# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
'Jason Love'
'Alexander J. Blake'
'Peter B. Hitchcock'
'Andrew Novak'
'Stuart D. Reid'
'Claire Wilson'

_publ_contact_author_name        'Dr Jason Love'
_publ_contact_author_address     
;
Department of Chemistry
University of Nottingham
University Park
Nottingham
NG7 2RD
UNITED KINGDOM
;

_publ_contact_author_email       JASON.LOVE@NOTTINGHAM.AC.UK

_publ_section_title              
;
The syntheses and structures of Group 1 expanded
dipyrrolides: the formation of a 12-rung amidolithium circular ladder
;

data_dippyr
_database_code_CSD               207484

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H50 K2 N4 O2'
_chemical_formula_weight         685.03

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   13.773(3)
_cell_length_b                   10.194(2)
_cell_length_c                   13.787(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.086(3)
_cell_angle_gamma                90.00
_cell_volume                     1877.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2080
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      19.8

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          1.01
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'SADABS v2.03'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            16994
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.54
_reflns_number_total             7990
_reflns_number_gt                5443
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'

_refine_special_details          
;
THF shows disorder, one molecule has 2 carbon atoms modelled over 2 half
occupied sites, the other has all 5 non-H atoms modelled over 2 sites with
occupancies 0.70:0.30. All partially occupied sites refined with isotropic
adps and geometry restraints.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.8587P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     'direct methods'
_atom_sites_solution_secondary   'difference Fourier'
_atom_sites_solution_hydrogens   'geometrically placed'
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0028(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_number_reflns         7979
_refine_ls_number_parameters     403
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.74917(7) -0.10430(11) 0.76640(9) 0.0371(3) Uani 1 1 d . . .
K2 K 0.56732(7) 0.09301(10) 0.52564(8) 0.0299(3) Uani 1 1 d . . .
O2 O 0.9387(3) -0.1877(4) 0.7549(3) 0.0579(11) Uiso 1 1 d D A .
N1 N 0.7905(3) 0.1707(4) 0.8088(3) 0.0333(10) Uani 1 1 d . A .
N2 N 0.5954(3) 0.0568(3) 0.7524(3) 0.0258(9) Uani 1 1 d . A .
N3 N 0.5654(2) -0.1508(3) 0.6019(3) 0.0233(8) Uani 1 1 d . . .
N4 N 0.7207(2) -0.1087(4) 0.5058(3) 0.0297(9) Uani 1 1 d . A .
C1 C 0.7107(3) 0.2432(5) 0.7842(3) 0.0300(11) Uani 1 1 d . . .
H1A H 0.7181 0.3358 0.7896 0.036 Uiso 1 1 calc R A .
C2 C 0.6108(3) 0.1896(5) 0.7488(3) 0.0259(10) Uani 1 1 d . A .
C3 C 0.5217(3) 0.2576(5) 0.7114(4) 0.0294(11) Uani 1 1 d . A .
H3A H 0.5116 0.3545 0.7142 0.035 Uiso 1 1 calc R . .
C4 C 0.4464(3) 0.1612(5) 0.6906(3) 0.0278(10) Uani 1 1 d . A .
H4A H 0.3727 0.1776 0.6772 0.033 Uiso 1 1 calc R . .
C5 C 0.4941(3) 0.0397(5) 0.7158(3) 0.0241(10) Uani 1 1 d . A .
C6 C 0.4494(3) -0.0976(5) 0.7104(3) 0.0229(9) Uani 1 1 d . . .
C7 C 0.5207(3) -0.1952(5) 0.6751(3) 0.0239(10) Uani 1 1 d . . .
C8 C 0.5529(3) -0.3213(5) 0.7059(4) 0.0283(10) Uani 1 1 d . A .
H8A H 0.5272 -0.3778 0.7534 0.034 Uiso 1 1 calc R . .
C9 C 0.6226(3) -0.3580(5) 0.6511(4) 0.0289(11) Uani 1 1 d . A .
H9A H 0.6495 -0.4482 0.6461 0.035 Uiso 1 1 calc R . .
C10 C 0.6291(3) -0.2497(5) 0.5882(3) 0.0256(10) Uani 1 1 d . . .
C11 C 0.7019(3) -0.2257(5) 0.5305(3) 0.0247(10) Uani 1 1 d . A .
H11A H 0.7431 -0.3003 0.5154 0.030 Uiso 1 1 calc R . .
C12 C 0.4388(3) -0.1440(4) 0.8147(3) 0.0243(10) Uani 1 1 d . A .
C13 C 0.4785(3) -0.0720(5) 0.9016(4) 0.0320(12) Uani 1 1 d . . .
H13A H 0.5129 0.0078 0.8974 0.038 Uiso 1 1 calc R A .
C14 C 0.4682(4) -0.1158(6) 0.9944(4) 0.0418(13) Uani 1 1 d . A .
H14A H 0.4958 -0.0658 1.0528 0.050 Uiso 1 1 calc R . .
C15 C 0.4177(4) -0.2322(5) 1.0024(4) 0.0420(14) Uani 1 1 d . . .
H15A H 0.4110 -0.2624 1.0657 0.050 Uiso 1 1 calc R A .
C16 C 0.3779(4) -0.3021(6) 0.9175(4) 0.0412(13) Uani 1 1 d . A .
H16A H 0.3431 -0.3814 0.9219 0.049 Uiso 1 1 calc R . .
C17 C 0.3877(4) -0.2585(5) 0.8240(4) 0.0350(12) Uani 1 1 d . . .
H17A H 0.3588 -0.3084 0.7659 0.042 Uiso 1 1 calc R A .
C18 C 0.3451(3) -0.0954(4) 0.6348(3) 0.0240(9) Uani 1 1 d . A .
C19 C 0.2589(3) -0.0620(5) 0.6665(4) 0.0339(12) Uani 1 1 d . . .
H19A H 0.2642 -0.0427 0.7350 0.041 Uiso 1 1 calc R A .
C20 C 0.1660(3) -0.0570(5) 0.5989(4) 0.0392(13) Uani 1 1 d . A .
H20A H 0.1086 -0.0336 0.6217 0.047 Uiso 1 1 calc R . .
C21 C 0.1558(3) -0.0858(5) 0.4985(4) 0.0369(12) Uani 1 1 d . . .
H21A H 0.0920 -0.0841 0.4527 0.044 Uiso 1 1 calc R A .
C22 C 0.2413(3) -0.1171(5) 0.4667(4) 0.0327(11) Uani 1 1 d . A .
H22A H 0.2362 -0.1365 0.3982 0.039 Uiso 1 1 calc R . .
C23 C 0.3336(3) -0.1202(5) 0.5343(3) 0.0284(10) Uani 1 1 d . . .
H23A H 0.3912 -0.1402 0.5106 0.034 Uiso 1 1 calc R A .
C24 C 0.8908(3) 0.2296(5) 0.8514(4) 0.0405(13) Uani 1 1 d . . .
C25 C 0.8867(4) 0.3718(6) 0.8896(5) 0.0583(17) Uani 1 1 d . A .
H25A H 0.8497 0.3732 0.9420 0.088 Uiso 1 1 calc R . .
H25B H 0.8529 0.4281 0.8340 0.088 Uiso 1 1 calc R . .
H25C H 0.9549 0.4039 0.9170 0.088 Uiso 1 1 calc R . .
C26 C 0.9418(4) 0.1430(6) 0.9384(4) 0.0491(15) Uani 1 1 d . A .
H26A H 0.9052 0.1478 0.9910 0.074 Uiso 1 1 calc R . .
H26B H 1.0107 0.1731 0.9649 0.074 Uiso 1 1 calc R . .
H26C H 0.9423 0.0521 0.9153 0.074 Uiso 1 1 calc R . .
C27 C 0.9485(3) 0.2224(7) 0.7692(4) 0.0557(18) Uani 1 1 d . A .
H27A H 0.9161 0.2794 0.7134 0.084 Uiso 1 1 calc R . .
H27B H 0.9485 0.1318 0.7455 0.084 Uiso 1 1 calc R . .
H27C H 1.0176 0.2515 0.7963 0.084 Uiso 1 1 calc R . .
C28 C 0.7974(3) -0.0828(5) 0.4482(4) 0.0327(12) Uani 1 1 d . . .
C29 C 0.7422(4) -0.0117(7) 0.3542(5) 0.0569(18) Uani 1 1 d . A .
H29A H 0.6940 -0.0716 0.3122 0.085 Uiso 1 1 calc R . .
H29B H 0.7903 0.0184 0.3171 0.085 Uiso 1 1 calc R . .
H29C H 0.7066 0.0640 0.3725 0.085 Uiso 1 1 calc R . .
C30 C 0.8733(4) 0.0109(6) 0.5148(5) 0.0526(16) Uani 1 1 d . A .
H30A H 0.8381 0.0884 0.5310 0.079 Uiso 1 1 calc R . .
H30B H 0.9233 0.0382 0.4791 0.079 Uiso 1 1 calc R . .
H30C H 0.9067 -0.0343 0.5767 0.079 Uiso 1 1 calc R . .
C31 C 0.8531(4) -0.2027(6) 0.4225(5) 0.0466(15) Uani 1 1 d . A .
H31A H 0.8053 -0.2624 0.3798 0.070 Uiso 1 1 calc R . .
H31B H 0.8866 -0.2482 0.4842 0.070 Uiso 1 1 calc R . .
H31C H 0.9030 -0.1745 0.3869 0.070 Uiso 1 1 calc R . .
O1 O 0.7668(5) -0.2306(6) 0.9470(5) 0.057(2) Uiso 0.70 1 d PD A 1
C32 C 0.7717(8) -0.1256(9) 1.0162(7) 0.063(3) Uiso 0.70 1 d PD A 1
H32A H 0.7251 -0.0540 0.9871 0.076 Uiso 0.70 1 calc PR A 1
H32C H 0.8405 -0.0898 1.0375 0.076 Uiso 0.70 1 calc PR A 1
C33 C 0.7411(8) -0.1897(11) 1.1012(8) 0.072(3) Uiso 0.70 1 d PD A 1
