# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 182/1422

data_global

# 1. SUBMISSION DETAILS

_publ_contact_letter

;

     Please consider this CIF submission for as supplementary data for chemcomm.
;

_publ_contact_author_name                       ' David Hodgson '

_publ_contact_author_address

;

Dyson Perrins  Laboratory
South Parks Road

OXFORD OX1 3QY

;

_publ_contact_author_phone                      ' 01865 275697 '
_publ_contact_author_fax       ?

_publ_contact_author_email        ' david.hodgson@chem.ox.ac.uk '
_publ_requested_journal                         'chem. comm'



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

# 3. TITLE AND AUTHOR LIST

_publ_section_title

;

 Efficient Rh(II) binaphtholphosphate catalysts for enantioselective
intramolecular andem carbonyl ylide formation-cycloaddition of
a-diazo-b-ketoesters
;

# The loop structure below should contain the names and addresses of all

# authors, in the required order of publication. Repeat as necessary.

loop_
        _publ_author_name
        _publ_author_address
        _publ_author_footnote
'David M. Hodgson '
;
Dyson Perrins Laboratory
Department of Chemistry
University of Oxford
South Parks Road
Oxford
UK OX1 3QY
;
?

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

# 4. TEXT

_publ_section_abstract  #Text of the abstract

;

?

;

_publ_section_comment  #Text of the paper

;

?

;

_publ_section_acknowledgements  # Acknowledgments

;

?

;

_publ_section_figure_captions  #Captions to figures

;

?

;

_publ_section_exptl_refinement

# see also _refine_ls_hydrogen for refinement keywords.

;

 H atoms placed geometrically after each cycle

;

_publ_section_exptl_prep

;

 ?

;

## -----------------REFERENCES ----------------------##

_publ_section_references # Add your own references - in alphabetic order

;
# SIR92
#
Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C.,
Polidori, G.  & Camalli, M. (1994) SIR92 - a program for automatic 
solution of
crystal structures by direct methods. J. Appl. Cryst. (27), 435-435

# Chebychev Weights
#
Carruthers, J.R. and Watkin, D.J. (1979),
Acta Cryst, A35, 698-699


# Extinction correction
#
Larson, A.C. (1970), Crystallographic Computing, Ed  Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294


# Azimutal absorption correction
#
North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968),
Acta Cryst, A24, 351-359

# CRYSTALS
#
Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) 
CRYSTALS
Issue 10. Chemical Crystallography Laboratory, OXFORD, UK.

#CAMERON
#
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.

# RC93
#
Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical
Crystallography Laboratory, Oxford, UK.
;

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


# Diffractometer details

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


# choose from:

#++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++      


_diffrn_measurement_device_type     '  Enraf-nonius CAD4 '

_diffrn_radiation_monochromator      graphite

_computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)'

_computing_data_reduction

;

RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)

;

_computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)'



# General computing

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


_computing_structure_refinement

;

CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)

;

_computing_publication_material

;

CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)

;

_computing_molecular_graphics

;

 CAMERON (Watkin, Prout & Pearce,  1996)

;

# choose one of the following two lines

# _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)'

_computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)'



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




_chemical_name_systematic       # IUPAC name, in full

;

?

;

_chemical_melting_point                    'not measured'

# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'

_refine_ls_matrix_type                      full

# choose from 'heavy, direct, difmap, geom'

_atom_sites_solution_primary                direct

# _atom_sites_solution_secondary            difmap

_atom_sites_solution_hydrogens              geom

# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'

