# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?

_publ_section_title              
;Capturing a [c2]Daisy Chain Using the
Threading-Followed-by-Swelling Approach
;
_publ_contact_author_name        'Prof. Sheng-Hsien Chiu'
_publ_contact_author_email       SHCHIU@NTU.EDU.TW
loop_
_publ_author_name
'Sheng-Hsien Chiu'
'Sheng-Yao Hsesh'
'Chien-Chen Lai'
'Yi-Hung Liu'
;
Shie-Ming Peng
;
'Shau-Hua Ueng'

data_ic12639
_database_code_depnum_ccdc_archive 'CCDC 664527'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H53 Cl12 F6 N2 O4 P'
_chemical_formula_weight         1316.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.8645(4)
_cell_length_b                   13.4307(3)
_cell_length_c                   18.2973(5)
_cell_angle_alpha                94.368(2)
_cell_angle_beta                 102.7600(10)
_cell_angle_gamma                100.435(2)
_cell_volume                     3010.00(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    27649
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21038
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.1181
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         27.48
_reflns_number_total             13743
_reflns_number_gt                5262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius BV)'
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Because of the large correlation between thermal parameters, the restraint
was necessary for convergence of the refinement process. In large
supermolecular structure with poor data to parameter ratios, they
often are needed with geometrical and anisotropic displacement parameters
restraints.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+3.4846P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13743
_refine_ls_number_parameters     704
_refine_ls_number_restraints     246
_refine_ls_R_factor_all          0.2352
_refine_ls_R_factor_gt           0.1094
_refine_ls_wR_factor_ref         0.3256
_refine_ls_wR_factor_gt          0.2561
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.005

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7752(3) 0.6618(3) 0.5601(2) 0.0650(11) Uani 1 1 d . . .
O2 O 1.0441(3) 0.8687(3) 0.7647(2) 0.0622(10) Uani 1 1 d . . .
O3 O 0.7755(4) 0.9058(4) 1.0083(3) 0.0875(14) Uani 1 1 d . . .
O4 O 0.3980(3) 0.5587(4) 0.7253(3) 0.0845(14) Uani 1 1 d . . .
N1 N 0.9830(3) 0.7803(3) 0.6149(3) 0.0562(11) Uani 1 1 d . . .
N2 N 1.1824(3) 1.2230(3) 0.2918(2) 0.0482(10) Uani 1 1 d . . .
H2A H 1.1923 1.2591 0.3371 0.058 Uiso 1 1 calc R . .
H2B H 1.1110 1.1956 0.2751 0.058 Uiso 1 1 calc R . .
C1 C 0.8491(6) 0.6696(5) 0.5126(4) 0.085(2) Uani 1 1 d . . .
H1B H 0.8108 0.6775 0.4621 0.102 Uiso 1 1 calc R . .
H1C H 0.8763 0.6070 0.5097 0.102 Uiso 1 1 calc R . .
C2 C 0.9437(4) 0.7583(4) 0.5406(3) 0.0572(14) Uani 1 1 d . . .
C3 C 0.9867(4) 0.8105(4) 0.4878(3) 0.0586(15) Uani 1 1 d . . .
H3A H 0.9546 0.7926 0.4366 0.070 Uiso 1 1 calc R . .
C4 C 1.0770(4) 0.8889(4) 0.5111(3) 0.0482(12) Uani 1 1 d . . .
C5 C 1.1187(4) 0.9109(4) 0.5881(3) 0.0583(14) Uani 1 1 d . . .
H5A H 1.1794 0.9630 0.6070 0.070 Uiso 1 1 calc R . .
C6 C 1.0713(4) 0.8566(4) 0.6374(3) 0.0556(14) Uani 1 1 d . . .
C7 C 1.1225(5) 0.8797(5) 0.7201(3) 0.0761(19) Uani 1 1 d . . .
H7A H 1.1722 0.8342 0.7344 0.091 Uiso 1 1 calc R . .
H7B H 1.1646 0.9490 0.7306 0.091 Uiso 1 1 calc R . .
C8 C 1.0967(5) 0.8917(6) 0.8427(3) 0.085(2) Uani 1 1 d . . .
H8A H 1.1454 0.9579 0.8518 0.102 Uiso 1 1 calc R . .
H8B H 1.1395 0.8410 0.8581 0.102 Uiso 1 1 calc R . .
C9 C 1.0122(5) 0.8920(5) 0.8874(3) 0.0667(17) Uani 1 1 d . . .
C10 C 0.9866(5) 0.8136(5) 0.9297(4) 0.0727(18) Uani 1 1 d . . .
H10A H 1.0232 0.7598 0.9315 0.087 Uiso 1 1 calc R . .
C11 C 0.9058(6) 0.8156(5) 0.9695(3) 0.0729(18) Uani 1 1 d . . .
H11A H 0.8886 0.7628 0.9976 0.087 Uiso 1 1 calc R . .
C12 C 0.8518(5) 0.8945(5) 0.9675(3) 0.0670(17) Uani 1 1 d . . .
C13 C 0.8776(6) 0.9725(5) 0.9262(4) 0.0723(17) Uani 1 1 d . . .
H13A H 0.8420 1.0269 0.9251 0.087 Uiso 1 1 calc R . .
C14 C 0.9559(6) 0.9699(5) 0.8868(3) 0.0760(19) Uani 1 1 d . . .
H14A H 0.9717 1.0228 0.8584 0.091 Uiso 1 1 calc R . .
C15 C 0.7246(6) 0.8158(6) 1.0345(4) 0.093(2) Uani 1 1 d . . .
H15A H 0.6813 0.8349 1.0684 0.112 Uiso 1 1 calc R . .
H15B H 0.7805 0.7843 1.0627 0.112 Uiso 1 1 calc R . .
C16 C 0.6524(5) 0.7392(5) 0.9705(4) 0.0720(17) Uani 1 1 d . . .
C17 C 0.6022(5) 0.7685(5) 0.9043(4) 0.0731(17) Uani 1 1 d . . .
H17A H 0.6165 0.8371 0.8973 0.088 Uiso 1 1 calc R . .
C18 C 0.5310(5) 0.7000(5) 0.8473(4) 0.0719(17) Uani 1 1 d . . .
H18A H 0.4980 0.7229 0.8029 0.086 Uiso 1 1 calc R . .
C19 C 0.5083(5) 0.5969(5) 0.8558(4) 0.0734(18) Uani 1 1 d . . .
C20 C 0.5610(6) 0.5677(6) 0.9220(5) 0.089(2) Uani 1 1 d . . .
H20A H 0.5486 0.4990 0.9288 0.107 Uiso 1 1 calc R . .
C21 C 0.6315(6) 0.6368(6) 0.9784(4) 0.090(2) Uani 1 1 d . . .
H21A H 0.6657 0.6142 1.0225 0.108 Uiso 1 1 calc R . .
C22 C 0.4244(6) 0.5211(6) 0.7965(4) 0.091(2) Uani 1 1 d . . .
H22A H 0.4519 0.4592 0.7898 0.109 Uiso 1 1 calc R . .
H22B H 0.3586 0.5036 0.8143 0.109 Uiso 1 1 calc R . .
C23 C 0.4703(5) 0.5589(5) 0.6801(4) 0.0678(17) Uani 1 1 d . . .
C24 C 0.5378(6) 0.4915(5) 0.6787(4) 0.0762(19) Uani 1 1 d . . .
H24A H 0.5378 0.4410 0.7107 0.091 Uiso 1 1 calc R . .
C25 C 0.6066(5) 0.4980(5) 0.6294(4) 0.0744(18) Uani 1 1 d . . .
H25A H 0.6524 0.4518 0.6292 0.089 Uiso 1 1 calc R . .
C26 C 0.6081(5) 0.5720(5) 0.5806(3) 0.0683(17) Uani 1 1 d . . .
C27 C 0.5379(6) 0.6373(5) 0.5817(4) 0.080(2) Uani 1 1 d . . .
H27A H 0.5351 0.6857 0.5479 0.096 Uiso 1 1 calc R . .
C28 C 0.4706(5) 0.6334(5) 0.6320(4) 0.0788(19) Uani 1 1 d . . .
H28A H 0.4262 0.6807 0.6332 0.095 Uiso 1 1 calc R . .
