# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Philip Patrick Power'
'Marcin Brynda'
'Anne F. Richards'

_publ_contact_author_name        'Prof Philip Patrick Power'
_publ_contact_author_address     
;
Chemistry
University of California, Davis
One Shields Avenue
Davis
CA
95616
UNITED STATES OF AMERICA
;

_publ_contact_author_email       PPPOWER@UCDAVIS.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Bonding in Isomers of Li2ArGeGeAr (Ar = Terphenyl):
A Doubly Reduced Digermyne or a Dilithium Salt of a Digermene?
;

data_test4
_database_code_depnum_ccdc_archive 'CCDC 230338'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (Jeff*GeLi(OEt2)diox)2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H88 Ge2 Li2 O5'
_chemical_formula_weight         1096.40

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'
Ge Ge 0.1547 1.8001 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2 / c'

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

_cell_length_a                   22.2752(15)
_cell_length_b                   11.5462(8)
_cell_length_c                   23.4339(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.2720(10)
_cell_angle_gamma                90.00
_cell_volume                     5964.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    875
_cell_measurement_theta_min      4.583
_cell_measurement_theta_max      59.509

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2328
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8248
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_process_details   'not applied'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         '50 frames remeasured'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  
;
frames measured at beginning and end of data collection
;
_diffrn_standards_decay_%        <0.1
_diffrn_reflns_number            32323
_diffrn_reflns_av_R_equivalents  0.1150
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6847
_reflns_number_gt                4206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART 5.054 (Bruker 2001)'
_computing_cell_refinement       'Bruker SAINT 6.35A (Bruker 2002)'
_computing_data_reduction        'Bruker SAINT 6.35A (Bruker 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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. A small peak of 1.5 e-A**-3
is unassigned within the diethyl ether,however does not show up on the
difference map and is beleived to be slight disorder within the diethyl
ether.This has no effect on the overall structure.
;

