#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:47:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178824 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/78/4107863.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4107863
loop_
_publ_author_name
'Alfred J. Wooten'
'Patrick J. Carroll'
'Patrick J. Walsh'
_publ_section_title
;
 Insight into Substrate Binding in Shibasaki's Li3(THF)n(BINOLate)3Ln
 Complexes and Implications in Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7407
_journal_page_last               7419
_journal_paper_doi               10.1021/ja7107933
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C72 H72 Li3 Lu N6 O6'
_chemical_formula_weight         1313.15
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.987(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.4512(11)
_cell_length_b                   15.2859(7)
_cell_length_c                   22.0196(11)
_cell_measurement_temperature    143(1)
_cell_volume                     6375.9(5)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26789
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7145
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.581
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         13537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0161P)²+0.1844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                11931
_reflns_number_total             13537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7107933-file002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'C 2 '
_cod_database_code               4107863
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Lu1 Lu 0.5000 0.399891(13) 1.0000 0.03283(8) Uani 1 2 d S
Li1 Li 0.6449(5) 0.4907(6) 1.0817(5) 0.058(2) Uani 1 1 d .
Li2 Li 0.5000 0.1988(11) 1.0000 0.045(4) Uani 1 2 d S
C1 C 0.6076(3) 0.2983(3) 0.9743(2) 0.0327(10) Uani 1 1 d .
C2 C 0.6134(3) 0.3194(3) 0.9142(2) 0.0400(11) Uani 1 1 d .
H2A H 0.5727 0.3238 0.8722 0.053 Uiso 1 1 calc R
C3 C 0.6773(3) 0.3332(4) 0.9175(3) 0.0440(13) Uani 1 1 d .
H3A H 0.6800 0.3442 0.8772 0.059 Uiso 1 1 calc R
C4 C 0.7413(4) 0.3311(5) 0.9824(3) 0.0425(16) Uani 1 1 d .
C5 C 0.8059(4) 0.3498(5) 0.9856(4) 0.0545(18) Uani 1 1 d .
H5 H 0.8085 0.3638 0.9457 0.073 Uiso 1 1 calc R
C6 C 0.8665(3) 0.3476(4) 1.0481(3) 0.0543(13) Uani 1 1 d .
H6 H 0.9100 0.3609 1.0507 0.072 Uiso 1 1 calc R
C7 C 0.8617(3) 0.3252(3) 1.1074(3) 0.0483(12) Uani 1 1 d .
H7 H 0.9025 0.3243 1.1496 0.064 Uiso 1 1 calc R
C8 C 0.7990(3) 0.3048(3) 1.1047(2) 0.0404(11) Uani 1 1 d .
H8 H 0.7975 0.2895 1.1449 0.054 Uiso 1 1 calc R
C9 C 0.7349(2) 0.3065(3) 1.0408(2) 0.0312(10) Uani 1 1 d .
C10 C 0.6678(3) 0.2892(3) 1.0370(2) 0.0293(10) Uani 1 1 d .
C11 C 0.6616(2) 0.2609(3) 1.0989(2) 0.0329(9) Uani 1 1 d .
C12 C 0.6902(2) 0.1790(3) 1.1311(2) 0.0394(11) Uani 1 1 d .
C13 C 0.7227(3) 0.1201(3) 1.1047(2) 0.0491(12) Uani 1 1 d .
H13 H 0.7251 0.1354 1.0649 0.065 Uiso 1 1 calc R
C14 C 0.7504(3) 0.0424(4) 1.1351(3) 0.0669(17) Uani 1 1 d .
H14 H 0.7714 0.0057 1.1163 0.089 Uiso 1 1 calc R
C15 C 0.7473(4) 0.0175(5) 1.1944(4) 0.084(2) Uani 1 1 d .
H15 H 0.7667 -0.0355 1.2155 0.112 Uiso 1 1 calc R
C16 C 0.7163(3) 0.0700(5) 1.2210(3) 0.0754(19) Uani 1 1 d .
H16 H 0.7136 0.0519 1.2601 0.100 Uiso 1 1 calc R
C17 C 0.6872(3) 0.1527(4) 1.1913(2) 0.0564(15) Uani 1 1 d .
C18 C 0.6545(3) 0.2093(4) 1.2180(2) 0.0665(17) Uani 1 1 d .
H18 H 0.6528 0.1937 1.2581 0.088 Uiso 1 1 calc R
C19 C 0.6252(3) 0.2862(4) 1.1868(2) 0.0557(14) Uani 1 1 d .
H19 H 0.6029 0.3215 1.2052 0.074 Uiso 1 1 calc R
C20 C 0.6283(2) 0.3140(3) 1.1259(2) 0.0362(10) Uani 1 1 d .