_refine_ls_hydrogen_treatment               noref

#***********************************************************************

_cell_length_a 6.415(2)
_cell_angle_alpha 90
_cell_length_b 19.871(5)
_cell_angle_beta  90
_cell_length_c 21.298(8)
_cell_angle_gamma 90
_cell_volume   2714.8
_symmetry_cell_setting 'Orthorhombic '
_symmetry_space_group_name_H-M 'P 21 21 21 '
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 'x+1/2,-y+1/2,-z'
 '-x,y+1/2,-z+1/2'
 '-x+1/2,-y,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
 'C   '    0.0170    0.0090    2.3100   20.8439
    1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
 'H   '    0.0000    0.0000    0.4930   10.5109
    0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
 'N   '    0.0290    0.0180   12.2126    0.0057
    3.1322    9.8933    2.0125   28.9975    1.1663    0.5826  -11.5290
'International_Tables_Vol_IV_Table_2.2B'
 'O   '    0.0470    0.0320    3.0485   13.2771
    2.2868    5.7011    1.5463    0.3239    0.8670   32.9089    0.2508
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C28 H33 N3 O9 '
_chemical_formula_moiety
' C28 H33 N3 O9 '
_chemical_compound_source
;
?
;
_chemical_formula_weight   555.58
_cell_measurement_reflns_used       25
_cell_measurement_theta_min       21
_cell_measurement_theta_max       43
_cell_measurement_temperature    190
_cell_formula_units_Z 4
_exptl_crystal_description ' prism '
_exptl_crystal_colour ' colourless '
_exptl_crystal_size_min 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_max 1.00
_exptl_crystal_density_diffrn 1.36
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_F_000 1179.76
_exptl_absorpt_coefficient_mu 0.85
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart ,1983)'
_exptl_absorpt_correction_T_min 0.64
_exptl_absorpt_correction_T_max 0.89
# Sheldrick geometric definitions 0.89 0.89
_diffrn_standards_interval_time 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 3
_diffrn_standards_decay_% 5.48
_diffrn_ambient_temperature        190
_diffrn_reflns_number 3133
_reflns_number_total 3133
_diffrn_reflns_av_R_equivalents 0.00
# Number of reflections with Friedels Law is 3133
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 2769
_diffrn_measured_fraction_theta_max 1.000
_reflns_number_gt 2545
_diffrn_reflns_theta_min 0.00
_diffrn_reflns_theta_max 74.33
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 26
_reflns_limit_h_min 0
_reflns_limit_h_max 8
_reflns_limit_k_min 0
_reflns_limit_k_max 24
_reflns_limit_l_min 0
_reflns_limit_l_max 26
_refine_diff_density_min -0.26
_refine_diff_density_max 0.22
_reflns_threshold_expression  >3.00\s(I)
_refine_ls_number_reflns 2545
_refine_ls_number_parameters 361
_refine_ls_R_factor_gt 0.0456
_refine_ls_wR_factor_ref 0.0398
_refine_ls_goodness_of_fit_ref 1.0493
_refine_ls_shift/su_max 0.000186
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979,
 1.50    -3.46    0.549    -1.73
;
_diffrn_radiation_type       'Cu K\a'
_diffrn_radiation_wavelength      1.54180
_diffrn_measurement_method \w/2\q

