# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2008


data_global

_journal_coden_Cambridge         177
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Andrew D Smith'
'Carmen Concellon'
'Caroline Joannesse'
'Carmen Simal'
'A Slawin'
'Jennifer E. Thomson'

_publ_contact_author_name        'Andrew D Smith'
_publ_contact_author_email       ADS10@ST-ANDREWS.AC.UK

_publ_section_title              
;
Amidine catalysed O- to C-carboxyl transfer of
heterocyclic carbonate derivatives
;

# Attachment '57.cif'

data_57
_database_code_depnum_ccdc_archive 'CCDC 684299'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H21 N O3'
_chemical_formula_sum            'C28 H21 N O3'
_chemical_formula_weight         419.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.312(3)
_cell_length_b                   8.6180(17)
_cell_length_c                   19.427(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.393(5)
_cell_angle_gamma                90.00
_cell_volume                     2168.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    6084
_cell_measurement_theta_min      1.5724
_cell_measurement_theta_max      28.5427

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.0800
_exptl_crystal_size_min          0.0500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9367
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13730
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.35
_reflns_number_total             3960
_reflns_number_gt                2745
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0646P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3960
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1537
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.14692(14) 0.1744(2) 0.24824(9) 0.0284(5) Uani 1 1 d . . .
C2 C -0.11496(17) 0.2717(3) 0.30430(12) 0.0300(5) Uani 1 1 d . . .
O2 O -0.12841(12) 0.41157(19) 0.30416(8) 0.0364(4) Uani 1 1 d . . .
C3 C -0.05772(16) 0.1735(3) 0.36845(11) 0.0265(5) Uani 1 1 d . . .
C4 C -0.06052(16) 0.0132(3) 0.33595(11) 0.0279(5) Uani 1 1 d . . .
C5 C -0.02059(17) -0.1263(3) 0.36531(12) 0.0312(6) Uani 1 1 d . . .
H5A H 0.0160 -0.1321 0.4134 0.037 Uiso 1 1 calc R . .
C6 C -0.03534(17) -0.2582(3) 0.32255(13) 0.0330(6) Uani 1 1 d . . .
H6A H -0.0089 -0.3553 0.3418 0.040 Uiso 1 1 calc R . .
C7 C -0.08804(18) -0.2489(3) 0.25255(13) 0.0344(6) Uani 1 1 d . . .
H7A H -0.0973 -0.3402 0.2244 0.041 Uiso 1 1 calc R . .
