# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Lechoslaw Latos-Grazynski'
_publ_contact_author_email       llg@wchuwr.chem.uni.wroc.pl
loop_
_publ_author_name
L.Latos-Grazynski
B.Szyszko
L.Szterenberg

# Attachment '- bs2abs.cif'

data_bs2abs
_database_code_depnum_ccdc_archive 'CCDC 863455'
#TrackingRef '- bs2abs.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'chloropalladium meso-anthriporphyrin'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C54 H34 Cl N3 Pd, 0.4(C6 H14), 0.1(H2 O), 1.15(C H2 Cl2)'
_chemical_formula_sum            'C57.55 H42.10 Cl3.30 N3 O0.10 Pd'
_chemical_formula_weight         1000.63

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   50.222(15)
_cell_length_b                   50.222(15)
_cell_length_c                   9.718(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     21227(11)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18056
_cell_measurement_theta_min      4.1050
_cell_measurement_theta_max      38.5506

_exptl_crystal_description       plates
_exptl_crystal_colour            dark-purple
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9203
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Xcalibur PX with Onyx CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            58940
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.22
_diffrn_reflns_theta_max         30.00
_reflns_number_total             13715
_reflns_number_gt                8722
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13715
_refine_ls_number_parameters     620
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.006
_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
Pd1 Pd 0.722380(4) 0.163279(4) 0.980622(19) 0.01702(6) Uani 1 1 d D . .
N1 N 0.76902(5) 0.18356(5) 0.9912(2) 0.0160(4) Uani 1 1 d . . .
N2 N 0.72023(5) 0.12825(5) 0.8708(2) 0.0181(4) Uani 1 1 d . . .
N3 N 0.67752(5) 0.14864(5) 0.9392(2) 0.0167(4) Uani 1 1 d . . .
Cl1 Cl 0.719736(17) 0.18711(3) 1.18089(11) 0.0199(3) Uani 0.929(7) 1 d P . .
Cl11 Cl 0.7210(3) 0.1774(5) 1.2076(10) 0.031(4) Uiso 0.071(7) 1 d PD . .
C1 C 0.70200(6) 0.21782(6) 0.9099(2) 0.0150(5) Uani 1 1 d . . .
C2 C 0.71999(6) 0.25087(6) 0.9459(2) 0.0156(5) Uani 1 1 d . . .
C3 C 0.70754(6) 0.27026(6) 0.9547(2) 0.0207(6) Uani 1 1 d . . .
H3 H 0.6861 0.2622 0.9418 0.025 Uiso 1 1 calc R . .
C4 C 0.72659(7) 0.30133(6) 0.9824(3) 0.0245(6) Uani 1 1 d . . .
H4 H 0.7182 0.3146 0.9857 0.029 Uiso 1 1 calc R . .
C5 C 0.75768(6) 0.31300(6) 1.0051(2) 0.0221(6) Uani 1 1 d . . .
H5 H 0.7706 0.3343 1.0236 0.027 Uiso 1 1 calc R . .
C6 C 0.77012(6) 0.29388(6) 1.0012(2) 0.0187(5) Uani 1 1 d . . .
H6 H 0.7913 0.3019 1.0207 0.022 Uiso 1 1 calc R . .
C7 C 0.75163(6) 0.26279(6) 0.9686(2) 0.0159(5) Uani 1 1 d . . .
C8 C 0.76354(5) 0.24118(5) 0.9487(2) 0.0151(5) Uani 1 1 d . . .
C9 C 0.74965(6) 0.22181(5) 0.8249(2) 0.0143(5) Uani 1 1 d . . .
C10 C 0.71821(6) 0.20976(6) 0.8047(2) 0.0152(5) Uani 1 1 d . . .
C11 C 0.70423(6) 0.19276(6) 0.6858(2) 0.0182(5) Uani 1 1 d . . .
H11 H 0.6828 0.1844 0.6722 0.022 Uiso 1 1 calc R . .
C12 C 0.72151(6) 0.18810(6) 0.5880(3) 0.0213(6) Uani 1 1 d . . .
H12 H 0.7120 0.1769 0.5066 0.026 Uiso 1 1 calc R . .
C13 C 0.75262(6) 0.19979(6) 0.6087(3) 0.0212(6) Uani 1 1 d . . .
H13 H 0.7644 0.1964 0.5417 0.025 Uiso 1 1 calc R . .
C14 C 0.76678(6) 0.21641(6) 0.7263(2) 0.0180(5) Uani 1 1 d . . .
H14 H 0.7881 0.2242 0.7402 0.022 Uiso 1 1 calc R . .
C15 C 0.78296(6) 0.23809(6) 1.0349(2) 0.0158(5) Uani 1 1 d . . .
C16 C 0.78943(6) 0.21294(6) 1.0207(2) 0.0169(5) Uani 1 1 d . . .
C17 C 0.81993(6) 0.21728(6) 1.0258(2) 0.0197(5) Uani 1 1 d . . .
H17 H 0.8382 0.2357 1.0495 0.024 Uiso 1 1 calc R . .
C18 C 0.81780(6) 0.19024(6) 0.9905(3) 0.0202(5) Uani 1 1 d . . .
H18 H 0.8343 0.1861 0.9840 0.024 Uiso 1 1 calc R . .
C19 C 0.78579(6) 0.16893(6) 0.9647(2) 0.0175(5) Uani 1 1 d . . .
C20 C 0.77416(6) 0.14042(6) 0.9034(2) 0.0178(5) Uani 1 1 d . . .
C21 C 0.74330(6) 0.12135(6) 0.8604(3) 0.0196(5) Uani 1 1 d . . .
C22 C 0.73123(6) 0.09123(6) 0.8063(3) 0.0256(6) Uani 1 1 d . . .
H22 H 0.7425 0.0810 0.7889 0.031 Uiso 1 1 calc R . .
C23 C 0.70054(6) 0.07949(6) 0.7838(3) 0.0258(6) Uani 1 1 d . . .
H23 H 0.6865 0.0599 0.7465 0.031 Uiso 1 1 calc R . .
C24 C 0.69382(6) 0.10277(6) 0.8281(3) 0.0199(5) Uani 1 1 d . . .
C25 C 0.66375(6) 0.09855(6) 0.8379(3) 0.0197(5) Uani 1 1 d . . .
C26 C 0.65628(6) 0.11909(6) 0.8940(2) 0.0181(5) Uani 1 1 d . . .
C27 C 0.62639(6) 0.11628(6) 0.8935(2) 0.0193(5) Uani 1 1 d . . .
H27 H 0.6075 0.0984 0.8706 0.023 Uiso 1 1 calc R . .
C28 C 0.62999(6) 0.14374(6) 0.9314(2) 0.0182(5) Uani 1 1 d . . .
H28 H 0.6141 0.1487 0.9416 0.022 Uiso 1 1 calc R . .
C29 C 0.66236(6) 0.16416(6) 0.9536(2) 0.0156(5) Uani 1 1 d . . .
C30 C 0.67602(6) 0.19741(6) 0.9753(2) 0.0154(5) Uani 1 1 d . . .
C31 C 0.79965(6) 0.26025(6) 1.1514(2) 0.0171(5) Uani 1 1 d . . .
C32 C 0.78570(6) 0.25548(6) 1.2799(3) 0.0222(6) Uani 1 1 d . . .
H32 H 0.7658 0.2383 1.2951 0.027 Uiso 1 1 calc R . .
C33 C 0.80114(7) 0.27611(7) 1.3855(3) 0.0274(6) Uani 1 1 d . . .
H33 H 0.7917 0.2729 1.4732 0.033 Uiso 1 1 calc R . .
C34 C 0.83000(7) 0.30114(6) 1.3653(3) 0.0257(6) Uani 1 1 d . . .
H34 H 0.8403 0.3152 1.4383 0.031 Uiso 1 1 calc R . .
C35 C 0.84388(6) 0.30566(6) 1.2383(3) 0.0246(6) Uani 1 1 d . . .
H35 H 0.8638 0.3229 1.2236 0.029 Uiso 1 1 calc R . .
C36 C 0.82879(6) 0.28512(6) 1.1321(3) 0.0242(6) Uani 1 1 d . . .
