# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1479767'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H62 Li2 N2 O2'
_chemical_formula_weight         616.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.4110(15)
_cell_length_b                   19.573(3)
_cell_length_c                   17.749(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.323(6)
_cell_angle_gamma                90
_cell_volume                     3957.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5598
_cell_measurement_theta_min      1.550
_cell_measurement_theta_max      27.458

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.061
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6108
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19128
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.550
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             8876
_reflns_number_gt                5598
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1104P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8876
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1884
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.8271(3) 0.18124(16) 0.76108(16) 0.0330(7) Uani 1 1 d . . . . .
Li2 Li 0.6288(3) 0.20659(17) 0.81569(18) 0.0356(7) Uani 1 1 d . . . . .
O1 O 0.91397(12) 0.22720(7) 0.69062(7) 0.0380(3) Uani 1 1 d . . . . .
O2 O 0.4873(2) 0.26543(14) 0.82465(14) 0.0364(6) Uani 0.66 1 d . . P A 1
O2A O 0.4898(6) 0.2390(3) 0.8414(3) 0.0492(18) Uiso 0.34 1 d . . P A 2
N1 N 0.79645(13) 0.20703(7) 0.86488(7) 0.0240(3) Uani 1 1 d . . . . .
N2 N 0.69266(13) 0.11902(7) 0.76792(7) 0.0252(3) Uani 1 1 d . . . . .
C1 C 0.75345(15) 0.14620(9) 0.89666(9) 0.0224(4) Uani 1 1 d . . . . .
C2 C 0.70028(15) 0.09779(9) 0.84380(9) 0.0240(4) Uani 1 1 d . . . . .
C3 C 0.65945(16) 0.03575(9) 0.87217(10) 0.0273(4) Uani 1 1 d . . . . .
H3A H 0.6259 0.0032 0.8376 0.033 Uiso 1 1 calc R U . . .
C4 C 0.66607(16) 0.01963(9) 0.94946(10) 0.0285(4) Uani 1 1 d . . . . .
C5 C 0.71132(15) 0.06870(10) 1.00097(9) 0.0276(4) Uani 1 1 d . . . . .
C6 C 0.75345(15) 0.13075(9) 0.97333(9) 0.0260(4) Uani 1 1 d . . . . .
H6A H 0.7834 0.1638 1.0086 0.031 Uiso 1 1 calc R U . . .
C7 C 0.62504(18) -0.05007(10) 0.97473(12) 0.0378(5) Uani 1 1 d . . . . .
H7A H 0.6889 -0.0728 1.0043 0.057 Uiso 1 1 calc R U . . .
H7B H 0.6023 -0.0779 0.9303 0.057 Uiso 1 1 calc R U . . .
H7C H 0.5575 -0.0445 1.0058 0.057 Uiso 1 1 calc R U . . .
C8 C 0.71702(19) 0.05624(12) 1.08569(10) 0.0411(5) Uani 1 1 d . . . . .
H8A H 0.6402 0.0406 1.1008 0.062 Uiso 1 1 calc R U . . .
H8B H 0.7382 0.0988 1.1122 0.062 Uiso 1 1 calc R U . . .
H8C H 0.7763 0.0213 1.0986 0.062 Uiso 1 1 calc R U . . .
C9 C 0.88713(15) 0.24443(9) 0.90375(9) 0.0238(4) Uani 1 1 d . . . . .
C10 C 0.99558(16) 0.21301(9) 0.93025(9) 0.0283(4) Uani 1 1 d . . . . .
C11 C 1.08624(17) 0.25463(11) 0.96040(10) 0.0354(5) Uani 1 1 d . . . . .
H11A H 1.1578 0.2338 0.9781 0.042 Uiso 1 1 calc R U . . .
C12 C 1.07613(19) 0.32466(11) 0.96545(11) 0.0419(5) Uani 1 1 d . . . . .
H12A H 1.1396 0.3513 0.9862 0.050 Uiso 1 1 calc R U . . .
C13 C 0.97162(19) 0.35580(10) 0.93971(11) 0.0385(5) Uani 1 1 d . . . . .
H13A H 0.9645 0.4041 0.9425 0.046 Uiso 1 1 calc R U . . .
C14 C 0.87692(16) 0.31701(9) 0.90975(9) 0.0276(4) Uani 1 1 d . . . . .
C15 C 0.76547(18) 0.35321(10) 0.88038(11) 0.0338(4) Uani 1 1 d . . . . .
H15A H 0.6988 0.3204 0.8839 0.041 Uiso 1 1 calc R U . . .
C16 C 0.7733(2) 0.37226(12) 0.79710(12) 0.0479(6) Uani 1 1 d . . . . .
H16A H 0.7018 0.3964 0.7793 0.072 Uiso 1 1 calc R U . . .
H16B H 0.7818 0.3306 0.7672 0.072 Uiso 1 1 calc R U . . .
H16C H 0.8415 0.4019 0.7915 0.072 Uiso 1 1 calc R U . . .
C17 C 0.7363(3) 0.41731(13) 0.92531(15) 0.0648(8) Uani 1 1 d . . . . .
H17A H 0.6576 0.4335 0.9089 0.097 Uiso 1 1 calc R U . . .
H17B H 0.7940 0.4531 0.9165 0.097 Uiso 1 1 calc R U . . .
H17C H 0.7386 0.4063 0.9792 0.097 Uiso 1 1 calc R U . . .
C18 C 1.02095(17) 0.13674(10) 0.92114(10) 0.0325(4) Uani 1 1 d . . . . .
H18A H 0.9477 0.1148 0.8990 0.039 Uiso 1 1 calc R U . . .
C19 C 1.1174(2) 0.12565(13) 0.86584(12) 0.0484(6) Uani 1 1 d . . . . .
H19A H 1.1273 0.0766 0.8572 0.073 Uiso 1 1 calc R U . . .
H19B H 1.1913 0.1450 0.8871 0.073 Uiso 1 1 calc R U . . .
H19C H 1.0951 0.1483 0.8179 0.073 Uiso 1 1 calc R U . . .
C20 C 1.05293(19) 0.10139(11) 0.99721(11) 0.0419(5) Uani 1 1 d . . . . .
H20A H 1.0692 0.0530 0.9885 0.063 Uiso 1 1 calc R U . . .
H20B H 0.9872 0.1056 1.0301 0.063 Uiso 1 1 calc R U . . .
H20C H 1.1227 0.1232 1.0214 0.063 Uiso 1 1 calc R U . . .
C21 C 0.67129(16) 0.06721(9) 0.71229(9) 0.0266(4) Uani 1 1 d . . . . .
C22 C 0.56514(17) 0.06665(9) 0.66664(10) 0.0303(4) Uani 1 1 d . . . . .
C23 C 0.55142(19) 0.01906(10) 0.60760(10) 0.0376(5) Uani 1 1 d . . . . .
H23A H 0.4808 0.0192 0.5765 0.045 Uiso 1 1 calc R U . . .
C24 C 0.6376(2) -0.02791(10) 0.59352(11) 0.0412(5) Uani 1 1 d . . . . .
H24A H 0.6260 -0.0599 0.5536 0.049 Uiso 1 1 calc R U . . .
C25 C 0.7409(2) -0.02793(10) 0.63816(11) 0.0386(5) Uani 1 1 d . . . . .
H25A H 0.7997 -0.0608 0.6290 0.046 Uiso 1 1 calc R U . . .
C26 C 0.76078(18) 0.01974(9) 0.69689(10) 0.0320(4) Uani 1 1 d . . . . .
C27 C 0.87989(19) 0.02035(11) 0.73998(11) 0.0393(5) Uani 1 1 d . . . . .
H27A H 0.8785 0.0571 0.7790 0.047 Uiso 1 1 calc R U . . .
C28 C 0.9056(2) -0.04781(13) 0.78106(15) 0.0620(7) Uani 1 1 d . . . . .
H28A H 0.9813 -0.0448 0.8099 0.093 Uiso 1 1 calc R U . . .
H28B H 0.9083 -0.0848 0.7439 0.093 Uiso 1 1 calc R U . . .
H28C H 0.8434 -0.0572 0.8155 0.093 Uiso 1 1 calc R U . . .
C29 C 0.9777(2) 0.03744(13) 0.68755(14) 0.0520(6) Uani 1 1 d . . . . .
H29A H 1.0529 0.0399 0.7170 0.078 Uiso 1 1 calc R U . . .
H29B H 0.9611 0.0816 0.6631 0.078 Uiso 1 1 calc R U . . .
H29C H 0.9816 0.0018 0.6490 0.078 Uiso 1 1 calc R U . . .
C30 C 0.46656(18) 0.11564(11) 0.68288(11) 0.0389(5) Uani 1 1 d . . . . .
H30A H 0.5038 0.1587 0.7029 0.047 Uiso 1 1 calc R U . . .
C31 C 0.3884(2) 0.13492(16) 0.61263(14) 0.0675(8) Uani 1 1 d . . . . .
H31A H 0.3332 0.1708 0.6258 0.101 Uiso 1 1 calc R U . . .
H31B H 0.3445 0.0946 0.5943 0.101 Uiso 1 1 calc R U . . .
H31C H 0.4376 0.1516 0.5731 0.101 Uiso 1 1 calc R U . . .
C32 C 0.3925(2) 0.08752(16) 0.74390(15) 0.0667(8) Uani 1 1 d . . . . .
H32A H 0.3331 0.1213 0.7560 0.100 Uiso 1 1 calc R U . . .
H32B H 0.4428 0.0776 0.7892 0.100 Uiso 1 1 calc R U . . .
H32C H 0.3536 0.0454 0.7259 0.100 Uiso 1 1 calc R U . . .
C33 C 0.7563(2) 0.20986(15) 0.59854(13) 0.0616(7) Uani 1 1 d . . . . .
H33A H 0.7350 0.2121 0.5443 0.092 Uiso 1 1 calc R U . . .
H33B H 0.7043 0.2397 0.6257 0.092 Uiso 1 1 calc R U . . .
H33C H 0.7483 0.1627 0.6162 0.092 Uiso 1 1 calc R U . . .
C34 C 0.8783(2) 0.23237(16) 0.61264(13) 0.0622(7) Uani 1 1 d . . . . .
H34A H 0.9304 0.2039 0.5829 0.075 Uiso 1 1 calc R U . . .
H34B H 0.8859 0.2804 0.5960 0.075 Uiso 1 1 calc R U . . .
C35 C 1.0134(2) 0.27043(13) 0.71361(14) 0.0539(6) Uani 1 1 d . . . . .
H35A H 1.0235 0.2706 0.7694 0.065 Uiso 1 1 calc R U . . .
H35B H 0.9966 0.3179 0.6969 0.065 Uiso 1 1 calc R U . . .
C36 C 1.1248(2) 0.24740(17) 0.68194(15) 0.0679(8) Uani 1 1 d . . . . .
H36A H 1.1899 0.2757 0.7025 0.102 Uiso 1 1 calc R U . . .
H36B H 1.1183 0.2518 0.6269 0.102 Uiso 1 1 calc R U . . .
H36C H 1.1395 0.1995 0.6956 0.102 Uiso 1 1 calc R U . . .
C37 C 0.4924(5) 0.3158(2) 0.7036(2) 0.0654(12) Uani 0.66 1 d . . P A 1
H37A H 0.4758 0.3571 0.6736 0.098 Uiso 0.66 1 calc R U P A 1
H37B H 0.4499 0.2770 0.6802 0.098 Uiso 0.66 1 calc R U P A 1
H37C H 0.5769 0.3065 0.7057 0.098 Uiso 0.66 1 calc R U P A 1
C37A C 0.4445(13) 0.3179(8) 0.7438(8) 0.094(5) Uiso 0.34 1 d . . P A 2
H37D H 0.4020 0.3608 0.7345 0.141 Uiso 0.34 1 calc R U P A 2
H37E H 0.4201 0.2846 0.7048 0.141 Uiso 0.34 1 calc R U P A 2
H37F H 0.5290 0.3261 0.7427 0.141 Uiso 0.34 1 calc R U P A 2
C38 C 0.4541(3) 0.32613(19) 0.7811(3) 0.0478(9) Uani 0.66 1 d . . P A 1
H38A H 0.4926 0.3670 0.8042 0.057 Uiso 0.66 1 calc R U P A 1
H38B H 0.3680 0.3328 0.7800 0.057 Uiso 0.66 1 calc R U P A 1
C38A C 0.4176(11) 0.2908(6) 0.8190(6) 0.084(3) Uiso 0.34 1 d . . P A 2
H38C H 0.4251 0.3281 0.8566 0.101 Uiso 0.34 1 calc R U P A 2
H38D H 0.3354 0.2745 0.8170 0.101 Uiso 0.34 1 calc R U P A 2
C39 C 0.4336(4) 0.2705(2) 0.8977(2) 0.0588(10) Uani 0.66 1 d . . P A 1
H39A H 0.3474 0.2747 0.8896 0.071 Uiso 0.66 1 calc R U P A 1
H39B H 0.4634 0.3115 0.9251 0.071 Uiso 0.66 1 calc R U P A 1
C39A C 0.4508(9) 0.2020(5) 0.9048(5) 0.062(3) Uiso 0.34 1 d . . P A 2
H39C H 0.4979 0.1596 0.9104 0.074 Uiso 0.34 1 calc R U P A 2
H39D H 0.3682 0.1882 0.8934 0.074 Uiso 0.34 1 calc R U P A 2
C40 C 0.4631(4) 0.2081(2) 0.9432(3) 0.0548(10) Uani 0.66 1 d . . P A 1
H40A H 0.4213 0.2093 0.9899 0.082 Uiso 0.66 1 calc R U P A 1
H40B H 0.5479 0.2067 0.9556 0.082 Uiso 0.66 1 calc R U P A 1
H40C H 0.4394 0.1674 0.9141 0.082 Uiso 0.66 1 calc R U P A 1
C40A C 0.4578(10) 0.2380(6) 0.9773(6) 0.083(3) Uiso 0.34 1 d . . P A 2
H40D H 0.4328 0.2074 1.0169 0.124 Uiso 0.34 1 calc R U P A 2
H40E H 0.4065 0.2782 0.9741 0.124 Uiso 0.34 1 calc R U P A 2
H40F H 0.5389 0.2526 0.9892 0.124 Uiso 0.34 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O1 1.870(3) . ?
Li1 N1 1.961(3) . ?
Li1 N2 1.968(4) . ?
Li1 Li2 2.562(5) . ?
Li1 C2 2.677(4) . ?
Li1 C1 2.684(3) . ?
Li2 O2A 1.792(7) . ?
Li2 O2 1.997(4) . ?
Li2 N1 2.057(3) . ?
Li2 N2 2.064(3) . ?
Li2 C1 2.291(3) . ?
Li2 C2 2.324(4) . ?
Li2 C39A 2.646(11) . ?
O1 C34 1.423(2) . ?
O1 C35 1.455(3) . ?
O2 C38 1.455(5) . ?
O2 C39 1.470(4) . ?
O2A C38A 1.351(12) . ?
O2A C39A 1.430(11) . ?
N1 C9 1.414(2) . ?
N1 C1 1.417(2) . ?
N2 C2 1.407(2) . ?
N2 C21 1.426(2) . ?
C1 C6 1.394(2) . ?
C1 C2 1.442(2) . ?
C2 C3 1.404(2) . ?
C3 C4 1.405(2) . ?
C4 C5 1.404(3) . ?
C4 C7 1.519(3) . ?
C5 C6 1.405(3) . ?
C5 C8 1.521(2) . ?
C9 C14 1.430(2) . ?
C9 C10 1.436(2) . ?
C10 C11 1.399(3) . ?
C10 C18 1.531(3) . ?
C11 C12 1.379(3) . ?
C12 C13 1.392(3) . ?
C13 C14 1.400(3) . ?
C14 C15 1.521(3) . ?
C15 C16 1.532(3) . ?
C15 C17 1.533(3) . ?
C18 C19 1.532(3) . ?
C18 C20 1.542(3) . ?
C21 C22 1.418(3) . ?
C21 C26 1.419(3) . ?
C22 C23 1.404(3) . ?
C22 C30 1.518(3) . ?
C23 C24 1.379(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.408(3) . ?
C26 C27 1.521(3) . ?
C27 C29 1.531(3) . ?
C27 C28 1.540(3) . ?
C30 C32 1.515(3) . ?
C30 C31 1.538(3) . ?
C33 C34 1.468(3) . ?
C35 C36 1.489(4) . ?
C37 C38 1.482(6) . ?
C37A C38A 1.483(16) . ?
C39 C40 1.491(5) . ?
C39A C40A 1.466(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li1 N1 129.39(18) . . ?
O1 Li1 N2 141.62(17) . . ?
N1 Li1 N2 85.35(14) . . ?
O1 Li1 Li2 132.35(18) . . ?
N1 Li1 Li2 52.05(11) . . ?
N2 Li1 Li2 52.22(11) . . ?
O1 Li1 C2 169.88(17) . . ?
N1 Li1 C2 60.67(10) . . ?
N2 Li1 C2 30.72(7) . . ?
Li2 Li1 C2 52.62(10) . . ?
O1 Li1 C1 158.13(16) . . ?
N1 Li1 C1 30.82(7) . . ?
N2 Li1 C1 60.05(10) . . ?
Li2 Li1 C1 51.73(10) . . ?
C2 Li1 C1 31.22(6) . . ?
O2A Li2 N1 134.9(3) . . ?
O2 Li2 N1 134.46(18) . . ?
O2A Li2 N2 137.5(3) . . ?
O2 Li2 N2 144.90(19) . . ?
N1 Li2 N2 80.54(13) . . ?
O2A Li2 C1 123.3(3) . . ?
O2 Li2 C1 136.31(19) . . ?
N1 Li2 C1 37.56(8) . . ?
N2 Li2 C1 66.92(11) . . ?
O2A Li2 C2 125.1(3) . . ?
O2 Li2 C2 141.9(2) . . ?
N1 Li2 C2 66.81(11) . . ?
N2 Li2 C2 36.81(8) . . ?
C1 Li2 C2 36.41(7) . . ?
O2A Li2 Li1 168.4(3) . . ?
O2 Li2 Li1 151.4(2) . . ?
N1 Li2 Li1 48.75(11) . . ?
N2 Li2 Li1 48.92(11) . . ?
C1 Li2 Li1 66.87(12) . . ?
C2 Li2 Li1 66.22(12) . . ?
O2A Li2 C39A 30.5(3) . . ?
N1 Li2 C39A 118.3(2) . . ?
N2 Li2 C39A 121.2(3) . . ?
C1 Li2 C39A 94.5(2) . . ?
C2 Li2 C39A 96.5(3) . . ?
Li1 Li2 C39A 160.9(3) . . ?
C34 O1 C35 113.93(18) . . ?
C34 O1 Li1 123.49(16) . . ?
C35 O1 Li1 121.81(16) . . ?
C38 O2 C39 107.8(3) . . ?
C38 O2 Li2 128.0(3) . . ?
C39 O2 Li2 119.3(2) . . ?
C38A O2A C39A 113.6(8) . . ?
C38A O2A Li2 136.3(7) . . ?
C39A O2A Li2 109.9(6) . . ?
C9 N1 C1 120.08(13) . . ?
C9 N1 Li1 115.22(15) . . ?
C1 N1 Li1 104.03(14) . . ?
C9 N1 Li2 147.74(14) . . ?
C1 N1 Li2 80.24(13) . . ?
Li1 N1 Li2 79.20(14) . . ?
C2 N2 C21 116.81(14) . . ?
C2 N2 Li1 103.68(13) . . ?
C21 N2 Li1 119.98(14) . . ?
C2 N2 Li2 81.71(13) . . ?
C21 N2 Li2 145.53(15) . . ?
Li1 N2 Li2 78.86(14) . . ?
C6 C1 N1 126.18(15) . . ?
C6 C1 C2 117.96(16) . . ?
N1 C1 C2 115.80(14) . . ?
C6 C1 Li2 133.55(15) . . ?
N1 C1 Li2 62.20(12) . . ?
C2 C1 Li2 73.04(12) . . ?
C6 C1 Li1 161.52(14) . . ?
N1 C1 Li1 45.15(10) . . ?
C2 C1 Li1 74.12(11) . . ?
Li2 C1 Li1 61.39(12) . . ?
C3 C2 N2 126.52(15) . . ?
C3 C2 C1 118.06(15) . . ?
N2 C2 C1 115.40(15) . . ?
C3 C2 Li2 138.54(16) . . ?
N2 C2 Li2 61.48(12) . . ?
C1 C2 Li2 70.55(12) . . ?
C3 C2 Li1 157.74(15) . . ?
N2 C2 Li1 45.60(10) . . ?
C1 C2 Li1 74.66(12) . . ?
Li2 C2 Li1 61.16(12) . . ?
C2 C3 C4 122.95(16) . . ?
C5 C4 C3 118.63(16) . . ?
C5 C4 C7 122.04(16) . . ?
C3 C4 C7 119.34(17) . . ?
C4 C5 C6 118.98(15) . . ?
C4 C5 C8 121.82(17) . . ?
C6 C5 C8 119.20(17) . . ?
C1 C6 C5 123.21(16) . . ?
N1 C9 C14 119.36(15) . . ?
N1 C9 C10 122.02(15) . . ?
C14 C9 C10 118.26(15) . . ?
C11 C10 C9 118.68(17) . . ?
C11 C10 C18 117.92(17) . . ?
C9 C10 C18 123.19(16) . . ?
C12 C11 C10 122.75(18) . . ?
C11 C12 C13 119.15(18) . . ?
C12 C13 C14 120.98(19) . . ?
C13 C14 C9 120.17(17) . . ?
C13 C14 C15 119.28(17) . . ?
C9 C14 C15 120.49(16) . . ?
C14 C15 C16 110.44(16) . . ?
C14 C15 C17 113.91(17) . . ?
C16 C15 C17 109.22(18) . . ?
C10 C18 C19 110.68(17) . . ?
C10 C18 C20 112.43(16) . . ?
C19 C18 C20 110.80(16) . . ?
C22 C21 C26 119.04(16) . . ?
C22 C21 N2 120.48(16) . . ?
C26 C21 N2 120.19(15) . . ?
C23 C22 C21 119.10(18) . . ?
C23 C22 C30 120.59(17) . . ?
C21 C22 C30 120.29(16) . . ?
C24 C23 C22 121.84(18) . . ?
C23 C24 C25 119.32(18) . . ?
C24 C25 C26 121.33(19) . . ?
C25 C26 C21 119.33(17) . . ?
C25 C26 C27 118.60(18) . . ?
C21 C26 C27 122.03(16) . . ?
C26 C27 C29 110.96(17) . . ?
C26 C27 C28 111.79(19) . . ?
C29 C27 C28 110.59(19) . . ?
C32 C30 C22 110.88(19) . . ?
C32 C30 C31 110.3(2) . . ?
C22 C30 C31 113.73(17) . . ?
O1 C34 C33 111.05(19) . . ?
O1 C35 C36 112.8(2) . . ?
O2 C38 C37 107.4(3) . . ?
O2A C38A C37A 112.3(11) . . ?
O2 C39 C40 109.3(3) . . ?
O2A C39A C40A 116.3(9) . . ?
O2A C39A Li2 39.5(4) . . ?
C40A C39A Li2 120.2(7) . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.106

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1479768'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H47 N2 Ta'
_chemical_formula_weight         652.67

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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.6170(19)
_cell_length_b                   17.966(3)
_cell_length_c                   16.185(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.038(7)
_cell_angle_gamma                90
_cell_volume                     3056.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5681
_cell_measurement_theta_min      1.703
_cell_measurement_theta_max      27.533

