# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2000
# CCDC Number: 440/198


data_ccd287

_audit_creation_method            SHELXL-97

#Manuscript 0/018B
#Compound 2b

_publ_contact_author_name
;
Gregory J. Kubas
;

_publ_contact_author_address
;
Chemistry Division
MS J514
Los Alamos National Laboratory
Los Alamos, NM 87545  USA
;

_publ_requested_journal  'Chemical Communications'

_publ_section_title
;
Triphenylmethyl Tris(p-methoxyphenyl)phosphonium
Cation: A Structurally Characterized Phosphomium
Analog of Hexaphenylethane
;



_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C72 H48 B F24 O3 P'
_chemical_formula_weight          1458.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 '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'
 'B'  'B'   0.0013   0.0007
 '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                    14.2714(8)
_cell_length_b                    15.7335(9)
_cell_length_c                    17.2879(9)
_cell_angle_alpha                 113.553(1)
_cell_angle_beta                  104.959(1)
_cell_angle_gamma                 97.734(1)
_cell_volume                      3311.7(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     203(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        irregular
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.21
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.463
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1480
_exptl_absorpt_coefficient_mu     0.158
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.97
_exptl_absorpt_correction_T_max   0.98
_exptl_absorpt_process_details    'SADABS (Sheldrick, 1996)'

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       203(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   'Bruker P4/CCD'
_diffrn_measurement_method        '\w and \f scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             12747
_diffrn_reflns_av_R_equivalents   0.0214
_diffrn_reflns_av_sigmaI/netI     0.0481
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.47
_diffrn_reflns_theta_max          23.28
_reflns_number_total              8914
_reflns_number_gt                 6928
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'SMART 4.210 (Bruker, 1996)'
_computing_cell_refinement        'SAINT 4.05  (Bruker, 1996)'
_computing_data_reduction         'SAINT 4.05  (Bruker, 1996)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'SHELXTL NT 5.10 (Bruker, 1997)'
_computing_publication_material   'SHELXTL NT 5.10 (Bruker, 1997)'

_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^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     noref
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          8914
_refine_ls_number_parameters      910
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0835
_refine_ls_R_factor_gt            0.0640
_refine_ls_wR_factor_ref          0.1793
_refine_ls_wR_factor_gt           0.1693
_refine_ls_goodness_of_fit_ref    1.540
_refine_ls_restrained_S_all       1.540
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.18622(7) 0.44847(7) 0.29183(6) 0.0289(3) Uani 1 1 d . . .
F1 F 0.08955(19) 0.09937(19) 0.06453(16) 0.0591(7) Uani 1 1 d . . .
F2 F 0.24595(18) 0.1091(2) 0.08773(16) 0.0674(8) Uani 1 1 d . . .
F3 F 0.1365(2) -0.0274(2) 0.00904(19) 0.0730(8) Uani 1 1 d . . .
F4 F -0.0628(2) 0.1089(2) -0.2956(2) 0.0936(11) Uani 1 1 d . . .
F5 F -0.0845(2) -0.0374(2) -0.3298(2) 0.1089(14) Uani 1 1 d . . .
F6 F -0.1311(2) 0.0506(3) -0.2288(2) 0.1129(14) Uani 1 1 d . . .
F7 F 0.2343(3) -0.1044(2) -0.56187(19) 0.0862(10) Uani 1 1 d . . .
F8 F 0.2649(7) -0.1347(3) -0.4533(2) 0.227(4) Uani 1 1 d . . .
F9 F 0.1280(5) -0.1163(3) -0.5043(4) 0.207(4) Uani 1 1 d . . .
F10 F 0.3440(3) 0.2321(2) -0.4921(2) 0.0926(11) Uani 1 1 d . . .
F11 F 0.2522(4) 0.3000(4) -0.4256(4) 0.192(3) Uani 1 1 d . . .
F12 F 0.4052(4) 0.3336(3) -0.3627(3) 0.1302(17) Uani 1 1 d . . .
F13 F 0.7108(2) 0.2421(2) -0.1022(3) 0.0983(12) Uani 1 1 d . . .
F14 F 0.7572(2) 0.1177(2) -0.1139(3) 0.1008(12) Uani 1 1 d . . .
F15 F 0.7522(2) 0.2156(3) 0.0077(3) 0.1259(16) Uani 1 1 d . . .
F16 F 0.5147(3) -0.1314(2) -0.0770(3) 0.1223(16) Uani 1 1 d . . .
F17 F 0.3672(3) -0.1534(3) -0.1443(4) 0.156(2) Uani 1 1 d . . .
F18 F 0.4648(5) -0.1815(2) -0.2110(3) 0.159(2) Uani 1 1 d . . .
F19 F 0.2268(2) 0.5425(2) 0.02966(19) 0.0718(8) Uani 1 1 d . . .
F20 F 0.3080(3) 0.5730(3) -0.0458(3) 0.1136(14) Uani 1 1 d . . .
F21 F 0.1752(3) 0.4586(2) -0.1096(2) 0.1158(15) Uani 1 1 d . . .
F22 F 0.5933(2) 0.5209(2) 0.18798(19) 0.0840(9) Uani 1 1 d . . .
F23 F 0.5845(3) 0.3791(2) 0.16140(19) 0.0920(11) Uani 1 1 d . . .
F24 F 0.4859(2) 0.4506(3) 0.22198(19) 0.1187(15) Uani 1 1 d . . .
O1 O 0.0066(2) 0.2989(2) -0.10339(17) 0.0465(7) Uani 1 1 d . . .
O2 O 0.4348(2) 0.1914(2) 0.35130(19) 0.0491(7) Uani 1 1 d . . .
O3 O 0.4536(2) 0.8336(2) 0.4079(2) 0.0617(9) Uani 1 1 d . . .
C1 C 0.0985(3) 0.4621(2) 0.3619(2) 0.0285(8) Uani 1 1 d . . .
C2 C 0.1214(3) 0.4007(3) 0.1727(2) 0.0311(9) Uani 1 1 d . . .
C3 C 0.0363(3) 0.4235(3) 0.1351(3) 0.0352(9) Uani 1 1 d . . .
H3 H 0.0064 0.4619 0.1725 0.042 Uiso 1 1 calc R . .
C4 C -0.0049(3) 0.3907(3) 0.0440(3) 0.0364(9) Uani 1 1 d . . .
H4 H -0.0630 0.4055 0.0201 0.044 Uiso 1 1 calc R . .
C5 C 0.0407(3) 0.3351(3) -0.0126(2) 0.0340(9) Uani 1 1 d . . .
C6 C 0.1271(3) 0.3135(3) 0.0243(3) 0.0366(9) Uani 1 1 d . . .
H6 H 0.1585 0.2773 -0.0129 0.044 Uiso 1 1 calc R . .
C7 C 0.1665(3) 0.3449(3) 0.1150(3) 0.0342(9) Uani 1 1 d . . .
H7 H 0.2239 0.3291 0.1387 0.041 Uiso 1 1 calc R . .
C8 C -0.0811(3) 0.3208(3) -0.1445(3) 0.0481(11) Uani 1 1 d . . .
H8A H -0.0962 0.2919 -0.2084 0.072 Uiso 1 1 calc R . .
H8B H -0.0691 0.3893 -0.1215 0.072 Uiso 1 1 calc R . .
H8C H -0.1370 0.2959 -0.1314 0.072 Uiso 1 1 calc R . .
C9 C 0.2597(3) 0.3684(3) 0.3069(2) 0.0299(8) Uani 1 1 d . . .
C10 C 0.3644(3) 0.3997(3) 0.3443(3) 0.0390(10) Uani 1 1 d . . .
H10 H 0.3971 0.4626 0.3601 0.047 Uiso 1 1 calc R . .
C11 C 0.4196(3) 0.3391(3) 0.3580(3) 0.0456(11) Uani 1 1 d . . .
H11 H 0.4894 0.3614 0.3834 0.055 Uiso 1 1 calc R . .
C12 C 0.3723(3) 0.2447(3) 0.3342(3) 0.0366(9) Uani 1 1 d . . .
C13 C 0.2686(3) 0.2114(3) 0.2950(2) 0.0351(9) Uani 1 1 d . . .
H13 H 0.2362 0.1481 0.2779 0.042 Uiso 1 1 calc R . .
C14 C 0.2137(3) 0.2729(3) 0.2816(2) 0.0346(9) Uani 1 1 d . . .
H14 H 0.1440 0.2502 0.2548 0.042 Uiso 1 1 calc R . .
C15 C 0.3914(4) 0.0935(3) 0.3274(3) 0.0623(13) Uani 1 1 d . . .
H15A H 0.4436 0.0649 0.3436 0.093 Uiso 1 1 calc R . .
H15B H 0.3559 0.0591 0.2638 0.093 Uiso 1 1 calc R . .
H15C H 0.3454 0.0906 0.3587 0.093 Uiso 1 1 calc R . .
C16 C 0.2716(3) 0.5623(3) 0.3260(3) 0.0314(9) Uani 1 1 d . . .
C17 C 0.3355(3) 0.6217(3) 0.4149(3) 0.0346(9) Uani 1 1 d . . .
H17 H 0.3374 0.6005 0.4582 0.042 Uiso 1 1 calc R . .
C18 C 0.3949(3) 0.7101(3) 0.4390(3) 0.0422(10) Uani 1 1 d . . .
H18 H 0.4373 0.7479 0.4983 0.051 Uiso 1 1 calc R . .
C19 C 0.3927(3) 0.7441(3) 0.3762(3) 0.0445(11) Uani 1 1 d . . .
C20 C 0.3324(3) 0.6863(3) 0.2876(3) 0.0447(11) Uani 1 1 d . . .
H20 H 0.3320 0.7076 0.2446 0.054 Uiso 1 1 calc R . .
C21 C 0.2726(3) 0.5963(3) 0.2632(3) 0.0377(10) Uani 1 1 d . . .
H21 H 0.2322 0.5578 0.2034 0.045 Uiso 1 1 calc R . .
C22 C 0.4507(4) 0.8736(4) 0.3472(4) 0.0789(17) Uani 1 1 d . . .
H22A H 0.4969 0.9366 0.3780 0.118 Uiso 1 1 calc R . .
H22B H 0.3838 0.8781 0.3240 0.118 Uiso 1 1 calc R . .
H22C H 0.4695 0.8330 0.2985 0.118 Uiso 1 1 calc R . .
C23 C 0.1702(3) 0.5145(3) 0.4610(2) 0.0298(8) Uani 1 1 d . . .
C24 C 0.2401(3) 0.4724(3) 0.4945(2) 0.0320(9) Uani 1 1 d . . .
H24 H 0.2406 0.4104 0.4578 0.038 Uiso 1 1 calc R . .
C25 C 0.3085(3) 0.5212(3) 0.5813(3) 0.0361(9) Uani 1 1 d . . .
H25 H 0.3554 0.4924 0.6017 0.043 Uiso 1 1 calc R . .
C26 C 0.3072(3) 0.6127(3) 0.6379(3) 0.0422(10) Uani 1 1 d . . .
H26 H 0.3534 0.6459 0.6961 0.051 Uiso 1 1 calc R . .
C27 C 0.2367(3) 0.6537(3) 0.6069(3) 0.0411(10) Uani 1 1 d . . .
H27 H 0.2347 0.7147 0.6448 0.049 Uiso 1 1 calc R . .
C28 C 0.1685(3) 0.6053(3) 0.5199(3) 0.0353(9) Uani 1 1 d . . .
H28 H 0.1208 0.6340 0.5004 0.042 Uiso 1 1 calc R . .
C29 C 0.0277(3) 0.5235(3) 0.3425(2) 0.0288(8) Uani 1 1 d . . .
C30 C 0.0641(3) 0.6116(3) 0.3440(2) 0.0334(9) Uani 1 1 d . . .
H30 H 0.1319 0.6325 0.3529 0.040 Uiso 1 1 calc R . .
C31 C 0.0004(3) 0.6683(3) 0.3323(3) 0.0401(10) Uani 1 1 d . . .
H31 H 0.0259 0.7267 0.3336 0.048 Uiso 1 1 calc R . .
C32 C -0.0998(3) 0.6386(3) 0.3188(3) 0.0444(11) Uani 1 1 d . . .
H32 H -0.1423 0.6764 0.3102 0.053 Uiso 1 1 calc R . .
C33 C -0.1373(3) 0.5526(3) 0.3178(3) 0.0457(11) Uani 1 1 d . . .
H33 H -0.2052 0.5326 0.3090 0.055 Uiso 1 1 calc R . .
C34 C -0.0741(3) 0.4959(3) 0.3298(3) 0.0359(9) Uani 1 1 d . . .
H34 H -0.1003 0.4382 0.3294 0.043 Uiso 1 1 calc R . .
C36 C 0.0371(3) 0.3276(3) 0.4000(3) 0.0379(10) Uani 1 1 d . . .
H36 H 0.0759 0.3677 0.4599 0.046 Uiso 1 1 calc R . .
C37 C -0.0194(3) 0.2361(3) 0.3758(3) 0.0491(11) Uani 1 1 d . . .
H37 H -0.0170 0.2152 0.4194 0.059 Uiso 1 1 calc R . .
C38 C -0.0788(3) 0.1761(3) 0.2879(4) 0.0545(12) Uani 1 1 d . . .
H38 H -0.1158 0.1145 0.2716 0.065 Uiso 1 1 calc R . .
C39 C -0.0826(3) 0.2084(3) 0.2250(3) 0.0514(12) Uani 1 1 d . . .
H39 H -0.1237 0.1687 0.1657 0.062 Uiso 1 1 calc R . .
C40 C -0.0263(3) 0.2993(3) 0.2481(3) 0.0422(10) Uani 1 1 d . . .
H40 H -0.0305 0.3200 0.2042 0.051 Uiso 1 1 calc R . .
C41 C 0.0366(3) 0.3602(3) 0.3365(3) 0.0315(9) Uani 1 1 d . . .
C42 C 0.2256(3) 0.1195(2) -0.1506(2) 0.0273(8) Uani 1 1 d . . .
C43 C 0.2305(3) 0.1069(2) -0.0734(2) 0.0303(8) Uani 1 1 d . . .
H43 H 0.2932 0.1195 -0.0317 0.036 Uiso 1 1 calc R . .
C44 C 0.1449(3) 0.0765(3) -0.0580(2) 0.0328(9) Uani 1 1 d . . .
C45 C 0.0499(3) 0.0574(3) -0.1185(3) 0.0373(9) Uani 1 1 d . . .
H45 H -0.0079 0.0368 -0.1083 0.045 Uiso 1 1 calc R . .
C46 C 0.0435(3) 0.0697(3) -0.1935(3) 0.0341(9) Uani 1 1 d . . .
C47 C 0.1294(3) 0.0997(2) -0.2095(2) 0.0313(9) Uani 1 1 d . . .
H47 H 0.1223 0.1068 -0.2614 0.038 Uiso 1 1 calc R . .
C48 C 0.1538(3) 0.0645(3) 0.0248(3) 0.0452(11) Uani 1 1 d . . .
C49 C -0.0574(3) 0.0475(3) -0.2614(3) 0.0471(11) Uani 1 1 d . . .
C50 C 0.3086(3) 0.1465(3) -0.2642(2) 0.0292(8) Uani 1 1 d . . .
C51 C 0.2758(3) 0.0495(3) -0.3300(3) 0.0353(9) Uani 1 1 d . . .
H51 H 0.2648 0.0019 -0.3120 0.042 Uiso 1 1 calc R . .
C52 C 0.2594(3) 0.0220(3) -0.4195(3) 0.0418(10) Uani 1 1 d . . .
C53 C 0.2743(3) 0.0912(3) -0.4489(3) 0.0442(11) Uani 1 1 d . . .
H53 H 0.2620 0.0731 -0.5096 0.053 Uiso 1 1 calc R . .
C54 C 0.3073(3) 0.1864(3) -0.3873(3) 0.0372(10) Uani 1 1 d . . .
C55 C 0.3246(3) 0.2138(3) -0.2962(2) 0.0313(9) Uani 1 1 d . . .
H55 H 0.3474 0.2789 -0.2557 0.038 Uiso 1 1 calc R . .
C56 C 0.2253(6) -0.0816(4) -0.4845(4) 0.0784(17) Uani 1 1 d . . .
C57 C 0.3209(4) 0.2598(3) -0.4191(3) 0.0548(12) Uani 1 1 d . . .
C58 C 0.4185(3) 0.1153(2) -0.1384(2) 0.0279(8) Uani 1 1 d . . .
C59 C 0.5193(3) 0.1610(3) -0.1182(2) 0.0315(9) Uani 1 1 d . . .
H59 H 0.5347 0.2221 -0.1146 0.038 Uiso 1 1 calc R . .
C60 C 0.5968(3) 0.1188(3) -0.1035(3) 0.0334(9) Uani 1 1 d . . .
C61 C 0.5770(3) 0.0273(3) -0.1088(3) 0.0375(9) Uani 1 1 d . . .
H61 H 0.6289 -0.0010 -0.0983 0.045 Uiso 1 1 calc R . .
C62 C 0.4785(3) -0.0203(2) -0.1302(2) 0.0308(9) Uani 1 1 d . . .
C63 C 0.4017(3) 0.0227(3) -0.1445(2) 0.0293(8) Uani 1 1 d . . .
H63 H 0.3361 -0.0113 -0.1588 0.035 Uiso 1 1 calc R . .
C64 C 0.7026(3) 0.1716(3) -0.0790(3) 0.0498(12) Uani 1 1 d . . .
C65 C 0.4557(3) -0.1193(3) -0.1401(3) 0.0387(10) Uani 1 1 d . . .
C66 C 0.3595(3) 0.2804(2) -0.0844(2) 0.0264(8) Uani 1 1 d . . .
C67 C 0.3044(3) 0.3440(3) -0.0952(2) 0.0314(9) Uani 1 1 d . . .
H67 H 0.2550 0.3245 -0.1505 0.038 Uiso 1 1 calc R . .
C68 C 0.3202(3) 0.4353(3) -0.0267(3) 0.0364(9) Uani 1 1 d . . .
C69 C 0.3942(3) 0.4668(3) 0.0562(3) 0.0412(10) Uani 1 1 d . . .
H69 H 0.4067 0.5285 0.1019 0.049 Uiso 1 1 calc R . .
C70 C 0.4485(3) 0.4053(3) 0.0694(2) 0.0352(9) Uani 1 1 d . . .
C71 C 0.4319(3) 0.3145(3) 0.0009(2) 0.0315(9) Uani 1 1 d . . .
H71 H 0.4703 0.2746 0.0118 0.038 Uiso 1 1 calc R . .
C72 C 0.2583(4) 0.5009(3) -0.0392(3) 0.0478(11) Uani 1 1 d . . .
C73 C 0.5247(4) 0.4376(3) 0.1588(3) 0.0560(12) Uani 1 1 d . . .
B1 B 0.3300(3) 0.1667(3) -0.1599(3) 0.0283(9) Uani 1 1 d . . .

