# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mountford, Philip' _publ_contact_author_email philip.mountford@chem.ox.ac.uk _publ_section_title ; Cationic and charge-neutral calcium tetrahydroborate complexes and their use in the controlled ring-opening polymerisation of rac-lactide ; _publ_author_name P.Mountford # Attachment '- Mountford Xray SI.CIF' data_COMPOUND_1-BPh4 _database_code_depnum_ccdc_archive 'CCDC 796412' #TrackingRef '- Mountford Xray SI.CIF' # Local code MGC61 _chemical_name_systematic ; [Ca(BH4)(THF)5][BPh4] ; _chemical_melting_point ? _publ_section_exptl_refinement ; B-bound H atoms were located from a Fourier difference map and positionally and isotropically refined. Similarity restraints were applied to the bridging B(1)-H distances and the H(1)-B(1)-H angles. A common u[iso] was refined for the found B-bound H atoms. Other H atoms were placed in calculated positions and refined in a riding model. ; _cell_length_a 9.6080(2) _cell_length_b 14.8383(3) _cell_length_c 15.2496(3) _cell_angle_alpha 94.1835(10) _cell_angle_beta 103.4250(9) _cell_angle_gamma 92.0870(10) _cell_volume 2105.85(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Ca 0.2262 0.3064 8.6266 10.4421 7.3873 0.6599 1.5899 85.7484 1.0211 178.4370 1.3751 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C44 H64 B2 Ca1 O5' _chemical_formula_moiety 'C20 H44 B1 Ca1 O5, C24 H20 B1' _chemical_compound_source ? _chemical_formula_weight 734.69 _cell_measurement_reflns_used 8531 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15200 _reflns_number_total 9500 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 5.114 _diffrn_reflns_theta_max 27.476 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.377 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 3.00 _oxford_diffrn_Wilson_scale 2.76 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.72 _refine_diff_density_max 1.16 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 6134 _refine_ls_number_restraints 45 _refine_ls_number_parameters 482 _oxford_refine_ls_R_factor_ref 0.0723 _refine_ls_wR_factor_ref 0.0815 _refine_ls_goodness_of_fit_ref 1.1028 _refine_ls_shift/su_max 0.004605 # The values computed from all data _oxford_reflns_number_all 9500 _refine_ls_R_factor_all 0.1082 _refine_ls_wR_factor_all 0.1119 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6818 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_gt 0.0858 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.70 1.39 1.34 0.250 0.256 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ca1 Ca 0.17178(6) 0.21733(4) 0.19228(4) 0.0325 1.0000 Uani D U . . . . . B1 B -0.0986(4) 0.1641(3) 0.1598(3) 0.0465 1.0000 Uani D . . . . . . B2 B 0.5026(3) 0.7347(2) 0.2961(2) 0.0308 1.0000 Uani . . . . . . . O1 O 0.2711(3) 0.1010(2) 0.11708(18) 0.0650 1.0000 Uani . U . . . . . O2 O 0.2337(2) 0.14218(15) 0.32682(13) 0.0400 1.0000 Uani . . . . . . . O3 O 0.1447(2) 0.35841(15) 0.26887(15) 0.0399 1.0000 Uani . . . . . . . O4 O 0.1595(2) 0.29237(18) 0.05527(14) 0.0476 1.0000 Uani . . . . . . . O5 O 0.41818(19) 0.27187(15) 0.23633(13) 0.0372 1.0000 Uani . . . . . . . C1 C 0.4101(4) 0.0651(4) 0.1505(4) 0.0850 1.0000 Uani . U . . . . . C2 C 0.3916(8) -0.0245(5) 0.1244(5) 0.1321 1.0000 Uani . U . . . . . C3 C 0.2309(7) -0.0456(4) 0.0780(4) 0.0995 1.0000 Uani . U . . . . . C4 C 0.1997(5) 0.0363(3) 0.0443(3) 0.0676 1.0000 Uani . U . . . . . C5 C 0.2385(5) 0.1821(3) 0.4164(2) 0.0575 1.0000 Uani . . . . . . . C6 C 0.1398(4) 0.1246(3) 0.4526(2) 0.0566 1.0000 Uani . . . . . . . C7 C 0.1398(7) 0.0350(3) 0.4100(3) 0.0829 1.0000 Uani . . . . . . . C8 C 0.2007(5) 0.0459(3) 0.3268(3) 0.0605 1.0000 Uani . . . . . . . C9 C 0.0157(3) 0.3843(2) 0.2959(2) 0.0471 1.0000 Uani . . . . . . . C10 C -0.0087(4) 0.4769(2) 0.2643(2) 0.0487 1.0000 Uani . . . . . . . C11 C 0.1445(4) 0.5194(2) 0.2841(3) 0.0485 1.0000 Uani . . . . . . . C12 C 0.2388(4) 0.4402(2) 0.2856(3) 0.0534 1.0000 Uani . . . . . . . C13 C 0.1957(5) 0.2614(3) -0.0288(2) 0.0591 1.0000 Uani . . . . . . . C14 C 0.1792(5) 0.3409(3) -0.0836(2) 0.0632 1.0000 Uani . . . . . . . C15 C 0.0598(6) 0.3885(3) -0.0549(3) 0.0683 1.0000 Uani . . . . . . . C16 C 0.0731(5) 0.3710(3) 0.0404(3) 0.0683 1.0000 Uani . . . . . . . C17 C 0.4953(3) 0.3078(3) 0.1739(2) 0.0560 1.0000 Uani . . . . . . . C18 C 0.6297(3) 0.3550(3) 0.2315(3) 0.0566 1.0000 Uani . . . . . . . C19 C 0.6629(3) 0.2987(3) 0.3117(2) 0.0473 1.0000 Uani . . . . . . . C20 C 0.5151(3) 0.2725(2) 0.3244(2) 0.0395 1.0000 Uani . . . . . . . C21 C 0.5848(3) 0.8354(2) 0.30026(19) 0.0341 1.0000 Uani . . . . . . . C22 C 0.5608(3) 0.9094(2) 0.3567(2) 0.0432 1.0000 Uani . . . . . . . C23 C 0.6316(4) 0.9938(2) 0.3618(3) 0.0553 1.0000 Uani . . . . . . . C24 C 0.7306(4) 1.0073(3) 0.3096(3) 0.0610 1.0000 Uani . . . . . . . C25 C 0.7573(4) 0.9363(3) 0.2537(3) 0.0538 1.0000 Uani . . . . . . . C26 C 0.6858(3) 0.8520(2) 0.2493(2) 0.0432 1.0000 Uani . . . . . . . C27 C 0.6088(3) 0.66806(19) 0.36035(17) 0.0303 1.0000 Uani . . . . . . . C28 C 0.7585(3) 0.6781(2) 0.37727(18) 0.0327 1.0000 Uani . . . . . . . C29 C 0.8492(3) 0.6182(2) 0.4257(2) 0.0383 1.0000 Uani . . . . . . . C30 C 0.7920(3) 0.5443(2) 0.4587(2) 0.0389 1.0000 Uani . . . . . . . C31 C 0.6450(3) 0.5323(2) 0.4438(2) 0.0406 1.0000 Uani . . . . . . . C32 C 0.5558(3) 0.5934(2) 0.39660(19) 0.0367 1.0000 Uani . . . . . . . C33 C 0.4614(3) 0.6865(2) 0.19146(18) 0.0331 1.0000 Uani . . . . . . . C34 C 0.4130(3) 0.7369(2) 0.1165(2) 0.0420 1.0000 Uani . . . . . . . C35 C 0.3631(4) 0.6970(3) 0.0286(2) 0.0496 1.0000 Uani . . . . . . . C36 C 0.3602(4) 0.6044(3) 0.0117(2) 0.0506 1.0000 Uani . . . . . . . C37 C 0.4098(4) 0.5524(3) 0.0826(2) 0.0515 1.0000 Uani . . . . . . . C38 C 0.4590(3) 0.5939(2) 0.1707(2) 0.0412 1.0000 Uani . . . . . . . C39 C 0.3544(3) 0.7494(2) 0.32983(19) 0.0329 1.0000 Uani . . . . . . . C40 C 0.3500(3) 0.7539(2) 0.4214(2) 0.0423 1.0000 Uani . . . . . . . C41 C 0.2287(4) 0.7768(3) 0.4513(2) 0.0497 1.0000 Uani . . . . . . . C42 C 0.1054(3) 0.7959(2) 0.3906(3) 0.0496 1.0000 Uani . . . . . . . C43 C 0.1040(3) 0.7915(2) 0.2999(3) 0.0481 1.0000 Uani . . . . . . . C44 C 0.2263(3) 0.7688(2) 0.2705(2) 0.0390 1.0000 Uani . . . . . . . H1 H -0.221(5) 0.1404(15) 0.1453(13) 0.075(7) 1.0000 Uiso D . . . . . . H2 H -0.0827(11) 0.2344(17) 0.128(3) 0.075(7) 1.0000 Uiso D . . . . . . H3 H -0.0491(16) 0.182(3) 0.2396(8) 0.075(7) 1.0000 Uiso D . . . . . . H4 H -0.0302(14) 0.1085(15) 0.129(3) 0.075(7) 1.0000 Uiso D . . . . . . H11 H 0.4382 0.0752 0.2145 0.0969 1.0000 Uiso R . . . . . . H12 H 0.4811 0.0917 0.1248 0.0969 1.0000 Uiso R . . . . . . H21 H 0.4155 -0.0582 0.1760 0.1260 1.0000 Uiso R . . . . . . H22 H 0.4499 -0.0409 0.0840 0.1260 1.0000 Uiso R . . . . . . H31 H 0.2181 -0.0933 0.0312 0.1116 1.0000 Uiso R . . . . . . H32 H 0.1745 -0.0596 0.1193 0.1116 1.0000 Uiso R . . . . . . H41 H 0.2369 0.0424 -0.0076 0.0782 1.0000 Uiso R . . . . . . H42 H 0.0994 0.0436 0.0292 0.0782 1.0000 Uiso R . . . . . . H51 H 0.2084 0.2424 0.4140 0.0715 1.0000 Uiso R . . . . . . H52 H 0.3330 0.1824 0.4532 0.0715 1.0000 Uiso R . . . . . . H61 H 0.1716 0.1248 0.5164 0.0691 1.0000 Uiso R . . . . . . H62 H 0.0459 0.1460 0.4378 0.0691 1.0000 Uiso R . . . . . . H71 H 0.0455 0.0076 0.3928 0.1010 1.0000 Uiso R . . . . . . H72 H 0.1996 -0.0012 0.4503 0.1010 1.0000 Uiso R . . . . . . H81 H 0.1311 0.0247 0.2734 0.0762 1.0000 Uiso R . . . . . . H82 H 0.2847 0.0132 0.3303 0.0762 1.0000 Uiso R . . . . . . H91 H 0.0290 0.3857 0.3597 0.0584 1.0000 Uiso R . . . . . . H92 H -0.0628 0.3433 0.2675 0.0584 1.0000 Uiso R . . . . . . H101 H -0.0658 0.5097 0.2974 0.0596 1.0000 Uiso R . . . . . . H102 H -0.0530 0.4740 0.2015 0.0596 1.0000 Uiso R . . . . . . H111 H 0.1557 0.5566 0.2378 0.0588 1.0000 Uiso R . . . . . . H112 H 0.1670 0.5542 0.3408 0.0588 1.0000 Uiso R . . . . . . H121 H 0.3033 0.4408 0.3432 0.0643 1.0000 Uiso R . . . . . . H122 H 0.2914 0.4429 0.2402 0.0643 1.0000 Uiso R . . . . . . H131 H 0.2912 0.2425 -0.0178 0.0748 1.0000 Uiso R . . . . . . H132 H 0.1316 0.2126 -0.0591 0.0748 1.0000 Uiso R . . . . . . H141 H 0.1549 0.3227 -0.1466 0.0785 1.0000 Uiso R . . . . . . H142 H 0.2648 0.3786 -0.0694 0.0785 1.0000 Uiso R . . . . . . H151 H 0.0690 0.4517 -0.0604 0.0866 1.0000 Uiso R . . . . . . H152 H -0.0301 0.3647 -0.0910 0.0866 1.0000 Uiso R . . . . . . H161 H -0.0188 0.3580 0.0511 0.0954 1.0000 Uiso R . . . . . . H162 H 0.1184 0.4219 0.0792 0.0954 1.0000 Uiso R . . . . . . H171 H 0.5185 0.2598 0.1360 0.0722 1.0000 Uiso R . . . . . . H172 H 0.4391 0.3489 0.1376 0.0722 1.0000 Uiso R . . . . . . H181 H 0.6131 0.4155 0.2499 0.0706 1.0000 Uiso R . . . . . . H182 H 0.7051 0.3553 0.2008 0.0706 1.0000 Uiso R . . . . . . H191 H 0.7112 0.2466 0.2983 0.0583 1.0000 Uiso R . . . . . . H192 H 0.7196 0.3327 0.3638 0.0583 1.0000 Uiso R . . . . . . H201 H 0.4886 0.3156 0.3658 0.0481 1.0000 Uiso R . . . . . . H202 H 0.5142 0.2142 0.3464 0.0481 1.0000 Uiso R . . . . . . H221 H 0.4941 0.9015 0.3931 0.0513 1.0000 Uiso R . . . . . . H231 H 0.6123 1.0424 0.4005 0.0642 1.0000 Uiso R . . . . . . H241 H 0.7791 1.0648 0.3125 0.0729 1.0000 Uiso R . . . . . . H251 H 0.8244 0.9450 0.2177 0.0656 1.0000 Uiso R . . . . . . H261 H 0.7070 0.8037 0.2110 0.0528 1.0000 Uiso R . . . . . . H281 H 0.8000 0.7280 0.3549 0.0391 1.0000 Uiso R . . . . . . H291 H 0.9502 0.6279 0.4363 0.0462 1.0000 Uiso R . . . . . . H301 H 0.8526 0.5025 0.4910 0.0474 1.0000 Uiso R . . . . . . H311 H 0.6042 0.4819 0.4660 0.0493 1.0000 Uiso R . . . . . . H321 H 0.4551 0.5840 0.3884 0.0442 1.0000 Uiso R . . . . . . H341 H 0.4151 0.8009 0.1264 0.0515 1.0000 Uiso R . . . . . . H351 H 0.3305 0.7337 -0.0197 0.0606 1.0000 Uiso R . . . . . . H361 H 0.3242 0.5767 -0.0478 0.0593 1.0000 Uiso R . . . . . . H371 H 0.4113 0.4887 0.0716 0.0619 1.0000 Uiso R . . . . . . H381 H 0.4922 0.5566 0.2185 0.0505 1.0000 Uiso R . . . . . . H401 H 0.4334 0.7405 0.4647 0.0511 1.0000 Uiso R . . . . . . H411 H 0.2312 0.7794 0.5141 0.0618 1.0000 Uiso R . . . . . . H421 H 0.0227 0.8122 0.4110 0.0622 1.0000 Uiso R . . . . . . H431 H 0.0193 0.8039 0.2572 0.0579 1.0000 Uiso R . . . . . . H441 H 0.2224 0.7662 0.2075 0.0468 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0243(3) 0.0445(3) 0.0273(3) -0.0007(2) 0.00450(19) 0.0003(2) B1 0.0292(16) 0.055(2) 0.051(2) 0.0046(17) 0.0039(14) -0.0091(15) B2 0.0240(13) 0.0385(17) 0.0289(14) 0.0019(12) 0.0044(11) 0.0025(12) O1 0.0406(13) 0.0880(19) 0.0555(15) -0.0349(14) 0.0001(11) 0.0127(12) O2 0.0419(11) 0.0474(12) 0.0296(10) 0.0011(9) 0.0082(8) -0.0033(9) O3 0.0272(9) 0.0439(12) 0.0487(12) -0.0041(9) 0.0129(9) -0.0070(8) O4 0.0387(11) 0.0755(16) 0.0324(11) 0.0129(10) 0.0115(9) 0.0189(11) O5 0.0249(9) 0.0548(13) 0.0321(10) 0.0087(9) 0.0067(8) -0.0036(8) C1 0.042(2) 0.107(4) 0.092(3) -0.048(3) 0.004(2) 0.021(2) C2 0.124(5) 0.107(4) 0.128(5) -0.041(4) -0.041(4) 0.069(4) C3 0.116(4) 0.082(4) 0.085(3) -0.017(3) 0.001(3) 0.002(3) C4 0.059(2) 0.075(3) 0.057(2) -0.029(2) -0.0011(18) 0.000(2) C5 0.087(3) 0.052(2) 0.0341(16) -0.0026(15) 0.0201(17) -0.0122(19) C6 0.052(2) 0.081(3) 0.0383(17) 0.0033(17) 0.0164(15) -0.0109(18) C7 0.130(5) 0.063(3) 0.055(2) 0.006(2) 0.022(3) -0.019(3) C8 0.092(3) 0.043(2) 0.052(2) 0.0068(16) 0.023(2) 0.0209(19) C9 0.0359(15) 0.053(2) 0.0547(19) -0.0099(15) 0.0214(14) -0.0059(14) C10 0.0413(16) 0.055(2) 0.0495(18) -0.0094(15) 0.0135(14) 0.0082(15) C11 0.0473(18) 0.0448(19) 0.0530(19) 0.0004(15) 0.0125(15) -0.0006(14) C12 0.0361(16) 0.0434(19) 0.079(2) -0.0054(17) 0.0144(16) -0.0109(14) C13 0.065(2) 0.080(3) 0.0346(17) 0.0033(17) 0.0145(16) 0.021(2) C14 0.090(3) 0.066(2) 0.0375(18) 0.0005(16) 0.0260(19) -0.001(2) C15 0.093(3) 0.068(3) 0.048(2) 0.0150(19) 0.018(2) 0.028(2) C16 0.070(3) 0.091(3) 0.058(2) 0.030(2) 0.031(2) 0.037(2) C17 0.0324(15) 0.096(3) 0.0439(18) 0.0292(19) 0.0106(13) -0.0039(17) C18 0.0315(15) 0.073(3) 0.066(2) 0.032(2) 0.0071(15) -0.0045(16) C19 0.0289(14) 0.060(2) 0.0518(19) 0.0153(16) 0.0038(13) -0.0010(14) C20 0.0307(13) 0.0513(18) 0.0347(14) 0.0075(13) 0.0034(11) -0.0029(12) C21 0.0239(12) 0.0395(15) 0.0355(14) 0.0080(12) -0.0014(10) 0.0024(11) C22 0.0409(16) 0.0413(17) 0.0432(17) 0.0077(13) -0.0005(13) 0.0051(13) C23 0.053(2) 0.0349(17) 0.070(2) 0.0072(16) -0.0028(17) 0.0044(15) C24 0.049(2) 0.0389(19) 0.087(3) 0.0242(19) -0.0040(19) -0.0041(15) C25 0.0355(16) 0.054(2) 0.071(2) 0.0273(19) 0.0050(16) -0.0031(15) C26 0.0310(14) 0.0481(18) 0.0514(18) 0.0138(14) 0.0086(13) 0.0019(13) C27 0.0278(12) 0.0366(15) 0.0242(12) -0.0030(10) 0.0039(10) -0.0007(11) C28 0.0286(13) 0.0354(15) 0.0334(14) 0.0001(11) 0.0075(11) -0.0011(11) C29 0.0287(13) 0.0475(17) 0.0369(15) 0.0010(13) 0.0043(11) 0.0060(12) C30 0.0414(15) 0.0430(17) 0.0319(14) 0.0062(12) 0.0053(12) 0.0130(13) C31 0.0431(16) 0.0448(17) 0.0356(15) 0.0099(13) 0.0109(13) 0.0012(13) C32 0.0292(13) 0.0473(17) 0.0323(14) 0.0045(12) 0.0053(11) -0.0025(12) C33 0.0245(12) 0.0468(17) 0.0283(13) 0.0023(11) 0.0072(10) 0.0003(11) C34 0.0415(16) 0.0533(19) 0.0307(14) 0.0051(13) 0.0065(12) 0.0048(14) C35 0.0423(17) 0.079(3) 0.0282(14) 0.0107(15) 0.0071(13) 0.0063(16) C36 0.0489(18) 0.071(2) 0.0300(15) -0.0087(15) 0.0108(13) 0.0007(16) C37 0.061(2) 0.058(2) 0.0331(16) -0.0075(15) 0.0102(15) -0.0025(17) C38 0.0443(16) 0.0485(18) 0.0313(14) 0.0010(13) 0.0106(12) 0.0011(14) C39 0.0258(12) 0.0371(15) 0.0342(14) -0.0008(11) 0.0057(10) -0.0022(11) C40 0.0333(14) 0.058(2) 0.0346(15) 0.0003(13) 0.0081(12) 0.0017(13) C41 0.0490(18) 0.060(2) 0.0458(18) 0.0006(15) 0.0243(15) 0.0030(16) C42 0.0344(15) 0.051(2) 0.068(2) -0.0046(16) 0.0248(15) 0.0004(14) C43 0.0252(13) 0.055(2) 0.060(2) -0.0030(16) 0.0045(13) 0.0027(13) C44 0.0286(13) 0.0468(17) 0.0399(15) -0.0001(13) 0.0054(12) 0.0021(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6241(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ca1 . O1 . 