C21 C 0.4625(2) 0.5760(3) 1.0468(2) 0.0354(10) Uani 1 1 d .
C22 C 0.4539(3) 0.5795(3) 1.1074(2) 0.0462(12) Uani 1 1 d .
H22 H 0.4289 0.5355 1.1156 0.062 Uiso 1 1 calc R
C23 C 0.4817(3) 0.6458(4) 1.1530(2) 0.0516(14) Uani 1 1 d .
H23 H 0.4746 0.6472 1.1915 0.069 Uiso 1 1 calc R
C24 C 0.5217(3) 0.7135(3) 1.1433(2) 0.0408(11) Uani 1 1 d .
C25 C 0.5537(3) 0.7794(4) 1.1925(2) 0.0511(14) Uani 1 1 d .
H25 H 0.5471 0.7805 1.2313 0.068 Uiso 1 1 calc R
C26 C 0.5940(4) 0.8414(5) 1.1847(3) 0.0580(19) Uani 1 1 d .
H26 H 0.6147 0.8849 1.2177 0.077 Uiso 1 1 calc R
C27 C 0.6045(3) 0.8401(4) 1.1260(3) 0.0590(15) Uani 1 1 d .
H27 H 0.6328 0.8823 1.1208 0.078 Uiso 1 1 calc R
C28 C 0.5733(3) 0.7770(3) 1.0771(2) 0.0454(12) Uani 1 1 d .
H28 H 0.5805 0.7775 1.0386 0.060 Uiso 1 1 calc R
C29 C 0.5309(3) 0.7116(4) 1.0831(3) 0.0357(14) Uani 1 1 d .
C30 C 0.4977(3) 0.6432(3) 1.0330(2) 0.0348(10) Uani 1 1 d .
C31 C 0.7776(5) 0.5671(8) 1.1575(5) 0.164(5) Uani 1 1 d .
H31A H 0.8038 0.5245 1.1930 0.218 Uiso 1 1 calc R
H31B H 0.8114 0.6076 1.1556 0.218 Uiso 1 1 calc R
C32 C 0.7331(5) 0.6138(7) 1.1766(7) 0.180(6) Uani 1 1 d .
H32A H 0.7605 0.6298 1.2246 0.239 Uiso 1 1 calc R
H32B H 0.7197 0.6677 1.1503 0.239 Uiso 1 1 calc R
C33 C 0.7358(4) 0.5746(7) 1.0388(4) 0.128(4) Uani 1 1 d .
H33A H 0.7110 0.5449 0.9956 0.192 Uiso 1 1 calc R
H33B H 0.7822 0.5901 1.0462 0.192 Uiso 1 1 calc R
H33C H 0.7105 0.6266 1.0384 0.192 Uiso 1 1 calc R
C34 C 0.6737(6) 0.5231(7) 1.2274(4) 0.135(4) Uani 1 1 d .
H34A H 0.6277 0.4995 1.2144 0.203 Uiso 1 1 calc R
H34B H 0.6875 0.5610 1.2663 0.203 Uiso 1 1 calc R
H34C H 0.7071 0.4761 1.2391 0.203 Uiso 1 1 calc R
C35 C 0.5127(8) 0.0181(5) 0.9760(9) 0.150(6) Uani 1 1 d .
H35A H 0.4972 -0.0348 0.9485 0.199 Uiso 1 1 calc R
H35B H 0.5639 0.0180 1.0000 0.199 Uiso 1 1 calc R
C36 C 0.5293(4) 0.1013(5) 0.8946(4) 0.113(3) Uani 1 1 d .
H36A H 0.5141 0.1511 0.8645 0.169 Uiso 1 1 calc R
H36B H 0.5233 0.0492 0.8681 0.169 Uiso 1 1 calc R
H36C H 0.5782 0.1079 0.9275 0.169 Uiso 1 1 calc R
N1 N 0.7412(3) 0.5208(3) 1.0905(3) 0.0842(17) Uani 1 1 d .
H1 H 0.7650 0.4712 1.0915 0.112 Uiso 1 1 calc R
N2 N 0.6720(3) 0.5737(4) 1.1686(3) 0.0873(19) Uani 1 1 d .
H2 H 0.6380 0.6154 1.1564 0.116 Uiso 1 1 calc R
N3 N 0.4876(3) 0.0950(4) 0.9304(3) 0.0813(18) Uani 1 1 d .
H3 H 0.4411 0.0884 0.8996 0.108 Uiso 1 1 calc R
O1 O 0.54284(15) 0.28887(18) 0.96851(14) 0.0317(7) Uani 1 1 d .
