 0.056 Uiso 1 1 calc R . . C9B C 0.6449(4) -0.1387(3) -0.02185(17) 0.0488(16) Uani 1 1 d . . . H9BA H 0.6546 -0.0970 -0.0159 0.059 Uiso 1 1 calc R . . C10B C 0.5756(4) -0.1538(3) -0.04506(16) 0.0480(15) Uani 1 1 d . . . H10B H 0.5385 -0.1221 -0.0545 0.058 Uiso 1 1 calc R . . C11B C 0.5587(4) -0.2144(3) -0.05495(16) 0.0429(14) Uani 1 1 d . . . H11B H 0.5108 -0.2244 -0.0708 0.051 Uiso 1 1 calc R . . C12B C 0.6159(4) -0.2605(2) -0.04035(15) 0.0375(13) Uani 1 1 d . . . C13B C 0.4113(4) -0.3786(3) -0.05009(16) 0.0441(14) Uani 1 1 d . . . H13C H 0.4035 -0.3419 -0.0351 0.053 Uiso 1 1 calc R . . H13D H 0.3580 -0.3807 -0.0661 0.053 Uiso 1 1 calc R . . C14B C 0.4101(5) -0.4349(3) -0.02653(18) 0.0543(17) Uani 1 1 d . . . H14D H 0.3576 -0.4326 -0.0105 0.081 Uiso 1 1 calc R . . H14E H 0.4667 -0.4365 -0.0128 0.081 Uiso 1 1 calc R . . H14F H 0.4052 -0.4717 -0.0411 0.081 Uiso 1 1 calc R . . C15B C 0.5040(5) -0.3126(3) -0.12089(18) 0.0593(18) Uani 1 1 d . . . H15C H 0.5451 -0.2768 -0.1191 0.071 Uiso 1 1 calc R . . H15D H 0.5202 -0.3351 -0.1427 0.071 Uiso 1 1 calc R . . C16B C 0.4089(6) -0.2910(5) -0.1237(3) 0.121(4) Uani 1 1 d . . . H16D H 0.4033 -0.2633 -0.1439 0.181 Uiso 1 1 calc R . . H16E H 0.3920 -0.2691 -0.1021 0.181 Uiso 1 1 calc R . . H16F H 0.3680 -0.3261 -0.1270 0.181 Uiso 1 1 calc R . . C17B C 0.5858(7) -0.4445(4) -0.0952(2) 0.089(3) Uani 1 1 d . . . H17C H 0.6007 -0.4684 -0.0738 0.107 Uiso 0.630(17) 1 calc PR A 1 H17D H 0.5400 -0.4684 -0.1086 0.107 Uiso 0.630(17) 1 calc PR A 1 H17E H 0.6464 -0.4467 -0.0837 0.107 Uiso 0.370(17) 1 d PR A 2 H17F H 0.5494 -0.4795 -0.0865 0.107 Uiso 0.370(17) 1 d PR A 2 C18B C 0.6613(8) -0.4418(5) -0.1148(3) 0.059(4) Uiso 0.630(17) 1 d P A 1 H18D H 0.6498 -0.4167 -0.1357 0.089 Uiso 0.630(17) 1 calc PR A 1 H18E H 0.6787 -0.4833 -0.1221 0.089 Uiso 0.630(17) 1 calc PR A 1 H18F H 0.7109 -0.4236 -0.1010 0.089 Uiso 0.630(17) 1 calc PR A 1 C18C C 0.5999(13) -0.4533(8) -0.1327(5) 0.053(6) Uiso 0.370(17) 1 d P A 2 H18G H 0.6217 -0.4150 -0.1432 0.079 Uiso 0.370(17) 1 calc PR A 2 H18H H 0.5420 -0.4652 -0.1438 0.079 Uiso 0.370(17) 1 calc PR A 2 H18I H 0.6454 -0.4856 -0.1364 0.079 Uiso 0.370(17) 1 calc PR A 2 C1T C 0.7806(6) -0.2046(4) 0.2433(2) 0.102(6) Uiso 0.50 1 d PGD . . C2T C 0.7638(6) -0.2666(3) 0.2487(2) 0.062(4) Uiso 0.50 1 d PGD . . H2TA H 0.7979 -0.2963 0.2360 0.075 Uiso 0.50 1 calc PR . . C3T C 0.6971(6) -0.2850(3) 0.2725(3) 0.073(4) Uiso 0.50 1 d PGD . . H3TA H 0.6857 -0.3273 0.2761 0.088 Uiso 0.50 1 calc PR . . C4T C 0.6473(6) -0.2414(4) 0.2910(2) 0.063(4) Uiso 0.50 1 d PGD . . H4TA H 0.6017 -0.2540 0.3073 0.075 Uiso 0.50 1 calc PR . . C5T C 0.6641(6) -0.1795(4) 0.2857(2) 0.063(4) Uiso 0.50 1 d PGD . . H5TA H 0.6300 -0.1497 0.2984 0.075 Uiso 0.50 1 calc PR . . C6T C 0.7307(6) -0.1611(3) 0.2619(2) 0.056(3) Uiso 0.50 1 d PGD . . H6TA H 0.7422 -0.1188 0.2582 0.067 Uiso 0.50 1 calc PR . . C7T C 0.8542(13) -0.1840(6) 0.2180(5) 0.159(10) Uiso 0.50 1 d PD . . H7TA H 0.8826 -0.2199 0.2070 0.239 Uiso 0.50 1 calc PR . . H7TB H 0.9007 -0.1607 0.2308 0.239 Uiso 0.50 1 calc PR . . H7TC H 0.8270 -0.1581 0.1997 0.239 Uiso 0.50 1 calc PR . . 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 0.0255(5) 0.0223(5) 0.0246(5) 0.0001(4) -0.0005(4) -0.0009(4) O1 0.041(2) 0.038(2) 0.035(2) -0.0009(17) -0.0017(17) -0.0151(17) O2 0.046(2) 0.042(2) 0.030(2) -0.0067(16) -0.0004(17) -0.0063(18) O3 0.032(2) 0.038(2) 0.046(2) 0.0056(18) -0.0005(17) 0.0037(17) O4 0.035(2) 0.041(2) 0.038(2) 0.0120(17) -0.0006(17) 0.0003(17) O5 0.0273(19) 0.041(2) 0.051(2) 0.0037(18) -0.0022(17) -0.0077(17) O6 0.039(2) 0.053(2) 0.047(2) -0.0019(19) -0.0009(19) 0.0133(19) O7 0.045(2) 0.036(2) 0.038(2) -0.0082(17) -0.0068(18) 0.0097(18) O8 0.045(2) 0.0263(19) 0.032(2) -0.0003(15) -0.0057(17) -0.0021(16) C1 0.048(4) 0.052(4) 0.052(4) 0.006(3) 0.008(3) -0.017(3) C2 0.075(5) 0.069(5) 0.057(5) -0.007(4) 0.004(4) -0.037(4) C3 0.069(5) 0.075(5) 0.050(4) -0.021(4) -0.004(4) -0.027(4) C4 0.089(5) 0.061(4) 0.032(3) -0.010(3) 0.014(3) -0.006(4) C5 0.034(3) 0.060(4) 0.077(5) 0.011(4) 0.011(3) 0.007(3) C6 0.041(3) 0.045(3) 0.047(4) 0.002(3) -0.017(3) 0.012(3) C7 0.061(4) 0.035(3) 0.043(4) 0.013(3) -0.005(3) 0.009(3) C8 0.054(4) 0.076(5) 0.042(4) 0.022(3) 0.006(3) -0.010(4) C9 0.059(4) 0.051(4) 0.067(5) -0.006(3) -0.010(4) -0.020(3) C10 0.033(3) 0.076(5) 0.086(5) -0.005(4) -0.017(3) 0.009(3) C11 0.026(3) 0.062(5) 0.120(7) 0.002(4) -0.013(4) 0.004(3) C12 0.069(5) 0.038(4) 0.078(5) -0.010(3) 0.005(4) 0.016(3) C13 0.060(4) 0.029(3) 0.061(4) -0.017(3) -0.001(3) 0.010(3) C14 0.079(5) 0.048(4) 0.028(3) -0.002(3) 0.004(3) -0.002(3) C15 0.089(5) 0.067(5) 0.041(4) -0.013(3) -0.025(4) 0.033(4) C16 0.061(4) 0.037(3) 0.045(4) 0.015(3) -0.011(3) 0.000(3) Ga1A 0.0447(4) 0.0447(4) 0.0337(4) -0.0054(3) 0.0067(3) -0.0005(3) N1A 0.034(3) 0.051(3) 0.030(2) -0.008(2) -0.001(2) 0.000(2) C1A 0.040(3) 0.032(3) 0.035(3) 0.002(2) 0.003(2) -0.004(2) C2A 0.037(3) 0.046(3) 0.040(3) 0.002(3) 0.002(3) -0.001(3) C3A 0.046(3) 0.037(3) 0.045(4) 0.003(3) -0.007(3) 0.002(3) C4A 0.062(4) 0.032(3) 0.033(3) 0.004(2) -0.015(3) -0.004(3) C5A 0.063(4) 0.029(3) 0.030(3) 0.003(2) 0.006(3) -0.007(3) C6A 0.046(3) 0.026(3) 0.032(3) -0.002(2) 0.005(3) -0.010(2) C7A 0.039(3) 0.029(3) 0.036(3) -0.005(2) 0.004(2) -0.006(2) C8A 0.041(3) 0.037(3) 0.045(3) -0.005(3) 0.014(3) -0.006(3) C9A 0.038(3) 0.045(4) 0.065(4) -0.002(3) 0.007(3) -0.009(3) C10A 0.037(3) 0.045(3) 0.058(4) -0.003(3) -0.014(3) -0.009(3) C11A 0.043(3) 0.046(3) 0.042(3) -0.009(3) -0.004(3) -0.009(3) C12A 0.036(3) 0.035(3) 0.038(3) -0.005(2) 0.006(3) -0.003(2) C13A 0.072(5) 0.044(4) 0.061(4) -0.016(3) -0.001(4) -0.006(3) C14A 0.152(9) 0.059(5) 0.098(7) -0.001(5) 0.038(7) -0.021(6) C15A 0.044(4) 0.084(5) 0.042(4) -0.004(3) 0.009(3) 0.014(3) C16A 0.058(4) 0.109(6) 0.058(5) 0.010(4) 0.010(4) 0.024(4) C17A 0.069(4) 0.044(4) 0.051(4) 0.001(3) 0.012(3) 0.009(3) C18A 0.091(6) 0.073(5) 0.053(5) 0.008(4) -0.004(4) 0.015(4) Ga1B 0.0486(4) 0.0388(4) 0.0388(4) -0.0013(3) 0.0026(3) 0.0076(3) N1B 0.031(2) 0.035(3) 0.047(3) 0.010(2) 0.004(2) 0.004(2) C1B 0.030(3) 0.040(3) 0.041(3) 0.011(3) 0.010(2) 0.008(2) C2B 0.042(3) 0.044(3) 0.052(4) 0.005(3) 0.008(3) 0.011(3) C3B 0.046(4) 0.048(4) 0.057(4) 0.019(3) 0.011(3) 0.019(3) C4B 0.035(3) 0.079(5) 0.050(4) 0.027(4) 0.005(3) 0.011(3) C5B 0.036(3) 0.059(4) 0.042(3) 0.009(3) 0.004(3) -0.004(3) C6B 0.026(3) 0.048(3) 0.044(3) 0.010(3) 0.014(2) -0.001(3) C7B 0.029(3) 0.045(3) 0.040(3) 0.009(3) 0.009(2) -0.002(2) C8B 0.043(3) 0.051(4) 0.046(4) 0.005(3) 0.012(3) -0.009(3) C9B 0.048(4) 0.040(3) 0.058(4) 0.002(3) 0.009(3) 0.001(3) C10B 0.048(4) 0.044(4) 0.052(4) 0.016(3) 0.013(3) 0.007(3) C11B 0.032(3) 0.042(3) 0.055(4) 0.009(3) 0.002(3) 0.011(3) C12B 0.029(3) 0.040(3) 0.043(3) 0.009(3) 0.009(2) 0.003(2) C13B 0.041(3) 0.043(3) 0.049(4) -0.004(3) -0.005(3) -0.002(3) C14B 0.066(4) 0.036(3) 0.061(4) -0.001(3) -0.003(3) -0.008(3) C15B 0.074(5) 0.064(5) 0.040(4) 0.006(3) -0.004(3) 0.004(4) C16B 0.074(6) 0.155(10) 0.133(9) 0.078(8) -0.009(6) 0.000(6) C17B 0.138(8) 0.070(5) 0.059(5) -0.008(4) 0.011(5) 0.048(5) _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 O8 2.422(4) . ? Ca1 O7 2.437(4) . ? Ca1 O2 2.444(4) . ? Ca1 O1 2.473(4) . ? Ca1 O5 2.471(4) . ? Ca1 O4 2.481(4) . ? Ca1 O6 2.492(4) . ? Ca1 O3 2.498(4) . ? O1 C2 1.398(7) . ? O1 C1 1.425(7) . ? O2 C3 1.408(7) . ? O2 C4 1.452(7) . ? O3 C6 1.423(7) . ? O3 C5 1.440(7) . ? O4 C8 1.432(7) . ? O4 C7 1.433(7) . ? O5 C10 1.406(7) . ? O5 C9 1.447(7) . ? O6 C11 1.420(7) . ? O6 C12 1.438(7) . ? O7 C14 1.431(7) . ? O7 C13 1.429(6) . ? O8 C15 1.421(7) . ? O8 C16 1.426(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.399(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.483(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.423(10) . ? C10 H10C 0.9900 . ? C10 H10D 0.9900 . ? C11 H11C 0.9900 . ? C11 H11D 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? C13 H13G 0.9800 . ? C14 C15 1.410(9) . ? C14 H14G 0.9900 . ? C14 H14H 0.9900 . ? C15 H15E 0.9900 . ? C15 H15F 0.9900 . ? C16 H16G 0.9800 . ? C16 H16H 0.9800 . ? C16 H16I 0.9800 . ? Ga1A C15A 2.003(6) . ? Ga1A C13A 2.003(6) . ? Ga1A C17A 2.013(6) . ? Ga1A N1A 2.012(4) . ? N1A C1A 1.382(7) . ? N1A C12A 1.391(7) . ? C1A C2A 1.405(8) . ? C1A C6A 1.412(8) . ? C2A C3A 1.390(8) . ? C2A H2AA 0.9500 . ? C3A C4A 1.377(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.403(8) . ? C4A H4AA 0.9500 . ? C5A C6A 1.422(8) . ? C5A H5AA 0.9500 . ? C6A C7A 1.429(8) . ? C7A C8A 1.396(8) . ? C7A C12A 1.429(8) . ? C8A C9A 1.365(8) . ? C8A H8AA 0.9500 . ? C9A C10A 1.414(9) . ? C9A H9AA 0.9500 . ? C10A C11A 1.377(8) . ? C10A H10A 0.9500 . ? C11A C12A 1.384(8) . ? C11A H11A 0.9500 . ? C13A C14A 1.538(11) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A C16A 1.553(9) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A C18A 1.527(10) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? Ga1B C15B 2.000(7) . ? Ga1B C17B 1.996(7) . ? Ga1B C13B 2.018(6) . ? Ga1B N1B 2.039(5) . ? N1B C1B 1.385(7) . ? N1B C12B 1.387(7) . ? C1B C6B 1.400(8) . ? C1B C2B 1.414(8) . ? C2B C3B 1.371(8) . ? C2B H2BA 0.9500 . ? C3B C4B 1.371(9) . ? C3B H3BA 0.9500 . ? C4B C5B 1.392(9) . ? C4B H4BA 0.9500 . ? C5B C6B 1.413(8) . ? C5B H5BA 0.9500 . ? C6B C7B 1.443(8) . ? C7B C12B 1.403(8) . ? C7B C8B 1.413(8) . ? C8B C9B 1.379(8) . ? C8B H8BA 0.9500 . ? C9B C10B 1.383(9) . ? C9B H9BA 0.9500 . ? C10B C11B 1.398(8) . ? C10B H10B 0.9500 . ? C11B C12B 1.423(7) . ? C11B H11B 0.9500 . ? C13B C14B 1.520(8) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B C16B 1.474(11) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B C18B 1.332(13) . ? C17B C18C 1.452(19) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C17B H17E 0.9900 . ? C17B H17F 0.9900 . ? C18B H17E 1.2054 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C18C H18G 0.9800 . ? C18C H18H 0.9800 . ? C18C H18I 0.9800 . ? C1T C2T 1.3900 . ? C1T C6T 1.3900 . ? C1T C7T 1.513(3) . ? C2T C3T 1.3900 . ? C2T H2TA 0.9500 . ? C3T C4T 1.3900 . ? C3T H3TA 0.9500 . ? C4T C5T 1.3900 . ? C4T H4TA 0.9500 . ? C5T C6T 1.3900 . ? C5T H5TA 0.9500 . ? C6T H6TA 0.9500 . ? C7T H7TA 0.9800 . ? C7T H7TB 0.9800 . ? C7T H7TC 0.9800 . ? 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 O8 Ca1 O7 67.22(12) . . ? O8 Ca1 O2 123.15(12) . . ? O7 Ca1 O2 154.93(13) . . ? O8 Ca1 O1 74.63(12) . . ? O7 Ca1 O1 100.06(13) . . ? O2 Ca1 O1 65.34(12) . . ? O8 Ca1 O5 81.70(12) . . ? O7 Ca1 O5 75.72(13) . . ? O2 Ca1 O5 126.10(13) . . ? O1 Ca1 O5 155.57(13) . . ? O8 Ca1 O4 157.08(13) . . ? O7 Ca1 O4 100.64(13) . . ? O2 Ca1 O4 76.23(13) . . ? O1 Ca1 O4 127.84(13) . . ? O5 Ca1 O4 76.32(12) . . ? O8 Ca1 O6 77.91(13) . . ? O7 Ca1 O6 130.56(13) . . ? O2 Ca1 O6 74.15(13) . . ? O1 Ca1 O6 103.28(14) . . ? O5 Ca1 O6 65.20(13) . . ? O4 Ca1 O6 98.36(13) . . ? O8 Ca1 O3 125.52(13) . . ? O7 Ca1 O3 74.05(13) . . ? O2 Ca1 O3 82.40(13) . . ? O1 Ca1 O3 76.15(13) . . ? O5 Ca1 O3 124.01(13) . . ? O4 Ca1 O3 64.63(12) . . ? O6 Ca1 O3 154.00(14) . . ? C2 O1 C1 113.8(4) . . ? C2 O1 Ca1 117.9(4) . . ? C1 O1 Ca1 127.3(3) . . ? C3 O2 C4 113.7(5) . . ? C3 O2 Ca1 118.8(3) . . ? C4 O2 Ca1 126.2(3) . . ? C6 O3 C5 112.2(4) . . ? C6 O3 Ca1 115.5(3) . . ? C5 O3 Ca1 128.5(3) . . ? C8 O4 C7 111.1(4) . . ? C8 O4 Ca1 127.5(3) . . ? C7 O4 Ca1 119.9(3) . . ? C10 O5 C9 112.2(5) . . ? C10 O5 Ca1 120.5(4) . . ? C9 O5 Ca1 126.9(4) . . ? C11 O6 C12 113.1(5) . . ? C11 O6 Ca1 115.2(4) . . ? C12 O6 Ca1 127.1(4) . . ? C14 O7 C13 111.3(4) . . ? C14 O7 Ca1 118.2(3) . . ? C13 O7 Ca1 129.8(3) . . ? C15 O8 C16 112.8(4) . . ? C15 O8 Ca1 116.9(3) . . ? C16 O8 Ca1 130.0(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 114.2(6) . . ? O1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? O1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 O2 112.8(6) . . ? C2 C3 H3A 109.0 . . ? O2 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? O2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? O2 C4 H4A 109.5 . . ? O2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 H5A 109.5 . . ? O3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 C7 108.3(5) . . ? O3 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? O3 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O4 C7 C6 109.1(4) . . ? O4 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O5 C10 C11 113.1(6) . . ? O5 C10 H10C 109.0 . . ? C11 C10 H10C 109.0 . . ? O5 C10 H10D 109.0 . . ? C11 C10 H10D 109.0 . . ? H10C C10 H10D 107.8 . . ? C10 C11 O6 114.0(6) . . ? C10 C11 H11C 108.7 . . ? O6 C11 H11C 108.7 . . ? C10 C11 H11D 108.7 . . ? O6 C11 H11D 108.7 . . ? H11C C11 H11D 107.6 . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 H13E 109.5 . . ? O7 C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? O7 C13 H13G 109.5 . . ? H13E C13 H13G 109.5 . . ? H13F C13 H13G 109.5 . . ? C15 C14 O7 114.1(5) . . ? C15 C14 H14G 108.7 . . ? O7 C14 H14G 108.7 . . ? C15 C14 H14H 108.7 . . ? O7 C14 H14H 108.7 . . ? H14G C14 H14H 107.6 . . ? C14 C15 O8 114.7(5) . . ? C14 C15 H15E 108.6 . . ? O8 C15 H15E 108.6 . . ? C14 C15 H15F 108.6 . . ? O8 C15 H15F 108.6 . . ? H15E C15 H15F 107.6 . . ? O8 C16 H16G 109.5 . . ? O8 C16 H16H 109.5 . . ? H16G C16 H16H 109.5 . . ? O8 C16 H16I 109.5 . . ? H16G C16 H16I 109.5 . . ? H16H C16 H16I 109.5 . . ? C15A Ga1A C13A 111.3(3) . . ? C15A Ga1A C17A 109.8(3) . . ? C13A Ga1A C17A 116.1(3) . . ? C15A Ga1A N1A 111.7(2) . . ? C13A Ga1A N1A 102.5(2) . . ? C17A Ga1A N1A 105.0(2) . . ? C1A N1A C12A 106.2(4) . . ? C1A N1A Ga1A 131.3(4) . . ? C12A N1A Ga1A 122.2(4) . . ? N1A C1A C2A 128.6(5) . . ? N1A C1A C6A 111.1(5) . . ? C2A C1A C6A 120.3(5) . . ? C3A C2A C1A 117.8(5) . . ? C3A C2A H2AA 121.1 . . ? C1A C2A H2AA 121.1 . . ? C4A C3A C2A 122.3(6) . . ? C4A C3A H3AA 118.8 . . ? C2A C3A H3AA 118.8 . . ? C3A C4A C5A 121.5(5) . . ? C3A C4A H4AA 119.2 . . ? C5A C4A H4AA 119.2 . . ? C4A C5A C6A 116.9(5) . . ? C4A C5A H5AA 121.6 . . ? C6A C5A H5AA 121.6 . . ? C1A C6A C5A 121.0(5) . . ? C1A C6A C7A 106.5(5) . . ? C5A C6A C7A 132.4(5) . . ? C8A C7A C12A 119.7(5) . . ? C8A C7A C6A 134.6(5) . . ? C12A C7A C6A 105.7(5) . . ? C9A C8A C7A 119.5(5) . . ? C9A C8A H8AA 120.3 . . ? C7A C8A H8AA 120.3 . . ? C8A C9A C10A 120.8(6) . . ? C8A C9A H9AA 119.6 . . ? C10A C9A H9AA 119.6 . . ? C11A C10A C9A 120.5(6) . . ? C11A C10A H10A 119.7 . . ? C9A C10A H10A 119.7 . . ? C10A C11A C12A 119.4(6) . . ? C10A C11A H11A 120.3 . . ? C12A C11A H11A 120.3 . . ? C11A C12A N1A 129.5(5) . . ? C11A C12A C7A 120.0(5) . . ? N1A C12A C7A 110.5(5) . . ? C14A C13A Ga1A 111.3(5) . . ? C14A C13A H13A 109.4 . . ? Ga1A C13A H13A 109.4 . . ? C14A C13A H13B 109.4 . . ? Ga1A C13A H13B 109.4 . . ? H13A C13A H13B 108.0 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C16A C15A Ga1A 110.3(5) . . ? C16A C15A H15A 109.6 . . ? Ga1A C15A H15A 109.6 . . ? C16A C15A H15B 109.6 . . ? Ga1A C15A H15B 109.6 . . ? H15A C15A H15B 108.1 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C18A C17A Ga1A 114.9(5) . . ? C18A C17A H17A 108.6 . . ? Ga1A C17A H17A 108.6 . . ? C18A C17A H17B 108.6 . . ? Ga1A C17A H17B 108.6 . . ? H17A C17A H17B 107.5 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C15B Ga1B C17B 109.7(3) . . ? C15B Ga1B C13B 112.4(3) . . ? C17B Ga1B C13B 115.5(3) . . ? C15B Ga1B N1B 107.5(3) . . ? C17B Ga1B N1B 107.9(3) . . ? C13B Ga1B N1B 103.2(2) . . ? C1B N1B C12B 105.0(5) . . ? C1B N1B Ga1B 128.8(4) . . ? C12B N1B Ga1B 126.2(4) . . ? N1B C1B C6B 111.7(5) . . ? N1B C1B C2B 128.3(5) . . ? C6B C1B C2B 119.9(5) . . ? C3B C2B C1B 118.0(6) . . ? C3B C2B H2BA 121.0 . . ? C1B C2B H2BA 121.0 . . ? C4B C3B C2B 122.6(6) . . ? C4B C3B H3BA 118.7 . . ? C2B C3B H3BA 118.7 . . ? C3B C4B C5B 120.9(6) . . ? C3B C4B H4BA 119.5 . . ? C5B C4B H4BA 119.5 . . ? C4B C5B C6B 117.8(6) . . ? C4B C5B H5BA 121.1 . . ? C6B C5B H5BA 121.1 . . ? C1B C6B C5B 120.7(5) . . ? C1B C6B C7B 106.0(5) . . ? C5B C6B C7B 133.1(6) . . ? C12B C7B C8B 120.7(5) . . ? C12B C7B C6B 105.2(5) . . ? C8B C7B C6B 134.0(5) . . ? C9B C8B C7B 118.4(6) . . ? C9B C8B H8BA 120.8 . . ? C7B C8B H8BA 120.8 . . ? C8B C9B C10B 121.5(6) . . ? C8B C9B H9BA 119.2 . . ? C10B C9B H9BA 119.2 . . ? C9B C10B C11B 121.7(6) . . ? C9B C10B H10B 119.2 . . ? C11B C10B H10B 119.2 . . ? C10B C11B C12B 117.5(6) . . ? C10B C11B H11B 121.2 . . ? C12B C11B H11B 121.2 . . ? N1B C12B C7B 112.0(5) . . ? N1B C12B C11B 127.8(5) . . ? C7B C12B C11B 120.2(5) . . ? C14B C13B Ga1B 115.7(4) . . ? C14B C13B H13C 108.4 . . ? Ga1B C13B H13C 108.4 . . ? C14B C13B H13D 108.4 . . ? Ga1B C13B H13D 108.4 . . ? H13C C13B H13D 107.4 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C16B C15B Ga1B 113.2(6) . . ? C16B C15B H15C 108.9 . . ? Ga1B C15B H15C 108.9 . . ? C16B C15B H15D 108.9 . . ? Ga1B C15B H15D 108.9 . . ? H15C C15B H15D 107.7 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18B C17B C18C 48.8(8) . . ? C18B C17B Ga1B 120.0(8) . . ? C18C C17B Ga1B 118.0(8) . . ? C18B C17B H17C 107.3 . . ? C18C C17B H17C 134.7 . . ? Ga1B C17B H17C 107.3 . . ? C18B C17B H17D 107.3 . . ? C18C C17B H17D 61.5 . . ? Ga1B C17B H17D 107.3 . . ? H17C C17B H17D 106.9 . . ? C18B C17B H17E 60.4 . . ? C18C C17B H17E 107.5 . . ? Ga1B C17B H17E 108.0 . . ? H17C C17B H17E 54.1 . . ? H17D C17B H17E 143.8 . . ? C18B C17B H17F 131.8 . . ? C18C C17B H17F 107.6 . . ? Ga1B C17B H17F 108.2 . . ? H17C C17B H17F 55.6 . . ? H17D C17B H17F 53.1 . . ? H17E C17B H17F 107.1 . . ? C17B C18B H17E 45.6 . . ? C17B C18B H18D 109.5 . . ? H17E C18B H18D 144.3 . . ? C17B C18B H18E 109.5 . . ? H17E C18B H18E 104.0 . . ? C17B C18B H18F 109.5 . . ? H17E C18B H18F 69.3 . . ? C17B C18C H18G 109.5 . . ? C17B C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? C17B C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? C2T C1T C6T 120.0 . . ? C2T C1T C7T 120.5(2) . . ? C6T C1T C7T 119.4(2) . . ? C3T C2T C1T 120.0 . . ? C3T C2T H2TA 120.0 . . ? C1T C2T H2TA 120.0 . . ? C4T C3T C2T 120.0 . . ? C4T C3T H3TA 120.0 . . ? C2T C3T H3TA 120.0 . . ? C3T C4T C5T 120.0 . . ? C3T C4T H4TA 120.0 . . ? C5T C4T H4TA 120.0 . . ? C4T C5T C6T 120.0 . . ? C4T C5T H5TA 120.0 . . ? C6T C5T H5TA 120.0 . . ? C5T C6T C1T 120.0 . . ? C5T C6T C7T 151.69(12) . . ? C1T C6T C7T 31.70(12) . . ? C5T C6T H6TA 120.0 . . ? C1T C6T H6TA 120.0 . . ? C7T C6T H6TA 88.3 . . ? C1T C7T C6T 28.85(11) . . ? C1T C7T H7TA 109.5 . . ? C6T C7T H7TA 138.3 . . ? C1T C7T H7TB 109.5 . . ? C6T C7T H7TB 93.8 . . ? H7TA C7T H7TB 109.5 . . ? C1T C7T H7TC 109.5 . . ? C6T C7T H7TC 93.6 . . ? H7TA C7T H7TC 109.5 . . ? H7TB C7T H7TC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.623 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.129 #==== END data_FO2960 _database_code_depnum_ccdc_archive 'CCDC 765647' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 V, C16 H32 Li O4, C4 H8 O' _chemical_formula_sum 'C56 H84 Li O5 V' _chemical_formula_weight 895.11 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.8019(5) _cell_length_b 17.3641(7) _cell_length_c 17.9993(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.473(2) _cell_angle_gamma 90.00 _cell_volume 5227.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 35187 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour green/pink _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35187 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.1129 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11904 _reflns_number_gt 6242 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0934P)^2^+0.3636P] 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 11904 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1503 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.011 _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 V V 0.77479(3) 0.77168(3) 0.50318(3) 0.02835(15) Uani 1 1 d . . . C1 C 0.69112(18) 0.68859(19) 0.53733(17) 0.0350(7) Uani 1 1 d . . . C2 C 0.64892(18) 0.71290(19) 0.59815(17) 0.0367(8) Uani 1 1 d . . . C3 C 0.59179(19) 0.6656(2) 0.62716(19) 0.0463(9) Uani 1 1 d . . . H3A H 0.5654 0.6835 0.6683 0.056 Uiso 1 1 calc R . . C4 C 0.5727(2) 0.5939(2) 0.5979(2) 0.0517(10) Uani 1 1 d . . . C5 C 0.6118(2) 0.5701(2) 0.5382(2) 0.0512(10) Uani 1 1 d . . . H5A H 0.5990 0.5210 0.5169 0.061 Uiso 1 1 calc R . . C6 C 0.67011(19) 0.61529(19) 0.50735(19) 0.0403(8) Uani 1 1 d . . . C7 C 0.6632(2) 0.7913(2) 0.63324(19) 0.0432(8) Uani 1 1 d . . . H7A H 0.6576 0.7881 0.6868 0.065 Uiso 1 1 calc R . . H7B H 0.6240 0.8280 0.6100 0.065 Uiso 1 1 calc R . . H7C H 0.7173 0.8088 0.6256 0.065 Uiso 1 1 calc R . . C8 C 0.5123(2) 0.5428(3) 0.6319(3) 0.0759(14) Uani 1 1 d . . . H8A H 0.5050 0.4951 0.6029 0.114 Uiso 1 1 calc R . . H8B H 0.4611 0.5699 0.6312 0.114 Uiso 1 1 calc R . . H8C H 0.5319 0.5305 0.6835 0.114 Uiso 1 1 calc R . . C9 C 0.7090(2) 0.5808(2) 0.4429(2) 0.0496(9) Uani 1 1 d . . . H9A H 0.7465 0.6181 0.4247 0.074 Uiso 1 1 calc R . . H9B H 0.6679 0.5679 0.4025 0.074 Uiso 1 1 calc R . . H9C H 0.7381 0.5340 0.4595 0.074 Uiso 1 1 calc R . . C10 C 0.85629(17) 0.73344(18) 0.42593(16) 0.0312(7) Uani 1 1 d . . . C11 C 0.90490(17) 0.67021(18) 0.44971(17) 0.0334(7) Uani 1 1 d . . . C12 C 0.96462(18) 0.64248(19) 0.40797(18) 0.0382(8) Uani 1 1 d . . . H12A H 0.9950 0.5989 0.4254 0.046 Uiso 1 1 calc R . . C13 C 0.98050(18) 0.6771(2) 0.34175(18) 0.0389(8) Uani 1 1 d . . . C14 C 0.93483(19) 0.74023(19) 0.31803(17) 0.0368(8) Uani 1 1 d . . . H14A H 0.9454 0.7654 0.2732 0.044 Uiso 1 1 calc R . . C15 C 0.87329(18) 0.76821(18) 0.35823(16) 0.0320(7) Uani 1 1 d . . . C16 C 0.89486(19) 0.63021(19) 0.52319(18) 0.0398(8) Uani 1 1 d . . . H16A H 0.9113 0.5762 0.5201 0.060 Uiso 1 1 calc R . . H16B H 0.8387 0.6326 0.5334 0.060 Uiso 1 1 calc R . . H16C H 0.9281 0.6559 0.5635 0.060 Uiso 1 1 calc R . . C17 C 1.0450(2) 0.6455(2) 0.2966(2) 0.0552(10) Uani 1 1 d . . . H17A H 1.0705 0.6009 0.3224 0.083 Uiso 1 1 calc R . . H17B H 1.0853 0.6854 0.2910 0.083 Uiso 1 1 calc R . . H17C H 1.0210 0.6297 0.2472 0.083 Uiso 1 1 calc R . . C18 C 0.8275(2) 0.83649(19) 0.32466(18) 0.0400(8) Uani 1 1 d . . . H18A H 0.8490 0.8512 0.2780 0.060 Uiso 1 1 calc R . . H18B H 0.8329 0.8798 0.3597 0.060 Uiso 1 1 calc R . . H18C H 0.7709 0.8228 0.3145 0.060 Uiso 1 1 calc R . . C19 C 0.86409(17) 0.80896(17) 0.58937(16) 0.0304(7) Uani 1 1 d . . . C20 C 0.88430(17) 0.77698(18) 0.66098(16) 0.0316(7) Uani 1 1 d . . . C21 C 0.94558(18) 0.80827(18) 0.71018(17) 0.0348(7) Uani 1 1 d . . . H21A H 0.9569 0.7854 0.7580 0.042 Uiso 1 1 calc R . . C22 C 0.99013(17) 0.87101(18) 0.69176(17) 0.0327(7) Uani 1 1 d . . . C23 C 0.97188(17) 0.90228(18) 0.62103(17) 0.0319(7) Uani 1 1 d . . . H23A H 1.0018 0.9452 0.6064 0.038 Uiso 1 1 calc R . . C24 C 0.91143(17) 0.87281(17) 0.57101(16) 0.0292(7) Uani 1 1 d . . . C25 C 0.8416(2) 0.70773(19) 0.68970(18) 0.0408(8) Uani 1 1 d . . . H25A H 0.8566 0.7019 0.7434 0.061 Uiso 1 1 calc R . . H25B H 0.8570 0.6613 0.6635 0.061 Uiso 1 1 calc R . . H25C H 0.7837 0.7152 0.6808 0.061 Uiso 1 1 calc R . . C26 C 1.05639(19) 0.9037(2) 0.74490(19) 0.0414(8) Uani 1 1 d . . . H26A H 1.0452 0.8932 0.7964 0.062 Uiso 1 1 calc R . . H26B H 1.0598 0.9594 0.7374 0.062 Uiso 1 1 calc R . . H26C H 1.1072 0.8796 0.7355 0.062 Uiso 1 1 calc R . . C27 C 0.89936(19) 0.91007(19) 0.49520(17) 0.0377(8) Uani 1 1 d . . . H27A H 0.9150 0.9644 0.4993 0.057 Uiso 1 1 calc R . . H27B H 0.8429 0.9063 0.4760 0.057 Uiso 1 1 calc R . . H27C H 0.9323 0.8837 0.4610 0.057 Uiso 1 1 calc R . . C28 C 0.68835(17) 0.85538(17) 0.46046(16) 0.0300(7) Uani 1 1 d . . . C29 C 0.67026(17) 0.92802(18) 0.49004(16) 0.0316(7) Uani 1 1 d . . . C30 C 0.60560(18) 0.97193(19) 0.45825(18) 0.0374(8) Uani 1 1 d . . . H30A H 0.5950 1.0203 0.4800 0.045 Uiso 1 1 calc R . . C31 C 0.55687(18) 0.9477(2) 0.39682(18) 0.0380(8) Uani 1 1 d . . . C32 C 0.57401(18) 0.87659(19) 0.36668(17) 0.0364(8) Uani 1 1 d . . . H32A H 0.5420 0.8586 0.3238 0.044 Uiso 1 1 calc R . . C33 C 0.63692(17) 0.83099(18) 0.39771(16) 0.0316(7) Uani 1 1 d . . . C34 C 0.71925(19) 0.96319(19) 0.55631(17) 0.0388(8) Uani 1 1 d . . . H34A H 0.6967 1.0134 0.5678 0.058 Uiso 1 1 calc R . . H34B H 0.7746 0.9699 0.5445 0.058 Uiso 1 1 calc R . . H34C H 0.7182 0.9291 0.5996 0.058 Uiso 1 1 calc R . . C35 C 0.4870(2) 0.9949(2) 0.3634(2) 0.0532(10) Uani 1 1 d . . . H35A H 0.4844 1.0433 0.3911 0.080 Uiso 1 1 calc R . . H35B H 0.4373 0.9660 0.3664 0.080 Uiso 1 1 calc R . . H35C H 0.4938 1.0061 0.3110 0.080 Uiso 1 1 calc R . . C36 C 0.6469(2) 0.7530(2) 0.36268(18) 0.0414(8) Uani 1 1 d . . . H36A H 0.6297 0.7556 0.3092 0.062 Uiso 1 1 calc R . . H36B H 0.6142 0.7150 0.3863 0.062 Uiso 1 1 