C8 C -0.12805(17) -0.1087(3) 0.22219(12) 0.0313(6) Uani 1 1 d . . .
H8A H -0.1637 -0.1025 0.1739 0.038 Uiso 1 1 calc R . .
C9 C -0.11351(16) 0.0208(3) 0.26545(12) 0.0284(5) Uani 1 1 d . . .
C10 C -0.20079(17) 0.2273(3) 0.17860(12) 0.0318(6) Uani 1 1 d . . .
H10A H -0.2312 0.3306 0.1831 0.038 Uiso 1 1 calc R . .
H10B H -0.2581 0.1548 0.1594 0.038 Uiso 1 1 calc R . .
C11 C -0.13163(17) 0.2384(3) 0.12705(12) 0.0300(5) Uani 1 1 d . . .
C12 C -0.04344(18) 0.3296(3) 0.14167(13) 0.0389(6) Uani 1 1 d . . .
H12A H -0.0246 0.3843 0.1852 0.047 Uiso 1 1 calc R . .
C13 C 0.01728(19) 0.3409(3) 0.09272(14) 0.0435(7) Uani 1 1 d . . .
H13A H 0.0774 0.4042 0.1028 0.052 Uiso 1 1 calc R . .
C14 C -0.0086(2) 0.2617(3) 0.02976(14) 0.0456(7) Uani 1 1 d . . .
H14A H 0.0335 0.2698 -0.0035 0.055 Uiso 1 1 calc R . .
C15 C -0.0954(2) 0.1708(4) 0.01521(14) 0.0528(8) Uani 1 1 d . . .
H15A H -0.1136 0.1150 -0.0281 0.063 Uiso 1 1 calc R . .
C16 C -0.1566(2) 0.1606(3) 0.06384(13) 0.0443(7) Uani 1 1 d . . .
H16A H -0.2172 0.0984 0.0531 0.053 Uiso 1 1 calc R . .
C17 C 0.05367(18) 0.2319(3) 0.38837(13) 0.0303(5) Uani 1 1 d . . .
O17 O 0.10429(12) 0.26230(19) 0.44582(9) 0.0377(4) Uani 1 1 d . . .
O18 O 0.08845(12) 0.2426(2) 0.32774(8) 0.0426(5) Uani 1 1 d . . .
C19 C 0.18931(18) 0.2995(3) 0.33179(12) 0.0360(6) Uani 1 1 d . . .
C20 C 0.2690(2) 0.1952(3) 0.33703(13) 0.0422(6) Uani 1 1 d . . .
H20A H 0.2582 0.0876 0.3431 0.051 Uiso 1 1 calc R . .
C21 C 0.3658(2) 0.2511(3) 0.33327(14) 0.0455(7) Uani 1 1 d . . .
H21A H 0.4214 0.1806 0.3359 0.055 Uiso 1 1 calc R . .
C22 C 0.38148(19) 0.4071(3) 0.32586(13) 0.0429(7) Uani 1 1 d . . .
H22A H 0.4479 0.4445 0.3238 0.051 Uiso 1 1 calc R . .
C23 C 0.30037(19) 0.5095(3) 0.32136(12) 0.0413(6) Uani 1 1 d . . .
H23A H 0.3111 0.6176 0.3165 0.050 Uiso 1 1 calc R . .
C24 C 0.20324(19) 0.4549(3) 0.32396(12) 0.0381(6) Uani 1 1 d . . .
H24A H 0.1471 0.5249 0.3203 0.046 Uiso 1 1 calc R . .
C25 C -0.11387(16) 0.1908(3) 0.42849(11) 0.0286(5) Uani 1 1 d . . .
C26 C -0.17309(18) 0.0707(3) 0.44595(12) 0.0350(6) Uani 1 1 d . . .
H26A H -0.1750 -0.0267 0.4228 0.042 Uiso 1 1 calc R . .
C27 C -0.22973(18) 0.0923(3) 0.49730(12) 0.0389(6) Uani 1 1 d . . .
H27A H -0.2702 0.0098 0.5089 0.047 Uiso 1 1 calc R . .
C28 C -0.22705(18) 0.2336(3) 0.53144(13) 0.0377(6) Uani 1 1 d . . .
H28A H -0.2657 0.2484 0.5664 0.045 Uiso 1 1 calc R . .
C29 C -0.16773(17) 0.3537(3) 0.51444(12) 0.0338(6) Uani 1 1 d . . .