H36 H 0.8386 0.2882 1.0452 0.029 Uiso 1 1 calc R . .
C37 C 0.79554(6) 0.12844(6) 0.8761(2) 0.0170(5) Uani 1 1 d . . .
C38 C 0.80347(7) 0.11455(7) 0.9771(3) 0.0274(6) Uani 1 1 d . . .
H38 H 0.7968 0.1142 1.0688 0.033 Uiso 1 1 calc R . .
C39 C 0.82096(7) 0.10112(7) 0.9480(3) 0.0306(7) Uani 1 1 d . . .
H39 H 0.8257 0.0911 1.0186 0.037 Uiso 1 1 calc R . .
C40 C 0.83151(6) 0.10229(6) 0.8164(3) 0.0249(6) Uani 1 1 d . . .
H40 H 0.8436 0.0931 0.7959 0.030 Uiso 1 1 calc R . .
C41 C 0.82456(7) 0.11672(7) 0.7147(3) 0.0288(7) Uani 1 1 d . . .
H41 H 0.8322 0.1178 0.6242 0.035 Uiso 1 1 calc R . .
C42 C 0.80652(7) 0.12975(7) 0.7430(3) 0.0262(6) Uani 1 1 d . . .
H42 H 0.8016 0.1396 0.6718 0.031 Uiso 1 1 calc R . .
C43 C 0.63843(6) 0.06970(6) 0.7759(3) 0.0219(6) Uani 1 1 d . . .
C44 C 0.63815(6) 0.06515(6) 0.6358(3) 0.0268(6) Uani 1 1 d . . .
H44 H 0.6545 0.0800 0.5807 0.032 Uiso 1 1 calc R . .
C45 C 0.61438(7) 0.03927(7) 0.5742(3) 0.0326(7) Uani 1 1 d . . .
H45 H 0.6143 0.0366 0.4774 0.039 Uiso 1 1 calc R . .
C46 C 0.59100(7) 0.01755(7) 0.6537(3) 0.0361(7) Uani 1 1 d . . .
H46 H 0.5747 -0.0003 0.6117 0.043 Uiso 1 1 calc R . .
C47 C 0.61447(7) 0.04765(6) 0.8554(3) 0.0296(7) Uani 1 1 d . . .
H47 H 0.6142 0.0506 0.9519 0.035 Uiso 1 1 calc R . .
C48 C 0.65968(6) 0.20714(6) 1.0751(2) 0.0181(5) Uani 1 1 d . . .
C49 C 0.63250(6) 0.20636(6) 1.0400(3) 0.0239(6) Uani 1 1 d . . .
H49 H 0.6242 0.2000 0.9503 0.029 Uiso 1 1 calc R . .
C50 C 0.61724(7) 0.21475(7) 1.1353(3) 0.0325(7) Uani 1 1 d . . .
H50 H 0.5984 0.2137 1.1107 0.039 Uiso 1 1 calc R . .
C52 C 0.65666(7) 0.22608(7) 1.2994(3) 0.0295(7) Uani 1 1 d . . .
H52 H 0.6653 0.2332 1.3880 0.035 Uiso 1 1 calc R . .
C53 C 0.67186(6) 0.21738(6) 1.2065(3) 0.0223(6) Uani 1 1 d . . .
H53 H 0.6906 0.2184 1.2322 0.027 Uiso 1 1 calc R . .
C60 C 0.62941(7) 0.22461(7) 1.2658(3) 0.0329(7) Uani 1 1 d . . .
H60 H 0.6190 0.2303 1.3311 0.039 Uiso 1 1 calc R . .
C61 C 0.59102(7) 0.02144(7) 0.7940(3) 0.0350(7) Uani 1 1 d . . .
H61 H 0.5750 0.0062 0.8488 0.042 Uiso 1 1 calc R . .
C1D C 0.73923(9) 0.13757(9) 0.3267(4) 0.0382(9) Uani 0.8343(19) 1 d P A 1
H1D1 H 0.7332 0.1225 0.2508 0.046 Uiso 0.8343(19) 1 calc PR A 1
H1D2 H 0.7311 0.1515 0.3052 0.046 Uiso 0.8343(19) 1 calc PR A 1
Cl2 Cl 0.77941(2) 0.15909(2) 0.33672(10) 0.0395(3) Uani 0.8343(19) 1 d P A 1
Cl3 Cl 0.72261(2) 0.11791(2) 0.48129(11) 0.0428(3) Uani 0.8343(19) 1 d P A 1
C1A C 0.6852(5) 0.0985(9) 0.232(3) 0.158(18) Uiso 0.1657(19) 1 d PD A 2
H1A1 H 0.6878 0.1189 0.2104 0.190 Uiso 0.1657(19) 1 calc PR A 2
H1A2 H 0.6961 0.0937 0.1604 0.190 Uiso 0.1657(19) 1 calc PR A 2
Cl1A Cl 0.7033(3) 0.1014(3) 0.3900(12) 0.129(4) Uiso 0.1657(19) 1 d PD A 2
Cl2A Cl 0.64828(16) 0.07277(15) 0.2232(6) 0.0543(18) Uiso 0.1657(19) 1 d PD A 2
C2A C 0.6697(11) 0.0187(7) 0.215(4) 0.099(15) Uiso 0.15 1 d PD B 3
H2A1 H 0.6809 0.0276 0.3020 0.118 Uiso 0.15 1 calc PR B 3
H2A2 H 0.6479 0.0127 0.2295 0.118 Uiso 0.15 1 calc PR B 3
Cl3A Cl 0.6848(6) 0.0464(4) 0.089(2) 0.232(9) Uiso 0.15 1 d PD B 3
Cl4A Cl 0.6715(3) -0.0137(3) 0.1791(13) 0.143(4) Uiso 0.15 1 d PD B 3
C1H C 0.59410(19) -0.07914(16) 0.5396(8) 0.036(2) Uiso 0.40 1 d PD C -5
H1H1 H 0.5740 -0.0870 0.5834 0.054 Uiso 0.40 1 calc PR C -5
H1H2 H 0.6085 -0.0797 0.6057 0.054 Uiso 0.40 1 calc PR C -5
H1H3 H 0.5921 -0.0920 0.4599 0.054 Uiso 0.40 1 calc PR C -5
C2H C 0.60614(19) -0.04584(17) 0.4920(11) 0.055(3) Uiso 0.40 1 d PD C -5
H2H1 H 0.6075 -0.0334 0.5733 0.066 Uiso 0.40 1 calc PR C -5
H2H2 H 0.5909 -0.0456 0.4283 0.066 Uiso 0.40 1 calc PR C -5
C3H C 0.63774(19) -0.03011(19) 0.4195(10) 0.058(3) Uiso 0.40 1 d PD C -5
H3H1 H 0.6535 -0.0298 0.4819 0.069 Uiso 0.40 1 calc PR C -5
H3H2 H 0.6368 -0.0419 0.3360 0.069 Uiso 0.40 1 calc PR C -5
C4H C 0.6466(4) 0.0026(2) 0.3799(18) 0.183(9) Uiso 0.40 1 d PD C -5
H4H1 H 0.6555 0.0160 0.4617 0.220 Uiso 0.40 1 calc PR C -5
H4H2 H 0.6277 0.0030 0.3544 0.220 Uiso 0.40 1 calc PR C -5
C5H C 0.6696(5) 0.0163(4) 0.261(2) 0.168(11) Uiso 0.40 1 d PD C -5
H5H1 H 0.6628 0.0018 0.1829 0.202 Uiso 0.40 1 calc PR C -5
H5H2 H 0.6901 0.0203 0.2913 0.202 Uiso 0.40 1 calc PR C -5
C6H C 0.6711(5) 0.0467(3) 0.2179(19) 0.166(9) Uiso 0.40 1 d PD C -5
H6H1 H 0.6858 0.0560 0.1418 0.249 Uiso 0.40 1 calc PR C -5
H6H2 H 0.6779 0.0609 0.2961 0.249 Uiso 0.40 1 calc PR C -5
H6H3 H 0.6507 0.0424 0.1880 0.249 Uiso 0.40 1 calc PR C -5
O1W O 0.6667 0.3333 1.011(4) 0.042(9) Uani 0.10 3 d SP . .