C29 C 0.6835(5) 0.5796(5) 0.5288(4) 0.088(2) Uani 1 1 d . . .
H29A H 0.7082 0.5161 0.5231 0.105 Uiso 1 1 calc R . .
H29B H 0.6458 0.5924 0.4795 0.105 Uiso 1 1 calc R . .
C30 C 1.1241(4) 0.9493(4) 0.4571(3) 0.0484(12) Uani 1 1 d . . .
C31 C 1.2103(5) 1.0310(4) 0.4812(3) 0.0743(19) Uani 1 1 d . . .
H31A H 1.2415 1.0473 0.5327 0.089 Uiso 1 1 calc R . .
C32 C 1.2518(5) 1.0897(5) 0.4312(3) 0.0739(18) Uani 1 1 d . . .
H32A H 1.3104 1.1440 0.4497 0.089 Uiso 1 1 calc R . .
C33 C 1.2082(4) 1.0691(4) 0.3555(3) 0.0528(13) Uani 1 1 d . . .
C34 C 1.1242(5) 0.9859(5) 0.3301(3) 0.0733(18) Uani 1 1 d . . .
H34A H 1.0942 0.9690 0.2785 0.088 Uiso 1 1 calc R . .
C35 C 1.0841(5) 0.9274(5) 0.3804(3) 0.0710(18) Uani 1 1 d . . .
H35A H 1.0280 0.8710 0.3617 0.085 Uiso 1 1 calc R . .
C36 C 1.2446(5) 1.1396(4) 0.3006(3) 0.0579(14) Uani 1 1 d U . .
H36A H 1.3216 1.1689 0.3188 0.069 Uiso 1 1 calc R . .
H36B H 1.2339 1.1004 0.2518 0.069 Uiso 1 1 calc R . .
C37 C 1.2167(4) 1.2930(4) 0.2380(3) 0.0569(13) Uani 1 1 d U . .
H37A H 1.2081 1.2542 0.1894 0.068 Uiso 1 1 calc R . .
H37B H 1.2929 1.3250 0.2568 0.068 Uiso 1 1 calc R . .
C38 C 1.1490(5) 1.3741(4) 0.2288(4) 0.0689(15) Uani 1 1 d U . .
H38A H 1.1564 1.4119 0.2777 0.083 Uiso 1 1 calc R . .
H38B H 1.0729 1.3421 0.2092 0.083 Uiso 1 1 calc R . .
C39 C 1.1855(6) 1.4477(5) 0.1748(4) 0.0872(17) Uani 1 1 d U . .
H39A H 1.2627 1.4759 0.1932 0.105 Uiso 1 1 calc R . .
H39B H 1.1747 1.4098 0.1255 0.105 Uiso 1 1 calc R . .
C40 C 1.1246(7) 1.5348(6) 0.1663(5) 0.1066(19) Uani 1 1 d U . .
H40A H 1.1197 1.5612 0.2167 0.128 Uiso 1 1 calc R . .
C41 C 1.1813(8) 1.6195(7) 0.1334(6) 0.131(2) Uani 1 1 d U . .
H41A H 1.2573 1.6344 0.1603 0.157 Uiso 1 1 calc R . .
H41B H 1.1781 1.5950 0.0815 0.157 Uiso 1 1 calc R . .
C42 C 1.1434(10) 1.7152(8) 0.1330(7) 0.150(3) Uani 1 1 d U . .
H42A H 1.1831 1.7684 0.1146 0.180 Uiso 1 1 calc R . .
C43 C 1.0542(11) 1.7346(9) 0.1575(7) 0.156(3) Uani 1 1 d U . .
H43A H 1.0572 1.8011 0.1776 0.187 Uiso 1 1 calc R . .
C44 C 0.9627(10) 1.6651(9) 0.1547(7) 0.153(3) Uani 1 1 d U . .
H44A H 0.9026 1.6970 0.1339 0.183 Uiso 1 1 calc R . .
H44B H 0.9605 1.6586 0.2068 0.183 Uiso 1 1 calc R . .
C45 C 0.9354(10) 1.5639(8) 0.1171(7) 0.150(3) Uani 1 1 d U . .
H45A H 0.8638 1.5380 0.0905 0.180 Uiso 1 1 calc R . .
C46 C 1.0121(8) 1.5013(7) 0.1183(6) 0.125(2) Uani 1 1 d U . .
H46A H 0.9923 1.4383 0.0888 0.150 Uiso 1 1 calc R . .
P1 P 0.72280(16) 0.77414(14) 0.26982(12) 0.0849(6) Uani 1 1 d . . .
F1 F 0.8419(4) 0.8070(7) 0.2788(7) 0.278(6) Uani 1 1 d . . .
F2 F 0.5958(5) 0.7398(5) 0.2566(4) 0.175(3) Uani 1 1 d . . .
F3 F 0.7116(4) 0.7041(4) 0.1942(3) 0.1326(18) Uani 1 1 d . . .
F4 F 0.7045(7) 0.8633(4) 0.2249(4) 0.194(3) Uani 1 1 d . . .
F5 F 0.7334(8) 0.8458(5) 0.3399(4) 0.228(4) Uani 1 1 d . . .
F6 F 0.7296(9) 0.6818(5) 0.3106(4) 0.238(5) Uani 1 1 d . . .
C47 C 0.8621(7) 0.4695(7) 0.3396(5) 0.118(3) Uani 1 1 d . . .
H47A H 0.8072 0.5121 0.3315 0.141 Uiso 1 1 calc R . .
Cl1 Cl 0.8496(3) 0.3951(3) 0.25585(16) 0.1572(11) Uani 1 1 d . . .
Cl2 Cl 0.9895(2) 0.5489(3) 0.3690(2) 0.1661(12) Uani 1 1 d . . .
Cl3 Cl 0.8388(2) 0.3929(2) 0.41063(15) 0.1309(9) Uani 1 1 d . . .
C49 C 0.5246(7) 0.9962(7) 0.2410(6) 0.128(3) Uani 1 1 d . . .
H49A H 0.5497 0.9328 0.2511 0.154 Uiso 1 1 calc R . .
Cl7 Cl 0.3828(2) 0.9679(3) 0.2148(2) 0.1626(12) Uani 1 1 d . . .
Cl8 Cl 0.5752(2) 1.0424(3) 0.1654(2) 0.1767(14) Uani 1 1 d . . .
Cl9 Cl 0.5696(4) 1.0793(4) 0.3211(3) 0.264(3) Uani 1 1 d . . .
C50 C 0.3831(7) 0.7693(10) -0.0059(6) 0.144(4) Uani 1 1 d . . .
H50A H 0.4390 0.7768 -0.0350 0.173 Uiso 1 1 calc R . .
Cl10 Cl 0.2797(3) 0.6704(3) -0.0522(2) 0.1916(16) Uani 1 1 d . . .
Cl11 Cl 0.3354(3) 0.8858(3) -0.00221(16) 0.1555(11) Uani 1 1 d . . .
Cl12 Cl 0.4438(2) 0.7476(2) 0.08417(15) 0.1294(9) Uani 1 1 d . . .
