# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Markus Albrecht' _publ_contact_author_email MARKUS.ALBRECHT@OC.RWTH-AACHEN.DE _publ_section_title ; Self-assembly of heterodinuclear triple-stranded helicates: control by coordination number and charge ; loop_ _publ_author_name 'Markus Albrecht' 'Roland Frohlich' 'Yufeng Liu.' 'Christophe Schalley' 'Sascha S. Zhu' data_fro4627 _database_code_depnum_ccdc_archive 'CCDC 706323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 La N7 O11 Ti' _chemical_formula_weight 1053.66 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0557(3) _cell_length_b 13.5293(3) _cell_length_c 14.6211(4) _cell_angle_alpha 87.912(1) _cell_angle_beta 84.021(1) _cell_angle_gamma 65.240(1) _cell_volume 2153.70(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6558 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.9408 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28190 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.92 _reflns_number_total 10191 _reflns_number_gt 8205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.6557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'at N from difmap, others geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10191 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 Ti Ti 1.00508(5) 1.28622(4) 0.26747(4) 0.02451(12) Uani 1 1 d . . . La La 0.784447(15) 1.556368(12) 0.245662(12) 0.02414(6) Uani 1 1 d . . . O1A O 1.02068(18) 1.40042(15) 0.18145(14) 0.0264(4) Uani 1 1 d . . . O2A O 1.17597(18) 1.25416(15) 0.27272(14) 0.0281(5) Uani 1 1 d . . . C1A C 1.1279(3) 1.4081(2) 0.1813(2) 0.0247(6) Uani 1 1 d . . . C2A C 1.2164(3) 1.3257(2) 0.2299(2) 0.0272(6) Uani 1 1 d . . . C3A C 1.3313(3) 1.3225(3) 0.2329(2) 0.0351(7) Uani 1 1 d . . . H3A H 1.3899 1.2668 0.2649 0.042 Uiso 1 1 calc R . . C4A C 1.3597(3) 1.4025(3) 0.1881(3) 0.0430(8) Uani 1 1 d . . . H4A H 1.4381 1.4010 0.1901 0.052 Uiso 1 1 calc R . . C5A C 1.2749(3) 1.4837(3) 0.1408(3) 0.0390(8) Uani 1 1 d . . . H5A H 1.2961 1.5371 0.1111 0.047 Uiso 1 1 calc R . . C6A C 1.1563(3) 1.4887(2) 0.1361(2) 0.0285(7) Uani 1 1 d . . . C7A C 1.0686(3) 1.5755(2) 0.0854(2) 0.0337(7) Uani 1 1 d . . . H7A H 1.0976 1.6156 0.0434 0.040 Uiso 1 1 calc R . . N8A N 0.9542(2) 1.59955(19) 0.09525(18) 0.0309(6) Uani 1 1 d . . . N9A N 0.8840(2) 1.6820(2) 0.0393(2) 0.0351(6) Uani 1 1 d . . . H9A H 0.919(3) 1.707(3) -0.006(3) 0.045(11) Uiso 1 1 d . . . C10A C 0.7634(3) 1.7076(2) 0.0448(2) 0.0300(7) Uani 1 1 d . . . O10A O 0.7174(2) 1.65928(18) 0.09817(16) 0.0382(5) Uani 1 1 d . . . C11A C 0.6871(3) 1.7963(2) -0.0142(2) 0.0360(8) Uani 1 1 d . . . C12A C 0.5673(3) 1.8095(3) -0.0211(3) 0.0459(9) Uani 1 1 d . . . H12A H 0.5375 1.7627 0.0110 0.055 Uiso 1 1 calc R . . C13A C 0.4924(4) 1.8911(3) -0.0749(3) 0.0607(12) Uani 1 1 d . . . H13A H 0.4116 1.8998 -0.0794 0.073 Uiso 1 1 calc R . . C14A C 0.5356(4) 1.9596(3) -0.1220(3) 0.0639(13) Uani 1 1 d . . . H14A H 0.4839 2.0152 -0.1583 0.077 Uiso 1 1 calc R . . C15A C 0.6525(4) 1.9479(3) -0.1165(3) 0.0578(12) Uani 1 1 d . . . H15A H 0.6816 1.9945 -0.1497 0.069 Uiso 1 1 calc R . . C16A C 0.7288(3) 1.8667(3) -0.0616(3) 0.0444(9) Uani 1 1 d . . . H16A H 0.8089 1.8597 -0.0567 0.053 Uiso 1 1 calc R . . O1B O 0.92981(18) 1.42081(14) 0.34939(14) 0.0254(4) Uani 1 1 d . . . O2B O 0.99124(19) 1.22243(15) 0.38285(15) 0.0307(5) Uani 1 1 d . . . C1B C 0.9180(3) 1.3991(2) 0.4390(2) 0.0252(6) Uani 1 1 d . . . C2B C 0.9564(3) 1.2874(2) 0.4587(2) 0.0277(6) Uani 1 1 d . . . C3B C 0.9529(3) 1.2532(2) 0.5486(2) 0.0350(7) Uani 1 1 d . . . H3B H 0.9776 1.1789 0.5620 0.042 Uiso 1 1 calc R . . C4B C 0.9122(3) 1.3308(3) 0.6194(2) 0.0374(8) Uani 1 1 d . . . H4B H 0.9110 1.3081 0.6809 0.045 Uiso 1 1 calc R . . C5B C 0.8737(3) 1.4399(2) 0.6001(2) 0.0333(7) Uani 1 1 d . . . H5B H 0.8479 1.4906 0.6488 0.040 Uiso 1 1 calc R . . C6B C 0.8724(3) 1.4764(2) 0.5092(2) 0.0276(6) Uani 1 1 d . . . C7B C 0.8290(3) 1.5925(2) 0.4923(2) 0.0272(6) Uani 1 1 d . . . H7B H 0.8175 1.6388 0.5422 0.033 Uiso 1 1 calc R . . N8B N 0.8052(2) 1.63532(18) 0.41214(17) 0.0262(5) Uani 1 1 d . . . N9B N 0.7720(2) 1.74730(19) 0.4098(2) 0.0290(6) Uani 1 1 d . . . H9B H 0.761(3) 1.776(2) 0.460(2) 0.020(8) Uiso 1 1 d . . . C10B C 0.7815(3) 1.7912(2) 0.3272(2) 0.0275(6) Uani 1 1 d . . . O10B O 0.8038(2) 1.73725(16) 0.25548(15) 0.0339(5) Uani 1 1 d . . . C11B C 0.7697(3) 1.9056(2) 0.3247(2) 0.0304(7) Uani 1 1 d . . . C12B C 0.7748(3) 1.9599(2) 0.4023(3) 0.0388(8) Uani 1 1 d . . . H12B H 0.7793 1.9266 0.4602 0.047 Uiso 1 1 calc R . . C13B C 0.7730(4) 2.0627(3) 0.3940(3) 0.0491(10) Uani 1 1 d . . . H13B H 0.7775 2.0987 0.4464 0.059 Uiso 1 1 calc R . . C14B C 0.7650(4) 2.1126(3) 0.3098(3) 0.0493(10) Uani 1 1 d . . . H14B H 0.7646 2.1821 0.3046 0.059 Uiso 1 1 calc R . . C15B C 0.7574(4) 2.0612(3) 0.2342(3) 0.0550(11) Uani 1 1 d . . . H15B H 0.7502 2.0960 0.1769 0.066 Uiso 1 1 calc R . . C16B C 0.7604(4) 1.9570(3) 0.2410(3) 0.0444(9) Uani 1 1 d . . . H16B H 0.7559 1.9217 0.1882 0.053 Uiso 1 1 calc R . . O1C O 0.83550(17) 1.35714(15) 0.22113(14) 0.0259(4) Uani 1 1 d . . . O2C O 1.01535(18) 1.17865(15) 0.18330(15) 0.0309(5) Uani 1 1 d . . . C1C C 0.8254(3) 1.3068(2) 0.1468(2) 0.0245(6) Uani 1 1 d . . . C2C C 0.9257(3) 1.2060(2) 0.1268(2) 0.0294(7) Uani 1 1 d . . . C3C C 0.9270(3) 1.1427(2) 0.0542(2) 0.0390(8) Uani 1 1 d . . . H3C H 0.9944 1.0760 0.0400 0.047 Uiso 1 1 calc R . . C4C C 0.8266(3) 1.1795(3) 0.0025(3) 0.0425(9) Uani 1 1 d . . . H4C H 0.8260 1.1363 -0.0461 0.051 Uiso 1 1 calc R . . C5C C 0.7279(3) 1.2786(2) 0.0218(2) 0.0347(7) Uani 1 1 d . . . H5C H 0.6612 1.3015 -0.0140 0.042 Uiso 1 1 calc R . . C6C C 0.7256(3) 1.3459(2) 0.0940(2) 0.0266(6) Uani 1 1 d . . . C7C C 0.6192(3) 1.4494(2) 0.1113(2) 0.0271(6) Uani 1 1 d . . . H7C H 0.5515 1.4632 0.0782 0.033 Uiso 1 1 calc R . . N8C N 0.6101(2) 1.52357(18) 0.16821(17) 0.0262(5) Uani 1 1 d . . . N9C N 0.4931(2) 1.61021(18) 0.17720(18) 0.0278(6) Uani 1 1 d . . . C10C C 0.4879(3) 1.6847(2) 0.2356(2) 0.0277(6) Uani 1 1 d . . . O10C O 0.57632(19) 1.68483(16) 0.27768(15) 0.0329(5) Uani 1 1 d . . . C11C C 0.3648(3) 1.7773(2) 0.2562(2) 0.0279(7) Uani 1 1 d . . . C12C C 0.3536(3) 1.8606(2) 0.3140(2) 0.0382(8) Uani 1 1 d . . . H12C H 0.4235 1.8594 0.3380 0.046 Uiso 1 1 calc R . . C13C C 0.2389(3) 1.9467(3) 0.3368(3) 0.0445(9) Uani 1 1 d . . . H13C H 0.2321 2.0026 0.3764 0.053 Uiso 1 1 calc R . . C14C C 0.1368(3) 1.9497(2) 0.3018(3) 0.0427(9) Uani 1 1 d . . . H14C H 0.0600 2.0077 0.3168 0.051 Uiso 1 1 calc R . . C15C C 0.1469(3) 1.8678(3) 0.2447(3) 0.0442(9) Uani 1 1 d . . . H15C H 0.0766 1.8702 0.2205 0.053 Uiso 1 1 calc R . . C16C C 0.2600(3) 1.7811(3) 0.2219(2) 0.0379(8) Uani 1 1 d . . . H16C H 0.2653 1.7250 0.1832 0.045 Uiso 1 1 calc R . . O101 O 0.6744(2) 1.48122(17) 0.37588(15) 0.0337(5) Uani 1 1 d . . . C102 C 0.5992(3) 1.4416(3) 0.3761(3) 0.0419(8) Uani 1 1 d . . . H102 H 0.5541 1.4556 0.3247 0.050 Uiso 1 1 calc R . . N103 N 0.5759(3) 1.3813(2) 0.4416(2) 0.0385(7) Uani 1 1 d . . . C104 C 0.6439(4) 1.3531(3) 0.5224(3) 0.0527(10) Uani 1 1 d . . . H10A H 0.7046 1.2782 0.5171 0.079 Uiso 1 1 calc R . . H10B H 0.5876 1.3614 0.5771 0.079 Uiso 1 1 calc R . . H10C H 0.6847 1.4009 0.5269 0.079 Uiso 1 1 calc R . . C105 C 0.4825(4) 1.3413(4) 0.4380(3) 0.0660(13) Uani 1 1 d . . . H10D H 0.4364 1.3728 0.3857 0.099 Uiso 1 1 calc R . . H10E H 0.4274 1.3616 0.4941 0.099 Uiso 1 1 calc R . . H10F H 0.5209 1.2626 0.4316 0.099 Uiso 1 1 calc R . . O201 O 0.6886(2) 1.84318(19) 0.58591(17) 0.0464(6) Uani 1 1 d . . . H201 H 0.7252 1.8209 0.6327 0.070 Uiso 1 1 calc R . . C202 C 0.5668(4) 1.9195(3) 0.6115(3) 0.0570(11) Uani 1 1 d . . . H20A H 0.5105 1.8869 0.6036 0.085 Uiso 1 1 calc R . . H20B H 0.5476 1.9833 0.5730 0.085 Uiso 1 1 calc R . . H20C H 0.5590 1.9404 0.6754 0.085 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 Ti 0.0244(3) 0.0229(2) 0.0256(3) 0.0001(2) -0.0025(2) -0.0092(2) La 0.02560(10) 0.02407(9) 0.02323(10) 0.00087(6) -0.00341(6) -0.01066(7) O1A 0.0239(10) 0.0306(10) 0.0256(12) 0.0022(8) -0.0025(8) -0.0125(8) O2A 0.0279(11) 0.0268(10) 0.0285(12) 0.0030(8) -0.0032(9) -0.0105(8) C1A 0.0249(15) 0.0308(14) 0.0182(15) -0.0040(11) 0.0000(11) -0.0117(12) C2A 0.0293(16) 0.0312(14) 0.0212(16) -0.0012(12) -0.0014(12) -0.0127(12) C3A 0.0282(17) 0.0424(17) 0.037(2) 0.0064(14) -0.0091(14) -0.0155(14) C4A 0.0299(18) 0.060(2) 0.045(2) 0.0086(17) -0.0063(15) -0.0245(16) C5A 0.0346(18) 0.0451(18) 0.043(2) 0.0064(16) -0.0018(15) -0.0232(15) C6A 0.0302(16) 0.0334(15) 0.0244(17) 0.0022(12) -0.0013(12) -0.0161(13) C7A 0.0353(18) 0.0365(16) 0.0313(19) 0.0071(13) 0.0011(14) -0.0185(14) N8A 0.0324(14) 0.0304(13) 0.0268(15) 0.0065(11) -0.0022(11) -0.0108(11) N9A 0.0330(15) 0.0372(14) 0.0309(16) 0.0134(12) -0.0007(12) -0.0122(12) C10A 0.0345(17) 0.0328(15) 0.0218(16) -0.0004(12) -0.0006(13) -0.0136(13) O10A 0.0388(13) 0.0508(13) 0.0314(13) 0.0114(10) -0.0076(10) -0.0250(11) C11A 0.0395(19) 0.0353(16) 0.0227(17) -0.0004(13) 0.0013(14) -0.0062(14) C12A 0.042(2) 0.050(2) 0.039(2) 0.0014(16) -0.0083(17) -0.0121(16) C13A 0.050(2) 0.067(3) 0.049(3) -0.002(2) -0.018(2) -0.005(2) C14A 0.066(3) 0.055(2) 0.036(2) 0.0049(19) -0.010(2) 0.009(2) C15A 0.065(3) 0.046(2) 0.037(2) 0.0147(17) 0.0064(19) -0.0022(19) C16A 0.043(2) 0.0399(18) 0.037(2) 0.0092(15) 0.0023(16) -0.0063(15) O1B 0.0288(11) 0.0248(9) 0.0224(11) 0.0015(8) -0.0024(8) -0.0112(8) O2B 0.0346(12) 0.0230(9) 0.0311(13) 0.0027(9) -0.0006(9) -0.0094(9) C1B 0.0252(15) 0.0280(14) 0.0228(16) 0.0077(12) -0.0056(12) -0.0113(12) C2B 0.0261(15) 0.0299(14) 0.0273(17) 0.0018(12) -0.0009(12) -0.0122(12) C3B 0.0352(18) 0.0322(15) 0.0348(19) 0.0099(14) -0.0039(14) -0.0120(13) C4B 0.0413(19) 0.0440(18) 0.0277(18) 0.0130(14) -0.0075(14) -0.0187(15) C5B 0.0354(17) 0.0372(16) 0.0276(18) 0.0004(13) -0.0021(14) -0.0156(14) C6B 0.0255(15) 0.0300(14) 0.0274(17) 0.0024(12) -0.0046(12) -0.0113(12) C7B 0.0277(15) 0.0297(14) 0.0259(17) -0.0015(12) -0.0012(12) -0.0138(12) N8B 0.0290(13) 0.0235(11) 0.0262(14) -0.0010(10) -0.0019(10) -0.0112(10) N9B 0.0376(15) 0.0243(12) 0.0246(15) -0.0024(11) -0.0013(12) -0.0128(11) C10B 0.0255(15) 0.0292(14) 0.0288(18) 0.0015(13) -0.0042(12) -0.0120(12) O10B 0.0461(13) 0.0345(11) 0.0263(12) -0.0014(9) -0.0014(10) -0.0222(10) C11B 0.0303(16) 0.0291(14) 0.0351(19) 0.0048(13) -0.0065(13) -0.0152(12) C12B 0.047(2) 0.0293(15) 0.040(2) 0.0003(14) -0.0026(16) -0.0162(14) C13B 0.065(3) 0.0312(17) 0.053(3) -0.0028(16) -0.004(2) -0.0223(17) C14B 0.056(2) 0.0349(17) 0.065(3) 0.0119(18) -0.009(2) -0.0266(17) C15B 0.078(3) 0.051(2) 0.052(3) 0.023(2) -0.019(2) -0.042(2) C16B 0.061(2) 0.0458(19) 0.040(2) 0.0096(16) -0.0131(18) -0.0338(18) O1C 0.0250(10) 0.0263(9) 0.0265(12) -0.0052(8) -0.0026(9) -0.0103(8) O2C 0.0287(11) 0.0258(10) 0.0359(13) -0.0033(9) -0.0041(9) -0.0086(8) C1C 0.0278(15) 0.0250(13) 0.0238(16) -0.0022(11) 0.0009(12) -0.0146(12) C2C 0.0300(16) 0.0308(14) 0.0306(18) -0.0010(13) -0.0023(13) -0.0160(13) C3C 0.043(2) 0.0299(15) 0.039(2) -0.0091(14) -0.0038(16) -0.0093(14) C4C 0.054(2) 0.0355(16) 0.038(2) -0.0101(15) -0.0096(17) -0.0167(16) C5C 0.0389(18) 0.0367(16) 0.0305(18) -0.0012(14) -0.0081(14) -0.0167(14) C6C 0.0294(16) 0.0287(14) 0.0249(16) -0.0009(12) -0.0018(12) -0.0152(12) C7C 0.0257(15) 0.0329(15) 0.0255(17) 0.0005(12) -0.0046(12) -0.0145(12) N8C 0.0232(12) 0.0271(12) 0.0275(14) 0.0030(10) -0.0019(10) -0.0102(10) N9C 0.0213(12) 0.0279(12) 0.0310(15) -0.0005(10) -0.0035(10) -0.0067(10) C10C 0.0286(16) 0.0292(14) 0.0229(16) 0.0054(12) -0.0008(12) -0.0104(12) O10C 0.0309(12) 0.0324(11) 0.0332(13) -0.0040(9) -0.0055(10) -0.0100(9) C11C 0.0291(16) 0.0263(14) 0.0251(17) 0.0039(12) 0.0008(13) -0.0096(12) C12C 0.0381(19) 0.0316(16) 0.041(2) -0.0006(14) -0.0032(15) -0.0106(14) C13C 0.049(2) 0.0278(16) 0.048(2) -0.0052(15) 0.0034(18) -0.0082(15) C14C 0.0367(19) 0.0280(15) 0.048(2) 0.0073(15) 0.0056(16) -0.0011(14) C15C 0.0318(18) 0.0427(18) 0.051(2) 0.0048(17) -0.0045(16) -0.0088(15) C16C 0.0361(18) 0.0368(16) 0.037(2) -0.0011(14) -0.0065(15) -0.0106(14) O101 0.0326(12) 0.0397(11) 0.0332(13) 0.0036(10) -0.0020(10) -0.0201(10) C102 0.043(2) 0.051(2) 0.034(2) -0.0018(16) -0.0010(16) -0.0224(17) N103 0.0400(16) 0.0420(15) 0.0376(17) -0.0010(13) 0.0034(13) -0.0227(13) C104 0.048(2) 0.055(2) 0.057(3) 0.0207(19) -0.0086(19) -0.0236(18) C105 0.070(3) 0.081(3) 0.069(3) -0.008(2) 0.007(2) -0.056(3) O201 0.0531(16) 0.0458(13) 0.0286(14) -0.0018(11) -0.0078(11) -0.0081(11) C202 0.052(2) 0.050(2) 0.060(3) 0.0047(19) -0.010(2) -0.0121(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 Ti O2B 1.891(2) . ? Ti O2C 1.896(2) . ? Ti O2A 1.929(2) . ? Ti O1A 2.014(2) . ? Ti O1B 2.0303(19) . ? Ti O1C 2.039(2) . ? Ti La 3.5332(5) . ? La O10C 2.387(2) . ? La O1B 2.529(2) . ? La O1C 2.5314(18) . ? La O10A 2.538(2) . ? La O10B 2.564(2) . ? La O101 2.623(2) . ? La N8C 2.686(2) . ? La N8B 2.769(2) . ? La O1A 2.8281(19) . ? La N8A 3.055(3) . ? O1A C1A 1.339(3) . ? O2A C2A 1.362(3) . ? C1A C6A 1.399(4) . ? C1A C2A 1.411(4) . ? C2A C3A 1.372(4) . ? C3A C4A 1.391(5) . ? C4A C5A 1.371(5) . ? C5A C6A 1.412(4) . ? C6A C7A 1.452(4) . ? C7A N8A 1.271(4) . ? N8A N9A 1.385(4) . ? N9A C10A 1.341(4) . ? C10A O10A 1.233(4) . ? C10A C11A 1.481(4) . ? C11A C16A 1.386(5) . ? C11A C12A 1.394(5) . ? C12A C13A 1.379(5) . ? C13A C14A 1.374(6) . ? C14A C15A 1.361(6) . ? C15A C16A 1.393(5) . ? O1B C1B 1.338(3) . ? O2B C2B 1.358(4) . ? C1B C6B 1.388(4) . ? C1B C2B 1.411(4) . ? C2B C3B 1.380(4) . ? C3B C4B 1.398(5) . ? C4B C5B 1.378(4) . ? C5B C6B 1.401(4) . ? C6B C7B 1.453(4) . ? C7B N8B 1.293(4) . ? N8B N9B 1.395(3) . ? N9B C10B 1.342(4) . ? C10B O10B 1.240(4) . ? C10B C11B 1.494(4) . ? C11B C16B 1.376(5) . ? C11B C12B 1.394(5) . ? C12B C13B 1.384(4) . ? C13B C14B 1.374(5) . ? C14B C15B 1.358(6) . ? C15B C16B 1.396(5) . ? O1C C1C 1.346(3) . ? O2C C2C 1.348(4) . ? C1C C6C 1.397(4) . ? C1C C2C 1.407(4) . ? C2C C3C 1.383(4) . ? C3C C4C 1.393(5) . ? C4C C5C 1.384(4) . ? C5C C6C 1.410(4) . ? C6C C7C 1.457(4) . ? C7C N8C 1.288(4) . ? N8C N9C 1.403(3) . ? N9C C10C 1.322(4) . ? C10C O10C 1.286(4) . ? C10C C11C 1.497(4) . ? C11C C12C 1.386(4) . ? C11C C16C 1.388(5) . ? C12C C13C 1.401(4) . ? C13C C14C 1.366(5) . ? C14C C15C 1.368(5) . ? C15C C16C 1.393(5) . ? O101 C102 1.231(4) . ? C102 N103 1.320(4) . ? N103 C105 1.446(5) . ? N103 C104 1.457(5) . ? O201 C202 1.416(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Ti O2C 102.75(9) . . ? O2B Ti O2A 93.50(9) . . ? O2C Ti O2A 101.58(9) . . ? O2B Ti O1A 155.79(9) . . ? O2C Ti O1A 101.40(9) . . ? O2A Ti O1A 79.99(8) . . ? O2B Ti O1B 79.56(8) . . ? O2C Ti O1B 159.34(9) . . ? O2A Ti O1B 98.74(8) . . ? O1A Ti O1B 78.45(8) . . ? O2B Ti O1C 108.53(9) . . ? O2C Ti O1C 79.17(8) . . ? O2A Ti O1C 157.34(9) . . ? O1A Ti O1C 77.70(8) . . ? O1B Ti O1C 80.65(8) . . ? O2B Ti La 114.49(6) . . ? O2C Ti La 119.07(7) . . ? O2A Ti La 121.17(6) . . ? O1A