# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'John Arnold'
_publ_contact_author_email       arnold@berkeley.edu
loop_
_publ_author_name
J.Arnold
'Heather Buckley'
'Penny Brothers'
'Daniel Gryko'

data_shelxl_hb012
_database_code_depnum_ccdc_archive 'CCDC 897226'
#TrackingRef '- hb012 Li revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            HB012
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H77 Li3 N4 O9'
_chemical_formula_weight         1019.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   14.9866(8)
_cell_length_b                   23.6356(12)
_cell_length_c                   16.4784(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.871(4)
_cell_angle_gamma                90.00
_cell_volume                     5712.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9870
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      67.03

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9124
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            55039
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         67.77
_reflns_number_total             10121
_reflns_number_gt                7768
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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^)+(0.1192P)^2^+5.1550P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10121
_refine_ls_number_parameters     700
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.2106
_refine_ls_wR_factor_gt          0.1901
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group

Li1 Li 0.4537(3) 0.26123(19) -0.1360(3) 0.0350(10) Uani 1 1 d . . .
Li2 Li 0.4544(3) 0.24659(19) -0.0123(3) 0.0352(10) Uani 1 1 d . . .
Li3 Li 0.3315(4) 0.1544(2) 0.2312(3) 0.0438(11) Uani 1 1 d . . .
O1 O -0.04227(14) 0.04410(9) -0.25577(13) 0.0457(5) Uani 1 1 d . . .
O2 O 0.42599(14) 0.25995(8) -0.25592(11) 0.0383(4) Uani 1 1 d . . .
O3 O 0.43094(14) 0.31661(8) -0.40551(12) 0.0395(5) Uani 1 1 d . . .
O4 O 0.48798(15) 0.24062(8) 0.11051(12) 0.0420(5) Uani 1 1 d . . .
O5 O 0.38735(14) 0.13922(9) 0.13428(13) 0.0427(5) Uani 1 1 d . . .
O6 O 0.25090(15) 0.22009(10) 0.17570(14) 0.0509(5) Uani 1 1 d . . .
O7 O 0.20786(17) 0.13190(10) 0.25668(15) 0.0555(6) Uani 1 1 d . . .
O8 O 0.39255(17) 0.08007(11) 0.30147(15) 0.0574(6) Uani 1 1 d . . .
O9 O 0.41690(16) 0.19225(11) 0.32328(14) 0.0564(6) Uani 1 1 d . . .
C1 C 0.62506(19) 0.29896(11) -0.03153(16) 0.0337(6) Uani 1 1 d . . .
C2 C 0.7200(2) 0.28731(12) -0.00598(17) 0.0380(6) Uani 1 1 d . . .
H2 H 0.7667 0.3135 0.0162 0.046 Uiso 1 1 calc R . .
C3 C 0.73069(19) 0.23024(12) -0.01987(16) 0.0359(6) Uani 1 1 d . . .
H3 H 0.7864 0.2097 -0.0093 0.043 Uiso 1 1 calc R . .
C4 C 0.64200(18) 0.20794(11) -0.05323(15) 0.0319(5) Uani 1 1 d . . .
C5 C 0.61104(18) 0.15181(11) -0.07491(15) 0.0309(5) Uani 1 1 d . . .
C6 C 0.51739(18) 0.13812(11) -0.09590(15) 0.0295(5) Uani 1 1 d . . .
C7 C 0.47995(19) 0.08336(11) -0.12091(15) 0.0320(6) Uani 1 1 d . . .
H7 H 0.5137 0.0500 -0.1258 0.038 Uiso 1 1 calc R . .
C8 C 0.38776(19) 0.08785(11) -0.13635(15) 0.0314(5) Uani 1 1 d . . .
H8 H 0.3452 0.0583 -0.1536 0.038 Uiso 1 1 calc R . .
C9 C 0.36648(18) 0.14625(11) -0.12162(15) 0.0296(5) Uani 1 1 d . . .
C10 C 0.27808(18) 0.16994(11) -0.13169(15) 0.0303(5) Uani 1 1 d . . .
C11 C 0.26074(18) 0.22798(11) -0.11712(15) 0.0312(5) Uani 1 1 d . . .
C12 C 0.17268(19) 0.25494(12) -0.13557(17) 0.0363(6) Uani 1 1 d . . .
H12 H 0.1157 0.2372 -0.1564 0.044 Uiso 1 1 calc R . .
C13 C 0.1868(2) 0.31074(12) -0.11736(18) 0.0381(6) Uani 1 1 d . . .
H13 H 0.1413 0.3393 -0.1230 0.046 Uiso 1 1 calc R . .
C14 C 0.28294(19) 0.31865(11) -0.08800(16) 0.0336(6) Uani 1 1 d . . .
C15 C 0.3259(2) 0.37132(11) -0.06767(16) 0.0346(6) Uani 1 1 d . . .
C16 C 0.4223(2) 0.37675(11) -0.04854(16) 0.0340(6) Uani 1 1 d . . .
C17 C 0.4805(2) 0.42407(11) -0.02538(17) 0.0375(6) Uani 1 1 d . . .
H17 H 0.4617 0.4620 -0.0194 0.045 Uiso 1 1 calc R . .
C18 C 0.5693(2) 0.40493(11) -0.01304(17) 0.0376(6) Uani 1 1 d . . .
H18 H 0.6232 0.4268 0.0037 0.045 Uiso 1 1 calc R . .
C19 C 0.56418(19) 0.34573(11) -0.03044(16) 0.0330(6) Uani 1 1 d . . .
C20 C 0.68049(18) 0.10682(11) -0.07679(16) 0.0314(5) Uani 1 1 d . . .
C21 C 0.72550(19) 0.10378(12) -0.14366(17) 0.0356(6) Uani 1 1 d . . .
C22 C 0.79106(19) 0.06234(12) -0.14470(18) 0.0364(6) Uani 1 1 d . . .
H22 H 0.8208 0.0606 -0.1903 0.044 Uiso 1 1 calc R . .
C23 C 0.81428(19) 0.02324(11) -0.08062(18) 0.0373(6) Uani 1 1 d . . .
C24 C 0.76931(19) 0.02646(11) -0.01485(18) 0.0374(6) Uani 1 1 d . . .
H24 H 0.7841 0.0000 0.0293 0.045 Uiso 1 1 calc R . .
C25 C 0.70331(18) 0.06730(11) -0.01185(17) 0.0339(6) Uani 1 1 d . . .
C26 C 0.7016(2) 0.14416(14) -0.21604(19) 0.0468(7) Uani 1 1 d . . .
H26A H 0.6413 0.1346 -0.2490 0.070 Uiso 1 1 calc R . .
H26B H 0.7472 0.1410 -0.2508 0.070 Uiso 1 1 calc R . .
H26C H 0.7009 0.1830 -0.1953 0.070 Uiso 1 1 calc R . .
C27 C 0.8857(2) -0.02122(13) -0.0832(2) 0.0464(7) Uani 1 1 d . . .
H27A H 0.9397 -0.0035 -0.0972 0.070 Uiso 1 1 calc R . .
H27B H 0.8613 -0.0496 -0.1252 0.070 Uiso 1 1 calc R . .
H27C H 0.9026 -0.0395 -0.0288 0.070 Uiso 1 1 calc R . .
C28 C 0.6561(2) 0.06854(13) 0.06016(18) 0.0406(6) Uani 1 1 d . . .
H28A H 0.6900 0.0451 0.1052 0.061 Uiso 1 1 calc R . .
H28B H 0.5940 0.0537 0.0427 0.061 Uiso 1 1 calc R . .
H28C H 0.6535 0.1076 0.0796 0.061 Uiso 1 1 calc R . .
C29 C 0.2679(2) 0.42324(11) -0.07171(17) 0.0359(6) Uani 1 1 d . . .
C30 C 0.2242(2) 0.43834(12) -0.00788(19) 0.0433(7) Uani 1 1 d . . .
C31 C 0.1699(2) 0.48674(12) -0.0153(2) 0.0466(7) Uani 1 1 d . . .
H31 H 0.1414 0.4968 0.0291 0.056 Uiso 1 1 calc R . .
C32 C 0.1561(2) 0.52045(12) -0.08509(19) 0.0424(7) Uani 1 1 d . . .
C33 C 0.1990(2) 0.50480(12) -0.14856(18) 0.0439(7) Uani 1 1 d . . .
H33 H 0.1901 0.5273 -0.1974 0.053 Uiso 1 1 calc R . .
C34 C 0.2547(2) 0.45737(11) -0.14330(17) 0.0391(6) Uani 1 1 d . . .
C35 C 0.2309(3) 0.40164(15) 0.0681(2) 0.0620(10) Uani 1 1 d . . .
H35A H 0.2911 0.3837 0.0814 0.093 Uiso 1 1 calc R . .
H35B H 0.1837 0.3723 0.0573 0.093 Uiso 1 1 calc R . .
H35C H 0.2222 0.4250 0.1150 0.093 Uiso 1 1 calc R . .
C36 C 0.0966(3) 0.57234(13) -0.0933(2) 0.0537(8) Uani 1 1 d . . .
H36A H 0.1330 0.6049 -0.0690 0.081 Uiso 1 1 calc R . .
H36B H 0.0467 0.5662 -0.0641 0.081 Uiso 1 1 calc R . .
H36C H 0.0714 0.5797 -0.1521 0.081 Uiso 1 1 calc R . .
C37 C 0.2975(3) 0.44156(14) -0.21502(19) 0.0525(8) Uani 1 1 d . . .
H37A H 0.2907 0.4730 -0.2546 0.079 Uiso 1 1 calc R . .
H37B H 0.2672 0.4079 -0.2425 0.079 Uiso 1 1 calc R . .
H37C H 0.3624 0.4335 -0.1947 0.079 Uiso 1 1 calc R . .
C38 C 0.19717(18) 0.13394(10) -0.16356(16) 0.0309(5) Uani 1 1 d . . .
C39 C 0.1310(2) 0.12371(12) -0.11701(17) 0.0360(6) Uani 1 1 d . . .
H39 H 0.1400 0.1381 -0.0621 0.043 Uiso 1 1 calc R . .
C40 C 0.0531(2) 0.09333(12) -0.14826(17) 0.0382(6) Uani 1 1 d . . .
H40 H 0.0093 0.0869 -0.1149 0.046 Uiso 1 1 calc R . .
C41 C 0.03849(19) 0.07211(12) -0.22885(17) 0.0367(6) Uani 1 1 d . . .
C42 C 0.1039(2) 0.08045(12) -0.27563(17) 0.0391(6) Uani 1 1 d . . .
H42 H 0.0957 0.0652 -0.3300 0.047 Uiso 1 1 calc R . .
C43 C 0.18148(19) 0.11119(12) -0.24274(17) 0.0350(6) Uani 1 1 d . . .
H43 H 0.2257 0.1169 -0.2757 0.042 Uiso 1 1 calc R . .
C44 C -0.0630(3) 0.02827(18) -0.3412(2) 0.0606(10) Uani 1 1 d . . .
H44A H -0.0233 -0.0030 -0.3503 0.091 Uiso 1 1 calc R . .
H44B H -0.0530 0.0607 -0.3753 0.091 Uiso 1 1 calc R . .
H44C H -0.1268 0.0163 -0.3566 0.091 Uiso 1 1 calc R . .
C45 C 0.4372(2) 0.20669(13) -0.29351(19) 0.0465(7) Uani 1 1 d . . .
H45A H 0.4476 0.2129 -0.3496 0.070 Uiso 1 1 calc R . .
H45B H 0.3820 0.1839 -0.2964 0.070 Uiso 1 1 calc R . .
H45C H 0.4895 0.1868 -0.2603 0.070 Uiso 1 1 calc R . .
C46 C 0.3507(2) 0.29186(13) -0.30054(18) 0.0411(6) Uani 1 1 d . . .
H46A H 0.3153 0.3074 -0.2612 0.049 Uiso 1 1 calc R . .
H46B H 0.3100 0.2666 -0.3396 0.049 Uiso 1 1 calc R . .
C47 C 0.3824(2) 0.33938(13) -0.34779(18) 0.0424(7) Uani 1 1 d . . .
H47A H 0.3294 0.3614 -0.3774 0.051 Uiso 1 1 calc R . .
H47B H 0.4225 0.3651 -0.3090 0.051 Uiso 1 1 calc R . .
C48 C 0.4535(2) 0.35874(15) -0.4589(2) 0.0520(8) Uani 1 1 d . . .
H48A H 0.4875 0.3892 -0.4258 0.078 Uiso 1 1 calc R . .
H48B H 0.3975 0.3741 -0.4932 0.078 Uiso 1 1 calc R . .
H48C H 0.4912 0.3421 -0.4948 0.078 Uiso 1 1 calc R . .
C49 C 0.5279(3) 0.29250(15) 0.1486(2) 0.0565(9) Uani 1 1 d . . .
