# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1902

#  CIF produced by WinGX routine CIF_UPDATE

#  Created on 1999-05-14 at 09:57:10

#  Using CIFtbx version 2.6.2 16 Jun 1998



#  Dictionary name : cif_core.dic

#  Dictionary vers : 2.1beta3

#  Request file    : c:\wingx\files\archive.dat

#  CIF files read  : s92 diffy



#

#     CCDC ELECTRONIC DATA DEPOSITION FORM (CIF)

#

#     This electronic data deposition form can be used:

#

#     (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or

#     (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC

#

#     A comprehensive archive of CIF resources is maintained by the IUCr

#     at its Chester office. This can be accessed

#     by anonymous ftp to ftp.iucr.org

#     or via the WWW at http://www.iucr.org/cif/home.html

#     If data items in this form are not available or not applicable

#     then ignore these items

#     A few items specific to CCDC input are indicated by _ccdc_

#

#     Submission and help information is provided at the end of this form

#-------------------------------------------------------------------------

#1    Global data block identification for start of deposition



data_global



#

#-------------------------------------------------------------------------

#2    Person making the deposition

#

_publ_contact_author               'Light, M.E.'

_publ_contact_author_email         'light@soton.ac.uk'



#-------------------------------------------------------------------------

#3    Publication details

#

#     Provide these details if the structure has been published,

#     accepted or submitted for publication

#

#     The CCDC journal deposition number, eg. 182/357,

#     should be included only if it has been assigned by the journal

#

loop_

_publ_author_name



'Bruce, D.'

'Light, M.E.'

'Gelbrich, T.'

'Coles, S.J.'



_journal_name_full                 ?

_journal_volume                    ?

_journal_page_first                ?

_journal_page_last                 ?

_journal_year                      ?

_ccdc_journal_depnumber            ?

#

#-------------------------------------------------------------------------

#4    Chemical and physical data

#

#     Note that the units for melting point are Kelvin

#     The compound_id is the identifier for the compound in the published

#       paper, eg. 4a, II, etc.

#     Provide a brief description of any significant biological activity,

#       eg. antimalarial activity

#     If the compound exhibits polymorphism provide brief details,

#       eg. monoclinic form, low-temperature phase, etc.

#     For chemdiag  leave blank - no longer necessary



_ccdc_compound_id                  ?

_ccdc_biological_activity          ?

_ccdc_polymorph                    ?



_ccdc_chemdiag_type                ?

_ccdc_chemdiag_records

;

?

;

#

#-------------------------------------------------------------------------

#5    Other data relating to the structure determination and refinement

#

#     Record the radiation type if not X-rays, eg. neutron

#     Record the temperature of the data collection (Kelvin)

#       if not room-temperature

#     Record R_squared if this is the only reliability factor given by

#       your refinement program

#     Describe briefly any disorder, eg. t-Butyl C31-33 disordered over

#       two sites with occupancies 0.6 and 0.4

#     Under ccdc_comments record any other important information



_ccdc_temp_data_collection          150

_ccdc_ls_R_squared                  ?

_ccdc_disorder                      ?

_ccdc_comments

;

?

;

#-------------------------------------------------------------------------

#6    Include your "standard" CIF file here

#     It should contain the following data items:

#       unit cell parameters and volume, z value, space group symbol,

#       R-factor(s), atomic coordinates with standard deviations,

#       occupancy factors, bond lengths and bond angles

#     Other data items may be present but will not necessarily be

#       included in the Cambridge Structural Database

#

#     Do NOT include structure factors

#

#

#-------------------------------------------------------------------------

#SUBMISSION INFORMATION

#

#     For a journal send the form to the address specified by the journal

#

#     For a private communication to the CCDC send the form to the address

#       deposit@ccdc.cam.ac.uk

#

#     For up-to-date information on deposition procedures, check the website

#       http://www.ccdc.cam.ac.uk/



data_s92



_audit_creation_date            1999-05-14T09:57:10-00:00

_audit_creation_method         'WinGX routine CIF_UPDATE'



#----------------------------------------------------------------------------#

#                   CHEMICAL INFORMATION                                     #

#----------------------------------------------------------------------------#



_chemical_name_systematic

;

 ?

;

_chemical_formula_sum                   'C51 H50 N2 O12 Re2'

_chemical_formula_weight                1255.33



#----------------------------------------------------------------------------#

#                   UNIT CELL INFORMATION                                    #

#----------------------------------------------------------------------------#



loop_

    _symmetry_equiv_pos_as_xyz

'x, y, z'



_cell_length_a                          9.1822(2)

_cell_length_b                          13.5268(2)

_cell_length_c                          21.4700(5)

_cell_angle_alpha                       74.1341(13)

_cell_angle_beta                        86.9295(11)

_cell_angle_gamma                       74.3192(13)

_cell_volume                            2469.05(9)

_cell_formula_units_Z                   2

_cell_measurement_temperature           150(2)

_cell_measurement_reflns_used           na

_cell_measurement_theta_min             na

_cell_measurement_theta_max             na



#----------------------------------------------------------------------------#

#                   CRYSTAL INFORMATION                                      #

#----------------------------------------------------------------------------#



_exptl_crystal_size_max                 0.3

_exptl_crystal_size_mid                 0.15

_exptl_crystal_size_min                 0.1

_exptl_crystal_density_meas             'not measured'

_exptl_crystal_density_diffrn           1.689

_exptl_crystal_density_method           'not measured'

_exptl_crystal_F_000                    1232

_exptl_special_details

;

 ?

;



#----------------------------------------------------------------------------#

#                   ABSORPTION CORRECTION                                    #

#----------------------------------------------------------------------------#



_exptl_absorpt_coefficient_mu           4.961

_exptl_absorpt_correction_type          'Empirical, SORTAV'

_exptl_absorpt_correction_T_min         0.3176

_exptl_absorpt_correction_T_max         0.6368



#----------------------------------------------------------------------------#

#                   DATA COLLECTION                                          #

#----------------------------------------------------------------------------#



_diffrn_ambient_temperature             150(2)

_diffrn_radiation_wavelength            0.71073

_diffrn_radiation_type                  MoK\a

_diffrn_radiation_monochromator         graphite

_diffrn_measurement_device_type         'Enraf Nonius KappaCCD area detector'

_diffrn_measurement_method

           'Phi and Omega scans to fill Ewald sphere'

_diffrn_standards_number                'not measured'

_diffrn_standards_interval_count        na

_diffrn_standards_interval_time         na

_diffrn_standards_decay_%               na

_diffrn_reflns_number                   35530

_diffrn_reflns_av_R_equivalents         0.0438

_diffrn_reflns_av_sigmaI/netI           0.0508

_diffrn_reflns_limit_h_min              -10

_diffrn_reflns_limit_h_max              10

_diffrn_reflns_limit_k_min              -16

_diffrn_reflns_limit_k_max              16

_diffrn_reflns_limit_l_min              -25

_diffrn_reflns_limit_l_max              25

_diffrn_reflns_theta_min                2.96

_diffrn_reflns_theta_max                25.03

_diffrn_reflns_theta_full               25.03

_diffrn_measured_fraction_theta_full

                                        0.989

_diffrn_measured_fraction_theta_max

                                        0.989

_reflns_number_total                    16870

_reflns_number_gt                       15479

_reflns_threshold_expression            >2sigma(I)



#----------------------------------------------------------------------------#

#                   COMPUTER PROGRAMS USED                                   #

#----------------------------------------------------------------------------#



_computing_data_collection

;

DENZO and COLLECT

;

_computing_cell_refinement              'DENZO and COLLECT'

_computing_data_reduction               'DENZO and COLLECT'

_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics           ORTEP

_computing_publication_material         CIFTAB



#----------------------------------------------------------------------------#

#                   REFINEMENT INFORMATION                                   #

#----------------------------------------------------------------------------#



_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                  fullcycle

_refine_ls_weighting_scheme             calc

_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              yes

_refine_ls_number_reflns                16870

_refine_ls_number_parameters            1212

_refine_ls_number_restraints            16

_refine_ls_R_factor_all                 0.0424

_refine_ls_R_factor_gt                  0.0372

_refine_ls_wR_factor_ref                0.0895

_refine_ls_wR_factor_gt                 0.086

_refine_ls_goodness_of_fit_ref          0.942

_refine_ls_restrained_S_all             1.535

_refine_ls_shift/su_max                 2.486

_refine_ls_shift/su_mean                0.136

_refine_ls_abs_structure_details

                                    'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack          0.370(16)

_refine_diff_density_max                1.599

_refine_diff_density_min                -1.823

_refine_diff_density_rms                0.128



#----------------------------------------------------------------------------#

#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #

#----------------------------------------------------------------------------#



loop_

    _atom_type_symbol

    _atom_type_description

    _atom_type_scat_dispersion_real

    _atom_type_scat_dispersion_imag

    _atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



loop_

    _atom_site_label

    _atom_site_type_symbol

    _atom_site_fract_x

    _atom_site_fract_y

    _atom_site_fract_z

    _atom_site_U_iso_or_equiv

    _atom_site_adp_type

    _atom_site_occupancy

    _atom_site_symmetry_multiplicity

    _atom_site_calc_flag

    _atom_site_refinement_flags

    _atom_site_disorder_assembly

    _atom_site_disorder_group

Re1 Re 0.0073(2) 0.58560(19) 0.08190(12) 0.02492(16) Uani 1 1 d . . .

Re2 Re 0.6745(2) 0.12711(19) -0.23624(12) 0.03102(17) Uani 1 1 d . . .

Re3 Re -0.2513(2) 1.07731(19) 1.10069(12) 0.03520(19) Uani 1 1 d . . .

Re4 Re 0.3919(2) 0.61754(19) 0.77704(12) 0.02615(16) Uani 1 1 d . . .

O1 O -0.6030(13) 0.8665(11) 0.2387(7) 0.041(3) Uani 1 1 d . . .

O2 O 0.1041(16) 0.3928(12) 0.2045(8) 0.052(4) Uani 1 1 d . . .

O3 O 0.0491(15) 0.7513(11) 0.1513(8) 0.045(4) Uani 1 1 d . . .

O4 O 0.3395(13) 0.5378(13) 0.0380(8) 0.053(4) Uani 1 1 d . . .

O5 O -0.0607(17) 0.7640(11) -0.0495(7) 0.049(4) Uani 1 1 d . . .

O6 O 0.0411(10) 0.3055(7) -0.0811(5) 0.029(2) Uani 1 1 d . . .

O7 O 0.1780(11) 0.4134(7) -0.1377(5) 0.026(2) Uani 1 1 d . . .

O8 O 0.778(2) -0.0029(12) -0.0947(8) 0.064(4) Uani 1 1 d . . .

O9 O 0.7212(19) 0.3135(12) -0.1904(8) 0.058(4) Uani 1 1 d . . .

O10 O 1.0029(15) 0.0641(13) -0.2905(8) 0.052(4) Uani 1 1 d . . .

O11 O 0.5567(17) 0.2878(11) -0.3708(7) 0.046(4) Uani 1 1 d . . .

O12 O 0.8684(13) -0.2555(11) -0.4179(7) 0.039(3) Uani 1 1 d . . .

O13 O -0.4710(14) 1.4672(11) 1.2788(7) 0.044(3) Uani 1 1 d . . .

O14 O -0.1310(17) 0.9151(14) 1.2341(8) 0.056(4) Uani 1 1 d . . .

O15 O -0.5712(15) 1.1302(14) 1.1561(9) 0.069(5) Uani 1 1 d . . .

O16 O -0.282(2) 0.8878(11) 1.0537(8) 0.061(4) Uani 1 1 d . . .

O17 O -0.3780(18) 1.2063(12) 0.9616(8) 0.060(4) Uani 1 1 d . . .

O18 O 0.3132(12) 0.9345(9) 0.9739(6) 0.052(3) Uani 1 1 d D . .

O19 O 0.1984(17) 0.8136(13) 0.9866(7) 0.154(9) Uani 1 1 d D . .

O20 O 0.4609(15) 0.4363(12) 0.9061(7) 0.046(4) Uani 1 1 d . . .

O21 O 0.0604(14) 0.6625(12) 0.8172(7) 0.046(3) Uani 1 1 d U . .

O22 O 0.2951(16) 0.8149(13) 0.6571(8) 0.059(5) Uani 1 1 d . . .

O23 O 0.3582(16) 0.4529(12) 0.7050(7) 0.049(4) Uani 1 1 d . . .

O24 O 1.0152(12) 0.3442(10) 0.6250(6) 0.039(3) Uani 1 1 d . . .

N1 N -0.2374(12) 0.6030(9) 0.0995(6) 0.020(3) Uani 1 1 d . . .

N2 N 0.5897(14) 0.0004(11) -0.2586(7) 0.031(3) Uani 1 1 d . . .

N3 N -0.1778(14) 1.2056(11) 1.1229(7) 0.028(3) Uani 1 1 d . . .

N4 N 0.6367(14) 0.6058(11) 0.7616(7) 0.029(3) Uani 1 1 d . . .

C1 C -1.187(3) 1.1155(16) 0.5565(9) 0.075(6) Uani 1 1 d . . .

H1A H -1.2079 1.0808 0.6012 0.113 Uiso 1 1 calc R . .

H1B H -1.2826 1.1474 0.5315 0.113 Uiso 1 1 calc R . .

H1C H -1.1377 1.1714 0.5563 0.113 Uiso 1 1 calc R . .

C2 C -1.082(3) 1.0316(16) 0.5256(9) 0.078(6) Uani 1 1 d . . .

H2A H -0.9864 0.9986 0.5514 0.093 Uiso 1 1 calc R . .

H2B H -1.1313 0.9746 0.5266 0.093 Uiso 1 1 calc R . .

C3 C -1.047(2) 1.0786(14) 0.4591(8) 0.058(5) Uani 1 1 d . . .

H3A H -0.9863 1.1294 0.4578 0.07 Uiso 1 1 calc R . .

H3B H -1.1418 1.1178 0.4336 0.07 Uiso 1 1 calc R . .

C4 C -0.955(3) 0.985(2) 0.4296(10) 0.092(8) Uani 1 1 d . . .

H4A H -0.8595 0.9466 0.4548 0.11 Uiso 1 1 calc R . .

H4B H -1.0151 0.9343 0.431 0.11 Uiso 1 1 calc R . .

C5 C -0.9195(18) 1.0378(15) 0.3576(9) 0.060(5) Uani 1 1 d . . .

H5A H -1.0152 1.0834 0.3349 0.072 Uiso 1 1 calc R . .

H5B H -0.8527 1.0843 0.3575 0.072 Uiso 1 1 calc R . .

C6 C -0.8439(18) 0.9573(15) 0.3201(8) 0.053(4) Uani 1 1 d . . .

H6A H -0.7478 0.9113 0.3424 0.063 Uiso 1 1 calc R . .

H6B H -0.9107 0.9112 0.3192 0.063 Uiso 1 1 calc R . .

C7 C -0.8123(18) 1.0118(13) 0.2524(8) 0.049(4) Uani 1 1 d . . .

H7A H -0.7403 1.0541 0.2535 0.059 Uiso 1 1 calc R . .

H7B H -0.9074 1.0616 0.2313 0.059 Uiso 1 1 calc R . .