Ti La 53.12(5) . . ? O1B Ti La 44.62(6) . . ? O1C Ti La 44.75(5) . . ? O10C La O1B 130.48(7) . . ? O10C La O1C 120.44(7) . . ? O1B La O1C 62.72(6) . . ? O10C La O10A 72.74(8) . . ? O1B La O10A 156.76(7) . . ? O1C La O10A 109.27(7) . . ? O10C La O10B 77.19(7) . . ? O1B La O10B 108.48(7) . . ? O1C La O10B 162.26(7) . . ? O10A La O10B 72.40(7) . . ? O10C La O101 70.44(7) . . ? O1B La O101 66.40(7) . . ? O1C La O101 68.12(6) . . ? O10A La O101 133.29(7) . . ? O10B La O101 124.33(7) . . ? O10C La N8C 61.86(7) . . ? O1B La N8C 123.89(6) . . ? O1C La N8C 66.69(7) . . ? O10A La N8C 63.97(7) . . ? O10B La N8C 126.54(7) . . ? O101 La N8C 73.71(7) . . ? O10C La N8B 81.51(7) . . ? O1B La N8B 63.33(6) . . ? O1C La N8B 121.97(7) . . ? O10A La N8B 128.76(7) . . ? O10B La N8B 58.89(7) . . ? O101 La N8B 72.26(7) . . ? N8C La N8B 136.45(7) . . ? O10C La O1A 171.34(7) . . ? O1B La O1A 56.71(6) . . ? O1C La O1A 56.31(6) . . ? O10A La O1A 100.28(7) . . ? O10B La O1A 105.97(6) . . ? O101 La O1A 112.82(6) . . ? N8C La O1A 110.72(6) . . ? N8B La O1A 107.07(6) . . ? O10C La N8A 120.74(7) . . ? O1B La N8A 103.95(7) . . ? O1C La N8A 102.66(6) . . ? O10A La N8A 54.84(7) . . ? O10B La N8A 63.22(7) . . ? O101 La N8A 168.72(6) . . ? N8C La N8A 109.31(7) . . ? N8B La N8A 109.41(7) . . ? O1A La N8A 55.90(6) . . ? O10C La Ti 147.29(5) . . ? O1B La Ti 34.33(4) . . ? O1C La Ti 34.55(5) . . ? O10A La Ti 127.49(5) . . ? O10B La Ti 130.23(5) . . ? O101 La Ti 78.10(5) . . ? N8C La Ti 101.21(5) . . ? N8B La Ti 97.54(5) . . ? O1A La Ti 34.73(4) . . ? N8A La Ti 90.62(5) . . ? C1A O1A Ti 113.56(17) . . ? C1A O1A La 127.69(16) . . ? Ti O1A La 92.16(7) . . ? C2A O2A Ti 116.32(17) . . ? O1A C1A C6A 124.9(3) . . ? O1A C1A C2A 115.1(3) . . ? C6A C1A C2A 119.9(3) . . ? O2A C2A C3A 125.0(3) . . ? O2A C2A C1A 114.0(3) . . ? C3A C2A C1A 121.0(3) . . ? C2A C3A C4A 119.2(3) . . ? C5A C4A C3A 120.9(3) . . ? C4A C5A C6A 121.2(3) . . ? C1A C6A C5A 117.9(3) . . ? C1A C6A C7A 122.2(3) . . ? C5A C6A C7A 119.9(3) . . ? N8A C7A C6A 122.8(3) . . ? C7A N8A N9A 115.3(3) . . ? C7A N8A La 133.7(2) . . ? N9A N8A La 109.09(18) . . ? C10A N9A N8A 117.5(3) . . ? O10A C10A N9A 120.7(3) . . ? O10A C10A C11A 121.2(3) . . ? N9A C10A C11A 118.1(3) . . ? C10A O10A La 132.1(2) . . ? C16A C11A C12A 118.9(3) . . ? C16A C11A C10A 123.2(3) . . ? C12A C11A C10A 117.8(3) . . ? C13A C12A C11A 120.1(4) . . ? C14A C13A C12A 120.2(4) . . ? C15A C14A C13A 120.7(4) . . ? C14A C15A C16A 119.8(4) . . ? C11A C16A C15A 120.3(4) . . ? C1B O1B Ti 113.88(16) . . ? C1B O1B La 132.40(16) . . ? Ti O1B La 101.05(8) . . ? C2B O2B Ti 117.83(17) . . ? O1B C1B C6B 125.2(2) . . ? O1B C1B C2B 114.1(2) . . ? C6B C1B C2B 120.7(3) . . ? O2B C2B C3B 125.7(3) . . ? O2B C2B C1B 114.0(3) . . ? C3B C2B C1B 120.3(3) . . ? C2B C3B C4B 118.9(3) . . ? C5B C4B C3B 120.9(3) . . ? C4B C5B C6B 120.9(3) . . ? C1B C6B C5B 118.2(3) . . ? C1B C6B C7B 122.8(3) . . ? C5B C6B C7B 118.9(3) . . ? N8B C7B C6B 123.4(3) . . ? C7B N8B N9B 114.2(2) . . ? C7B N8B La 133.58(18) . . ? N9B N8B La 111.97(18) . . ? C10B N9B N8B 117.0(3) . . ? O10B C10B N9B 121.1(3) . . ? O10B C10B C11B 121.0(3) . . ? N9B C10B C11B 117.8(3) . . ? C10B O10B La 124.22(19) . . ? C16B C11B C12B 118.9(3) . . ? C16B C11B C10B 118.2(3) . . ? C12B C11B C10B 122.8(3) . . ? C13B C12B C11B 119.9(3) . . ? C14B C13B C12B 120.5(4) . . ? C15B C14B C13B 119.9(3) . . ? C14B C15B C16B 120.4(4) . . ? C11B C16B C15B 120.3(4) . . ? C1C O1C Ti 113.30(16) . . ? C1C O1C La 129.40(17) . . ? Ti O1C La 100.71(8) . . ? C2C O2C Ti 117.42(17) . . ? O1C C1C C6C 125.3(2) . . ? O1C C1C C2C 113.4(3) . . ? C6C C1C C2C 121.3(3) . . ? O2C C2C C3C 124.8(3) . . ? O2C C2C C1C 115.0(3) . . ? C3C C2C C1C 120.3(3) . . ? C2C C3C C4C 118.9(3) . . ? C5C C4C C3C 121.0(3) . . ? C4C C5C C6C 121.2(3) . . ? C1C C6C C5C 117.2(3) . . ? C1C C6C C7C 123.9(3) . . ? C5C C6C C7C 118.9(3) . . ? N8C C7C C6C 125.5(3) . . ? C7C N8C N9C 113.2(2) . . ? C7C N8C La 130.39(19) . . ? N9C N8C La 115.34(16) . . ? C10C N9C N8C 111.2(2) . . ? O10C C10C N9C 127.0(3) . . ? O10C C10C C11C 116.9(3) . . ? N9C C10C C11C 116.0(3) . . ? C10C O10C La 123.17(18) . . ? C12C C11C C16C 118.5(3) . . ? C12C C11C C10C 119.2(3) . . ? C16C C11C C10C 122.3(3) . . ? C11C C12C C13C 120.5(3) . . ? C14C C13C C12C 120.2(3) . . ? C13C C14C C15C 119.7(3) . . ? C14C C15C C16C 120.9(4) . . ? C11C C16C C15C 120.2(3) . . ? C102 O101 La 133.4(2) . . ? O101 C102 N103 126.1(4) . . ? C102 N103 C105 122.6(4) . . ? C102 N103 C104 120.6(3) . . ? C105 N103 C104 116.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2B Ti La O10C -39.55(13) . . . . ? O2C Ti La O10C 82.51(13) . . . . ? O2A Ti La O10C -150.28(12) . . . . ? O1A Ti La O10C 164.79(12) . . . . ? O1B Ti La O10C -81.38(13) . . . . ? O1C Ti La O10C 52.54(13) . . . . ? O2B Ti La O1B 41.83(11) . . . . ? O2C Ti La O1B 163.89(11) . . . . ? O2A Ti La O1B -68.90(11) . . . . ? O1A Ti La O1B -113.83(11) . . . . ? O1C Ti La O1B 133.92(11) . . . . ? O2B Ti La O1C -92.09(11) . . . . ? O2C Ti La O1C 29.97(11) . . . . ? O2A Ti La O1C 157.18(11) . . . . ? O1A Ti La O1C 112.25(11) . . . . ? O1B Ti La O1C -133.92(11) . . . . ? O2B Ti La O10A -159.71(10) . . . . ? O2C Ti La O10A -37.65(10) . . . . ? O2A Ti La O10A 89.56(10) . . . . ? O1A Ti La O10A 44.63(10) . . . . ? O1B Ti La O10A 158.46(10) . . . . ? O1C Ti La O10A -67.62(10) . . . . ? O2B Ti La O10B 101.67(10) . . . . ? O2C Ti La O10B -136.26(10) . . . . ? O2A Ti La O10B -9.05(10) . . . . ? O1A Ti La O10B -53.99(10) . . . . ? O1B Ti La O10B 59.84(10) . . . . ? O1C Ti La O10B -166.23(10) . . . . ? O2B Ti La O101 -23.53(9) . . . . ? O2C Ti La O101 98.53(9) . . . . ? O2A Ti La O101 -134.26(9) . . . . ? O1A Ti La O101 -179.20(9) . . . . ? O1B Ti La O101 -65.37(9) . . . . ? O1C Ti La O101 68.56(10) . . . . ? O2B Ti La N8C -94.02(9) . . . . ? O2C Ti La N8C 28.04(9) . . . . ? O2A Ti La N8C 155.25(9) . . . . ? O1A Ti La N8C 110.32(9) . . . . ? O1B Ti La N8C -135.85(9) . . . . ? O1C Ti La N8C -1.93(10) . . . . ? O2B Ti La N8B 46.47(9) . . . . ? O2C Ti La N8B 168.53(9) . . . . ? O2A Ti La N8B -64.26(9) . . . . ? O1A Ti La N8B -109.19(9) . . . . ? O1B Ti La N8B 4.64(9) . . . . ? O1C Ti La N8B 138.56(10) . . . . ? O2B Ti La O1A 155.66(11) . . . . ? O2C Ti La O1A -82.28(11) . . . . ? O2A Ti La O1A 44.93(10) . . . . ? O1B Ti La O1A 113.83(11) . . . . ? O1C Ti La O1A -112.25(11) . . . . ? O2B Ti La N8A 156.14(9) . . . . ? O2C Ti La N8A -81.79(9) . . . . ? O2A Ti La N8A 45.42(9) . . . . ? O1A Ti La N8A 0.48(9) . . . . ? O1B Ti La N8A 114.31(9) . . . . ? O1C Ti La N8A -111.76(10) . . . . ? O2B Ti O1A C1A 67.0(3) . . . . ? O2C Ti O1A C1A -108.93(18) . . . . ? O2A Ti O1A C1A -9.00(17) . . . . ? O1B Ti O1A C1A 92.16(18) . . . . ? O1C Ti O1A C1A 174.97(18) . . . . ? La Ti O1A C1A 133.14(19) . . . . ? O2B Ti O1A La -66.1(2) . . . . ? O2C Ti O1A La 117.93(8) . . . . ? O2A Ti O1A La -142.14(8) . . . . ? O1B Ti O1A La -40.98(7) . . . . ? O1C Ti O1A La 41.83(7) . . . . ? O10C La O1A C1A 128.0(4) . . . . ? O1B La O1A C1A -84.2(2) . . . . ? O1C La O1A C1A -161.4(2) . . . . ? O10A La O1A C1A 92.2(2) . . . . ? O10B La O1A C1A 17.7(2) . . . . ? O101 La O1A C1A -121.5(2) . . . . ? N8C La O1A C1A 158.1(2) . . . . ? N8B La O1A C1A -44.0(2) . . . . ? N8A La O1A C1A 58.3(2) . . . . ? Ti La O1A C1A -122.3(2) . . . . ? O10C La O1A Ti -109.7(4) . . . . ? O1B La O1A Ti 38.11(7) . . . . ? O1C La O1A Ti -39.11(7) . . . . ? O10A La O1A Ti -145.49(8) . . . . ? O10B La O1A Ti 140.03(7) . . . . ? O101 La O1A Ti 0.85(9) . . . . ? N8C La O1A Ti -79.58(9) . . . . ? N8B La O1A Ti 78.35(8) . . . . ? N8A La O1A Ti -179.42(11) . . . . ? O2B Ti O2A C2A -148.90(19) . . . . ? O2C Ti O2A C2A 107.31(19) . . . . ? O1A Ti O2A C2A 7.60(19) . . . . ? O1B Ti O2A C2A -68.9(2) . . . . ? O1C Ti O2A C2A 17.7(3) . . . . ? La Ti O2A C2A -27.4(2) . . . . ? Ti O1A C1A C6A -172.3(2) . . . . ? La O1A C1A C6A -59.4(4) . . . . ? Ti O1A C1A C2A 8.9(3) . . . . ? La O1A C1A C2A 121.8(2) . . . . ? Ti O2A C2A C3A 173.8(2) . . . . ? Ti O2A C2A C1A -5.1(3) . . . . ? O1A C1A C2A O2A -2.8(4) . . . . ? C6A C1A C2A O2A 178.3(2) . . . . ? O1A C1A C2A C3A 178.2(3) . . . . ? C6A C1A C2A C3A -0.7(4) . . . . ? O2A C2A C3A C4A -178.2(3) . . . . ? C1A C2A C3A C4A 0.7(5) . . . . ? C2A C3A C4A C5A -0.3(5) . . . . ? C3A C4A C5A C6A -0.1(6) . . . . ? O1A C1A C6A C5A -178.5(3) . . . . ? C2A C1A C6A C5A 0.3(4) . . . . ? O1A C1A C6A C7A 1.4(5) . . . . ? C2A C1A C6A C7A -179.8(3) . . . . ? C4A C5A C6A C1A 0.1(5) . . . . ? C4A C5A C6A C7A -179.8(3) . . . . ? C1A C6A C7A N8A 16.6(5) . . . . ? C5A C6A C7A N8A -163.5(3) . . . . ? C6A C7A N8A N9A -177.9(3) . . . . ? C6A C7A N8A La 19.6(5) . . . . ? O10C La N8A C7A 147.4(3) . . . . ? O1B La N8A C7A -10.5(3) . . . . ? O1C La N8A C7A -75.1(3) . . . . ? O10A La N8A C7A -179.9(3) . . . . ? O10B La N8A C7A 93.5(3) . . . . ? O101 La N8A C7A -40.8(5) . . . . ? N8C La N8A C7A -144.5(3) . . . . ? N8B La N8A C7A 55.8(3) . . . . ? O1A La N8A C7A -42.1(3) . . . . ? Ti La N8A C7A -42.4(3) . . . . ? O10C La N8A N9A -15.9(2) . . . . ? O1B La N8A N9A -173.69(18) . . . . ? O1C La N8A N9A 121.66(19) . . . . ? O10A La N8A N9A 16.86(18) . . . . ? O10B La N8A N9A -69.78(19) . . . . ? O101 La N8A N9A 155.9(3) . . . . ? N8C La N8A N9A 52.2(2) . . . . ? N8B La N8A N9A -107.45(19) . . . . ? O1A La N8A N9A 154.7(2) . . . . ? Ti La N8A N9A 154.33(19) . . . . ? C7A N8A N9A C10A 177.6(3) . . . . ? La N8A N9A C10A -15.7(3) . . . . ? N8A N9A C10A O10A 0.3(5) . . . . ? N8A N9A C10A C11A 179.5(3) . . . . ? N9A C10A O10A La 24.0(4) . . . . ? C11A C10A O10A La -155.2(2) . . . . ? O10C La O10A C10A 128.4(3) . . . . ? O1B La O10A C10A -49.2(4) . . . . ? O1C La O10A C10A -114.6(3) . . . . ? O10B La O10A C10A 46.8(3) . . . . ? O101 La O10A C10A 167.7(2) . . . . ? N8C La O10A C10A -165.0(3) . . . . ? N8B La O10A C10A 65.0(3) . . . . ? O1A La O10A C10A -56.9(3) . . . . ? N8A La O10A C10A -22.5(2) . . . . ? Ti La O10A C10A -80.9(3) . . . . ? O10A C10A C11A C16A 167.1(3) . . . . ? N9A C10A C11A C16A -12.2(5) . . . . ? O10A C10A C11A C12A -12.3(5) . . . . ? N9A C10A C11A C12A 168.4(3) . . . . ? C16A C11A C12A C13A 0.4(5) . . . . ? C10A C11A C12A C13A 179.8(3) . . . . ? C11A C12A C13A C14A 0.1(6) . . . . ? C12A C13A C14A C15A 0.2(6) . . . . ? C13A C14A C15A C16A -1.0(6) . . . . ? C12A C11A C16A C15A -1.2(5) . . . . ? C10A C11A C16A C15A 179.4(3) . . . . ? C14A C15A C16A C11A 1.5(6) . . . . ? O2B Ti O1B C1B 5.02(19) . . . . ? O2C Ti O1B C1B 103.5(3) . . . . ? O2A Ti O1B C1B -86.95(19) . . . . ? O1A Ti O1B C1B -164.8(2) . . . . ? O1C Ti O1B C1B 115.99(19) . . . . ? La Ti O1B C1B 146.9(2) . . . . ? O2B Ti O1B La -141.89(9) . . . . ? O2C Ti O1B La -43.4(3) . . . . ? O2A Ti O1B La 126.13(8) . . . . ? O1A Ti O1B La 48.31(8) . . . . ? O1C Ti O1B La -30.92(8) . . . . ? O10C La O1B C1B -2.1(3) . . . . ? O1C La O1B C1B -110.1(2) . . . . ? O10A La O1B C1B 175.0(2) . . . . ? O10B La O1B C1B 86.6(2) . . . . ? O101 La O1B C1B -33.5(2) . . . . ? N8C La O1B C1B -82.1(2) . . . . ? N8B La O1B C1B 47.7(2) . . . . ? O1A La O1B C1B -176.0(2) . . . . ? N8A La O1B C1B 152.7(2) . . . . ? Ti La O1B C1B -137.5(3) . . . . ? O10C La O1B Ti 135.37(8) . . . . ? O1C La O1B Ti 27.36(7) . . . . ? O10A La O1B Ti -47.58(19) . . . . ? O10B La O1B Ti -135.89(8) . . . . ? O101 La O1B Ti 103.93(9) . . . . ? N8C La O1B Ti 55.39(11) . . . . ? N8B La O1B Ti -174.85(10) . . . . ? O1A La O1B Ti -38.56(7) . . . . ? N8A La O1B Ti -69.88(9) . . . . ? O2C Ti O2B C2B -166.5(2) . . . . ? O2A Ti O2B C2B 90.8(2) . . . . ? O1A Ti O2B C2B 17.6(3) . . . . ? O1B Ti O2B C2B -7.4(2) . . . . ? O1C Ti O2B C2B -83.8(2) . . . . ? La Ti O2B C2B -35.9(2) . . . . ? Ti O1B C1B C6B 178.1(2) . . . . ? La O1B C1B C6B -48.4(4) . . . . ? Ti O1B C1B C2B -1.9(3) . . . . ? La O1B C1B C2B 131.6(2) . . . . ? Ti O2B C2B C3B -173.4(3) . . . . ? Ti O2B C2B C1B 8.6(3) . . . . ? O1B C1B C2B O2B -3.9(4) . . . . ? C6B C1B C2B O2B 176.0(3) . . . . ? O1B C1B C2B C3B 177.9(3) . . . . ? C6B C1B C2B C3B -2.1(5) . . . . ? O2B C2B C3B C4B -178.6(3) . . . . ? C1B C2B C3B C4B -0.7(5) . . . . ? C2B C3B C4B C5B 1.3(5) . . . . ? C3B C4B C5B C6B 1.0(5) . . . . ? O1B C1B C6B C5B -175.7(3) . . . . ? C2B C1B C6B C5B 4.3(4) . . . . ? O1B C1B C6B C7B 1.5(5) . . . . ? C2B C1B C6B C7B -178.5(3) . . . . ? C4B C5B C6B C1B -3.8(5) . . . . ? C4B C5B C6B C7B 178.9(3) . . . . ? C1B C6B C7B N8B 14.6(5) . . . . ? C5B C6B C7B N8B -168.2(3) . . . . ? C6B C7B N8B N9B -176.2(3) . . . . ? C6B C7B N8B La 10.8(4) . . . . ? O10C La N8B C7B 114.1(3) . . . . ? O1B La N8B C7B -30.0(3) . . . . ? O1C La N8B C7B -6.6(3) . . . . ? O10A La N8B C7B 173.8(2) . . . . ? O10B La N8B C7B -165.8(3) . . . . ? O101 La N8B C7B 42.0(3) . . . . ? N8C La N8B C7B 82.2(3) . . . . ? O1A La N8B C7B -67.2(3) . . . . ? N8A La N8B C7B -126.2(3) . . . . ? Ti La N8B C7B -32.9(3) . . . . ? O10C La N8B N9B -59.11(18) . . . . ? O1B La N8B N9B 156.85(19) . . . . ? O1C La N8B N9B -179.82(16) . . . . ? O10A La N8B N9B 0.6(2) . . . . ? O10B La N8B N9B 21.00(16) . . . . ? O101 La N8B N9B -131.19(19) . . . . ? N8C La N8B N9B -90.99(19) . . . . ? O1A La N8B N9B 119.68(17) . . . . ? N8A La N8B N9B 60.59(18) . . . . ? Ti La N8B N9B 153.93(17) . . . . ? C7B N8B N9B C10B 160.8(3) . . . . ? La N8B N9B C10B -24.7(3) . . . . ? N8B N9B C10B O10B 8.9(4) . . . . ? N8B N9B C10B C11B -168.6(2) . . . . ? N9B C10B O10B La 15.3(4) . . . . ? C11B C10B O10B La -167.3(2) . . . . ? O10C La O10B C10B 68.0(2) . . . . ? O1B La O10B C10B -60.8(2) . . . . ? O1C La O10B C10B -118.0(3) . . . . ? O10A La O10B C10B 143.7(2) . . . . ? O101 La O10B C10B 12.8(3) . . . . ? N8C La O10B C10B 107.6(2) . . . . ? N8B La O10B C10B -19.7(2) . . . . ? O1A La O10B C10B -120.3(2) . . . . ? N8A La O10B C10B -157.4(3) . . . . ? Ti La O10B C10B -91.7(2) . . . . ? O10B C10B C11B C16B 12.4(4) . . . . ? N9B C10B C11B C16B -170.1(3) . . . . ? O10B C10B C11B C12B -163.9(3) . . . . ? N9B C10B C11B C12B 13.6(4) . . . . ? C16B C11B C12B C13B -1.4(5) . . . . ? C10B C11B C12B C13B 174.9(3) . . . . ? C11B C12B C13B C14B 0.8(6) . . . . ? C12B C13B C14B C15B 0.6(6) . . . . ? C13B C14B C15B C16B -1.3(6) . . . . ? C12B C11B C16B C15B 0.7(5) . . . . ? C10B C11B C16B C15B -175.7(3) . . . . ? C14B C15B C16B C11B 0.6(6) . . . . ? O2B Ti O1C C1C -111.87(18) . . . . ? O2C Ti O1C C1C -11.92(18) . . . . ? O2A Ti O1C C1C 82.2(3) . . . . ? O1A Ti O1C C1C 92.43(18) . . . . ? O1B Ti O1C C1C 172.53(19) . . . . ? La Ti O1C C1C 141.7(2) . . . . ? O2B Ti O1C La 106.44(9) . . . . ? O2C Ti O1C La -153.61(10) . . . . ? O2A Ti O1C La -59.5(2) . . . . ? O1A Ti O1C La -49.26(8) . . . . ? O1B Ti O1C La 30.85(7) . . . . ? O10C La O1C C1C 77.3(2) . . . . ? O1B La O1C C1C -159.7(2) . . . . ? O10A La O1C C1C -3.5(2) . . . . ? O10B La O1C C1C -95.9(3) . . . . ? O101 La O1C C1C 126.4(2) . . . . ? N8C La O1C C1C 45.4(2) . . . . ? N8B La O1C C1C 176.8(2) . . . . ? O1A La O1C