H33A H 0.6773 -0.1516 1.1090 0.086 Uiso 0.70 1 calc PR A 1
H33B H 0.7928 -0.1753 1.1641 0.086 Uiso 0.70 1 calc PR A 1
C34 C 0.7284(11) -0.3355(17) 1.0793(8) 0.102(5) Uiso 0.70 1 d PD A 1
H34A H 0.7897 -0.3848 1.1114 0.122 Uiso 0.70 1 calc PR A 1
H34B H 0.6710 -0.3717 1.1021 0.122 Uiso 0.70 1 calc PR A 1
C35 C 0.7094(8) -0.3391(9) 0.9684(7) 0.065(3) Uiso 0.70 1 d PD A 1
H35A H 0.7327 -0.4227 0.9454 0.078 Uiso 0.70 1 calc PR A 1
H35B H 0.6374 -0.3276 0.9364 0.078 Uiso 0.70 1 calc PR A 1
O1' O 0.7994(11) -0.2106(12) 0.9602(10) 0.041(4) Uiso 0.30 1 d PD A 2
C32' C 0.7683(18) -0.1701(19) 1.0470(14) 0.060(6) Uiso 0.30 1 d PD A 2
H32B H 0.7090 -0.1128 1.0244 0.072 Uiso 0.30 1 calc PR A 2
H32D H 0.8223 -0.1150 1.0875 0.072 Uiso 0.30 1 calc PR A 2
C33' C 0.7423(14) -0.271(2) 1.1148(15) 0.043(4) Uiso 0.30 1 d PD A 2
H33C H 0.6731 -0.2600 1.1222 0.052 Uiso 0.30 1 calc PR A 2
H33D H 0.7895 -0.2697 1.1816 0.052 Uiso 0.30 1 calc PR A 2
C34' C 0.7530(14) -0.393(2) 1.0587(12) 0.046(5) Uiso 0.30 1 d PD A 2
H34C H 0.8142 -0.4425 1.0917 0.055 Uiso 0.30 1 calc PR A 2
H34D H 0.6940 -0.4513 1.0519 0.055 Uiso 0.30 1 calc PR A 2
C35' C 0.7602(16) -0.3403(15) 0.9601(12) 0.051(5) Uiso 0.30 1 d PD A 2
H35C H 0.8028 -0.4002 0.9318 0.061 Uiso 0.30 1 calc PR A 2
H35D H 0.6925 -0.3418 0.9145 0.061 Uiso 0.30 1 calc PR A 2
C36 C 0.9246(8) -0.3175(9) 0.7147(12) 0.061(4) Uiso 0.50 1 d PD A 1
H36A H 0.8885 -0.3149 0.6432 0.073 Uiso 0.50 1 calc PR A 1
H36B H 0.8852 -0.3709 0.7514 0.073 Uiso 0.50 1 calc PR A 1
C37 C 1.0249(7) -0.3737(13) 0.7262(12) 0.077(5) Uiso 0.50 1 d PD A 1
H37A H 1.0385 -0.3880 0.6597 0.093 Uiso 0.50 1 calc PR A 1
H37B H 1.0295 -0.4592 0.7610 0.093 Uiso 0.50 1 calc PR A 1
C36' C 0.9275(7) -0.3245(7) 0.7631(11) 0.048(3) Uiso 0.50 1 d PD A 2
H36C H 0.8762 -0.3571 0.7047 0.058 Uiso 0.50 1 calc PR A 2
H36D H 0.9047 -0.3446 0.8243 0.058 Uiso 0.50 1 calc PR A 2
C37' C 1.0253(5) -0.3916(8) 0.7678(8) 0.024(2) Uiso 0.50 1 d PD A 2
H37C H 1.0245 -0.4374 0.7043 0.029 Uiso 0.50 1 calc PR A 2
H37D H 1.0411 -0.4557 0.8234 0.029 Uiso 0.50 1 calc PR A 2
C38 C 1.0991(4) -0.2803(5) 0.7854(5) 0.0587(16) Uiso 1 1 d D . .
H38A H 1.1487 -0.2544 0.7476 0.070 Uiso 1 1 calc R A 1
H38B H 1.1351 -0.3207 0.8494 0.070 Uiso 1 1 calc R A 1
C39 C 1.0403(4) -0.1641(6) 0.8041(5) 0.0522(15) Uiso 1 1 d D A .
H39A H 1.0474 -0.1523 0.8767 0.063 Uiso 1 1 calc R . .
H39B H 1.0646 -0.0837 0.7773 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0252(5) 0.0346(6) 0.0478(7) -0.0039(6) 0.0019(5) 0.0024(5)
K2 0.0280(5) 0.0306(5) 0.0333(6) 0.0047(5) 0.0115(4) 0.0028(4)
N1 0.024(2) 0.036(2) 0.038(3) -0.004(2) 0.0043(18) -0.0081(17)
N2 0.0235(18) 0.025(2) 0.028(2) -0.0018(16) 0.0045(16) -0.0021(15)
N3 0.0198(17) 0.026(2) 0.027(2) 0.0026(16) 0.0115(16) 0.0000(15)
N4 0.0247(18) 0.032(2) 0.036(2) 0.001(2) 0.0132(17) 0.0000(18)
C1 0.033(2) 0.032(3) 0.026(3) 0.001(2) 0.010(2) -0.010(2)
C2 0.029(2) 0.030(3) 0.022(3) -0.003(2) 0.012(2) -0.0058(19)
C3 0.033(2) 0.025(2) 0.030(3) 0.005(2) 0.009(2) 0.003(2)
C4 0.025(2) 0.030(3) 0.030(3) 0.002(2) 0.009(2) -0.0007(19)
C5 0.019(2) 0.030(2) 0.025(3) 0.0006(19) 0.0082(19) -0.0007(18)
C6 0.0201(19) 0.024(2) 0.025(2) 0.003(2) 0.0063(17) 0.0025(19)
C7 0.016(2) 0.033(3) 0.022(3) -0.002(2) 0.0033(18) -0.0071(18)
C8 0.030(2) 0.027(3) 0.030(3) 0.001(2) 0.012(2) -0.0019(19)
C9 0.027(2) 0.023(2) 0.036(3) -0.003(2) 0.007(2) 0.0018(19)
C10 0.019(2) 0.030(3) 0.029(3) -0.002(2) 0.0067(19) 0.0008(18)
C11 0.022(2) 0.026(3) 0.025(3) -0.002(2) 0.0059(19) 0.0041(18)
C12 0.0173(19) 0.030(3) 0.027(3) 0.0003(19) 0.0080(18) 0.0037(17)
C13 0.034(2) 0.039(3) 0.026(3) -0.002(2) 0.012(2) -0.005(2)
C14 0.045(3) 0.050(3) 0.030(3) 0.008(3) 0.009(2) 0.008(3)
C15 0.058(3) 0.045(3) 0.028(3) 0.013(3) 0.021(3) 0.011(3)
C16 0.041(3) 0.039(3) 0.049(4) 0.008(3) 0.023(3) -0.005(2)
C17 0.036(3) 0.033(3) 0.038(3) 0.001(2) 0.012(2) -0.005(2)
C18 0.025(2) 0.023(2) 0.024(3) -0.002(2) 0.0055(18) -0.0048(19)
C19 0.028(2) 0.041(3) 0.036(3) -0.004(2) 0.013(2) -0.003(2)
C20 0.022(2) 0.055(4) 0.042(3) -0.003(3) 0.009(2) -0.002(2)
C21 0.020(2) 0.045(3) 0.042(3) 0.000(3) 0.000(2) -0.002(2)
C22 0.033(2) 0.034(3) 0.031(3) 0.000(2) 0.008(2) -0.003(2)
C23 0.030(2) 0.028(3) 0.029(3) 0.000(2) 0.009(2) 0.000(2)
C24 0.029(2) 0.042(3) 0.045(4) 0.002(3) -0.002(2) -0.013(2)
C25 0.042(3) 0.045(4) 0.075(5) -0.007(3) -0.011(3) -0.011(3)
C26 0.044(3) 0.062(4) 0.033(3) 0.008(3) -0.006(3) -0.011(3)
C27 0.022(2) 0.093(5) 0.048(4) 0.011(3) 0.001(2) -0.020(3)
C28 0.025(2) 0.038(3) 0.039(3) 0.001(2) 0.015(2) 0.001(2)
C29 0.042(3) 0.076(5) 0.059(4) 0.033(4) 0.025(3) 0.007(3)
C30 0.038(3) 0.049(4) 0.079(5) -0.015(3) 0.029(3) -0.015(3)
C31 0.035(3) 0.054(4) 0.061(4) -0.002(3) 0.030(3) -0.002(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
K1 N2 2.650(4) . ?
K1 O1 2.761(7) . ?
K1 O2 2.786(4) . ?
K1 O1' 2.809(14) . ?
K1 N1 2.892(4) . ?
K1 N3 2.997(4) . ?
K1 C10 2.998(5) . ?
K1 C7 3.227(4) . ?
K1 C9 3.302(5) . ?
K1 C11 3.392(5) . ?
K1 C8 3.436(5) . ?
K1 C2 3.527(5) . ?
K2 N3 2.701(4) . ?
K2 N4 3.008(4) . ?
K2 N2 3.077(4) . ?
K2 C5 3.078(4) . ?
K2 C2 3.145(5) . ?
K2 C9 3.151(5) 2_656 ?
K2 C4 3.205(5) . ?
K2 C10 3.208(4) 2_656 ?
K2 C3 3.249(5) . ?
K2 C8 3.334(5) 2_656 ?
K2 C23 3.412(5) 2_656 ?
K2 N3 3.419(4) 2_656 ?
O2 C36' 1.410(7) . ?
O2 C39 1.419(6) . ?
O2 C36 1.430(8) . ?
N1 C1 1.300(6) . ?
N1 C24 1.489(6) . ?
N2 C2 1.373(6) . ?
N2 C5 1.375(5) . ?
N3 C7 1.380(5) . ?
N3 C10 1.380(5) . ?
N3 K2 3.419(4) 2_646 ?
N4 C11 1.284(6) . ?
N4 C28 1.492(5) . ?
C1 C2 1.450(6) . ?
C2 C3 1.394(6) . ?
C3 C4 1.407(6) . ?
C4 C5 1.406(6) . ?
C5 C6 1.523(6) . ?
C6 C12 1.554(6) . ?
C6 C18 1.556(6) . ?
C6 C7 1.557(6) . ?
C7 C8 1.392(7) . ?
C7 K2 3.487(5) 2_646 ?
C8 C9 1.409(6) . ?
C9 C10 1.420(6) . ?
C10 C11 1.444(6) . ?
C10 K2 3.208(4) 2_646 ?
C12 C17 1.385(6) . ?
C12 C13 1.398(7) . ?
C13 C14 1.395(7) . ?
C14 C15 1.394(8) . ?
C15 C16 1.366(8) . ?
C16 C17 1.401(7) . ?
C18 C23 1.380(6) . ?
C18 C19 1.403(6) . ?
C19 C20 1.389(7) . ?
C20 C21 1.389(7) . ?
C21 C22 1.390(6) . ?
C22 C23 1.381(6) . ?
C23 K2 3.412(5) 2_646 ?
C24 C26 1.516(7) . ?
C24 C27 1.536(8) . ?
C24 C25 1.548(8) . ?
C28 C29 1.518(8) . ?
C28 C31 1.530(7) . ?
C28 C30 1.543(7) . ?
O1 C32 1.425(7) . ?
O1 C35 1.431(7) . ?
C32 C33 1.490(8) . ?
C33 C34 1.518(19) . ?
C34 C35 1.488(8) . ?
O1' C32' 1.427(8) . ?
O1' C35' 1.428(8) . ?
C32' C33' 1.492(9) . ?
C33' C34' 1.49(3) . ?
C34' C35' 1.490(8) . ?
C36 C37 1.468(8) . ?
C37 C38 1.487(8) . ?
C36' C37' 1.499(7) . ?
C37' C38 1.503(7) . ?
C38 C39 1.493(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 O1 104.38(17) . . ?
N2 K1 O2 158.18(13) . . ?
O1 K1 O2 91.76(17) . . ?
N2 K1 O1' 108.4(3) . . ?
O1 K1 O1' 10.0(3) . . ?
O2 K1 O1' 85.4(3) . . ?
N2 K1 N1 61.87(11) . . ?
O1 K1 N1 107.46(16) . . ?
O2 K1 N1 99.58(12) . . ?
O1' K1 N1 101.0(3) . . ?
N2 K1 N3 61.95(10) . . ?
O1 K1 N3 118.78(17) . . ?
O2 K1 N3 122.63(12) . . ?