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.618
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24798
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.703
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7023
_reflns_number_gt                5681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²+1.3334P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7023
_refine_ls_number_parameters     332
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.49847(2) 0.00870(2) 0.20909(2) 0.01916(7) Uani 1 1 d . . . . .
N1 N 0.3408(3) 0.07292(18) 0.2182(2) 0.0172(7) Uani 1 1 d . . . . .
N2 N 0.5591(3) 0.08488(18) 0.3005(2) 0.0166(7) Uani 1 1 d . . . . .
C1 C 0.3471(4) 0.1239(2) 0.2851(2) 0.0161(8) Uani 1 1 d . . . . .
C2 C 0.4678(4) 0.1312(2) 0.3303(3) 0.0158(8) Uani 1 1 d . . . . .
C3 C 0.4883(4) 0.1779(2) 0.3994(3) 0.0210(9) Uani 1 1 d . . . . .
H3A H 0.5706 0.1823 0.4306 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3866(4) 0.2181(2) 0.4221(3) 0.0231(9) Uani 1 1 d . . . . .
H4A H 0.3998 0.2500 0.4694 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2656(4) 0.2121(2) 0.3764(3) 0.0222(9) Uani 1 1 d . . . . .
H5A H 0.1970 0.2401 0.3923 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2455(4) 0.1653(2) 0.3077(3) 0.0198(9) Uani 1 1 d . . . . .
H6A H 0.1633 0.1614 0.2761 0.024 Uiso 1 1 calc R U . . .
C7 C 0.3991(4) -0.0229(2) 0.0873(3) 0.0235(9) Uani 1 1 d . . . . .
H7A H 0.3974 0.0195 0.0491 0.035 Uiso 1 1 calc R U . . .
H7B H 0.3118 -0.0376 0.0928 0.035 Uiso 1 1 calc R U . . .
H7C H 0.4433 -0.0647 0.0653 0.035 Uiso 1 1 calc R U . . .
C8 C 0.6725(5) 0.0162(3) 0.1573(4) 0.0416(14) Uani 1 1 d . . . . .
H8A H 0.7416 0.0306 0.2011 0.062 Uiso 1 1 calc R U . . .
H8B H 0.6638 0.0537 0.1129 0.062 Uiso 1 1 calc R U . . .
H8C H 0.6920 -0.0322 0.1342 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4931(5) -0.0953(3) 0.2726(3) 0.0366(13) Uani 1 1 d . . . . .
H9A H 0.4579 -0.0877 0.3248 0.055 Uiso 1 1 calc R U . . .
H9B H 0.5795 -0.1154 0.2850 0.055 Uiso 1 1 calc R U . . .
H9C H 0.4395 -0.1304 0.2371 0.055 Uiso 1 1 calc R U . . .
C10 C 0.6897(4) 0.1019(2) 0.3337(3) 0.0169(8) Uani 1 1 d . . . . .
C11 C 0.7526(4) 0.1602(2) 0.2967(3) 0.0214(9) Uani 1 1 d . . . . .
C12 C 0.8754(4) 0.1776(2) 0.3324(3) 0.0264(10) Uani 1 1 d . . . . .
H12A H 0.9197 0.2161 0.3083 0.032 Uiso 1 1 calc R U . . .
C13 C 0.9354(4) 0.1409(2) 0.4021(3) 0.0257(10) Uani 1 1 d . . . . .
H13A H 1.0193 0.1545 0.4255 0.031 Uiso 1 1 calc R U . . .
C14 C 0.8732(4) 0.0845(2) 0.4372(3) 0.0226(9) Uani 1 1 d . . . . .
H14A H 0.9147 0.0597 0.4853 0.027 Uiso 1 1 calc R U . . .
C15 C 0.7500(4) 0.0631(2) 0.4037(3) 0.0182(8) Uani 1 1 d . . . . .
C16 C 0.6863(4) 0.0008(2) 0.4449(3) 0.0235(9) Uani 1 1 d . . . . .
H16A H 0.5996 -0.0067 0.4129 0.028 Uiso 1 1 calc R U . . .
C17 C 0.7609(5) -0.0721(3) 0.4415(4) 0.0419(14) Uani 1 1 d . . . . .
H17A H 0.7708 -0.0831 0.3834 0.063 Uiso 1 1 calc R U . . .
H17B H 0.7144 -0.1128 0.4640 0.063 Uiso 1 1 calc R U . . .
H17C H 0.8449 -0.0669 0.4747 0.063 Uiso 1 1 calc R U . . .
C18 C 0.6702(6) 0.0205(3) 0.5352(3) 0.0433(14) Uani 1 1 d . . . . .
H18A H 0.6152 0.0643 0.5354 0.065 Uiso 1 1 calc R U . . .
H18B H 0.7536 0.0314 0.5670 0.065 Uiso 1 1 calc R U . . .
H18C H 0.6316 -0.0216 0.5608 0.065 Uiso 1 1 calc R U . . .
C19 C 0.6895(4) 0.2041(2) 0.2225(3) 0.0279(10) Uani 1 1 d . . . . .
H19A H 0.6105 0.1768 0.1987 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7724(5) 0.2127(3) 0.1532(3) 0.0399(13) Uani 1 1 d . . . . .
H20A H 0.7229 0.2364 0.1046 0.060 Uiso 1 1 calc R U . . .
H20B H 0.8011 0.1635 0.1373 0.060 Uiso 1 1 calc R U . . .
H20C H 0.8465 0.2436 0.1732 0.060 Uiso 1 1 calc R U . . .
C21 C 0.6502(6) 0.2810(3) 0.2496(4) 0.0467(15) Uani 1 1 d . . . . .
H21A H 0.5956 0.2757 0.2933 0.070 Uiso 1 1 calc R U . . .
H21B H 0.6036 0.3070 0.2016 0.070 Uiso 1 1 calc R U . . .
H21C H 0.7263 0.3095 0.2713 0.070 Uiso 1 1 calc R U . . .
C22 C 0.2248(4) 0.0781(2) 0.1597(3) 0.0192(9) Uani 1 1 d . . . . .
C23 C 0.1232(4) 0.0289(2) 0.1663(3) 0.0196(9) Uani 1 1 d . . . . .
C24 C 0.0128(4) 0.0368(3) 0.1099(3) 0.0269(10) Uani 1 1 d . . . . .
H24A H -0.0568 0.0043 0.1135 0.032 Uiso 1 1 calc R U . . .
C25 C 0.0021(5) 0.0909(3) 0.0484(3) 0.0301(11) Uani 1 1 d . . . . .
H25A H -0.0740 0.0951 0.0102 0.036 Uiso 1 1 calc R U . . .
C26 C 0.1020(5) 0.1387(3) 0.0428(3) 0.0298(11) Uani 1 1 d . . . . .
H26A H 0.0938 0.1757 0.0004 0.036 Uiso 1 1 calc R U . . .
C27 C 0.2145(5) 0.1341(2) 0.0979(3) 0.0257(10) Uani 1 1 d . . . . .
C28 C 0.3219(5) 0.1896(3) 0.0919(3) 0.0408(10) Uani 1 1 d D . . . .
H28A H 0.3994 0.1763 0.1316 0.049 Uiso 0.5 1 calc R U P A 1
H28B H 0.3856 0.1808 0.1426 0.049 Uiso 0.5 1 calc R U P B 2
C29 C 0.2726(17) 0.2660(6) 0.1120(9) 0.0408(10) Uani 0.5 1 d D . P C 1
H29A H 0.2418 0.2644 0.1663 0.061 Uiso 0.5 1 calc R U P C 1
H29B H 0.2026 0.2803 0.0688 0.061 Uiso 0.5 1 calc R U P C 1
H29C H 0.3414 0.3026 0.1138 0.061 Uiso 0.5 1 calc R U P C 1
C30 C 0.3503(11) 0.1862(7) -0.0019(6) 0.0408(10) Uani 0.5 1 d D . P C 1
H30A H 0.3715 0.1350 -0.0156 0.061 Uiso 0.5 1 calc R U P C 1
H30B H 0.4220 0.2190 -0.0084 0.061 Uiso 0.5 1 calc R U P C 1
H30C H 0.2749 0.2025 -0.0394 0.061 Uiso 0.5 1 calc R U P C 1
C29A C 0.2854(17) 0.2726(5) 0.0952(10) 0.0408(10) Uani 0.5 1 d D . P C 2
H29D H 0.2379 0.2809 0.1421 0.061 Uiso 0.5 1 calc R U P C 2
H29E H 0.2324 0.2865 0.0430 0.061 Uiso 0.5 1 calc R U P C 2
H29F H 0.3628 0.3031 0.1027 0.061 Uiso 0.5 1 calc R U P C 2
C30A C 0.3950(10) 0.1819(7) 0.0184(6) 0.0408(10) Uani 0.5 1 d D . P C 2
H30D H 0.4591 0.2213 0.0207 0.061 Uiso 0.5 1 calc R U P C 2
H30E H 0.3361 0.1860 -0.0337 0.061 Uiso 0.5 1 calc R U P C 2
H30F H 0.4370 0.1332 0.0207 0.061 Uiso 0.5 1 calc R U P C 2
C31 C 0.1326(4) -0.0324(2) 0.2326(3) 0.0231(9) Uani 1 1 d . . . . .
H31A H 0.2175 -0.0283 0.2679 0.028 Uiso 1 1 calc R U . . .
C32 C 0.0299(5) -0.0238(3) 0.2891(3) 0.0398(13) Uani 1 1 d . . . . .
H32A H 0.0362 0.0257 0.3148 0.060 Uiso 1 1 calc R U . . .
H32B H 0.0415 -0.0619 0.3328 0.060 Uiso 1 1 calc R U . . .
H32C H -0.0541 -0.0297 0.2560 0.060 Uiso 1 1 calc R U . . .
C33 C 0.1230(5) -0.1094(3) 0.1919(3) 0.0347(12) Uani 1 1 d . . . . .
H33A H 0.1904 -0.1150 0.1567 0.052 Uiso 1 1 calc R U . . .
H33B H 0.0398 -0.1147 0.1575 0.052 Uiso 1 1 calc R U . . .
H33C H 0.1325 -0.1478 0.2353 0.052 Uiso 1 1 calc R U . . .


_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
Ta1 N2 2.052(3) . ?
Ta1 N1 2.055(3) . ?
Ta1 C9 2.136(5) . ?
Ta1 C8 2.138(5) . ?
Ta1 C7 2.177(4) . ?
N1 C1 1.414(5) . ?
N1 C22 1.448(5) . ?
N2 C2 1.412(5) . ?
N2 C10 1.448(5) . ?
C1 C2 1.389(5) . ?
C1 C6 1.401(5) . ?
C2 C3 1.391(6) . ?
C3 C4 1.391(6) . ?
C4 C5 1.394(6) . ?
C5 C6 1.387(6) . ?
C10 C15 1.406(6) . ?
C10 C11 1.419(6) . ?
C11 C12 1.386(6) . ?
C11 C19 1.512(6) . ?
C12 C13 1.383(7) . ?
C13 C14 1.375(6) . ?
C14 C15 1.398(6) . ?
C15 C16 1.510(6) . ?
C16 C17 1.535(6) . ?
C16 C18 1.536(7) . ?
C19 C21 1.525(7) . ?
C19 C20 1.528(6) . ?
C22 C23 1.410(6) . ?
C22 C27 1.412(6) . ?
C23 C24 1.388(6) . ?
C23 C31 1.531(6) . ?
C24 C25 1.385(6) . ?
C25 C26 1.378(7) . ?
C26 C27 1.389(6) . ?
C27 C28 1.530(7) . ?
C28 C30A 1.514(9) . ?
C28 C29 1.520(10) . ?
C28 C29A 1.543(9) . ?
C28 C30 1.589(10) . ?
C31 C32 1.526(6) . ?
C31 C33 1.530(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ta1 N1 75.55(13) . . ?
N2 Ta1 C9 105.23(16) . . ?
N1 Ta1 C9 112.31(17) . . ?
N2 Ta1 C8 92.26(17) . . ?
N1 Ta1 C8 138.58(18) . . ?
C9 Ta1 C8 109.1(2) . . ?
N2 Ta1 C7 152.90(15) . . ?
N1 Ta1 C7 85.09(14) . . ?
C9 Ta1 C7 99.53(18) . . ?
C8 Ta1 C7 89.87(19) . . ?
C1 N1 C22 113.9(3) . . ?
C1 N1 Ta1 117.8(3) . . ?
C22 N1 Ta1 128.0(2) . . ?
C2 N2 C10 114.6(3) . . ?
C2 N2 Ta1 118.5(3) . . ?
C10 N2 Ta1 126.6(3) . . ?
C2 C1 C6 120.0(4) . . ?
C2 C1 N1 113.9(3) . . ?
C6 C1 N1 126.0(4) . . ?
C1 C2 C3 120.6(4) . . ?
C1 C2 N2 113.1(3) . . ?
C3 C2 N2 126.3(4) . . ?
C4 C3 C2 119.1(4) . . ?
C3 C4 C5 120.7(4) . . ?
C6 C5 C4 120.0(4) . . ?
C5 C6 C1 119.5(4) . . ?
C15 C10 C11 121.2(4) . . ?
C15 C10 N2 119.9(4) . . ?
C11 C10 N2 118.9(4) . . ?
C12 C11 C10 117.4(4) . . ?
C12 C11 C19 120.1(4) . . ?
C10 C11 C19 122.5(4) . . ?
C13 C12 C11 122.2(4) . . ?
C14 C13 C12 119.7(4) . . ?
C13 C14 C15 121.3(4) . . ?
C14 C15 C10 118.1(4) . . ?
C14 C15 C16 119.0(4) . . ?
C10 C15 C16 122.8(4) . . ?
C15 C16 C17 110.5(4) . . ?
C15 C16 C18 111.5(4) . . ?
C17 C16 C18 111.0(4) . . ?
C11 C19 C21 110.6(4) . . ?
C11 C19 C20 113.5(4) . . ?
C21 C19 C20 109.2(4) . . ?
C23 C22 C27 121.1(4) . . ?
C23 C22 N1 120.0(4) . . ?
C27 C22 N1 118.9(4) . . ?
C24 C23 C22 118.1(4) . . ?
C24 C23 C31 120.1(4) . . ?
C22 C23 C31 121.9(4) . . ?
C25 C24 C23 121.4(4) . . ?
C26 C25 C24 119.9(4) . . ?
C25 C26 C27 121.4(4) . . ?
C26 C27 C22 118.2(4) . . ?
C26 C27 C28 120.1(4) . . ?
C22 C27 C28 121.7(4) . . ?
C30A C28 C27 117.2(6) . . ?
C29 C28 C27 107.0(7) . . ?
C30A C28 C29A 106.0(7) . . ?
C27 C28 C29A 115.8(7) . . ?
C29 C28 C30 110.9(7) . . ?
C27 C28 C30 106.1(6) . . ?
C32 C31 C33 109.9(4) . . ?
C32 C31 C23 111.4(4) . . ?
C33 C31 C23 110.7(4) . . ?

_refine_diff_density_max         0.787
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.211

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1479769'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H66 Cl Li N2 O2 Ta'
_chemical_formula_weight         842.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   11.0302(4)
_cell_length_b                   23.2106(8)
_cell_length_c                   17.0382(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.6064(15)
_cell_angle_gamma                90
_cell_volume                     4134.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7996
_cell_measurement_theta_min      1.536
_cell_measurement_theta_max      27.511

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             1740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    2.757
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39363
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.536
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9494
_reflns_number_gt                7996
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0382P)²+2.0474P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9494
_refine_ls_number_parameters     450
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.182
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.96515(2) 0.05249(2) 0.26009(2) 0.01732(5) Uani 1 1 d . . . . .
Li1 Li 1.1364(5) -0.1574(2) 0.2227(3) 0.0227(11) Uani 1 1 d . . . . .
Cl1 Cl 0.95817(9) 0.13626(4) 0.17337(6) 0.0353(2) Uani 1 1 d . . . . .
O1 O 1.2283(12) -0.2277(6) 0.2610(10) 0.051(3) Uani 0.6 1 d D U P A 1
O1A O 1.2435(14) -0.2268(8) 0.2628(10) 0.019(2) Uiso 0.4 1 d D U P A 2
O2 O 1.1474(3) -0.15580(12) 0.10744(15) 0.0395(6) Uani 1 1 d . . . . .
N1 N 1.1988(2) -0.09397(11) 0.31081(15) 0.0168(5) Uani 1 1 d . . . . .
N2 N 0.9587(2) -0.12975(11) 0.22526(16) 0.0174(5) Uani 1 1 d . . . . .
C1 C 1.1030(3) -0.06358(13) 0.31576(19) 0.0161(6) Uani 1 1 d . . . . .
C2 C 0.9715(3) -0.08203(13) 0.26647(18) 0.0160(6) Uani 1 1 d . . . . .
C3 C 0.8725(3) -0.04181(13) 0.2697(2) 0.0200(6) Uani 1 1 d . . . . .
H3A H 0.7840 -0.0493 0.2316 0.024 Uiso 1 1 calc R U . . .
C4 C 0.8840(3) -0.01035(13) 0.3436(2) 0.0209(6) Uani 1 1 d . . . . .
H4A H 0.8071 0.0002 0.3596 0.025 Uiso 1 1 calc R U . . .
C5 C 1.0054(3) 0.00555(13) 0.39145(19) 0.0196(6) Uani 1 1 d . . . . .
H5A H 1.0210 0.0279 0.4439 0.024 Uiso 1 1 calc R U . . .
C6 C 1.1082(3) -0.01074(13) 0.36135(19) 0.0184(6) Uani 1 1 d . . . . .
H6A H 1.1951 0.0047 0.3921 0.022 Uiso 1 1 calc R U . . .
C7 C 0.7596(3) 0.07315(15) 0.2250(2) 0.0281(7) Uani 1 1 d . . . . .
H7A H 0.7484 0.1101 0.2497 0.042 Uiso 1 1 calc R U . . .
H7B H 0.7153 0.0428 0.2450 0.042 Uiso 1 1 calc R U . . .
H7C H 0.7239 0.0758 0.1645 0.042 Uiso 1 1 calc R U . . .
C8 C 1.0398(3) 0.01428(13) 0.16599(19) 0.0200(6) Uani 1 1 d . . . . .
H8A H 1.1195 0.0337 0.1676 0.030 Uiso 1 1 calc R U . . .
H8B H 0.9767 0.0190 0.1109 0.030 Uiso 1 1 calc R U . . .
H8C H 1.0565 -0.0268 0.1776 0.030 Uiso 1 1 calc R U . . .
C9 C 1.0832(3) 0.11444(14) 0.3521(2) 0.0265(7) Uani 1 1 d . . . . .
H9A H 1.1561 0.1268 0.3352 0.040 Uiso 1 1 calc R U . . .
H9B H 1.1145 0.0958 0.4065 0.040 Uiso 1 1 calc R U . . .
H9C H 1.0312 0.1480 0.3553 0.040 Uiso 1 1 calc R U . . .
C10 C 1.3219(3) -0.08439(13) 0.3715(2) 0.0196(6) Uani 1 1 d . . . . .
C11 C 1.4202(3) -0.05804(15) 0.3486(2) 0.0278(8) Uani 1 1 d . . . . .
C12 C 1.5410(4) -0.05357(18) 0.4087(3) 0.0416(10) Uani 1 1 d . . . . .
H12A H 1.6085 -0.0356 0.3945 0.050 Uiso 1 1 calc R U . . .
C13 C 1.5643(3) -0.07435(19) 0.4874(3) 0.0422(10) Uani 1 1 d . . . . .
H13A H 1.6469 -0.0706 0.5271 0.051 Uiso 1 1 calc R U . . .
C14 C 1.4664(3) -0.10086(16) 0.5088(2) 0.0331(8) Uani 1 1 d . . . . .
H14A H 1.4831 -0.1153 0.5633 0.040 Uiso 1 1 calc R U . . .
C15 C 1.3445(3) -0.10667(14) 0.4519(2) 0.0233(7) Uani 1 1 d . . . . .
C16 C 1.2428(3) -0.13803(16) 0.4782(2) 0.0289(8) Uani 1 1 d . . . . .
H16A H 1.1636 -0.1399 0.4290 0.035 Uiso 1 1 calc R U . . .
C17 C 1.2102(5) -0.1064(2) 0.5461(3) 0.0523(12) Uani 1 1 d . . . . .
H17A H 1.1409 -0.1266 0.5590 0.078 Uiso 1 1 calc R U . . .
H17B H 1.1827 -0.0671 0.5278 0.078 Uiso 1 1 calc R U . . .
H17C H 1.2857 -0.1049 0.5957 0.078 Uiso 1 1 calc R U . . .
C18 C 1.2822(5) -0.19974(19) 0.5058(3) 0.0576(13) Uani 1 1 d . . . . .
H18A H 1.3059 -0.2199 0.4623 0.086 Uiso 1 1 calc R U . . .
H18B H 1.2104 -0.2198 0.5160 0.086 Uiso 1 1 calc R U . . .
H18C H 1.3555 -0.1992 0.5568 0.086 Uiso 1 1 calc R U . . .
C19 C 1.3972(4) -0.03339(19) 0.2625(2) 0.0373(9) Uani 1 1 d . . . . .
H19A H 1.3098 -0.0456 0.2273 0.045 Uiso 1 1 calc R U . . .
C20 C 1.4006(5) 0.0323(2) 0.2636(3) 0.0499(11) Uani 1 1 d . . . . .
H20A H 1.3782 0.0467 0.2067 0.075 Uiso 1 1 calc R U . . .
H20B H 1.4868 0.0454 0.2953 0.075 Uiso 1 1 calc R U . . .
H20C H 1.3391 0.0469 0.2894 0.075 Uiso 1 1 calc R U . . .
C21 C 1.4936(5) -0.0570(2) 0.2224(3) 0.0534(13) Uani 1 1 d . . . . .
H21A H 1.4728 -0.0421 0.1658 0.080 Uiso 1 1 calc R U . . .
H21B H 1.4895 -0.0992 0.2211 0.080 Uiso 1 1 calc R U . . .
H21C H 1.5801 -0.0447 0.2549 0.080 Uiso 1 1 calc R U . . .
C22 C 0.8337(3) -0.15464(14) 0.19139(19) 0.0200(6) Uani 1 1 d . . . . .
C23 C 0.7524(3) -0.14096(14) 0.1117(2) 0.0238(7) Uani 1 1 d . . . . .
C24 C 0.6356(3) -0.17002(16) 0.0822(2) 0.0301(8) Uani 1 1 d . . . . .
H24A H 0.5785 -0.1606 0.0290 0.036 Uiso 1 1 calc R U . . .
C25 C 0.6015(3) -0.21170(17) 0.1279(2) 0.0342(9) Uani 1 1 d . . . . .
H25A H 0.5220 -0.2312 0.1062 0.041 Uiso 1 1 calc R U . . .
C26 C 0.6829(3) -0.22540(16) 0.2058(2) 0.0312(8) Uani 1 1 d . . . . .
H26A H 0.6590 -0.2546 0.2370 0.037 Uiso 1 1 calc R U . . .
C27 C 0.7993(3) -0.19709(15) 0.2393(2) 0.0252(7) Uani 1 1 d . . . . .
C28 C 0.8861(4) -0.21092(16) 0.3268(2) 0.0358(9) Uani 1 1 d . . . . .
H28A H 0.9760 -0.2034 0.3282 0.043 Uiso 1 1 calc R U . . .
C29 C 0.8590(5) -0.17142(19) 0.3902(3) 0.0499(12) Uani 1 1 d . . . . .
H29A H 0.9206 -0.1791 0.4450 0.075 Uiso 1 1 calc R U . . .
H29B H 0.7721 -0.1784 0.3916 0.075 Uiso 1 1 calc R U . . .
H29C H 0.8667 -0.1312 0.3750 0.075 Uiso 1 1 calc R U . . .
C30 C 0.8793(5) -0.27415(19) 0.3514(3) 0.0568(13) Uani 1 1 d . . . . .
H30A H 0.8882 -0.2993 0.3074 0.085 Uiso 1 1 calc R U . . .
H30B H 0.7968 -0.2814 0.3598 0.085 Uiso 1 1 calc R U . . .
H30C H 0.9487 -0.2821 0.4029 0.085 Uiso 1 1 calc R U . . .
C31 C 0.7879(4) -0.09711(18) 0.0575(2) 0.0381(9) Uani 1 1 d . . . . .
H31A H 0.8753 -0.0822 0.0880 0.046 Uiso 1 1 calc R U . . .
C32 C 0.6950(6) -0.0458(2) 0.0374(3) 0.0649(15) Uani 1 1 d . . . . .
H32A H 0.7226 -0.0178 0.0035 0.097 Uiso 1 1 calc R U . . .
H32B H 0.6944 -0.0273 0.0890 0.097 Uiso 1 1 calc R U . . .
H32C H 0.6087 -0.0594 0.0069 0.097 Uiso 1 1 calc R U . . .
C33 C 0.7921(4) -0.1245(2) -0.0231(3) 0.0526(12) Uani 1 1 d . . . . .
H33A H 0.8258 -0.0965 -0.0540 0.079 Uiso 1 1 calc R U . . .
H33B H 0.7056 -0.1360 -0.0566 0.079 Uiso 1 1 calc R U . . .
H33C H 0.8477 -0.1584 -0.0104 0.079 Uiso 1 1 calc R U . . .
C34 C 1.1767(4) -0.10939(17) 0.0610(2) 0.0368(9) Uani 1 1 d . . . . .
H34A H 1.1939 -0.0747 0.0967 0.044 Uiso 0.5 1 calc R U P B 1
H34B H 1.0990 -0.1013 0.0136 0.044 Uiso 0.5 1 calc R U P B 1
H34C H 1.2156 -0.0762 0.0965 0.044 Uiso 0.5 1 calc R U P C 2
H34D H 1.1008 -0.0965 0.0153 0.044 Uiso 0.5 1 calc R U P C 2
C35 C 1.2880(8) -0.1166(4) 0.0270(5) 0.0353(19) Uiso 0.5 1 d . . P D 1
H35A H 1.3022 -0.0804 0.0017 0.053 Uiso 0.5 1 calc R U P D 1
H35B H 1.2678 -0.1472 -0.0149 0.053 Uiso 0.5 1 calc R U P D 1
H35C H 1.3654 -0.1270 0.0722 0.053 Uiso 0.5 1 calc R U P D 1
C35A C 1.2731(8) -0.1412(4) 0.0294(5) 0.039(2) Uiso 0.5 1 d . . P D 2
H35D H 1.2740 -0.1246 -0.0239 0.047 Uiso 0.5 1 calc R U P D 2
H35E H 1.3601 -0.1380 0.0699 0.047 Uiso 0.5 1 calc R U P D 2
C36 C 1.1906(9) -0.2493(4) 0.0490(6) 0.054(2) Uiso 0.5 1 d . . P E 1
H36A H 1.1386 -0.2810 0.0176 0.081 Uiso 0.5 1 calc R U P E 1
H36B H 1.2410 -0.2630 0.1042 0.081 Uiso 0.5 1 calc R U P E 1
H36C H 1.2482 -0.2352 0.0198 0.081 Uiso 0.5 1 calc R U P E 1
C36A C 1.2331(8) -0.2016(4) 0.0185(5) 0.0402(19) Uiso 0.5 1 d . . P D 2
H36D H 1.3039 -0.2273 0.0491 0.048 Uiso 0.5 1 calc R U P D 2
H36E H 1.2049 -0.2124 -0.0408 0.048 Uiso 0.5 1 calc R U P D 2
C37 C 1.1123(5) -0.2055(2) 0.0567(3) 0.0550(12) Uani 1 1 d . . . . .
H37A H 1.0434 -0.2241 0.0732 0.066 Uiso 0.5 1 calc R U P E 1
H37B H 1.0713 -0.1908 -0.0002 0.066 Uiso 0.5 1 calc R U P E 1
H37C H 1.0279 -0.2014 0.0135 0.066 Uiso 0.5 1 calc R U P E 2
H37D H 1.1144 -0.2411 0.0891 0.066 Uiso 0.5 1 calc R U P E 2
C38 C 1.4551(15) -0.2201(8) 0.3417(10) 0.085(3) Uani 0.6 1 d D U P A 1
H38A H 1.5407 -0.2154 0.3368 0.127 Uiso 0.6 1 calc R U P A 1
H38B H 1.4547 -0.2534 0.3770 0.127 Uiso 0.6 1 calc R U P A 1
H38C H 1.4320 -0.1854 0.3664 0.127 Uiso 0.6 1 calc R U P A 1
C38A C 1.4721(12) -0.2170(6) 0.3432(7) 0.018(2) Uiso 0.4 1 d D U P A 2
H38D H 1.5576 -0.2170 0.3373 0.027 Uiso 0.4 1 calc R U P A 2
H38E H 1.4622 -0.2511 0.3744 0.027 Uiso 0.4 1 calc R U P A 2
H38F H 1.4613 -0.1822 0.3730 0.027 Uiso 0.4 1 calc R U P A 2
C39 C 1.3632(10) -0.2292(5) 0.2603(7) 0.0425(18) Uani 0.6 1 d D U P A 1
H39A H 1.3799 -0.2670 0.2389 0.051 Uiso 0.6 1 calc R U P A 1
H39B H 1.3749 -0.1990 0.2222 0.051 Uiso 0.6 1 calc R U P A 1
C39A C 1.3724(13) -0.2179(6) 0.2586(8) 0.029(3) Uiso 0.4 1 d D U P A 2
H39C H 1.3751 -0.1809 0.2303 0.035 Uiso 0.4 1 calc R U P A 2
H39D H 1.3929 -0.2491 0.2253 0.035 Uiso 0.4 1 calc R U P A 2
C40 C 1.2057(9) -0.2814(4) 0.2883(7) 0.0425(18) Uani 0.6 1 d D U P A 1
H40A H 1.2061 -0.2792 0.3464 0.051 Uiso 0.6 1 calc R U P A 1
H40B H 1.2729 -0.3088 0.2855 0.051 Uiso 0.6 1 calc R U P A 1
C40A C 1.187(2) -0.2742(9) 0.2945(13) 0.094(8) Uiso 0.4 1 d D U P A 2
H40C H 1.1308 -0.2584 0.3248 0.113 Uiso 0.4 1 calc R U P A 2
H40D H 1.2553 -0.2968 0.3344 0.113 Uiso 0.4 1 calc R U P A 2
C41 C 1.0771(10) -0.3011(5) 0.2329(8) 0.085(3) Uani 0.6 1 d D U P A 1
H41A H 1.0468 -0.3330 0.2594 0.127 Uiso 0.6 1 calc R U P A 1
H41B H 1.0845 -0.3140 0.1799 0.127 Uiso 0.6 1 calc R U P A 1
H41C H 1.0163 -0.2690 0.2234 0.127 Uiso 0.6 1 calc R U P A 1
C41A C 1.1098(11) -0.3132(5) 0.2277(7) 0.035(3) Uiso 0.4 1 d D U P A 2
H41D H 1.0953 -0.3498 0.2520 0.053 Uiso 0.4 1 calc R U P A 2
H41E H 1.1562 -0.3204 0.1883 0.053 Uiso 0.4 1 calc R U P A 2
H41F H 1.0273 -0.2951 0.1989 0.053 Uiso 0.4 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 C7 2.205(3) . ?
Ta1 C8 2.209(3) . ?
Ta1 C9 2.218(3) . ?
Ta1 C5 2.400(3) . ?
Ta1 C4 2.402(3) . ?
Ta1 C6 2.426(3) . ?
Ta1 Cl1 2.4283(9) . ?
Ta1 C3 2.443(3) . ?
Li1 O1 1.921(16) . ?
Li1 O1A 1.99(2) . ?
Li1 O2 2.006(6) . ?
Li1 N1 2.059(6) . ?
Li1 N2 2.076(6) . ?
Li1 C1 2.787(6) . ?
O1 C40 1.381(12) . ?
O1 C39 1.493(12) . ?
O1A C40A 1.455(17) . ?
O1A C39A 1.461(14) . ?
O2 C37 1.419(5) . ?
O2 C34 1.433(5) . ?
N1 C1 1.295(4) . ?
N1 C10 1.438(4) . ?
N2 C2 1.295(4) . ?
N2 C22 1.436(4) . ?
C1 C6 1.443(4) . ?
C1 C2 1.488(4) . ?
C2 C3 1.451(4) . ?
C3 C4 1.426(4) . ?
C4 C5 1.377(4) . ?
C5 C6 1.437(4) . ?
C10 C11 1.405(5) . ?
C10 C15 1.409(5) . ?
C11 C12 1.401(5) . ?
C11 C19 1.518(5) . ?
C12 C13 1.370(6) . ?
C13 C14 1.389(6) . ?
C14 C15 1.390(4) . ?
C15 C16 1.519(5) . ?
C16 C17 1.509(5) . ?
C16 C18 1.527(6) . ?
C19 C20 1.525(6) . ?
C19 C21 1.536(6) . ?
C22 C23 1.404(4) . ?
C22 C27 1.407(5) . ?
C23 C24 1.398(4) . ?
C23 C31 1.508(5) . ?
C24 C25 1.368(5) . ?
C25 C26 1.381(5) . ?
C26 C27 1.392(4) . ?
C27 C28 1.526(5) . ?
C28 C29 1.518(6) . ?
C28 C30 1.535(5) . ?
C31 C33 1.527(6) . ?
C31 C32 1.537(6) . ?
C34 C35 1.524(9) . ?
C34 C35A 1.527(9) . ?
C35A C36A 1.462(12) . ?
C36 C37 1.367(10) . ?
C36A C37 1.662(9) . ?
C38 C39 1.448(13) . ?
C38A C39A 1.509(13) . ?
C40 C41 1.502(11) . ?
C40A C41A 1.489(17) . ?