_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^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00044(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6847
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_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
Li1 Li 0.2323(3) 0.5066(5) 0.0725(3) 0.0255(13) Uani 1 1 d . . .
Ge1 Ge 0.247107(15) 0.29634(3) 0.043629(15) 0.01780(12) Uani 1 1 d . . .
O1 O 0.21859(10) 0.5741(2) 0.14491(10) 0.0249(5) Uani 1 1 d . . .
O2 O 0.23332(10) 0.64860(19) 0.02801(9) 0.0215(5) Uani 1 1 d . . .
C1 C 0.25216(14) 0.1591(3) 0.09690(13) 0.0159(7) Uani 1 1 d . . .
C2 C 0.19956(14) 0.1003(3) 0.10920(13) 0.0180(7) Uani 1 1 d . . .
C3 C 0.20436(14) 0.0004(3) 0.14357(14) 0.0214(7) Uani 1 1 d . . .
H3A H 0.1685 -0.0386 0.1505 0.026 Uiso 1 1 calc R . .
C4 C 0.26033(15) -0.0423(3) 0.16765(14) 0.0211(7) Uani 1 1 d . . .
H4A H 0.2632 -0.1118 0.1896 0.025 Uiso 1 1 calc R . .
C5 C 0.31223(14) 0.0180(3) 0.15917(14) 0.0212(7) Uani 1 1 d . . .
H5A H 0.3508 -0.0089 0.1768 0.025 Uiso 1 1 calc R . .
C6 C 0.30878(14) 0.1174(3) 0.12522(14) 0.0192(7) Uani 1 1 d . . .
C7 C 0.36611(14) 0.1869(3) 0.12542(14) 0.0206(7) Uani 1 1 d . . .
C8 C 0.40892(15) 0.1610(3) 0.08899(15) 0.0220(7) Uani 1 1 d . . .
C9 C 0.46291(14) 0.2240(3) 0.09408(15) 0.0254(8) Uani 1 1 d . . .
H9A H 0.4914 0.2069 0.0688 0.031 Uiso 1 1 calc R . .
C10 C 0.47626(15) 0.3107(3) 0.13473(16) 0.0279(8) Uani 1 1 d . . .
C11 C 0.43326(15) 0.3355(3) 0.17058(16) 0.0274(8) Uani 1 1 d . . .
H11A H 0.4412 0.3955 0.1984 0.033 Uiso 1 1 calc R . .
C12 C 0.37880(15) 0.2745(3) 0.16668(14) 0.0223(8) Uani 1 1 d . . .
C13 C 0.39680(15) 0.0709(3) 0.04240(16) 0.0292(9) Uani 1 1 d . . .
H13A H 0.3797 0.0015 0.0580 0.044 Uiso 1 1 calc R . .
H13B H 0.4349 0.0508 0.0284 0.044 Uiso 1 1 calc R . .
H13C H 0.3680 0.1016 0.0104 0.044 Uiso 1 1 calc R . .
C14 C 0.53515(15) 0.3777(4) 0.13990(18) 0.0381(10) Uani 1 1 d . . .
H14A H 0.5551 0.3756 0.1800 0.057 Uiso 1 1 calc R . .
H14B H 0.5267 0.4583 0.1282 0.057 Uiso 1 1 calc R . .
H14C H 0.5618 0.3427 0.1148 0.057 Uiso 1 1 calc R . .
C15 C 0.33369(16) 0.3039(3) 0.20680(15) 0.0298(8) Uani 1 1 d . . .
H15A H 0.3217 0.2330 0.2252 0.045 Uiso 1 1 calc R . .
H15B H 0.2978 0.3399 0.1848 0.045 Uiso 1 1 calc R . .
H15C H 0.3523 0.3580 0.2364 0.045 Uiso 1 1 calc R . .
C16 C 0.13688(14) 0.1489(3) 0.09206(14) 0.0196(7) Uani 1 1 d . . .
C17 C 0.09727(15) 0.1074(3) 0.04477(15) 0.0230(8) Uani 1 1 d . . .
C18 C 0.03749(15) 0.1467(3) 0.03554(16) 0.0260(8) Uani 1 1 d . . .
H18A H 0.0109 0.1184 0.0032 0.031 Uiso 1 1 calc R . .
C19 C 0.01558(15) 0.2254(3) 0.07173(17) 0.0300(9) Uani 1 1 d . . .
C20 C 0.05551(15) 0.2677(3) 0.11799(16) 0.0263(8) Uani 1 1 d . . .
H20A H 0.0416 0.3235 0.1429 0.032 Uiso 1 1 calc R . .
C21 C 0.11558(15) 0.2303(3) 0.12874(14) 0.0213(8) Uani 1 1 d . . .
C22 C 0.11815(15) 0.0226(3) 0.00291(16) 0.0284(8) Uani 1 1 d . . .
H22A H 0.0858 0.0110 -0.0296 0.043 Uiso 1 1 calc R . .
H22B H 0.1280 -0.0515 0.0224 0.043 Uiso 1 1 calc R . .
H22C H 0.1543 0.0532 -0.0113 0.043 Uiso 1 1 calc R . .
C23 C -0.04995(17) 0.2646(4) 0.0619(2) 0.0445(11) Uani 1 1 d . . .
H23A H -0.0604 0.2917 0.0221 0.067 Uiso 1 1 calc R . .
H23B H -0.0556 0.3278 0.0885 0.067 Uiso 1 1 calc R . .
H23C H -0.0763 0.1995 0.0686 0.067 Uiso 1 1 calc R . .
C24 C 0.15721(16) 0.2788(3) 0.17951(15) 0.0309(9) Uani 1 1 d . . .
H24A H 0.1779 0.2150 0.2020 0.046 Uiso 1 1 calc R . .
H24B H 0.1334 0.3235 0.2039 0.046 Uiso 1 1 calc R . .
H24C H 0.1874 0.3293 0.1657 0.046 Uiso 1 1 calc R . .
C25 C 0.11308(16) 0.5585(4) 0.11059(17) 0.0359(9) Uani 1 1 d . . .
H25A H 0.0725 0.5636 0.1219 0.054 Uiso 1 1 calc R . .
H25B H 0.1207 0.4788 0.0992 0.054 Uiso 1 1 calc R . .
H25C H 0.1157 0.6107 0.0781 0.054 Uiso 1 1 calc R . .
C26 C 0.15964(16) 0.5928(3) 0.16061(16) 0.0306(9) Uani 1 1 d . . .
H26A H 0.1546 0.6754 0.1702 0.037 Uiso 1 1 calc R . .
H26B H 0.1546 0.5457 0.1949 0.037 Uiso 1 1 calc R . .
C27 C 0.26642(16) 0.6026(3) 0.19035(15) 0.0315(9) Uani 1 1 d . . .
H27A H 0.2680 0.5449 0.2218 0.038 Uiso 1 1 calc R . .
H27B H 0.2590 0.6798 0.2063 0.038 Uiso 1 1 calc R . .
C28 C 0.32580(17) 0.6030(4) 0.16595(18) 0.0394(10) Uani 1 1 d . . .
H28A H 0.3594 0.6169 0.1971 0.059 Uiso 1 1 calc R . .
H28B H 0.3250 0.6643 0.1370 0.059 Uiso 1 1 calc R . .
H28C H 0.3315 0.5278 0.1480 0.059 Uiso 1 1 calc R . .
C29 C 0.21938(16) 0.7623(3) 0.04745(15) 0.0235(8) Uani 1 1 d . . .
H29A H 0.2194 0.7610 0.0897 0.028 Uiso 1 1 calc R . .
H29B H 0.1783 0.7853 0.0290 0.028 Uiso 1 1 calc R . .
C30 C 0.26520(16) 0.8499(3) 0.03282(13) 0.0222(7) Uani 1 1 d . . .
H30A H 0.2543 0.9277 0.0457 0.027 Uiso 1 1 calc R . .
H30B H 0.3059 0.8299 0.0533 0.027 Uiso 1 1 calc R . .
O3 O 0.0125(2) 0.3555(4) 0.2493(3) 0.0334(14) Uiso 0.50 1 d P A -1
C31 C 0.0120(5) 0.1523(7) 0.2517(7) 0.059(3) Uiso 0.50 1 d P A -1
H31A H -0.0118 0.0821 0.2412 0.089 Uiso 0.50 1 calc PR A -1
H31B H 0.0236 0.1550 0.2937 0.089 Uiso 0.50 1 calc PR A -1
H31C H 0.0486 0.1515 0.2330 0.089 Uiso 0.50 1 calc PR A -1
C32 C -0.0261(4) 0.2587(8) 0.2319(4) 0.047(2) Uiso 0.50 1 d P A -1
H32A H -0.0380 0.2580 0.1896 0.056 Uiso 0.50 1 calc PR A -1
H32B H -0.0632 0.2615 0.2506 0.056 Uiso 0.50 1 calc PR A -1
C33 C -0.0241(4) 0.4582(8) 0.2328(4) 0.044(2) Uiso 0.50 1 d P A -1
H33A H -0.0606 0.4598 0.2524 0.053 Uiso 0.50 1 calc PR A -1
H33B H -0.0369 0.4606 0.1905 0.053 Uiso 0.50 1 calc PR A -1
C34 C 0.0194(3) 0.5618(6) 0.2530(4) 0.0320(19) Uiso 0.50 1 d P A -1
H34A H -0.0018 0.6351 0.2432 0.048 Uiso 0.50 1 calc PR A -1
H34B H 0.0555 0.5576 0.2336 0.048 Uiso 0.50 1 calc PR A -1
H34C H 0.0316 0.5574 0.2948 0.048 Uiso 0.50 1 calc PR A -1