calc R . . H36C H 0.7032 0.7376 0.3699 0.062 Uiso 1 1 calc R . . Li Li 0.7373(3) 0.7162(3) 0.0575(3) 0.0427(13) Uani 1 1 d . . . O1 O 0.67577(15) 0.80168(15) 0.08746(16) 0.0584(7) Uani 1 1 d . . . O2 O 0.73817(14) 0.64053(13) 0.13686(12) 0.0432(6) Uani 1 1 d . . . O3 O 0.84586(14) 0.74725(14) 0.04692(14) 0.0479(6) Uani 1 1 d . . . O4 O 0.68860(15) 0.67547(16) -0.03562(13) 0.0559(7) Uani 1 1 d . . . C37 C 0.6883(3) 0.8801(2) 0.0710(3) 0.097(2) Uani 1 1 d . . . H37A H 0.6886 0.8873 0.0165 0.116 Uiso 1 1 calc R . . H37B H 0.7405 0.8975 0.0956 0.116 Uiso 1 1 calc R . . C38 C 0.6223(3) 0.9255(2) 0.0991(3) 0.0674(12) Uani 1 1 d . . . H38A H 0.5796 0.9361 0.0586 0.081 Uiso 1 1 calc R . . H38B H 0.6422 0.9749 0.1211 0.081 Uiso 1 1 calc R . . C39 C 0.5927(2) 0.8735(3) 0.1576(2) 0.0612(11) Uani 1 1 d . . . H39A H 0.6241 0.8806 0.2065 0.073 Uiso 1 1 calc R . . H39B H 0.5355 0.8827 0.1633 0.073 Uiso 1 1 calc R . . C40 C 0.6056(2) 0.7950(3) 0.1264(3) 0.0713(13) Uani 1 1 d . . . H40A H 0.6138 0.7565 0.1669 0.086 Uiso 1 1 calc R . . H40B H 0.5591 0.7792 0.0919 0.086 Uiso 1 1 calc R . . C41 C 0.7812(2) 0.6585(2) 0.20779(18) 0.0444(8) Uani 1 1 d . . . H41A H 0.7439 0.6749 0.2441 0.053 Uiso 1 1 calc R . . H41B H 0.8203 0.7002 0.2023 0.053 Uiso 1 1 calc R . . C42 C 0.8231(2) 0.5856(2) 0.2330(2) 0.0581(10) Uani 1 1 d . . . H42A H 0.8319 0.5831 0.2881 0.070 Uiso 1 1 calc R . . H42B H 0.8752 0.5808 0.2119 0.070 Uiso 1 1 calc R . . C43 C 0.7655(2) 0.5243(2) 0.2026(2) 0.0530(10) Uani 1 1 d . . . H43A H 0.7942 0.4762 0.1924 0.064 Uiso 1 1 calc R . . H43B H 0.7255 0.5130 0.2381 0.064 Uiso 1 1 calc R . . C44 C 0.7263(2) 0.5585(2) 0.1316(2) 0.0464(9) Uani 1 1 d . . . H44A H 0.7509 0.5377 0.0879 0.056 Uiso 1 1 calc R . . H44B H 0.6685 0.5463 0.1259 0.056 Uiso 1 1 calc R . . C45 C 0.9138(2) 0.6981(2) 0.0663(2) 0.0577(10) Uani 1 1 d . . . H45A H 0.8962 0.6456 0.0786 0.069 Uiso 1 1 calc R . . H45B H 0.9474 0.7190 0.1098 0.069 Uiso 1 1 calc R . . C46 C 0.9590(2) 0.6966(3) -0.0010(2) 0.0616(11) Uani 1 1 d . . . H46A H 0.9390 0.6552 -0.0358 0.074 Uiso 1 1 calc R . . H46B H 1.0168 0.6886 0.0130 0.074 Uiso 1 1 calc R . . C47 C 0.9438(2) 0.7747(3) -0.0359(2) 0.0620(11) Uani 1 1 d . . . H47A H 0.9280 0.7700 -0.0901 0.074 Uiso 1 1 calc R . . H47B H 0.9921 0.8074 -0.0283 0.074 Uiso 1 1 calc R . . C48 C 0.8756(2) 0.8089(2) 0.0040(2) 0.0568(10) Uani 1 1 d . . . H48A H 0.8955 0.8517 0.0371 0.068 Uiso 1 1 calc R . . H48B H 0.8329 0.8288 -0.0326 0.068 Uiso 1 1 calc R . . C49 C 0.7182(3) 0.6867(3) -0.1065(2) 0.0634(11) Uani 1 1 d . . . H49A H 0.7698 0.6595 -0.1084 0.076 Uiso 1 1 calc R . . H49B H 0.7268 0.7422 -0.1154 0.076 Uiso 1 1 calc R . . C50 C 0.6573(3) 0.6552(3) -0.1637(2) 0.0811(14) Uani 1 1 d . . . H50A H 0.6821 0.6181 -0.1964 0.097 Uiso 1 1 calc R . . H50B H 0.6323 0.6972 -0.1950 0.097 Uiso 1 1 calc R . . C51 C 0.5965(2) 0.6159(2) -0.1215(2) 0.0622(11) Uani 1 1 d . . . H51A H 0.6085 0.5603 -0.1152 0.075 Uiso 1 1 calc R . . H51B H 0.5420 0.6221 -0.1469 0.075 Uiso 1 1 calc R . . C52 C 0.6050(2) 0.6569(3) -0.0480(2) 0.0606(11) Uani 1 1 d . . . H52A H 0.5720 0.7042 -0.0501 0.073 Uiso 1 1 calc R . . H52B H 0.5886 0.6233 -0.0077 0.073 Uiso 1 1 calc R . . O1T O 0.25411(18) 0.0898(2) 0.12621(16) 0.0790(9) Uani 1 1 d . . . C1T C 0.2886(3) 0.0160(3) 0.1440(3) 0.0738(14) Uani 1 1 d . . . H1TA H 0.3456 0.0150 0.1344 0.089 Uiso 1 1 calc R . . H1TB H 0.2598 -0.0249 0.1139 0.089 Uiso 1 1 calc R . . C2T C 0.2800(3) 0.0048(3) 0.2253(3) 0.0871(16) Uani 1 1 d . . . H2TA H 0.2763 -0.0506 0.2375 0.104 Uiso 1 1 calc R . . H2TB H 0.3259 0.0275 0.2563 0.104 Uiso 1 1 calc R . . C3T C 0.2050(3) 0.0452(3) 0.2378(2) 0.0680(12) Uani 1 1 d . . . H3TA H 0.2085 0.0690 0.2880 0.082 Uiso 1 1 calc R . . H3TB H 0.1589 0.0095 0.2326 0.082 Uiso 1 1 calc R . . C4T C 0.1974(3) 0.1049(3) 0.1785(2) 0.0727(13) Uani 1 1 d . . . H4TA H 0.1426 0.1042 0.1528 0.087 Uiso 1 1 calc R . . H4TB H 0.2073 0.1565 0.2009 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 V 0.0261(3) 0.0317(3) 0.0279(3) -0.0002(2) 0.0057(2) 0.0011(2) C1 0.0295(16) 0.0387(19) 0.0360(17) 0.0040(14) -0.0019(14) 0.0004(14) C2 0.0281(16) 0.049(2) 0.0334(17) 0.0082(15) 0.0032(13) -0.0021(14) C3 0.0325(18) 0.064(3) 0.042(2) 0.0165(18) 0.0042(15) 0.0013(17) C4 0.0344(19) 0.060(3) 0.059(2) 0.024(2) -0.0007(18) -0.0101(17) C5 0.045(2) 0.042(2) 0.063(2) 0.0152(18) -0.0132(19) -0.0082(17) C6 0.0382(18) 0.0350(19) 0.046(2) 0.0062(15) -0.0055(15) -0.0006(15) C7 0.0378(18) 0.054(2) 0.0400(19) -0.0021(16) 0.0145(15) -0.0019(16) C8 0.051(2) 0.092(3) 0.084(3) 0.040(3) 0.000(2) -0.026(2) C9 0.050(2) 0.041(2) 0.056(2) -0.0063(17) -0.0023(18) 0.0009(17) C10 0.0277(15) 0.0335(17) 0.0324(16) -0.0056(14) 0.0026(13) -0.0027(13) C11 0.0311(16) 0.0333(18) 0.0363(17) -0.0040(14) 0.0057(14) 0.0004(13) C12 0.0314(16) 0.0379(19) 0.0454(19) -0.0076(15) 0.0048(15) 0.0028(14) C13 0.0264(16) 0.047(2) 0.0447(19) -0.0129(16) 0.0096(14) -0.0019(15) C14 0.0373(17) 0.044(2) 0.0303(16) -0.0049(14) 0.0090(14) -0.0064(15) C15 0.0322(16) 0.0353(17) 0.0290(15) -0.0029(14) 0.0049(13) -0.0011(14) C16 0.0367(18) 0.0407(19) 0.0423(19) 0.0056(15) 0.0064(15) 0.0081(15) C17 0.044(2) 0.069(3) 0.055(2) -0.011(2) 0.0215(18) 0.0051(19) C18 0.0472(19) 0.0394(19) 0.0348(17) 0.0020(15) 0.0108(15) 0.0004(15) C19 0.0276(15) 0.0309(17) 0.0332(16) 0.0004(13) 0.0057(13) 0.0049(13) C20 0.0303(15) 0.0339(17) 0.0309(16) -0.0019(14) 0.0049(13) 0.0029(13) C21 0.0352(17) 0.0375(18) 0.0325(17) 0.0020(14) 0.0063(14) 0.0086(14) C22 0.0249(15) 0.0370(18) 0.0367(17) -0.0060(14) 0.0049(13) 0.0072(13) C23 0.0279(15) 0.0301(17) 0.0389(18) -0.0041(14) 0.0085(14) 0.0012(13) C24 0.0288(15) 0.0289(17) 0.0301(16) 0.0006(13) 0.0049(13) 0.0058(13) C25 0.0426(19) 0.041(2) 0.0391(18) 0.0067(15) 0.0050(15) -0.0044(15) C26 0.0350(18) 0.042(2) 0.046(2) -0.0074(16) -0.0029(15) 0.0055(15) C27 0.0353(17) 0.0401(19) 0.0373(18) 0.0028(14) 0.0016(14) -0.0042(14) C28 0.0253(15) 0.0349(17) 0.0310(16) 0.0017(13) 0.0094(13) 0.0014(13) C29 0.0271(15) 0.0378(18) 0.0307(16) 0.0006(14) 0.0067(13) 0.0024(13) C30 0.0347(17) 0.0369(19) 0.0420(19) 0.0014(15) 0.0103(15) 0.0059(14) C31 0.0264(16) 0.047(2) 0.0417(19) 0.0117(16) 0.0105(15) 0.0084(14) C32 0.0290(16) 0.050(2) 0.0298(16) 0.0054(15) 0.0016(13) -0.0007(15) C33 0.0263(15) 0.0404(18) 0.0290(16) -0.0007(13) 0.0068(13) 0.0003(13) C34 0.0399(18) 0.0387(19) 0.0384(18) -0.0051(15) 0.0074(15) 0.0033(15) C35 0.0361(19) 0.070(3) 0.053(2) 0.011(2) 0.0031(17) 0.0125(18) C36 0.0403(18) 0.050(2) 0.0333(17) -0.0077(15) -0.0019(15) -0.0018(15) Li 0.037(3) 0.048(4) 0.042(3) 0.005(3) 0.004(2) -0.003(3) O1 0.0528(15) 0.0440(15) 0.0831(19) 0.0136(13) 0.0317(14) 0.0055(12) O2 0.0502(14) 0.0377(13) 0.0401(13) -0.0020(10) -0.0048(11) -0.0045(11) O3 0.0388(13) 0.0486(15) 0.0585(15) 0.0056(12) 0.0156(12) 0.0032(11) O4 0.0510(15) 0.0726(18) 0.0434(14) 0.0022(13) 0.0003(12) -0.0152(13) C37 0.123(4) 0.044(3) 0.137(5) 0.022(3) 0.083(4) 0.015(3) C38 0.082(3) 0.048(2) 0.075(3) -0.004(2) 0.022(2) 0.007(2) C39 0.057(2) 0.081(3) 0.047(2) -0.006(2) 0.0149(19) 0.003(2) C40 0.054(2) 0.072(3) 0.092(3) 0.013(3) 0.033(2) 0.006(2) C41 0.050(2) 0.045(2) 0.0380(18) -0.0078(16) 0.0019(16) -0.0077(17) C42 0.053(2) 0.061(3) 0.059(2) 0.006(2) -0.0052(19) -0.007(2) C43 0.048(2) 0.042(2) 0.069(3) 0.0032(19) 0.0025(19) -0.0003(17) C44 0.049(2) 0.042(2) 0.049(2) -0.0107(17) 0.0078(17) -0.0048(16) C45 0.049(2) 0.058(3) 0.067(3) 0.010(2) 0.014(2) 0.0129(19) C46 0.047(2) 0.076(3) 0.065(3) 0.005(2) 0.019(2) 0.011(2) C47 0.053(2) 0.076(3) 0.060(2) 0.008(2) 0.020(2) -0.005(2) C48 0.054(2) 0.050(2) 0.067(3) 0.008(2) 0.011(2) -0.0062(19) C49 0.069(3) 0.075(3) 0.047(2) 0.010(2) 0.007(2) -0.013(2) C50 0.103(4) 0.091(4) 0.050(3) -0.012(2) 0.012(3) -0.016(3) C51 0.052(2) 0.054(3) 0.076(3) -0.004(2) -0.015(2) -0.0018(19) C52 0.047(2) 0.080(3) 0.053(2) 0.002(2) 0.0000(19) -0.007(2) O1T 0.075(2) 0.112(3) 0.0517(17) 0.0170(17) 0.0175(15) 0.0215(19) C1T 0.052(2) 0.082(3) 0.086(3) -0.046(3) -0.002(2) 0.005(2) C2T 0.081(3) 0.080(3) 0.104(4) 0.032(3) 0.029(3) 0.019(3) C3T 0.078(3) 0.068(3) 0.059(3) 0.007(2) 0.010(2) 0.014(2) C4T 0.086(3) 0.070(3) 0.065(3) 0.014(2) 0.027(2) 0.022(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 V C28 2.145(3) . ? V C1 2.145(3) . ? V C10 2.148(3) . ? V C19 2.152(3) . ? C1 C6 1.414(5) . ? C1 C2 1.424(4) . ? C2 C3 1.401(4) . ? C2 C7 1.511(5) . ? C3 C4 1.377(5) . ? C4 C5 1.375(5) . ? C4 C8 1.520(5) . ? C5 C6 1.410(5) . ? C6 C9 1.509(5) . ? C10 C11 1.410(4) . ? C10 C15 1.413(4) . ? C11 C12 1.395(4) . ? C11 C16 1.518(4) . ? C12 C13 1.384(5) . ? C13 C14 1.382(5) . ? C13 C17 1.519(4) . ? C14 C15 1.404(4) . ? C15 C18 1.508(4) . ? C19 C20 1.415(4) . ? C19 C24 1.422(4) . ? C20 C21 1.402(4) . ? C20 C25 1.516(4) . ? C21 C22 1.380(4) . ? C22 C23 1.391(4) . ? C22 C26 1.507(4) . ? C23 C24 1.389(4) . ? C24 C27 1.506(4) . ? C28 C29 1.413(4) . ? C28 C33 1.420(4) . ? C29 C30 1.404(4) . ? C29 C34 1.512(4) . ? C30 C31 1.377(5) . ? C31 C32 1.390(5) . ? C31 C35 1.509(4) . ? C32 C33 1.394(4) . ? C33 C36 1.511(4) . ? Li O1 1.915(6) . ? Li O4 1.928(6) . ? Li O3 1.929(6) . ? Li O2 1.940(6) . ? O1 C37 1.414(5) . ? O1 C40 1.432(4) . ? O2 C44 1.439(4) . ? O2 C41 1.440(4) . ? O3 C48 1.438(4) . ? O3 C45 1.441(4) . ? O4 C49 1.426(4) . ? O4 C52 1.438(4) . ? C37 C38 1.488(6) . ? C38 C39 1.508(6) . ? C39 C40 1.498(6) . ? C41 C42 1.497(5) . ? C42 C43 1.505(5) . ? C43 C44 1.505(5) . ? C45 C46 1.491(5) . ? C46 C47 1.506(6) . ? C47 C48 1.528(5) . ? C49 C50 1.486(6) . ? C50 C51 1.496(6) . ? C51 C52 1.497(6) . ? O1T C4T 1.426(5) . ? O1T C1T 1.430(5) . ? C1T C2T 1.498(6) . ? C2T C3T 1.478(6) . ? C3T C4T 1.485(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 C28 V C1 96.81(11) . . ? C28 V C10 115.41(11) . . ? C1 V C10 116.96(12) . . ? C28 V C19 117.14(11) . . ? C1 V C19 115.26(12) . . ? C10 V C19 96.66(11) . . ? C6 C1 C2 115.8(3) . . ? C6 C1 V 130.0(2) . . ? C2 C1 V 114.1(2) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 C7 117.4(3) . . ? C1 C2 C7 121.2(3) . . ? C4 C3 C2 122.0(3) . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C8 121.7(4) . . ? C3 C4 C8 120.9(4) . . ? C4 C5 C6 122.8(4) . . ? C5 C6 C1 120.5(3) . . ? C5 C6 C9 116.8(3) . . ? C1 C6 C9 122.7(3) . . ? C11 C10 C15 115.8(3) . . ? C11 C10 V 115.5(2) . . ? C15 C10 V 128.3(2) . . ? C12 C11 C10 122.0(3) . . ? C12 C11 C16 117.2(3) . . ? C10 C11 C16 120.8(3) . . ? C13 C12 C11 121.4(3) . . ? C14 C13 C12 117.6(3) . . ? C14 C13 C17 121.7(3) . . ? C12 C13 C17 120.7(3) . . ? C13 C14 C15 122.0(3) . . ? C14 C15 C10 121.1(3) . . ? C14 C15 C18 116.0(3) . . ? C10 C15 C18 123.0(3) . . ? C20 C19 C24 115.3(3) . . ? C20 C19 V 129.0(2) . . ? C24 C19 V 115.7(2) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 C25 115.8(3) . . ? C19 C20 C25 122.8(3) . . ? C22 C21 C20 122.5(3) . . ? C21 C22 C23 116.8(3) . . ? C21 C22 C26 121.9(3) . . ? C23 C22 C26 121.3(3) . . ? C24 C23 C22 122.2(3) . . ? C23 C24 C19 121.8(3) . . ? C23 C24 C27 117.1(3) . . ? C19 C24 C27 121.0(3) . . ? C29 C28 C33 115.4(3) . . ? C29 C28 V 129.2(2) . . ? C33 C28 V 115.0(2) . . ? C30 C29 C28 121.1(3) . . ? C30 C29 C34 116.4(3) . . ? C28 C29 C34 122.5(3) . . ? C31 C30 C29 122.6(3) . . ? C30 C31 C32 117.1(3) . . ? C30 C31 C35 122.3(3) . . ? C32 C31 C35 120.6(3) . . ? C31 C32 C33 121.7(3) . . ? C32 C33 C28 122.0(3) . . ? C32 C33 C36 116.9(3) . . ? C28 C33 C36 121.1(3) . . ? O1 Li O4 109.5(3) . . ? O1 Li O3 110.6(3) . . ? O4 Li O3 110.1(3) . . ? O1 Li O2 106.5(3) . . ? O4 Li O2 111.4(3) . . ? O3 Li O2 108.7(3) . . ? C37 O1 C40 109.1(3) . . ? C37 O1 Li 126.3(3) . . ? C40 O1 Li 124.5(3) . . ? C44 O2 C41 109.1(2) . . ? C44 O2 Li 129.0(3) . . ? C41 O2 Li 118.3(3) . . ? C48 O3 C45 105.3(3) . . ? C48 O3 Li 129.9(3) . . ? C45 O3 Li 123.0(3) . . ? C49 O4 C52 108.2(3) . . ? C49 O4 Li 124.9(3) . . ? C52 O4 Li 122.9(3) . . ? O1 C37 C38 108.0(3) . . ? C37 C38 C39 103.1(4) . . ? C40 C39 C38 102.3(3) . . ? O1 C40 C39 105.4(3) . . ? O2 C41 C42 105.5(3) . . ? C41 C42 C43 102.8(3) . . ? C44 C43 C42 104.1(3) . . ? O2 C44 C43 106.7(3) . . ? O3 C45 C46 105.4(3) . . ? C45 C46 C47 104.2(3) . . ? C46 C47 C48 105.0(3) . . ? O3 C48 C47 106.1(3) . . ? O4 C49 C50 107.1(3) . . ? C49 C50 C51 105.9(3) . . ? C50 C51 C52 102.7(3) . . ? O4 C52 C51 104.6(3) . . ? C4T O1T C1T 