C1C -93.2(2) . . . . ? N8A La O1C C1C -60.4(2) . . . . ? Ti La O1C C1C -132.5(2) . . . . ? O10C La O1C Ti -150.16(8) . . . . ? O1B La O1C Ti -27.20(7) . . . . ? O10A La O1C Ti 128.99(8) . . . . ? O10B La O1C Ti 36.6(3) . . . . ? O101 La O1C Ti -101.04(9) . . . . ? N8C La O1C Ti 177.94(10) . . . . ? N8B La O1C Ti -50.66(11) . . . . ? O1A La O1C Ti 39.32(7) . . . . ? N8A La O1C Ti 72.14(9) . . . . ? O2B Ti O2C C2C 118.0(2) . . . . ? O2A Ti O2C C2C -145.7(2) . . . . ? O1A Ti O2C C2C -63.7(2) . . . . ? O1B Ti O2C C2C 23.7(4) . . . . ? O1C Ti O2C C2C 11.2(2) . . . . ? La Ti O2C C2C -9.8(2) . . . . ? Ti O1C C1C C6C -171.2(2) . . . . ? La O1C C1C C6C -43.3(4) . . . . ? Ti O1C C1C C2C 10.6(3) . . . . ? La O1C C1C C2C 138.6(2) . . . . ? Ti O2C C2C C3C 171.5(3) . . . . ? Ti O2C C2C C1C -8.8(3) . . . . ? O1C C1C C2C O2C -1.8(4) . . . . ? C6C C1C C2C O2C 179.9(3) . . . . ? O1C C1C C2C C3C 177.9(3) . . . . ? C6C C1C C2C C3C -0.4(5) . . . . ? O2C C2C C3C C4C 178.4(3) . . . . ? C1C C2C C3C C4C -1.2(5) . . . . ? C2C C3C C4C C5C 1.3(5) . . . . ? C3C C4C C5C C6C 0.2(5) . . . . ? O1C C1C C6C C5C -176.2(3) . . . . ? C2C C1C C6C C5C 1.9(4) . . . . ? O1C C1C C6C C7C 1.8(5) . . . . ? C2C C1C C6C C7C 179.9(3) . . . . ? C4C C5C C6C C1C -1.8(5) . . . . ? C4C C5C C6C C7C -179.9(3) . . . . ? C1C C6C C7C N8C 9.6(5) . . . . ? C5C C6C C7C N8C -172.4(3) . . . . ? C6C C7C N8C N9C -174.4(3) . . . . ? C6C C7C N8C La 18.4(4) . . . . ? O10C La N8C C7C 177.0(3) . . . . ? O1B La N8C C7C -61.1(3) . . . . ? O1C La N8C C7C -34.1(2) . . . . ? O10A La N8C C7C 93.5(3) . . . . ? O10B La N8C C7C 132.2(2) . . . . ? O101 La N8C C7C -106.8(3) . . . . ? N8B La N8C C7C -146.6(2) . . . . ? O1A La N8C C7C 1.9(3) . . . . ? N8A La N8C C7C 61.8(3) . . . . ? Ti La N8C C7C -32.9(3) . . . . ? O10C La N8C N9C 9.99(17) . . . . ? O1B La N8C N9C 131.82(17) . . . . ? O1C La N8C N9C 158.9(2) . . . . ? O10A La N8C N9C -73.52(18) . . . . ? O10B La N8C N9C -34.8(2) . . . . ? O101 La N8C N9C 86.14(18) . . . . ? N8B La N8C N9C 46.3(2) . . . . ? O1A La N8C N9C -165.10(17) . . . . ? N8A La N8C N9C -105.28(18) . . . . ? Ti La N8C N9C 160.06(17) . . . . ? C7C N8C N9C C10C -179.6(3) . . . . ? La N8C N9C C10C -10.3(3) . . . . ? N8C N9C C10C O10C 2.9(4) . . . . ? N8C N9C C10C C11C -175.6(2) . . . . ? N9C C10C O10C La 7.8(4) . . . . ? C11C C10C O10C La -173.75(18) . . . . ? O1B La O10C C10C -121.0(2) . . . . ? O1C La O10C C10C -42.4(2) . . . . ? O10A La O10C C10C 60.2(2) . . . . ? O10B La O10C C10C 135.5(2) . . . . ? O101 La O10C C10C -90.5(2) . . . . ? N8C La O10C C10C -9.0(2) . . . . ? N8B La O10C C10C -164.6(2) . . . . ? O1A La O10C C10C 23.1(5) . . . . ? N8A La O10C C10C 87.8(2) . . . . ? Ti La O10C C10C -73.8(2) . . . . ? O10C C10C C11C C12C 3.9(4) . . . . ? N9C C10C C11C C12C -177.4(3) . . . . ? O10C C10C C11C C16C -173.8(3) . . . . ? N9C C10C C11C C16C 4.8(4) . . . . ? C16C C11C C12C C13C -0.2(5) . . . . ? C10C C11C C12C C13C -178.0(3) . . . . ? C11C C12C C13C C14C -0.4(5) . . . . ? C12C C13C C14C C15C 0.4(5) . . . . ? C13C C14C C15C C16C 0.2(6) . . . . ? C12C C11C C16C C15C 0.8(5) . . . . ? C10C C11C C16C C15C 178.6(3) . . . . ? C14C C15C C16C C11C -0.8(5) . . . . ? O10C La O101 C102 75.1(3) . . . . ? O1B La O101 C102 -129.8(3) . . . . ? O1C La O101 C102 -61.2(3) . . . . ? O10A La O101 C102 35.2(3) . . . . ? O10B La O101 C102 133.2(3) . . . . ? N8C La O101 C102 9.8(3) . . . . ? N8B La O101 C102 162.2(3) . . . . ? O1A La O101 C102 -96.3(3) . . . . ? N8A La O101 C102 -97.5(5) . . . . ? Ti La O101 C102 -95.8(3) . . . . ? La O101 C102 N103 160.6(2) . . . . ? O101 C102 N103 C105 177.6(3) . . . . ? O101 C102 N103 C104 -1.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.703 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.096 data_fro4653 _database_code_depnum_ccdc_archive 'CCDC 706324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H59 Ga La N9 O14' _chemical_formula_weight 1254.72 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 41.5050(9) _cell_length_b 41.5050(9) _cell_length_c 21.8734(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 32632.3(12) _cell_formula_units_Z 18 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17934 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11520 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8238 _exptl_absorpt_correction_T_max 0.9420 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '\w and \f scans' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62991 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12755 _reflns_number_gt 8727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. Diffracting power of the crystals was poor due to a huge amount of disordered solbents and to the size. The three non-coordinated DMFs were refined with geometrical restraints (SAME from the coordinated one) and one common isotropic thermal parameter. One methanol is refined with split positions using same isotropic thermal parameters (EADP) and geometrical restraints (SADI). Structure still has big voids but no chemically meaningful electron density could be found. ; _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^)+(0.1136P)^2^+401.8556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12755 _refine_ls_number_parameters 660 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2443 _refine_ls_wR_factor_gt 0.2167 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.120 _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 Ga Ga 0.38495(3) -0.03686(3) 0.96118(4) 0.0426(3) Uani 1 1 d . . . La La 0.439159(14) -0.008091(15) 0.833225(19) 0.03935(18) Uani 1 1 d . . . O1A O 0.38695(15) -0.00705(16) 0.8869(2) 0.0401(13) Uani 1 1 d . . . O2A O 0.33299(16) -0.05007(17) 0.9610(2) 0.0446(14) Uani 1 1 d . . . C1A C 0.3529(2) -0.0136(2) 0.8717(4) 0.041(2) Uani 1 1 d . . . C2A C 0.3241(2) -0.0355(2) 0.9136(3) 0.040(2) Uani 1 1 d . . . C3A C 0.2889(3) -0.0410(3) 0.9027(4) 0.053(2) Uani 1 1 d . . . H3A H 0.2696 -0.0552 0.9304 0.064 Uiso 1 1 calc R . . C4A C 0.2816(3) -0.0261(3) 0.8518(4) 0.059(3) Uani 1 1 d . . . H4A H 0.2574 -0.0301 0.8455 0.070 Uiso 1 1 calc R . . C5A C 0.3089(3) -0.0054(3) 0.8104(4) 0.052(2) Uani 1 1 d . . . H5A H 0.3034 0.0045 0.7759 0.062 Uiso 1 1 calc R . . C6A C 0.3456(2) 0.0010(2) 0.8192(4) 0.041(2) Uani 1 1 d . . . C7A C 0.3735(2) 0.0221(2) 0.7731(4) 0.042(2) Uani 1 1 d . . . H7A H 0.3677 0.0346 0.7433 0.050 Uiso 1 1 calc R . . N8A N 0.4056(2) 0.0247(2) 0.7700(3) 0.0404(16) Uani 1 1 d . . . N9A N 0.4281(2) 0.0469(2) 0.7214(3) 0.0458(18) Uani 1 1 d . . . H9A H 0.4192 0.0551 0.6933 0.055 Uiso 1 1 calc R . . C10A C 0.4634(3) 0.0547(3) 0.7201(4) 0.044(2) Uani 1 1 d . . . O11A O 0.47732(16) 0.04347(18) 0.7587(3) 0.0501(15) Uani 1 1 d . . . C12A C 0.4877(3) 0.0807(3) 0.6698(4) 0.047(2) Uani 1 1 d . . . C13A C 0.5219(3) 0.0825(3) 0.6614(4) 0.062(3) Uani 1 1 d . . . H13A H 0.5276 0.0666 0.6838 0.074 Uiso 1 1 calc R . . C14A C 0.5475(3) 0.1075(3) 0.6201(5) 0.072(3) Uani 1 1 d . . . H14A H 0.5706 0.1089 0.6144 0.086 Uiso 1 1 calc R . . C15A C 0.5384(3) 0.1305(3) 0.5871(5) 0.077(3) Uani 1 1 d . . . H15A H 0.5554 0.1476 0.5588 0.093 Uiso 1 1 calc R . . C16A C 0.5047(4) 0.1284(4) 0.5960(5) 0.084(4) Uani 1 1 d . . . H16A H 0.4988 0.1442 0.5738 0.101 Uiso 1 1 calc R . . C17A C 0.4793(3) 0.1033(3) 0.6376(4) 0.068(3) Uani 1 1 d . . . H17A H 0.4562 0.1019 0.6433 0.081 Uiso 1 1 calc R . . O1B O 0.44026(15) -0.01091(16) 0.9460(2) 0.0410(13) Uani 1 1 d . . . O2B O 0.39939(17) -0.00346(17) 1.0295(2) 0.0487(15) Uani 1 1 d . . . C1B C 0.4588(2) 0.0150(2) 0.9885(3) 0.039(2) Uani 1 1 d . . . C2B C 0.4363(3) 0.0183(3) 1.0352(3) 0.043(2) Uani 1 1 d . . . C3B C 0.4541(3) 0.0432(3) 1.0813(4) 0.052(2) Uani 1 1 d . . . H3B H 0.4399 0.0457 1.1124 0.062 Uiso 1 1 calc R . . C4B C 0.4923(3) 0.0648(3) 1.0834(4) 0.054(2) Uani 1 1 d . . . H4B H 0.5036 0.0810 1.1166 0.065 Uiso 1 1 calc R . . C5B C 0.5140(3) 0.0630(3) 1.0375(4) 0.052(2) Uani 1 1 d . . . H5B H 0.5400 0.0782 1.0389 0.062 Uiso 1 1 calc R . . C6B C 0.4969(2) 0.0380(2) 0.9880(3) 0.041(2) Uani 1 1 d . . . C7B C 0.5208(2) 0.0375(2) 0.9388(4) 0.043(2) Uani 1 1 d . . . H7B H 0.5466 0.0495 0.9456 0.052 Uiso 1 1 calc R . . N8B N 0.50797(19) 0.0213(2) 0.8865(3) 0.0403(16) Uani 1 1 d . . . N9B N 0.5349(2) 0.0237(2) 0.8464(3) 0.0468(18) Uani 1 1 d . . . H9B H 0.5585 0.0383 0.8538 0.056 Uiso 1 1 calc R . . C10B C 0.5235(3) 0.0030(3) 0.7962(4) 0.047(2) Uani 1 1 d . . . O11B O 0.48991(18) -0.01752(19) 0.7849(3) 0.0533(16) Uani 1 1 d . . . C12B C 0.5523(2) 0.0052(3) 0.7536(4) 0.048(2) Uani 1 1 d . . . C13B C 0.5447(3) 0.0019(3) 0.6917(4) 0.068(3) Uani 1 1 d . . . H13B H 0.5219 -0.0013 0.6778 0.081 Uiso 1 1 calc R . . C14B C 0.5704(4) 0.0031(4) 0.6498(5) 0.086(4) Uani 1 1 d . . . H14B H 0.5650 0.0013 0.6078 0.103 Uiso 1 1 calc R . . C15B C 0.6031(3) 0.0070(4) 0.6693(5) 0.081(4) Uani 1 1 d . . . H15B H 0.6202 0.0073 0.6408 0.097 Uiso 1 1 calc R . . C16B C 0.6114(3) 0.0104(3) 0.7317(5) 0.071(3) Uani 1 1 d . . . H16B H 0.6342 0.0132 0.7453 0.085 Uiso 1 1 calc R . . C17B C 0.5860(3) 0.0097(3) 0.7731(4) 0.058(3) Uani 1 1 d . . . H17B H 0.5917 0.0122 0.8151 0.070 Uiso 1 1 calc R . . O1C O 0.38828(16) -0.06808(16) 0.8924(2) 0.0441(14) Uani 1 1 d . . . O2C O 0.37699(17) -0.07906(17) 1.0103(2) 0.0498(15) Uani 1 1 d . . . C1C C 0.3906(2) -0.0966(3) 0.9149(4) 0.046(2) Uani 1 1 d . . . C2C C 0.3835(3) -0.1032(3) 0.9789(4) 0.052(2) Uani 1 1 d . . . C3C C 0.3834(3) -0.1341(3) 1.0060(5) 0.068(3) Uani 1 1 d . . . H3C H 0.3777 -0.1391 1.0477 0.082 Uiso 1 1 calc R . . C4C C 0.3915(4) -0.1571(3) 0.9717(5) 0.080(4) Uani 1 1 d . . . H4C H 0.3923 -0.1771 0.9905 0.096 Uiso 1 1 calc R . . C5C C 0.3984(3) -0.1509(3) 0.9098(5) 0.075(3) Uani 1 1 d . . . H5C H 0.4029 -0.1673 0.8865 0.090 Uiso 1 1 calc R . . C6C C 0.3989(3) -0.1197(3) 0.8808(4) 0.053(2) Uani 1 1 d . . . C7C C 0.4080(3) -0.1129(3) 0.8159(4) 0.061(3) Uani 1 1 d . . . H7C H 0.4080 -0.1320 0.7927 0.073 Uiso 1 1 calc R . . N8C N 0.4159(2) -0.0831(2) 0.7890(3) 0.053(2) Uani 1 1 d . . . N9C N 0.4230(2) -0.0822(2) 0.7269(3) 0.056(2) Uani 1 1 d . . . H9C H 0.4257 -0.0996 0.7096 0.067 Uiso 1 1 calc R . . C10C C 0.4256(3) -0.0542(3) 0.6951(4) 0.052(2) Uani 1 1 d . . . O11C O 0.42275(19) -0.0288(2) 0.7188(3) 0.0543(16) Uani 1 1 d . . . C12C C 0.4325(3) -0.0540(3) 0.6271(4) 0.058(3) Uani 1 1 d . . . C13C C 0.4199(4) -0.0867(4) 0.5946(5) 0.098(5) Uani 1 1 d . . . H13C H 0.4075 -0.1097 0.6150 0.117 Uiso 1 1 calc R . . C14C C 0.4257(5) -0.0857(5) 0.5319(6) 0.119(6) Uani 1 1 d . . . H14C H 0.4173 -0.1078 0.5096 0.143 Uiso 1 1 calc R . . C15C C 0.4437(5) -0.0520(5) 0.5033(6) 0.104(5) Uani 1 1 d . . . H15C H 0.4482 -0.0511 0.4610 0.124 Uiso 1 1 calc R . . C16C C 0.4552(4) -0.0196(4) 0.5347(5) 0.081(4) Uani 1 1 d . . . H16C H 0.4671 0.0033 0.5138 0.098 Uiso 1 1 calc R . . C17C C 0.4494(3) -0.0204(3) 0.5973(4) 0.062(3) Uani 1 1 d . . . H17C H 0.4570 0.0018 0.6190 0.075 Uiso 1 1 calc R . . O21 O 0.46309(18) 0.06023(18) 0.8760(3) 0.0525(16) Uani 1 1 d D . . C22 C 0.4497(3) 0.0712(3) 0.9166(4) 0.056(2) Uani 1 1 d D . . H22 H 0.4245 0.0556 0.9270 0.067 Uiso 1 1 calc R . . N23 N 0.4680(3) 0.1024(2) 0.9453(4) 0.068(2) Uani 1 1 d D . . C24 C 0.4502(5) 0.1130(4) 0.9920(5) 0.112(5) Uani 1 1 d D . . H24A H 0.4503 0.1354 0.9793 0.168 Uiso 1 1 calc R . . H24B H 0.4637 0.1175 1.0301 0.168 Uiso 1 1 calc R . . H24C H 0.4248 0.0930 0.9976 0.168 Uiso 1 1 calc R . . C25 C 0.5074(3) 0.1276(4) 0.9343(6) 0.095(4) Uani 1 1 d D . . H25A H 0.5162 0.1174 0.9029 0.143 Uiso 1 1 calc R . . H25B H 0.5212 0.1309 0.9718 0.143 Uiso 1 1 calc R . . H25C H 0.5111 0.1515 0.9210 0.143 Uiso 1 1 calc R . . O31 O 0.6152(6) 0.1926(6) 0.8676(10) 0.255(6) Uiso 1 1 d D . . C32 C 0.5868(8) 0.1892(7) 0.8401(13) 0.255(6) Uiso 1 1 d D . . H32 H 0.5782 0.2058 0.8484 0.306 Uiso 1 1 calc R . . N33 N 0.5696(6) 0.1628(6) 0.8006(11) 0.255(6) Uiso 1 1 d D . . C34 C 0.5725(8) 0.1296(7) 0.8024(13) 0.255(6) Uiso 1 1 d D . . H34A H 0.5979 0.1357 0.7941 0.383 Uiso 1 1 d R . . H34B H 0.5560 0.1115 0.7727 0.383 Uiso 1 1 d R . . H34C H 0.5655 0.1193 0.8432 0.383 Uiso 1 1 d R . . C35 C 0.5371(7) 0.1599(8) 0.7698(13) 0.255(6) Uiso 1 1 d D . . H35A H 0.5153 0.1460 0.7953 0.383 Uiso 1 1 calc R . . H35B H 0.5334 0.1471 0.7311 0.383 Uiso 1 1 calc R . . H35C H 0.5409 0.1846 0.7625 0.383 Uiso 1 1 calc R . . O41 O 0.6381(13) 0.1699(12) 0.5714(18) 0.263(12) Uiso 0.50 1 d PD . . C42 C 0.6591(15) 0.2034(12) 0.5862(19) 0.263(12) Uiso 0.50 1 d PD . . H42 H 0.6777 0.2195 0.5589 0.316 Uiso 0.50 1 calc PR . . N43 N 0.6555(13) 0.2160(10) 0.6379(17) 0.263(12) Uiso 0.50 1 d PD . . C44 C 0.6801(15) 0.2543(11) 0.655(2) 0.263(12) Uiso 0.50 1 d PD . . H44A H 0.6969 0.2554 0.6870 0.395 Uiso 0.50 1 calc PR . . H44B H 0.6655 0.2650 0.6703 0.395 Uiso 0.50 1 calc PR . . H44C H 0.6944 0.2683 0.6199 0.395 Uiso 0.50 1 calc PR . . C45 C 0.6315(15) 0.1914(13) 0.6861(19) 0.263(12) Uiso 0.50 1 d PD . . H45A H 0.6316 0.1681 0.6847 0.395 Uiso 0.50 1 calc PR . . H45B H 0.6064 0.1867 0.6800 0.395 Uiso 0.50 1 calc PR . . H45C H 0.6406 0.2032 0.7255 0.395 Uiso 0.50 1 calc PR . . O51 O 0.4204(7) 0.0854(9) 0.4037(14) 0.180(7) Uiso 0.50 1 d PD . . C52 C 0.4393(8) 0.0816(10) 0.4460(15) 0.180(7) Uiso 0.50 1 d PD . . H52 H 0.4286 0.0649 0.4787 0.216 Uiso 0.50 1 calc PR . . N53 N 0.4746(7) 0.1033(8) 0.4393(14) 0.180(7) Uiso 0.50 1 d PD . . C54 C 0.4992(10) 0.0881(11) 0.436(2) 0.180(7) Uiso 0.50 1 d PD . . H54A H 0.5147 0.0952 0.4722 0.270 Uiso 0.50 1 calc PR . . H54B H 0.5148 0.0978 0.3999 0.270 Uiso 0.50 1 calc PR . . H54C H 0.4845 0.0612 0.4333 0.270 Uiso 0.50 1 calc PR . . C55 C 0.4872(10) 0.1387(9) 0.408(2) 0.180(7) Uiso 0.50 1 d PD . . H55A H 0.5116 0.1569 0.4226 0.270 Uiso 0.50 1 calc PR . . H55B H 0.4698 0.1474 0.4155 0.270 Uiso 0.50 1 calc PR . . H55C H 0.4884 0.1352 0.3641 0.270 Uiso 0.50 1 calc PR . . O101 O 0.39178(18) -0.0758(2) 1.1271(3) 0.070(2) Uani 1 1 d D . . H101 H 0.3866 -0.0770 1.0902 0.105 Uiso 1 1 calc R . . C102 C 0.3596(3) -0.0970(4) 1.1604(5) 0.092(4) Uani 1 1 d D . . H10A H 0.3642 -0.0899 1.2031 0.139 Uiso 1 1 calc R . . H10B H 0.3521 -0.1231 1.1564 0.139 Uiso 1 1 calc R . . H10C H 0.3400 -0.0930 1.1450 0.139 Uiso 1 1 calc R . . O111 O 0.4522(6) -0.1308(6) 0.7082(10) 0.130(5) Uiso 0.541(10) 1 d PD A 1 H111 H 0.4540 -0.1448 0.7334 0.195 Uiso 0.541(10) 1 calc PR A 1 C112 C 0.4188(8) -0.1496(10) 0.6791(16) 0.155(10) Uiso 0.541(10) 1 d PD A 1 H11A H 0.4004 -0.1463 0.7013 0.233 Uiso 0.541(10) 1 calc PR A 1 H11B H 0.4109 -0.1759 0.6775 0.233 Uiso 0.541(10) 1 calc PR A 1 H11C H 0.4211 -0.1401 0.6379 0.233 Uiso 0.541(10) 1 calc PR A 1 O121 O 0.5033(7) -0.1196(7) 0.7534(11) 0.130(5) Uiso 0.459(10) 1 d PD A 2 H121 H 0.5200 -0.0988 0.7420 0.195 Uiso 0.459(10) 1 calc PR A 2 C122 C 0.5177(12) -0.1342(12) 0.7940(18) 0.155(10) Uiso 0.459(10) 1 d PD A 2 H12A H 0.5382 -0.1142 0.8161 0.233 Uiso 0.459(10) 1 calc PR A 2 H12B H 0.5266 -0.1484 