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 0.035(3) 0.016(3) 0.025(3) 0.001(2) 0.002(3) -0.003(3)
Ge1 0.02125(19) 0.01482(17) 0.01691(18) 0.00124(16) 0.00136(12) 0.00025(16)
O1 0.0275(13) 0.0279(14) 0.0197(13) -0.0015(10) 0.0049(10) 0.0009(11)
O2 0.0319(14) 0.0163(12) 0.0174(12) 0.0001(10) 0.0067(10) 0.0003(10)
C1 0.0207(16) 0.0136(15) 0.0134(16) -0.0052(12) 0.0023(13) 0.0016(13)
C2 0.0179(16) 0.0208(17) 0.0146(16) -0.0032(14) -0.0003(13) -0.0040(13)
C3 0.0220(17) 0.0208(18) 0.0220(19) 0.0003(14) 0.0052(14) -0.0044(14)
C4 0.0278(19) 0.0167(17) 0.0186(18) 0.0036(14) 0.0031(14) 0.0004(14)
C5 0.0177(16) 0.0238(18) 0.0199(18) -0.0012(14) -0.0055(13) -0.0010(14)
C6 0.0213(17) 0.0181(17) 0.0180(17) -0.0003(14) 0.0027(13) 0.0001(14)
C7 0.0186(16) 0.0202(18) 0.0219(17) 0.0056(14) -0.0008(13) 0.0012(14)
C8 0.0203(17) 0.0206(17) 0.0230(18) 0.0058(14) -0.0046(14) 0.0048(14)
C9 0.0175(17) 0.028(2) 0.0297(19) 0.0077(16) 0.0000(14) 0.0021(14)
C10 0.0211(17) 0.029(2) 0.031(2) 0.0071(17) -0.0035(15) -0.0030(16)
C11 0.0273(19) 0.0241(19) 0.028(2) 0.0042(16) -0.0059(15) -0.0049(15)
C12 0.0220(17) 0.021(2) 0.0217(18) 0.0065(14) -0.0027(13) -0.0009(14)
C13 0.0230(19) 0.032(2) 0.033(2) 0.0012(17) 0.0027(16) 0.0065(16)
C14 0.0198(19) 0.049(3) 0.044(3) 0.005(2) -0.0005(17) -0.0077(18)
C15 0.035(2) 0.031(2) 0.0224(19) -0.0071(17) 0.0017(15) -0.0095(18)
C16 0.0218(17) 0.0162(17) 0.0214(18) 0.0054(14) 0.0048(14) -0.0025(14)
C17 0.0228(18) 0.0180(18) 0.028(2) 0.0047(15) 0.0021(15) -0.0028(14)
C18 0.0203(18) 0.0187(18) 0.036(2) 0.0047(16) -0.0049(15) -0.0041(14)
C19 0.0206(18) 0.021(2) 0.048(2) 0.0107(17) 0.0009(16) 0.0009(14)
C20 0.0253(19) 0.022(2) 0.033(2) 0.0025(15) 0.0086(15) 0.0034(14)
C21 0.0219(17) 0.022(2) 0.0214(18) 0.0056(14) 0.0060(14) -0.0010(13)
C22 0.0212(18) 0.028(2) 0.034(2) -0.0017(17) -0.0041(15) -0.0034(15)
C23 0.026(2) 0.031(2) 0.072(3) -0.004(2) -0.007(2) 0.0058(17)
C24 0.030(2) 0.034(2) 0.027(2) -0.0042(17) 0.0009(15) 0.0077(17)
C25 0.028(2) 0.037(2) 0.044(3) 0.0039(19) 0.0067(18) -0.0009(17)
C26 0.032(2) 0.033(2) 0.029(2) 0.0020(17) 0.0138(17) 0.0054(17)
C27 0.042(2) 0.029(2) 0.0207(19) -0.0020(16) -0.0040(16) -0.0029(18)
C28 0.034(2) 0.043(3) 0.039(2) 0.007(2) -0.0039(18) -0.0029(19)
C29 0.0322(19) 0.0165(18) 0.0226(19) -0.0048(14) 0.0059(15) -0.0002(15)
C30 0.0330(19) 0.0196(17) 0.0138(17) 0.0002(14) 0.0031(14) 0.0009(15)