107.4(3) . . ? O1T C1T C2T 105.1(3) . . ? C3T C2T C1T 104.4(4) . . ? C2T C3T C4T 103.8(4) . . ? O1T C4T C3T 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.430 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.063 #==== END data_FO2903 _database_code_depnum_ccdc_archive 'CCDC 765648' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Ca I O5, C36 H44 V, 2(C4 H8 O)' _chemical_formula_sum 'C64 H100 Ca I O7 V' _chemical_formula_weight 1199.36 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.668(3) _cell_length_b 34.081(7) _cell_length_c 15.403(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.43(3) _cell_angle_gamma 90.00 _cell_volume 6378(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 44403 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour violett _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44403 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.47 _reflns_number_total 14552 _reflns_number_gt 9859 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0965P)^2^+5.4587P] 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 14552 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.010 _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 Ca Ca 0.58351(6) -0.10645(2) 0.90826(5) 0.03844(17) Uani 1 1 d . A . I I 0.38384(2) -0.053253(9) 0.86199(2) 0.06144(12) Uani 1 1 d . . . O1 O 0.7418(2) -0.14786(8) 0.96247(19) 0.0544(7) Uani 1 1 d . . . O2 O 0.6002(2) -0.10793(10) 0.76104(18) 0.0628(8) Uani 1 1 d . . . O3 O 0.4810(3) -0.16442(8) 0.8706(2) 0.0637(8) Uani 1 1 d . . . O4 O 0.5768(2) -0.10895(9) 1.05925(18) 0.0583(7) Uani 1 1 d . . . O5 O 0.7040(2) -0.05275(7) 0.9394(2) 0.0536(7) Uani 1 1 d . . . C1 C 0.7849(4) -0.16241(15) 1.0544(3) 0.0718(13) Uani 1 1 d . . . H1A H 0.7275 -0.1773 1.0727 0.086 Uiso 1 1 calc R . . H1B H 0.8094 -0.1403 1.0971 0.086 Uiso 1 1 calc R . . C2 C 0.8800(5) -0.18856(17) 1.0549(4) 0.0845(16) Uani 1 1 d . . . H2A H 0.9507 -0.1748 1.0810 0.101 Uiso 1 1 calc R . . H2B H 0.8787 -0.2126 1.0908 0.101 Uiso 1 1 calc R . . C3 C 0.8660(5) -0.19827(18) 0.9604(4) 0.0925(19) Uani 1 1 d . . . H3A H 0.8173 -0.2213 0.9416 0.111 Uiso 1 1 calc R . . H3B H 0.9376 -0.2036 0.9489 0.111 Uiso 1 1 calc R . . C4 C 0.8137(5) -0.16165(17) 0.9125(4) 0.0821(16) Uani 1 1 d . . . H4A H 0.8704 -0.1417 0.9121 0.099 Uiso 1 1 calc R . . H4B H 0.7718 -0.1676 0.8492 0.099 Uiso 1 1 calc R . . C5 C 0.6896(6) -0.0899(2) 0.7307(5) 0.0416(16) Uiso 0.50 1 d P A 1 H5A H 0.7603 -0.1037 0.7561 0.050 Uiso 0.50 1 calc PR A 1 H5B H 0.6989 -0.0618 0.7474 0.050 Uiso 0.50 1 calc PR A 1 C5A C 0.6778(14) -0.1134(5) 0.7161(11) 0.121(5) Uiso 0.50 1 d P A 2 H5AA H 0.6892 -0.1418 0.7098 0.146 Uiso 0.50 1 calc PR A 2 H5AB H 0.7485 -0.1019 0.7521 0.146 Uiso 0.50 1 calc PR A 2 C6 C 0.6463(5) -0.0954(2) 0.6264(4) 0.0888(17) Uani 1 1 d . . . H6A H 0.6786 -0.0757 0.5939 0.107 Uiso 0.50 1 calc PR A 1 H6B H 0.6621 -0.1220 0.6080 0.107 Uiso 0.50 1 calc PR A 1 H6C H 0.6853 -0.0701 0.6283 0.107 Uiso 0.50 1 d PR A 2 H6D H 0.6617 -0.1122 0.5791 0.107 Uiso 0.50 1 d PR A 2 C7 C 0.5285(5) -0.0892(2) 0.6103(4) 0.0969(19) Uani 1 1 d . A . H7A H 0.4866 -0.0988 0.5497 0.116 Uiso 1 1 calc R . . H7B H 0.5115 -0.0611 0.6156 0.116 Uiso 1 1 calc R . . C8 C 0.5037(5) -0.1128(2) 0.6837(4) 0.100(2) Uani 1 1 d . A . H8A H 0.4368 -0.1029 0.6976 0.120 Uiso 1 1 calc R . . H8B H 0.4926 -0.1408 0.6660 0.120 Uiso 1 1 calc R . . C9 C 0.5393(7) -0.2014(2) 0.8568(6) 0.057(2) Uiso 0.50 1 d P A 1 H9A H 0.5805 -0.2130 0.9154 0.068 Uiso 0.50 1 calc PR A 1 H9B H 0.5908 -0.1962 0.8203 0.068 Uiso 0.50 1 calc PR A 1 C10 C 0.4466(8) -0.2278(3) 0.8068(7) 0.062(2) Uiso 0.50 1 d P A 1 H10A H 0.4597 -0.2553 0.8277 0.074 Uiso 0.50 1 calc PR A 1 H10B H 0.4359 -0.2268 0.7406 0.074 Uiso 0.50 1 calc PR A 1 C11 C 0.3336(9) -0.2075(3) 0.8360(8) 0.073(3) Uiso 0.50 1 d P A 1 H11A H 0.2677 -0.2058 0.7830 0.087 Uiso 0.50 1 calc PR A 1 H11B H 0.3155 -0.2225 0.8848 0.087 Uiso 0.50 1 calc PR A 1 C12 C 0.3721(9) -0.1735(3) 0.8631(8) 0.079(3) Uiso 0.50 1 d P A 1 H12A H 0.3605 -0.1692 0.9233 0.095 Uiso 0.50 1 calc PR A 1 H12B H 0.3259 -0.1540 0.8216 0.095 Uiso 0.50 1 calc PR A 1 C9A C 0.5002(12) -0.2017(4) 0.9001(9) 0.096(4) Uiso 0.50 1 d P A 2 H9AA H 0.4925 -0.2034 0.9622 0.115 Uiso 0.50 1 calc PR A 2 H9AB H 0.5770 -0.2087 0.9031 0.115 Uiso 0.50 1 calc PR A 2 C10A C 0.4271(10) -0.2299(3) 0.8434(8) 0.074(3) Uiso 0.50 1 d P A 2 H10C H 0.3954 -0.2481 0.8796 0.089 Uiso 0.50 1 calc PR A 2 H10D H 0.4647 -0.2452 0.8064 0.089 Uiso 0.50 1 calc PR A 2 C11A C 0.3385(8) -0.2024(3) 0.7843(7) 0.065(2) Uiso 0.50 1 d P A 2 H11C H 0.3303 -0.2078 0.7196 0.078 Uiso 0.50 1 calc PR A 2 H11D H 0.2669 -0.2077 0.7961 0.078 Uiso 0.50 1 calc PR A 2 C12A C 0.3653(10) -0.1653(3) 0.8018(9) 0.082(3) Uiso 0.50 1 d P A 2 H12C H 0.3112 -0.1523 0.8276 0.099 Uiso 0.50 1 calc PR A 2 H12D H 0.3663 -0.1514 0.7456 0.099 Uiso 0.50 1 calc PR A 2 C13 C 0.4789(5) -0.12396(15) 1.0796(3) 0.0730(13) Uani 1 1 d . A . H13A H 0.4958 -0.1487 1.1144 0.088 Uiso 1 1 calc R . . H13B H 0.4199 -0.1291 1.0231 0.088 Uiso 1 1 calc R . . C14 C 0.4446(6) -0.09363(18) 1.1333(4) 0.0875(17) Uani 1 1 d . . . H14B H 0.4055 -0.1053 1.1743 0.105 Uiso 1 1 calc R A . H14C H 0.3958 -0.0742 1.0936 0.105 Uiso 1 1 calc R . . C15 C 0.5482(6) -0.07546(18) 1.1848(4) 0.0888(17) Uani 1 1 d . A . H15A H 0.5792 -0.0894 1.2427 0.107 Uiso 1 1 calc R . . H15B H 0.5364 -0.0476 1.1978 0.107 Uiso 1 1 calc R . . C16 C 0.6224(6) -0.0786(2) 1.1271(4) 0.105(2) Uani 1 1 d . A . H16B H 0.6268 -0.0532 1.0972 0.126 Uiso 1 1 calc R . . H16C H 0.6973 -0.0860 1.1638 0.126 Uiso 1 1 calc R . . C17 C 0.6724(4) -0.01102(14) 0.9207(4) 0.0778(15) Uani 1 1 d . A . H17A H 0.6395 -0.0068 0.8551 0.093 Uiso 1 1 calc R . . H17B H 0.6184 -0.0031 0.9530 0.093 Uiso 1 1 calc R . . C18 C 0.7741(5) 0.01139(15) 0.9534(4) 0.0867(17) Uani 1 1 d . . . H18A H 0.8090 0.0156 0.9042 0.104 Uiso 0.50 1 calc PR A 1 H18B H 0.7594 0.0372 0.9769 0.104 Uiso 0.50 1 calc PR A 1 H18C H 0.7779 0.0323 0.9098 0.104 Uiso 0.50 1 d PR A 2 H18D H 0.7797 0.0236 1.0129 0.104 Uiso 0.50 1 d PR A 2 C19 C 0.8440(7) -0.0120(2) 1.0246(6) 0.0530(19) Uiso 0.50 1 d P A 1 H19A H 0.8236 -0.0094 1.0818 0.064 Uiso 0.50 1 calc PR A 1 H19B H 0.9226 -0.0051 1.0355 0.064 Uiso 0.50 1 calc PR A 1 C19A C 0.8564(13) -0.0144(4) 0.9620(11) 0.109(4) Uiso 0.50 1 d P A 2 H19C H 0.9215 -0.0059 1.0110 0.131 Uiso 0.50 1 calc PR A 2 H19D H 0.8775 -0.0158 0.9049 0.131 Uiso 0.50 1 calc PR A 2 C20 C 0.8186(5) -0.05314(16) 0.9836(6) 0.104(3) Uani 1 1 d . A . H20A H 0.8611 -0.0584 0.9399 0.125 Uiso 0.50 1 calc PR B 1 H20B H 0.8367 -0.0734 1.0315 0.125 Uiso 0.50 1 calc PR B 1 H20C H 0.8557 -0.0745 0.9601 0.125 Uiso 0.50 1 calc PR B 2 H20D H 0.8328 -0.0565 1.0498 0.125 Uiso 0.50 1 calc PR B 2 V V 0.18407(5) -0.136102(16) 0.34873(4) 0.03501(14) Uani 1 1 d . . . C21 C 0.2392(3) -0.08190(10) 0.4189(2) 0.0383(7) Uani 1 1 d . . . C22 C 0.2325(3) -0.08021(11) 0.5091(2) 0.0438(8) Uani 1 1 d . . . C23 C 0.2683(3) -0.04771(12) 0.5635(3) 0.0511(10) Uani 1 1 d . . . H23A H 0.2610 -0.0476 0.6232 0.061 Uiso 1 1 calc R . . C24 C 0.3145(4) -0.01544(13) 0.5336(3) 0.0560(10) Uani 1 1 d . . . C25 C 0.3256(3) -0.01712(11) 0.4464(3) 0.0515(9) Uani 1 1 d . . . H25A H 0.3598 0.0041 0.4248 0.062 Uiso 1 1 calc R . . C26 C 0.2875(3) -0.04936(10) 0.3894(2) 0.0417(8) Uani 1 1 d . . . C27 C 0.1900(4) -0.11458(12) 0.5512(3) 0.0536(10) Uani 1 1 d . . . H27A H 0.1630 -0.1053 0.6013 0.080 Uiso 1 1 calc R . . H27B H 0.2497 -0.1335 0.5742 0.080 Uiso 1 1 calc R . . H27C H 0.1298 -0.1273 0.5055 0.080 Uiso 1 1 calc R . . C28 C 0.3551(5) 0.01962(15) 0.5937(3) 0.0791(15) Uani 1 1 d . . . H28A H 0.4289 0.0268 0.5908 0.119 Uiso 1 1 calc R . . H28B H 0.3579 0.0130 0.6563 0.119 Uiso 1 1 calc R . . H28C H 0.3049 0.0418 0.5732 0.119 Uiso 1 1 calc R . . C29 C 0.3024(4) -0.04640(11) 0.2957(2) 0.0491(9) Uani 1 1 d . . . H29A H 0.2800 -0.0711 0.2632 0.074 Uiso 1 1 calc R . . H29B H 0.3800 -0.0412 0.3005 0.074 Uiso 1 1 calc R . . H29C H 0.2570 -0.0249 0.2626 0.074 Uiso 1 1 calc R . . C30 C 0.3088(3) -0.17373(11) 0.4318(2) 0.0435(8) Uani 1 1 d . . . C31 C 0.4184(3) -0.16548(11) 0.4318(2) 0.0462(9) Uani 1 1 d . . . C32 C 0.5075(4) -0.18635(13) 0.4869(3) 0.0592(11) Uani 1 1 d . . . H32A H 0.5799 -0.1802 0.4848 0.071 Uiso 1 1 calc R . . C33 C 0.4927(4) -0.21571(15) 0.5441(3) 0.0704(13) Uani 1 1 d . . . C34 C 0.3868(4) -0.22404(13) 0.5449(3) 0.0634(12) Uani 1 1 d . . . H34A H 0.3748 -0.2444 0.5832 0.076 Uiso 1 1 calc R . . C35 C 0.2969(3) -0.20367(12) 0.4915(3) 0.0513(9) Uani 1 1 d . . . C36 C 0.4435(3) -0.13368(12) 0.3721(3) 0.0495(9) Uani 1 1 d . . . H36A H 0.5105 -0.1405 0.3557 0.074 Uiso 1 1 calc R . . H36B H 0.4544 -0.1087 0.4049 0.074 Uiso 1 1 calc R . . H36C H 0.3819 -0.1312 0.3171 0.074 Uiso 1 1 calc R . . C37 C 0.5908(5) -0.2379(2) 0.6034(4) 0.103(2) Uani 1 1 d . . . H37A H 0.5683 -0.2647 0.6133 0.154 Uiso 1 1 calc R . . H37B H 0.6178 -0.2245 0.6618 0.154 Uiso 1 1 calc R . . H37C H 0.6494 -0.2389 0.5734 0.154 Uiso 1 1 calc R . . C38 C 0.1866(4) -0.21562(14) 0.5028(3) 0.0645(12) Uani 1 1 d . . . H38A H 0.1726 -0.2433 0.4860 0.097 Uiso 1 1 calc R . . H38B H 0.1286 -0.1994 0.4636 0.097 Uiso 1 1 calc R . . H38C H 0.1871 -0.2120 0.5660 0.097 Uiso 1 1 calc R . . C39 C 0.1739(3) -0.13650(9) 0.2069(2) 0.0365(7) Uani 1 1 d . . . C40 C 0.2230(3) -0.16282(9) 0.1593(2) 0.0384(7) Uani 1 1 d . . . C41 C 0.2054(3) -0.16012(11) 0.0657(2) 0.0431(8) Uani 1 1 d . . . H41A H 0.2389 -0.1789 0.0362 0.052 Uiso 1 1 calc R . . C42 C 0.1406(3) -0.13092(11) 0.0148(2) 0.0441(8) Uani 1 1 d . . . C43 C 0.0908(3) -0.10510(10) 0.0602(2) 0.0410(8) Uani 1 1 d . . . H43A H 0.0458 -0.0848 0.0270 0.049 Uiso 1 1 calc R . . C44 C 0.1046(3) -0.10791(9) 0.1529(2) 0.0359(7) Uani 1 1 d . . . C45 C 0.2987(4) -0.19560(11) 0.2061(3) 0.0522(10) Uani 1 1 d . . . H45A H 0.2685 -0.2209 0.1804 0.078 Uiso 1 1 calc R . . H45B H 0.3049 -0.1952 0.2710 0.078 Uiso 1 1 calc R . . H45C H 0.3717 -0.1919 0.1973 0.078 Uiso 1 1 calc R . . C46 C 0.1254(4) -0.12768(15) -0.0858(3) 0.0642(12) Uani 1 1 d . . . H46A H 0.0524 -0.1168 -0.1153 0.096 Uiso 1 1 calc R . . H46B H 0.1318 -0.1538 -0.1107 0.096 Uiso 1 1 calc R . . H46C H 0.1820 -0.1104 -0.0968 0.096 Uiso 1 1 calc R . . C47 C 0.0416(3) -0.07936(10) 0.1950(2) 0.0423(8) Uani 1 1 d . . . H47A H 0.0296 -0.0548 0.1603 0.063 Uiso 1 1 calc R . . H47B H 0.0840 -0.0739 0.2577 0.063 Uiso 1 1 calc R . . H47C H -0.0296 -0.0908 0.1943 0.063 Uiso 1 1 calc R . . C48 C 0.0178(3) -0.15219(10) 0.3369(2) 0.0403(8) Uani 1 1 d . . . C49 C -0.0142(3) -0.19082(10) 0.3035(2) 0.0442(8) Uani 1 1 d . . . C50 C -0.1201(3) -0.20549(12) 0.2940(2) 0.0492(9) Uani 1 1 d . . . H50A H -0.1372 -0.2315 0.2728 0.059 Uiso 1 1 calc R . . C51 C -0.1997(3) -0.18318(13) 0.3146(3) 0.0527(10) Uani 1 1 d . . . C52 C -0.1722(3) -0.14521(12) 0.3443(3) 0.0505(9) Uani 1 1 d . . . H52A H -0.2269 -0.1291 0.3575 0.061 Uiso 1 1 calc R . . C53 C -0.0678(3) -0.12972(11) 0.3554(2) 0.0421(8) Uani 1 1 d . . . C54 C 0.0679(4) -0.21740(11) 0.2779(3) 0.0555(10) Uani 1 1 d . . . H54A H 0.0491 -0.2449 0.2853 0.083 Uiso 1 1 calc R . . H54B H 0.1420 -0.2119 0.3171 0.083 Uiso 1 1 calc R . . H54C H 0.0657 -0.2127 0.2146 0.083 Uiso 1 1 calc R . . C55 C -0.3120(4) -0.20026(17) 0.3075(4) 0.0778(15) Uani 1 1 d . . . H55A H -0.3132 -0.2280 0.2902 0.117 Uiso 1 1 calc R . . H55B H -0.3679 -0.1859 0.2616 0.117 Uiso 1 1 calc R . . H55C H -0.3275 -0.1981 0.3661 0.117 Uiso 1 1 calc R . . C56 C -0.0499(4) -0.08785(12) 0.3894(3) 0.0540(10) Uani 1 1 d . . . H56A H -0.1033 -0.0706 0.3485 0.081 Uiso 1 1 calc R . . H56B H 0.0249 -0.0795 0.3916 0.081 Uiso 1 1 calc R . . H56C H -0.0596 -0.0863 0.4502 0.081 Uiso 1 1 calc R . . O1TA O -0.0697(6) -0.06075(18) -0.2781(5) 0.141(2) Uani 1 1 d . . . C1TA C -0.0162(9) -0.0328(3) -0.2267(7) 0.067(2) Uiso 0.50 1 d P C 1 H1TC H 0.0279 -0.0433 -0.1676 0.080 Uiso 0.50 1 calc PR C 1 H1TD H -0.0675 -0.0127 -0.2160 0.080 Uiso 0.50 1 calc PR C 1 C1TC C 0.0581(15) -0.0491(5) -0.2445(12) 0.122(5) Uiso 0.50 1 d P C 2 H1TE H 0.0839 -0.0472 -0.1777 0.147 Uiso 0.50 1 calc PR C 2 H1TF H 0.1037 -0.0686 -0.2650 0.147 Uiso 0.50 1 calc PR C 2 C2TA C 0.0625(5) -0.01451(19) -0.2824(5) 0.0991(19) Uani 1 1 d . . . H2TC H 0.0789 0.0135 -0.2681 0.119 Uiso 0.50 1 calc PR C 1 H2TD H 