O1' K1 N3 128.7(3) . . ?
N1 K1 N3 113.25(11) . . ?
N2 K1 C10 88.57(12) . . ?
O1 K1 C10 114.71(17) . . ?
O2 K1 C10 98.05(12) . . ?
O1' K1 C10 123.2(3) . . ?
N1 K1 C10 133.42(13) . . ?
N3 K1 C10 26.62(10) . . ?
N2 K1 C7 57.53(11) . . ?
O1 K1 C7 94.66(17) . . ?
O2 K1 C7 136.74(12) . . ?
O1' K1 C7 104.5(3) . . ?
N1 K1 C7 118.84(11) . . ?
N3 K1 C7 25.27(10) . . ?
C10 K1 C7 41.20(11) . . ?
N2 K1 C9 97.54(11) . . ?
O1 K1 C9 89.36(17) . . ?
O2 K1 C9 97.22(12) . . ?
O1' K1 C9 97.7(3) . . ?
N1 K1 C9 155.71(12) . . ?
N3 K1 C9 42.46(10) . . ?
C10 K1 C9 25.46(12) . . ?
C7 K1 C9 40.28(11) . . ?
N2 K1 C11 101.10(11) . . ?
O1 K1 C11 130.44(16) . . ?
O2 K1 C11 78.35(11) . . ?
O1' K1 C11 135.8(3) . . ?
N1 K1 C11 122.02(12) . . ?
N3 K1 C11 44.51(9) . . ?
C10 K1 C11 25.17(10) . . ?
C7 K1 C11 65.15(11) . . ?
C9 K1 C11 45.33(11) . . ?
N2 K1 C8 79.25(11) . . ?
O1 K1 C8 79.05(17) . . ?
O2 K1 C8 118.84(12) . . ?
O1' K1 C8 88.8(3) . . ?
N1 K1 C8 141.07(11) . . ?
N3 K1 C8 40.93(11) . . ?
C10 K1 C8 40.36(12) . . ?
C7 K1 C8 23.86(11) . . ?
C9 K1 C8 24.03(11) . . ?
C11 K1 C8 64.91(11) . . ?
N2 K1 C2 19.90(11) . . ?
O1 K1 C2 112.70(16) . . ?
O2 K1 C2 138.88(12) . . ?
O1' K1 C2 113.4(3) . . ?
N1 K1 C2 42.86(10) . . ?
N3 K1 C2 74.89(10) . . ?
C10 K1 C2 100.52(12) . . ?
C7 K1 C2 75.98(11) . . ?
C9 K1 C2 114.77(11) . . ?
C11 K1 C2 105.63(11) . . ?
C8 K1 C2 98.64(11) . . ?
N3 K2 N4 58.66(10) . . ?
N3 K2 N2 60.32(10) . . ?
N4 K2 N2 95.32(10) . . ?
N3 K2 C5 57.97(11) . . ?
N4 K2 C5 109.85(12) . . ?
N2 K2 C5 25.81(10) . . ?
N3 K2 C2 85.69(12) . . ?
N4 K2 C2 109.38(12) . . ?
N2 K2 C2 25.46(11) . . ?
C5 K2 C2 41.08(12) . . ?
N3 K2 C9 111.22(12) . 2_656 ?
N4 K2 C9 120.49(12) . 2_656 ?
N2 K2 C9 132.85(11) . 2_656 ?
C5 K2 C9 107.71(12) . 2_656 ?
C2 K2 C9 129.16(12) . 2_656 ?
N3 K2 C4 82.38(11) . . ?
N4 K2 C4 135.28(12) . . ?
N2 K2 C4 42.59(11) . . ?
C5 K2 C4 25.75(11) . . ?
C2 K2 C4 41.10(11) . . ?
C9 K2 C4 92.14(12) 2_656 . ?
N3 K2 C10 124.29(11) . 2_656 ?
N4 K2 C10 145.56(12) . 2_656 ?
N2 K2 C10 116.08(10) . 2_656 ?
C5 K2 C10 95.33(11) . 2_656 ?
C2 K2 C10 105.04(12) . 2_656 ?
C9 K2 C10 25.78(12) 2_656 2_656 ?
C4 K2 C10 73.54(12) . 2_656 ?
N3 K2 C3 98.40(12) . . ?
N4 K2 C3 134.39(11) . . ?
N2 K2 C3 42.40(11) . . ?
C5 K2 C3 41.69(12) . . ?
C2 K2 C3 25.13(11) . . ?
C9 K2 C3 104.15(12) 2_656 . ?
C4 K2 C3 25.17(11) . . ?
C10 K2 C3 79.98(12) 2_656 . ?
N3 K2 C8 124.33(12) . 2_656 ?
N4 K2 C8 106.75(11) . 2_656 ?
N2 K2 C8 156.09(10) . 2_656 ?
C5 K2 C8 132.24(11) . 2_656 ?
C2 K2 C8 141.83(12) . 2_656 ?
C9 K2 C8 24.89(11) 2_656 2_656 ?
C4 K2 C8 113.55(12) . 2_656 ?
C10 K2 C8 40.31(11) 2_656 2_656 ?
C3 K2 C8 118.25(12) . 2_656 ?
N3 K2 C23 157.66(11) . 2_656 ?
N4 K2 C23 103.45(11) . 2_656 ?
N2 K2 C23 112.96(11) . 2_656 ?
C5 K2 C23 126.22(12) . 2_656 ?
C2 K2 C23 88.65(12) . 2_656 ?
C9 K2 C23 89.01(12) 2_656 2_656 ?
C4 K2 C23 107.07(12) . 2_656 ?
C10 K2 C23 78.05(11) 2_656 2_656 ?
C3 K2 C23 85.07(12) . 2_656 ?
C8 K2 C23 71.25(11) 2_656 2_656 ?
N3 K2 N3 148.03(6) . 2_656 ?
N4 K2 N3 140.80(10) . 2_656 ?
N2 K2 N3 122.23(9) . 2_656 ?
C5 K2 N3 109.14(10) . 2_656 ?
C2 K2 N3 102.39(11) . 2_656 ?
C9 K2 N3 40.70(10) 2_656 2_656 ?
C4 K2 N3 83.92(10) . 2_656 ?
C10 K2 N3 23.76(9) 2_656 2_656 ?
C3 K2 N3 80.17(10) . 2_656 ?
C8 K2 N3 39.55(10) 2_656 2_656 ?
C23 K2 N3 54.29(10) 2_656 2_656 ?
C36' O2 C39 104.2(6) . . ?
C36' O2 C36 27.0(7) . . ?
C39 O2 C36 111.6(6) . . ?
C36' O2 K1 100.0(4) . . ?
C39 O2 K1 138.6(3) . . ?
C36 O2 K1 105.3(5) . . ?
C1 N1 C24 121.2(4) . . ?
C1 N1 K1 112.7(3) . . ?
C24 N1 K1 126.0(3) . . ?
C2 N2 C5 105.3(4) . . ?
C2 N2 K1 119.0(3) . . ?
C5 N2 K1 132.1(3) . . ?
C2 N2 K2 80.0(3) . . ?
C5 N2 K2 77.2(2) . . ?
K1 N2 K2 92.82(11) . . ?
C7 N3 C10 105.8(4) . . ?
C7 N3 K2 129.4(3) . . ?
C10 N3 K2 123.6(3) . . ?
C7 N3 K1 86.7(2) . . ?
C10 N3 K1 76.7(2) . . ?
K2 N3 K1 93.59(11) . . ?
C7 N3 K2 81.2(2) . 2_646 ?
C10 N3 K2 69.5(2) . 2_646 ?
K2 N3 K2 123.87(13) . 2_646 ?
K1 N3 K2 139.23(12) . 2_646 ?
C11 N4 C28 121.4(4) . . ?
C11 N4 K2 114.8(3) . . ?
C28 N4 K2 122.1(3) . . ?
N1 C1 C2 123.1(5) . . ?
N2 C2 C3 111.9(4) . . ?
N2 C2 C1 120.2(4) . . ?
C3 C2 C1 127.9(4) . . ?
N2 C2 K2 74.5(3) . . ?
C3 C2 K2 81.6(3) . . ?
C1 C2 K2 112.8(3) . . ?
N2 C2 K1 41.1(2) . . ?
C3 C2 K1 149.3(3) . . ?
C1 C2 K1 81.1(3) . . ?
K2 C2 K1 76.87(10) . . ?
C2 C3 C4 105.5(4) . . ?
C2 C3 K2 73.3(3) . . ?
C4 C3 K2 75.7(3) . . ?
C5 C4 C3 106.7(4) . . ?
C5 C4 K2 72.1(2) . . ?
C3 C4 K2 79.2(3) . . ?
N2 C5 C4 110.5(4) . . ?
N2 C5 C6 119.7(4) . . ?
C4 C5 C6 129.7(4) . . ?
N2 C5 K2 77.0(2) . . ?
C4 C5 K2 82.2(3) . . ?
C6 C5 K2 109.5(3) . . ?
C5 C6 C12 111.3(4) . . ?
C5 C6 C18 108.4(4) . . ?
C12 C6 C18 110.2(3) . . ?
C5 C6 C7 108.9(3) . . ?
C12 C6 C7 107.7(3) . . ?
C18 C6 C7 110.4(4) . . ?
N3 C7 C8 111.1(4) . . ?
N3 C7 C6 116.5(4) . . ?
C8 C7 C6 132.3(4) . . ?
N3 C7 K1 68.0(2) . . ?
C8 C7 K1 86.5(3) . . ?
C6 C7 K1 108.9(3) . . ?
N3 C7 K2 75.7(2) . 2_646 ?
C8 C7 K2 72.1(3) . 2_646 ?
C6 C7 K2 121.3(2) . 2_646 ?
K1 C7 K2 127.23(13) . 2_646 ?
C7 C8 C9 106.8(4) . . ?
C7 C8 K1 69.7(2) . . ?
C9 C8 K1 72.7(3) . . ?
C8 C9 C10 105.9(4) . . ?
C8 C9 K1 83.3(3) . . ?
C10 C9 K1 65.2(2) . . ?
N3 C10 C9 110.4(4) . . ?
N3 C10 C11 120.1(4) . . ?
C9 C10 C11 128.6(4) . . ?
N3 C10 K1 76.6(2) . . ?
C9 C10 K1 89.3(3) . . ?
C11 C10 K1 92.9(3) . . ?
N3 C10 K2 86.7(2) . 2_646 ?
C9 C10 K2 74.9(2) . 2_646 ?
C11 C10 K2 115.5(3) . 2_646 ?
K1 C10 K2 151.58(15) . 2_646 ?
N4 C11 C10 121.0(4) . . ?
N4 C11 K1 84.9(3) . . ?
C10 C11 K1 62.0(2) . . ?
C17 C12 C13 117.7(4) . . ?
C17 C12 C6 120.4(4) . . ?
C13 C12 C6 121.9(4) . . ?
C14 C13 C12 120.8(5) . . ?
C15 C14 C13 120.6(5) . . ?
C16 C15 C14 118.7(5) . . ?
C15 C16 C17 121.1(5) . . ?
C12 C17 C16 121.1(5) . . ?
C23 C18 C19 117.3(4) . . ?
C23 C18 C6 122.2(4) . . ?
C19 C18 C6 120.5(4) . . ?
C20 C19 C18 120.8(5) . . ?
C19 C20 C21 120.9(4) . . ?
C20 C21 C22 118.4(4) . . ?
C23 C22 C21 120.2(5) . . ?
C18 C23 C22 122.4(4) . . ?
C18 C23 K2 116.4(3) . 2_646 ?
C22 C23 K2 102.3(3) . 2_646 ?
N1 C24 C26 106.5(4) . . ?
N1 C24 C27 106.6(4) . . ?
C26 C24 C27 109.4(5) . . ?
N1 C24 C25 113.8(4) . . ?
C26 C24 C25 109.0(5) . . ?
C27 C24 C25 111.3(5) . . ?
N4 C28 C29 105.5(4) . . ?
N4 C28 C31 116.2(4) . . ?
C29 C28 C31 111.0(5) . . ?
N4 C28 C30 104.9(4) . . ?
C29 C28 C30 109.8(5) . . ?
C31 C28 C30 109.1(4) . . ?
C32 O1 C35 112.4(7) . . ?
C32 O1 K1 103.5(5) . . ?
C35 O1 K1 127.9(6) . . ?
O1 C32 C33 102.8(8) . . ?
C32 C33 C34 108.3(9) . . ?
C35 C34 C33 102.2(10) . . ?
O1 C35 C34 103.0(9) . . ?
C32' O1' C35' 94.5(14) . . ?
C32' O1' K1 129.1(12) . . ?
C35' O1' K1 110.5(10) . . ?
O1' C32' C33' 119.5(16) . . ?
C32' C33' C34' 100.6(14) . . ?
C35' C34' C33' 101.9(16) . . ?
O1' C35' C34' 116.4(15) . . ?
O2 C36 C37 106.5(8) . . ?
C36 C37 C38 108.3(9) . . ?
O2 C36' C37' 109.9(7) . . ?
C36' C37' C38 103.2(6) . . ?
C37 C38 C39 105.8(6) . . ?
C37 C38 C37' 23.2(7) . . ?
C39 C38 C37' 104.6(5) . . ?
O2 C39 C38 107.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.065