H49A H 0.5940 0.2917 0.1524 0.085 Uiso 1 1 calc R . .
H49B H 0.5150 0.2960 0.2043 0.085 Uiso 1 1 calc R . .
H49C H 0.5017 0.3249 0.1148 0.085 Uiso 1 1 calc R . .
C50 C 0.5262(2) 0.19299(14) 0.15647(19) 0.0445(7) Uani 1 1 d . . .
H50A H 0.5200 0.1968 0.2149 0.053 Uiso 1 1 calc R . .
H50B H 0.5920 0.1903 0.1556 0.053 Uiso 1 1 calc R . .
C51 C 0.4777(2) 0.14040(13) 0.11908(19) 0.0443(7) Uani 1 1 d . . .
H51A H 0.4753 0.1399 0.0586 0.053 Uiso 1 1 calc R . .
H51B H 0.5116 0.1065 0.1437 0.053 Uiso 1 1 calc R . .
C52 C 0.3326(3) 0.09949(16) 0.0807(2) 0.0549(8) Uani 1 1 d . . .
H52A H 0.3246 0.1125 0.0231 0.082 Uiso 1 1 calc R . .
H52B H 0.2729 0.0963 0.0957 0.082 Uiso 1 1 calc R . .
H52C H 0.3627 0.0625 0.0863 0.082 Uiso 1 1 calc R . .
C53 C 0.2611(3) 0.24589(18) 0.0998(3) 0.0678(11) Uani 1 1 d . . .
H53A H 0.2353 0.2210 0.0532 0.102 Uiso 1 1 calc R . .
H53B H 0.3260 0.2521 0.1008 0.102 Uiso 1 1 calc R . .
H53C H 0.2290 0.2823 0.0932 0.102 Uiso 1 1 calc R . .
C54 C 0.1571(2) 0.21151(17) 0.1767(2) 0.0580(9) Uani 1 1 d . . .
H54A H 0.1275 0.1889 0.1280 0.070 Uiso 1 1 calc R . .
H54B H 0.1252 0.2483 0.1748 0.070 Uiso 1 1 calc R . .
C55 C 0.1523(2) 0.18088(17) 0.2547(2) 0.0580(9) Uani 1 1 d . . .
H55A H 0.1753 0.2051 0.3035 0.070 Uiso 1 1 calc R . .
H55B H 0.0886 0.1700 0.2551 0.070 Uiso 1 1 calc R . .
C56 C 0.1907(3) 0.09260(19) 0.3154(3) 0.0843(14) Uani 1 1 d . . .
H56A H 0.2088 0.1088 0.3711 0.126 Uiso 1 1 calc R . .
H56B H 0.2258 0.0580 0.3118 0.126 Uiso 1 1 calc R . .
H56C H 0.1255 0.0835 0.3043 0.126 Uiso 1 1 calc R . .
C57 C 0.4081(3) 0.02543(16) 0.2702(3) 0.0674(10) Uani 1 1 d . . .
H57A H 0.4612 0.0269 0.2442 0.101 Uiso 1 1 calc R . .
H57B H 0.3543 0.0137 0.2290 0.101 Uiso 1 1 calc R . .
H57C H 0.4193 -0.0019 0.3159 0.101 Uiso 1 1 calc R . .
C58 C 0.4688(3) 0.09991(19) 0.3597(2) 0.0646(10) Uani 1 1 d . . .
H58A H 0.5215 0.1047 0.3327 0.078 Uiso 1 1 calc R . .
H58B H 0.4858 0.0722 0.4054 0.078 Uiso 1 1 calc R . .
C59 C 0.4450(3) 0.1546(2) 0.3928(2) 0.0665(10) Uani 1 1 d . . .
H59A H 0.3948 0.1495 0.4229 0.080 Uiso 1 1 calc R . .
H59B H 0.4983 0.1704 0.4317 0.080 Uiso 1 1 calc R . .
C60 C 0.4028(3) 0.24890(17) 0.3467(3) 0.0654(10) Uani 1 1 d . . .
H60A H 0.3549 0.2497 0.3792 0.098 Uiso 1 1 calc R . .
H60B H 0.3844 0.2722 0.2969 0.098 Uiso 1 1 calc R . .
H60C H 0.4596 0.2639 0.3803 0.098 Uiso 1 1 calc R . .
N1 N 0.58033(15) 0.25086(9) -0.06024(14) 0.0334(5) Uani 1 1 d . . .
N2 N 0.44589(14) 0.17560(9) -0.09612(13) 0.0294(5) Uani 1 1 d . . .
N3 N 0.32675(15) 0.26686(9) -0.08747(13) 0.0308(5) Uani 1 1 d . . .
N4 N 0.47560(16) 0.33033(9) -0.05144(14) 0.0359(5) 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
C53 0.072(3) 0.064(2) 0.071(3) 0.0243(19) 0.022(2) 0.013(2)
Li1 0.040(3) 0.035(2) 0.028(2) 0.0010(17) 0.0030(18) -0.0024(19)
Li2 0.039(2) 0.034(2) 0.031(2) -0.0015(17) 0.0031(18) -0.0015(19)
Li3 0.044(3) 0.048(3) 0.039(3) -0.002(2) 0.008(2) -0.002(2)
O1 0.0421(11) 0.0544(13) 0.0417(11) -0.0123(9) 0.0109(9) -0.0172(10)
O2 0.0465(11) 0.0358(10) 0.0310(10) 0.0011(8) 0.0041(8) 0.0043(8)
O3 0.0416(11) 0.0378(10) 0.0383(10) 0.0077(8) 0.0062(8) -0.0009(8)
O4 0.0532(13) 0.0382(11) 0.0329(10) -0.0031(8) 0.0048(9) -0.0079(9)
O5 0.0429(11) 0.0435(11) 0.0423(11) -0.0051(9) 0.0101(9) -0.0051(9)
O6 0.0470(12) 0.0517(13) 0.0544(13) 0.0053(10) 0.0116(10) 0.0014(10)
O7 0.0635(15) 0.0455(13) 0.0634(15) 0.0006(10) 0.0267(12) -0.0050(11)
O8 0.0558(14) 0.0570(14) 0.0571(14) 0.0085(11) 0.0063(11) -0.0027(11)
O9 0.0549(14) 0.0666(15) 0.0489(13) -0.0120(11) 0.0137(11) -0.0104(12)
C1 0.0403(15) 0.0314(13) 0.0275(13) -0.0013(10) 0.0028(11) -0.0050(11)
C2 0.0374(15) 0.0368(14) 0.0361(14) -0.0016(11) -0.0011(12) -0.0071(12)
C3 0.0339(14) 0.0392(15) 0.0325(14) 0.0003(11) 0.0018(11) -0.0007(11)
C4 0.0339(14) 0.0320(13) 0.0280(12) 0.0011(10) 0.0021(10) 0.0010(11)
C5 0.0345(14) 0.0317(13) 0.0251(12) -0.0005(10) 0.0031(10) 0.0035(11)
C6 0.0353(14) 0.0286(12) 0.0237(12) 0.0012(9) 0.0034(10) 0.0025(10)
C7 0.0386(15) 0.0280(13) 0.0291(13) -0.0025(10) 0.0062(11) 0.0031(11)
C8 0.0393(15) 0.0260(12) 0.0274(12) -0.0024(9) 0.0035(11) -0.0035(10)
C9 0.0342(14) 0.0275(12) 0.0264(12) 0.0019(9) 0.0050(10) -0.0011(10)
C10 0.0342(14) 0.0289(13) 0.0271(12) 0.0009(9) 0.0046(10) 0.0002(10)
C11 0.0351(14) 0.0292(13) 0.0281(12) 0.0011(10) 0.0038(10) -0.0003(11)
C12 0.0349(15) 0.0338(14) 0.0371(14) 0.0000(11) 0.0001(11) 0.0028(11)
C13 0.0391(15) 0.0328(14) 0.0406(15) 0.0013(11) 0.0035(12) 0.0068(12)
C14 0.0411(15) 0.0289(13) 0.0293(13) 0.0008(10) 0.0036(11) 0.0020(11)
C15 0.0464(16) 0.0266(13) 0.0294(13) 0.0004(10) 0.0047(11) 0.0023(11)
C16 0.0449(16) 0.0265(12) 0.0290(13) -0.0003(10) 0.0037(11) 0.0012(11)
C17 0.0530(17) 0.0260(13) 0.0339(14) -0.0032(10) 0.0099(12) -0.0046(12)
C18 0.0475(17) 0.0300(14) 0.0343(14) -0.0029(11) 0.0060(12) -0.0073(12)
C19 0.0373(14) 0.0309(13) 0.0288(13) -0.0007(10) 0.0020(11) -0.0041(11)
C20 0.0291(13) 0.0291(13) 0.0328(13) -0.0040(10) -0.0009(10) -0.0006(10)
C21 0.0354(14) 0.0344(14) 0.0350(14) -0.0041(11) 0.0024(11) -0.0009(11)
C22 0.0336(14) 0.0353(14) 0.0396(15) -0.0073(11) 0.0060(11) -0.0003(11)
C23 0.0305(14) 0.0291(13) 0.0494(16) -0.0078(11) 0.0018(12) -0.0031(11)
C24 0.0374(15) 0.0268(13) 0.0437(16) 0.0026(11) -0.0016(12) -0.0023(11)
C25 0.0325(14) 0.0312(13) 0.0352(14) -0.0027(10) 0.0003(11) -0.0032(11)
C26 0.0576(19) 0.0484(17) 0.0360(15) 0.0008(13) 0.0133(14) 0.0101(15)
C27 0.0388(16) 0.0330(15) 0.066(2) -0.0003(13) 0.0083(14) 0.0026(12)
C28 0.0447(16) 0.0376(15) 0.0380(15) 0.0065(12) 0.0051(12) 0.0032(12)
C29 0.0441(16) 0.0261(13) 0.0350(14) -0.0022(10) 0.0022(12) -0.0012(11)
C30 0.0546(18) 0.0338(15) 0.0422(16) 0.0032(12) 0.0113(14) 0.0042(13)
C31 0.062(2) 0.0328(15) 0.0476(17) -0.0017(12) 0.0178(15) 0.0062(14)
C32 0.0527(18) 0.0262(13) 0.0459(16) -0.0023(11) 0.0048(13) 0.0006(12)
C33 0.0600(19) 0.0301(14) 0.0367(15) 0.0046(11) -0.0012(13) 0.0032(13)
C34 0.0537(17) 0.0283(13) 0.0326(14) -0.0024(11) 0.0027(12) 0.0008(12)
C35 0.090(3) 0.0502(19) 0.054(2) 0.0155(16) 0.0345(19) 0.0262(19)
C36 0.069(2) 0.0321(15) 0.058(2) 0.0008(14) 0.0082(17) 0.0106(15)
C37 0.074(2) 0.0480(18) 0.0352(16) 0.0045(13) 0.0098(15) 0.0154(16)
C38 0.0345(14) 0.0242(12) 0.0326(13) 0.0019(10) 0.0032(11) 0.0024(10)
C39 0.0409(15) 0.0379(14) 0.0286(13) -0.0045(11) 0.0056(11) -0.0035(12)
C40 0.0404(15) 0.0422(15) 0.0344(14) -0.0027(11) 0.0129(12) -0.0051(12)
C41 0.0343(14) 0.0371(14) 0.0380(14) -0.0042(11) 0.0055(12) -0.0052(11)
C42 0.0439(16) 0.0415(15) 0.0319(14) -0.0084(11) 0.0082(12) -0.0068(12)
C43 0.0348(14) 0.0368(14) 0.0349(14) -0.0015(11) 0.0104(11) -0.0038(11)
C44 0.058(2) 0.077(2) 0.0471(19) -0.0148(17) 0.0114(16) -0.0291(19)
C45 0.064(2) 0.0379(16) 0.0385(16) -0.0019(12) 0.0116(14) 0.0030(14)
C46 0.0435(16) 0.0462(16) 0.0332(14) 0.0022(12) 0.0066(12) 0.0063(13)
C47 0.0489(17) 0.0385(15) 0.0367(15) 0.0016(12) 0.0016(13) 0.0074(13)
C48 0.0491(19) 0.0514(19) 0.0559(19) 0.0172(15) 0.0121(15) -0.0065(15)
C49 0.078(2) 0.0494(19) 0.0412(17) -0.0068(14) 0.0094(16) -0.0164(17)
C50 0.0401(16) 0.0544(18) 0.0387(16) 0.0034(13) 0.0071(13) -0.0023(14)
C51 0.0506(18) 0.0442(16) 0.0404(16) 0.0027(12) 0.0147(13) 0.0026(14)
C52 0.061(2) 0.058(2) 0.0451(18) -0.0099(15) 0.0103(15) -0.0158(17)
C54 0.0406(18) 0.060(2) 0.070(2) -0.0044(17) 0.0040(16) -0.0003(15)
C55 0.0432(18) 0.071(2) 0.064(2) -0.0051(18) 0.0213(16) 0.0026(16)
C56 0.089(3) 0.064(3) 0.116(4) 0.020(2) 0.059(3) 0.000(2)
C57 0.075(3) 0.053(2) 0.074(3) 0.0084(18) 0.014(2) 0.0036(19)
C58 0.054(2) 0.084(3) 0.052(2) 0.0031(19) 0.0010(17) 0.0015(19)
C59 0.060(2) 0.096(3) 0.0423(19) -0.0044(19) 0.0078(16) -0.002(2)
C60 0.056(2) 0.076(3) 0.069(2) -0.029(2) 0.0244(18) -0.0126(19)
N1 0.0345(12) 0.0288(11) 0.0344(12) -0.0037(9) 0.0015(9) -0.0015(9)
N2 0.0321(11) 0.0278(11) 0.0277(10) 0.0000(8) 0.0045(9) 0.0016(9)
N3 0.0359(12) 0.0255(10) 0.0297(11) -0.0007(8) 0.0033(9) 0.0010(9)
N4 0.0411(13) 0.0257(11) 0.0378(12) -0.0018(9) 0.0012(10) -0.0015(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C53 O6 1.428(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
Li1 O2 1.934(5) . ?