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
C7 Ta1 C8 118.66(13) . . ?
C7 Ta1 C9 111.83(13) . . ?
C8 Ta1 C9 120.18(12) . . ?
C7 Ta1 C5 102.71(12) . . ?
C8 Ta1 C5 119.59(11) . . ?
C9 Ta1 C5 75.10(12) . . ?
C7 Ta1 C4 75.38(12) . . ?
C8 Ta1 C4 118.83(11) . . ?
C9 Ta1 C4 102.74(12) . . ?
C5 Ta1 C4 33.34(10) . . ?
C7 Ta1 C6 134.73(12) . . ?
C8 Ta1 C6 87.98(11) . . ?
C9 Ta1 C6 77.72(12) . . ?
C5 Ta1 C6 34.63(10) . . ?
C4 Ta1 C6 59.46(10) . . ?
C7 Ta1 Cl1 80.24(10) . . ?
C8 Ta1 Cl1 80.02(8) . . ?
C9 Ta1 Cl1 78.97(9) . . ?
C5 Ta1 Cl1 153.06(8) . . ?
C4 Ta1 Cl1 154.35(8) . . ?
C6 Ta1 Cl1 143.56(7) . . ?
C7 Ta1 C3 78.30(12) . . ?
C8 Ta1 C3 87.12(11) . . ?
C9 Ta1 C3 134.20(12) . . ?
C5 Ta1 C3 59.17(11) . . ?
C4 Ta1 C3 34.22(11) . . ?
C6 Ta1 C3 66.50(10) . . ?
Cl1 Ta1 C3 145.63(8) . . ?
O1 Li1 O2 99.1(5) . . ?
O1A Li1 O2 97.9(5) . . ?
O1 Li1 N1 110.0(5) . . ?
O1A Li1 N1 107.8(5) . . ?
O2 Li1 N1 126.1(3) . . ?
O1 Li1 N2 130.9(5) . . ?
O1A Li1 N2 134.9(5) . . ?
O2 Li1 N2 111.6(3) . . ?
N1 Li1 N2 82.0(2) . . ?
O1 Li1 C1 128.4(6) . . ?
O1A Li1 C1 127.6(5) . . ?
O2 Li1 C1 127.1(3) . . ?
N1 Li1 C1 25.83(11) . . ?
N2 Li1 C1 56.57(16) . . ?
C40 O1 C39 105.6(11) . . ?
C40 O1 Li1 138.5(9) . . ?
C39 O1 Li1 115.9(8) . . ?
C40A O1A C39A 131.9(17) . . ?
C40A O1A Li1 117.5(13) . . ?
C39A O1A Li1 110.5(10) . . ?
C37 O2 C34 109.9(3) . . ?
C37 O2 Li1 119.4(3) . . ?
C34 O2 Li1 130.5(3) . . ?
C1 N1 C10 118.1(3) . . ?
C1 N1 Li1 110.3(2) . . ?
C10 N1 Li1 130.9(2) . . ?
C2 N2 C22 119.1(3) . . ?
C2 N2 Li1 109.6(2) . . ?
C22 N2 Li1 131.2(2) . . ?
N1 C1 C6 127.2(3) . . ?
N1 C1 C2 118.4(3) . . ?
C6 C1 C2 114.4(3) . . ?
N1 C1 Li1 43.85(18) . . ?
C6 C1 Li1 168.7(2) . . ?
C2 C1 Li1 74.7(2) . . ?
N2 C2 C3 128.2(3) . . ?
N2 C2 C1 118.0(3) . . ?
C3 C2 C1 113.8(3) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 Ta1 71.30(17) . . ?
C2 C3 Ta1 103.78(19) . . ?
C5 C4 C3 117.1(3) . . ?
C5 C4 Ta1 73.27(18) . . ?
C3 C4 Ta1 74.48(18) . . ?
C4 C5 C6 116.6(3) . . ?
C4 C5 Ta1 73.40(18) . . ?
C6 C5 Ta1 73.65(18) . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 Ta1 71.71(17) . . ?
C1 C6 Ta1 103.08(19) . . ?
C11 C10 C15 121.1(3) . . ?
C11 C10 N1 120.1(3) . . ?
C15 C10 N1 118.5(3) . . ?
C12 C11 C10 117.8(4) . . ?
C12 C11 C19 120.3(3) . . ?
C10 C11 C19 121.8(3) . . ?
C13 C12 C11 121.8(4) . . ?
C12 C13 C14 119.6(3) . . ?
C13 C14 C15 121.3(4) . . ?
C14 C15 C10 118.3(3) . . ?
C14 C15 C16 118.8(3) . . ?
C10 C15 C16 122.9(3) . . ?
C17 C16 C15 111.9(3) . . ?
C17 C16 C18 109.5(3) . . ?
C15 C16 C18 112.1(3) . . ?
C11 C19 C20 111.7(3) . . ?
C11 C19 C21 111.7(4) . . ?
C20 C19 C21 110.1(3) . . ?
C23 C22 C27 120.8(3) . . ?
C23 C22 N2 122.2(3) . . ?
C27 C22 N2 116.8(3) . . ?
C24 C23 C22 118.0(3) . . ?
C24 C23 C31 119.7(3) . . ?
C22 C23 C31 122.3(3) . . ?
C25 C24 C23 121.7(3) . . ?
C24 C25 C26 119.8(3) . . ?
C25 C26 C27 121.1(3) . . ?
C26 C27 C22 118.5(3) . . ?
C26 C27 C28 120.7(3) . . ?
C22 C27 C28 120.8(3) . . ?
C29 C28 C27 111.3(3) . . ?
C29 C28 C30 110.2(4) . . ?
C27 C28 C30 113.5(3) . . ?
C23 C31 C33 111.0(3) . . ?
C23 C31 C32 112.0(4) . . ?
C33 C31 C32 109.4(4) . . ?
O2 C34 C35 118.5(5) . . ?
O2 C34 C35A 97.8(4) . . ?
C36A C35A C34 107.0(7) . . ?
C35A C36A C37 104.5(6) . . ?
C36 C37 O2 127.2(6) . . ?
O2 C37 C36A 95.5(4) . . ?
C38 C39 O1 112.6(12) . . ?
O1A C39A C38A 112.3(12) . . ?
O1 C40 C41 107.4(10) . . ?
O1A C40A C41A 112.5(16) . . ?

_refine_diff_density_max         0.946
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.199

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 1479770'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H69 N4 Ta'
_chemical_formula_weight         859.00

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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   14.1372(15)
_cell_length_b                   15.1014(15)
_cell_length_c                   20.108(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.647(4)
_cell_angle_gamma                90
_cell_volume                     4264.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6127
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             1784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.613
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37634
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.720
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9755
_reflns_number_gt                6127
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0461P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9755
_refine_ls_number_parameters     471
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.956
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.41094(2) 0.74462(2) 0.04016(2) 0.01489(7) Uani 1 1 d . . . . .
N1 N 0.2902(3) 0.7717(2) 0.08546(19) 0.0165(9) Uani 1 1 d . . . . .
N2 N 0.3022(3) 0.7342(2) -0.03852(19) 0.0172(9) Uani 1 1 d . . . . .
N3 N 0.5632(3) 0.7571(3) 0.0809(2) 0.0253(10) Uani 1 1 d . . . . .
N4 N 0.4624(3) 0.6774(2) 0.13061(19) 0.0177(9) Uani 1 1 d . . . . .
C1 C 0.2149(4) 0.8051(3) 0.0401(3) 0.0199(11) Uani 1 1 d . . . . .
C2 C 0.2207(4) 0.7834(3) -0.0278(2) 0.0195(11) Uani 1 1 d . . . . .
C3 C 0.1484(4) 0.8104(3) -0.0765(3) 0.0262(13) Uani 1 1 d . . . . .
H3A H 0.1510 0.7951 -0.1221 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0720(4) 0.8602(4) -0.0583(3) 0.0342(15) Uani 1 1 d . . . . .
H4A H 0.0225 0.8785 -0.0914 0.041 Uiso 1 1 calc R U . . .
C5 C 0.0685(4) 0.8824(4) 0.0077(3) 0.0319(14) Uani 1 1 d . . . . .
H5A H 0.0167 0.9168 0.0197 0.038 Uiso 1 1 calc R U . . .
C6 C 0.1391(4) 0.8555(3) 0.0568(3) 0.0247(12) Uani 1 1 d . . . . .
H6A H 0.1358 0.8717 0.1021 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4645(4) 0.6324(3) -0.0151(2) 0.0182(11) Uani 1 1 d . . . . .
H7A H 0.4810 0.6532 -0.0585 0.027 Uiso 1 1 calc R U . . .
H7B H 0.4151 0.5868 -0.0223 0.027 Uiso 1 1 calc R U . . .
H7C H 0.5212 0.6075 0.0109 0.027 Uiso 1 1 calc R U . . .
C8 C 0.4323(4) 0.8805(3) 0.0093(2) 0.0194(12) Uani 1 1 d . . . . .
H8A H 0.3706 0.9071 -0.0068 0.029 Uiso 1 1 calc R U . . .
H8B H 0.4734 0.8811 -0.0267 0.029 Uiso 1 1 calc R U . . .
H8C H 0.4624 0.9145 0.0475 0.029 Uiso 1 1 calc R U . . .
C9 C 0.2726(4) 0.7671(3) 0.1544(2) 0.0192(11) Uani 1 1 d . . . . .
C10 C 0.2008(4) 0.7101(3) 0.1730(3) 0.0231(12) Uani 1 1 d . . . . .
C11 C 0.1858(4) 0.7056(3) 0.2402(3) 0.0296(13) Uani 1 1 d . . . . .
H11A H 0.1392 0.6661 0.2535 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2381(4) 0.7580(3) 0.2883(3) 0.0336(13) Uani 1 1 d . . . . .
H12A H 0.2265 0.7544 0.3338 0.040 Uiso 1 1 calc R U . . .
C13 C 0.3062(4) 0.8149(3) 0.2700(3) 0.0298(14) Uani 1 1 d . . . . .
H13A H 0.3400 0.8517 0.3029 0.036 Uiso 1 1 calc R U . . .
C14 C 0.3270(4) 0.8195(3) 0.2027(2) 0.0242(13) Uani 1 1 d . . . . .
C15 C 0.4016(4) 0.8829(3) 0.1839(3) 0.0271(13) Uani 1 1 d . . . . .
H15A H 0.4293 0.8554 0.1452 0.033 Uiso 1 1 calc R U . . .
C16 C 0.3561(5) 0.9696(3) 0.1582(3) 0.0373(15) Uani 1 1 d . . . . .
H16A H 0.3022 0.9571 0.1244 0.056 Uiso 1 1 calc R U . . .
H16B H 0.4033 1.0055 0.1383 0.056 Uiso 1 1 calc R U . . .
H16C H 0.3336 1.0022 0.1955 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4847(5) 0.8982(4) 0.2381(3) 0.0416(17) Uani 1 1 d . . . . .
H17A H 0.5152 0.8414 0.2508 0.062 Uiso 1 1 calc R U . . .
H17B H 0.4612 0.9251 0.2773 0.062 Uiso 1 1 calc R U . . .
H17C H 0.5312 0.9378 0.2210 0.062 Uiso 1 1 calc R U . . .
C18 C 0.1380(4) 0.6524(3) 0.1230(3) 0.0268(13) Uani 1 1 d . . . . .
H18A H 0.1555 0.6657 0.0773 0.032 Uiso 1 1 calc R U . . .
C19 C 0.0322(4) 0.6743(4) 0.1230(4) 0.0465(17) Uani 1 1 d . . . . .
H19A H -0.0045 0.6457 0.0846 0.070 Uiso 1 1 calc R U . . .
H19B H 0.0232 0.7386 0.1200 0.070 Uiso 1 1 calc R U . . .
H19C H 0.0103 0.6525 0.1645 0.070 Uiso 1 1 calc R U . . .
C20 C 0.1544(5) 0.5541(3) 0.1359(3) 0.0390(16) Uani 1 1 d . . . . .
H20A H 0.1097 0.5198 0.1051 0.058 Uiso 1 1 calc R U . . .
H20B H 0.1442 0.5403 0.1822 0.058 Uiso 1 1 calc R U . . .
H20C H 0.2198 0.5388 0.1288 0.058 Uiso 1 1 calc R U . . .
C21 C 0.2942(4) 0.6873(3) -0.1017(2) 0.0167(11) Uani 1 1 d . . . . .
C22 C 0.3299(4) 0.7243(3) -0.1579(2) 0.0215(11) Uani 1 1 d . . . . .
C23 C 0.3226(4) 0.6751(3) -0.2174(3) 0.0269(13) Uani 1 1 d . . . . .
H23A H 0.3478 0.6989 -0.2554 0.032 Uiso 1 1 calc R U . . .
C24 C 0.2796(4) 0.5928(3) -0.2220(3) 0.0303(14) Uani 1 1 d . . . . .
H24A H 0.2754 0.5603 -0.2627 0.036 Uiso 1 1 calc R U . . .
C25 C 0.2429(4) 0.5582(3) -0.1668(3) 0.0282(13) Uani 1 1 d . . . . .
H25A H 0.2122 0.5022 -0.1703 0.034 Uiso 1 1 calc R U . . .
C26 C 0.2499(4) 0.6041(3) -0.1058(2) 0.0217(12) Uani 1 1 d . . . . .
C27 C 0.2062(4) 0.5626(3) -0.0467(3) 0.0289(13) Uani 1 1 d . . . . .
H27A H 0.2292 0.5969 -0.0055 0.035 Uiso 1 1 calc R U . . .
C28 C 0.2366(5) 0.4650(3) -0.0349(3) 0.0383(16) Uani 1 1 d . . . . .
H28A H 0.2109 0.4426 0.0051 0.057 Uiso 1 1 calc R U . . .
H28B H 0.3062 0.4611 -0.0284 0.057 Uiso 1 1 calc R U . . .
H28C H 0.2118 0.4293 -0.0737 0.057 Uiso 1 1 calc R U . . .
C29 C 0.0976(4) 0.5703(4) -0.0582(3) 0.0406(16) Uani 1 1 d . . . . .
H29A H 0.0797 0.6324 -0.0660 0.061 Uiso 1 1 calc R U . . .
H29B H 0.0704 0.5485 -0.0186 0.061 Uiso 1 1 calc R U . . .
H29D H 0.0732 0.5349 -0.0973 0.061 Uiso 1 1 calc R U . . .
C30 C 0.3759(4) 0.8150(3) -0.1553(2) 0.0231(12) Uani 1 1 d . . . . .
H30A H 0.3715 0.8401 -0.1097 0.028 Uiso 1 1 calc R U . . .
C31 C 0.4812(4) 0.8089(4) -0.1647(3) 0.0350(15) Uani 1 1 d . . . . .
H31A H 0.5146 0.7736 -0.1284 0.052 Uiso 1 1 calc R U . . .
H31B H 0.5086 0.8685 -0.1640 0.052 Uiso 1 1 calc R U . . .
H31C H 0.4879 0.7807 -0.2078 0.052 Uiso 1 1 calc R U . . .
C32 C 0.3265(5) 0.8796(3) -0.2064(3) 0.0383(16) Uani 1 1 d . . . . .
H32A H 0.3566 0.9380 -0.2004 0.057 Uiso 1 1 calc R U . . .
H32B H 0.2590 0.8844 -0.1999 0.057 Uiso 1 1 calc R U . . .
H32C H 0.3321 0.8580 -0.2517 0.057 Uiso 1 1 calc R U . . .
C33 C 0.5538(4) 0.7022(3) 0.1311(2) 0.0204(11) Uani 1 1 d . . . . .
C34 C 0.6344(4) 0.6733(4) 0.1812(3) 0.0320(14) Uani 1 1 d . . . . .
H34A H 0.6656 0.7255 0.2028 0.048 Uiso 1 1 calc R U . . .
H34B H 0.6805 0.6397 0.1586 0.048 Uiso 1 1 calc R U . . .
H34C H 0.6098 0.6359 0.2152 0.048 Uiso 1 1 calc R U . . .
C35 C 0.6564(4) 0.7942(3) 0.0695(3) 0.0257(12) Uani 1 1 d . . . . .
H35A H 0.7065 0.7572 0.0954 0.031 Uiso 1 1 calc R U . . .
C36 C 0.6691(5) 0.8886(4) 0.0950(3) 0.0405(16) Uani 1 1 d . . . . .
H36A H 0.6604 0.8903 0.1431 0.049 Uiso 1 1 calc R U . . .
H36B H 0.6198 0.9268 0.0706 0.049 Uiso 1 1 calc R U . . .
C37 C 0.7678(5) 0.9243(4) 0.0855(3) 0.0435(17) Uani 1 1 d . . . . .
H37A H 0.8171 0.8895 0.1131 0.052 Uiso 1 1 calc R U . . .
H37B H 0.7732 0.9867 0.1004 0.052 Uiso 1 1 calc R U . . .
C38 C 0.7842(5) 0.9182(4) 0.0116(3) 0.0426(17) Uani 1 1 d . . . . .
H38A H 0.7387 0.9577 -0.0152 0.051 Uiso 1 1 calc R U . . .
H38B H 0.8494 0.9388 0.0064 0.051 Uiso 1 1 calc R U . . .
C39 C 0.7716(5) 0.8247(5) -0.0146(4) 0.0514(19) Uani 1 1 d . . . . .
H39A H 0.8214 0.7862 0.0089 0.062 Uiso 1 1 calc R U . . .
H39B H 0.7790 0.8238 -0.0630 0.062 Uiso 1 1 calc R U . . .
C40 C 0.6720(4) 0.7886(4) -0.0038(3) 0.0408(16) Uani 1 1 d . . . . .
H40A H 0.6223 0.8233 -0.0311 0.049 Uiso 1 1 calc R U . . .
H40B H 0.6665 0.7261 -0.0188 0.049 Uiso 1 1 calc R U . . .
C41 C 0.4284(4) 0.6023(3) 0.1675(2) 0.0199(12) Uani 1 1 d . . . . .
H41A H 0.3581 0.5995 0.1539 0.024 Uiso 1 1 calc R U . . .
C42 C 0.4406(4) 0.6114(3) 0.2454(3) 0.0279(14) Uani 1 1 d . . . . .
H42A H 0.5092 0.6126 0.2623 0.033 Uiso 1 1 calc R U . . .
H42B H 0.4118 0.6678 0.2582 0.033 Uiso 1 1 calc R U . . .
C43 C 0.3926(4) 0.5340(3) 0.2769(3) 0.0316(14) Uani 1 1 d . . . . .
H43A H 0.3233 0.5355 0.2624 0.038 Uiso 1 1 calc R U . . .
H43B H 0.4022 0.5398 0.3263 0.038 Uiso 1 1 calc R U . . .
C44 C 0.4334(5) 0.4457(3) 0.2567(3) 0.0347(15) Uani 1 1 d . . . . .
H44A H 0.4003 0.3966 0.2770 0.042 Uiso 1 1 calc R U . . .
H44B H 0.5019 0.4425 0.2737 0.042 Uiso 1 1 calc R U . . .
C45 C 0.4211(5) 0.4355(3) 0.1803(3) 0.0331(15) Uani 1 1 d . . . . .
H45A H 0.3524 0.4330 0.1638 0.040 Uiso 1 1 calc R U . . .
H45B H 0.4507 0.3792 0.1681 0.040 Uiso 1 1 calc R U . . .
C46 C 0.4675(4) 0.5134(3) 0.1467(3) 0.0283(13) Uani 1 1 d . . . . .
H46A H 0.5373 0.5118 0.1594 0.034 Uiso 1 1 calc R U . . .
H46B H 0.4553 0.5070 0.0975 0.034 Uiso 1 1 calc R U . . .


_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
Ta1 N1 2.067(4) . ?
Ta1 N2 2.080(4) . ?
Ta1 N4 2.136(4) . ?
Ta1 C8 2.175(4) . ?
Ta1 C7 2.208(4) . ?
Ta1 N3 2.221(4) . ?
Ta1 C33 2.642(5) . ?
N1 C1 1.411(6) . ?
N1 C9 1.438(6) . ?
N2 C2 1.408(7) . ?
N2 C21 1.448(6) . ?
N3 C33 1.325(6) . ?
N3 C35 1.473(7) . ?
N4 C33 1.344(6) . ?
N4 C41 1.466(6) . ?
C1 C6 1.387(7) . ?
C1 C2 1.416(7) . ?
C2 C3 1.393(7) . ?
C3 C4 1.399(8) . ?
C4 C5 1.375(8) . ?
C5 C6 1.382(7) . ?
C9 C14 1.410(7) . ?
C9 C10 1.414(7) . ?
C10 C11 1.393(7) . ?
C10 C18 1.534(7) . ?
C11 C12 1.393(8) . ?
C12 C13 1.372(8) . ?
C13 C14 1.420(7) . ?
C14 C15 1.505(8) . ?
C15 C16 1.524(7) . ?
C15 C17 1.524(8) . ?
C18 C20 1.521(7) . ?
C18 C19 1.532(8) . ?
C21 C26 1.402(6) . ?
C21 C22 1.406(7) . ?
C22 C23 1.401(7) . ?
C22 C30 1.515(7) . ?
C23 C24 1.382(7) . ?
C24 C25 1.380(7) . ?
C25 C26 1.404(7) . ?
C26 C27 1.534(7) . ?
C27 C29 1.531(8) . ?
C27 C28 1.546(7) . ?
C30 C31 1.525(8) . ?
C30 C32 1.526(7) . ?
C33 C34 1.496(7) . ?
C35 C36 1.518(7) . ?
C35 C40 1.518(8) . ?
C36 C37 1.529(8) . ?
C37 C38 1.533(8) . ?
C38 C39 1.511(8) . ?
C39 C40 1.549(8) . ?
C41 C46 1.529(7) . ?
C41 C42 1.562(7) . ?
C42 C43 1.525(7) . ?
C43 C44 1.527(7) . ?
C44 C45 1.532(7) . ?
C45 C46 1.541(7) . ?