0.1320 -0.0294 -0.2725 0.119 Uiso 0.50 1 calc PR C 1 H2TE H 0.1380 -0.0076 -0.2835 0.119 Uiso 0.50 1 d PR C 2 H2TF H 0.0343 0.0062 -0.2497 0.119 Uiso 0.50 1 d PR C 2 C3TA C -0.0130(7) -0.0203(2) -0.3762(4) 0.107(2) Uani 1 1 d . C . H3TC H -0.0576 0.0035 -0.3973 0.128 Uiso 1 1 calc R . . H3TD H 0.0294 -0.0266 -0.4194 0.128 Uiso 1 1 calc R . . C4TA C -0.0805(8) -0.0521(3) -0.3676(8) 0.154(4) Uani 1 1 d . C . H4TC H -0.1583 -0.0455 -0.3984 0.185 Uiso 1 1 calc R . . H4TD H -0.0605 -0.0754 -0.3978 0.185 Uiso 1 1 calc R . . O1TB O 0.8333(4) -0.18719(19) 0.6634(3) 0.1318(19) Uani 1 1 d . . . C1TB C 0.9295(5) -0.17369(19) 0.7168(4) 0.0860(16) Uani 1 1 d . . . H1TA H 0.9544 -0.1904 0.7713 0.103 Uiso 1 1 calc R . . H1TB H 0.9198 -0.1466 0.7367 0.103 Uiso 1 1 calc R . . C2TB C 1.0124(6) -0.1740(2) 0.6665(5) 0.108(2) Uani 1 1 d . . . H2TA H 1.0729 -0.1925 0.6941 0.130 Uiso 1 1 calc R . . H2TB H 1.0437 -0.1475 0.6646 0.130 Uiso 1 1 calc R . . C3TB C 0.9485(6) -0.1874(3) 0.5735(5) 0.140(3) Uani 1 1 d . . . H3TA H 0.9640 -0.1702 0.5267 0.168 Uiso 1 1 calc R . . H3TB H 0.9682 -0.2147 0.5626 0.168 Uiso 1 1 calc R . . C4TB C 0.8403(6) -0.1850(4) 0.5713(5) 0.154(4) Uani 1 1 d . . . H4TA H 0.7985 -0.2068 0.5349 0.185 Uiso 1 1 calc R . . H4TB H 0.8086 -0.1599 0.5432 0.185 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 Ca 0.0378(4) 0.0409(4) 0.0377(4) -0.0015(3) 0.0125(3) -0.0038(3) I 0.05423(19) 0.0695(2) 0.05792(19) 0.00029(13) 0.01156(13) 0.00612(13) O1 0.0510(16) 0.0543(16) 0.0610(17) 0.0110(13) 0.0211(13) 0.0105(13) O2 0.0514(17) 0.100(2) 0.0422(15) -0.0046(14) 0.0212(13) -0.0053(15) O3 0.0613(18) 0.0478(16) 0.088(2) -0.0183(15) 0.0300(16) -0.0169(13) O4 0.0622(18) 0.0742(19) 0.0417(14) 0.0005(13) 0.0202(13) 0.0068(15) O5 0.0407(14) 0.0489(15) 0.0660(18) 0.0034(12) 0.0069(13) -0.0070(11) C1 0.075(3) 0.076(3) 0.055(3) 0.001(2) 0.004(2) 0.012(3) C2 0.085(4) 0.082(4) 0.080(4) 0.012(3) 0.014(3) 0.026(3) C3 0.106(4) 0.096(4) 0.083(4) 0.020(3) 0.040(3) 0.055(4) C4 0.087(4) 0.096(4) 0.074(3) 0.025(3) 0.039(3) 0.026(3) C6 0.085(4) 0.126(5) 0.065(3) 0.023(3) 0.035(3) 0.015(4) C7 0.079(4) 0.154(6) 0.053(3) 0.016(3) 0.013(3) 0.014(4) C8 0.076(4) 0.158(6) 0.070(3) -0.027(4) 0.027(3) -0.019(4) C13 0.096(4) 0.071(3) 0.067(3) 0.004(2) 0.048(3) -0.007(3) C14 0.115(5) 0.090(4) 0.072(3) -0.009(3) 0.050(3) -0.006(3) C15 0.120(5) 0.093(4) 0.062(3) -0.020(3) 0.040(3) -0.015(4) C16 0.105(5) 0.139(6) 0.073(4) -0.044(4) 0.029(3) -0.036(4) C17 0.072(3) 0.055(3) 0.100(4) 0.007(3) 0.014(3) -0.004(2) C18 0.080(4) 0.062(3) 0.109(4) 0.005(3) 0.013(3) -0.017(3) C20 0.054(3) 0.068(3) 0.167(7) 0.018(3) -0.009(4) -0.013(2) V 0.0401(3) 0.0350(3) 0.0323(3) 0.0038(2) 0.0142(2) 0.0066(2) C21 0.0370(17) 0.0460(19) 0.0334(16) -0.0003(14) 0.0123(14) 0.0045(15) C22 0.0424(19) 0.056(2) 0.0337(17) -0.0014(15) 0.0122(15) 0.0037(16) C23 0.052(2) 0.069(3) 0.0328(18) -0.0083(17) 0.0131(16) 0.0026(19) C24 0.057(2) 0.061(2) 0.047(2) -0.0158(18) 0.0094(19) -0.002(2) C25 0.058(2) 0.048(2) 0.047(2) -0.0055(16) 0.0127(18) -0.0082(18) C26 0.0435(19) 0.045(2) 0.0368(17) -0.0002(14) 0.0114(15) 0.0018(15) C27 0.060(2) 0.069(3) 0.0365(19) -0.0001(17) 0.0204(18) -0.001(2) C28 0.098(4) 0.075(3) 0.061(3) -0.031(2) 0.019(3) -0.017(3) C29 0.063(2) 0.046(2) 0.0396(19) 0.0012(15) 0.0164(18) -0.0085(17) C30 0.051(2) 0.048(2) 0.0363(17) 0.0077(15) 0.0193(16) 0.0120(16) C31 0.051(2) 0.054(2) 0.0367(18) 0.0105(15) 0.0171(16) 0.0139(17) C32 0.051(2) 0.075(3) 0.051(2) 0.018(2) 0.0130(19) 0.016(2) C33 0.070(3) 0.083(3) 0.055(3) 0.028(2) 0.013(2) 0.031(3) C34 0.071(3) 0.065(3) 0.056(2) 0.029(2) 0.022(2) 0.019(2) C35 0.058(2) 0.051(2) 0.048(2) 0.0170(17) 0.0200(18) 0.0126(18) C36 0.048(2) 0.060(2) 0.044(2) 0.0099(17) 0.0194(17) 0.0083(18) C37 0.083(4) 0.122(5) 0.095(4) 0.062(4) 0.013(3) 0.041(4) C38 0.073(3) 0.063(3) 0.064(3) 0.027(2) 0.030(2) 0.011(2) C39 0.0425(18) 0.0318(16) 0.0366(17) -0.0012(13) 0.0136(14) 0.0019(14) C40 0.0449(19) 0.0363(17) 0.0372(17) -0.0009(13) 0.0169(15) 0.0026(14) C41 0.044(2) 0.049(2) 0.0396(18) -0.0101(15) 0.0174(15) -0.0022(16) C42 0.0409(19) 0.057(2) 0.0357(17) -0.0040(15) 0.0132(15) -0.0078(16) C43 0.0411(19) 0.0415(18) 0.0375(18) 0.0044(14) 0.0065(15) -0.0025(15) C44 0.0391(18) 0.0337(16) 0.0351(17) -0.0008(13) 0.0111(14) -0.0001(13) C45 0.065(3) 0.047(2) 0.050(2) -0.0008(16) 0.0231(19) 0.0149(18) C46 0.065(3) 0.095(3) 0.0340(19) 0.002(2) 0.0157(19) 0.002(2) C47 0.049(2) 0.0377(18) 0.0395(18) 0.0018(14) 0.0109(15) 0.0124(15) C48 0.0444(19) 0.0406(18) 0.0368(17) 0.0035(14) 0.0133(15) 0.0044(15) C49 0.052(2) 0.0396(18) 0.0428(19) 0.0008(15) 0.0169(16) 0.0041(16) C50 0.054(2) 0.051(2) 0.0427(19) -0.0064(16) 0.0132(17) -0.0064(18) C51 0.042(2) 0.075(3) 0.0396(19) -0.0081(18) 0.0088(16) -0.0070(19) C52 0.042(2) 0.066(2) 0.044(2) -0.0088(17) 0.0121(16) 0.0067(18) C53 0.0432(19) 0.047(2) 0.0368(17) -0.0006(14) 0.0120(15) 0.0064(16) C54 0.066(3) 0.039(2) 0.069(3) 0.0010(18) 0.030(2) 0.0030(18) C55 0.047(2) 0.111(4) 0.079(3) -0.037(3) 0.022(2) -0.022(3) C56 0.054(2) 0.052(2) 0.061(2) -0.0091(18) 0.0238(19) 0.0055(18) O1TA 0.155(5) 0.143(5) 0.146(5) 0.019(4) 0.076(5) -0.028(4) C2TA 0.088(4) 0.084(4) 0.127(6) 0.004(4) 0.033(4) 0.008(3) C3TA 0.136(6) 0.103(5) 0.079(4) 0.008(3) 0.028(4) -0.005(4) C4TA 0.120(7) 0.158(9) 0.157(9) 0.025(7) -0.006(6) -0.038(6) O1TB 0.092(3) 0.208(6) 0.109(4) -0.021(4) 0.050(3) -0.037(4) C1TB 0.070(3) 0.105(4) 0.085(4) -0.007(3) 0.025(3) -0.006(3) C2TB 0.081(4) 0.146(6) 0.102(5) 0.024(4) 0.031(4) -0.025(4) C3TB 0.081(5) 0.267(11) 0.082(4) 0.008(6) 0.041(4) 0.001(6) C4TB 0.080(5) 0.305(13) 0.075(4) -0.004(6) 0.020(4) 0.006(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 Ca O2 2.337(3) . ? Ca O5 2.344(3) . ? Ca O3 2.345(3) . ? Ca O4 2.353(3) . ? Ca O1 2.401(3) . ? Ca I 3.0286(9) . ? O1 C4 1.427(6) . ? O1 C1 1.453(5) . ? O2 C5A 1.366(17) . ? O2 C8 1.456(6) . ? O2 C5 1.476(8) . ? O3 C9A 1.349(13) . ? O3 C12 1.387(11) . ? O3 C9 1.506(9) . ? O3 C12A 1.546(12) . ? O4 C13 1.456(6) . ? O4 C16 1.468(6) . ? O5 C20 1.419(6) . ? O5 C17 1.483(5) . ? C1 C2 1.497(7) . ? C2 C3 1.454(8) . ? C3 C4 1.505(7) . ? C5 C6 1.555(9) . ? C5A C6 1.460(17) . ? C6 C7 1.457(8) . ? C7 C8 1.494(9) . ? C9 C10 1.507(13) . ? C10 C11 1.759(15) . ? C11 C12 1.279(14) . ? C9A C10A 1.444(16) . ? C10A C11A 1.545(14) . ? C11A C12A 1.317(14) . ? C13 C14 1.464(7) . ? C14 C15 1.465(8) . ? C15 C16 1.468(8) . ? C17 C18 1.459(7) . ? C18 C19A 1.340(15) . ? C18 C19 1.440(10) . ? C19 C20 1.535(10) . ? C19A C20 1.476(15) . ? V C48 2.134(4) . ? V C39 2.152(3) . ? V C21 2.154(4) . ? V C30 2.153(3) . ? C21 C26 1.402(5) . ? C21 C22 1.418(5) . ? C22 C23 1.386(5) . ? C22 C27 1.510(5) . ? C23 C24 1.385(6) . ? C24 C25 1.391(6) . ? C24 C28 1.510(6) . ? C25 C26 1.404(5) . ? C26 C29 1.511(5) . ? C30 C35 1.410(5) . ? C30 C31 1.417(6) . ? C31 C32 1.399(5) . ? C31 C36 1.511(5) . ? C32 C33 1.382(6) . ? C33 C34 1.375(7) . ? C33 C37 1.519(6) . ? C34 C35 1.387(6) . ? C35 C38 1.512(6) . ? C39 C44 1.414(5) . ? C39 C40 1.409(5) . ? C40 C41 1.398(5) . ? C40 C45 1.515(5) . ? C41 C42 1.384(5) . ? C42 C43 1.381(5) . ? C42 C46 1.512(5) . ? C43 C44 1.393(5) . ? C44 C47 1.515(5) . ? C48 C53 1.421(5) . ? C48 C49 1.429(5) . ? C49 C50 1.400(6) . ? C49 C54 1.514(5) . ? C50 C51 1.370(6) . ? C51 C52 1.384(6) . ? C51 C55 1.511(6) . ? C52 C53 1.389(6) . ? C53 C56 1.515(5) . ? O1TA C1TA 1.300(11) . ? O1TA C4TA 1.380(11) . ? O1TA C1TC 1.604(18) . ? C1TA C2TA 1.613(12) . ? C1TC C2TA 1.322(16) . ? C2TA C3TA 1.503(9) . ? C3TA C4TA 1.407(10) . ? O1TB C1TB 1.344(7) . ? O1TB C4TB 1.448(8) . ? C1TB C2TB 1.472(8) . ? C2TB C3TB 1.504(10) . ? C3TB C4TB 1.363(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ca O5 89.02(11) . . ? O2 Ca O3 86.43(12) . . ? O5 Ca O3 172.44(11) . . ? O2 Ca O4 175.52(11) . . ? O5 Ca O4 91.68(11) . . ? O3 Ca O4 92.39(11) . . ? O2 Ca O1 91.65(11) . . ? O5 Ca O1 87.49(10) . . ? O3 Ca O1 86.60(11) . . ? O4 Ca O1 83.97(10) . . ? O2 Ca I 94.78(8) . . ? O5 Ca I 91.88(7) . . ? O3 Ca I 94.52(8) . . ? O4 Ca I 89.61(8) . . ? O1 Ca I 173.53(8) . . ? C4 O1 C1 107.0(3) . . ? C4 O1 Ca 127.1(3) . . ? C1 O1 Ca 125.9(3) . . ? C5A O2 C8 97.3(8) . . ? C5A O2 C5 33.8(7) . . ? C8 O2 C5 109.3(4) . . ? C5A O2 Ca 140.4(7) . . ? C8 O2 Ca 120.7(3) . . ? C5 O2 Ca 125.9(3) . . ? C9A O3 C12 84.2(8) . . ? C9A O3 C9 37.8(6) . . ? C12 O3 C9 108.5(6) . . ? C9A O3 C12A 104.9(7) . . ? C12 O3 C12A 37.9(6) . . ? C9 O3 C12A 107.1(6) . . ? C9A O3 Ca 132.6(6) . . ? C12 O3 Ca 132.6(5) . . ? C9 O3 Ca 118.7(4) . . ? C12A O3 Ca 122.5(5) . . ? C13 O4 C16 106.4(4) . . ? C13 O4 Ca 119.8(3) . . ? C16 O4 Ca 124.2(3) . . ? C20 O5 C17 106.6(3) . . ? C20 O5 Ca 127.5(3) . . ? C17 O5 Ca 125.8(3) . . ? O1 C1 C2 106.7(4) . . ? C3 C2 C1 105.1(4) . . ? C2 C3 C4 102.4(5) . . ? O1 C4 C3 105.6(4) . . ? O2 C5 C6 101.5(5) . . ? O2 C5A C6 112.3(12) . . ? C5A C6 C7 102.4(8) . . ? C5A C6 C5 31.9(7) . . ? C7 C6 C5 101.8(5) . . ? C6 C7 C8 102.6(5) . . ? O2 C8 C7 104.4(5) . . ? O3 C9 C10 103.3(7) . . ? C9 C10 C11 101.9(7) . . ? C12 C11 C10 100.2(9) . . ? C11 C12 O3 120.5(10) . . ? O3 C9A C10A 113.6(10) . . ? C9A C10A C11A 100.8(9) . . ? C12A C11A C10A 111.1(9) . . ? C11A C12A O3 107.4(9) . . ? O4 C13 C14 106.3(4) . . ? C13 C14 C15 103.9(5) . . ? C14 C15 C16 105.7(4) . . ? O4 C16 C15 107.0(5) . . ? C18 C17 O5 105.8(4) . . ? C19A C18 C19 43.0(7) . . ? C19A C18 C17 106.1(8) . . ? C19 C18 C17 105.4(5) . . ? C18 C19 C20 100.4(6) . . ? C18 C19A C20 108.4(11) . . ? O5 C20 C19A 103.7(7) . . ? O5 C20 C19 104.8(5) . . ? C19A C20 C19 39.7(6) . . ? C48 V C39 97.89(13) . . ? C48 V C21 115.82(14) . . ? C39 V C21 115.62(13) . . ? C48 V C30 116.02(14) . . ? C39 V C30 115.01(13) . . ? C21 V C30 97.66(14) . . ? C26 C21 C22 116.0(3) . . ? C26 C21 V 128.7(3) . . ? C22 C21 V 115.2(3) . . ? C23 C22 C21 121.7(4) . . ? C23 C22 C27 117.2(3) . . ? C21 C22 C27 121.1(3) . . ? C22 C23 C24 122.1(4) . . ? C23 C24 C25 117.2(4) . . ? C23 C24 C28 121.8(4) . . ? C25 C24 C28 121.0(4) . . ? C24 C25 C26 121.7(4) . . ? C25 C26 C21 121.4(3) . . ? C25 C26 C29 115.5(3) . . ? C21 C26 C29 123.1(3) . . ? C35 C30 C31 115.4(3) . . ? C35 C30 V 128.5(3) . . ? C31 C30 V 115.9(2) . . ? C32 C31 C30 121.4(4) . . ? C32 C31 C36 117.4(4) . . ? C30 C31 C36 121.1(3) . . ? C33 C32 C31 121.6(4) . . ? C32 C33 C34 117.7(4) . . ? C32 C33 C37 120.6(5) . . ? C34 C33 C37 121.7(4) . . ? C33 C34 C35 122.0(4) . . ? C34 C35 C30 121.9(4) . . ? C34 C35 C38 115.3(4) . . ? C30 C35 C38 122.9(3) . . ? C44 C39 C40 115.2(3) . . ? C44 C39 V 116.2(2) . . ? C40 C39 V 128.5(2) . . ? C41 C40 C39 121.9(3) . . ? C41 C40 C45 115.7(3) . . ? C39 C40 C45 122.3(3) . . ? C42 C41 C40 121.8(3) . . ? C41 C42 C43 117.0(3) . . ? C41 C42 C46 121.1(4) . . ? C43 C42 C46 121.9(4) . . ? C42 C43 C44 122.1(3) . . ? C43 C44 C39 121.8(3) . . ? C43 C44 C47 117.8(3) . . ? C39 C44 C47 120.4(3) . . ? C53 C48 C49 114.4(3) . . ? C53 C48 V 129.4(3) . . ? C49 C48 V 116.1(3) . . ? C50 C49 C48 122.2(3) . . ? C50 C49 C54 117.9(3) . . ? C48 C49 C54 119.9(3) . . ? C51 C50 C49 121.6(4) . . ? C50 C51 C52 117.5(4) . . ? C50 C51 C55 120.5(4) . . ? C52 C51 C55 121.9(4) . . ? C51 C52 C53 122.6(4) . . ? C52 C53 C48 121.6(3) . . ? C52 C53 C56 116.4(3) . . ? C48 C53 C56 121.9(3) . . ? C1TA O1TA C4TA 109.8(7) . . ? C1TA O1TA C1TC 46.9(7) . . ? C4TA O1TA C1TC 94.3(8) . . ? O1TA C1TA C2TA 104.7(7) . . ? C2TA C1TC O1TA 104.1(12) . . ? C1TC C2TA C3TA 102.2(9) . . ? C1TC C2TA C1TA 46.5(9) . . ? C3TA C2TA C1TA 98.0(6) . . ? C4TA C3TA C2TA 104.5(6) . . ? O1TA C4TA C3TA 111.5(8) . . ? C1TB O1TB C4TB 106.6(5) . . ? O1TB C1TB C2TB 109.5(5) . . ? C1TB C2TB C3TB 103.4(5) . . ? C4TB C3TB C2TB 105.8(7) . . ? C3TB C4TB O1TB 108.2(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.888 _refine_diff_density_min -1.042 _refine_diff_density_rms 0.080 #==== END data_FO2880 _database_code_depnum_ccdc_archive 'CCDC 765649' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Ca O6, 2(C36 H44 V), 4(C4 H8 O)' _chemical_formula_sum 'C112 H168 Ca O10 V2' _chemical_formula_weight 1816.42 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5165(8) _cell_length_b 13.9755(6) _cell_length_c 14.9650(7) _cell_angle_alpha 76.564(3) _cell_angle_beta 71.192(3) _cell_angle_gamma 88.512(3) _cell_volume 2599.