# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Naoto Chatani'
_publ_contact_author_email       CHATANI@CHEM.ENG.OSAKA-U.AC.JP

_publ_section_title              
;
Synthesis of [RhCl(CO)(cyclopentadienone)]2 from [RhCl(cod)]2
and a 1,6-diyne under CO: Application to Rh(I)-catalyzed tandem
[2+2+1] carbonylative cycloaddition of diynes and Claisen Rearrangement
;
loop_
_publ_author_name
'Naoto Chatani'
'Yoshiya Fukumoto'
'Sang Ick Lee'

# Attachment 'Compound_8.cif'

data_8(CCDC_752604)
_database_code_depnum_ccdc_archive 'CCDC 752604'
#TrackingRef 'Compound_8.cif'

#==============================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            8
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H28 Cl3 N2 O Rh'
_chemical_formula_weight         653.81

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.1035(5)
_cell_length_b                   12.2818(7)
_cell_length_c                   13.9760(7)
_cell_angle_alpha                112.1714(17)
_cell_angle_beta                 97.0413(16)
_cell_angle_gamma                100.9423(18)
_cell_volume                     1387.97(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6240
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_T_max  0.8964
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13659
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6240
_reflns_number_gt                5626
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'

_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^)+(0.0394P)^2^+1.6293P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6240
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3235(3) -0.1501(3) 0.8773(2) 0.0158(6) Uani 1 1 d . . .
C2 C 0.4187(3) -0.2234(3) 0.8144(2) 0.0136(5) Uani 1 1 d . . .
C3 C 0.5364(3) -0.1387(3) 0.8006(2) 0.0140(5) Uani 1 1 d . . .
C4 C 0.5014(3) -0.0238(3) 0.8313(2) 0.0164(6) Uani 1 1 d . . .
C5 C 0.3610(3) -0.0319(3) 0.8692(2) 0.0145(6) Uani 1 1 d . . .
O1 O 0.2214(2) -0.18514(19) 0.91892(16) 0.0190(4) Uani 1 1 d . . .
C6 C 0.4113(3) -0.3514(3) 0.7920(2) 0.0165(6) Uani 1 1 d . . .
C7 C 0.3334(4) -0.4090(3) 0.8481(2) 0.0195(6) Uani 1 1 d . . .
H1 H 0.2770 -0.3673 0.8962 0.023 Uiso 1 1 calc R . .
C8 C 0.3386(4) -0.5260(3) 0.8335(3) 0.0248(7) Uani 1 1 d . . .
H2 H 0.2862 -0.5635 0.8723 0.030 Uiso 1 1 calc R . .
C9 C 0.4186(4) -0.5890(3) 0.7634(3) 0.0250(7) Uani 1 1 d . . .
H3 H 0.4251 -0.6680 0.7560 0.030 Uiso 1 1 calc R . .
C10 C 0.4896(4) -0.5354(3) 0.7038(2) 0.0234(7) Uani 1 1 d . . .
H4 H 0.5414 -0.5793 0.6533 0.028 Uiso 1 1 calc R . .
C11 C 0.4854(3) -0.4181(3) 0.7174(2) 0.0200(6) Uani 1 1 d . . .
H5 H 0.5335 -0.3829 0.6756 0.024 Uiso 1 1 calc R . .
C12 C 0.6891(3) -0.1313(3) 0.7684(2) 0.0206(6) Uani 1 1 d . . .
H6 H 0.6841 -0.2023 0.7024 0.025 Uiso 1 1 calc R . .
H7 H 0.7706 -0.1264 0.8249 0.025 Uiso 1 1 calc R . .
C13 C 0.7166(3) -0.0125(3) 0.7514(2) 0.0210(6) Uani 1 1 d . . .
H8 H 0.6793 -0.0303 0.6761 0.025 Uiso 1 1 calc R . .
H9 H 0.8273 0.0289 0.7719 0.025 Uiso 1 1 calc R . .
C14 C 0.6270(3) 0.0686(3) 0.8219(2) 0.0193(6) Uani 1 1 d . . .
H10 H 0.6925 0.1245 0.8919 0.023 Uiso 1 1 calc R . .
H11 H 0.5846 0.1167 0.7877 0.023 Uiso 1 1 calc R . .
C15 C 0.2864(3) 0.0666(3) 0.9136(2) 0.0163(6) Uani 1 1 d . . .
C16 C 0.3676(4) 0.1884(3) 0.9530(2) 0.0200(6) Uani 1 1 d . . .
H12 H 0.4720 0.2081 0.9487 0.024 Uiso 1 1 calc R . .
C17 C 0.2982(4) 0.2811(3) 0.9982(2) 0.0229(7) Uani 1 1 d . . .
H13 H 0.3555 0.3636 1.0256 0.027 Uiso 1 1 calc R . .
C18 C 0.1449(4) 0.2536(3) 1.0034(3) 0.0254(7) Uani 1 1 d . . .
H14 H 0.0972 0.3169 1.0346 0.030 Uiso 1 1 calc R . .
C19 C 0.0622(4) 0.1330(3) 0.9628(2) 0.0221(6) Uani 1 1 d . . .
H15 H -0.0428 0.1138 0.9656 0.027 Uiso 1 1 calc R . .
C20 C 0.1311(3) 0.0405(3) 0.9183(2) 0.0191(6) Uani 1 1 d . . .
H16 H 0.0728 -0.0417 0.8905 0.023 Uiso 1 1 calc R . .
Rh1 Rh 0.32462(2) -0.155339(19) 0.705338(16) 0.01252(8) Uani 1 1 d . . .
N1 N 0.0955(3) -0.2773(2) 0.6346(2) 0.0166(5) Uani 1 1 d . . .
C21 C 0.0111(4) -0.3186(3) 0.6913(3) 0.0213(6) Uani 1 1 d . . .
H17 H 0.0512 -0.2918 0.7648 0.026 Uiso 1 1 calc R . .
C22 C -0.1328(4) -0.3992(3) 0.6472(3) 0.0271(7) Uani 1 1 d . . .
H18 H -0.1892 -0.4274 0.6899 0.032 Uiso 1 1 calc R . .
C23 C -0.1933(4) -0.4380(3) 0.5409(3) 0.0269(7) Uani 1 1 d . . .
H19 H -0.2921 -0.4926 0.5093 0.032 Uiso 1 1 calc R . .
C24 C -0.1069(4) -0.3957(3) 0.4815(3) 0.0233(7) Uani 1 1 d . . .
H20 H -0.1452 -0.4208 0.4080 0.028 Uiso 1 1 calc R . .
C25 C 0.0365(4) -0.3159(3) 0.5308(2) 0.0206(6) Uani 1 1 d . . .
H21 H 0.0956 -0.2874 0.4895 0.025 Uiso 1 1 calc R . .
N2 N 0.2532(3) -0.0377(2) 0.64154(19) 0.0167(5) Uani 1 1 d . . .
C26 C 0.1259(4) -0.0016(3) 0.6596(2) 0.0212(6) Uani 1 1 d . . .
H22 H 0.0605 -0.0385 0.6930 0.025 Uiso 1 1 calc R . .
C27 C 0.0853(4) 0.0870(3) 0.6318(3) 0.0265(7) Uani 1 1 d . . .
H23 H -0.0062 0.1104 0.6458 0.032 Uiso 1 1 calc R . .
C28 C 0.1788(4) 0.1404(3) 0.5840(3) 0.0318(8) Uani 1 1 d . . .
H24 H 0.1533 0.2020 0.5648 0.038 Uiso 1 1 calc R . .
C29 C 0.3108(4) 0.1044(3) 0.5636(3) 0.0271(7) Uani 1 1 d . . .
H25 H 0.3771 0.1406 0.5303 0.033 Uiso 1 1 calc R . .
C30 C 0.3442(4) 0.0145(3) 0.5929(2) 0.0206(6) Uani 1 1 d . . .
H26 H 0.4341 -0.0114 0.5782 0.025 Uiso 1 1 calc R . .
Cl1 Cl 0.40920(8) -0.25914(6) 0.54299(5) 0.01780(15) Uani 1 1 d . . .
C31 C 0.0907(6) -0.3519(5) 0.1711(3) 0.0532(12) Uani 1 1 d . . .
H27 H 0.0034 -0.4196 0.1615 0.064 Uiso 1 1 calc R . .
H28 H 0.0487 -0.2882 0.1593 0.064 Uiso 1 1 calc R . .
Cl2 Cl 0.19870(13) -0.29149(11) 0.30118(7) 0.0429(2) Uani 1 1 d . . .
Cl3 Cl 0.20094(13) -0.40532(9) 0.07751(7) 0.0425(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0152(13) 0.0170(14) 0.0145(13) 0.0056(11) 0.0017(11) 0.0051(11)
C2 0.0176(13) 0.0191(14) 0.0076(12) 0.0088(10) 0.0021(10) 0.0062(11)
C3 0.0146(13) 0.0197(14) 0.0088(12) 0.0069(11) 0.0023(10) 0.0048(11)
C4 0.0161(14) 0.0156(14) 0.0141(13) 0.0038(11) 0.0016(11) 0.0024(11)
C5 0.0188(14) 0.0156(14) 0.0089(12) 0.0052(10) 0.0039(10) 0.0031(11)
O1 0.0189(10) 0.0215(11) 0.0214(11) 0.0109(9) 0.0113(8) 0.0074(9)
C6 0.0129(13) 0.0170(14) 0.0168(14) 0.0047(11) 0.0009(11) 0.0038(11)
C7 0.0230(15) 0.0197(15) 0.0174(14) 0.0085(12) 0.0076(12) 0.0052(12)
C8 0.0264(16) 0.0201(16) 0.0290(17) 0.0133(13) 0.0056(13) 0.0024(13)
C9 0.0258(17) 0.0143(15) 0.0308(17) 0.0074(13) 0.0003(14) 0.0034(13)
C10 0.0259(16) 0.0223(16) 0.0202(15) 0.0047(12) 0.0072(13) 0.0092(13)
C11 0.0192(15) 0.0219(16) 0.0189(15) 0.0076(12) 0.0054(12) 0.0057(12)
C12 0.0136(14) 0.0246(16) 0.0210(15) 0.0054(12) 0.0052(11) 0.0064(12)
C13 0.0159(14) 0.0237(16) 0.0226(15) 0.0094(12) 0.0073(12) 0.0015(12)
C14 0.0169(14) 0.0180(15) 0.0186(14) 0.0046(12) 0.0044(11) 0.0005(12)
C15 0.0217(15) 0.0204(15) 0.0093(12) 0.0079(11) 0.0052(11) 0.0063(12)
C16 0.0185(14) 0.0210(15) 0.0190(14) 0.0068(12) 0.0041(12) 0.0047(12)
C17 0.0299(17) 0.0188(15) 0.0196(15) 0.0082(12) 0.0014(13) 0.0074(13)
C18 0.0313(18) 0.0239(17) 0.0214(16) 0.0054(13) 0.0051(13) 0.0167(14)
C19 0.0191(15) 0.0293(17) 0.0222(15) 0.0118(13) 0.0073(12) 0.0118(13)
C20 0.0177(14) 0.0198(15) 0.0205(15) 0.0088(12) 0.0060(12) 0.0041(12)
Rh1 0.01225(12) 0.01306(12) 0.01218(12) 0.00496(9) 0.00412(8) 0.00262(8)
N1 0.0141(12) 0.0152(12) 0.0211(13) 0.0078(10) 0.0048(10) 0.0038(10)
C21 0.0211(15) 0.0189(15) 0.0244(16) 0.0104(12) 0.0038(12) 0.0040(12)
C22 0.0218(16) 0.0252(17) 0.0369(19) 0.0178(15) 0.0076(14) 0.0008(13)
C23 0.0173(15) 0.0179(15) 0.040(2) 0.0100(14) -0.0009(14) 0.0008(13)
C24 0.0211(15) 0.0186(15) 0.0268(16) 0.0085(13) -0.0033(13) 0.0044(13)
C25 0.0195(15) 0.0188(15) 0.0214(15) 0.0068(12) 0.0020(12) 0.0045(12)
N2 0.0208(12) 0.0143(12) 0.0146(12) 0.0066(9) 0.0022(10) 0.0032(10)
C26 0.0192(15) 0.0219(16) 0.0200(15) 0.0060(12) 0.0040(12) 0.0053(13)
C27 0.0293(17) 0.0235(16) 0.0261(17) 0.0095(13) 0.0006(14) 0.0105(14)
C28 0.039(2) 0.0197(16) 0.0341(19) 0.0117(14) -0.0044(16) 0.0067(15)
C29 0.0369(19) 0.0184(16) 0.0249(17) 0.0118(13) 0.0041(14) 0.0001(14)
C30 0.0247(16) 0.0193(15) 0.0174(14) 0.0081(12) 0.0070(12) 0.0017(12)
Cl1 0.0199(3) 0.0173(3) 0.0145(3) 0.0043(3) 0.0072(3) 0.0034(3)
C31 0.053(3) 0.084(4) 0.032(2) 0.024(2) 0.0124(19) 0.035(3)
Cl2 0.0539(6) 0.0610(7) 0.0266(5) 0.0218(4) 0.0153(4) 0.0313(5)
Cl3 0.0550(6) 0.0349(5) 0.0312(5) 0.0067(4) 0.0169(4) 0.0065(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.248(4) . ?
C1 C5 1.478(4) . ?
C1 C2 1.490(4) . ?
C1 Rh1 2.381(3) . ?
C2 C3 1.431(4) . ?
C2 C6 1.469(4) . ?
C2 Rh1 2.160(3) . ?
C3 C4 1.422(4) . ?
C3 C12 1.510(4) . ?
C3 Rh1 2.133(3) . ?
C4 C5 1.443(4) . ?
C4 C14 1.507(4) . ?
C4 Rh1 2.114(3) . ?
C5 C15 1.468(4) . ?
C5 Rh1 2.158(3) . ?
C6 C11 1.397(4) . ?
C6 C7 1.408(4) . ?
C7 C8 1.384(4) . ?
C7 H1 0.9500 . ?
C8 C9 1.381(5) . ?
C8 H2 0.9500 . ?
C9 C10 1.388(5) . ?
C9 H3 0.9500 . ?
C10 C11 1.388(4) . ?
C10 H4 0.9500 . ?
C11 H5 0.9500 . ?
C12 C13 1.544(4) . ?
C12 H6 0.9900 . ?
C12 H7 0.9900 . ?
C13 C14 1.547(4) . ?
C13 H8 0.9900 . ?
C13 H9 0.9900 . ?
C14 H10 0.9900 . ?
C14 H11 0.9900 . ?
C15 C16 1.396(4) . ?
C15 C20 1.404(4) . ?
C16 C17 1.388(4) . ?
C16 H12 0.9500 . ?
C17 C18 1.390(5) . ?
C17 H13 0.9500 . ?
C18 C19 1.386(5) . ?
C18 H14 0.9500 . ?
C19 C20 1.379(4) . ?
C19 H15 0.9500 . ?
C20 H16 0.9500 . ?
Rh1 N2 2.120(2) . ?
Rh1 N1 2.182(2) . ?
Rh1 Cl1 2.4463(7) . ?
N1 C21 1.334(4) . ?
N1 C25 1.346(4) . ?
C21 C22 1.388(4) . ?
C21 H17 0.9500 . ?
C22 C23 1.379(5) . ?
C22 H18 0.9500 . ?
C23 C24 1.382(5) . ?
C23 H19 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H20 0.9500 . ?
C25 H21 0.9500 . ?
N2 C26 1.337(4) . ?
N2 C30 1.350(4) . ?
C26 C27 1.382(4) . ?
C26 H22 0.9500 . ?
C27 C28 1.363(5) . ?
C27 H23 0.9500 . ?
C28 C29 1.382(5) . ?
C28 H24 0.9500 . ?
C29 C30 1.385(4) . ?
C29 H25 0.9500 . ?
C30 H26 0.9500 . ?
C31 Cl3 1.753(4) . ?
C31 Cl2 1.758(4) . ?
C31 H27 0.9900 . ?
C31 H28 0.9900 . ?