C8 C -0.7471(16) 0.9337(12) 0.2130(7) 0.042(4) Uani 1 1 d . . .

H8A H -0.8171 0.8894 0.2132 0.05 Uiso 1 1 calc R . .

H8B H -0.7364 0.9734 0.1676 0.05 Uiso 1 1 calc R . .

C9 C -0.5195(14) 0.8014(11) 0.2033(6) 0.029(3) Uani 1 1 d . . .

C10 C -0.3762(14) 0.7420(11) 0.2282(7) 0.035(3) Uani 1 1 d . . .

H10 H -0.3417 0.7463 0.2681 0.042 Uiso 1 1 calc R . .

C11 C -0.2832(18) 0.6757(15) 0.1936(10) 0.032(5) Uani 1 1 d . . .

H11 H -0.1856 0.634 0.2104 0.039 Uiso 1 1 calc R . .

C12 C -0.334(2) 0.6706(17) 0.1342(10) 0.032(5) Uani 1 1 d . . .

C13 C -0.4797(19) 0.7260(16) 0.1140(9) 0.033(4) Uani 1 1 d . . .

H13 H -0.5177 0.7178 0.0759 0.04 Uiso 1 1 calc R . .

C14 C -0.5721(19) 0.7918(16) 0.1457(10) 0.031(4) Uani 1 1 d . . .

H14 H -0.671 0.8307 0.1292 0.037 Uiso 1 1 calc R . .

C15 C 0.066(2) 0.4633(18) 0.1598(12) 0.034(5) Uani 1 1 d . . .

C16 C 0.032(2) 0.6893(18) 0.1275(11) 0.036(5) Uani 1 1 d . . .

C17 C 0.214(3) 0.557(2) 0.0563(15) 0.045(7) Uani 1 1 d . . .

C18 C -0.037(3) 0.700(2) -0.0011(13) 0.034(6) Uani 1 1 d . . .

C19 C -0.298(2) 0.5542(17) 0.0684(11) 0.025(4) Uani 1 1 d . . .

H19 H -0.4026 0.557 0.0729 0.03 Uiso 1 1 calc R . .

C20 C -0.208(2) 0.4965(15) 0.0274(10) 0.029(4) Uani 1 1 d . . .

C21 C -0.053(2) 0.4892(15) 0.0254(9) 0.022(4) Uani 1 1 d . . .

C22 C 0.0332(17) 0.4285(14) -0.0143(8) 0.027(4) Uani 1 1 d . . .

H22 H 0.1388 0.4216 -0.0183 0.032 Uiso 1 1 calc R . .

C23 C -0.039(2) 0.3783(15) -0.0480(9) 0.033(4) Uani 1 1 d . . .

C24 C -0.191(2) 0.3863(17) -0.0454(11) 0.043(5) Uani 1 1 d . . .

H24 H -0.2354 0.3512 -0.069 0.051 Uiso 1 1 calc R . .

C25 C -0.277(2) 0.4458(18) -0.0083(10) 0.043(5) Uani 1 1 d . . .

H25 H -0.3826 0.4536 -0.0061 0.051 Uiso 1 1 calc R . .

C26 C 0.1478(19) 0.3271(12) -0.1218(8) 0.039(4) Uani 1 1 d . . .

C27 C 0.2261(19) 0.2363(14) -0.1487(9) 0.031(4) Uani 1 1 d . . .

C28 C 0.370(2) 0.2352(17) -0.1727(10) 0.041(5) Uani 1 1 d . . .

H28 H 0.4152 0.2893 -0.1699 0.049 Uiso 1 1 calc R . .

C29 C 0.451(3) 0.154(2) -0.2016(12) 0.035(6) Uani 1 1 d . . .

C30 C 0.377(2) 0.0746(17) -0.2040(10) 0.037(5) Uani 1 1 d . . .

C31 C 0.233(2) 0.0752(17) -0.1807(10) 0.043(5) Uani 1 1 d . . .

H31 H 0.1857 0.0222 -0.1838 0.052 Uiso 1 1 calc R . .

C32 C 0.159(2) 0.1574(19) -0.1525(10) 0.045(6) Uani 1 1 d . . .

H32 H 0.0613 0.159 -0.1355 0.054 Uiso 1 1 calc R . .

C33 C 0.4547(18) -0.0024(16) -0.2369(10) 0.033(4) Uani 1 1 d . . .

H33 H 0.409 -0.0544 -0.2429 0.039 Uiso 1 1 calc R . .

C34 C 0.742(3) 0.0393(18) -0.1463(13) 0.038(6) Uani 1 1 d . . .

C35 C 0.710(3) 0.244(2) -0.2090(11) 0.047(6) Uani 1 1 d . . .

C36 C 0.878(3) 0.0882(17) -0.2694(12) 0.040(5) Uani 1 1 d . . .

C37 C 0.600(3) 0.2247(19) -0.3217(13) 0.034(5) Uani 1 1 d . . .

C38 C 0.6650(19) -0.0699(15) -0.2966(10) 0.027(4) Uani 1 1 d . . .

C39 C 0.585(2) -0.0804(15) -0.3463(9) 0.028(4) Uani 1 1 d . . .

H39 H 0.4802 -0.0446 -0.3532 0.033 Uiso 1 1 calc R . .

C40 C 0.660(2) -0.1453(15) -0.3870(10) 0.035(5) Uani 1 1 d . . .

H40 H 0.6063 -0.1511 -0.4219 0.043 Uiso 1 1 calc R . .

C41 C 0.804(2) -0.1970(14) -0.3762(9) 0.033(4) Uani 1 1 d . . .

C42 C 0.8880(18) -0.1889(14) -0.3243(9) 0.027(4) Uani 1 1 d . . .

H42 H 0.9916 -0.2269 -0.3164 0.033 Uiso 1 1 calc R . .

C43 C 0.813(2) -0.1233(15) -0.2856(8) 0.030(4) Uani 1 1 d . . .

H43 H 0.8667 -0.1161 -0.2512 0.036 Uiso 1 1 calc R . .

C44 C 1.0243(19) -0.3145(17) -0.4095(10) 0.038(5) Uani 1 1 d . . .

H44A H 1.0412 -0.3692 -0.3672 0.046 Uiso 1 1 calc R . .

H44B H 1.0893 -0.2663 -0.4108 0.046 Uiso 1 1 calc R . .

C45 C 1.061(2) -0.3665(17) -0.4642(10) 0.035(5) Uani 1 1 d . . .

H45A H 1.053 -0.3105 -0.5057 0.042 Uiso 1 1 calc R . .

H45B H 0.986 -0.4063 -0.4657 0.042 Uiso 1 1 calc R . .

C46 C 1.221(2) -0.4433(19) -0.4571(11) 0.049(6) Uani 1 1 d . . .

H46A H 1.2238 -0.5018 -0.4172 0.059 Uiso 1 1 calc R . .

H46B H 1.2355 -0.4754 -0.494 0.059 Uiso 1 1 calc R . .

C47 C 1.352(2) -0.4004(19) -0.4540(11) 0.044(6) Uani 1 1 d . . .

H47A H 1.4427 -0.4608 -0.4394 0.053 Uiso 1 1 calc R . .

H47B H 1.3326 -0.3594 -0.4213 0.053 Uiso 1 1 calc R . .

C48 C 1.386(3) -0.326(2) -0.5204(15) 0.074(9) Uani 1 1 d . . .

H48A H 1.394 -0.3642 -0.5545 0.089 Uiso 1 1 calc R . .

H48B H 1.3008 -0.2612 -0.5326 0.089 Uiso 1 1 calc R . .

C49 C 1.525(3) -0.297(2) -0.5169(11) 0.059(7) Uani 1 1 d . . .

H49A H 1.6093 -0.362 -0.5035 0.07 Uiso 1 1 calc R . .

H49B H 1.5155 -0.2574 -0.4835 0.07 Uiso 1 1 calc R . .

C50 C 1.560(3) -0.229(3) -0.5800(15) 0.089(10) Uani 1 1 d . . .

H50A H 1.4782 -0.1616 -0.591 0.107 Uiso 1 1 calc R . .

H50B H 1.558 -0.2661 -0.6137 0.107 Uiso 1 1 calc R . .

C51 C 1.715(3) -0.201(3) -0.5827(16) 0.081(9) Uani 1 1 d . . .

H51A H 1.7427 -0.1764 -0.628 0.121 Uiso 1 1 calc R . .

H51B H 1.7938 -0.2643 -0.5605 0.121 Uiso 1 1 calc R . .

H51C H 1.707 -0.1442 -0.5613 0.121 Uiso 1 1 calc R . .

C53 C -1.312(4) 1.408(3) 1.4472(17) 0.084(9) Uani 1 1 d . . .

H53A H -1.3127 1.3621 1.4188 0.126 Uiso 1 1 calc R . .

H53B H -1.3902 1.4752 1.4323 0.126 Uiso 1 1 calc R . .

H53C H -1.3327 1.3716 1.4916 0.126 Uiso 1 1 calc R . .

C54 C -1.164(3) 1.429(2) 1.4455(14) 0.068(7) Uani 1 1 d . . .

H54A H -1.1615 1.4673 1.4785 0.081 Uiso 1 1 calc R . .

H54B H -1.0864 1.3598 1.4584 0.081 Uiso 1 1 calc R . .

C55 C -1.123(3) 1.490(3) 1.3845(14) 0.070(8) Uani 1 1 d . . .

H55A H -1.209 1.5535 1.3689 0.084 Uiso 1 1 calc R . .

H55B H -1.113 1.4464 1.3534 0.084 Uiso 1 1 calc R . .

C56 C -0.974(3) 1.531(2) 1.3794(11) 0.063(7) Uani 1 1 d . . .

H56A H -0.9747 1.5647 1.4149 0.075 Uiso 1 1 calc R . .

H56B H -0.8854 1.468 1.3868 0.075 Uiso 1 1 calc R . .

C57 C -0.955(3) 1.609(3) 1.3160(13) 0.061(8) Uani 1 1 d . . .

H57A H -1.0479 1.6688 1.3061 0.074 Uiso 1 1 calc R . .

H57B H -0.9426 1.573 1.281 0.074 Uiso 1 1 calc R . .

C58 C -0.818(2) 1.6558(18) 1.3155(12) 0.054(6) Uani 1 1 d . . .

H58A H -0.8201 1.7102 1.2737 0.065 Uiso 1 1 calc R . .

H58B H -0.8315 1.6928 1.3502 0.065 Uiso 1 1 calc R . .

C59 C -0.667(2) 1.5784(19) 1.3245(12) 0.050(6) Uani 1 1 d . . .

H59A H -0.6653 1.5228 1.3657 0.06 Uiso 1 1 calc R . .

H59B H -0.5905 1.6157 1.3283 0.06 Uiso 1 1 calc R . .

C60 C -0.624(2) 1.5243(19) 1.2693(11) 0.046(5) Uani 1 1 d . . .

H60A H -0.6873 1.4755 1.27 0.055 Uiso 1 1 calc R . .

H60B H -0.6391 1.5786 1.2269 0.055 Uiso 1 1 calc R . .

C61 C -0.4097(18) 1.4079(16) 1.2363(10) 0.032(4) Uani 1 1 d . . .

C62 C -0.483(2) 1.3963(16) 1.1872(10) 0.035(5) Uani 1 1 d . . .

H62 H -0.5862 1.4345 1.1778 0.042 Uiso 1 1 calc R . .

C63 C -0.4093(19) 1.3289(14) 1.1503(10) 0.031(4) Uani 1 1 d . . .

H63 H -0.4632 1.3202 1.1165 0.037 Uiso 1 1 calc R . .

C64 C -0.255(2) 1.2729(15) 1.1622(10) 0.028(4) Uani 1 1 d . . .

C65 C -0.180(2) 1.2863(17) 1.2127(11) 0.040(5) Uani 1 1 d . . .

H65 H -0.0765 1.2492 1.2216 0.048 Uiso 1 1 calc R . .

C66 C -0.251(2) 1.3502(18) 1.2490(11) 0.042(5) Uani 1 1 d . . .

H66 H -0.1974 1.358 1.2832 0.05 Uiso 1 1 calc R . .

C67 C -0.170(3) 0.974(2) 1.1866(14) 0.040(6) Uani 1 1 d . . .

C68 C -0.456(3) 1.111(2) 1.1373(13) 0.048(6) Uani 1 1 d . . .

C69 C -0.275(3) 0.9578(17) 1.0743(11) 0.045(6) Uani 1 1 d . . .

C70 C -0.329(3) 1.163(2) 1.0137(12) 0.039(6) Uani 1 1 d . . .

C71 C -0.047(2) 1.2134(16) 1.1048(10) 0.034(5) Uani 1 1 d . . .

H71 H -0.0093 1.2676 1.113 0.041 Uiso 1 1 calc R . .

C72 C 0.045(2) 1.1394(17) 1.0715(10) 0.039(5) Uani 1 1 d . . .

C73 C -0.019(3) 1.061(2) 1.0632(12) 0.038(6) Uani 1 1 d . . .

C74 C 0.071(3) 0.9904(18) 1.0327(12) 0.045(6) Uani 1 1 d . . .

H74 H 0.0345 0.9343 1.0262 0.054 Uiso 1 1 calc R . .

C75 C 0.216(2) 0.999(2) 1.0106(10) 0.058(9) Uani 1 1 d . . .

C76 C 0.278(2) 1.073(2) 1.0189(12) 0.055(6) Uani 1 1 d . . .

H76 H 0.3761 1.0765 1.0038 0.066 Uiso 1 1 calc R . .

C77 C 0.194(2) 1.143(2) 1.0495(10) 0.050(6) Uani 1 1 d . . .

H77 H 0.2352 1.1967 1.0569 0.059 Uiso 1 1 calc R . .

C78 C 0.2846(18) 0.8588(16) 0.9660(9) 0.126(6) Uani 1 1 d DU . .

C79 C 0.396(3) 0.8130(18) 0.9139(11) 0.058(6) Uani 1 1 d D . .

C80 C 0.345(3) 0.763(2) 0.8758(13) 0.061(6) Uani 1 1 d . . .

H80 H 0.2417 0.7631 0.8773 0.073 Uiso 1 1 calc R . .

C81 C 0.442(2) 0.7117(18) 0.8343(11) 0.038(5) Uani 1 1 d . . .

C82 C 0.592(2) 0.7160(16) 0.8344(10) 0.031(4) Uani 1 1 d . . .

C83 C 0.649(3) 0.7661(15) 0.8721(9) 0.041(5) Uani 1 1 d . . .

H83 H 0.7529 0.7662 0.87 0.049 Uiso 1 1 calc R . .

C84 C 0.553(3) 0.8163(15) 0.9131(9) 0.046(5) Uani 1 1 d . . .

H84 H 0.5884 0.8513 0.9395 0.055 Uiso 1 1 calc R . .

C85 C 0.690(2) 0.6581(16) 0.7930(12) 0.031(5) Uani 1 1 d . . .

H85 H 0.7934 0.6587 0.7891 0.037 Uiso 1 1 calc R . .

C86 C 0.442(2) 0.5000(18) 0.8583(12) 0.030(5) Uani 1 1 d . . .