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
P1 0.0294(5) 0.0313(6) 0.0289(6) 0.0147(5) 0.0116(4) 0.0101(4)
F1 0.0623(16) 0.0864(19) 0.0533(16) 0.0393(15) 0.0406(14) 0.0302(15)
F2 0.0463(15) 0.122(2) 0.0408(15) 0.0462(16) 0.0148(13) 0.0121(15)
F3 0.117(2) 0.0642(19) 0.0697(19) 0.0482(16) 0.0471(18) 0.0364(17)
F4 0.0605(18) 0.104(2) 0.112(3) 0.078(2) -0.0161(17) 0.0061(17)
F5 0.072(2) 0.078(2) 0.087(2) -0.013(2) -0.0322(18) 0.0232(18)
F6 0.0341(16) 0.221(4) 0.092(2) 0.080(3) 0.0199(17) 0.034(2)
F7 0.142(3) 0.0603(19) 0.0371(17) 0.0036(15) 0.0309(17) 0.0295(19)
F8 0.517(12) 0.051(2) 0.048(2) 0.0073(19) 0.007(4) 0.102(4)
F9 0.235(6) 0.093(3) 0.165(5) -0.059(3) 0.127(5) -0.087(4)
F10 0.167(3) 0.089(2) 0.078(2) 0.0603(19) 0.083(2) 0.055(2)
F11 0.229(5) 0.263(6) 0.403(8) 0.309(6) 0.265(6) 0.220(5)
F12 0.222(5) 0.072(2) 0.090(3) 0.051(2) 0.044(3) -0.008(3)
F13 0.0495(17) 0.092(2) 0.192(4) 0.100(3) 0.045(2) 0.0155(16)
F14 0.0542(18) 0.0646(19) 0.188(4) 0.040(2) 0.071(2) 0.0239(16)
F15 0.054(2) 0.174(4) 0.088(3) 0.037(3) 0.0000(19) -0.038(2)
F16 0.145(3) 0.063(2) 0.122(3) 0.066(2) -0.034(3) -0.004(2)
F17 0.088(3) 0.090(3) 0.370(7) 0.157(4) 0.107(4) 0.041(2)
F18 0.353(7) 0.0299(17) 0.117(3) 0.0199(19) 0.148(4) 0.026(3)
F19 0.098(2) 0.0770(19) 0.0706(19) 0.0379(16) 0.0508(17) 0.0590(17)
F20 0.153(3) 0.107(3) 0.205(4) 0.126(3) 0.133(3) 0.094(3)
F21 0.139(3) 0.089(2) 0.071(2) 0.0043(19) -0.014(2) 0.083(2)
F22 0.079(2) 0.076(2) 0.0548(18) 0.0138(16) -0.0029(15) -0.0090(17)
F23 0.107(3) 0.083(2) 0.0515(18) 0.0227(17) -0.0140(17) 0.027(2)
F24 0.083(2) 0.212(4) 0.0349(17) 0.050(2) 0.0137(16) -0.005(3)
O1 0.0576(18) 0.0596(19) 0.0295(16) 0.0211(15) 0.0174(14) 0.0300(15)
O2 0.0518(18) 0.0474(18) 0.0550(19) 0.0291(15) 0.0137(15) 0.0250(15)
O3 0.0512(19) 0.0498(19) 0.084(2) 0.0442(18) 0.0082(17) -0.0037(15)
C1 0.033(2) 0.029(2) 0.026(2) 0.0124(17) 0.0140(16) 0.0078(16)
C2 0.034(2) 0.030(2) 0.032(2) 0.0153(18) 0.0130(17) 0.0101(17)
C3 0.039(2) 0.037(2) 0.031(2) 0.0119(19) 0.0167(18) 0.0170(18)
C4 0.035(2) 0.041(2) 0.035(2) 0.016(2) 0.0119(18) 0.0195(18)
C5 0.045(2) 0.030(2) 0.028(2) 0.0133(18) 0.0135(18) 0.0105(18)
C6 0.044(2) 0.041(2) 0.036(2) 0.018(2) 0.0235(19) 0.0241(19)
C7 0.038(2) 0.039(2) 0.036(2) 0.021(2) 0.0177(19) 0.0207(19)
C8 0.049(3) 0.064(3) 0.036(2) 0.028(2) 0.013(2) 0.020(2)
C9 0.032(2) 0.033(2) 0.027(2) 0.0144(18) 0.0128(17) 0.0111(17)
C10 0.036(2) 0.040(2) 0.051(3) 0.028(2) 0.017(2) 0.0122(19)
C11 0.033(2) 0.055(3) 0.063(3) 0.036(2) 0.020(2) 0.018(2)
C12 0.044(2) 0.042(2) 0.034(2) 0.022(2) 0.0176(19) 0.021(2)
C13 0.042(2) 0.031(2) 0.030(2) 0.0116(18) 0.0121(18) 0.0106(18)
C14 0.033(2) 0.036(2) 0.033(2) 0.0126(19) 0.0110(17) 0.0140(18)
C15 0.080(4) 0.043(3) 0.063(3) 0.024(2) 0.016(3) 0.032(3)
C16 0.031(2) 0.034(2) 0.038(2) 0.0213(19) 0.0162(18) 0.0125(17)
C17 0.032(2) 0.039(2) 0.034(2) 0.020(2) 0.0105(18) 0.0048(18)
C18 0.035(2) 0.044(2) 0.044(3) 0.023(2) 0.0070(19) 0.0026(19)
C19 0.031(2) 0.040(2) 0.064(3) 0.030(2) 0.012(2) 0.0037(19)
C20 0.036(2) 0.055(3) 0.061(3) 0.043(2) 0.016(2) 0.012(2)
C21 0.034(2) 0.046(3) 0.043(2) 0.027(2) 0.0149(19) 0.0144(19)
C22 0.064(3) 0.073(4) 0.120(5) 0.076(4) 0.018(3) 0.005(3)
C23 0.033(2) 0.031(2) 0.030(2) 0.0166(19) 0.0153(17) 0.0053(17)
C24 0.038(2) 0.030(2) 0.033(2) 0.0173(19) 0.0167(18) 0.0087(17)
C25 0.036(2) 0.041(2) 0.034(2) 0.022(2) 0.0104(18) 0.0061(18)
C26 0.044(2) 0.039(2) 0.031(2) 0.013(2) 0.0038(19) -0.001(2)
C27 0.050(3) 0.030(2) 0.033(2) 0.008(2) 0.012(2) 0.0051(19)
C28 0.037(2) 0.035(2) 0.034(2) 0.014(2) 0.0164(19) 0.0086(18)
C29 0.033(2) 0.030(2) 0.024(2) 0.0092(17) 0.0134(16) 0.0105(17)
C30 0.032(2) 0.033(2) 0.037(2) 0.0123(18) 0.0174(18) 0.0125(17)
C31 0.053(3) 0.034(2) 0.037(2) 0.017(2) 0.019(2) 0.016(2)
C32 0.048(3) 0.055(3) 0.047(3) 0.031(2) 0.023(2) 0.028(2)
C33 0.034(2) 0.058(3) 0.057(3) 0.033(2) 0.020(2) 0.017(2)
C34 0.032(2) 0.042(2) 0.040(2) 0.022(2) 0.0159(18) 0.0112(18)
C36 0.033(2) 0.030(2) 0.049(3) 0.016(2) 0.0149(19) 0.0054(18)
C37 0.045(3) 0.040(3) 0.072(3) 0.033(3) 0.022(2) 0.011(2)
C38 0.045(3) 0.028(2) 0.084(4) 0.020(3) 0.022(3) 0.006(2)
C39 0.037(2) 0.037(2) 0.060(3) 0.005(2) 0.016(2) 0.000(2)
C40 0.037(2) 0.038(2) 0.043(3) 0.012(2) 0.017(2) 0.0036(19)
C41 0.027(2) 0.026(2) 0.038(2) 0.0097(19) 0.0138(18) 0.0071(16)
C42 0.028(2) 0.0250(19) 0.029(2) 0.0118(17) 0.0104(16) 0.0070(16)
C43 0.031(2) 0.030(2) 0.029(2) 0.0120(18) 0.0101(17) 0.0088(17)
C44 0.038(2) 0.032(2) 0.033(2) 0.0173(18) 0.0155(18) 0.0106(17)
C45 0.032(2) 0.038(2) 0.048(3) 0.022(2) 0.0196(19) 0.0092(18)
C46 0.032(2) 0.030(2) 0.036(2) 0.0146(19) 0.0066(18) 0.0035(17)
C47 0.038(2) 0.030(2) 0.028(2) 0.0147(18) 0.0116(18) 0.0119(17)
C48 0.043(3) 0.056(3) 0.048(3) 0.028(2) 0.025(2) 0.016(2)
C49 0.035(2) 0.056(3) 0.049(3) 0.023(3) 0.013(2) 0.012(2)
C50 0.031(2) 0.029(2) 0.028(2) 0.0127(18) 0.0119(16) 0.0087(16)
C51 0.044(2) 0.032(2) 0.033(2) 0.017(2) 0.0155(18) 0.0079(18)
C52 0.057(3) 0.033(2) 0.031(2) 0.011(2) 0.012(2) 0.011(2)
C53 0.066(3) 0.045(3) 0.027(2) 0.015(2) 0.020(2) 0.024(2)
C54 0.054(3) 0.037(2) 0.035(2) 0.021(2) 0.026(2) 0.021(2)
C55 0.037(2) 0.029(2) 0.032(2) 0.0145(18) 0.0154(17) 0.0130(17)
C56 0.134(6) 0.040(3) 0.046(4) 0.015(3) 0.024(3) 0.007(3)
C57 0.096(4) 0.040(3) 0.045(3) 0.023(2) 0.038(3) 0.026(3)
C58 0.035(2) 0.027(2) 0.023(2) 0.0118(17) 0.0115(16) 0.0068(16)
C59 0.037(2) 0.028(2) 0.033(2) 0.0152(18) 0.0155(17) 0.0070(17)
C60 0.032(2) 0.030(2) 0.040(2) 0.0161(19) 0.0145(18) 0.0089(17)
C61 0.037(2) 0.038(2) 0.044(2) 0.020(2) 0.0174(19) 0.0180(19)
C62 0.040(2) 0.025(2) 0.024(2) 0.0085(17) 0.0105(17) 0.0081(17)
C63 0.029(2) 0.033(2) 0.025(2) 0.0118(17) 0.0111(16) 0.0054(17)
C64 0.033(2) 0.045(3) 0.079(4) 0.033(3) 0.021(2) 0.013(2)
C65 0.046(3) 0.027(2) 0.040(3) 0.014(2) 0.013(2) 0.0104(19)
C66 0.0282(19) 0.028(2) 0.025(2) 0.0133(17) 0.0115(16) 0.0072(16)
C67 0.037(2) 0.035(2) 0.024(2) 0.0128(19) 0.0140(17) 0.0110(18)
C68 0.048(2) 0.031(2) 0.035(2) 0.013(2) 0.021(2) 0.0147(19)
C69 0.059(3) 0.026(2) 0.029(2) 0.0024(19) 0.019(2) 0.007(2)
C70 0.044(2) 0.032(2) 0.024(2) 0.0108(19) 0.0072(17) 0.0060(18)
C71 0.034(2) 0.032(2) 0.029(2) 0.0154(19) 0.0104(17) 0.0067(17)
C72 0.068(3) 0.039(3) 0.040(3) 0.014(2) 0.025(2) 0.025(2)
C73 0.074(3) 0.043(3) 0.036(3) 0.013(2) 0.007(2) 0.009(3)
B1 0.031(2) 0.027(2) 0.029(2) 0.013(2) 0.0112(19) 0.0073(18)