2.355(2) yes Ca1 . O2 . 2.371(2) yes Ca1 . O3 . 2.374(2) yes Ca1 . O4 . 2.419(2) yes Ca1 . O5 . 2.3987(19) yes Ca1 . H2 . 2.444(10) no Ca1 . H3 . 2.445(9) no Ca1 . H4 . 2.445(9) no B1 . H1 . 1.18(5) no B1 . H2 . 1.203(10) no B1 . H3 . 1.206(10) no B1 . H4 . 1.207(10) no B2 . C21 . 1.655(4) yes B2 . C27 . 1.652(4) yes B2 . C33 . 1.653(4) yes B2 . C39 . 1.639(4) yes O1 . C1 . 1.450(5) yes O1 . C4 . 1.437(4) yes O2 . C5 . 1.439(4) yes O2 . C8 . 1.453(4) yes O3 . C9 . 1.451(4) yes O3 . C12 . 1.457(4) yes O4 . C13 . 1.452(4) yes O4 . C16 . 1.457(5) yes O5 . C17 . 1.454(3) yes O5 . C20 . 1.445(3) yes C1 . C2 . 1.353(8) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C2 . C3 . 1.552(9) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C3 . C4 . 1.370(8) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . H41 . 0.950 no C4 . H42 . 0.950 no C5 . C6 . 1.478(5) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C6 . C7 . 1.436(6) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C7 . C8 . 1.532(6) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . C10 . 1.498(5) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C10 . C11 . 1.534(5) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C11 . C12 . 1.507(5) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C13 . C14 . 1.487(6) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C14 . C15 . 1.502(6) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C15 . C16 . 1.473(5) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C17 . C18 . 1.500(5) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C18 . C19 . 1.511(5) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C19 . C20 . 1.518(4) yes C19 . H191 . 0.950 no C19 . H192 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C21 . C22 . 1.404(5) yes C21 . C26 . 1.402(4) yes C22 . C23 . 1.391(5) yes C22 . H221 . 0.950 no C23 . C24 . 1.393(6) yes C23 . H231 . 0.950 no C24 . C25 . 1.376(6) yes C24 . H241 . 0.950 no C25 . C26 . 1.395(5) yes C25 . H251 . 0.950 no C26 . H261 . 0.950 no C27 . C28 . 1.401(4) yes C27 . C32 . 1.404(4) yes C28 . C29 . 1.396(4) yes C28 . H281 . 0.950 no C29 . C30 . 1.387(5) yes C29 . H291 . 0.950 no C30 . C31 . 1.380(4) yes C30 . H301 . 0.950 no C31 . C32 . 1.393(4) yes C31 . H311 . 0.950 no C32 . H321 . 0.950 no C33 . C34 . 1.409(4) yes C33 . C38 . 1.387(5) yes C34 . C35 . 1.393(4) yes C34 . H341 . 0.950 no C35 . C36 . 1.376(6) yes C35 . H351 . 0.950 no C36 . C37 . 1.378(5) yes C36 . H361 . 0.950 no C37 . C38 . 1.404(4) yes C37 . H371 . 0.950 no C38 . H381 . 0.950 no C39 . C40 . 1.403(4) yes C39 . C44 . 1.401(4) yes C40 . C41 . 1.391(4) yes C40 . H401 . 0.950 no C41 . C42 . 1.376(5) yes C41 . H411 . 0.950 no C42 . C43 . 1.377(5) yes C42 . H421 . 0.950 no C43 . C44 . 1.396(4) yes C43 . H431 . 0.950 no C44 . H441 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Ca1 . O2 . 89.12(10) yes O1 . Ca1 . O3 . 161.31(9) yes O2 . Ca1 . O3 . 94.12(8) yes O1 . Ca1 . O4 . 84.20(10) yes O2 . Ca1 . O4 . 168.38(7) yes O3 . Ca1 . O4 . 89.30(8) yes O1 . Ca1 . O5 . 81.40(8) yes O2 . Ca1 . O5 . 83.18(7) yes O3 . Ca1 . O5 . 80.72(7) yes O4 . Ca1 . O5 . 86.42(7) yes O1 . Ca1 . H2 . 114.0(10) no O2 . Ca1 . H2 . 117.5(6) no O3 . Ca1 . H2 . 80.7(9) no O4 . Ca1 . H2 . 74.0(6) no O5 . Ca1 . H2 . 153.0(3) no O1 . Ca1 . H3 . 118.5(10) no O2 . Ca1 . H3 . 72.2(7) no O3 . Ca1 . H3 . 79.9(9) no O4 . Ca1 . H3 . 119.3(7) no O5 . Ca1 . H3 . 147.3(3) no O1 . Ca1 . H4 . 75.7(3) no O2 . Ca1 . H4 . 91.5(11) no O3 . Ca1 . H4 . 122.5(3) no O4 . Ca1 . H4 . 96.0(11) no O5 . Ca1 . H4 . 156.6(3) no H2 . Ca1 . H3 . 45.4(9) no H2 . Ca1 . H4 . 47.1(9) no H3 . Ca1 . H4 . 48.0(8) no H1 . B1 . H2 . 111.2(8) no H1 . B1 . H3 . 111.2(8) no H2 . B1 . H3 . 103(3) no H1 . B1 . H4 . 111.6(8) no H2 . B1 . H4 . 108(3) no H3 . B1 . H4 . 111(3) no C21 . B2 . C27 . 110.0(2) yes C21 . B2 . C33 . 110.7(2) yes C27 . B2 . C33 . 108.0(2) yes C21 . B2 . C39 . 107.7(2) yes C27 . B2 . C39 . 111.7(2) yes C33 . B2 . C39 . 108.8(2) yes Ca1 . O1 . C1 . 125.3(2) yes Ca1 . O1 . C4 . 128.5(2) yes C1 . O1 . C4 . 104.4(3) yes Ca1 . O2 . C5 . 125.3(2) yes Ca1 . O2 . C8 . 121.3(2) yes C5 . O2 . C8 . 107.0(3) yes Ca1 . O3 . C9 . 124.90(17) yes Ca1 . O3 . C12 . 128.95(18) yes C9 . O3 . C12 . 105.5(2) yes Ca1 . O4 . C13 . 130.4(2) yes Ca1 . O4 . C16 . 118.77(19) yes C13 . O4 . C16 . 109.0(3) yes Ca1 . O5 . C17 . 123.33(17) yes Ca1 . O5 . C20 . 127.78(16) yes C17 . O5 . C20 . 108.9(2) yes O1 . C1 . C2 . 105.0(4) yes O1 . C1 . H11 . 110.1 no C2 . C1 . H11 . 110.8 no O1 . C1 . H12 . 111.6 no C2 . C1 . H12 . 109.8 no H11 . C1 . H12 . 109.5 no C1 . C2 . C3 . 107.9(4) yes C1 . C2 . H21 . 109.8 no C3 . C2 . H21 . 108.5 no C1 . C2 . H22 . 110.7 no C3 . C2 . H22 . 110.4 no H21 . C2 . H22 . 109.5 no C2 . C3 . C4 . 98.9(5) yes C2 . C3 . H31 . 111.7 no C4 . C3 . H31 . 112.0 no C2 . C3 . H32 . 113.1 no C4 . C3 . H32 . 111.4 no H31 . C3 . H32 . 109.5 no O1 . C4 . C3 . 103.7(4) yes O1 . C4 . H41 . 110.6 no C3 . C4 . H41 . 110.5 no O1 . C4 . H42 . 111.0 no C3 . C4 . H42 . 111.5 no H41 . C4 . H42 . 109.5 no O2 . C5 . C6 . 105.9(3) yes O2 . C5 . H51 . 110.4 no C6 . C5 . H51 . 110.7 no O2 . C5 . H52 . 110.2 no C6 . C5 . H52 . 110.2 no H51 . C5 . H52 . 109.5 no C5 . C6 . C7 . 106.4(3) yes C5 . C6 . H61 . 110.4 no C7 . C6 . H61 . 110.6 no C5 . C6 . H62 . 110.1 no C7 . C6 . H62 . 109.8 no H61 . C6 . H62 . 109.5 no C6 . C7 . C8 . 106.1(3) yes C6 . C7 . H71 . 110.8 no C8 . C7 . H71 . 110.7 no C6 . C7 . H72 . 109.9 no C8 . C7 . H72 . 109.8 no H71 . C7 . H72 . 109.5 no C7 . C8 . O2 . 105.9(3) yes C7 . C8 . H81 . 109.9 no O2 . C8 . H81 . 110.3 no C7 . C8 . H82 . 110.8 no O2 . C8 . H82 . 110.5 no H81 . C8 . H82 . 109.5 no O3 . C9 . C10 . 104.4(3) yes O3 . C9 . H91 . 110.8 no C10 . C9 . H91 . 110.8 no O3 . C9 . H92 . 110.5 no C10 . C9 . H92 . 110.8 no H91 . C9 . H92 . 109.5 no C9 . C10 . C11 . 102.0(3) yes C9 . C10 . H101 . 111.3 no C11 . C10 . H101 . 111.3 no C9 . C10 . H102 . 111.3 no C11 . C10 . H102 . 111.2 no H101 . C10 . H102 . 109.5 no C10 . C11 . C12 . 105.0(3) yes C10 . C11 . H111 . 110.7 no C12 . C11 . H111 . 110.3 no C10 . C11 . H112 . 110.5 no C12 . C11 . H112 . 110.8 no H111 . C11 . H112 . 109.5 no C11 . C12 . O3 . 107.0(3) yes C11 . C12 . H121 . 109.8 no O3 . C12 . H121 . 109.8 no C11 . C12 . H122 . 110.4 no O3 . C12 . H122 . 110.4 no H121 . C12 . H122 . 109.5 no O4 . C13 . C14 . 105.0(3) yes O4 . C13 . H131 . 110.7 no C14 . C13 . H131 . 110.9 no O4 . C13 . H132 . 110.4 no C14 . C13 . H132 . 110.3 no H131 . C13 . H132 . 109.5 no C13 . C14 . C15 . 103.0(3) yes C13 . C14 . H141 . 111.4 no C15 . C14 . H141 . 111.5 no C13 . C14 . H142 . 110.8 no C15 . C14 . H142 . 110.7 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 105.7(3) yes C14 . C15 . H151 . 110.8 no C16 . C15 . H151 . 110.3 no C14 . C15 . H152 . 