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 C1 C5 126.6(3) . . ?
O1 C1 C2 127.2(3) . . ?
C5 C1 C2 105.8(2) . . ?
O1 C1 Rh1 133.4(2) . . ?
C5 C1 Rh1 63.00(14) . . ?
C2 C1 Rh1 63.00(14) . . ?
C3 C2 C6 127.0(3) . . ?
C3 C2 C1 106.1(2) . . ?
C6 C2 C1 125.7(2) . . ?
C3 C2 Rh1 69.49(15) . . ?
C6 C2 Rh1 126.22(19) . . ?
C1 C2 Rh1 79.10(16) . . ?
C4 C3 C2 109.8(2) . . ?
C4 C3 C12 110.2(3) . . ?
C2 C3 C12 140.0(3) . . ?
C4 C3 Rh1 69.73(16) . . ?
C2 C3 Rh1 71.58(15) . . ?
C12 C3 Rh1 125.74(19) . . ?
C3 C4 C5 108.6(3) . . ?
C3 C4 C14 110.9(3) . . ?
C5 C4 C14 140.3(3) . . ?
C3 C4 Rh1 71.15(16) . . ?
C5 C4 Rh1 71.91(16) . . ?
C14 C4 Rh1 125.5(2) . . ?
C4 C5 C15 127.2(3) . . ?
C4 C5 C1 106.8(2) . . ?
C15 C5 C1 124.8(2) . . ?
C4 C5 Rh1 68.62(15) . . ?
C15 C5 Rh1 127.17(19) . . ?
C1 C5 Rh1 79.41(16) . . ?
C11 C6 C7 118.1(3) . . ?
C11 C6 C2 121.2(3) . . ?
C7 C6 C2 120.6(3) . . ?
C8 C7 C6 120.3(3) . . ?
C8 C7 H1 119.8 . . ?
C6 C7 H1 119.8 . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H2 119.5 . . ?
C7 C8 H2 119.5 . . ?
C8 C9 C10 119.1(3) . . ?
C8 C9 H3 120.4 . . ?
C10 C9 H3 120.4 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H4 119.7 . . ?
C9 C10 H4 119.7 . . ?
C10 C11 C6 120.7(3) . . ?
C10 C11 H5 119.7 . . ?
C6 C11 H5 119.7 . . ?
C3 C12 C13 102.6(2) . . ?
C3 C12 H6 111.2 . . ?
C13 C12 H6 111.2 . . ?
C3 C12 H7 111.2 . . ?
C13 C12 H7 111.2 . . ?
H6 C12 H7 109.2 . . ?
C12 C13 C14 106.7(2) . . ?
C12 C13 H8 110.4 . . ?
C14 C13 H8 110.4 . . ?
C12 C13 H9 110.4 . . ?
C14 C13 H9 110.4 . . ?
H8 C13 H9 108.6 . . ?
C4 C14 C13 102.2(2) . . ?
C4 C14 H10 111.3 . . ?
C13 C14 H10 111.3 . . ?
C4 C14 H11 111.3 . . ?
C13 C14 H11 111.3 . . ?
H10 C14 H11 109.2 . . ?
C16 C15 C20 118.1(3) . . ?
C16 C15 C5 121.1(3) . . ?
C20 C15 C5 120.8(3) . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H12 119.5 . . ?
C15 C16 H12 119.5 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H13 119.9 . . ?
C18 C17 H13 119.9 . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H14 120.3 . . ?
C17 C18 H14 120.3 . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H15 119.7 . . ?
C18 C19 H15 119.7 . . ?
C19 C20 C15 120.7(3) . . ?
C19 C20 H16 119.6 . . ?
C15 C20 H16 119.6 . . ?
C4 Rh1 N2 98.00(10) . . ?
C4 Rh1 C3 39.13(11) . . ?
N2 Rh1 C3 131.39(10) . . ?
C4 Rh1 C5 39.47(11) . . ?
N2 Rh1 C5 96.14(10) . . ?
C3 Rh1 C5 65.67(11) . . ?
C4 Rh1 C2 66.19(11) . . ?
N2 Rh1 C2 162.13(10) . . ?
C3 Rh1 C2 38.93(11) . . ?
C5 Rh1 C2 66.47(10) . . ?
C4 Rh1 N1 154.85(11) . . ?
N2 Rh1 N1 87.66(9) . . ?
C3 Rh1 N1 140.93(10) . . ?
C5 Rh1 N1 115.74(10) . . ?
C2 Rh1 N1 103.31(10) . . ?
C4 Rh1 C1 62.55(11) . . ?
N2 Rh1 C1 128.34(10) . . ?
C3 Rh1 C1 61.98(10) . . ?
C5 Rh1 C1 37.59(10) . . ?
C2 Rh1 C1 37.91(10) . . ?
N1 Rh1 C1 94.77(10) . . ?
C4 Rh1 Cl1 114.55(8) . . ?
N2 Rh1 Cl1 89.74(7) . . ?
C3 Rh1 Cl1 91.48(7) . . ?
C5 Rh1 Cl1 153.89(8) . . ?
C2 Rh1 Cl1 104.16(8) . . ?
N1 Rh1 Cl1 89.84(7) . . ?
C1 Rh1 Cl1 141.74(7) . . ?
C21 N1 C25 117.8(3) . . ?
C21 N1 Rh1 121.6(2) . . ?
C25 N1 Rh1 120.5(2) . . ?
N1 C21 C22 122.5(3) . . ?
N1 C21 H17 118.7 . . ?
C22 C21 H17 118.7 . . ?
C23 C22 C21 119.5(3) . . ?
C23 C22 H18 120.2 . . ?
C21 C22 H18 120.2 . . ?
C22 C23 C24 118.4(3) . . ?
C22 C23 H19 120.8 . . ?
C24 C23 H19 120.8 . . ?
C23 C24 C25 118.9(3) . . ?
C23 C24 H20 120.5 . . ?
C25 C24 H20 120.5 . . ?
N1 C25 C24 122.8(3) . . ?
N1 C25 H21 118.6 . . ?
C24 C25 H21 118.6 . . ?
C26 N2 C30 118.0(3) . . ?
C26 N2 Rh1 120.7(2) . . ?
C30 N2 Rh1 120.8(2) . . ?
N2 C26 C27 122.7(3) . . ?
N2 C26 H22 118.6 . . ?
C27 C26 H22 118.6 . . ?
C28 C27 C26 118.9(3) . . ?
C28 C27 H23 120.5 . . ?
C26 C27 H23 120.5 . . ?
C27 C28 C29 119.6(3) . . ?
C27 C28 H24 120.2 . . ?
C29 C28 H24 120.2 . . ?
C28 C29 C30 118.6(3) . . ?
C28 C29 H25 120.7 . . ?
C30 C29 H25 120.7 . . ?
N2 C30 C29 122.1(3) . . ?
N2 C30 H26 118.9 . . ?
C29 C30 H26 118.9 . . ?
Cl3 C31 Cl2 111.8(3) . . ?
Cl3 C31 H27 109.2 . . ?
Cl2 C31 H27 109.2 . . ?
Cl3 C31 H28 109.2 . . ?
Cl2 C31 H28 109.2 . . ?
H27 C31 H28 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -169.7(3) . . . . ?
C5 C1 C2 C3 17.1(3) . . . . ?
Rh1 C1 C2 C3 64.73(17) . . . . ?
O1 C1 C2 C6 -1.5(5) . . . . ?
C5 C1 C2 C6 -174.7(3) . . . . ?
Rh1 C1 C2 C6 -127.1(3) . . . . ?
O1 C1 C2 Rh1 125.6(3) . . . . ?
C5 C1 C2 Rh1 -47.62(19) . . . . ?
C6 C2 C3 C4 180.0(3) . . . . ?
C1 C2 C3 C4 -12.0(3) . . . . ?
Rh1 C2 C3 C4 59.47(19) . . . . ?
C6 C2 C3 C12 -3.6(5) . . . . ?
C1 C2 C3 C12 164.4(3) . . . . ?
Rh1 C2 C3 C12 -124.1(4) . . . . ?
C6 C2 C3 Rh1 120.5(3) . . . . ?
C1 C2 C3 Rh1 -71.46(18) . . . . ?
C2 C3 C4 C5 2.0(3) . . . . ?
C12 C3 C4 C5 -175.6(2) . . . . ?
Rh1 C3 C4 C5 62.56(19) . . . . ?
C2 C3 C4 C14 177.6(2) . . . . ?
C12 C3 C4 C14 0.1(3) . . . . ?
Rh1 C3 C4 C14 -121.8(2) . . . . ?
C2 C3 C4 Rh1 -60.60(19) . . . . ?
C12 C3 C4 Rh1 121.8(2) . . . . ?
C3 C4 C5 C15 176.8(3) . . . . ?
C14 C4 C5 C15 3.1(6) . . . . ?
Rh1 C4 C5 C15 -121.2(3) . . . . ?
C3 C4 C5 C1 9.0(3) . . . . ?
C14 C4 C5 C1 -164.6(3) . . . . ?
Rh1 C4 C5 C1 71.09(19) . . . . ?
C3 C4 C5 Rh1 -62.07(19) . . . . ?
C14 C4 C5 Rh1 124.3(4) . . . . ?
O1 C1 C5 C4 170.7(3) . . . . ?
C2 C1 C5 C4 -16.0(3) . . . . ?
Rh1 C1 C5 C4 -63.65(18) . . . . ?
O1 C1 C5 C15 2.6(5) . . . . ?
C2 C1 C5 C15 175.8(2) . . . . ?
Rh1 C1 C5 C15 128.2(3) . . . . ?
O1 C1 C5 Rh1 -125.6(3) . . . . ?
C2 C1 C5 Rh1 47.62(18) . . . . ?
C3 C2 C6 C11 -25.6(4) . . . . ?
C1 C2 C6 C11 168.7(3) . . . . ?
Rh1 C2 C6 C11 64.9(4) . . . . ?
C3 C2 C6 C7 152.2(3) . . . . ?
C1 C2 C6 C7 -13.6(4) . . . . ?
Rh1 C2 C6 C7 -117.3(3) . . . . ?
C11 C6 C7 C8 3.7(4) . . . . ?
C2 C6 C7 C8 -174.1(3) . . . . ?
C6 C7 C8 C9 -0.6(5) . . . . ?
C7 C8 C9 C10 -2.6(5) . . . . ?