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 17683 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17683 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11543 _reflns_number_gt 6490 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0638P)^2^+0.8836P] 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 11543 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.006 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 V V 0.10924(4) 0.25586(3) 0.74847(3) 0.02902(15) Uani 1 1 d . . . C1 C 0.1665(2) 0.1274(2) 0.6975(2) 0.0317(7) Uani 1 1 d . . . C2 C 0.1095(2) 0.0371(2) 0.7522(2) 0.0320(7) Uani 1 1 d . . . C3 C 0.1310(3) -0.0505(2) 0.7220(2) 0.0376(8) Uani 1 1 d . . . H3A H 0.0914 -0.1093 0.7616 0.045 Uiso 1 1 calc R . . C4 C 0.2081(3) -0.0543(2) 0.6363(2) 0.0413(8) Uani 1 1 d . . . C5 C 0.2656(3) 0.0323(2) 0.5818(2) 0.0401(8) Uani 1 1 d . . . H5A H 0.3195 0.0313 0.5228 0.048 Uiso 1 1 calc R . . C6 C 0.2472(2) 0.1213(2) 0.6105(2) 0.0332(7) Uani 1 1 d . . . C7 C 0.0205(3) 0.0327(2) 0.8455(2) 0.0392(8) Uani 1 1 d . . . H7A H 0.0197 -0.0300 0.8918 0.059 Uiso 1 1 calc R . . H7B H -0.0460 0.0378 0.8320 0.059 Uiso 1 1 calc R . . H7C H 0.0299 0.0874 0.8733 0.059 Uiso 1 1 calc R . . C8 C 0.2295(3) -0.1500(3) 0.6038(3) 0.0596(11) Uani 1 1 d . . . H8A H 0.2319 -0.2032 0.6588 0.089 Uiso 1 1 calc R . . H8B H 0.2968 -0.1429 0.5514 0.089 Uiso 1 1 calc R . . H8C H 0.1737 -0.1660 0.5802 0.089 Uiso 1 1 calc R . . C9 C 0.3166(3) 0.2095(2) 0.5447(2) 0.0441(8) Uani 1 1 d . . . H9A H 0.3218 0.2128 0.4772 0.066 Uiso 1 1 calc R . . H9B H 0.3865 0.2034 0.5512 0.066 Uiso 1 1 calc R . . H9C H 0.2867 0.2696 0.5629 0.066 Uiso 1 1 calc R . . C10 C 0.2092(2) 0.3873(2) 0.6764(2) 0.0306(7) Uani 1 1 d . . . C11 C 0.3115(2) 0.3818(2) 0.6826(2) 0.0317(7) Uani 1 1 d . . . C12 C 0.3848(2) 0.4611(2) 0.6423(2) 0.0346(7) Uani 1 1 d . . . H12A H 0.4534 0.4524 0.6459 0.042 Uiso 1 1 calc R . . C13 C 0.3600(2) 0.5530(2) 0.5967(2) 0.0357(7) Uani 1 1 d . . . C14 C 0.2597(3) 0.5608(2) 0.5919(2) 0.0376(8) Uani 1 1 d . . . H14A H 0.2404 0.6228 0.5621 0.045 Uiso 1 1 calc R . . C15 C 0.1850(2) 0.4813(2) 0.6292(2) 0.0324(7) Uani 1 1 d . . . C16 C 0.3451(2) 0.2872(2) 0.7359(2) 0.0376(7) Uani 1 1 d . . . H16A H 0.4212 0.2838 0.7093 0.056 Uiso 1 1 calc R . . H16B H 0.3106 0.2306 0.7276 0.056 Uiso 1 1 calc R . . H16C H 0.3252 0.2861 0.8052 0.056 Uiso 1 1 calc R . . C17 C 0.4397(3) 0.6388(2) 0.5562(2) 0.0461(9) Uani 1 1 d . . . H17A H 0.4066 0.6986 0.5336 0.069 Uiso 1 1 calc R . . H17B H 0.4973 0.6254 0.5017 0.069 Uiso 1 1 calc R . . H17C H 0.4670 0.6480 0.6070 0.069 Uiso 1 1 calc R . . C18 C 0.0797(3) 0.5015(2) 0.6164(2) 0.0424(8) Uani 1 1 d . . . H18A H 0.0524 0.5594 0.6409 0.064 Uiso 1 1 calc R . . H18B H 0.0312 0.4443 0.6526 0.064 Uiso 1 1 calc R . . H18C H 0.0871 0.5140 0.5473 0.064 Uiso 1 1 calc R . . C19 C 0.0985(2) 0.2584(2) 0.8938(2) 0.0308(7) Uani 1 1 d . . . C20 C 0.1413(2) 0.1942(2) 0.9586(2) 0.0326(7) Uani 1 1 d . . . C21 C 0.1289(3) 0.2083(2) 1.0509(2) 0.0376(8) Uani 1 1 d . . . H21A H 0.1588 0.1637 1.0922 0.045 Uiso 1 1 calc R . . C22 C 0.0739(3) 0.2856(2) 1.0842(2) 0.0367(7) Uani 1 1 d . . . C23 C 0.0325(2) 0.3494(2) 1.0214(2) 0.0348(7) Uani 1 1 d . . . H23A H -0.0047 0.4032 1.0421 0.042 Uiso 1 1 calc R . . C24 C 0.0435(2) 0.3373(2) 0.9289(2) 0.0324(7) Uani 1 1 d . . . C25 C 0.1999(3) 0.1056(2) 0.9325(2) 0.0412(8) Uani 1 1 d . . . H25A H 0.2699 0.1094 0.9381 0.062 Uiso 1 1 calc R . . H25B H 0.2061 0.1047 0.8656 0.062 Uiso 1 1 calc R . . H25C H 0.1616 0.0452 0.9769 0.062 Uiso 1 1 calc R . . C26 C 0.0594(3) 0.2986(3) 1.1852(2) 0.0494(9) Uani 1 1 d . . . H26C H -0.0106 0.3216 1.2123 0.074 Uiso 1 1 calc R . . H26D H 0.1123 0.3471 1.1819 0.074 Uiso 1 1 calc R . . H26E H 0.0670 0.2354 1.2269 0.074 Uiso 1 1 calc R . . C27 C -0.0052(3) 0.4117(2) 0.8668(2) 0.0384(8) Uani 1 1 d . . . H27A H -0.0602 0.4439 0.9085 0.058 Uiso 1 1 calc R . . H27B H -0.0355 0.3780 0.8304 0.058 Uiso 1 1 calc R . . H27C H 0.0487 0.4612 0.8213 0.058 Uiso 1 1 calc R . . C28 C -0.0402(2) 0.2519(2) 0.7281(2) 0.0322(7) Uani 1 1 d . . . C29 C -0.1404(2) 0.2263(2) 0.8000(2) 0.0343(7) Uani 1 1 d . . . C30 C -0.2300(2) 0.2202(2) 0.7741(2) 0.0371(7) Uani 1 1 d . . . H30A H -0.2950 0.2003 0.8242 0.045 Uiso 1 1 calc R . . C31 C -0.2282(2) 0.2418(2) 0.6784(2) 0.0377(7) Uani 1 1 d . . . C32 C -0.1315(3) 0.2662(2) 0.6072(2) 0.0372(7) Uani 1 1 d . . . H32A H -0.1273 0.2809 0.5408 0.045 Uiso 1 1 calc R . . C33 C -0.0401(2) 0.2698(2) 0.6307(2) 0.0338(7) Uani 1 1 d . . . C34 C -0.1564(3) 0.2019(2) 0.9077(2) 0.0395(8) Uani 1 1 d . . . H34A H -0.2076 0.2451 0.9388 0.059 Uiso 1 1 calc R . . H34B H -0.0897 0.2118 0.9180 0.059 Uiso 1 1 calc R . . H34C H -0.1822 0.1331 0.9362 0.059 Uiso 1 1 calc R . . C35 C -0.3278(3) 0.2361(3) 0.6545(3) 0.0536(9) Uani 1 1 d . . . H35A H -0.3178 0.1965 0.6064 0.080 Uiso 1 1 calc R . . H35B H -0.3458 0.3026 0.6280 0.080 Uiso 1 1 calc R . . H35C H -0.3847 0.2054 0.7137 0.080 Uiso 1 1 calc R . . C36 C 0.0625(3) 0.2891(2) 0.5473(2) 0.0411(8) Uani 1 1 d . . . H36A H 0.0509 0.3297 0.4891 0.062 Uiso 1 1 calc R . . H36B H 0.0899 0.2263 0.5344 0.062 Uiso 1 1 calc R . . H36C H 0.1131 0.3238 0.5647 0.062 Uiso 1 1 calc R . . Ca Ca 0.5000 0.5000 1.0000 0.0365(2) Uani 1 2 d S . . O1 O 0.46671(18) 0.33465(16) 1.00520(16) 0.0456(6) Uani 1 1 d . B . O2 O 0.36465(18) 0.53845(16) 0.93503(16) 0.0421(5) Uani 1 1 d . . . O3 O 0.37796(18) 0.48049(17) 1.15905(15) 0.0464(6) Uani 1 1 d . . . C37 C 0.3956(3) 0.2627(3) 1.0858(3) 0.0549(10) Uani 1 1 d . B . H37A H 0.3221 0.2805 1.0953 0.066 Uiso 1 1 calc R . . H37B H 0.4110 0.2603 1.1466 0.066 Uiso 1 1 calc R . . C38 C 0.4124(4) 0.1642(3) 1.0596(3) 0.0672(12) Uani 1 1 d . . . H38A H 0.4198 0.1133 1.1150 0.081 Uiso 0.50 1 calc PR A 1 H38B H 0.3521 0.1440 1.0430 0.081 Uiso 0.50 1 calc PR A 1 H38C H 0.3450 0.1270 1.0766 0.081 Uiso 0.50 1 calc PR A 2 H38D H 0.4574 0.1242 1.0929 0.081 Uiso 0.50 1 calc PR A 2 C39 C 0.5085(6) 0.1756(5) 0.9756(5) 0.0453(17) Uiso 0.50 1 d P B 1 H39A H 0.5028 0.1356 0.9307 0.054 Uiso 0.50 1 calc PR B 1 H39B H 0.5701 0.1564 0.9964 0.054 Uiso 0.50 1 calc PR B 1 C39A C 0.4674(7) 0.1933(6) 0.9482(6) 0.055(2) Uiso 0.50 1 d P B 2 H39C H 0.5202 0.1455 0.9277 0.067 Uiso 0.50 1 calc PR B 2 H39D H 0.4157 0.1948 0.9137 0.067 Uiso 0.50 1 calc PR B 2 C40 C 0.5158(4) 0.2879(3) 0.9273(3) 0.0742(13) Uani 1 1 d . . . H40A H 0.5897 0.3123 0.8946 0.089 Uiso 0.50 1 calc PR B 1 H40B H 0.4788 0.3011 0.8787 0.089 Uiso 0.50 1 calc PR B 1 H40C H 0.5092 0.3282 0.8658 0.089 Uiso 0.50 1 calc PR B 2 H40D H 0.5911 0.2822 0.9192 0.089 Uiso 0.50 1 calc PR B 2 C41 C 0.3079(3) 0.4728(3) 0.9030(3) 0.0505(9) Uani 1 1 d . . . H41A H 0.2692 0.4189 0.9585 0.061 Uiso 1 1 calc R . . H41B H 0.3572 0.4435 0.8529 0.061 Uiso 1 1 calc R . . C42 C 0.2333(3) 0.5347(3) 0.8618(3) 0.0483(9) Uani 1 1 d . . . H42A H 0.2301 0.5166 0.8026 0.058 Uiso 1 1 calc R . . H42B H 0.1620 0.5268 0.9100 0.058 Uiso 1 1 calc R . . C43 C 0.2771(4) 0.6373(3) 0.8385(3) 0.0661(12) Uani 1 1 d . . . H43A H 0.3285 0.6551 0.7721 0.079 Uiso 1 1 calc R . . H43B H 0.2209 0.6847 0.8434 0.079 Uiso 1 1 calc R . . C44 C 0.3285(4) 0.6366(3) 0.9125(3) 0.0666(12) Uani 1 1 d . . . H44A H 0.3881 0.6861 0.8865 0.080 Uiso 1 1 calc R . . H44B H 0.2782 0.6520 0.9714 0.080 Uiso 1 1 calc R . . C45 C 0.2695(3) 0.5075(3) 1.1805(3) 0.0560(10) Uani 1 1 d . . . H45A H 0.2311 0.4684 1.1537 0.067 Uiso 1 1 calc R . . H45B H 0.2660 0.5783 1.1514 0.067 Uiso 1 1 calc R . . C46 C 0.2226(3) 0.4868(3) 1.2882(3) 0.0685(12) Uani 1 1 d . . . H46A H 0.1807 0.5420 1.3082 0.082 Uiso 1 1 calc R . . H46B H 0.1769 0.4257 1.3134 0.082 Uiso 1 1 calc R . . C47 C 0.3125(4) 0.4755(4) 1.3247(3) 0.0856(15) Uani 1 1 d . . . H47A H 0.3333 0.5390 1.3339 0.103 Uiso 1 1 calc R . . H47B H 0.2947 0.4261 1.3876 0.103 Uiso 1 1 calc R . . C48 C 0.3971(4) 0.4426(4) 1.2504(3) 0.0700(13) Uani 1 1 d . . . H48A H 0.4659 0.4687 1.2473 0.084 Uiso 1 1 calc R . . H48B H 0.3968 0.3698 1.2653 0.084 Uiso 1 1 calc R . . O1TB O 0.2428(2) 0.1234(2) 1.26566(19) 0.0734(9) Uani 1 1 d . . . C1TB C 0.1933(3) 0.1488(3) 1.3552(3) 0.0582(10) Uani 1 1 d . . . H1TC H 0.1749 0.2186 1.3440 0.070 Uiso 1 1 calc R . . H1TD H 0.2402 0.1392 1.3951 0.070 Uiso 1 1 calc R . . C2TB C 0.0964(4) 0.0822(3) 1.4056(3) 0.0714(13) Uani 1 1 d . . . H2TC H 0.0819 0.0642 1.4767 0.086 Uiso 1 1 calc R . . H2TD H 0.0349 0.1138 1.3915 0.086 Uiso 1 1 calc R . . C3TB C 0.1224(5) -0.0055(4) 1.3637(4) 0.1016(19) Uani 1 1 d . . . H3TC H 0.1420 -0.0595 1.4097 0.122 Uiso 1 1 calc R . . H3TD H 0.0613 -0.0291 1.3504 0.122 Uiso 1 1 calc R . . C4TB C 0.2100(4) 0.0245(3) 1.2735(3) 0.0720(13) Uani 1 1 d . . . H4TC H 0.2683 -0.0197 1.2747 0.086 Uiso 1 1 calc R . . H4TD H 0.1880 0.0210 1.2173 0.086 Uiso 1 1 calc R . . O1TA O 0.5727(3) 0.1489(2) 1.2096(3) 0.0885(10) Uani 1 1 d . . . C1TA C 0.5091(5) 0.1201(4) 1.3081(4) 0.0888(16) Uani 1 1 d . . . H1TA H 0.4407 0.1507 1.3173 0.107 Uiso 1 1 calc R . . H1TB H 0.5434 0.1417 1.3499 0.107 Uiso 1 1 calc R . . C2TA C 0.4938(4) 0.0124(3) 1.3342(3) 0.0772(14) Uani 1 1 d . . . H2TA H 0.4194 -0.0079 1.3493 0.093 Uiso 1 1 calc R . . H2TB H 0.5159 -0.0166 1.3913 0.093 Uiso 1 1 calc R . . C3TA C 0.5621(4) -0.0195(3) 1.2451(3) 0.0849(16) Uani 1 1 d . . . H3TA H 0.6032 -0.0759 1.2633 0.102 Uiso 1 1 calc R . . H3TB H 0.5192 -0.0386 1.2088 0.102 Uiso 1 1 calc R . . C4TA C 0.6309(4) 0.0678(4) 1.1872(3) 0.0765(13) Uani 1 1 d . . . H4TA H 0.6956 0.0671 1.2047 0.092 Uiso 1 1 calc R . . H4TB H 0.6503 0.0703 1.1170 0.092 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 V 0.0272(3) 0.0268(3) 0.0319(3) -0.0086(2) -0.0067(2) -0.0010(2) C1 0.0297(17) 0.0333(16) 0.0325(15) -0.0086(13) -0.0096(13) -0.0020(13) C2 0.0298(17) 0.0319(15) 0.0372(16) -0.0123(13) -0.0116(13) 0.0000(13) C3 0.0389(19) 0.0289(16) 0.0431(17) -0.0084(14) -0.0107(15) -0.0020(14) C4 0.048(2) 0.0342(17) 0.0481(19) -0.0173(15) -0.0187(16) 0.0058(15) C5 0.040(2) 0.0422(18) 0.0382(17) -0.0175(15) -0.0079(14) 0.0069(15) C6 0.0313(17) 0.0342(16) 0.0350(15) -0.0107(13) -0.0102(13) 0.0023(13) C7 0.0382(19) 0.0313(16) 0.0405(17) -0.0070(14) -0.0032(14) -0.0049(14) C8 0.077(3) 0.041(2) 0.062(2) -0.0295(18) -0.012(2) 0.0080(19) C9 0.037(2) 0.0421(19) 0.0451(18) -0.0136(15) -0.0004(15) -0.0020(15) C10 0.0298(17) 0.0311(15) 0.0330(15) -0.0102(13) -0.0110(13) -0.0003(13) C11 0.0305(17) 0.0302(15) 0.0351(15) -0.0109(13) -0.0093(13) 0.0014(13) C12 0.0273(17) 0.0385(17) 0.0383(16) -0.0136(14) -0.0074(13) -0.0025(14) C13 0.0326(18) 0.0331(16) 0.0398(16) -0.0104(14) -0.0080(14) -0.0036(14) C14 0.043(2) 0.0276(15) 0.0400(17) -0.0040(14) -0.0127(15) -0.0011(14) C15 0.0308(17) 0.0320(15) 0.0328(15) -0.0069(13) -0.0087(13) -0.0013(13) C16 0.0284(18) 0.0340(16) 0.0524(19) -0.0104(15) -0.0158(15) 0.0038(13) C17 0.043(2) 0.0413(18) 0.0482(19) -0.0076(16) -0.0077(16) -0.0092(16) C18 0.037(2) 0.0379(17) 0.0513(19) -0.0052(15) -0.0161(16) -0.0006(15) C19 0.0271(16) 0.0279(15) 0.0372(16) -0.0089(13) -0.0091(13) -0.0014(12) C20 0.0281(17) 0.0315(16) 0.0369(16) -0.0087(13) -0.0080(13) -0.0016(13) C21 0.041(2) 0.0322(16) 0.0367(16) -0.0021(14) -0.0135(14) -0.0007(14) C22 0.041(2) 0.0357(17) 0.0345(16) -0.0087(14) -0.0120(14) -0.0080(15) C23 0.0353(18) 0.0301(15) 0.0392(16) -0.0130(14) -0.0090(14) 0.0011(13) C24 0.0278(17) 0.0309(15) 0.0379(16) -0.0091(13) -0.0090(13) -0.0002(13) C25 0.042(2) 0.0357(17) 0.0449(18) -0.0084(15) -0.0145(15) 0.0059(15) C26 0.065(3) 0.046(2) 0.0416(18) -0.0153(16) -0.0190(17) -0.0022(18) C27 0.0386(19) 0.0373(17) 0.0435(17) -0.0166(15) -0.0146(15) 0.0093(14) C28 0.0342(18) 0.0244(14) 0.0369(16) -0.0115(13) -0.0066(13) -0.0011(13) C29 0.0294(17) 0.0306(15) 0.0413(17) -0.0121(14) -0.0068(14) 0.0014(13) C30 0.0261(17) 0.0369(17) 0.0431(18) -0.0116(14) -0.0025(14) -0.0036(13) C31 0.0311(18) 0.0369(17) 0.0467(18) -0.0123(15) -0.0130(14) 0.0019(14) C32 0.042(2) 0.0337(16) 0.0379(16) -0.0102(14) -0.0141(15) 0.0017(14) C33 0.0344(18) 0.0287(15) 0.0377(16) -0.0109(13) -0.0086(14) 0.0006(13) C34 0.0312(18) 0.0449(18) 0.0381(16) -0.0125(15) -0.0034(14) 0.0012(14) C35 0.038(2) 0.068(2) 0.059(2) -0.0185(19) -0.0190(18) 0.0012(18) C36 0.0363(19) 0.0474(19) 0.0365(17) -0.0096(15) -0.0072(14) -0.0025(15) Ca 0.0312(5) 0.0415(5) 0.0370(5) -0.0113(4) -0.0097(4) -0.0001(4) O1 0.0420(14) 0.0438(13) 