O2W O 0.6667 0.3333 1.172(10) 0.15(3) Uiso 0.10 3 d SP . .
O3W O 0.6667 0.3333 1.257(5) 0.066(14) Uiso 0.10 3 d SP . .

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
Pd1 0.01460(10) 0.01486(10) 0.02208(10) 0.00043(8) 0.00060(8) 0.00772(9)
N1 0.0132(11) 0.0146(11) 0.0214(11) -0.0011(8) -0.0007(8) 0.0077(9)
N2 0.0167(11) 0.0143(11) 0.0235(11) -0.0005(9) 0.0028(9) 0.0079(9)
N3 0.0147(11) 0.0150(11) 0.0196(11) -0.0009(8) -0.0007(8) 0.0068(9)
Cl1 0.0195(4) 0.0243(6) 0.0162(4) 0.0015(4) 0.0016(3) 0.0113(3)
C1 0.0165(13) 0.0174(13) 0.0165(12) 0.0003(10) -0.0028(10) 0.0124(11)
C2 0.0180(13) 0.0149(12) 0.0130(11) 0.0032(9) 0.0037(9) 0.0074(11)
C3 0.0187(14) 0.0228(14) 0.0234(13) 0.0033(11) 0.0035(11) 0.0126(12)
C4 0.0324(16) 0.0220(15) 0.0259(14) 0.0007(11) 0.0040(12) 0.0187(13)
C5 0.0295(16) 0.0150(13) 0.0212(13) -0.0016(10) 0.0009(11) 0.0107(12)
C6 0.0195(14) 0.0168(13) 0.0189(12) -0.0002(10) -0.0004(10) 0.0085(11)
C7 0.0192(13) 0.0158(13) 0.0129(11) 0.0024(9) 0.0028(10) 0.0089(11)
C8 0.0121(12) 0.0118(12) 0.0184(12) -0.0002(9) 0.0032(9) 0.0038(10)
C9 0.0158(12) 0.0112(12) 0.0161(12) 0.0021(9) 0.0010(9) 0.0070(10)
C10 0.0138(12) 0.0144(12) 0.0193(12) 0.0039(10) 0.0022(10) 0.0084(11)
C11 0.0152(13) 0.0171(13) 0.0216(13) 0.0002(10) -0.0005(10) 0.0076(11)
C12 0.0205(14) 0.0222(14) 0.0205(13) -0.0052(11) -0.0003(10) 0.0101(12)
C13 0.0210(14) 0.0224(14) 0.0209(13) -0.0014(10) 0.0051(11) 0.0115(12)
C14 0.0140(13) 0.0156(13) 0.0238(13) -0.0005(10) 0.0018(10) 0.0071(11)
C15 0.0142(12) 0.0145(13) 0.0184(12) 0.0002(10) 0.0022(10) 0.0070(11)
C16 0.0178(13) 0.0164(13) 0.0175(12) -0.0012(10) 0.0000(10) 0.0094(11)
C17 0.0148(13) 0.0204(14) 0.0218(13) -0.0026(10) -0.0016(10) 0.0072(11)
C18 0.0162(13) 0.0238(14) 0.0242(13) -0.0012(11) -0.0014(10) 0.0127(12)
C19 0.0156(13) 0.0176(13) 0.0212(13) 0.0012(10) 0.0003(10) 0.0096(11)
C20 0.0190(13) 0.0178(13) 0.0191(12) 0.0042(10) 0.0030(10) 0.0110(11)
C21 0.0190(14) 0.0167(13) 0.0253(13) 0.0007(10) 0.0010(11) 0.0104(11)
C22 0.0220(15) 0.0163(14) 0.0395(16) -0.0035(12) 0.0015(12) 0.0103(12)
C23 0.0195(14) 0.0148(14) 0.0447(17) -0.0015(12) 0.0038(12) 0.0097(12)
C24 0.0186(14) 0.0142(13) 0.0261(13) -0.0007(10) 0.0007(11) 0.0076(11)
C25 0.0193(14) 0.0145(13) 0.0237(13) 0.0035(10) 0.0011(11) 0.0073(11)
C26 0.0145(13) 0.0161(13) 0.0216(13) 0.0026(10) 0.0015(10) 0.0061(11)
C27 0.0139(13) 0.0177(13) 0.0226(13) 0.0015(10) 0.0005(10) 0.0050(11)
C28 0.0149(13) 0.0210(14) 0.0194(12) 0.0021(10) 0.0029(10) 0.0094(11)
C29 0.0149(13) 0.0187(13) 0.0137(11) 0.0025(9) 0.0028(9) 0.0088(11)
C30 0.0145(12) 0.0181(13) 0.0156(12) 0.0006(10) -0.0011(9) 0.0097(11)
C31 0.0174(13) 0.0169(13) 0.0208(12) -0.0032(10) -0.0050(10) 0.0113(11)
C32 0.0213(14) 0.0217(14) 0.0243(14) -0.0039(11) -0.0005(11) 0.0113(12)
C33 0.0304(17) 0.0333(17) 0.0227(14) -0.0069(12) -0.0004(12) 0.0191(14)
C34 0.0311(16) 0.0255(15) 0.0260(14) -0.0106(12) -0.0091(12) 0.0183(14)
C35 0.0218(15) 0.0177(14) 0.0316(15) -0.0032(11) -0.0037(11) 0.0080(12)
C36 0.0253(15) 0.0220(15) 0.0231(13) -0.0010(11) -0.0001(11) 0.0102(13)
C37 0.0151(13) 0.0142(13) 0.0220(13) -0.0006(10) -0.0001(10) 0.0075(11)
C38 0.0367(17) 0.0369(17) 0.0208(14) 0.0059(12) 0.0062(12) 0.0275(15)
C39 0.0355(18) 0.0409(19) 0.0282(15) 0.0074(13) 0.0017(13) 0.0286(16)
C40 0.0204(14) 0.0252(15) 0.0338(15) -0.0030(12) 0.0001(12) 0.0150(13)
C41 0.0359(17) 0.0376(18) 0.0236(14) 0.0022(12) 0.0092(12) 0.0264(15)
C42 0.0345(17) 0.0325(17) 0.0213(13) 0.0055(12) 0.0030(12) 0.0241(15)
C43 0.0165(13) 0.0147(13) 0.0337(15) -0.0027(11) -0.0015(11) 0.0072(11)
C44 0.0212(15) 0.0203(15) 0.0372(16) -0.0018(12) -0.0002(12) 0.0090(12)
C45 0.0325(18) 0.0261(16) 0.0367(17) -0.0067(13) -0.0050(13) 0.0127(14)
C46 0.0253(17) 0.0206(16) 0.055(2) -0.0093(14) -0.0101(15) 0.0056(14)
C47 0.0269(16) 0.0193(15) 0.0349(16) -0.0010(12) 0.0018(13) 0.0059(13)
C48 0.0156(13) 0.0154(13) 0.0213(13) 0.0044(10) 0.0052(10) 0.0063(11)
C49 0.0237(15) 0.0299(16) 0.0231(13) -0.0009(11) 0.0012(11) 0.0173(13)
C50 0.0285(17) 0.045(2) 0.0362(17) -0.0027(14) 0.0019(13) 0.0277(16)
C52 0.0327(17) 0.0342(17) 0.0200(14) -0.0077(12) 0.0024(12) 0.0155(14)
C53 0.0184(14) 0.0225(14) 0.0234(13) -0.0017(11) -0.0005(11) 0.0083(12)
C60 0.0338(18) 0.0407(19) 0.0293(16) -0.0088(13) 0.0061(13) 0.0224(16)
C61 0.0246(16) 0.0174(15) 0.050(2) 0.0018(13) 0.0028(14) 0.0007(13)
C1D 0.042(2) 0.040(2) 0.046(2) 0.0092(18) -0.0004(18) 0.030(2)
Cl2 0.0387(6) 0.0362(6) 0.0463(6) 0.0023(4) 0.0085(4) 0.0209(5)
Cl3 0.0460(6) 0.0377(6) 0.0525(7) 0.0137(5) 0.0140(5) 0.0269(5)
O1W 0.037(14) 0.037(14) 0.05(2) 0.000 0.000 0.018(7)

_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
Pd1 N2 2.014(2) . ?