C87 C 0.185(3) 0.645(2) 0.8014(12) 0.034(6) Uani 1 1 d . . .

C88 C 0.336(3) 0.741(2) 0.7003(11) 0.038(6) Uani 1 1 d . . .

C89 C 0.372(2) 0.5157(17) 0.7300(10) 0.032(5) Uani 1 1 d . . .

C90 C 0.7408(18) 0.5461(14) 0.7246(9) 0.020(4) Uani 1 1 d . . .

C91 C 0.6934(19) 0.5326(15) 0.6690(10) 0.030(4) Uani 1 1 d . . .

H91 H 0.5935 0.5688 0.6527 0.035 Uiso 1 1 calc R . .

C92 C 0.7875(16) 0.4678(13) 0.6366(7) 0.034(3) Uani 1 1 d . . .

H92 H 0.7537 0.4626 0.5968 0.041 Uiso 1 1 calc R . .

C93 C 0.9332(16) 0.4086(11) 0.6607(8) 0.033(3) Uani 1 1 d . . .

C94 C 0.983(2) 0.4245(16) 0.7159(10) 0.033(4) Uani 1 1 d . . .

H94 H 1.0851 0.3916 0.7307 0.039 Uiso 1 1 calc R . .

C95 C 0.8858(18) 0.4883(14) 0.7501(9) 0.028(4) Uani 1 1 d . . .

H95 H 0.9175 0.4927 0.7904 0.033 Uiso 1 1 calc R . .

C96 C 1.1596(15) 0.2763(12) 0.6549(8) 0.036(4) Uani 1 1 d . . .

H96A H 1.1447 0.236 0.6997 0.043 Uiso 1 1 calc R . .

H96B H 1.2295 0.32 0.6564 0.043 Uiso 1 1 calc R . .

C97 C 1.2237(17) 0.2004(12) 0.6137(8) 0.043(4) Uani 1 1 d . . .

H97A H 1.3183 0.1502 0.635 0.052 Uiso 1 1 calc R . .

H97B H 1.1511 0.1581 0.6135 0.052 Uiso 1 1 calc R . .

C98 C 1.2574(19) 0.2482(13) 0.5452(8) 0.044(4) Uani 1 1 d . . .

H98A H 1.3219 0.2967 0.5443 0.052 Uiso 1 1 calc R . .

H98B H 1.1616 0.2913 0.5216 0.052 Uiso 1 1 calc R . .

C99 C 1.338(2) 0.1639(15) 0.5106(9) 0.054(5) Uani 1 1 d . . .

H99A H 1.4369 0.1241 0.5326 0.065 Uiso 1 1 calc R . .

H99B H 1.2769 0.1125 0.5144 0.065 Uiso 1 1 calc R . .

C100 C 1.363(2) 0.2082(12) 0.4426(9) 0.055(5) Uani 1 1 d . . .

H10A H 1.4149 0.2648 0.4386 0.066 Uiso 1 1 calc R . .

H10B H 1.2635 0.2417 0.4199 0.066 Uiso 1 1 calc R . .

C101 C 1.458(3) 0.1253(17) 0.4090(9) 0.069(6) Uani 1 1 d . . .

H10C H 1.5519 0.086 0.4347 0.082 Uiso 1 1 calc R . .

H10D H 1.4 0.0732 0.4087 0.082 Uiso 1 1 calc R . .

C102 C 1.498(3) 0.1721(19) 0.3414(12) 0.085(7) Uani 1 1 d . . .

H10E H 1.5501 0.2271 0.3416 0.102 Uiso 1 1 calc R . .

H10F H 1.403 0.2083 0.3153 0.102 Uiso 1 1 calc R . .

C103 C 1.597(3) 0.0931(18) 0.3088(10) 0.071(6) Uani 1 1 d . . .

H10G H 1.6173 0.1305 0.2646 0.107 Uiso 1 1 calc R . .

H10H H 1.5452 0.0392 0.3073 0.107 Uiso 1 1 calc R . .

H10I H 1.6926 0.0585 0.3333 0.107 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

Re1 0.0155(3) 0.0267(3) 0.0338(4) -0.0100(3) 0.0004(2) -0.0057(2)

Re2 0.0345(3) 0.0257(4) 0.0347(4) -0.0123(3) 0.0012(3) -0.0069(3)

Re3 0.0423(4) 0.0249(4) 0.0394(4) -0.0134(3) -0.0021(3) -0.0053(3)

Re4 0.0158(3) 0.0257(3) 0.0359(4) -0.0074(3) 0.0013(2) -0.0048(2)

O1 0.028(6) 0.050(8) 0.049(8) -0.034(7) 0.005(5) 0.003(5)

O2 0.051(8) 0.047(9) 0.052(10) 0.013(7) -0.019(7) -0.028(7)

O3 0.043(7) 0.035(8) 0.068(10) -0.029(7) 0.000(7) -0.012(6)

O4 0.007(5) 0.076(9) 0.071(9) -0.013(7) 0.005(5) -0.007(5)

O5 0.061(9) 0.032(7) 0.044(8) 0.005(6) -0.010(7) -0.011(6)

O6 0.031(5) 0.026(5) 0.035(5) -0.018(4) 0.011(4) -0.006(4)

O7 0.031(5) 0.014(4) 0.029(5) 0.002(4) 0.008(4) -0.012(4)

O8 0.094(11) 0.045(9) 0.052(9) -0.009(7) -0.023(8) -0.017(8)

O9 0.096(11) 0.042(8) 0.052(9) -0.028(7) -0.002(8) -0.033(8)

O10 0.032(6) 0.063(9) 0.071(10) -0.024(8) 0.007(6) -0.023(6)

O11 0.066(9) 0.031(8) 0.036(8) -0.007(6) 0.000(6) -0.007(6)

O12 0.031(6) 0.046(8) 0.047(8) -0.029(6) 0.007(5) -0.006(5)

O13 0.043(7) 0.053(8) 0.047(8) -0.031(7) 0.006(6) -0.014(6)

O14 0.045(8) 0.069(11) 0.046(9) -0.001(8) -0.005(7) -0.013(7)

O15 0.029(6) 0.078(11) 0.110(14) -0.040(10) 0.015(7) -0.021(7)

O16 0.112(12) 0.028(7) 0.051(9) -0.014(7) 0.003(8) -0.027(7)

O17 0.076(10) 0.044(9) 0.056(9) 0.000(7) -0.029(8) -0.017(7)

O18 0.042(6) 0.052(7) 0.067(8) -0.022(6) -0.005(6) -0.014(5)

O19 0.129(15) 0.184(19) 0.25(2) -0.177(19) 0.124(15) -0.108(14)

O20 0.042(7) 0.058(9) 0.041(8) -0.006(7) -0.010(6) -0.024(7)

O21 0.037(3) 0.049(4) 0.049(4) -0.0107(18) 0.0029(16) -0.0100(18)

O22 0.042(8) 0.051(10) 0.066(11) 0.017(8) -0.013(8) -0.012(7)

O23 0.064(9) 0.058(9) 0.039(8) -0.016(7) -0.007(7) -0.035(7)

O24 0.022(5) 0.045(8) 0.045(8) -0.014(6) -0.001(5) 0.003(5)

N1 0.016(5) 0.022(7) 0.028(8) -0.012(6) 0.004(5) -0.009(5)

N2 0.026(6) 0.023(7) 0.044(9) -0.012(6) -0.002(6) -0.005(6)

N3 0.022(6) 0.035(8) 0.027(8) -0.012(6) 0.001(5) -0.001(6)

N4 0.026(6) 0.033(8) 0.030(8) -0.008(6) -0.001(6) -0.009(6)

C1 0.101(16) 0.070(13) 0.054(12) -0.017(10) 0.040(11) -0.029(12)

C2 0.110(18) 0.068(13) 0.043(11) 0.005(9) 0.004(11) -0.024(12)

C3 0.072(12) 0.052(10) 0.045(10) -0.008(8) 0.010(9) -0.015(9)

C4 0.087(16) 0.15(2) 0.069(14) -0.069(15) 0.046(12) -0.057(16)

C5 0.034(9) 0.076(12) 0.090(14) -0.061(11) 0.021(9) -0.013(8)

C6 0.035(8) 0.073(12) 0.051(10) -0.032(9) 0.009(7) -0.001(8)

C7 0.041(9) 0.047(9) 0.059(11) -0.024(8) 0.006(8) -0.002(7)

C8 0.033(8) 0.039(8) 0.044(9) -0.013(7) 0.004(6) 0.008(6)

C9 0.024(6) 0.039(7) 0.026(7) -0.011(6) -0.012(5) -0.005(6)

C10 0.021(6) 0.032(7) 0.046(8) -0.017(6) 0.008(6) 0.007(6)

C11 0.014(7) 0.028(10) 0.050(13) -0.010(9) -0.006(8) 0.001(7)

C12 0.027(9) 0.041(11) 0.035(11) -0.017(9) 0.001(8) -0.012(8)

C13 0.023(8) 0.050(12) 0.030(10) -0.018(9) -0.004(7) -0.008(8)

C14 0.015(8) 0.041(11) 0.037(11) -0.016(9) -0.001(7) -0.003(7)

C15 0.008(8) 0.040(13) 0.062(15) -0.026(11) 0.005(8) -0.009(8)

C16 0.015(8) 0.047(12) 0.046(13) -0.013(10) -0.007(8) -0.007(8)

C17 0.030(11) 0.032(13) 0.074(18) -0.014(12) -0.014(11) -0.005(9)

C18 0.025(11) 0.039(13) 0.043(13) -0.015(10) -0.001(9) -0.015(9)

C19 0.009(7) 0.036(11) 0.032(11) -0.009(9) 0.005(7) -0.008(7)

C20 0.035(10) 0.027(10) 0.032(11) -0.015(8) -0.003(8) -0.014(8)

C21 0.031(9) 0.021(9) 0.022(10) -0.015(8) 0.002(7) -0.010(7)

C22 0.020(7) 0.031(9) 0.023(8) -0.014(7) 0.007(6) 0.008(7)

C23 0.042(10) 0.022(9) 0.031(9) -0.011(7) -0.005(8) 0.004(8)

C24 0.039(10) 0.041(11) 0.057(13) -0.018(10) -0.001(9) -0.021(9)

C25 0.041(10) 0.058(13) 0.045(11) -0.031(10) 0.008(8) -0.023(9)

C26 0.036(9) 0.035(8) 0.043(10) 0.009(7) -0.018(8) -0.020(7)

C27 0.027(8) 0.029(8) 0.035(9) -0.015(7) -0.005(7) 0.004(7)

C28 0.042(10) 0.033(11) 0.039(11) -0.017(9) -0.005(8) 0.013(8)

C29 0.046(11) 0.026(11) 0.031(12) -0.009(9) -0.012(9) -0.001(9)

C30 0.028(9) 0.037(11) 0.035(11) -0.012(9) 0.000(8) 0.011(8)

C31 0.027(8) 0.048(11) 0.038(11) 0.001(9) -0.004(8) 0.004(8)

C32 0.021(8) 0.066(16) 0.029(10) -0.009(10) 0.006(7) 0.015(9)

C33 0.017(7) 0.035(11) 0.038(11) -0.007(9) 0.003(7) 0.002(7)

C34 0.035(11) 0.026(12) 0.055(14) -0.014(10) -0.011(10) -0.005(9)

C35 0.050(12) 0.063(15) 0.031(12) -0.020(10) 0.000(9) -0.012(10)

C36 0.051(12) 0.022(10) 0.050(13) -0.008(9) -0.003(10) -0.014(9)

C37 0.040(11) 0.032(12) 0.040(12) -0.017(10) 0.007(9) -0.016(9)

C38 0.025(9) 0.025(10) 0.037(11) -0.012(8) 0.010(8) -0.014(8)

C39 0.022(8) 0.035(11) 0.030(10) -0.011(8) -0.002(8) -0.009(8)

C40 0.041(10) 0.029(10) 0.043(12) -0.013(9) -0.018(9) -0.013(8)

C41 0.053(11) 0.020(9) 0.030(10) -0.013(8) 0.004(9) -0.010(8)

C42 0.022(8) 0.028(10) 0.030(10) -0.007(8) 0.002(7) -0.003(7)

C43 0.036(9) 0.039(11) 0.019(9) -0.013(8) 0.004(7) -0.014(8)

C44 0.029(9) 0.049(13) 0.043(12) -0.022(10) 0.005(8) -0.014(9)

C45 0.029(9) 0.041(12) 0.034(11) -0.014(9) 0.011(8) -0.008(8)

C46 0.032(10) 0.075(16) 0.050(13) -0.044(12) 0.003(9) 0.001(10)

C47 0.043(11) 0.047(14) 0.036(12) -0.013(10) 0.005(9) 0.001(10)

C48 0.046(13) 0.063(17) 0.12(2) -0.027(16) -0.041(15) -0.020(12)

C49 0.072(16) 0.066(16) 0.027(11) -0.008(11) 0.002(11) -0.006(13)

C50 0.064(16) 0.14(3) 0.063(18) 0.002(18) 0.000(14) -0.053(18)

C51 0.045(13) 0.12(3) 0.08(2) -0.021(18) 0.003(13) -0.022(14)

C53 0.10(2) 0.066(19) 0.07(2) 0.008(15) 0.003(16) -0.023(16)

C54 0.066(15) 0.064(16) 0.062(17) -0.001(13) -0.022(13) -0.012(13)

C55 0.042(13) 0.11(2) 0.08(2) -0.046(18) 0.002(13) -0.035(14)

C56 0.053(12) 0.11(2) 0.038(13) -0.036(14) -0.002(10) -0.031(13)

C57 0.049(14) 0.09(2) 0.054(16) -0.039(15) -0.004(12) -0.013(13)

C58 0.060(13) 0.041(12) 0.056(15) -0.005(10) -0.009(11) -0.011(10)

C59 0.053(12) 0.052(14) 0.063(15) -0.044(12) 0.002(11) -0.015(10)

C60 0.042(11) 0.055(15) 0.045(13) -0.028(11) 0.010(10) -0.008(10)

C61 0.017(8) 0.035(11) 0.049(12) -0.015(9) 0.004(8) -0.010(7)

C62 0.029(9) 0.032(11) 0.048(13) -0.018(10) 0.003(8) -0.007(8)

C63 0.023(8) 0.026(10) 0.049(12) -0.014(9) 0.002(8) -0.011(7)

C64 0.029(9) 0.025(10) 0.032(11) -0.014(8) 0.004(8) -0.004(8)

C65 0.041(10) 0.035(12) 0.046(13) -0.020(10) 0.002(9) -0.002(9)

C66 0.026(9) 0.061(14) 0.046(13) -0.025(11) 0.000(8) -0.013(9)

C67 0.028(10) 0.042(13) 0.059(15) -0.028(11) 0.006(9) -0.008(9)

C68 0.049(13) 0.047(13) 0.057(15) -0.017(11) -0.017(11) -0.022(11)

C69 0.066(13) 0.020(10) 0.037(13) 0.008(9) -0.002(10) -0.008(9)

C70 0.055(14) 0.033(13) 0.037(13) -0.014(10) -0.001(10) -0.017(10)

C71 0.043(11) 0.030(10) 0.027(10) 0.003(8) -0.004(8) -0.014(8)