C48 C 0.3467(10) 0.8222(10) 0.4088(8) 0.160(3) Uani 0.553(5) 1 d PU A 1
H48A H 0.3374 0.8931 0.4122 0.192 Uiso 0.553(5) 1 calc PR A 1
Cl4 Cl 0.4770(8) 0.8136(9) 0.4060(6) 0.192(4) Uani 0.553(5) 1 d PU A 1
Cl5 Cl 0.3081(7) 0.7605(7) 0.4805(4) 0.171(3) Uani 0.553(5) 1 d PU A 1
Cl6 Cl 0.2638(7) 0.7490(5) 0.3242(5) 0.211(3) Uani 0.553(5) 1 d PU A 1
C48' C 0.3467(10) 0.8222(10) 0.4088(8) 0.160(3) Uani 0.447(5) 1 d PU A 2
H48B H 0.3133 0.8721 0.3806 0.192 Uiso 0.447(5) 1 calc PR A 2
Cl4' Cl 0.2489(8) 0.7201(6) 0.4167(7) 0.180(3) Uani 0.447(5) 1 d PU A 2
Cl5' Cl 0.4173(9) 0.8770(9) 0.4997(6) 0.224(4) Uani 0.447(5) 1 d PU A 2
Cl6' Cl 0.4414(10) 0.7799(8) 0.3652(7) 0.165(3) Uani 0.447(5) 1 d PU A 2

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 0.067(2) 0.062(2) 0.055(2) -0.0083(18) 0.019(2) -0.0161(19)
O2 0.056(2) 0.079(3) 0.043(2) 0.0025(19) 0.0080(18) -0.0034(19)
O3 0.083(3) 0.097(3) 0.073(3) -0.017(3) 0.024(3) -0.001(3)
O4 0.063(3) 0.099(3) 0.083(3) -0.004(3) 0.026(3) -0.010(2)
N1 0.051(3) 0.062(3) 0.052(3) 0.001(2) 0.016(2) -0.001(2)
N2 0.047(2) 0.046(2) 0.050(3) 0.006(2) 0.012(2) 0.0052(19)
C1 0.098(5) 0.084(4) 0.058(4) -0.012(3) 0.034(4) -0.029(4)
C2 0.059(3) 0.057(3) 0.052(3) -0.001(3) 0.019(3) -0.002(3)
C3 0.063(3) 0.061(3) 0.045(3) -0.004(3) 0.013(3) -0.002(3)
C4 0.052(3) 0.048(3) 0.047(3) 0.005(2) 0.015(3) 0.011(2)
C5 0.053(3) 0.060(3) 0.054(4) 0.006(3) 0.008(3) -0.001(3)
C6 0.050(3) 0.067(3) 0.047(3) 0.005(3) 0.013(3) 0.005(3)
C7 0.055(4) 0.111(5) 0.052(4) 0.013(3) 0.013(3) -0.010(3)
C8 0.063(4) 0.130(6) 0.048(4) 0.004(4) 0.007(3) -0.008(4)
C9 0.059(4) 0.085(4) 0.041(3) -0.006(3) 0.000(3) -0.001(3)
C10 0.079(4) 0.069(4) 0.060(4) -0.001(3) 0.005(4) 0.008(3)
C11 0.079(4) 0.075(4) 0.053(4) 0.004(3) 0.014(3) -0.010(4)
C12 0.061(4) 0.078(4) 0.049(4) -0.016(3) 0.010(3) -0.003(3)
C13 0.077(4) 0.066(4) 0.062(4) -0.005(3) 0.003(4) 0.008(3)
C14 0.079(5) 0.082(5) 0.047(4) 0.006(3) -0.005(3) -0.010(4)
C15 0.082(5) 0.126(6) 0.064(4) 0.003(4) 0.026(4) -0.004(4)
C16 0.065(4) 0.088(5) 0.063(4) 0.009(4) 0.023(3) 0.007(3)
C17 0.080(4) 0.068(4) 0.064(4) 0.005(3) 0.013(4) 0.002(3)
C18 0.075(4) 0.074(4) 0.065(4) 0.013(3) 0.015(3) 0.011(3)
C19 0.076(4) 0.071(4) 0.077(5) 0.010(4) 0.035(4) 0.002(3)
C20 0.101(6) 0.078(5) 0.098(6) 0.030(5) 0.047(5) 0.009(4)
C21 0.092(5) 0.101(6) 0.074(5) 0.022(4) 0.014(4) 0.015(5)
C22 0.087(5) 0.089(5) 0.089(5) -0.003(4) 0.038(4) -0.016(4)
C23 0.055(4) 0.069(4) 0.064(4) -0.008(3) 0.009(3) -0.014(3)
C24 0.076(4) 0.068(4) 0.078(5) 0.007(3) 0.024(4) -0.007(4)
C25 0.069(4) 0.061(4) 0.086(5) -0.006(4) 0.022(4) -0.001(3)
C26 0.058(4) 0.069(4) 0.061(4) -0.008(3) 0.007(3) -0.016(3)
C27 0.070(4) 0.078(5) 0.074(5) 0.017(4) 0.000(4) -0.017(4)
C28 0.056(4) 0.075(4) 0.102(5) 0.009(4) 0.020(4) 0.005(3)
C29 0.083(5) 0.085(4) 0.076(5) -0.022(4) 0.027(4) -0.030(4)
C30 0.045(3) 0.047(3) 0.053(3) 0.007(2) 0.011(3) 0.010(2)
C31 0.090(5) 0.070(4) 0.046(3) 0.007(3) 0.004(3) -0.011(3)
C32 0.073(4) 0.075(4) 0.057(4) 0.015(3) 0.004(3) -0.019(3)
C33 0.056(3) 0.051(3) 0.055(3) 0.009(3) 0.016(3) 0.013(3)
C34 0.086(4) 0.073(4) 0.049(3) 0.011(3) 0.009(3) -0.007(3)
C35 0.073(4) 0.066(4) 0.058(4) 0.007(3) 0.005(3) -0.015(3)
C36 0.059(3) 0.060(3) 0.056(3) 0.013(3) 0.016(3) 0.009(3)
C37 0.055(3) 0.055(3) 0.061(3) 0.015(2) 0.017(3) 0.006(2)
C38 0.068(3) 0.065(3) 0.078(4) 0.022(3) 0.020(3) 0.016(3)
C39 0.087(3) 0.074(3) 0.107(4) 0.040(3) 0.026(3) 0.017(3)
C40 0.110(4) 0.083(3) 0.132(4) 0.048(3) 0.022(4) 0.026(3)
C41 0.135(4) 0.098(4) 0.161(5) 0.049(4) 0.022(4) 0.027(4)
C42 0.153(5) 0.111(4) 0.181(5) 0.051(5) 0.020(5) 0.024(5)
C43 0.165(6) 0.114(5) 0.187(6) 0.030(5) 0.015(5) 0.053(5)
C44 0.151(5) 0.139(5) 0.181(6) 0.042(5) 0.034(5) 0.057(5)
C45 0.140(5) 0.129(5) 0.179(5) 0.051(5) 0.017(5) 0.034(5)
C46 0.121(4) 0.099(4) 0.158(5) 0.045(4) 0.017(4) 0.040(4)
P1 0.0855(14) 0.0673(11) 0.0827(13) -0.0021(10) -0.0065(10) 0.0034(9)
F1 0.064(3) 0.264(9) 0.431(14) -0.130(9) -0.002(6) -0.010(4)
F2 0.120(4) 0.161(5) 0.232(7) -0.041(5) 0.069(5) -0.009(4)
F3 0.151(4) 0.113(3) 0.120(4) -0.021(3) 0.049(3) -0.012(3)
F4 0.283(9) 0.103(4) 0.186(6) 0.039(4) 0.035(6) 0.029(5)
F5 0.347(11) 0.162(6) 0.126(5) -0.085(4) 0.058(6) -0.035(6)
F6 0.388(12) 0.119(5) 0.147(6) 0.039(4) -0.060(7) 0.042(6)
C47 0.111(7) 0.139(7) 0.100(6) -0.006(6) 0.023(5) 0.026(6)
Cl1 0.176(3) 0.199(3) 0.1098(19) -0.0093(19) 0.0515(19) 0.064(2)
Cl2 0.135(2) 0.173(3) 0.180(3) 0.013(2) 0.043(2) 0.003(2)
Cl3 0.1325(19) 0.157(2) 0.1228(19) 0.0285(17) 0.0539(16) 0.0468(17)
C49 0.085(6) 0.101(6) 0.196(11) 0.012(7) 0.018(6) 0.034(5)
Cl7 0.1022(18) 0.188(3) 0.194(3) -0.023(2) 0.0326(19) 0.0428(18)
Cl8 0.128(2) 0.180(3) 0.229(4) 0.101(3) 0.027(2) 0.037(2)
Cl9 0.241(5) 0.225(4) 0.257(5) -0.108(4) -0.073(4) 0.088(4)
C50 0.079(6) 0.244(12) 0.113(7) -0.023(8) 0.032(5) 0.049(7)
Cl10 0.148(3) 0.236(4) 0.149(3) -0.069(3) -0.006(2) 0.022(2)
Cl11 0.145(2) 0.194(3) 0.121(2) 0.031(2) 0.0052(18) 0.047(2)
Cl12 0.1097(17) 0.160(2) 0.1153(19) 0.0052(16) 0.0107(14) 0.0423(15)
C48 0.172(5) 0.161(5) 0.176(5) 0.040(5) 0.054(5) 0.082(4)
Cl4 0.143(5) 0.226(8) 0.201(8) 0.070(6) 0.021(5) 0.033(5)
Cl5 0.195(6) 0.213(6) 0.162(5) 0.091(5) 0.087(5) 0.107(5)
Cl6 0.239(6) 0.166(5) 0.187(6) -0.019(4) -0.032(5) 0.059(5)
C48' 0.172(5) 0.161(5) 0.176(5) 0.040(5) 0.054(5) 0.082(4)
Cl4' 0.178(6) 0.147(5) 0.256(8) 0.053(6) 0.107(6) 0.057(5)
Cl5' 0.222(7) 0.245(8) 0.200(7) -0.015(6) -0.004(6) 0.115(6)
Cl6' 0.203(8) 0.136(5) 0.200(8) 0.037(5) 0.119(6) 0.054(5)

_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 C1 1.418(7) . ?