0.0482(13) -0.0143(11) -0.0081(11) -0.0020(11) O2 0.0417(14) 0.0419(12) 0.0514(13) -0.0173(11) -0.0224(11) 0.0031(10) O3 0.0347(14) 0.0605(15) 0.0379(12) -0.0096(11) -0.0049(10) 0.0022(11) C37 0.050(2) 0.050(2) 0.054(2) -0.0153(18) -0.0009(18) -0.0064(18) C38 0.065(3) 0.058(2) 0.074(3) -0.024(2) -0.009(2) -0.009(2) C40 0.085(3) 0.060(3) 0.066(3) -0.031(2) 0.001(2) 0.008(2) C41 0.048(2) 0.047(2) 0.065(2) -0.0169(18) -0.0266(19) -0.0045(17) C42 0.038(2) 0.060(2) 0.055(2) -0.0239(18) -0.0199(17) 0.0057(17) C43 0.065(3) 0.057(2) 0.082(3) 0.001(2) -0.044(2) -0.002(2) C44 0.092(3) 0.042(2) 0.091(3) -0.025(2) -0.060(3) 0.019(2) C45 0.034(2) 0.071(3) 0.055(2) -0.011(2) -0.0081(17) 0.0028(18) C46 0.051(3) 0.080(3) 0.060(2) -0.014(2) 0.001(2) 0.005(2) C47 0.064(3) 0.134(5) 0.051(2) -0.027(3) -0.006(2) 0.016(3) C48 0.063(3) 0.104(4) 0.042(2) -0.014(2) -0.0188(19) 0.016(3) O1TB 0.081(2) 0.0616(17) 0.0608(17) -0.0140(14) 0.0011(15) -0.0174(15) C1TB 0.072(3) 0.056(2) 0.049(2) -0.0108(18) -0.022(2) -0.009(2) C2TB 0.071(3) 0.056(2) 0.073(3) -0.014(2) -0.004(2) -0.012(2) C3TB 0.104(4) 0.067(3) 0.110(4) -0.036(3) 0.010(3) -0.027(3) C4TB 0.089(4) 0.053(2) 0.070(3) -0.012(2) -0.022(2) -0.007(2) O1TA 0.085(2) 0.0507(17) 0.109(3) -0.0048(18) -0.013(2) -0.0047(17) C1TA 0.097(4) 0.076(3) 0.090(3) -0.040(3) -0.012(3) 0.008(3) C2TA 0.068(3) 0.077(3) 0.071(3) -0.013(2) -0.005(2) 0.008(2) C3TA 0.097(4) 0.055(3) 0.077(3) -0.014(2) 0.003(3) 0.020(3) C4TA 0.050(3) 0.093(3) 0.077(3) -0.016(3) -0.011(2) 0.018(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 V C28 2.141(3) . ? V C1 2.142(3) . ? V C19 2.142(3) . ? V C10 2.152(3) . ? C1 C2 1.421(4) . ? C1 C6 1.423(4) . ? C2 C3 1.394(4) . ? C2 C7 1.510(4) . ? C3 C4 1.379(4) . ? C4 C5 1.383(4) . ? C4 C8 1.518(4) . ? C5 C6 1.398(4) . ? C6 C9 1.507(4) . ? C10 C11 1.415(4) . ? C10 C15 1.424(4) . ? C11 C12 1.391(4) . ? C11 C16 1.517(4) . ? C12 C13 1.395(4) . ? C13 C14 1.380(4) . ? C13 C17 1.508(4) . ? C14 C15 1.405(4) . ? C15 C18 1.507(4) . ? C19 C20 1.418(4) . ? C19 C24 1.421(4) . ? C20 C21 1.395(4) . ? C20 C25 1.512(4) . ? C21 C22 1.393(4) . ? C22 C23 1.383(4) . ? C22 C26 1.513(4) . ? C23 C24 1.393(4) . ? C24 C27 1.512(4) . ? C28 C33 1.420(4) . ? C28 C29 1.424(4) . ? C29 C30 1.396(4) . ? C29 C34 1.512(4) . ? C30 C31 1.386(4) . ? C31 C32 1.384(4) . ? C31 C35 1.509(5) . ? C32 C33 1.394(4) . ? C33 C36 1.516(4) . ? Ca O2 2.331(2) 2_667 ? Ca O2 2.331(2) . ? Ca O1 2.344(2) . ? Ca O1 2.344(2) 2_667 ? Ca O3 2.377(2) . ? Ca O3 2.377(2) 2_667 ? O1 C40 1.435(4) . ? O1 C37 1.459(4) . ? O2 C44 1.446(4) . ? O2 C41 1.462(4) . ? O3 C48 1.449(4) . ? O3 C45 1.456(4) . ? C37 C38 1.508(5) . ? C38 C39 1.469(8) . ? C38 C39A 1.550(8) . ? C39 C40 1.559(8) . ? C39A C40 1.412(9) . ? C41 C42 1.502(5) . ? C42 C43 1.486(5) . ? C43 C44 1.483(5) . ? C45 C46 1.489(5) . ? C46 C47 1.475(6) . ? C47 C48 1.465(6) . ? O1TB C1TB 1.414(4) . ? O1TB C4TB 1.430(5) . ? C1TB C2TB 1.500(5) . ? C2TB C3TB 1.488(6) . ? C3TB C4TB 1.460(6) . ? O1TA C4TA 1.406(5) . ? O1TA C1TA 1.415(6) . ? C1TA C2TA 1.467(6) . ? C2TA C3TA 1.513(6) . ? C3TA C4TA 1.468(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 C28 V C1 97.27(11) . . ? C28 V C19 113.23(11) . . ? C1 V C19 118.13(11) . . ? C28 V C10 117.75(11) . . ? C1 V C10 114.79(11) . . ? C19 V C10 97.03(11) . . ? C2 C1 C6 115.0(3) . . ? C2 C1 V 115.9(2) . . ? C6 C1 V 128.7(2) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 C7 116.9(3) . . ? C1 C2 C7 120.9(3) . . ? C4 C3 C2 121.7(3) . . ? C3 C4 C5 117.4(3) . . ? C3 C4 C8 121.1(3) . . ? C5 C4 C8 121.5(3) . . ? C4 C5 C6 122.4(3) . . ? C5 C6 C1 121.2(3) . . ? C5 C6 C9 116.7(3) . . ? C1 C6 C9 122.1(3) . . ? C11 C10 C15 115.1(3) . . ? C11 C10 V 115.4(2) . . ? C15 C10 V 129.2(2) . . ? C12 C11 C10 122.6(3) . . ? C12 C11 C16 117.1(3) . . ? C10 C11 C16 120.3(3) . . ? C11 C12 C13 121.7(3) . . ? C14 C13 C12 116.7(3) . . ? C14 C13 C17 122.5(3) . . ? C12 C13 C17 120.7(3) . . ? C13 C14 C15 123.0(3) . . ? C14 C15 C10 120.8(3) . . ? C14 C15 C18 116.4(3) . . ? C10 C15 C18 122.8(3) . . ? C20 C19 C24 115.7(3) . . ? C20 C19 V 129.0(2) . . ? C24 C19 V 115.3(2) . . ? C21 C20 C19 121.5(3) . . ? C21 C20 C25 116.7(3) . . ? C19 C20 C25 121.8(3) . . ? C22 C21 C20 122.0(3) . . ? C23 C22 C21 117.2(3) . . ? C23 C22 C26 121.6(3) . . ? C21 C22 C26 121.2(3) . . ? C22 C23 C24 122.2(3) . . ? C23 C24 C19 121.4(3) . . ? C23 C24 C27 117.5(3) . . ? C19 C24 C27 121.1(3) . . ? C33 C28 C29 114.8(3) . . ? C33 C28 V 116.7(2) . . ? C29 C28 V 128.3(2) . . ? C30 C29 C28 121.2(3) . . ? C30 C29 C34 116.0(3) . . ? C28 C29 C34 122.8(3) . . ? C31 C30 C29 122.8(3) . . ? C32 C31 C30 117.0(3) . . ? C32 C31 C35 122.4(3) . . ? C30 C31 C35 120.6(3) . . ? C31 C32 C33 121.5(3) . . ? C32 C33 C28 122.6(3) . . ? C32 C33 C36 117.2(3) . . ? C28 C33 C36 120.1(3) . . ? O2 Ca O2 180.0 2_667 . ? O2 Ca O1 92.48(8) 2_667 . ? O2 Ca O1 87.52(8) . . ? O2 Ca O1 87.52(8) 2_667 2_667 ? O2 Ca O1 92.48(8) . 2_667 ? O1 Ca O1 179.999(2) . 2_667 ? O2 Ca O3 90.20(8) 2_667 . ? O2 Ca O3 89.80(8) . . ? O1 Ca O3 90.10(8) . . ? O1 Ca O3 89.90(8) 2_667 . ? O2 Ca O3 89.80(8) 2_667 2_667 ? O2 Ca O3 90.20(8) . 2_667 ? O1 Ca O3 89.90(8) . 2_667 ? O1 Ca O3 90.10(8) 2_667 2_667 ? O3 Ca O3 180.00(7) . 2_667 ? C40 O1 C37 108.9(3) . . ? C40 O1 Ca 124.2(2) . . ? C37 O1 Ca 126.94(19) . . ? C44 O2 C41 108.2(3) . . ? C44 O2 Ca 124.0(2) . . ? C41 O2 Ca 127.6(2) . . ? C48 O3 C45 108.1(3) . . ? C48 O3 Ca 127.2(2) . . ? C45 O3 Ca 124.64(19) . . ? O1 C37 C38 106.9(3) . . ? C39 C38 C37 107.2(4) . . ? C39 C38 C39A 30.4(4) . . ? C37 C38 C39A 102.8(4) . . ? C38 C39 C40 102.9(5) . . ? C40 C39A C38 106.2(6) . . ? C39A C40 O1 109.5(4) . . ? C39A C40 C39 30.5(4) . . ? O1 C40 C39 105.5(4) . . ? O2 C41 C42 106.5(3) . . ? C43 C42 C41 104.4(3) . . ? C44 C43 C42 104.2(3) . . ? O2 C44 C43 106.2(3) . . ? O3 C45 C46 107.0(3) . . ? C47 C46 C45 105.1(3) . . ? C48 C47 C46 105.7(4) . . ? O3 C48 C47 106.3(4) . . ? C1TB O1TB C4TB 108.9(3) . . ? O1TB C1TB C2TB 106.6(3) . . ? C3TB C2TB C1TB 103.3(4) . . ? C4TB C3TB C2TB 107.3(4) . . ? O1TB C4TB C3TB 107.5(4) . . ? C4TA O1TA C1TA 107.2(3) . . ? O1TA C1TA C2TA 107.9(4) . . ? C1TA C2TA C3TA 104.5(4) . . ? C4TA C3TA C2TA 104.1(4) . . ? O1TA C4TA C3TA 105.5(4) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.363 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.060 #==== END data_FO2934 _database_code_depnum_ccdc_archive 'CCDC 765650' #TrackingRef '- newjchem.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H44 V), C24 H48 O6 Sr, 4(C4 H8 O)' _chemical_formula_sum 'C112 H168 O10 Sr V2' _chemical_formula_weight 1863.96 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5257(14) _cell_length_b 13.9195(12) _cell_length_c 15.1196(17) _cell_angle_alpha 76.359(6) _cell_angle_beta 71.204(4) _cell_angle_gamma 88.437(7) _cell_volume 2615.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 16820 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16820 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.1456 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11235 _reflns_number_gt 5655 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0573P)^2^+2.7587P] 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 11235 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1774 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.001 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 V V 0.10866(6) 0.25531(5) 0.74705(6) 0.0314(2) Uani 1 1 d . . . C1 C 0.1652(4) 0.1257(3) 0.6968(3) 0.0352(11) Uani 1 1 d . . . C2 C 0.1087(4) 0.0355(3) 0.7515(3) 0.0337(11) Uani 1 1 d . . . C3 C 0.1284(4) -0.0529(3) 0.7221(4) 0.0415(12) Uani 1 1 d . . . H3A H 0.0886 -0.1117 0.7616 0.050 Uiso 1 1 calc R . . C4 C 0.2043(4) -0.0561(4) 0.6369(4) 0.0420(12) Uani 1 1 d . . . C5 C 0.2621(4) 0.0308(4) 0.5817(4) 0.0434(12) Uani 1 1 d . . . H5A H 0.3149 0.0300 0.5226 0.052 Uiso 1 1 calc R . . C6 C 0.2441(4) 0.1201(3) 0.6114(4) 0.0379(11) Uani 1 1 d . . . C7 C 0.0206(4) 0.0317(4) 0.8443(4) 0.0445(13) Uani 1 1 d . . . H7A H 0.0204 -0.0308 0.8906 0.067 Uiso 1 1 calc R . . H7B H -0.0462 0.0364 0.8316 0.067 Uiso 1 1 calc R . . H7C H 0.0305 0.0872 0.8707 0.067 Uiso 1 1 calc R . . C8 C 0.2236(5) -0.1518(4) 0.6035(4) 0.0599(16) Uani 1 1 d . . . H8A H 0.2228 -0.2067 0.6580 0.090 Uiso 1 1 calc R . . H8B H 0.2918 -0.1458 0.5531 0.090 Uiso 1 1 calc R . . H8C H 0.1685 -0.1647 0.5780 0.090 Uiso 1 1 calc R . . C9 C 0.3151(4) 0.2083(4) 0.5448(4) 0.0456(13) Uani 1 1 d . . . H9A H 0.2863 0.2693 0.5619 0.068 Uiso 1 1 calc R . . H9B H 0.3201 0.2110 0.4781 0.068 Uiso 1 1 calc R . . H9C H 0.3849 0.2015 0.5514 0.068 Uiso 1 1 calc R . . C10 C 0.2075(4) 0.3876(3) 0.6749(3) 0.0334(11) Uani 1 1 d . . . C11 C 0.3112(4) 0.3816(3) 0.6802(3) 0.0344(11) Uani 1 1 d . . . C12 C 0.3841(4) 0.4609(3) 0.6407(4) 0.0383(11) Uani 1 1 d . . . H12A H 0.4525 0.4522 0.6450 0.046 Uiso 1 1 calc R . . C13 C 0.3596(4) 0.5538(3) 0.5944(3) 0.0370(11) Uani 1 1 d . . . C14 C 0.2589(4) 0.5620(3) 0.5902(3) 0.0378(11) Uani 1 1 d . . . H14A H 0.2393 0.6242 0.5606 0.045 Uiso 1 1 calc R . . C15 C 0.1845(4) 0.4816(3) 0.6282(3) 0.0357(11) Uani 1 1 d . . . C16 C 0.3452(4) 0.2870(3) 0.7330(4) 0.0394(12) Uani 1 1 d . . . H16A H 0.4203 0.2812 0.7030 0.059 Uiso 1 1 calc R . . H16B H 0.3064 0.2302 0.7297 0.059 Uiso 1 1 calc R . . H16C H 0.3308 0.2884 0.8005 0.059 Uiso 1 1 calc R . . C17 C 0.4384(4) 0.6408(4) 0.5540(4) 0.0462(13) Uani 1 1 d . . . H17A H 0.4066 0.6990 0.5258 0.069 Uiso 1 1 calc R . . H17B H 0.4994 0.6252 0.5044 0.069 Uiso 1 1 calc R . . H17C H 0.4603 0.6547 0.6058 0.069 Uiso 1 1 calc R . . C18 C 0.0780(4) 0.5022(4) 0.6158(4) 0.0454(13) Uani 1 1 d . . . H18A H 0.0302 0.4438 0.6501 0.068 Uiso 1 1 calc R . . H18B H 0.0854 0.5171 0.5473 0.068 Uiso 1 1 calc R . . H18C H 0.0498 0.5589 0.6421 0.068 Uiso 1 1 calc R . . C19 C 0.0993(3) 0.2581(3) 0.8900(3) 0.0335(11) Uani 1 1 d . . . C20 C 0.1425(4) 0.1937(3) 0.9540(4) 0.0363(11) Uani 1 1 d . . . C21 C 0.1308(4) 0.2084(3) 1.0455(3) 0.0384(11) Uani 1 1 d . . . H21A H 0.1607 0.1635 1.0865 0.046 Uiso 1 1 calc R . . C22 C 0.0774(4) 0.2858(3) 1.0777(3) 0.0389(11) Uani 1 1 d . . . C23 C 0.0343(4) 0.3494(3) 1.0162(4) 0.0374(11) Uani 1 1 d . . . H23A H -0.0030 0.4033 1.0369 0.045 Uiso 1 1 calc R . . C24 C 0.0438(4) 0.3371(3) 0.9252(3) 0.0347(11) Uani 1 1 d . . . C25 C 0.2020(4) 0.1046(4) 0.9284(4) 0.0473(13) Uani 1 1 d . . . H25A H 0.2074 0.1030 0.8625 0.071 Uiso 1 1 calc R . . H25B H 0.1646 0.0439 0.9731 0.071 Uiso 1 1 calc R . . H25C H 0.2722 0.1094 0.9329 0.071 Uiso 1 1 calc R . . C26 C 0.0649(5) 0.3007(4) 1.1769(4) 0.0550(15) Uani 1 1 d . . . H26A H 0.0992 0.2483 1.2102 0.083 Uiso 1 1 calc R . . H26B H -0.0096 0.2982 1.2140 0.083 Uiso 1 1 calc R . . H26C H 0.0971 0.3653 1.1705 0.083 Uiso 1 1 calc R . . C27 C -0.0046(4) 0.4121(3) 0.8632(4) 0.0379(11) Uani 1 1 d . . . H27A H -0.0584 0.4458 0.9041 0.057 Uiso 1 1 calc R . . H27B H -0.0364 0.3781 0.8284 0.057 Uiso 1 1 calc R . . H27C H 0.0497 0.4608 0.8170 0.057 Uiso 1 1 calc R . . C28 C -0.0421(4) 0.2508(3) 0.7272(3) 0.0330(11) Uani 1 1 d . . . C29 C -0.1406(4) 0.2247(3) 0.7988(4) 0.0355(11) Uani 1 1 d . . . C30 C -0.2306(4) 0.2184(3) 0.7727(4) 0.0394(12) Uani 1 1 d . . . H30A H -0.2956 0.1987 0.8225 0.047 Uiso 1 1 calc R . . C31 C -0.2295(4) 0.2393(3) 0.6787(4) 0.0396(12) Uani 1 1 d . . . C32 C -0.1325(4) 0.2641(3) 0.6076(4) 0.0395(12) Uani 1 1 d . . . H32A H -0.1282 0.2787 0.5418 0.047 Uiso 1 1 calc R . . C33 C -0.0411(4) 0.2679(3) 0.6316(4) 0.0341(11) Uani 1 1 d . . . C34 C -0.1578(4) 0.1999(4) 0.9061(3) 0.0399(12) Uani 1 1 d . . . H34A H -0.0926 0.2140 0.9170 0.060 Uiso 1 1 calc R . . H34B H -0.1792 0.1296 0.9335 0.060 Uiso 1 1 calc R . . H34C H -0.2126 0.2402 0.9370 0.060 Uiso 1 1 calc R . . C35 C -0.3284(4) 0.2329(4) 0.6542(4) 0.0554(15) Uani 1 1 d . . . H35A H -0.3857 0.2029 0.7127 0.083 Uiso 1 1 calc R . . H35B H -0.3178 0.1921 0.6075 0.083 Uiso 1 1 calc R . . H35C H -0.3459 0.2995 0.6264 0.083 Uiso 1 1 calc R . . C36 C 0.0609(4) 0.2886(4) 0.5486(4) 0.0424(12) Uani 1 1 d . . . H36A H 0.0493 0.3324 0.4922 0.064 Uiso 1 1 calc R . . H36B H 0.0870 0.2261 0.5331 0.064 Uiso 1 1 calc R . . H36C H 0.1126 0.3205 0.5668 0.064 Uiso 1 1 calc R . . Sr Sr 0.5000 0.5000 1.0000 0.0463(2) Uani 1 2 d S . . O1 O 0.4641(3) 0.3238(3) 1.0048(3) 