C72 0.033(9) 0.040(11) 0.034(11) -0.005(9) -0.002(8) 0.004(8)

C73 0.040(11) 0.035(13) 0.029(12) -0.009(10) 0.007(9) 0.007(10)

C74 0.047(13) 0.035(11) 0.045(13) -0.014(9) -0.013(10) 0.010(9)

C75 0.040(12) 0.08(2) 0.023(10) -0.020(12) -0.007(9) 0.042(12)

C76 0.041(11) 0.066(14) 0.059(14) -0.024(11) -0.005(10) -0.006(10)

C77 0.028(9) 0.079(15) 0.028(10) -0.001(10) 0.016(8) -0.008(9)

C78 0.108(7) 0.120(7) 0.223(7) -0.100(2) 0.0923(18) -0.110(3)

C79 0.080(16) 0.045(12) 0.045(12) -0.024(10) 0.029(11) -0.005(11)

C80 0.051(12) 0.060(14) 0.084(17) -0.040(13) 0.004(11) -0.016(11)

C81 0.032(10) 0.035(12) 0.040(13) -0.001(10) 0.003(9) -0.005(9)

C82 0.035(10) 0.025(10) 0.034(11) -0.011(8) 0.008(8) -0.009(8)

C83 0.064(13) 0.035(10) 0.026(10) -0.002(8) -0.007(9) -0.024(9)

C84 0.094(17) 0.028(10) 0.024(9) -0.017(8) 0.006(10) -0.022(11)

C85 0.026(9) 0.021(10) 0.045(13) -0.011(9) 0.001(8) -0.005(7)

C86 0.015(9) 0.031(11) 0.048(13) -0.018(9) 0.002(8) -0.004(8)

C87 0.029(11) 0.040(13) 0.032(12) -0.010(10) 0.007(9) -0.009(10)

C88 0.028(10) 0.055(16) 0.034(13) -0.003(10) -0.001(9) -0.022(10)

C89 0.025(9) 0.037(12) 0.030(11) 0.004(9) 0.001(8) -0.012(8)

C90 0.016(7) 0.015(8) 0.030(10) -0.004(7) 0.001(7) -0.006(6)

C91 0.018(8) 0.038(11) 0.035(11) -0.015(9) 0.004(7) -0.007(7)

C92 0.028(7) 0.056(10) 0.026(8) -0.018(7) -0.004(6) -0.015(7)

C93 0.025(7) 0.030(8) 0.044(9) -0.018(7) 0.015(7) -0.001(6)

C94 0.020(8) 0.037(10) 0.037(11) -0.008(9) -0.006(8) -0.001(7)

C95 0.026(8) 0.027(9) 0.033(11) -0.010(8) 0.001(7) -0.010(7)

C96 0.015(7) 0.034(8) 0.053(10) -0.017(7) 0.002(6) 0.007(6)

C97 0.029(8) 0.035(8) 0.065(12) -0.022(8) 0.003(8) 0.002(7)

C98 0.037(9) 0.033(9) 0.057(11) -0.017(8) -0.007(8) 0.003(7)

C99 0.053(12) 0.053(11) 0.048(11) -0.009(9) 0.014(9) -0.007(9)

C100 0.078(14) 0.018(8) 0.052(12) 0.002(7) -0.004(10) 0.006(8)

C101 0.078(15) 0.063(13) 0.053(12) -0.023(10) 0.021(11) 0.004(11)

C102 0.089(17) 0.075(15) 0.11(2) -0.049(14) 0.047(15) -0.034(13)

C103 0.090(16) 0.074(14) 0.052(12) -0.035(11) 0.022(11) -0.012(12)





#----------------------------------------------------------------------------#

#                   MOLECULAR GEOMETRY                                       #

#----------------------------------------------------------------------------#



_geom_special_details

;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

    _geom_bond_atom_site_label_1

    _geom_bond_atom_site_label_2

    _geom_bond_distance

    _geom_bond_site_symmetry_2

    _geom_bond_publ_flag

Re1 C17 1.92(3) . ?

Re1 C15 1.98(2) . ?

Re1 C16 1.98(2) . ?

Re1 C18 1.99(3) . ?

Re1 C21 2.193(15) . ?

Re1 N1 2.217(12) . ?

Re2 C35 1.93(2) . ?

Re2 C36 1.95(2) . ?

Re2 C37 1.97(3) . ?

Re2 C34 2.00(3) . ?

Re2 C29 2.12(3) . ?

Re2 N2 2.233(13) . ?

Re3 C69 1.92(2) . ?

Re3 C70 1.96(3) . ?

Re3 C68 1.98(3) . ?

Re3 C67 2.02(3) . ?

Re3 N3 2.195(14) . ?

Re3 C73 2.21(3) . ?

Re4 C87 1.90(2) . ?

Re4 C89 1.97(2) . ?

Re4 C88 1.97(2) . ?

Re4 C86 1.99(2) . ?

Re4 C81 2.14(2) . ?

Re4 N4 2.223(14) . ?

O1 C9 1.371(18) . ?

O1 C8 1.427(19) . ?

O2 C15 1.14(2) . ?

O3 C16 1.14(2) . ?

O4 C17 1.18(3) . ?

O5 C18 1.14(3) . ?

O6 C26 1.316(17) . ?

O6 C23 1.398(19) . ?

O7 C26 1.226(15) . ?

O8 C34 1.12(3) . ?

O9 C35 1.15(2) . ?

O10 C36 1.20(2) . ?

O11 C37 1.17(3) . ?

O12 C41 1.362(18) . ?

O12 C44 1.432(18) . ?

O13 C61 1.375(19) . ?

O13 C60 1.40(2) . ?

O14 C67 1.12(3) . ?

O15 C68 1.10(3) . ?

O16 C69 1.16(2) . ?

O17 C70 1.16(2) . ?

O18 C78 1.18(2) . ?

O18 C75 1.44(2) . ?

O19 C78 1.13(2) . ?

O20 C86 1.13(2) . ?

O21 C87 1.16(2) . ?

O22 C88 1.15(2) . ?

O23 C89 1.16(2) . ?

O24 C93 1.365(13) . ?

O24 C96 1.458(14) . ?

N1 C19 1.294(18) . ?

N1 C12 1.43(2) . ?

N2 C33 1.308(17) . ?

N2 C38 1.434(19) . ?

N3 C71 1.26(2) . ?

N3 C64 1.432(19) . ?

N4 C85 1.296(19) . ?

N4 C90 1.431(19) . ?

C1 C2 1.55(3) . ?

C2 C3 1.45(2) . ?

C3 C4 1.58(3) . ?

C4 C5 1.57(3) . ?

C5 C6 1.53(2) . ?

C6 C7 1.49(2) . ?

C7 C8 1.51(2) . ?

C9 C10 1.391(19) . ?

C9 C14 1.401(18) . ?

C10 C11 1.404(19) . ?

C11 C12 1.40(3) . ?

C12 C13 1.37(3) . ?

C13 C14 1.36(3) . ?

C19 C20 1.42(3) . ?

C20 C21 1.40(3) . ?

C20 C25 1.42(2) . ?

C21 C22 1.41(2) . ?

C22 C23 1.41(2) . ?

C23 C24 1.37(3) . ?

C24 C25 1.36(3) . ?

C26 C27 1.49(3) . ?

C27 C28 1.39(3) . ?

C27 C32 1.39(3) . ?

C28 C29 1.43(3) . ?

C29 C30 1.42(3) . ?

C30 C31 1.39(3) . ?

C30 C33 1.43(3) . ?

C31 C32 1.41(3) . ?

C38 C43 1.35(2) . ?

C38 C39 1.39(2) . ?

C39 C40 1.43(3) . ?

C40 C41 1.31(3) . ?

C41 C42 1.44(2) . ?

C42 C43 1.40(2) . ?

C44 C45 1.51(3) . ?

C45 C46 1.54(3) . ?

C46 C47 1.48(3) . ?

C47 C48 1.57(4) . ?

C48 C49 1.45(3) . ?

C49 C50 1.49(4) . ?

C50 C51 1.57(4) . ?

C53 C54 1.46(4) . ?

C54 C55 1.44(4) . ?

C55 C56 1.59(3) . ?

C56 C57 1.52(4) . ?

C57 C58 1.54(3) . ?

C58 C59 1.48(3) . ?

C59 C60 1.54(3) . ?

C61 C62 1.35(3) . ?

C61 C66 1.46(3) . ?

C62 C63 1.39(3) . ?

C63 C64 1.41(2) . ?

C64 C65 1.39(3) . ?

C65 C66 1.34(3) . ?

C71 C72 1.45(3) . ?

C72 C73 1.40(3) . ?

C72 C77 1.44(3) . ?

C73 C74 1.37(3) . ?

C74 C75 1.42(4) . ?

C75 C76 1.33(4) . ?

C76 C77 1.35(3) . ?

C78 C79 1.61(3) . ?

C79 C80 1.36(3) . ?

C79 C84 1.45(3) . ?

C80 C81 1.41(3) . ?

C81 C82 1.40(3) . ?

C82 C83 1.39(3) . ?

C82 C85 1.46(3) . ?

C83 C84 1.39(3) . ?

C90 C91 1.37(3) . ?

C90 C95 1.40(2) . ?

C91 C92 1.36(2) . ?

C92 C93 1.40(2) . ?

C93 C94 1.38(2) . ?

C94 C95 1.39(3) . ?

C96 C97 1.52(2) . ?

C97 C98 1.49(2) . ?

C98 C99 1.53(2) . ?

C99 C100 1.45(2) . ?

C100 C101 1.54(2) . ?

C101 C102 1.49(3) . ?

C102 C103 1.51(3) . ?



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

C17 Re1 C15 89.2(11) . . ?

C17 Re1 C16 92.6(10) . . ?

C15 Re1 C16 93.1(9) . . ?

C17 Re1 C18 86.5(11) . . ?

C15 Re1 C18 174.5(11) . . ?

C16 Re1 C18 90.5(9) . . ?

C17 Re1 C21 93.9(9) . . ?

C15 Re1 C21 93.2(8) . . ?

C16 Re1 C21 171.0(7) . . ?

C18 Re1 C21 83.7(8) . . ?

C17 Re1 N1 170.0(8) . . ?

C15 Re1 N1 92.4(6) . . ?

C16 Re1 N1 97.2(6) . . ?

C18 Re1 N1 91.4(7) . . ?

C21 Re1 N1 76.2(5) . . ?

C35 Re2 C36 93.6(9) . . ?

C35 Re2 C37 90.3(9) . . ?

C36 Re2 C37 90.7(10) . . ?

C35 Re2 C34 85.3(9) . . ?

C36 Re2 C34 92.3(10) . . ?

C37 Re2 C34 174.8(10) . . ?

C35 Re2 C29 92.5(10) . . ?

C36 Re2 C29 173.8(9) . . ?

C37 Re2 C29 90.4(10) . . ?

C34 Re2 C29 87.1(10) . . ?

C35 Re2 N2 168.7(7) . . ?

C36 Re2 N2 97.7(6) . . ?

C37 Re2 N2 90.5(6) . . ?

C34 Re2 N2 93.3(6) . . ?

C29 Re2 N2 76.2(7) . . ?

C69 Re3 C70 85.9(9) . . ?

C69 Re3 C68 95.0(10) . . ?

C70 Re3 C68 91.5(11) . . ?

C69 Re3 C67 87.7(9) . . ?

C70 Re3 C67 173.5(9) . . ?

C68 Re3 C67 90.2(10) . . ?

C69 Re3 N3 168.4(8) . . ?

C70 Re3 N3 94.0(6) . . ?

C68 Re3 N3 96.7(6) . . ?

C67 Re3 N3 92.1(6) . . ?

C69 Re3 C73 93.3(10) . . ?

C70 Re3 C73 88.5(10) . . ?

C68 Re3 C73 171.7(10) . . ?

C67 Re3 C73 90.7(10) . . ?

N3 Re3 C73 75.1(7) . . ?

C87 Re4 C89 93.2(9) . . ?

C87 Re4 C88 89.2(10) . . ?

C89 Re4 C88 93.4(9) . . ?

C87 Re4 C86 88.6(10) . . ?

C89 Re4 C86 90.1(8) . . ?

C88 Re4 C86 176.0(11) . . ?

C87 Re4 C81 92.2(9) . . ?

C89 Re4 C81 171.9(7) . . ?

C88 Re4 C81 92.6(9) . . ?

C86 Re4 C81 84.2(8) . . ?

C87 Re4 N4 168.3(7) . . ?

C89 Re4 N4 98.4(6) . . ?

C88 Re4 N4 91.4(7) . . ?

C86 Re4 N4 90.1(6) . . ?

C81 Re4 N4 76.0(6) . . ?

C9 O1 C8 118.0(12) . . ?

C26 O6 C23 121.4(11) . . ?

C41 O12 C44 120.2(11) . . ?

C61 O13 C60 117.4(11) . . ?

C78 O18 C75 121.1(17) . . ?

C93 O24 C96 114.2(9) . . ?

C19 N1 C12 118.4(11) . . ?

C19 N1 Re1 114.1(9) . . ?

C12 N1 Re1 127.1(7) . . ?

C33 N2 C38 119.8(11) . . ?

C33 N2 Re2 114.0(9) . . ?

C38 N2 Re2 126.1(9) . . ?

C71 N3 C64 116.6(12) . . ?

C71 N3 Re3 116.5(9) . . ?

C64 N3 Re3 126.5(9) . . ?

C85 N4 C90 117.4(11) . . ?

C85 N4 Re4 113.6(9) . . ?

C90 N4 Re4 129.0(8) . . ?

C3 C2 C1 112.0(17) . . ?

C2 C3 C4 108.1(17) . . ?

C5 C4 C3 107(2) . . ?

C6 C5 C4 113.9(18) . . ?

C7 C6 C5 111.2(16) . . ?

C6 C7 C8 112.2(14) . . ?

O1 C8 C7 110.9(14) . . ?

O1 C9 C10 116.0(12) . . ?

O1 C9 C14 123.7(11) . . ?

C10 C9 C14 120.3(12) . . ?

C9 C10 C11 118.9(13) . . ?

C12 C11 C10 120.4(14) . . ?

C13 C12 C11 117.9(18) . . ?

C13 C12 N1 122.3(15) . . ?

C11 C12 N1 119.6(15) . . ?

C14 C13 C12 123.2(16) . . ?

C13 C14 C9 119.0(14) . . ?

O2 C15 Re1 177.9(16) . . ?

O3 C16 Re1 176.8(19) . . ?

O4 C17 Re1 176(2) . . ?

O5 C18 Re1 178(2) . . ?

N1 C19 C20 119.7(15) . . ?

C21 C20 C19 118.0(15) . . ?

C21 C20 C25 122.5(19) . . ?

C19 C20 C25 119.5(17) . . ?

C20 C21 C22 116.4(15) . . ?

C20 C21 Re1 111.9(12) . . ?

C22 C21 Re1 131.6(13) . . ?

C23 C22 C21 119.1(15) . . ?

C24 C23 O6 113.4(15) . . ?

C24 C23 C22 123.7(18) . . ?

O6 C23 C22 122.6(15) . . ?

C25 C24 C23 118.0(17) . . ?