C8 C9 C10 C11 2.5(5) . . . . ?
C9 C10 C11 C6 0.7(5) . . . . ?
C7 C6 C11 C10 -3.8(4) . . . . ?
C2 C6 C11 C10 174.1(3) . . . . ?
C4 C3 C12 C13 -16.3(3) . . . . ?
C2 C3 C12 C13 167.2(3) . . . . ?
Rh1 C3 C12 C13 62.7(3) . . . . ?
C3 C12 C13 C14 26.1(3) . . . . ?
C3 C4 C14 C13 16.2(3) . . . . ?
C5 C4 C14 C13 -170.3(3) . . . . ?
Rh1 C4 C14 C13 -65.1(3) . . . . ?
C12 C13 C14 C4 -26.0(3) . . . . ?
C4 C5 C15 C16 -19.5(4) . . . . ?
C1 C5 C15 C16 146.2(3) . . . . ?
Rh1 C5 C15 C16 -109.6(3) . . . . ?
C4 C5 C15 C20 160.9(3) . . . . ?
C1 C5 C15 C20 -33.4(4) . . . . ?
Rh1 C5 C15 C20 70.8(3) . . . . ?
C20 C15 C16 C17 1.8(4) . . . . ?
C5 C15 C16 C17 -177.8(3) . . . . ?
C15 C16 C17 C18 -1.0(5) . . . . ?
C16 C17 C18 C19 -0.3(5) . . . . ?
C17 C18 C19 C20 0.6(5) . . . . ?
C18 C19 C20 C15 0.3(5) . . . . ?
C16 C15 C20 C19 -1.5(4) . . . . ?
C5 C15 C20 C19 178.1(3) . . . . ?
C3 C4 Rh1 N2 -152.29(16) . . . . ?
C5 C4 Rh1 N2 89.96(17) . . . . ?
C14 C4 Rh1 N2 -49.6(3) . . . . ?
C5 C4 Rh1 C3 -117.8(2) . . . . ?
C14 C4 Rh1 C3 102.7(3) . . . . ?
C3 C4 Rh1 C5 117.8(2) . . . . ?
C14 C4 Rh1 C5 -139.6(3) . . . . ?
C3 C4 Rh1 C2 36.40(16) . . . . ?
C5 C4 Rh1 C2 -81.35(17) . . . . ?
C14 C4 Rh1 C2 139.1(3) . . . . ?
C3 C4 Rh1 N1 106.1(3) . . . . ?
C5 C4 Rh1 N1 -11.7(3) . . . . ?
C14 C4 Rh1 N1 -151.3(2) . . . . ?
C3 C4 Rh1 C1 78.45(17) . . . . ?
C5 C4 Rh1 C1 -39.30(15) . . . . ?
C14 C4 Rh1 C1 -178.9(3) . . . . ?
C3 C4 Rh1 Cl1 -58.90(17) . . . . ?
C5 C4 Rh1 Cl1 -176.65(13) . . . . ?
C14 C4 Rh1 Cl1 43.8(3) . . . . ?
C2 C3 Rh1 C4 120.2(2) . . . . ?
C12 C3 Rh1 C4 -100.8(3) . . . . ?
C4 C3 Rh1 N2 37.9(2) . . . . ?
C2 C3 Rh1 N2 158.10(15) . . . . ?
C12 C3 Rh1 N2 -62.9(3) . . . . ?
C4 C3 Rh1 C5 -38.13(16) . . . . ?
C2 C3 Rh1 C5 82.10(17) . . . . ?
C12 C3 Rh1 C5 -138.9(3) . . . . ?
C4 C3 Rh1 C2 -120.2(2) . . . . ?
C12 C3 Rh1 C2 139.0(3) . . . . ?
C4 C3 Rh1 N1 -139.61(18) . . . . ?
C2 C3 Rh1 N1 -19.4(2) . . . . ?
C12 C3 Rh1 N1 119.6(2) . . . . ?
C4 C3 Rh1 C1 -80.01(18) . . . . ?
C2 C3 Rh1 C1 40.22(15) . . . . ?
C12 C3 Rh1 C1 179.2(3) . . . . ?
C4 C3 Rh1 Cl1 128.82(16) . . . . ?
C2 C3 Rh1 Cl1 -110.94(15) . . . . ?
C12 C3 Rh1 Cl1 28.0(2) . . . . ?
C15 C5 Rh1 C4 121.2(3) . . . . ?
C1 C5 Rh1 C4 -112.9(2) . . . . ?
C4 C5 Rh1 N2 -95.13(17) . . . . ?
C15 C5 Rh1 N2 26.1(3) . . . . ?
C1 C5 Rh1 N2 152.00(16) . . . . ?
C4 C5 Rh1 C3 37.80(16) . . . . ?
C15 C5 Rh1 C3 159.0(3) . . . . ?
C1 C5 Rh1 C3 -75.07(17) . . . . ?
C4 C5 Rh1 C2 80.56(18) . . . . ?
C15 C5 Rh1 C2 -158.2(3) . . . . ?
C1 C5 Rh1 C2 -32.31(16) . . . . ?
C4 C5 Rh1 N1 174.51(15) . . . . ?
C15 C5 Rh1 N1 -64.3(3) . . . . ?
C1 C5 Rh1 N1 61.64(18) . . . . ?
C4 C5 Rh1 C1 112.9(2) . . . . ?
C15 C5 Rh1 C1 -125.9(3) . . . . ?
C4 C5 Rh1 Cl1 6.9(3) . . . . ?
C15 C5 Rh1 Cl1 128.1(2) . . . . ?
C1 C5 Rh1 Cl1 -105.9(2) . . . . ?
C3 C2 Rh1 C4 -36.58(16) . . . . ?
C6 C2 Rh1 C4 -158.1(3) . . . . ?
C1 C2 Rh1 C4 75.32(17) . . . . ?
C3 C2 Rh1 N2 -65.8(4) . . . . ?
C6 C2 Rh1 N2 172.7(3) . . . . ?
C1 C2 Rh1 N2 46.1(4) . . . . ?
C6 C2 Rh1 C3 -121.5(3) . . . . ?
C1 C2 Rh1 C3 111.9(2) . . . . ?
C3 C2 Rh1 C5 -79.85(17) . . . . ?
C6 C2 Rh1 C5 158.6(3) . . . . ?
C1 C2 Rh1 C5 32.05(16) . . . . ?
C3 C2 Rh1 N1 167.59(15) . . . . ?
C6 C2 Rh1 N1 46.1(3) . . . . ?
C1 C2 Rh1 N1 -80.51(17) . . . . ?
C3 C2 Rh1 C1 -111.9(2) . . . . ?
C6 C2 Rh1 C1 126.6(3) . . . . ?
C3 C2 Rh1 Cl1 74.34(15) . . . . ?
C6 C2 Rh1 Cl1 -47.2(2) . . . . ?
C1 C2 Rh1 Cl1 -173.76(14) . . . . ?
O1 C1 Rh1 C4 157.3(3) . . . . ?
C5 C1 Rh1 C4 41.30(17) . . . . ?
C2 C1 Rh1 C4 -85.79(18) . . . . ?
O1 C1 Rh1 N2 79.5(3) . . . . ?
C5 C1 Rh1 N2 -36.5(2) . . . . ?
C2 C1 Rh1 N2 -163.61(16) . . . . ?
O1 C1 Rh1 C3 -158.2(3) . . . . ?
C5 C1 Rh1 C3 85.76(18) . . . . ?
C2 C1 Rh1 C3 -41.33(16) . . . . ?
O1 C1 Rh1 C5 116.0(4) . . . . ?
C2 C1 Rh1 C5 -127.1(2) . . . . ?
O1 C1 Rh1 C2 -116.9(4) . . . . ?
C5 C1 Rh1 C2 127.1(2) . . . . ?
O1 C1 Rh1 N1 -11.3(3) . . . . ?
C5 C1 Rh1 N1 -127.30(17) . . . . ?
C2 C1 Rh1 N1 105.61(16) . . . . ?
O1 C1 Rh1 Cl1 -107.1(3) . . . . ?
C5 C1 Rh1 Cl1 136.89(15) . . . . ?
C2 C1 Rh1 Cl1 9.8(2) . . . . ?
C4 Rh1 N1 C21 -24.0(4) . . . . ?
N2 Rh1 N1 C21 -127.9(2) . . . . ?
C3 Rh1 N1 C21 50.2(3) . . . . ?
C5 Rh1 N1 C21 -32.2(3) . . . . ?
C2 Rh1 N1 C21 37.8(2) . . . . ?
C1 Rh1 N1 C21 0.4(2) . . . . ?
Cl1 Rh1 N1 C21 142.4(2) . . . . ?
C4 Rh1 N1 C25 157.9(3) . . . . ?
N2 Rh1 N1 C25 54.0(2) . . . . ?
C3 Rh1 N1 C25 -127.9(2) . . . . ?
C5 Rh1 N1 C25 149.7(2) . . . . ?
C2 Rh1 N1 C25 -140.2(2) . . . . ?
C1 Rh1 N1 C25 -177.7(2) . . . . ?
Cl1 Rh1 N1 C25 -35.7(2) . . . . ?
C25 N1 C21 C22 0.2(5) . . . . ?
Rh1 N1 C21 C22 -177.9(2) . . . . ?
N1 C21 C22 C23 -0.7(5) . . . . ?
C21 C22 C23 C24 0.6(5) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C21 N1 C25 C24 0.3(5) . . . . ?
Rh1 N1 C25 C24 178.4(2) . . . . ?
C23 C24 C25 N1 -0.3(5) . . . . ?
C4 Rh1 N2 C26 -102.8(2) . . . . ?
C3 Rh1 N2 C26 -125.8(2) . . . . ?
C5 Rh1 N2 C26 -63.1(2) . . . . ?
C2 Rh1 N2 C26 -76.0(4) . . . . ?
N1 Rh1 N2 C26 52.6(2) . . . . ?
C1 Rh1 N2 C26 -41.6(3) . . . . ?
Cl1 Rh1 N2 C26 142.4(2) . . . . ?
C4 Rh1 N2 C30 69.0(2) . . . . ?
C3 Rh1 N2 C30 46.0(3) . . . . ?
C5 Rh1 N2 C30 108.8(2) . . . . ?
C2 Rh1 N2 C30 95.8(4) . . . . ?
N1 Rh1 N2 C30 -135.6(2) . . . . ?
C1 Rh1 N2 C30 130.2(2) . . . . ?
Cl1 Rh1 N2 C30 -45.7(2) . . . . ?
C30 N2 C26 C27 -0.8(4) . . . . ?
Rh1 N2 C26 C27 171.3(2) . . . . ?
N2 C26 C27 C28 -0.1(5) . . . . ?
C26 C27 C28 C29 0.5(5) . . . . ?
C27 C28 C29 C30 -0.1(5) . . . . ?
C26 N2 C30 C29 1.2(4) . . . . ?
Rh1 N2 C30 C29 -170.8(2) . . . . ?
C28 C29 C30 N2 -0.8(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.664
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.144