_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
P1 C9 1.798(4) . ?
P1 C16 1.798(4) . ?
P1 C2 1.804(4) . ?
P1 C1 1.931(3) . ?
F1 C48 1.332(4) . ?
F2 C48 1.345(5) . ?
F3 C48 1.334(5) . ?
F4 C49 1.320(5) . ?
F5 C49 1.302(5) . ?
F6 C49 1.312(5) . ?
F7 C56 1.285(6) . ?
F8 C56 1.279(7) . ?
F9 C56 1.320(8) . ?
F10 C57 1.306(5) . ?
F11 C57 1.241(6) . ?
F12 C57 1.363(6) . ?
F13 C64 1.323(5) . ?
F14 C64 1.305(5) . ?
F15 C64 1.311(5) . ?
F16 C65 1.292(5) . ?
F17 C65 1.276(5) . ?
F18 C65 1.278(5) . ?
F19 C72 1.334(5) . ?
F20 C72 1.315(5) . ?
F21 C72 1.314(5) . ?
F22 C73 1.342(5) . ?
F23 C73 1.342(5) . ?
F24 C73 1.307(5) . ?
O1 C5 1.357(4) . ?
O1 C8 1.429(5) . ?
O2 C12 1.360(4) . ?
O2 C15 1.424(5) . ?
O3 C19 1.358(5) . ?
O3 C22 1.418(5) . ?
C1 C41 1.550(5) . ?
C1 C23 1.550(5) . ?
C1 C29 1.554(5) . ?
C2 C3 1.387(5) . ?
C2 C7 1.401(5) . ?
C3 C4 1.373(5) . ?
C4 C5 1.395(5) . ?
C5 C6 1.387(5) . ?
C6 C7 1.367(5) . ?
C9 C14 1.392(5) . ?
C9 C10 1.393(5) . ?
C10 C11 1.367(5) . ?
C11 C12 1.390(6) . ?
C12 C13 1.384(5) . ?
C13 C14 1.376(5) . ?
C16 C21 1.392(5) . ?
C16 C17 1.402(5) . ?
C17 C18 1.365(5) . ?
C18 C19 1.386(6) . ?
C19 C20 1.381(6) . ?
C20 C21 1.386(5) . ?
C23 C28 1.392(5) . ?
C23 C24 1.398(5) . ?
C24 C25 1.383(5) . ?
C25 C26 1.386(5) . ?
C26 C27 1.374(6) . ?
C27 C28 1.386(5) . ?
C29 C34 1.392(5) . ?
C29 C30 1.402(5) . ?
C30 C31 1.389(5) . ?
C31 C32 1.370(6) . ?
C32 C33 1.379(6) . ?
C33 C34 1.387(5) . ?
C36 C41 1.383(5) . ?
C36 C37 1.389(5) . ?
C37 C38 1.376(6) . ?
C38 C39 1.364(6) . ?
C39 C40 1.386(6) . ?
C40 C41 1.397(5) . ?
C42 C47 1.388(5) . ?
C42 C43 1.411(5) . ?
C42 B1 1.649(5) . ?
C43 C44 1.381(5) . ?
C44 C45 1.389(5) . ?
C44 C48 1.492(5) . ?
C45 C46 1.368(5) . ?
C46 C47 1.388(5) . ?
C46 C49 1.496(5) . ?
C50 C55 1.395(5) . ?
C50 C51 1.410(5) . ?
C50 B1 1.637(5) . ?
C51 C52 1.373(5) . ?
C52 C53 1.386(5) . ?
C52 C56 1.483(6) . ?
C53 C54 1.371(5) . ?
C54 C55 1.398(5) . ?
C54 C57 1.475(6) . ?
C58 C63 1.399(5) . ?
C58 C59 1.404(5) . ?
C58 B1 1.632(5) . ?
C59 C60 1.384(5) . ?
C60 C61 1.389(5) . ?
C60 C64 1.483(5) . ?
C61 C62 1.379(5) . ?
C62 C63 1.384(5) . ?
C62 C65 1.477(5) . ?
C66 C67 1.392(5) . ?
C66 C71 1.401(5) . ? 
C66 B1 1.652(5) . ?
C67 C68 1.390(5) . ?
C68 C69 1.387(5) . ?
C68 C72 1.489(6) . ?
C69 C70 1.371(5) . ?
C70 C71 1.382(5) . ?
C70 C73 1.478(6) . ?