C24 C25 C20 120.3(19) . . ?

O7 C26 O6 124.1(15) . . ?

O7 C26 C27 122.9(16) . . ?

O6 C26 C27 112.9(13) . . ?

C28 C27 C32 120.2(18) . . ?

C28 C27 C26 116.9(16) . . ?

C32 C27 C26 122.9(16) . . ?

C27 C28 C29 121(2) . . ?

C30 C29 C28 117(2) . . ?

C30 C29 Re2 114.5(17) . . ?

C28 C29 Re2 128.6(18) . . ?

C31 C30 C29 123(2) . . ?

C31 C30 C33 120.3(19) . . ?

C29 C30 C33 116.3(19) . . ?

C30 C31 C32 117(2) . . ?

C27 C32 C31 121.9(18) . . ?

N2 C33 C30 118.4(17) . . ?

O8 C34 Re2 174.9(18) . . ?

O9 C35 Re2 175(2) . . ?

O10 C36 Re2 179.2(17) . . ?

O11 C37 Re2 175.8(16) . . ?

C43 C38 C39 120.1(18) . . ?

C43 C38 N2 121.0(14) . . ?

C39 C38 N2 118.9(15) . . ?

C38 C39 C40 119.7(16) . . ?

C41 C40 C39 120.0(15) . . ?

C40 C41 O12 116.6(15) . . ?

C40 C41 C42 121.2(17) . . ?

O12 C41 C42 122.1(16) . . ?

C43 C42 C41 118.0(15) . . ?

C38 C43 C42 121.0(15) . . ?

O12 C44 C45 106.8(13) . . ?

C44 C45 C46 112.5(15) . . ?

C47 C46 C45 118.4(19) . . ?

C46 C47 C48 113.7(17) . . ?

C49 C48 C47 111.6(19) . . ?

C48 C49 C50 112(2) . . ?

C49 C50 C51 116(2) . . ?

C55 C54 C53 116(2) . . ?

C54 C55 C56 120(2) . . ?

C57 C56 C55 116.1(19) . . ?

C56 C57 C58 114.5(19) . . ?

C59 C58 C57 116(2) . . ?

C58 C59 C60 113.9(19) . . ?

O13 C60 C59 107.6(15) . . ?

C62 C61 O13 126.5(15) . . ?

C62 C61 C66 118.8(18) . . ?

O13 C61 C66 114.7(15) . . ?

C61 C62 C63 120.4(17) . . ?

C62 C63 C64 121.0(16) . . ?

C65 C64 C63 118.0(18) . . ?

C65 C64 N3 121.0(15) . . ?

C63 C64 N3 121.0(15) . . ?

C66 C65 C64 121.3(18) . . ?

C65 C66 C61 120.5(18) . . ?

O14 C67 Re3 176.5(18) . . ?

O15 C68 Re3 178(2) . . ?

O16 C69 Re3 174(2) . . ?

O17 C70 Re3 174.0(17) . . ?

N3 C71 C72 119.6(17) . . ?

C73 C72 C77 121(2) . . ?

C73 C72 C71 115.7(19) . . ?

C77 C72 C71 123(2) . . ?

C74 C73 C72 115(2) . . ?

C74 C73 Re3 132(2) . . ?

C72 C73 Re3 113.0(17) . . ?

C73 C74 C75 121(2) . . ?

C76 C75 C74 124(2) . . ?

C76 C75 O18 111(2) . . ?

C74 C75 O18 125(2) . . ?

C75 C76 C77 117(2) . . ?

C76 C77 C72 122(2) . . ?

O19 C78 O18 134(2) . . ?

O19 C78 C79 115(2) . . ?

O18 C78 C79 110.4(16) . . ?

C80 C79 C84 121(2) . . ?

C80 C79 C78 119(2) . . ?

C84 C79 C78 119.3(17) . . ?

C79 C80 C81 122(2) . . ?

C82 C81 C80 116(2) . . ?

C82 C81 Re4 115.9(16) . . ?

C80 C81 Re4 128.2(16) . . ?

C83 C82 C81 125(2) . . ?

C83 C82 C85 121.3(18) . . ?

C81 C82 C85 114.1(17) . . ?

C82 C83 C84 119(2) . . ?

C83 C84 C79 117.5(17) . . ?

N4 C85 C82 120.3(16) . . ?

O20 C86 Re4 175.2(17) . . ?

O21 C87 Re4 178.8(19) . . ?

O22 C88 Re4 176(2) . . ?

O23 C89 Re4 176.9(16) . . ?

C91 C90 C95 119.1(17) . . ?

C91 C90 N4 120.4(13) . . ?

C95 C90 N4 119.8(14) . . ?

C92 C91 C90 121.0(15) . . ?

C91 C92 C93 121.3(14) . . ?

O24 C93 C94 126.1(13) . . ?

O24 C93 C92 116.0(13) . . ?

C94 C93 C92 117.8(14) . . ?

C93 C94 C95 120.6(15) . . ?

C94 C95 C90 119.7(16) . . ?

O24 C96 C97 106.8(12) . . ?

C98 C97 C96 117.2(13) . . ?

C97 C98 C99 112.5(13) . . ?

C100 C99 C98 113.5(15) . . ?

C99 C100 C101 113.8(14) . . ?

C102 C101 C100 114.0(17) . . ?

C101 C102 C103 114.9(19) . . ?





data_s92-2



_audit_creation_date            1999-05-14T10:46:13-00:00

_audit_creation_method         'WinGX routine CIF_UPDATE'



#----------------------------------------------------------------------------#

#                   CHEMICAL INFORMATION                                     #

#----------------------------------------------------------------------------#



_chemical_name_systematic

;

 ?

;

_chemical_formula_sum                   'C43 H34 N2 O12 Re2'

_chemical_formula_weight                1143.12



#----------------------------------------------------------------------------#

#                   UNIT CELL INFORMATION                                    #

#----------------------------------------------------------------------------#



loop_

    _symmetry_equiv_pos_as_xyz

'x, y, z'

'-x, -y, -z'



_cell_length_a                          8.5056(2)

_cell_length_b                          11.9274(3)

_cell_length_c                          21.6445(8)

_cell_angle_alpha                       82.0034(19)

_cell_angle_beta                        82.2317(18)

_cell_angle_gamma                       71.9589(18)

_cell_volume                            2057.66(10)

_cell_formula_units_Z                   2

_cell_measurement_temperature           150(2)

_cell_measurement_reflns_used           na

_cell_measurement_theta_min             na

_cell_measurement_theta_max             na



#----------------------------------------------------------------------------#

#                   CRYSTAL INFORMATION                                      #

#----------------------------------------------------------------------------#



_exptl_crystal_size_max                 0.15

_exptl_crystal_size_mid                 0.07

_exptl_crystal_size_min                 0.04

_exptl_crystal_density_meas             'not measured'

_exptl_crystal_density_diffrn           1.845

_exptl_crystal_density_method           'not measured'

_exptl_crystal_F_000                    1104

_exptl_special_details

;

 ?

;



#----------------------------------------------------------------------------#

#                   ABSORPTION CORRECTION                                    #

#----------------------------------------------------------------------------#



_exptl_absorpt_coefficient_mu           5.943

_exptl_absorpt_correction_type          'Empirical, SORTAV'

_exptl_absorpt_correction_T_min         0.4693

_exptl_absorpt_correction_T_max         0.797



#----------------------------------------------------------------------------#

#                   DATA COLLECTION                                          #

#----------------------------------------------------------------------------#



_diffrn_ambient_temperature             150(2)

_diffrn_radiation_wavelength            0.71073

_diffrn_radiation_type                  MoK\a

_diffrn_radiation_monochromator         graphite

_diffrn_measurement_device_type         'Enraf Nonius KappaCCD area detector'

_diffrn_measurement_method

                                      'Phi and Omega scans to fill Ewald sphere'

_diffrn_standards_number                'not measured'

_diffrn_standards_interval_count        na

_diffrn_standards_interval_time         na

_diffrn_standards_decay_%               na

_diffrn_reflns_number                   28995

_diffrn_reflns_av_R_equivalents         0.0596

_diffrn_reflns_av_sigmaI/netI           0.0559

_diffrn_reflns_limit_h_min              -10

_diffrn_reflns_limit_h_max              10

_diffrn_reflns_limit_k_min              -14

_diffrn_reflns_limit_k_max              14

_diffrn_reflns_limit_l_min              -25

_diffrn_reflns_limit_l_max              25

_diffrn_reflns_theta_min                2.49

_diffrn_reflns_theta_max                25.25

_diffrn_reflns_theta_full               25.25

_diffrn_measured_fraction_theta_full

                                        0.985

_diffrn_measured_fraction_theta_max

                                        0.985

_reflns_number_total                    7333

_reflns_number_gt                       5818

_reflns_threshold_expression            >2sigma(I)



#----------------------------------------------------------------------------#

#                   COMPUTER PROGRAMS USED                                   #

#----------------------------------------------------------------------------#



_computing_data_collection

;

        DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998)

;

_computing_cell_refinement              'DENZO and COLLECT'

_computing_data_reduction               'DENZO and COLLECT'

_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics           ORTEP

_computing_publication_material         CIFTAB



#----------------------------------------------------------------------------#

#                   REFINEMENT INFORMATION                                   #

#----------------------------------------------------------------------------#



_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 w=1/[\s^2^(Fo^2^)+(0.0486P)^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           mixed

_refine_ls_extinction_method            none

_refine_ls_extinction_coef              yes

_refine_ls_number_reflns                7333

_refine_ls_number_parameters            545

_refine_ls_number_restraints            18

_refine_ls_R_factor_all                 0.0521

_refine_ls_R_factor_gt                  0.0367

_refine_ls_wR_factor_ref                0.0898

_refine_ls_wR_factor_gt                 0.0847

_refine_ls_goodness_of_fit_ref          1.005

_refine_ls_restrained_S_all             1.008

_refine_ls_shift/su_max                 0.001

_refine_ls_shift/su_mean                0

_refine_diff_density_max                1.271

_refine_diff_density_min                -2.051

_refine_diff_density_rms                0.159



#----------------------------------------------------------------------------#

#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #

#----------------------------------------------------------------------------#



loop_

    _atom_type_symbol

    _atom_type_description

    _atom_type_scat_dispersion_real

    _atom_type_scat_dispersion_imag

    _atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



loop_

    _atom_site_label

    _atom_site_type_symbol

    _atom_site_fract_x

    _atom_site_fract_y

    _atom_site_fract_z

    _atom_site_U_iso_or_equiv

    _atom_site_adp_type

    _atom_site_occupancy

    _atom_site_calc_flag

    _atom_site_refinement_flags

    _atom_site_disorder_assembly

    _atom_site_disorder_group

Re1 Re 0.13488(3) -0.115199(18) -0.123870(11) 0.02514(9) Uani 1 d . . .

Re2 Re 0.52116(3) 0.547054(18) 0.298893(11) 0.02758(9) Uani 1 d . . .

O1 O -0.0973(7) -0.1529(6) -0.3502(3) 0.0786(19) Uani 1 d D . .

O2 O 0.1936(5) -0.1286(4) 0.0166(2) 0.0375(10) Uani 1 d . . .

O3 O 0.5144(5) -0.1910(4) -0.1719(2) 0.0370(11) Uani 1 d . . .

O4 O -0.2506(5) -0.0494(4) -0.0957(2) 0.0453(12) Uani 1 d . . .

O5 O 0.1489(7) -0.3795(4) -0.1117(3) 0.0708(18) Uani 1 d . . .

O6 O 0.4611(5) 0.2860(3) 0.0397(2) 0.0372(10) Uani 1 d . . .

O7 O 0.2126(5) 0.4212(3) 0.0366(2) 0.0345(10) Uani 1 d . . .

O8 O 0.5250(6) 0.2896(4) 0.2841(2) 0.0483(13) Uani 1 d . . .

O9 O 0.6774(8) 0.4705(4) 0.4231(3) 0.077(2) Uani 1 d . . .

O10 O 0.1771(7) 0.6128(5) 0.3782(3) 0.0681(17) Uani 1 d . . .

O11 O 0.8750(6) 0.5174(5) 0.2299(3) 0.0794(19) Uani 1 d . . .

O12 O 0.6300(5) 0.9300(3) 0.3852(2) 0.0370(11) Uani 1 d D . .

N1 N 0.4039(5) 0.6428(4) 0.2136(2) 0.0236(11) Uani 1 d . . .

N2 N 0.1362(5) 0.0707(4) -0.1472(2) 0.0226(10) Uani 1 d . . .

C43 C 0.7285(10) 1.2042(6) 0.5121(3) 0.053(2) Uani 1 d D . .

H43A H 0.7264 1.2865 0.5131 0.08 Uiso 1 calc R . .

H43B H 0.8408 1.1515 0.5178 0.08 Uiso 1 calc R . .

H43C H 0.65 1.1835 0.5458 0.08 Uiso 1 calc R . .

C42 C 0.6791(8) 1.1902(5) 0.4490(3) 0.0322(14) Uani 1 d D . .

H42A H 0.566 1.2439 0.4432 0.039 Uiso 1 calc R . .

H42B H 0.7566 1.2134 0.4149 0.039 Uiso 1 calc R . .

C41 C 0.6823(8) 1.0657(5) 0.4448(3) 0.0345(15) Uani 1 d D . .

H41A H 0.6114 1.041 0.481 0.041 Uiso 1 calc R . .

H41B H 0.7973 1.0132 0.448 0.041 Uiso 1 calc R . .

C40 C 0.6227(7) 1.0488(4) 0.3845(3) 0.0323(14) Uani 1 d D . .

H40A H 0.5071 1.0999 0.381 0.039 Uiso 1 calc R . .

H40B H 0.6938 1.0716 0.3479 0.039 Uiso 1 calc R . .