110.0 no C16 . C15 . H152 . 110.5 no H151 . C15 . H152 . 109.5 no C15 . C16 . O4 . 106.1(3) yes C15 . C16 . H161 . 110.3 no O4 . C16 . H161 . 109.9 no C15 . C16 . H162 . 110.4 no O4 . C16 . H162 . 110.7 no H161 . C16 . H162 . 109.5 no O5 . C17 . C18 . 105.9(3) yes O5 . C17 . H171 . 110.0 no C18 . C17 . H171 . 110.1 no O5 . C17 . H172 . 110.6 no C18 . C17 . H172 . 110.8 no H171 . C17 . H172 . 109.5 no C17 . C18 . C19 . 102.5(3) yes C17 . C18 . H181 . 110.9 no C19 . C18 . H181 . 110.9 no C17 . C18 . H182 . 111.5 no C19 . C18 . H182 . 111.4 no H181 . C18 . H182 . 109.5 no C18 . C19 . C20 . 102.7(2) yes C18 . C19 . H191 . 110.8 no C20 . C19 . H191 . 110.8 no C18 . C19 . H192 . 111.4 no C20 . C19 . H192 . 111.5 no H191 . C19 . H192 . 109.5 no C19 . C20 . O5 . 106.3(2) yes C19 . C20 . H201 . 110.0 no O5 . C20 . H201 . 110.2 no C19 . C20 . H202 . 110.4 no O5 . C20 . H202 . 110.4 no H201 . C20 . H202 . 109.5 no B2 . C21 . C22 . 122.3(3) yes B2 . C21 . C26 . 122.2(3) yes C22 . C21 . C26 . 115.5(3) yes C21 . C22 . C23 . 122.6(3) yes C21 . C22 . H221 . 118.8 no C23 . C22 . H221 . 118.6 no C22 . C23 . C24 . 119.9(4) yes C22 . C23 . H231 . 120.3 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 119.1(3) yes C23 . C24 . H241 . 120.5 no C25 . C24 . H241 . 120.3 no C24 . C25 . C26 . 120.3(3) yes C24 . C25 . H251 . 119.7 no C26 . C25 . H251 . 119.9 no C21 . C26 . C25 . 122.5(3) yes C21 . C26 . H261 . 118.6 no C25 . C26 . H261 . 118.9 no B2 . C27 . C28 . 122.3(2) yes B2 . C27 . C32 . 122.5(2) yes C28 . C27 . C32 . 115.1(3) yes C27 . C28 . C29 . 122.9(3) yes C27 . C28 . H281 . 118.5 no C29 . C28 . H281 . 118.6 no C28 . C29 . C30 . 120.0(3) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 119.8 no C29 . C30 . C31 . 118.8(3) yes C29 . C30 . H301 . 120.8 no C31 . C30 . H301 . 120.4 no C30 . C31 . C32 . 120.6(3) yes C30 . C31 . H311 . 119.8 no C32 . C31 . H311 . 119.6 no C27 . C32 . C31 . 122.6(3) yes C27 . C32 . H321 . 118.7 no C31 . C32 . H321 . 118.7 no B2 . C33 . C34 . 121.7(3) yes B2 . C33 . C38 . 123.4(3) yes C34 . C33 . C38 . 114.6(3) yes C33 . C34 . C35 . 123.0(3) yes C33 . C34 . H341 . 118.4 no C35 . C34 . H341 . 118.7 no C34 . C35 . C36 . 120.2(3) yes C34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 119.9 no C35 . C36 . C37 . 119.0(3) yes C35 . C36 . H361 . 120.7 no C37 . C36 . H361 . 120.3 no C36 . C37 . C38 . 119.9(3) yes C36 . C37 . H371 . 120.0 no C38 . C37 . H371 . 120.1 no C37 . C38 . C33 . 123.2(3) yes C37 . C38 . H381 . 118.4 no C33 . C38 . H381 . 118.4 no B2 . C39 . C40 . 122.6(2) yes B2 . C39 . C44 . 122.2(2) yes C40 . C39 . C44 . 114.8(3) yes C39 . C40 . C41 . 122.8(3) yes C39 . C40 . H401 . 118.5 no C41 . C40 . H401 . 118.7 no C40 . C41 . C42 . 120.4(3) yes C40 . C41 . H411 . 119.7 no C42 . C41 . H411 . 119.8 no C41 . C42 . C43 . 118.9(3) yes C41 . C42 . H421 . 120.6 no C43 . C42 . H421 . 120.6 no C42 . C43 . C44 . 120.3(3) yes C42 . C43 . H431 . 119.8 no C44 . C43 . H431 . 119.9 no C39 . C44 . C43 . 122.8(3) yes C39 . C44 . H441 . 118.7 no C43 . C44 . H441 . 118.6 no B1 . H2 . Ca1 . 84.1(5) no B1 . H3 . Ca1 . 84.0(5) no B1 . H4 . Ca1 . 83.9(5) no #===end data_COMPOUND_2-BPh4 _database_code_depnum_ccdc_archive 'CCDC 796413' #TrackingRef '- Mountford Xray SI.CIF' # Local code MGC62 _chemical_name_systematic ; [Ca{HC(Me2pz)3}(BH4)(THF)2][BPh4] . 2(THF) ; _chemical_melting_point ? _publ_section_exptl_refinement ; The THF molecules of crystallization were refined subject to loose similarity restraints on the APDs. One carbon was split over two sites (C(50) and C(501) and refined as such). B-bound H atoms were located from a Fourier map and positionally and isotropically refined. Other H atoms were placed in calculated positions, with the orientations of methyl hydrogens being confirmed by reference to a Fourier difference map. ; _cell_length_a 10.3958(2) _cell_length_b 15.0936(4) _cell_length_c 17.5126(4) _cell_angle_alpha 82.3488(12) _cell_angle_beta 82.0004(12) _cell_angle_gamma 80.4508(7) _cell_volume 2666.36(11) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Ca 0.2262 0.3064 8.6266 10.4421 7.3873 0.6599 1.5899 85.7484 1.0211 178.4370 1.3751 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C56 H78 B2 Ca1 N6 O4' _chemical_formula_moiety 'C48 H62 B2 Ca1 N6 O2, 2 (C4 H8 O)' _chemical_compound_source ? _chemical_formula_weight 960.98 _cell_measurement_reflns_used 8526 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15844 _reflns_number_total 9271 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_min 5.172 _diffrn_reflns_theta_max 25.032 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.032 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.35 _oxford_diffrn_Wilson_scale 0.62 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.37 _refine_diff_density_max 0.92 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 7488 _refine_ls_number_restraints 38 _refine_ls_number_parameters 647 _oxford_refine_ls_R_factor_ref 0.0440 _refine_ls_wR_factor_ref 0.0464 _refine_ls_goodness_of_fit_ref 1.0955 _refine_ls_shift/su_max 0.019404 # The values computed from all data _oxford_reflns_number_all 9271 _refine_ls_R_factor_all 0.0553 _refine_ls_wR_factor_all 0.0594 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7647 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_gt 0.0471 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.409 0.325 0.243 0.983E-01 0.606E-01 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ca1 Ca 0.80347(3) 0.79001(2) 0.179761(19) 0.0231 1.0000 Uani . . . . . . . B1 B 1.0242(2) 0.76821(17) 0.09156(14) 0.0361 1.0000 Uani . . . . . . . B2 B 1.14384(19) 1.15109(13) 0.29485(11) 0.0246 1.0000 Uani . . . . . . . N1 N 0.79079(14) 0.63698(10) 0.25332(8) 0.0264 1.0000 Uani . . . . . . . N2 N 0.67919(14) 0.59845(10) 0.25601(8) 0.0254 1.0000 Uani . . . . . . . N3 N 0.65692(14) 0.71660(10) 0.11401(8) 0.0254 1.0000 Uani . . . . . . . N4 N 0.55331(14) 0.68156(10) 0.15801(8) 0.0252 1.0000 Uani . . . . . . . N5 N 0.58380(14) 0.80467(10) 0.26392(8) 0.0257 1.0000 Uani . . . . . . . N6 N 0.52425(14) 0.72910(10) 0.28511(8) 0.0264 1.0000 Uani . . . . . . . O1 O 0.72064(12) 0.93903(8) 0.13062(8) 0.0325 1.0000 Uani . . . . . . . O2 O 0.86991(12) 0.83025(9) 0.29346(7) 0.0299 1.0000 Uani . . . . . . . O3 O 1.68470(17) 1.37703(14) 0.08949(13) 0.0702 1.0000 Uani . . . . . . . O4 O 0.4129(2) 0.42062(16) 0.46103(14) 0.0818 1.0000 Uani . U . . . . . C1 C 0.88288(18) 0.56775(12) 0.27214(10) 0.0295 1.0000 Uani . . . . . . . C2 C 0.83135(19) 0.48594(13) 0.28609(11) 0.0333 1.0000 Uani . . . . . . . C3 C 0.70084(19) 0.50722(12) 0.27511(10) 0.0294 1.0000 Uani . . . . . . . C4 C 1.01991(19) 0.58319(14) 0.27673(13) 0.0400 1.0000 Uani . . . . . . . C5 C 0.5966(2) 0.44945(13) 0.28053(13) 0.0398 1.0000 Uani . . . . . . . C6 C 0.62640(18) 0.72821(12) 0.04149(10) 0.0273 1.0000 Uani . . . . . . . C7 C 0.50325(19) 