O1 C29 1.439(6) . ?
O2 C8 1.423(7) . ?
O2 C7 1.425(7) . ?
O3 C12 1.380(7) . ?
O3 C15 1.435(8) . ?
O4 C23 1.374(8) . ?
O4 C22 1.426(8) . ?
N1 C2 1.331(7) . ?
N1 C6 1.348(7) . ?
N2 C36 1.489(7) . ?
N2 C37 1.493(6) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C1 C2 1.507(8) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C3 1.388(7) . ?
C3 C4 1.382(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(7) . ?
C4 C30 1.487(7) . ?
C5 C6 1.379(7) . ?
C5 H5A 0.9300 . ?
C6 C7 1.495(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.497(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.376(9) . ?
C9 C10 1.388(9) . ?
C10 C11 1.398(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.368(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.372(9) . ?
C13 C14 1.366(9) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C15 C16 1.511(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.364(9) . ?
C16 C21 1.377(9) . ?
C17 C18 1.378(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.390(9) . ?
C18 H18A 0.9300 . ?
C19 C20 1.374(10) . ?
C19 C22 1.515(9) . ?
C20 C21 1.372(10) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.366(9) . ?
C23 C28 1.382(9) . ?
C24 C25 1.392(9) . ?
C24 H24A 0.9300 . ?
C25 C26 1.386(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.370(9) . ?
C26 C29 1.494(9) . ?
C27 C28 1.394(10) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C35 1.372(7) . ?
C30 C31 1.377(7) . ?
C31 C32 1.384(8) . ?
C31 H31A 0.9300 . ?
C32 C33 1.361(8) . ?
C32 H32A 0.9300 . ?
C33 C34 1.376(8) . ?
C33 C36 1.522(7) . ?
C34 C35 1.381(8) . ?
C34 H34A 0.9300 . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.510(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.537(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.520(10) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.479(11) . ?
C40 C46 1.487(12) . ?
C40 H40A 0.9800 . ?
C41 C42 1.454(13) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.380(15) . ?
C42 H42A 0.9300 . ?
C43 C44 1.352(15) . ?
C43 H43A 0.9300 . ?
C44 C45 1.423(14) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.405(13) . ?
C45 H45A 0.9300 . ?
C46 H46A 0.9300 . ?
P1 F1 1.484(6) . ?
P1 F6 1.502(6) . ?
P1 F5 1.509(6) . ?
P1 F4 1.528(6) . ?
P1 F2 1.574(6) . ?
P1 F3 1.576(5) . ?
C47 Cl1 1.724(9) . ?
C47 Cl2 1.733(9) . ?
C47 Cl3 1.762(10) . ?
C47 H47A 0.9800 . ?
C49 Cl9 1.695(10) . ?
C49 Cl7 1.743(9) . ?
C49 Cl8 1.762(11) . ?
C49 H49A 0.9800 . ?
C50 Cl10 1.716(11) . ?
C50 Cl12 1.731(11) . ?
C50 Cl11 1.783(12) . ?
C50 H50A 0.9800 . ?
C48 Cl4 1.712(15) . ?
C48 Cl5 1.720(13) . ?
C48 Cl6 1.777(15) . ?
C48 H48A 0.9800 . ?

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
C1 O1 C29 110.1(4) . . ?
C8 O2 C7 110.3(4) . . ?
C12 O3 C15 116.9(6) . . ?
C23 O4 C22 117.8(6) . . ?
C2 N1 C6 115.8(4) . . ?
C36 N2 C37 112.3(4) . . ?
C36 N2 H2A 109.1 . . ?
C37 N2 H2A 109.1 . . ?
C36 N2 H2B 109.1 . . ?
C37 N2 H2B 109.1 . . ?
H2A N2 H2B 107.9 . . ?
O1 C1 C2 112.2(5) . . ?
O1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
O1 C1 H1C 109.2 . . ?
C2 C1 H1C 109.2 . . ?
H1B C1 H1C 107.9 . . ?
N1 C2 C3 123.8(5) . . ?
N1 C2 C1 117.7(5) . . ?
C3 C2 C1 118.5(5) . . ?
C4 C3 C2 120.3(5) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 115.9(5) . . ?
C5 C4 C30 121.6(5) . . ?
C3 C4 C30 122.4(5) . . ?
C6 C5 C4 120.8(5) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
N1 C6 C5 123.4(5) . . ?
N1 C6 C7 117.8(5) . . ?
C5 C6 C7 118.8(5) . . ?
O2 C7 C6 112.4(4) . . ?
O2 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
O2 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
O2 C8 C9 109.0(5) . . ?
O2 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O2 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C14 C9 C10 117.6(6) . . ?
C14 C9 C8 120.7(6) . . ?
C10 C9 C8 121.6(7) . . ?
C9 C10 C11 120.0(7) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C12 C11 C10 120.5(6) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 119.6(6) . . ?
C11 C12 O3 124.5(6) . . ?
C13 C12 O3 115.8(7) . . ?
C14 C13 C12 119.8(7) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C13 C14 C9 122.5(6) . . ?
C13 C14 H14A 118.8 . . ?
C9 C14 H14A 118.8 . . ?
O3 C15 C16 112.3(5) . . ?
O3 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
O3 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C21 117.5(6) . . ?
C17 C16 C15 121.8(6) . . ?
C21 C16 C15 120.7(7) . . ?
C16 C17 C18 122.2(6) . . ?
C16 C17 H17A 118.9 . . ?
C18 C17 H17A 118.9 . . ?
C17 C18 C19 120.3(6) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C20 C19 C18 117.1(6) . . ?
C20 C19 C22 121.4(6) . . ?
C18 C19 C22 121.4(7) . . ?
C21 C20 C19 122.0(7) . . ?
C21 C20 H20A 119.0 . . ?
C19 C20 H20A 119.0 . . ?
C20 C21 C16 120.9(7) . . ?
C20 C21 H21A 119.6 . . ?
C16 C21 H21A 119.6 . . ?
O4 C22 C19 113.2(5) . . ?
O4 C22 H22A 108.9 . . ?
C19 C22 H22A 108.9 . . ?
O4 C22 H22B 108.9 . . ?
C19 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 O4 125.4(6) . . ?
C24 C23 C28 119.4(6) . . ?
O4 C23 C28 115.3(7) . . ?
C23 C24 C25 120.3(6) . . ?
C23 C24 H24A 119.8 . . ?
C25 C24 H24A 119.8 . . ?
C26 C25 C24 121.3(7) . . ?
C26 C25 H25A 119.4 . . ?
C24 C25 H25A 119.4 . . ?
C27 C26 C25 117.5(6) . . ?
C27 C26 C29 121.5(7) . . ?
C25 C26 C29 120.9(7) . . ?
C26 C27 C28 121.9(6) . . ?
C26 C27 H27A 119.1 . . ?
C28 C27 H27A 119.1 . . ?
C23 C28 C27 119.6(7) . . ?
C23 C28 H28A 120.2 . . ?
C27 C28 H28A 120.2 . . ?
O1 C29 C26 109.0(5) . . ?
O1 C29 H29A 109.9 . . ?
C26 C29 H29A 109.9 . . ?
O1 C29 H29B 109.9 . . ?
C26 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C35 C30 C31 116.1(5) . . ?
C35 C30 C4 122.0(5) . . ?
C31 C30 C4 121.9(5) . . ?
C30 C31 C32 122.0(5) . . ?
C30 C31 H31A 119.0 . . ?
C32 C31 H31A 119.0 . . ?