C1 C -0.180(2) -0.3352(12) -0.4962(5) 0.065(4) Uani 0.671(7) d PD A 1

H1A H -0.1316 -0.3218 -0.5393 0.097 Uiso 0.671(7) calc PR A 1

H1B H -0.2988 -0.2913 -0.4928 0.097 Uiso 0.671(7) calc PR A 1

H1C H -0.1666 -0.4201 -0.4854 0.097 Uiso 0.671(7) calc PR A 1

C2 C -0.0924(14) -0.2923(11) -0.4511(4) 0.083(4) Uani 0.671(7) d PD A 1

H2A H 0.0276 -0.336 -0.4551 0.099 Uiso 0.671(7) calc PR A 1

H2B H -0.1044 -0.207 -0.4626 0.099 Uiso 0.671(7) calc PR A 1

C3 C -0.1626(14) -0.3106(11) -0.3853(4) 0.063(3) Uani 0.671(7) d PD A 1

H3A H -0.1528 -0.3958 -0.3747 0.076 Uiso 0.671(7) calc PR A 1

H3B H -0.2824 -0.2662 -0.3818 0.076 Uiso 0.671(7) calc PR A 1

C4 C -0.0795(14) -0.2719(7) -0.3375(4) 0.053(3) Uani 0.671(7) d PD A 1

H4A H -0.1311 -0.2882 -0.2948 0.063 Uiso 0.671(7) calc PR A 1

H4B H 0.0399 -0.3171 -0.3395 0.063 Uiso 0.671(7) calc PR A 1

C1' C -0.182(5) -0.3861(19) -0.5030(12) 0.065(4) Uani 0.329(7) d PD A 2

H1A' H -0.1983 -0.3844 -0.5472 0.097 Uiso 0.329(7) calc PR A 2

H1B' H -0.2683 -0.414 -0.4764 0.097 Uiso 0.329(7) calc PR A 2

H1C' H -0.0726 -0.4398 -0.4945 0.097 Uiso 0.329(7) calc PR A 2

C2' C -0.195(4) -0.2614(16) -0.4889(9) 0.083(4) Uani 0.329(7) d PD A 2

H2A' H -0.1144 -0.2308 -0.5181 0.099 Uiso 0.329(7) calc PR A 2

H2B' H -0.308 -0.2081 -0.4955 0.099 Uiso 0.329(7) calc PR A 2

C3' C -0.161(4) -0.2611(16) -0.4232(7) 0.063(3) Uani 0.329(7) d PD A 2

H3A' H -0.0607 -0.3274 -0.4139 0.076 Uiso 0.329(7) calc PR A 2

H3B' H -0.2555 -0.2752 -0.3944 0.076 Uiso 0.329(7) calc PR A 2

C4' C -0.135(3) -0.1461(15) -0.4104(6) 0.053(3) Uani 0.329(7) d PD A 2

H4A' H -0.0438 -0.1296 -0.4401 0.063 Uiso 0.329(7) calc PR A 2

H4B' H -0.2375 -0.0798 -0.4173 0.063 Uiso 0.329(7) calc PR A 2

C5 C 0.0626(7) -0.0701(5) -0.2183(3) 0.0310(14) Uani 1 d . . .

C6 C 0.0481(7) 0.0485(5) -0.2422(3) 0.0308(14) Uani 1 d . . .

C7 C -0.0108(7) 0.0964(6) -0.3009(3) 0.0407(16) Uani 1 d . . .

H7 H -0.0178 0.1762 -0.3162 0.049 Uiso 1 calc R . .

C8 C -0.0584(8) 0.0263(6) -0.3359(3) 0.0448(18) Uani 1 d . . .

H8 H -0.0988 0.0576 -0.3754 0.054 Uiso 1 calc R . .

C9 C -0.0466(8) -0.0906(6) -0.3128(3) 0.0393(17) Uani 1 d . . .

C10 C 0.0146(7) -0.1376(6) -0.2559(3) 0.0357(15) Uani 1 d . . .

H10 H 0.0245 -0.2183 -0.2418 0.043 Uiso 1 calc R . .

C11 C 0.1770(7) -0.1251(5) -0.0360(3) 0.0285(14) Uani 1 d . . .

C12 C 0.3769(8) -0.1648(5) -0.1539(3) 0.0282(14) Uani 1 d . . .

C13 C -0.1092(8) -0.0712(5) -0.1036(3) 0.0325(14) Uani 1 d . . .

C14 C 0.1408(8) -0.2791(6) -0.1154(4) 0.0468(19) Uani 1 d . . .

C15 C 0.0947(7) 0.1168(5) -0.2023(3) 0.0305(14) Uani 1 d . . .

H15 H 0.0951 0.1958 -0.2164 0.037 Uiso 1 calc R . .

C16 C 0.1829(6) 0.1388(5) -0.1074(3) 0.0228(12) Uani 1 d . . .

C17 C 0.3321(6) 0.0899(5) -0.0800(3) 0.0242(13) Uani 1 d . . .

H17 H 0.4018 0.0133 -0.0886 0.029 Uiso 1 calc R . .

C18 C 0.3775(6) 0.1521(5) -0.0408(3) 0.0251(13) Uani 1 d . . .

H18 H 0.4806 0.1196 -0.0232 0.03 Uiso 1 calc R . .

C19 C 0.2736(6) 0.2634(5) -0.0261(3) 0.0234(13) Uani 1 d . . .

C20 C 0.1249(7) 0.3127(5) -0.0536(3) 0.0288(14) Uani 1 d . . .

H20 H 0.0542 0.3887 -0.0445 0.035 Uiso 1 calc R . .

C21 C 0.0809(7) 0.2500(5) -0.0945(3) 0.0288(14) Uani 1 d . . .

H21 H -0.0196 0.2836 -0.1137 0.035 Uiso 1 calc R . .

C22 C 0.3268(6) 0.3227(5) 0.0189(3) 0.0261(13) Uani 1 d . . .

C23 C 0.2599(6) 0.4779(5) 0.0817(3) 0.0283(14) Uani 1 d . . .

C24 C 0.2203(7) 0.4513(5) 0.1441(3) 0.0286(14) Uani 1 d . . .

H24 H 0.1626 0.3941 0.1575 0.034 Uiso 1 calc R . .

C25 C 0.2637(7) 0.5070(5) 0.1874(3) 0.0301(14) Uani 1 d . . .

H25 H 0.2348 0.4893 0.2309 0.036 Uiso 1 calc R . .

C26 C 0.3510(7) 0.5905(5) 0.1677(3) 0.0259(13) Uani 1 d . . .

C27 C 0.3850(7) 0.6186(5) 0.1045(3) 0.0286(14) Uani 1 d . . .

H27 H 0.4412 0.6765 0.0908 0.034 Uiso 1 calc R . .

C28 C 0.3388(7) 0.5640(5) 0.0610(3) 0.0323(15) Uani 1 d . . .

H28 H 0.3607 0.585 0.0174 0.039 Uiso 1 calc R . .

C29 C 0.5204(8) 0.3854(6) 0.2887(3) 0.0342(15) Uani 1 d . . .

C30 C 0.6196(10) 0.4955(5) 0.3767(4) 0.0465(19) Uani 1 d . . .

C31 C 0.3013(9) 0.5864(5) 0.3484(3) 0.0415(17) Uani 1 d . . .

C32 C 0.7449(9) 0.5251(6) 0.2532(4) 0.0452(18) Uani 1 d . . .

C33 C 0.3925(7) 0.7561(5) 0.2045(3) 0.0272(14) Uani 1 d . . .

H33 H 0.3448 0.8038 0.1689 0.033 Uiso 1 calc R . .

C35 C 0.4529(6) 0.8068(5) 0.2490(3) 0.0243(13) Uani 1 d . . .

C34 C 0.5224(7) 0.7282(5) 0.3000(3) 0.0265(13) Uani 1 d . . .

C36 C 0.4443(7) 0.9266(5) 0.2426(3) 0.0286(14) Uani 1 d . . .

H36 H 0.398 0.977 0.2074 0.034 Uiso 1 calc . . .

C37 C 0.5025(7) 0.9723(4) 0.2868(3) 0.0262(13) Uani 1 d . . .

H37 H 0.4957 1.0539 0.2827 0.031 Uiso 1 calc . . .

C38 C 0.5721(7) 0.8958(5) 0.3379(3) 0.0292(14) Uani 1 d . . .

C39 C 0.5821(8) 0.7749(5) 0.3432(3) 0.0329(15) Uani 1 d . . .

H39 H 0.6315 0.724 0.3777 0.039 Uiso 1 calc . . .



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

Re1 0.02427(14) 0.02210(14) 0.03237(17) -0.00571(10) -0.00737(10) -0.00847(11)

Re2 0.03557(15) 0.02014(14) 0.03043(17) -0.00352(10) -0.00809(11) -0.01074(11)

O1 0.062(3) 0.111(5) 0.081(5) -0.057(4) -0.015(3) -0.028(4)

O2 0.037(2) 0.040(3) 0.038(3) 0.000(2) -0.007(2) -0.015(2)

O3 0.034(3) 0.033(2) 0.040(3) -0.005(2) -0.001(2) -0.005(2)

O4 0.026(2) 0.064(3) 0.049(3) 0.002(2) -0.012(2) -0.018(2)

O5 0.081(4) 0.024(3) 0.117(5) -0.005(3) -0.022(4) -0.026(3)

O6 0.029(2) 0.037(2) 0.047(3) -0.014(2) -0.014(2) -0.004(2)

O7 0.027(2) 0.031(2) 0.049(3) -0.019(2) -0.0111(19) -0.0040(19)

O8 0.081(4) 0.019(2) 0.052(3) -0.006(2) -0.015(3) -0.021(2)

O9 0.136(6) 0.041(3) 0.069(4) 0.002(3) -0.064(4) -0.026(3)

O10 0.068(4) 0.056(3) 0.069(4) -0.011(3) 0.029(3) -0.014(3)

O11 0.036(3) 0.085(4) 0.113(6) -0.019(4) 0.009(3) -0.015(3)

O12 0.061(3) 0.024(2) 0.035(3) -0.0022(18) -0.016(2) -0.022(2)

N1 0.025(2) 0.025(3) 0.025(3) -0.002(2) -0.002(2) -0.013(2)

N2 0.020(2) 0.024(2) 0.025(3) -0.009(2) -0.003(2) -0.007(2)

C43 0.085(6) 0.056(5) 0.035(5) -0.009(3) -0.006(4) -0.044(4)

C42 0.047(4) 0.036(3) 0.017(3) -0.003(3) 0.002(3) -0.019(3)

C41 0.047(4) 0.037(3) 0.027(4) -0.003(3) -0.006(3) -0.022(3)

C40 0.039(3) 0.027(3) 0.037(4) -0.008(3) -0.002(3) -0.017(3)

C1 0.078(7) 0.069(11) 0.054(7) -0.034(7) -0.027(6) -0.011(10)

C2 0.065(9) 0.061(8) 0.125(13) -0.029(8) -0.029(8) -0.006(7)

C3 0.086(8) 0.058(8) 0.046(9) -0.012(6) 0.002(7) -0.024(7)

C4 0.069(7) 0.043(6) 0.059(7) -0.016(5) -0.019(6) -0.026(5)

C1' 0.078(7) 0.069(11) 0.054(7) -0.034(7) -0.027(6) -0.011(10)

C2' 0.065(9) 0.061(8) 0.125(13) -0.029(8) -0.029(8) -0.006(7)

C3' 0.086(8) 0.058(8) 0.046(9) -0.012(6) 0.002(7) -0.024(7)

C4' 0.069(7) 0.043(6) 0.059(7) -0.016(5) -0.019(6) -0.026(5)

C5 0.020(3) 0.037(3) 0.037(4) -0.012(3) -0.005(3) -0.006(3)

C6 0.026(3) 0.041(4) 0.026(4) -0.010(3) -0.002(3) -0.008(3)

C7 0.035(3) 0.047(4) 0.038(4) -0.006(3) -0.009(3) -0.006(3)

C8 0.038(4) 0.070(5) 0.027(4) -0.012(3) -0.013(3) -0.008(4)

C9 0.032(3) 0.054(4) 0.037(4) -0.022(3) -0.013(3) -0.008(3)

C10 0.030(3) 0.041(4) 0.042(4) -0.017(3) -0.004(3) -0.013(3)

C11 0.022(3) 0.017(3) 0.048(5) 0.004(3) -0.009(3) -0.009(3)

C12 0.036(4) 0.023(3) 0.028(4) -0.005(2) -0.008(3) -0.010(3)

C13 0.038(4) 0.038(4) 0.029(4) -0.003(3) -0.009(3) -0.019(3)

C14 0.032(4) 0.042(4) 0.063(5) -0.005(4) -0.012(3) -0.003(3)

C15 0.029(3) 0.032(3) 0.034(4) -0.007(3) -0.006(3) -0.011(3)

C16 0.021(3) 0.023(3) 0.028(3) -0.006(2) -0.003(2) -0.010(2)

C17 0.016(3) 0.024(3) 0.032(4) -0.006(2) -0.004(2) -0.004(2)

C18 0.018(3) 0.024(3) 0.036(4) -0.005(3) -0.008(2) -0.006(2)

C19 0.021(3) 0.028(3) 0.027(4) -0.005(2) 0.000(2) -0.015(3)

C20 0.025(3) 0.025(3) 0.038(4) -0.008(3) -0.008(3) -0.006(3)

C21 0.025(3) 0.028(3) 0.036(4) -0.007(3) -0.012(3) -0.004(3)

C22 0.018(3) 0.023(3) 0.038(4) -0.004(3) -0.004(3) -0.006(3)

C23 0.019(3) 0.032(3) 0.037(4) -0.016(3) -0.008(3) -0.004(3)

C24 0.026(3) 0.022(3) 0.041(4) -0.003(3) -0.009(3) -0.010(3)

C25 0.028(3) 0.028(3) 0.034(4) -0.005(3) -0.006(3) -0.006(3)

C26 0.025(3) 0.021(3) 0.036(4) -0.004(3) -0.004(3) -0.011(3)

C27 0.026(3) 0.031(3) 0.034(4) -0.003(3) -0.008(3) -0.014(3)

C28 0.033(3) 0.038(4) 0.030(4) -0.016(3) -0.002(3) -0.012(3)

C29 0.037(4) 0.032(4) 0.031(4) -0.001(3) -0.008(3) -0.004(3)

C30 0.079(5) 0.024(3) 0.045(5) -0.002(3) -0.026(4) -0.020(4)

C31 0.064(5) 0.026(3) 0.039(4) -0.002(3) 0.004(4) -0.023(3)

C32 0.042(4) 0.038(4) 0.060(5) -0.008(3) -0.011(4) -0.014(3)

C33 0.024(3) 0.032(3) 0.029(4) -0.004(3) -0.010(3) -0.009(3)

C35 0.022(3) 0.021(3) 0.034(4) -0.007(2) -0.003(2) -0.011(2)

C34 0.029(3) 0.018(3) 0.036(4) -0.006(2) -0.002(3) -0.011(3)

C36 0.031(3) 0.028(3) 0.030(4) 0.004(3) -0.007(3) -0.014(3)

C37 0.031(3) 0.013(3) 0.036(4) 0.001(2) -0.007(3) -0.009(2)

C38 0.038(3) 0.027(3) 0.029(4) -0.009(3) -0.008(3) -0.014(3)

C39 0.042(4) 0.022(3) 0.037(4) -0.003(3) -0.015(3) -0.009(3)





#----------------------------------------------------------------------------#

#                   MOLECULAR GEOMETRY                                       #

#----------------------------------------------------------------------------#



_geom_special_details

;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

    _geom_bond_atom_site_label_1

    _geom_bond_atom_site_label_2

    _geom_bond_distance

    _geom_bond_site_symmetry_2

    _geom_bond_publ_flag

Re1 C14 1.924(7) . ?

Re1 C11 1.963(7) . ?

Re1 C13 1.980(6) . ?

Re1 C12 2.000(6) . ?

Re1 C5 2.162(6) . ?

Re1 N2 2.208(4) . ?

Re2 C30 1.921(7) . ?

Re2 C29 1.973(7) . ?

Re2 C31 1.980(7) . ?

Re2 C32 1.981(7) . ?

Re2 C34 2.167(5) . ?

Re2 N1 2.216(5) . ?

O1 C9 1.362(8) . ?

O1 C4' 1.370(7) . ?

O1 C4 1.373(6) . ?

O2 C11 1.160(7) . ?

O3 C12 1.141(7) . ?

O4 C13 1.143(7) . ?

O5 C14 1.170(8) . ?

O6 C22 1.215(6) . ?