0.70211(13) 0.03929(11) 0.0319 1.0000 Uani . . . . . . . C8 C 0.45854(17) 0.67275(12) 0.11409(11) 0.0291 1.0000 Uani . . . . . . . C9 C 0.7195(2) 0.76287(14) -0.02402(11) 0.0339 1.0000 Uani . . . . . . . C10 C 0.33475(19) 0.63788(15) 0.14858(13) 0.0403 1.0000 Uani . . . . . . . C11 C 0.52956(17) 0.86065(13) 0.31670(10) 0.0298 1.0000 Uani . . . . . . . C12 C 0.43795(19) 0.82038(14) 0.37131(11) 0.0352 1.0000 Uani . . . . . . . C13 C 0.43575(18) 0.73666(13) 0.35015(10) 0.0322 1.0000 Uani . . . . . . . C14 C 0.5644(2) 0.95306(13) 0.31186(12) 0.0362 1.0000 Uani . . . . . . . C15 C 0.3588(2) 0.66307(15) 0.38525(13) 0.0444 1.0000 Uani . . . . . . . C16 C 0.55649(17) 0.65352(12) 0.23987(10) 0.0253 1.0000 Uani . . . . . . . C17 C 0.7927(2) 1.01456(14) 0.11624(14) 0.0443 1.0000 Uani . . . . . . . C18 C 0.6907(3) 1.09692(15) 0.11398(15) 0.0536 1.0000 Uani . . . . . . . C19 C 0.5743(2) 1.06717(15) 0.08713(13) 0.0455 1.0000 Uani . . . . . . . C20 C 0.6076(2) 0.96614(14) 0.08958(14) 0.0422 1.0000 Uani . . . . . . . C21 C 0.84388(19) 0.78707(14) 0.37222(10) 0.0343 1.0000 Uani . . . . . . . C22 C 0.9680(2) 0.78444(16) 0.41057(12) 0.0436 1.0000 Uani . . . . . . . C23 C 1.0639(2) 0.82516(14) 0.34639(13) 0.0395 1.0000 Uani . . . . . . . C24 C 0.97296(19) 0.88413(13) 0.29447(12) 0.0345 1.0000 Uani . . . . . . . C25 C 0.98666(18) 1.18519(12) 0.32161(10) 0.0273 1.0000 Uani . . . . . . . C26 C 0.9535(2) 1.24615(13) 0.37781(11) 0.0350 1.0000 Uani . . . . . . . C27 C 0.8242(2) 1.27183(15) 0.40947(13) 0.0483 1.0000 Uani . . . . . . . C28 C 0.7226(2) 1.23728(17) 0.38627(14) 0.0514 1.0000 Uani . . . . . . . C29 C 0.7512(2) 1.17863(16) 0.33027(14) 0.0464 1.0000 Uani . . . . . . . C30 C 0.88112(18) 1.15347(14) 0.29872(11) 0.0347 1.0000 Uani . . . . . . . C31 C 1.16616(16) 1.07758(12) 0.23089(10) 0.0249 1.0000 Uani . . . . . . . C32 C 1.11265(18) 1.09913(13) 0.16035(10) 0.0310 1.0000 Uani . . . . . . . C33 C 1.1328(2) 1.03974(15) 0.10390(11) 0.0374 1.0000 Uani . . . . . . . C34 C 1.2097(2) 0.95590(15) 0.11559(12) 0.0393 1.0000 Uani . . . . . . . C35 C 1.2669(2) 0.93303(14) 0.18347(12) 0.0359 1.0000 Uani . . . . . . . C36 C 1.24459(17) 0.99297(12) 0.23986(11) 0.0283 1.0000 Uani . . . . . . . C37 C 1.20222(17) 1.10302(12) 0.37578(10) 0.0251 1.0000 Uani . . . . . . . C38 C 1.14413(18) 1.03111(12) 0.41821(10) 0.0284 1.0000 Uani . . . . . . . C39 C 1.18789(19) 0.98412(13) 0.48577(10) 0.0314 1.0000 Uani . . . . . . . C40 C 1.29302(19) 1.00865(13) 0.51440(11) 0.0334 1.0000 Uani . . . . . . . C41 C 1.35038(19) 1.08113(14) 0.47601(11) 0.0333 1.0000 Uani . . . . . . . C42 C 1.30511(18) 1.12734(13) 0.40806(10) 0.0284 1.0000 Uani . . . . . . . C43 C 1.22029(17) 1.23461(12) 0.25198(10) 0.0253 1.0000 Uani . . . . . . . C44 C 1.15642(19) 1.31985(12) 0.22484(11) 0.0303 1.0000 Uani . . . . . . . C45 C 1.2242(2) 1.38661(13) 0.18266(11) 0.0352 1.0000 Uani . . . . . . . C46 C 1.3596(2) 1.37107(13) 0.16702(11) 0.0349 1.0000 Uani . . . . . . . C47 C 1.42646(19) 1.28787(13) 0.19320(11) 0.0330 1.0000 Uani . . . . . . . C48 C 1.35773(18) 1.22148(12) 0.23362(10) 0.0281 1.0000 Uani . . . . . . . C49 C 1.6883(2) 1.46413(19) 0.05091(16) 0.0602 1.0000 Uani D . . . . . . C50 C 1.8133(5) 1.4942(3) 0.0624(5) 0.0473 0.3000 Uani D . . . . . . C51 C 1.9013(2) 1.40637(18) 0.07893(16) 0.0592 1.0000 Uani D . . . . . . C52 C 1.8110(2) 1.33967(16) 0.10982(15) 0.0526 1.0000 Uani D . . . . . . C53 C 0.3251(2) 0.4498(2) 0.52472(14) 0.0577 1.0000 Uani D U . . . . . C54 C 0.1907(3) 0.4659(2) 0.50089(17) 0.0659 1.0000 Uani D U . . . . . C55 C 0.2075(4) 0.3993(3) 0.4405(2) 0.1127 1.0000 Uani D U . . . . . C56 C 0.3488(4) 0.3589(3) 0.4380(3) 0.1083 1.0000 Uani D U . . . . . C501 C 1.8289(3) 1.4686(3) 0.0216(2) 0.0579 0.7000 Uani D . . . . . . H1 H 1.123(2) 0.7614(17) 0.0530(15) 0.055(7) 1.0000 Uiso . . . . . . . H2 H 0.948(3) 0.8341(19) 0.0704(16) 0.064(8) 1.0000 Uiso . . . . . . . H3 H 1.039(3) 0.7801(18) 0.1556(16) 0.063(8) 1.0000 Uiso . . . . . . . H4 H 0.966(2) 0.7097(16) 0.0989(13) 0.046(6) 1.0000 Uiso . . . . . . . H21 H 0.8775 0.4277 0.3003 0.0399 1.0000 Uiso R . . . . . . H41 H 1.0723 0.5271 0.2905 0.0493 1.0000 Uiso R . . . . . . H42 H 1.0185 0.6226 0.3149 0.0493 1.0000 Uiso R . . . . . . H43 H 1.0558 0.6096 0.2278 0.0493 1.0000 Uiso R . . . . . . H51 H 0.5646 0.4548 0.2317 0.0497 1.0000 Uiso R . . . . . . H52 H 0.5266 0.4683 0.3187 0.0497 1.0000 Uiso R . . . . . . H53 H 0.6320 0.3883 0.2946 0.0497 1.0000 Uiso R . . . . . . H71 H 0.4600 0.7042 -0.0054 0.0406 1.0000 Uiso R . . . . . . H91 H 0.7988 0.7695 -0.0059 0.0439 1.0000 Uiso R . . . . . . H92 H 0.6789 0.8195 -0.0464 0.0439 1.0000 Uiso R . . . . . . H93 H 0.7367 0.7211 -0.0616 0.0439 1.0000 Uiso R . . . . . . H101 H 0.3553 0.5785 0.1737 0.0515 1.0000 Uiso R . . . . . . H102 H 0.2818 0.6368 0.1088 0.0515 1.0000 Uiso R . . . . . . H103 H 0.2883 0.6762 0.1854 0.0515 1.0000 Uiso R . . . . . . H121 H 0.3874 0.8463 0.4146 0.0424 1.0000 Uiso R . . . . . . H141 H 0.5163 0.9828 0.3539 0.0463 1.0000 Uiso R . . . . . . H142 H 0.5435 0.9865 0.2641 0.0463 1.0000 Uiso R . . . . . . H143 H 0.6557 0.9488 0.3146 0.0463 1.0000 Uiso R . . . . . . H151 H 0.4173 0.6102 0.4000 0.0531 1.0000 Uiso R . . . . . . H152 H 0.3029 0.6818 0.4298 0.0531 1.0000 Uiso R . . . . . . H153 H 0.3074 0.6504 0.3484 0.0531 1.0000 Uiso R . . . . . . H161 H 0.4898 0.6166 0.2556 0.0314 1.0000 Uiso R . . . . . . H171 H 0.8469 1.0131 0.0679 0.0569 1.0000 Uiso R . . . . . . H172 H 0.8454 1.0136 0.1565 0.0569 1.0000 Uiso R . . . . . . H181 H 0.7209 1.1448 0.0788 0.0677 1.0000 Uiso R . . . . . . H182 H 0.6677 1.1161 0.1643 0.0677 1.0000 Uiso R . . . . . . H191 H 0.5628 1.0942 0.0359 0.0549 1.0000 Uiso R . . . . . . H192 H 0.4965 1.0830 0.1210 0.0549 1.0000 Uiso R . . . . . . H201 H 0.6277 0.9497 0.0382 0.0533 1.0000 Uiso R . . . . . . H202 H 0.5359 0.9380 0.1156 0.0533 1.0000 Uiso R . . . . . . H211 H 0.7707 0.8208 0.3996 0.0424 1.0000 Uiso R . . . . . . H212 H 0.8267 0.7274 0.3713 0.0424 1.0000 Uiso R . . . . . . H221 H 0.9499 0.8199 0.4529 0.0539 1.0000 Uiso R . . . . . . H222 H 1.0023 0.7242 0.4285 0.0539 1.0000 Uiso R . . . . . . H231 H 1.1173 0.8596 0.3666 0.0502 1.0000 Uiso R . . . . . . H232 H 1.1183 0.7793 0.3195 0.0502 1.0000 Uiso R . . . . . . H241 H 0.9383 0.9393 0.3154 0.0460 1.0000 Uiso R . . . . . . H242 H 1.0166 0.8967 0.2437 0.0460 1.0000 Uiso R . . . . . . H261 H 1.0216 1.2709 0.3945 0.0416 1.0000 Uiso R . . . . . . H271 H 0.8059 1.3131 0.4474 0.0545 1.0000 Uiso R . . . . . . H281 H 0.6346 1.2540 0.4085 0.0545 1.0000 Uiso R . . . . . . H291 H 0.6822 1.1554 0.3131 0.0546 1.0000 Uiso R . . . . . . H301 H 0.8985 1.1129 0.2602 0.0414 1.0000 Uiso R . . . . . . H321 H 1.0605 1.1564 0.1509 0.0392 1.0000 Uiso R . . . . . . H331 H 1.0938 1.0566 0.0572 0.0482 1.0000 Uiso R . . . . . . H341 H 1.2233 0.9151 0.0774 0.0492 1.0000 Uiso R . . . . . . H351 H 1.3209 0.8763 