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
O1 0.4487(3) -0.0661(1) 0.44325(11) 0.0294 1.0000 Uani
N2 0.2695(4) -0.02053(12) 0.44738(13) 0.0277 1.0000 Uani
C3 0.2523(6) 0.01102(14) 0.39621(15) 0.0283 1.0000 Uani
C4 0.0732(5) 0.06146(14) 0.39234(14) 0.0243 1.0000 Uani
O5 -0.0462(4) 0.0448(1) 0.3385(1) 0.0291 1.0000 Uani
C6 0.0841(6) 0.06629(15) 0.28571(15) 0.0294 1.0000 Uani
C7 0.1663(5) 0.13592(15) 0.30642(15) 0.0266 1.0000 Uani
C8 0.1552(5) 0.13332(14) 0.37842(14) 0.0275 1.0000 Uani
C9 0.0224(6) 0.18756(17) 0.27355(16) 0.0371 1.0000 Uani
C10 -0.1572(7) 0.14792(19) 0.24544(18) 0.0436 1.0000 Uani
C11 -0.0602(7) 0.07933(18) 0.23026(16) 0.0391 1.0000 Uani
C12 0.2528(7) 0.01363(18) 0.27795(16) 0.0418 1.0000 Uani
C13 0.3857(6) 0.00629(19) 0.33746(18) 0.0436 1.0000 Uani
C14 -0.0647(5) 0.06049(14) 0.45027(15) 0.0255 1.0000 Uani
O15 0.0329(3) 0.0925(1) 0.4967(1) 0.0266 1.0000 Uani
C16 -0.0752(5) 0.09630(14) 0.55655(14) 0.0247 1.0000 Uani
C17 0.0826(5) 0.11762(14) 0.60690(14) 0.0226 1.0000 Uani
C18 0.1901(5) 0.18280(15) 0.58311(16) 0.0299 1.0000 Uani
C19 0.0160(6) 0.23662(16) 0.5874(2) 0.0422 1.0000 Uani
C20 -0.1728(5) 0.19639(16) 0.61190(18) 0.0356 1.0000 Uani
C21 -0.0690(5) 0.14634(15) 0.65821(15) 0.0285 1.0000 Uani
C22 0.0410(6) 0.1798(2) 0.71377(17) 0.0429 1.0000 Uani
C23 -0.2197(6) 0.09451(19) 0.68559(16) 0.0373 1.0000 Uani
C24 -0.2467(5) 0.15074(17) 0.55829(16) 0.0346 1.0000 Uani
C25 0.2311(6) 0.06151(17) 0.62480(16) 0.0343 1.0000 Uani
O26 -0.2363(4) 0.03649(12) 0.45329(11) 0.0375 1.0000 Uani
C27 0.5304(5) -0.07758(15) 0.50020(16) 0.0295 1.0000 Uani
O28 0.4581(4) -0.06185(14) 0.54950(13) 0.0465 1.0000 Uani
C29 0.7362(5) -0.11440(14) 0.49476(16) 0.0293 1.0000 Uani
C30 0.8414(5) -0.12720(15) 0.55052(16) 0.0296 1.0000 Uani
C31 1.0335(5) -0.15923(16) 0.54744(16) 0.0321 1.0000 Uani
N32 1.1502(5) -0.17018(15) 0.60651(15) 0.0412 1.0000 Uani
O33 1.0861(5) -0.14291(16) 0.65373(13) 0.0548 1.0000 Uani
O34 1.3058(5) -0.20554(15) 0.60381(15) 0.0641 1.0000 Uani
C35 1.1208(5) -0.18000(15) 0.49187(17) 0.0305 1.0000 Uani
C36 1.0153(5) -0.16507(15) 0.43759(16) 0.0308 1.0000 Uani
C37 0.8227(5) -0.13235(15) 0.43743(15) 0.0280 1.0000 Uani
N38 1.1105(5) -0.18291(15) 0.37690(16) 0.0413 1.0000 Uani
O39 1.2704(5) -0.21676(15) 0.37834(14) 0.0572 1.0000 Uani
O40 1.0279(5) -0.16324(16) 0.32909(13) 0.0598 1.0000 Uani