O7 C22 1.337(6) . ?

O7 C23 1.425(7) . ?

O8 C29 1.149(7) . ?

O9 C30 1.139(8) . ?

O10 C31 1.139(8) . ?

O11 C32 1.134(8) . ?

O12 C38 1.355(7) . ?

O12 C40 1.396(5) . ?

N1 C33 1.314(7) . ?

N1 C26 1.431(7) . ?

N2 C15 1.289(7) . ?

N2 C16 1.431(7) . ?

C43 C42 1.526(8) . ?

C42 C41 1.492(7) . ?

C41 C40 1.523(7) . ?

C1 C2 1.532(9) . ?

C2 C3 1.484(8) . ?

C3 C4 1.521(8) . ?

C1' C2' 1.528(9) . ?

C2' C3' 1.489(9) . ?

C3' C4' 1.522(8) . ?

C5 C10 1.397(8) . ?

C5 C6 1.410(9) . ?

C6 C7 1.408(8) . ?

C6 C15 1.435(8) . ?

C7 C8 1.379(9) . ?

C8 C9 1.392(10) . ?

C9 C10 1.380(9) . ?

C16 C21 1.383(7) . ?

C16 C17 1.397(7) . ?

C17 C18 1.365(7) . ?

C18 C19 1.399(7) . ?

C19 C20 1.394(7) . ?

C19 C22 1.471(8) . ?

C20 C21 1.389(8) . ?

C23 C24 1.365(8) . ?

C23 C28 1.388(8) . ?

C24 C25 1.370(8) . ?

C25 C26 1.407(8) . ?

C26 C27 1.375(8) . ?

C27 C28 1.378(8) . ?

C33 C35 1.430(8) . ?

C35 C36 1.397(7) . ?

C35 C34 1.410(8) . ?

C34 C39 1.377(8) . ?

C36 C37 1.378(8) . ?

C37 C38 1.402(8) . ?

C38 C39 1.407(8) . ?



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

C14 Re1 C11 91.8(3) . . ?

C14 Re1 C13 89.1(3) . . ?

C11 Re1 C13 93.2(2) . . ?

C14 Re1 C12 88.6(3) . . ?

C11 Re1 C12 93.2(2) . . ?

C13 Re1 C12 173.3(2) . . ?

C14 Re1 C5 97.4(3) . . ?

C11 Re1 C5 169.2(2) . . ?

C13 Re1 C5 81.5(2) . . ?

C12 Re1 C5 92.6(2) . . ?

C14 Re1 N2 172.3(3) . . ?

C11 Re1 N2 95.3(2) . . ?

C13 Re1 N2 93.5(2) . . ?

C12 Re1 N2 88.07(19) . . ?

C5 Re1 N2 75.8(2) . . ?

C30 Re2 C29 92.3(3) . . ?

C30 Re2 C31 87.8(3) . . ?

C29 Re2 C31 93.8(3) . . ?

C30 Re2 C32 89.9(3) . . ?

C29 Re2 C32 93.1(3) . . ?

C31 Re2 C32 172.8(3) . . ?

C30 Re2 C34 92.9(2) . . ?

C29 Re2 C34 174.3(2) . . ?

C31 Re2 C34 88.8(2) . . ?

C32 Re2 C34 84.5(2) . . ?

C30 Re2 N1 168.4(2) . . ?

C29 Re2 N1 99.3(2) . . ?

C31 Re2 N1 90.2(2) . . ?

C32 Re2 N1 90.7(2) . . ?

C34 Re2 N1 75.6(2) . . ?

C9 O1 C4' 140.3(9) . . ?

C9 O1 C4 123.0(6) . . ?

C4' O1 C4 94.7(9) . . ?

C22 O7 C23 115.1(4) . . ?

C38 O12 C40 119.5(4) . . ?

C33 N1 C26 119.2(5) . . ?

C33 N1 Re2 114.9(4) . . ?

C26 N1 Re2 125.8(3) . . ?

C15 N2 C16 119.8(5) . . ?

C15 N2 Re1 114.8(4) . . ?

C16 N2 Re1 125.4(4) . . ?

C41 C42 C43 111.5(5) . . ?

C42 C41 C40 113.6(5) . . ?

O12 C40 C41 109.1(4) . . ?

C3 C2 C1 111.3(6) . . ?

C2 C3 C4 114.3(6) . . ?

O1 C4 C3 109.4(7) . . ?

C3' C2' C1' 111.3(7) . . ?

C2' C3' C4' 113.6(7) . . ?

O1 C4' C3' 111.0(11) . . ?

C10 C5 C6 116.4(6) . . ?

C10 C5 Re1 129.3(5) . . ?

C6 C5 Re1 114.0(4) . . ?

C7 C6 C5 122.0(6) . . ?

C7 C6 C15 122.6(6) . . ?

C5 C6 C15 115.4(6) . . ?

C8 C7 C6 119.4(6) . . ?

C7 C8 C9 119.6(6) . . ?

O1 C9 C10 123.8(7) . . ?

O1 C9 C8 115.5(6) . . ?

C10 C9 C8 120.7(6) . . ?

C9 C10 C5 122.0(6) . . ?

O2 C11 Re1 176.6(5) . . ?

O3 C12 Re1 178.5(5) . . ?

O4 C13 Re1 175.0(6) . . ?

O5 C14 Re1 177.8(7) . . ?

N2 C15 C6 119.8(6) . . ?

C21 C16 C17 120.0(5) . . ?

C21 C16 N2 121.1(5) . . ?

C17 C16 N2 118.9(5) . . ?

C18 C17 C16 119.9(5) . . ?

C17 C18 C19 120.6(5) . . ?

C20 C19 C18 119.5(5) . . ?

C20 C19 C22 122.9(5) . . ?

C18 C19 C22 117.6(5) . . ?

C21 C20 C19 119.6(5) . . ?

C16 C21 C20 120.3(5) . . ?

O6 C22 O7 121.7(5) . . ?

O6 C22 C19 124.0(5) . . ?

O7 C22 C19 114.3(4) . . ?

C24 C23 C28 121.0(6) . . ?

C24 C23 O7 120.0(5) . . ?

C28 C23 O7 118.9(6) . . ?

C23 C24 C25 120.0(6) . . ?

C24 C25 C26 120.0(6) . . ?

C27 C26 C25 119.0(6) . . ?

C27 C26 N1 121.7(5) . . ?

C25 C26 N1 119.3(5) . . ?

C26 C27 C28 120.9(6) . . ?

C27 C28 C23 119.0(6) . . ?

O8 C29 Re2 177.4(5) . . ?

O9 C30 Re2 176.7(6) . . ?

O10 C31 Re2 176.8(6) . . ?

O11 C32 Re2 175.2(7) . . ?

N1 C33 C35 119.0(5) . . ?

C36 C35 C34 121.8(5) . . ?

C36 C35 C33 122.3(5) . . ?

C34 C35 C33 115.9(5) . . ?

C39 C34 C35 116.9(5) . . ?

C39 C34 Re2 128.5(4) . . ?

C35 C34 Re2 114.5(4) . . ?

C37 C36 C35 120.5(5) . . ?

C36 C37 C38 118.7(5) . . ?

O12 C38 C37 124.5(5) . . ?

O12 C38 C39 115.3(5) . . ?

C37 C38 C39 120.2(5) . . ?

C34 C39 C38 121.9(5) . . ?





data_s92-3



_audit_creation_date            1999-05-14T10:49:02-00:00

_audit_creation_method         'WinGX routine CIF_UPDATE'



#----------------------------------------------------------------------------#

#                   CHEMICAL INFORMATION                                     #

#----------------------------------------------------------------------------#



_chemical_name_systematic

;

 ?

;

_chemical_formula_sum                   'C35 H36 N2 O4'

_chemical_formula_weight                548.66



#----------------------------------------------------------------------------#

#                   UNIT CELL INFORMATION                                    #

#----------------------------------------------------------------------------#



loop_

    _symmetry_equiv_pos_as_xyz

'x, y, z'

'-x, -y, -z'



_cell_length_a                          7.2025(6)

_cell_length_b                          10.1729(13)

_cell_length_c                          20.231(3)

_cell_angle_alpha                       83.619(5)

_cell_angle_beta                        87.892(8)

_cell_angle_gamma                       83.518(8)

_cell_volume                            1463.3(3)

_cell_formula_units_Z                   2

_cell_measurement_temperature           293(2)

_cell_measurement_reflns_used           na

_cell_measurement_theta_min             na

_cell_measurement_theta_max             na



#----------------------------------------------------------------------------#

#                   CRYSTAL INFORMATION                                      #

#----------------------------------------------------------------------------#



_exptl_crystal_density_meas             'not measured'

_exptl_crystal_density_diffrn           1.245

_exptl_crystal_density_method           'not measured'

_exptl_crystal_F_000                    584

_exptl_special_details

;

 ?

;



#----------------------------------------------------------------------------#

#                   ABSORPTION CORRECTION                                    #

#----------------------------------------------------------------------------#



_exptl_absorpt_coefficient_mu           0.081

_exptl_absorpt_correction_type          'Empirical, SORTAV'

_exptl_absorpt_correction_T_min         0.9393

_exptl_absorpt_correction_T_max         0.9843



#----------------------------------------------------------------------------#

#                   DATA COLLECTION                                          #

#----------------------------------------------------------------------------#



_diffrn_ambient_temperature             293(2)

_diffrn_radiation_wavelength            0.71073

_diffrn_radiation_type                  MoK\a

_diffrn_radiation_monochromator         graphite

_diffrn_measurement_device_type         'Enraf Nonius KappaCCD area detector'

_diffrn_measurement_method

               'Phi and Omega scans to fill Ewald sphere'

_diffrn_standards_number                'not measured'

_diffrn_standards_interval_count        na

_diffrn_standards_interval_time         na

_diffrn_standards_decay_%               na

_diffrn_reflns_number                   20691

_diffrn_reflns_av_R_equivalents         0.1048

_diffrn_reflns_av_sigmaI/netI           0.1168

_diffrn_reflns_limit_h_min              -8

_diffrn_reflns_limit_h_max              8

_diffrn_reflns_limit_k_min              -12

_diffrn_reflns_limit_k_max              12

_diffrn_reflns_limit_l_min              -25

_diffrn_reflns_limit_l_max              25

_diffrn_reflns_theta_min                3

_diffrn_reflns_theta_max                26.37

_diffrn_reflns_theta_full               26.37

_diffrn_measured_fraction_theta_full

                                        0.933

_diffrn_measured_fraction_theta_max

                                        0.933

_reflns_number_total                    5576

_reflns_number_gt                       2712

_reflns_threshold_expression            >2sigma(I)



#----------------------------------------------------------------------------#

#                   COMPUTER PROGRAMS USED                                   #

#----------------------------------------------------------------------------#



_computing_data_collection

;

        DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998)

;

_computing_cell_refinement              'DENZO and COLLECT'

_computing_data_reduction               'DENZO and COLLECT'

_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics           ORTEP

_computing_publication_material         CIFTAB



#----------------------------------------------------------------------------#

#                   REFINEMENT INFORMATION                                   #

#----------------------------------------------------------------------------#



_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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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           mixed

_refine_ls_extinction_method            none

_refine_ls_extinction_coef              yes

_refine_ls_number_reflns                5576

_refine_ls_number_parameters            372

_refine_ls_number_restraints            0

_refine_ls_R_factor_all                 0.1704

_refine_ls_R_factor_gt                  0.0782

_refine_ls_wR_factor_ref                0.2201

_refine_ls_wR_factor_gt                 0.1828

_refine_ls_goodness_of_fit_ref          1.077

_refine_ls_restrained_S_all             1.077

_refine_ls_shift/su_max                 0.013

_refine_ls_shift/su_mean                0.002

_refine_diff_density_max                1.086

_refine_diff_density_min                -0.36

_refine_diff_density_rms                0.068



#----------------------------------------------------------------------------#

#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #

#----------------------------------------------------------------------------#



loop_

    _atom_type_symbol

    _atom_type_description

    _atom_type_scat_dispersion_real

    _atom_type_scat_dispersion_imag

    _atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



loop_

    _atom_site_label

    _atom_site_type_symbol

    _atom_site_fract_x

    _atom_site_fract_y

    _atom_site_fract_z

    _atom_site_U_iso_or_equiv

    _atom_site_adp_type

    _atom_site_occupancy

    _atom_site_calc_flag

    _atom_site_refinement_flags

    _atom_site_disorder_assembly

    _atom_site_disorder_group

O1 O 0.5955(3) 0.1767(2) 0.34786(11) 0.0391(7) Uani 1 d . . .

O2 O 2.0640(3) -0.2925(3) 0.04303(13) 0.0528(8) Uani 1 d . . .

N1 N 1.3595(3) -0.0573(3) 0.21014(14) 0.0336(7) Uani 1 d . . .

O4 O 3.2926(3) -0.6162(2) -0.33970(12) 0.0400(7) Uani 1 d . . .

N2 N 2.6624(4) -0.4010(3) -0.13517(14) 0.0366(8) Uani 1 d . . .

C19 C 2.2126(4) -0.3242(4) -0.00290(18) 0.0375(9) Uani 1 d . . .

C12 C 1.5044(4) -0.0899(3) 0.16273(17) 0.0307(8) Uani 1 d . . .

C8 C 1.0440(4) 0.0387(3) 0.22981(17) 0.0314(8) Uani 1 d . . .

C29 C 3.1335(4) -0.5911(3) -0.30158(17) 0.0325(9) Uani 1 d . . .

C22 C 2.5067(4) -0.3812(3) -0.09077(17) 0.0330(9) Uani 1 d . . .

C10 C 0.9005(4) 0.0741(4) 0.33638(18) 0.0384(9) Uani 1 d . . .

H10 H 0.908 0.066 0.3825 0.046 Uiso 1 calc R . .

C25 C 2.6766(4) -0.4985(4) -0.16921(18) 0.0368(9) Uani 1 d . . .

H25 H 2.5843 -0.5559 -0.1637 0.044 Uiso 1 calc R . .

C7 C 0.8784(4) 0.0969(3) 0.19964(18) 0.0352(9) Uani 1 d . . .

H7 H 0.8711 0.1049 0.1535 0.042 Uiso 1 calc R . .

C6 C 0.7243(4) 0.1431(3) 0.23764(17) 0.0346(9) Uani 1 d . . .

H6 H 0.6144 0.1806 0.2171 0.041 Uiso 1 calc R . .

C26 C 2.8307(4) -0.5264(3) -0.21699(16) 0.0313(9) Uani 1 d . . .

C30 C 3.1202(4) -0.4739(4) -0.27164(18) 0.0377(9) Uani 1 d . . .

H30 H 3.2124 -0.4168 -0.2801 0.045 Uiso 1 calc R . .

C27 C 2.8445(4) -0.6406(4) -0.24926(17) 0.0352(9) Uani 1 d . . .

H27 H 2.7505 -0.6965 -0.2422 0.042 Uiso 1 calc R . .

C17 C 1.6266(4) -0.2039(3) 0.17731(17) 0.0339(9) Uani 1 d . . .

H17 H 1.6122 -0.2575 0.2171 0.041 Uiso 1 calc R . .