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 Ta1 N2 76.99(15) . . ?
N1 Ta1 N4 86.35(16) . . ?
N2 Ta1 N4 139.52(15) . . ?
N1 Ta1 C8 95.03(18) . . ?
N2 Ta1 C8 88.22(16) . . ?
N4 Ta1 C8 130.29(16) . . ?
N1 Ta1 C7 136.29(17) . . ?
N2 Ta1 C7 79.94(16) . . ?
N4 Ta1 C7 87.77(16) . . ?
C8 Ta1 C7 120.9(2) . . ?
N1 Ta1 N3 129.47(15) . . ?
N2 Ta1 N3 152.39(17) . . ?
N4 Ta1 N3 60.41(16) . . ?
C8 Ta1 N3 82.23(17) . . ?
C7 Ta1 N3 82.90(17) . . ?
N1 Ta1 C33 110.32(16) . . ?
N2 Ta1 C33 161.19(15) . . ?
N4 Ta1 C33 30.39(16) . . ?
C8 Ta1 C33 107.83(17) . . ?
C7 Ta1 C33 83.30(16) . . ?
N3 Ta1 C33 30.07(15) . . ?
C1 N1 C9 116.0(4) . . ?
C1 N1 Ta1 112.7(3) . . ?
C9 N1 Ta1 131.2(3) . . ?
C2 N2 C21 114.2(4) . . ?
C2 N2 Ta1 112.9(3) . . ?
C21 N2 Ta1 132.9(3) . . ?
C33 N3 C35 121.8(4) . . ?
C33 N3 Ta1 92.8(3) . . ?
C35 N3 Ta1 145.2(3) . . ?
C33 N4 C41 125.7(4) . . ?
C33 N4 Ta1 96.1(3) . . ?
C41 N4 Ta1 134.3(3) . . ?
C6 C1 N1 125.9(5) . . ?
C6 C1 C2 119.5(5) . . ?
N1 C1 C2 114.6(4) . . ?
C3 C2 N2 126.4(5) . . ?
C3 C2 C1 119.4(5) . . ?
N2 C2 C1 114.2(4) . . ?
C2 C3 C4 119.9(5) . . ?
C5 C4 C3 120.0(5) . . ?
C4 C5 C6 120.9(5) . . ?
C5 C6 C1 120.2(5) . . ?
C14 C9 C10 120.7(5) . . ?
C14 C9 N1 119.7(4) . . ?
C10 C9 N1 119.6(4) . . ?
C11 C10 C9 118.7(5) . . ?
C11 C10 C18 117.8(5) . . ?
C9 C10 C18 123.4(5) . . ?
C12 C11 C10 121.1(5) . . ?
C13 C12 C11 120.2(5) . . ?
C12 C13 C14 121.0(5) . . ?
C9 C14 C13 118.2(5) . . ?
C9 C14 C15 121.7(5) . . ?
C13 C14 C15 120.0(5) . . ?
C14 C15 C16 110.6(5) . . ?
C14 C15 C17 114.9(5) . . ?
C16 C15 C17 111.9(5) . . ?
C20 C18 C19 109.9(5) . . ?
C20 C18 C10 112.2(5) . . ?
C19 C18 C10 111.6(5) . . ?
C26 C21 C22 120.6(4) . . ?
C26 C21 N2 118.6(4) . . ?
C22 C21 N2 120.8(4) . . ?
C23 C22 C21 118.5(5) . . ?
C23 C22 C30 119.9(5) . . ?
C21 C22 C30 121.6(4) . . ?
C24 C23 C22 121.5(5) . . ?
C25 C24 C23 119.3(5) . . ?
C24 C25 C26 121.4(5) . . ?
C21 C26 C25 118.6(5) . . ?
C21 C26 C27 122.6(4) . . ?
C25 C26 C27 118.8(4) . . ?
C29 C27 C26 109.9(5) . . ?
C29 C27 C28 110.5(5) . . ?
C26 C27 C28 112.3(5) . . ?
C22 C30 C31 111.2(4) . . ?
C22 C30 C32 113.2(4) . . ?
C31 C30 C32 109.4(5) . . ?
N3 C33 N4 110.5(4) . . ?
N3 C33 C34 124.0(5) . . ?
N4 C33 C34 125.5(5) . . ?
N3 C33 Ta1 57.1(3) . . ?
N4 C33 Ta1 53.5(2) . . ?
C34 C33 Ta1 177.0(4) . . ?
N3 C35 C36 112.2(5) . . ?
N3 C35 C40 111.3(4) . . ?
C36 C35 C40 110.9(5) . . ?
C35 C36 C37 111.3(5) . . ?
C36 C37 C38 110.0(5) . . ?
C39 C38 C37 111.7(5) . . ?
C38 C39 C40 110.6(5) . . ?
C35 C40 C39 110.7(5) . . ?
N4 C41 C46 113.0(4) . . ?
N4 C41 C42 115.7(4) . . ?
C46 C41 C42 110.5(4) . . ?
C43 C42 C41 110.2(4) . . ?
C42 C43 C44 111.1(5) . . ?
C43 C44 C45 110.6(4) . . ?
C44 C45 C46 111.0(4) . . ?
C41 C46 C45 111.4(5) . . ?

_refine_diff_density_max         1.478
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.148

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1479771'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H66 Li N2 O2 Ta'
_chemical_formula_weight         818.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   21.1920(16)
_cell_length_b                   18.2269(12)
_cell_length_c                   21.3088(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8230.8(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6607
_cell_measurement_theta_min      1.756
_cell_measurement_theta_max      27.515

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_F_000             3392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.705
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70581
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.756
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9454
_reflns_number_gt                6607
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+1.2689P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9454
_refine_ls_number_parameters     466
_refine_ls_number_restraints     173
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.1160
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.147
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta -0.89838(2) 0.54780(2) 0.78987(2) 0.02133(8) Uani 1 1 d . . . . .
Li1 Li -0.8048(4) 0.7442(4) 0.6392(3) 0.0260(16) Uani 1 1 d . . . . .
O1 O -0.88323(18) 0.8007(2) 0.61014(18) 0.0493(10) Uani 1 1 d . . . . .
N1 N -0.81073(15) 0.63274(17) 0.63099(16) 0.0180(7) Uani 1 1 d . . . . .
N2 N -0.78417(16) 0.71881(18) 0.73089(16) 0.0181(7) Uani 1 1 d . . . . .
C1 C -0.80974(18) 0.6021(2) 0.68639(19) 0.0160(8) Uani 1 1 d . . . . .
C2 C -0.79474(18) 0.6492(2) 0.74116(19) 0.0167(8) Uani 1 1 d . . . . .
C3 C -0.7959(2) 0.6124(2) 0.80033(19) 0.0213(9) Uani 1 1 d . . . . .
H3A H -0.7894 0.6430 0.8387 0.026 Uiso 1 1 calc R U . . .
C4 C -0.7858(2) 0.5351(2) 0.8061(2) 0.0235(10) Uani 1 1 d . . . . .
H4A H -0.7686 0.5133 0.8456 0.028 Uiso 1 1 calc R U . . .
C5 C -0.8007(2) 0.4920(2) 0.7557(2) 0.0236(10) Uani 1 1 d . . . . .
H5A H -0.7945 0.4376 0.7569 0.028 Uiso 1 1 calc R U . . .
C6 C -0.8245(2) 0.5278(2) 0.7012(2) 0.0226(10) Uani 1 1 d . . . . .
H6A H -0.8394 0.4959 0.6661 0.027 Uiso 1 1 calc R U . . .
C7 C -0.8865(3) 0.5569(3) 0.8921(2) 0.0396(13) Uani 1 1 d . . . . .
H7A H -0.8970 0.5099 0.9118 0.059 Uiso 1 1 calc R U . . .
H7B H -0.9147 0.5951 0.9083 0.059 Uiso 1 1 calc R U . . .
H7C H -0.8427 0.5697 0.9017 0.059 Uiso 1 1 calc R U . . .
C8 C -0.9368(2) 0.6432(2) 0.7422(2) 0.0243(10) Uani 1 1 d . . . . .
H8A H -0.9722 0.6282 0.7156 0.036 Uiso 1 1 calc R U . . .
H8B H -0.9039 0.6657 0.7161 0.036 Uiso 1 1 calc R U . . .
H8C H -0.9515 0.6789 0.7734 0.036 Uiso 1 1 calc R U . . .
C9 C -0.9269(2) 0.4374(3) 0.7565(3) 0.0364(12) Uani 1 1 d . . . . .
H9A H -0.9356 0.4057 0.7927 0.055 Uiso 1 1 calc R U . . .
H9B H -0.8928 0.4161 0.7314 0.055 Uiso 1 1 calc R U . . .
H9C H -0.9650 0.4416 0.7307 0.055 Uiso 1 1 calc R U . . .
C10 C -0.9984(2) 0.5414(3) 0.8236(3) 0.0357(12) Uani 1 1 d . . . . .
H10A H -1.0030 0.4993 0.8518 0.054 Uiso 1 1 calc R U . . .
H10B H -1.0267 0.5355 0.7876 0.054 Uiso 1 1 calc R U . . .
H10C H -1.0091 0.5865 0.8462 0.054 Uiso 1 1 calc R U . . .
C11 C -0.8122(2) 0.5864(2) 0.57656(19) 0.0204(9) Uani 1 1 d . . . . .
C12 C -0.7542(2) 0.5597(2) 0.5536(2) 0.0226(9) Uani 1 1 d . . . . .
C13 C -0.7547(2) 0.5160(2) 0.5002(2) 0.0257(10) Uani 1 1 d . . . . .
H13A H -0.7160 0.4971 0.4844 0.031 Uiso 1 1 calc R U . . .
C14 C -0.8103(2) 0.4997(2) 0.4699(2) 0.0280(10) Uani 1 1 d . . . . .
H14A H -0.8098 0.4693 0.4337 0.034 Uiso 1 1 calc R U . . .
C15 C -0.8664(2) 0.5272(2) 0.4917(2) 0.0285(11) Uani 1 1 d . . . . .
H15A H -0.9044 0.5161 0.4701 0.034 Uiso 1 1 calc R U . . .
C16 C -0.8684(2) 0.5712(2) 0.5450(2) 0.0229(9) Uani 1 1 d . . . . .
C17 C -0.9314(2) 0.5994(3) 0.5695(2) 0.0323(11) Uani 1 1 d . . . . .
H17A H -0.9225 0.6347 0.6043 0.039 Uiso 1 1 calc R U . . .
C18 C -0.9710(2) 0.5370(3) 0.5962(3) 0.0442(14) Uani 1 1 d . . . . .
H18A H -1.0104 0.5568 0.6132 0.066 Uiso 1 1 calc R U . . .
H18B H -0.9474 0.5125 0.6298 0.066 Uiso 1 1 calc R U . . .
H18C H -0.9805 0.5017 0.5629 0.066 Uiso 1 1 calc R U . . .
C19 C -0.9692(3) 0.6402(3) 0.5190(3) 0.0458(14) Uani 1 1 d . . . . .
H19A H -0.9443 0.6815 0.5031 0.069 Uiso 1 1 calc R U . . .
H19B H -1.0086 0.6586 0.5372 0.069 Uiso 1 1 calc R U . . .
H19C H -0.9789 0.6065 0.4844 0.069 Uiso 1 1 calc R U . . .
C20 C -0.6916(2) 0.5778(3) 0.5869(2) 0.0301(11) Uani 1 1 d . . . . .
H20A H -0.6983 0.6245 0.6105 0.036 Uiso 1 1 calc R U . . .
C21 C -0.6734(2) 0.5193(3) 0.6350(3) 0.0487(15) Uani 1 1 d . . . . .
H21A H -0.7071 0.5147 0.6663 0.073 Uiso 1 1 calc R U . . .
H21B H -0.6341 0.5337 0.6558 0.073 Uiso 1 1 calc R U . . .
H21C H -0.6674 0.4722 0.6137 0.073 Uiso 1 1 calc R U . . .
C22 C -0.6361(2) 0.5908(3) 0.5420(2) 0.0411(13) Uani 1 1 d . . . . .
H22A H -0.6473 0.6291 0.5118 0.062 Uiso 1 1 calc R U . . .
H22B H -0.6264 0.5452 0.5195 0.062 Uiso 1 1 calc R U . . .
H22C H -0.5990 0.6063 0.5661 0.062 Uiso 1 1 calc R U . . .
C23 C -0.7572(2) 0.7600(2) 0.78147(18) 0.0206(9) Uani 1 1 d . . . . .
C24 C -0.7929(2) 0.8124(2) 0.8139(2) 0.0273(10) Uani 1 1 d . . . . .
C25 C -0.7636(3) 0.8531(2) 0.8610(2) 0.0352(12) Uani 1 1 d . . . . .
H25A H -0.7875 0.8881 0.8839 0.042 Uiso 1 1 calc R U . . .
C26 C -0.7009(3) 0.8435(3) 0.8748(2) 0.0406(13) Uani 1 1 d . . . . .
H26A H -0.6816 0.8726 0.9064 0.049 Uiso 1 1 calc R U . . .
C27 C -0.6665(3) 0.7927(3) 0.8434(2) 0.0375(13) Uani 1 1 d . . . . .
H27A H -0.6231 0.7869 0.8536 0.045 Uiso 1 1 calc R U . . .
C28 C -0.6929(2) 0.7486(2) 0.7967(2) 0.0281(10) Uani 1 1 d . . . . .
C29 C -0.6519(2) 0.6923(3) 0.7643(3) 0.0357(12) Uani 1 1 d . . . . .
H29A H -0.6792 0.6646 0.7342 0.043 Uiso 1 1 calc R U . . .
C30 C -0.6242(3) 0.6368(3) 0.8105(3) 0.0533(16) Uani 1 1 d . . . . .
H30A H -0.6582 0.6158 0.8360 0.080 Uiso 1 1 calc R U . . .
H30B H -0.5938 0.6615 0.8380 0.080 Uiso 1 1 calc R U . . .
H30C H -0.6029 0.5976 0.7873 0.080 Uiso 1 1 calc R U . . .
C31 C -0.5989(3) 0.7286(4) 0.7263(3) 0.0552(17) Uani 1 1 d . . . . .
H31A H -0.5754 0.6910 0.7032 0.083 Uiso 1 1 calc R U . . .
H31B H -0.5703 0.7545 0.7549 0.083 Uiso 1 1 calc R U . . .
H31C H -0.6172 0.7637 0.6966 0.083 Uiso 1 1 calc R U . . .
C32 C -0.8609(8) 0.8217(8) 0.8048(6) 0.035(3) Uani 0.7 1 d . U P A 1
H32A H -0.8732 0.7935 0.7665 0.042 Uiso 0.7 1 calc R U P A 1
C32A C -0.8647(18) 0.8304(19) 0.7913(15) 0.020(5) Uiso 0.3 1 d . U P A 2
H32B H -0.8770 0.7948 0.7577 0.024 Uiso 0.3 1 calc R U P A 2
C33 C -0.8769(6) 0.9045(6) 0.7930(5) 0.053(3) Uani 0.7 1 d . U P A 1
H33A H -0.9225 0.9098 0.7863 0.080 Uiso 0.7 1 calc R U P A 1
H33B H -0.8542 0.9218 0.7557 0.080 Uiso 0.7 1 calc R U P A 1
H33C H -0.8642 0.9336 0.8295 0.080 Uiso 0.7 1 calc R U P A 1
C33A C -0.8730(13) 0.9038(13) 0.7682(10) 0.034(6) Uiso 0.3 1 d . U P A 2
H33D H -0.9181 0.9141 0.7636 0.051 Uiso 0.3 1 calc R U P A 2
H33E H -0.8522 0.9086 0.7273 0.051 Uiso 0.3 1 calc R U P A 2
H33F H -0.8543 0.9387 0.7978 0.051 Uiso 0.3 1 calc R U P A 2
C34 C -0.9000(6) 0.7950(6) 0.8578(6) 0.054(3) Uani 0.7 1 d . U P A 1
H34A H -0.9447 0.7989 0.8467 0.081 Uiso 0.7 1 calc R U P A 1
H34B H -0.8915 0.8248 0.8951 0.081 Uiso 0.7 1 calc R U P A 1
H34C H -0.8895 0.7436 0.8666 0.081 Uiso 0.7 1 calc R U P A 1
C34A C -0.9117(18) 0.8193(17) 0.8517(18) 0.063(9) Uiso 0.3 1 d . U P A 2
H34D H -0.9079 0.7690 0.8675 0.095 Uiso 0.3 1 calc R U P A 2
H34E H -0.9554 0.8286 0.8389 0.095 Uiso 0.3 1 calc R U P A 2
H34F H -0.8999 0.8539 0.8850 0.095 Uiso 0.3 1 calc R U P A 2
C35 C -0.8863(5) 0.8385(7) 0.5505(7) 0.042(2) Uiso 0.5 1 d D . P B 1
H35A H -0.8827 0.8029 0.5156 0.050 Uiso 0.5 1 calc R U P B 1
H35B H -0.8512 0.8742 0.5471 0.050 Uiso 0.5 1 calc R U P B 1
C36 C -0.9486(5) 0.8777(7) 0.5473(6) 0.048(3) Uiso 0.5 1 d D . P B 1
H36A H -0.9630 0.8816 0.5032 0.057 Uiso 0.5 1 calc R U P B 1
H36B H -0.9448 0.9278 0.5649 0.057 Uiso 0.5 1 calc R U P B 1
C37 C -0.9951(7) 0.8324(11) 0.5857(8) 0.069(7) Uiso 0.5 1 d D . P B 1
H37A H -1.0284 0.8636 0.6043 0.083 Uiso 0.5 1 calc R U P B 1
H37B H -1.0151 0.7937 0.5598 0.083 Uiso 0.5 1 calc R U P B 1
C38 C -0.9539(7) 0.8001(8) 0.6350(6) 0.066(4) Uiso 0.5 1 d D . P B 1
H38A H -0.9673 0.7492 0.6442 0.079 Uiso 0.5 1 calc R U P B 1
H38B H -0.9572 0.8292 0.6741 0.079 Uiso 0.5 1 calc R U P B 1
C35A C -0.8855(5) 0.8197(8) 0.5437(6) 0.042(2) Uiso 0.5 1 d D . P B 2
H35C H -0.8770 0.7762 0.5172 0.050 Uiso 0.5 1 calc R U P B 2
H35D H -0.8544 0.8584 0.5336 0.050 Uiso 0.5 1 calc R U P B 2
C36A C -0.9524(5) 0.8470(7) 0.5346(5) 0.042(3) Uiso 0.5 1 d D . P B 2
H36C H -0.9528 0.9004 0.5259 0.051 Uiso 0.5 1 calc R U P B 2
H36D H -0.9731 0.8211 0.4993 0.051 Uiso 0.5 1 calc R U P B 2
C37A C -0.9857(5) 0.8304(8) 0.5958(5) 0.029(4) Uiso 0.5 1 d D . P B 2
H37C H -1.0168 0.8691 0.6059 0.035 Uiso 0.5 1 calc R U P B 2
H37D H -1.0078 0.7826 0.5935 0.035 Uiso 0.5 1 calc R U P B 2
C38A C -0.9345(4) 0.8281(5) 0.6442(4) 0.023(2) Uiso 0.5 1 d D . P B 2
H38C H -0.9255 0.8776 0.6610 0.027 Uiso 0.5 1 calc R U P B 2
H38D H -0.9457 0.7950 0.6793 0.027 Uiso 0.5 1 calc R U P B 2
O2 O -0.73955(18) 0.78960(17) 0.58642(18) 0.0437(10) Uani 1 1 d . . . . .
C39 C -0.7059(12) 0.8486(19) 0.6205(12) 0.030(6) Uiso 0.3 1 d D U P C 1
H39A H -0.6981 0.8344 0.6647 0.036 Uiso 0.3 1 calc R U P C 1
H39B H -0.7305 0.8948 0.6198 0.036 Uiso 0.3 1 calc R U P C 1
C40 C -0.6431(9) 0.8575(10) 0.5844(9) 0.024(4) Uiso 0.3 1 d D U P C 1
H40A H -0.6421 0.9043 0.5608 0.028 Uiso 0.3 1 calc R U P C 1
H40B H -0.6065 0.8559 0.6133 0.028 Uiso 0.3 1 calc R U P C 1
C41 C -0.6428(10) 0.7918(12) 0.5399(12) 0.066(7) Uiso 0.3 1 d D U P C 1
H41A H -0.6212 0.7492 0.5592 0.079 Uiso 0.3 1 calc R U P C 1
H41B H -0.6217 0.8041 0.4998 0.079 Uiso 0.3 1 calc R U P C 1
C42 C -0.7149(10) 0.7756(15) 0.5296(13) 0.030(5) Uiso 0.3 1 d D U P C 1
H42A H -0.7331 0.8084 0.4972 0.036 Uiso 0.3 1 calc R U P C 1
H42B H -0.7220 0.7239 0.5171 0.036 Uiso 0.3 1 calc R U P C 1
C39A C -0.6978(5) 0.8483(8) 0.6045(6) 0.047(3) Uani 0.7 1 d D U P C 2
H39C H -0.6910 0.8479 0.6504 0.056 Uiso 0.7 1 calc R U P C 2
H39D H -0.7160 0.8963 0.5925 0.056 Uiso 0.7 1 calc R U P C 2
C40A C -0.6351(5) 0.8354(7) 0.5698(6) 0.076(3) Uani 0.7 1 d D U P C 2
H40C H -0.6123 0.8821 0.5629 0.091 Uiso 0.7 1 calc R U P C 2
H40D H -0.6076 0.8011 0.5933 0.091 Uiso 0.7 1 calc R U P C 2
C41A C -0.6569(5) 0.8023(5) 0.5086(5) 0.069(3) Uani 0.7 1 d D U P C 2
H41C H -0.6311 0.7586 0.4983 0.082 Uiso 0.7 1 calc R U P C 2
H41D H -0.6525 0.8384 0.4742 0.082 Uiso 0.7 1 calc R U P C 2
C42A C -0.7285(6) 0.7799(9) 0.5170(7) 0.076(4) Uani 0.7 1 d D U P C 2
H42C H -0.7565 0.8122 0.4922 0.092 Uiso 0.7 1 calc R U P C 2
H42D H -0.7356 0.7283 0.5041 0.092 Uiso 0.7 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 C8 2.173(4) . ?
Ta1 C7 2.198(5) . ?
Ta1 C9 2.218(5) . ?
Ta1 C10 2.240(5) . ?
Ta1 C5 2.419(4) . ?
Ta1 C4 2.421(4) . ?
Ta1 C6 2.480(4) . ?
Ta1 C3 2.481(4) . ?
Li1 O2 1.965(8) . ?
Li1 N1 2.043(8) . ?
Li1 O1 2.052(8) . ?
Li1 N2 2.054(8) . ?
Li1 C1 2.780(8) . ?
Li1 C2 2.786(8) . ?
O1 C38A 1.398(9) . ?
O1 C35 1.447(14) . ?
O1 C35A 1.458(14) . ?
O1 C38 1.589(14) . ?
N1 C1 1.306(5) . ?
N1 C11 1.435(5) . ?
N2 C2 1.307(5) . ?
N2 C23 1.432(5) . ?
C1 C6 1.425(6) . ?
C1 C2 1.483(6) . ?
C2 C3 1.428(6) . ?
C3 C4 1.431(6) . ?
C4 C5 1.367(6) . ?
C5 C6 1.425(6) . ?
C11 C16 1.397(6) . ?
C11 C12 1.410(6) . ?
C12 C13 1.389(6) . ?
C12 C20 1.540(6) . ?
C13 C14 1.377(6) . ?
C14 C15 1.372(6) . ?
C15 C16 1.390(6) . ?
C16 C17 1.523(6) . ?
C17 C18 1.523(7) . ?
C17 C19 1.533(7) . ?
C20 C21 1.527(7) . ?
C20 C22 1.535(7) . ?
C23 C24 1.401(6) . ?
C23 C28 1.417(6) . ?
C24 C25 1.394(6) . ?
C24 C32 1.463(17) . ?
C24 C32A 1.63(4) . ?
C25 C26 1.371(7) . ?
C26 C27 1.356(7) . ?
C27 C28 1.397(6) . ?
C28 C29 1.512(7) . ?
C29 C30 1.529(7) . ?
C29 C31 1.534(8) . ?
C32 C34 1.483(18) . ?
C32 C33 1.567(18) . ?
C32A C33A 1.44(4) . ?
C32A C34A 1.64(5) . ?
C35 C36 1.503(11) . ?
C36 C37 1.524(14) . ?
C37 C38 1.488(13) . ?
C35A C36A 1.516(11) . ?
C36A C37A 1.514(12) . ?
C37A C38A 1.497(12) . ?
O2 C42 1.34(3) . ?
O2 C39A 1.441(13) . ?
O2 C39 1.48(3) . ?
O2 C42A 1.508(14) . ?
C39 C40 1.547(15) . ?
C40 C41 1.527(18) . ?
C41 C42 1.573(15) . ?
C39A C40A 1.536(11) . ?
C40A C41A 1.509(14) . ?
C41A C42A 1.581(12) . ?