Pd1 N3 2.030(2) . ?
Pd1 N1 2.037(2) . ?
Pd1 Cl11 2.3287(12) . ?
Pd1 Cl1 2.3232(9) . ?
N1 C16 1.341(3) . ?
N1 C19 1.390(3) . ?
N2 C24 1.368(3) . ?
N2 C21 1.369(3) . ?
N3 C29 1.342(3) . ?
N3 C26 1.396(3) . ?
C1 C30 1.349(3) . ?
C1 C2 1.481(3) . ?
C1 C10 1.484(3) . ?
C2 C3 1.399(3) . ?
C2 C7 1.407(3) . ?
C3 C4 1.389(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.490(3) . ?
C8 C15 1.352(3) . ?
C8 C9 1.484(3) . ?
C9 C10 1.394(3) . ?
C9 C14 1.402(3) . ?
C10 C11 1.399(3) . ?
C11 C12 1.383(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.460(3) . ?
C15 C31 1.514(3) . ?
C16 C17 1.436(3) . ?
C17 C18 1.352(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.439(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(3) . ?
C20 C21 1.418(4) . ?
C20 C37 1.494(3) . ?
C21 C22 1.420(4) . ?
C22 C23 1.365(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.436(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.420(4) . ?
C25 C26 1.374(4) . ?
C25 C43 1.495(4) . ?
C26 C27 1.436(3) . ?
C27 C28 1.350(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.440(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.469(3) . ?
C30 C48 1.501(3) . ?
C31 C36 1.382(4) . ?
C31 C32 1.392(3) . ?
C32 C33 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.373(4) . ?
C37 C42 1.395(4) . ?
C38 C39 1.378(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.375(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.369(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.385(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.380(4) . ?
C43 C47 1.393(4) . ?
C44 C45 1.386(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.373(4) . ?
C45 H45 0.9500 . ?
C46 C61 1.378(4) . ?
C46 H46 0.9500 . ?
C47 C61 1.388(4) . ?
C47 H47 0.9500 . ?
C48 C49 1.388(4) . ?
C48 C53 1.398(3) . ?
C49 C50 1.395(4) . ?
C49 H49 0.9500 . ?
C50 C60 1.387(4) . ?
C50 H50 0.9500 . ?
C52 C60 1.373(4) . ?
C52 C53 1.387(4) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C1D Cl2 1.752(4) . ?
C1D Cl3 1.762(4) . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
C1A Cl2A 1.650(19) . ?
C1A Cl1A 1.749(18) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A Cl4A 1.708(18) . ?
C2A Cl3A 1.720(19) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1H C2H 1.538(5) . ?
C1H H1H1 0.9800 . ?
C1H H1H2 0.9800 . ?
C1H H1H3 0.9800 . ?
C2H C3H 1.544(5) . ?
C2H H2H1 0.9900 . ?
C2H H2H2 0.9900 . ?
C3H C4H 1.522(5) . ?
C3H H3H1 0.9900 . ?
C3H H3H2 0.9900 . ?
C4H C5H 1.529(5) . ?
C4H H4H1 0.9900 . ?
C4H H4H2 0.9900 . ?
C5H C6H 1.546(5) . ?
C5H H5H1 0.9900 . ?
C5H H5H2 0.9900 . ?
C6H H6H1 0.9800 . ?
C6H H6H2 0.9800 . ?
C6H H6H3 0.9800 . ?
O1W O2W 1.56(10) . ?
O2W O3W 0.83(9) . ?

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
N2 Pd1 N3 90.78(8) . . ?
N2 Pd1 N1 90.54(8) . . ?
N3 Pd1 N1 168.97(8) . . ?
N2 Pd1 Cl11 140.4(7) . . ?
N3 Pd1 Cl11 95.8(4) . . ?
N1 Pd1 Cl11 90.1(4) . . ?
N2 Pd1 Cl1 154.44(7) . . ?
N3 Pd1 Cl1 90.78(6) . . ?
N1 Pd1 Cl1 92.75(6) . . ?
Cl11 Pd1 Cl1 14.4(7) . . ?
C16 N1 C19 106.8(2) . . ?
C16 N1 Pd1 128.04(17) . . ?
C19 N1 Pd1 125.13(16) . . ?
C24 N2 C21 106.7(2) . . ?
C24 N2 Pd1 125.54(17) . . ?
C21 N2 Pd1 125.30(17) . . ?
C29 N3 C26 107.3(2) . . ?
C29 N3 Pd1 128.19(17) . . ?
C26 N3 Pd1 124.52(17) . . ?
C30 C1 C2 123.8(2) . . ?
C30 C1 C10 124.9(2) . . ?
C2 C1 C10 111.0(2) . . ?
C3 C2 C7 119.8(2) . . ?
C3 C2 C1 124.1(2) . . ?
C7 C2 C1 116.1(2) . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 120.5(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 119.3(2) . . ?
C6 C7 C8 124.0(2) . . ?
C2 C7 C8 116.7(2) . . ?
C15 C8 C9 123.8(2) . . ?
C15 C8 C7 125.4(2) . . ?
C9 C8 C7 110.7(2) . . ?
C10 C9 C14 119.4(2) . . ?
C10 C9 C8 117.2(2) . . ?
C14 C9 C8 123.3(2) . . ?
C9 C10 C11 119.7(2) . . ?
C9 C10 C1 116.2(2) . . ?
C11 C10 C1 124.0(2) . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.5(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C9 120.1(2) . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
C8 C15 C16 121.8(2) . . ?
C8 C15 C31 123.0(2) . . ?
C16 C15 C31 115.2(2) . . ?
N1 C16 C17 110.2(2) . . ?
N1 C16 C15 126.4(2) . . ?
C17 C16 C15 123.2(2) . . ?
C18 C17 C16 107.2(2) . . ?
C18 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C17 C18 C19 106.8(2) . . ?
C17 C18 H18 126.6 . . ?
C19 C18 H18 126.6 . . ?
C20 C19 N1 125.0(2) . . ?
C20 C19 C18 125.5(2) . . ?
N1 C19 C18 108.8(2) . . ?
C19 C20 C21 125.4(2) . . ?
C19 C20 C37 118.5(2) . . ?
C21 C20 C37 116.0(2) . . ?
N2 C21 C20 125.8(2) . . ?
N2 C21 C22 109.5(2) . . ?
C20 C21 C22 124.7(2) . . ?
C23 C22 C21 107.9(2) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
C22 C23 C24 106.0(2) . . ?
C22 C23 H23 127.0 . . ?
C24 C23 H23 127.0 . . ?
N2 C24 C25 125.5(2) . . ?
N2 C24 C23 109.9(2) . . ?
C25 C24 C23 124.4(2) . . ?
C26 C25 C24 125.7(2) . . ?
C26 C25 C43 117.9(2) . . ?
C24 C25 C43 116.3(2) . . ?
C25 C26 N3 124.9(2) . . ?
C25 C26 C27 126.1(2) . . ?
N3 C26 C27 108.1(2) . . ?
C28 C27 C26 107.4(2) . . ?
C28 C27 H27 126.3 . . ?
C26 C27 H27 126.3 . . ?
C27 C28 C29 107.2(2) . . ?
C27 C28 H28 126.4 . . ?
C29 C28 H28 126.4 . . ?
N3 C29 C28 109.7(2) . . ?
N3 C29 C30 126.7(2) . . ?
C28 C29 C30 123.4(2) . . ?
C1 C30 C29 121.3(2) . . ?
C1 C30 C48 122.4(2) . . ?
C29 C30 C48 116.3(2) . . ?
C36 C31 C32 119.5(2) . . ?
C36 C31 C15 120.6(2) . . ?
C32 C31 C15 119.9(2) . . ?
C33 C32 C31 119.3(3) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C34 C33 C32 121.1(3) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 119.5(2) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 120.0(3) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 120.6(3) . . ?
C31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C38 C37 C42 118.6(2) . . ?
C38 C37 C20 121.8(2) . . ?
C42 C37 C20 119.5(2) . . ?
C37 C38 C39 121.3(2) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C40 C39 C38 119.8(3) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C41 C40 C39 119.9(3) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.5(2) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C41 C42 C37 119.9(2) . . ?