0.1919 0.0445 1.0000 Uiso R . . . . . . H361 H 1.2845 0.9757 0.2862 0.0357 1.0000 Uiso R . . . . . . H381 H 1.0715 1.0137 0.3997 0.0356 1.0000 Uiso R . . . . . . H391 H 1.1458 0.9355 0.5121 0.0383 1.0000 Uiso R . . . . . . H401 H 1.3249 0.9760 0.5598 0.0405 1.0000 Uiso R . . . . . . H411 H 1.4210 1.0994 0.4959 0.0412 1.0000 Uiso R . . . . . . H421 H 1.3457 1.1771 0.3829 0.0355 1.0000 Uiso R . . . . . . H441 H 1.0636 1.3327 0.2357 0.0372 1.0000 Uiso R . . . . . . H451 H 1.1769 1.4430 0.1644 0.0426 1.0000 Uiso R . . . . . . H461 H 1.4057 1.4169 0.1390 0.0441 1.0000 Uiso R . . . . . . H471 H 1.5195 1.2763 0.1832 0.0412 1.0000 Uiso R . . . . . . H481 H 1.4056 1.1645 0.2498 0.0346 1.0000 Uiso R . . . . . . H491 H 1.6561 1.5082 0.0857 0.0720 1.0000 Uiso R . . . . . . H492 H 1.6365 1.4736 0.0092 0.0720 1.0000 Uiso R . . . . . . H501 H 1.8012 1.5302 0.1041 0.0611 0.3000 Uiso R . . . . . . H502 H 1.8478 1.5273 0.0162 0.0611 0.3000 Uiso R . . . . . . H511 H 1.9174 1.4382 0.1191 0.0722 1.0000 Uiso R . . . . . . H512 H 1.9823 1.3775 0.0551 0.0722 1.0000 Uiso R . . . . . . H521 H 1.8079 1.3283 0.1647 0.0644 1.0000 Uiso R . . . . . . H522 H 1.8405 1.2847 0.0875 0.0644 1.0000 Uiso R . . . . . . H531 H 0.3297 0.4046 0.5679 0.0701 1.0000 Uiso R . . . . . . H532 H 0.3464 0.5040 0.5383 0.0701 1.0000 Uiso R . . . . . . H541 H 0.1262 0.4521 0.5429 0.0798 1.0000 Uiso R . . . . . . H542 H 0.1683 0.5265 0.4788 0.0798 1.0000 Uiso R . . . . . . H551 H 0.1521 0.3544 0.4560 0.1453 1.0000 Uiso R . . . . . . H552 H 0.1890 0.4299 0.3914 0.1453 1.0000 Uiso R . . . . . . H561 H 0.3839 0.3473 0.3866 0.1308 1.0000 Uiso R . . . . . . H562 H 0.3579 0.3042 0.4717 0.1308 1.0000 Uiso R . . . . . . H5011 H 1.8478 1.5284 0.0191 0.0733 0.7000 Uiso R . . . . . . H5012 H 1.8502 1.4484 -0.0284 0.0733 0.7000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.02238(18) 0.02458(18) 0.02264(18) -0.00379(13) -0.00331(13) -0.00296(13) B1 0.0297(11) 0.0434(13) 0.0334(12) -0.0076(10) 0.0019(9) -0.0024(10) B2 0.0247(10) 0.0263(10) 0.0224(9) -0.0021(8) -0.0033(7) -0.0030(8) N1 0.0250(7) 0.0259(8) 0.0278(8) -0.0026(6) -0.0032(6) -0.0024(6) N2 0.0271(7) 0.0237(7) 0.0246(7) -0.0007(6) -0.0022(6) -0.0037(6) N3 0.0257(7) 0.0289(8) 0.0225(7) -0.0034(6) -0.0014(6) -0.0072(6) N4 0.0243(7) 0.0277(8) 0.0246(7) -0.0023(6) -0.0033(6) -0.0066(6) N5 0.0248(7) 0.0263(8) 0.0259(7) -0.0058(6) -0.0026(6) -0.0016(6) N6 0.0253(7) 0.0275(8) 0.0245(7) -0.0025(6) 0.0015(6) -0.0023(6) O1 0.0301(7) 0.0267(7) 0.0405(7) 0.0002(5) -0.0085(6) -0.0035(5) O2 0.0292(7) 0.0366(7) 0.0262(6) -0.0051(5) -0.0064(5) -0.0076(5) O3 0.0434(10) 0.0767(13) 0.0894(14) 0.0134(11) -0.0058(9) -0.0256(9) O4 0.0724(13) 0.0868(15) 0.0891(15) -0.0294(12) 0.0182(11) -0.0282(12) C1 0.0289(9) 0.0300(9) 0.0268(9) -0.0030(7) -0.0026(7) 0.0027(7) C2 0.0387(10) 0.0261(9) 0.0309(10) -0.0008(7) -0.0025(8) 0.0036(8) C3 0.0393(10) 0.0238(9) 0.0236(9) -0.0017(7) -0.0009(7) -0.0034(8) C4 0.0305(10) 0.0381(11) 0.0483(12) -0.0025(9) -0.0073(9) 0.0038(8) C5 0.0460(12) 0.0285(10) 0.0438(12) 0.0016(8) -0.0027(9) -0.0088(9) C6 0.0322(9) 0.0251(9) 0.0256(9) -0.0055(7) -0.0061(7) -0.0030(7) C7 0.0338(10) 0.0331(10) 0.0311(10) -0.0025(8) -0.0125(8) -0.0052(8) C8 0.0265(9) 0.0261(9) 0.0353(10) -0.0020(7) -0.0094(7) -0.0023(7) C9 0.0388(10) 0.0405(11) 0.0236(9) -0.0038(8) -0.0051(8) -0.0080(8) C10 0.0294(10) 0.0448(12) 0.0483(12) 0.0020(9) -0.0110(9) -0.0107(9) C11 0.0261(9) 0.0355(10) 0.0271(9) -0.0085(7) -0.0073(7) 0.0047(7) C12 0.0304(10) 0.0451(12) 0.0261(9) -0.0083(8) 0.0004(8) 0.0060(8) C13 0.0264(9) 0.0406(11) 0.0248(9) -0.0002(8) 0.0016(7) 0.0027(8) C14 0.0355(10) 0.0356(10) 0.0386(11) -0.0150(8) -0.0086(8) 0.0036(8) C15 0.0382(11) 0.0481(13) 0.0394(12) 0.0027(9) 0.0106(9) -0.0034(9) C16 0.0245(8) 0.0272(9) 0.0237(8) -0.0015(7) -0.0019(7) -0.0046(7) C17 0.0461(12) 0.0349(11) 0.0553(13) -0.0023(10) -0.0112(10) -0.0141(9) C18 0.0766(17) 0.0286(11) 0.0580(15) -0.0041(10) -0.0202(13) -0.0050(11) C19 0.0517(13) 0.0372(12) 0.0425(12) -0.0010(9) -0.0100(10) 0.0086(10) C20 0.0396(11) 0.0371(11) 0.0520(13) -0.0027(9) -0.0196(10) -0.0016(9) C21 0.0357(10) 0.0445(11) 0.0232(9) -0.0065(8) -0.0013(8) -0.0068(8) C22 0.0495(13) 0.0472(13) 0.0359(11) -0.0023(9) -0.0174(9) -0.0039(10) C23 0.0362(11) 0.0385(11) 0.0480(12) -0.0044(9) -0.0178(9) -0.0072(9) C24 0.0349(10) 0.0346(10) 0.0383(11) -0.0047(8) -0.0118(8) -0.0111(8) C25 0.0295(9) 0.0266(9) 0.0220(8) 0.0045(7) -0.0019(7) -0.0003(7) C26 0.0403(11) 0.0330(10) 0.0264(9) 0.0004(8) 0.0028(8) 0.0016(8) C27 0.0549(14) 0.0409(12) 0.0350(11) 0.0022(9) 0.0146(10) 0.0117(10) C28 0.0331(11) 0.0545(14) 0.0477(13) 0.0205(11) 0.0124(10) 0.0128(10) C29 0.0270(10) 0.0548(14) 0.0494(13) 0.0168(11) -0.0038(9) -0.0018(9) C30 0.0291(10) 0.0385(11) 0.0331(10) 0.0050(8) -0.0036(8) -0.0029(8) C31 0.0219(8) 0.0285(9) 0.0247(9) -0.0022(7) 0.0004(7) -0.0083(7) C32 0.0318(10) 0.0363(10) 0.0253(9) -0.0019(8) -0.0020(7) -0.0089(8) C33 0.0430(11) 0.0512(13) 0.0221(9) -0.0058(8) -0.0012(8) -0.0204(10) C34 0.0448(12) 0.0459(12) 0.0313(10) -0.0169(9) 0.0100(9) -0.0209(10) C35 0.0362(10) 0.0328(10) 0.0380(11) -0.0094(8) 0.0056(8) -0.0073(8) C36 0.0258(9) 0.0316(9) 0.0281(9) -0.0058(7) -0.0010(7) -0.0061(7) C37 0.0251(8) 0.0257(9) 0.0235(8) -0.0065(7) -0.0018(7) 0.0017(7) C38 0.0296(9) 0.0294(9) 0.0261(9) -0.0051(7) -0.0039(7) -0.0022(7) C39 0.0374(10) 0.0299(9) 0.0237(9) -0.0014(7) 0.0004(7) -0.0007(8) C40 0.0393(10) 0.0354(10) 0.0233(9) -0.0036(8) -0.0071(8) 0.0040(8) C41 0.0325(10) 0.0410(11) 0.0280(9) -0.0105(8) -0.0083(8) -0.0015(8) C42 0.0305(9) 0.0299(9) 0.0250(9) -0.0066(7) -0.0022(7) -0.0032(7) C43 0.0295(9) 0.0260(9) 0.0207(8) -0.0065(7) -0.0021(7) -0.0031(7) C44 0.0321(9) 0.0288(9) 0.0283(9) -0.0037(7) -0.0007(7) -0.0013(7) C45 0.0472(12) 0.0239(9) 0.0328(10) -0.0026(8) -0.0024(8) -0.0030(8) C46 0.0446(11) 0.0306(10) 0.0317(10) -0.0052(8) 0.0012(8) -0.0153(8) C47 0.0315(10) 0.0380(11) 0.0314(10) -0.0078(8) 0.0001(8) -0.0110(8) C48 0.0289(9) 0.0283(9) 0.0272(9) -0.0056(7) -0.0019(7) -0.0036(7) C49 0.0514(14) 0.0645(17) 0.0594(15) -0.0006(13) -0.0072(12) 0.0016(12) C50 0.075(6) 0.039(4) 0.028(4) -0.010(3) 0.012(4) -0.020(4) C51 0.0406(13) 0.0680(17) 0.0702(17) -0.0063(13) -0.0065(12) -0.0134(12) C52 0.0561(14) 0.0471(13) 0.0526(14) -0.0009(11) -0.0049(11) -0.0070(11) C53 0.0531(14) 0.0760(18) 0.0433(13) -0.0090(12) -0.0009(11) -0.0103(13) C54 0.0548(15) 0.0766(19) 0.0644(17) -0.0042(14) -0.0072(13) -0.0072(14) C55 0.114(3) 0.150(4) 0.096(3) -0.022(3) -0.053(2) -0.042(3) C56 0.112(3) 0.083(2) 0.134(3) -0.044(2) 0.048(3) -0.055(2) C501 0.059(2) 0.064(3) 0.050(2) 0.011(2) -0.0032(18) -0.0244(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3114(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ca1 . N1 . 2.5046(15) yes Ca1 . N3 . 2.5025(14) yes Ca1 . N5 . 2.5335(15) yes Ca1 . O1 . 2.3643(13) yes Ca1 . O2 . 