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
C8 Ta1 C7 116.45(18) . . ?
C8 Ta1 C9 118.33(19) . . ?
C7 Ta1 C9 114.6(2) . . ?
C8 Ta1 C10 80.66(17) . . ?
C7 Ta1 C10 78.1(2) . . ?
C9 Ta1 C10 78.32(19) . . ?
C8 Ta1 C5 121.10(15) . . ?
C7 Ta1 C5 103.43(18) . . ?
C9 Ta1 C5 75.86(17) . . ?
C10 Ta1 C5 152.14(16) . . ?
C8 Ta1 C4 120.83(16) . . ?
C7 Ta1 C4 75.72(17) . . ?
C9 Ta1 C4 103.15(17) . . ?
C10 Ta1 C4 151.73(18) . . ?
C5 Ta1 C4 32.81(15) . . ?
C8 Ta1 C6 89.88(15) . . ?
C7 Ta1 C6 133.91(17) . . ?
C9 Ta1 C6 78.17(18) . . ?
C10 Ta1 C6 146.47(18) . . ?
C5 Ta1 C6 33.78(14) . . ?
C4 Ta1 C6 58.20(15) . . ?
C8 Ta1 C3 89.41(15) . . ?
C7 Ta1 C3 77.02(17) . . ?
C9 Ta1 C3 134.28(17) . . ?
C10 Ta1 C3 145.49(17) . . ?
C5 Ta1 C3 58.47(14) . . ?
C4 Ta1 C3 33.92(13) . . ?
C6 Ta1 C3 65.51(14) . . ?
O2 Li1 N1 114.4(4) . . ?
O2 Li1 O1 100.7(3) . . ?
N1 Li1 O1 115.0(4) . . ?
O2 Li1 N2 119.3(4) . . ?
N1 Li1 N2 82.6(3) . . ?
O1 Li1 N2 124.9(4) . . ?
O2 Li1 C1 128.7(4) . . ?
N1 Li1 C1 26.15(15) . . ?
O1 Li1 C1 123.1(4) . . ?
N2 Li1 C1 56.9(2) . . ?
O2 Li1 C2 130.9(4) . . ?
N1 Li1 C2 56.9(2) . . ?
O1 Li1 C2 127.6(4) . . ?
N2 Li1 C2 26.16(15) . . ?
C1 Li1 C2 30.90(14) . . ?
C38A O1 C35A 113.2(6) . . ?
C35 O1 C38 104.7(7) . . ?
C38A O1 Li1 130.7(5) . . ?
C35 O1 Li1 122.8(5) . . ?
C35A O1 Li1 116.0(5) . . ?
C38 O1 Li1 131.3(5) . . ?
C1 N1 C11 118.6(3) . . ?
C1 N1 Li1 110.3(3) . . ?
C11 N1 Li1 131.0(3) . . ?
C2 N2 C23 116.8(3) . . ?
C2 N2 Li1 110.0(3) . . ?
C23 N2 Li1 133.0(3) . . ?
N1 C1 C6 127.1(4) . . ?
N1 C1 C2 117.9(4) . . ?
C6 C1 C2 115.0(4) . . ?
N1 C1 Li1 43.6(2) . . ?
C6 C1 Li1 166.8(3) . . ?
C2 C1 Li1 74.8(3) . . ?
N2 C2 C3 127.3(4) . . ?
N2 C2 C1 117.8(4) . . ?
C3 C2 C1 114.8(4) . . ?
N2 C2 Li1 43.9(2) . . ?
C3 C2 Li1 168.2(3) . . ?
C1 C2 Li1 74.3(3) . . ?
C2 C3 C4 122.4(4) . . ?
C2 C3 Ta1 99.1(3) . . ?
C4 C3 Ta1 70.8(2) . . ?
C5 C4 C3 117.6(4) . . ?
C5 C4 Ta1 73.5(3) . . ?
C3 C4 Ta1 75.3(2) . . ?
C4 C5 C6 117.3(4) . . ?
C4 C5 Ta1 73.7(3) . . ?
C6 C5 Ta1 75.5(3) . . ?
C5 C6 C1 122.6(4) . . ?
C5 C6 Ta1 70.8(2) . . ?
C1 C6 Ta1 99.7(3) . . ?
C16 C11 C12 120.5(4) . . ?
C16 C11 N1 121.7(4) . . ?
C12 C11 N1 117.7(4) . . ?
C13 C12 C11 118.5(4) . . ?
C13 C12 C20 120.4(4) . . ?
C11 C12 C20 121.1(4) . . ?
C14 C13 C12 120.9(4) . . ?
C15 C14 C13 120.3(4) . . ?
C14 C15 C16 121.0(4) . . ?
C15 C16 C11 118.8(4) . . ?
C15 C16 C17 120.2(4) . . ?
C11 C16 C17 121.0(4) . . ?
C16 C17 C18 111.0(4) . . ?
C16 C17 C19 112.4(4) . . ?
C18 C17 C19 109.7(4) . . ?
C21 C20 C22 109.4(4) . . ?
C21 C20 C12 112.2(4) . . ?
C22 C20 C12 114.0(4) . . ?
C24 C23 C28 120.4(4) . . ?
C24 C23 N2 120.9(4) . . ?
C28 C23 N2 118.6(4) . . ?
C25 C24 C23 118.5(5) . . ?
C25 C24 C32 118.2(7) . . ?
C23 C24 C32 123.1(7) . . ?
C25 C24 C32A 121.4(13) . . ?
C23 C24 C32A 119.7(13) . . ?
C26 C25 C24 121.2(5) . . ?
C27 C26 C25 120.2(5) . . ?
C26 C27 C28 121.9(5) . . ?
C27 C28 C23 117.7(4) . . ?
C27 C28 C29 119.1(4) . . ?
C23 C28 C29 123.2(4) . . ?
C28 C29 C30 112.0(5) . . ?
C28 C29 C31 111.6(4) . . ?
C30 C29 C31 110.2(4) . . ?
C24 C32 C34 114.3(11) . . ?
C24 C32 C33 110.4(11) . . ?
C34 C32 C33 108.5(11) . . ?
C33A C32A C24 114(3) . . ?
C33A C32A C34A 108(3) . . ?
C24 C32A C34A 108(2) . . ?
O1 C35 C36 107.8(9) . . ?
C35 C36 C37 106.6(10) . . ?
C38 C37 C36 102.4(10) . . ?
C37 C38 O1 108.4(9) . . ?
O1 C35A C36A 103.5(8) . . ?
C37A C36A C35A 105.0(9) . . ?
C38A C37A C36A 105.1(8) . . ?
O1 C38A C37A 102.5(7) . . ?
C42 O2 C39 113.1(12) . . ?
C39A O2 C42A 104.7(7) . . ?
C42 O2 Li1 135.2(9) . . ?
C39A O2 Li1 126.3(5) . . ?
C39 O2 Li1 111.3(9) . . ?
C42A O2 Li1 128.4(6) . . ?
O2 C39 C40 104.3(12) . . ?
C41 C40 C39 103.3(13) . . ?
C40 C41 C42 103.3(13) . . ?
O2 C42 C41 102.4(15) . . ?
O2 C39A C40A 106.8(8) . . ?
C41A C40A C39A 102.3(8) . . ?
C40A C41A C42A 107.4(8) . . ?
O2 C42A C41A 103.3(8) . . ?

_refine_diff_density_max         0.788
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.249

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1479772'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H51.40 Li N2 O'
_chemical_formula_weight         535.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   8.9697(4)
_cell_length_b                   21.8449(8)
_cell_length_c                   17.0042(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.395(2)
_cell_angle_gamma                90
_cell_volume                     3322.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5599
_cell_measurement_theta_min      1.520
_cell_measurement_theta_max      27.612

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_F_000             1170
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.063
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28427
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.520
_diffrn_reflns_theta_max         27.612
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7647
_reflns_number_gt                5599
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0977P)²+1.4354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7647
_refine_ls_number_parameters     379
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1896
_refine_ls_wR_factor_gt          0.1718
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.8174(4) 0.21108(14) 0.27608(18) 0.0390(7) Uani 1 1 d . . . . .
O1A O 0.7455(8) 0.28883(19) 0.2402(3) 0.0496(12) Uani 0.7 1 d D U P A 1
O1 O 0.721(2) 0.2845(7) 0.2518(8) 0.058(4) Uiso 0.3 1 d D U P A 2
N1 N 0.94424(17) 0.20671(6) 0.37432(8) 0.0277(3) Uani 1 1 d . . . . .
N2 N 0.85606(16) 0.12341(6) 0.26379(8) 0.0258(3) Uani 1 1 d . . . . .
C1 C 1.00012(18) 0.15019(7) 0.38343(9) 0.0240(3) Uani 1 1 d . . . . .
C2 C 0.94904(18) 0.10457(7) 0.32434(9) 0.0226(3) Uani 1 1 d . . . . .
C3 C 0.99926(19) 0.04321(7) 0.33736(10) 0.0262(3) Uani 1 1 d . . . . .
H3A H 0.9629 0.0125 0.3013 0.031 Uiso 1 1 calc R U . . .
C4 C 1.09772(19) 0.02645(7) 0.39950(10) 0.0278(4) Uani 1 1 d . . . . .
C5 C 1.1545(2) 0.07170(8) 0.45433(9) 0.0293(4) Uani 1 1 d . . . . .
C6 C 1.10524(19) 0.13104(8) 0.44581(9) 0.0281(4) Uani 1 1 d . . . . .
H6A H 1.1429 0.1607 0.4831 0.034 Uiso 1 1 calc R U . . .
C7 C 1.2652(3) 0.05416(10) 0.52169(12) 0.0445(5) Uani 1 1 d . . . . .
H7A H 1.3504 0.0331 0.5010 0.067 Uiso 1 1 calc R U . . .
H7B H 1.2169 0.0269 0.5578 0.067 Uiso 1 1 calc R U . . .
H7C H 1.3002 0.0911 0.5501 0.067 Uiso 1 1 calc R U . . .
C8 C 1.1444(2) -0.03945(8) 0.41009(12) 0.0399(5) Uani 1 1 d . . . . .
H8A H 1.2535 -0.0424 0.4106 0.060 Uiso 1 1 calc R U . . .
H8B H 1.0983 -0.0639 0.3664 0.060 Uiso 1 1 calc R U . . .
H8C H 1.1119 -0.0549 0.4601 0.060 Uiso 1 1 calc R U . . .
C9 C 0.79669(19) 0.07883(7) 0.20875(9) 0.0250(3) Uani 1 1 d . . . . .
C10 C 0.87015(19) 0.06437(8) 0.14111(10) 0.0299(4) Uani 1 1 d . . . . .
C11 C 0.8020(2) 0.02325(8) 0.08671(11) 0.0360(4) Uani 1 1 d . . . . .
H11A H 0.8510 0.0131 0.0409 0.043 Uiso 1 1 calc R U . . .
C12 C 0.6655(2) -0.00298(8) 0.09773(11) 0.0365(4) Uani 1 1 d . . . . .
H12A H 0.6209 -0.0307 0.0598 0.044 Uiso 1 1 calc R U . . .
C13 C 0.5942(2) 0.01146(8) 0.16437(11) 0.0322(4) Uani 1 1 d . . . . .
H13A H 0.5002 -0.0067 0.1720 0.039 Uiso 1 1 calc R U . . .
C14 C 0.65698(19) 0.05211(7) 0.22074(9) 0.0271(4) Uani 1 1 d . . . . .
C15 C 0.5754(2) 0.06932(9) 0.29258(11) 0.0354(4) Uani 1 1 d . . . . .
H15A H 0.6525 0.0800 0.3360 0.042 Uiso 1 1 calc R U . . .
C16 C 0.4804(3) 0.01741(12) 0.32218(13) 0.0518(6) Uani 1 1 d . . . . .
H16A H 0.4451 0.0286 0.3734 0.078 Uiso 1 1 calc R U . . .
H16B H 0.5407 -0.0199 0.3279 0.078 Uiso 1 1 calc R U . . .
H16C H 0.3943 0.0102 0.2843 0.078 Uiso 1 1 calc R U . . .
C17 C 0.4787(3) 0.12618(11) 0.27519(14) 0.0531(6) Uani 1 1 d . . . . .
H17A H 0.4323 0.1385 0.3231 0.080 Uiso 1 1 calc R U . . .
H17B H 0.4005 0.1168 0.2335 0.080 Uiso 1 1 calc R U . . .
H17C H 0.5413 0.1596 0.2579 0.080 Uiso 1 1 calc R U . . .
C18 C 1.0217(2) 0.09114(10) 0.12633(12) 0.0405(5) Uani 1 1 d . . . . .
H18A H 1.0458 0.1237 0.1666 0.049 Uiso 1 1 calc R U . . .
C19 C 1.0220(3) 0.12049(11) 0.04415(15) 0.0556(6) Uani 1 1 d . . . . .
H19A H 1.1202 0.1387 0.0378 0.083 Uiso 1 1 calc R U . . .
H19B H 0.9450 0.1524 0.0386 0.083 Uiso 1 1 calc R U . . .
H19C H 1.0009 0.0891 0.0036 0.083 Uiso 1 1 calc R U . . .
C20 C 1.1440(2) 0.04263(13) 0.13527(13) 0.0537(6) Uani 1 1 d . . . . .
H20A H 1.2404 0.0612 0.1256 0.081 Uiso 1 1 calc R U . . .
H20B H 1.1214 0.0097 0.0971 0.081 Uiso 1 1 calc R U . . .
H20C H 1.1489 0.0258 0.1889 0.081 Uiso 1 1 calc R U . . .
C21 C 0.9750(2) 0.25231(7) 0.43277(10) 0.0279(4) Uani 1 1 d . . . . .
C22 C 1.0683(2) 0.30170(8) 0.41596(10) 0.0318(4) Uani 1 1 d . . . . .
C23 C 1.0882(2) 0.34914(9) 0.47111(12) 0.0395(5) Uani 1 1 d . . . . .
H23A H 1.1512 0.3826 0.4606 0.047 Uiso 1 1 calc R U . . .
C24 C 1.0181(3) 0.34821(9) 0.54030(12) 0.0455(5) Uani 1 1 d . . . . .
H24A H 1.0340 0.3805 0.5774 0.055 Uiso 1 1 calc R U . . .
C25 C 0.9248(2) 0.30017(9) 0.55572(11) 0.0408(5) Uani 1 1 d . . . . .
H25A H 0.8763 0.3001 0.6035 0.049 Uiso 1 1 calc R U . . .
C26 C 0.8998(2) 0.25163(8) 0.50296(10) 0.0322(4) Uani 1 1 d . . . . .
C27 C 0.7899(2) 0.20073(9) 0.51826(11) 0.0398(5) Uani 1 1 d . . . . .
H27A H 0.8365 0.1611 0.5037 0.048 Uiso 1 1 calc R U . . .
C28 C 0.7532(3) 0.19585(11) 0.60409(14) 0.0576(6) Uani 1 1 d . . . . .
H28A H 0.6885 0.1603 0.6104 0.086 Uiso 1 1 calc R U . . .
H28B H 0.7016 0.2331 0.6192 0.086 Uiso 1 1 calc R U . . .
H28C H 0.8460 0.1910 0.6379 0.086 Uiso 1 1 calc R U . . .
C29 C 0.6436(3) 0.20777(11) 0.46649(14) 0.0540(6) Uani 1 1 d . . . . .
H29A H 0.5763 0.1739 0.4768 0.081 Uiso 1 1 calc R U . . .
H29B H 0.6648 0.2073 0.4108 0.081 Uiso 1 1 calc R U . . .
H29C H 0.5961 0.2467 0.4787 0.081 Uiso 1 1 calc R U . . .
C30 C 1.1459(2) 0.30237(8) 0.33967(11) 0.0362(4) Uani 1 1 d . . . . .
H30A H 1.0772 0.2823 0.2983 0.043 Uiso 1 1 calc R U . . .
C31 C 1.1784(3) 0.36655(10) 0.31048(15) 0.0569(6) Uani 1 1 d . . . . .
H31A H 1.2149 0.3641 0.2577 0.085 Uiso 1 1 calc R U . . .
H31B H 1.2546 0.3859 0.3467 0.085 Uiso 1 1 calc R U . . .
H31C H 1.0866 0.3910 0.3083 0.085 Uiso 1 1 calc R U . . .
C32 C 1.2885(3) 0.26451(12) 0.34816(16) 0.0609(7) Uani 1 1 d . . . . .
H32A H 1.3340 0.2634 0.2976 0.091 Uiso 1 1 calc R U . . .
H32B H 1.2647 0.2227 0.3640 0.091 Uiso 1 1 calc R U . . .
H32C H 1.3588 0.2830 0.3883 0.091 Uiso 1 1 calc R U . . .
C33A C 0.8167(5) 0.2552(2) 0.1165(2) 0.0691(9) Uani 0.7 1 d D U P A 1
H33A H 0.8256 0.2681 0.0619 0.104 Uiso 0.7 1 calc R U P A 1
H33B H 0.7524 0.2189 0.1170 0.104 Uiso 0.7 1 calc R U P A 1
H33C H 0.9161 0.2452 0.1412 0.104 Uiso 0.7 1 calc R U P A 1
C33 C 0.6918(11) 0.3812(4) 0.1944(6) 0.069(2) Uiso 0.3 1 d D U P A 2
H33D H 0.7764 0.4105 0.1986 0.082 Uiso 0.3 1 calc R U P A 2
H33E H 0.6213 0.3943 0.1499 0.082 Uiso 0.3 1 calc R U P A 2
C34A C 0.7506(8) 0.3051(3) 0.1606(3) 0.0824(12) Uani 0.7 1 d D U P A 1
H34A H 0.8112 0.3427 0.1566 0.099 Uiso 0.7 1 calc R U P A 1
H34B H 0.6482 0.3138 0.1374 0.099 Uiso 0.7 1 calc R U P A 1
C34 C 0.7493(15) 0.3179(5) 0.1785(7) 0.062(3) Uiso 0.3 1 d D U P A 2
H34C H 0.6936 0.2993 0.1320 0.075 Uiso 0.3 1 calc R U P A 2
H34D H 0.8572 0.3187 0.1699 0.075 Uiso 0.3 1 calc R U P A 2
C35A C 0.7343(7) 0.3406(2) 0.2947(3) 0.0824(12) Uani 0.7 1 d D U P A 1
H35A H 0.7374 0.3241 0.3491 0.099 Uiso 0.7 1 calc R U P A 1
H35B H 0.8241 0.3666 0.2914 0.099 Uiso 0.7 1 calc R U P A 1
C35 C 0.6892(11) 0.3285(4) 0.3172(5) 0.052(2) Uiso 0.3 1 d D U P A 2
H35C H 0.7809 0.3411 0.3492 0.062 Uiso 0.3 1 calc R U P A 2
H35D H 0.6149 0.3121 0.3518 0.062 Uiso 0.3 1 calc R U P A 2
C36A C 0.6042(6) 0.3793(3) 0.2827(3) 0.0691(9) Uani 0.7 1 d D U P A 1
H36A H 0.5960 0.4052 0.3291 0.104 Uiso 0.7 1 calc R U P A 1
H36B H 0.5145 0.3537 0.2745 0.104 Uiso 0.7 1 calc R U P A 1
H36C H 0.6135 0.4051 0.2362 0.104 Uiso 0.7 1 calc R U P A 1
C36 C 0.6224(12) 0.3820(5) 0.2613(5) 0.046(2) Uiso 0.3 1 d D . P A 2
H36D H 0.5137 0.3759 0.2495 0.055 Uiso 0.3 1 calc R U P A 2
H36E H 0.6381 0.4221 0.2879 0.055 Uiso 0.3 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O1 1.852(15) . ?
Li1 O1A 1.901(5) . ?
Li1 N1 1.950(3) . ?
Li1 N2 1.961(3) . ?
Li1 C1 2.707(3) . ?
Li1 C2 2.708(3) . ?
O1A C34A 1.403(7) . ?
O1A C35A 1.471(6) . ?
O1 C34 1.482(14) . ?
O1 C35 1.515(14) . ?
N1 C1 1.337(2) . ?
N1 C21 1.419(2) . ?
N2 C2 1.339(2) . ?
N2 C9 1.4252(19) . ?
C1 C6 1.427(2) . ?
C1 C2 1.464(2) . ?
C2 C3 1.426(2) . ?
C3 C4 1.374(2) . ?
C4 C5 1.426(2) . ?
C4 C8 1.506(2) . ?
C5 C6 1.374(2) . ?
C5 C7 1.507(2) . ?
C9 C10 1.405(2) . ?
C9 C14 1.411(2) . ?
C10 C11 1.396(2) . ?
C10 C18 1.518(3) . ?
C11 C12 1.377(3) . ?
C12 C13 1.380(3) . ?
C13 C14 1.393(2) . ?
C14 C15 1.519(2) . ?
C15 C16 1.527(3) . ?
C15 C17 1.531(3) . ?
C18 C20 1.525(3) . ?
C18 C19 1.538(3) . ?
C21 C22 1.408(3) . ?
C21 C26 1.415(3) . ?
C22 C23 1.400(2) . ?
C22 C30 1.519(3) . ?
C23 C24 1.376(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.396(2) . ?
C26 C27 1.522(3) . ?
C27 C28 1.524(3) . ?
C27 C29 1.531(3) . ?
C30 C32 1.521(3) . ?
C30 C31 1.523(3) . ?
C33A C34A 1.475(6) . ?
C33 C36 1.337(11) . ?
C33 C34 1.508(12) . ?
C35A C36A 1.442(7) . ?
C35 C36 1.593(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li1 N1 117.7(5) . . ?
O1A Li1 N1 118.7(2) . . ?
O1 Li1 N2 154.9(6) . . ?
O1A Li1 N2 153.8(2) . . ?
N1 Li1 N2 86.96(14) . . ?
O1 Li1 C1 145.4(5) . . ?
O1A Li1 C1 145.9(2) . . ?
N1 Li1 C1 27.75(7) . . ?
N2 Li1 C1 59.26(9) . . ?
O1 Li1 C2 175.0(5) . . ?
O1A Li1 C2 173.9(3) . . ?
N1 Li1 C2 59.07(9) . . ?
N2 Li1 C2 27.90(7) . . ?
C1 Li1 C2 31.36(6) . . ?
C34A O1A C35A 114.9(4) . . ?
C34A O1A Li1 120.1(4) . . ?
C35A O1A Li1 121.5(3) . . ?
C34 O1 C35 111.0(10) . . ?
C34 O1 Li1 120.6(10) . . ?
C35 O1 Li1 119.9(9) . . ?
C1 N1 C21 121.06(13) . . ?
C1 N1 Li1 109.48(13) . . ?
C21 N1 Li1 129.41(14) . . ?
C2 N2 C9 118.31(13) . . ?
C2 N2 Li1 108.85(13) . . ?
C9 N2 Li1 132.63(14) . . ?
N1 C1 C6 125.26(14) . . ?
N1 C1 C2 117.03(14) . . ?
C6 C1 C2 117.71(14) . . ?
N1 C1 Li1 42.78(10) . . ?
C6 C1 Li1 167.62(13) . . ?
C2 C1 Li1 74.35(11) . . ?
N2 C2 C3 125.38(14) . . ?
N2 C2 C1 117.54(13) . . ?
C3 C2 C1 117.06(14) . . ?
N2 C2 Li1 43.24(10) . . ?
C3 C2 Li1 168.51(13) . . ?
C1 C2 Li1 74.29(10) . . ?
C4 C3 C2 123.15(15) . . ?
C3 C4 C5 119.62(14) . . ?
C3 C4 C8 120.21(16) . . ?
C5 C4 C8 120.16(16) . . ?
C6 C5 C4 119.31(15) . . ?
C6 C5 C7 120.54(16) . . ?
C4 C5 C7 120.14(15) . . ?
C5 C6 C1 122.95(15) . . ?
C10 C9 C14 120.18(14) . . ?
C10 C9 N2 121.07(15) . . ?
C14 C9 N2 118.62(14) . . ?
C11 C10 C9 118.55(16) . . ?
C11 C10 C18 119.37(16) . . ?
C9 C10 C18 122.08(15) . . ?
C12 C11 C10 121.75(17) . . ?
C11 C12 C13 119.29(16) . . ?
C12 C13 C14 121.49(17) . . ?
C13 C14 C9 118.73(15) . . ?
C13 C14 C15 121.12(16) . . ?
C9 C14 C15 120.13(14) . . ?
C14 C15 C16 113.38(16) . . ?
C14 C15 C17 110.26(16) . . ?
C16 C15 C17 110.14(18) . . ?
C10 C18 C20 111.24(18) . . ?
C10 C18 C19 112.02(17) . . ?
C20 C18 C19 109.21(18) . . ?
C22 C21 C26 120.55(15) . . ?
C22 C21 N1 118.84(15) . . ?
C26 C21 N1 120.24(16) . . ?
C23 C22 C21 118.57(17) . . ?
C23 C22 C30 121.47(17) . . ?
C21 C22 C30 119.96(15) . . ?
C24 C23 C22 121.27(19) . . ?
C23 C24 C25 119.81(17) . . ?
C24 C25 C26 121.69(18) . . ?
C25 C26 C21 118.08(18) . . ?
C25 C26 C27 121.28(17) . . ?
C21 C26 C27 120.58(15) . . ?
C26 C27 C28 113.89(17) . . ?
C26 C27 C29 111.49(17) . . ?
C28 C27 C29 108.63(19) . . ?
C22 C30 C32 110.54(16) . . ?
C22 C30 C31 113.51(16) . . ?
C32 C30 C31 110.56(19) . . ?
C36 C33 C34 110.6(9) . . ?
O1A C34A C33A 110.3(4) . . ?
O1 C34 C33 102.6(9) . . ?
C36A C35A O1A 117.0(5) . . ?
O1 C35 C36 96.4(8) . . ?
C33 C36 C35 108.6(8) . . ?