H29A H -0.1654 0.4506 0.5380 0.041 Uiso 1 1 calc R . .
C30 C -0.11202(17) 0.3329(3) 0.46333(12) 0.0318(6) Uani 1 1 d . . .
H30A H -0.0721 0.4161 0.4518 0.038 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0320(11) 0.0270(11) 0.0255(11) 0.0025(8) 0.0052(8) 0.0004(8)
C2 0.0308(13) 0.0297(15) 0.0304(13) -0.0005(11) 0.0088(10) -0.0014(10)
O2 0.0444(10) 0.0250(10) 0.0386(10) 0.0021(7) 0.0074(7) -0.0001(7)
C3 0.0259(13) 0.0263(13) 0.0253(12) -0.0003(10) 0.0016(9) 0.0000(9)
C4 0.0295(13) 0.0271(13) 0.0292(13) -0.0010(10) 0.0108(10) -0.0012(10)
C5 0.0311(14) 0.0300(14) 0.0326(13) 0.0016(11) 0.0076(10) -0.0012(10)
C6 0.0312(14) 0.0289(14) 0.0417(15) 0.0035(11) 0.0143(11) 0.0034(10)
C7 0.0404(15) 0.0266(14) 0.0413(15) -0.0053(11) 0.0198(11) -0.0034(11)
C8 0.0345(14) 0.0314(14) 0.0306(13) -0.0023(11) 0.0129(10) -0.0047(10)
C9 0.0299(13) 0.0255(13) 0.0324(13) 0.0006(10) 0.0121(9) -0.0011(10)
C10 0.0313(13) 0.0347(14) 0.0274(13) 0.0031(10) 0.0027(10) 0.0008(10)
C11 0.0319(13) 0.0286(14) 0.0287(13) 0.0014(10) 0.0054(10) 0.0005(10)
C12 0.0388(15) 0.0392(16) 0.0395(15) -0.0092(12) 0.0108(11) -0.0046(12)
C13 0.0352(15) 0.0479(18) 0.0499(17) -0.0016(13) 0.0149(12) -0.0082(12)
C14 0.0439(17) 0.0593(19) 0.0379(16) 0.0011(14) 0.0182(12) 0.0004(14)
C15 0.0592(19) 0.069(2) 0.0313(15) -0.0101(14) 0.0126(12) -0.0137(15)
C16 0.0443(16) 0.0575(19) 0.0303(14) -0.0024(13) 0.0072(11) -0.0153(13)
C17 0.0385(14) 0.0238(13) 0.0298(14) 0.0001(10) 0.0100(10) 0.0014(10)
O17 0.0365(10) 0.0467(11) 0.0288(10) -0.0027(8) 0.0055(7) -0.0053(8)
O18 0.0363(10) 0.0626(13) 0.0293(10) -0.0035(8) 0.0081(7) -0.0140(8)
C19 0.0322(14) 0.0486(17) 0.0284(14) -0.0026(12) 0.0094(10) -0.0061(12)
C20 0.0466(17) 0.0406(16) 0.0398(16) 0.0015(12) 0.0106(12) 0.0019(13)
C21 0.0359(16) 0.056(2) 0.0461(17) -0.0018(13) 0.0117(12) 0.0074(13)
C22 0.0344(15) 0.061(2) 0.0356(15) -0.0029(13) 0.0134(11) -0.0076(13)
C23 0.0457(16) 0.0424(17) 0.0377(15) 0.0002(12) 0.0132(11) -0.0086(13)
C24 0.0382(15) 0.0433(17) 0.0334(14) -0.0008(12) 0.0097(11) 0.0026(12)
C25 0.0267(13) 0.0297(13) 0.0274(13) 0.0006(10) 0.0019(9) 0.0018(10)
C26 0.0400(15) 0.0322(15) 0.0331(14) -0.0036(11) 0.0094(11) -0.0029(11)
C27 0.0396(15) 0.0433(16) 0.0351(15) -0.0014(12) 0.0116(11) -0.0066(12)
C28 0.0360(15) 0.0435(17) 0.0354(15) -0.0001(12) 0.0118(11) 0.0045(12)
C29 0.0360(14) 0.0329(14) 0.0299(14) -0.0039(11) 0.0022(10) 0.0078(11)
C30 0.0339(14) 0.0281(14) 0.0320(13) 0.0010(11) 0.0049(10) 0.0030(10)