Li1 N1 2.061(5) . ?
Li1 Li2 2.065(6) . ?
Li1 N4 2.128(5) . ?
Li1 N2 2.138(5) . ?
Li1 N3 2.214(5) . ?
Li2 O4 1.988(5) . ?
Li2 N3 2.108(5) . ?
Li2 N4 2.126(5) . ?
Li2 N2 2.160(5) . ?
Li2 N1 2.193(5) . ?
Li3 O5 1.982(5) . ?
Li3 O9 1.986(6) . ?
Li3 O7 2.052(6) . ?
Li3 O6 2.062(6) . ?
Li3 O8 2.198(6) . ?
O1 C41 1.371(3) . ?
O1 C44 1.428(4) . ?
O2 C45 1.428(3) . ?
O2 C46 1.429(3) . ?
O3 C48 1.415(3) . ?
O3 C47 1.417(4) . ?
O4 C50 1.411(4) . ?
O4 C49 1.449(4) . ?
O5 C51 1.428(4) . ?
O5 C52 1.427(4) . ?
O6 C54 1.424(4) . ?
O7 C56 1.403(5) . ?
O7 C55 1.423(4) . ?
O8 C58 1.413(4) . ?
O8 C57 1.427(5) . ?
O9 C60 1.421(4) . ?
O9 C59 1.444(5) . ?
C1 N1 1.355(3) . ?
C1 C2 1.425(4) . ?
C1 C19 1.436(4) . ?
C2 C3 1.383(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.430(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.361(3) . ?
C4 C5 1.427(4) . ?
C5 C6 1.412(4) . ?
C5 C20 1.493(4) . ?
C6 N2 1.390(3) . ?
C6 C7 1.437(4) . ?
C7 C8 1.356(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.449(4) . ?
C8 H8 0.9500 . ?
C9 N2 1.367(3) . ?
C9 C10 1.416(4) . ?
C10 C11 1.426(4) . ?
C10 C38 1.486(4) . ?
C11 N3 1.365(3) . ?
C11 C12 1.441(4) . ?
C12 C13 1.359(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.434(4) . ?
C13 H13 0.9500 . ?
C14 N3 1.388(3) . ?
C14 C15 1.410(4) . ?
C15 C16 1.421(4) . ?
C15 C29 1.497(4) . ?
C16 N4 1.364(3) . ?
C16 C17 1.421(4) . ?
C17 C18 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.427(4) . ?
C18 H18 0.9500 . ?
C19 N4 1.351(4) . ?
C20 C21 1.407(4) . ?
C20 C25 1.409(4) . ?
C21 C22 1.390(4) . ?
C21 C26 1.512(4) . ?
C22 C23 1.393(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(4) . ?
C23 C27 1.506(4) . ?
C24 C25 1.390(4) . ?
C24 H24 0.9500 . ?
C25 C28 1.502(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.394(4) . ?
C29 C34 1.409(4) . ?
C30 C31 1.395(4) . ?
C30 C35 1.510(4) . ?
C31 C32 1.379(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.387(4) . ?
C32 C36 1.506(4) . ?
C33 C34 1.389(4) . ?
C33 H33 0.9500 . ?
C34 C37 1.503(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C43 1.386(4) . ?
C38 C39 1.394(4) . ?
C39 C40 1.378(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.394(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.380(4) . ?
C42 C43 1.384(4) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.499(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.506(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C54 C55 1.490(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.475(6) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 C53 H53A 109.5 . . ?
O6 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
O6 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O2 Li1 N1 126.5(3) . . ?
O2 Li1 Li2 164.2(3) . . ?
N1 Li1 Li2 64.2(2) . . ?
O2 Li1 N4 130.8(2) . . ?
N1 Li1 N4 72.27(17) . . ?
Li2 Li1 N4 60.89(19) . . ?
O2 Li1 N2 106.6(2) . . ?
N1 Li1 N2 78.63(18) . . ?
Li2 Li1 N2 61.81(18) . . ?
N4 Li1 N2 122.4(2) . . ?
O2 Li1 N3 110.5(2) . . ?
N1 Li1 N3 122.7(2) . . ?
Li2 Li1 N3 58.92(19) . . ?
N4 Li1 N3 75.27(17) . . ?
N2 Li1 N3 80.83(17) . . ?
O4 Li2 Li1 164.9(3) . . ?
O4 Li2 N3 128.6(3) . . ?
Li1 Li2 N3 64.1(2) . . ?
O4 Li2 N4 110.6(2) . . ?
Li1 Li2 N4 61.02(19) . . ?
N3 Li2 N4 77.57(18) . . ?
O4 Li2 N2 124.4(2) . . ?
Li1 Li2 N2 60.77(19) . . ?
N3 Li2 N2 82.78(18) . . ?
N4 Li2 N2 121.5(2) . . ?
O4 Li2 N1 108.2(2) . . ?
Li1 Li2 N1 57.80(19) . . ?
N3 Li2 N1 121.5(2) . . ?
N4 Li2 N1 69.78(16) . . ?
N2 Li2 N1 75.38(17) . . ?
O5 Li3 O9 112.6(3) . . ?
O5 Li3 O7 131.8(3) . . ?
O9 Li3 O7 115.3(3) . . ?
O5 Li3 O6 94.9(2) . . ?
O9 Li3 O6 103.1(3) . . ?
O7 Li3 O6 79.3(2) . . ?
O5 Li3 O8 94.6(2) . . ?
O9 Li3 O8 79.9(2) . . ?
O7 Li3 O8 88.9(2) . . ?
O6 Li3 O8 168.0(3) . . ?
C41 O1 C44 116.4(2) . . ?
C45 O2 C46 113.1(2) . . ?
C45 O2 Li1 115.9(2) . . ?
C46 O2 Li1 119.9(2) . . ?
C48 O3 C47 111.8(2) . . ?
C50 O4 C49 110.9(2) . . ?
C50 O4 Li2 126.4(2) . . ?
C49 O4 Li2 112.1(2) . . ?
C51 O5 C52 110.5(2) . . ?
C51 O5 Li3 135.3(2) . . ?
C52 O5 Li3 109.5(2) . . ?
C54 O6 C53 110.8(3) . . ?
C54 O6 Li3 112.2(3) . . ?
C53 O6 Li3 123.5(3) . . ?
C56 O7 C55 111.4(3) . . ?
C56 O7 Li3 127.9(3) . . ?
C55 O7 Li3 109.5(2) . . ?
C58 O8 C57 112.1(3) . . ?
C58 O8 Li3 106.5(3) . . ?
C57 O8 Li3 127.9(3) . . ?
C60 O9 C59 113.6(3) . . ?
C60 O9 Li3 121.6(3) . . ?
C59 O9 Li3 111.4(3) . . ?
N1 C1 C2 109.5(2) . . ?
N1 C1 C19 112.4(2) . . ?
C2 C1 C19 138.0(3) . . ?
C3 C2 C1 106.4(2) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.0(2) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 119.5(2) . . ?
N1 C4 C3 108.6(2) . . ?
C5 C4 C3 131.9(2) . . ?
C6 C5 C4 122.0(2) . . ?
C6 C5 C20 119.6(2) . . ?
C4 C5 C20 118.4(2) . . ?
N2 C6 C5 125.6(2) . . ?
N2 C6 C7 108.5(2) . . ?
C5 C6 C7 125.9(2) . . ?
C8 C7 C6 107.8(2) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
C7 C8 C9 107.1(2) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
N2 C9 C10 124.7(2) . . ?
N2 C9 C8 109.1(2) . . ?
C10 C9 C8 126.2(2) . . ?
C9 C10 C11 124.0(2) . . ?
C9 C10 C38 119.4(2) . . ?
C11 C10 C38 116.5(2) . . ?
N3 C11 C10 124.3(2) . . ?
N3 C11 C12 110.0(2) . . ?
C10 C11 C12 125.5(2) . . ?
C13 C12 C11 106.7(2) . . ?
C13 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
C12 C13 C14 107.5(2) . . ?
C12 C13 H13 126.2 . . ?
C14 C13 H13 126.2 . . ?
N3 C14 C15 125.8(3) . . ?
N3 C14 C13 109.2(2) . . ?
C15 C14 C13 124.9(3) . . ?
C14 C15 C16 121.8(2) . . ?
C14 C15 C29 118.7(3) . . ?
C16 C15 C29 119.4(2) . . ?
N4 C16 C15 119.7(2) . . ?
N4 C16 C17 108.2(3) . . ?
C15 C16 C17 132.1(3) . . ?
C18 C17 C16 107.5(2) . . ?
C18 C17 H17 126.2 . . ?
C16 C17 H17 126.2 . . ?
C17 C18 C19 106.3(2) . . ?
C17 C18 H18 126.8 . . ?
C19 C18 H18 126.8 . . ?
N4 C19 C18 109.0(2) . . ?
N4 C19 C1 112.5(2) . . ?
C18 C19 C1 138.5(3) . . ?
C21 C20 C25 118.7(2) . . ?
C21 C20 C5 120.1(2) . . ?
C25 C20 C5 121.2(2) . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 C26 119.2(3) . . ?
C20 C21 C26 120.8(2) . . ?
C21 C22 C23 121.7(3) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C24 C23 C22 118.0(3) . . ?
C24 C23 C27 121.4(3) . . ?
C22 C23 C27 120.7(3) . . ?
C25 C24 C23 121.9(3) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C20 119.8(3) . . ?
C24 C25 C28 119.7(2) . . ?
C20 C25 C28 120.5(2) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 118.6(3) . . ?
C30 C29 C15 122.3(2) . . ?
C34 C29 C15 119.1(2) . . ?
C29 C30 C31 120.0(3) . . ?
C29 C30 C35 121.2(3) . . ?
C31 C30 C35 118.8(3) . . ?
C32 C31 C30 122.1(3) . . ?
C32 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
C31 C32 C33 117.5(3) . . ?
C31 C32 C36 122.0(3) . . ?
C33 C32 C36 120.5(3) . . ?
C32 C33 C34 122.3(3) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
C33 C34 C29 119.6(3) . . ?
C33 C34 C37 120.0(3) . . ?
C29 C34 C37 120.5(3) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C43 C38 C39 116.7(2) . . ?
C43 C38 C10 121.5(2) . . ?
C39 C38 C10 121.7(2) . . ?
C40 C39 C38 122.0(2) . . ?
C40 C39 H39 119.0 . . ?
C38 C39 H39 119.0 . . ?
C39 C40 C41 119.9(3) . . ?
C39 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
O1 C41 C42 124.7(2) . . ?
O1 C41 C40 115.9(2) . . ?
C42 C41 C40 119.4(3) . . ?
C41 C42 C43 119.5(3) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C42 C43 C38 122.6(2) . . ?
C42 C43 H43 118.7 . . ?
C38 C43 H43 118.7 . . ?
O1 C44 H44A 109.5 . . ?
O1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O2 C45 H45A 109.5 . . ?
O2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O2 C46 C47 111.2(2) . . ?
O2 C46 H46A 109.4 . . ?
C47 C46 H46A 109.4 . . ?
O2 C46 H46B 109.4 . . ?
C47 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
O3 C47 C46 109.0(2) . . ?
O3 C47 H47A 109.9 . . ?
C46 C47 H47A 109.9 . . ?
O3 C47 H47B 109.9 . . ?
C46 C47 H47B 109.9 . . ?
H47A C47 H47B 108.3 . . ?
O3 C48 H48A 109.5 . . ?
O3 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O3 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O4 C49 H49A 109.5 . . ?
O4 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O4 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O4 C50 C51 109.3(2) . . ?
O4 C50 H50A 109.8 . . ?
C51 C50 H50A 109.8 . . ?
O4 C50 H50B 109.8 . . ?