data_dpyrph
_database_code_CSD               207485

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H18 N2 O2'
_chemical_formula_sum            'C23 H18 N2 O2'
_chemical_formula_weight         354.39

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, 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                   28.294(2)
_cell_length_b                   9.1628(8)
_cell_length_c                   29.053(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7532.1(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7962
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.75

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  '?  # theoretical value = 0.9532'
_exptl_absorpt_correction_T_max  '?  # theoretical value = 0.9608'
_exptl_absorpt_process_details   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            94471
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         29.18
_reflns_number_total             9821
_reflns_number_gt                7141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2001)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.067P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_atom_sites_solution_hydrogens   'geometrically placed'
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9821
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1131
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.012

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.52967(3) 0.22327(9) 0.19543(3) 0.03028(19) Uani 1 1 d . . .
O2 O 0.71463(3) 0.10267(11) 0.19587(3) 0.0400(2) Uani 1 1 d . . .
O3 O 0.60185(3) 0.48664(9) 0.24422(3) 0.0371(2) Uani 1 1 d . . .
O4 O 0.63923(3) -0.08312(10) 0.26708(3) 0.0392(2) Uani 1 1 d . . .
N1 N 0.57257(3) 0.21658(10) 0.28535(3) 0.0238(2) Uani 1 1 d . . .
H1A H 0.5862 0.2854 0.2689 0.029 Uiso 1 1 calc R . .
N2 N 0.67621(3) 0.20353(10) 0.28307(3) 0.0262(2) Uani 1 1 d . . .
H2A H 0.6602 0.1259 0.2745 0.031 Uiso 1 1 calc R . .
N3 N 0.62049(3) 0.32039(10) 0.16212(3) 0.0261(2) Uani 1 1 d . . .
H3A H 0.5951 0.2854 0.1757 0.031 Uiso 1 1 calc R . .
N4 N 0.61937(3) 0.00482(10) 0.17439(3) 0.0263(2) Uani 1 1 d . . .
H4A H 0.6447 0.0503 0.1845 0.032 Uiso 1 1 calc R . .
C1 C 0.51449(4) 0.14505(13) 0.22635(4) 0.0275(2) Uani 1 1 d . . .
H1B H 0.4873 0.0876 0.2199 0.033 Uiso 1 1 calc R . .
C2 C 0.53459(4) 0.13370(12) 0.27146(4) 0.0252(2) Uani 1 1 d . . .
C3 C 0.52391(4) 0.03860(13) 0.30687(4) 0.0300(3) Uani 1 1 d . . .
H3B H 0.4992 -0.0315 0.3070 0.036 Uiso 1 1 calc R . .
C4 C 0.55611(4) 0.06447(13) 0.34233(4) 0.0292(3) Uani 1 1 d . . .
H4B H 0.5574 0.0144 0.3709 0.035 Uiso 1 1 calc R . .
C5 C 0.58587(4) 0.17575(12) 0.32847(4) 0.0243(2) Uani 1 1 d . . .
C6 C 0.62639(4) 0.24978(12) 0.35379(4) 0.0241(2) Uani 1 1 d . . .
C7 C 0.66638(4) 0.28638(13) 0.32061(4) 0.0262(2) Uani 1 1 d . . .
C8 C 0.69951(5) 0.39789(14) 0.32225(5) 0.0361(3) Uani 1 1 d . . .
H8A H 0.7012 0.4729 0.3448 0.043 Uiso 1 1 calc R . .
C9 C 0.73004(5) 0.38024(15) 0.28484(5) 0.0382(3) Uani 1 1 d . . .
H9A H 0.7563 0.4404 0.2775 0.046 Uiso 1 1 calc R . .
C10 C 0.71504(4) 0.25920(14) 0.26043(4) 0.0309(3) Uani 1 1 d . . .
C11 C 0.73195(4) 0.20380(15) 0.21763(4) 0.0355(3) Uani 1 1 d . . .
H11A H 0.7591 0.2495 0.2049 0.043 Uiso 1 1 calc R . .
C12 C 0.64332(4) 0.14215(12) 0.39133(4) 0.0263(2) Uani 1 1 d . . .
C13 C 0.61872(5) 0.13214(13) 0.43278(4) 0.0331(3) Uani 1 1 d . . .
H13A H 0.5924 0.1944 0.4381 0.040 Uiso 1 1 calc R . .
C14 C 0.63195(5) 0.03290(14) 0.46637(4) 0.0372(3) Uani 1 1 d . . .
H14A H 0.6150 0.0282 0.4945 0.045 Uiso 1 1 calc R . .
C15 C 0.66980(5) -0.05910(14) 0.45894(5) 0.0376(3) Uani 1 1 d . . .
H15A H 0.6791 -0.1269 0.4820 0.045 Uiso 1 1 calc R . .
C16 C 0.69411(5) -0.05197(15) 0.41779(5) 0.0416(3) Uani 1 1 d . . .
H16A H 0.7199 -0.1161 0.4124 0.050 Uiso 1 1 calc R . .
C17 C 0.68108(4) 0.04835(14) 0.38431(4) 0.0333(3) Uani 1 1 d . . .
H17A H 0.6983 0.0528 0.3562 0.040 Uiso 1 1 calc R . .
C18 C 0.61006(4) 0.39504(12) 0.37605(4) 0.0251(2) Uani 1 1 d . . .
C19 C 0.63795(4) 0.45837(13) 0.41026(4) 0.0307(3) Uani 1 1 d . . .
H19A H 0.6654 0.4086 0.4208 0.037 Uiso 1 1 calc R . .
C20 C 0.62643(5) 0.59198(14) 0.42911(4) 0.0344(3) Uani 1 1 d . . .
H20A H 0.6459 0.6337 0.4522 0.041 Uiso 1 1 calc R . .
C21 C 0.58638(5) 0.66520(14) 0.41424(5) 0.0352(3) Uani 1 1 d . . .
H21A H 0.5786 0.7579 0.4268 0.042 Uiso 1 1 calc R . .
C22 C 0.55796(5) 0.60282(14) 0.38117(4) 0.0346(3) Uani 1 1 d . . .
H22A H 0.5303 0.6521 0.3712 0.042 Uiso 1 1 calc R . .
C23 C 0.56967(4) 0.46774(13) 0.36236(4) 0.0286(3) Uani 1 1 d . . .
H23A H 0.5496 0.4251 0.3398 0.034 Uiso 1 1 calc R . .
C24 C 0.63449(5) 0.51607(13) 0.21813(4) 0.0316(3) Uani 1 1 d . . .
H24A H 0.6538 0.5971 0.2260 0.038 Uiso 1 1 calc R . .
C25 C 0.64594(4) 0.43916(13) 0.17699(4) 0.0287(3) Uani 1 1 d . . .
C26 C 0.68286(5) 0.45937(14) 0.14652(4) 0.0345(3) Uani 1 1 d . . .
H26A H 0.7063 0.5336 0.1481 0.041 Uiso 1 1 calc R . .
C27 C 0.67945(4) 0.35079(14) 0.11303(4) 0.0325(3) Uani 1 1 d . . .
H27A H 0.7002 0.3379 0.0876 0.039 Uiso 1 1 calc R . .
C28 C 0.64058(4) 0.26506(12) 0.12320(4) 0.0252(2) Uani 1 1 d . . .
C29 C 0.61910(4) 0.13460(12) 0.09827(4) 0.0243(2) Uani 1 1 d . . .
C30 C 0.59817(4) 0.02923(12) 0.13300(4) 0.0251(2) Uani 1 1 d . . .
C31 C 0.55991(4) -0.06345(13) 0.12958(4) 0.0311(3) Uani 1 1 d . . .