2.3780(12) yes Ca1 . H2 . 2.36(3) no Ca1 . H3 . 2.40(3) no Ca1 . H4 . 2.33(2) no B1 . H1 . 1.15(3) no B1 . H2 . 1.22(3) no B1 . H3 . 1.19(3) no B1 . H4 . 1.14(2) no B2 . C25 . 1.651(3) yes B2 . C31 . 1.647(3) yes B2 . C37 . 1.650(3) yes B2 . C43 . 1.643(3) yes N1 . N2 . 1.374(2) yes N1 . C1 . 1.335(2) yes N2 . C3 . 1.362(2) yes N2 . C16 . 1.443(2) yes N3 . N4 . 1.372(2) yes N3 . C6 . 1.334(2) yes N4 . C8 . 1.364(2) yes N4 . C16 . 1.443(2) yes N5 . N6 . 1.371(2) yes N5 . C11 . 1.338(2) yes N6 . C13 . 1.366(2) yes N6 . C16 . 1.443(2) yes O1 . C17 . 1.442(2) yes O1 . C20 . 1.436(2) yes O2 . C21 . 1.455(2) yes O2 . C24 . 1.452(2) yes O3 . C49 . 1.400(3) yes O3 . C52 . 1.414(3) yes O4 . C53 . 1.409(3) yes O4 . C56 . 1.363(4) yes C1 . C2 . 1.405(3) yes C1 . C4 . 1.496(3) yes C2 . C3 . 1.376(3) yes C2 . H21 . 0.949 no C3 . C5 . 1.486(3) yes C4 . H41 . 0.949 no C4 . H42 . 0.950 no C4 . H43 . 0.951 no C5 . H51 . 0.950 no C5 . H52 . 0.951 no C5 . H53 . 0.949 no C6 . C7 . 1.407(3) yes C6 . C9 . 1.492(3) yes C7 . C8 . 1.368(3) yes C7 . H71 . 0.949 no C8 . C10 . 1.490(3) yes C9 . H91 . 0.949 no C9 . H92 . 0.949 no C9 . H93 . 0.950 no C10 . H101 . 0.949 no C10 . H102 . 0.949 no C10 . H103 . 0.950 no C11 . C12 . 1.405(3) yes C11 . C14 . 1.487(3) yes C12 . C13 . 1.368(3) yes C12 . H121 . 0.951 no C13 . C15 . 1.492(3) yes C14 . H141 . 0.951 no C14 . H142 . 0.949 no C14 . H143 . 0.949 no C15 . H151 . 0.949 no C15 . H152 . 0.951 no C15 . H153 . 0.949 no C16 . H161 . 0.950 no C17 . C18 . 1.494(3) yes C17 . H171 . 0.951 no C17 . H172 . 0.949 no C18 . C19 . 1.510(3) yes C18 . H181 . 0.950 no C18 . H182 . 0.951 no C19 . C20 . 1.503(3) yes C19 . H191 . 0.950 no C19 . H192 . 0.950 no C20 . H201 . 0.951 no C20 . H202 . 0.950 no C21 . C22 . 1.528(3) yes C21 . H211 . 0.950 no C21 . H212 . 0.950 no C22 . C23 . 1.531(3) yes C22 . H221 . 0.950 no C22 . H222 . 0.949 no C23 . C24 . 1.503(3) yes C23 . H231 . 0.949 no C23 . H232 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.951 no C25 . C26 . 1.406(3) yes C25 . C30 . 1.393(3) yes C26 . C27 . 1.394(3) yes C26 . H261 . 0.949 no C27 . C28 . 1.383(4) yes C27 . H271 . 0.950 no C28 . C29 . 1.377(4) yes C28 . H281 . 0.950 no C29 . C30 . 1.397(3) yes C29 . H291 . 0.949 no C30 . H301 . 0.950 no C31 . C32 . 1.402(3) yes C31 . C36 . 1.399(3) yes C32 . C33 . 1.393(3) yes C32 . H321 . 0.949 no C33 . C34 . 1.387(3) yes C33 . H331 . 0.949 no C34 . C35 . 1.381(3) yes C34 . H341 . 0.950 no C35 . C36 . 1.397(3) yes C35 . H351 . 0.949 no C36 . H361 . 0.949 no C37 . C38 . 1.404(3) yes C37 . C42 . 1.397(3) yes C38 . C39 . 1.389(3) yes C38 . H381 . 0.949 no C39 . C40 . 1.385(3) yes C39 . H391 . 0.950 no C40 . C41 . 1.383(3) yes C40 . H401 . 0.949 no C41 . C42 . 1.396(3) yes C41 . H411 . 0.949 no C42 . H421 . 0.950 no C43 . C44 . 1.401(3) yes C43 . C48 . 1.407(3) yes C44 . C45 . 1.397(3) yes C44 . H441 . 0.949 no C45 . C46 . 1.382(3) yes C45 . H451 . 0.949 no C46 . C47 . 1.384(3) yes C46 . H461 . 0.950 no C47 . C48 . 1.387(3) yes C47 . H471 . 0.949 no C48 . H481 . 0.949 no C49 . C50 . 1.492(4) yes C49 . C501 . 1.490(3) yes C49 . H491 . 0.950 no C49 . H492 . 0.949 no C50 . C51 . 1.499(4) yes C50 . C501 . 0.840(7) yes C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H5011 . 0.923 no C51 . C52 . 1.488(3) yes C51 . C501 . 1.478(3) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C52 . H521 . 0.950 no C52 . H522 . 0.950 no C53 . C54 . 1.486(3) yes C53 . H531 . 0.950 no C53 . H532 . 0.950 no C54 . C55 . 1.527(4) yes C54 . H541 . 0.951 no C54 . H542 . 0.949 no C55 . C56 . 1.490(4) yes C55 . H551 . 0.950 no C55 . H552 . 0.950 no C56 . H561 . 0.951 no C56 . H562 . 0.949 no C501 . H502 . 0.928 no C501 . H5011 . 0.950 no C501 . H5012 . 0.951 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ca1 . N3 . 73.34(5) yes N1 . Ca1 . N5 . 74.40(5) yes N3 . Ca1 . N5 . 74.42(5) yes N1 . Ca1 . O1 . 155.72(5) yes N3 . Ca1 . O1 . 94.82(5) yes N5 . Ca1 . O1 . 82.08(5) yes N1 . Ca1 . O2 . 86.42(5) yes N3 . Ca1 . O2 . 151.27(5) yes N5 . Ca1 . O2 . 80.70(5) yes O1 . Ca1 . O2 . 95.77(5) yes N1 . Ca1 . H2 . 129.9(7) no N3 . Ca1 . H2 . 98.9(7) no N5 . Ca1 . H2 . 152.7(7) no O1 . Ca1 . H2 . 72.0(7) no O2 . Ca1 . H2 . 109.8(7) no N1 . Ca1 . H3 . 98.6(7) no N3 . Ca1 . H3 . 127.9(7) no N5 . Ca1 . H3 . 154.5(7) no O1 . Ca1 . H3 . 105.2(7) no O2 . Ca1 . H3 . 74.3(7) no N1 . Ca1 . H4 . 83.2(6) no N3 . Ca1 . H4 . 81.9(6) no N5 . Ca1 . H4 . 151.1(6) no O1 . Ca1 . H4 . 116.7(6) no O2 . Ca1 . H4 . 116.4(6) no H2 . Ca1 . H3 . 46.9(9) no H2 . Ca1 . H4 . 46.8(9) no H3 . Ca1 . H4 . 46.1(9) no H1 . B1 . H2 . 113.2(18) no H1 . B1 . H3 . 110.5(18) no H2 . B1 . H3 . 103.9(18) no H1 . B1 . H4 . 117.8(17) no H2 . B1 . H4 . 104.6(17) no H3 . B1 . H4 . 105.7(18) no C25 . B2 . C31 . 112.27(14) yes C25 . B2 . C37 . 104.52(13) yes C31 . B2 . C37 . 110.04(14) yes C25 . B2 . C43 . 112.22(14) yes C31 . B2 . C43 . 104.91(13) yes C37 . B2 . C43 . 113.05(14) yes Ca1 . N1 . N2 . 119.43(10) yes Ca1 . N1 . C1 . 132.38(12) yes N2 . N1 . C1 . 104.46(14) yes N1 . N2 . C3 . 112.35(14) yes N1 . N2 . C16 . 120.64(14) yes C3 . N2 . C16 . 127.01(15) yes Ca1 . N3 . N4 . 118.68(10) yes Ca1 . N3 . C6 . 132.30(11) yes N4 . N3 . C6 . 104.85(14) yes N3 . N4 . C8 . 111.93(14) yes N3 . N4 . C16 . 120.66(13) yes C8 . N4 . C16 . 127.28(15) yes Ca1 . N5 . N6 . 118.54(10) yes Ca1 . N5 . C11 . 132.25(12) yes N6 . N5 . C11 . 104.49(14) yes N5 . N6 . C13 . 112.33(15) yes N5 . N6 . C16 . 120.47(13) yes C13 . N6 . C16 . 127.20(15) yes Ca1 . O1 . C17 . 125.66(12) yes Ca1 . O1 . C20 . 126.48(11) yes C17 . O1 . C20 . 105.72(15) yes Ca1 . O2 . C21 . 126.51(11) yes Ca1 . O2 . C24 . 125.12(11) yes C21 . O2 . C24 . 106.37(13) yes C49 . O3 . C52 . 109.44(18) yes C53 . O4 . C56 . 101.2(2) yes N1 . C1 . C2 . 111.08(16) yes N1 . C1 . C4 . 120.46(17) yes C2 . C1 . C4 . 128.46(17) yes C1 . C2 . C3 . 106.31(16) yes C1 . C2 . H21 . 126.7 no C3 . C2 . H21 . 126.9 no C2 . C3 . N2 . 105.79(16) yes C2 . C3 . C5 . 131.28(17) yes N2 . C3 . C5 . 122.93(17) yes C1 . C4 . H41 . 109.4 no C1 . C4 . H42 . 109.3 no H41 . C4 . H42 . 109.5 no C1 . C4 . H43 . 109.6 no H41 . C4 . H43 . 109.4 no H42 . C4 . H43 . 109.5 no C3 . C5 . H51 . 109.4 no C3 . C5 . H52 . 109.6 no H51 . C5 . H52 . 109.6 no C3 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.4 no H52 . C5 . H53 . 109.4 no N3 . C6 . C7 . 110.70(16) yes N3 . C6 . C9 . 120.40(16) yes C7 . C6 . C9 . 128.89(16) yes C6 . C7 . C8 . 106.48(16) yes C6 . C7 . H71 . 126.7 no C8 . C7 . H71 . 126.8 no C7 . C8 . N4 . 106.03(16) yes C7 . C8 . C10 . 131.69(17) yes N4 . C8 . C10 . 122.27(17) yes C6 . C9 . H91 . 110.3 no C6 . C9 . H92 . 108.4 no H91 . C9 . H92 . 110.1 no C6 . C9 . H93 . 108.3 no H91 . C9 . H93 . 110.2 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.5 no C8 . C10 . H102 . 109.6 no H101 . C10 . H102 . 109.4 no C8 . C10 . H103 . 109.4 no H101 . C10 . H103 . 