C41 C42 H42 120.1 . . ?
C37 C42 H42 120.1 . . ?
C44 C43 C47 118.9(2) . . ?
C44 C43 C25 119.4(2) . . ?
C47 C43 C25 121.7(2) . . ?
C43 C44 C45 120.9(3) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C46 C45 C44 119.7(3) . . ?
C46 C45 H45 120.1 . . ?
C44 C45 H45 120.1 . . ?
C45 C46 C61 120.3(3) . . ?
C45 C46 H46 119.8 . . ?
C61 C46 H46 119.8 . . ?
C61 C47 C43 120.1(3) . . ?
C61 C47 H47 119.9 . . ?
C43 C47 H47 119.9 . . ?
C49 C48 C53 118.5(2) . . ?
C49 C48 C30 121.5(2) . . ?
C53 C48 C30 120.0(2) . . ?
C48 C49 C50 120.6(3) . . ?
C48 C49 H49 119.7 . . ?
C50 C49 H49 119.7 . . ?
C60 C50 C49 120.3(3) . . ?
C60 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C60 C52 C53 121.3(3) . . ?
C60 C52 H52 119.4 . . ?
C53 C52 H52 119.4 . . ?
C52 C53 C48 120.1(3) . . ?
C52 C53 H53 119.9 . . ?
C48 C53 H53 119.9 . . ?
C52 C60 C50 119.1(3) . . ?
C52 C60 H60 120.5 . . ?
C50 C60 H60 120.5 . . ?
C46 C61 C47 120.0(3) . . ?
C46 C61 H61 120.0 . . ?
C47 C61 H61 120.0 . . ?
Cl2 C1D Cl3 112.0(2) . . ?
Cl2 C1D H1D1 109.2 . . ?
Cl3 C1D H1D1 109.2 . . ?
Cl2 C1D H1D2 109.2 . . ?
Cl3 C1D H1D2 109.2 . . ?
H1D1 C1D H1D2 107.9 . . ?
Cl2A C1A Cl1A 116.5(16) . . ?
Cl2A C1A H1A1 108.2 . . ?
Cl1A C1A H1A1 108.2 . . ?
Cl2A C1A H1A2 108.2 . . ?
Cl1A C1A H1A2 108.2 . . ?
H1A1 C1A H1A2 107.3 . . ?
Cl4A C2A Cl3A 114.5(14) . . ?
Cl4A C2A H2A1 108.6 . . ?
Cl3A C2A H2A1 108.6 . . ?
Cl4A C2A H2A2 108.6 . . ?
Cl3A C2A H2A2 108.6 . . ?
H2A1 C2A H2A2 107.6 . . ?
C2H C1H H1H1 109.5 . . ?
C2H C1H H1H2 109.5 . . ?
H1H1 C1H H1H2 109.5 . . ?
C2H C1H H1H3 109.5 . . ?
H1H1 C1H H1H3 109.5 . . ?
H1H2 C1H H1H3 109.5 . . ?
C1H C2H C3H 116.0(6) . . ?
C1H C2H H2H1 108.3 . . ?
C3H C2H H2H1 108.3 . . ?
C1H C2H H2H2 108.3 . . ?
C3H C2H H2H2 108.3 . . ?
H2H1 C2H H2H2 107.4 . . ?
C4H C3H C2H 109.8(6) . . ?
C4H C3H H3H1 109.7 . . ?
C2H C3H H3H1 109.7 . . ?
C4H C3H H3H2 109.7 . . ?
C2H C3H H3H2 109.7 . . ?
H3H1 C3H H3H2 108.2 . . ?
C3H C4H C5H 115.1(7) . . ?
C3H C4H H4H1 108.5 . . ?
C5H C4H H4H1 108.5 . . ?
C3H C4H H4H2 108.5 . . ?
C5H C4H H4H2 108.5 . . ?
H4H1 C4H H4H2 107.5 . . ?
C4H C5H C6H 107.7(7) . . ?
C4H C5H H5H1 110.2 . . ?
C6H C5H H5H1 110.2 . . ?
C4H C5H H5H2 110.2 . . ?
C6H C5H H5H2 110.2 . . ?
H5H1 C5H H5H2 108.5 . . ?
C5H C6H H6H1 109.5 . . ?
C5H C6H H6H2 109.5 . . ?
H6H1 C6H H6H2 109.5 . . ?
C5H C6H H6H3 109.5 . . ?
H6H1 C6H H6H3 109.5 . . ?
H6H2 C6H H6H3 109.5 . . ?
O3W O2W O1W 180.00(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.092

# Attachment '- monokation.cif'

data_monokation
_database_code_depnum_ccdc_archive 'CCDC 863456'
#TrackingRef '- monokation.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'meso-anthriporphyrin monocation'
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H36 N3, C2 F3 O2, 0.5(C2 H F3 O2)'
_chemical_formula_sum            'C57 H36.5 F4.5 N3 O3'
_chemical_formula_weight         896.0

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.249 0.250 0.034 557.1 55.7
2 0.751 0.750 -0.043 557.4 54.7
_platon_squeeze_details          
;
The residual electron-density count was assessed as 110.4 electrons per unit cell, which is approximately consistent with nearly two molecules of trifluoroacetic acid per unit cell which yields 0.5 trifluoroacetic acid per formula unit.
;

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

_cell_length_a                   16.924(5)
_cell_length_b                   24.465(8)
_cell_length_c                   11.989(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.57(3)
_cell_angle_gamma                90.00
_cell_volume                     4959(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9782
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      38.48

_exptl_crystal_description       plates
_exptl_crystal_colour            dark-purple
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1854
_exptl_absorpt_coefficient_mu    0.09
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Xcalibur PX with Onyx CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41162
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         27.50
_reflns_number_total             11387
_reflns_number_gt                6041
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11387
_refine_ls_number_parameters     585
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.2046
_refine_ls_wR_factor_gt          0.1899
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.89171(13) 0.07928(10) 0.11621(19) 0.0193(5) Uani 1 1 d . . .
H1 H 0.8408 0.0848 0.1235 0.023 Uiso 1 1 calc R . .
N2 N 0.75495(12) -0.00031(9) 0.19266(19) 0.0200(5) Uani 1 1 d . . .
N3 N 0.61015(12) 0.07593(10) 0.11966(19) 0.0192(5) Uani 1 1 d . . .
H3 H 0.6611 0.0829 0.1281 0.023 Uiso 1 1 calc R . .
C1 C 0.66224(15) 0.16765(11) 0.0042(2) 0.0162(6) Uani 1 1 d . . .
C2 C 0.70302(15) 0.20993(11) 0.0593(2) 0.0168(6) Uani 1 1 d . . .
C3 C 0.78807(15) 0.21170(11) 0.0597(2) 0.0171(6) Uani 1 1 d . . .
C4 C 0.82884(14) 0.17047(11) 0.0039(2) 0.0164(6) Uani 1 1 d . . .
C5 C 0.91498(15) 0.16418(12) 0.0189(2) 0.0185(6) Uani 1 1 d . . .
C6 C 0.94216(16) 0.11530(12) 0.0652(2) 0.0197(6) Uani 1 1 d . . .
C7 C 1.01848(16) 0.08977(12) 0.0679(2) 0.0224(6) Uani 1 1 d . . .
H7 H 1.0651 0.1044 0.0382 0.027 Uiso 1 1 calc R . .
C8 C 1.01226(16) 0.04109(12) 0.1202(2) 0.0217(6) Uani 1 1 d . . .
H8 H 1.0538 0.0155 0.1331 0.026 Uiso 1 1 calc R . .
C9 C 0.93175(16) 0.03462(12) 0.1530(2) 0.0196(6) Uani 1 1 d . . .
C10 C 0.90258(16) -0.00812(12) 0.2205(2) 0.0204(6) Uani 1 1 d . . .
C11 C 0.82462(16) -0.01938(12) 0.2450(2) 0.0230(6) Uani 1 1 d . . .
C12 C 0.80141(17) -0.05285(13) 0.3364(3) 0.0291(7) Uani 1 1 d . . .
H12 H 0.8365 -0.0716 0.3873 0.035 Uiso 1 1 calc R . .
C13 C 0.72217(17) -0.05342(13) 0.3381(3) 0.0286(7) Uani 1 1 d . . .