H71 0.3119 0.1482 0.2953 0.0312 1.0000 Uiso
H81 0.2952 0.1401 0.3973 0.0326 1.0000 Uiso
H82 0.0561 0.1682 0.3947 0.0326 1.0000 Uiso
H91 -0.0310 0.2214 0.3043 0.0456 1.0000 Uiso
H92 0.1023 0.2119 0.2396 0.0456 1.0000 Uiso
H101 -0.2728 0.1428 0.2757 0.0510 1.0000 Uiso
H102 -0.2092 0.1700 0.2059 0.0510 1.0000 Uiso
H111 -0.1654 0.0432 0.2260 0.0475 1.0000 Uiso
H112 0.0261 0.0812 0.1900 0.0475 1.0000 Uiso
H121 0.1853 -0.0312 0.2677 0.0514 1.0000 Uiso
H122 0.3467 0.0264 0.2425 0.0514 1.0000 Uiso
H131 0.4878 0.0418 0.3378 0.0522 1.0000 Uiso
H132 0.4496 -0.0394 0.3365 0.0522 1.0000 Uiso
H161 -0.1380 0.0508 0.5633 0.0309 1.0000 Uiso
H181 0.3106 0.1949 0.6105 0.0339 1.0000 Uiso
H182 0.2386 0.1770 0.5389 0.0339 1.0000 Uiso
H191 0.0554 0.2739 0.6168 0.0496 1.0000 Uiso
H192 -0.0149 0.2565 0.5450 0.0496 1.0000 Uiso
H201 -0.2860 0.2249 0.6302 0.0397 1.0000 Uiso
H221 -0.0639 0.1969 0.7444 0.0513 1.0000 Uiso
H222 0.1329 0.1457 0.7351 0.0513 1.0000 Uiso
H223 0.1290 0.2178 0.6983 0.0513 1.0000 Uiso
H231 -0.3101 0.1164 0.7180 0.0433 1.0000 Uiso
H232 -0.1364 0.0576 0.7063 0.0433 1.0000 Uiso
H233 -0.3066 0.0750 0.6517 0.0433 1.0000 Uiso
H241 -0.3853 0.1312 0.5666 0.0415 1.0000 Uiso
H242 -0.2497 0.1766 0.5174 0.0415 1.0000 Uiso
H251 0.3292 0.0770 0.6581 0.0426 1.0000 Uiso
H252 0.1487 0.0218 0.6415 0.0426 1.0000 Uiso
H253 0.3111 0.0464 0.5871 0.0426 1.0000 Uiso
H301 0.7790 -0.1137 0.5920 0.0363 1.0000 Uiso
H351 1.2543 -0.2058 0.4910 0.0358 1.0000 Uiso
H371 0.7463 -0.1220 0.3972 0.0357 1.0000 Uiso
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 0.0187(11) 0.025(1) 0.0445(13) -0.0000(9) -0.001(1) 0.004(1)
N2 0.0184(13) 0.0238(11) 0.0409(14) 0.0017(11) -0.0010(12) 0.0014(11)
C3 0.0226(16) 0.0239(13) 0.0383(16) -0.0025(12) -0.0003(16) -0.0032(13)
C4 0.0225(15) 0.0200(12) 0.0302(15) -0.0016(11) 0.0001(13) -0.0022(12)
O5 0.0262(12) 0.028(1) 0.0333(11) -0.0020(9) -0.0044(11) -0.0055(9)
C6 0.0311(18) 0.0285(14) 0.0284(15) -0.0013(12) -0.0016(14) -0.0024(14)
C7 0.0230(15) 0.0260(14) 0.0308(15) 0.0013(12) -0.0003(13) -0.0042(12)
C8 0.0286(17) 0.0243(14) 0.0296(15) 0.0003(12) 0.0019(14) -0.0064(13)
C9 0.041(2) 0.0325(16) 0.0380(17) 0.0008(13) -0.0071(17) 0.0021(17)
C10 0.038(2) 0.046(2) 0.046(2) -0.0001(17) -0.0143(18) 0.0003(18)
C11 0.042(2) 0.0401(18) 0.0352(18) -0.0018(14) -0.0136(17) -0.0073(17)