109.4 no H102 . C10 . H103 . 109.6 no N5 . C11 . C12 . 110.74(17) yes N5 . C11 . C14 . 121.23(17) yes C12 . C11 . C14 . 128.00(17) yes C11 . C12 . C13 . 106.70(16) yes C11 . C12 . H121 . 126.6 no C13 . C12 . H121 . 126.7 no C12 . C13 . N6 . 105.73(16) yes C12 . C13 . C15 . 131.65(17) yes N6 . C13 . C15 . 122.62(18) yes C11 . C14 . H141 . 109.4 no C11 . C14 . H142 . 109.7 no H141 . C14 . H142 . 109.6 no C11 . C14 . H143 . 109.3 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.4 no C13 . C15 . H151 . 109.5 no C13 . C15 . H152 . 109.4 no H151 . C15 . H152 . 109.5 no C13 . C15 . H153 . 109.5 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.5 no N2 . C16 . N4 . 112.17(14) yes N2 . C16 . N6 . 112.04(14) yes N4 . C16 . N6 . 112.05(14) yes N2 . C16 . H161 . 106.8 no N4 . C16 . H161 . 106.8 no N6 . C16 . H161 . 106.6 no O1 . C17 . C18 . 105.39(18) yes O1 . C17 . H171 . 110.4 no C18 . C17 . H171 . 110.2 no O1 . C17 . H172 . 110.6 no C18 . C17 . H172 . 110.7 no H171 . C17 . H172 . 109.5 no C17 . C18 . C19 . 104.72(18) yes C17 . C18 . H181 . 111.0 no C19 . C18 . H181 . 110.8 no C17 . C18 . H182 . 110.3 no C19 . C18 . H182 . 110.4 no H181 . C18 . H182 . 109.5 no C18 . C19 . C20 . 105.05(17) yes C18 . C19 . H191 . 110.3 no C20 . C19 . H191 . 110.8 no C18 . C19 . H192 . 110.7 no C20 . C19 . H192 . 110.3 no H191 . C19 . H192 . 109.6 no C19 . C20 . O1 . 107.08(17) yes C19 . C20 . H201 . 109.8 no O1 . C20 . H201 . 109.8 no C19 . C20 . H202 . 110.4 no O1 . C20 . H202 . 110.2 no H201 . C20 . H202 . 109.5 no O2 . C21 . C22 . 106.26(16) yes O2 . C21 . H211 . 110.5 no C22 . C21 . H211 . 110.4 no O2 . C21 . H212 . 110.1 no C22 . C21 . H212 . 110.1 no H211 . C21 . H212 . 109.5 no C21 . C22 . C23 . 104.48(16) yes C21 . C22 . H221 . 110.5 no C23 . C22 . H221 . 110.5 no C21 . C22 . H222 . 110.9 no C23 . C22 . H222 . 111.0 no H221 . C22 . H222 . 109.5 no C22 . C23 . C24 . 102.31(16) yes C22 . C23 . H231 . 111.4 no C24 . C23 . H231 . 111.4 no C22 . C23 . H232 . 111.1 no C24 . C23 . H232 . 111.0 no H231 . C23 . H232 . 109.5 no C23 . C24 . O2 . 103.49(15) yes C23 . C24 . H241 . 110.7 no O2 . C24 . H241 . 110.9 no C23 . C24 . H242 . 111.2 no O2 . C24 . H242 . 110.9 no H241 . C24 . H242 . 109.5 no B2 . C25 . C26 . 118.21(16) yes B2 . C25 . C30 . 126.14(16) yes C26 . C25 . C30 . 115.41(17) yes C25 . C26 . C27 . 122.3(2) yes C25 . C26 . H261 . 118.8 no C27 . C26 . H261 . 118.9 no C26 . C27 . C28 . 120.5(2) yes C26 . C27 . H271 . 119.7 no C28 . C27 . H271 . 119.8 no C27 . C28 . C29 . 118.84(19) yes C27 . C28 . H281 . 120.4 no C29 . C28 . H281 . 120.8 no C28 . C29 . C30 . 120.3(2) yes C28 . C29 . H291 . 119.7 no C30 . C29 . H291 . 120.0 no C29 . C30 . C25 . 122.7(2) yes C29 . C30 . H301 . 118.8 no C25 . C30 . H301 . 118.5 no B2 . C31 . C32 . 121.01(16) yes B2 . C31 . C36 . 123.63(15) yes C32 . C31 . C36 . 115.25(16) yes C31 . C32 . C33 . 122.59(19) yes C31 . C32 . H321 . 118.5 no C33 . C32 . H321 . 118.9 no C32 . C33 . C34 . 120.32(19) yes C32 . C33 . H331 . 119.9 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 118.87(18) yes C33 . C34 . H341 . 120.6 no C35 . C34 . H341 . 120.5 no C34 . C35 . C36 . 120.10(19) yes C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 120.1 no C31 . C36 . C35 . 122.84(18) yes C31 . C36 . H361 . 118.5 no C35 . C36 . H361 . 118.6 no B2 . C37 . C38 . 118.47(15) yes B2 . C37 . C42 . 126.31(16) yes C38 . C37 . C42 . 115.22(16) yes C37 . C38 . C39 . 123.25(17) yes C37 . C38 . H381 . 118.4 no C39 . C38 . H381 . 118.4 no C38 . C39 . C40 . 119.58(18) yes C38 . C39 . H391 . 120.1 no C40 . C39 . H391 . 120.3 no C39 . C40 . C41 . 119.17(17) yes C39 . C40 . H401 . 120.2 no C41 . C40 . H401 . 120.6 no C40 . C41 . C42 . 120.33(17) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 119.9 no C37 . C42 . C41 . 122.37(18) yes C37 . C42 . H421 . 118.8 no C41 . C42 . H421 . 118.8 no B2 . C43 . C44 . 124.09(16) yes B2 . C43 . C48 . 120.73(15) yes C44 . C43 . C48 . 114.94(16) yes C43 . C44 . C45 . 122.46(18) yes C43 . C44 . H441 . 118.7 no C45 . C44 . H441 . 118.9 no C44 . C45 . C46 . 120.53(18) yes C44 . C45 . H451 . 119.7 no C46 . C45 . H451 . 119.8 no C45 . C46 . C47 . 118.81(18) yes C45 . C46 . H461 . 120.4 no C47 . C46 . H461 . 120.7 no C46 . C47 . C48 . 120.09(18) yes C46 . C47 . H471 . 119.8 no C48 . C47 . H471 . 120.1 no C43 . C48 . C47 . 123.15(17) yes C43 . C48 . H481 . 118.3 no C47 . C48 . H481 . 118.5 no O3 . C49 . C50 . 108.7(3) yes O3 . C49 . C501 . 106.0(2) yes C50 . C49 . C501 . 32.7(3) yes O3 . C49 . H491 . 110.4 no C50 . C49 . H491 . 79.3 no C501 . C49 . H491 . 110.3 no O3 . C49 . H492 . 109.9 no C50 . C49 . H492 . 133.7 no C501 . C49 . H492 . 110.7 no H491 . C49 . H492 . 109.5 no C49 . C50 . C51 . 102.7(3) yes C49 . C50 . C501 . 73.5(4) yes C51 . C50 . C501 . 72.2(4) yes C49 . C50 . H501 . 111.7 no C51 . C50 . H501 . 112.0 no C501 . C50 . H501 . 171.6 no C49 . C50 . H502 . 110.4 no C51 . C50 . H502 . 110.4 no C501 . C50 . H502 . 62.1 no H501 . C50 . H502 . 109.5 no C49 . C50 . H5011 . 112.6 no C51 . C50 . H5011 . 111.4 no C501 . C50 . H5011 . 65.0 no H501 . C50 . H5011 . 106.6 no H502 . C50 . H5011 . 3.0 no C50 . C51 . C52 . 105.1(3) yes C50 . C51 . C501 . 32.8(3) yes C52 . C51 . C501 . 103.8(2) yes C50 . C51 . H511 . 79.8 no C52 . C51 . H511 . 110.8 no C501 . C51 . H511 . 110.4 no C50 . C51 . H512 . 135.4 no C52 . C51 . H512 . 111.1 no C501 . C51 . H512 . 111.1 no H511 . C51 . H512 . 109.6 no C51 . C52 . O3 . 107.7(2) yes C51 . C52 . H521 . 110.1 no O3 . C52 . H521 . 109.8 no C51 . C52 . H522 . 109.8 no O3 . C52 . H522 . 109.8 no H521 . C52 . H522 . 109.5 no O4 . C53 . C54 . 107.4(2) yes O4 . C53 . H531 . 110.1 no C54 . C53 . H531 . 109.7 no O4 . C53 . H532 . 109.9 no C54 . C53 . H532 . 110.2 no H531 . C53 . H532 . 109.4 no C53 . C54 . C55 . 100.4(2) yes C53 . C54 . H541 . 112.1 no C55 . C54 . H541 . 111.6 no C53 . C54 . H542 . 111.4 no C55 . C54 . H542 . 111.8 no H541 . C54 . H542 . 109.5 no C54 . C55 . C56 . 103.5(3) yes C54 . C55 . H551 . 111.0 no C56 . C55 . H551 . 111.2 no C54 . C55 . H552 . 110.9 no C56 . C55 . H552 . 110.7 no H551 . C55 . H552 . 109.5 no C55 . C56 . O4 . 107.0(3) yes C55 . C56 . H561 . 110.3 no O4 . C56 . H561 . 109.4 no C55 . C56 . H562 . 110.0 no O4 . C56 . H562 . 110.6 no H561 . C56 . H562 . 109.5 no C49 . C501 . C51 . 103.8(2) yes C49 . C501 . C50 . 73.8(4) yes C51 . C501 . C50 . 75.0(4) yes C49 . C501 . H502 . 112.0 no C51 . C501 . H502 . 113.7 no C50 . C501 . H502 . 64.8 no C49 . C501 . H5011 . 111.0 no C51 . C501 . H5011 . 111.4 no C50 . C501 . H5011 . 61.7 no H502 . C501 . H5011 . 3.2 no C49 . C501 . H5012 . 110.7 no C51 . C501 . H5012 . 110.4 no C50 . C501 . H5012 . 171.1 no H502 . C501 . H5012 . 106.4 no H5011 . C501 . H5012 . 109.4 no B1 . H2 . Ca1 . 86.3(14) no B1 . H3 . Ca1 . 84.5(14) no B1 . H4 . Ca1 . 89.2(13) no C50 . H502 . C501 . 53.1 no C501 . H5011 . C50 . 53.3 no #===end