H13 H 0.6922 -0.0723 0.3910 0.034 Uiso 1 1 calc R . .
C14 C 0.68987(16) -0.02083(12) 0.2471(2) 0.0223(6) Uani 1 1 d . . .
C15 C 0.60941(15) -0.01141(12) 0.2236(2) 0.0190(6) Uani 1 1 d . . .
C16 C 0.57468(16) 0.03023(12) 0.1575(2) 0.0205(6) Uani 1 1 d . . .
C17 C 0.49238(16) 0.03424(12) 0.1216(2) 0.0227(6) Uani 1 1 d . . .
H17 H 0.4530 0.0075 0.1337 0.027 Uiso 1 1 calc R . .
C18 C 0.48033(16) 0.08246(12) 0.0678(2) 0.0214(6) Uani 1 1 d . . .
H18 H 0.4311 0.0954 0.0370 0.026 Uiso 1 1 calc R . .
C19 C 0.55496(15) 0.11061(12) 0.0653(2) 0.0186(6) Uani 1 1 d . . .
C20 C 0.57648(15) 0.15910(11) 0.0179(2) 0.0167(6) Uani 1 1 d . . .
C21 C 0.66329(16) 0.24918(12) 0.1260(2) 0.0194(6) Uani 1 1 d . . .
H21 H 0.6074 0.2475 0.1301 0.023 Uiso 1 1 calc R . .
C22 C 0.70469(16) 0.28922(12) 0.1839(2) 0.0236(6) Uani 1 1 d . . .
H22 H 0.6773 0.3155 0.2258 0.028 Uiso 1 1 calc R . .
C23 C 0.78740(17) 0.29116(12) 0.1811(2) 0.0251(7) Uani 1 1 d . . .
H23 H 0.8157 0.3194 0.2198 0.030 Uiso 1 1 calc R . .
C24 C 0.82753(16) 0.25305(12) 0.1235(2) 0.0208(6) Uani 1 1 d . . .
H24 H 0.8837 0.2542 0.1261 0.025 Uiso 1 1 calc R . .
C25 C 0.70224(15) 0.13005(11) -0.0635(2) 0.0167(6) Uani 1 1 d . . .
C26 C 0.78657(15) 0.13125(11) -0.0630(2) 0.0167(6) Uani 1 1 d . . .
C27 C 0.82592(16) 0.09406(12) -0.1347(2) 0.0199(6) Uani 1 1 d . . .
H27 H 0.8821 0.0939 -0.1345 0.024 Uiso 1 1 calc R . .
C28 C 0.78449(17) 0.05928(13) -0.2022(3) 0.0275(7) Uani 1 1 d . . .
H28 H 0.8119 0.0351 -0.2490 0.033 Uiso 1 1 calc R . .
C29 C 0.70093(17) 0.05823(13) -0.2046(3) 0.0303(7) Uani 1 1 d . . .
H29 H 0.6726 0.0339 -0.2534 0.036 Uiso 1 1 calc R . .
C30 C 0.66101(16) 0.09232(12) -0.1364(2) 0.0206(6) Uani 1 1 d . . .
H30 H 0.6049 0.0909 -0.1375 0.025 Uiso 1 1 calc R . .
C31 C 0.96778(16) 0.20865(12) -0.0134(2) 0.0227(6) Uani 1 1 d . . .
C32 C 0.94132(17) 0.24487(12) -0.0983(3) 0.0252(7) Uani 1 1 d . . .
H32 H 0.8909 0.2394 -0.1347 0.030 Uiso 1 1 calc R . .
C33 C 0.98746(19) 0.28808(14) -0.1293(3) 0.0341(8) Uani 1 1 d . . .
H33 H 0.9691 0.3121 -0.1872 0.041 Uiso 1 1 calc R . .
C34 C 1.06041(19) 0.29658(14) -0.0764(3) 0.0376(9) Uani 1 1 d . . .
H34 H 1.0925 0.3263 -0.0982 0.045 Uiso 1 1 calc R . .
C35 C 1.08654(18) 0.26220(14) 0.0074(3) 0.0365(9) Uani 1 1 d . . .
H35 H 1.1366 0.2686 0.0441 0.044 Uiso 1 1 calc R . .
C36 C 1.04146(16) 0.21832(13) 0.0397(3) 0.0265(7) Uani 1 1 d . . .
H36 H 1.0606 0.1948 0.0979 0.032 Uiso 1 1 calc R . .
C37 C 0.96366(16) -0.04385(12) 0.2791(2) 0.0225(6) Uani 1 1 d . . .
C38 C 1.01824(17) -0.02129(14) 0.3572(2) 0.0278(7) Uani 1 1 d . . .
H38 H 1.0204 0.0172 0.3678 0.033 Uiso 1 1 calc R . .
C39 C 1.06962(18) -0.05553(14) 0.4194(3) 0.0305(7) Uani 1 1 d . . .
H39 H 1.1064 -0.0403 0.4729 0.037 Uiso 1 1 calc R . .
C40 C 1.06691(18) -0.11102(14) 0.4033(3) 0.0319(8) Uani 1 1 d . . .
H40 H 1.1011 -0.1342 0.4469 0.038 Uiso 1 1 calc R . .
C41 C 1.01496(17) -0.13320(13) 0.3245(3) 0.0314(8) Uani 1 1 d . . .
H41 H 1.0143 -0.1716 0.3125 0.038 Uiso 1 1 calc R . .
C42 C 0.96335(17) -0.09967(13) 0.2621(3) 0.0269(7) Uani 1 1 d . . .
H42 H 0.9277 -0.1153 0.2076 0.032 Uiso 1 1 calc R . .
C43 C 0.55436(16) -0.04890(12) 0.2808(2) 0.0216(6) Uani 1 1 d . . .
C44 C 0.55973(17) -0.10484(13) 0.2679(3) 0.0267(7) Uani 1 1 d . . .
H44 H 0.5963 -0.1196 0.2181 0.032 Uiso 1 1 calc R . .
C45 C 0.51185(18) -0.13984(14) 0.3274(3) 0.0316(8) Uani 1 1 d . . .
H45 H 0.5158 -0.1783 0.3181 0.038 Uiso 1 1 calc R . .
C46 C 0.45886(18) -0.11846(14) 0.3996(3) 0.0319(8) Uani 1 1 d . . .
H46 H 0.4267 -0.1422 0.4408 0.038 Uiso 1 1 calc R . .
C47 C 0.45248(17) -0.06279(14) 0.4122(2) 0.0285(7) Uani 1 1 d . . .
H47 H 0.4154 -0.0484 0.4616 0.034 Uiso 1 1 calc R . .
C48 C 0.49923(16) -0.02750(14) 0.3538(2) 0.0259(7) Uani 1 1 d . . .
H48 H 0.4942 0.0109 0.3629 0.031 Uiso 1 1 calc R . .
C49 C 0.51984(16) 0.20192(12) -0.0181(2) 0.0208(6) Uani 1 1 d . . .
C50 C 0.44861(16) 0.21072(13) 0.0339(3) 0.0274(7) Uani 1 1 d . . .
H50 H 0.4340 0.1876 0.0932 0.033 Uiso 1 1 calc R . .
C51 C 0.39954(18) 0.25299(15) -0.0012(3) 0.0388(9) Uani 1 1 d . . .
H51 H 0.3510 0.2586 0.0340 0.047 Uiso 1 1 calc R . .
C52 C 0.42003(19) 0.28717(15) -0.0865(3) 0.0414(9) Uani 1 1 d . . .
H52 H 0.3858 0.3162 -0.1096 0.050 Uiso 1 1 calc R . .
C53 C 0.48974(18) 0.27923(13) -0.1382(3) 0.0330(8) Uani 1 1 d . . .
H53 H 0.5035 0.3024 -0.1979 0.040 Uiso 1 1 calc R . .
C54 C 0.54033(17) 0.23714(12) -0.1033(3) 0.0268(7) Uani 1 1 d . . .
H54 H 0.5893 0.2324 -0.1379 0.032 Uiso 1 1 calc R . .
C1A C 0.71206(19) 0.13252(15) 0.3891(3) 0.0354(8) Uani 1 1 d . . .