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
C9 P1 C16 108.05(16) . . ?
C9 P1 C2 107.03(17) . . ?
C16 P1 C2 106.19(17) . . ?
C9 P1 C1 109.63(16) . . ?
C16 P1 C1 111.37(16) . . ?
C2 P1 C1 114.29(16) . . ?
C5 O1 C8 118.2(3) . . ?
C12 O2 C15 118.3(3) . . ?
C19 O3 C22 117.9(4) . . ?
C41 C1 C23 112.2(3) . . ?
C41 C1 C29 110.6(3) . . ?
C23 C1 C29 110.6(3) . . ?
C41 C1 P1 108.2(2) . . ?
C23 C1 P1 104.9(2) . . ?
C29 C1 P1 110.1(2) . . ?
C3 C2 C7 118.0(3) . . ?
C3 C2 P1 124.4(3) . . ?
C7 C2 P1 117.3(3) . . ?
C4 C3 C2 121.6(3) . . ?
C3 C4 C5 119.7(3) . . ?
O1 C5 C6 116.0(3) . . ?
O1 C5 C4 124.7(3) . . ?
C6 C5 C4 119.3(3) . . ?
C7 C6 C5 120.6(3) . . ?
C6 C7 C2 120.9(3) . . ?
C14 C9 C10 117.9(3) . . ?
C14 C9 P1 120.9(3) . . ?
C10 C9 P1 121.2(3) . . ?
C11 C10 C9 120.8(4) . . ?
C10 C11 C12 120.6(4) . . ?
O2 C12 C13 125.1(4) . . ?
O2 C12 C11 115.3(3) . . ?
C13 C12 C11 119.5(3) . . ?
C14 C13 C12 119.5(4) . . ?
C13 C14 C9 121.7(3) . . ?
C21 C16 C17 117.3(3) . . ?
C21 C16 P1 119.5(3) . . ?
C17 C16 P1 123.1(3) . . ?
C18 C17 C16 121.3(4) . . ?
C17 C18 C19 120.7(4) . . ?
O3 C19 C20 124.9(4) . . ?
O3 C19 C18 115.7(4) . . ?
C20 C19 C18 119.4(4) . . ?
C19 C20 C21 119.8(4) . . ?
C20 C21 C16 121.5(4) . . ?
C28 C23 C24 117.3(3) . . ?
C28 C23 C1 121.6(3) . . ?
C24 C23 C1 121.1(3) . . ?
C25 C24 C23 121.4(3) . . ?
C24 C25 C26 120.2(4) . . ?
C27 C26 C25 119.2(4) . . ?
C26 C27 C28 120.8(4) . . ?
C27 C28 C23 121.1(4) . . ?
C34 C29 C30 117.4(3) . . ?
C34 C29 C1 120.4(3) . . ?
C30 C29 C1 122.0(3) . . ?
C31 C30 C29 120.9(3) . . ?
C32 C31 C30 120.4(4) . . ?
C31 C32 C33 119.8(4) . . ?
C32 C33 C34 120.1(4) . . ?
C33 C34 C29 121.3(4) . . ?
C41 C36 C37 121.2(4) . . ?
C38 C37 C36 120.5(4) . . ?
C39 C38 C37 119.0(4) . . ?
C38 C39 C40 121.1(4) . . ?
C39 C40 C41 120.7(4) . . ?
C36 C41 C40 117.4(3) . . ?
C36 C41 C1 122.1(3) . . ?
C40 C41 C1 120.4(3) . . ?
C47 C42 C43 115.7(3) . . ?
C47 C42 B1 124.5(3) . . ?
C43 C42 B1 119.4(3) . . ?
C44 C43 C42 121.9(3) . . ?
C43 C44 C45 120.7(3) . . ?
C43 C44 C48 120.0(3) . . ?
C45 C44 C48 119.3(3) . . ?
C46 C45 C44 118.3(3) . . ?
C45 C46 C47 121.2(3) . . ?
C45 C46 C49 119.9(3) . . ?
C47 C46 C49 118.9(3) . . ?
C46 C47 C42 122.2(3) . . ?
F1 C48 F3 105.6(3) . . ?
F1 C48 F2 105.9(3) . . ?
F3 C48 F2 105.9(3) . . ?
F1 C48 C44 113.2(3) . . ?
F3 C48 C44 112.9(4) . . ?
F2 C48 C44 112.6(3) . . ?
F5 C49 F6 105.3(4) . . ?
F5 C49 F4 105.8(4) . . ?
F6 C49 F4 104.2(4) . . ?
F5 C49 C46 113.8(4) . . ?
F6 C49 C46 113.6(4) . . ?
F4 C49 C46 113.2(4) . . ?
C55 C50 C51 115.1(3) . . ?
C55 C50 B1 127.9(3) . . ?
C51 C50 B1 116.9(3) . . ?
C52 C51 C50 123.1(3) . . ?
C51 C52 C53 120.0(4) . . ?
C51 C52 C56 119.8(4) . . ?
C53 C52 C56 120.2(4) . . ?
C54 C53 C52 119.0(4) . . ?
C53 C54 C55 120.6(3) . . ?
C53 C54 C57 118.9(4) . . ?
C55 C54 C57 120.5(4) . . ?
C50 C55 C54 122.1(3) . . ?
F8 C56 F7 107.6(6) . . ?
F8 C56 F9 103.1(6) . . ?
F7 C56 F9 103.2(5) . . ?
F8 C56 C52 113.6(5) . . ?
F7 C56 C52 117.1(4) . . ?
F9 C56 C52 110.8(5) . . ?
F11 C57 F10 109.9(5) . . ?
F11 C57 F12 104.2(5) . . ?
F10 C57 F12 98.3(4) . . ?
F11 C57 C54 115.7(4) . . ?
F10 C57 C54 114.9(4) . . ?
F12 C57 C54 111.8(4) . . ?
C63 C58 C59 115.0(3) . . ?
C63 C58 B1 124.6(3) . . ?
C59 C58 B1 120.2(3) . . ?
C60 C59 C58 122.6(3) . . ?
C59 C60 C61 120.5(3) . . ?
C59 C60 C64 120.5(3) . . ?
C61 C60 C64 118.9(3) . . ?
C62 C61 C60 118.3(3) . . ?
C61 C62 C63 120.7(3) . . ?
C61 C62 C65 119.0(3) . . ?
C63 C62 C65 120.3(3) . . ?
C62 C63 C58 122.8(3) . . ?
F14 C64 F15 105.1(4) . . ?
F14 C64 F13 106.2(4) . . ?
F15 C64 F13 103.1(4) . . ?
F14 C64 C60 114.3(4) . . ?
F15 C64 C60 113.7(4) . . ?
F13 C64 C60 113.5(4) . . ?
F17 C65 F18 104.0(4) . . ?
F17 C65 F16 104.5(4) . . ?
F18 C65 F16 102.7(4) . . ?
F17 C65 C62 116.0(3) . . ?
F18 C65 C62 113.4(4) . . ?
F16 C65 C62 114.7(3) . . ?
C67 C66 C71 115.2(3) . . ?
C67 C66 B1 122.8(3) . . ?
C71 C66 B1 121.2(3) . . ?
C68 C67 C66 122.7(3) . . ?
C69 C68 C67 120.0(3) . . ?
C69 C68 C72 118.4(3) . . ?
C67 C68 C72 121.7(4) . . ?
C70 C69 C68 118.7(3) . . ?
C69 C70 C71 120.8(3) . . ?
C69 C70 C73 118.6(4) . . ?
C71 C70 C73 120.6(4) . . ?
C70 C71 C66 122.6(3) . . ?
F21 C72 F20 106.9(4) . . ?
F21 C72 F19 104.1(4) . . ?
F20 C72 F19 104.8(4) . . ?
F21 C72 C68 114.4(4) . . ?
F20 C72 C68 113.0(4) . . ?
F19 C72 C68 112.7(3) . . ?
F24 C73 F23 107.9(4) . . ?
F24 C73 F22 105.5(4) . . ?
F23 C73 F22 100.9(4) . . ?
F24 C73 C70 113.2(4) . . ?
F23 C73 C70 114.2(4) . . ?
F22 C73 C70 114.0(4) . . ?
C58 B1 C50 105.1(3) . . ?
C58 B1 C42 112.0(3) . . ?
C50 B1 C42 109.2(3) . . ?
C58 B1 C66 111.8(3) . . ?
C50 B1 C66 116.4(3) . . ?
C42 B1 C66 102.5(3) . . ?

loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
P1 C1 C23 C24 -62.3(4) . . . . ?
P1 C1 C23 C28 117.1(3) . . . . ?
P1 C1 C29 C30 -48.7(4) . . . . ?
P1 C1 C29 C34 136.3(3) . . . . ?
P1 C1 C41 C36 123.5(3) . . . . ?
P1 C1 C41 C40 -59.7(4) . . . . ?

_refine_diff_density_max    0.748
_refine_diff_density_min   -0.604
_refine_diff_density_rms    0.059