O2 O 0.59938(15) 0.3900(2) 1.09755(13) 0.0365(7) Uani 1 1 d .
O3 O 0.4342(2) 0.5068(3) 1.0041(2) 0.0365(11) Uani 1 1 d .
Lu1' Lu 0.5000 0.630585(13) 0.5000 0.03235(8) Uani 1 2 d S
Li1' Li 0.4397(5) 0.5386(5) 0.5880(4) 0.0452(19) Uani 1 1 d .
Li2' Li 0.5000 0.8351(12) 0.5000 0.047(4) Uani 1 2 d S
C1' C 0.3695(3) 0.7323(3) 0.4811(2) 0.0316(10) Uani 1 1 d .
C2' C 0.3034(3) 0.7102(3) 0.4230(2) 0.0404(11) Uani 1 1 d .
H2'1 H 0.3006 0.7054 0.3797 0.054 Uiso 1 1 calc R
C3' C 0.2456(3) 0.6963(3) 0.4307(3) 0.0398(12) Uani 1 1 d .
H3'1 H 0.2030 0.6838 0.3922 0.053 Uiso 1 1 calc R
C4' C 0.2483(4) 0.7004(4) 0.4963(4) 0.0407(14) Uani 1 1 d .
C5' C 0.1872(3) 0.6810(5) 0.5040(3) 0.0459(16) Uani 1 1 d .
H5' H 0.1448 0.6666 0.4658 0.061 Uiso 1 1 calc R
C6' C 0.1912(3) 0.6838(3) 0.5681(3) 0.0545(14) Uani 1 1 d .
H6' H 0.1515 0.6717 0.5733 0.072 Uiso 1 1 calc R
C7' C 0.2550(3) 0.7050(3) 0.6253(3) 0.0478(12) Uani 1 1 d .
H7' H 0.2573 0.7064 0.6686 0.064 Uiso 1 1 calc R
C8' C 0.3141(2) 0.7237(3) 0.6192(2) 0.0370(10) Uani 1 1 d .
H8' H 0.3560 0.7376 0.6581 0.049 Uiso 1 1 calc R
C9' C 0.3120(2) 0.7222(3) 0.5537(2) 0.0318(10) Uani 1 1 d .
C10' C 0.3734(2) 0.7413(3) 0.5455(2) 0.0295(10) Uani 1 1 d .
C11' C 0.4407(2) 0.7699(3) 0.60488(19) 0.0303(9) Uani 1 1 d .
C12' C 0.4450(2) 0.8541(3) 0.6365(2) 0.0337(10) Uani 1 1 d .
C13' C 0.3859(3) 0.9107(3) 0.6144(2) 0.0406(11) Uani 1 1 d .
H13' H 0.3432 0.8941 0.5776 0.054 Uiso 1 1 calc R
C14' C 0.3905(3) 0.9894(3) 0.6460(3) 0.0524(13) Uani 1 1 d .
H14' H 0.3509 1.0251 0.6309 0.070 Uiso 1 1 calc R
C15' C 0.4551(3) 1.0166(3) 0.7017(3) 0.0556(14) Uani 1 1 d .
H15' H 0.4581 1.0697 0.7236 0.074 Uiso 1 1 calc R
C16' C 0.5124(3) 0.9642(3) 0.7225(2) 0.0487(13) Uani 1 1 d .
H16' H 0.5549 0.9827 0.7587 0.065 Uiso 1 1 calc R
C17' C 0.5100(3) 0.8825(3) 0.6915(2) 0.0388(11) Uani 1 1 d .
C18' C 0.5691(3) 0.8280(3) 0.7128(2) 0.0422(11) Uani 1 1 d .
H18' H 0.6120 0.8465 0.7483 0.056 Uiso 1 1 calc R
C19' C 0.5655(2) 0.7492(3) 0.6831(2) 0.0407(11) Uani 1 1 d .
H19' H 0.6059 0.7147 0.6985 0.054 Uiso 1 1 calc R
C20' C 0.5004(2) 0.7184(3) 0.6282(2) 0.0311(9) Uani 1 1 d .
C21' C 0.5838(2) 0.4552(3) 0.54390(19) 0.0308(9) Uani 1 1 d .
C22' C 0.6522(2) 0.4494(3) 0.6036(2) 0.0404(11) Uani 1 1 d .
H22' H 0.6863 0.4911 0.6100 0.054 Uiso 1 1 calc R
C23' C 0.6676(2) 0.3856(3) 0.6497(2) 0.0445(12) Uani 1 1 d .
H23' H 0.7127 0.3829 0.6870 0.059 Uiso 1 1 calc R
C24' C 0.6172(2) 0.3224(3) 0.6432(2) 0.0377(10) Uani 1 1 d .