C12 0.050(2) 0.0414(19) 0.0341(17) -0.0060(15) 0.0003(18) 0.013(2)
C13 0.043(2) 0.048(2) 0.0397(19) 0.0010(16) 0.0088(19) 0.0187(18)
C14 0.0202(15) 0.0215(12) 0.0348(15) 0.0031(12) -0.0002(13) -0.0015(12)
O15 0.016(1) 0.0346(11) 0.029(1) -0.0008(9) 0.0031(9) -0.0032(9)
C16 0.0155(14) 0.0308(14) 0.0278(15) 0.0029(12) -0.0001(13) -0.0025(12)
C17 0.0131(14) 0.0246(13) 0.0301(15) -0.0019(11) 0.0023(12) 0.0026(11)
C18 0.0189(15) 0.0270(14) 0.0437(18) 0.0009(13) 0.0072(14) -0.0040(13)
C19 0.0314(19) 0.0284(15) 0.067(2) 0.0079(16) 0.0059(19) 0.0039(15)
C20 0.0213(17) 0.0302(15) 0.055(2) 0.0043(15) 0.0100(17) 0.0118(14)
C21 0.0194(15) 0.0295(15) 0.0368(17) -0.0026(13) 0.0061(15) 0.0015(13)
C22 0.035(2) 0.052(2) 0.0416(19) -0.0125(16) 0.0036(17) -0.0011(19)
C23 0.0269(18) 0.051(2) 0.0343(17) 0.0052(15) 0.0075(15) -0.0064(16)
C24 0.0162(15) 0.0453(18) 0.0424(18) 0.0071(15) 0.0010(15) 0.0098(15)
C25 0.0244(17) 0.0365(16) 0.0421(18) 0.0028(14) -0.0070(16) 0.0116(15)
O26 0.0237(12) 0.0458(13) 0.0432(12) -0.0012(11) 0.0023(12) -0.0161(11)
C27 0.0264(17) 0.0247(13) 0.0374(17) 0.0032(12) 0.0044(15) 0.0019(13)
O28 0.0379(15) 0.0562(15) 0.0454(14) 0.0039(12) 0.0038(13) 0.0257(14)
C29 0.0249(16) 0.0207(13) 0.0424(17) 0.0012(12) 0.0022(16) -0.0010(13)
C30 0.0239(16) 0.0251(14) 0.0398(17) -0.0001(13) 0.0071(15) 0.0037(13)
C31 0.0265(17) 0.0272(15) 0.0426(18) 0.0015(14) -0.0052(15) 0.0009(14)
N32 0.0331(17) 0.0430(16) 0.0475(18) 0.0006(14) -0.0103(15) 0.0045(14)
O33 0.0390(16) 0.086(2) 0.0394(14) -0.0039(14) -0.0047(13) 0.0141(16)
O34 0.054(2) 0.0684(19) 0.0695(19) -0.0087(16) -0.0219(17) 0.0403(17)
C35 0.0171(15) 0.0215(13) 0.053(2) -0.0014(13) 0.0029(14) 0.0014(12)
C36 0.0244(16) 0.0219(14) 0.0460(19) -0.0017(13) 0.0057(15) -0.0015(13)
C37 0.0247(16) 0.0240(14) 0.0354(16) 0.0000(12) 0.0001(14) -0.0008(12)
N38 0.0366(18) 0.0361(15) 0.0511(18) -0.0022(13) 0.0107(16) 0.0028(14)
O39 0.0419(17) 0.0652(18) 0.0644(18) -0.0097(15) 0.0102(16) 0.0230(16)
O40 0.058(2) 0.075(2) 0.0463(16) 0.0030(15) 0.0113(15) 0.0219(18)
_refine_ls_extinction_method
    'None'
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
O1 . N2 . 1.466(3)    yes
O1 . C27 . 1.341(4)    yes
N2 . C3 . 1.262(4)    yes
C3 . C4 . 1.527(4)    yes
C3 . C13 . 1.519(5)    yes
C4 . O5 . 1.418(4)    yes
C4 . C8 . 1.550(4)    yes
C4 . C14 . 1.518(4)    yes
O5 . C6 . 1.464(4)    yes