data_ccd270

_audit_creation_method SHELXL-97

#Manuscript 0/018P
#Compound 1

_publ_contact_author_name
;
Gregory J. Kubas
;
_publ_contact_author_address
;
Chemistry Division
MS J514
Los Alamos National Laboratory
Los Alamos, NM 87545 USA
;
_publ_requested_journal 'Chemical Communications'
_publ_section_title
;
Triphenylmethyl Tris(p-methoxyphenyl)phosphonium
Cation: A Structurally Characterized Phosphomium
Analog of Hexaphenylethane
;
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C58 H40 B Cl4 F24 O3 P'
_chemical_formula_weight 1424.48
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'
'B' 'B' 0.0013 0.0007
'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 monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.1573(7)
_cell_length_b 25.790(2)
_cell_length_c 17.873(1)
_cell_angle_alpha 90.00
_cell_angle_beta 108.646(1)
_cell_angle_gamma 90.00
_cell_volume 6183.3(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description irregular
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.530
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2864
_exptl_absorpt_coefficient_mu 0.333
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.93
_exptl_absorpt_correction_T_max 0.95
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(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 'Bruker P4/CCD'
_diffrn_measurement_method '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 22661
_diffrn_reflns_av_R_equivalents 0.0280
_diffrn_reflns_av_sigmaI/netI 0.0344
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 1.44
_diffrn_reflns_theta_max 23.36
_reflns_number_total 8419
_reflns_number_gt 6578
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART 4.210 (Bruker, 1996)'
_computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)'
_computing_data_reduction 'SAINT 4.05 (Bruker, 1996)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics 'SHELXTL NT 5.10 (Bruker, 1997)'
_computing_publication_material 'SHELXTL NT 5.10 (Bruker, 1997)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^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 noref
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8419
_refine_ls_number_parameters 973
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0854
_refine_ls_R_factor_gt 0.0685
_refine_ls_wR_factor_ref 0.2149
_refine_ls_wR_factor_gt 0.2022
_refine_ls_goodness_of_fit_ref 1.513
_refine_ls_restrained_S_all 1.513
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.24565(7) 0.06376(4) 0.76210(5) 0.0396(3) Uani 1 1 d . . .
O1 O 0.15836(19) 0.02453(10) 0.73254(15) 0.0485(7) Uani 1 1 d . . .
O2 O 0.19895(19) 0.11638(9) 0.77426(15) 0.0464(6) Uani 1 1 d . . .
O3 O 0.28930(19) 0.07179(10) 0.69374(14) 0.0497(7) Uani 1 1 d . . .
B1 B 0.1649(3) 0.25151(14) 1.1691(2) 0.0320(9) Uani 1 1 d . . .
Cl4 Cl -0.0807(2) 0.10562(9) 1.32981(14) 0.1550(9) Uani 1 1 d . . .
Cl3 Cl 0.1213(2) 0.07134(13) 1.3774(2) 0.2021(14) Uani 1 1 d . . .
C1 C 0.0835(3) 0.04145(17) 0.6573(2) 0.0566(11) Uani 1 1 d . . .
H1A H 0.0179 0.0428 0.6635 0.068 Uiso 1 1 calc R . .
H1B H 0.0812 0.0168 0.6158 0.068 Uiso 1 1 calc R . .
C2 C 0.1196(3) 0.13298(16) 0.7011(2) 0.0559(11) Uani 1 1 d . . .
H2A H 0.1348 0.1673 0.6859 0.067 Uiso 1 1 calc R . .
H2B H 0.0562 0.1347 0.7111 0.067 Uiso 1 1 calc R . .
C3 C 0.2138(3) 0.09195(18) 0.6214(2) 0.0589(12) Uani 1 1 d . . .
H3A H 0.2094 0.0692 0.5772 0.071 Uiso 1 1 calc R . .
H3B H 0.2333 0.1261 0.6090 0.071 Uiso 1 1 calc R . .
C4 C 0.1119(3) 0.09507(16) 0.6347(2) 0.0537(11) Uani 1 1 d . . .
C5 C 0.0327(4) 0.1134(2) 0.5582(3) 0.0770(15) Uani 1 1 d . . .
H5A H -0.0310 0.1154 0.5664 0.115 Uiso 1 1 calc R . .
H5B H 0.0291 0.0892 0.5165 0.115 Uiso 1 1 calc R . .
H5C H 0.0507 0.1470 0.5440 0.115 Uiso 1 1 calc R . .
C6 C 0.3388(3) 0.04073(13) 0.8517(2) 0.0371(8) Uani 1 1 d . . .
C7 C 0.3481(3) -0.01854(13) 0.8430(2) 0.0388(8) Uani 1 1 d . . .
C8 C 0.3569(3) -0.03979(16) 0.7741(2) 0.0562(11) Uani 1 1 d . . .
H8A H 0.3530 -0.0185 0.7313 0.067 Uiso 1 1 calc R . .
C9 C 0.3716(4) -0.09261(17) 0.7691(3) 0.0650(12) Uani 1 1 d . . .
H9A H 0.3759 -0.1067 0.7223 0.078 Uiso 1 1 calc R . .
C10 C 0.3797(3) -0.12423(16) 0.8323(3) 0.0597(12) Uani 1 1 d . . .
H10A H 0.3906 -0.1596 0.8290 0.072 Uiso 1 1 calc R . .
C11 C 0.3717(3) -0.10344(15) 0.9003(3) 0.0529(11) Uani 1 1 d . . .
H11A H 0.3778 -0.1249 0.9434 0.064 Uiso 1 1 calc R . .
C12 C 0.3546(3) -0.05089(14) 0.9064(2) 0.0445(9) Uani 1 1 d . . .
H12A H 0.3476 -0.0375 0.9526 0.053 Uiso 1 1 calc R . .
C13 C 0.3003(3) 0.05467(13) 0.9209(2) 0.0378(8) Uani 1 1 d . . .
C14 C 0.3616(3) 0.07755(15) 0.9890(2) 0.0467(9) Uani 1 1 d . . .
H14A H 0.4266 0.0863 0.9926 0.056 Uiso 1 1 calc R . .
C15 C 0.3276(4) 0.08765(17) 1.0515(3) 0.0587(11) Uani 1 1 d . . .
H15A H 0.3695 0.1037 1.0965 0.070 Uiso 1 1 calc R . .
C16 C 0.2323(4) 0.07427(17) 1.0484(3) 0.0614(12) Uani 1 1 d . . .
H16A H 0.2099 0.0807 1.0911 0.074 Uiso 1 1 calc R . .
C17 C 0.1705(3) 0.05104(18) 0.9808(3) 0.0608(12) Uani 1 1 d . . .
H17A H 0.1058 0.0420 0.9776 0.073 Uiso 1 1 calc R . .
C18 C 0.2043(3) 0.04128(15) 0.9182(2) 0.0503(10) Uani 1 1 d . . .
H18A H 0.1621 0.0254 0.8731 0.060 Uiso 1 1 calc R . .
C19 C 0.4380(3) 0.06865(14) 0.8582(2) 0.0385(8) Uani 1 1 d . . .
C20 C 0.5253(3) 0.04076(15) 0.8686(2) 0.0445(9) Uani 1 1 d . . .
H20A H 0.5240 0.0047 0.8692 0.053 Uiso 1 1 calc R . .
C21 C 0.6138(3) 0.06629(17) 0.8780(2) 0.0549(11) Uani 1 1 d . . .
H21A H 0.6720 0.0473 0.8852 0.066 Uiso 1 1 calc R . .
C22 C 0.6169(3) 0.11985(17) 0.8766(2) 0.0540(11) Uani 1 1 d . . .
H22A H 0.6769 0.1369 0.8831 0.065 Uiso 1 1 calc R . .
C23 C 0.5312(3) 0.14769(16) 0.8657(2) 0.0528(11) Uani 1 1 d . . .
H23A H 0.5330 0.1837 0.8646 0.063 Uiso 1 1 calc R . .
C24 C 0.4421(3) 0.12244(14) 0.8564(2) 0.0447(9) Uani 1 1 d . . .
H24A H 0.3842 0.1417 0.8488 0.054 Uiso 1 1 calc R . .
C25 C 0.2347(2) 0.22137(12) 1.24796(19) 0.0307(8) Uani 1 1 d . . .
C26 C 0.2840(3) 0.17470(12) 1.2460(2) 0.0366(8) Uani 1 1 d . . .
H26A H 0.2871 0.1626 1.1978 0.044 Uiso 1 1 calc R . .
C27 C 0.3286(3) 0.14569(13) 1.3137(2) 0.0405(9) Uani 1 1 d . A .
C28 C 0.3254(3) 0.16190(14) 1.3861(2) 0.0438(9) Uani 1 1 d . . .
H28A H 0.3551 0.1425 1.4314 0.053 Uiso 1 1 calc R . .
C29 C 0.2769(3) 0.20769(13) 1.3900(2) 0.0393(9) Uani 1 1 d . B .
C30 C 0.2330(3) 0.23670(12) 1.32258(19) 0.0337(8) Uani 1 1 d . . .
H30A H 0.2012 0.2675 1.3271 0.040 Uiso 1 1 calc R . .
C31 C 0.3776(4) 0.09519(18) 1.3077(3) 0.0616(13) Uani 1 1 d . . .
C32 C 0.2690(4) 0.22575(18) 1.4679(2) 0.0590(12) Uani 1 1 d . . .
C33 C 0.0552(2) 0.22565(12) 1.15758(18) 0.0299(8) Uani 1 1 d . . .
C34 C -0.0136(3) 0.24614(13) 1.19005(19) 0.0336(8) Uani 1 1 d . . .
H34A H 0.0000 0.2778 1.2163 0.040 Uiso 1 1 calc R . .
C35 C -0.1023(3) 0.22085(14) 1.1846(2) 0.0369(8) Uani 1 1 d . C .
C36 C -0.1243(3) 0.17344(14) 1.1477(2) 0.0402(9) Uani 1 1 d . . .
H36A H -0.1835 0.1565 1.1443 0.048 Uiso 1 1 calc R . .
C37 C -0.0569(3) 0.15151(13) 1.1160(2) 0.0380(8) Uani 1 1 d . D .