C25' C 0.6299(3) 0.2587(4) 0.6947(2) 0.0556(14) Uani 1 1 d .
H25' H 0.6735 0.2575 0.7340 0.074 Uiso 1 1 calc R
C26' C 0.5801(4) 0.2000(6) 0.6877(3) 0.072(2) Uani 1 1 d .
H26' H 0.5896 0.1597 0.7226 0.096 Uiso 1 1 calc R
C27' C 0.5147(3) 0.1988(4) 0.6291(3) 0.0634(16) Uani 1 1 d .
H27' H 0.4810 0.1575 0.6246 0.084 Uiso 1 1 calc R
C28' C 0.5003(3) 0.2593(3) 0.5775(2) 0.0464(12) Uani 1 1 d .
H28' H 0.4568 0.2575 0.5380 0.062 Uiso 1 1 calc R
C29' C 0.5497(3) 0.3236(4) 0.5830(3) 0.0359(14) Uani 1 1 d .
C30' C 0.5346(2) 0.3892(3) 0.5321(2) 0.0307(9) Uani 1 1 d .
C31' C 0.3807(4) 0.4197(6) 0.6461(4) 0.117(4) Uani 1 1 d .
H31C H 0.3501 0.4091 0.6666 0.156 Uiso 1 1 calc R
H31D H 0.3807 0.3673 0.6213 0.156 Uiso 1 1 calc R
C32' C 0.4496(5) 0.4350(7) 0.6988(5) 0.126(3) Uani 1 1 d .
H32C H 0.4665 0.3834 0.7277 0.168 Uiso 1 1 calc R
H32D H 0.4489 0.4831 0.7272 0.168 Uiso 1 1 calc R
C33' C 0.2931(3) 0.4627(5) 0.5332(3) 0.084(2) Uani 1 1 d .
H33D H 0.2737 0.5098 0.5008 0.126 Uiso 1 1 calc R
H33E H 0.2573 0.4394 0.5431 0.126 Uiso 1 1 calc R
H33F H 0.3098 0.4176 0.5141 0.126 Uiso 1 1 calc R
C34' C 0.5631(4) 0.4896(5) 0.7282(3) 0.095(3) Uani 1 1 d .
H34D H 0.5954 0.5022 0.7105 0.142 Uiso 1 1 calc R
H34E H 0.5836 0.4468 0.7642 0.142 Uiso 1 1 calc R
H34F H 0.5537 0.5422 0.7463 0.142 Uiso 1 1 calc R
C35' C 0.4633(5) 1.0148(5) 0.4757(6) 0.106(3) Uani 1 1 d .
H35C H 0.4533 1.0655 0.4460 0.141 Uiso 1 1 calc R
H35D H 0.4360 1.0203 0.5002 0.141 Uiso 1 1 calc R
C36' C 0.3640(4) 0.9308(4) 0.3980(4) 0.086(2) Uani 1 1 d .
H36D H 0.3499 0.8797 0.3692 0.129 Uiso 1 1 calc R
H36E H 0.3446 0.9819 0.3701 0.129 Uiso 1 1 calc R
H36F H 0.3471 0.9267 0.4312 0.129 Uiso 1 1 calc R
N1' N 0.3507(3) 0.4948(3) 0.5954(2) 0.0623(13) Uani 1 1 d .
H1' H 0.3352 0.5378 0.6136 0.083 Uiso 1 1 calc R
N2' N 0.4966(3) 0.4553(3) 0.6724(2) 0.0630(13) Uani 1 1 d .
H2' H 0.5064 0.4050 0.6565 0.084 Uiso 1 1 calc R
N3' N 0.4407(3) 0.9368(3) 0.4333(2) 0.0584(13) Uani 1 1 d .
H3' H 0.4550 0.9422 0.4007 0.078 Uiso 1 1 calc R
O1' O 0.42673(15) 0.74144(18) 0.47223(14) 0.0314(6) Uani 1 1 d .
O2' O 0.49936(15) 0.64047(19) 0.59995(13) 0.0336(6) Uani 1 1 d .
O3' O 0.5696(2) 0.5231(3) 0.5010(2) 0.0358(10) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O3 Lu1 O3 83.4(2) . 2_657
O3 Lu1 O1 101.00(13) . 2_657
O3 Lu1 O1 164.92(13) 2_657 2_657
O3 Lu1 O1 164.92(12) . .
O3 Lu1 O1 101.00(13) 2_657 .
O1 Lu1 O1 78.51(15) 2_657 .
O3 Lu1 O2 110.94(13) . .
O3 Lu1 O2 75.23(14) 2_657 .
O1 Lu1 O2 89.77(11) 2_657 .