H31A H 0.5387 -0.0702 0.1043 0.037 Uiso 1 1 calc R . .
C32 C 0.55804(4) -0.14607(13) 0.17024(4) 0.0335(3) Uani 1 1 d . . .
H32A H 0.5354 -0.2193 0.1774 0.040 Uiso 1 1 calc R . .
C33 C 0.59512(4) -0.10157(12) 0.19799(4) 0.0299(3) Uani 1 1 d . . .
C34 C 0.60754(5) -0.13980(13) 0.24460(4) 0.0336(3) Uani 1 1 d . . .
H34A H 0.5897 -0.2149 0.2590 0.040 Uiso 1 1 calc R . .
C35 C 0.57940(4) 0.18554(13) 0.06510(4) 0.0270(2) Uani 1 1 d . . .
C36 C 0.55352(4) 0.31205(14) 0.07333(5) 0.0342(3) Uani 1 1 d . . .
H36A H 0.5603 0.3701 0.0996 0.041 Uiso 1 1 calc R . .
C37 C 0.51778(5) 0.35385(16) 0.04334(5) 0.0424(3) Uani 1 1 d . . .
H37A H 0.5001 0.4399 0.0495 0.051 Uiso 1 1 calc R . .
C38 C 0.50758(5) 0.27197(16) 0.00479(5) 0.0429(3) Uani 1 1 d . . .
H38A H 0.4833 0.3017 -0.0157 0.052 Uiso 1 1 calc R . .
C39 C 0.53298(5) 0.14656(16) -0.00374(5) 0.0391(3) Uani 1 1 d . . .
H39A H 0.5263 0.0897 -0.0303 0.047 Uiso 1 1 calc R . .
C40 C 0.56838(4) 0.10327(14) 0.02640(4) 0.0320(3) Uani 1 1 d . . .
H40A H 0.5854 0.0158 0.0205 0.038 Uiso 1 1 calc R . .
C41 C 0.65827(4) 0.05626(12) 0.07031(4) 0.0243(2) Uani 1 1 d . . .
C42 C 0.67816(4) 0.12635(13) 0.03235(4) 0.0270(2) Uani 1 1 d . . .
H42A H 0.6675 0.2209 0.0239 0.032 Uiso 1 1 calc R . .
C43 C 0.71333(4) 0.05930(14) 0.00685(4) 0.0291(3) Uani 1 1 d . . .
H43A H 0.7272 0.1092 -0.0184 0.035 Uiso 1 1 calc R . .
C44 C 0.72832(4) -0.08014(14) 0.01800(4) 0.0317(3) Uani 1 1 d . . .
H44A H 0.7524 -0.1262 0.0004 0.038 Uiso 1 1 calc R . .
C45 C 0.70811(4) -0.15154(14) 0.05473(4) 0.0321(3) Uani 1 1 d . . .
H45A H 0.7179 -0.2479 0.0621 0.038 Uiso 1 1 calc R . .
C46 C 0.67345(4) -0.08345(13) 0.08106(4) 0.0289(3) Uani 1 1 d . . .
H46A H 0.6601 -0.1332 0.1066 0.035 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0287(4) 0.0313(4) 0.0308(4) -0.0033(4) -0.0008(4) 0.0029(3)
O2 0.0322(5) 0.0517(6) 0.0362(5) -0.0047(4) 0.0031(4) 0.0044(4)
O3 0.0478(5) 0.0291(5) 0.0344(5) -0.0033(4) 0.0085(4) -0.0017(4)
O4 0.0463(5) 0.0330(5) 0.0384(5) -0.0004(4) -0.0018(4) 0.0018(4)
N1 0.0235(5) 0.0240(5) 0.0238(5) -0.0018(4) 0.0004(4) -0.0011(4)
N2 0.0234(5) 0.0283(5) 0.0268(5) 0.0001(4) -0.0008(4) -0.0004(4)
N3 0.0270(5) 0.0230(5) 0.0283(5) -0.0014(4) 0.0039(4) -0.0007(4)
N4 0.0270(5) 0.0250(5) 0.0270(5) 0.0003(4) 0.0032(4) 0.0002(4)
C1 0.0223(6) 0.0277(6) 0.0326(6) -0.0084(5) 0.0004(5) 0.0010(4)
C2 0.0218(5) 0.0249(6) 0.0289(6) -0.0076(5) 0.0018(5) 0.0002(4)
C3 0.0282(6) 0.0272(6) 0.0347(7) -0.0058(5) 0.0049(5) -0.0044(5)
C4 0.0335(6) 0.0261(6) 0.0281(6) -0.0004(5) 0.0040(5) -0.0009(5)
C5 0.0253(6) 0.0234(5) 0.0244(6) -0.0027(4) 0.0010(4) 0.0018(4)
C6 0.0254(6) 0.0234(6) 0.0236(5) -0.0020(4) -0.0022(4) 0.0005(4)
C7 0.0260(6) 0.0270(6) 0.0257(6) 0.0006(5) -0.0025(5) 0.0012(5)
C8 0.0370(7) 0.0353(7) 0.0361(7) -0.0028(6) 0.0005(6) -0.0089(6)
C9 0.0317(7) 0.0429(8) 0.0398(7) 0.0031(6) 0.0022(6) -0.0094(6)
C10 0.0246(6) 0.0372(7) 0.0309(6) 0.0046(5) 0.0016(5) 0.0007(5)
C11 0.0259(6) 0.0467(8) 0.0339(7) 0.0049(6) 0.0029(5) 0.0037(5)
C12 0.0297(6) 0.0236(6) 0.0256(6) -0.0019(5) -0.0050(5) -0.0007(4)
C13 0.0404(7) 0.0292(6) 0.0296(6) 0.0003(5) 0.0015(5) 0.0028(5)
C14 0.0505(8) 0.0335(7) 0.0277(6) 0.0013(5) -0.0020(6) -0.0074(6)
C15 0.0462(8) 0.0314(7) 0.0353(7) 0.0064(6) -0.0157(6) -0.0049(6)
C16 0.0392(7) 0.0402(8) 0.0452(8) 0.0041(6) -0.0105(6) 0.0104(6)
C17 0.0331(7) 0.0370(7) 0.0300(6) 0.0012(5) -0.0037(5) 0.0048(5)
C18 0.0279(6) 0.0233(5) 0.0241(6) -0.0004(4) -0.0002(5) -0.0002(4)
C19 0.0315(6) 0.0292(6) 0.0314(6) -0.0017(5) -0.0079(5) 0.0036(5)
C20 0.0401(7) 0.0304(6) 0.0328(7) -0.0060(5) -0.0083(5) -0.0014(5)
C21 0.0416(7) 0.0255(6) 0.0386(7) -0.0063(5) -0.0024(6) 0.0044(5)
C22 0.0340(7) 0.0323(7) 0.0375(7) -0.0036(6) -0.0056(5) 0.0082(5)
C23 0.0283(6) 0.0305(6) 0.0270(6) -0.0031(5) -0.0045(5) 0.0006(5)
C24 0.0370(7) 0.0233(6) 0.0345(7) -0.0013(5) -0.0007(5) -0.0008(5)
C25 0.0314(6) 0.0235(6) 0.0313(6) -0.0010(5) -0.0017(5) -0.0004(5)
C26 0.0352(7) 0.0307(6) 0.0376(7) -0.0034(5) 0.0034(6) -0.0086(5)
C27 0.0303(6) 0.0343(7) 0.0329(7) -0.0035(5) 0.0061(5) -0.0061(5)
C28 0.0251(5) 0.0247(6) 0.0259(6) -0.0002(5) 0.0015(5) 0.0014(4)
C29 0.0233(5) 0.0247(6) 0.0248(6) -0.0007(5) 0.0019(4) -0.0006(4)
C30 0.0252(6) 0.0241(6) 0.0261(6) -0.0020(5) 0.0036(5) 0.0018(4)
C31 0.0292(6) 0.0298(6) 0.0344(7) -0.0030(5) 0.0023(5) -0.0025(5)
C32 0.0358(7) 0.0262(6) 0.0384(7) -0.0005(5) 0.0095(6) -0.0042(5)
C33 0.0349(6) 0.0226(6) 0.0324(6) 0.0006(5) 0.0095(5) 0.0021(5)
C34 0.0423(7) 0.0231(6) 0.0354(7) 0.0006(5) 0.0081(6) 0.0026(5)
C35 0.0233(6) 0.0293(6) 0.0284(6) 0.0045(5) 0.0023(5) -0.0029(5)
C36 0.0325(7) 0.0334(7) 0.0368(7) 0.0055(6) 0.0018(5) 0.0027(5)
C37 0.0349(7) 0.0397(7) 0.0525(9) 0.0162(7) 0.0000(6) 0.0062(6)
C38 0.0332(7) 0.0523(9) 0.0434(8) 0.0197(7) -0.0077(6) -0.0051(6)
C39 0.0339(7) 0.0488(8) 0.0347(7) 0.0093(6) -0.0056(6) -0.0128(6)
C40 0.0281(6) 0.0345(7) 0.0333(7) 0.0020(5) -0.0006(5) -0.0051(5)
C41 0.0211(5) 0.0281(6) 0.0238(5) -0.0038(4) -0.0011(4) -0.0004(4)
C42 0.0251(6) 0.0291(6) 0.0266(6) -0.0019(5) -0.0010(5) -0.0007(5)
C43 0.0251(6) 0.0374(7) 0.0249(6) -0.0044(5) 0.0007(5) -0.0046(5)
C44 0.0243(6) 0.0384(7) 0.0324(6) -0.0100(5) 0.0007(5) 0.0011(5)
C45 0.0304(6) 0.0293(6) 0.0364(7) -0.0042(5) -0.0024(5) 0.0044(5)
C46 0.0293(6) 0.0294(6) 0.0279(6) -0.0009(5) 0.0001(5) -0.0003(5)