_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 1.931(6) . ?
Li1 O2 1.945(6) . ?
Li1 Ge1 2.554(6) . ?
Ge1 C1 2.011(3) . ?
Ge1 Ge1 2.3278(7) 7 ?
O1 C26 1.430(4) . ?
O1 C27 1.432(4) . ?
O2 C30 1.431(4) 7_565 ?
O2 C29 1.438(4) . ?
C1 C2 1.419(4) . ?
C1 C6 1.422(4) . ?
C2 C3 1.402(5) . ?
C2 C16 1.505(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.392(5) . ?
C6 C7 1.507(4) . ?
C7 C12 1.399(5) . ?
C7 C8 1.401(5) . ?
C8 C9 1.396(5) . ?
C8 C13 1.504(5) . ?
C9 C10 1.384(5) . ?
C10 C11 1.392(5) . ?
C10 C14 1.513(5) . ?
C11 C12 1.395(5) . ?
C12 C15 1.510(5) . ?
C16 C17 1.398(5) . ?
C16 C21 1.402(5) . ?
C17 C18 1.394(4) . ?
C17 C22 1.506(5) . ?
C18 C19 1.379(5) . ?
C19 C20 1.389(5) . ?
C19 C23 1.514(5) . ?
C20 C21 1.394(4) . ?
C21 C24 1.507(5) . ?
C25 C26 1.502(5) . ?
C27 C28 1.515(5) . ?
C29 C30 1.510(5) . ?
C30 O2 1.431(4) 7_565 ?
O3 C32 1.434(9) . ?
O3 C33 1.459(9) . ?
C31 C32 1.527(12) . ?
C33 C34 1.569(10) . ?