C6 . C7 . 1.545(4)    yes
C6 . C11 . 1.523(5)    yes
C6 . C12 . 1.515(5)    yes
C7 . C8 . 1.536(4)    yes
C7 . C9 . 1.547(5)    yes
C7 . H71 . 0.994(3)    no
C8 . H81 . 0.994(3)    no
C8 . H82 . 1.002(3)    no
C9 . C10 . 1.519(5)    yes
C9 . H91 . 1.000(4)    no
C9 . H92 . 1.009(4)    no
C10 . C11 . 1.533(5)    yes
C10 . H101 . 0.987(4)    no
C10 . H102 . 1.007(4)    no
C11 . H111 . 0.989(4)    no
C11 . H112 . 1.021(4)    no
C12 . C13 . 1.534(5)    yes
C12 . H121 . 1.014(4)    no
C12 . H122 . 0.999(4)    no
C13 . H131 . 0.964(4)    no
C13 . H132 . 0.996(4)    no
C14 . O15 . 1.332(4)    yes
C14 . O26 . 1.201(4)    yes
O15 . C16 . 1.454(4)    yes
C16 . C17 . 1.534(4)    yes
C16 . C24 . 1.543(4)    yes
C16 . H161 . 1.001(3)    no
C17 . C18 . 1.552(4)    yes
C17 . C21 . 1.570(4)    yes
C17 . C25 . 1.515(4)    yes
C18 . C19 . 1.549(5)    yes
C18 . H181 . 0.998(3)    no
C18 . H182 . 0.998(3)    no
C19 . C20 . 1.542(5)    yes
C19 . H191 . 1.002(4)    no
C19 . H192 . 1.007(4)    no
C20 . C21 . 1.551(4)    yes
C20 . C24 . 1.533(5)    yes
C20 . H201 . 1.000(3)    no
C21 . C22 . 1.529(5)    yes
C21 . C23 . 1.529(4)    yes
C22 . H221 . 0.997(4)    no
C22 . H222 . 1.007(4)    no
C22 . H223 . 0.999(4)    no
C23 . H231 . 1.000(4)    no
C23 . H232 . 1.010(4)    no
C23 . H233 . 0.991(4)    no
C24 . H241 . 0.986(3)    no
C24 . H242 . 1.011(3)    no
C25 . H251 . 0.996(3)    no
C25 . H252 . 1.015(4)    no
C25 . H253 . 0.999(3)    no
C27 . O28 . 1.189(4)    yes
C27 . C29 . 1.514(5)    yes
C29 . C30 . 1.390(5)    yes
C29 . C37 . 1.388(5)    yes
C30 . C31 . 1.389(5)    yes
C30 . H301 . 1.006(3)    no
C31 . N32 . 1.480(4)    yes
C31 . C35 . 1.373(5)    yes
N32 . O33 . 1.214(4)    yes
N32 . O34 . 1.222(4)    yes
C35 . C36 . 1.372(5)    yes
C35 . H351 . 0.998(3)    no
C36 . C37 . 1.396(5)    yes
C36 . N38 . 1.473(4)    yes
C37 . H371 . 1.009(3)    no
N38 . O39 . 1.227(4)    yes
N38 . O40 . 1.213(4)    yes
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
N2 . O1 . C27 . 110.9(2)    yes
O1 . N2 . C3 . 108.9(3)    yes
N2 . C3 . C4 . 116.0(3)    yes
N2 . C3 . C13 . 129.2(3)    yes
C4 . C3 . C13 . 114.8(3)    yes
C3 . C4 . O5 . 107.2(2)    yes
C3 . C4 . C8 . 111.1(3)    yes
O5 . C4 . C8 . 104.1(2)    yes
C3 . C4 . C14 . 112.7(2)    yes
O5 . C4 . C14 . 109.9(3)    yes
C8 . C4 . C14 . 111.4(2)    yes
C4 . O5 . C6 . 104.2(2)    yes