C33 C32 C31 121.0(5) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C32 C33 C34 117.9(5) . . ?
C32 C33 C36 121.6(5) . . ?
C34 C33 C36 120.4(5) . . ?
C33 C34 C35 120.5(6) . . ?
C33 C34 H34A 119.7 . . ?
C35 C34 H34A 119.7 . . ?
C30 C35 C34 122.4(5) . . ?
C30 C35 H35A 118.8 . . ?
C34 C35 H35A 118.8 . . ?
N2 C36 C33 111.4(4) . . ?
N2 C36 H36A 109.3 . . ?
C33 C36 H36A 109.4 . . ?
N2 C36 H36B 109.3 . . ?
C33 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
N2 C37 C38 110.4(4) . . ?
N2 C37 H37A 109.6 . . ?
C38 C37 H37A 109.6 . . ?
N2 C37 H37B 109.6 . . ?
C38 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
C37 C38 C39 110.7(5) . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 C38 113.4(6) . . ?
C40 C39 H39A 108.9 . . ?
C38 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C41 C40 C46 107.9(7) . . ?
C41 C40 C39 112.1(7) . . ?
C46 C40 C39 112.3(7) . . ?
C41 C40 H40A 108.1 . . ?
C46 C40 H40A 108.1 . . ?
C39 C40 H40A 108.1 . . ?
C42 C41 C40 118.9(9) . . ?
C42 C41 H41A 107.6 . . ?
C40 C41 H41A 107.6 . . ?
C42 C41 H41B 107.6 . . ?
C40 C41 H41B 107.6 . . ?
H41A C41 H41B 107.0 . . ?
C43 C42 C41 126.1(10) . . ?
C43 C42 H42A 116.9 . . ?
C41 C42 H42A 116.9 . . ?
C44 C43 C42 125.5(12) . . ?
C44 C43 H43A 117.3 . . ?
C42 C43 H43A 117.2 . . ?
C43 C44 C45 126.0(12) . . ?
C43 C44 H44A 105.8 . . ?
C45 C44 H44A 105.8 . . ?
C43 C44 H44B 105.8 . . ?
C45 C44 H44B 105.8 . . ?
H44A C44 H44B 106.2 . . ?
C46 C45 C44 122.7(11) . . ?
C46 C45 H45A 118.7 . . ?
C44 C45 H45A 118.6 . . ?
C45 C46 C40 120.7(10) . . ?
C45 C46 H46A 119.6 . . ?
C40 C46 H46A 119.7 . . ?
F1 P1 F6 95.7(6) . . ?
F1 P1 F5 88.1(5) . . ?
F6 P1 F5 94.8(5) . . ?
F1 P1 F4 89.5(6) . . ?
F6 P1 F4 174.5(5) . . ?
F5 P1 F4 87.2(4) . . ?
F1 P1 F2 177.6(6) . . ?
F6 P1 F2 85.9(5) . . ?
F5 P1 F2 93.6(5) . . ?
F4 P1 F2 88.8(4) . . ?
F1 P1 F3 91.5(4) . . ?
F6 P1 F3 88.2(4) . . ?
F5 P1 F3 177.0(4) . . ?
F4 P1 F3 89.8(4) . . ?
F2 P1 F3 86.7(3) . . ?
Cl1 C47 Cl2 111.3(5) . . ?
Cl1 C47 Cl3 110.7(5) . . ?
Cl2 C47 Cl3 109.6(5) . . ?
Cl1 C47 H47A 108.4 . . ?
Cl2 C47 H47A 108.4 . . ?
Cl3 C47 H47A 108.4 . . ?
Cl9 C49 Cl7 110.6(6) . . ?
Cl9 C49 Cl8 112.5(6) . . ?
Cl7 C49 Cl8 109.4(6) . . ?
Cl9 C49 H49A 108.1 . . ?
Cl7 C49 H49A 108.1 . . ?
Cl8 C49 H49A 108.1 . . ?
Cl10 C50 Cl12 112.8(7) . . ?
Cl10 C50 Cl11 110.6(5) . . ?
Cl12 C50 Cl11 110.1(5) . . ?
Cl10 C50 H50A 107.7 . . ?
Cl12 C50 H50A 107.7 . . ?
Cl11 C50 H50A 107.7 . . ?
Cl4 C48 Cl5 110.8(8) . . ?
Cl4 C48 Cl6 104.8(8) . . ?
Cl5 C48 Cl6 105.1(8) . . ?
Cl4 C48 H48A 111.9 . . ?
Cl5 C48 H48A 111.9 . . ?
Cl6 C48 H48A 111.9 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.065

# Attachment 'B716331B-ic12839.cif'

data_ic12839
_database_code_depnum_ccdc_archive 'CCDC 664528'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H43 F6 N2 O4 P'
_chemical_formula_weight         796.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   12.50690(10)
_cell_length_b                   17.0522(2)
_cell_length_c                   18.6392(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3975.19(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    51136
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26553
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.48
_reflns_number_total             9055
_reflns_number_gt                6808
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius BV)'
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Because of the large correlation between thermal parameters, the restraint
was necessary for convergence of the refinement process. In large
supermolecular structure with poor data to parameter ratios, they
often are needed with geometrical and anisotropic displacement parameters
restraints.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+0.4777P] 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     SHELXL
_refine_ls_extinction_coef       0.022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(13)
_refine_ls_number_reflns         9055
_refine_ls_number_parameters     524
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1510
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.41921(14) 0.96509(9) 0.25818(8) 0.0561(4) Uani 1 1 d . . .
O2 O 0.49042(15) 1.16648(10) 0.42924(10) 0.0645(4) Uani 1 1 d . . .
O3 O 0.91696(19) 1.01977(14) 0.53387(18) 0.1056(9) Uani 1 1 d . . .
O4 O 0.65163(19) 0.67918(10) 0.39081(11) 0.0791(6) Uani 1 1 d . . .
N1 N 0.36920(16) 1.11282(12) 0.31717(10) 0.0547(4) Uani 1 1 d . A .
C1 C 0.3542(2) 1.01943(17) 0.22031(14) 0.0681(7) Uani 1 1 d . . .
H1A H 0.2989 0.9915 0.1943 0.082 Uiso 1 1 calc R . .
H1B H 0.3975 1.0479 0.1858 0.082 Uiso 1 1 calc R . .
C2 C 0.3040(2) 1.07595(14) 0.27167(12) 0.0559(5) Uani 1 1 d . . .
C3 C 0.1944(2) 1.09025(16) 0.26832(15) 0.0671(6) Uani 1 1 d . . .
H3A H 0.1513 1.0621 0.2369 0.080 Uiso 1 1 calc R . .
C4 C 0.1511(2) 1.14656(19) 0.31215(17) 0.0749(8) Uani 1 1 d . . .
H4A H 0.0786 1.1584 0.3101 0.090 Uiso 1 1 calc R . .
C5 C 0.2173(2) 1.18486(18) 0.35909(15) 0.0712(7) Uani 1 1 d . A .
H5A H 0.1900 1.2231 0.3896 0.085 Uiso 1 1 calc R . .
C6 C 0.3258(2) 1.16629(14) 0.36086(13) 0.0582(6) Uani 1 1 d . . .
C7 C 0.3977(3) 1.20952(17) 0.41138(18) 0.0770(8) Uani 1 1 d U A .
H7A H 0.4187 1.2588 0.3896 0.092 Uiso 1 1 calc R . .
H7B H 0.3585 1.2214 0.4549 0.092 Uiso 1 1 calc R . .
C8 C 0.5507(8) 1.2066(6) 0.4841(7) 0.080(2) Uani 0.66(3) 1 d PU A 1
H8A H 0.5105 1.2082 0.5285 0.096 Uiso 0.66(3) 1 calc PR A 1
H8B H 0.5661 1.2600 0.4693 0.096 Uiso 0.66(3) 1 calc PR A 1
C8' C 0.5732(17) 1.2159(10) 0.4576(15) 0.082(3) Uani 0.34(3) 1 d PU A 2
H8'1 H 0.5438 1.2528 0.4919 0.099 Uiso 0.34(3) 1 calc PR A 2
H8'2 H 0.6075 1.2451 0.4193 0.099 Uiso 0.34(3) 1 calc PR A 2
C9 C 0.6536(3) 1.16102(18) 0.49420(18) 0.0765(8) Uani 1 1 d U . .