C38 C 0.0301(3) 0.17761(13) 1.1205(2) 0.0373(8) Uani 1 1 d . . .
H38A H 0.0739 0.1625 1.0977 0.045 Uiso 1 1 calc R . .
C39 C -0.1748(4) 0.24544(17) 1.2188(3) 0.0585(12) Uani 1 1 d . . .
C40 C -0.0763(4) 0.09967(19) 1.0782(3) 0.0653(13) Uani 1 1 d . . .
C41 C 0.1668(3) 0.31503(12) 1.18237(18) 0.0330(8) Uani 1 1 d . . .
C42 C 0.2520(3) 0.34097(13) 1.2268(2) 0.0373(8) Uani 1 1 d . . .
H42A H 0.3085 0.3218 1.2532 0.045 Uiso 1 1 calc R . .
C43 C 0.2557(3) 0.39483(13) 1.2331(2) 0.0408(9) Uani 1 1 d . E .
C44 C 0.1722(3) 0.42456(13) 1.1955(2) 0.0424(9) Uani 1 1 d . . .
H44A H 0.1735 0.4605 1.2008 0.051 Uiso 1 1 calc R . .
C45 C 0.0875(3) 0.39948(13) 1.1503(2) 0.0376(8) Uani 1 1 d . . .
C46 C 0.0850(3) 0.34636(12) 1.14310(19) 0.0346(8) Uani 1 1 d . . .
H46A H 0.0270 0.3307 1.1111 0.041 Uiso 1 1 calc R . .
C47 C 0.3502(4) 0.42102(17) 1.2812(3) 0.0588(12) Uani 1 1 d . . .
C48 C -0.0017(3) 0.43119(14) 1.1080(2) 0.0488(10) Uani 1 1 d . . .
C49 C 0.1996(3) 0.24361(12) 1.09097(19) 0.0329(8) Uani 1 1 d . . .
C50 C 0.1306(3) 0.24266(13) 1.0148(2) 0.0384(9) Uani 1 1 d . . .
H50A H 0.0630 0.2434 1.0091 0.046 Uiso 1 1 calc R . .
C51 C 0.1591(3) 0.24061(15) 0.9471(2) 0.0448(9) Uani 1 1 d . F .
C52 C 0.2586(3) 0.23995(14) 0.9529(2) 0.0452(10) Uani 1 1 d . . .
H52A H 0.2780 0.2383 0.9079 0.054 Uiso 1 1 calc R . .
C53 C 0.3292(3) 0.24186(13) 1.0276(2) 0.0376(9) Uani 1 1 d . . .
C54 C 0.3000(3) 0.24354(12) 1.0947(2) 0.0341(8) Uani 1 1 d . . .
H54A H 0.3489 0.2447 1.1439 0.041 Uiso 1 1 calc R . .
C55 C 0.0812(4) 0.2404(2) 0.8674(3) 0.0708(14) Uani 1 1 d . . .
C56 C 0.4359(3) 0.24065(15) 1.0342(3) 0.0515(10) Uani 1 1 d . . .
C58 C 0.0290(7) 0.1233(4) 1.3341(5) 0.206(6) Uani 1 1 d . . .
H58A H 0.0470 0.1544 1.3661 0.248 Uiso 1 1 calc R . .
H58B H 0.0301 0.1315 1.2814 0.248 Uiso 1 1 calc R . .
C57 C 0.3028(7) -0.0656(4) 0.5156(6) 0.155(3) Uani 1 1 d . . .
F2 F 0.4695(4) 0.0929(2) 1.3576(4) 0.179(3) Uani 1 1 d . A .
F1 F 0.3683(9) 0.0608(3) 1.3595(4) 0.092(3) Uani 0.50 1 d P A 1
F3 F 0.3583(15) 0.0748(5) 1.2435(5) 0.165(9) Uani 0.50 1 d P A 1
F1' F 0.3152(11) 0.0578(3) 1.2890(16) 0.202(9) Uani 0.50 1 d P A 2
F3' F 0.4245(9) 0.0959(4) 1.2580(7) 0.111(4) Uani 0.50 1 d P A 2
F4 F 0.1970(12) 0.1981(5) 1.4881(7) 0.114(4) Uani 0.50 1 d P B 1
F6 F 0.3526(14) 0.2174(7) 1.5238(7) 0.137(7) Uani 0.50 1 d P B 1
F5 F 0.2449(13) 0.2715(4) 1.4722(6) 0.087(4) Uani 0.50 1 d P B 1
F4' F 0.1771(9) 0.2301(8) 1.4662(6) 0.132(7) Uani 0.50 1 d P B 2
F6' F 0.3134(11) 0.1992(5) 1.5282(7) 0.091(6) Uani 0.50 1 d P B 2
F5' F 0.3070(18) 0.2746(6) 1.4821(9) 0.166(9) Uani 0.50 1 d P B 2
F7 F -0.1292(6) 0.2519(4) 1.2994(5) 0.089(3) Uani 0.50 1 d P C 1
F8 F -0.2668(7) 0.2443(4) 1.1666(6) 0.093(4) Uani 0.50 1 d P C 1
F7' F -0.1835(10) 0.2246(6) 1.2788(7) 0.142(5) Uani 0.50 1 d P C 2
F8' F -0.2560(9) 0.2255(5) 1.2080(12) 0.174(9) Uani 0.50 1 d P C 2
F9 F -0.1751(3) 0.29735(13) 1.2131(2) 0.1114(12) Uani 1 1 d . C .
F10 F -0.0145(6) 0.0831(4) 1.0498(9) 0.092(5) Uani 0.50 1 d P D 1
F11 F -0.0893(9) 0.0645(3) 1.1324(6) 0.104(4) Uani 0.50 1 d P D 1
F10' F -0.0548(17) 0.0990(7) 1.0105(11) 0.226(11) Uani 0.50 1 d P D 2
F11' F -0.0227(13) 0.0633(4) 1.1166(11) 0.171(8) Uani 0.50 1 d P D 2
F12 F -0.1678(3) 0.09227(14) 1.0356(3) 0.1195(14) Uani 1 1 d . D .
F13 F 0.3740(11) 0.4070(8) 1.3556(5) 0.110(5) Uani 0.50 1 d P E 1
F14 F 0.4250(6) 0.4110(7) 1.2614(10) 0.095(3) Uani 0.50 1 d P E 1
F15 F 0.3411(10) 0.4723(3) 1.2823(14) 0.130(8) Uani 0.50 1 d P E 1
F14' F 0.4194(12) 0.3900(4) 1.3246(16) 0.144(7) Uani 0.50 1 d P E 2
F13' F 0.3412(8) 0.4554(7) 1.3280(11) 0.108(4) Uani 0.50 1 d P E 2
F15' F 0.3928(15) 0.4450(12) 1.2338(8) 0.165(7) Uani 0.50 1 d P E 2
F16 F -0.0191(2) 0.46980(10) 1.1514(2) 0.0879(9) Uani 1 1 d . . .
F17 F 0.0054(3) 0.45348(15) 1.0438(2) 0.1128(13) Uani 1 1 d . . .
F18 F -0.08664(19) 0.40440(9) 1.08485(17) 0.0751(8) Uani 1 1 d . . .
F19 F 0.0695(16) 0.2899(5) 0.8342(9) 0.144(6) Uani 0.50 1 d P F 1
F20 F 0.1167(14) 0.2426(8) 0.8090(9) 0.104(8) Uani 0.50 1 d P F 1
F21 F -0.0076(9) 0.2291(9) 0.8653(6) 0.101(4) Uani 0.50 1 d P F 1
F19' F 0.0120(16) 0.2690(13) 0.8615(7) 0.174(10) Uani 0.50 1 d P F 2
F20' F 0.1020(15) 0.2142(10) 0.8163(9) 0.124(7) Uani 0.50 1 d P F 2
F21' F 0.0425(16) 0.1899(6) 0.8542(8) 0.145(5) Uani 0.50 1 d P F 2
F22 F 0.4691(2) 0.19385(11) 1.0263(2) 0.1031(11) Uani 1 1 d . . .
F23 F 0.49624(19) 0.25869(13) 1.10194(17) 0.0828(9) Uani 1 1 d . . .
F24 F 0.4563(2) 0.26902(13) 0.97804(18) 0.0865(9) Uani 1 1 d . . .
Cl2 Cl 0.2798(5) -0.12600(13) 0.4959(4) 0.157(2) Uani 0.50 1 d P G 1
Cl1 Cl 0.2169(4) -0.03522(18) 0.5455(4) 0.1533(19) Uani 0.50 1 d P G 1
Cl1' Cl 0.2198(4) -0.02495(18) 0.4693(3) 0.1541(18) Uani 0.50 1 d P G 2
Cl2' Cl 0.2480(5) -0.1203(3) 0.5534(6) 0.251(4) Uani 0.50 1 d P G 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
P1 0.0373(6) 0.0415(5) 0.0407(5) 0.0021(4) 0.0136(4) -0.0044(4)
O1 0.0462(16) 0.0482(15) 0.0483(15) 0.0006(12) 0.0110(12) -0.0102(12)
O2 0.0420(15) 0.0433(14) 0.0528(15) 0.0030(12) 0.0136(12) 0.0026(12)
O3 0.0422(15) 0.0665(17) 0.0431(14) 0.0101(13) 0.0171(12) 0.0013(13)
B1 0.037(2) 0.0280(19) 0.030(2) -0.0024(15) 0.0097(17) -0.0014(16)
Cl4 0.188(2) 0.1396(18) 0.1285(17) 0.0476(14) 0.0384(16) -0.0127(16)
Cl3 0.168(3) 0.207(3) 0.264(4) -0.045(3) 0.115(3) -0.057(2)
C1 0.045(2) 0.066(3) 0.052(2) -0.002(2) 0.005(2) -0.011(2)
C2 0.040(2) 0.053(2) 0.067(3) 0.012(2) 0.007(2) 0.0038(19)
C3 0.063(3) 0.069(3) 0.041(2) 0.015(2) 0.012(2) -0.001(2)
C4 0.045(2) 0.061(3) 0.050(2) 0.009(2) 0.0074(19) -0.004(2)
C5 0.063(3) 0.093(4) 0.060(3) 0.011(3) 0.000(2) -0.002(3)
C6 0.041(2) 0.0338(18) 0.0380(19) 0.0030(15) 0.0148(16) -0.0029(16)
C7 0.036(2) 0.0367(19) 0.046(2) -0.0009(16) 0.0153(16) -0.0032(15)
C8 0.068(3) 0.054(3) 0.051(2) -0.003(2) 0.026(2) -0.001(2)
C9 0.070(3) 0.054(3) 0.075(3) -0.017(2) 0.028(3) 0.002(2)
C10 0.043(2) 0.040(2) 0.098(4) -0.007(2) 0.024(2) -0.0019(18)
C11 0.044(2) 0.040(2) 0.076(3) 0.015(2) 0.020(2) 0.0022(18)
C12 0.038(2) 0.044(2) 0.053(2) 0.0049(18) 0.0167(18) -0.0027(17)
C13 0.041(2) 0.0342(18) 0.043(2) -0.0006(15) 0.0199(17) -0.0016(16)
C14 0.042(2) 0.052(2) 0.048(2) -0.0049(18) 0.0179(18) -0.0055(18)
C15 0.063(3) 0.065(3) 0.052(3) -0.013(2) 0.024(2) -0.009(2)
C16 0.074(3) 0.070(3) 0.052(3) -0.011(2) 0.037(2) -0.004(2)
C17 0.053(3) 0.074(3) 0.067(3) -0.008(2) 0.034(2) -0.008(2)
C18 0.052(3) 0.054(2) 0.051(2) -0.0079(19) 0.025(2) -0.013(2)
C19 0.037(2) 0.046(2) 0.0343(19) 0.0045(15) 0.0133(16) -0.0054(17)
C20 0.046(2) 0.045(2) 0.047(2) 0.0023(17) 0.0218(18) 0.0006(18)
C21 0.042(2) 0.070(3) 0.058(3) 0.006(2) 0.024(2) -0.002(2)
C22 0.044(3) 0.069(3) 0.052(2) 0.005(2) 0.020(2) -0.016(2)
C23 0.057(3) 0.048(2) 0.052(2) 0.0087(18) 0.017(2) -0.013(2)
C24 0.044(2) 0.045(2) 0.045(2) 0.0076(17) 0.0127(18) -0.0060(18)
C25 0.0288(18) 0.0302(17) 0.0334(18) -0.0023(14) 0.0103(15) -0.0024(14)
C26 0.039(2) 0.0339(18) 0.0394(19) -0.0037(15) 0.0164(16) -0.0016(16)