# Attachment 'Compound_6.cif'

data_8(CCDC_752605)
_database_code_depnum_ccdc_archive 'CCDC 752605'
#TrackingRef 'Compound_6.cif'

#==============================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            6
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 Cl2 O4 Rh2'
_chemical_formula_weight         877.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   10.2579(3)
_cell_length_b                   11.3113(3)
_cell_length_c                   15.1156(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6735(9)
_cell_angle_gamma                90.00
_cell_volume                     1696.66(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3870
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.45

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16585
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.45
_reflns_number_total             3871
_reflns_number_gt                3402
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
# Carroll K. Johnson and M. N. Burnett, ORNL-6895, ORTEP-III(version 1.0.2),
# A FORTRAN Thermal-Ellipsoid Plot Program, Oak Ridge National Labratory,
# Oak Ridge, Tennessee.
# Ortep-3 for Windows, Version 1.05 Louis J. Farrugia,

_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^)+(0.0782P)^2^+16.6092P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3871
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1667
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3208(7) 0.1627(6) 1.0231(4) 0.0311(14) Uani 1 1 d . . .
C2 C 0.3096(6) 0.0343(6) 0.9972(4) 0.0287(13) Uani 1 1 d . . .
C3 C 0.2742(6) 0.0289(6) 0.9015(4) 0.0270(12) Uani 1 1 d . . .
C4 C 0.2344(7) 0.1432(6) 0.8636(4) 0.0283(13) Uani 1 1 d . . .
C5 C 0.2457(7) 0.2256(6) 0.9374(4) 0.0287(13) Uani 1 1 d . . .
C6 C 0.2683(7) -0.0595(6) 0.8261(4) 0.0312(14) Uani 1 1 d . . .
H1 H 0.2213 -0.1326 0.8365 0.037 Uiso 1 1 calc R . .
H2 H 0.3597 -0.0799 0.8204 0.037 Uiso 1 1 calc R . .
C7 C 0.1868(9) 0.0080(7) 0.7402(4) 0.0393(17) Uani 1 1 d . . .
H3 H 0.2209 -0.0123 0.6864 0.047 Uiso 1 1 calc R . .
H4 H 0.0904 -0.0141 0.7269 0.047 Uiso 1 1 calc R . .
C8 C 0.2035(8) 0.1410(7) 0.7602(4) 0.0334(15) Uani 1 1 d . . .
H5 H 0.2786 0.1744 0.7380 0.040 Uiso 1 1 calc R . .
H6 H 0.1197 0.1849 0.7322 0.040 Uiso 1 1 calc R . .
O1 O 0.3702(6) 0.2067(5) 1.0973(3) 0.0400(12) Uani 1 1 d . . .
Rh1 Rh 0.09749(5) 0.09259(4) 0.94069(3) 0.02229(18) Uani 1 1 d . . .
C9 C 0.3574(7) -0.0629(6) 1.0627(5) 0.0309(14) Uani 1 1 d . . .
C10 C 0.3768(7) -0.0460(7) 1.1564(5) 0.0364(15) Uani 1 1 d . . .
H7 H 0.3556 0.0280 1.1790 0.044 Uiso 1 1 calc R . .
C11 C 0.4276(8) -0.1383(8) 1.2174(5) 0.0437(18) Uani 1 1 d . . .
H8 H 0.4429 -0.1255 1.2813 0.052 Uiso 1 1 calc R . .
C12 C 0.4554(8) -0.2473(8) 1.1858(6) 0.049(2) Uani 1 1 d . . .
H9 H 0.4883 -0.3095 1.2277 0.058 Uiso 1 1 calc R . .
C13 C 0.4355(8) -0.2658(8) 1.0933(6) 0.0484(19) Uani 1 1 d . . .
H10 H 0.4539 -0.3411 1.0714 0.058 Uiso 1 1 calc R . .
C14 C 0.3886(8) -0.1747(7) 1.0322(5) 0.0391(16) Uani 1 1 d . . .
H11 H 0.3773 -0.1878 0.9686 0.047 Uiso 1 1 calc R . .
C15 C 0.2179(8) 0.3535(6) 0.9294(5) 0.0360(15) Uani 1 1 d . . .
C16 C 0.2182(10) 0.4140(8) 0.8506(6) 0.049(2) Uani 1 1 d . . .
H12 H 0.2377 0.3732 0.8005 0.059 Uiso 1 1 calc R . .
C17 C 0.1900(10) 0.5349(8) 0.8435(7) 0.059(2) Uani 1 1 d . . .
H13 H 0.1918 0.5751 0.7886 0.070 Uiso 1 1 calc R . .
C18 C 0.1609(11) 0.5949(7) 0.9110(7) 0.061(3) Uani 1 1 d . . .
H14 H 0.1423 0.6772 0.9049 0.073 Uiso 1 1 calc R . .
C19 C 0.1580(18) 0.5368(9) 0.9897(6) 0.099(5) Uani 1 1 d . . .
H15 H 0.1368 0.5791 1.0386 0.119 Uiso 1 1 calc R . .
C20 C 0.1856(18) 0.4166(8) 0.9990(7) 0.090(5) Uani 1 1 d . . .
H16 H 0.1823 0.3774 1.0539 0.109 Uiso 1 1 calc R . .
Cl1 Cl -0.02482(16) -0.09825(12) 0.91449(10) 0.0249(3) Uani 1 1 d . . .
C21 C -0.0501(7) 0.1840(6) 0.8747(5) 0.0324(14) Uani 1 1 d . . .
O2 O -0.1285(6) 0.2487(5) 0.8334(4) 0.0472(13) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(4) 0.035(3) 0.023(3) 0.003(3) 0.007(3) -0.006(3)
C2 0.023(3) 0.033(3) 0.029(3) 0.002(3) 0.006(2) -0.004(2)
C3 0.023(3) 0.035(3) 0.025(3) 0.003(3) 0.010(2) -0.003(2)
C4 0.033(3) 0.036(3) 0.018(3) 0.001(2) 0.008(2) -0.006(3)
C5 0.033(3) 0.032(3) 0.022(3) 0.000(2) 0.008(2) -0.015(3)
C6 0.034(3) 0.034(3) 0.028(3) -0.008(3) 0.013(3) -0.003(3)
C7 0.059(5) 0.043(4) 0.015(3) -0.004(3) 0.008(3) -0.004(3)
C8 0.044(4) 0.041(4) 0.016(3) 0.004(3) 0.008(3) -0.008(3)
O1 0.051(3) 0.045(3) 0.021(2) -0.002(2) 0.002(2) -0.017(2)
Rh1 0.0285(3) 0.0209(3) 0.0179(3) 0.00043(16) 0.00665(18) -0.00222(17)
C9 0.023(3) 0.036(3) 0.033(3) 0.008(3) 0.006(3) 0.001(3)
C10 0.032(4) 0.049(4) 0.028(3) 0.006(3) 0.006(3) -0.002(3)
C11 0.033(4) 0.065(5) 0.028(3) 0.011(3) -0.002(3) 0.002(4)
C12 0.034(4) 0.057(5) 0.051(5) 0.024(4) 0.004(3) 0.007(3)
C13 0.043(4) 0.051(5) 0.050(5) 0.011(4) 0.010(4) 0.013(4)
C14 0.039(4) 0.042(4) 0.036(4) 0.005(3) 0.010(3) 0.005(3)
C15 0.045(4) 0.029(3) 0.031(3) -0.002(3) 0.005(3) -0.015(3)
C16 0.057(5) 0.048(5) 0.046(5) 0.017(4) 0.019(4) 0.008(4)
C17 0.063(6) 0.049(5) 0.065(6) 0.028(5) 0.019(5) 0.005(4)
C18 0.077(7) 0.025(4) 0.071(6) 0.007(4) 0.000(5) -0.008(4)
C19 0.228(17) 0.034(5) 0.033(5) -0.006(4) 0.028(7) 0.010(7)
C20 0.210(16) 0.029(4) 0.039(5) -0.011(4) 0.043(7) -0.012(6)
Cl1 0.0339(8) 0.0207(6) 0.0225(7) -0.0041(5) 0.0115(6) -0.0056(5)
C21 0.038(4) 0.024(3) 0.035(3) -0.006(3) 0.009(3) -0.005(3)
O2 0.051(3) 0.038(3) 0.045(3) 0.010(2) -0.002(3) 0.008(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
C1 O1 1.216(8) . ?
C1 C2 1.501(10) . ?
C1 C5 1.507(9) . ?
C1 Rh1 2.445(7) . ?
C2 C3 1.401(9) . ?
C2 C9 1.477(9) . ?
C2 Rh1 2.227(6) . ?
C3 C4 1.431(9) . ?
C3 C6 1.506(9) . ?
C3 Rh1 2.168(6) . ?
C4 C5 1.435(9) . ?
C4 C8 1.514(8) . ?
C4 Rh1 2.119(6) . ?
C5 C15 1.474(10) . ?
C5 Rh1 2.149(6) . ?
C6 C7 1.555(10) . ?
C6 H1 0.9900 . ?
C6 H2 0.9900 . ?
C7 C8 1.535(10) . ?
C7 H3 0.9900 . ?
C7 H4 0.9900 . ?
C8 H5 0.9900 . ?
C8 H6 0.9900 . ?
Rh1 C21 1.895(7) . ?
Rh1 Cl1 2.4777(14) . ?
Rh1 Cl1 2.4857(14) 3_557 ?
C9 C10 1.392(9) . ?
C9 C14 1.411(10) . ?
C10 C11 1.403(11) . ?
C10 H7 0.9500 . ?
C11 C12 1.378(13) . ?
C11 H8 0.9500 . ?
C12 C13 1.376(12) . ?
C12 H9 0.9500 . ?
C13 C14 1.387(11) . ?
C13 H10 0.9500 . ?
C14 H11 0.9500 . ?
C15 C16 1.375(10) . ?
C15 C20 1.378(12) . ?
C16 C17 1.396(12) . ?
C16 H12 0.9500 . ?
C17 C18 1.320(15) . ?
C17 H13 0.9500 . ?
C18 C19 1.366(14) . ?
C18 H14 0.9500 . ?
C19 C20 1.389(14) . ?
C19 H15 0.9500 . ?
C20 H16 0.9500 . ?
Cl1 Rh1 2.4857(14) 3_557 ?
C21 O2 1.148(9) . ?