C10 C 0.7447(3) 1.16322(17) 0.45236(16) 0.0763(8) Uani 1 1 d . A .
H10A H 0.7482 1.1976 0.4137 0.092 Uiso 1 1 calc R . .
C11 C 0.8302(2) 1.11517(18) 0.46709(16) 0.0730(7) Uani 1 1 d . . .
H11A H 0.8909 1.1172 0.4383 0.088 Uiso 1 1 calc R A .
C12 C 0.8265(2) 1.06420(18) 0.52417(18) 0.0731(7) Uani 1 1 d . A .
C13 C 0.7381(3) 1.0625(2) 0.56858(17) 0.0823(8) Uani 1 1 d . . .
H13A H 0.7361 1.0293 0.6082 0.099 Uiso 1 1 calc R A .
C14 C 0.6520(3) 1.1113(2) 0.55286(19) 0.0840(9) Uani 1 1 d . A .
H14A H 0.5922 1.1105 0.5824 0.101 Uiso 1 1 calc R . .
C15 C 0.9104(3) 0.9471(2) 0.5723(2) 0.1086(14) Uani 1 1 d . . .
H15A H 0.8644 0.9538 0.6137 0.130 Uiso 1 1 calc R . .
H15B H 0.9810 0.9329 0.5895 0.130 Uiso 1 1 calc R . .
C16 C 0.8674(3) 0.88152(18) 0.52625(18) 0.0787(8) Uani 1 1 d . . .
C17 C 0.9263(3) 0.8530(2) 0.4695(2) 0.0950(10) Uani 1 1 d . . .
H17A H 0.9903 0.8771 0.4570 0.114 Uiso 1 1 calc R . .
C18 C 0.8909(3) 0.7888(2) 0.43080(18) 0.0901(9) Uani 1 1 d . . .
H18A H 0.9313 0.7707 0.3923 0.108 Uiso 1 1 calc R . .
C19 C 0.7975(2) 0.75146(16) 0.44806(14) 0.0682(7) Uani 1 1 d . . .
C20 C 0.7374(3) 0.7801(2) 0.50360(17) 0.0803(8) Uani 1 1 d . . .
H20A H 0.6732 0.7559 0.5156 0.096 Uiso 1 1 calc R . .
C21 C 0.7716(3) 0.8448(2) 0.54188(17) 0.0845(9) Uani 1 1 d . . .
H21A H 0.7292 0.8641 0.5789 0.101 Uiso 1 1 calc R . .
C22 C 0.7636(3) 0.67989(18) 0.40715(18) 0.0877(10) Uani 1 1 d . . .
H22A H 0.8038 0.6772 0.3627 0.105 Uiso 1 1 calc R . .
H22B H 0.7809 0.6336 0.4351 0.105 Uiso 1 1 calc R . .
C23 C 0.6135(2) 0.73601(13) 0.34499(13) 0.0615(6) Uani 1 1 d . . .
C24 C 0.6751(2) 0.77902(15) 0.29867(14) 0.0614(6) Uani 1 1 d . . .
H24A H 0.7488 0.7720 0.2972 0.074 Uiso 1 1 calc R . .
C25 C 0.6256(2) 0.83374(14) 0.25364(12) 0.0581(5) Uani 1 1 d . . .
H25A H 0.6670 0.8629 0.2219 0.070 Uiso 1 1 calc R . .
C26 C 0.51628(19) 0.84522(13) 0.25557(12) 0.0538(5) Uani 1 1 d . . .
C27 C 0.4557(2) 0.80035(17) 0.30256(15) 0.0673(6) Uani 1 1 d . . .
H27A H 0.3819 0.8066 0.3040 0.081 Uiso 1 1 calc R . .
C28 C 0.5044(3) 0.74647(16) 0.34722(16) 0.0718(7) Uani 1 1 d . . .
H28A H 0.4633 0.7171 0.3790 0.086 Uiso 1 1 calc R . .
C29 C 0.4615(2) 0.90594(16) 0.21077(13) 0.0654(7) Uani 1 1 d . . .
H29A H 0.5118 0.9293 0.1775 0.078 Uiso 1 1 calc R . .
H29B H 0.4040 0.8822 0.1834 0.078 Uiso 1 1 calc R . .
N2 N 0.52208(16) 0.99939(12) 0.39334(11) 0.0534(4) Uani 1 1 d . . .
C30 C 0.6362(2) 0.97553(15) 0.38694(13) 0.0593(6) Uani 1 1 d . . .
H30A H 0.6389 0.9194 0.3786 0.071 Uiso 1 1 calc R . .
H30B H 0.6714 0.9858 0.4323 0.071 Uiso 1 1 calc R . .
C31 C 0.69798(19) 1.01565(14) 0.32863(13) 0.0552(5) Uani 1 1 d . . .
C32 C 0.6630(2) 1.08212(15) 0.29297(15) 0.0626(6) Uani 1 1 d . . .
H32A H 0.5945 1.1013 0.3010 0.075 Uiso 1 1 calc R . .
C33 C 0.7302(2) 1.11967(19) 0.24562(18) 0.0791(8) Uani 1 1 d . . .
H33A H 0.7071 1.1652 0.2230 0.095 Uiso 1 1 calc R . .
C34 C 0.8304(3) 1.0913(2) 0.2311(2) 0.0838(9) Uani 1 1 d . . .
H34A H 0.8749 1.1170 0.1988 0.101 Uiso 1 1 calc R . .
C35 C 0.8644(2) 1.0241(2) 0.2652(2) 0.0852(9) Uani 1 1 d . . .
H35A H 0.9320 1.0041 0.2555 0.102 Uiso 1 1 calc R . .
C36 C 0.7994(2) 0.98654(17) 0.31323(17) 0.0709(7) Uani 1 1 d . . .
H36A H 0.8232 0.9411 0.3358 0.085 Uiso 1 1 calc R . .
C37 C 0.4660(3) 0.95256(17) 0.45020(16) 0.0732(7) Uani 1 1 d . . .
H37A H 0.4570 0.8991 0.4336 0.088 Uiso 1 1 calc R . .
H37B H 0.5100 0.9512 0.4930 0.088 Uiso 1 1 calc R . .
C38 C 0.3589(2) 0.98623(16) 0.46848(13) 0.0638(6) Uani 1 1 d . . .
C39 C 0.3503(2) 1.0370(2) 0.52610(15) 0.0753(8) Uani 1 1 d . . .
H39A H 0.4105 1.0491 0.5531 0.090 Uiso 1 1 calc R . .
C40 C 0.2533(3) 1.0694(2) 0.54357(19) 0.0909(10) Uani 1 1 d . . .
H40A H 0.2487 1.1031 0.5827 0.109 Uiso 1 1 calc R . .
C41 C 0.1649(3) 1.0536(3) 0.5052(2) 0.0983(12) Uani 1 1 d . . .
H41A H 0.1002 1.0771 0.5171 0.118 Uiso 1 1 calc R . .
C42 C 0.1708(3) 1.0020(3) 0.4477(2) 0.0957(11) Uani 1 1 d . . .
H42A H 0.1095 0.9903 0.4215 0.115 Uiso 1 1 calc R . .
C43 C 0.2676(3) 0.96761(19) 0.42916(16) 0.0778(8) Uani 1 1 d . . .
H43A H 0.2715 0.9326 0.3910 0.093 Uiso 1 1 calc R . .
P1 P 0.58142(8) 0.66592(5) 0.76189(5) 0.0827(3) Uani 1 1 d . . .
F1 F 0.5695(4) 0.6081(2) 0.69772(16) 0.1789(16) Uani 1 1 d . . .
F2 F 0.5764(4) 0.7231(3) 0.8266(2) 0.2051(18) Uani 1 1 d . . .
F3 F 0.7002(2) 0.6658(3) 0.7687(3) 0.236(2) Uani 1 1 d . . .
F4 F 0.5726(3) 0.59379(18) 0.81416(15) 0.1435(11) Uani 1 1 d . . .
F5 F 0.4561(2) 0.6664(2) 0.7593(2) 0.1819(15) Uani 1 1 d . . .
F6 F 0.5841(5) 0.7350(2) 0.7102(2) 0.236(3) Uani 1 1 d . . .