C27 0.039(2) 0.0353(19) 0.048(2) 0.0060(16) 0.0145(17) 0.0079(16)
C28 0.046(2) 0.041(2) 0.039(2) 0.0071(16) 0.0062(17) 0.0068(18)
C29 0.041(2) 0.039(2) 0.0349(19) -0.0010(16) 0.0085(16) -0.0006(17)
C30 0.036(2) 0.0272(17) 0.0362(19) -0.0030(14) 0.0095(15) 0.0010(14)
C31 0.070(3) 0.057(3) 0.054(3) 0.009(2) 0.014(3) 0.030(3)
C32 0.078(4) 0.059(3) 0.033(2) 0.001(2) 0.008(2) 0.013(3)
C33 0.035(2) 0.0285(17) 0.0269(16) 0.0033(14) 0.0102(14) 0.0025(14)
C34 0.039(2) 0.0319(17) 0.0323(18) 0.0004(14) 0.0147(16) -0.0005(15)
C35 0.037(2) 0.042(2) 0.0348(19) -0.0019(15) 0.0156(16) 0.0022(16)
C36 0.032(2) 0.047(2) 0.045(2) -0.0056(17) 0.0154(17) -0.0062(16)
C37 0.034(2) 0.0378(19) 0.044(2) -0.0063(15) 0.0154(17) -0.0045(16)
C38 0.034(2) 0.040(2) 0.0417(19) -0.0047(16) 0.0165(16) 0.0018(16)
C39 0.058(3) 0.051(3) 0.078(3) -0.019(2) 0.038(3) -0.004(2)
C40 0.053(3) 0.057(3) 0.089(4) -0.028(3) 0.027(3) -0.025(3)
C41 0.039(2) 0.0334(18) 0.0310(17) -0.0006(14) 0.0173(16) -0.0010(15)
C42 0.038(2) 0.0340(18) 0.043(2) -0.0043(15) 0.0170(17) -0.0036(16)
C43 0.042(2) 0.0355(19) 0.050(2) -0.0063(16) 0.0213(18) -0.0091(17)
C44 0.055(3) 0.0282(18) 0.047(2) 0.0008(16) 0.0208(19) -0.0017(17)
C45 0.044(2) 0.0326(19) 0.042(2) 0.0036(15) 0.0215(17) 0.0000(16)
C46 0.039(2) 0.0340(19) 0.0326(18) 0.0022(14) 0.0138(15) -0.0006(15)
C47 0.055(3) 0.044(3) 0.074(3) -0.007(2) 0.015(3) -0.012(2)
C48 0.058(3) 0.0294(19) 0.060(2) 0.0071(18) 0.020(2) 0.0003(19)
C49 0.040(2) 0.0250(16) 0.0347(19) -0.0014(13) 0.0128(16) 0.0000(14)
C50 0.032(2) 0.046(2) 0.038(2) -0.0012(16) 0.0133(16) 0.0023(16)
C51 0.048(3) 0.052(2) 0.037(2) 0.0007(17) 0.0176(18) 0.0014(18)
C52 0.052(3) 0.053(2) 0.039(2) -0.0005(17) 0.0263(19) 0.0023(19)
C53 0.038(2) 0.0349(19) 0.047(2) -0.0006(15) 0.0237(18) 0.0000(15)
C54 0.032(2) 0.0325(18) 0.0378(19) -0.0013(14) 0.0117(16) -0.0017(15)
C55 0.055(3) 0.119(5) 0.038(3) -0.008(3) 0.015(2) 0.000(3)
C56 0.048(3) 0.052(2) 0.061(3) -0.003(2) 0.028(2) -0.002(2)
C58 0.180(9) 0.224(10) 0.126(6) 0.123(7) -0.076(6) -0.102(8)
C57 0.113(6) 0.178(9) 0.193(9) 0.028(7) 0.074(6) 0.019(6)
F2 0.149(5) 0.151(4) 0.191(5) -0.035(4) -0.010(4) 0.094(4)
F1 0.178(10) 0.040(4) 0.077(4) 0.027(3) 0.068(5) 0.050(5)
F3 0.29(2) 0.101(10) 0.046(4) -0.021(5) -0.024(8) 0.143(12)
F1' 0.168(11) 0.034(4) 0.48(3) -0.070(11) 0.210(17) -0.033(6)
F3' 0.156(10) 0.099(7) 0.127(10) 0.037(6) 0.111(9) 0.087(6)
F4 0.153(14) 0.144(9) 0.074(7) -0.019(5) 0.077(9) -0.053(8)
F6 0.113(10) 0.208(19) 0.046(8) -0.048(9) -0.036(6) 0.076(10)
F5 0.171(12) 0.049(6) 0.048(5) 0.004(4) 0.048(7) 0.052(7)
F4' 0.099(8) 0.25(2) 0.052(5) 0.004(9) 0.036(5) 0.077(12)
F6' 0.165(18) 0.083(5) 0.035(5) 0.027(5) 0.047(9) 0.058(7)
F5' 0.33(2) 0.094(9) 0.068(6) -0.042(6) 0.056(13) -0.074(13)
F7 0.077(5) 0.137(7) 0.073(5) -0.052(4) 0.049(4) -0.015(4)
F8 0.034(4) 0.125(8) 0.124(6) -0.011(5) 0.032(4) 0.032(5)
F7' 0.132(10) 0.245(15) 0.095(7) 0.084(9) 0.098(7) 0.110(10)
F8' 0.101(11) 0.141(10) 0.35(2) -0.189(14) 0.165(13) -0.097(9)
F9 0.100(3) 0.082(2) 0.179(4) -0.037(2) 0.083(3) 0.0098(19)
F10 0.055(4) 0.065(5) 0.190(14) -0.084(7) 0.086(7) -0.026(4)
F11 0.189(11) 0.031(4) 0.105(6) -0.011(3) 0.065(8) -0.036(5)
F10' 0.37(3) 0.191(16) 0.189(15) -0.160(13) 0.199(17) -0.180(16)
F11' 0.176(14) 0.055(6) 0.204(17) -0.033(8) -0.049(12) 0.035(9)
F12 0.073(2) 0.102(2) 0.172(4) -0.084(3) 0.022(2) -0.0230(18)
F13 0.097(8) 0.157(15) 0.058(4) -0.019(6) -0.002(5) -0.060(8)
F14 0.035(4) 0.135(10) 0.119(9) -0.047(7) 0.032(6) -0.023(5)
F15 0.080(7) 0.033(3) 0.224(17) -0.006(7) -0.029(11) -0.021(3)
F14' 0.090(9) 0.063(5) 0.202(17) -0.006(9) -0.061(9) -0.015(6)
F13' 0.085(6) 0.102(10) 0.130(9) -0.080(8) 0.026(7) -0.022(8)
F15' 0.112(12) 0.257(19) 0.126(8) 0.007(12) 0.037(9) -0.125(12)
F16 0.0720(19) 0.0587(16) 0.122(2) -0.0230(16) 0.0151(17) 0.0209(14)
F17 0.098(2) 0.142(3) 0.111(2) 0.088(2) 0.051(2) 0.056(2)
F18 0.0526(16) 0.0511(14) 0.108(2) 0.0032(14) 0.0072(14) 0.0067(12)
F19 0.169(13) 0.126(8) 0.087(8) 0.056(7) -0.030(7) 0.001(9)
F20 0.076(6) 0.21(2) 0.034(4) 0.023(9) 0.025(3) 0.003(12)
F21 0.052(5) 0.202(14) 0.045(4) -0.018(8) 0.009(3) -0.025(8)
F19' 0.127(15) 0.29(2) 0.062(7) -0.036(13) -0.025(9) 0.154(16)
F20' 0.121(16) 0.192(17) 0.046(8) -0.040(10) 0.011(7) 0.062(13)
F21' 0.137(11) 0.198(13) 0.066(6) -0.024(7) -0.015(6) -0.074(11)
F22 0.0632(19) 0.0726(19) 0.185(4) -0.022(2) 0.056(2) 0.0129(15)
F23 0.0444(15) 0.132(3) 0.0730(18) -0.0220(16) 0.0209(14) -0.0186(15)
F24 0.0621(18) 0.126(3) 0.0827(19) 0.0170(17) 0.0395(15) -0.0162(16)
Cl2 0.250(6) 0.0531(17) 0.241(6) -0.022(2) 0.181(5) 0.002(2)
Cl1 0.168(4) 0.121(3) 0.203(5) -0.067(3) 0.103(4) -0.003(3)
Cl1' 0.171(4) 0.121(3) 0.145(4) 0.006(3) 0.013(3) 0.013(3)
Cl2' 0.155(5) 0.251(8) 0.258(8) 0.107(7) -0.059(6) -0.046(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
P1 O3 1.549(3) . ?
P1 O1 1.553(3) . ?
P1 O2 1.555(3) . ?
P1 C6 1.818(4) . ?
O1 C1 1.487(5) . ?
O2 C2 1.489(5) . ?
O3 C3 1.483(5) . ?
B1 C49 1.635(5) . ?
B1 C25 1.636(5) . ?
B1 C33 1.642(5) . ?
B1 C41 1.654(5) . ?
Cl4 C58 1.597(10) . ?
Cl3 C58 1.860(11) . ?
C1 C4 1.530(6) . ?
C2 C4 1.514(6) . ?
C3 C4 1.537(6) . ?
C4 C5 1.539(6) . ?
C6 C13 1.546(5) . ?
C6 C7 1.546(5) . ?
C6 C19 1.549(5) . ?
C7 C12 1.385(5) . ?
C7 C8 1.390(5) . ?
C8 C9 1.385(6) . ?
C9 C10 1.368(7) . ?
C10 C11 1.366(6) . ?
C11 C12 1.387(5) . ?
C13 C14 1.380(5) . ?
C13 C18 1.388(5) . ?
C14 C15 1.376(6) . ?
C15 C16 1.376(6) . ?
C16 C17 1.382(6) . ?
C17 C18 1.373(6) . ?
C19 C24 1.389(5) . ?
C19 C20 1.390(5) . ?
C20 C21 1.378(6) . ?
C21 C22 1.382(6) . ?
C22 C23 1.370(6) . ?
C23 C24 1.382(5) . ?
C25 C26 1.397(5) . ?
C25 C30 1.398(5) . ?
C26 C27 1.390(5) . ?
C27 C28 1.375(5) . ?
C27 C31 1.495(5) . ?
C28 C29 1.378(5) . ?
C29 C30 1.386(5) . ?
C29 C32 1.505(6) . ?
C31 F3 1.210(9) . ?
C31 F3' 1.268(10) . ?
C31 F1' 1.276(11) . ?
C31 F1 1.318(8) . ?
C31 F2 1.324(7) . ?
C32 F5 1.237(10) . ?
C32 F6' 1.261(11) . ?
C32 F4' 1.296(12) . ?
C32 F6 1.299(15) . ?
C32 F5' 1.362(14) . ?
C32 F4 1.383(11) . ?
C33 C34 1.388(5) . ?
C33 C38 1.397(5) . ?
C34 C35 1.391(5) . ?
C35 C36 1.377(5) . ?
C35 C39 1.493(6) . ?
C36 C37 1.377(5) . ?
C37 C38 1.384(5) . ?
C37 C40 1.483(6) . ?
C39 F8' 1.216(10) . ?
C39 F7' 1.241(9) . ?
C39 F8 1.338(11) . ?
C39 F9 1.343(5) . ?
C39 F7 1.388(9) . ?
C40 F10 1.221(9) . ?
C40 F11' 1.262(11) . ?
C40 F12 1.290(6) . ?
C40 F10' 1.339(16) . ?
C40 F11 1.382(10) . ?
C41 C42 1.385(5) . ?
C41 C46 1.403(5) . ?
C42 C43 1.393(5) . ?
C43 C44 1.389(5) . ?
C43 C47 1.500(6) . ?
C44 C45 1.374(5) . ?
C45 C46 1.375(5) . ?
C45 C48 1.492(5) . ?
C47 F14 1.246(9) . ?
C47 F13' 1.253(10) . ?
C47 F14' 1.311(11) . ?
C47 F13 1.314(11) . ?
C47 F15 1.331(10) . ?
C47 F15' 1.338(12) . ?
C48 F17 1.316(5) . ?
C48 F16 1.332(5) . ?
C48 F18 1.333(5) . ?
C49 C50 1.399(5) . ?
C49 C54 1.401(5) . ?
C50 C51 1.393(5) . ?
C51 C52 1.379(6) . ?
C51 C55 1.496(6) . ?
C52 C53 1.390(5) . ?
C53 C54 1.389(5) . ?
C53 C56 1.477(6) . ?
C55 F19' 1.205(11) . ?