0.7719 0.233 Uiso 0.459(10) 1 calc PR A 2 H12C H 0.4985 -0.1503 0.8226 0.233 Uiso 0.459(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga 0.0425(6) 0.0563(6) 0.0285(5) 0.0046(4) 0.0036(4) 0.0244(5) La 0.0418(3) 0.0557(4) 0.0260(3) 0.0026(2) 0.00095(19) 0.0284(3) O1A 0.038(3) 0.052(4) 0.033(3) 0.008(2) 0.004(2) 0.025(3) O2A 0.043(3) 0.056(4) 0.032(3) 0.007(3) 0.006(2) 0.023(3) C1A 0.045(5) 0.047(5) 0.040(5) -0.004(4) -0.002(4) 0.029(4) C2A 0.036(5) 0.048(5) 0.032(4) -0.001(4) 0.002(3) 0.017(4) C3A 0.041(5) 0.062(6) 0.047(5) 0.008(4) 0.012(4) 0.018(5) C4A 0.033(5) 0.077(7) 0.059(6) 0.011(5) -0.004(4) 0.022(5) C5A 0.046(6) 0.063(6) 0.053(5) 0.000(5) -0.007(4) 0.032(5) C6A 0.042(5) 0.050(5) 0.035(4) -0.003(4) -0.006(4) 0.026(4) C7A 0.046(5) 0.049(5) 0.032(4) -0.003(4) -0.005(4) 0.026(4) N8A 0.047(4) 0.050(4) 0.028(3) 0.005(3) 0.004(3) 0.027(4) N9A 0.047(5) 0.061(5) 0.031(4) 0.012(3) 0.007(3) 0.029(4) C10A 0.051(6) 0.059(6) 0.029(4) -0.007(4) -0.002(4) 0.033(5) O11A 0.045(4) 0.066(4) 0.043(3) 0.012(3) 0.001(3) 0.030(3) C12A 0.050(6) 0.054(6) 0.037(5) 0.005(4) 0.010(4) 0.026(5) C13A 0.067(7) 0.072(7) 0.051(6) 0.012(5) 0.016(5) 0.039(6) C14A 0.071(7) 0.094(9) 0.059(6) 0.012(6) 0.028(6) 0.048(7) C15A 0.084(9) 0.090(9) 0.064(7) 0.029(6) 0.034(6) 0.047(7) C16A 0.092(9) 0.102(10) 0.068(7) 0.040(7) 0.029(7) 0.056(8) C17A 0.074(7) 0.089(8) 0.055(6) 0.034(6) 0.026(5) 0.051(7) O1B 0.041(3) 0.056(4) 0.027(3) 0.004(3) 0.003(2) 0.025(3) O2B 0.046(4) 0.065(4) 0.032(3) -0.002(3) 0.003(3) 0.025(3) C1B 0.044(5) 0.055(5) 0.022(4) 0.000(4) -0.003(3) 0.027(4) C2B 0.056(6) 0.056(6) 0.024(4) 0.009(4) 0.003(4) 0.034(5) C3B 0.062(6) 0.073(7) 0.027(4) 0.001(4) 0.003(4) 0.040(6) C4B 0.057(6) 0.066(6) 0.037(5) -0.007(4) -0.003(4) 0.029(5) C5B 0.048(6) 0.068(7) 0.036(5) -0.004(4) -0.009(4) 0.027(5) C6B 0.042(5) 0.052(5) 0.034(4) 0.006(4) -0.002(4) 0.026(4) C7B 0.041(5) 0.053(5) 0.035(5) 0.008(4) 0.002(4) 0.022(4) N8B 0.041(4) 0.060(5) 0.029(3) 0.008(3) 0.005(3) 0.032(4) N9B 0.039(4) 0.066(5) 0.036(4) 0.006(3) 0.005(3) 0.027(4) C10B 0.054(6) 0.068(6) 0.032(5) 0.003(4) -0.002(4) 0.040(5) O11B 0.046(4) 0.076(5) 0.044(3) -0.005(3) -0.003(3) 0.035(4) C12B 0.046(5) 0.067(6) 0.038(5) 0.003(4) 0.003(4) 0.034(5) C13B 0.076(7) 0.111(9) 0.036(5) -0.002(5) -0.003(5) 0.062(7) C14B 0.105(10) 0.143(12) 0.040(6) -0.001(6) 0.005(6) 0.085(10) C15B 0.076(8) 0.123(11) 0.060(7) 0.008(7) 0.028(6) 0.063(8) C16B 0.061(7) 0.103(9) 0.066(7) -0.001(6) 0.005(5) 0.055(7) C17B 0.054(6) 0.088(8) 0.041(5) 0.008(5) 0.011(4) 0.042(6) O1C 0.051(4) 0.046(3) 0.037(3) 0.001(3) 0.001(3) 0.025(3) O2C 0.058(4) 0.056(4) 0.035(3) 0.010(3) 0.003(3) 0.028(3) C1C 0.045(5) 0.048(5) 0.046(5) 0.004(4) -0.002(4) 0.023(5) C2C 0.052(6) 0.060(6) 0.042(5) 0.007(4) -0.008(4) 0.025(5) C3C 0.076(8) 0.076(8) 0.049(6) 0.016(5) 0.001(5) 0.036(6) C4C 0.125(11) 0.067(8) 0.066(7) 0.011(6) 0.002(7) 0.061(8) C5C 0.095(9) 0.068(7) 0.077(8) 0.002(6) 0.007(6) 0.052(7) C6C 0.056(6) 0.054(6) 0.049(5) 0.003(4) 0.001(4) 0.026(5) C7C 0.078(7) 0.070(7) 0.048(6) -0.013(5) 0.002(5) 0.048(6) N8C 0.069(5) 0.058(5) 0.036(4) 0.001(4) 0.004(4) 0.034(4) N9C 0.072(6) 0.066(5) 0.044(4) -0.007(4) 0.003(4) 0.045(5) C10C 0.049(6) 0.065(7) 0.043(5) -0.007(5) 0.001(4) 0.029(5) O11C 0.068(4) 0.074(5) 0.034(3) -0.007(3) -0.006(3) 0.046(4) C12C 0.050(6) 0.082(8) 0.047(5) -0.007(5) 0.006(4) 0.036(6) C13C 0.148(13) 0.089(9) 0.041(6) -0.015(6) 0.012(7) 0.048(9) C14C 0.183(17) 0.102(12) 0.054(8) -0.010(8) 0.025(9) 0.058(12) C15C 0.144(14) 0.131(13) 0.049(7) -0.013(8) 0.023(8) 0.078(11) C16C 0.092(9) 0.111(10) 0.055(7) 0.015(7) 0.017(6) 0.061(8) C17C 0.067(7) 0.084(8) 0.042(5) 0.006(5) 0.002(5) 0.044(6) O21 0.064(4) 0.060(4) 0.039(3) 0.003(3) -0.002(3) 0.035(4) C22 0.065(7) 0.055(6) 0.046(5) -0.001(5) -0.011(5) 0.028(5) N23 0.088(7) 0.066(6) 0.056(5) -0.005(4) -0.008(5) 0.043(6) C24 0.189(17) 0.127(13) 0.069(8) -0.030(8) -0.029(9) 0.115(13) C25 0.089(10) 0.081(9) 0.096(10) -0.003(7) -0.016(8) 0.027(8) O101 0.047(4) 0.102(6) 0.039(3) 0.010(3) 0.006(3) 0.020(4) C102 0.074(8) 0.122(11) 0.059(7) 0.014(7) 0.015(6) 0.032(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga O2B 1.919(6) . ? Ga O2C 1.937(6) . ? Ga O2A 1.941(6) . ? Ga O1B 2.017(5) . ? Ga O1A 2.018(5) . ? Ga O1C 2.035(5) . ? Ga La 3.4110(10) . ? La O1B 2.472(5) . ? La O1A 2.484(5) . ? La O11A 2.521(6) . ? La O11B 2.555(6) . ? La O11C 2.622(6) . ? La O1C 2.660(6) . ? La O21 2.662(6) . ? La N8B 2.743(7) . ? La N8A 2.756(7) . ? La N8C 2.924(8) . ? O1A C1A 1.342(10) . ? O2A C2A 1.343(10) . ? C1A C6A 1.399(11) . ? C1A C2A 1.415(11) . ? C2A C3A 1.383(12) . ? C3A C4A 1.381(13) . ? C4A C5A 1.367(13) . ? C5A C6A 1.422(12) . ? C6A C7A 1.454(12) . ? C7A N8A 1.282(10) . ? N8A N9A 1.411(9) . ? N9A C10A 1.331(11) . ? C10A O11A 1.241(10) . ? C10A C12A 1.518(12) . ? C12A C17A 1.351(13) . ? C12A C13A 1.396(13) . ? C13A C14A 1.385(14) . ? C14A C15A 1.392(16) . ? C15A C16A 1.372(16) . ? C16A C17A 1.389(14) . ? O1B C1B 1.335(10) . ? O2B C2B 1.338(10) . ? C1B C6B 1.380(12) . ? C1B C2B 1.436(11) . ? C2B C3B 1.368(12) . ? C3B C4B 1.376(13) . ? C4B C5B 1.377(13) . ? C5B C6B 1.420(12) . ? C6B C7B 1.469(11) . ? C7B N8B 1.299(10) . ? N8B N9B 1.385(9) . ? N9B C10B 1.327(11) . ? C10B O11B 1.244(11) . ? C10B C12B 1.480(12) . ? C12B C13B 1.381(12) . ? C12B C17B 1.386(13) . ? C13B C14B 1.385(15) . ? C14B C15B 1.355(16) . ? C15B C16B 1.398(15) . ? C16B C17B 1.378(13) . ? O1C C1C 1.330(10) . ? O2C C2C 1.351(11) . ? C1C C6C 1.386(13) . ? C1C C2C 1.427(12) . ? C2C C3C 1.410(14) . ? C3C C4C 1.379(15) . ? C4C C5C 1.381(15) . ? C5C C6C 1.433(14) . ? C6C C7C 1.462(13) . ? C7C N8C 1.256(12) . ? N8C N9C 1.387(10) . ? N9C C10C 1.310(12) . ? C10C O11C 1.235(11) . ? C10C C12C 1.513(13) . ? C12C C17C 1.372(14) . ? C12C C13C 1.383(15) . ? C13C C14C 1.389(16) . ? C14C C15C 1.36(2) . ? C15C C16C 1.367(18) . ? C16C C17C 1.388(14) . ? O21 C22 1.249(10) . ? C22 N23 1.290(12) . ? N23 C24 1.451(13) . ? N23 C25 1.453(13) . ? O31 C32 1.266(13) . ? C32 N33 1.294(14) . ? N33 C34 1.441(15) . ? N33 C35 1.460(15) . ? O41 C42 1.258(14) . ? C42 N43 1.285(14) . ? N43 C44 1.446(16) . ? N43 C45 1.459(16) . ? O51 C52 1.271(13) . ? C52 N53 1.289(14) . ? N53 C54 1.443(15) . ? N53 C55 1.463(15) . ? O101 C102 1.382(11) . ? O111 C112 1.362(14) . ? O121 C122 1.368(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Ga O2C 94.1(3) . . ? O2B Ga O2A 96.1(2) . . ? O2C Ga O2A 94.7(3) . . ? O2B Ga O1B 83.2(2) . . ? O2C Ga O1B 102.0(2) . . ? O2A Ga O1B 163.3(2) . . ? O2B Ga O1A 106.3(2) . . ? O2C Ga O1A 159.5(2) . . ? O2A Ga O1A 82.6(2) . . ? O1B Ga O1A 81.6(2) . . ? O2B Ga O1C 160.0(2) . . ? O2C Ga O1C 82.5(2) . . ? O2A Ga O1C 103.8(2) . . ? O1B Ga O1C 78.3(2) . . ? O1A Ga O1C 78.5(2) . . ? O2B Ga La 118.22(18) . . ? O2C Ga La 123.77(19) . . ? O2A Ga La 122.87(15) . . ? O1B Ga La 45.80(14) . . ? O1A Ga La 46.15(15) . . ? O1C Ga La 51.20(16) . . ? O1B La O1A 64.26(17) . . ? O1B La O11A 131.8(2) . . ? O1A La O11A 118.32(19) . . ? O1B La O11B 111.67(18) . . ? O1A La O11B 172.36(19) . . ? O11A La O11B 69.3(2) . . ? O1B La O11C 160.9(2) . . ? O1A La O11C 111.78(19) . . ? O11A La O11C 67.1(2) . . ? O11B La O11C 69.77(19) . . ? O1B La O1C 59.64(17) . . ? O1A La O1C 59.67(18) . . ? O11A La O1C 167.67(18) . . ? O11B La O1C 112.78(19) . . ? O11C La O1C 101.72(19) . . ? O1B La O21 72.18(18) . . ? O1A La O21 71.31(19) . . ? O11A La O21 65.26(19) . . ? O11B La O21 114.3(2) . . ? O11C La O21 125.56(19) . . ? O1C La O21 121.66(18) . . ? O1B La N8B 63.69(18) . . ? O1A La N8B 120.97(18) . . ? O11A La N8B 79.91(19) . . ? O11B La N8B 59.3(2) . . ? O11C La N8B 126.41(19) . . ? O1C La N8B 111.85(18) . . ? O21 La N8B 68.0(2) . . ? O1B La N8A 123.37(18) . . ? O1A La N8A 64.43(18) . . ? O11A La N8A 60.96(19) . . ? O11B La N8A 121.79(19) . . ? O11C La N8A 64.57(19) . . ? O1C La N8A 110.23(19) . . ? O21 La N8A 70.23(19) . . ? N8B La N8A 131.6(2) . . ? O1B La N8C 106.48(19) . . ? O1A La N8C 110.4(2) . . ? O11A La N8C 115.0(2) . . ? O11B La N8C 63.8(2) . . ? O11C La N8C 56.1(2) . . ? O1C La N8C 58.66(19) . . ? O21 La N8C 177.3(2) . . ? N8B La N8C 109.3(2) . . ? N8A La N8C 112.4(2) . . ? O1B La Ga 35.80(13) . . ? O1A La Ga 35.86(12) . . ? O11A La Ga 148.45(15) . . ? O11B La Ga 137.35(14) . . ? O11C La Ga 130.57(15) . . ? O1C La Ga 36.59(12) . . ? O21 La Ga 85.08(13) . . ? N8B La Ga 99.49(13) . . ? N8A La Ga 100.18(14) . . ? N8C La Ga 95.17(15) . . ? C1A O1A Ga 111.1(5) . . ? C1A O1A La 135.9(5) . . ? Ga O1A La 98.0(2) . . ? C2A O2A Ga 112.9(5) . . ? O1A C1A C6A 123.4(8) . . ? O1A C1A C2A 115.7(7) . . ? C6A C1A C2A 120.9(8) . . ? O2A C2A C3A 124.2(7) . . ? O2A C2A C1A 117.2(7) . . ? C3A C2A C1A 118.6(8) . . ? C4A C3A C2A 121.0(8) . . ? C5A C4A C3A 121.1(9) . . ? C4A C5A C6A 120.2(9) . . ? C1A C6A C5A 118.2(8) . . ? C1A C6A C7A 123.4(8) . . ? C5A C6A C7A 118.4(8) . . ? N8A C7A C6A 124.7(8) . . ? C7A N8A N9A 114.5(7) . . ? C7A N8A La 133.7(5) . . ? N9A N8A La 111.6(5) . . ? C10A N9A N8A 117.6(7) . . ? O11A C10A N9A 123.8(8) . . ? O11A C10A C12A 119.3(8) . . ? N9A C10A C12A 116.8(8) . . ? C10A O11A La 123.1(6) . . ? C17A C12A C13A 120.3(9) . . ? C17A C12A C10A 123.9(8) . . ? C13A C12A C10A 115.6(8) . . ? C14A C13A C12A 120.2(10) . . ? C13A C14A C15A 119.0(10) . . ? C16A C15A C14A 120.1(10) . . ? C15A C16A C17A 120.5(11) . . ? C12A C17A C16A 120.0(10) . . ? C1B O1B Ga 111.1(5) . . ? C1B O1B La 132.3(5) . . ? Ga O1B La 98.4(2) . . ? C2B O2B Ga 113.5(5) . . ? O1B C1B C6B 123.5(7) . . ? O1B C1B C2B 115.5(7) . . ? C6B C1B C2B 121.0(8) . . ? O2B C2B C3B 125.7(8) . . ? O2B C2B C1B 116.7(7) . . ? C3B C2B C1B 117.6(8) . . ? C2B C3B C4B 122.0(8) . . ? C3B C4B C5B 120.7(8) . . ? C4B C5B C6B 119.7(9) . . ? C1B C6B C5B 118.7(8) . . ? C1B C6B C7B 122.9(8) . . ? C5B C6B C7B 118.3(8) . . ? N8B C7B C6B 123.2(8) . . ? C7B N8B N9B 114.5(7) . . ? C7B N8B La 132.1(5) . . ? N9B N8B La 112.7(5) . . ? C10B N9B N8B 117.7(7) . . ? O11B C10B N9B 121.4(8) . . ? O11B C10B C12B 120.8(8) . . ? N9B C10B C12B 117.8(8) . . ? C10B O11B La 122.8(6) . . ? C13B C12B C17B 118.6(8) . . ? C13B C12B C10B 118.3(8) . . ? C17B C12B C10B 123.0(8) . . ? C12B C13B C14B 120.9(10) . . ? C15B C14B C13B 120.2(10) . . ? C14B C15B C16B 120.0(10) . . ? C17B C16B C15B 119.6(10) . . ? C16B C17B C12B 120.7(9) . . ? C1C O1C Ga 110.6(5) . . ? C1C O1C La 129.6(5) . . ? Ga O1C La 92.2(2) . . ? C2C O2C Ga 112.5(5) . . ? O1C C1C C6C 124.7(8) . . ? O1C C1C C2C 115.8(8) . . ? C6C C1C C2C 119.5(8) . . ? O2C C2C C3C 123.4(8) . . ? O2C C2C C1C 116.9(8) . . ? C3C C2C C1C 119.6(9) . . ? C4C C3C C2C 120.5(10) . . ? C3C C4C C5C 120.2(10) . . ? C4C C5C C6C 120.7(10) . . ? C1C C6C C5C 119.3(9) . . ? C1C C6C C7C 121.3(9) . . ? C5C C6C C7C 119.3(9) . . ? N8C C7C C6C 124.0(9) . . ? C7C N8C N9C 115.5(8) . . ? C7C N8C La 132.7(6) . . ? N9C N8C La 110.1(5) . . ? C10C N9C N8C 117.7(8) . . ? O11C C10C N9C 122.3(8) . . ? O11C C10C C12C 120.4(9) . . ? N9C C10C C12C 117.3(9) . . ? C10C O11C La 124.1(6) . . ? C17C C12C C13C 120.1(10) . . ? C17C C12C C10C 118.3(9) . . ? C13C C12C C10C 121.5(10) . . ? C12C C13C C14C 120.3(13) . . ? C15C C14C C13C 118.8(13) . . ? C14C C15C C16C 121.4(12) . . ? C15C C16C C17C 120.0(13) . . ? C12C C17C C16C 119.4(11) . . ? C22 O21 La 129.9(6) . . ? O21 C22 N23 124.4(9) . . ? C22 N23 C24 120.8(10) . . ? C22 N23 C25 122.0(9) . . ? C24 N23 C25 117.1(10) . . ? O31 C32 N33 120.2(16) . . ? C32 N33 C34 121.1(15) . . ? C32 N33 C35 118.3(15) . . ? C34 N33 C35 116.8(15) . . ? O41 C42 N43 121(2) . . ? C42 N43 C44 121.2(17) . . ? C42 N43 C45 121.9(17) . . ? C44 N43 C45 116.0(16) . . ? O51 C52 N53 112.8(16) . . ? C52 N53 C54 120.5(18) . . ? C52 N53 C55 117.6(15) . . ? C54 N53 C55 116.0(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2B Ga La O1B 44.8(3) . . . . ? O2C Ga La O1B -72.5(3) . . . . ? O2A Ga La O1B 164.2(3) . . . . ? O1A Ga La O1B 130.6(3) . . . . ? O1C Ga La O1B -114.7(3) . . . . ? O2B Ga La O1A -85.8(3) . . . . ? O2C Ga La O1A 157.0(3) . . . . ? O2A Ga La O1A 33.6(3) . . . . ? O1B Ga La O1A -130.6(3) . . . . ? O1C Ga La O1A 114.7(3) . . . . ? O2B Ga La O11A -40.7(3) . . . . ? O2C Ga La O11A -157.9(3) . . . . ? O2A Ga La O11A 78.7(3) . . . . ? O1B Ga La O11A -85.5(3) . . . . ? O1A Ga La O11A 45.1(3) . . . . ? O1C Ga La O11A 159.8(3) . . . . ? O2B Ga La O11B 99.8(3) . . . . ? O2C Ga La O11B -17.5(3) . . . . ? O2A Ga La O11B -140.8(3) . . . . ? O1B Ga La O11B 55.0(3) . . . . ? O1A Ga La O11B -174.4(3) . . . . ? O1C Ga La O11B -59.7(3) . . . . ? O2B Ga La O11C -155.3(3) . . . . ? O2C Ga La O11C 87.5(3) . . . . ? O2A Ga La O11C -35.9(3) . . . . ? O1B Ga La O11C 159.9(3) . . . . ? O1A Ga La O11C -69.5(3) . . . . ? O1C Ga La O11C 45.2(3) . . . . ? O2B Ga La O1C 159.5(3) . . . . ? O2C Ga La O1C 42.3(3) . . . . ? O2A Ga La O1C -81.1(3) . . . . ? O1B Ga La O1C 114.7(3) . . . . ? O1A Ga La O1C -114.7(3) . . . . ? O2B Ga La O21 -21.3(3) . . . . ? O2C Ga La O21 -138.5(3) . . . . ? O2A Ga La O21 98.1(3) . . . . ? O1B Ga La O21 -66.1(3) . . . . ? O1A Ga La O21 64.5(3) . . . . ? O1C Ga La O21 179.2(2) . . . . ? O2B Ga La N8B 45.4(3) . . . . ? O2C Ga La N8B -71.8(3) . . . . ? O2A Ga La N8B 164.8(3) . . . . ? O1B Ga La N8B 0.7(3) . . . . ? O1A Ga La N8B 131.3(3) . . . . ? O1C Ga La N8B -114.1(3) . . . . ? O2B Ga La N8A -90.2(3) . . . . ? O2C Ga La N8A 152.6(3) . . . . ? O2A Ga La N8A 29.2(3) . . . . ? O1B Ga La N8A -134.9(3) . . . . ? O1A Ga La N8A -4.3(3) . . . . ? O1C Ga La N8A 110.3(3) . . . . ? O2B Ga La N8C 156.0(3) . . . . ? O2C Ga La N8C 38.8(3) . . . . ? O2A Ga La N8C -84.6(3) . . . . ? O1B Ga La N8C 111.2(3) . . . . ? O1A Ga La N8C -118.2(3) . . . . ? O1C Ga La N8C -3.5(3) . . . . ? O2B Ga O1A C1A -100.1(5) . . . . ? O2C Ga O1A C1A 77.9(9) . . . . ? O2A Ga O1A C1A -5.8(5) . . . . ? O1B Ga O1A C1A 179.7(5) . . . . ? O1C Ga O1A C1A 100.0(5) . . . . ? La Ga O1A C1A 146.3(6) . . . . ? O2B Ga O1A La 113.7(2) . . . . ? O2C Ga O1A La -68.4(7) . . . . ? O2A Ga O1A La -152.1(2) . . . . ? O1B Ga O1A La 33.4(2) . . . . ? O1C Ga O1A La -46.3(2) . . . . ? O1B La O1A C1A -161.4(8) . . . . ? O11A La O1A C1A 73.1(7) . . . . ? O11B La O1A C1A -102.1(15) . . . . ? O11C La O1A C1A -1.8(8) . . . . ? O1C La O1A C1A -93.0(7) . . . . ? O21 La O1A C1A 119.9(7) . . . . ? N8B La O1A C1A 168.3(7) . . . . ? N8A La O1A C1A 43.4(7) . . . . ? N8C La O1A C1A -62.4(7) . . . . ? Ga La O1A C1A -131.8(8) . . . . ? O1B La O1A Ga -29.5(2) . . . . ? O11A La O1A Ga -155.1(2) . . . . ? O11B La O1A Ga 29.7(15) . . . . ? O11C La O1A Ga 130.0(2) . . . . ? O1C La O1A Ga 38.87(19) . . . . ? O21 La O1A Ga -108.3(2) . . . . ? N8B La O1A Ga -59.9(3) . . . . ? N8A La O1A Ga 175.3(3) . . . . ? N8C La O1A Ga 69.5(3) . . . . ? O2B Ga O2A C2A 108.5(5) . . . . ? O2C Ga O2A C2A -156.8(5) . . . . ? O1B Ga O2A C2A 21.9(11) . . . . ? O1A Ga O2A C2A 2.8(5) . . . . ? O1C Ga O2A C2A -73.4(6) . . . . ? La Ga O2A C2A -20.9(6) . . . . ? Ga O1A C1A C6A -174.8(7) . . . . ? La