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 C1 C2 128.5(6) . . ?
O1 C1 C5 127.1(7) . . ?
C2 C1 C5 104.2(5) . . ?
O1 C1 Rh1 136.1(5) . . ?
C2 C1 Rh1 63.5(3) . . ?
C5 C1 Rh1 60.5(3) . . ?
C3 C2 C9 128.0(6) . . ?
C3 C2 C1 107.0(5) . . ?
C9 C2 C1 123.7(6) . . ?
C3 C2 Rh1 69.1(4) . . ?
C9 C2 Rh1 127.1(4) . . ?
C1 C2 Rh1 79.4(4) . . ?
C2 C3 C4 110.4(6) . . ?
C2 C3 C6 139.5(6) . . ?
C4 C3 C6 110.1(5) . . ?
C2 C3 Rh1 73.7(4) . . ?
C4 C3 Rh1 68.6(4) . . ?
C6 C3 Rh1 123.4(4) . . ?
C3 C4 C5 108.4(5) . . ?
C3 C4 C8 111.2(6) . . ?
C5 C4 C8 140.2(6) . . ?
C3 C4 Rh1 72.4(3) . . ?
C5 C4 Rh1 71.5(3) . . ?
C8 C4 Rh1 124.7(5) . . ?
C4 C5 C15 126.7(6) . . ?
C4 C5 C1 106.5(6) . . ?
C15 C5 C1 125.4(6) . . ?
C4 C5 Rh1 69.2(3) . . ?
C15 C5 Rh1 124.4(5) . . ?
C1 C5 Rh1 81.9(4) . . ?
C3 C6 C7 102.5(5) . . ?
C3 C6 H1 111.3 . . ?
C7 C6 H1 111.3 . . ?
C3 C6 H2 111.3 . . ?
C7 C6 H2 111.3 . . ?
H1 C6 H2 109.2 . . ?
C8 C7 C6 107.9(5) . . ?
C8 C7 H3 110.1 . . ?
C6 C7 H3 110.1 . . ?
C8 C7 H4 110.1 . . ?
C6 C7 H4 110.1 . . ?
H3 C7 H4 108.4 . . ?
C4 C8 C7 101.7(5) . . ?
C4 C8 H5 111.4 . . ?
C7 C8 H5 111.4 . . ?
C4 C8 H6 111.4 . . ?
C7 C8 H6 111.4 . . ?
H5 C8 H6 109.3 . . ?
C21 Rh1 C4 96.6(3) . . ?
C21 Rh1 C5 94.7(3) . . ?
C4 Rh1 C5 39.3(2) . . ?
C21 Rh1 C3 130.5(3) . . ?
C4 Rh1 C3 39.0(3) . . ?
C5 Rh1 C3 65.2(3) . . ?
C21 Rh1 C2 159.4(3) . . ?
C4 Rh1 C2 64.6(2) . . ?
C5 Rh1 C2 65.7(3) . . ?
C3 Rh1 C2 37.1(2) . . ?
C21 Rh1 C1 127.7(3) . . ?
C4 Rh1 C1 61.7(2) . . ?
C5 Rh1 C1 37.6(2) . . ?
C3 Rh1 C1 60.4(2) . . ?
C2 Rh1 C1 37.1(2) . . ?
C21 Rh1 Cl1 95.0(2) . . ?
C4 Rh1 Cl1 121.81(18) . . ?
C5 Rh1 Cl1 159.89(19) . . ?
C3 Rh1 Cl1 95.26(18) . . ?
C2 Rh1 Cl1 102.08(17) . . ?
C1 Rh1 Cl1 137.31(17) . . ?
C21 Rh1 Cl1 94.1(2) . 3_557 ?
C4 Rh1 Cl1 150.00(18) . 3_557 ?
C5 Rh1 Cl1 111.98(17) . 3_557 ?
C3 Rh1 Cl1 135.01(17) . 3_557 ?
C2 Rh1 Cl1 98.71(17) . 3_557 ?
C1 Rh1 Cl1 89.68(15) . 3_557 ?
Cl1 Rh1 Cl1 84.87(5) . 3_557 ?
C10 C9 C14 118.1(7) . . ?
C10 C9 C2 121.1(7) . . ?
C14 C9 C2 120.8(6) . . ?
C9 C10 C11 120.0(8) . . ?
C9 C10 H7 120.0 . . ?
C11 C10 H7 120.0 . . ?
C12 C11 C10 120.9(7) . . ?
C12 C11 H8 119.5 . . ?
C10 C11 H8 119.5 . . ?
C13 C12 C11 119.8(7) . . ?
C13 C12 H9 120.1 . . ?
C11 C12 H9 120.1 . . ?
C12 C13 C14 120.1(8) . . ?
C12 C13 H10 119.9 . . ?
C14 C13 H10 119.9 . . ?
C13 C14 C9 121.1(7) . . ?
C13 C14 H11 119.4 . . ?
C9 C14 H11 119.4 . . ?
C16 C15 C20 117.2(8) . . ?
C16 C15 C5 121.1(7) . . ?
C20 C15 C5 121.7(7) . . ?
C15 C16 C17 120.5(9) . . ?
C15 C16 H12 119.7 . . ?
C17 C16 H12 119.7 . . ?
C18 C17 C16 121.8(9) . . ?
C18 C17 H13 119.1 . . ?
C16 C17 H13 119.1 . . ?
C17 C18 C19 119.0(8) . . ?
C17 C18 H14 120.5 . . ?
C19 C18 H14 120.5 . . ?
C18 C19 C20 120.6(10) . . ?
C18 C19 H15 119.7 . . ?
C20 C19 H15 119.7 . . ?
C15 C20 C19 120.8(9) . . ?
C15 C20 H16 119.6 . . ?
C19 C20 H16 119.6 . . ?
Rh1 Cl1 Rh1 95.13(5) . 3_557 ?
O2 C21 Rh1 172.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -166.6(7) . . . . ?
C5 C1 C2 C3 18.1(7) . . . . ?
Rh1 C1 C2 C3 64.1(4) . . . . ?
O1 C1 C2 C9 1.4(11) . . . . ?
C5 C1 C2 C9 -173.9(6) . . . . ?
Rh1 C1 C2 C9 -127.8(6) . . . . ?
O1 C1 C2 Rh1 129.3(7) . . . . ?
C5 C1 C2 Rh1 -46.0(4) . . . . ?
C9 C2 C3 C4 -179.4(6) . . . . ?
C1 C2 C3 C4 -12.0(7) . . . . ?
Rh1 C2 C3 C4 59.1(4) . . . . ?
C9 C2 C3 C6 -1.3(13) . . . . ?
C1 C2 C3 C6 166.0(8) . . . . ?
Rh1 C2 C3 C6 -122.8(9) . . . . ?
C9 C2 C3 Rh1 121.5(7) . . . . ?
C1 C2 C3 Rh1 -71.2(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C6 C3 C4 C5 -178.1(5) . . . . ?
Rh1 C3 C4 C5 62.8(4) . . . . ?
C2 C3 C4 C8 176.7(5) . . . . ?
C6 C3 C4 C8 -2.0(7) . . . . ?
Rh1 C3 C4 C8 -121.1(5) . . . . ?
C2 C3 C4 Rh1 -62.2(5) . . . . ?
C6 C3 C4 Rh1 119.1(5) . . . . ?
C3 C4 C5 C15 178.5(6) . . . . ?
C8 C4 C5 C15 4.2(13) . . . . ?
Rh1 C4 C5 C15 -118.1(7) . . . . ?
C3 C4 C5 C1 11.0(7) . . . . ?
C8 C4 C5 C1 -163.3(8) . . . . ?
Rh1 C4 C5 C1 74.4(4) . . . . ?
C3 C4 C5 Rh1 -63.4(4) . . . . ?
C8 C4 C5 Rh1 122.3(9) . . . . ?
O1 C1 C5 C4 166.9(7) . . . . ?
C2 C1 C5 C4 -17.6(7) . . . . ?
Rh1 C1 C5 C4 -65.4(4) . . . . ?
O1 C1 C5 C15 -0.7(11) . . . . ?
C2 C1 C5 C15 174.7(6) . . . . ?
Rh1 C1 C5 C15 126.9(7) . . . . ?
O1 C1 C5 Rh1 -127.6(7) . . . . ?
C2 C1 C5 Rh1 47.8(4) . . . . ?
C2 C3 C6 C7 168.3(8) . . . . ?
C4 C3 C6 C7 -13.7(7) . . . . ?
Rh1 C3 C6 C7 63.5(7) . . . . ?
C3 C6 C7 C8 24.3(7) . . . . ?
C3 C4 C8 C7 16.8(7) . . . . ?
C5 C4 C8 C7 -168.9(8) . . . . ?
Rh1 C4 C8 C7 -65.9(7) . . . . ?
C6 C7 C8 C4 -25.1(7) . . . . ?
C3 C4 Rh1 C21 -153.6(4) . . . . ?
C5 C4 Rh1 C21 89.3(4) . . . . ?
C8 C4 Rh1 C21 -49.5(6) . . . . ?
C3 C4 Rh1 C5 117.1(5) . . . . ?
C8 C4 Rh1 C5 -138.8(8) . . . . ?
C5 C4 Rh1 C3 -117.1(5) . . . . ?
C8 C4 Rh1 C3 104.0(7) . . . . ?
C3 C4 Rh1 C2 35.3(4) . . . . ?
C5 C4 Rh1 C2 -81.9(4) . . . . ?
C8 C4 Rh1 C2 139.3(7) . . . . ?
C3 C4 Rh1 C1 76.9(4) . . . . ?
C5 C4 Rh1 C1 -40.2(4) . . . . ?
C8 C4 Rh1 C1 -179.1(7) . . . . ?
C3 C4 Rh1 Cl1 -53.5(4) . . . . ?
C5 C4 Rh1 Cl1 -170.7(3) . . . . ?
C8 C4 Rh1 Cl1 50.5(6) . . . . ?
C3 C4 Rh1 Cl1 96.2(5) . . . 3_557 ?
C5 C4 Rh1 Cl1 -20.9(6) . . . 3_557 ?
C8 C4 Rh1 Cl1 -159.7(4) . . . 3_557 ?
C4 C5 Rh1 C21 -94.7(4) . . . . ?
C15 C5 Rh1 C21 26.3(6) . . . . ?
C1 C5 Rh1 C21 154.1(4) . . . . ?
C15 C5 Rh1 C4 121.0(7) . . . . ?
C1 C5 Rh1 C4 -111.2(6) . . . . ?
C4 C5 Rh1 C3 38.1(4) . . . . ?
C15 C5 Rh1 C3 159.1(6) . . . . ?
C1 C5 Rh1 C3 -73.1(4) . . . . ?
C4 C5 Rh1 C2 79.1(4) . . . . ?
C15 C5 Rh1 C2 -159.9(6) . . . . ?
C1 C5 Rh1 C2 -32.1(4) . . . . ?
C4 C5 Rh1 C1 111.2(6) . . . . ?
C15 C5 Rh1 C1 -127.8(7) . . . . ?
C4 C5 Rh1 Cl1 23.7(8) . . . . ?
C15 C5 Rh1 Cl1 144.7(5) . . . . ?
C1 C5 Rh1 Cl1 -87.5(6) . . . . ?
C4 C5 Rh1 Cl1 168.9(3) . . . 3_557 ?
C15 C5 Rh1 Cl1 -70.1(5) . . . 3_557 ?
C1 C5 Rh1 Cl1 57.7(4) . . . 3_557 ?
C2 C3 Rh1 C21 155.8(4) . . . . ?
C4 C3 Rh1 C21 35.5(5) . . . . ?
C6 C3 Rh1 C21 -65.1(6) . . . . ?
C2 C3 Rh1 C4 120.2(5) . . . . ?
C6 C3 Rh1 C4 -100.6(6) . . . . ?
C2 C3 Rh1 C5 81.8(4) . . . . ?
C4 C3 Rh1 C5 -38.4(4) . . . . ?
C6 C3 Rh1 C5 -139.0(6) . . . . ?
C4 C3 Rh1 C2 -120.2(5) . . . . ?
C6 C3 Rh1 C2 139.2(7) . . . . ?
C2 C3 Rh1 C1 39.7(4) . . . . ?
C4 C3 Rh1 C1 -80.5(4) . . . . ?
C6 C3 Rh1 C1 178.8(6) . . . . ?
C2 C3 Rh1 Cl1 -103.1(4) . . . . ?
C4 C3 Rh1 Cl1 136.7(3) . . . . ?
C6 C3 Rh1 Cl1 36.1(5) . . . . ?
C2 C3 Rh1 Cl1 -15.1(5) . . . 3_557 ?
C4 C3 Rh1 Cl1 -135.3(3) . . . 3_557 ?
C6 C3 Rh1 Cl1 124.1(5) . . . 3_557 ?
C3 C2 Rh1 C21 -62.7(9) . . . . ?
C9 C2 Rh1 C21 174.8(7) . . . . ?
C1 C2 Rh1 C21 50.2(9) . . . . ?
C3 C2 Rh1 C4 -37.0(4) . . . . ?
C9 C2 Rh1 C4 -159.5(7) . . . . ?
C1 C2 Rh1 C4 76.0(4) . . . . ?
C3 C2 Rh1 C5 -80.5(4) . . . . ?
C9 C2 Rh1 C5 157.0(7) . . . . ?
C1 C2 Rh1 C5 32.5(3) . . . . ?
C9 C2 Rh1 C3 -122.5(8) . . . . ?
C1 C2 Rh1 C3 113.0(5) . . . . ?
C3 C2 Rh1 C1 -113.0(5) . . . . ?
C9 C2 Rh1 C1 124.5(7) . . . . ?
C3 C2 Rh1 Cl1 82.7(4) . . . . ?
C9 C2 Rh1 Cl1 -39.8(6) . . . . ?
C1 C2 Rh1 Cl1 -164.3(3) . . . . ?
C3 C2 Rh1 Cl1 169.3(3) . . . 3_557 ?
C9 C2 Rh1 Cl1 46.8(6) . . . 3_557 ?
C1 C2 Rh1 Cl1 -77.8(3) . . . 3_557 ?
O1 C1 Rh1 C21 80.8(8) . . . . ?
C2 C1 Rh1 C21 -160.1(4) . . . . ?
C5 C1 Rh1 C21 -33.4(5) . . . . ?
O1 C1 Rh1 C4 156.4(8) . . . . ?
C2 C1 Rh1 C4 -84.5(4) . . . . ?
C5 C1 Rh1 C4 42.1(4) . . . . ?
O1 C1 Rh1 C5 114.3(9) . . . . ?
C2 C1 Rh1 C5 -126.6(5) . . . . ?
O1 C1 Rh1 C3 -158.8(8) . . . . ?
C2 C1 Rh1 C3 -39.7(4) . . . . ?
C5 C1 Rh1 C3 86.9(4) . . . . ?
O1 C1 Rh1 C2 -119.1(9) . . . . ?
C5 C1 Rh1 C2 126.6(5) . . . . ?
O1 C1 Rh1 Cl1 -96.2(8) . . . . ?
C2 C1 Rh1 Cl1 22.9(4) . . . . ?
C5 C1 Rh1 Cl1 149.6(3) . . . . ?
O1 C1 Rh1 Cl1 -14.1(7) . . . 3_557 ?
C2 C1 Rh1 Cl1 105.0(3) . . . 3_557 ?
C5 C1 Rh1 Cl1 -128.4(4) . . . 3_557 ?
C3 C2 C9 C10 -173.9(6) . . . . ?
C1 C2 C9 C10 20.6(10) . . . . ?
Rh1 C2 C9 C10 -82.6(8) . . . . ?
C3 C2 C9 C14 8.0(10) . . . . ?
C1 C2 C9 C14 -157.5(7) . . . . ?
Rh1 C2 C9 C14 99.4(7) . . . . ?
C14 C9 C10 C11 0.8(10) . . . . ?
C2 C9 C10 C11 -177.3(6) . . . . ?
C9 C10 C11 C12 -1.8(11) . . . . ?
C10 C11 C12 C13 1.1(12) . . . . ?
C11 C12 C13 C14 0.6(13) . . . . ?
C12 C13 C14 C9 -1.5(12) . . . . ?
C10 C9 C14 C13 0.9(11) . . . . ?
C2 C9 C14 C13 179.0(7) . . . . ?
C4 C5 C15 C16 -20.7(12) . . . . ?
C1 C5 C15 C16 144.5(8) . . . . ?
Rh1 C5 C15 C16 -109.3(8) . . . . ?
C4 C5 C15 C20 156.8(10) . . . . ?
C1 C5 C15 C20 -38.0(13) . . . . ?
Rh1 C5 C15 C20 68.2(11) . . . . ?
C20 C15 C16 C17 1.6(15) . . . . ?
C5 C15 C16 C17 179.2(8) . . . . ?
C15 C16 C17 C18 -0.7(16) . . . . ?
C16 C17 C18 C19 -0.2(18) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
C16 C15 C20 C19 -2(2) . . . . ?
C5 C15 C20 C19 -179.1(13) . . . . ?
C18 C19 C20 C15 1(3) . . . . ?
C21 Rh1 Cl1 Rh1 -93.7(2) . . . 3_557 ?
C4 Rh1 Cl1 Rh1 165.3(2) . . . 3_557 ?
C5 Rh1 Cl1 Rh1 147.9(5) . . . 3_557 ?
C3 Rh1 Cl1 Rh1 134.81(17) . . . 3_557 ?
C2 Rh1 Cl1 Rh1 97.83(17) . . . 3_557 ?
C1 Rh1 Cl1 Rh1 83.9(2) . . . 3_557 ?
Cl1 Rh1 Cl1 Rh1 0.0 3_557 . . 3_557 ?
C4 Rh1 C21 O2 -33(5) . . . . ?
C5 Rh1 C21 O2 6(5) . . . . ?
C3 Rh1 C21 O2 -55(5) . . . . ?
C2 Rh1 C21 O2 -10(5) . . . . ?
C1 Rh1 C21 O2 26(5) . . . . ?
Cl1 Rh1 C21 O2 -156(4) . . . . ?
Cl1 Rh1 C21 O2 119(4) 3_557 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         6.350
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.204

#==============================================================================
data_11a(CCDC_752606)
_database_code_depnum_ccdc_archive 'CCDC 752606'
#TrackingRef '11a.cif'