H2 H 0.4929(19) 0.9939(14) 0.3532(14) 0.045(6) Uiso 1 1 d . . .
H1 H 0.518(2) 1.0531(18) 0.4026(14) 0.058(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0687(9) 0.0510(8) 0.0485(7) -0.0029(7) -0.0091(7) 0.0117(7)
O2 0.0706(10) 0.0507(9) 0.0722(10) -0.0104(8) -0.0109(9) 0.0057(8)
O3 0.0703(13) 0.0809(14) 0.166(3) 0.0055(16) -0.0346(15) -0.0070(12)
O4 0.1139(16) 0.0465(9) 0.0770(12) 0.0062(9) -0.0335(11) 0.0038(10)
N1 0.0586(10) 0.0508(10) 0.0547(10) 0.0027(8) 0.0001(8) 0.0106(9)
C1 0.0854(18) 0.0683(15) 0.0507(12) -0.0013(11) -0.0115(12) 0.0268(14)
C2 0.0624(13) 0.0553(12) 0.0501(11) 0.0060(10) -0.0017(10) 0.0114(10)
C3 0.0625(14) 0.0701(15) 0.0685(15) 0.0080(13) -0.0052(12) 0.0059(12)
C4 0.0569(14) 0.0840(19) 0.0838(19) 0.0118(16) 0.0067(13) 0.0150(14)
C5 0.0709(16) 0.0707(16) 0.0720(16) -0.0003(13) 0.0122(13) 0.0209(13)
C6 0.0649(13) 0.0515(12) 0.0583(13) 0.0038(10) 0.0029(11) 0.0107(11)
C7 0.093(2) 0.0561(14) 0.0820(17) -0.0129(13) -0.0113(15) 0.0223(14)
C8 0.091(4) 0.063(3) 0.086(4) -0.025(3) -0.016(3) 0.009(3)
C8' 0.092(5) 0.063(4) 0.091(6) -0.019(5) -0.019(5) 0.001(4)
C9 0.0818(18) 0.0614(15) 0.0862(19) -0.0229(14) -0.0220(15) -0.0003(14)
C10 0.098(2) 0.0616(15) 0.0690(16) -0.0084(13) -0.0190(16) -0.0131(15)
C11 0.0775(17) 0.0698(16) 0.0717(16) -0.0126(14) -0.0011(14) -0.0158(14)
C12 0.0619(15) 0.0662(15) 0.0912(19) -0.0065(14) -0.0207(14) -0.0124(13)
C13 0.091(2) 0.0847(19) 0.0711(17) 0.0026(16) -0.0159(16) -0.0205(17)
C14 0.0737(17) 0.095(2) 0.083(2) -0.0251(18) 0.0029(15) -0.0173(17)
C15 0.115(3) 0.080(2) 0.131(3) 0.007(2) -0.075(3) -0.011(2)
C16 0.0869(19) 0.0695(16) 0.0797(18) 0.0048(15) -0.0392(16) -0.0017(15)
C17 0.094(2) 0.100(3) 0.091(2) 0.023(2) -0.012(2) -0.016(2)
C18 0.100(2) 0.101(2) 0.0694(17) 0.0096(18) 0.0022(17) 0.008(2)
C19 0.0802(17) 0.0674(15) 0.0570(13) 0.0044(12) -0.0162(13) 0.0132(13)
C20 0.0722(17) 0.087(2) 0.0813(18) -0.0098(16) -0.0083(15) -0.0100(16)
C21 0.085(2) 0.096(2) 0.0728(17) -0.0258(17) -0.0130(15) 0.0011(17)
C22 0.120(3) 0.0651(17) 0.0785(18) -0.0008(14) -0.0286(18) 0.0252(17)
C23 0.0896(18) 0.0401(10) 0.0549(13) -0.0014(10) -0.0159(12) 0.0002(11)
C24 0.0674(14) 0.0586(13) 0.0581(13) -0.0081(11) -0.0046(11) 0.0114(11)
C25 0.0755(15) 0.0496(11) 0.0493(11) -0.0001(10) 0.0042(11) 0.0045(11)
C26 0.0665(14) 0.0467(11) 0.0480(11) -0.0042(9) -0.0058(10) 0.0044(10)
C27 0.0648(14) 0.0592(14) 0.0778(16) 0.0037(13) -0.0045(12) -0.0048(12)
C28 0.0847(19) 0.0546(14) 0.0761(17) 0.0109(13) -0.0040(14) -0.0137(13)
C29 0.0871(17) 0.0598(14) 0.0492(12) -0.0062(11) -0.0060(12) 0.0172(13)
N2 0.0610(11) 0.0523(11) 0.0469(10) -0.0007(8) -0.0047(9) -0.0004(9)
C30 0.0659(14) 0.0567(12) 0.0552(12) -0.0036(11) -0.0080(11) 0.0104(11)
C31 0.0551(12) 0.0523(12) 0.0583(12) -0.0086(10) -0.0086(10) 0.0031(10)
C32 0.0604(13) 0.0600(14) 0.0674(14) 0.0008(12) -0.0011(11) 0.0133(12)
C33 0.0813(18) 0.0683(16) 0.0878(19) 0.0120(16) 0.0058(16) 0.0076(14)
C34 0.0685(17) 0.083(2) 0.100(2) 0.0039(18) 0.0161(16) -0.0046(15)
C35 0.0549(15) 0.0826(19) 0.118(3) -0.0035(19) 0.0078(16) 0.0046(14)
C36 0.0587(14) 0.0595(14) 0.0946(19) 0.0014(14) -0.0049(13) 0.0107(12)
C37 0.0899(19) 0.0656(15) 0.0640(15) 0.0124(13) 0.0076(14) 0.0007(14)
C38 0.0713(15) 0.0676(14) 0.0525(13) 0.0121(11) 0.0025(11) -0.0121(13)
C39 0.0777(18) 0.093(2) 0.0555(14) 0.0038(14) 0.0058(13) -0.0185(16)
C40 0.082(2) 0.116(3) 0.0747(18) -0.0020(19) 0.0236(17) -0.012(2)
C41 0.074(2) 0.131(3) 0.090(2) 0.016(2) 0.0247(18) -0.010(2)
C42 0.0719(19) 0.124(3) 0.091(2) 0.030(2) -0.0063(17) -0.0326(19)
C43 0.087(2) 0.0838(19) 0.0628(15) 0.0113(14) -0.0061(14) -0.0260(16)
P1 0.0859(5) 0.0751(5) 0.0872(5) 0.0036(4) -0.0076(4) -0.0001(4)
F1 0.300(5) 0.132(2) 0.1047(17) -0.0237(18) 0.037(2) -0.042(3)
F2 0.241(4) 0.190(4) 0.184(3) -0.100(3) -0.054(3) 0.014(3)
F3 0.0774(17) 0.293(6) 0.337(6) 0.095(5) 0.024(3) -0.006(2)
F4 0.171(3) 0.140(2) 0.1200(19) 0.0487(18) -0.0283(19) -0.0192(19)
F5 0.108(2) 0.179(3) 0.258(4) -0.020(4) -0.044(2) 0.0147(19)
F6 0.379(6) 0.134(3) 0.195(3) 0.080(3) -0.115(4) -0.120(3)

_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 C1 1.420(3) . ?
O1 C29 1.441(3) . ?
O2 C7 1.412(3) . ?
O2 C8' 1.435(17) . ?
O2 C8 1.443(8) . ?
O3 C12 1.374(4) . ?
O3 C15 1.434(4) . ?
O4 C23 1.377(3) . ?
O4 C22 1.433(4) . ?
N1 C2 1.334(3) . ?
N1 C6 1.338(3) . ?
C1 C2 1.497(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.393(4) . ?
C3 C4 1.372(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.393(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.496(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.516(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8' C9 1.535(18) . ?
C8' H8'1 0.9700 . ?
C8' H8'2 0.9700 . ?
C9 C10 1.381(5) . ?
C9 C14 1.384(5) . ?
C10 C11 1.375(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.375(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(5) . ?
C13 C14 1.392(5) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C15 C16 1.509(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.378(5) . ?
C16 C21 1.383(5) . ?
C17 C18 1.384(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.368(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.370(4) . ?
C19 C22 1.500(4) . ?
C20 C21 1.382(4) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.371(4) . ?
C23 C28 1.376(4) . ?