C2A C 0.77682(17) 0.11897(13) 0.3090(3) 0.0278(7) Uani 1 1 d . . .
F1A F 0.72622(13) 0.11287(10) 0.49022(16) 0.0558(6) Uani 1 1 d . . .
F2A F 0.70602(15) 0.18670(10) 0.4021(2) 0.0707(7) Uani 1 1 d . . .
F3A F 0.64052(11) 0.11553(12) 0.35330(18) 0.0722(9) Uani 1 1 d . . .
O1X O 0.75434(10) 0.11325(8) 0.20693(16) 0.0216(4) Uani 1 1 d . . .
O2X O 0.84314(15) 0.11480(16) 0.3493(2) 0.0756(11) 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
N1 0.0122(11) 0.0230(14) 0.0229(12) 0.0005(11) 0.0026(9) 0.0005(9)
N2 0.0154(12) 0.0181(13) 0.0264(13) 0.0006(11) 0.0027(10) -0.0006(9)
N3 0.0109(11) 0.0224(14) 0.0245(13) 0.0020(11) 0.0012(9) -0.0017(9)
C1 0.0169(13) 0.0165(15) 0.0152(13) 0.0026(12) 0.0017(11) 0.0022(11)
C2 0.0170(14) 0.0166(15) 0.0168(14) 0.0045(12) 0.0011(11) 0.0004(11)
C3 0.0169(13) 0.0177(15) 0.0165(13) 0.0035(12) -0.0004(11) -0.0006(11)
C4 0.0146(13) 0.0166(15) 0.0179(14) 0.0028(12) 0.0010(11) -0.0016(10)
C5 0.0168(14) 0.0221(16) 0.0166(14) -0.0018(12) 0.0017(11) 0.0022(11)
C6 0.0176(14) 0.0251(16) 0.0166(14) -0.0020(13) 0.0022(11) -0.0041(11)
C7 0.0145(14) 0.0278(17) 0.0251(15) -0.0021(14) 0.0022(11) -0.0003(11)
C8 0.0177(14) 0.0244(17) 0.0233(15) 0.0011(13) 0.0035(12) 0.0037(11)
C9 0.0189(14) 0.0196(16) 0.0201(15) -0.0008(12) -0.0027(11) 0.0042(11)
C10 0.0186(14) 0.0219(16) 0.0209(14) 0.0035(13) 0.0029(11) 0.0020(11)
C11 0.0233(15) 0.0207(16) 0.0250(15) -0.0007(13) 0.0023(12) 0.0029(12)
C12 0.0231(16) 0.0299(18) 0.0344(18) 0.0164(15) 0.0046(13) 0.0060(13)
C13 0.0266(17) 0.0283(18) 0.0311(17) 0.0121(15) 0.0048(13) -0.0015(13)
C14 0.0209(15) 0.0194(16) 0.0269(16) 0.0025(13) 0.0032(12) -0.0018(11)
C15 0.0195(14) 0.0185(16) 0.0191(14) 0.0035(12) 0.0010(11) -0.0025(11)
C16 0.0195(15) 0.0213(16) 0.0208(15) -0.0010(12) 0.0039(12) -0.0033(11)
C17 0.0176(15) 0.0274(17) 0.0233(15) 0.0019(13) 0.0031(12) -0.0047(12)
C18 0.0146(14) 0.0280(17) 0.0214(15) 0.0017(13) -0.0012(11) -0.0001(11)
C19 0.0155(14) 0.0245(16) 0.0158(13) 0.0003(12) -0.0006(11) 0.0018(11)
C20 0.0149(13) 0.0201(15) 0.0148(13) -0.0028(12) -0.0019(10) -0.0009(11)
C21 0.0177(14) 0.0196(16) 0.0210(15) 0.0007(12) 0.0007(11) 0.0017(11)
C22 0.0290(16) 0.0189(16) 0.0231(15) -0.0014(13) 0.0030(12) 0.0006(12)
C23 0.0294(16) 0.0228(17) 0.0228(15) -0.0048(13) 0.0003(13) -0.0049(13)
C24 0.0184(14) 0.0212(16) 0.0228(15) 0.0015(13) 0.0011(11) -0.0036(11)
C25 0.0161(14) 0.0155(15) 0.0184(14) 0.0033(12) 0.0000(11) -0.0001(10)
C26 0.0169(14) 0.0163(15) 0.0168(14) 0.0027(12) 0.0007(11) -0.0012(10)
C27 0.0160(14) 0.0194(16) 0.0243(15) 0.0004(13) 0.0014(11) 0.0004(11)
C28 0.0245(16) 0.0255(18) 0.0325(17) -0.0111(14) 0.0032(13) 0.0043(12)
C29 0.0246(16) 0.0261(18) 0.0396(19) -0.0128(15) -0.0033(14) -0.0005(13)
C30 0.0157(14) 0.0224(16) 0.0237(15) -0.0010(13) -0.0009(11) -0.0016(11)
C31 0.0216(15) 0.0209(16) 0.0261(16) -0.0048(13) 0.0074(12) -0.0003(12)
C32 0.0221(15) 0.0256(17) 0.0281(17) 0.0018(14) 0.0024(13) -0.0015(12)
C33 0.0361(19) 0.0273(19) 0.0399(19) 0.0073(16) 0.0152(15) -0.0014(14)
C34 0.0326(19) 0.0250(19) 0.056(2) -0.0002(17) 0.0167(16) -0.0118(14)
C35 0.0183(16) 0.035(2) 0.057(2) -0.0126(18) 0.0069(15) -0.0089(13)
C36 0.0159(15) 0.0276(18) 0.0362(18) -0.0018(15) 0.0019(13) -0.0002(12)
C37 0.0189(15) 0.0264(17) 0.0223(15) 0.0052(13) 0.0038(12) 0.0042(12)
C38 0.0257(16) 0.0319(19) 0.0261(16) 0.0034(14) 0.0050(13) 0.0038(13)
C39 0.0251(17) 0.041(2) 0.0255(17) 0.0031(15) 0.0004(13) 0.0066(14)
C40 0.0268(17) 0.037(2) 0.0323(18) 0.0131(16) 0.0091(14) 0.0132(14)
C41 0.0282(17) 0.0242(18) 0.042(2) 0.0113(15) 0.0101(15) 0.0080(13)
C42 0.0205(15) 0.0254(17) 0.0351(18) 0.0029(14) 0.0031(13) 0.0020(12)
C43 0.0170(14) 0.0271(17) 0.0204(15) 0.0025(13) -0.0010(11) -0.0033(11)
C44 0.0264(16) 0.0255(18) 0.0283(17) 0.0027(14) 0.0025(13) -0.0032(12)
C45 0.0373(19) 0.0265(18) 0.0307(18) 0.0043(15) -0.0004(15) -0.0069(14)
C46 0.0299(18) 0.039(2) 0.0270(17) 0.0100(16) 0.0000(14) -0.0132(14)
C47 0.0234(16) 0.041(2) 0.0214(16) 0.0018(15) 0.0034(12) -0.0048(13)
C48 0.0235(16) 0.0327(19) 0.0215(15) -0.0005(14) -0.0006(12) -0.0048(13)
C49 0.0170(14) 0.0206(16) 0.0244(15) -0.0029(13) -0.0034(11) 0.0001(11)
C50 0.0153(15) 0.0328(18) 0.0338(17) -0.0056(15) -0.0016(12) -0.0011(12)
C51 0.0215(17) 0.040(2) 0.055(2) -0.0133(19) -0.0051(16) 0.0084(14)
C52 0.0311(19) 0.032(2) 0.059(2) -0.0077(19) -0.0178(17) 0.0136(15)
C53 0.0357(19) 0.0258(18) 0.0361(19) 0.0049(15) -0.0129(15) 0.0048(14)
C54 0.0279(16) 0.0245(17) 0.0277(17) -0.0038(14) -0.0005(13) -0.0012(13)
C1A 0.0311(18) 0.045(2) 0.0305(18) -0.0039(17) 0.0011(14) 0.0008(15)
C2A 0.0231(16) 0.0337(19) 0.0269(17) -0.0062(15) 0.0031(13) -0.0021(13)
F1A 0.0551(14) 0.0832(18) 0.0298(11) 0.0081(11) 0.0103(10) -0.0003(12)
F2A 0.0951(19) 0.0512(16) 0.0667(16) -0.0205(13) 0.0122(14) 0.0291(13)
F3A 0.0230(11) 0.150(3) 0.0446(13) -0.0370(15) 0.0109(9) -0.0188(13)
O1X 0.0205(10) 0.0248(12) 0.0195(10) 0.0022(9) 0.0010(8) -0.0001(8)
O2X 0.0269(14) 0.163(3) 0.0361(15) -0.0297(18) -0.0052(12) 0.0107(17)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C9 1.349(3) . ?