C51 C50 H50B 109.8 . . ?
H50A C50 H50B 108.3 . . ?
O5 C51 C50 109.9(2) . . ?
O5 C51 H51A 109.7 . . ?
C50 C51 H51A 109.7 . . ?
O5 C51 H51B 109.7 . . ?
C50 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?
O5 C52 H52A 109.5 . . ?
O5 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O5 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C54 C55 107.6(3) . . ?
O6 C54 H54A 110.2 . . ?
C55 C54 H54A 110.2 . . ?
O6 C54 H54B 110.2 . . ?
C55 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?
O7 C55 C54 106.4(3) . . ?
O7 C55 H55A 110.4 . . ?
C54 C55 H55A 110.4 . . ?
O7 C55 H55B 110.4 . . ?
C54 C55 H55B 110.4 . . ?
H55A C55 H55B 108.6 . . ?
O7 C56 H56A 109.5 . . ?
O7 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O7 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O8 C57 H57A 109.5 . . ?
O8 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O8 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O8 C58 C59 108.5(3) . . ?
O8 C58 H58A 110.0 . . ?
C59 C58 H58A 110.0 . . ?
O8 C58 H58B 110.0 . . ?
C59 C58 H58B 110.0 . . ?
H58A C58 H58B 108.4 . . ?
O9 C59 C58 107.5(3) . . ?
O9 C59 H59A 110.2 . . ?
C58 C59 H59A 110.2 . . ?
O9 C59 H59B 110.2 . . ?
C58 C59 H59B 110.2 . . ?
H59A C59 H59B 108.5 . . ?
O9 C60 H60A 109.5 . . ?
O9 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O9 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C1 N1 C4 108.5(2) . . ?
C1 N1 Li1 116.1(2) . . ?
C4 N1 Li1 131.7(2) . . ?
C1 N1 Li2 108.3(2) . . ?
C4 N1 Li2 123.7(2) . . ?
Li1 N1 Li2 57.98(19) . . ?
C9 N2 C6 107.4(2) . . ?
C9 N2 Li1 119.0(2) . . ?
C6 N2 Li1 120.9(2) . . ?
C9 N2 Li2 121.6(2) . . ?
C6 N2 Li2 123.3(2) . . ?
Li1 N2 Li2 57.42(18) . . ?
C11 N3 C14 106.5(2) . . ?
C11 N3 Li2 124.1(2) . . ?
C14 N3 Li2 125.1(2) . . ?
C11 N3 Li1 116.3(2) . . ?
C14 N3 Li1 119.4(2) . . ?
Li2 N3 Li1 57.02(18) . . ?
C19 N4 C16 109.0(2) . . ?
C19 N4 Li2 111.9(2) . . ?
C16 N4 Li2 127.8(2) . . ?
C19 N4 Li1 112.7(2) . . ?
C16 N4 Li1 128.9(2) . . ?
Li2 N4 Li1 58.08(18) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.070

# Attachment '- hb026 - Zr.cif'

data_shelxl_hb026
_database_code_depnum_ccdc_archive 'CCDC 897227'
#TrackingRef '- hb026 - Zr.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            HB026
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H42 N4 O Zr'
_chemical_formula_weight         794.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.2272(9)
_cell_length_b                   19.8419(10)
_cell_length_c                   20.2471(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7724.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3296
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9342
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            127751
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         26.18
_reflns_number_total             7116
_reflns_number_gt                5315
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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^)+(0.0333P)^2^+9.2735P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7116
_refine_ls_number_parameters     503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.004
_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
C1 C 0.87162(13) 0.29401(13) 0.30864(12) 0.0172(6) Uani 1 1 d . . .
C2 C 0.89584(13) 0.22660(13) 0.29552(13) 0.0212(6) Uani 1 1 d . . .
H2 H 0.9009 0.2067 0.2531 0.025 Uiso 1 1 calc R . .
C3 C 0.91055(13) 0.19573(13) 0.35553(12) 0.0197(6) Uani 1 1 d . . .
H3 H 0.9271 0.1511 0.3619 0.024 Uiso 1 1 calc R . .
C4 C 0.89586(12) 0.24462(13) 0.40600(12) 0.0166(6) Uani 1 1 d . . .
C5 C 0.90918(12) 0.24328(13) 0.47472(12) 0.0163(6) Uani 1 1 d . . .
C6 C 0.90623(12) 0.30280(13) 0.51476(12) 0.0170(6) Uani 1 1 d . . .
C7 C 0.92332(13) 0.30915(14) 0.58294(13) 0.0210(6) Uani 1 1 d . . .
H7 H 0.9362 0.2733 0.6115 0.025 Uiso 1 1 calc R . .
C8 C 0.91800(13) 0.37706(14) 0.60081(13) 0.0212(6) Uani 1 1 d . . .
H8 H 0.9267 0.3947 0.6436 0.025 Uiso 1 1 calc R . .
C9 C 0.89727(13) 0.41592(13) 0.54404(12) 0.0183(6) Uani 1 1 d . . .
C10 C 0.88849(12) 0.48859(13) 0.53932(12) 0.0182(6) Uani 1 1 d . . .
C11 C 0.87272(13) 0.52578(13) 0.48119(12) 0.0190(6) Uani 1 1 d . . .
C12 C 0.87002(14) 0.59969(13) 0.47299(13) 0.0222(6) Uani 1 1 d . . .
H12 H 0.8769 0.6321 0.5069 0.027 Uiso 1 1 calc R . .
C13 C 0.85597(14) 0.61344(14) 0.40840(13) 0.0221(6) Uani 1 1 d . . .
H13 H 0.8513 0.6569 0.3892 0.026 Uiso 1 1 calc R . .
C14 C 0.84932(13) 0.54861(13) 0.37400(13) 0.0184(6) Uani 1 1 d . . .
C15 C 0.83887(13) 0.53766(13) 0.30630(13) 0.0190(6) Uani 1 1 d . . .
C16 C 0.83988(12) 0.47130(13) 0.27669(12) 0.0176(6) Uani 1 1 d . . .
C17 C 0.84502(13) 0.45112(14) 0.20954(13) 0.0219(6) Uani 1 1 d . . .
H17 H 0.8422 0.4802 0.1724 0.026 Uiso 1 1 calc R . .
C18 C 0.85511(13) 0.38035(14) 0.20712(13) 0.0208(6) Uani 1 1 d . . .
H18 H 0.8605 0.3539 0.1683 0.025 Uiso 1 1 calc R . .
C19 C 0.85572(12) 0.35609(13) 0.27329(12) 0.0174(6) Uani 1 1 d . . .
C20 C 0.93255(13) 0.17655(13) 0.50461(12) 0.0178(6) Uani 1 1 d . . .
C21 C 0.88674(13) 0.12338(13) 0.51973(12) 0.0188(6) Uani 1 1 d . . .
C22 C 0.91016(15) 0.06314(14) 0.54989(13) 0.0233(6) Uani 1 1 d . . .
H22 H 0.8776 0.0283 0.5588 0.028 Uiso 1 1 calc R . .
C23 C 0.97768(15) 0.05392(14) 0.56643(13) 0.0260(7) Uani 1 1 d . . .
C24 C 1.02231(15) 0.10598(15) 0.54905(14) 0.0283(7) Uani 1 1 d . . .
H24 H 1.0704 0.1004 0.5586 0.034 Uiso 1 1 calc R . .
C25 C 1.00149(13) 0.16700(14) 0.51810(13) 0.0224(6) Uani 1 1 d . . .
C26 C 0.81276(14) 0.13132(15) 0.50401(15) 0.0278(7) Uani 1 1 d . . .
H26A H 0.7976 0.1768 0.5162 0.042 Uiso 1 1 calc R . .
H26B H 0.7856 0.0980 0.5288 0.042 Uiso 1 1 calc R . .
H26C H 0.8056 0.1245 0.4566 0.042 Uiso 1 1 calc R . .
C27 C 1.00104(18) -0.01007(15) 0.60314(15) 0.0371(8) Uani 1 1 d . . .
H27A H 1.0120 0.0012 0.6491 0.056 Uiso 1 1 calc R . .
H27B H 1.0425 -0.0287 0.5816 0.056 Uiso 1 1 calc R . .
H27C H 0.9636 -0.0435 0.6021 0.056 Uiso 1 1 calc R . .
C28 C 1.05270(14) 0.22133(16) 0.49984(16) 0.0348(7) Uani 1 1 d . . .
H28A H 1.0379 0.2430 0.4587 0.052 Uiso 1 1 calc R . .
H28B H 1.0989 0.2013 0.4938 0.052 Uiso 1 1 calc R . .
H28C H 1.0546 0.2550 0.5352 0.052 Uiso 1 1 calc R . .
C29 C 0.89624(13) 0.52994(13) 0.60103(12) 0.0188(6) Uani 1 1 d . . .
C30 C 0.84022(14) 0.54256(14) 0.64104(13) 0.0246(6) Uani 1 1 d . . .
H30 H 0.7963 0.5240 0.6296 0.030 Uiso 1 1 calc R . .
C31 C 0.84541(14) 0.58156(14) 0.69773(14) 0.0265(7) Uani 1 1 d . . .
H31 H 0.8052 0.5890 0.7239 0.032 Uiso 1 1 calc R . .
C32 C 0.90670(14) 0.60915(14) 0.71640(13) 0.0223(6) Uani 1 1 d . . .
C33 C 0.96345(14) 0.59682(15) 0.67830(14) 0.0288(7) Uani 1 1 d . . .
H33 H 1.0074 0.6148 0.6906 0.035 Uiso 1 1 calc R . .
C34 C 0.95745(14) 0.55760(15) 0.62091(14) 0.0295(7) Uani 1 1 d . . .
H34 H 0.9978 0.5501 0.5949 0.035 Uiso 1 1 calc R . .
C35 C 0.96704(15) 0.68021(16) 0.79333(14) 0.0312(7) Uani 1 1 d . . .
H35A H 1.0034 0.6467 0.8019 0.047 Uiso 1 1 calc R . .
H35B H 0.9580 0.7061 0.8337 0.047 Uiso 1 1 calc R . .
H35C H 0.9825 0.7108 0.7583 0.047 Uiso 1 1 calc R . .
C36 C 0.82970(14) 0.59867(13) 0.26136(13) 0.0206(6) Uani 1 1 d . . .
C37 C 0.76435(15) 0.61731(14) 0.24176(14) 0.0262(6) Uani 1 1 d . . .
C38 C 0.75681(18) 0.67124(15) 0.19622(14) 0.0352(8) Uani 1 1 d . . .
H38 H 0.7112 0.6834 0.1827 0.042 Uiso 1 1 calc R . .
C39 C 0.81176(19) 0.70666(15) 0.17073(14) 0.0357(8) Uani 1 1 d . . .
C40 C 0.87532(18) 0.68776(15) 0.19132(14) 0.0333(7) Uani 1 1 d . . .
H40 H 0.9148 0.7112 0.1749 0.040 Uiso 1 1 calc R . .
C41 C 0.88557(15) 0.63405(14) 0.23677(13) 0.0258(6) Uani 1 1 d . . .
C42 C 0.70391(15) 0.58057(16) 0.26958(16) 0.0367(8) Uani 1 1 d . . .
H42A H 0.7122 0.5319 0.2665 0.055 Uiso 1 1 calc R . .
H42B H 0.6619 0.5922 0.2446 0.055 Uiso 1 1 calc R . .
H42C H 0.6977 0.5933 0.3160 0.055 Uiso 1 1 calc R . .
C43 C 0.8006(2) 0.76515(16) 0.12159(16) 0.0547(11) Uani 1 1 d . . .
H43A H 0.8457 0.7847 0.1097 0.082 Uiso 1 1 calc R . .
H43B H 0.7714 0.7998 0.1421 0.082 Uiso 1 1 calc R . .
H43C H 0.7776 0.7481 0.0818 0.082 Uiso 1 1 calc R . .
C44 C 0.95558(15) 0.61575(16) 0.25900(15) 0.0338(7) Uani 1 1 d . . .
H44A H 0.9625 0.6315 0.3044 0.051 Uiso 1 1 calc R . .
H44B H 0.9901 0.6368 0.2300 0.051 Uiso 1 1 calc R . .
H44C H 0.9610 0.5667 0.2574 0.051 Uiso 1 1 calc R . .
C45 C 0.70498(14) 0.34391(17) 0.38980(15) 0.0335(7) Uani 1 1 d . . .
H45 H 0.6991 0.3180 0.3507 0.040 Uiso 1 1 calc R . .
C46 C 0.72276(13) 0.31856(15) 0.45157(14) 0.0263(7) Uani 1 1 d . . .
H46 H 0.7311 0.2727 0.4623 0.032 Uiso 1 1 calc R . .
C47 C 0.72606(14) 0.37426(17) 0.49582(14) 0.0354(8) Uani 1 1 d . . .
H47 H 0.7369 0.3720 0.5415 0.043 Uiso 1 1 calc R . .