O1A C1A C6A -47.0(12) . . . . ? Ga O1A C1A C2A 7.7(9) . . . . ? La O1A C1A C2A 135.4(6) . . . . ? Ga O2A C2A C3A 179.3(7) . . . . ? Ga O2A C2A C1A 0.6(9) . . . . ? O1A C1A C2A O2A -5.8(11) . . . . ? C6A C1A C2A O2A 176.6(7) . . . . ? O1A C1A C2A C3A 175.5(8) . . . . ? C6A C1A C2A C3A -2.1(13) . . . . ? O2A C2A C3A C4A -177.9(9) . . . . ? C1A C2A C3A C4A 0.7(14) . . . . ? C2A C3A C4A C5A 0.4(16) . . . . ? C3A C4A C5A C6A -0.2(16) . . . . ? O1A C1A C6A C5A -175.1(8) . . . . ? C2A C1A C6A C5A 2.3(13) . . . . ? O1A C1A C6A C7A 5.7(13) . . . . ? C2A C1A C6A C7A -176.9(8) . . . . ? C4A C5A C6A C1A -1.2(14) . . . . ? C4A C5A C6A C7A 178.1(9) . . . . ? C1A C6A C7A N8A 11.2(14) . . . . ? C5A C6A C7A N8A -168.0(8) . . . . ? C6A C7A N8A N9A -179.6(7) . . . . ? C6A C7A N8A La 5.9(13) . . . . ? O1B La N8A C7A -49.4(8) . . . . ? O1A La N8A C7A -22.5(7) . . . . ? O11A La N8A C7A -172.6(8) . . . . ? O11B La N8A C7A 152.5(7) . . . . ? O11C La N8A C7A 110.6(8) . . . . ? O1C La N8A C7A 16.9(8) . . . . ? O21 La N8A C7A -100.6(8) . . . . ? N8B La N8A C7A -132.2(7) . . . . ? N8C La N8A C7A 80.3(8) . . . . ? Ga La N8A C7A -19.6(8) . . . . ? O1B La N8A N9A 136.1(5) . . . . ? O1A La N8A N9A 163.0(6) . . . . ? O11A La N8A N9A 12.8(5) . . . . ? O11B La N8A N9A -22.1(6) . . . . ? O11C La N8A N9A -63.9(5) . . . . ? O1C La N8A N9A -157.7(5) . . . . ? O21 La N8A N9A 84.8(5) . . . . ? N8B La N8A N9A 53.2(6) . . . . ? N8C La N8A N9A -94.3(5) . . . . ? Ga La N8A N9A 165.8(5) . . . . ? C7A N8A N9A C10A 171.5(8) . . . . ? La N8A N9A C10A -12.8(9) . . . . ? N8A N9A C10A O11A 0.6(13) . . . . ? N8A N9A C10A C12A -176.1(7) . . . . ? N9A C10A O11A La 14.5(12) . . . . ? C12A C10A O11A La -168.8(6) . . . . ? O1B La O11A C10A -124.8(6) . . . . ? O1A La O11A C10A -45.1(7) . . . . ? O11B La O11A C10A 134.2(7) . . . . ? O11C La O11A C10A 58.2(6) . . . . ? O1C La O11A C10A 32.1(13) . . . . ? O21 La O11A C10A -94.7(7) . . . . ? N8B La O11A C10A -165.0(7) . . . . ? N8A La O11A C10A -14.5(6) . . . . ? N8C La O11A C10A 88.3(7) . . . . ? Ga La O11A C10A -73.3(7) . . . . ? O11A C10A C12A C17A -159.0(10) . . . . ? N9A C10A C12A C17A 17.9(14) . . . . ? O11A C10A C12A C13A 15.9(12) . . . . ? N9A C10A C12A C13A -167.2(8) . . . . ? C17A C12A C13A C14A 0.3(16) . . . . ? C10A C12A C13A C14A -174.8(9) . . . . ? C12A C13A C14A C15A -0.4(17) . . . . ? C13A C14A C15A C16A 0.4(19) . . . . ? C14A C15A C16A C17A 0(2) . . . . ? C13A C12A C17A C16A -0.2(17) . . . . ? C10A C12A C17A C16A 174.5(10) . . . . ? C15A C16A C17A C12A 0(2) . . . . ? O2B Ga O1B C1B 0.4(5) . . . . ? O2C Ga O1B C1B -92.4(5) . . . . ? O2A Ga O1B C1B 89.0(9) . . . . ? O1A Ga O1B C1B 108.1(5) . . . . ? O1C Ga O1B C1B -172.0(5) . . . . ? La Ga O1B C1B 141.8(6) . . . . ? O2B Ga O1B La -141.3(3) . . . . ? O2C Ga O1B La 125.9(2) . . . . ? O2A Ga O1B La -52.7(9) . . . . ? O1A Ga O1B La -33.6(2) . . . . ? O1C Ga O1B La 46.3(2) . . . . ? O1A La O1B C1B -99.1(7) . . . . ? O11A La O1B C1B 6.9(7) . . . . ? O11B La O1B C1B 88.0(7) . . . . ? O11C La O1B C1B 178.6(6) . . . . ? O1C La O1B C1B -167.5(7) . . . . ? O21 La O1B C1B -21.7(6) . . . . ? N8B La O1B C1B 52.0(6) . . . . ? N8A La O1B C1B -72.1(7) . . . . ? N8C La O1B C1B 155.8(6) . . . . ? Ga La O1B C1B -128.7(7) . . . . ? O1A La O1B Ga 29.6(2) . . . . ? O11A La O1B Ga 135.6(2) . . . . ? O11B La O1B Ga -143.3(2) . . . . ? O11C La O1B Ga -52.7(7) . . . . ? O1C La O1B Ga -38.9(2) . . . . ? O21 La O1B Ga 107.0(2) . . . . ? N8B La O1B Ga -179.3(3) . . . . ? N8A La O1B Ga 56.5(3) . . . . ? N8C La O1B Ga -75.5(3) . . . . ? O2C Ga O2B C2B 99.4(6) . . . . ? O2A Ga O2B C2B -165.4(5) . . . . ? O1B Ga O2B C2B -2.2(5) . . . . ? O1A Ga O2B C2B -81.3(6) . . . . ? O1C Ga O2B C2B 20.0(11) . . . . ? La Ga O2B C2B -32.8(6) . . . . ? Ga O1B C1B C6B -177.4(6) . . . . ? La O1B C1B C6B -53.3(11) . . . . ? Ga O1B C1B C2B 1.4(8) . . . . ? La O1B C1B C2B 125.5(6) . . . . ? Ga O2B C2B C3B -176.7(7) . . . . ? Ga O2B C2B C1B 3.6(9) . . . . ? O1B C1B C2B O2B -3.3(11) . . . . ? C6B C1B C2B O2B 175.5(7) . . . . ? O1B C1B C2B C3B 177.0(7) . . . . ? C6B C1B C2B C3B -4.2(12) . . . . ? O2B C2B C3B C4B -179.3(9) . . . . ? C1B C2B C3B C4B 0.4(13) . . . . ? C2B C3B C4B C5B 2.3(15) . . . . ? C3B C4B C5B C6B -1.2(14) . . . . ? O1B C1B C6B C5B -176.0(8) . . . . ? C2B C1B C6B C5B 5.3(12) . . . . ? O1B C1B C6B C7B 3.1(13) . . . . ? C2B C1B C6B C7B -175.6(8) . . . . ? C4B C5B C6B C1B -2.5(13) . . . . ? C4B C5B C6B C7B 178.3(8) . . . . ? C1B C6B C7B N8B 14.4(13) . . . . ? C5B C6B C7B N8B -166.5(8) . . . . ? C6B C7B N8B N9B -179.7(7) . . . . ? C6B C7B N8B La 10.8(12) . . . . ? O1B La N8B C7B -31.0(7) . . . . ? O1A La N8B C7B -0.5(8) . . . . ? O11A La N8B C7B 116.6(8) . . . . ? O11B La N8B C7B -171.6(8) . . . . ? O11C La N8B C7B 168.1(7) . . . . ? O1C La N8B C7B -67.3(8) . . . . ? O21 La N8B C7B 49.3(7) . . . . ? N8A La N8B C7B 81.5(8) . . . . ? N8C La N8B C7B -130.3(7) . . . . ? Ga La N8B C7B -31.4(8) . . . . ? O1B La N8B N9B 159.4(6) . . . . ? O1A La N8B N9B -170.1(5) . . . . ? O11A La N8B N9B -53.0(5) . . . . ? O11B La N8B N9B 18.8(5) . . . . ? O11C La N8B N9B -1.5(6) . . . . ? O1C La N8B N9B 123.1(5) . . . . ? O21 La N8B N9B -120.3(5) . . . . ? N8A La N8B N9B -88.2(6) . . . . ? N8C La N8B N9B 60.1(5) . . . . ? Ga La N8B N9B 159.0(5) . . . . ? C7B N8B N9B C10B 169.6(8) . . . . ? La N8B N9B C10B -18.8(9) . . . . ? N8B N9B C10B O11B 0.9(12) . . . . ? N8B N9B C10B C12B -179.2(7) . . . . ? N9B C10B O11B La 20.9(11) . . . . ? C12B C10B O11B La -159.0(6) . . . . ? O1B La O11B C10B -58.7(7) . . . . ? O1A La O11B C10B -115.1(14) . . . . ? O11A La O11B C10B 69.4(6) . . . . ? O11C La O11B C10B 141.7(7) . . . . ? O1C La O11B C10B -123.7(6) . . . . ? O21 La O11B C10B 20.8(7) . . . . ? N8B La O11B C10B -21.0(6) . . . . ? N8A La O11B C10B 101.8(6) . . . . ? N8C La O11B C10B -157.0(7) . . . . ? Ga La O11B C10B -89.7(7) . . . . ? O11B C10B C12B C13B 34.0(14) . . . . ? N9B C10B C12B C13B -145.9(10) . . . . ? O11B C10B C12B C17B -144.5(10) . . . . ? N9B C10B C12B C17B 35.6(14) . . . . ? C17B C12B C13B C14B -0.4(17) . . . . ? C10B C12B C13B C14B -179.0(11) . . . . ? C12B C13B C14B C15B 1(2) . . . . ? C13B C14B C15B C16B -1(2) . . . . ? C14B C15B C16B C17B 0(2) . . . . ? C15B C16B C17B C12B 0.5(18) . . . . ? C13B C12B C17B C16B -0.5(16) . . . . ? C10B C12B C17B C16B 178.0(10) . . . . ? O2B Ga O1C C1C 69.8(9) . . . . ? O2C Ga O1C C1C -11.6(5) . . . . ? O2A Ga O1C C1C -104.6(5) . . . . ? O1B Ga O1C C1C 92.4(6) . . . . ? O1A Ga O1C C1C 176.1(6) . . . . ? La Ga O1C C1C 134.1(6) . . . . ? O2B Ga O1C La -64.3(7) . . . . ? O2C Ga O1C La -145.7(2) . . . . ? O2A Ga O1C La 121.3(2) . . . . ? O1B Ga O1C La -41.68(19) . . . . ? O1A Ga O1C La 41.98(19) . . . . ? O1B La O1C C1C -81.3(7) . . . . ? O1A La O1C C1C -157.3(7) . . . . ? O11A La O1C C1C 118.6(10) . . . . ? O11B La O1C C1C 21.3(7) . . . . ? O11C La O1C C1C 94.1(7) . . . . ? O21 La O1C C1C -120.2(6) . . . . ? N8B La O1C C1C -43.3(7) . . . . ? N8A La O1C C1C 161.1(6) . . . . ? N8C La O1C C1C 56.6(6) . . . . ? Ga La O1C C1C -119.3(7) . . . . ? O1B La O1C Ga 38.00(19) . . . . ? O1A La O1C Ga -38.08(19) . . . . ? O11A La O1C Ga -122.2(8) . . . . ? O11B La O1C Ga 140.6(2) . . . . ? O11C La O1C Ga -146.6(2) . . . . ? O21 La O1C Ga -0.9(3) . . . . ? N8B La O1C Ga 76.0(2) . . . . ? N8A La O1C Ga -79.6(2) . . . . ? N8C La O1C Ga 175.9(3) . . . . ? O2B Ga O2C C2C -150.1(6) . . . . ? O2A Ga O2C C2C 113.4(6) . . . . ? O1B Ga O2C C2C -66.2(6) . . . . ? O1A Ga O2C C2C 31.9(10) . . . . ? O1C Ga O2C C2C 10.1(6) . . . . ? La Ga O2C C2C -21.9(6) . . . . ? Ga O1C C1C C6C -169.5(8) . . . . ? La O1C C1C C6C -58.1(11) . . . . ? Ga O1C C1C C2C 10.8(9) . . . . ? La O1C C1C C2C 122.2(7) . . . . ? Ga O2C C2C C3C 173.3(8) . . . . ? Ga O2C C2C C1C -7.2(10) . . . . ? O1C C1C C2C O2C -2.8(12) . . . . ? C6C C1C C2C O2C 177.5(8) . . . . ? O1C C1C C2C C3C 176.6(9) . . . . ? C6C C1C C2C C3C -3.1(14) . . . . ? O2C C2C C3C C4C -177.9(10) . . . . ? C1C C2C C3C C4C 2.7(16) . . . . ? C2C C3C C4C C5C -2.5(19) . . . . ? C3C C4C C5C C6C 3(2) . . . . ? O1C C1C C6C C5C -176.4(9) . . . . ? C2C C1C C6C C5C 3.3(14) . . . . ? O1C C1C C6C C7C 3.3(15) . . . . ? C2C C1C C6C C7C -177.1(9) . . . . ? C4C C5C C6C C1C -3.1(17) . . . . ? C4C C5C C6C C7C 177.2(11) . . . . ? C1C C6C C7C N8C 14.1(16) . . . . ? C5C C6C C7C N8C -166.3(11) . . . . ? C6C C7C N8C N9C -178.7(9) . . . . ? C6C C7C N8C La 17.6(16) . . . . ? O1B La N8C C7C -1.4(10) . . . . ? O1A La N8C C7C -69.5(10) . . . . ? O11A La N8C C7C 153.4(9) . . . . ? O11B La N8C C7C 105.0(10) . . . . ? O11C La N8C C7C -172.6(10) . . . . ? O1C La N8C C7C -38.6(9) . . . . ? O21 La N8C C7C 59(5) . . . . ? N8B La N8C C7C 65.8(10) . . . . ? N8A La N8C C7C -139.3(9) . . . . ? Ga La N8C C7C -36.1(10) . . . . ? O1B La N8C N9C -165.8(5) . . . . ? O1A La N8C N9C 126.1(5) . . . . ? O11A La N8C N9C -10.9(6) . . . . ? O11B La N8C N9C -59.3(5) . . . . ? O11C La N8C N9C 23.0(5) . . . . ? O1C La N8C N9C 157.1(6) . . . . ? O21 La N8C N9C -105(4) . . . . ? N8B La N8C N9C -98.5(6) . . . . ? N8A La N8C N9C 56.3(6) . . . . ? Ga La N8C N9C 159.5(5) . . . . ? C7C N8C N9C C10C 169.6(9) . . . . ? La N8C N9C C10C -23.1(10) . . . . ? N8C N9C C10C O11C 1.5(14) . . . . ? N8C N9C C10C C12C -178.6(8) . . . . ? N9C C10C O11C La 27.2(13) . . . . ? C12C C10C O11C La -152.8(7) . . . . ? O1B La O11C C10C -53.1(10) . . . . ? O1A La O11C C10C -127.1(7) . . . . ? O11A La O11C C10C 120.2(8) . . . . ? O11B La O11C C10C 44.9(7) . . . . ? O1C La O11C C10C -65.3(8) . . . . ? O21 La O11C C10C 150.9(7) . . . . ? N8B La O11C C10C 63.4(8) . . . . ? N8A La O11C C10C -172.3(8) . . . . ? N8C La O11C C10C -26.5(7) . . . . ? Ga La O11C C10C -90.9(7) . . . . ? O11C C10C C12C C17C 25.1(14) . . . . ? N9C C10C C12C C17C -154.8(10) . . . . ? O11C C10C C12C C13C -150.7(12) . . . . ? N9C C10C C12C C13C 29.4(15) . . . . ? C17C C12C C13C C14C 2(2) . . . . ? C10C C12C C13C C14C 178.2(14) . . . . ? C12C C13C C14C C15C 0(3) . . . . ? C13C C14C C15C C16C -2(3) . . . . ? C14C C15C C16C C17C 1(2) . . . . ? C13C C12C C17C C16C -2.8(17) . . . . ? C10C C12C C17C C16C -178.6(10) . . . . ? C15C C16C C17C C12C 0.9(18) . . . . ? O1B La O21 C22 -49.4(7) . . . . ? O1A La O21 C22 18.7(7) . . . . ? O11A La O21 C22 153.7(8) . . . . ? O11B La O21 C22 -155.7(7) . . . . ? O11C La O21 C22 122.5(7) . . . . ? O1C La O21 C22 -14.7(8) . . . . ? N8B La O21 C22 -117.6(8) . . . . ? N8A La O21 C22 87.4(7) . . . . ? N8C La O21 C22 -111(4) . . . . ? Ga La O21 C22 -15.3(7) . . . . ? La O21 C22 N23 160.4(7) . . . . ? O21 C22 N23 C24 179.9(9) . . . . ? O21 C22 N23 C25 -2.6(16) . . . . ? O31 C32 N33 C34 23(5) . . . . ? O31 C32 N33 C35 -180(3) . . . . ? O41 C42 N43 C44 179(6) . . . . ? O41 C42 N43 C45 10(12) . . . . ? O51 C52 N53 C54 -123(4) . . . . ? O51 C52 N53 C55 29(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.941 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.138 data_fro4754 _database_code_depnum_ccdc_archive 'CCDC 706325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H43 Br3 Ca N8 O12 Ti' _chemical_formula_weight 1251.61 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0297(2) _cell_length_b 13.9988(2) _cell_length_c 17.2548(3) _cell_angle_alpha 77.225(1) _cell_angle_beta 86.651(1) _cell_angle_gamma 65.781(1) _cell_volume 2582.68(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2861 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 2.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5031 _exptl_absorpt_correction_T_max 0.7772 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28227 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.25 _reflns_number_total 12451 _reflns_number_gt 8414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.6926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'at N9 and water from difmap, others geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12451 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Ca Ca 0.53175(5) 0.16566(5) 0.76652(3) 0.02493(13) Uani 1 1 d . . . Ti Ti 0.79732(5) 0.02119(4) 0.87353(3) 0.02452(12) Uani 1 1 d . . . O1A O 0.75323(17) 0.03167(16) 0.76150(11) 0.0262(4) Uani 1 1 d . . . O2A O 0.95214(18) -0.00117(17) 0.82503(12) 0.0295(5) Uani 1 1 d . . . C1A C 0.8410(3) 0.0307(2) 0.71013(17) 0.0251(6) Uani 1 1 d . . . C2A C 0.9533(3) 0.0114(2) 0.74442(17) 0.0269(6) Uani 1 1 d . . . C3A C 1.0515(3) 0.0085(3) 0.69866(19) 0.0367(8) Uani 1 1 d . . . H3A H 1.1266 -0.0060 0.7224 0.044 Uiso 1 1 calc R . . C4A C 1.0376(3) 0.0274(3) 0.6164(2) 0.0427(9) Uani 1 1 d . . . H4A H 1.1037 0.0262 0.5842 0.051 Uiso 1 1 calc R . . C5A C 0.9275(3) 0.0478(3) 0.5820(2) 0.0398(8) Uani 1 1 d . . . H5A H 0.9199 0.0603 0.5264 0.048 Uiso 1 1 calc R . . C6A C 0.8269(3) 0.0504(2) 0.62767(18) 0.0298(7) Uani 1 1 d . . . C7A C 0.7120(3) 0.0747(2) 0.58821(18) 0.0309(7) Uani 1 1 d . . . H7A H 0.7105 0.0797 0.5330 0.037 Uiso 1 1 calc R . . N8A N 0.6130(2) 0.08970(19) 0.62505(14) 0.0285(6) Uani 1 1 d . . . N9A N 0.5126(2) 0.1139(2) 0.57705(16) 0.0308(6) Uani 1 1 d . . . H9A H 0.517(3) 0.126(3) 0.531(2) 0.033(10) Uiso 1 1 d . . . C10A C 0.4046(3) 0.1371(2) 0.61165(17) 0.0278(6) Uani 1 1 d . . . O10A O 0.3947(2) 0.13248(18) 0.68384(12) 0.0339(5) Uani 1 1 d . . . C11A C 0.2961(3) 0.1697(2) 0.55838(17) 0.0295(7) Uani 1 1 d . . . C12A C 0.3036(3) 0.1481(3) 0.4838(2) 0.0431(9) Uani 1 1 d . . . H12A H 0.3804 0.1090 0.4652 0.052 Uiso 1 1 calc R . . C13A C 0.2000(3) 0.1830(3) 0.4353(2) 0.0441(9) Uani 1 1 d . . . H13A H 0.2063 0.1680 0.3843 0.053 Uiso 1 1 calc R . . C14A C 0.0885(3) 0.2396(3) 0.4632(2) 0.0407(8) Uani 1 1 d . . . C15A C 0.0783(3) 0.2621(4) 0.5375(2) 0.0541(10) Uani 1 1 d . . . H15A H 0.0015 0.3018 0.5558 0.065 Uiso 1 1 calc R . . C16A C 0.1823(3) 0.2254(3) 0.5852(2) 0.0460(9) Uani 1 1 d . . . H16A H 0.1754 0.2386 0.6367 0.055 Uiso 1 1 calc R . . Br1A Br -0.05358(4) 0.28557(4) 0.39854(2) 0.05785(13) Uani 1 1 d . . . O1B O 0.69294(18) 0.17920(16) 0.84239(11) 0.0261(4) Uani 1 1 d . . . O2B O 0.83425(19) 0.07019(17) 0.96090(12) 0.0308(5) Uani 1 1 d . . . C1B C 0.6923(3) 0.2353(2) 0.89543(16) 0.0252(6) Uani 1 1 d . . . C2B C 0.7742(3) 0.1755(3) 0.96117(17) 0.0298(7) Uani 1 1 d . . . C3B C 0.7850(3) 0.2239(3) 1.02049(19) 0.0396(8) Uani 1 1 d . . . H3B H 0.8403 0.1842 1.0639 0.047 Uiso 1 1 calc R . . C4B C 0.7125(3) 0.3322(3) 1.0145(2) 0.0445(9) Uani 1 1 d . . . H4B H 0.7189 0.3658 1.0546 0.053 Uiso 1 1 calc R . . C5B C 0.6314(3) 0.3915(3) 0.9512(2) 0.0386(8) Uani 1 1 d . . . H5B H 0.5833 0.4647 0.9487 0.046 Uiso 1 1 calc R . . C6B C 0.6197(3) 0.3439(2) 0.89015(18) 0.0291(7) Uani 1 1 d . . . C7B C 0.5378(3) 0.4093(2) 0.82212(18) 0.0294(7) Uani 1 1 d . . . H7B H 0.5001 0.4841 0.8170 0.035 Uiso 1 1 calc R . . N8B N 0.5152(2) 0.3682(2) 0.76875(15) 0.0287(6) Uani 1 1 d . . . N9B N 0.4450(2) 0.4411(2) 0.70324(15) 0.0304(6) Uani 1 1 d . . . H9B H 0.395(3) 0.509(3) 0.708(2) 0.041(10) Uiso 