_refine_diff_density_max         0.716
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.050

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_10
_database_code_depnum_ccdc_archive 'CCDC 1479773'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H58 N5 Ta'
_chemical_formula_weight         813.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4591(8)
_cell_length_b                   12.8533(10)
_cell_length_c                   16.2426(13)
_cell_angle_alpha                69.066(3)
_cell_angle_beta                 82.852(4)
_cell_angle_gamma                76.536(3)
_cell_volume                     1981.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8284
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.68

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             836
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.808
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23806
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         27.685
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             9050
_reflns_number_gt                8242
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0218P)²+0.3785P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9050
_refine_ls_number_parameters     447
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0499
_refine_ls_wR_factor_gt          0.0482
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.69057(2) 0.73958(2) 0.75132(2) 0.01435(3) Uani 1 1 d . . . . .
N1 N 0.49852(18) 0.75057(15) 0.79740(12) 0.0151(4) Uani 1 1 d . . . . .
N2 N 0.67179(18) 0.83101(15) 0.83617(11) 0.0148(4) Uani 1 1 d . . . . .
N3 N 0.62458(19) 0.70162(17) 0.65390(12) 0.0202(4) Uani 1 1 d . . . . .
N4 N 0.75325(19) 0.65842(16) 0.64893(12) 0.0173(4) Uani 1 1 d . . . . .
N5 N 0.8006(2) 0.61361(17) 0.59113(13) 0.0228(4) Uani 1 1 d . . . . .
C1 C 0.4600(2) 0.78948(18) 0.86929(14) 0.0148(4) Uani 1 1 d . . . . .
C2 C 0.5572(2) 0.83295(18) 0.89134(14) 0.0151(4) Uani 1 1 d . . . . .
C3 C 0.5315(2) 0.87300(19) 0.96233(15) 0.0196(5) Uani 1 1 d . . . . .
H3A H 0.5963 0.9026 0.9781 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4118(2) 0.8698(2) 1.00993(15) 0.0222(5) Uani 1 1 d . . . . .
H4A H 0.3953 0.8967 1.0584 0.027 Uiso 1 1 calc R U . . .
C5 C 0.3163(2) 0.8274(2) 0.98710(16) 0.0234(5) Uani 1 1 d . . . . .
H5B H 0.2342 0.8262 1.0196 0.028 Uiso 1 1 calc R U . . .
C6 C 0.3401(2) 0.7868(2) 0.91708(15) 0.0207(5) Uani 1 1 d . . . . .
H6A H 0.2747 0.7573 0.9018 0.025 Uiso 1 1 calc R U . . .
C7 C 0.8147(2) 0.8560(2) 0.66745(16) 0.0243(5) Uani 1 1 d . . . . .
H7A H 0.8232 0.9091 0.6963 0.037 Uiso 1 1 calc R U . . .
H7B H 0.7745 0.8986 0.6105 0.037 Uiso 1 1 calc R U . . .
H7C H 0.9020 0.8123 0.6580 0.037 Uiso 1 1 calc R U . . .
C8 C 0.8000(2) 0.5854(2) 0.83925(16) 0.0251(5) Uani 1 1 d . . . . .
H8A H 0.7751 0.5809 0.9004 0.038 Uiso 1 1 calc R U . . .
H8B H 0.8944 0.5849 0.8281 0.038 Uiso 1 1 calc R U . . .
H8C H 0.7806 0.5199 0.8294 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5422(2) 0.6963(2) 0.59065(16) 0.0270(6) Uani 1 1 d . . . . .
H9A H 0.5452 0.6166 0.5984 0.040 Uiso 1 1 calc R U . . .
H9B H 0.5744 0.7352 0.5307 0.040 Uiso 1 1 calc R U . . .
H9C H 0.4514 0.7336 0.6001 0.040 Uiso 1 1 calc R U . . .
C10 C 0.9409(2) 0.5716(2) 0.59403(15) 0.0200(5) Uani 1 1 d . . . . .
C11 C 1.0222(2) 0.6366(2) 0.53207(15) 0.0225(5) Uani 1 1 d . . . . .
C12 C 1.1566(2) 0.5921(2) 0.53043(16) 0.0244(5) Uani 1 1 d . . . . .
H12A H 1.2126 0.6360 0.4886 0.029 Uiso 1 1 calc R U . . .
C13 C 1.2118(2) 0.4859(2) 0.58771(16) 0.0250(5) Uani 1 1 d . . . . .
C14 C 1.1273(3) 0.4222(2) 0.64629(16) 0.0263(5) Uani 1 1 d . . . . .
H14A H 1.1634 0.3488 0.6854 0.032 Uiso 1 1 calc R U . . .
C15 C 0.9923(2) 0.4616(2) 0.65001(16) 0.0238(5) Uani 1 1 d . . . . .
C16 C 0.9657(3) 0.7519(2) 0.46818(17) 0.0339(6) Uani 1 1 d . . . . .
H16A H 1.0320 0.7766 0.4213 0.051 Uiso 1 1 calc R U . . .
H16B H 0.9401 0.8068 0.4994 0.051 Uiso 1 1 calc R U . . .
H16C H 0.8882 0.7475 0.4423 0.051 Uiso 1 1 calc R U . . .
C17 C 1.3580(3) 0.4412(3) 0.58650(19) 0.0361(6) Uani 1 1 d . . . . .
H17A H 1.3758 0.3583 0.6017 0.054 Uiso 1 1 calc R U . . .
H17B H 1.3972 0.4604 0.6296 0.054 Uiso 1 1 calc R U . . .
H17C H 1.3963 0.4756 0.5274 0.054 Uiso 1 1 calc R U . . .
C18 C 0.9034(3) 0.3852(2) 0.70978(19) 0.0349(6) Uani 1 1 d . . . . .
H18A H 0.9505 0.3057 0.7263 0.052 Uiso 1 1 calc R U . . .
H18B H 0.8246 0.3949 0.6787 0.052 Uiso 1 1 calc R U . . .
H18C H 0.8776 0.4054 0.7631 0.052 Uiso 1 1 calc R U . . .
C19 C 0.3905(2) 0.72594(19) 0.76470(14) 0.0164(4) Uani 1 1 d . . . . .
C20 C 0.3757(2) 0.6130(2) 0.78852(15) 0.0200(5) Uani 1 1 d . . . . .
C21 C 0.2689(2) 0.5937(2) 0.75548(16) 0.0262(5) Uani 1 1 d . . . . .
H21A H 0.2570 0.5179 0.7704 0.031 Uiso 1 1 calc R U . . .
C22 C 0.1814(3) 0.6812(2) 0.70231(17) 0.0302(6) Uani 1 1 d . . . . .
H22A H 0.1103 0.6658 0.6804 0.036 Uiso 1 1 calc R U . . .
C23 C 0.1969(2) 0.7927(2) 0.68038(16) 0.0273(6) Uani 1 1 d . . . . .
H23A H 0.1354 0.8532 0.6438 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3008(2) 0.8173(2) 0.71106(15) 0.0203(5) Uani 1 1 d . . . . .
C25 C 0.3140(3) 0.9405(2) 0.68667(17) 0.0274(6) Uani 1 1 d . . . . .
H25A H 0.3891 0.9403 0.7193 0.033 Uiso 1 1 calc R U . . .
C26 C 0.3474(4) 0.9930(3) 0.5881(2) 0.0531(9) Uani 1 1 d . . . . .
H26A H 0.4308 0.9492 0.5725 0.080 Uiso 1 1 calc R U . . .
H26B H 0.3556 1.0718 0.5747 0.080 Uiso 1 1 calc R U . . .
H26C H 0.2773 0.9915 0.5540 0.080 Uiso 1 1 calc R U . . .
C27 C 0.1915(3) 1.0118(2) 0.7157(2) 0.0405(7) Uani 1 1 d . . . . .
H27A H 0.1736 0.9770 0.7792 0.061 Uiso 1 1 calc R U . . .
H27B H 0.1163 1.0155 0.6836 0.061 Uiso 1 1 calc R U . . .
H27C H 0.2058 1.0888 0.7030 0.061 Uiso 1 1 calc R U . . .
C28 C 0.4658(2) 0.5140(2) 0.85084(16) 0.0239(5) Uani 1 1 d . . . . .
H28A H 0.5367 0.5444 0.8651 0.029 Uiso 1 1 calc R U . . .
C29 C 0.5321(3) 0.4245(2) 0.8086(2) 0.0391(7) Uani 1 1 d . . . . .
H29A H 0.5789 0.4607 0.7533 0.059 Uiso 1 1 calc R U . . .
H29B H 0.4650 0.3905 0.7964 0.059 Uiso 1 1 calc R U . . .
H29C H 0.5947 0.3651 0.8491 0.059 Uiso 1 1 calc R U . . .
C30 C 0.3922(3) 0.4599(3) 0.93726(18) 0.0385(7) Uani 1 1 d . . . . .
H30A H 0.3533 0.5176 0.9644 0.058 Uiso 1 1 calc R U . . .
H30B H 0.4536 0.3987 0.9775 0.058 Uiso 1 1 calc R U . . .
H30C H 0.3223 0.4286 0.9254 0.058 Uiso 1 1 calc R U . . .
C31 C 0.7530(2) 0.90548(19) 0.84218(14) 0.0176(5) Uani 1 1 d . . . . .
C32 C 0.7234(2) 1.0218(2) 0.78931(15) 0.0204(5) Uani 1 1 d . . . . .
C33 C 0.7999(3) 1.0934(2) 0.79709(17) 0.0265(6) Uani 1 1 d . . . . .
H33A H 0.7821 1.1718 0.7620 0.032 Uiso 1 1 calc R U . . .
C34 C 0.9005(3) 1.0527(2) 0.85455(18) 0.0288(6) Uani 1 1 d . . . . .
H34A H 0.9522 1.1026 0.8580 0.035 Uiso 1 1 calc R U . . .
C35 C 0.9266(2) 0.9396(2) 0.90727(17) 0.0275(6) Uani 1 1 d . . . . .
H35A H 0.9961 0.9125 0.9469 0.033 Uiso 1 1 calc R U . . .
C36 C 0.8522(2) 0.8641(2) 0.90324(15) 0.0210(5) Uani 1 1 d . . . . .
C37 C 0.8799(2) 0.7416(2) 0.96563(16) 0.0271(6) Uani 1 1 d . . . . .
H37A H 0.8138 0.7027 0.9558 0.032 Uiso 1 1 calc R U . . .
C38 C 1.0166(3) 0.6783(3) 0.9462(2) 0.0435(8) Uani 1 1 d . . . . .
H38A H 1.0269 0.6872 0.8834 0.065 Uiso 1 1 calc R U . . .
H38B H 1.0268 0.5973 0.9815 0.065 Uiso 1 1 calc R U . . .
H38C H 1.0838 0.7097 0.9611 0.065 Uiso 1 1 calc R U . . .
C39 C 0.8642(3) 0.7342(3) 1.06284(18) 0.0470(8) Uani 1 1 d . . . . .
H39A H 0.7750 0.7724 1.0749 0.071 Uiso 1 1 calc R U . . .
H39B H 0.9283 0.7713 1.0746 0.071 Uiso 1 1 calc R U . . .
H39C H 0.8791 0.6541 1.1009 0.071 Uiso 1 1 calc R U . . .
C40 C 0.6106(3) 1.0712(2) 0.72663(16) 0.0257(5) Uani 1 1 d . . . . .
H40A H 0.5878 1.0066 0.7149 0.031 Uiso 1 1 calc R U . . .
C41 C 0.6477(3) 1.1554(2) 0.63763(18) 0.0406(7) Uani 1 1 d . . . . .
H41A H 0.7297 1.1203 0.6132 0.061 Uiso 1 1 calc R U . . .
H41B H 0.6598 1.2242 0.6460 0.061 Uiso 1 1 calc R U . . .
H41C H 0.5772 1.1755 0.5968 0.061 Uiso 1 1 calc R U . . .
C42 C 0.4868(3) 1.1286(2) 0.76801(19) 0.0333(6) Uani 1 1 d . . . . .
H42A H 0.4602 1.0733 0.8232 0.050 Uiso 1 1 calc R U . . .
H42B H 0.4154 1.1565 0.7269 0.050 Uiso 1 1 calc R U . . .
H42C H 0.5060 1.1925 0.7803 0.050 Uiso 1 1 calc R U . . .


_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
Ta1 N1 2.0456(18) . ?
Ta1 N3 2.0491(19) . ?
Ta1 N2 2.0740(17) . ?
Ta1 C8 2.146(2) . ?
Ta1 C7 2.188(2) . ?
Ta1 N4 2.2211(18) . ?
N1 C1 1.408(3) . ?
N1 C19 1.448(3) . ?
N2 C2 1.405(3) . ?
N2 C31 1.454(3) . ?
N3 N4 1.335(3) . ?
N3 C9 1.449(3) . ?
N4 N5 1.264(3) . ?
N5 C10 1.442(3) . ?
C1 C6 1.391(3) . ?
C1 C2 1.405(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.386(3) . ?
C5 C6 1.386(3) . ?
C10 C11 1.396(3) . ?
C10 C15 1.401(3) . ?
C11 C12 1.390(3) . ?
C11 C16 1.506(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.388(3) . ?
C13 C17 1.503(3) . ?
C14 C15 1.386(3) . ?
C15 C18 1.514(3) . ?
C19 C20 1.404(3) . ?
C19 C24 1.406(3) . ?
C20 C21 1.404(3) . ?
C20 C28 1.513(3) . ?
C21 C22 1.368(4) . ?
C22 C23 1.392(4) . ?
C23 C24 1.392(3) . ?
C24 C25 1.523(3) . ?
C25 C27 1.522(4) . ?
C25 C26 1.529(4) . ?
C28 C30 1.526(3) . ?
C28 C29 1.533(4) . ?
C31 C36 1.402(3) . ?
C31 C32 1.415(3) . ?
C32 C33 1.399(3) . ?
C32 C40 1.523(3) . ?
C33 C34 1.375(4) . ?
C34 C35 1.380(4) . ?
C35 C36 1.401(3) . ?
C36 C37 1.520(3) . ?
C37 C38 1.529(4) . ?
C37 C39 1.538(4) . ?
C40 C41 1.533(3) . ?
C40 C42 1.538(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ta1 N3 83.71(7) . . ?
N1 Ta1 N2 75.57(7) . . ?
N3 Ta1 N2 152.50(8) . . ?
N1 Ta1 C8 106.59(8) . . ?
N3 Ta1 C8 108.16(9) . . ?
N2 Ta1 C8 95.12(8) . . ?
N1 Ta1 C7 137.13(8) . . ?
N3 Ta1 C7 97.76(8) . . ?
N2 Ta1 C7 85.79(8) . . ?
C8 Ta1 C7 113.34(10) . . ?
N1 Ta1 N4 117.33(7) . . ?
N3 Ta1 N4 36.16(7) . . ?
N2 Ta1 N4 166.45(7) . . ?
C8 Ta1 N4 85.34(8) . . ?
C7 Ta1 N4 81.63(8) . . ?
C1 N1 C19 112.78(17) . . ?
C1 N1 Ta1 118.43(14) . . ?
C19 N1 Ta1 128.77(14) . . ?
C2 N2 C31 112.47(17) . . ?
C2 N2 Ta1 117.20(13) . . ?
C31 N2 Ta1 129.97(14) . . ?
N4 N3 C9 117.94(19) . . ?
N4 N3 Ta1 78.96(12) . . ?
C9 N3 Ta1 162.88(17) . . ?
N5 N4 N3 120.56(19) . . ?
N5 N4 Ta1 174.16(16) . . ?
N3 N4 Ta1 64.89(11) . . ?
N4 N5 C10 113.86(19) . . ?
C6 C1 C2 120.6(2) . . ?
C6 C1 N1 126.17(19) . . ?
C2 C1 N1 113.23(18) . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 N2 127.6(2) . . ?
C1 C2 N2 113.65(18) . . ?
C4 C3 C2 120.3(2) . . ?
C5 C4 C3 120.3(2) . . ?
C6 C5 C4 120.2(2) . . ?
C5 C6 C1 119.7(2) . . ?
C11 C10 C15 121.0(2) . . ?
C11 C10 N5 118.4(2) . . ?
C15 C10 N5 120.1(2) . . ?
C12 C11 C10 118.4(2) . . ?
C12 C11 C16 120.7(2) . . ?
C10 C11 C16 120.9(2) . . ?
C13 C12 C11 122.2(2) . . ?
C12 C13 C14 117.6(2) . . ?
C12 C13 C17 121.2(2) . . ?
C14 C13 C17 121.2(2) . . ?
C15 C14 C13 122.6(2) . . ?
C14 C15 C10 118.0(2) . . ?
C14 C15 C18 120.5(2) . . ?
C10 C15 C18 121.4(2) . . ?
C20 C19 C24 121.7(2) . . ?
C20 C19 N1 119.8(2) . . ?
C24 C19 N1 118.5(2) . . ?
C19 C20 C21 117.6(2) . . ?
C19 C20 C28 122.7(2) . . ?
C21 C20 C28 119.7(2) . . ?
C22 C21 C20 121.7(2) . . ?
C21 C22 C23 119.8(2) . . ?
C24 C23 C22 121.2(2) . . ?
C23 C24 C19 118.0(2) . . ?
C23 C24 C25 119.9(2) . . ?
C19 C24 C25 122.1(2) . . ?
C27 C25 C24 111.6(2) . . ?
C27 C25 C26 111.3(2) . . ?
C24 C25 C26 111.5(2) . . ?
C20 C28 C30 111.2(2) . . ?
C20 C28 C29 112.0(2) . . ?
C30 C28 C29 110.6(2) . . ?
C36 C31 C32 121.1(2) . . ?
C36 C31 N2 120.4(2) . . ?
C32 C31 N2 118.3(2) . . ?
C33 C32 C31 117.9(2) . . ?
C33 C32 C40 119.5(2) . . ?
C31 C32 C40 122.5(2) . . ?
C34 C33 C32 121.3(2) . . ?
C33 C34 C35 120.3(2) . . ?
C34 C35 C36 121.0(2) . . ?
C35 C36 C31 118.3(2) . . ?
C35 C36 C37 119.2(2) . . ?
C31 C36 C37 122.5(2) . . ?
C36 C37 C38 111.4(2) . . ?
C36 C37 C39 111.9(2) . . ?
C38 C37 C39 110.4(2) . . ?
C32 C40 C41 112.7(2) . . ?
C32 C40 C42 111.7(2) . . ?
C41 C40 C42 109.6(2) . . ?

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.081

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ax3_0m
_database_code_depnum_ccdc_archive 'CCDC 1479774'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H88 N4 Ta2'
_chemical_formula_weight         1275.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.9017(5)
_cell_length_b                   19.5480(4)
_cell_length_c                   22.0555(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.2620(11)
_cell_angle_gamma                90
_cell_volume                     6850.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11283
_cell_measurement_theta_min      1.282
_cell_measurement_theta_max      27.541