_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
O1 C1 1.2269(14) . ?
O2 C11 1.2241(16) . ?
O3 C24 1.2245(15) . ?
O4 C34 1.2250(15) . ?
N1 C5 1.3604(14) . ?
N1 C2 1.3762(14) . ?
N2 C7 1.3576(15) . ?
N2 C10 1.3785(15) . ?
N3 C28 1.3633(14) . ?
N3 C25 1.3744(15) . ?
N4 C30 1.3624(14) . ?
N4 C33 1.3752(15) . ?
C1 C2 1.4325(16) . ?
C2 C3 1.3816(17) . ?
C3 C4 1.3955(17) . ?
C4 C5 1.3825(16) . ?
C5 C6 1.5218(15) . ?
C6 C7 1.5237(16) . ?
C6 C12 1.5464(16) . ?
C6 C18 1.5502(15) . ?
C7 C8 1.3874(16) . ?
C8 C9 1.3977(18) . ?
C9 C10 1.3831(18) . ?
C10 C11 1.4258(18) . ?
C12 C17 1.3863(16) . ?
C12 C13 1.3939(16) . ?
C13 C14 1.3855(18) . ?
C14 C15 1.3799(19) . ?
C15 C16 1.381(2) . ?
C16 C17 1.3881(18) . ?
C18 C23 1.3813(16) . ?
C18 C19 1.3954(16) . ?
C19 C20 1.3802(17) . ?
C20 C21 1.3858(17) . ?
C21 C22 1.3771(18) . ?
C22 C23 1.3931(17) . ?
C24 C25 1.4250(17) . ?
C25 C26 1.3819(17) . ?
C26 C27 1.3950(17) . ?
C27 C28 1.3834(16) . ?
C28 C29 1.5240(16) . ?
C29 C30 1.5168(15) . ?
C29 C41 1.5504(15) . ?
C29 C35 1.5520(16) . ?
C30 C31 1.3793(16) . ?
C31 C32 1.4038(17) . ?
C32 C33 1.3845(18) . ?
C33 C34 1.4421(18) . ?
C35 C40 1.3889(17) . ?
C35 C36 1.3918(17) . ?
C36 C37 1.3887(18) . ?
C37 C38 1.379(2) . ?
C38 C39 1.378(2) . ?
C39 C40 1.3883(18) . ?
C41 C46 1.3858(16) . ?
C41 C42 1.3948(16) . ?
C42 C43 1.3845(16) . ?
C43 C44 1.3847(18) . ?
C44 C45 1.3759(17) . ?
C45 C46 1.3917(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
C5 N1 C2 109.53(9) . . ?
C7 N2 C10 109.86(10) . . ?
C28 N3 C25 109.68(10) . . ?
C30 N4 C33 109.68(10) . . ?
O1 C1 C2 124.99(11) . . ?
N1 C2 C3 107.48(10) . . ?
N1 C2 C1 122.56(10) . . ?
C3 C2 C1 129.81(11) . . ?
C2 C3 C4 107.45(10) . . ?
C5 C4 C3 107.93(11) . . ?
N1 C5 C4 107.61(10) . . ?
N1 C5 C6 122.08(10) . . ?
C4 C5 C6 130.30(11) . . ?
C5 C6 C7 110.59(9) . . ?
C5 C6 C12 106.86(9) . . ?
C7 C6 C12 110.89(9) . . ?
C5 C6 C18 111.09(9) . . ?
C7 C6 C18 107.23(9) . . ?
C12 C6 C18 110.22(9) . . ?
N2 C7 C8 107.51(10) . . ?
N2 C7 C6 122.49(10) . . ?
C8 C7 C6 129.95(11) . . ?
C7 C8 C9 107.80(11) . . ?
C10 C9 C8 107.57(11) . . ?
N2 C10 C9 107.25(11) . . ?
N2 C10 C11 123.50(12) . . ?
C9 C10 C11 129.03(12) . . ?
O2 C11 C10 125.85(12) . . ?
C17 C12 C13 118.11(11) . . ?
C17 C12 C6 122.03(10) . . ?
C13 C12 C6 119.77(10) . . ?
C14 C13 C12 121.12(12) . . ?
C15 C14 C13 120.03(13) . . ?
C14 C15 C16 119.55(12) . . ?
C15 C16 C17 120.38(13) . . ?
C12 C17 C16 120.80(12) . . ?
C23 C18 C19 118.19(10) . . ?
C23 C18 C6 122.72(10) . . ?
C19 C18 C6 119.05(10) . . ?
C20 C19 C18 121.19(11) . . ?
C19 C20 C21 119.93(11) . . ?
C22 C21 C20 119.60(12) . . ?
C21 C22 C23 120.24(11) . . ?
C18 C23 C22 120.82(11) . . ?
O3 C24 C25 125.57(12) . . ?
N3 C25 C26 107.51(10) . . ?
N3 C25 C24 122.42(11) . . ?
C26 C25 C24 130.01(11) . . ?
C25 C26 C27 107.39(11) . . ?
C28 C27 C26 108.12(11) . . ?
N3 C28 C27 107.30(10) . . ?
N3 C28 C29 121.30(10) . . ?
C27 C28 C29 131.36(10) . . ?
C30 C29 C28 109.81(9) . . ?
C30 C29 C41 109.44(9) . . ?
C28 C29 C41 109.09(9) . . ?
C30 C29 C35 108.77(9) . . ?
C28 C29 C35 110.36(9) . . ?
C41 C29 C35 109.34(9) . . ?
N4 C30 C31 107.93(10) . . ?
N4 C30 C29 121.31(10) . . ?
C31 C30 C29 130.58(11) . . ?
C30 C31 C32 107.52(11) . . ?
C33 C32 C31 107.62(11) . . ?
N4 C33 C32 107.24(11) . . ?
N4 C33 C34 121.25(11) . . ?
C32 C33 C34 131.29(11) . . ?
O4 C34 C33 125.17(12) . . ?
C40 C35 C36 118.23(11) . . ?
C40 C35 C29 120.13(10) . . ?
C36 C35 C29 121.64(11) . . ?
C37 C36 C35 120.34(13) . . ?
C38 C37 C36 120.80(13) . . ?
C39 C38 C37 119.39(13) . . ?
C38 C39 C40 120.08(13) . . ?
C39 C40 C35 121.16(12) . . ?
C46 C41 C42 118.59(11) . . ?
C46 C41 C29 122.08(10) . . ?
C42 C41 C29 119.31(10) . . ?
C43 C42 C41 120.59(11) . . ?
C42 C43 C44 120.28(11) . . ?
C45 C44 C43 119.54(11) . . ?
C44 C45 C46 120.40(12) . . ?
C41 C46 C45 120.57(11) . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.22
_refine_diff_density_rms         0.04

data_feb2401
_database_code_CSD               207486

_audit_creation_date             2001-02-19T09:15:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            ((Ph2C(C4H2NCH2NtBu)2Li4)3).5(C5H12)
_chemical_formula_moiety         '(C93 H108 Li12 N12).5(C5 H12)'
_chemical_formula_sum            'C118 H168 Li12 N12'
_chemical_formula_weight         1837.92
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R-3c
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z+1/2'
'-x+y, -x, z'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x-y+2/3, x+1/3, -z+1/3'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x-y+1/3, x+2/3, -z+2/3'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   22.3735(5)
_cell_length_b                   22.3735(5)
_cell_length_c                   38.3087(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     16607.2(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11267
_cell_measurement_theta_min      3.705
_cell_measurement_theta_max      22.986
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5976
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION NOT APPLIED                        #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.062

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_number            20451
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         3.83
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total             2545
_reflns_number_gt                2074
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The trimeric Li complex is well defined but there are two areas of poorly
defined solvate density both of which are assumed to be pentane.
One lies across a 2-fold rotation axis and the other along a 3-fold rotation
axis, the latter being very poorly defined. solvate molecules were included
ad isootropic carbon atoms with H atoms omitted.

Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+36.3420P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2545
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.07
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.145
_refine_ls_wR_factor_gt          0.1343
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.038

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.81681(19) 0.54233(19) 0.08937(10) 0.0343(9) Uani 1 1 d . . .
Li2 Li 0.61177(19) 0.43893(19) 0.11680(10) 0.0350(9) Uani 1 1 d . . .
N1 N 0.72397(9) 0.51952(9) 0.10638(5) 0.0292(5) Uani 1 1 d . . 1
N2 N 0.83676(9) 0.48364(9) 0.12432(5) 0.0301(5) Uani 1 1 d . . 1
C1 C 0.76480(11) 0.44803(11) 0.13722(6) 0.0329(6) Uani 1 1 d . . 1
H1B H 0.765 0.433 0.1615 0.039 Uiso 1 1 calc R . 1
H1A H 0.738 0.4059 0.123 0.039 Uiso 1 1 calc R . 1
C2 C 0.72666(11) 0.48802(11) 0.13699(6) 0.0294(5) Uani 1 1 d . . 1
C3 C 0.69023(11) 0.49881(11) 0.16300(6) 0.0336(6) Uani 1 1 d . . 1
H3 H 0.6843 0.4827 0.1864 0.04 Uiso 1 1 calc R . 1
C4 C 0.66347(11) 0.53866(11) 0.14806(6) 0.0333(6) Uani 1 1 d . . 1
H4 H 0.636 0.5542 0.1595 0.04 Uiso 1 1 calc R . 1
C5 C 0.68492(11) 0.55054(11) 0.11372(6) 0.0294(5) Uani 1 1 d . . 1
C6 C 0.6667 0.58301(13) 0.0833 0.0301(7) Uani 1 2 d S . 1
C7 C 0.72847(12) 0.65414(11) 0.07372(6) 0.0333(6) Uani 1 1 d . A 1
C8 C 0.72194(14) 0.69418(12) 0.04784(7) 0.0493(7) Uani 1 1 d . A 1
H8 H 0.6788 0.6776 0.0365 0.059 Uiso 1 1 calc R A 1
C9 C 0.77693(15) 0.75748(14) 0.03834(8) 0.0615(9) Uani 1 1 d . A 1
H9 H 0.7713 0.7837 0.0205 0.074 Uiso 1 1 calc R A 1
C10 C 0.83986(15) 0.78275(14) 0.05465(8) 0.0562(8) Uani 1 1 d . A 1
H10 H 0.8779 0.8258 0.0478 0.067 Uiso 1 1 calc R A 1
C11 C 0.84710(13) 0.74508(13) 0.08089(7) 0.0457(7) Uani 1 1 d . A 1
H11 H 0.8901 0.7627 0.0926 0.055 Uiso 1 1 calc R A 1
C12 C 0.79189(11) 0.68125(11) 0.09043(6) 0.0360(6) Uani 1 1 d . A 1
H12 H 0.7976 0.6558 0.1087 0.043 Uiso 1 1 calc R A 1
C13 C 0.88766(11) 0.53465(12) 0.14912(6) 0.0331(6) Uani 1 1 d . B 1
C14 C 0.88490(13) 0.60195(12) 0.15034(7) 0.0426(6) Uani 1 1 d . B 1
H14C H 0.8895 0.6202 0.1266 0.064 Uiso 1 1 calc R B 1
H14B H 0.9228 0.6359 0.1649 0.064 Uiso 1 1 calc R B 1
H14A H 0.8407 0.5926 0.1603 0.064 Uiso 1 1 calc R B 1
C15 C 0.95857(13) 0.55165(14) 0.13534(8) 0.0515(7) Uani 1 1 d . B 1
H15C H 0.9642 0.569 0.1114 0.077 Uiso 1 1 calc R B 1
H15B H 0.9624 0.5099 0.1356 0.077 Uiso 1 1 calc R B 1
H15A H 0.9946 0.587 0.1502 0.077 Uiso 1 1 calc R B 1
C16 C 0.88025(15) 0.50699(13) 0.18647(7) 0.0482(7) Uani 1 1 d . B 1
H16C H 0.8349 0.4954 0.1957 0.072 Uiso 1 1 calc R B 1
H16B H 0.9164 0.5423 0.2012 0.072 Uiso 1 1 calc R B 1
H16A H 0.8847 0.4656 0.1863 0.072 Uiso 1 1 calc R B 1
C17 C 0.2228(8) 0.3333 0.0833 0.274(7) Uiso 1 2 d S . 1
C18 C 0.2122(6) 0.2634(6) 0.0785(3) 0.126(4) Uiso 0.5 1 d P . 1
C18A C 0.1954(14) 0.2829(14) 0.0592(7) 0.261(10) Uiso 0.5 1 d P . 1
C19 C 0.1482(5) 0.2076(5) 0.0591(2) 0.212(3) Uiso 1 1 d . . 1
C20 C 1 1 0.1016(8) 0.319(11) Uiso 1 3 d S . 1
C21 C 0.950(2) 0.985(3) 0.0718(12) 0.32(2) Uiso 0.33 1 d P . 1
C22 C 1 1 0.0352(5) 0.193(5) Uiso 1 3 d S . 1
C23 C 1.037(3) 1.0521(17) 0.0091(10) 0.279(19) Uiso 0.33 1 d P . 1
M1 C 0.6978 0.5191 0.1336 0.01 Uiso 0 1 d P . 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Li1 0.033(2) 0.035(2) 0.035(2) 0.0004(17) 0.0014(16) 0.0167(17)
Li2 0.033(2) 0.033(2) 0.037(2) -0.0003(17) 0.0005(16) 0.0147(17)
N1 0.0295(10) 0.0273(10) 0.0314(11) -0.0003(8) -0.0018(8) 0.0146(8)
N2 0.0277(10) 0.0310(10) 0.0309(10) -0.0040(8) -0.0043(8) 0.0141(8)
C1 0.0325(13) 0.0310(12) 0.0348(13) 0.0014(10) -0.0040(10) 0.0156(10)
C2 0.0260(11) 0.0269(12) 0.0325(13) -0.0011(10) -0.0039(10) 0.0112(10)
C3 0.0340(13) 0.0356(13) 0.0279(13) -0.0015(10) -0.0014(10) 0.0149(11)
C4 0.0307(12) 0.0331(13) 0.0369(14) -0.0060(10) 0.0001(10) 0.0164(10)
C5 0.0256(12) 0.0262(12) 0.0358(13) -0.0041(10) -0.0032(10) 0.0125(10)
C6 0.0291(17) 0.0267(12) 0.0354(18) -0.0013(7) -0.0027(14) 0.0145(8)
C7 0.0330(13) 0.0274(12) 0.0402(14) -0.0023(10) -0.0027(10) 0.0156(10)
C8 0.0436(15) 0.0326(14) 0.0635(18) 0.0052(13) -0.0161(13) 0.0128(12)
C9 0.0621(19) 0.0348(15) 0.069(2) 0.0130(14) -0.0156(16) 0.0101(14)
C10 0.0496(17) 0.0336(14) 0.0647(19) 0.0059(13) 0.0007(14) 0.0052(13)
C11 0.0335(14) 0.0376(14) 0.0577(17) -0.0084(13) -0.0046(12) 0.0115(12)
C12 0.0344(13) 0.0312(13) 0.0414(14) -0.0052(11) -0.0042(11) 0.0156(11)
C13 0.0329(13) 0.0340(13) 0.0332(13) -0.0045(10) -0.0061(10) 0.0173(11)
C14 0.0429(15) 0.0348(13) 0.0470(16) -0.0082(11) -0.0111(12) 0.0171(12)
C15 0.0342(14) 0.0532(17) 0.0618(18) -0.0182(14) -0.0092(12) 0.0179(13)
C16 0.0608(17) 0.0433(15) 0.0399(15) -0.0082(12) -0.0170(13) 0.0255(14)

#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N1 1.985(4) . ?
Li1 N2 2.002(4) 15_544 ?
Li1 N2 2.074(4) . ?
Li1 Li1 2.327(7) 15_544 ?
Li1 Li2 2.387(5) 17_654 ?
Li2 M1 1.971(4) . ?
Li2 N2 2.056(4) 2_655 ?
Li2 C5 2.200(4) . ?
Li2 N1 2.234(4) 17_654 ?
Li2 C4 2.274(4) . ?
Li2 N1 2.277(4) . ?
Li2 C2 2.364(4) . ?
Li2 C3 2.378(4) . ?
N1 C2 1.385(3) . ?
N1 C5 1.389(3) . ?
N1 Li2 2.234(4) 17_654 ?
N2 C1 1.479(3) . ?
N2 C13 1.484(3) . ?
N2 Li1 2.002(4) 15_544 ?
N2 Li2 2.056(4) 4_665 ?
C1 C2 1.514(3) . ?
C2 C3 1.383(3) . ?
C3 C4 1.419(3) . ?
C4 C5 1.380(3) . ?
C5 C6 1.532(3) . ?
C6 C5 1.532(3) 17_654 ?
C6 C7 1.543(3) . ?
C6 C7 1.543(3) 17_654 ?
C7 C12 1.389(3) . ?
C7 C8 1.392(3) . ?
C8 C9 1.382(4) . ?
C9 C10 1.377(4) . ?
C10 C11 1.372(4) . ?
C11 C12 1.391(3) . ?
C13 C15 1.529(3) . ?
C13 C16 1.535(3) . ?
C13 C14 1.538(3) . ?
C17 C18A 1.35(3) . ?
C17 C18A 1.35(3) 18_554 ?
C17 C18 1.472(13) . ?
C17 C18 1.472(13) 18_554 ?
C18 C18A 1.02(3) . ?
C18 C19 1.541(14) . ?
C18A C19 1.47(2) . ?
C20 C21 1.51(4) 2_765 ?
C20 C21 1.51(4) . ?
C20 C21 1.51(4) 4_675 ?
C21 C22 1.72(4) . ?
C21 C21 1.73(7) 4_675 ?
C21 C21 1.73(7) 2_765 ?
C22 C23 1.45(4) . ?
C22 C23 1.45(4) 4_675 ?
C22 C23 1.45(4) 2_765 ?
C22 C21 1.72(4) 4_675 ?
C22 C21 1.72(4) 2_765 ?
C22 C23 1.99(4) 19_775 ?
C22 C23 1.99(4) 20_565 ?
C22 C23 1.99(4) 22_655 ?
C23 C23 1.25(4) 20_565 ?
C23 C23 1.25(4) 22_655 ?
C23 C23 1.80(5) 4_675 ?
C23 C23 1.80(5) 2_765 ?
C23 C22 1.99(4) 19_775 ?