O1 Lu1 O2 84.14(10) . .
O3 Lu1 O2 75.23(14) . 2_657
O3 Lu1 O2 110.94(13) 2_657 2_657
O1 Lu1 O2 84.14(10) 2_657 2_657
O1 Lu1 O2 89.76(11) . 2_657
O2 Lu1 O2 172.14(16) . 2_657
O3 Lu1 Li2 138.31(12) . .
O3 Lu1 Li2 138.31(11) 2_657 .
O1 Lu1 Li2 39.26(8) 2_657 .
O1 Lu1 Li2 39.26(8) . .
O2 Lu1 Li2 86.07(8) . .
O2 Lu1 Li2 86.07(8) 2_657 .
O3 Lu1 Li1 97.6(2) . .
O3 Lu1 Li1 36.7(2) 2_657 .
O1 Lu1 Li1 128.27(19) 2_657 .
O1 Lu1 Li1 94.3(2) . .
O2 Lu1 Li1 38.6(2) . .
O2 Lu1 Li1 147.5(2) 2_657 .
Li2 Lu1 Li1 116.64(17) . .
O3 Lu1 Li1 36.7(2) . 2_657
O3 Lu1 Li1 97.6(2) 2_657 2_657
O1 Lu1 Li1 94.3(2) 2_657 2_657
O1 Lu1 Li1 128.27(19) . 2_657
O2 Lu1 Li1 147.5(2) . 2_657
O2 Lu1 Li1 38.6(2) 2_657 2_657
Li2 Lu1 Li1 116.64(17) . 2_657
Li1 Lu1 Li1 126.7(3) . 2_657
O3 Li1 O2 89.6(4) 2_657 .
O3 Li1 N1 117.8(6) 2_657 .
O2 Li1 N1 137.4(5) . .
O3 Li1 N2 124.2(5) 2_657 .
O2 Li1 N2 105.0(5) . .
N1 Li1 N2 86.7(4) . .
O3 Li1 C32 130.0(5) 2_657 .
O2 Li1 C32 128.5(6) . .
N1 Li1 C32 58.3(3) . .
N2 Li1 C32 28.9(3) . .
O3 Li1 Lu1 44.3(2) 2_657 .
O2 Li1 Lu1 45.2(2) . .
N1 Li1 Lu1 148.8(5) . .
N2 Li1 Lu1 124.3(5) . .
C32 Li1 Lu1 151.8(4) . .
O1 Li2 O1 90.4(7) 2_657 .
O1 Li2 N3 101.0(2) 2_657 2_657
O1 Li2 N3 149.0(2) . 2_657
O1 Li2 N3 149.0(2) 2_657 .
O1 Li2 N3 101.0(2) . .
N3 Li2 N3 83.9(7) 2_657 .
O1 Li2 Lu1 45.2(4) 2_657 .
O1 Li2 Lu1 45.2(4) . .
N3 Li2 Lu1 138.0(4) 2_657 .
N3 Li2 Lu1 138.0(4) . .
O1 C1 C10 121.6(4) . .
O1 C1 C2 118.3(4) . .
C10 C1 C2 120.1(5) . .
C3 C2 C1 120.9(4) . .
C2 C3 C4 121.1(5) . .
C5 C4 C9 122.2(6) . .
C5 C4 C3 120.6(5) . .
C9 C4 C3 117.2(6) . .
C6 C5 C4 119.8(6) . .
C5 C6 C7 119.3(5) . .
C8 C7 C6 121.4(5) . .
C7 C8 C9 120.9(5) . .
C4 C9 C10 121.6(5) . .
C4 C9 C8 116.3(5) . .
C10 C9 C8 122.0(4) . .
C1 C10 C9 118.9(4) . .
C1 C10 C11 119.8(4) . .
C9 C10 C11 121.3(4) . .
C20 C11 C12 119.2(4) . .
C20 C11 C10 120.5(4) . .
C12 C11 C10 120.4(4) . .
C17 C12 C13 116.8(4) . .
C17 C12 C11 121.1(5) . .
C13 C12 C11 122.1(4) . .
C14 C13 C12 122.5(5) . .
C13 C14 C15 120.1(6) . .
C16 C15 C14 119.9(6) . .
C15 C16 C17 122.0(6) . .
C18 C17 C12 118.0(5) . .
C18 C17 C16 123.4(5) . .
C12 C17 C16 118.6(5) . .
C19 C18 C17 121.6(5) . .
C18 C19 C20 121.0(5) . .
O2 C20 C11 122.1(4) . .
O2 C20 C19 118.8(4) . .
C11 C20 C19 119.1(4) . .
O3 C21 C30 122.5(4) . .