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             2584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.227
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6454
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'Apex 2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Alpha Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65508
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.282
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15746
_reflns_number_gt                11283
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15746
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.65865(2) 0.21099(2) 0.30740(2) 0.02337(5) Uani 1 1 d . . . . .
Ta2 Ta 0.76242(2) 0.31257(2) 0.34810(2) 0.02265(5) Uani 1 1 d . . . . .
N1 N 0.5410(2) 0.19871(16) 0.27031(15) 0.0266(8) Uani 1 1 d . . . . .
N2 N 0.6578(2) 0.10717(17) 0.30422(14) 0.0265(8) Uani 1 1 d . . . . .
N3 N 0.7837(2) 0.36920(16) 0.42447(13) 0.0224(8) Uani 1 1 d . . . . .
N4 N 0.8608(2) 0.36864(17) 0.31938(14) 0.0280(8) Uani 1 1 d . . . . .
C1 C 0.5214(3) 0.1288(2) 0.25545(18) 0.0318(11) Uani 1 1 d . . . . .
C2 C 0.5840(3) 0.0812(2) 0.27343(18) 0.0308(10) Uani 1 1 d . . . . .
C3 C 0.5711(4) 0.0116(2) 0.2603(2) 0.0452(13) Uani 1 1 d . . . . .
H3A H 0.6133 -0.0211 0.2712 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4962(4) -0.0090(3) 0.2314(3) 0.0611(17) Uani 1 1 d . . . . .
H4A H 0.4873 -0.0561 0.2228 0.073 Uiso 1 1 calc R U . . .
C5 C 0.4358(4) 0.0369(3) 0.2153(2) 0.0594(16) Uani 1 1 d . . . . .
H5A H 0.3846 0.0217 0.1961 0.071 Uiso 1 1 calc R U . . .
C6 C 0.4481(3) 0.1075(2) 0.2266(2) 0.0470(13) Uani 1 1 d . . . . .
H6A H 0.4061 0.1397 0.2143 0.056 Uiso 1 1 calc R U . . .
C7 C 0.4709(3) 0.2453(2) 0.2568(2) 0.0312(10) Uani 1 1 d . . . . .
C8 C 0.4100(3) 0.2572(2) 0.3011(2) 0.0405(12) Uani 1 1 d . . . . .
C9 C 0.3449(3) 0.3030(3) 0.2868(3) 0.0567(16) Uani 1 1 d . . . . .
H9A H 0.3040 0.3125 0.3159 0.068 Uiso 1 1 calc R U . . .
C10 C 0.3390(3) 0.3346(3) 0.2310(3) 0.0578(16) Uani 1 1 d . . . . .
H10A H 0.2941 0.3655 0.2222 0.069 Uiso 1 1 calc R U . . .
C11 C 0.3971(3) 0.3220(2) 0.1882(3) 0.0488(14) Uani 1 1 d . . . . .
H11A H 0.3920 0.3447 0.1501 0.059 Uiso 1 1 calc R U . . .
C12 C 0.4638(3) 0.2766(2) 0.1993(2) 0.0359(11) Uani 1 1 d . . . . .
C13 C 0.5228(3) 0.2624(2) 0.1493(2) 0.0470(10) Uani 1 1 d D . . . .
H13A H 0.5698 0.2317 0.1634 0.056 Uiso 0.5 1 calc R U P A 1
H13B H 0.5662 0.2321 0.1693 0.056 Uiso 0.5 1 calc R U P B 2
C14 C 0.4765(10) 0.2337(6) 0.0928(5) 0.0470(10) Uani 0.5 1 d D . P C 1
H14A H 0.4444 0.1931 0.1038 0.070 Uiso 0.5 1 calc R U P C 1
H14B H 0.5175 0.2212 0.0627 0.070 Uiso 0.5 1 calc R U P C 1
H14C H 0.4380 0.2684 0.0756 0.070 Uiso 0.5 1 calc R U P C 1
C14A C 0.4818(10) 0.2160(5) 0.1005(5) 0.0470(10) Uani 0.5 1 d D . P C 2
H14D H 0.5215 0.2079 0.0684 0.070 Uiso 0.5 1 calc R U P C 2
H14E H 0.4310 0.2381 0.0832 0.070 Uiso 0.5 1 calc R U P C 2
H14F H 0.4666 0.1722 0.1188 0.070 Uiso 0.5 1 calc R U P C 2
C15 C 0.5559(9) 0.3276(6) 0.1213(6) 0.0470(10) Uani 0.5 1 d D . P C 1
H15A H 0.5750 0.3590 0.1536 0.070 Uiso 0.5 1 calc R U P C 1
H15B H 0.5110 0.3493 0.0964 0.070 Uiso 0.5 1 calc R U P C 1
H15C H 0.6032 0.3165 0.0959 0.070 Uiso 0.5 1 calc R U P C 1
C15A C 0.5734(8) 0.3258(6) 0.1327(6) 0.0470(10) Uani 0.5 1 d D . P C 2
H15D H 0.6144 0.3135 0.1025 0.070 Uiso 0.5 1 calc R U P C 2
H15E H 0.6031 0.3437 0.1691 0.070 Uiso 0.5 1 calc R U P C 2
H15F H 0.5352 0.3609 0.1158 0.070 Uiso 0.5 1 calc R U P C 2
C16 C 0.4131(3) 0.2192(3) 0.3607(2) 0.0536(15) Uani 1 1 d . . . . .
H16A H 0.4693 0.1965 0.3655 0.064 Uiso 1 1 calc R U . . .
C17 C 0.3442(4) 0.1625(3) 0.3617(3) 0.0746(19) Uani 1 1 d . . . . .
H17A H 0.3478 0.1387 0.4008 0.112 Uiso 1 1 calc R U . . .
H17B H 0.3529 0.1298 0.3289 0.112 Uiso 1 1 calc R U . . .
H17C H 0.2885 0.1835 0.3560 0.112 Uiso 1 1 calc R U . . .
C18 C 0.4029(4) 0.2669(4) 0.4151(3) 0.086(2) Uani 1 1 d . . . . .
H18A H 0.4074 0.2402 0.4528 0.129 Uiso 1 1 calc R U . . .
H18B H 0.3476 0.2891 0.4118 0.129 Uiso 1 1 calc R U . . .
H18C H 0.4471 0.3018 0.4156 0.129 Uiso 1 1 calc R U . . .
C19 C 0.7125(3) 0.0543(2) 0.32873(19) 0.0313(10) Uani 1 1 d . . . . .
C20 C 0.7781(3) 0.0289(2) 0.2953(2) 0.0424(13) Uani 1 1 d . . . . .
C21 C 0.8291(4) -0.0230(3) 0.3199(3) 0.0609(17) Uani 1 1 d . . . . .
H21A H 0.8737 -0.0413 0.2975 0.073 Uiso 1 1 calc R U . . .
C22 C 0.8142(4) -0.0477(3) 0.3774(3) 0.0692(19) Uani 1 1 d . . . . .
H22A H 0.8503 -0.0817 0.3949 0.083 Uiso 1 1 calc R U . . .
C23 C 0.7492(4) -0.0241(3) 0.4092(2) 0.0561(16) Uani 1 1 d . . . . .
H23A H 0.7392 -0.0432 0.4478 0.067 Uiso 1 1 calc R U . . .
C24 C 0.6964(3) 0.0277(2) 0.3864(2) 0.0367(11) Uani 1 1 d . . . . .
C25 C 0.6221(3) 0.0513(2) 0.4225(2) 0.0426(13) Uani 1 1 d . . . . .
H25A H 0.5989 0.0937 0.4028 0.051 Uiso 1 1 calc R U . . .
C26 C 0.5519(4) -0.0026(3) 0.4215(2) 0.0606(17) Uani 1 1 d . . . . .
H26A H 0.5031 0.0156 0.4419 0.091 Uiso 1 1 calc R U . . .
H26B H 0.5722 -0.0439 0.4425 0.091 Uiso 1 1 calc R U . . .
H26C H 0.5356 -0.0139 0.3794 0.091 Uiso 1 1 calc R U . . .
C27 C 0.6475(4) 0.0687(3) 0.4885(2) 0.0641(18) Uani 1 1 d . . . . .
H27A H 0.5992 0.0885 0.5085 0.096 Uiso 1 1 calc R U . . .
H27B H 0.6939 0.1018 0.4894 0.096 Uiso 1 1 calc R U . . .
H27C H 0.6657 0.0270 0.5099 0.096 Uiso 1 1 calc R U . . .
C28 C 0.7958(4) 0.0536(2) 0.2323(2) 0.0499(14) Uani 1 1 d . . . . .
H28A H 0.7538 0.0902 0.2216 0.060 Uiso 1 1 calc R U . . .
C29 C 0.7826(5) -0.0052(3) 0.1853(2) 0.082(2) Uani 1 1 d . . . . .
H29A H 0.7967 0.0112 0.1449 0.123 Uiso 1 1 calc R U . . .
H29B H 0.7237 -0.0201 0.1845 0.123 Uiso 1 1 calc R U . . .
H29C H 0.8192 -0.0438 0.1968 0.123 Uiso 1 1 calc R U . . .
C30 C 0.8831(4) 0.0851(3) 0.2282(3) 0.078(2) Uani 1 1 d . . . . .
H30A H 0.8912 0.1006 0.1866 0.117 Uiso 1 1 calc R U . . .
H30B H 0.9259 0.0507 0.2394 0.117 Uiso 1 1 calc R U . . .
H30C H 0.8885 0.1241 0.2559 0.117 Uiso 1 1 calc R U . . .
C31 C 0.8083(3) 0.2073(2) 0.3612(2) 0.0332(11) Uani 1 1 d . . . . .
H31A H 0.7655 0.1751 0.3455 0.050 Uiso 1 1 calc R U . . .
H31B H 0.8196 0.1989 0.4046 0.050 Uiso 1 1 calc R U . . .
H31C H 0.8602 0.2011 0.3393 0.050 Uiso 1 1 calc R U . . .
C32 C 0.7482(3) 0.2507(2) 0.24247(17) 0.0294(10) Uani 1 1 d . . . . .
H32A H 0.7819 0.2873 0.2617 0.044 Uiso 1 1 calc R U . . .
H32B H 0.7172 0.2688 0.2067 0.044 Uiso 1 1 calc R U . . .
H32C H 0.7854 0.2137 0.2301 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6446(3) 0.2443(2) 0.40114(17) 0.0302(10) Uani 1 1 d . . . . .
H33A H 0.6853 0.2807 0.4109 0.045 Uiso 1 1 calc R U . . .
H33B H 0.6549 0.2055 0.4286 0.045 Uiso 1 1 calc R U . . .
H33C H 0.5874 0.2616 0.4059 0.045 Uiso 1 1 calc R U . . .
C34 C 0.6425(3) 0.3437(2) 0.30473(18) 0.0296(10) Uani 1 1 d . . . . .
H34A H 0.6106 0.3030 0.2918 0.044 Uiso 1 1 calc R U . . .
H34B H 0.6531 0.3722 0.2693 0.044 Uiso 1 1 calc R U . . .
H34C H 0.6101 0.3699 0.3336 0.044 Uiso 1 1 calc R U . . .
C35 C 0.8451(3) 0.4213(2) 0.41688(18) 0.0267(10) Uani 1 1 d . . . . .
C36 C 0.8856(3) 0.4216(2) 0.36120(19) 0.0316(10) Uani 1 1 d . . . . .
C37 C 0.9444(3) 0.4713(2) 0.3504(2) 0.0419(13) Uani 1 1 d . . . . .
H37A H 0.9718 0.4718 0.3129 0.050 Uiso 1 1 calc R U . . .
C38 C 0.9640(3) 0.5206(3) 0.3934(2) 0.0475(14) Uani 1 1 d . . . . .
H38A H 1.0047 0.5546 0.3852 0.057 Uiso 1 1 calc R U . . .
C39 C 0.9254(3) 0.5208(2) 0.4479(2) 0.0441(13) Uani 1 1 d . . . . .
H39A H 0.9387 0.5552 0.4772 0.053 Uiso 1 1 calc R U . . .
C40 C 0.8664(3) 0.4704(2) 0.46009(19) 0.0330(11) Uani 1 1 d . . . . .
H40A H 0.8406 0.4697 0.4982 0.040 Uiso 1 1 calc R U . . .
C41 C 0.7478(3) 0.3682(2) 0.48372(18) 0.0299(10) Uani 1 1 d . . . . .
C42 C 0.7833(3) 0.3252(2) 0.52907(19) 0.0384(12) Uani 1 1 d . . . . .
C43 C 0.7472(4) 0.3256(3) 0.5855(2) 0.0573(17) Uani 1 1 d . . . . .
H43A H 0.7690 0.2959 0.6164 0.069 Uiso 1 1 calc R U . . .
C44 C 0.6809(5) 0.3677(4) 0.5977(2) 0.073(2) Uani 1 1 d . . . . .
H44A H 0.6583 0.3676 0.6370 0.087 Uiso 1 1 calc R U . . .
C45 C 0.6471(4) 0.4100(3) 0.5534(2) 0.0593(17) Uani 1 1 d . . . . .
H45A H 0.6005 0.4383 0.5621 0.071 Uiso 1 1 calc R U . . .
C46 C 0.6804(3) 0.4121(2) 0.4954(2) 0.0386(12) Uani 1 1 d . . . . .
C47 C 0.6417(3) 0.4606(2) 0.4479(2) 0.0460(13) Uani 1 1 d . . . . .
H47A H 0.6722 0.4541 0.4095 0.055 Uiso 1 1 calc R U . . .
C48 C 0.6533(4) 0.5358(2) 0.4680(3) 0.0718(19) Uani 1 1 d . . . . .
H48A H 0.7135 0.5470 0.4704 0.108 Uiso 1 1 calc R U . . .
H48B H 0.6296 0.5422 0.5080 0.108 Uiso 1 1 calc R U . . .
H48C H 0.6243 0.5659 0.4385 0.108 Uiso 1 1 calc R U . . .
C49 C 0.5495(3) 0.4440(3) 0.4346(2) 0.0566(15) Uani 1 1 d . . . . .
H49A H 0.5266 0.4752 0.4034 0.085 Uiso 1 1 calc R U . . .
H49B H 0.5183 0.4494 0.4717 0.085 Uiso 1 1 calc R U . . .
H49C H 0.5443 0.3967 0.4202 0.085 Uiso 1 1 calc R U . . .
C50 C 0.8579(4) 0.2801(2) 0.5188(2) 0.0538(12) Uani 1 1 d D . . . .
H50A H 0.8648 0.2846 0.4741 0.065 Uiso 0.5 1 calc R U P D 1
H50B H 0.8714 0.2773 0.4750 0.065 Uiso 0.5 1 calc R U P E 2
C51 C 0.8497(11) 0.2015(5) 0.5269(5) 0.0538(12) Uani 0.5 1 d D . P F 1
H51A H 0.9024 0.1793 0.5163 0.081 Uiso 0.5 1 calc R U P F 1
H51B H 0.8035 0.1844 0.5003 0.081 Uiso 0.5 1 calc R U P F 1
H51C H 0.8379 0.1912 0.5692 0.081 Uiso 0.5 1 calc R U P F 1
C51A C 0.8346(11) 0.2087(5) 0.5456(5) 0.0538(12) Uani 0.5 1 d D . P F 2
H51D H 0.8825 0.1776 0.5428 0.081 Uiso 0.5 1 calc R U P F 2
H51E H 0.7860 0.1898 0.5225 0.081 Uiso 0.5 1 calc R U P F 2
H51F H 0.8205 0.2141 0.5882 0.081 Uiso 0.5 1 calc R U P F 2
C52 C 0.9391(9) 0.3127(7) 0.5453(6) 0.0538(12) Uani 0.5 1 d D . P F 1
H52A H 0.9874 0.2844 0.5352 0.081 Uiso 0.5 1 calc R U P F 1
H52B H 0.9361 0.3161 0.5895 0.081 Uiso 0.5 1 calc R U P F 1
H52C H 0.9456 0.3586 0.5281 0.081 Uiso 0.5 1 calc R U P F 1
C52A C 0.9357(9) 0.3008(7) 0.5597(6) 0.0538(12) Uani 0.5 1 d D . P F 2
H52D H 0.9839 0.2722 0.5499 0.081 Uiso 0.5 1 calc R U P F 2
H52E H 0.9229 0.2943 0.6024 0.081 Uiso 0.5 1 calc R U P F 2
H52F H 0.9493 0.3490 0.5527 0.081 Uiso 0.5 1 calc R U P F 2
C53 C 0.9117(3) 0.3643(2) 0.2665(2) 0.0333(11) Uani 1 1 d . . . . .
C54 C 0.9834(3) 0.3226(2) 0.2686(2) 0.0456(13) Uani 1 1 d . . . . .
C55 C 1.0278(4) 0.3158(3) 0.2153(3) 0.0662(19) Uani 1 1 d . . . . .
H55A H 1.0761 0.2872 0.2154 0.079 Uiso 1 1 calc R U . . .
C56 C 1.0035(4) 0.3486(3) 0.1638(3) 0.071(2) Uani 1 1 d . . . . .
H56A H 1.0338 0.3417 0.1281 0.086 Uiso 1 1 calc R U . . .
C57 C 0.9353(4) 0.3919(3) 0.1624(2) 0.0567(16) Uani 1 1 d . . . . .
H57A H 0.9202 0.4158 0.1261 0.068 Uiso 1 1 calc R U . . .
C58 C 0.8878(3) 0.4012(2) 0.2141(2) 0.0390(12) Uani 1 1 d . . . . .
C59 C 0.8162(4) 0.4527(3) 0.2113(2) 0.0551(15) Uani 1 1 d . . . . .
H59A H 0.7881 0.4511 0.2511 0.066 Uiso 1 1 calc R U . . .
C60 C 0.7505(4) 0.4357(3) 0.1619(3) 0.076(2) Uani 1 1 d . . . . .
H60A H 0.7036 0.4681 0.1637 0.114 Uiso 1 1 calc R U . . .
H60B H 0.7297 0.3891 0.1678 0.114 Uiso 1 1 calc R U . . .
H60C H 0.7758 0.4391 0.1221 0.114 Uiso 1 1 calc R U . . .
C61 C 0.8486(5) 0.5258(3) 0.2025(3) 0.089(2) Uani 1 1 d . . . . .
H61A H 0.8014 0.5580 0.2035 0.134 Uiso 1 1 calc R U . . .
H61B H 0.8751 0.5292 0.1632 0.134 Uiso 1 1 calc R U . . .
H61C H 0.8901 0.5370 0.2350 0.134 Uiso 1 1 calc R U . . .
C62 C 1.0176(4) 0.2885(3) 0.3265(3) 0.0606(16) Uani 1 1 d . . . . .
H62A H 0.9707 0.2873 0.3554 0.073 Uiso 1 1 calc R U . . .
C63 C 1.0889(4) 0.3290(3) 0.3569(3) 0.088(2) Uani 1 1 d . . . . .
H63A H 1.1113 0.3039 0.3924 0.132 Uiso 1 1 calc R U . . .
H63B H 1.0678 0.3736 0.3696 0.132 Uiso 1 1 calc R U . . .
H63C H 1.1337 0.3356 0.3281 0.132 Uiso 1 1 calc R U . . .
C64 C 1.0475(5) 0.2148(3) 0.3182(4) 0.103(3) Uani 1 1 d . . . . .
H64A H 1.0506 0.1917 0.3577 0.155 Uiso 1 1 calc R U . . .
H64B H 1.1033 0.2150 0.3009 0.155 Uiso 1 1 calc R U . . .
H64C H 1.0077 0.1906 0.2908 0.155 Uiso 1 1 calc R U . . .


_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
Ta1 N1 2.027(4) . ?
Ta1 N2 2.031(3) . ?
Ta1 C33 2.187(4) . ?
Ta1 C32 2.201(4) . ?
Ta1 C34 2.608(4) . ?
Ta1 C31 2.617(4) . ?
Ta1 Ta2 2.7121(2) . ?
Ta2 N4 2.031(3) . ?
Ta2 N3 2.033(3) . ?
Ta2 C34 2.186(4) . ?
Ta2 C31 2.198(4) . ?
Ta2 C33 2.613(4) . ?
Ta2 C32 2.627(4) . ?
N1 C1 1.436(5) . ?
N1 C7 1.460(5) . ?
N2 C2 1.425(5) . ?
N2 C19 1.443(5) . ?
N3 C35 1.425(5) . ?
N3 C41 1.447(5) . ?
N4 C36 1.431(5) . ?
N4 C53 1.449(5) . ?
C1 C6 1.371(6) . ?
C1 C2 1.408(6) . ?
C2 C3 1.404(6) . ?
C3 C4 1.388(7) . ?
C4 C5 1.353(8) . ?
C5 C6 1.413(6) . ?
C7 C12 1.409(6) . ?
C7 C8 1.423(6) . ?
C8 C9 1.395(7) . ?
C8 C16 1.509(7) . ?
C9 C10 1.375(8) . ?
C10 C11 1.369(8) . ?
C11 C12 1.397(6) . ?
C12 C13 1.502(7) . ?
C13 C15 1.518(10) . ?
C13 C14 1.529(10) . ?
C13 C15A 1.530(10) . ?
C13 C14A 1.534(10) . ?
C16 C18 1.534(7) . ?
C16 C17 1.559(7) . ?
C19 C20 1.392(6) . ?
C19 C24 1.407(6) . ?
C20 C21 1.396(7) . ?
C20 C28 1.508(6) . ?
C21 C22 1.386(8) . ?
C22 C23 1.352(8) . ?
C23 C24 1.396(7) . ?
C24 C25 1.521(7) . ?
C25 C26 1.533(7) . ?
C25 C27 1.535(6) . ?
C28 C30 1.525(8) . ?
C28 C29 1.558(7) . ?
C35 C40 1.385(5) . ?
C35 C36 1.409(6) . ?
C36 C37 1.377(6) . ?
C37 C38 1.378(6) . ?
C38 C39 1.371(6) . ?
C39 C40 1.395(6) . ?
C41 C46 1.404(6) . ?
C41 C42 1.408(6) . ?
C42 C43 1.391(7) . ?
C42 C50 1.503(7) . ?
C43 C44 1.373(9) . ?
C44 C45 1.374(8) . ?
C45 C46 1.405(6) . ?
C46 C47 1.524(7) . ?
C47 C49 1.519(7) . ?
C47 C48 1.545(7) . ?
C50 C52 1.534(11) . ?
C50 C51 1.552(10) . ?
C50 C52A 1.556(10) . ?
C50 C51A 1.565(10) . ?
C53 C54 1.400(7) . ?
C53 C58 1.403(6) . ?
C54 C55 1.401(7) . ?
C54 C62 1.523(8) . ?
C55 C56 1.347(9) . ?
C56 C57 1.375(8) . ?
C57 C58 1.403(7) . ?
C58 C59 1.518(8) . ?
C59 C60 1.517(7) . ?
C59 C61 1.535(7) . ?
C62 C63 1.516(8) . ?
C62 C64 1.531(8) . ?

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 Ta1 N2 82.11(13) . . ?
N1 Ta1 C33 106.85(15) . . ?
N2 Ta1 C33 109.23(14) . . ?
N1 Ta1 C32 112.97(14) . . ?
N2 Ta1 C32 109.50(14) . . ?
C33 Ta1 C32 127.06(15) . . ?
N1 Ta1 C34 91.16(13) . . ?
N2 Ta1 C34 173.25(14) . . ?
C33 Ta1 C34 73.23(14) . . ?
C32 Ta1 C34 72.54(14) . . ?
N1 Ta1 C31 171.11(13) . . ?
N2 Ta1 C31 89.61(13) . . ?
C33 Ta1 C31 72.80(15) . . ?
C32 Ta1 C31 72.81(15) . . ?
C34 Ta1 C31 97.14(13) . . ?
N1 Ta1 Ta2 139.49(9) . . ?
N2 Ta1 Ta2 138.29(10) . . ?
C33 Ta1 Ta2 63.42(11) . . ?
C32 Ta1 Ta2 63.64(10) . . ?
C34 Ta1 Ta2 48.46(9) . . ?
C31 Ta1 Ta2 48.68(9) . . ?
N4 Ta2 N3 81.94(13) . . ?
N4 Ta2 C34 112.48(15) . . ?
N3 Ta2 C34 108.94(14) . . ?
N4 Ta2 C31 106.89(16) . . ?
N3 Ta2 C31 110.94(14) . . ?
C34 Ta2 C31 126.67(16) . . ?
N4 Ta2 C33 171.59(13) . . ?
N3 Ta2 C33 90.34(12) . . ?
C34 Ta2 C33 73.14(15) . . ?
C31 Ta2 C33 72.71(15) . . ?
N4 Ta2 C32 90.69(13) . . ?
N3 Ta2 C32 172.45(13) . . ?
C34 Ta2 C32 72.38(14) . . ?
C31 Ta2 C32 72.66(15) . . ?
C33 Ta2 C32 97.12(12) . . ?
N4 Ta2 Ta1 139.26(9) . . ?
N3 Ta2 Ta1 138.78(9) . . ?
C34 Ta2 Ta1 63.27(11) . . ?
C31 Ta2 Ta1 63.41(12) . . ?
C33 Ta2 Ta1 48.46(8) . . ?
C32 Ta2 Ta1 48.66(9) . . ?
C1 N1 C7 113.0(3) . . ?
C1 N1 Ta1 113.1(3) . . ?
C7 N1 Ta1 133.9(3) . . ?
C2 N2 C19 113.3(3) . . ?
C2 N2 Ta1 112.1(3) . . ?
C19 N2 Ta1 134.4(3) . . ?
C35 N3 C41 114.3(3) . . ?
C35 N3 Ta2 112.6(2) . . ?
C41 N3 Ta2 133.1(3) . . ?
C36 N4 C53 114.4(3) . . ?
C36 N4 Ta2 112.6(3) . . ?
C53 N4 Ta2 132.9(3) . . ?
C6 C1 C2 120.5(4) . . ?
C6 C1 N1 124.6(4) . . ?
C2 C1 N1 114.9(4) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 N2 123.6(4) . . ?
C1 C2 N2 117.3(4) . . ?
C4 C3 C2 119.4(5) . . ?
C5 C4 C3 121.1(5) . . ?
C4 C5 C6 120.5(5) . . ?
C1 C6 C5 119.3(5) . . ?
C12 C7 C8 120.9(4) . . ?
C12 C7 N1 119.3(4) . . ?
C8 C7 N1 119.8(4) . . ?
C9 C8 C7 118.0(5) . . ?
C9 C8 C16 120.8(5) . . ?
C7 C8 C16 121.1(5) . . ?
C10 C9 C8 120.9(5) . . ?
C11 C10 C9 120.8(5) . . ?
C10 C11 C12 121.4(5) . . ?
C11 C12 C7 117.9(5) . . ?
C11 C12 C13 118.7(5) . . ?
C7 C12 C13 123.4(4) . . ?
C12 C13 C15 112.4(7) . . ?
C12 C13 C14 111.9(7) . . ?
C15 C13 C14 98.1(7) . . ?
C12 C13 C15A 112.1(7) . . ?
C12 C13 C14A 111.3(7) . . ?
C15A C13 C14A 121.7(8) . . ?
C8 C16 C18 112.4(5) . . ?
C8 C16 C17 111.3(4) . . ?
C18 C16 C17 108.9(5) . . ?
C20 C19 C24 121.0(4) . . ?
C20 C19 N2 120.7(4) . . ?
C24 C19 N2 118.3(4) . . ?
C19 C20 C21 119.3(5) . . ?
C19 C20 C28 123.0(4) . . ?
C21 C20 C28 117.7(5) . . ?
C22 C21 C20 119.4(5) . . ?
C23 C22 C21 121.2(5) . . ?
C22 C23 C24 121.5(5) . . ?
C23 C24 C19 117.7(5) . . ?
C23 C24 C25 120.0(4) . . ?
C19 C24 C25 122.3(4) . . ?
C24 C25 C26 111.4(4) . . ?
C24 C25 C27 112.5(5) . . ?
C26 C25 C27 109.3(4) . . ?
C20 C28 C30 112.8(5) . . ?
C20 C28 C29 110.6(4) . . ?
C30 C28 C29 110.9(5) . . ?
Ta2 C31 Ta1 67.91(12) . . ?
Ta1 C32 Ta2 67.70(10) . . ?
Ta1 C33 Ta2 68.13(11) . . ?
Ta2 C34 Ta1 68.26(11) . . ?
C40 C35 C36 119.3(4) . . ?
C40 C35 N3 124.4(4) . . ?
C36 C35 N3 116.3(4) . . ?
C37 C36 C35 119.4(4) . . ?
C37 C36 N4 124.8(4) . . ?
C35 C36 N4 115.8(4) . . ?
C36 C37 C38 120.7(4) . . ?
C39 C38 C37 120.6(4) . . ?
C38 C39 C40 119.6(4) . . ?
C35 C40 C39 120.3(4) . . ?
C46 C41 C42 121.5(4) . . ?
C46 C41 N3 119.2(4) . . ?
C42 C41 N3 119.2(4) . . ?
C43 C42 C41 117.6(5) . . ?
C43 C42 C50 119.7(5) . . ?
C41 C42 C50 122.7(4) . . ?
C44 C43 C42 121.8(5) . . ?
C43 C44 C45 120.2(5) . . ?
C44 C45 C46 121.0(6) . . ?
C41 C46 C45 117.9(5) . . ?
C41 C46 C47 123.0(4) . . ?
C45 C46 C47 119.1(5) . . ?
C49 C47 C46 111.1(4) . . ?
C49 C47 C48 111.2(4) . . ?
C46 C47 C48 110.8(5) . . ?
C42 C50 C52 110.8(8) . . ?
C42 C50 C51 119.5(8) . . ?
C52 C50 C51 116.2(8) . . ?
C42 C50 C52A 111.9(7) . . ?
C42 C50 C51A 105.4(7) . . ?
C52A C50 C51A 102.0(7) . . ?
C54 C53 C58 121.4(4) . . ?
C54 C53 N4 119.2(4) . . ?
C58 C53 N4 119.4(4) . . ?
C53 C54 C55 117.7(5) . . ?
C53 C54 C62 123.1(4) . . ?
C55 C54 C62 119.2(5) . . ?
C56 C55 C54 121.6(6) . . ?
C55 C56 C57 120.8(5) . . ?
C56 C57 C58 120.7(6) . . ?
C53 C58 C57 117.7(5) . . ?
C53 C58 C59 123.6(4) . . ?
C57 C58 C59 118.7(5) . . ?
C60 C59 C58 112.2(5) . . ?
C60 C59 C61 109.7(5) . . ?
C58 C59 C61 111.6(5) . . ?
C63 C62 C54 112.2(5) . . ?
C63 C62 C64 108.3(5) . . ?
C54 C62 C64 114.5(6) . . ?