#==============================================================================
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            11a
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H20 O2'
_chemical_formula_weight         364.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.6916(2)
_cell_length_b                   8.6917(2)
_cell_length_c                   24.9284(5)
_cell_angle_alpha                87.5344(12)
_cell_angle_beta                 87.5267(12)
_cell_angle_gamma                89.2463(12)
_cell_volume                     1879.59(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    7100
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      71.65

_exptl_crystal_description       prizm
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8144
_exptl_absorpt_correction_T_max  0.8897
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34157
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         71.65
_reflns_number_total             7100
_reflns_number_gt                5581
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0885P)^2^+0.2680P] 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_extinction_coef       ?
_refine_ls_number_reflns         7100
_refine_ls_number_parameters     513
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1647
_refine_ls_wR_factor_gt          0.1517
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
O1 O 0.14157(15) 0.23051(15) 0.92229(5) 0.0401(3) Uani 1 1 d . . .
O2 O 0.76964(16) 0.85884(14) 0.57767(5) 0.0400(3) Uani 1 1 d . . .
C3 C 0.68220(19) 0.48584(19) 0.54810(6) 0.0272(4) Uani 1 1 d . . .
O4 O 0.07889(19) 0.27182(17) 0.82060(6) 0.0537(4) Uani 1 1 d . . .
C5 C 0.3554(2) 0.36852(19) 0.87587(6) 0.0297(4) Uani 1 1 d . . .
O3 O 0.72838(18) 0.92158(17) 0.67931(6) 0.0537(4) Uani 1 1 d . . .
C7 C 0.5144(2) 0.31764(18) 0.95193(6) 0.0270(4) Uani 1 1 d . . .
C8 C 0.5104(2) 0.39169(19) 0.89932(7) 0.0289(4) Uani 1 1 d . . .
C9 C 0.84591(19) 0.65823(19) 0.48264(7) 0.0286(4) Uani 1 1 d . . .
C10 C 0.6316(2) 0.64526(19) 0.62407(7) 0.0298(4) Uani 1 1 d . . .
C11 C 0.6084(2) 0.48977(19) 0.60057(7) 0.0293(4) Uani 1 1 d . . .
C12 C 0.3419(2) 0.15391(18) 1.01729(7) 0.0289(4) Uani 1 1 d . . .
C57 C 0.2769(2) 0.27010(19) 0.92279(7) 0.0295(4) Uani 1 1 d . . .
C58 C 0.6450(2) 0.33658(19) 0.52378(7) 0.0332(4) Uani 1 1 d . . .
H25 H 0.7402 0.2800 0.5130 0.040 Uiso 1 1 calc R . .
H26 H 0.5819 0.3545 0.4919 0.040 Uiso 1 1 calc R . .
C59 C 0.7299(2) 0.72317(19) 0.57733(7) 0.0299(4) Uani 1 1 d . . .
C60 C 0.75900(19) 0.61803(19) 0.53337(7) 0.0276(4) Uani 1 1 d . . .
C61 C 0.2588(2) -0.0030(2) 1.11499(7) 0.0407(5) Uani 1 1 d . . .
H7 H 0.2295 -0.0544 1.1482 0.049 Uiso 1 1 calc R . .
C62 C 0.3752(2) 0.6712(2) 0.67390(7) 0.0388(4) Uani 1 1 d . . .
H35 H 0.4108 0.5951 0.6990 0.047 Uiso 1 1 calc R . .
C63 C 0.4283(2) 0.1669(2) 1.06298(7) 0.0399(5) Uani 1 1 d . . .
H8 H 0.5170 0.2300 1.0610 0.048 Uiso 1 1 calc R . .
C20 C 1.0024(2) 0.7408(2) 0.38507(7) 0.0403(5) Uani 1 1 d . . .
H9 H 1.0537 0.7702 0.3519 0.048 Uiso 1 1 calc R . .
C21 C 0.3820(2) 0.24056(18) 0.96661(6) 0.0268(4) Uani 1 1 d . . .
C22 C 0.6632(2) 0.3550(2) 0.97620(7) 0.0340(4) Uani 1 1 d . . .
H29 H 0.7199 0.2599 0.9870 0.041 Uiso 1 1 calc R . .
H30 H 0.6452 0.4181 1.0080 0.041 Uiso 1 1 calc R . .
C23 C 0.4729(2) 0.72361(19) 0.63156(7) 0.0306(4) Uani 1 1 d . . .
C24 C 0.3292(2) 0.6250(2) 0.82607(7) 0.0392(4) Uani 1 1 d . . .
H36 H 0.4054 0.5893 0.8010 0.047 Uiso 1 1 calc R . .
C25 C 0.4181(2) 0.83613(19) 0.59576(7) 0.0327(4) Uani 1 1 d . . .
H37 H 0.4838 0.8741 0.5669 0.039 Uiso 1 1 calc R . .
C26 C 0.6416(2) 0.4673(2) 0.88674(7) 0.0366(4) Uani 1 1 d . . .
H31 H 0.6614 0.5262 0.8543 0.044 Uiso 1 1 calc R . .
C27 C 0.9427(2) 0.7855(2) 0.47817(7) 0.0346(4) Uani 1 1 d . . .
H10 H 0.9563 0.8451 0.5086 0.041 Uiso 1 1 calc R . .
C28 C 0.2690(2) 0.8940(2) 0.60150(8) 0.0409(5) Uani 1 1 d . . .
H38 H 0.2333 0.9707 0.5766 0.049 Uiso 1 1 calc R . .
C29 C 0.8327(2) 0.5717(2) 0.43700(7) 0.0399(5) Uani 1 1 d . . .
H11 H 0.7694 0.4832 0.4391 0.048 Uiso 1 1 calc R . .
C30 C 0.5330(2) 0.3590(2) 0.61329(7) 0.0362(4) Uani 1 1 d . . .
H32 H 0.4743 0.3394 0.6459 0.043 Uiso 1 1 calc R . .
C31 C 0.2764(2) 0.52743(19) 0.86845(7) 0.0306(4) Uani 1 1 d . . .
C32 C 0.1064(2) 0.7311(2) 0.89827(8) 0.0408(5) Uani 1 1 d . . .
H39 H 0.0295 0.7668 0.9231 0.049 Uiso 1 1 calc R . .
C33 C 0.1639(2) 0.5821(2) 0.90415(7) 0.0334(4) Uani 1 1 d . . .
H40 H 0.1258 0.5165 0.9330 0.040 Uiso 1 1 calc R . .
C34 C 0.4987(3) 0.2353(2) 0.79894(7) 0.0400(5) Uani 1 1 d . . .
H12 H 0.5922 0.2591 0.8149 0.048 Uiso 1 1 calc R . .
C35 C 0.2237(3) 0.2405(2) 0.79915(8) 0.0418(5) Uani 1 1 d . . .
C36 C 0.5537(2) 0.2469(2) 0.56904(8) 0.0385(4) Uani 1 1 d . . .
H27 H 0.4528 0.2147 0.5567 0.046 Uiso 1 1 calc R . .
H28 H 0.6119 0.1543 0.5814 0.046 Uiso 1 1 calc R . .
C37 C 0.2148(2) 0.0575(2) 1.02182(7) 0.0343(4) Uani 1 1 d . . .
H13 H 0.1551 0.0443 0.9913 0.041 Uiso 1 1 calc R . .
C38 C 0.7527(2) 0.4462(2) 0.93090(8) 0.0388(4) Uani 1 1 d . . .
H33 H 0.7850 0.5470 0.9433 0.047 Uiso 1 1 calc R . .
H34 H 0.8453 0.3879 0.9185 0.047 Uiso 1 1 calc R . .
C39 C 0.3590(2) 0.27914(19) 0.82379(7) 0.0340(4) Uani 1 1 d . . .
C40 C 0.7210(2) 0.6409(2) 0.67619(7) 0.0340(4) Uani 1 1 d . . .
C41 C 0.7651(2) 0.5017(2) 0.70113(7) 0.0403(5) Uani 1 1 d . . .
H14 H 0.7416 0.4082 0.6851 0.048 Uiso 1 1 calc R . .
C42 C 0.2712(3) 0.7738(2) 0.82024(8) 0.0447(5) Uani 1 1 d . . .
H41 H 0.3079 0.8394 0.7911 0.054 Uiso 1 1 calc R . .
C43 C 0.2259(2) 0.7293(2) 0.67976(8) 0.0443(5) Uani 1 1 d . . .
H42 H 0.1602 0.6927 0.7089 0.053 Uiso 1 1 calc R . .
C44 C 0.7592(2) 0.7769(2) 0.70078(8) 0.0427(5) Uani 1 1 d . . .
C45 C 0.1740(2) -0.0197(2) 1.07020(8) 0.0392(4) Uani 1 1 d . . .
H15 H 0.0867 -0.0847 1.0724 0.047 Uiso 1 1 calc R . .
C46 C 0.3694(3) 0.1237(2) 0.72729(8) 0.0549(6) Uani 1 1 d . . .
H16 H 0.3726 0.0717 0.6945 0.066 Uiso 1 1 calc R . .
C47 C 1.0194(2) 0.8258(2) 0.42973(8) 0.0392(4) Uani 1 1 d . . .
H17 H 1.0844 0.9131 0.4274 0.047 Uiso 1 1 calc R . .
C48 C 0.2308(3) 0.1651(2) 0.75085(8) 0.0531(6) Uani 1 1 d . . .
H18 H 0.1381 0.1423 0.7341 0.064 Uiso 1 1 calc R . .
C49 C 0.1604(3) 0.8277(2) 0.85645(8) 0.0440(5) Uani 1 1 d . . .
H43 H 0.1219 0.9302 0.8526 0.053 Uiso 1 1 calc R . .
C50 C 0.5041(3) 0.1574(2) 0.75117(8) 0.0500(6) Uani 1 1 d . . .
H19 H 0.6004 0.1277 0.7351 0.060 Uiso 1 1 calc R . .
C51 C 0.8759(2) 0.6304(3) 0.77263(8) 0.0560(6) Uani 1 1 d . . .
H20 H 0.9277 0.6270 0.8055 0.067 Uiso 1 1 calc R . .
C52 C 0.8423(2) 0.4955(3) 0.74871(8) 0.0496(5) Uani 1 1 d . . .
H21 H 0.8717 0.3990 0.7647 0.060 Uiso 1 1 calc R . .