1 1 d . . . C10B C 0.4342(3) 0.3998(2) 0.64236(18) 0.0287(7) Uani 1 1 d . . . O10B O 0.4792(2) 0.30263(16) 0.64528(12) 0.0316(5) Uani 1 1 d . . . C11B C 0.3693(3) 0.4775(2) 0.56864(18) 0.0311(7) Uani 1 1 d . . . C12B C 0.3696(3) 0.5788(3) 0.54613(19) 0.0355(7) Uani 1 1 d . . . H12B H 0.4053 0.6031 0.5803 0.043 Uiso 1 1 calc R . . C13B C 0.3176(3) 0.6442(3) 0.4737(2) 0.0413(9) Uani 1 1 d . . . H13B H 0.3178 0.7129 0.4583 0.050 Uiso 1 1 calc R . . C14B C 0.2657(3) 0.6082(3) 0.42426(19) 0.0370(8) Uani 1 1 d . . . C15B C 0.2625(4) 0.5083(3) 0.4465(2) 0.0522(10) Uani 1 1 d . . . H15B H 0.2246 0.4850 0.4131 0.063 Uiso 1 1 calc R . . C16B C 0.3157(4) 0.4436(3) 0.5185(2) 0.0486(10) Uani 1 1 d . . . H16B H 0.3155 0.3749 0.5336 0.058 Uiso 1 1 calc R . . Br1B Br 0.19749(4) 0.69615(3) 0.32369(2) 0.05208(12) Uani 1 1 d . . . O1C O 0.63021(17) 0.02412(16) 0.88617(11) 0.0263(4) Uani 1 1 d . . . O2C O 0.83631(18) -0.12236(16) 0.93077(12) 0.0301(5) Uani 1 1 d . . . C1C C 0.6276(3) -0.0704(2) 0.92004(16) 0.0249(6) Uani 1 1 d . . . C2C C 0.7423(3) -0.1528(2) 0.94637(16) 0.0270(6) Uani 1 1 d . . . C3C C 0.7520(3) -0.2538(3) 0.98426(19) 0.0362(8) Uani 1 1 d . . . H3C H 0.8287 -0.3093 1.0013 0.043 Uiso 1 1 calc R . . C4C C 0.6467(3) -0.2723(3) 0.9969(2) 0.0413(8) Uani 1 1 d . . . H4C H 0.6524 -0.3408 1.0228 0.050 Uiso 1 1 calc R . . C5C C 0.5338(3) -0.1915(3) 0.97190(19) 0.0353(7) Uani 1 1 d . . . H5C H 0.4635 -0.2054 0.9816 0.042 Uiso 1 1 calc R . . C6C C 0.5224(3) -0.0887(2) 0.93207(16) 0.0269(6) Uani 1 1 d . . . C7C C 0.4020(3) -0.0042(2) 0.90742(17) 0.0276(6) Uani 1 1 d . . . H7C H 0.3330 -0.0163 0.9263 0.033 Uiso 1 1 calc R . . N8C N 0.3863(2) 0.0858(2) 0.86101(14) 0.0257(5) Uani 1 1 d . . . N9C N 0.2655(2) 0.1571(2) 0.84562(15) 0.0286(6) Uani 1 1 d . . . H9C H 0.212(3) 0.132(3) 0.860(2) 0.033(9) Uiso 1 1 d . . . C10C C 0.2422(3) 0.2582(2) 0.80970(17) 0.0270(6) Uani 1 1 d . . . O10C O 0.32412(19) 0.28941(17) 0.78703(13) 0.0325(5) Uani 1 1 d . . . C11C C 0.1111(3) 0.3349(3) 0.79753(19) 0.0317(7) Uani 1 1 d . . . C12C C 0.0792(3) 0.4239(3) 0.7353(2) 0.0394(8) Uani 1 1 d . . . H12C H 0.1394 0.4333 0.7011 0.047 Uiso 1 1 calc R . . C13C C -0.0402(3) 0.4991(3) 0.7228(2) 0.0468(9) Uani 1 1 d . . . H13C H -0.0621 0.5589 0.6801 0.056 Uiso 1 1 calc R . . C14C C -0.1267(3) 0.4840(3) 0.7747(3) 0.0474(9) Uani 1 1 d . . . C15C C -0.0974(3) 0.3967(3) 0.8368(2) 0.0449(9) Uani 1 1 d . . . H15C H -0.1578 0.3881 0.8711 0.054 Uiso 1 1 calc R . . C16C C 0.0217(3) 0.3215(3) 0.8483(2) 0.0386(8) Uani 1 1 d . . . H16C H 0.0426 0.2610 0.8905 0.046 Uiso 1 1 calc R . . Br1C Br -0.29035(4) 0.58807(4) 0.75745(4) 0.07820(17) Uani 1 1 d . . . O100 O 1.1047(3) 0.0631(3) 0.89075(18) 0.0534(8) Uani 1 1 d . . . H1AA H 1.113(4) 0.034(4) 0.937(3) 0.066(14) Uiso 1 1 d . . . H1AB H 1.061(5) 0.058(4) 0.869(3) 0.070(17) Uiso 1 1 d . . . O101 O 0.5661(3) 0.1514(4) 0.41055(17) 0.0999(14) Uani 1 1 d . . . C102 C 0.6010(4) 0.1846(4) 0.3457(3) 0.0725(14) Uani 1 1 d . . . H102 H 0.6565 0.2162 0.3456 0.087 Uiso 1 1 calc R . . N103 N 0.5664(3) 0.1790(3) 0.27703(17) 0.0509(8) Uani 1 1 d . . . C104 C 0.6175(5) 0.2137(4) 0.2033(2) 0.0717(14) Uani 1 1 d . . . H10A H 0.6677 0.2491 0.2137 0.108 Uiso 1 1 calc R . . H10B H 0.5519 0.2632 0.1654 0.108 Uiso 1 1 calc R . . H10C H 0.6670 0.1518 0.1815 0.108 Uiso 1 1 calc R . . C105 C 0.4806(5) 0.1319(3) 0.2709(3) 0.0656(12) Uani 1 1 d . . . H10D H 0.5243 0.0609 0.2601 0.098 Uiso 1 1 calc R . . H10E H 0.4212 0.1768 0.2281 0.098 Uiso 1 1 calc R . . H10F H 0.4391 0.1264 0.3206 0.098 Uiso 1 1 calc R . . O111 O 0.2609(2) 0.6220(2) 0.74593(16) 0.0487(6) Uani 1 1 d . . . C112 C 0.2118(3) 0.5776(3) 0.7976(2) 0.0440(9) Uani 1 1 d . . . H112 H 0.2501 0.5024 0.8131 0.053 Uiso 1 1 calc R . . N113 N 0.1107(3) 0.6259(2) 0.83288(19) 0.0472(8) Uani 1 1 d . . . C114 C 0.0430(4) 0.7403(3) 0.8123(3) 0.0660(12) Uani 1 1 d . . . H11A H 0.0878 0.7721 0.7745 0.099 Uiso 1 1 calc R . . H11B H 0.0314 0.7691 0.8598 0.099 Uiso 1 1 calc R . . H11C H -0.0358 0.7569 0.7887 0.099 Uiso 1 1 calc R . . C115 C 0.0631(5) 0.5660(4) 0.8957(3) 0.0767(14) Uani 1 1 d . . . H11D H 0.1130 0.4898 0.9020 0.115 Uiso 1 1 calc R . . H11E H -0.0202 0.5810 0.8817 0.115 Uiso 1 1 calc R . . H11F H 0.0650 0.5874 0.9452 0.115 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 0.0228(3) 0.0278(3) 0.0231(3) -0.0014(2) -0.0013(2) -0.0111(2) Ti 0.0209(3) 0.0301(3) 0.0222(2) -0.0017(2) -0.00133(19) -0.0117(2) O1A 0.0220(10) 0.0355(11) 0.0214(9) -0.0049(9) 0.0006(8) -0.0127(9) O2A 0.0236(11) 0.0404(12) 0.0249(10) -0.0053(9) -0.0011(8) -0.0141(9) C1A 0.0253(15) 0.0243(14) 0.0248(14) -0.0064(12) 0.0013(11) -0.0086(12) C2A 0.0241(15) 0.0306(15) 0.0255(14) -0.0070(12) 0.0014(11) -0.0103(13) C3A 0.0245(16) 0.0432(19) 0.0380(18) -0.0073(15) 0.0047(13) -0.0106(14) C4A 0.0343(19) 0.056(2) 0.0380(18) -0.0144(17) 0.0142(15) -0.0184(17) C5A 0.0329(18) 0.052(2) 0.0288(16) -0.0153(15) 0.0065(13) -0.0095(16) C6A 0.0289(16) 0.0312(16) 0.0284(15) -0.0112(13) 0.0030(12) -0.0092(13) C7A 0.0359(18) 0.0331(16) 0.0232(14) -0.0108(13) 0.0000(13) -0.0112(14) N8A 0.0263(14) 0.0286(13) 0.0273(13) -0.0055(11) -0.0045(10) -0.0076(11) N9A 0.0308(15) 0.0375(15) 0.0214(13) -0.0067(12) -0.0063(11) -0.0101(12) C10A 0.0301(16) 0.0257(15) 0.0276(15) -0.0050(12) -0.0026(12) -0.0112(13) O10A 0.0379(13) 0.0443(13) 0.0247(11) -0.0074(10) 0.0000(9) -0.0218(11) C11A 0.0324(17) 0.0292(16) 0.0275(15) -0.0041(13) -0.0018(12) -0.0139(14) C12A 0.0337(19) 0.053(2) 0.0375(18) -0.0204(17) -0.0031(14) -0.0069(16) C13A 0.036(2) 0.057(2) 0.0366(18) -0.0172(17) -0.0046(15) -0.0131(17) C14A 0.0346(19) 0.047(2) 0.0385(18) 0.0035(16) -0.0084(15) -0.0199(16) C15A 0.0273(19) 0.082(3) 0.050(2) -0.017(2) 0.0048(16) -0.0174(19) C16A 0.037(2) 0.068(3) 0.0354(18) -0.0172(18) 0.0069(15) -0.0218(19) Br1A 0.0357(2) 0.0794(3) 0.0526(2) 0.0048(2) -0.01350(17) -0.0254(2) O1B 0.0289(11) 0.0289(10) 0.0229(10) -0.0055(8) -0.0007(8) -0.0141(9) O2B 0.0282(11) 0.0379(12) 0.0258(10) -0.0024(9) -0.0052(8) -0.0144(10) C1B 0.0246(15) 0.0348(16) 0.0225(14) -0.0067(12) 0.0055(11) -0.0186(13) C2B 0.0289(16) 0.0418(18) 0.0246(14) -0.0063(13) 0.0048(12) -0.0213(14) C3B 0.042(2) 0.057(2) 0.0282(16) -0.0106(16) -0.0018(14) -0.0278(18) C4B 0.050(2) 0.056(2) 0.0383(19) -0.0212(17) 0.0044(16) -0.0270(19) C5B 0.0362(19) 0.046(2) 0.0427(19) -0.0224(16) 0.0114(15) -0.0204(16) C6B 0.0268(16) 0.0363(17) 0.0300(15) -0.0108(13) 0.0069(12) -0.0176(14) C7B 0.0249(16) 0.0302(16) 0.0351(16) -0.0108(14) 0.0076(13) -0.0121(13) N8B 0.0232(13) 0.0291(13) 0.0300(13) -0.0024(11) 0.0015(10) -0.0090(11) N9B 0.0304(14) 0.0257(14) 0.0304(14) -0.0028(11) 0.0001(11) -0.0082(12) C10B 0.0257(15) 0.0275(16) 0.0317(16) -0.0025(13) 0.0043(12) -0.0120(13) O10B 0.0380(13) 0.0256(11) 0.0287(11) -0.0028(9) 0.0009(9) -0.0119(10) C11B 0.0303(17) 0.0297(16) 0.0310(16) -0.0025(13) 0.0025(13) -0.0121(13) C12B 0.0357(18) 0.0307(16) 0.0357(17) -0.0029(14) 0.0023(14) -0.0115(14) C13B 0.047(2) 0.0272(17) 0.0425(19) 0.0007(15) 0.0084(16) -0.0132(16) C14B 0.0354(18) 0.0347(17) 0.0280(16) 0.0035(14) 0.0027(13) -0.0068(15) C15B 0.069(3) 0.046(2) 0.041(2) 0.0083(17) -0.0209(18) -0.028(2) C16B 0.066(3) 0.0368(19) 0.045(2) 0.0072(16) -0.0145(18) -0.0284(19) Br1B 0.0590(3) 0.0436(2) 0.03317(18) 0.00815(16) -0.00073(16) -0.00876(18) O1C 0.0216(10) 0.0288(11) 0.0279(10) 0.0002(9) 0.0000(8) -0.0128(9) O2C 0.0235(11) 0.0308(11) 0.0319(11) 0.0006(9) -0.0031(9) -0.0103(9) C1C 0.0269(15) 0.0300(15) 0.0187(13) -0.0024(12) 0.0000(11) -0.0139(13) C2C 0.0258(15) 0.0338(16) 0.0217(14) -0.0041(12) 0.0020(11) -0.0136(13) C3C 0.0364(18) 0.0322(17) 0.0325(16) 0.0039(14) -0.0027(14) -0.0114(15) C4C 0.043(2) 0.0346(18) 0.045(2) 0.0041(15) 0.0001(16) -0.0212(16) C5C 0.0352(18) 0.0408(18) 0.0341(17) -0.0019(14) 0.0026(14) -0.0230(15) C6C 0.0292(16) 0.0332(16) 0.0210(14) -0.0052(12) 0.0024(11) -0.0159(13) C7C 0.0258(16) 0.0356(16) 0.0251(14) -0.0056(13) 0.0054(12) -0.0174(13) N8C 0.0188(12) 0.0347(14) 0.0239(12) -0.0065(11) 0.0019(9) -0.0113(11) N9C 0.0203(13) 0.0347(14) 0.0316(13) -0.0039(11) 0.0020(10) -0.0138(12) C10C 0.0243(15) 0.0348(16) 0.0246(14) -0.0086(13) 0.0034(11) -0.0141(13) O10C 0.0254(11) 0.0333(11) 0.0400(12) -0.0067(10) 0.0068(9) -0.0143(9) C11C 0.0266(16) 0.0353(17) 0.0361(17) -0.0106(14) 0.0041(13) -0.0145(14) C12C 0.0314(18) 0.0416(19) 0.0453(19) -0.0054(16) 0.0054(15) -0.0175(16) C13C 0.039(2) 0.0377(19) 0.055(2) 0.0029(17) -0.0027(17) -0.0130(16) C14C 0.0245(18) 0.040(2) 0.072(3) -0.0121(19) 0.0029(17) -0.0083(15) C15C 0.0247(17) 0.045(2) 0.062(2) -0.0098(18) 0.0126(16) -0.0131(15) C16C 0.0303(18) 0.0381(18) 0.0458(19) -0.0068(16) 0.0066(15) -0.0141(15) Br1C 0.0326(2) 0.0536(3) 0.1213(4) -0.0039(3) 0.0045(2) 0.00144(19) O100 0.0538(18) 0.082(2) 0.0359(15) 0.0181(14) -0.0182(13) -0.0525(17) O101 0.085(3) 0.166(4) 0.0303(15) -0.011(2) 0.0064(16) -0.039(3) C102 0.064(3) 0.104(4) 0.043(2) -0.021(2) 0.003(2) -0.026(3) N103 0.065(2) 0.0526(19) 0.0326(16) -0.0092(14) 0.0061(15) -0.0225(17) C104 0.095(4) 0.093(4) 0.040(2) -0.012(2) 0.014(2) -0.053(3) C105 0.091(4) 0.053(2) 0.057(3) -0.009(2) 0.005(2) -0.035(3) O111 0.0425(15) 0.0419(14) 0.0561(16) -0.0144(13) 0.0032(12) -0.0098(12) C112 0.042(2) 0.0373(19) 0.051(2) -0.0153(17) -0.0067(17) -0.0097(17) N113 0.0398(18) 0.0490(18) 0.0540(19) -0.0228(15) 0.0053(14) -0.0139(15) C114 0.050(3) 0.054(3) 0.077(3) -0.029(2) 0.001(2) 0.003(2) C115 0.079(4) 0.088(4) 0.079(3) -0.030(3) 0.029(3) -0.047(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca O10B 2.416(2) . ? Ca O10C 2.446(2) . ? Ca O1C 2.4783(19) . ? Ca O10A 2.483(2) . ? Ca O1B 2.493(2) . ? Ca O1A 2.563(2) . ? Ca N8C 2.726(2) . ? Ca N8B 2.769(3) . ? Ca N8A 2.839(3) . ? Ca Ti 3.3827(7) . ? Ti O2C 1.907(2) . ? Ti O2A 1.929(2) . ? Ti O2B 1.930(2) . ? Ti O1A 1.993(2) . ? Ti O1C 1.994(2) . ? Ti O1B 2.008(2) . ? O1A C1A 1.336(3) . ? O2A C2A 1.363(3) . ? C1A C6A 1.395(4) . ? C1A C2A 1.403(4) . ? C2A C3A 1.373(4) . ? C3A C4A 1.392(5) . ? C4A C5A 1.376(5) . ? C5A C6A 1.398(4) . ? C6A C7A 1.452(4) . ? C7A N8A 1.278(4) . ? N8A N9A 1.384(3) . ? N9A C10A 1.342(4) . ? C10A O10A 1.234(3) . ? C10A C11A 1.490(4) . ? C11A C12A 1.376(5) . ? C11A C16A 1.380(5) . ? C12A C13A 1.390(5) . ? C13A C14A 1.372(5) . ? C14A C15A 1.373(5) . ? C14A Br1A 1.893(3) . ? C15A C16A 1.383(5) . ? O1B C1B 1.330(4) . ? O2B C2B 1.351(4) . ? C1B C6B 1.393(4) . ? C1B C2B 1.411(4) . ? C2B C3B 1.385(5) . ? C3B C4B 1.388(5) . ? C4B C5B 1.376(5) . ? C5B C6B 1.406(5) . ? C6B C7B 1.452(4) . ? C7B N8B 1.282(4) . ? N8B N9B 1.388(3) . ? N9B C10B 1.342(4) . ? C10B O10B 1.230(4) . ? C10B C11B 1.489(4) . ? C11B C16B 1.374(5) . ? C11B C12B 1.387(4) . ? C12B C13B 1.381(5) . ? C13B C14B 1.372(5) . ? C14B C15B 1.382(5) . ? C14B Br1B 1.896(3) . ? C15B C16B 1.376(5) . ? O1C C1C 1.335(3) . ? O2C C2C 1.357(3) . ? C1C C6C 1.387(4) . ? C1C C2C 1.405(4) . ? C2C C3C 1.381(4) . ? C3C C4C 1.390(5) . ? C4C C5C 1.379(5) . ? C5C C6C 1.405(4) . ? C6C C7C 1.456(4) . ? C7C N8C 1.282(4) . ? N8C N9C 1.384(3) . ? N9C C10C 1.332(4) . ? C10C O10C 1.243(3) . ? C10C C11C 1.494(4) . ? C11C C12C 1.384(5) . ? C11C C16C 1.394(4) . ? C12C C13C 1.383(5) . ? C13C C14C 1.384(5) . ? C14C C15C 1.370(5) . ? C14C Br1C 1.900(3) . ? C15C C16C 1.380(5) . ? O101 C102 1.233(5) . ? C102 N103 1.306(5) . ? N103 C105 1.454(5) . ? N103 C104 1.453(5) . ? O111 C112 1.235(4) . ? C112 N113 1.314(5) . ? N113 C114 1.438(5) . ? N113 C115 1.457(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 O10B Ca O10C 76.42(7) . . ? O10B Ca O1C 167.69(7) . . ? O10C Ca O1C 113.62(7) . . ? O10B Ca O10A 72.29(7) . . ? O10C Ca O10A 73.71(8) . . ? O1C Ca O10A 116.52(7) . . ? O10B Ca O1B 108.82(7) . . ? O10C Ca O1B 114.22(8) . . ? O1C Ca O1B 61.20(6) . . ? O10A Ca O1B 172.06(8) . . ? O10B Ca O1A 108.94(7) . . ? O10C Ca O1A 173.74(7) . . ? O1C Ca O1A 60.65(6) . . ? O10A Ca O1A 110.70(7) . . ? O1B Ca O1A 61.40(7) . . ? O10B Ca N8C 129.28(7) . . ? O10C Ca N8C 61.56(7) . . ? O1C Ca N8C 63.03(7) . . ? O10A Ca N8C 69.78(7) . . ? O1B Ca N8C 113.40(7) . . ? O1A Ca N8C 115.19(7) . . ? O10B Ca N8B 60.27(7) . . ? O10C Ca N8B 67.40(7) . . ? O1C Ca N8B 115.73(7) . . ? O10A Ca N8B 123.65(7) . . ? O1B Ca N8B 61.88(7) . . ? O1A Ca N8B 112.04(7) . . ? N8C Ca N8B 119.46(8) . . ? O10B Ca N8A 64.79(7) . . ? O10C Ca N8A 125.21(7) . . ? O1C Ca N8A 111.27(7) . . ? O10A Ca N8A 58.92(7) . . ? O1B Ca N8A 114.05(7) . . ? O1A Ca N8A 60.86(7) . . ? N8C Ca N8A 117.90(8) . . ? N8B Ca N8A 117.17(7) . . ? O10B Ca Ti 131.95(6) . . ? O10C Ca Ti 137.92(6) . . ? O1C Ca Ti 35.74(4) . . ? O10A Ca Ti 137.56(6) . . ? O1B Ca Ti 36.12(5) . . ? O1A Ca Ti 35.93(4) . . ? N8C Ca Ti 98.74(5) . . ? N8B Ca Ti 97.92(5) . . ? N8A Ca Ti 96.77(5) . . ? O2C Ti O2A 98.30(9) . . ? O2C Ti O2B 95.74(9) . . ? O2A Ti O2B 94.17(9) . . ? O2C Ti O1A 108.09(9) . . ? O2A Ti O1A 79.71(8) . . ? O2B Ti O1A 155.97(9) . . ? O2C Ti O1C 80.05(8) . . ? O2A Ti O1C 157.36(9) . . ? O2B Ti O1C 108.47(9) . . ? O1A Ti O1C 79.40(8) . . ? O2C Ti O1B 154.95(9) . . ? O2A Ti O1B 106.49(9) . . ? O2B Ti O1B 79.14(8) . . ? O1A Ti O1B 80.39(8) . . ? O1C Ti O1B 78.45(8) . . ? O2C Ti Ca 121.14(6) . . ? O2A Ti Ca 121.12(6) . . ? O2B Ti Ca 120.17(7) . . ? O1A Ti Ca 49.00(6) . . ? O1C Ti Ca 46.56(5) . . ? O1B Ti Ca 47.04(6) . . ? C1A O1A Ti 114.46(17) . . ? C1A O1A Ca 132.49(16) . . ? Ti O1A Ca 95.07(8) . . ? C2A O2A Ti 116.64(17) . . ? O1A C1A C6A 125.0(3) . . ? O1A C1A C2A 115.2(2) . . ? C6A C1A C2A 119.8(3) . . ? O2A C2A C3A 125.2(3) . . ? O2A C2A C1A 113.4(2) . . ? C3A C2A C1A 121.4(3) . . ? C2A C3A C4A 118.8(3) . . ? C5A C4A C3A 120.3(3) . . ? C4A C5A C6A 121.7(3) . . ? C1A C6A C5A 118.0(3) . . ? C1A C6A C7A 122.6(3) . . ? C5A C6A C7A 119.4(3) . . ? N8A C7A C6A 123.0(3) . . ? C7A N8A N9A 114.6(3) . . ? C7A N8A Ca 131.2(2) . . ? N9A N8A Ca 109.03(18) . . ? C10A N9A N8A 117.2(3) . . ? O10A C10A N9A 122.0(3) . . ? O10A C10A C11A 121.4(3) . . ? N9A C10A C11A 116.6(3) . . ? C10A O10A Ca 123.80(19) . . ? C12A C11A C16A 118.4(3) . . ? C12A C11A C10A 123.5(3) . . ? C16A C11A C10A 118.1(3) . . ? C11A C12A C13A 121.4(3) . . ? C14A C13A C12A 118.8(3) . . ? C13A C14A C15A 121.1(3) . . ? C13A C14A Br1A 119.2(3) . . ? C15A C14A Br1A 119.7(3) . . ? C14A C15A C16A 119.2(4) . . ? C11A C16A C15A 121.1(3) . . ? C1B O1B Ti 115.08(17) . . ? C1B O1B Ca 134.56(18) . . ? Ti O1B Ca 96.84(8) . . ? C2B O2B Ti 117.19(18) . . ? O1B C1B C6B 125.5(3) . . ? O1B C1B C2B 114.3(3) . . ? C6B C1B C2B 120.1(3) . . ? O2B C2B C3B 125.2(3) . . ? O2B C2B C1B 114.0(3) . . ? C3B C2B C1B 120.7(3) . . ? C2B C3B C4B 118.7(3) . . ? C5B C4B C3B 121.3(3) . . ? C4B C5B C6B 120.8(3) . . ? C1B C6B C5B 118.3(3) . . ? C1B C6B C7B 121.9(3) . . ? C5B C6B C7B 119.7(3) . . ? N8B C7B C6B 122.0(3) . . ? C7B N8B N9B 115.6(3) . . ? C7B N8B Ca 133.73(19) . . ? N9B N8B Ca 109.16(18) . . ? C10B N9B N8B 116.2(3) . . ? O10B C10B N9B 122.3(3) . . ? O10B C10B C11B 120.8(3) . . ? N9B C10B C11B 116.9(3) . . ? C10B O10B Ca 124.75(19) . . ? C16B C11B C12B 119.3(3) . . ? C16B C11B C10B 118.1(3) . . ? C12B C11B C10B 122.4(3) . . ? C13B C12B C11B 120.2(3) . . ? C14B C13B C12B 119.5(3) . . ? C13B C14B C15B 121.0(3) . . ? C13B C14B Br1B 119.7(2) . . ? C15B C14B Br1B 119.2(3) . . ? C16B C15B C14B 118.8(4) . . ? C11B C16B C15B 121.2(3) . . ? C1C O1C Ti 114.38(17) . . ? C1C O1C Ca 135.26(17) . . ? Ti O1C Ca 97.70(7) . . ? C2C O2C Ti 116.89(17) . . ? O1C C1C C6C 124.6(3) . . ? O1C C1C C2C 114.5(2) . . ? C6C C1C C2C 120.8(3) . . ? O2C C2C C3C 125.8(3) . . ? O2C C2C C1C 113.9(2) . . ? C3C C2C C1C 120.4(3) . . ? C2C C3C C4C 119.0(3) . . ? C5C C4C C3C 120.9(3) . . ? C4C C5C C6C 120.9(3) . . ? C1C C6C C5C 118.1(3) . . ? C1C C6C C7C 122.1(3) . . ? C5C C6C C7C 119.8(3) . . ? N8C C7C C6C 122.7(3) . . ? C7C N8C N9C 114.5(2) . . ? C7C N8C Ca 135.3(2) . . ? N9C N8C Ca 109.50(16) . . ? C10C N9C N8C 117.9(2) . . ? O10C C10C N9C 122.7(3) . . ? O10C C10C C11C 120.4(3) . . ? N9C C10C C11C 116.9(3) . . ? C10C O10C Ca 122.37(19) . . ? C12C C11C C16C 119.4(3) . . ? C12C C11C C10C 118.4(3) . . ? C16C C11C C10C 122.1(3) . . ? C13C C12C C11C 120.8(3) . . ? C12C C13C C14C 118.4(3) . . ? C15C C14C C13C 121.9(3) . . ? C15C C14C Br1C 119.9(3) . . ? C13C C14C Br1C 118.1(3) . . ? C14C C15C C16C 119.3(3) . . ? C15C C16C C11C 120.2(3) . . ? O101 C102 N103 124.7(5) . . ? C102 N103 C105 121.8(4) . . ? C102 N103 C104 121.6(4) . . ? C105 N103 C104 116.5(3) . . ? O111 C112 N113 125.9(3) . . ? C112 N113 C114 121.6(3) . . ? C112 N113 C115 121.5(4) . . ? C114 N113 C115 116.