C48 C 0.71006(15) 0.43455(17) 0.4592(2) 0.0444(9) Uani 1 1 d . . .
H48 H 0.7086 0.4792 0.4760 0.053 Uiso 1 1 calc R . .
C49 C 0.69716(15) 0.41458(19) 0.39467(18) 0.0437(9) Uani 1 1 d . . .
H49 H 0.6850 0.4438 0.3593 0.052 Uiso 1 1 calc R . .
N1 N 0.87078(10) 0.30333(10) 0.37604(10) 0.0160(5) Uani 1 1 d . . .
N2 N 0.88950(10) 0.36930(11) 0.49215(10) 0.0168(5) Uani 1 1 d . . .
N3 N 0.85921(10) 0.49548(10) 0.42027(10) 0.0169(5) Uani 1 1 d . . .
N4 N 0.84459(10) 0.41185(10) 0.31426(10) 0.0170(5) Uani 1 1 d . . .
O1 O 0.90590(9) 0.64742(10) 0.77350(9) 0.0289(5) Uani 1 1 d . . .
Zr1 Zr 0.820706(12) 0.392574(12) 0.415305(12) 0.01496(8) 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
C1 0.0134(12) 0.0218(15) 0.0162(13) -0.0028(12) 0.0007(10) -0.0017(11)
C2 0.0229(14) 0.0224(15) 0.0185(14) -0.0028(12) 0.0022(11) 0.0010(12)
C3 0.0201(13) 0.0172(14) 0.0217(14) 0.0001(12) 0.0008(11) 0.0026(11)
C4 0.0114(12) 0.0177(14) 0.0208(14) 0.0023(12) 0.0006(10) -0.0005(10)
C5 0.0097(12) 0.0200(14) 0.0192(13) 0.0034(12) 0.0003(10) 0.0010(10)
C6 0.0132(12) 0.0205(15) 0.0172(13) 0.0022(12) 0.0007(10) 0.0018(11)
C7 0.0212(13) 0.0237(15) 0.0181(14) 0.0040(13) -0.0010(11) 0.0035(11)
C8 0.0185(13) 0.0298(16) 0.0152(13) -0.0009(12) -0.0029(10) 0.0019(12)
C9 0.0144(13) 0.0230(15) 0.0174(14) -0.0023(12) -0.0009(10) -0.0005(11)
C10 0.0133(12) 0.0225(15) 0.0188(14) -0.0018(12) 0.0006(10) -0.0013(11)
C11 0.0164(13) 0.0217(15) 0.0190(14) -0.0034(12) 0.0025(11) 0.0002(11)
C12 0.0256(14) 0.0178(15) 0.0232(15) -0.0046(12) 0.0011(11) -0.0013(12)
C13 0.0257(14) 0.0168(14) 0.0236(15) 0.0029(13) 0.0001(11) 0.0007(12)
C14 0.0141(12) 0.0193(14) 0.0218(14) 0.0043(12) 0.0013(11) 0.0004(11)
C15 0.0159(13) 0.0201(15) 0.0210(14) 0.0023(12) 0.0007(10) 0.0004(11)
C16 0.0123(12) 0.0221(15) 0.0183(13) 0.0044(12) -0.0015(10) -0.0007(11)
C17 0.0226(14) 0.0241(16) 0.0191(14) 0.0052(12) -0.0015(11) 0.0004(12)
C18 0.0209(14) 0.0262(16) 0.0152(13) -0.0027(12) -0.0015(11) -0.0008(12)
C19 0.0150(13) 0.0197(14) 0.0176(14) -0.0021(12) 0.0003(10) -0.0005(11)
C20 0.0204(13) 0.0198(14) 0.0132(13) -0.0019(12) -0.0008(10) 0.0040(11)
C21 0.0215(13) 0.0192(15) 0.0157(13) -0.0015(11) 0.0015(11) 0.0025(11)
C22 0.0332(16) 0.0207(15) 0.0159(14) 0.0009(12) 0.0029(12) 0.0002(12)
C23 0.0393(17) 0.0230(16) 0.0157(14) -0.0017(12) -0.0009(12) 0.0136(14)
C24 0.0251(15) 0.0324(17) 0.0274(15) -0.0019(14) -0.0061(12) 0.0093(14)
C25 0.0184(13) 0.0236(15) 0.0253(15) -0.0006(13) -0.0034(11) 0.0041(12)
C26 0.0237(15) 0.0244(15) 0.0353(17) 0.0038(14) 0.0015(12) -0.0014(12)
C27 0.051(2) 0.0317(18) 0.0284(17) 0.0045(15) -0.0046(14) 0.0150(16)
C28 0.0193(15) 0.0385(18) 0.0466(19) 0.0060(16) -0.0062(13) 0.0005(13)
C29 0.0231(14) 0.0167(14) 0.0165(14) 0.0005(11) 0.0001(10) 0.0015(11)
C30 0.0192(14) 0.0276(16) 0.0271(16) -0.0046(13) 0.0003(11) -0.0050(12)
C31 0.0237(15) 0.0304(16) 0.0253(15) -0.0051(14) 0.0089(12) -0.0055(13)
C32 0.0260(15) 0.0206(15) 0.0202(14) -0.0022(13) 0.0022(11) -0.0022(12)
C33 0.0197(14) 0.0393(18) 0.0275(15) -0.0087(14) -0.0022(12) -0.0050(13)
C34 0.0199(14) 0.0425(18) 0.0260(16) -0.0110(14) 0.0044(12) 0.0001(13)
C35 0.0302(16) 0.0395(18) 0.0240(15) -0.0099(14) -0.0009(13) -0.0088(14)
C36 0.0271(15) 0.0174(14) 0.0173(13) -0.0022(12) -0.0036(11) 0.0010(12)
C37 0.0319(16) 0.0211(15) 0.0257(15) -0.0026(13) -0.0054(12) 0.0058(12)
C38 0.049(2) 0.0288(17) 0.0278(17) -0.0040(15) -0.0116(15) 0.0161(15)
C39 0.070(2) 0.0199(16) 0.0168(15) -0.0001(13) -0.0042(15) 0.0072(16)
C40 0.055(2) 0.0248(17) 0.0201(15) 0.0022(14) 0.0032(14) -0.0066(15)
C41 0.0362(17) 0.0238(15) 0.0173(14) 0.0004(13) -0.0002(12) -0.0034(13)
C42 0.0262(16) 0.0365(18) 0.047(2) -0.0044(16) -0.0066(14) 0.0072(14)
C43 0.110(3) 0.0294(19) 0.0245(18) 0.0073(16) -0.0059(19) 0.021(2)
C44 0.0317(16) 0.0393(19) 0.0305(17) 0.0069(15) 0.0026(13) -0.0104(14)
C45 0.0165(14) 0.056(2) 0.0279(16) 0.0008(16) 0.0003(12) -0.0088(14)
C46 0.0144(13) 0.0318(17) 0.0328(17) 0.0081(15) 0.0018(12) -0.0041(12)
C47 0.0205(15) 0.066(2) 0.0194(15) -0.0049(16) 0.0080(12) -0.0132(15)
C48 0.0212(16) 0.0311(19) 0.081(3) -0.0156(19) 0.0252(17) -0.0006(14)
C49 0.0163(15) 0.062(2) 0.053(2) 0.022(2) 0.0013(14) 0.0047(15)
N1 0.0147(10) 0.0177(12) 0.0157(11) 0.0003(10) 0.0003(9) 0.0024(9)
N2 0.0165(11) 0.0181(12) 0.0159(11) -0.0008(10) -0.0005(9) 0.0014(9)
N3 0.0153(11) 0.0185(12) 0.0167(11) 0.0007(10) -0.0001(9) 0.0019(9)
N4 0.0148(10) 0.0189(12) 0.0174(11) 0.0014(10) 0.0012(9) 0.0001(9)
O1 0.0252(10) 0.0384(12) 0.0230(10) -0.0138(9) 0.0061(8) -0.0099(9)
Zr1 0.01271(12) 0.01670(14) 0.01547(13) 0.00078(11) 0.00081(10) 0.00080(10)

_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
C1 N1 1.377(3) . ?
C1 C2 1.441(4) . ?
C1 C19 1.457(4) . ?
C2 C3 1.390(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.437(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.399(3) . ?
C4 C5 1.415(3) . ?
C5 C6 1.434(4) . ?
C5 C20 1.524(4) . ?
C6 C7 1.425(4) . ?
C6 N2 1.433(3) . ?
C7 C8 1.399(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.440(4) . ?
C8 H8 0.9500 . ?
C9 N2 1.408(3) . ?
C9 C10 1.455(4) . ?
C10 C11 1.422(4) . ?
C10 C29 1.502(4) . ?
C11 N3 1.396(3) . ?
C11 C12 1.477(4) . ?
C12 C13 1.363(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.468(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.402(4) . ?
C14 N3 1.423(3) . ?
C15 C16 1.447(4) . ?
C15 C36 1.525(4) . ?
C16 N4 1.406(3) . ?
C16 C17 1.421(4) . ?
C17 C18 1.418(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.424(4) . ?
C18 H18 0.9500 . ?
C19 N4 1.399(3) . ?
C20 C25 1.367(3) . ?
C20 C21 1.408(4) . ?
C21 C22 1.416(4) . ?
C21 C26 1.466(4) . ?
C22 C23 1.353(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(4) . ?
C23 C27 1.538(4) . ?
C24 C25 1.421(4) . ?
C24 H24 0.9500 . ?
C25 C28 1.506(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C34 1.360(4) . ?
C29 C30 1.371(4) . ?
C30 C31 1.388(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.353(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.359(4) . ?
C32 O1 1.383(3) . ?
C33 C34 1.403(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 O1 1.402(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.369(4) . ?
C36 C41 1.376(4) . ?
C37 C38 1.420(4) . ?
C37 C42 1.483(4) . ?
C38 C39 1.370(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.345(4) . ?
C39 C43 1.544(4) . ?
C40 C41 1.422(4) . ?
C40 H40 0.9500 . ?
C41 C44 1.465(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.391(4) . ?
C45 C49 1.414(5) . ?
C45 Zr1 2.480(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.424(4) . ?
C46 Zr1 2.498(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.441(5) . ?
C47 Zr1 2.470(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.388(5) . ?
C48 Zr1 2.452(3) . ?
C48 H48 0.9500 . ?
C49 Zr1 2.451(3) . ?
C49 H49 0.9500 . ?
N1 Zr1 2.167(2) . ?
N2 Zr1 2.094(2) . ?
N3 Zr1 2.174(2) . ?
N4 Zr1 2.131(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.1(2) . . ?
N1 C1 C19 111.8(2) . . ?
C2 C1 C19 139.6(2) . . ?
C3 C2 C1 108.3(2) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
C2 C3 C4 106.5(2) . . ?
C2 C3 H3 126.7 . . ?
C4 C3 H3 126.7 . . ?
N1 C4 C5 120.3(2) . . ?
N1 C4 C3 108.8(2) . . ?
C5 C4 C3 130.6(2) . . ?
C4 C5 C6 122.2(2) . . ?
C4 C5 C20 117.4(2) . . ?
C6 C5 C20 120.2(2) . . ?
C7 C6 N2 106.3(2) . . ?
C7 C6 C5 127.7(2) . . ?
N2 C6 C5 125.9(2) . . ?
C8 C7 C6 108.6(2) . . ?
C8 C7 H7 125.7 . . ?
C6 C7 H7 125.7 . . ?
C7 C8 C9 109.2(2) . . ?
C7 C8 H8 125.4 . . ?
C9 C8 H8 125.4 . . ?
N2 C9 C8 105.8(2) . . ?
N2 C9 C10 126.2(2) . . ?
C8 C9 C10 128.0(2) . . ?
C11 C10 C9 126.4(2) . . ?
C11 C10 C29 115.2(2) . . ?
C9 C10 C29 118.4(2) . . ?
N3 C11 C10 123.2(2) . . ?
N3 C11 C12 108.8(2) . . ?
C10 C11 C12 128.0(2) . . ?
C13 C12 C11 108.3(2) . . ?
C13 C12 H12 125.9 . . ?
C11 C12 H12 125.9 . . ?
C12 C13 C14 107.3(2) . . ?
C12 C13 H13 126.4 . . ?
C14 C13 H13 126.4 . . ?
C15 C14 N3 123.2(2) . . ?
C15 C14 C13 127.7(2) . . ?
N3 C14 C13 109.0(2) . . ?
C14 C15 C16 123.0(2) . . ?
C14 C15 C36 118.5(2) . . ?
C16 C15 C36 118.5(2) . . ?
N4 C16 C17 106.1(2) . . ?
N4 C16 C15 122.7(2) . . ?
C17 C16 C15 130.8(2) . . ?
C18 C17 C16 108.8(2) . . ?
C18 C17 H17 125.6 . . ?
C16 C17 H17 125.6 . . ?