O3 C21 C22 117.7(4) . .
C30 C21 C22 119.8(4) . .
C23 C22 C21 121.0(5) . .
C22 C23 C24 121.3(4) . .
C25 C24 C23 121.3(4) . .
C25 C24 C29 120.0(5) . .
C23 C24 C29 118.7(5) . .
C26 C25 C24 121.3(5) . .
C25 C26 C27 119.7(6) . .
C28 C27 C26 120.2(6) . .
C27 C28 C29 122.0(5) . .
C28 C29 C24 116.9(5) . .
C28 C29 C30 123.7(5) . .
C24 C29 C30 119.4(5) . .
C21 C30 C29 119.5(4) . .
C21 C30 C30 120.1(3) . 2_657
C29 C30 C30 120.4(4) . 2_657
C32 C31 N1 115.1(8) . .
N2 C32 C31 118.3(8) . .
N2 C32 Li1 48.4(4) . .
C31 C32 Li1 75.5(5) . .
C35 C35 N3 111.5(9) 2_657 .
C33 N1 C31 109.9(8) . .
C33 N1 Li1 111.9(6) . .
C31 N1 Li1 103.9(6) . .
C32 N2 C34 119.0(9) . .
C32 N2 Li1 102.7(6) . .
C34 N2 Li1 110.7(5) . .
C36 N3 C35 107.6(7) . .
C36 N3 Li2 116.1(5) . .
C35 N3 Li2 102.8(7) . .
C1 O1 Li2 132.8(4) . .
C1 O1 Lu1 117.1(3) . .
Li2 O1 Lu1 95.5(4) . .
C20 O2 Li1 128.0(4) . .
C20 O2 Lu1 122.8(2) . .
Li1 O2 Lu1 96.2(3) . .
C21 O3 Li1 134.6(4) . 2_657
C21 O3 Lu1 121.6(3) . .
Li1 O3 Lu1 99.0(3) 2_657 .
O1' Lu1' O1' 78.87(15) 2_656 .
O1' Lu1' O3' 165.43(12) 2_656 2_656
O1' Lu1' O3' 100.32(13) . 2_656
O1' Lu1' O3' 100.32(13) 2_656 .
O1' Lu1' O3' 165.43(12) . .
O3' Lu1' O3' 84.1(2) 2_656 .
O1' Lu1' O2' 90.46(10) 2_656 .
O1' Lu1' O2' 83.48(10) . .
O3' Lu1' O2' 75.03(13) 2_656 .
O3' Lu1' O2' 111.09(13) . .
O1' Lu1' O2' 83.48(10) 2_656 2_656
O1' Lu1' O2' 90.46(10) . 2_656
O3' Lu1' O2' 111.09(13) 2_656 2_656
O3' Lu1' O2' 75.03(13) . 2_656
O2' Lu1' O2' 172.17(15) . 2_656
O1' Lu1' Li1' 128.73(16) 2_656 .
O1' Lu1' Li1' 94.00(17) . .
O3' Lu1' Li1' 36.71(18) 2_656 .
O3' Lu1' Li1' 97.65(19) . .
O2' Lu1' Li1' 38.37(17) . .
O2' Lu1' Li1' 147.73(17) 2_656 .
O1' Lu1' Li1' 94.00(17) 2_656 2_656
O1' Lu1' Li1' 128.73(16) . 2_656
O3' Lu1' Li1' 97.65(19) 2_656 2_656
O3' Lu1' Li1' 36.71(18) . 2_656
O2' Lu1' Li1' 147.73(16) . 2_656
O2' Lu1' Li1' 38.37(16) 2_656 2_656
Li1' Lu1' Li1' 126.5(3) . 2_656
O1' Lu1' Li2' 39.43(8) 2_656 .
O1' Lu1' Li2' 39.43(8) . .
O3' Lu1' Li2' 137.95(11) 2_656 .
O3' Lu1' Li2' 137.95(11) . .
O2' Lu1' Li2' 86.08(7) . .
O2' Lu1' Li2' 86.08(7) 2_656 .
Li1' Lu1' Li2' 116.76(15) . .
Li1' Lu1' Li2' 116.76(15) 2_656 .
O3' Li1' O2' 89.0(4) 2_656 .
O3' Li1' N1' 112.5(4) 2_656 .
O2' Li1' N1' 143.6(5) . .
O3' Li1' N2' 125.1(5) 2_656 .
O2' Li1' N2' 107.0(4) . .
N1' Li1' N2' 84.9(4) . .
O3' Li1' Lu1' 44.4(2) 2_656 .
O2' Li1' Lu1' 44.66(18) . .
N1' Li1' Lu1' 147.9(4) . .