_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
N1 C2 1.362(3) . ?
N1 C9 1.412(3) . ?
N1 C10 1.450(3) . ?
C2 O2 1.218(3) . ?
C2 C3 1.553(3) . ?
C3 C4 1.516(3) . ?
C3 C17 1.528(3) . ?
C3 C25 1.531(3) . ?
C4 C5 1.383(3) . ?
C4 C9 1.389(3) . ?
C5 C6 1.395(3) . ?
C5 H5A 0.9500 . ?
C6 C7 1.381(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.394(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.383(3) . ?
C8 H8A 0.9500 . ?
C10 C11 1.512(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C16 1.371(3) . ?
C11 C12 1.386(3) . ?
C12 C13 1.387(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.373(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.371(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.386(3) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 O17 1.192(3) . ?
C17 O18 1.365(3) . ?
O18 C19 1.414(3) . ?
C19 C24 1.366(4) . ?
C19 C20 1.375(4) . ?
C20 C21 1.394(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.374(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.381(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.388(3) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 C26 1.390(3) . ?
C25 C30 1.397(3) . ?
C26 C27 1.395(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.384(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.387(3) . ?
C28 H28A 0.9500 . ?
C29 C30 1.382(3) . ?
C29 H29A 0.9500 . ?
C30 H30A 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
C2 N1 C9 111.42(18) . . ?
C2 N1 C10 123.2(2) . . ?
C9 N1 C10 125.18(18) . . ?
O2 C2 N1 126.1(2) . . ?
O2 C2 C3 125.9(2) . . ?
N1 C2 C3 108.07(19) . . ?
C4 C3 C17 109.53(17) . . ?
C4 C3 C25 115.89(18) . . ?
C17 C3 C25 113.04(18) . . ?
C4 C3 C2 101.68(17) . . ?
C17 C3 C2 106.90(17) . . ?
C25 C3 C2 108.84(17) . . ?
C5 C4 C9 120.4(2) . . ?
C5 C4 C3 130.6(2) . . ?
C9 C4 C3 109.01(19) . . ?
C4 C5 C6 118.4(2) . . ?
C4 C5 H5A 120.8 . . ?
C6 C5 H5A 120.8 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 . . ?
C6 C7 C8 121.6(2) . . ?
C6 C7 H7A 119.2 . . ?
C8 C7 H7A 119.2 . . ?
C9 C8 C7 117.1(2) . . ?
C9 C8 H8A 121.4 . . ?
C7 C8 H8A 121.4 . . ?
C8 C9 C4 121.9(2) . . ?
C8 C9 N1 128.4(2) . . ?
C4 C9 N1 109.73(19) . . ?
N1 C10 C11 113.10(18) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C16 C11 C12 118.6(2) . . ?
C16 C11 C10 120.2(2) . . ?
C12 C11 C10 121.1(2) . . ?
C11 C12 C13 120.0(2) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C14 C13 C12 120.7(2) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C15 C14 C13 119.6(2) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 119.8(2) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
C11 C16 C15 121.4(2) . . ?
C11 C16 H16A 119.3 . . ?
C15 C16 H16A 119.3 . . ?
O17 C17 O18 124.2(2) . . ?
O17 C17 C3 127.9(2) . . ?
O18 C17 C3 107.88(19) . . ?
C17 O18 C19 118.88(18) . . ?
C24 C19 C20 121.8(2) . . ?
C24 C19 O18 119.0(2) . . ?
C20 C19 O18 118.9(2) . . ?
C19 C20 C21 118.5(3) . . ?
C19 C20 H20A 120.8 . . ?
C21 C20 H20A 120.8 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21A 119.7 . . ?
C20 C21 H21A 119.7 . . ?
C21 C22 C23 119.8(2) . . ?
C21 C22 H22A 120.1 . . ?
C23 C22 H22A 120.1 . . ?
C22 C23 C24 120.1(3) . . ?
C22 C23 H23A 119.9 . . ?
C24 C23 H23A 119.9 . . ?
C19 C24 C23 119.2(2) . . ?
C19 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C26 C25 C30 118.8(2) . . ?
C26 C25 C3 121.2(2) . . ?
C30 C25 C3 119.8(2) . . ?
C25 C26 C27 120.4(2) . . ?
C25 C26 H26A 119.8 . . ?
C27 C26 H26A 119.8 . . ?
C28 C27 C26 120.1(2) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 119.7(2) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
C30 C29 C28 120.3(2) . . ?
C30 C29 H29A 119.9 . . ?
C28 C29 H29A 119.9 . . ?
C29 C30 C25 120.6(2) . . ?
C29 C30 H30A 119.7 . . ?
C25 C30 H30A 119.7 . . ?