C53 C 0.3870(3) 0.0895(2) 1.11093(8) 0.0477(5) Uani 1 1 d . . .
H22 H 0.4473 0.1001 1.1414 0.057 Uiso 1 1 calc R . .
C54 C 0.9101(3) 0.6126(3) 0.38903(8) 0.0476(5) Uani 1 1 d . . .
H23 H 0.8996 0.5521 0.3586 0.057 Uiso 1 1 calc R . .
C55 C 0.8344(2) 0.7702(3) 0.74888(8) 0.0534(6) Uani 1 1 d . . .
H24 H 0.8574 0.8629 0.7656 0.064 Uiso 1 1 calc R . .
C56 C 0.1724(2) 0.8400(2) 0.64348(8) 0.0436(5) Uani 1 1 d . . .
H44 H 0.0700 0.8788 0.6473 0.052 Uiso 1 1 calc R . .
H46 H 0.090(4) 0.277(3) 0.8661(13) 0.100(10) Uiso 1 1 d . . .
H45 H 0.717(4) 0.907(4) 0.6329(15) 0.119(12) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0327(8) 0.0421(7) 0.0460(8) 0.0079(6) -0.0124(6) -0.0119(6)
O2 0.0432(8) 0.0311(7) 0.0460(7) -0.0110(5) 0.0069(6) -0.0118(6)
C3 0.0231(9) 0.0269(8) 0.0321(8) -0.0016(6) -0.0080(7) 0.0012(7)
O4 0.0557(10) 0.0535(9) 0.0538(9) 0.0007(7) -0.0243(8) -0.0082(7)
C5 0.0320(10) 0.0299(8) 0.0275(8) -0.0014(7) -0.0045(7) -0.0031(7)
O3 0.0549(10) 0.0527(9) 0.0555(9) -0.0236(7) -0.0007(7) -0.0074(7)
C7 0.0272(9) 0.0237(8) 0.0306(8) -0.0058(6) -0.0031(7) 0.0014(7)
C8 0.0282(9) 0.0284(8) 0.0305(8) -0.0047(6) -0.0020(7) 0.0013(7)
C9 0.0242(9) 0.0315(8) 0.0305(8) -0.0005(7) -0.0056(7) 0.0020(7)
C10 0.0291(10) 0.0314(9) 0.0295(8) -0.0035(7) -0.0044(7) -0.0042(7)
C11 0.0282(10) 0.0292(8) 0.0308(8) 0.0005(7) -0.0069(7) -0.0003(7)
C12 0.0335(10) 0.0231(8) 0.0303(8) -0.0035(6) -0.0025(7) 0.0009(7)
C57 0.0295(10) 0.0260(8) 0.0335(9) -0.0023(6) -0.0054(7) -0.0057(7)
C58 0.0350(10) 0.0271(8) 0.0388(9) -0.0053(7) -0.0115(8) 0.0001(7)
C59 0.0268(9) 0.0302(9) 0.0333(9) -0.0042(7) -0.0037(7) -0.0043(7)
C60 0.0247(9) 0.0288(8) 0.0300(8) -0.0031(7) -0.0070(7) 0.0007(7)
C61 0.0507(13) 0.0366(10) 0.0337(10) 0.0040(8) 0.0034(9) 0.0047(9)
C62 0.0357(11) 0.0447(11) 0.0357(9) -0.0024(8) 0.0021(8) -0.0024(8)
C63 0.0455(12) 0.0387(10) 0.0361(10) 0.0021(8) -0.0093(8) -0.0093(9)
C20 0.0347(11) 0.0510(11) 0.0341(10) 0.0044(8) 0.0034(8) 0.0043(9)
C21 0.0284(9) 0.0235(8) 0.0292(8) -0.0055(6) -0.0043(7) 0.0008(7)
C22 0.0287(10) 0.0347(9) 0.0397(10) -0.0087(7) -0.0076(7) 0.0009(7)
C23 0.0292(10) 0.0310(9) 0.0326(9) -0.0089(7) -0.0038(7) -0.0036(7)
C24 0.0472(12) 0.0350(10) 0.0353(9) 0.0031(7) -0.0030(8) -0.0040(9)
C25 0.0337(10) 0.0303(9) 0.0347(9) -0.0065(7) -0.0031(7) -0.0029(7)
C26 0.0339(11) 0.0367(10) 0.0388(10) -0.0021(8) 0.0034(8) -0.0050(8)
C27 0.0328(10) 0.0344(9) 0.0367(9) -0.0029(7) -0.0013(8) -0.0027(8)
C28 0.0393(11) 0.0367(10) 0.0478(11) -0.0097(8) -0.0074(9) 0.0021(8)
C29 0.0386(11) 0.0459(11) 0.0357(9) -0.0079(8) 0.0002(8) -0.0096(9)
C30 0.0363(11) 0.0331(9) 0.0388(10) 0.0056(7) -0.0034(8) -0.0043(8)
C31 0.0316(10) 0.0297(9) 0.0315(8) -0.0025(7) -0.0104(7) -0.0041(7)
C32 0.0381(11) 0.0375(10) 0.0481(11) -0.0067(8) -0.0110(9) 0.0015(8)
C33 0.0313(10) 0.0346(9) 0.0351(9) -0.0030(7) -0.0085(7) -0.0038(8)
C34 0.0569(13) 0.0297(9) 0.0332(9) -0.0015(7) 0.0001(9) -0.0014(9)
C35 0.0519(13) 0.0386(10) 0.0355(10) 0.0024(8) -0.0114(9) -0.0065(9)
C36 0.0391(11) 0.0276(9) 0.0495(11) -0.0007(8) -0.0078(9) -0.0035(8)
C37 0.0344(11) 0.0323(9) 0.0364(9) -0.0001(7) -0.0044(8) -0.0025(8)
C38 0.0273(10) 0.0395(10) 0.0501(11) -0.0071(8) -0.0010(8) -0.0032(8)
C39 0.0475(12) 0.0275(8) 0.0274(8) -0.0009(7) -0.0065(8) -0.0032(8)
C40 0.0255(10) 0.0485(11) 0.0283(8) -0.0048(7) -0.0013(7) -0.0040(8)
C41 0.0293(10) 0.0569(12) 0.0348(10) 0.0005(8) -0.0026(8) -0.0013(9)
C42 0.0550(14) 0.0352(10) 0.0441(11) 0.0056(8) -0.0110(9) -0.0076(9)
C43 0.0359(11) 0.0530(12) 0.0442(11) -0.0096(9) 0.0050(9) -0.0082(9)
C44 0.0371(11) 0.0548(12) 0.0370(10) -0.0125(9) 0.0005(8) -0.0075(9)
C45 0.0379(11) 0.0331(9) 0.0455(11) 0.0049(8) 0.0036(8) -0.0012(8)
C46 0.102(2) 0.0331(10) 0.0303(10) -0.0026(8) -0.0029(11) -0.0188(12)
C47 0.0330(11) 0.0373(10) 0.0465(11) 0.0040(8) 0.0037(8) -0.0010(8)
C48 0.0831(18) 0.0401(11) 0.0377(11) 0.0010(8) -0.0196(11) -0.0187(11)
C49 0.0495(13) 0.0293(9) 0.0547(12) -0.0017(8) -0.0195(10) -0.0003(8)
C50 0.0815(17) 0.0316(10) 0.0363(10) -0.0047(8) 0.0086(10) -0.0040(10)
C51 0.0326(12) 0.105(2) 0.0306(10) -0.0022(11) -0.0045(8) -0.0196(12)
C52 0.0327(11) 0.0800(16) 0.0356(10) 0.0096(10) -0.0061(8) -0.0039(11)
C53 0.0599(14) 0.0510(12) 0.0327(10) 0.0024(8) -0.0118(9) -0.0072(10)
C54 0.0497(13) 0.0614(13) 0.0324(10) -0.0093(9) 0.0003(9) -0.0073(10)
C55 0.0400(13) 0.0837(17) 0.0385(11) -0.0191(11) -0.0001(9) -0.0217(12)
C56 0.0287(10) 0.0483(11) 0.0554(12) -0.0176(9) -0.0032(9) 0.0001(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C57 1.231(2) . ?
O2 C59 1.234(2) . ?
C3 C60 1.365(2) . ?
C3 C11 1.434(2) . ?
C3 C58 1.500(2) . ?
O4 C35 1.375(3) . ?
O4 H46 1.15(3) . ?
C5 C8 1.511(2) . ?
C5 C39 1.540(2) . ?
C5 C31 1.542(2) . ?
C5 C57 1.557(2) . ?
O3 C44 1.373(3) . ?
O3 H45 1.18(4) . ?
C7 C21 1.367(2) . ?
C7 C8 1.437(2) . ?
C7 C22 1.496(2) . ?
C8 C26 1.342(2) . ?
C9 C27 1.397(2) . ?
C9 C29 1.400(2) . ?
C9 C60 1.476(2) . ?
C10 C11 1.515(2) . ?
C10 C23 1.538(2) . ?
C10 C40 1.541(2) . ?
C10 C59 1.551(2) . ?
C11 C30 1.339(2) . ?
C12 C37 1.393(2) . ?
C12 C63 1.401(2) . ?
C12 C21 1.474(2) . ?
C57 C21 1.466(2) . ?
C58 C36 1.540(3) . ?
C58 H25 0.9900 . ?
C58 H26 0.9900 . ?
C59 C60 1.468(2) . ?
C61 C45 1.378(3) . ?
C61 C53 1.380(3) . ?
C61 H7 0.9500 . ?
C62 C23 1.391(2) . ?
C62 C43 1.390(3) . ?
C62 H35 0.9500 . ?
C63 C53 1.382(3) . ?
C63 H8 0.9500 . ?
C20 C54 1.380(3) . ?
C20 C47 1.377(3) . ?
C20 H9 0.9500 . ?
C22 C38 1.540(3) . ?
C22 H29 0.9900 . ?
C22 H30 0.9900 . ?
C23 C25 1.389(3) . ?
C24 C42 1.386(3) . ?
C24 C31 1.392(2) . ?
C24 H36 0.9500 . ?
C25 C28 1.388(3) . ?
C25 H37 0.9500 . ?
C26 C38 1.499(3) . ?
C26 H31 0.9500 . ?
C27 C47 1.388(2) . ?
C27 H10 0.9500 . ?
C28 C56 1.383(3) . ?
C28 H38 0.9500 . ?
C29 C54 1.382(3) . ?
C29 H11 0.9500 . ?
C30 C36 1.506(3) . ?
C30 H32 0.9500 . ?
C31 C33 1.386(3) . ?
C32 C49 1.380(3) . ?
C32 C33 1.386(3) . ?
C32 H39 0.9500 . ?
C33 H40 0.9500 . ?
C34 C39 1.395(3) . ?
C34 C50 1.394(3) . ?
C34 H12 0.9500 . ?
C35 C48 1.394(3) . ?
C35 C39 1.401(3) . ?
C36 H27 0.9900 . ?
C36 H28 0.9900 . ?
C37 C45 1.389(2) . ?
C37 H13 0.9500 . ?
C38 H33 0.9900 . ?
C38 H34 0.9900 . ?
C40 C41 1.393(3) . ?
C40 C44 1.405(3) . ?
C41 C52 1.386(3) . ?
C41 H14 0.9500 . ?
C42 C49 1.382(3) . ?
C42 H41 0.9500 . ?
C43 C56 1.382(3) . ?
C43 H42 0.9500 . ?
C44 C55 1.389(3) . ?
C45 H15 0.9500 . ?
C46 C48 1.368(4) . ?
C46 C50 1.377(3) . ?
C46 H16 0.9500 . ?
C47 H17 0.9500 . ?
C48 H18 0.9500 . ?
C49 H43 0.9500 . ?
C50 H19 0.9500 . ?
C51 C52 1.378(3) . ?
C51 C55 1.380(4) . ?
C51 H20 0.9500 . ?
C52 H21 0.9500 . ?
C53 H22 0.9500 . ?
C54 H23 0.9500 . ?
C55 H24 0.9500 . ?
C56 H44 0.9500 . ?