O5 . C6 . C7 . 103.7(2)    yes
O5 . C6 . C11 . 107.4(3)    yes
C7 . C6 . C11 . 106.0(3)    yes
O5 . C6 . C12 . 106.8(3)    yes
C7 . C6 . C12 . 113.9(3)    yes
C11 . C6 . C12 . 117.9(3)    yes
C6 . C7 . C8 . 103.8(2)    yes
C6 . C7 . C9 . 105.1(3)    yes
C8 . C7 . C9 . 116.5(3)    yes
C6 . C7 . H71 . 118.2(3)    no
C8 . C7 . H71 . 106.8(3)    no
C9 . C7 . H71 . 106.8(3)    no
C4 . C8 . C7 . 103.7(2)    yes
C4 . C8 . H81 . 110.8(3)    no
C7 . C8 . H81 . 111.0(3)    no
C4 . C8 . H82 . 110.8(3)    no
C7 . C8 . H82 . 110.6(3)    no
H81 . C8 . H82 . 109.8(3)    no
C7 . C9 . C10 . 106.7(3)    yes
C7 . C9 . H91 . 110.7(3)    no
C10 . C9 . H91 . 110.3(4)    no
C7 . C9 . H92 . 109.8(3)    no
C10 . C9 . H92 . 110.6(3)    no
H91 . C9 . H92 . 108.8(3)    no
C9 . C10 . C11 . 103.7(3)    yes
C9 . C10 . H101 . 111.5(3)    no
C11 . C10 . H101 . 110.5(3)    no
C9 . C10 . H102 . 110.8(3)    no
C11 . C10 . H102 . 110.2(3)    no
H101 . C10 . H102 . 110.0(4)    no
C6 . C11 . C10 . 103.6(3)    yes
C6 . C11 . H111 . 111.2(3)    no
C10 . C11 . H111 . 112.8(4)    no
C6 . C11 . H112 . 109.1(3)    no
C10 . C11 . H112 . 111.4(3)    no
H111 . C11 . H112 . 108.7(3)    no
C6 . C12 . C13 . 111.9(3)    yes
C6 . C12 . H121 . 109.0(4)    no
C13 . C12 . H121 . 109.4(3)    no
C6 . C12 . H122 . 109.8(3)    no
C13 . C12 . H122 . 108.3(4)    no
H121 . C12 . H122 . 108.4(3)    no
C3 . C13 . C12 . 111.2(3)    yes
C3 . C13 . H131 . 109.4(3)    no
C12 . C13 . H131 . 108.3(3)    no
C3 . C13 . H132 . 107.8(3)    no
C12 . C13 . H132 . 107.3(3)    no
H131 . C13 . H132 . 112.8(4)    no
C4 . C14 . O15 . 108.9(2)    yes
C4 . C14 . O26 . 125.6(3)    yes
O15 . C14 . O26 . 125.5(3)    yes
C14 . O15 . C16 . 116.8(2)    yes
O15 . C16 . C17 . 108.2(2)    yes
O15 . C16 . C24 . 113.4(2)    yes
C17 . C16 . C24 . 105.1(2)    yes
O15 . C16 . H161 . 105.7(2)    no
C17 . C16 . H161 . 114.5(3)    no
C24 . C16 . H161 . 110.1(3)    no
C16 . C17 . C18 . 107.2(2)    yes
C16 . C17 . C21 . 100.3(2)    yes
C18 . C17 . C21 . 101.5(2)    yes
C16 . C17 . C25 . 112.8(2)    yes
C18 . C17 . C25 . 114.6(3)    yes
C21 . C17 . C25 . 118.8(3)    yes
C17 . C18 . C19 . 103.7(2)    yes
C17 . C18 . H181 . 110.7(3)    no
C19 . C18 . H181 . 110.9(3)    no
C17 . C18 . H182 . 110.5(3)    no
C19 . C18 . H182 . 111.1(3)    no
H181 . C18 . H182 . 109.8(3)    no
C18 . C19 . C20 . 103.2(2)    yes