N2' Li1' Lu1' 125.6(4) . .
O1' Li2' O1' 88.4(7) . 2_656
O1' Li2' N3' 150.86(16) . 2_656
O1' Li2' N3' 100.62(17) 2_656 2_656
O1' Li2' N3' 100.62(17) . .
O1' Li2' N3' 150.86(16) 2_656 .
N3' Li2' N3' 84.9(7) 2_656 .
O1' Li2' Lu1' 44.2(4) . .
O1' Li2' Lu1' 44.2(4) 2_656 .
N3' Li2' Lu1' 137.6(4) 2_656 .
N3' Li2' Lu1' 137.6(4) . .
O1' C1' C10' 121.3(4) . .
O1' C1' C2' 119.0(4) . .
C10' C1' C2' 119.7(4) . .
C3' C2' C1' 120.6(4) . .
C2' C3' C4' 121.4(5) . .
C9' C4' C3' 119.1(6) . .
C9' C4' C5' 120.2(6) . .
C3' C4' C5' 120.7(6) . .
C6' C5' C4' 119.8(5) . .
C5' C6' C7' 119.9(5) . .
C8' C7' C6' 121.4(5) . .
C7' C8' C9' 120.5(4) . .
C4' C9' C8' 118.3(5) . .
C4' C9' C10' 119.9(5) . .
C8' C9' C10' 121.8(4) . .
C1' C10' C9' 119.1(4) . .
C1' C10' C11' 119.7(4) . .
C9' C10' C11' 121.2(4) . .
C20' C11' C12' 119.3(4) . .
C20' C11' C10' 120.5(4) . .
C12' C11' C10' 120.1(4) . .
C17' C12' C13' 117.9(4) . .
C17' C12' C11' 119.9(4) . .
C13' C12' C11' 122.2(4) . .
C14' C13' C12' 121.4(5) . .
C13' C14' C15' 120.4(5) . .
C16' C15' C14' 118.9(5) . .
C15' C16' C17' 122.5(5) . .
C18' C17' C16' 122.8(4) . .
C18' C17' C12' 118.4(4) . .
C16' C17' C12' 118.8(4) . .
C19' C18' C17' 122.0(4) . .
C18' C19' C20' 120.7(4) . .
O2' C20' C11' 121.6(4) . .
O2' C20' C19' 118.8(4) . .
C11' C20' C19' 119.6(4) . .
O3' C21' C30' 121.9(4) . .
O3' C21' C22' 119.2(4) . .
C30' C21' C22' 118.9(4) . .
C23' C22' C21' 121.4(5) . .
C22' C23' C24' 121.4(4) . .
C23' C24' C25' 122.7(4) . .
C23' C24' C29' 118.8(4) . .
C25' C24' C29' 118.6(5) . .
C26' C25' C24' 121.4(5) . .
C25' C26' C27' 121.0(6) . .
C28' C27' C26' 119.5(6) . .
C27' C28' C29' 121.7(5) . .
C28' C29' C30' 122.7(5) . .
C28' C29' C24' 117.7(5) . .
C30' C29' C24' 119.6(5) . .
C21' C30' C29' 119.4(4) . .
C21' C30' C30' 120.4(3) . 2_656
C29' C30' C30' 120.1(4) . 2_656
C32' C31' N1' 113.6(6) . .
C31' C32' N2' 112.0(7) . .
C35' C35' N3' 113.6(6) 2_656 .
C33' N1' C31' 108.8(5) . .
C33' N1' Li1' 116.3(4) . .
C31' N1' Li1' 102.1(4) . .
C32' N2' C34' 109.5(6) . .
C32' N2' Li1' 105.4(5) . .
C34' N2' Li1' 116.9(5) . .
C35' N3' C36' 110.5(6) . .
C35' N3' Li2' 104.4(6) . .
C36' N3' Li2' 119.2(5) . .
C1' O1' Li2' 132.4(4) . .
C1' O1' Lu1' 117.7(3) . .
Li2' O1' Lu1' 96.3(4) . .
C20' O2' Li1' 129.7(4) . .
C20' O2' Lu1' 121.1(2) . .
Li1' O2' Lu1' 97.0(3) . .
C21' O3' Li1' 135.0(4) . 2_656
C21' O3' Lu1' 120.8(3) . .
Li1' O3' Lu1' 98.9(3) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O3 2.189(4) .
Lu1 O3 2.189(4) 2_657
Lu1 O1 2.192(3) 2_657
Lu1 O1 2.192(3) .
Lu1 O2 2.210(3) .
Lu1 O2 2.210(3) 2_657
Lu1 Li2 3.073(17) .
Lu1 Li1 3.094(9) .