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 O2 98.4(3) . . ?
O1 Li1 Ge1 131.2(3) . . ?
O2 Li1 Ge1 130.3(3) . . ?
C1 Ge1 Ge1 100.24(9) . 7 ?
C1 Ge1 Li1 125.63(16) . . ?
Ge1 Ge1 Li1 134.04(13) 7 . ?
C26 O1 C27 112.7(3) . . ?
C26 O1 Li1 123.7(3) . . ?
C27 O1 Li1 123.5(3) . . ?
C30 O2 C29 109.9(3) 7_565 . ?
C30 O2 Li1 123.2(3) 7_565 . ?
C29 O2 Li1 125.5(3) . . ?
C2 C1 C6 116.5(3) . . ?
C2 C1 Ge1 121.9(2) . . ?
C6 C1 Ge1 121.5(2) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 C16 116.8(3) . . ?
C1 C2 C16 122.0(3) . . ?
C4 C3 C2 121.2(3) . . ?
C3 C4 C5 118.8(3) . . ?
C4 C5 C6 121.1(3) . . ?
C5 C6 C1 121.2(3) . . ?
C5 C6 C7 117.4(3) . . ?
C1 C6 C7 121.1(3) . . ?
C12 C7 C8 119.2(3) . . ?
C12 C7 C6 118.3(3) . . ?
C8 C7 C6 122.4(3) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 C13 119.0(3) . . ?
C7 C8 C13 121.6(3) . . ?
C10 C9 C8 122.2(3) . . ?
C9 C10 C11 117.8(3) . . ?
C9 C10 C14 121.5(3) . . ?
C11 C10 C14 120.7(3) . . ?
C10 C11 C12 121.6(3) . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 C15 119.7(3) . . ?
C7 C12 C15 120.4(3) . . ?
C17 C16 C21 119.0(3) . . ?
C17 C16 C2 122.6(3) . . ?
C21 C16 C2 118.0(3) . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 C22 119.2(3) . . ?
C16 C17 C22 121.4(3) . . ?
C19 C18 C17 122.3(3) . . ?
C18 C19 C20 117.9(3) . . ?
C18 C19 C23 121.4(3) . . ?
C20 C19 C23 120.6(3) . . ?
C19 C20 C21 121.5(3) . . ?
C20 C21 C16 119.9(3) . . ?
C20 C21 C24 119.5(3) . . ?
C16 C21 C24 120.6(3) . . ?
O1 C26 C25 108.4(3) . . ?
O1 C27 C28 108.5(3) . . ?
O2 C29 C30 110.8(3) . . ?
O2 C30 C29 110.3(3) 7_565 . ?
C32 O3 C33 105.6(6) . . ?
O3 C32 C31 104.9(7) . . ?
O3 C33 C34 104.0(6) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.093