0.0550(10) Uani 1 1 d . . . O2 O 0.3541(3) 0.5389(3) 0.9342(3) 0.0514(10) Uani 1 1 d . . . O3 O 0.3733(3) 0.4806(3) 1.1685(3) 0.0556(10) Uani 1 1 d . . . C37 C 0.3951(5) 0.2524(4) 1.0872(5) 0.0675(17) Uani 1 1 d . . . H37A H 0.3212 0.2691 1.0978 0.081 Uiso 1 1 calc R . . H37B H 0.4123 0.2525 1.1461 0.081 Uiso 1 1 calc R . . C38 C 0.4122(5) 0.1523(4) 1.0642(5) 0.0655(17) Uani 1 1 d . . . H38A H 0.4368 0.1063 1.1126 0.079 Uiso 1 1 calc R . . H38B H 0.3467 0.1235 1.0631 0.079 Uiso 1 1 calc R . . C39 C 0.4939(7) 0.1709(5) 0.9668(6) 0.107(3) Uani 1 1 d . . . H39A H 0.5613 0.1454 0.9722 0.129 Uiso 1 1 calc R . . H39B H 0.4723 0.1372 0.9246 0.129 Uiso 1 1 calc R . . C40 C 0.5045(7) 0.2759(6) 0.9278(5) 0.093(2) Uani 1 1 d . . . H40A H 0.5791 0.2968 0.8933 0.111 Uiso 1 1 calc R . . H40B H 0.4655 0.2944 0.8815 0.111 Uiso 1 1 calc R . . C41 C 0.3042(5) 0.4758(4) 0.8957(5) 0.0566(15) Uani 1 1 d . . . H41A H 0.2652 0.4189 0.9473 0.068 Uiso 1 1 calc R . . H41B H 0.3571 0.4502 0.8454 0.068 Uiso 1 1 calc R . . C42 C 0.2308(4) 0.5386(4) 0.8536(4) 0.0536(14) Uani 1 1 d . . . H42A H 0.1583 0.5278 0.8990 0.064 Uiso 1 1 calc R . . H42B H 0.2320 0.5238 0.7924 0.064 Uiso 1 1 calc R . . C43 C 0.2723(5) 0.6429(4) 0.8371(5) 0.0640(17) Uani 1 1 d . . . H43A H 0.3280 0.6638 0.7740 0.077 Uiso 1 1 calc R . . H43B H 0.2158 0.6901 0.8402 0.077 Uiso 1 1 calc R . . C44 C 0.3141(6) 0.6359(4) 0.9172(5) 0.0705(19) Uani 1 1 d . . . H44A H 0.3705 0.6876 0.8997 0.085 Uiso 1 1 calc R . . H44B H 0.2581 0.6446 0.9755 0.085 Uiso 1 1 calc R . . C45 C 0.2673(5) 0.5126(5) 1.1904(5) 0.0640(17) Uani 1 1 d . . . H45A H 0.2264 0.4767 1.1633 0.077 Uiso 1 1 calc R . . H45B H 0.2672 0.5844 1.1624 0.077 Uiso 1 1 calc R . . C46 C 0.2212(5) 0.4905(5) 1.2967(5) 0.0733(19) Uani 1 1 d . . . H46A H 0.1727 0.4311 1.3209 0.088 Uiso 1 1 calc R . . H46B H 0.1826 0.5471 1.3173 0.088 Uiso 1 1 calc R . . C47 C 0.3112(6) 0.4727(6) 1.3330(5) 0.087(2) Uani 1 1 d . . . H47A H 0.3369 0.5347 1.3415 0.104 Uiso 1 1 calc R . . H47B H 0.2917 0.4227 1.3952 0.104 Uiso 1 1 calc R . . C48 C 0.3898(6) 0.4366(6) 1.2585(5) 0.083(2) Uani 1 1 d . . . H48A H 0.4608 0.4557 1.2559 0.100 Uiso 1 1 calc R . . H48B H 0.3826 0.3635 1.2722 0.100 Uiso 1 1 calc R . . O1TB O 0.2408(4) 0.1248(3) 1.2673(3) 0.0782(13) Uani 1 1 d . . . C1TB C 0.1897(5) 0.1525(4) 1.3535(4) 0.0602(16) Uani 1 1 d . . . H1TC H 0.1715 0.2227 1.3400 0.072 Uiso 1 1 calc R . . H1TD H 0.2354 0.1445 1.3941 0.072 Uiso 1 1 calc R . . C2TB C 0.0926(5) 0.0862(5) 1.4037(5) 0.0748(19) Uani 1 1 d . . . H2TC H 0.0766 0.0704 1.4744 0.090 Uiso 1 1 calc R . . H2TD H 0.0319 0.1171 1.3875 0.090 Uiso 1 1 calc R . . C3TB C 0.1195(6) -0.0043(5) 1.3658(6) 0.095(3) Uani 1 1 d . . . H3TC H 0.1407 -0.0565 1.4122 0.113 Uiso 1 1 calc R . . H3TD H 0.0588 -0.0304 1.3539 0.113 Uiso 1 1 calc R . . C4TB C 0.2069(6) 0.0274(5) 1.2751(5) 0.079(2) Uani 1 1 d . . . H4TC H 0.2651 -0.0174 1.2751 0.094 Uiso 1 1 calc R . . H4TD H 0.1838 0.0251 1.2198 0.094 Uiso 1 1 calc R . . O1TA O 0.5674(4) 0.1524(3) 1.2102(4) 0.0870(15) Uani 1 1 d . . . C1TA C 0.5084(7) 0.1244(6) 1.3083(6) 0.094(2) Uani 1 1 d . . . H1TA H 0.4393 0.1540 1.3196 0.112 Uiso 1 1 calc R . . H1TB H 0.5451 0.1477 1.3469 0.112 Uiso 1 1 calc R . . C2TA C 0.4949(6) 0.0154(5) 1.3361(5) 0.076(2) Uani 1 1 d . . . H2TA H 0.4213 -0.0063 1.3495 0.091 Uiso 1 1 calc R . . H2TB H 0.5152 -0.0118 1.3941 0.091 Uiso 1 1 calc R . . C3TA C 0.5660(6) -0.0173(5) 1.2509(5) 0.083(2) Uani 1 1 d . . . H3TA H 0.6102 -0.0702 1.2710 0.100 Uiso 1 1 calc R . . H3TB H 0.5252 -0.0420 1.2162 0.100 Uiso 1 1 calc R . . C4TA C 0.6310(5) 0.0737(6) 1.1895(5) 0.079(2) Uani 1 1 d . . . H4TA H 0.6958 0.0784 1.2057 0.094 Uiso 1 1 calc R . . H4TB H 0.6502 0.0739 1.1205 0.094 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 V 0.0302(4) 0.0295(4) 0.0363(5) -0.0107(3) -0.0108(4) -0.0007(3) C1 0.031(3) 0.035(3) 0.041(3) -0.008(2) -0.013(2) -0.002(2) C2 0.031(3) 0.036(3) 0.037(3) -0.012(2) -0.013(2) -0.001(2) C3 0.048(3) 0.030(3) 0.052(3) -0.010(2) -0.023(3) -0.005(2) C4 0.048(3) 0.039(3) 0.046(3) -0.019(2) -0.019(3) 0.008(2) C5 0.044(3) 0.048(3) 0.043(3) -0.021(2) -0.015(3) 0.005(2) C6 0.035(3) 0.039(3) 0.044(3) -0.015(2) -0.016(2) 0.002(2) C7 0.043(3) 0.038(3) 0.048(3) -0.012(2) -0.008(3) -0.005(2) C8 0.082(5) 0.043(3) 0.059(4) -0.027(3) -0.018(3) 0.008(3) C9 0.040(3) 0.046(3) 0.050(3) -0.017(3) -0.009(3) 0.000(2) C10 0.034(3) 0.032(2) 0.039(3) -0.014(2) -0.014(2) 0.001(2) C11 0.030(3) 0.037(3) 0.038(3) -0.014(2) -0.010(2) -0.001(2) C12 0.034(3) 0.038(3) 0.047(3) -0.016(2) -0.015(2) 0.003(2) C13 0.037(3) 0.036(3) 0.040(3) -0.014(2) -0.010(2) -0.006(2) C14 0.044(3) 0.031(2) 0.038(3) -0.006(2) -0.014(2) -0.001(2) C15 0.032(3) 0.036(3) 0.042(3) -0.011(2) -0.013(2) 0.001(2) C16 0.032(3) 0.033(3) 0.055(3) -0.008(2) -0.019(2) 0.002(2) C17 0.041(3) 0.041(3) 0.053(3) -0.010(2) -0.010(3) -0.007(2) C18 0.042(3) 0.041(3) 0.056(4) -0.010(2) -0.020(3) 0.005(2) C19 0.028(2) 0.033(2) 0.042(3) -0.010(2) -0.014(2) -0.003(2) C20 0.035(3) 0.032(3) 0.044(3) -0.010(2) -0.015(2) 0.002(2) C21 0.043(3) 0.039(3) 0.035(3) -0.007(2) -0.017(2) -0.001(2) C22 0.043(3) 0.039(3) 0.035(3) -0.014(2) -0.009(2) -0.006(2) C23 0.034(3) 0.033(3) 0.046(3) -0.016(2) -0.009(2) 0.001(2) C24 0.031(3) 0.035(3) 0.041(3) -0.014(2) -0.013(2) -0.002(2) C25 0.048(3) 0.039(3) 0.057(4) -0.014(2) -0.019(3) 0.010(2) C26 0.075(4) 0.053(3) 0.046(3) -0.019(3) -0.028(3) 0.006(3) C27 0.037(3) 0.036(3) 0.047(3) -0.015(2) -0.019(2) 0.005(2) C28 0.031(3) 0.030(2) 0.041(3) -0.015(2) -0.012(2) 0.002(2) C29 0.032(3) 0.032(2) 0.044(3) -0.015(2) -0.010(2) 0.001(2) C30 0.031(3) 0.040(3) 0.048(3) -0.016(2) -0.008(2) -0.002(2) C31 0.037(3) 0.035(3) 0.051(3) -0.012(2) -0.017(3) 0.000(2) C32 0.043(3) 0.038(3) 0.042(3) -0.014(2) -0.018(3) -0.002(2) C33 0.030(3) 0.030(2) 0.044(3) -0.011(2) -0.012(2) -0.001(2) C34 0.033(3) 0.046(3) 0.039(3) -0.014(2) -0.008(2) 0.001(2) C35 0.039(3) 0.069(4) 0.068(4) -0.025(3) -0.025(3) 0.002(3) C36 0.038(3) 0.046(3) 0.044(3) -0.012(2) -0.014(2) 0.000(2) Sr 0.0402(4) 0.0576(5) 0.0452(5) -0.0167(4) -0.0160(4) -0.0002(3) O1 0.053(2) 0.057(2) 0.054(3) -0.0182(19) -0.012(2) -0.0013(19) O2 0.055(2) 0.053(2) 0.061(3) -0.0226(19) -0.033(2) 0.0031(18) O3 0.046(2) 0.074(3) 0.045(2) -0.0157(19) -0.0117(19) 0.008(2) C37 0.057(4) 0.067(4) 0.068(5) -0.017(3) -0.005(3) -0.005(3) C38 0.065(4) 0.061(4) 0.071(5) -0.023(3) -0.016(4) -0.005(3) C39 0.116(7) 0.069(5) 0.098(6) -0.036(4) 0.031(5) -0.025(5) C40 0.112(7) 0.085(5) 0.064(5) -0.024(4) -0.004(5) 0.021(5) C41 0.056(4) 0.057(4) 0.068(4) -0.024(3) -0.027(3) 0.002(3) C42 0.042(3) 0.066(4) 0.062(4) -0.029(3) -0.018(3) 0.002(3) C43 0.068(4) 0.059(4) 0.068(4) -0.001(3) -0.036(4) -0.002(3) C44 0.092(5) 0.055(4) 0.089(5) -0.029(3) -0.055(4) 0.009(4) C45 0.046(4) 0.076(4) 0.069(5) -0.018(3) -0.017(3) 0.004(3) C46 0.054(4) 0.080(5) 0.069(5) -0.012(4) -0.002(4) 0.004(3) C47 0.073(5) 0.126(7) 0.053(4) -0.022(4) -0.009(4) 0.007(5) C48 0.071(5) 0.123(6) 0.056(4) -0.020(4) -0.024(4) 0.028(4) O1TB 0.085(3) 0.064(3) 0.068(3) -0.020(2) 0.005(3) -0.019(2) C1TB 0.062(4) 0.060(4) 0.058(4) -0.009(3) -0.021(3) -0.013(3) C2TB 0.076(5) 0.059(4) 0.077(5) -0.020(3) -0.005(4) -0.013(3) C3TB 0.094(6) 0.069(5) 0.107(7) -0.035(4) -0.002(5) -0.020(4) C4TB 0.095(6) 0.059(4) 0.074(5) -0.017(3) -0.013(4) -0.016(4) O1TA 0.085(4) 0.055(3) 0.108(4) -0.015(3) -0.017(3) -0.001(3) C1TA 0.090(6) 0.086(6) 0.110(7) -0.054(5) -0.019(5) 0.015(5) C2TA 0.070(5) 0.067(4) 0.080(5) -0.022(4) -0.006(4) 0.009(4) C3TA 0.095(6) 0.058(4) 0.077(5) -0.014(4) -0.003(4) 0.021(4) C4TA 0.053(4) 0.104(6) 0.075(5) -0.021(4) -0.017(4) 0.019(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 V C19 2.133(5) . ? V C10 2.148(5) . ? V C1 2.147(5) . ? V C28 2.159(5) . ? C1 C6 1.403(7) . ? C1 C2 1.414(6) . ? C2 C3 1.395(6) . ? C2 C7 1.510(7) . ? C3 C4 1.375(7) . ? C4 C5 1.388(7) . ? C4 C8 1.520(6) . ? C5 C6 1.408(6) . ? C6 C9 1.518(7) . ? C10 C15 1.411(6) . ? C10 C11 1.430(6) . ? C11 C12 1.384(6) . ? C11 C16 1.512(6) . ? C12 C13 1.403(6) . ? C13 C14 1.384(7) . ? C13 C17 1.509(6) . ? C14 C15 1.408(6) . ? C15 C18 1.522(6) . ? C19 C20 1.417(6) . ? C19 C24 1.425(6) . ? C20 C21 1.404(6) . ? C20 C25 1.520(6) . ? C21 C22 1.378(6) . ? C22 C23 1.386(7) . ? C22 C26 1.518(7) . ? C23 C24 1.390(6) . ? C24 C27 1.515(6) . ? C28 C33 1.404(6) . ? C28 C29 1.410(6) . ? C29 C30 1.407(6) . ? C29 C34 1.518(7) . ? C30 C31 1.377(7) . ? C31 C32 1.392(7) . ? C31 C35 1.509(7) . ? C32 C33 1.402(6) . ? C33 C36 1.516(7) . ? Sr O2 2.476(3) 2_667 ? Sr O2 2.476(3) . ? Sr O1 2.493(4) 2_667 ? Sr O1 2.493(4) . ? Sr O3 2.528(4) 2_667 ? Sr O3 2.528(4) . ? O1 C40 1.426(7) . ? O1 C37 1.459(7) . ? O2 C44 1.438(6) . ? O2 C41 1.447(6) . ? O3 C48 1.439(7) . ? O3 C45 1.447(6) . ? C37 C38 1.509(8) . ? C38 C39 1.498(9) . ? C39 C40 1.433(9) . ? C41 C42 1.500(7) . ? C42 C43 1.506(8) . ? C43 C44 1.476(8) . ? C45 C46 1.483(9) . ? C46 C47 1.480(9) . ? C47 C48 1.455(9) . ? O1TB C1TB 1.402(7) . ? O1TB C4TB 1.409(7) . ? C1TB C2TB 1.499(8) . ? C2TB C3TB 1.492(9) . ? C3TB C4TB 1.474(10) . ? O1TA C4TA 1.405(8) . ? O1TA C1TA 1.403(9) . ? C1TA C2TA 1.475(9) . ? C2TA C3TA 1.499(9) . ? C3TA C4TA 1.490(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 V C10 96.97(17) . . ? C19 V C1 118.18(17) . . ? C10 V C1 115.15(18) . . ? C19 V C28 113.51(18) . . ? C10 V C28 117.57(17) . . ? C1 V C28 96.86(16) . . ? C6 C1 C2 115.4(4) . . ? C6 C1 V 128.3(4) . . ? C2 C1 V 116.0(3) . . ? C3 C2 C1 122.6(5) . . ? C3 C2 C7 116.7(4) . . ? C1 C2 C7 120.7(4) . . ? C4 C3 C2 121.0(5) . . ? C3 C4 C5 118.0(4) . . ? C3 C4 C8 121.0(5) . . ? C5 C4 C8 121.0(5) . . ? C4 C5 C6 121.4(5) . . ? C1 C6 C5 121.5(5) . . ? C1 C6 C9 123.1(4) . . ? C5 C6 C9 115.4(5) . . ? C15 C10 C11 114.6(4) . . ? C15 C10 V 130.2(3) . . ? C11 C10 V 115.0(3) . . ? C12 C11 C10 122.8(4) . . ? C12 C11 C16 116.7(4) . . ? C10 C11 C16 120.5(4) . . ? C11 C12 C13 121.7(4) . . ? C14 C13 C12 116.6(4) . . ? C14 C13 C17 121.9(4) . . ? C12 C13 C17 121.5(4) . . ? C13 C14 C15 122.5(4) . . ? C14 C15 C10 121.8(4) . . ? C14 C15 C18 116.0(4) . . ? C10 C15 C18 122.1(4) . . ? C20 C19 C24 115.4(4) . . ? C20 C19 V 129.1(3) . . ? C24 C19 V 115.4(3) . . ? C21 C20 C19 121.4(4) . . ? C21 C20 C25 116.5(4) . . ? C19 C20 C25 122.1(4) . . ? C22 C21 C20 122.0(4) . . ? C23 C22 C21 117.4(4) . . ? C23 C22 C26 121.0(4) . . ? C21 C22 C26 121.6(5) . . ? C22 C23 C24 122.2(4) . . ? C23 C24 C19 121.5(4) . . ? C23 C24 C27 117.8(4) . . ? C19 C24 C27 120.7(4) . . ? C33 C28 C29 116.0(4) . . ? C33 C28 V 116.1(3) . . ? C29 C28 V 127.7(3) . . ? C30 C29 C28 120.3(4) . . ? C30 C29 C34 115.6(4) . . ? C28 C29 C34 124.2(4) . . ? C31 C30 C29 123.3(5) . . ? C30 C31 C32 116.8(4) . . ? C30 C31 C35 121.5(5) . . ? C32 C31 C35 121.7(5) . . ? C31 C32 C33 120.9(5) . . ? C32 C33 C28 122.6(5) . . ? C32 C33 C36 116.5(4) . . ? C28 C33 C36 120.9(4) . . ? O2 Sr O2 180.000(1) 2_667 . ? O2 Sr O1 86.49(12) 2_667 2_667 ? O2 Sr O1 93.51(12) . 2_667 ? O2 Sr O1 93.51(12) 2_667 . ? O2 Sr O1 86.49(12) . . ? O1 Sr O1 180.00(19) 2_667 . ? O2 Sr O3 89.92(12) 2_667 2_667 ? O2 Sr O3 90.08(12) . 2_667 ? O1 Sr O3 91.09(13) 2_667 2_667 ? O1 Sr O3 88.91(13) . 2_667 ? O2 Sr O3 90.08(12) 2_667 . ? O2 Sr O3 89.92(12) . . ? O1 Sr O3 88.91(13) 2_667 . ? O1 Sr O3 91.09(13) . . ? O3 Sr O3 180.000(1) 2_667 . ? C40 O1 C37 108.2(5) . . ? C40 O1 Sr 126.5(4) . . ? C37 O1 Sr 125.3(3) . . ? C44 O2 C41 108.4(4) . . ? C44 O2 Sr 123.4(3) . . ? C41 O2 Sr 127.7(3) . . ? C48 O3 C45 107.5(4) . . ? C48 O3 Sr 128.3(3) . . ? C45 O3 Sr 124.2(3) . . ? O1 C37 C38 106.7(5) . . ? C39 C38 C37 105.3(5) . . ? C40 C39 C38 107.0(6) . . ? O1 C40 C39 108.7(6) . . ? O2 C41 C42 106.5(4) . . ? C41 C42 C43 103.8(4) . . ? C44 C43 C42 102.7(5) . . ? O2 C44 C43 106.2(4) . . ? O3 C45 C46 107.0(5) . . ? C45 C46 C47 105.3(5) . . ? C48 C47 C46 104.1(6) . . ? O3 C48 C47 107.2(5) . . ? C1TB O1TB C4TB 109.4(5) . . ? O1TB C1TB C2TB 106.8(5) . . ? C3TB C2TB C1TB 103.4(6) . . ? C4TB C3TB C2TB 105.6(6) . . ? O1TB C4TB C3TB 108.3(5) . . ? C4TA O1TA C1TA 106.8(5) . . ? O1TA C1TA C2TA 107.8(5) . . ? C1TA C2TA C3TA 104.6(6) . . ? C4TA C3TA C2TA 104.2(6) . . ? O1TA C4TA C3TA 104.8(5) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.305 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.069