C55 F20' 1.245(15) . ?
C55 F21 1.280(11) . ?
C55 F20 1.297(14) . ?
C55 F19 1.394(11) . ?
C55 F21' 1.405(12) . ?
C56 F22 1.320(5) . ?
C56 F23 1.323(5) . ?
C56 F24 1.346(5) . ?
C57 Cl1' 1.595(10) . ?
C57 Cl2 1.606(11) . ?
C57 Cl1 1.672(10) . ?
C57 Cl2' 1.838(12) . ?
F2 F1 1.664(11) . ?
F2 F3' 1.690(12) . ?
F7' F8' 1.350(18) . ?
F19 F20 1.53(3) . ?
F20' F21' 1.387(19) . ?
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
O3 P1 O1 107.06(15) . . ?
O3 P1 O2 106.74(15) . . ?
O1 P1 O2 106.76(15) . . ?
O3 P1 C6 112.21(16) . . ?
O1 P1 C6 111.17(15) . . ?
O2 P1 C6 112.53(15) . . ?
C1 O1 P1 112.1(2) . . ?
C2 O2 P1 111.3(2) . . ?
C3 O3 P1 112.1(2) . . ?
C49 B1 C25 114.4(3) . . ?
C49 B1 C33 111.9(3) . . ?
C25 B1 C33 101.6(3) . . ?
C49 B1 C41 104.5(3) . . ?
C25 B1 C41 111.7(3) . . ?
C33 B1 C41 113.1(3) . . ?
O1 C1 C4 109.4(3) . . ?
O2 C2 C4 110.3(3) . . ?
O3 C3 C4 109.5(3) . . ?
C2 C4 C1 109.6(4) . . ?
C2 C4 C3 108.6(3) . . ?
C1 C4 C3 109.4(4) . . ?
C2 C4 C5 110.3(4) . . ?
C1 C4 C5 109.5(3) . . ?
C3 C4 C5 109.4(4) . . ?
C13 C6 C7 111.9(3) . . ?
C13 C6 C19 112.0(3) . . ?
C7 C6 C19 111.3(3) . . ?
C13 C6 P1 106.7(2) . . ?
C7 C6 P1 107.2(2) . . ?
C19 C6 P1 107.5(2) . . ?
C12 C7 C8 119.0(4) . . ?
C12 C7 C6 120.0(3) . . ?
C8 C7 C6 120.8(3) . . ?
C9 C8 C7 120.2(4) . . ?
C10 C9 C8 120.4(4) . . ?
C11 C10 C9 119.5(4) . . ?
C10 C11 C12 121.3(4) . . ?
C7 C12 C11 119.5(4) . . ?
C14 C13 C18 118.0(3) . . ?
C14 C13 C6 121.4(3) . . ?
C18 C13 C6 120.4(3) . . ?
C15 C14 C13 120.8(4) . . ?
C16 C15 C14 120.9(4) . . ?
C15 C16 C17 118.8(4) . . ?
C18 C17 C16 120.3(4) . . ?
C17 C18 C13 121.2(4) . . ?
C24 C19 C20 118.6(3) . . ?
C24 C19 C6 120.4(3) . . ?
C20 C19 C6 121.0(3) . . ?
C21 C20 C19 120.3(4) . . ?
C20 C21 C22 120.5(4) . . ?
C23 C22 C21 119.7(4) . . ?
C22 C23 C24 120.2(4) . . ?
C23 C24 C19 120.7(4) . . ?
C26 C25 C30 115.3(3) . . ?
C26 C25 B1 123.8(3) . . ?
C30 C25 B1 119.8(3) . . ?
C27 C26 C25 122.3(3) . . ?
C28 C27 C26 120.8(3) . . ?
C28 C27 C31 119.2(3) . . ?
C26 C27 C31 119.9(3) . . ?
C27 C28 C29 118.4(3) . . ?
C28 C29 C30 120.7(3) . . ?
C28 C29 C32 119.8(3) . . ?
C30 C29 C32 119.5(3) . . ?
C29 C30 C25 122.5(3) . . ?
F3 C31 F3' 49.7(9) . . ?
F3 C31 F1' 59.8(10) . . ?
F3' C31 F1' 107.5(10) . . ?
F3 C31 F1 109.3(9) . . ?
F3' C31 F1 133.9(6) . . ?
F1' C31 F1 57.4(10) . . ?
F3 C31 F2 119.7(9) . . ?
F3' C31 F2 81.4(7) . . ?
F1' C31 F2 126.3(10) . . ?
F1 C31 F2 78.1(5) . . ?
F3 C31 C27 118.5(5) . . ?
F3' C31 C27 113.4(6) . . ?
F1' C31 C27 112.3(6) . . ?
F1 C31 C27 112.5(5) . . ?
F2 C31 C27 111.6(4) . . ?
F5 C32 F6' 122.4(8) . . ?
F5 C32 F4' 67.9(9) . . ?
F6' C32 F4' 106.8(9) . . ?
F5 C32 F6 108.1(10) . . ?
F6' C32 F6 34.0(9) . . ?
F4' C32 F6 133.8(9) . . ?
F5 C32 F5' 37.5(9) . . ?
F6' C32 F5' 106.5(10) . . ?
F4' C32 F5' 105.0(11) . . ?
F6 C32 F5' 78.5(11) . . ?
F5 C32 F4 103.5(9) . . ?
F6' C32 F4 72.9(9) . . ?
F4' C32 F4 39.9(7) . . ?
F6 C32 F4 106.3(9) . . ?
F5' C32 F4 135.1(10) . . ?
F5 C32 C29 117.1(6) . . ?
F6' C32 C29 117.2(7) . . ?
F4' C32 C29 112.1(6) . . ?
F6 C32 C29 110.0(8) . . ?
F5' C32 C29 108.5(8) . . ?
F4 C32 C29 111.1(6) . . ?
C34 C33 C38 115.5(3) . . ?
C34 C33 B1 123.7(3) . . ?
C38 C33 B1 120.4(3) . . ?
C33 C34 C35 122.1(3) . . ?
C36 C35 C34 120.7(3) . . ?
C36 C35 C39 119.6(3) . . ?
C34 C35 C39 119.7(3) . . ?
C35 C36 C37 118.8(3) . . ?
C36 C37 C38 119.8(3) . . ?
C36 C37 C40 120.4(3) . . ?
C38 C37 C40 119.8(3) . . ?
C37 C38 C33 123.0(3) . . ?
F8' C39 F7' 66.7(10) . . ?
F8' C39 F8 38.7(11) . . ?
F7' C39 F8 104.4(9) . . ?
F8' C39 F9 115.4(9) . . ?
F7' C39 F9 120.0(9) . . ?
F8 C39 F9 89.5(6) . . ?
F8' C39 F7 108.6(10) . . ?
F7' C39 F7 45.3(9) . . ?
F8 C39 F7 138.8(7) . . ?
F9 C39 F7 87.0(5) . . ?
F8' C39 C35 119.6(5) . . ?
F7' C39 C35 116.1(6) . . ?
F8 C39 C35 110.4(6) . . ?
F9 C39 C35 112.2(4) . . ?
F7 C39 C35 108.8(5) . . ?
F10 C40 F11' 65.2(11) . . ?
F10 C40 F12 114.8(7) . . ?
F11' C40 F12 121.8(8) . . ?
F10 C40 F10' 38.7(10) . . ?
F11' C40 F10' 102.2(12) . . ?
F12 C40 F10' 86.5(10) . . ?
F10 C40 F11 109.6(9) . . ?
F11' C40 F11 47.4(10) . . ?
F12 C40 F11 89.0(6) . . ?
F10' C40 F11 138.2(9) . . ?
F10 C40 C37 116.9(5) . . ?
F11' C40 C37 115.5(6) . . ?
F12 C40 C37 114.0(4) . . ?
F10' C40 C37 111.1(8) . . ?
F11 C40 C37 108.6(5) . . ?
C42 C41 C46 115.9(3) . . ?
C42 C41 B1 122.1(3) . . ?
C46 C41 B1 121.7(3) . . ?
C41 C42 C43 122.1(3) . . ?
C44 C43 C42 120.5(3) . . ?
C44 C43 C47 119.6(3) . . ?
C42 C43 C47 119.9(3) . . ?
C45 C44 C43 118.1(3) . . ?
C44 C45 C46 121.0(3) . . ?
C44 C45 C48 118.5(3) . . ?
C46 C45 C48 120.4(3) . . ?
C45 C46 C41 122.3(3) . . ?
F14 C47 F13' 127.9(7) . . ?
F14 C47 F14' 59.9(10) . . ?
F13' C47 F14' 104.7(10) . . ?
F14 C47 F13 105.3(8) . . ?
F13' C47 F13 64.3(8) . . ?
F14' C47 F13 48.1(9) . . ?
F14 C47 F15 107.9(9) . . ?
F13' C47 F15 41.9(7) . . ?
F14' C47 F15 131.1(7) . . ?
F13 C47 F15 104.6(10) . . ?
F14 C47 F15' 47.2(9) . . ?
F13' C47 F15' 105.0(10) . . ?
F14' C47 F15' 104.7(12) . . ?
F13 C47 F15' 138.3(8) . . ?
F15 C47 F15' 67.4(10) . . ?
F14 C47 C43 115.3(5) . . ?
F13' C47 C43 116.0(7) . . ?
F14' C47 C43 115.2(5) . . ?
F13 C47 C43 110.4(5) . . ?
F15 C47 C43 112.5(6) . . ?
F15' C47 C43 110.2(6) . . ?
F17 C48 F16 105.1(3) . . ?
F17 C48 F18 105.6(4) . . ?
F16 C48 F18 104.6(3) . . ?
F17 C48 C45 113.2(4) . . ?
F16 C48 C45 113.5(3) . . ?
F18 C48 C45 114.0(3) . . ?
C50 C49 C54 115.3(3) . . ?
C50 C49 B1 121.8(3) . . ?
C54 C49 B1 122.5(3) . . ?
C51 C50 C49 122.7(3) . . ?
C52 C51 C50 120.5(3) . . ?
C52 C51 C55 119.7(4) . . ?
C50 C51 C55 119.8(4) . . ?
C51 C52 C53 118.4(3) . . ?
C54 C53 C52 120.6(3) . . ?
C54 C53 C56 120.7(3) . . ?
C52 C53 C56 118.6(3) . . ?
C53 C54 C49 122.5(3) . . ?
F19' C55 F20' 130.2(11) . . ?
F19' C55 F21 51.2(12) . . ?
F20' C55 F21 108.3(11) . . ?
F19' C55 F20 114.6(14) . . ?
F20' C55 F20 35.9(11) . . ?
F21 C55 F20 128.1(10) . . ?
F19' C55 F19 54.5(12) . . ?
F20' C55 F19 102.1(10) . . ?
F21 C55 F19 102.4(9) . . ?
F20 C55 F19 69.0(11) . . ?
F19' C55 F21' 106.9(14) . . ?
F20' C55 F21' 62.8(10) . . ?
F21 C55 F21' 57.1(7) . . ?
F20 C55 F21' 97.8(10) . . ?
F19 C55 F21' 142.2(7) . . ?
F19' C55 C51 114.4(7) . . ?
F20' C55 C51 115.1(10) . . ?
F21 C55 C51 116.5(6) . . ?
F20 C55 C51 114.1(9) . . ?
F19 C55 C51 110.7(6) . . ?
F21' C55 C51 107.0(6) . . ?
F22 C56 F23 105.8(4) . . ?
F22 C56 F24 104.3(4) . . ?
F23 C56 F24 105.1(3) . . ?
F22 C56 C53 113.7(3) . . ?
F23 C56 C53 114.3(3) . . ?
F24 C56 C53 112.7(3) . . ?
Cl4 C58 Cl3 110.9(4) . . ?
Cl1' C57 Cl2 117.4(7) . . ?
Cl1' C57 Cl1 50.7(4) . . ?
Cl2 C57 Cl1 114.1(6) . . ?
Cl1' C57 Cl2' 111.6(6) . . ?
Cl2 C57 Cl2' 42.1(4) . . ?
Cl1 C57 Cl2' 78.9(6) . . ?
C31 F2 F1 50.8(4) . . ?
C31 F2 F3' 47.9(4) . . ?
F1 F2 F3' 90.4(5) . . ?
C31 F1 F2 51.1(4) . . ?
C31 F3' F2 50.8(5) . . ?
C39 F7' F8' 55.8(7) . . ?
C39 F8' F7' 57.5(7) . . ?
C55 F19 F20 52.5(7) . . ?
C55 F20 F19 58.5(9) . . ?
C55 F20' F21' 64.2(9) . . ?
F20' F21' C55 53.0(8) . . ?
_refine_diff_density_max 0.976
_refine_diff_density_min -0.780
_refine_diff_density_rms 0.060