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
C60 C3 C11 113.08(15) . . ?
C60 C3 C58 138.01(16) . . ?
C11 C3 C58 108.83(15) . . ?
C35 O4 H46 106.7(16) . . ?
C8 C5 C39 115.24(15) . . ?
C8 C5 C31 108.20(13) . . ?
C39 C5 C31 111.73(13) . . ?
C8 C5 C57 99.43(13) . . ?
C39 C5 C57 109.99(13) . . ?
C31 C5 C57 111.68(14) . . ?
C44 O3 H45 106.0(17) . . ?
C21 C7 C8 113.01(15) . . ?
C21 C7 C22 138.08(16) . . ?
C8 C7 C22 108.83(15) . . ?
C26 C8 C7 111.09(16) . . ?
C26 C8 C5 138.74(16) . . ?
C7 C8 C5 110.05(15) . . ?
C27 C9 C29 117.51(16) . . ?
C27 C9 C60 121.16(15) . . ?
C29 C9 C60 121.32(16) . . ?
C11 C10 C23 108.07(14) . . ?
C11 C10 C40 114.97(14) . . ?
C23 C10 C40 111.82(13) . . ?
C11 C10 C59 99.37(13) . . ?
C23 C10 C59 111.93(14) . . ?
C40 C10 C59 110.09(14) . . ?
C30 C11 C3 111.27(16) . . ?
C30 C11 C10 138.60(17) . . ?
C3 C11 C10 110.01(14) . . ?
C37 C12 C63 117.36(16) . . ?
C37 C12 C21 121.18(15) . . ?
C63 C12 C21 121.45(16) . . ?
O1 C57 C21 126.46(16) . . ?
O1 C57 C5 122.24(15) . . ?
C21 C57 C5 111.23(14) . . ?
C3 C58 C36 104.10(14) . . ?
C3 C58 H25 110.9 . . ?
C36 C58 H25 110.9 . . ?
C3 C58 H26 110.9 . . ?
C36 C58 H26 110.9 . . ?
H25 C58 H26 109.0 . . ?
O2 C59 C60 126.27(16) . . ?
O2 C59 C10 122.35(15) . . ?
C60 C59 C10 111.29(14) . . ?
C3 C60 C59 106.16(15) . . ?
C3 C60 C9 129.01(15) . . ?
C59 C60 C9 124.70(14) . . ?
C45 C61 C53 119.05(18) . . ?
C45 C61 H7 120.5 . . ?
C53 C61 H7 120.5 . . ?
C23 C62 C43 120.61(19) . . ?
C23 C62 H35 119.7 . . ?
C43 C62 H35 119.7 . . ?
C53 C63 C12 121.19(18) . . ?
C53 C63 H8 119.4 . . ?
C12 C63 H8 119.4 . . ?
C54 C20 C47 119.33(17) . . ?
C54 C20 H9 120.3 . . ?
C47 C20 H9 120.3 . . ?
C7 C21 C57 106.19(14) . . ?
C7 C21 C12 128.94(16) . . ?
C57 C21 C12 124.72(15) . . ?
C7 C22 C38 104.03(14) . . ?
C7 C22 H29 111.0 . . ?
C38 C22 H29 111.0 . . ?
C7 C22 H30 111.0 . . ?
C38 C22 H30 111.0 . . ?
H29 C22 H30 109.0 . . ?
C25 C23 C62 118.35(17) . . ?
C25 C23 C10 123.07(16) . . ?
C62 C23 C10 118.40(16) . . ?
C42 C24 C31 120.44(19) . . ?
C42 C24 H36 119.8 . . ?
C31 C24 H36 119.8 . . ?
C28 C25 C23 121.09(18) . . ?
C28 C25 H37 119.5 . . ?
C23 C25 H37 119.5 . . ?
C8 C26 C38 110.81(16) . . ?
C8 C26 H31 124.6 . . ?
C38 C26 H31 124.6 . . ?
C47 C27 C9 120.74(17) . . ?
C47 C27 H10 119.6 . . ?
C9 C27 H10 119.6 . . ?
C56 C28 C25 120.04(19) . . ?
C56 C28 H38 120.0 . . ?
C25 C28 H38 120.0 . . ?
C54 C29 C9 121.23(18) . . ?
C54 C29 H11 119.4 . . ?
C9 C29 H11 119.4 . . ?
C11 C30 C36 110.91(16) . . ?
C11 C30 H32 124.5 . . ?
C36 C30 H32 124.5 . . ?
C33 C31 C24 118.51(17) . . ?
C33 C31 C5 123.21(15) . . ?
C24 C31 C5 118.09(16) . . ?
C49 C32 C33 120.26(19) . . ?
C49 C32 H39 119.9 . . ?
C33 C32 H39 119.9 . . ?
C32 C33 C31 120.90(18) . . ?
C32 C33 H40 119.5 . . ?
C31 C33 H40 119.5 . . ?
C39 C34 C50 121.5(2) . . ?
C39 C34 H12 119.2 . . ?
C50 C34 H12 119.2 . . ?
O4 C35 C48 116.4(2) . . ?
O4 C35 C39 123.13(17) . . ?
C48 C35 C39 120.5(2) . . ?
C30 C36 C58 104.57(14) . . ?
C30 C36 H27 110.8 . . ?
C58 C36 H27 110.8 . . ?
C30 C36 H28 110.8 . . ?
C58 C36 H28 110.8 . . ?
H27 C36 H28 108.9 . . ?
C45 C37 C12 121.04(17) . . ?
C45 C37 H13 119.5 . . ?
C12 C37 H13 119.5 . . ?
C26 C38 C22 104.91(15) . . ?
C26 C38 H33 110.8 . . ?
C22 C38 H33 110.8 . . ?
C26 C38 H34 110.8 . . ?
C22 C38 H34 110.8 . . ?
H33 C38 H34 108.8 . . ?
C34 C39 C35 117.41(17) . . ?
C34 C39 C5 120.76(17) . . ?
C35 C39 C5 121.82(17) . . ?
C41 C40 C44 117.42(18) . . ?
C41 C40 C10 121.24(16) . . ?
C44 C40 C10 121.33(17) . . ?
C52 C41 C40 122.0(2) . . ?
C52 C41 H14 119.0 . . ?
C40 C41 H14 119.0 . . ?
C49 C42 C24 120.55(19) . . ?
C49 C42 H41 119.7 . . ?
C24 C42 H41 119.7 . . ?
C56 C43 C62 120.37(19) . . ?
C56 C43 H42 119.8 . . ?
C62 C43 H42 119.8 . . ?
O3 C44 C55 116.18(19) . . ?
O3 C44 C40 123.40(18) . . ?
C55 C44 C40 120.4(2) . . ?
C61 C45 C37 120.68(18) . . ?
C61 C45 H15 119.7 . . ?
C37 C45 H15 119.7 . . ?
C48 C46 C50 119.90(19) . . ?
C48 C46 H16 120.1 . . ?
C50 C46 H16 120.1 . . ?
C20 C47 C27 120.76(18) . . ?
C20 C47 H17 119.6 . . ?
C27 C47 H17 119.6 . . ?
C46 C48 C35 120.8(2) . . ?
C46 C48 H18 119.6 . . ?
C35 C48 H18 119.6 . . ?
C32 C49 C42 119.33(19) . . ?
C32 C49 H43 120.3 . . ?
C42 C49 H43 120.3 . . ?
C46 C50 C34 119.8(2) . . ?
C46 C50 H19 120.1 . . ?
C34 C50 H19 120.1 . . ?
C52 C51 C55 120.0(2) . . ?
C52 C51 H20 120.0 . . ?
C55 C51 H20 120.0 . . ?
C51 C52 C41 119.5(2) . . ?
C51 C52 H21 120.2 . . ?
C41 C52 H21 120.2 . . ?
C63 C53 C61 120.65(19) . . ?
C63 C53 H22 119.7 . . ?
C61 C53 H22 119.7 . . ?
C20 C54 C29 120.40(18) . . ?
C20 C54 H23 119.8 . . ?
C29 C54 H23 119.8 . . ?
C51 C55 C44 120.6(2) . . ?
C51 C55 H24 119.7 . . ?
C44 C55 H24 119.7 . . ?
C43 C56 C28 119.53(19) . . ?
C43 C56 H44 120.2 . . ?
C28 C56 H44 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 C7 C8 C26 179.31(15) . . . . ?
C22 C7 C8 C26 2.1(2) . . . . ?
C21 C7 C8 C5 2.53(19) . . . . ?
C22 C7 C8 C5 -174.69(13) . . . . ?
C39 C5 C8 C26 66.4(3) . . . . ?
C31 C5 C8 C26 -59.4(3) . . . . ?
C57 C5 C8 C26 -176.1(2) . . . . ?
C39 C5 C8 C7 -118.11(15) . . . . ?
C31 C5 C8 C7 116.03(15) . . . . ?
C57 C5 C8 C7 -0.64(16) . . . . ?
C60 C3 C11 C30 179.32(16) . . . . ?
C58 C3 C11 C30 2.1(2) . . . . ?
C60 C3 C11 C10 2.5(2) . . . . ?
C58 C3 C11 C10 -174.77(14) . . . . ?
C23 C10 C11 C30 -59.4(3) . . . . ?
C40 C10 C11 C30 66.2(3) . . . . ?
C59 C10 C11 C30 -176.3(2) . . . . ?
C23 C10 C11 C3 116.15(15) . . . . ?
C40 C10 C11 C3 -118.18(16) . . . . ?
C59 C10 C11 C3 -0.73(18) . . . . ?
C8 C5 C57 O1 175.90(16) . . . . ?
C39 C5 C57 O1 -62.7(2) . . . . ?
C31 C5 C57 O1 61.9(2) . . . . ?
C8 C5 C57 C21 -1.26(17) . . . . ?
C39 C5 C57 C21 120.09(15) . . . . ?
C31 C5 C57 C21 -115.26(15) . . . . ?
C60 C3 C58 C36 179.0(2) . . . . ?
C11 C3 C58 C36 -4.81(18) . . . . ?
C11 C10 C59 O2 175.80(17) . . . . ?
C23 C10 C59 O2 61.9(2) . . . . ?
C40 C10 C59 O2 -63.1(2) . . . . ?
C11 C10 C59 C60 -1.03(18) . . . . ?
C23 C10 C59 C60 -114.95(15) . . . . ?
C40 C10 C59 C60 120.03(16) . . . . ?
C11 C3 C60 C59 -3.0(2) . . . . ?
C58 C3 C60 C59 173.06(19) . . . . ?
C11 C3 C60 C9 -178.91(16) . . . . ?
C58 C3 C60 C9 -2.8(3) . . . . ?
O2 C59 C60 C3 -174.20(18) . . . . ?
C10 C59 C60 C3 2.48(19) . . . . ?
O2 C59 C60 C9 1.9(3) . . . . ?
C10 C59 C60 C9 178.61(15) . . . . ?
C27 C9 C60 C3 -167.14(18) . . . . ?
C29 C9 C60 C3 13.8(3) . . . . ?
C27 C9 C60 C59 17.6(3) . . . . ?
C29 C9 C60 C59 -161.40(18) . . . . ?
C37 C12 C63 C53 -1.4(3) . . . . ?
C21 C12 C63 C53 177.70(18) . . . . ?
C8 C7 C21 C57 -3.23(18) . . . . ?
C22 C7 C21 C57 172.83(19) . . . . ?
C8 C7 C21 C12 -178.81(15) . . . . ?
C22 C7 C21 C12 -2.7(3) . . . . ?
O1 C57 C21 C7 -174.25(17) . . . . ?
C5 C57 C21 C7 2.77(18) . . . . ?
O1 C57 C21 C12 1.6(3) . . . . ?
C5 C57 C21 C12 178.58(14) . . . . ?
C37 C12 C21 C7 -167.35(17) . . . . ?
C63 C12 C21 C7 13.6(3) . . . . ?
C37 C12 C21 C57 17.8(2) . . . . ?
C63 C12 C21 C57 -161.23(17) . . . . ?
C21 C7 C22 C38 178.95(19) . . . . ?
C8 C7 C22 C38 -4.88(18) . . . . ?
C43 C62 C23 C25 0.6(3) . . . . ?
C43 C62 C23 C10 -174.61(16) . . . . ?
C11 C10 C23 C25 -100.07(18) . . . . ?
C40 C10 C23 C25 132.41(17) . . . . ?
C59 C10 C23 C25 8.4(2) . . . . ?
C11 C10 C23 C62 74.92(18) . . . . ?
C40 C10 C23 C62 -52.6(2) . . . . ?
C59 C10 C23 C62 -176.65(15) . . . . ?
C62 C23 C25 C28 -0.8(2) . . . . ?
C10 C23 C25 C28 174.24(16) . . . . ?
C7 C8 C26 C38 1.8(2) . . . . ?
C5 C8 C26 C38 177.25(19) . . . . ?
C29 C9 C27 C47 1.6(3) . . . . ?
C60 C9 C27 C47 -177.52(16) . . . . ?
C23 C25 C28 C56 0.2(3) . . . . ?
C27 C9 C29 C54 -1.3(3) . . . . ?
C60 C9 C29 C54 177.76(18) . . . . ?
C3 C11 C30 C36 1.7(2) . . . . ?
C10 C11 C30 C36 177.3(2) . . . . ?
C42 C24 C31 C33 0.6(3) . . . . ?
C42 C24 C31 C5 -174.55(17) . . . . ?
C8 C5 C31 C33 -100.05(19) . . . . ?
C39 C5 C31 C33 132.06(17) . . . . ?
C57 C5 C31 C33 8.4(2) . . . . ?
C8 C5 C31 C24 74.90(18) . . . . ?
C39 C5 C31 C24 -53.0(2) . . . . ?
C57 C5 C31 C24 -176.67(15) . . . . ?
C49 C32 C33 C31 0.1(3) . . . . ?
C24 C31 C33 C32 -0.8(3) . . . . ?
C5 C31 C33 C32 174.16(16) . . . . ?
C11 C30 C36 C58 -4.7(2) . . . . ?
C3 C58 C36 C30 5.54(18) . . . . ?
C63 C12 C37 C45 1.4(3) . . . . ?
C21 C12 C37 C45 -177.64(16) . . . . ?
C8 C26 C38 C22 -4.8(2) . . . . ?
C7 C22 C38 C26 5.68(18) . . . . ?
C50 C34 C39 C35 0.6(3) . . . . ?
C50 C34 C39 C5 -178.55(16) . . . . ?
O4 C35 C39 C34 177.45(17) . . . . ?
C48 C35 C39 C34 -1.8(3) . . . . ?
O4 C35 C39 C5 -3.4(3) . . . . ?
C48 C35 C39 C5 177.34(16) . . . . ?
C8 C5 C39 C34 -4.8(2) . . . . ?
C31 C5 C39 C34 119.19(18) . . . . ?
C57 C5 C39 C34 -116.18(18) . . . . ?
C8 C5 C39 C35 176.05(16) . . . . ?
C31 C5 C39 C35 -59.9(2) . . . . ?
C57 C5 C39 C35 64.7(2) . . . . ?
C11 C10 C40 C41 -4.7(2) . . . . ?
C23 C10 C40 C41 118.98(18) . . . . ?
C59 C10 C40 C41 -115.94(18) . . . . ?
C11 C10 C40 C44 176.17(16) . . . . ?
C23 C10 C40 C44 -60.1(2) . . . . ?
C59 C10 C40 C44 65.0(2) . . . . ?
C44 C40 C41 C52 0.7(3) . . . . ?
C10 C40 C41 C52 -178.41(17) . . . . ?
C31 C24 C42 C49 0.1(3) . . . . ?
C23 C62 C43 C56 0.1(3) . . . . ?
C41 C40 C44 O3 177.20(17) . . . . ?
C10 C40 C44 O3 -3.7(3) . . . . ?
C41 C40 C44 C55 -1.7(3) . . . . ?
C10 C40 C44 C55 177.40(17) . . . . ?
C53 C61 C45 C37 -1.2(3) . . . . ?
C12 C37 C45 C61 -0.2(3) . . . . ?
C54 C20 C47 C27 -1.2(3) . . . . ?
C9 C27 C47 C20 -0.3(3) . . . . ?
C50 C46 C48 C35 -0.5(3) . . . . ?
O4 C35 C48 C46 -177.52(18) . . . . ?
C39 C35 C48 C46 1.8(3) . . . . ?
C33 C32 C49 C42 0.7(3) . . . . ?
C24 C42 C49 C32 -0.8(3) . . . . ?
C48 C46 C50 C34 -0.7(3) . . . . ?
C39 C34 C50 C46 0.7(3) . . . . ?
C55 C51 C52 C41 -0.7(3) . . . . ?
C40 C41 C52 C51 0.5(3) . . . . ?
C12 C63 C53 C61 0.0(3) . . . . ?
C45 C61 C53 C63 1.2(3) . . . . ?
C47 C20 C54 C29 1.4(3) . . . . ?
C9 C29 C54 C20 -0.1(3) . . . . ?
C52 C51 C55 C44 -0.3(3) . . . . ?
O3 C44 C55 C51 -177.46(19) . . . . ?
C40 C44 C55 C51 1.5(3) . . . . ?
C62 C43 C56 C28 -0.7(3) . . . . ?
C25 C28 C56 C43 0.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        71.65
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.061