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 Li1 N2 114.39(19) . 15_544 ?
N1 Li1 N2 98.87(17) . . ?
N2 Li1 N2 104.94(18) 15_544 . ?
N1 Li1 Li1 137.33(13) . 15_544 ?
N2 Li1 Li1 56.65(16) 15_544 15_544 ?
N2 Li1 Li1 53.73(15) . 15_544 ?
N1 Li1 Li2 60.63(14) . 17_654 ?
N2 Li1 Li2 55.04(14) 15_544 17_654 ?
N2 Li1 Li2 123.18(19) . 17_654 ?
Li1 Li1 Li2 104.2(2) 15_544 17_654 ?
M1 Li2 N2 152.8(2) . 2_655 ?
M1 Li2 C5 31.91(8) . . ?
N2 Li2 C5 154.6(2) 2_655 . ?
M1 Li2 N1 103.37(16) . 17_654 ?
N2 Li2 N1 102.64(17) 2_655 17_654 ?
C5 Li2 N1 76.96(14) . 17_654 ?
M1 Li2 C4 31.66(8) . . ?
N2 Li2 C4 128.6(2) 2_655 . ?
C5 Li2 C4 35.88(10) . . ?
N1 Li2 C4 109.96(17) 17_654 . ?
M1 Li2 N1 31.61(7) . . ?
N2 Li2 N1 169.3(2) 2_655 . ?
C5 Li2 N1 36.10(9) . . ?
N1 Li2 N1 77.93(14) 17_654 . ?
C4 Li2 N1 59.79(12) . . ?
M1 Li2 C2 29.51(7) . . ?
N2 Li2 C2 140.2(2) 2_655 . ?
C5 Li2 C2 58.08(12) . . ?
N1 Li2 C2 110.86(16) 17_654 . ?
C4 Li2 C2 58.02(12) . . ?
N1 Li2 C2 34.66(9) . . ?
M1 Li2 C3 30.02(8) . . ?
N2 Li2 C3 123.44(19) 2_655 . ?
C5 Li2 C3 58.66(12) . . ?
N1 Li2 C3 133.38(18) 17_654 . ?
C4 Li2 C3 35.44(10) . . ?
N1 Li2 C3 58.23(11) . . ?
C2 Li2 C3 33.90(9) . . ?
C2 N1 C5 106.32(17) . . ?
C2 N1 Li1 95.89(16) . . ?
C5 N1 Li1 140.96(18) . . ?
C2 N1 Li2 133.72(17) . 17_654 ?
C5 N1 Li2 112.62(16) . 17_654 ?
Li1 N1 Li2 68.62(15) . 17_654 ?
C2 N1 Li2 76.10(15) . . ?
C5 N1 Li2 68.93(15) . . ?
Li1 N1 Li2 149.17(16) . . ?
Li2 N1 Li2 95.22(15) 17_654 . ?
C1 N2 C13 114.22(17) . . ?
C1 N2 Li1 131.07(18) . 15_544 ?
C13 N2 Li1 114.23(17) . 15_544 ?
C1 N2 Li2 88.11(16) . 4_665 ?
C13 N2 Li2 121.99(17) . 4_665 ?
Li1 N2 Li2 72.04(16) 15_544 4_665 ?
C1 N2 Li1 92.07(16) . . ?
C13 N2 Li1 104.57(16) . . ?
Li1 N2 Li1 69.62(18) 15_544 . ?
Li2 N2 Li1 128.54(17) 4_665 . ?
N2 C1 C2 117.57(18) . . ?
C3 C2 N1 109.99(19) . . ?
C3 C2 C1 130.9(2) . . ?
N1 C2 C1 119.12(19) . . ?
C3 C2 Li2 73.62(16) . . ?
N1 C2 Li2 69.25(14) . . ?
C1 C2 Li2 122.05(17) . . ?
C2 C3 C4 106.8(2) . . ?
C2 C3 Li2 72.48(15) . . ?
C4 C3 Li2 68.25(15) . . ?
C5 C4 C3 106.86(19) . . ?
C5 C4 Li2 69.16(16) . . ?
C3 C4 Li2 76.31(16) . . ?
C4 C5 N1 109.99(19) . . ?
C4 C5 C6 131.79(19) . . ?
N1 C5 C6 117.79(18) . . ?
C4 C5 Li2 74.97(16) . . ?
N1 C5 Li2 74.97(15) . . ?
C6 C5 Li2 110.83(16) . . ?
C5 C6 C5 105.2(2) 17_654 . ?
C5 C6 C7 110.62(12) 17_654 . ?
C5 C6 C7 110.90(11) . . ?
C5 C6 C7 110.90(11) 17_654 17_654 ?
C5 C6 C7 110.62(12) . 17_654 ?
C7 C6 C7 108.6(2) . 17_654 ?
C12 C7 C8 117.4(2) . . ?
C12 C7 C6 122.22(19) . . ?
C8 C7 C6 120.38(19) . . ?
C9 C8 C7 121.4(2) . . ?
C10 C9 C8 120.3(3) . . ?
C11 C10 C9 119.4(2) . . ?
C10 C11 C12 120.4(2) . . ?
C7 C12 C11 121.1(2) . . ?
N2 C13 C15 105.79(18) . . ?
N2 C13 C16 113.59(19) . . ?
C15 C13 C16 108.2(2) . . ?
N2 C13 C14 112.42(18) . . ?
C15 C13 C14 108.2(2) . . ?
C16 C13 C14 108.5(2) . . ?
C18A C17 C18A 176(3) . 18_554 ?
C18A C17 C18 42.2(11) . . ?
C18A C17 C18 140.1(15) 18_554 . ?
C18A C17 C18 140.1(15) . 18_554 ?
C18A C17 C18 42.2(11) 18_554 18_554 ?
C18 C17 C18 136.5(17) . 18_554 ?
C18A C18 C17 62.4(18) . . ?
C18A C18 C19 66.7(17) . . ?
C17 C18 C19 120.8(11) . . ?
C18 C18A C17 75(2) . . ?
C18 C18A C19 73.8(19) . . ?
C17 C18A C19 136(2) . . ?
C18A C19 C18 39.5(10) . . ?
C21 C20 C21 69(3) 2_765 . ?
C21 C20 C21 69(3) 2_765 4_675 ?
C21 C20 C21 69(3) . 4_675 ?
C20 C21 C22 103(3) . . ?
C20 C21 C21 55.3(13) . 4_675 ?
C22 C21 C21 59.9(12) . 4_675 ?
C20 C21 C21 55.3(13) . 2_765 ?
C22 C21 C21 59.9(12) . 2_765 ?
C21 C21 C21 60.000(13) 4_675 2_765 ?
C23 C22 C23 77(2) . 4_675 ?
C23 C22 C23 77(2) . 2_765 ?
C23 C22 C23 77(2) 4_675 2_765 ?
C23 C22 C21 98.5(19) . 4_675 ?
C23 C22 C21 142(3) 4_675 4_675 ?
C23 C22 C21 140(3) 2_765 4_675 ?
C23 C22 C21 140(3) . 2_765 ?
C23 C22 C21 98.5(19) 4_675 2_765 ?
C23 C22 C21 142(3) 2_765 2_765 ?
C21 C22 C21 60(2) 4_675 2_765 ?
C23 C22 C21 142(3) . . ?
C23 C22 C21 140(3) 4_675 . ?
C23 C22 C21 98.5(19) 2_765 . ?
C21 C22 C21 60(2) 4_675 . ?
C21 C22 C21 60(2) 2_765 . ?
C23 C22 C23 78(2) . 19_775 ?
C23 C22 C23 38.8(9) 4_675 19_775 ?
C23 C22 C23 38.8(9) 2_765 19_775 ?
C21 C22 C23 176(2) 4_675 19_775 ?
C21 C22 C23 123(2) 2_765 19_775 ?
C21 C22 C23 122(2) . 19_775 ?
C23 C22 C23 38.8(9) . 20_565 ?
C23 C22 C23 38.8(9) 4_675 20_565 ?
C23 C22 C23 78(2) 2_765 20_565 ?
C21 C22 C23 123(2) 4_675 20_565 ?
C21 C22 C23 122(2) 2_765 20_565 ?
C21 C22 C23 176(2) . 20_565 ?
C23 C22 C23 54(2) 19_775 20_565 ?
C23 C22 C23 38.8(9) . 22_655 ?
C23 C22 C23 78(2) 4_675 22_655 ?
C23 C22 C23 38.8(9) 2_765 22_655 ?
C21 C22 C23 122(2) 4_675 22_655 ?
C21 C22 C23 176(2) 2_765 22_655 ?
C21 C22 C23 123(2) . 22_655 ?
C23 C22 C23 54(2) 19_775 22_655 ?
C23 C22 C23 54(2) 20_565 22_655 ?
C23 C23 C23 92(5) 20_565 22_655 ?
C23 C23 C22 95(2) 20_565 . ?
C23 C23 C22 95(2) 22_655 . ?
C23 C23 C23 44(2) 20_565 4_675 ?
C23 C23 C23 90.000(9) 22_655 4_675 ?
C22 C23 C23 51.4(10) . 4_675 ?
C23 C23 C23 90.000(19) 20_565 2_765 ?
C23 C23 C23 44(2) 22_655 2_765 ?
C22 C23 C23 51.4(10) . 2_765 ?
C23 C23 C23 60.000(6) 4_675 2_765 ?
C23 C23 C22 46(3) 20_565 19_775 ?
C23 C23 C22 46(3) 22_655 19_775 ?
C22 C23 C22 102(2) . 19_775 ?
C23 C23 C22 63.1(10) 4_675 19_775 ?
C23 C23 C22 63.1(10) 2_765 19_775 ?