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.118

# SQUEEZE RESULTS (Version =  11015)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 666 149 ' '
2 0.000 0.500 1.000 666 149 ' '
3 0.382 0.077 0.881 8 0 ' '
4 0.382 0.423 0.381 8 0 ' '
5 0.618 0.577 0.619 8 0 ' '
6 0.618 0.923 0.119 8 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K2L
_database_code_depnum_ccdc_archive 'CCDC 1479775'
_audit_update_record             
;
2016-05-13 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H78 K2 N2 O8'
_chemical_formula_weight         865.30

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.8034(7)
_cell_length_b                   27.6688(19)
_cell_length_c                   17.1421(12)
_cell_angle_alpha                90
_cell_angle_beta                 98.503(2)
_cell_angle_gamma                90
_cell_volume                     5067.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    149(2)
_cell_measurement_reflns_used    33778
_cell_measurement_theta_min      1.472
_cell_measurement_theta_max      24.997

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.235
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   Apex2

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      149(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33778
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.472
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             8874
_reflns_number_gt                6787
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0879P)²+3.3924P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8874
_refine_ls_number_parameters     552
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1597
_refine_ls_wR_factor_gt          0.1423
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.24195(5) 0.13870(2) 0.13651(3) 0.03007(16) Uani 1 1 d . . . . .
K2 K 0.26400(5) 0.10924(2) 0.46401(3) 0.03028(16) Uani 1 1 d . . . . .
O1 O 0.03981(17) 0.10471(7) 0.36553(11) 0.0388(5) Uani 1 1 d . . . . .
O2 O 0.03787(19) 0.14080(7) 0.51893(12) 0.0436(5) Uani 1 1 d . . . . .
O3 O 0.3488(2) 0.13703(8) 0.62353(13) 0.0518(6) Uani 1 1 d . . . . .
O4 O 0.2652(2) 0.04512(7) 0.58051(13) 0.0504(5) Uani 1 1 d . . . . .
O5 O 0.1096(2) 0.05892(9) 0.04220(13) 0.0573(6) Uani 1 1 d . . . . .
O6 O -0.00955(18) 0.14488(7) 0.07102(12) 0.0440(5) Uani 1 1 d . . . . .
O7 O 0.2978(2) 0.16613(9) -0.01650(14) 0.0601(6) Uani 1 1 d . . . . .
O8 O 0.1877(2) 0.23514(8) 0.08385(15) 0.0654(7) Uani 1 1 d . . . . .
N1 N 0.35790(18) 0.16926(7) 0.27962(12) 0.0250(4) Uani 1 1 d . . . . .
N2 N 0.34386(17) 0.07186(7) 0.24284(11) 0.0214(4) Uani 1 1 d . . . . .
C1 C 0.4166(2) 0.13706(8) 0.33281(13) 0.0204(5) Uani 1 1 d . . . . .
C2 C 0.4047(2) 0.08548(8) 0.31476(12) 0.0194(5) Uani 1 1 d . . . . .
C3 C 0.4592(2) 0.05288(9) 0.37336(14) 0.0253(5) Uani 1 1 d . . . . .
H3A H 0.4465 0.0175 0.3636 0.030 Uiso 1 1 calc R U . . .
C4 C 0.5311(2) 0.06770(9) 0.44473(14) 0.0294(6) Uani 1 1 d . . . . .
H4A H 0.5726 0.0432 0.4828 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5493(2) 0.11610(10) 0.45921(14) 0.0307(6) Uani 1 1 d . . . . .
H5A H 0.6073 0.1272 0.5068 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4915(2) 0.15014(9) 0.40402(14) 0.0272(5) Uani 1 1 d . . . . .
H6A H 0.5114 0.1851 0.4136 0.033 Uiso 1 1 calc R U . . .
C7 C 0.3886(2) 0.21780(9) 0.29258(14) 0.0252(5) Uani 1 1 d . . . . .
C8 C 0.4978(2) 0.23725(9) 0.26747(15) 0.0299(6) Uani 1 1 d . . . . .
C9 C 0.5217(2) 0.28656(10) 0.27404(16) 0.0351(6) Uani 1 1 d . . . . .
H9A H 0.5945 0.2993 0.2566 0.042 Uiso 1 1 calc R U . . .
C10 C 0.4411(3) 0.31764(10) 0.30562(17) 0.0380(7) Uani 1 1 d . . . . .
H10A H 0.4583 0.3513 0.3095 0.046 Uiso 1 1 calc R U . . .
C11 C 0.3362(3) 0.29900(9) 0.33128(16) 0.0351(6) Uani 1 1 d . . . . .
H11A H 0.2811 0.3202 0.3530 0.042 Uiso 1 1 calc R U . . .
C12 C 0.3087(2) 0.24987(9) 0.32617(14) 0.0276(5) Uani 1 1 d . . . . .
C13 C 0.1931(2) 0.23061(10) 0.35635(15) 0.0316(6) Uani 1 1 d . . . . .
H13A H 0.1913 0.1948 0.3484 0.038 Uiso 1 1 calc R U . . .
C14 C 0.1963(3) 0.24005(12) 0.44424(18) 0.0489(8) Uani 1 1 d . . . . .
H14A H 0.2753 0.2280 0.4732 0.073 Uiso 1 1 calc R U . . .
H14B H 0.1261 0.2234 0.4627 0.073 Uiso 1 1 calc R U . . .
H14C H 0.1897 0.2749 0.4533 0.073 Uiso 1 1 calc R U . . .
C15 C 0.0738(3) 0.25127(12) 0.3094(2) 0.0476(8) Uani 1 1 d . . . . .
H15A H 0.0703 0.2428 0.2536 0.071 Uiso 1 1 calc R U . . .
H15B H 0.0737 0.2865 0.3151 0.071 Uiso 1 1 calc R U . . .
H15C H 0.0008 0.2377 0.3294 0.071 Uiso 1 1 calc R U . . .
C16 C 0.5854(2) 0.20430(10) 0.23099(17) 0.0357(6) Uani 1 1 d . . . . .
H16A H 0.5619 0.1703 0.2423 0.043 Uiso 1 1 calc R U . . .
C17 C 0.5694(3) 0.20970(13) 0.14207(18) 0.0504(8) Uani 1 1 d . . . . .
H17A H 0.4809 0.2059 0.1202 0.076 Uiso 1 1 calc R U . . .
H17B H 0.6188 0.1849 0.1199 0.076 Uiso 1 1 calc R U . . .
H17C H 0.5983 0.2418 0.1286 0.076 Uiso 1 1 calc R U . . .
C18 C 0.7219(3) 0.21094(15) 0.2670(2) 0.0605(10) Uani 1 1 d . . . . .
H18A H 0.7305 0.2064 0.3243 0.091 Uiso 1 1 calc R U . . .
H18B H 0.7494 0.2436 0.2555 0.091 Uiso 1 1 calc R U . . .
H18C H 0.7736 0.1871 0.2445 0.091 Uiso 1 1 calc R U . . .
C19 C 0.3651(2) 0.02500(8) 0.21751(13) 0.0221(5) Uani 1 1 d . . . . .
C20 C 0.4644(2) 0.01701(9) 0.17287(14) 0.0263(5) Uani 1 1 d D . . . .
C21 C 0.4795(2) -0.02836(10) 0.14056(15) 0.0328(6) Uani 1 1 d . . . . .
H21A H 0.5465 -0.0335 0.1114 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3994(3) -0.06615(10) 0.14987(16) 0.0361(6) Uani 1 1 d . . . . .
H22A H 0.4098 -0.0966 0.1261 0.043 Uiso 1 1 calc R U . . .
C23 C 0.3039(3) -0.05902(9) 0.19423(15) 0.0335(6) Uani 1 1 d . . . . .
H23A H 0.2492 -0.0850 0.2013 0.040 Uiso 1 1 calc R U . . .
C24 C 0.2864(2) -0.01443(9) 0.22870(14) 0.0266(5) Uani 1 1 d . . . . .
C25 C 0.1820(2) -0.00820(10) 0.27820(15) 0.0325(6) Uani 1 1 d . . . . .
H25A H 0.1893 0.0251 0.3011 0.039 Uiso 1 1 calc R U . . .
C26 C 0.1944(3) -0.04421(13) 0.34715(19) 0.0532(8) Uani 1 1 d . . . . .
H26A H 0.2773 -0.0409 0.3788 0.080 Uiso 1 1 calc R U . . .
H26B H 0.1842 -0.0772 0.3265 0.080 Uiso 1 1 calc R U . . .
H26C H 0.1297 -0.0375 0.3802 0.080 Uiso 1 1 calc R U . . .
C27 C 0.0537(3) -0.01224(12) 0.22767(18) 0.0454(7) Uani 1 1 d . . . . .
H27A H 0.0484 0.0107 0.1837 0.068 Uiso 1 1 calc R U . . .
H27B H -0.0116 -0.0048 0.2599 0.068 Uiso 1 1 calc R U . . .
H27C H 0.0418 -0.0452 0.2069 0.068 Uiso 1 1 calc R U . . .
C28 C 0.5450(8) 0.0594(3) 0.1550(5) 0.030(2) Uani 0.7 1 d D . P A 1
H28A H 0.4938 0.0895 0.1544 0.036 Uiso 0.7 1 calc R U P A 1
C28A C 0.5635(18) 0.0571(7) 0.1663(11) 0.019(5) Uiso 0.3 1 d D . P A 2
H28B H 0.5380 0.0857 0.1959 0.023 Uiso 0.3 1 calc R U P A 2
C29 C 0.6607(4) 0.06442(16) 0.2213(2) 0.0325(9) Uani 0.7 1 d D . P A 1
H29A H 0.6317 0.0679 0.2726 0.049 Uiso 0.7 1 calc R U P A 1
H29B H 0.7093 0.0930 0.2111 0.049 Uiso 0.7 1 calc R U P A 1
H29C H 0.7133 0.0356 0.2218 0.049 Uiso 0.7 1 calc R U P A 1
C29A C 0.6902(14) 0.0476(5) 0.1967(9) 0.063(3) Uiso 0.3 1 d . . P A 2
H29D H 0.6983 0.0425 0.2538 0.095 Uiso 0.3 1 calc R U P A 2
H29E H 0.7419 0.0752 0.1858 0.095 Uiso 0.3 1 calc R U P A 2
H29F H 0.7182 0.0186 0.1715 0.095 Uiso 0.3 1 calc R U P A 2
C30 C 0.5938(5) 0.0555(2) 0.0764(3) 0.0528(14) Uani 0.7 1 d . . P A 1
H30A H 0.5242 0.0482 0.0346 0.079 Uiso 0.7 1 calc R U P A 1
H30B H 0.6562 0.0296 0.0793 0.079 Uiso 0.7 1 calc R U P A 1
H30C H 0.6325 0.0862 0.0647 0.079 Uiso 0.7 1 calc R U P A 1
C30A C 0.5508(16) 0.0728(6) 0.0773(9) 0.063(3) Uiso 0.3 1 d D . P A 2
H30D H 0.4658 0.0847 0.0597 0.095 Uiso 0.3 1 calc R U P A 2
H30E H 0.5675 0.0450 0.0450 0.095 Uiso 0.3 1 calc R U P A 2
H30F H 0.6113 0.0985 0.0716 0.095 Uiso 0.3 1 calc R U P A 2
C31 C 0.0369(3) 0.11191(11) 0.28288(16) 0.0398(7) Uani 1 1 d . . . . .
H31A H -0.0313 0.0928 0.2539 0.060 Uiso 1 1 calc R U . . .
H31B H 0.1167 0.1016 0.2676 0.060 Uiso 1 1 calc R U . . .
H31C H 0.0231 0.1462 0.2704 0.060 Uiso 1 1 calc R U . . .
C32 C -0.0703(3) 0.12200(12) 0.39196(18) 0.0433(7) Uani 1 1 d . . . . .
H32A H -0.1443 0.1049 0.3638 0.052 Uiso 1 1 calc R U . . .
H32B H -0.0804 0.1570 0.3804 0.052 Uiso 1 1 calc R U . . .
C33 C -0.0618(3) 0.11376(12) 0.47855(19) 0.0466(8) Uani 1 1 d . . . . .
H33A H -0.1412 0.1236 0.4964 0.056 Uiso 1 1 calc R U . . .
H33B H -0.0483 0.0790 0.4903 0.056 Uiso 1 1 calc R U . . .
C34 C 0.0435(3) 0.13752(13) 0.60193(18) 0.0495(8) Uani 1 1 d . . . . .
H34A H -0.0356 0.1489 0.6169 0.074 Uiso 1 1 calc R U . . .
H34B H 0.1124 0.1576 0.6277 0.074 Uiso 1 1 calc R U . . .
H34C H 0.0575 0.1038 0.6185 0.074 Uiso 1 1 calc R U . . .
C35 C 0.4168(4) 0.18042(16) 0.6335(3) 0.0853(14) Uani 1 1 d . . . . .
H35A H 0.4561 0.1834 0.6886 0.128 Uiso 1 1 calc R U . . .
H35B H 0.3602 0.2078 0.6198 0.128 Uiso 1 1 calc R U . . .
H35C H 0.4817 0.1804 0.5992 0.128 Uiso 1 1 calc R U . . .
C36 C 0.4165(3) 0.09610(15) 0.6529(2) 0.0610(10) Uani 1 1 d . . . . .
H36A H 0.4621 0.1031 0.7062 0.073 Uiso 1 1 calc R U . . .
H36B H 0.4787 0.0878 0.6181 0.073 Uiso 1 1 calc R U . . .
C37 C 0.3299(3) 0.05470(14) 0.65702(18) 0.0559(9) Uani 1 1 d . . . . .
H37A H 0.3779 0.0258 0.6776 0.067 Uiso 1 1 calc R U . . .
H37B H 0.2693 0.0625 0.6932 0.067 Uiso 1 1 calc R U . . .
C38 C 0.1901(4) 0.00329(12) 0.5776(2) 0.0639(10) Uani 1 1 d . . . . .
H38A H 0.2433 -0.0250 0.5919 0.096 Uiso 1 1 calc R U . . .
H38B H 0.1450 -0.0009 0.5240 0.096 Uiso 1 1 calc R U . . .
H38C H 0.1299 0.0066 0.6147 0.096 Uiso 1 1 calc R U . . .
C39 C 0.1941(3) 0.02905(13) 0.0109(2) 0.0571(9) Uani 1 1 d . . . . .
H39A H 0.1481 0.0068 -0.0273 0.086 Uiso 1 1 calc R U . . .
H39B H 0.2427 0.0105 0.0536 0.086 Uiso 1 1 calc R U . . .
H39C H 0.2508 0.0489 -0.0153 0.086 Uiso 1 1 calc R U . . .
C40 C 0.0224(3) 0.08081(14) -0.0156(2) 0.0605(9) Uani 1 1 d . . . . .
H40A H -0.0209 0.0558 -0.0508 0.073 Uiso 1 1 calc R U . . .
H40B H 0.0661 0.1029 -0.0479 0.073 Uiso 1 1 calc R U . . .
C41 C -0.0715(3) 0.10864(14) 0.0227(2) 0.0601(9) Uani 1 1 d . . . . .
H41A H -0.1343 0.1235 -0.0183 0.072 Uiso 1 1 calc R U . . .
H41B H -0.1157 0.0866 0.0547 0.072 Uiso 1 1 calc R U . . .
C42 C -0.0950(4) 0.17637(17) 0.0999(3) 0.0818(14) Uani 1 1 d . . . . .
H42A H -0.1526 0.1897 0.0556 0.123 Uiso 1 1 calc R U . . .
H42B H -0.0491 0.2028 0.1293 0.123 Uiso 1 1 calc R U . . .
H42C H -0.1426 0.1585 0.1349 0.123 Uiso 1 1 calc R U . . .
C43 C 0.3905(5) 0.1486(2) -0.0553(3) 0.1121(19) Uani 1 1 d . . . . .
H43A H 0.3549 0.1399 -0.1094 0.168 Uiso 1 1 calc R U . . .
H43B H 0.4281 0.1200 -0.0278 0.168 Uiso 1 1 calc R U . . .
H43C H 0.4548 0.1735 -0.0565 0.168 Uiso 1 1 calc R U . . .
C44 C 0.2630(4) 0.21365(17) -0.0411(2) 0.0778(12) Uani 1 1 d . . . . .
H44A H 0.2370 0.2141 -0.0989 0.093 Uiso 1 1 calc R U . . .
H44B H 0.3357 0.2355 -0.0283 0.093 Uiso 1 1 calc R U . . .
C45 C 0.1571(5) 0.23120(16) -0.0008(3) 0.0841(14) Uani 1 1 d . . . . .
H45A H 0.1300 0.2633 -0.0225 0.101 Uiso 1 1 calc R U . . .
H45B H 0.0856 0.2088 -0.0133 0.101 Uiso 1 1 calc R U . . .
C46 C 0.2539(3) 0.27664(12) 0.1085(2) 0.0583(9) Uani 1 1 d . . . . .
H46A H 0.2056 0.3051 0.0882 0.087 Uiso 1 1 calc R U . . .
H46B H 0.3344 0.2764 0.0885 0.087 Uiso 1 1 calc R U . . .
H46C H 0.2687 0.2777 0.1663 0.087 Uiso 1 1 calc R U . . .


_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
K1 N2 2.7133(19) . ?
K1 N1 2.719(2) . ?
K1 O6 2.787(2) . ?
K1 O8 2.850(2) . ?
K1 O7 2.879(2) . ?
K1 O5 2.974(2) . ?
K1 C45 3.506(4) . ?
K2 O4 2.670(2) . ?
K2 O1 2.7428(19) . ?
K2 O3 2.858(2) . ?
K2 O2 2.880(2) . ?
K2 C6 3.021(2) . ?
K2 C1 3.077(2) . ?
K2 C5 3.101(3) . ?
K2 C4 3.168(3) . ?
K2 C3 3.203(2) . ?
K2 C2 3.231(2) . ?
K2 C36 3.429(3) . ?
O1 C32 1.418(3) . ?
O1 C31 1.426(3) . ?
O2 C33 1.407(4) . ?
O2 C34 1.418(4) . ?
O3 C36 1.401(4) . ?
O3 C35 1.405(4) . ?
O4 C38 1.410(4) . ?
O4 C37 1.417(4) . ?
O5 C39 1.396(4) . ?
O5 C40 1.400(4) . ?
O6 C41 1.406(4) . ?
O6 C42 1.411(4) . ?
O7 C43 1.370(5) . ?
O7 C44 1.415(5) . ?
O8 C46 1.386(4) . ?
O8 C45 1.443(5) . ?
N1 C1 1.363(3) . ?
N1 C7 1.393(3) . ?
N2 C2 1.362(3) . ?
N2 C19 1.397(3) . ?
C1 C6 1.408(3) . ?
C1 C2 1.462(3) . ?
C2 C3 1.412(3) . ?
C3 C4 1.410(3) . ?
C4 C5 1.371(4) . ?
C5 C6 1.413(4) . ?
C7 C12 1.418(3) . ?
C7 C8 1.421(3) . ?
C8 C9 1.390(4) . ?
C8 C16 1.514(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.375(4) . ?
C11 C12 1.391(4) . ?
C12 C13 1.517(4) . ?
C13 C14 1.525(4) . ?
C13 C15 1.526(4) . ?
C16 C17 1.516(4) . ?
C16 C18 1.523(4) . ?
C19 C24 1.414(3) . ?
C19 C20 1.424(3) . ?
C20 C21 1.391(4) . ?
C20 C28 1.518(7) . ?
C20 C28A 1.557(15) . ?
C21 C22 1.381(4) . ?
C22 C23 1.383(4) . ?
C23 C24 1.393(4) . ?
C24 C25 1.518(3) . ?
C25 C27 1.527(4) . ?
C25 C26 1.536(4) . ?
C28 C30 1.522(9) . ?
C28 C29 1.567(9) . ?
C28A C29A 1.41(2) . ?
C28A C30A 1.573(18) . ?
C32 C33 1.491(4) . ?
C36 C37 1.487(5) . ?
C40 C41 1.500(5) . ?
C44 C45 1.501(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 K1 N1 61.24(6) . . ?
N2 K1 O6 125.94(6) . . ?
N1 K1 O6 129.48(6) . . ?
N2 K1 O8 153.51(7) . . ?
N1 K1 O8 92.31(7) . . ?
O6 K1 O8 70.88(7) . . ?
N2 K1 O7 132.29(7) . . ?
N1 K1 O7 127.54(7) . . ?
O6 K1 O7 86.57(7) . . ?
O8 K1 O7 61.68(8) . . ?
N2 K1 O5 88.51(6) . . ?
N1 K1 O5 147.29(7) . . ?
O6 K1 O5 57.65(6) . . ?
O8 K1 O5 117.57(7) . . ?
O7 K1 O5 81.32(7) . . ?
N2 K1 C45 171.27(9) . . ?
N1 K1 C45 114.73(9) . . ?
O6 K1 C45 62.77(9) . . ?
O8 K1 C45 23.47(9) . . ?
O7 K1 C45 42.71(10) . . ?
O5 K1 C45 96.89(9) . . ?
O4 K2 O1 109.64(7) . . ?
O4 K2 O3 59.84(7) . . ?
O1 K2 O3 136.90(6) . . ?
O4 K2 O2 82.38(6) . . ?
O1 K2 O2 60.04(6) . . ?
O3 K2 O2 76.88(6) . . ?
O4 K2 C6 126.11(7) . . ?
O1 K2 C6 119.76(6) . . ?
O3 K2 C6 93.63(7) . . ?
O2 K2 C6 140.33(7) . . ?
O4 K2 C1 140.28(7) . . ?
O1 K2 C1 94.67(6) . . ?
O3 K2 C1 120.11(6) . . ?
O2 K2 C1 137.32(6) . . ?
C6 K2 C1 26.69(6) . . ?
O4 K2 C5 99.54(7) . . ?
O1 K2 C5 141.00(6) . . ?
O3 K2 C5 80.20(7) . . ?
O2 K2 C5 152.18(7) . . ?
C6 K2 C5 26.65(7) . . ?
C1 K2 C5 47.40(6) . . ?
O4 K2 C4 86.18(7) . . ?
O1 K2 C4 130.86(6) . . ?
O3 K2 C4 91.69(6) . . ?
O2 K2 C4 166.80(6) . . ?
C6 K2 C4 45.66(7) . . ?
C1 K2 C4 54.53(6) . . ?
C5 K2 C4 25.23(7) . . ?
O4 K2 C3 96.24(6) . . ?
O1 K2 C3 105.30(6) . . ?
O3 K2 C3 117.03(6) . . ?
O2 K2 C3 163.14(6) . . ?
C6 K2 C3 52.43(7) . . ?
C1 K2 C3 45.96(6) . . ?
C5 K2 C3 44.67(6) . . ?
C4 K2 C3 25.56(6) . . ?
O4 K2 C2 120.42(6) . . ?
O1 K2 C2 88.81(6) . . ?
O3 K2 C2 133.69(6) . . ?
O2 K2 C2 147.30(6) . . ?
C6 K2 C2 45.97(6) . . ?
C1 K2 C2 26.66(6) . . ?
C5 K2 C2 53.54(6) . . ?
C4 K2 C2 45.67(6) . . ?
C3 K2 C2 25.35(6) . . ?
O4 K2 C36 43.50(8) . . ?
O1 K2 C36 146.49(8) . . ?
O3 K2 C36 23.58(8) . . ?
O2 K2 C36 92.05(8) . . ?
C6 K2 C36 93.43(8) . . ?
C1 K2 C36 118.84(8) . . ?
C5 K2 C36 72.00(8) . . ?
C4 K2 C36 75.06(8) . . ?
C3 K2 C36 98.50(8) . . ?
C2 K2 C36 120.65(7) . . ?
C32 O1 C31 112.0(2) . . ?
C32 O1 K2 119.63(16) . . ?
C31 O1 K2 119.54(15) . . ?
C33 O2 C34 112.1(2) . . ?
C33 O2 K2 107.63(16) . . ?
C34 O2 K2 113.34(17) . . ?
C36 O3 C35 114.2(3) . . ?
C36 O3 K2 101.73(18) . . ?
C35 O3 K2 115.8(2) . . ?
C38 O4 C37 112.9(3) . . ?
C38 O4 K2 125.4(2) . . ?
C37 O4 K2 121.02(19) . . ?
C39 O5 C40 113.2(3) . . ?
C39 O5 K1 111.03(19) . . ?
C40 O5 K1 106.4(2) . . ?
C41 O6 C42 111.6(3) . . ?
C41 O6 K1 123.00(18) . . ?
C42 O6 K1 123.1(2) . . ?
C43 O7 C44 111.4(3) . . ?
C43 O7 K1 128.0(3) . . ?
C44 O7 K1 115.7(2) . . ?
C46 O8 C45 113.6(3) . . ?
C46 O8 K1 127.34(19) . . ?
C45 O8 K1 104.7(2) . . ?
C1 N1 C7 116.58(19) . . ?
C1 N1 K1 120.48(14) . . ?
C7 N1 K1 120.70(14) . . ?
C2 N2 C19 117.31(19) . . ?
C2 N2 K1 120.87(14) . . ?
C19 N2 K1 119.52(13) . . ?
N1 C1 C6 124.3(2) . . ?
N1 C1 C2 118.6(2) . . ?
C6 C1 C2 117.1(2) . . ?
N1 C1 K2 113.94(14) . . ?
C6 C1 K2 74.45(13) . . ?
C2 C1 K2 82.55(12) . . ?
N2 C2 C3 124.2(2) . . ?
N2 C2 C1 118.5(2) . . ?
C3 C2 C1 117.3(2) . . ?
N2 C2 K2 123.56(14) . . ?
C3 C2 K2 76.23(13) . . ?
C1 C2 K2 70.79(11) . . ?
C4 C3 C2 123.4(2) . . ?
C4 C3 K2 75.84(14) . . ?
C2 C3 K2 78.42(13) . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 K2 74.65(15) . . ?
C3 C4 K2 78.60(14) . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 K2 80.12(15) . . ?
C6 C5 K2 73.51(14) . . ?
C1 C6 C5 123.3(2) . . ?
C1 C6 K2 78.86(13) . . ?
C5 C6 K2 79.84(14) . . ?
N1 C7 C12 121.6(2) . . ?
N1 C7 C8 120.4(2) . . ?
C12 C7 C8 118.0(2) . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 C16 120.3(2) . . ?
C7 C8 C16 119.7(2) . . ?
C10 C9 C8 121.3(2) . . ?
C11 C10 C9 119.1(2) . . ?
C10 C11 C12 121.7(3) . . ?
C11 C12 C7 120.0(2) . . ?
C11 C12 C13 120.1(2) . . ?
C7 C12 C13 120.0(2) . . ?
C12 C13 C14 112.1(2) . . ?
C12 C13 C15 111.2(2) . . ?
C14 C13 C15 110.6(3) . . ?
C8 C16 C17 111.8(2) . . ?
C8 C16 C18 112.7(2) . . ?
C17 C16 C18 110.8(3) . . ?
N2 C19 C24 123.0(2) . . ?
N2 C19 C20 118.8(2) . . ?
C24 C19 C20 118.0(2) . . ?
C21 C20 C19 119.7(2) . . ?
C21 C20 C28 120.8(4) . . ?
C19 C20 C28 119.3(4) . . ?
C21 C20 C28A 119.4(8) . . ?
C19 C20 C28A 120.6(8) . . ?
C22 C21 C20 121.7(2) . . ?
C21 C22 C23 119.1(2) . . ?
C22 C23 C24 121.2(2) . . ?
C23 C24 C19 120.3(2) . . ?
C23 C24 C25 119.8(2) . . ?
C19 C24 C25 120.0(2) . . ?
C24 C25 C27 111.2(2) . . ?
C24 C25 C26 111.7(2) . . ?
C27 C25 C26 110.9(2) . . ?
C20 C28 C30 114.1(6) . . ?
C20 C28 C29 110.0(6) . . ?
C30 C28 C29 107.8(6) . . ?
C29A C28A C20 118.7(14) . . ?
C29A C28A C30A 110.4(14) . . ?
C20 C28A C30A 107.8(12) . . ?
O1 C32 C33 109.6(2) . . ?
O2 C33 C32 109.8(2) . . ?
O3 C36 C37 109.9(3) . . ?
O3 C36 K2 54.69(14) . . ?
C37 C36 K2 84.73(18) . . ?
O4 C37 C36 109.2(3) . . ?
O5 C40 C41 109.9(3) . . ?
O6 C41 C40 109.3(3) . . ?
O7 C44 C45 110.6(3) . . ?
O8 C45 C44 114.2(3) . . ?
O8 C45 K1 51.85(16) . . ?
C44 C45 K1 86.1(2) . . ?

_refine_diff_density_max         0.793
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-4