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10B Ca Ti O2C -147.65(11) . . . . ? O10C Ca Ti O2C 90.72(11) . . . . ? O1C Ca Ti O2C 31.74(11) . . . . ? O10A Ca Ti O2C -35.51(11) . . . . ? O1B Ca Ti O2C 152.09(11) . . . . ? O1A Ca Ti O2C -87.44(11) . . . . ? N8C Ca Ti O2C 34.00(10) . . . . ? N8B Ca Ti O2C 155.59(9) . . . . ? N8A Ca Ti O2C -85.68(10) . . . . ? O10B Ca Ti O2A -23.46(11) . . . . ? O10C Ca Ti O2A -145.09(11) . . . . ? O1C Ca Ti O2A 155.93(12) . . . . ? O10A Ca Ti O2A 88.68(11) . . . . ? O1B Ca Ti O2A -83.73(11) . . . . ? O1A Ca Ti O2A 36.75(11) . . . . ? N8C Ca Ti O2A 158.19(10) . . . . ? N8B Ca Ti O2A -80.22(10) . . . . ? N8A Ca Ti O2A 38.51(10) . . . . ? O10B Ca Ti O2B 93.24(10) . . . . ? O10C Ca Ti O2B -28.39(11) . . . . ? O1C Ca Ti O2B -87.37(11) . . . . ? O10A Ca Ti O2B -154.62(10) . . . . ? O1B Ca Ti O2B 32.97(10) . . . . ? O1A Ca Ti O2B 153.45(11) . . . . ? N8C Ca Ti O2B -85.11(9) . . . . ? N8B Ca Ti O2B 36.48(9) . . . . ? N8A Ca Ti O2B 155.21(9) . . . . ? O10B Ca Ti O1A -60.21(11) . . . . ? O10C Ca Ti O1A 178.16(11) . . . . ? O1C Ca Ti O1A 119.18(11) . . . . ? O10A Ca Ti O1A 51.93(11) . . . . ? O1B Ca Ti O1A -120.47(11) . . . . ? N8C Ca Ti O1A 121.44(10) . . . . ? N8B Ca Ti O1A -116.97(9) . . . . ? N8A Ca Ti O1A 1.77(9) . . . . ? O10B Ca Ti O1C -179.39(12) . . . . ? O10C Ca Ti O1C 58.98(11) . . . . ? O10A Ca Ti O1C -67.25(11) . . . . ? O1B Ca Ti O1C 120.34(12) . . . . ? O1A Ca Ti O1C -119.18(11) . . . . ? N8C Ca Ti O1C 2.26(10) . . . . ? N8B Ca Ti O1C 123.85(10) . . . . ? N8A Ca Ti O1C -117.42(10) . . . . ? O10B Ca Ti O1B 60.27(11) . . . . ? O10C Ca Ti O1B -61.36(11) . . . . ? O1C Ca Ti O1B -120.34(12) . . . . ? O10A Ca Ti O1B 172.40(11) . . . . ? O1A Ca Ti O1B 120.47(11) . . . . ? N8C Ca Ti O1B -118.09(10) . . . . ? N8B Ca Ti O1B 3.50(9) . . . . ? N8A Ca Ti O1B 122.24(9) . . . . ? O2C Ti O1A C1A -102.33(19) . . . . ? O2A Ti O1A C1A -6.87(19) . . . . ? O2B Ti O1A C1A 70.1(3) . . . . ? O1C Ti O1A C1A -178.1(2) . . . . ? O1B Ti O1A C1A 101.99(19) . . . . ? Ca Ti O1A C1A 141.8(2) . . . . ? O2C Ti O1A Ca 115.91(8) . . . . ? O2A Ti O1A Ca -148.63(9) . . . . ? O2B Ti O1A Ca -71.7(2) . . . . ? O1C Ti O1A Ca 40.16(7) . . . . ? O1B Ti O1A Ca -39.77(7) . . . . ? O10B Ca O1A C1A 6.8(3) . . . . ? O10C Ca O1A C1A -141.5(6) . . . . ? O1C Ca O1A C1A -166.0(3) . . . . ? O10A Ca O1A C1A 84.4(2) . . . . ? O1B Ca O1A C1A -94.8(2) . . . . ? N8C Ca O1A C1A 161.1(2) . . . . ? N8B Ca O1A C1A -57.9(3) . . . . ? N8A Ca O1A C1A 51.8(2) . . . . ? Ti Ca O1A C1A -130.2(3) . . . . ? O10B Ca O1A Ti 136.98(8) . . . . ? O10C Ca O1A Ti -11.4(7) . . . . ? O1C Ca O1A Ti -35.81(7) . . . . ? O10A Ca O1A Ti -145.39(7) . . . . ? O1B Ca O1A Ti 35.35(7) . . . . ? N8C Ca O1A Ti -68.73(10) . . . . ? N8B Ca O1A Ti 72.23(9) . . . . ? N8A Ca O1A Ti -177.99(10) . . . . ? O2C Ti O2A C2A 113.3(2) . . . . ? O2B Ti O2A C2A -150.2(2) . . . . ? O1A Ti O2A C2A 6.3(2) . . . . ? O1C Ti O2A C2A 29.3(3) . . . . ? O1B Ti O2A C2A -70.3(2) . . . . ? Ca Ti O2A C2A -21.0(2) . . . . ? Ti O1A C1A C6A -171.6(2) . . . . ? Ca O1A C1A C6A -48.3(4) . . . . ? Ti O1A C1A C2A 6.3(3) . . . . ? Ca O1A C1A C2A 129.6(2) . . . . ? Ti O2A C2A C3A 173.8(3) . . . . ? Ti O2A C2A C1A -4.8(3) . . . . ? O1A C1A C2A O2A -1.1(4) . . . . ? C6A C1A C2A O2A 176.9(3) . . . . ? O1A C1A C2A C3A -179.8(3) . . . . ? C6A C1A C2A C3A -1.8(5) . . . . ? O2A C2A C3A C4A -177.2(3) . . . . ? C1A C2A C3A C4A 1.3(5) . . . . ? C2A C3A C4A C5A -0.4(5) . . . . ? C3A C4A C5A C6A 0.1(6) . . . . ? O1A C1A C6A C5A 179.2(3) . . . . ? C2A C1A C6A C5A 1.4(5) . . . . ? O1A C1A C6A C7A 0.0(5) . . . . ? C2A C1A C6A C7A -177.8(3) . . . . ? C4A C5A C6A C1A -0.6(5) . . . . ? C4A C5A C6A C7A 178.6(3) . . . . ? C1A C6A C7A N8A 6.7(5) . . . . ? C5A C6A C7A N8A -172.4(3) . . . . ? C6A C7A N8A N9A 178.9(3) . . . . ? C6A C7A N8A Ca 27.6(4) . . . . ? O10B Ca N8A C7A 89.9(3) . . . . ? O10C Ca N8A C7A 139.3(2) . . . . ? O1C Ca N8A C7A -77.4(3) . . . . ? O10A Ca N8A C7A 173.6(3) . . . . ? O1B Ca N8A C7A -10.5(3) . . . . ? O1A Ca N8A C7A -42.4(2) . . . . ? N8C Ca N8A C7A -147.3(2) . . . . ? N8B Ca N8A C7A 58.9(3) . . . . ? Ti Ca N8A C7A -43.6(3) . . . . ? O10B Ca N8A N9A -62.66(18) . . . . ? O10C Ca N8A N9A -13.2(2) . . . . ? O1C Ca N8A N9A 130.05(17) . . . . ? O10A Ca N8A N9A 21.09(17) . . . . ? O1B Ca N8A N9A -163.05(17) . . . . ? O1A Ca N8A N9A 165.0(2) . . . . ? N8C Ca N8A N9A 60.20(19) . . . . ? N8B Ca N8A N9A -93.61(19) . . . . ? Ti Ca N8A N9A 163.86(17) . . . . ? C7A N8A N9A C10A -175.9(3) . . . . ? Ca N8A N9A C10A -18.3(3) . . . . ? N8A N9A C10A O10A -3.3(4) . . . . ? N8A N9A C10A C11A 176.2(3) . . . . ? N9A C10A O10A Ca 29.8(4) . . . . ? C11A C10A O10A Ca -149.6(2) . . . . ? O10B Ca O10A C10A 44.0(2) . . . . ? O10C Ca O10A C10A 124.6(2) . . . . ? O1C Ca O10A C10A -126.7(2) . . . . ? O1B Ca O10A C10A -55.4(6) . . . . ? O1A Ca O10A C10A -60.1(2) . . . . ? N8C Ca O10A C10A -170.4(2) . . . . ? N8B Ca O10A C10A 77.0(2) . . . . ? N8A Ca O10A C10A -26.8(2) . . . . ? Ti Ca O10A C10A -89.7(2) . . . . ? O10A C10A C11A C12A -161.1(3) . . . . ? N9A C10A C11A C12A 19.4(5) . . . . ? O10A C10A C11A C16A 19.4(4) . . . . ? N9A C10A C11A C16A -160.1(3) . . . . ? C16A C11A C12A C13A 1.3(5) . . . . ? C10A C11A C12A C13A -178.1(3) . . . . ? C11A C12A C13A C14A -0.3(6) . . . . ? C12A C13A C14A C15A 0.1(6) . . . . ? C12A C13A C14A Br1A -179.0(3) . . . . ? C13A C14A C15A C16A -0.9(6) . . . . ? Br1A C14A C15A C16A 178.1(3) . . . . ? C12A C11A C16A C15A -2.2(5) . . . . ? C10A C11A C16A C15A 177.3(3) . . . . ? C14A C15A C16A C11A 2.0(6) . . . . ? O2C Ti O1B C1B 75.6(3) . . . . ? O2A Ti O1B C1B -95.79(19) . . . . ? O2B Ti O1B C1B -4.61(18) . . . . ? O1A Ti O1B C1B -171.96(19) . . . . ? O1C Ti O1B C1B 107.00(19) . . . . ? Ca Ti O1B C1B 146.8(2) . . . . ? O2C Ti O1B Ca -71.1(2) . . . . ? O2A Ti O1B Ca 117.45(8) . . . . ? O2B Ti O1B Ca -151.37(9) . . . . ? O1A Ti O1B Ca 41.28(7) . . . . ? O1C Ti O1B Ca -39.76(8) . . . . ? O10B Ca O1B C1B 87.2(2) . . . . ? O10C Ca O1B C1B 4.0(2) . . . . ? O1C Ca O1B C1B -100.7(2) . . . . ? O10A Ca O1B C1B -176.1(4) . . . . ? O1A Ca O1B C1B -171.0(2) . . . . ? N8C Ca O1B C1B -64.0(2) . . . . ? N8B Ca O1B C1B 48.1(2) . . . . ? N8A Ca O1B C1B 157.3(2) . . . . ? Ti Ca O1B C1B -135.8(3) . . . . ? O10B Ca O1B Ti -136.98(8) . . . . ? O10C Ca O1B Ti 139.84(7) . . . . ? O1C Ca O1B Ti 35.12(7) . . . . ? O10A Ca O1B Ti -40.2(5) . . . . ? O1A Ca O1B Ti -35.17(7) . . . . ? N8C Ca O1B Ti 71.82(9) . . . . ? N8B Ca O1B Ti -176.07(10) . . . . ? N8A Ca O1B Ti -66.89(9) . . . . ? O2C Ti O2B C2B -152.49(19) . . . . ? O2A Ti O2B C2B 108.7(2) . . . . ? O1A Ti O2B C2B 34.7(3) . . . . ? O1C Ti O2B C2B -71.1(2) . . . . ? O1B Ti O2B C2B 2.72(19) . . . . ? Ca Ti O2B C2B -21.2(2) . . . . ? Ti O1B C1B C6B -174.5(2) . . . . ? Ca O1B C1B C6B -44.3(4) . . . . ? Ti O1B C1B C2B 5.6(3) . . . . ? Ca O1B C1B C2B 135.8(2) . . . . ? Ti O2B C2B C3B 177.1(2) . . . . ? Ti O2B C2B C1B -0.5(3) . . . . ? O1B C1B C2B O2B -3.4(3) . . . . ? C6B C1B C2B O2B 176.7(2) . . . . ? O1B C1B C2B C3B 178.9(3) . . . . ? C6B C1B C2B C3B -1.0(4) . . . . ? O2B C2B C3B C4B -176.7(3) . . . . ? C1B C2B C3B C4B 0.8(5) . . . . ? C2B C3B C4B C5B -0.2(5) . . . . ? C3B C4B C5B C6B -0.2(5) . . . . ? O1B C1B C6B C5B -179.2(3) . . . . ? C2B C1B C6B C5B 0.6(4) . . . . ? O1B C1B C6B C7B -2.3(4) . . . . ? C2B C1B C6B C7B 177.6(3) . . . . ? C4B C5B C6B C1B 0.0(5) . . . . ? C4B C5B C6B C7B -177.1(3) . . . . ? C1B C6B C7B N8B 9.8(4) . . . . ? C5B C6B C7B N8B -173.3(3) . . . . ? C6B C7B N8B N9B -173.8(2) . . . . ? C6B C7B N8B Ca 22.1(4) . . . . ? O10B Ca N8B C7B -174.5(3) . . . . ? O10C Ca N8B C7B 98.7(3) . . . . ? O1C Ca N8B C7B -7.7(3) . . . . ? O10A Ca N8B C7B 148.7(3) . . . . ? O1B Ca N8B C7B -37.9(3) . . . . ? O1A Ca N8B C7B -74.6(3) . . . . ? N8C Ca N8B C7B 64.5(3) . . . . ? N8A Ca N8B C7B -142.1(3) . . . . ? Ti Ca N8B C7B -40.3(3) . . . . ? O10B Ca N8B N9B 20.69(16) . . . . ? O10C Ca N8B N9B -66.14(17) . . . . ? O1C Ca N8B N9B -172.48(16) . . . . ? O10A Ca N8B N9B -16.1(2) . . . . ? O1B Ca N8B N9B 157.3(2) . . . . ? O1A Ca N8B N9B 120.60(17) . . . . ? N8C Ca N8B N9B -100.29(18) . . . . ? N8A Ca N8B N9B 53.10(19) . . . . ? Ti Ca N8B N9B 154.94(17) . . . . ? C7B N8B N9B C10B 171.5(3) . . . . ? Ca N8B N9B C10B -20.6(3) . . . . ? N8B N9B C10B O10B 3.1(4) . . . . ? N8B N9B C10B C11B -174.3(2) . . . . ? N9B C10B O10B Ca 22.2(4) . . . . ? C11B C10B O10B Ca -160.5(2) . . . . ? O10C Ca O10B C10B 48.5(2) . . . . ? O1C Ca O10B C10B -97.2(4) . . . . ? O10A Ca O10B C10B 125.5(2) . . . . ? O1B Ca O10B C10B -62.8(2) . . . . ? O1A Ca O10B C10B -128.1(2) . . . . ? N8C Ca O10B C10B 82.4(3) . . . . ? N8B Ca O10B C10B -23.0(2) . . . . ? N8A Ca O10B C10B -171.2(3) . . . . ? Ti Ca O10B C10B -95.5(2) . . . . ? O10B C10B C11B C16B 27.1(5) . . . . ? N9B C10B C11B C16B -155.5(3) . . . . ? O10B C10B C11B C12B -147.7(3) . . . . ? N9B C10B C11B C12B 29.7(4) . . . . ? C16B C11B C12B C13B -0.7(5) . . . . ? C10B C11B C12B C13B 174.0(3) . . . . ? C11B C12B C13B C14B 0.0(5) . . . . ? C12B C13B C14B C15B 1.3(5) . . . . ? C12B C13B C14B Br1B -178.6(3) . . . . ? C13B C14B C15B C16B -1.9(6) . . . . ? Br1B C14B C15B C16B 177.9(3) . . . . ? C12B C11B C16B C15B 0.0(6) . . . . ? C10B C11B C16B C15B -175.0(4) . . . . ? C14B C15B C16B C11B 1.3(6) . . . . ? O2C Ti O1C C1C -4.78(19) . . . . ? O2A Ti O1C C1C 82.9(3) . . . . ? O2B Ti O1C C1C -97.56(19) . . . . ? O1A Ti O1C C1C 105.92(19) . . . . ? O1B Ti O1C C1C -171.8(2) . . . . ? Ca Ti O1C C1C 148.0(2) . . . . ? O2C Ti O1C Ca -152.80(10) . . . . ? O2A Ti O1C Ca -65.1(2) . . . . ? O2B Ti O1C Ca 114.42(9) . . . . ? O1A Ti O1C Ca -42.09(8) . . . . ? O1B Ti O1C Ca 40.14(8) . . . . ? O10B Ca O1C C1C -134.6(4) . . . . ? O10C Ca O1C C1C 82.1(3) . . . . ? O10A Ca O1C C1C -0.8(3) . . . . ? O1B Ca O1C C1C -172.2(3) . . . . ? O1A Ca O1C C1C -100.7(3) . . . . ? N8C Ca O1C C1C 45.8(2) . . . . ? N8B Ca O1C C1C 157.3(2) . . . . ? N8A Ca O1C C1C -65.7(3) . . . . ? Ti Ca O1C C1C -136.7(3) . . . . ? O10B Ca O1C Ti 2.1(4) . . . . ? O10C Ca O1C Ti -141.18(8) . . . . ? O10A Ca O1C Ti 135.93(8) . . . . ? O1B Ca O1C Ti -35.48(7) . . . . ? O1A Ca O1C Ti 35.99(7) . . . . ? N8C Ca O1C Ti -177.50(11) . . . . ? N8B Ca O1C Ti -65.94(10) . . . . ? N8A Ca O1C Ti 71.07(10) . . . . ? O2A Ti O2C C2C -153.2(2) . . . . ? O2B Ti O2C C2C 111.7(2) . . . . ? O1A Ti O2C C2C -71.4(2) . . . . ? O1C Ti O2C C2C 3.9(2) . . . . ? O1B Ti O2C C2C 35.1(3) . . . . ? Ca Ti O2C C2C -18.9(2) . . . . ? Ti O1C C1C C6C -177.4(2) . . . . ? Ca O1C C1C C6C -45.6(4) . . . . ? Ti O1C C1C C2C 4.8(3) . . . . ? Ca O1C C1C C2C 136.6(2) . . . . ? Ti O2C C2C C3C 177.5(3) . . . . ? Ti O2C C2C C1C -2.5(3) . . . . ? O1C C1C C2C O2C -1.7(4) . . . . ? C6C C1C C2C O2C -179.6(3) . . . . ? O1C C1C C2C C3C 178.4(3) . . . . ? C6C C1C C2C C3C 0.5(5) . . . . ? O2C C2C C3C C4C 179.2(3) . . . . ? C1C C2C C3C C4C -0.9(5) . . . . ? C2C C3C C4C C5C 0.2(5) . . . . ? C3C C4C C5C C6C 0.8(6) . . . . ? O1C C1C C6C C5C -177.1(3) . . . . ? C2C C1C C6C C5C 0.6(4) . . . . ? O1C C1C C6C C7C 0.6(5) . . . . ? C2C C1C C6C C7C 178.3(3) . . . . ? C4C C5C C6C C1C -1.2(5) . . . . ? C4C C5C C6C C7C -179.0(3) . . . . ? C1C C6C C7C N8C 12.9(5) . . . . ? C5C C6C C7C N8C -169.4(3) . . . . ? C6C C7C N8C N9C -178.6(3) . . . . ? C6C C7C N8C Ca 11.7(5) . . . . ? O10B Ca N8C C7C 150.9(3) . . . . ? O10C Ca N8C C7C -171.1(3) . . . . ? O1C Ca N8C C7C -29.2(3) . . . . ? O10A Ca N8C C7C 107.0(3) . . . . ? O1B Ca N8C C7C -65.2(3) . . . . ? O1A Ca N8C C7C 2.9(3) . . . . ? N8B Ca N8C C7C -135.0(3) . . . . ? N8A Ca N8C C7C 71.8(3) . . . . ? Ti Ca N8C C7C -30.7(3) . . . . ? O10B Ca N8C N9C -19.2(2) . . . . ? O10C Ca N8C N9C 18.84(17) . . . . ? O1C Ca N8C N9C 160.7(2) . . . . ? O10A Ca N8C N9C -63.09(18) . . . . ? O1B Ca N8C N9C 124.75(18) . . . . ? O1A Ca N8C N9C -167.15(17) . . . . ? N8B Ca N8C N9C 55.0(2) . . . . ? N8A Ca N8C N9C -98.23(19) . . . . ? Ti Ca N8C N9C 159.26(17) . . . . ? C7C N8C N9C C10C 168.4(3) . . . . ? Ca N8C N9C C10C -19.2(3) . . . . ? N8C N9C C10C O10C 2.9(4) . . . . ? N8C N9C C10C C11C -176.9(3) . . . . ? N9C C10C O10C Ca 19.4(4) . . . . ? C11C C10C O10C Ca -160.8(2) . . . . ? O10B Ca O10C C10C 130.4(2) . . . . ? O1C Ca O10C C10C -57.2(2) . . . . ? O10A Ca O10C C10C 55.2(2) . . . . ? O1B Ca O10C C10C -124.8(2) . . . . ? O1A Ca O10C C10C -80.3(7) . . . . ? N8C Ca O10C C10C -20.3(2) . . . . ? N8B Ca O10C C10C -166.5(2) . . . . ? N8A Ca O10C C10C 85.3(2) . . . . ? Ti Ca O10C C10C -90.3(2) . . . . ? O10C C10C C11C C12C 26.4(5) . . . . ? N9C C10C C11C C12C -153.8(3) . . . . ? O10C C10C C11C C16C -151.3(3) . . . . ? N9C C10C C11C C16C 28.5(5) . . . . ? C16C C11C C12C C13C -0.3(6) . . . . ? C10C C11C C12C C13C -178.0(3) . . . . ? C11C C12C C13C C14C 0.9(6) . . . . ? C12C C13C C14C C15C -0.9(6) . . . . ? C12C C13C C14C Br1C 179.7(3) . . . . ? C13C C14C C15C C16C 0.3(6) . . . . ? Br1C C14C C15C C16C 179.6(3) . . . . ? C14C C15C C16C C11C 0.4(6) . . . . ? C12C C11C C16C C15C -0.4(5) . . . . ? C10C C11C C16C C15C 177.3(3) . . . . ? O101 C102 N103 C105 0.2(8) . . . . ? O101 C102 N103 C104 -176.0(5) . . . . ? O111 C112 N113 C114 1.6(6) . . . . ? O111 C112 N113 C115 -177.