Lu1 Li1 3.094(9) 2_657
Li1 O3 1.871(10) 2_657
Li1 O2 1.940(10) .
Li1 N1 2.034(11) .
Li1 N2 2.138(11) .
Li1 C32 2.789(12) .
Li2 O1 1.954(12) 2_657
Li2 O1 1.954(12) .
Li2 N3 2.134(14) 2_657
Li2 N3 2.134(14) .
C1 O1 1.342(6) .
C1 C10 1.384(6) .
C1 C2 1.423(6) .
C2 C3 1.356(7) .
C3 C4 1.444(8) .
C4 C5 1.385(10) .
C4 C9 1.407(7) .
C5 C6 1.380(8) .
C6 C7 1.400(7) .
C7 C8 1.355(7) .
C8 C9 1.434(6) .
C9 C10 1.427(7) .
C10 C11 1.494(6) .
C11 C20 1.386(6) .
C11 C12 1.429(6) .
C12 C17 1.414(6) .
C12 C13 1.420(7) .
C13 C14 1.356(7) .
C14 C15 1.390(9) .
C15 C16 1.341(10) .
C16 C17 1.426(8) .
C17 C18 1.406(8) .
C18 C19 1.357(8) .
C19 C20 1.438(6) .
C20 O2 1.326(5) .
C21 O3 1.355(6) .
C21 C30 1.390(6) .
C21 C22 1.430(6) .
C22 C23 1.353(7) .
C23 C24 1.421(7) .
C24 C25 1.401(7) .
C24 C29 1.430(7) .
C25 C26 1.346(9) .
C26 C27 1.411(8) .
C27 C28 1.365(7) .
C28 C29 1.400(8) .
C29 C30 1.442(8) .
C30 C30 1.502(8) 2_657
C31 C32 1.405(12) .
C31 N1 1.484(9) .
C32 N2 1.380(11) .
C33 N1 1.365(9) .
C34 N2 1.493(10) .
C35 C35 1.40(2) 2_657
C35 N3 1.474(13) .
C36 N3 1.447(10) .
O3 Li1 1.871(10) 2_657
Lu1' O1' 2.194(3) 2_656
Lu1' O1' 2.194(3) .
Lu1' O3' 2.212(4) 2_656
Lu1' O3' 2.212(4) .
Lu1' O2' 2.213(3) .
Lu1' O2' 2.213(3) 2_656
Lu1' Li1' 3.124(8) .
Lu1' Li1' 3.124(8) 2_656
Lu1' Li2' 3.127(18) .
Li1' O3' 1.891(9) 2_656
Li1' O2' 1.954(9) .
Li1' N1' 2.100(10) .
Li1' N2' 2.106(9) .
Li2' O1' 1.998(13) .
Li2' O1' 1.998(13) 2_656
Li2' N3' 2.107(14) 2_656
Li2' N3' 2.107(14) .
C1' O1' 1.338(5) .
C1' C10' 1.388(6) .
C1' C2' 1.434(6) .
C2' C3' 1.344(7) .
C3' C4' 1.419(8) .
C4' C9' 1.398(8) .
C4' C5' 1.431(9) .
C5' C6' 1.372(8) .
C6' C7' 1.395(7) .
C7' C8' 1.367(7) .
C8' C9' 1.422(6) .
C9' C10' 1.441(7) .
C10' C11' 1.488(6) .
C11' C20' 1.380(6) .
C11' C12' 1.446(6) .
C12' C17' 1.418(6) .
C12' C13' 1.419(6) .
C13' C14' 1.371(6) .
C14' C15' 1.415(8) .
C15' C16' 1.354(8) .
C16' C17' 1.413(6) .
C17' C18' 1.401(7) .
C18' C19' 1.357(7) .
C19' C20' 1.431(6) .
C20' O2' 1.340(5) .
C21' O3' 1.339(6) .
C21' C30' 1.393(6) .
C21' C22' 1.442(6) .
C22' C23' 1.333(7) .
C23' C24' 1.406(7) .
C24' C25' 1.420(7) .
C24' C29' 1.433(7) .
C25' C26' 1.348(10) .
C26' C27' 1.390(9) .
C27' C28' 1.383(7) .
C28' C29' 1.407(8) .
C29' C30' 1.425(7) .
C30' C30' 1.494(8) 2_656
C31' C32' 1.406(10) .
C31' N1' 1.518(8) .
C32' N2' 1.413(8) .
C33' N1' 1.433(7) .
C34' N2' 1.475(8) .
C35' C35' 1.430(17) 2_656
C35' N3' 1.449(10) .
C36' N3' 1.454(8) .
O3' Li1' 1.891(9) 2_656