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
C9 N1 C2 O2 176.6(2) . . . . ?
C10 N1 C2 O2 1.5(3) . . . . ?
C9 N1 C2 C3 -3.0(2) . . . . ?
C10 N1 C2 C3 -178.22(18) . . . . ?
O2 C2 C3 C4 -177.0(2) . . . . ?
N1 C2 C3 C4 2.7(2) . . . . ?
O2 C2 C3 C17 -62.2(3) . . . . ?
N1 C2 C3 C17 117.49(19) . . . . ?
O2 C2 C3 C25 60.2(3) . . . . ?
N1 C2 C3 C25 -120.11(19) . . . . ?
C17 C3 C4 C5 65.8(3) . . . . ?
C25 C3 C4 C5 -63.5(3) . . . . ?
C2 C3 C4 C5 178.7(2) . . . . ?
C17 C3 C4 C9 -114.29(19) . . . . ?
C25 C3 C4 C9 116.4(2) . . . . ?
C2 C3 C4 C9 -1.4(2) . . . . ?
C9 C4 C5 C6 -0.3(3) . . . . ?
C3 C4 C5 C6 179.6(2) . . . . ?
C4 C5 C6 C7 0.4(3) . . . . ?
C5 C6 C7 C8 0.1(3) . . . . ?
C6 C7 C8 C9 -0.6(3) . . . . ?
C7 C8 C9 C4 0.7(3) . . . . ?
C7 C8 C9 N1 -179.2(2) . . . . ?
C5 C4 C9 C8 -0.2(3) . . . . ?
C3 C4 C9 C8 179.83(19) . . . . ?
C5 C4 C9 N1 179.68(18) . . . . ?
C3 C4 C9 N1 -0.2(2) . . . . ?
C2 N1 C9 C8 -177.9(2) . . . . ?
C10 N1 C9 C8 -2.9(3) . . . . ?
C2 N1 C9 C4 2.1(2) . . . . ?
C10 N1 C9 C4 177.21(18) . . . . ?
C2 N1 C10 C11 101.3(2) . . . . ?
C9 N1 C10 C11 -73.3(3) . . . . ?
N1 C10 C11 C16 124.4(2) . . . . ?
N1 C10 C11 C12 -57.1(3) . . . . ?
C16 C11 C12 C13 0.2(4) . . . . ?
C10 C11 C12 C13 -178.4(2) . . . . ?
C11 C12 C13 C14 -0.5(4) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
C12 C11 C16 C15 0.5(4) . . . . ?
C10 C11 C16 C15 179.0(2) . . . . ?
C14 C15 C16 C11 -0.8(4) . . . . ?
C4 C3 C17 O17 -117.1(3) . . . . ?
C25 C3 C17 O17 13.7(3) . . . . ?
C2 C3 C17 O17 133.4(2) . . . . ?
C4 C3 C17 O18 62.1(2) . . . . ?
C25 C3 C17 O18 -167.04(18) . . . . ?
C2 C3 C17 O18 -47.3(2) . . . . ?
O17 C17 O18 C19 -2.8(3) . . . . ?
C3 C17 O18 C19 177.91(19) . . . . ?
C17 O18 C19 C24 -90.8(3) . . . . ?
C17 O18 C19 C20 95.1(3) . . . . ?
C24 C19 C20 C21 -0.8(4) . . . . ?
O18 C19 C20 C21 173.1(2) . . . . ?
C19 C20 C21 C22 1.2(4) . . . . ?
C20 C21 C22 C23 -0.7(4) . . . . ?
C21 C22 C23 C24 -0.3(4) . . . . ?
C20 C19 C24 C23 -0.1(3) . . . . ?
O18 C19 C24 C23 -174.1(2) . . . . ?
C22 C23 C24 C19 0.7(4) . . . . ?
C4 C3 C25 C26 -7.0(3) . . . . ?
C17 C3 C25 C26 -134.6(2) . . . . ?
C2 C3 C25 C26 106.8(2) . . . . ?
C4 C3 C25 C30 177.60(19) . . . . ?
C17 C3 C25 C30 50.0(3) . . . . ?
C2 C3 C25 C30 -68.6(2) . . . . ?
C30 C25 C26 C27 0.1(3) . . . . ?
C3 C25 C26 C27 -175.3(2) . . . . ?
C25 C26 C27 C28 -0.2(4) . . . . ?
C26 C27 C28 C29 -0.1(4) . . . . ?
C27 C28 C29 C30 0.4(4) . . . . ?
C28 C29 C30 C25 -0.5(3) . . . . ?
C26 C25 C30 C29 0.2(3) . . . . ?
C3 C25 C30 C29 175.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.054