C17 C18 C19 107.7(2) . . ?
C17 C18 H18 126.2 . . ?
C19 C18 H18 126.2 . . ?
N4 C19 C18 106.8(2) . . ?
N4 C19 C1 114.2(2) . . ?
C18 C19 C1 138.6(2) . . ?
C25 C20 C21 117.3(2) . . ?
C25 C20 C5 119.1(2) . . ?
C21 C20 C5 123.6(2) . . ?
C20 C21 C22 121.8(2) . . ?
C20 C21 C26 118.6(2) . . ?
C22 C21 C26 119.5(2) . . ?
C23 C22 C21 121.7(3) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C24 115.4(3) . . ?
C22 C23 C27 120.8(3) . . ?
C24 C23 C27 123.8(3) . . ?
C23 C24 C25 124.9(3) . . ?
C23 C24 H24 117.6 . . ?
C25 C24 H24 117.6 . . ?
C20 C25 C24 118.7(3) . . ?
C20 C25 C28 119.1(2) . . ?
C24 C25 C28 122.3(2) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C29 C30 115.6(2) . . ?
C34 C29 C10 123.6(2) . . ?
C30 C29 C10 120.9(2) . . ?
C29 C30 C31 122.3(2) . . ?
C29 C30 H30 118.9 . . ?
C31 C30 H30 118.9 . . ?
C32 C31 C30 121.3(3) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 117.9(3) . . ?
C31 C32 O1 116.5(2) . . ?
C33 C32 O1 125.6(2) . . ?
C32 C33 C34 120.3(3) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C29 C34 C33 122.7(3) . . ?
C29 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
O1 C35 H35A 109.5 . . ?
O1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C41 118.3(2) . . ?
C37 C36 C15 119.6(2) . . ?
C41 C36 C15 122.0(2) . . ?
C36 C37 C38 119.0(3) . . ?
C36 C37 C42 118.5(3) . . ?
C38 C37 C42 122.5(3) . . ?
C39 C38 C37 123.5(3) . . ?
C39 C38 H38 118.2 . . ?
C37 C38 H38 118.2 . . ?
C40 C39 C38 116.2(3) . . ?
C40 C39 C43 122.4(3) . . ?
C38 C39 C43 121.4(3) . . ?
C39 C40 C41 122.4(3) . . ?
C39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
C36 C41 C40 120.5(3) . . ?
C36 C41 C44 118.7(2) . . ?
C40 C41 C44 120.8(3) . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C49 108.8(3) . . ?
C46 C45 Zr1 74.51(16) . . ?
C49 C45 Zr1 72.23(17) . . ?
C46 C45 H45 125.6 . . ?
C49 C45 H45 125.6 . . ?
Zr1 C45 H45 119.4 . . ?
C45 C46 C47 107.2(3) . . ?
C45 C46 Zr1 73.04(16) . . ?
C47 C46 Zr1 72.25(15) . . ?
C45 C46 H46 126.4 . . ?
C47 C46 H46 126.4 . . ?
Zr1 C46 H46 120.2 . . ?
C46 C47 C48 108.1(3) . . ?
C46 C47 Zr1 74.44(15) . . ?
C48 C47 Zr1 72.28(16) . . ?
C46 C47 H47 125.9 . . ?
C48 C47 H47 125.9 . . ?
Zr1 C47 H47 119.2 . . ?
C49 C48 C47 106.6(3) . . ?
C49 C48 Zr1 73.54(17) . . ?
C47 C48 Zr1 73.68(16) . . ?
C49 C48 H48 126.7 . . ?
C47 C48 H48 126.7 . . ?
Zr1 C48 H48 118.2 . . ?
C48 C49 C45 109.3(3) . . ?
C48 C49 Zr1 73.57(17) . . ?
C45 C49 Zr1 74.46(17) . . ?
C48 C49 H49 125.4 . . ?
C45 C49 H49 125.4 . . ?
Zr1 C49 H49 118.4 . . ?
C1 N1 C4 108.3(2) . . ?
C1 N1 Zr1 118.59(16) . . ?
C4 N1 Zr1 132.42(16) . . ?
C9 N2 C6 110.0(2) . . ?
C9 N2 Zr1 118.47(16) . . ?
C6 N2 Zr1 125.61(16) . . ?
C11 N3 C14 106.7(2) . . ?
C11 N3 Zr1 120.56(16) . . ?
C14 N3 Zr1 128.29(16) . . ?
C19 N4 C16 110.6(2) . . ?
C19 N4 Zr1 117.39(16) . . ?
C16 N4 Zr1 130.98(17) . . ?
C32 O1 C35 119.0(2) . . ?
N2 Zr1 N4 128.08(8) . . ?
N2 Zr1 N1 79.14(8) . . ?
N4 Zr1 N1 72.47(8) . . ?
N2 Zr1 N3 87.57(8) . . ?
N4 Zr1 N3 78.61(8) . . ?
N1 Zr1 N3 129.28(8) . . ?
N2 Zr1 C49 141.10(10) . . ?
N4 Zr1 C49 90.76(10) . . ?
N1 Zr1 C49 120.91(11) . . ?
N3 Zr1 C49 99.82(10) . . ?
N2 Zr1 C48 110.72(11) . . ?
N4 Zr1 C48 118.30(11) . . ?
N1 Zr1 C48 142.78(9) . . ?
N3 Zr1 C48 87.69(9) . . ?
C49 Zr1 C48 32.89(12) . . ?
N2 Zr1 C47 86.70(9) . . ?
N4 Zr1 C47 144.95(9) . . ?
N1 Zr1 C47 116.70(10) . . ?
N3 Zr1 C47 111.01(9) . . ?
C49 Zr1 C47 54.88(11) . . ?
C48 Zr1 C47 34.04(11) . . ?
N2 Zr1 C45 129.47(9) . . ?
N4 Zr1 C45 93.63(9) . . ?
N1 Zr1 C45 90.24(10) . . ?
N3 Zr1 C45 132.90(10) . . ?
C49 Zr1 C45 33.31(11) . . ?
C48 Zr1 C45 55.19(11) . . ?
C47 Zr1 C45 54.49(10) . . ?
N2 Zr1 C46 97.36(9) . . ?
N4 Zr1 C46 123.37(9) . . ?
N1 Zr1 C46 87.84(9) . . ?
N3 Zr1 C46 142.66(9) . . ?
C49 Zr1 C46 54.86(10) . . ?
C48 Zr1 C46 55.88(10) . . ?
C47 Zr1 C46 33.31(10) . . ?
C45 Zr1 C46 32.44(9) . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.067

# Attachment '- hb028b Ti.cif'

data_shelxl_hb028b
_database_code_depnum_ccdc_archive 'CCDC 897228'
#TrackingRef '- hb028b Ti.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            HB028b
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H52 N4 O Ti'
_chemical_formula_weight         820.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8502(10)
_cell_length_b                   14.0504(13)
_cell_length_c                   14.6264(13)
_cell_angle_alpha                96.477(4)
_cell_angle_beta                 93.780(4)
_cell_angle_gamma                104.095(4)
_cell_volume                     2138.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      4.64
_cell_measurement_theta_max      67.33

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7921
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            34085
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         68.13
_reflns_number_total             7564
_reflns_number_gt                7230
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2011
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX

_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^)+(0.0690P)^2^+0.9522P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7564
_refine_ls_number_parameters     553
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35729(16) 0.60471(12) 0.51412(11) 0.0292(3) Uani 1 1 d . . .
C2 C 0.44281(16) 0.69880(12) 0.53734(11) 0.0283(3) Uani 1 1 d . . .
C3 C 0.53016(18) 0.74927(13) 0.47877(12) 0.0328(4) Uani 1 1 d . . .
H3 H 0.5341 0.7292 0.4150 0.039 Uiso 1 1 calc R . .
C4 C 0.60628(17) 0.83107(13) 0.53102(12) 0.0328(4) Uani 1 1 d . . .
H4 H 0.6729 0.8785 0.5100 0.039 Uiso 1 1 calc R . .
C5 C 0.56910(16) 0.83356(12) 0.62276(12) 0.0294(3) Uani 1 1 d . . .
C6 C 0.63353(17) 0.90029(12) 0.69957(12) 0.0309(4) Uani 1 1 d . . .
C7 C 0.59605(17) 0.89310(13) 0.78862(12) 0.0324(4) Uani 1 1 d . . .
C8 C 0.6604(2) 0.94120(14) 0.87622(13) 0.0396(4) Uani 1 1 d . . .
H8 H 0.7350 0.9946 0.8861 0.047 Uiso 1 1 calc R . .
C9 C 0.5949(2) 0.89638(14) 0.94355(13) 0.0413(4) Uani 1 1 d . . .
H9 H 0.6156 0.9129 1.0085 0.050 Uiso 1 1 calc R . .
C10 C 0.49057(18) 0.82071(14) 0.89787(12) 0.0352(4) Uani 1 1 d . . .
C11 C 0.40564(18) 0.73596(14) 0.92153(12) 0.0346(4) Uani 1 1 d . . .
C12 C 0.38603(19) 0.68696(15) 1.00135(12) 0.0388(4) Uani 1 1 d . . .
H12 H 0.4168 0.7147 1.0634 0.047 Uiso 1 1 calc R . .
C13 C 0.31475(18) 0.59268(15) 0.97221(12) 0.0375(4) Uani 1 1 d . . .
H13 H 0.2876 0.5426 1.0103 0.045 Uiso 1 1 calc R . .
C14 C 0.28832(17) 0.58293(14) 0.87393(12) 0.0328(4) Uani 1 1 d . . .
C15 C 0.23475(17) 0.49931(14) 0.80990(12) 0.0329(4) Uani 1 1 d . . .
C16 C 0.23699(16) 0.50200(13) 0.71417(12) 0.0315(4) Uani 1 1 d . . .
C17 C 0.18349(18) 0.42100(14) 0.64363(12) 0.0360(4) Uani 1 1 d . . .
H17 H 0.1339 0.3577 0.6529 0.043 Uiso 1 1 calc R . .
C18 C 0.21553(18) 0.44966(13) 0.56087(12) 0.0342(4) Uani 1 1 d . . .
H18 H 0.1916 0.4105 0.5021 0.041 Uiso 1 1 calc R . .
C19 C 0.29183(17) 0.54955(13) 0.57830(11) 0.0298(4) Uani 1 1 d . . .
C20 C 0.18754(18) 0.40006(14) 0.84237(12) 0.0356(4) Uani 1 1 d . . .
C21 C 0.0682(2) 0.37435(17) 0.87706(14) 0.0442(5) Uani 1 1 d . . .
C22 C 0.0264(2) 0.28009(17) 0.90344(14) 0.0486(5) Uani 1 1 d . . .
H22 H -0.0546 0.2625 0.9268 0.058 Uiso 1 1 calc R . .
C23 C 0.0984(2) 0.21184(16) 0.89678(13) 0.0486(5) Uani 1 1 d . . .
C24 C 0.2177(2) 0.23940(15) 0.86446(13) 0.0444(5) Uani 1 1 d . . .
H24 H 0.2695 0.1937 0.8608 0.053 Uiso 1 1 calc R . .
C25 C 0.26362(19) 0.33292(14) 0.83712(12) 0.0373(4) Uani 1 1 d . . .
C26 C -0.0147(2) 0.4451(2) 0.8832(2) 0.0652(7) Uani 1 1 d . . .
H26A H -0.0457 0.4530 0.8208 0.098 Uiso 1 1 calc R . .
H26B H 0.0347 0.5093 0.9154 0.098 Uiso 1 1 calc R . .
H26C H -0.0876 0.4192 0.9174 0.098 Uiso 1 1 calc R . .
C27 C 0.0497(3) 0.10879(17) 0.92272(18) 0.0651(7) Uani 1 1 d . . .
H27A H -0.0268 0.1061 0.9555 0.098 Uiso 1 1 calc R . .
H27B H 0.1159 0.0931 0.9629 0.098 Uiso 1 1 calc R . .
H27C H 0.0284 0.0606 0.8666 0.098 Uiso 1 1 calc R . .
C28 C 0.3949(2) 0.35900(15) 0.80383(15) 0.0436(5) Uani 1 1 d . . .
H28A H 0.4296 0.3006 0.7996 0.065 Uiso 1 1 calc R . .
H28B H 0.4512 0.4123 0.8475 0.065 Uiso 1 1 calc R . .
H28C H 0.3891 0.3809 0.7428 0.065 Uiso 1 1 calc R . .
C29 C 0.34363(17) 0.55912(13) 0.41568(11) 0.0300(4) Uani 1 1 d . . .
C30 C 0.37468(16) 0.47035(13) 0.38974(12) 0.0306(4) Uani 1 1 d . . .
H30 H 0.4048 0.4370 0.4361 0.037 Uiso 1 1 calc R . .
C31 C 0.36273(17) 0.42900(13) 0.29737(12) 0.0315(4) Uani 1 1 d . . .