C24 C25 1.399(3) . ?
C24 H24A 0.9300 . ?
C25 C26 1.382(4) . ?
C25 H25A 0.9300 . ?
C26 C27 1.388(4) . ?
C26 C29 1.497(3) . ?
C27 C28 1.381(4) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
N2 C30 1.489(3) . ?
N2 C37 1.501(3) . ?
N2 H2 0.84(3) . ?
N2 H1 0.93(3) . ?
C30 C31 1.499(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.385(3) . ?
C31 C36 1.392(3) . ?
C32 C33 1.376(4) . ?
C32 H32A 0.9300 . ?
C33 C34 1.371(4) . ?
C33 H33A 0.9300 . ?
C34 C35 1.377(5) . ?
C34 H34A 0.9300 . ?
C35 C36 1.368(5) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 C38 1.497(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.383(4) . ?
C38 C43 1.393(4) . ?
C39 C40 1.372(5) . ?
C39 H39A 0.9300 . ?
C40 C41 1.344(5) . ?
C40 H40A 0.9300 . ?
C41 C42 1.390(6) . ?
C41 H41A 0.9300 . ?
C42 C43 1.389(5) . ?
C42 H42A 0.9300 . ?
C43 H43A 0.9300 . ?
P1 F3 1.491(3) . ?
P1 F6 1.522(3) . ?
P1 F2 1.552(3) . ?
P1 F1 1.558(3) . ?
P1 F5 1.568(3) . ?
P1 F4 1.573(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
C1 O1 C29 111.20(17) . . ?
C7 O2 C8' 112.0(7) . . ?
C7 O2 C8 110.4(3) . . ?
C8' O2 C8 23.7(8) . . ?
C12 O3 C15 119.7(3) . . ?
C23 O4 C22 117.7(2) . . ?
C2 N1 C6 117.4(2) . . ?
O1 C1 C2 110.03(19) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 C3 123.2(2) . . ?
N1 C2 C1 116.9(2) . . ?
C3 C2 C1 119.8(2) . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
N1 C6 C5 122.4(2) . . ?
N1 C6 C7 118.3(2) . . ?
C5 C6 C7 119.2(2) . . ?
O2 C7 C6 112.7(2) . . ?
O2 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
O2 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
O2 C8 C9 106.8(5) . . ?
O2 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
O2 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
O2 C8' C9 106.2(11) . . ?
O2 C8' H8'1 110.5 . . ?
C9 C8' H8'1 110.5 . . ?
O2 C8' H8'2 110.5 . . ?
C9 C8' H8'2 110.5 . . ?
H8'1 C8' H8'2 108.7 . . ?
C10 C9 C14 118.4(3) . . ?
C10 C9 C8 128.0(7) . . ?
C14 C9 C8 113.6(7) . . ?
C10 C9 C8' 105.8(12) . . ?
C14 C9 C8' 135.7(12) . . ?
C8 C9 C8' 22.3(8) . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
O3 C12 C11 115.0(3) . . ?
O3 C12 C13 124.6(3) . . ?
C11 C12 C13 120.3(3) . . ?
C12 C13 C14 118.7(3) . . ?
C12 C13 H13A 120.7 . . ?
C14 C13 H13A 120.7 . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
O3 C15 C16 112.1(3) . . ?
O3 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
O3 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C21 117.8(3) . . ?
C17 C16 C15 120.5(4) . . ?
C21 C16 C15 121.6(4) . . ?
C16 C17 C18 120.5(3) . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C19 C18 C17 121.3(3) . . ?
C19 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
C18 C19 C20 118.7(3) . . ?
C18 C19 C22 120.0(3) . . ?
C20 C19 C22 121.2(3) . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20A 119.8 . . ?
C21 C20 H20A 119.8 . . ?
C20 C21 C16 121.4(3) . . ?
C20 C21 H21A 119.3 . . ?
C16 C21 H21A 119.3 . . ?
O4 C22 C19 113.0(3) . . ?
O4 C22 H22A 109.0 . . ?
C19 C22 H22A 109.0 . . ?
O4 C22 H22B 109.0 . . ?
C19 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C28 120.5(2) . . ?
C24 C23 O4 124.9(3) . . ?
C28 C23 O4 114.6(2) . . ?
C23 C24 C25 119.1(2) . . ?
C23 C24 H24A 120.5 . . ?
C25 C24 H24A 120.5 . . ?
C26 C25 C24 121.1(2) . . ?
C26 C25 H25A 119.4 . . ?
C24 C25 H25A 119.4 . . ?
C25 C26 C27 118.6(2) . . ?
C25 C26 C29 122.5(2) . . ?
C27 C26 C29 118.9(2) . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27A 119.8 . . ?
C26 C27 H27A 119.8 . . ?
C23 C28 C27 120.3(3) . . ?
C23 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
O1 C29 C26 108.06(18) . . ?
O1 C29 H29A 110.1 . . ?
C26 C29 H29A 110.1 . . ?
O1 C29 H29B 110.1 . . ?
C26 C29 H29B 110.1 . . ?
H29A C29 H29B 108.4 . . ?
C30 N2 C37 111.0(2) . . ?
C30 N2 H2 108.4(16) . . ?
C37 N2 H2 111.5(17) . . ?
C30 N2 H1 109.3(16) . . ?
C37 N2 H1 111.6(16) . . ?
H2 N2 H1 105(2) . . ?
N2 C30 C31 115.3(2) . . ?
N2 C30 H30A 108.4 . . ?
C31 C30 H30A 108.4 . . ?
N2 C30 H30B 108.4 . . ?
C31 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
C32 C31 C36 118.7(2) . . ?
C32 C31 C30 124.0(2) . . ?
C36 C31 C30 117.2(2) . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32A 120.1 . . ?
C31 C32 H32A 120.1 . . ?
C34 C33 C32 121.3(3) . . ?
C34 C33 H33A 119.3 . . ?
C32 C33 H33A 119.3 . . ?
C33 C34 C35 119.0(3) . . ?
C33 C34 H34A 120.5 . . ?
C35 C34 H34A 120.5 . . ?
C36 C35 C34 120.6(3) . . ?
C36 C35 H35A 119.7 . . ?
C34 C35 H35A 119.7 . . ?
C35 C36 C31 120.6(3) . . ?
C35 C36 H36A 119.7 . . ?
C31 C36 H36A 119.7 . . ?
C38 C37 N2 112.0(2) . . ?
C38 C37 H37A 109.2 . . ?
N2 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
N2 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C39 C38 C43 119.1(3) . . ?
C39 C38 C37 119.1(3) . . ?
C43 C38 C37 121.8(3) . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39A 119.8 . . ?
C38 C39 H39A 119.8 . . ?
C41 C40 C39 121.4(4) . . ?
C41 C40 H40A 119.3 . . ?
C39 C40 H40A 119.3 . . ?
C40 C41 C42 119.6(4) . . ?
C40 C41 H41A 120.2 . . ?
C42 C41 H41A 120.2 . . ?
C43 C42 C41 120.4(3) . . ?
C43 C42 H42A 119.8 . . ?
C41 C42 H42A 119.8 . . ?
C42 C43 C38 119.2(3) . . ?
C42 C43 H43A 120.4 . . ?
C38 C43 H43A 120.4 . . ?
F3 P1 F6 91.9(3) . . ?
F3 P1 F2 88.5(3) . . ?
F6 P1 F2 90.4(3) . . ?
F3 P1 F1 99.2(3) . . ?
F6 P1 F1 90.4(2) . . ?
F2 P1 F1 172.2(3) . . ?
F3 P1 F5 176.8(3) . . ?
F6 P1 F5 89.9(3) . . ?
F2 P1 F5 88.9(3) . . ?
F1 P1 F5 83.4(2) . . ?
F3 P1 F4 90.9(2) . . ?
F6 P1 F4 177.1(3) . . ?
F2 P1 F4 90.4(2) . . ?
F1 P1 F4 88.50(18) . . ?
F5 P1 F4 87.3(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O1 0.84(3) 2.06(3) 2.889(3) 173(2) .
N2 H1 O2 0.93(3) 2.03(3) 2.953(3) 172(2) .
N2 H2 N1 0.84(3) 2.64(2) 3.068(3) 113(2) .
N2 H2 N1 0.84(3) 2.64(2) 3.068(3) 113(2) .

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.034