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.919 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.079 data_fro4809 _database_code_depnum_ccdc_archive 'CCDC 706326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H15 Ca F3 N2 O7 S' _chemical_formula_weight 476.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6605(2) _cell_length_b 15.0299(3) _cell_length_c 12.9695(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.361(1) _cell_angle_gamma 90.00 _cell_volume 2003.82(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2093 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8482 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15558 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4752 _reflns_number_gt 3017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.1980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'at O from difmap, others geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4752 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Ca Ca 0.86780(4) 0.07800(3) 0.95818(4) 0.03351(15) Uani 1 1 d . . . C1 C 0.8802(2) -0.08962(15) 1.13557(19) 0.0326(5) Uani 1 1 d . . . O1 O 0.92857(14) -0.04044(10) 1.07076(13) 0.0336(4) Uani 1 1 d . . . O2 O 1.06731(16) -0.17821(12) 1.16027(15) 0.0453(5) Uani 1 1 d . . . H2 H 1.109(3) -0.214(2) 1.195(3) 0.068 Uiso 1 1 d . . . C2 C 0.9506(2) -0.16441(16) 1.1851(2) 0.0380(6) Uani 1 1 d . . . C3 C 0.9061(3) -0.21971(19) 1.2514(2) 0.0516(7) Uani 1 1 d . . . H3 H 0.9550 -0.2699 1.2812 0.062 Uiso 1 1 calc R . . C4 C 0.7885(3) -0.2018(2) 1.2750(3) 0.0605(9) Uani 1 1 d . . . H4 H 0.7574 -0.2394 1.3206 0.073 Uiso 1 1 calc R . . C5 C 0.7193(2) -0.12868(19) 1.2306(2) 0.0499(7) Uani 1 1 d . . . H5 H 0.6409 -0.1156 1.2476 0.060 Uiso 1 1 calc R . . C6 C 0.7614(2) -0.07245(16) 1.1604(2) 0.0367(6) Uani 1 1 d . . . C7 C 0.6765(2) 0.00172(17) 1.1186(2) 0.0404(6) Uani 1 1 d . . . H7 H 0.6024 0.0083 1.1442 0.048 Uiso 1 1 calc R . . N8 N 0.69199(18) 0.05912(13) 1.05036(16) 0.0337(5) Uani 1 1 d . . . N9 N 0.59695(19) 0.12533(15) 1.02556(18) 0.0378(5) Uani 1 1 d . . . H9 H 0.549(3) 0.1251(18) 1.058(2) 0.045 Uiso 1 1 d . . . C10 C 0.6114(2) 0.19050(17) 0.9595(2) 0.0380(6) Uani 1 1 d . . . O11 O 0.70207(16) 0.18838(12) 0.91687(15) 0.0517(5) Uani 1 1 d . . . C12 C 0.5179(2) 0.26665(17) 0.9420(2) 0.0406(6) Uani 1 1 d . . . C13 C 0.4083(3) 0.2682(2) 0.9804(2) 0.0567(8) Uani 1 1 d . . . H13 H 0.3876 0.2187 1.0171 0.068 Uiso 1 1 calc R . . C14 C 0.3296(3) 0.3424(2) 0.9646(3) 0.0720(10) Uani 1 1 d . . . H14 H 0.2559 0.3437 0.9914 0.086 Uiso 1 1 calc R . . C15 C 0.3584(3) 0.4144(2) 0.9097(3) 0.0771(11) Uani 1 1 d . . . H15 H 0.3037 0.4645 0.8984 0.093 Uiso 1 1 calc R . . C16 C 0.4670(3) 0.4135(2) 0.8712(3) 0.0715(10) Uani 1 1 d . . . H16 H 0.4869 0.4629 0.8339 0.086 Uiso 1 1 calc R . . C17 C 0.5463(3) 0.3395(2) 0.8878(2) 0.0554(8) Uani 1 1 d . . . H17 H 0.6206 0.3387 0.8618 0.066 Uiso 1 1 calc R . . O21 O 0.9813(2) 0.16841(13) 1.10272(17) 0.0581(6) Uani 1 1 d . . . H21 H 1.031(4) 0.141(3) 1.144(3) 0.087 Uiso 1 1 d . . . C22 C 1.0068(3) 0.2600(2) 1.1082(3) 0.0672(9) Uani 1 1 d . . . H22A H 1.0760 0.2728 1.0746 0.101 Uiso 1 1 calc R . . H22B H 1.0333 0.2784 1.1825 0.101 Uiso 1 1 calc R . . H22C H 0.9289 0.2920 1.0714 0.101 Uiso 1 1 calc R . . S1 S 0.67742(6) -0.08520(4) 0.78167(5) 0.03642(18) Uani 1 1 d . . . O101 O 0.78712(18) -0.02730(14) 0.81589(16) 0.0592(6) Uani 1 1 d . . . O102 O 0.71204(17) -0.17337(12) 0.75705(16) 0.0529(5) Uani 1 1 d . . . O103 O 0.58636(18) -0.08154(12) 0.84432(17) 0.0544(5) Uani 1 1 d . . . C31 C 0.5913(3) -0.0400(2) 0.6532(3) 0.0599(8) Uani 1 1 d . . . F101 F 0.5507(3) 0.04065(16) 0.66338(19) 0.1117(8) Uani 1 1 d . . . F102 F 0.4883(2) -0.08873(17) 0.60985(18) 0.1107(9) Uani 1 1 d . . . F103 F 0.6636(2) -0.03717(18) 0.58681(16) 0.0991(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0312(3) 0.0307(3) 0.0414(3) 0.0044(2) 0.0146(2) 0.00368(19) C1 0.0341(12) 0.0311(13) 0.0336(13) 0.0021(11) 0.0106(10) 0.0004(10) O1 0.0336(8) 0.0288(9) 0.0418(10) 0.0057(8) 0.0161(7) 0.0012(6) O2 0.0385(10) 0.0452(12) 0.0578(13) 0.0205(9) 0.0228(8) 0.0141(8) C2 0.0347(13) 0.0374(15) 0.0460(15) 0.0089(12) 0.0179(11) 0.0053(10) C3 0.0508(15) 0.0475(17) 0.0637(19) 0.0266(15) 0.0278(14) 0.0149(13) C4 0.0571(17) 0.061(2) 0.074(2) 0.0363(17) 0.0376(15) 0.0158(15) C5 0.0431(14) 0.0534(19) 0.0624(19) 0.0190(15) 0.0304(13) 0.0121(13) C6 0.0376(13) 0.0348(14) 0.0418(15) 0.0039(11) 0.0175(11) 0.0038(10) C7 0.0359(13) 0.0404(15) 0.0505(17) 0.0059(13) 0.0214(11) 0.0042(10) N8 0.0314(10) 0.0317(11) 0.0399(12) 0.0019(9) 0.0128(8) 0.0061(8) N9 0.0336(11) 0.0385(13) 0.0470(13) 0.0084(11) 0.0206(9) 0.0091(9) C10 0.0329(12) 0.0408(15) 0.0414(15) 0.0045(12) 0.0121(10) 0.0045(10) O11 0.0469(10) 0.0498(12) 0.0672(13) 0.0222(10) 0.0305(9) 0.0158(8) C12 0.0388(13) 0.0407(15) 0.0417(15) 0.0054(12) 0.0098(11) 0.0093(11) C13 0.0468(15) 0.058(2) 0.071(2) 0.0209(16) 0.0261(14) 0.0172(13) C14 0.0555(18) 0.078(2) 0.092(3) 0.026(2) 0.0354(17) 0.0340(17) C15 0.076(2) 0.061(2) 0.099(3) 0.022(2) 0.031(2) 0.0366(17) C16 0.076(2) 0.050(2) 0.096(3) 0.0284(19) 0.0354(19) 0.0202(16) C17 0.0509(16) 0.0538(19) 0.067(2) 0.0179(16) 0.0245(14) 0.0141(13) O21 0.0707(14) 0.0379(12) 0.0558(14) -0.0025(10) -0.0005(10) 0.0079(9) C22 0.071(2) 0.0431(19) 0.086(3) -0.0073(17) 0.0182(17) -0.0079(15) S1 0.0338(3) 0.0364(4) 0.0403(4) -0.0034(3) 0.0119(3) -0.0030(2) O101 0.0559(12) 0.0599(14) 0.0587(13) -0.0105(10) 0.0098(9) -0.0265(9) O102 0.0548(11) 0.0373(11) 0.0700(14) -0.0078(10) 0.0226(9) 0.0045(8) O103 0.0545(11) 0.0536(13) 0.0649(13) -0.0009(10) 0.0327(10) 0.0054(9) C31 0.0529(18) 0.063(2) 0.061(2) 0.0043(17) 0.0093(15) 0.0059(15) F101 0.154(2) 0.0767(16) 0.1012(18) 0.0316(13) 0.0272(15) 0.0568(15) F102 0.0762(14) 0.139(2) 0.0884(17) 0.0108(14) -0.0281(12) -0.0224(13) F103 0.1062(16) 0.141(2) 0.0563(13) 0.0266(14) 0.0319(11) 0.0129(14) _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 O1 2.2845(16) . ? Ca O1 2.3672(15) 3_757 ? Ca O21 2.371(2) . ? Ca O11 2.3790(17) . ? Ca O2 2.3811(18) 3_757 ? Ca O101 2.4103(19) . ? Ca N8 2.492(2) . ? Ca C10 3.218(2) . ? Ca C1 3.234(2) 3_757 ? Ca Ca 3.6053(9) 3_757 ? C1 O1 1.322(3) . ? C1 C2 1.409(3) . ? C1 C6 1.411(3) . ? C1 Ca 3.234(2) 3_757 ? O1 Ca 2.3672(15) 3_757 ? O2 C2 1.381(3) . ? O2 Ca 2.3811(18) 3_757 ? C2 C3 1.368(3) . ? C3 C4 1.393(4) . ? C4 C5 1.363(4) . ? C5 C6 1.399(3) . ? C6 C7 1.448(3) . ? C7 N8 1.277(3) . ? N8 N9 1.396(3) . ? N9 C10 1.336(3) . ? C10 O11 1.235(3) . ? C10 C12 1.494(3) . ? C12 C17 1.377(4) . ? C12 C13 1.387(4) . ? C13 C14 1.378(4) . ? C14 C15 1.374(5) . ? C15 C16 1.378(5) . ? C16 C17 1.379(4) . ? O21 C22 1.401(3) . ? S1 O103 1.4225(19) . ? S1 O101 1.4307(18) . ? S1 O102 1.4341(18) . ? S1 C31 1.808(3) . ? C31 F103 1.300(4) . ? C31 F101 1.306(4) . ? C31 F102 1.316(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ca O1 78.39(6) . 3_757 ? O1 Ca O21 86.70(7) . . ? O1 Ca O21 87.98(7) 3_757 . ? O1 Ca O11 139.05(6) . . ? O1 Ca O11 142.01(6) 3_757 . ? O21 Ca O11 88.36(7) . . ? O1 Ca O2 145.44(6) . 3_757 ? O1 Ca O2 67.25(6) 3_757 3_757 ? O21 Ca O2 88.45(8) . 3_757 ? O11 Ca O2 74.87(6) . 3_757 ? O1 Ca O101 87.76(7) . . ? O1 Ca O101 83.01(6) 3_757 . ? O21 Ca O101 170.22(7) . . ? O11 Ca O101 101.09(7) . . ? O2 Ca O101 91.55(7) 3_757 . ? O1 Ca N8 74.13(6) . . ? O1 Ca N8 152.47(6) 3_757 . ? O21 Ca N8 88.68(7) . . ? O11 Ca N8 65.13(6) . . ? O2 Ca N8 139.95(6) 3_757 . ? O101 Ca N8 97.55(7) . . ? O1 Ca C10 120.22(6) . . ? O1 Ca C10 160.41(6) 3_757 . ? O21 Ca C10 87.18(7) . . ? O11 Ca C10 18.85(6) . . ? O2 Ca C10 93.64(6) 3_757 . ? O101 Ca C10 102.58(7) . . ? N8 Ca C10 46.32(6) . . ? O1 Ca C1 99.16(6) . 3_757 ? O1 Ca C1 20.80(6) 3_757 3_757 ? O21 Ca C1 88.03(7) . 3_757 ? O11 Ca C1 121.27(6) . 3_757 ? O2 Ca C1 46.45(6) 3_757 3_757 ? O101 Ca C1 84.90(6) . 3_757 ? N8 Ca C1 172.70(6) . 3_757 ? C10 Ca C1 139.92(6) . 3_757 ? O1 Ca Ca 40.03(4) . 3_757 ? O1 Ca Ca 38.37(4) 3_757 3_757 ? O21 Ca Ca 86.58(5) . 3_757 ? O11 Ca Ca 174.91(6) . 3_757 ? O2 Ca Ca 105.54(4) 3_757 3_757 ? O101 Ca Ca 83.99(5) . 3_757 ? N8 Ca Ca 114.14(5) . 3_757 ? C10 Ca Ca 159.64(5) . 3_757 ? C1 Ca Ca 59.14(4) 3_757 3_757 ? O1 C1 C2 119.1(2) . . ? O1 C1 C6 124.6(2) . . ? C2 C1 C6 116.3(2) . . ? O1 C1 Ca 39.47(10) . 3_757 ? C2 C1 Ca 79.60(13) . 3_757 ? C6 C1 Ca 164.03(17) . 3_757 ? C1 O1 Ca 138.55(14) . . ? C1 O1 Ca 119.73(14) . 3_757 ? Ca O1 Ca 101.61(6) . 3_757 ? C2 O2 Ca 119.30(14) . 3_757 ? C3 C2 O2 122.6(2) . . ? C3 C2 C1 122.7(2) . . ? O2 C2 C1 114.7(2) . . ? C2 C3 C4 120.1(2) . . ? C5 C4 C3 118.7(3) . . ? C4 C5 C6 122.1(2) . . ? C5 C6 C1 120.0(2) . . ? C5 C6 C7 115.6(2) . . ? C1 C6 C7 124.4(2) . . ? N8 C7 C6 126.7(2) . . ? C7 N8 N9 114.98(19) . . ? C7 N8 Ca 131.35(15) . . ? N9 N8 Ca 113.61(14) . . ? C10 N9 N8 118.08(19) . . ? O11 C10 N9 120.3(2) . . ? O11 C10 C12 121.4(2) . . ? N9 C10 C12 118.3(2) . . ? O11 C10 Ca 38.48(11) . . ? N9 C10 Ca 81.97(13) . . ? C12 C10 Ca 159.13(17) . . ? C10 O11 Ca 122.67(16) . . ? C17 C12 C13 119.3(2) . . ? C17 C12 C10 117.3(2) . . ? C13 C12 C10 123.3(2) . . ? C14 C13 C12 119.9(3) . . ? C15 C14 C13 120.3(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C17 119.3(3) . . ? C12 C17 C16 120.9(3) . . ? C22 O21 Ca 130.9(2) . . ? O103 S1 O101 115.13(12) . . ? O103 S1 O102 114.70(11) . . ? O101 S1 O102 113.18(12) . . ? O103 S1 C31 104.77(13) . . ? O101 S1 C31 103.36(14) . . ? O102 S1 C31 103.88(14) . . ? S1 O101 Ca 137.18(12) . . ? F103 C31 F101 107.9(3) . . ? F103 C31 F102 108.0(3) . . ? F101 C31 F102 107.4(3) . . ? F103 C31 S1 112.2(2) . . ? F101 C31 S1 110.9(2) . . ? F102 C31 S1 110.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 O1 Ca 174.44(17) . . . . ? C6 C1 O1 Ca -6.1(4) . . . . ? Ca C1 O1 Ca 175.3(3) 3_757 . . . ? C2 C1 O1 Ca -0.8(3) . . . 3_757 ? C6 C1 O1 Ca 178.61(18) . . . 3_757 ? O1 Ca O1 C1 -175.8(3) 3_757 . . . ? O21 Ca O1 C1 95.6(2) . . . . ? O11 Ca O1 C1 11.9(3) . . . . ? O2 Ca O1 C1 178.0(2) 3_757 . . . ? O101 Ca O1 C1 -92.5(2) . . . . ? N8 Ca O1 C1 6.0(2) . . . . ? C10 Ca O1 C1 10.8(2) . . . . ? C1 Ca O1 C1 -176.95(19) 3_757 . . . ? Ca Ca O1 C1 -175.8(3) 3_757 . . . ? O1 Ca O1 Ca 0.0 3_757 . . 3_757 ? O21 Ca O1 Ca -88.62(8) . . . 3_757 ? O11 Ca O1 Ca -172.28(9) . . . 3_757 ? O2 Ca O1 Ca -6.17(14) 3_757 . . 3_757 ? O101 Ca O1 Ca 83.32(7) . . . 3_757 ? N8 Ca O1 Ca -178.19(8) . . . 3_757 ? C10 Ca O1 Ca -173.41(6) . . . 3_757 ? C1 Ca O1 Ca -1.15(7) 3_757 . . 3_757 ? Ca O2 C2 C3 179.1(2) 3_757 . . . ? Ca O2 C2 C1 0.1(3) 3_757 . . . ? O1 C1 C2 C3 -178.6(2) . . . . ? C6 C1 C2 C3 1.9(4) . . . . ? Ca C1 C2 C3 -179.1(3) 3_757 . . . ? O1 C1 C2 O2 0.5(3) . . . . ? C6 C1 C2 O2 -179.0(2) . . . . ? Ca C1 C2 O2 -0.04(19) 3_757 . . . ? O2 C2 C3 C4 179.1(3) . . . . ? C1 C2 C3 C4 -1.9(5) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 C6 1.5(5) . . . . ? C4 C5 C6 C1 -1.4(5) . . . . ? C4 C5 C6 C7 179.1(3) . . . . ? O1 C1 C6 C5 -179.7(2) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? Ca C1 C6 C5 -176.5(5) 3_757 . . . ? O1 C1 C6 C7 -0.3(4) . . . . ? C2 C1 C6 C7 179.2(2) . . . . ? Ca C1 C6 C7 3.0(8) 3_757 . . . ? C5 C6 C7 N8 -176.8(3) . . . . ? C1 C6 C7 N8 3.7(4) . . . . ? C6 C7 N8 N9 -178.5(2) . . . . ? C6 C7 N8 Ca -1.4(4) . . . . ? O1 Ca N8 C7 -2.1(2) . . . . ? O1 Ca N8 C7 -5.9(3) 3_757 . . . ? O21 Ca N8 C7 -89.0(2) . . . . ? O11 Ca N8 C7 -177.8(2) . . . . ? O2 Ca N8 C7 -175.1(2) 3_757 . . . ? O101 Ca N8 C7 83.4(2) . . . . ? C10 Ca N8 C7 -176.4(3) . . . . ? C1 Ca N8 C7 -25.8(6) 3_757 . . . ? Ca Ca N8 C7 -3.4(2) 3_757 . . . ? O1 Ca N8 N9 175.06(17) . . . . ? O1 Ca N8 N9 171.21(14) 3_757 . . . ? O21 Ca N8 N9 88.12(16) . . . . ? O11 Ca N8 N9 -0.68(15) . . . . ? O2 Ca N8 N9 2.1(2) 3_757 . . . ? O101 Ca N8 N9 -99.45(16) . . . . ? C10 Ca N8 N9 0.77(14) . . . . ? C1 Ca N8 N9 151.4(4) 3_757 . . . ? Ca Ca N8 N9 173.78(14) 3_757 . . . ? C7 N8 N9 C10 176.1(2) . . . . ? Ca N8 N9 C10 -1.5(3) . . . . ? N8 N9 C10 O11 4.5(4) . . . . ? N8 N9 C10 C12 -173.5(2) . . . . ? N8 N9 C10 Ca 1.08(19) . . . . ? O1 Ca C10 O11 177.70(19) . . . . ? O1 Ca C10 O11 17.3(3) 3_757 . . . ? O21 Ca C10 O11 93.2(2) . . . . ? O2 Ca C10 O11 4.9(2) 3_757 . . . ? O101 Ca C10 O11 -87.5(2) . . . . ? N8 Ca C10 O11 -175.9(2) . . . . ? C1 Ca C10 O11 9.6(2) 3_757 . . . ? Ca Ca C10 O11 165.46(17) 3_757 . . . ? O1 Ca C10 N9 -7.09(17) . . . . ? O1 Ca C10 N9 -167.52(17) 3_757 . . . ? O21 Ca C10 N9 -91.61(15) . . . . ? O11 Ca C10 N9 175.2(3) . . . . ? O2 Ca C10 N9 -179.88(15) 3_757 . . . ? O101 Ca C10 N9 87.71(15) . . . . ? N8 Ca C10 N9 -0.74(13) . . . . ? C1 Ca C10 N9 -175.18(13) 3_757 . . . ? Ca Ca C10 N9 -19.3(3) 3_757 . . . ? O1 Ca C10 C12 159.4(5) . . . . ? O1 Ca C10 C12 -1.0(6) 3_757 . . . ? O21 Ca C10 C12 74.9(5) . . . . ? O11 Ca C10 C12 -18.3(4) . . . . ? O2 Ca C10 C12 -13.4(5) 3_757 . . . ? O101 Ca C10 C12 -105.8(5) . . . . ? N8 Ca C10 C12 165.7(5) . . . . ? C1 Ca C10 C12 -8.7(5) 3_757 . . . ? Ca Ca C10 C12 147.1(4) 3_757 . . . ? N9 C10 O11 Ca -5.5(3) . . . . ? C12 C10 O11 Ca 172.46(17) . . . . ? O1 Ca O11 C10 -3.0(3) . . . . ? O1 Ca O11 C10 -170.69(18) 3_757 . . . ? O21 Ca O11 C10 -86.1(2) . . . . ? O2 Ca O11 C10 -174.9(2) 3_757 . . . ? O101 Ca O11 C10 96.5(2) . . . . ? N8 Ca O11 C10 3.23(19) . . . . ? C1 Ca O11 C10 -172.77(19) 3_757 . . . ? Ca Ca O11 C10 -79.7(6) 3_757 . . . ? O11 C10 C12 C17 -8.1(4) . . . . ? N9 C10 C12 C17 169.9(2) . . . . ? Ca C10 C12 C17 5.2(6) . . . . ? O11 C10 C12 C13 174.0(3) . . . . ? N9 C10 C12 C13 -8.0(4) . . . . ? Ca C10 C12 C13 -172.7(4) . . . . ? C17 C12 C13 C14 -0.4(5) . . . . ? C10 C12 C13 C14 177.4(3) . . . . ? C12 C13 C14 C15 0.9(6) . . . . ? C13 C14 C15 C16 -0.8(6) . . . . ? C14 C15 C16 C17 0.3(6) . . . . ? C13 C12 C17 C16 -0.1(5) . . . . ? C10 C12 C17 C16 -178.1(3) . . . . ? C15 C16 C17 C12 0.2(5) . . . . ? O1 Ca O21 C22 175.4(3) . . . . ? O1 Ca O21 C22 96.9(3) 3_757 . . . ? O11 Ca O21 C22 -45.2(3) . . . . ? O2 Ca O21 C22 29.7(3) 3_757 . . . ? O101 Ca O21 C22 119.8(4) . . . . ? N8 Ca O21 C22 -110.4(3) . . . . ? C10 Ca O21 C22 -64.1(3) . . . . ? C1 Ca O21 C22 76.1(3) 3_757 . . . ? Ca Ca O21 C22 135.3(3) 3_757 . . . ? O103 S1 O101 Ca 1.5(2) . . . . ? O102 S1 O101 Ca -133.21(17) . . . . ? C31 S1 O101 Ca 115.1(2) . . . . ? O1 Ca O101 S1 74.89(19) . . . . ? O1 Ca O101 S1 153.5(2) 3_757 . . . ? O21 Ca O101 S1 130.4(4) . . . . ? O11 Ca O101 S1 -64.8(2) . . . . ? O2 Ca O101 S1 -139.68(19) 3_757 . . . ? N8 Ca O101 S1 1.2(2) . . . . ? C10 Ca O101 S1 -45.6(2) . . . . ? C1 Ca O101 S1 174.30(19) 3_757 . . . ? Ca Ca O101 S1 114.86(19) 3_757 . . . ? O103 S1 C31 F103 178.7(2) . . . . ? O101 S1 C31 F103 57.7(3) . . . . ? O102 S1 C31 F103 -60.7(3) . . . . ? O103 S1 C31 F101 58.0(3) . . . . ? O101 S1 C31 F101 -63.0(3) . . . . ? O102 S1 C31 F101 178.6(2) . . . . ? O103 S1 C31 F102 -60.9(3) . . . . ? O101 S1 C31 F102 178.2(2) . . . . ? O102 S1 C31 F102 59.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.281 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.059 #====================================================================== _eof