C15 C 1.7940(4) -0.1584(4) 0.07391(17) 0.0337(9) Uani 1 d . . .

C14 C 1.6750(4) -0.0434(4) 0.05990(18) 0.0361(9) Uani 1 d . . .

H14 H 1.6913 0.0108 0.0205 0.043 Uiso 1 calc R . .

C11 C 1.2016(4) -0.0052(3) 0.18720(18) 0.0345(9) Uani 1 d . . .

H11 H 1.1866 0.0052 0.1414 0.041 Uiso 1 calc R . .

C5 C 0.7360(4) 0.1328(3) 0.30599(18) 0.0328(9) Uani 1 d . . .

C4 C 0.4236(4) 0.2368(4) 0.31850(18) 0.0408(10) Uani 1 d . . .

H4A H 0.3698 0.1737 0.2943 0.049 Uiso 1 calc R . .

H4B H 0.4462 0.3137 0.2876 0.049 Uiso 1 calc R . .

C13 C 1.5311(4) -0.0080(4) 0.10412(17) 0.0358(9) Uani 1 d . . .

H13 H 1.4525 0.0703 0.0946 0.043 Uiso 1 calc R . .

C16 C 1.7698(4) -0.2384(4) 0.13312(18) 0.0365(9) Uani 1 d . . .

H16 H 1.8503 -0.3156 0.143 0.044 Uiso 1 calc R . .

C28 C 2.9926(4) -0.6739(4) -0.29131(17) 0.0365(9) Uani 1 d . . .

H28 H 2.9981 -0.7508 -0.3125 0.044 Uiso 1 calc R . .

C24 C 2.3915(5) -0.3010(3) 0.01209(17) 0.0367(9) Uani 1 d . . .

H24 H 2.4135 -0.2663 0.0514 0.044 Uiso 1 calc R . .

C31 C 2.9717(4) -0.4417(3) -0.22947(17) 0.0354(9) Uani 1 d . . .

H31 H 2.9648 -0.3635 -0.2092 0.042 Uiso 1 calc R . .

C21 C 2.3254(4) -0.4058(4) -0.10401(18) 0.0394(10) Uani 1 d . . .

H21 H 2.3031 -0.4422 -0.1428 0.047 Uiso 1 calc R . .

C18 C 1.9394(4) -0.1928(4) 0.02452(18) 0.0382(10) Uani 1 d . . .

C9 C 1.0513(4) 0.0283(3) 0.29850(17) 0.0357(9) Uani 1 d . . .

H9 H 1.1602 -0.0103 0.3194 0.043 Uiso 1 calc R . .

C23 C 2.5356(5) -0.3302(3) -0.03214(18) 0.0380(9) Uani 1 d . . .

H23 H 2.656 -0.3151 -0.0222 0.046 Uiso 1 calc R . .

C20 C 2.1794(5) -0.3767(4) -0.06010(19) 0.0427(10) Uani 1 d . . .

H20 H 2.059 -0.3928 -0.0694 0.051 Uiso 1 calc R . .

C3 C 0.2919(5) 0.2784(4) 0.37397(18) 0.0440(10) Uani 1 d . . .

H3A H 0.1692 0.3068 0.3558 0.053 Uiso 1 calc R . .

H3B H 0.2805 0.2018 0.4063 0.053 Uiso 1 calc R . .

C33 C 3.5121(4) -0.7467(4) -0.40212(18) 0.0413(10) Uani 1 d . . .

H33A H 3.607 -0.7421 -0.3699 0.05 Uiso 1 calc R . .

H33B H 3.514 -0.6695 -0.4348 0.05 Uiso 1 calc R . .

C32 C 3.3238(4) -0.7414(4) -0.36711(18) 0.0397(10) Uani 1 d . . .

H32A H 3.227 -0.7482 -0.3983 0.048 Uiso 1 calc R . .

H32B H 3.3219 -0.8144 -0.332 0.048 Uiso 1 calc R . .

C34 C 3.5607(5) -0.8711(4) -0.43666(19) 0.0478(11) Uani 1 d . . .

H34A H 3.4663 -0.8756 -0.4691 0.057 Uiso 1 calc R . .

H34B H 3.5585 -0.9485 -0.4041 0.057 Uiso 1 calc R . .

C2 C 0.3518(5) 0.3882(4) 0.4087(2) 0.0512(11) Uani 1 d . . .

H2A H 0.3783 0.4612 0.3759 0.061 Uiso 1 calc R . .

H2B H 0.4661 0.3563 0.4321 0.061 Uiso 1 calc R . .

C35 C 3.7518(5) -0.8759(4) -0.4717(2) 0.0581(12) Uani 1 d . . .

H35A H 3.7512 -0.8044 -0.5069 0.087 Uiso 1 calc R . .

H35B H 3.7793 -0.9594 -0.4899 0.087 Uiso 1 calc R . .

H35C H 3.8453 -0.867 -0.4403 0.087 Uiso 1 calc R . .

C1 C 0.2032(5) 0.4391(4) 0.4582(2) 0.0629(13) Uani 1 d . . .

H1A H 0.0898 0.471 0.4353 0.094 Uiso 1 calc R . .

H1B H 0.2465 0.5103 0.4787 0.094 Uiso 1 calc R . .

H1C H 0.1799 0.368 0.4918 0.094 Uiso 1 calc R . .

O3 O 1.9558(3) -0.1242(3) -0.03092(15) 0.0595(8) Uani 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 0.0299(13) 0.0476(17) 0.0368(15) -0.0046(12) 0.0031(10) 0.0073(11)

O2 0.0455(16) 0.063(2) 0.0412(17) 0.0048(14) 0.0104(12) 0.0179(13)

N1 0.0283(16) 0.0357(19) 0.0360(19) -0.0056(15) 0.0037(13) 0.0005(13)

O4 0.0362(14) 0.0390(16) 0.0449(16) -0.0116(13) 0.0110(11) -0.0006(11)

N2 0.0301(16) 0.040(2) 0.0380(19) -0.0063(16) 0.0016(13) 0.0038(13)

C19 0.028(2) 0.042(3) 0.036(2) 0.0027(19) 0.0084(16) 0.0101(16)

C12 0.0267(18) 0.032(2) 0.033(2) -0.0058(17) 0.0005(15) -0.0003(15)

C8 0.0277(18) 0.031(2) 0.035(2) -0.0065(17) 0.0014(15) -0.0017(14)

C29 0.029(2) 0.032(2) 0.034(2) -0.0025(18) 0.0025(15) 0.0024(15)

C22 0.0271(19) 0.037(2) 0.032(2) -0.0024(18) 0.0030(15) 0.0051(15)

C10 0.036(2) 0.045(2) 0.033(2) -0.0036(18) 0.0017(16) 0.0012(16)

C25 0.0254(19) 0.040(2) 0.042(2) 0.000(2) 0.0005(15) 0.0016(16)

C7 0.032(2) 0.040(2) 0.034(2) -0.0057(18) -0.0006(15) -0.0031(16)

C6 0.0257(19) 0.038(2) 0.040(2) -0.0078(19) 0.0020(15) -0.0014(15)

C26 0.0254(18) 0.035(2) 0.031(2) 0.0000(17) -0.0006(14) 0.0062(15)

C30 0.032(2) 0.036(2) 0.045(2) -0.0013(19) -0.0007(16) -0.0036(16)

C27 0.0290(19) 0.038(2) 0.038(2) -0.0051(19) 0.0036(15) -0.0017(15)

C17 0.0292(19) 0.039(2) 0.033(2) -0.0032(17) -0.0018(15) 0.0000(16)

C15 0.0221(18) 0.047(3) 0.033(2) -0.0097(19) -0.0009(14) -0.0029(16)

C14 0.0279(19) 0.045(3) 0.034(2) -0.0008(18) -0.0007(15) -0.0036(16)

C11 0.035(2) 0.036(2) 0.033(2) -0.0045(18) 0.0038(16) -0.0032(16)

C5 0.0292(19) 0.031(2) 0.038(2) -0.0071(18) 0.0051(15) -0.0016(15)

C4 0.0253(19) 0.053(3) 0.042(2) -0.007(2) 0.0014(15) 0.0067(16)

C13 0.0275(19) 0.041(2) 0.038(2) -0.0046(19) -0.0014(15) 0.0001(16)

C16 0.030(2) 0.039(2) 0.039(2) -0.0075(19) -0.0030(16) 0.0038(16)

C28 0.036(2) 0.033(2) 0.041(2) -0.0100(18) 0.0010(16) -0.0024(16)

C24 0.045(2) 0.035(2) 0.029(2) -0.0068(17) 0.0048(16) 0.0031(16)

C31 0.032(2) 0.032(2) 0.041(2) -0.0080(18) 0.0011(16) 0.0031(16)

C21 0.031(2) 0.051(3) 0.036(2) -0.0098(19) -0.0013(16) 0.0042(17)

C18 0.0249(19) 0.062(3) 0.027(2) -0.009(2) -0.0028(15) 0.0041(18)

C9 0.0279(19) 0.038(2) 0.039(2) -0.0017(18) -0.0010(15) 0.0022(15)

C23 0.036(2) 0.036(2) 0.042(2) -0.0012(19) -0.0006(17) -0.0057(16)

C20 0.028(2) 0.054(3) 0.044(3) -0.007(2) -0.0007(16) 0.0071(17)

C3 0.032(2) 0.055(3) 0.041(2) -0.001(2) 0.0023(16) 0.0071(17)

C33 0.040(2) 0.044(3) 0.040(2) -0.0092(19) 0.0046(16) 0.0019(17)

C32 0.034(2) 0.042(2) 0.043(2) -0.011(2) 0.0043(16) -0.0002(16)

C34 0.045(2) 0.052(3) 0.044(3) -0.011(2) 0.0080(18) 0.0036(19)

C2 0.047(2) 0.051(3) 0.052(3) -0.009(2) 0.0122(19) 0.006(2)

C35 0.055(3) 0.066(3) 0.049(3) -0.009(2) 0.0105(19) 0.011(2)

C1 0.060(3) 0.068(3) 0.055(3) -0.013(2) 0.016(2) 0.015(2)

O3 0.0493(17) 0.069(2) 0.056(2) -0.0033(17) 0.0067(13) 0.0056(14)





#----------------------------------------------------------------------------#

#                   MOLECULAR GEOMETRY                                       #

#----------------------------------------------------------------------------#



_geom_special_details

;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

    _geom_bond_atom_site_label_1

    _geom_bond_atom_site_label_2

    _geom_bond_distance

    _geom_bond_site_symmetry_2

    _geom_bond_publ_flag

O1 C5 1.364(4) . ?

O1 C4 1.436(4) . ?

O2 C18 1.308(4) . ?

O2 C19 1.424(4) . ?

N1 C11 1.280(4) . ?

N1 C12 1.427(4) . ?

O4 C29 1.374(3) . ?

O4 C32 1.437(4) . ?

N2 C25 1.262(4) . ?

N2 C22 1.422(4) . ?

C19 C20 1.367(5) . ?

C19 C24 1.386(5) . ?

C12 C17 1.386(4) . ?

C12 C13 1.391(5) . ?

C8 C9 1.384(5) . ?

C8 C7 1.400(4) . ?

C8 C11 1.460(4) . ?

C29 C30 1.388(5) . ?

C29 C28 1.386(5) . ?

C22 C23 1.378(5) . ?

C22 C21 1.397(5) . ?

C10 C9 1.374(4) . ?

C10 C5 1.397(5) . ?

C25 C26 1.469(4) . ?

C7 C6 1.394(4) . ?

C6 C5 1.380(5) . ?

C26 C27 1.387(5) . ?

C26 C31 1.403(5) . ?

C30 C31 1.377(4) . ?

C27 C28 1.375(4) . ?

C17 C16 1.380(4) . ?

C15 C14 1.379(5) . ?

C15 C16 1.388(5) . ?

C15 C18 1.461(4) . ?

C14 C13 1.387(4) . ?

C4 C3 1.508(4) . ?

C24 C23 1.374(4) . ?

C21 C20 1.379(4) . ?

C18 O3 1.263(4) . ?

C3 C2 1.494(5) . ?

C33 C32 1.505(4) . ?

C33 C34 1.513(5) . ?

C34 C35 1.523(4) . ?

C2 C1 1.525(4) . ?



loop_

    _geom_angle_atom_site_label_1

    _geom_angle_atom_site_label_2

    _geom_angle_atom_site_label_3

    _geom_angle

    _geom_angle_site_symmetry_1

    _geom_angle_site_symmetry_3

    _geom_angle_publ_flag

C5 O1 C4 117.4(3) . . ?

C18 O2 C19 117.5(3) . . ?

C11 N1 C12 117.0(3) . . ?

C29 O4 C32 118.3(3) . . ?

C25 N2 C22 119.6(3) . . ?

C20 C19 C24 121.0(3) . . ?

C20 C19 O2 120.7(3) . . ?

C24 C19 O2 118.3(3) . . ?

C17 C12 C13 119.3(3) . . ?

C17 C12 N1 118.5(3) . . ?

C13 C12 N1 122.1(3) . . ?

C9 C8 C7 118.3(3) . . ?

C9 C8 C11 123.3(3) . . ?

C7 C8 C11 118.3(3) . . ?

O4 C29 C30 115.3(3) . . ?

O4 C29 C28 124.7(3) . . ?

C30 C29 C28 120.0(3) . . ?

C23 C22 C21 118.2(3) . . ?

C23 C22 N2 117.7(3) . . ?

C21 C22 N2 124.1(3) . . ?

C9 C10 C5 120.3(3) . . ?

N2 C25 C26 123.8(3) . . ?

C6 C7 C8 121.0(3) . . ?

C5 C6 C7 119.5(3) . . ?

C27 C26 C31 118.0(3) . . ?

C27 C26 C25 120.6(3) . . ?

C31 C26 C25 121.3(3) . . ?

C31 C30 C29 120.5(3) . . ?

C28 C27 C26 122.2(3) . . ?

C16 C17 C12 120.4(3) . . ?

C14 C15 C16 119.4(3) . . ?

C14 C15 C18 118.1(3) . . ?

C16 C15 C18 122.4(3) . . ?

C15 C14 C13 120.6(3) . . ?

N1 C11 C8 122.9(3) . . ?

O1 C5 C6 124.5(3) . . ?

O1 C5 C10 115.8(3) . . ?

C6 C5 C10 119.7(3) . . ?

O1 C4 C3 107.7(3) . . ?

C14 C13 C12 119.9(3) . . ?

C17 C16 C15 120.3(3) . . ?

C27 C28 C29 119.0(3) . . ?

C23 C24 C19 118.8(3) . . ?

C30 C31 C26 120.2(3) . . ?

C20 C21 C22 120.6(3) . . ?

O3 C18 O2 120.8(3) . . ?

O3 C18 C15 122.7(3) . . ?

O2 C18 C15 116.3(3) . . ?

C10 C9 C8 121.1(3) . . ?

C24 C23 C22 121.8(3) . . ?

C19 C20 C21 119.7(3) . . ?

C2 C3 C4 114.1(3) . . ?

C32 C33 C34 113.3(3) . . ?

O4 C32 C33 107.2(3) . . ?

C33 C34 C35 112.9(3) . . ?

C3 C2 C1 112.3(3) . . ?