H31 H 0.3843 0.3681 0.2810 0.038 Uiso 1 1 calc R . .
C32 C 0.31903(17) 0.47772(13) 0.22969(12) 0.0327(4) Uani 1 1 d . . .
C33 C 0.29242(18) 0.56836(14) 0.25415(12) 0.0360(4) Uani 1 1 d . . .
H33 H 0.2665 0.6033 0.2075 0.043 Uiso 1 1 calc R . .
C34 C 0.30340(18) 0.60806(13) 0.34589(12) 0.0344(4) Uani 1 1 d . . .
H34 H 0.2833 0.6696 0.3618 0.041 Uiso 1 1 calc R . .
C35 C 0.3349(3) 0.35488(17) 0.10807(14) 0.0519(5) Uani 1 1 d . . .
H35A H 0.4248 0.3621 0.1289 0.078 Uiso 1 1 calc R . .
H35B H 0.3223 0.3411 0.0405 0.078 Uiso 1 1 calc R . .
H35C H 0.2815 0.3000 0.1346 0.078 Uiso 1 1 calc R . .
C36 C 0.75937(18) 0.96744(13) 0.68591(12) 0.0328(4) Uani 1 1 d . . .
C37 C 0.77662(19) 1.06964(13) 0.68579(12) 0.0361(4) Uani 1 1 d . . .
C38 C 0.8949(2) 1.12596(13) 0.66700(13) 0.0395(4) Uani 1 1 d . . .
H38 H 0.9073 1.1953 0.6675 0.047 Uiso 1 1 calc R . .
C39 C 0.99478(19) 1.08396(14) 0.64769(13) 0.0387(4) Uani 1 1 d . . .
C40 C 0.97733(19) 0.98388(14) 0.65161(14) 0.0398(4) Uani 1 1 d . . .
H40 H 1.0460 0.9545 0.6406 0.048 Uiso 1 1 calc R . .
C41 C 0.86185(18) 0.92497(14) 0.67119(14) 0.0381(4) Uani 1 1 d . . .
C42 C 0.6694(2) 1.11835(15) 0.70382(17) 0.0499(5) Uani 1 1 d . . .
H42A H 0.7039 1.1903 0.7167 0.075 Uiso 1 1 calc R . .
H42B H 0.6279 1.0941 0.7572 0.075 Uiso 1 1 calc R . .
H42C H 0.6069 1.1023 0.6493 0.075 Uiso 1 1 calc R . .
C43 C 1.1202(2) 1.14410(16) 0.62261(16) 0.0483(5) Uani 1 1 d . . .
H43A H 1.1826 1.1040 0.6217 0.072 Uiso 1 1 calc R . .
H43B H 1.1517 1.2031 0.6685 0.072 Uiso 1 1 calc R . .
H43C H 1.1078 1.1642 0.5614 0.072 Uiso 1 1 calc R . .
C44 C 0.8511(2) 0.81639(15) 0.67600(19) 0.0511(5) Uani 1 1 d . . .
H44A H 0.8113 0.7976 0.7317 0.077 Uiso 1 1 calc R . .
H44B H 0.9364 0.8044 0.6781 0.077 Uiso 1 1 calc R . .
H44C H 0.7985 0.7768 0.6212 0.077 Uiso 1 1 calc R . .
C45 C 0.11271(19) 0.71387(16) 0.70037(15) 0.0423(4) Uani 1 1 d . . .
C46 C 0.16345(18) 0.75246(14) 0.62278(13) 0.0365(4) Uani 1 1 d . . .
C47 C 0.24667(18) 0.84636(14) 0.65101(14) 0.0389(4) Uani 1 1 d . . .
C48 C 0.2472(2) 0.86718(17) 0.74754(16) 0.0490(5) Uani 1 1 d . . .
C49 C 0.1631(2) 0.7842(2) 0.77798(14) 0.0516(6) Uani 1 1 d . . .
C50 C 0.0122(2) 0.6180(2) 0.6975(2) 0.0715(8) Uani 1 1 d . . .
H50A H -0.0717 0.6279 0.6789 0.107 Uiso 1 1 calc R . .
H50B H 0.0118 0.5965 0.7590 0.107 Uiso 1 1 calc R . .
H50C H 0.0311 0.5673 0.6529 0.107 Uiso 1 1 calc R . .
C51 C 0.1206(2) 0.7079(2) 0.52391(16) 0.0579(6) Uani 1 1 d . . .
H51A H 0.0984 0.6355 0.5197 0.087 Uiso 1 1 calc R . .
H51B H 0.1897 0.7296 0.4852 0.087 Uiso 1 1 calc R . .
H51C H 0.0456 0.7295 0.5025 0.087 Uiso 1 1 calc R . .
C52 C 0.3113(2) 0.9135(2) 0.5859(2) 0.0647(7) Uani 1 1 d . . .
H52A H 0.3526 0.8764 0.5420 0.097 Uiso 1 1 calc R . .
H52B H 0.3757 0.9691 0.6212 0.097 Uiso 1 1 calc R . .
H52C H 0.2477 0.9388 0.5521 0.097 Uiso 1 1 calc R . .
C53 C 0.3128(3) 0.9630(2) 0.8057(3) 0.0926(12) Uani 1 1 d . . .
H53A H 0.3907 0.9939 0.7788 0.139 Uiso 1 1 calc R . .
H53B H 0.3350 0.9505 0.8685 0.139 Uiso 1 1 calc R . .
H53C H 0.2557 1.0074 0.8078 0.139 Uiso 1 1 calc R . .
C54 C 0.1230(3) 0.7770(3) 0.87422(18) 0.0963(13) Uani 1 1 d . . .
H54A H 0.0452 0.8000 0.8798 0.144 Uiso 1 1 calc R . .
H54B H 0.1913 0.8183 0.9193 0.144 Uiso 1 1 calc R . .
H54C H 0.1065 0.7080 0.8862 0.144 Uiso 1 1 calc R . .
N1 N 0.29953(14) 0.58237(10) 0.67256(9) 0.0287(3) Uani 1 1 d . . .
N2 N 0.46580(13) 0.75263(10) 0.62510(9) 0.0276(3) Uani 1 1 d . . .
N3 N 0.49064(14) 0.82176(11) 0.80448(10) 0.0311(3) Uani 1 1 d . . .
N4 N 0.34168(14) 0.67306(11) 0.84554(10) 0.0318(3) Uani 1 1 d . . .
O1 O 0.30036(14) 0.44369(10) 0.13738(8) 0.0408(3) Uani 1 1 d . . .
Ti1 Ti 0.33800(3) 0.72925(2) 0.721812(19) 0.02771(11) 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
C1 0.0316(9) 0.0301(8) 0.0263(8) 0.0059(6) 0.0014(6) 0.0082(7)
C2 0.0318(9) 0.0295(8) 0.0246(8) 0.0063(6) 0.0027(6) 0.0084(7)
C3 0.0383(10) 0.0327(9) 0.0280(8) 0.0075(7) 0.0067(7) 0.0078(7)
C4 0.0335(9) 0.0314(9) 0.0338(9) 0.0098(7) 0.0070(7) 0.0056(7)
C5 0.0292(9) 0.0288(8) 0.0317(8) 0.0081(7) 0.0043(7) 0.0080(7)
C6 0.0311(9) 0.0271(8) 0.0348(9) 0.0065(7) 0.0017(7) 0.0071(7)
C7 0.0330(9) 0.0285(8) 0.0344(9) 0.0046(7) 0.0017(7) 0.0056(7)
C8 0.0425(11) 0.0343(9) 0.0356(10) 0.0022(7) -0.0016(8) 0.0004(8)
C9 0.0505(12) 0.0380(10) 0.0290(9) -0.0010(7) -0.0027(8) 0.0031(9)
C10 0.0413(10) 0.0370(9) 0.0258(8) 0.0022(7) 0.0017(7) 0.0085(8)
C11 0.0376(10) 0.0375(9) 0.0266(8) 0.0026(7) 0.0022(7) 0.0065(8)
C12 0.0440(11) 0.0474(11) 0.0231(8) 0.0049(7) 0.0032(7) 0.0081(9)
C13 0.0392(10) 0.0457(10) 0.0275(9) 0.0106(7) 0.0051(7) 0.0071(8)
C14 0.0313(9) 0.0397(9) 0.0274(8) 0.0098(7) 0.0051(7) 0.0059(7)
C15 0.0282(9) 0.0392(9) 0.0295(9) 0.0100(7) 0.0031(7) 0.0025(7)
C16 0.0291(9) 0.0340(9) 0.0295(8) 0.0095(7) 0.0021(7) 0.0021(7)
C17 0.0368(10) 0.0344(9) 0.0311(9) 0.0086(7) -0.0007(7) -0.0024(7)
C18 0.0360(9) 0.0341(9) 0.0275(8) 0.0046(7) -0.0025(7) 0.0007(7)
C19 0.0321(9) 0.0313(8) 0.0251(8) 0.0055(6) -0.0006(6) 0.0060(7)
C20 0.0360(10) 0.0401(10) 0.0234(8) 0.0084(7) -0.0003(7) -0.0053(8)
C21 0.0367(10) 0.0577(12) 0.0341(10) 0.0167(9) 0.0021(8) -0.0003(9)
C22 0.0409(11) 0.0589(13) 0.0353(10) 0.0160(9) 0.0042(8) -0.0123(10)
C23 0.0617(14) 0.0412(11) 0.0292(9) 0.0070(8) 0.0041(9) -0.0137(10)
C24 0.0615(13) 0.0354(10) 0.0305(9) 0.0061(8) 0.0061(9) 0.0000(9)
C25 0.0457(11) 0.0354(9) 0.0247(8) 0.0061(7) 0.0027(7) -0.0025(8)
C26 0.0399(13) 0.0917(19) 0.0715(16) 0.0425(15) 0.0180(11) 0.0135(12)
C27 0.0862(19) 0.0432(12) 0.0521(13) 0.0115(10) 0.0175(13) -0.0151(12)
C28 0.0480(12) 0.0416(10) 0.0439(11) 0.0158(8) 0.0109(9) 0.0100(9)
C29 0.0317(9) 0.0308(8) 0.0257(8) 0.0070(6) 0.0025(6) 0.0033(7)
C30 0.0303(9) 0.0329(8) 0.0277(8) 0.0081(7) 0.0006(7) 0.0047(7)
C31 0.0314(9) 0.0298(8) 0.0313(8) 0.0049(7) 0.0038(7) 0.0031(7)
C32 0.0332(9) 0.0358(9) 0.0255(8) 0.0054(7) 0.0046(7) 0.0009(7)
C33 0.0425(10) 0.0374(9) 0.0280(8) 0.0120(7) 0.0009(7) 0.0072(8)
C34 0.0426(10) 0.0305(8) 0.0308(9) 0.0076(7) 0.0034(7) 0.0093(8)
C35 0.0765(16) 0.0489(12) 0.0296(10) -0.0013(8) 0.0060(10) 0.0175(11)
C36 0.0353(10) 0.0303(9) 0.0298(8) 0.0062(7) 0.0007(7) 0.0023(7)
C37 0.0446(11) 0.0308(9) 0.0314(9) 0.0060(7) 0.0027(8) 0.0057(8)
C38 0.0524(12) 0.0268(8) 0.0347(9) 0.0071(7) 0.0038(8) -0.0002(8)
C39 0.0413(11) 0.0353(9) 0.0335(9) 0.0048(7) 0.0019(8) -0.0013(8)
C40 0.0339(10) 0.0379(10) 0.0463(11) 0.0072(8) 0.0041(8) 0.0058(8)
C41 0.0345(10) 0.0322(9) 0.0449(10) 0.0087(8) 0.0014(8) 0.0025(7)
C42 0.0591(14) 0.0329(10) 0.0609(13) 0.0120(9) 0.0135(11) 0.0128(9)
C43 0.0479(12) 0.0409(11) 0.0502(12) 0.0091(9) 0.0108(9) -0.0026(9)
C44 0.0351(11) 0.0366(10) 0.0837(16) 0.0161(10) 0.0083(10) 0.0087(8)
C45 0.0320(10) 0.0483(11) 0.0520(11) 0.0190(9) 0.0070(8) 0.0139(8)
C46 0.0323(9) 0.0407(10) 0.0392(10) 0.0081(8) 0.0008(7) 0.0136(8)
C47 0.0322(10) 0.0390(10) 0.0484(11) 0.0119(8) 0.0039(8) 0.0119(8)
C48 0.0437(11) 0.0493(12) 0.0543(12) -0.0096(10) -0.0076(9) 0.0231(10)
C49 0.0478(13) 0.0821(16) 0.0393(11) 0.0162(11) 0.0126(9) 0.0381(12)
C50 0.0333(12) 0.0655(16) 0.124(3) 0.0490(17) 0.0095(13) 0.0110(11)
C51 0.0538(13) 0.0775(16) 0.0458(12) -0.0043(11) -0.0148(10) 0.0336(12)
C52 0.0444(13) 0.0621(15) 0.102(2) 0.0492(15) 0.0163(13) 0.0204(11)
C53 0.086(2) 0.0699(18) 0.114(3) -0.0488(18) -0.0429(19) 0.0474(17)
C54 0.092(2) 0.192(4) 0.0433(14) 0.0325(19) 0.0289(14) 0.096(3)
N1 0.0299(7) 0.0307(7) 0.0244(7) 0.0069(5) 0.0017(5) 0.0041(6)
N2 0.0295(7) 0.0270(7) 0.0262(7) 0.0054(5) 0.0023(5) 0.0060(6)
N3 0.0348(8) 0.0308(7) 0.0264(7) 0.0033(6) 0.0015(6) 0.0061(6)
N4 0.0332(8) 0.0359(8) 0.0247(7) 0.0057(6) 0.0028(6) 0.0048(6)
O1 0.0547(8) 0.0421(7) 0.0241(6) 0.0032(5) 0.0034(5) 0.0098(6)
Ti1 0.02844(18) 0.03055(17) 0.02348(16) 0.00497(12) 0.00250(12) 0.00559(13)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C19 1.404(2) . ?