C18 . C19 . H191 . 111.4(3)    no
C20 . C19 . H191 . 111.7(3)    no
C18 . C19 . H192 . 111.1(3)    no
C20 . C19 . H192 . 110.6(4)    no
H191 . C19 . H192 . 108.7(3)    no
C19 . C20 . C21 . 102.1(3)    yes
C19 . C20 . C24 . 107.3(3)    yes
C21 . C20 . C24 . 103.1(2)    yes
C19 . C20 . H201 . 114.1(3)    no
C21 . C20 . H201 . 115.3(3)    no
C24 . C20 . H201 . 113.6(3)    no
C17 . C21 . C20 . 93.2(2)    yes
C17 . C21 . C22 . 114.3(3)    yes
C20 . C21 . C22 . 114.3(3)    yes
C17 . C21 . C23 . 114.4(3)    yes
C20 . C21 . C23 . 113.8(3)    yes
C22 . C21 . C23 . 106.8(3)    yes
C21 . C22 . H221 . 110.1(3)    no
C21 . C22 . H222 . 109.1(3)    no
H221 . C22 . H222 . 109.2(4)    no
C21 . C22 . H223 . 109.6(3)    no
H221 . C22 . H223 . 109.8(4)    no
H222 . C22 . H223 . 109.0(4)    no
C21 . C23 . H231 . 109.7(3)    no
C21 . C23 . H232 . 108.8(3)    no
H231 . C23 . H232 . 108.7(3)    no
C21 . C23 . H233 . 110.0(3)    no
H231 . C23 . H233 . 110.3(4)    no
H232 . C23 . H233 . 109.4(4)    no
C16 . C24 . C20 . 102.3(3)    yes
C16 . C24 . H241 . 111.8(3)    no
C20 . C24 . H241 . 112.2(3)    no
C16 . C24 . H242 . 110.5(3)    no
C20 . C24 . H242 . 110.2(3)    no
H241 . C24 . H242 . 109.7(3)    no
C17 . C25 . H251 . 110.4(3)    no
C17 . C25 . H252 . 109.5(3)    no
H251 . C25 . H252 . 108.6(3)    no
C17 . C25 . H253 . 110.0(3)    no
H251 . C25 . H253 . 109.9(3)    no
H252 . C25 . H253 . 108.4(3)    no
O1 . C27 . O28 . 127.0(3)    yes
O1 . C27 . C29 . 110.7(3)    yes
O28 . C27 . C29 . 122.3(3)    yes
C27 . C29 . C30 . 116.5(3)    yes
C27 . C29 . C37 . 122.7(3)    yes
C30 . C29 . C37 . 120.7(3)    yes
C29 . C30 . C31 . 118.3(3)    yes
C29 . C30 . H301 . 120.5(3)    no
C31 . C30 . H301 . 121.1(3)    no
C30 . C31 . N32 . 118.4(3)    yes
C30 . C31 . C35 . 122.7(3)    yes
N32 . C31 . C35 . 118.8(3)    yes
C31 . N32 . O33 . 117.8(3)    yes
C31 . N32 . O34 . 117.2(3)    yes
O33 . N32 . O34 . 124.9(3)    yes
C31 . C35 . C36 . 117.4(3)    yes
C31 . C35 . H351 . 121.4(3)    no
C36 . C35 . H351 . 121.2(3)    no
C35 . C36 . C37 . 122.6(3)    yes
C35 . C36 . N38 . 118.9(3)    yes
C37 . C36 . N38 . 118.5(3)    yes
C29 . C37 . C36 . 118.1(3)    yes
C29 . C37 . H371 . 120.1(3)    no
C36 . C37 . H371 . 121.8(3)    no
C36 . N38 . O39 . 117.2(3)    yes
C36 . N38 . O40 . 118.6(3)    yes
O39 . N38 . O40 . 124.3(3)    yes