C1 C2 1.408(2) . ?
C1 C29 1.491(2) . ?
C2 N2 1.389(2) . ?
C2 C3 1.432(2) . ?
C3 C4 1.358(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.426(2) . ?
C4 H4 0.9500 . ?
C5 N2 1.394(2) . ?
C5 C6 1.403(2) . ?
C6 C7 1.397(3) . ?
C6 C36 1.498(3) . ?
C7 N3 1.377(2) . ?
C7 C8 1.429(3) . ?
C8 C9 1.373(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.419(3) . ?
C9 H9 0.9500 . ?
C10 N3 1.368(2) . ?
C10 C11 1.410(3) . ?
C11 N4 1.370(2) . ?
C11 C12 1.423(3) . ?
C12 C13 1.365(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.432(2) . ?
C13 H13 0.9500 . ?
C14 N4 1.380(2) . ?
C14 C15 1.394(3) . ?
C15 C16 1.407(2) . ?
C15 C20 1.505(2) . ?
C16 N1 1.394(2) . ?
C16 C17 1.425(3) . ?
C17 C18 1.359(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.430(2) . ?
C18 H18 0.9500 . ?
C19 N1 1.394(2) . ?
C20 C25 1.396(3) . ?
C20 C21 1.401(3) . ?
C21 C22 1.398(3) . ?
C21 C26 1.494(3) . ?
C22 C23 1.376(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(3) . ?
C23 C27 1.516(3) . ?
C24 C25 1.400(3) . ?
C24 H24 0.9500 . ?
C25 C28 1.509(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.389(2) . ?
C29 C34 1.397(2) . ?
C30 C31 1.394(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(3) . ?
C31 H31 0.9500 . ?
C32 O1 1.365(2) . ?
C32 C33 1.387(3) . ?
C33 C34 1.380(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 O1 1.418(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C41 1.402(3) . ?
C36 C37 1.402(3) . ?
C37 C38 1.397(3) . ?
C37 C42 1.509(3) . ?
C38 C39 1.384(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.381(3) . ?
C39 C43 1.509(3) . ?
C40 C41 1.390(3) . ?
C40 H40 0.9500 . ?
C41 C44 1.511(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.400(3) . ?
C45 C49 1.402(3) . ?
C45 C50 1.507(3) . ?
C45 Ti1 2.3972(19) . ?
C46 C47 1.405(3) . ?
C46 C51 1.505(3) . ?
C46 Ti1 2.4159(18) . ?
C47 C48 1.408(3) . ?
C47 C52 1.502(3) . ?
C47 Ti1 2.4094(18) . ?
C48 C49 1.429(4) . ?
C48 C53 1.496(3) . ?
C48 Ti1 2.384(2) . ?
C49 C54 1.507(3) . ?
C49 Ti1 2.3764(19) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N1 Ti1 2.0389(15) . ?
N2 Ti1 2.0429(14) . ?
N3 Ti1 2.0561(15) . ?
N4 Ti1 2.0562(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
C19 C1 C2 124.26(15) . . ?
C19 C1 C29 118.69(15) . . ?
C2 C1 C29 116.91(15) . . ?
N2 C2 C1 124.63(15) . . ?
N2 C2 C3 108.77(15) . . ?
C1 C2 C3 126.23(15) . . ?
C4 C3 C2 107.48(15) . . ?
C4 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
C3 C4 C5 108.33(16) . . ?
C3 C4 H4 125.8 . . ?
C5 C4 H4 125.8 . . ?
N2 C5 C6 125.64(15) . . ?
N2 C5 C4 108.42(15) . . ?
C6 C5 C4 125.65(16) . . ?
C7 C6 C5 122.01(16) . . ?
C7 C6 C36 120.02(16) . . ?
C5 C6 C36 116.92(16) . . ?
N3 C7 C6 121.17(16) . . ?
N3 C7 C8 107.96(16) . . ?
C6 C7 C8 130.27(17) . . ?
C9 C8 C7 107.65(17) . . ?
C9 C8 H8 126.2 . . ?
C7 C8 H8 126.2 . . ?
C8 C9 C10 107.04(16) . . ?
C8 C9 H9 126.5 . . ?
C10 C9 H9 126.5 . . ?
N3 C10 C11 113.04(16) . . ?
N3 C10 C9 109.13(16) . . ?
C11 C10 C9 136.40(17) . . ?
N4 C11 C10 112.57(15) . . ?
N4 C11 C12 109.04(16) . . ?
C10 C11 C12 136.83(17) . . ?
C13 C12 C11 107.22(16) . . ?
C13 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
C12 C13 C14 107.72(16) . . ?
C12 C13 H13 126.1 . . ?
C14 C13 H13 126.1 . . ?
N4 C14 C15 121.05(15) . . ?
N4 C14 C13 108.01(16) . . ?
C15 C14 C13 130.45(17) . . ?
C14 C15 C16 121.74(16) . . ?
C14 C15 C20 120.02(15) . . ?
C16 C15 C20 117.79(16) . . ?
N1 C16 C15 125.66(16) . . ?
N1 C16 C17 108.41(15) . . ?
C15 C16 C17 125.79(16) . . ?
C18 C17 C16 108.39(16) . . ?
C18 C17 H17 125.8 . . ?
C16 C17 H17 125.8 . . ?
C17 C18 C19 107.52(16) . . ?
C17 C18 H18 126.2 . . ?
C19 C18 H18 126.2 . . ?
N1 C19 C1 124.35(15) . . ?
N1 C19 C18 108.67(15) . . ?
C1 C19 C18 126.82(16) . . ?
C25 C20 C21 119.88(18) . . ?
C25 C20 C15 119.32(16) . . ?
C21 C20 C15 120.80(18) . . ?
C22 C21 C20 118.8(2) . . ?
C22 C21 C26 120.4(2) . . ?
C20 C21 C26 120.74(19) . . ?
C23 C22 C21 122.3(2) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 118.12(19) . . ?
C22 C23 C27 121.6(2) . . ?
C24 C23 C27 120.3(2) . . ?
C23 C24 C25 121.6(2) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C20 C25 C24 119.24(19) . . ?
C20 C25 C28 121.67(17) . . ?
C24 C25 C28 119.09(19) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 117.94(16) . . ?
C30 C29 C1 122.14(15) . . ?
C34 C29 C1 119.87(15) . . ?
C29 C30 C31 121.59(16) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C32 C31 C30 119.26(16) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
O1 C32 C31 124.77(17) . . ?
O1 C32 C33 115.39(16) . . ?
C31 C32 C33 119.84(16) . . ?
C34 C33 C32 120.31(16) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C29 120.98(17) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?
O1 C35 H35A 109.5 . . ?
O1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C41 C36 C37 119.65(17) . . ?
C41 C36 C6 117.95(16) . . ?
C37 C36 C6 122.38(17) . . ?
C38 C37 C36 118.69(18) . . ?
C38 C37 C42 120.18(17) . . ?
C36 C37 C42 121.12(18) . . ?
C39 C38 C37 122.11(17) . . ?
C39 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C40 C39 C38 118.22(18) . . ?
C40 C39 C43 119.80(19) . . ?
C38 C39 C43 121.97(18) . . ?
C39 C40 C41 121.72(19) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C40 C41 C36 119.47(17) . . ?
C40 C41 C44 118.55(18) . . ?
C36 C41 C44 121.99(17) . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C49 107.79(19) . . ?
C46 C45 C50 125.0(2) . . ?
C49 C45 C50 127.0(2) . . ?
C46 C45 Ti1 73.82(11) . . ?
C49 C45 Ti1 72.11(11) . . ?
C50 C45 Ti1 124.24(14) . . ?
C45 C46 C47 109.10(18) . . ?
C45 C46 C51 125.3(2) . . ?
C47 C46 C51 125.0(2) . . ?
C45 C46 Ti1 72.35(11) . . ?
C47 C46 Ti1 72.81(11) . . ?
C51 C46 Ti1 128.14(13) . . ?
C46 C47 C48 107.64(18) . . ?
C46 C47 C52 124.2(2) . . ?
C48 C47 C52 127.9(2) . . ?
C46 C47 Ti1 73.33(11) . . ?
C48 C47 Ti1 71.93(11) . . ?
C52 C47 Ti1 124.74(14) . . ?
C47 C48 C49 107.48(18) . . ?
C47 C48 C53 125.9(3) . . ?
C49 C48 C53 126.3(3) . . ?
C47 C48 Ti1 73.90(11) . . ?
C49 C48 Ti1 72.23(12) . . ?
C53 C48 Ti1 124.28(15) . . ?
C45 C49 C48 107.98(18) . . ?
C45 C49 C54 125.1(3) . . ?
C48 C49 C54 126.5(3) . . ?
C45 C49 Ti1 73.74(11) . . ?
C48 C49 Ti1 72.82(11) . . ?
C54 C49 Ti1 124.43(15) . . ?
C45 C50 H50A 109.5 . . ?
C45 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C45 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C47 C52 H52A 109.5 . . ?
C47 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C47 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C48 C53 H53A 109.5 . . ?
C48 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C48 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C49 C54 H54A 109.5 . . ?
C49 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C49 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C19 N1 C16 106.85(14) . . ?
C19 N1 Ti1 121.63(11) . . ?
C16 N1 Ti1 128.11(12) . . ?
C2 N2 C5 106.94(14) . . ?
C2 N2 Ti1 122.34(11) . . ?
C5 N2 Ti1 129.02(11) . . ?
C10 N3 C7 108.13(15) . . ?
C10 N3 Ti1 117.30(12) . . ?
C7 N3 Ti1 134.44(12) . . ?
C11 N4 C14 107.87(14) . . ?
C11 N4 Ti1 117.47(12) . . ?
C14 N4 Ti1 134.60(12) . . ?
C32 O1 C35 117.58(15) . . ?
N1 Ti1 N2 87.02(6) . . ?
N1 Ti1 N3 131.56(6) . . ?
N2 Ti1 N3 81.12(6) . . ?
N1 Ti1 N4 80.98(6) . . ?
N2 Ti1 N4 132.82(6) . . ?
N3 Ti1 N4 73.86(6) . . ?
N1 Ti1 C49 115.43(8) . . ?
N2 Ti1 C49 141.67(7) . . ?
N3 Ti1 C49 102.07(8) . . ?
N4 Ti1 C49 83.31(7) . . ?
N1 Ti1 C48 144.32(7) . . ?
N2 Ti1 C48 110.04(7) . . ?
N3 Ti1 C48 83.09(7) . . ?
N4 Ti1 C48 105.89(7) . . ?
C49 Ti1 C48 34.95(9) . . ?
N1 Ti1 C45 87.35(7) . . ?
N2 Ti1 C45 127.34(6) . . ?
N3 Ti1 C45 135.96(7) . . ?
N4 Ti1 C45 97.63(7) . . ?
C49 Ti1 C45 34.15(8) . . ?
C48 Ti1 C45 57.24(8) . . ?
N1 Ti1 C47 124.04(6) . . ?
N2 Ti1 C47 84.66(6) . . ?
N3 Ti1 C47 101.47(6) . . ?
N4 Ti1 C47 138.78(7) . . ?
C49 Ti1 C47 57.13(7) . . ?
C48 Ti1 C47 34.17(7) . . ?
C45 Ti1 C47 56.78(7) . . ?
N1 Ti1 C46 92.30(6) . . ?
N2 Ti1 C46 94.27(6) . . ?
N3 Ti1 C46 135.11(6) . . ?
N4 Ti1 C46 131.43(6) . . ?
C49 Ti1 C46 56.37(7) . . ?
C48 Ti1 C46 56.47(7) . . ?
C45 Ti1 C46 33.82(7) . . ?
C47 Ti1 C46 33.86(7) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.046