N1 C6 1.388(3) . ?
N2 C11 1.391(4) . ?
N2 C14 1.399(3) . ?
N3 C16 1.357(3) . ?
N3 C19 1.401(3) . ?
C1 C2 1.394(4) . ?
C1 C25 1.419(4) . ?
C1 C20 1.483(4) . ?
C2 C21 1.436(4) . ?
C2 C3 1.440(4) . ?
C3 C4 1.408(4) . ?
C3 C24 1.417(4) . ?
C4 C26 1.423(4) . ?
C4 C5 1.469(4) . ?
C5 C6 1.388(4) . ?
C5 C31 1.471(4) . ?
C6 C7 1.434(4) . ?
C7 C8 1.352(4) . ?
C8 C9 1.444(4) . ?
C9 C10 1.424(4) . ?
C10 C11 1.392(4) . ?
C10 C37 1.504(4) . ?
C11 C12 1.436(4) . ?
C12 C13 1.342(4) . ?
C13 C14 1.439(4) . ?
C14 C15 1.397(4) . ?
C15 C16 1.403(4) . ?
C15 C43 1.496(4) . ?
C16 C17 1.443(4) . ?
C17 C18 1.356(4) . ?
C18 C19 1.440(4) . ?
C19 C20 1.372(4) . ?
C20 C49 1.472(4) . ?
C21 C22 1.374(4) . ?
C22 C23 1.403(4) . ?
C23 C24 1.360(4) . ?
C25 C26 1.427(4) . ?
C25 C30 1.431(4) . ?
C26 C27 1.435(4) . ?
C27 C28 1.349(4) . ?
C28 C29 1.413(4) . ?
C29 C30 1.367(4) . ?
C31 C36 1.395(4) . ?
C31 C32 1.407(4) . ?
C32 C33 1.375(4) . ?
C33 C34 1.378(5) . ?
C34 C35 1.369(5) . ?
C35 C36 1.382(4) . ?
C37 C42 1.381(4) . ?
C37 C38 1.398(4) . ?
C38 C39 1.399(4) . ?
C39 C40 1.372(5) . ?
C40 C41 1.373(5) . ?
C41 C42 1.391(4) . ?
C43 C44 1.381(4) . ?
C43 C48 1.409(4) . ?
C44 C45 1.397(4) . ?
C45 C46 1.377(5) . ?
C46 C47 1.375(5) . ?
C47 C48 1.382(4) . ?
C49 C54 1.392(4) . ?
C49 C50 1.398(4) . ?
C50 C51 1.380(4) . ?
C51 C52 1.378(5) . ?
C52 C53 1.371(5) . ?
C53 C54 1.392(4) . ?
C1A F1A 1.316(4) . ?
C1A F3A 1.333(4) . ?
C1A F2A 1.339(4) . ?
C1A C2A 1.525(4) . ?
C2A O2X 1.206(4) . ?
C2A O1X 1.273(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 N1 C6 110.4(2) . . ?
C11 N2 C14 109.8(2) . . ?
C16 N3 C19 111.0(2) . . ?
C2 C1 C25 120.9(2) . . ?
C2 C1 C20 121.2(2) . . ?
C25 C1 C20 117.8(2) . . ?
C1 C2 C21 121.7(2) . . ?
C1 C2 C3 119.8(2) . . ?
C21 C2 C3 118.1(2) . . ?
C4 C3 C24 122.6(2) . . ?
C4 C3 C2 119.2(2) . . ?
C24 C3 C2 118.0(2) . . ?
C3 C4 C26 120.4(2) . . ?
C3 C4 C5 121.4(2) . . ?
C26 C4 C5 118.0(2) . . ?
C6 C5 C4 116.7(2) . . ?
C6 C5 C31 123.2(2) . . ?
C4 C5 C31 120.1(2) . . ?
C5 C6 N1 121.6(2) . . ?
C5 C6 C7 131.8(3) . . ?
N1 C6 C7 106.6(2) . . ?
C8 C7 C6 107.8(2) . . ?
C7 C8 C9 108.5(2) . . ?
N1 C9 C10 126.8(2) . . ?
N1 C9 C8 106.7(2) . . ?
C10 C9 C8 126.2(2) . . ?
C11 C10 C9 128.4(3) . . ?
C11 C10 C37 115.1(2) . . ?
C9 C10 C37 116.4(2) . . ?
N2 C11 C10 129.1(3) . . ?
N2 C11 C12 106.3(2) . . ?
C10 C11 C12 124.6(3) . . ?
C13 C12 C11 109.0(3) . . ?
C12 C13 C14 109.2(3) . . ?
C15 C14 N2 128.8(3) . . ?
C15 C14 C13 125.3(3) . . ?
N2 C14 C13 105.8(2) . . ?
C14 C15 C16 127.9(3) . . ?
C14 C15 C43 115.3(2) . . ?
C16 C15 C43 116.8(2) . . ?
N3 C16 C15 127.4(2) . . ?
N3 C16 C17 106.2(2) . . ?
C15 C16 C17 126.3(3) . . ?
C18 C17 C16 108.9(2) . . ?
C17 C18 C19 108.2(2) . . ?
C20 C19 N3 122.2(2) . . ?
C20 C19 C18 132.2(3) . . ?
N3 C19 C18 105.6(2) . . ?
C19 C20 C49 123.8(2) . . ?
C19 C20 C1 116.6(2) . . ?
C49 C20 C1 119.7(2) . . ?
C22 C21 C2 121.1(2) . . ?
C21 C22 C23 119.9(3) . . ?
C24 C23 C22 120.7(3) . . ?
C23 C24 C3 122.0(3) . . ?
C1 C25 C26 119.1(2) . . ?
C1 C25 C30 122.4(2) . . ?
C26 C25 C30 118.4(2) . . ?
C4 C26 C25 119.6(2) . . ?
C4 C26 C27 122.0(2) . . ?
C25 C26 C27 118.4(2) . . ?
C28 C27 C26 121.1(3) . . ?
C27 C28 C29 121.1(3) . . ?
C30 C29 C28 119.9(3) . . ?
C29 C30 C25 121.2(3) . . ?
C36 C31 C32 118.2(3) . . ?
C36 C31 C5 123.1(3) . . ?
C32 C31 C5 118.6(3) . . ?
C33 C32 C31 120.9(3) . . ?
C32 C33 C34 119.9(3) . . ?
C35 C34 C33 119.9(3) . . ?
C34 C35 C36 121.2(3) . . ?
C35 C36 C31 119.8(3) . . ?
C42 C37 C38 119.2(3) . . ?
C42 C37 C10 120.5(3) . . ?
C38 C37 C10 120.2(3) . . ?
C37 C38 C39 119.8(3) . . ?
C40 C39 C38 120.1(3) . . ?
C39 C40 C41 120.3(3) . . ?
C40 C41 C42 120.3(3) . . ?
C37 C42 C41 120.4(3) . . ?
C44 C43 C48 119.1(3) . . ?
C44 C43 C15 120.7(3) . . ?
C48 C43 C15 120.0(3) . . ?
C43 C44 C45 120.5(3) . . ?
C46 C45 C44 119.8(3) . . ?
C47 C46 C45 120.1(3) . . ?
C46 C47 C48 120.9(3) . . ?
C47 C48 C43 119.5(3) . . ?
C54 C49 C50 118.7(3) . . ?
C54 C49 C20 118.4(3) . . ?
C50 C49 C20 122.8(3) . . ?
C51 C50 C49 119.9(3) . . ?
C52 C51 C50 120.8(3) . . ?
C53 C52 C51 120.0(3) . . ?
C52 C53 C54 119.9(3) . . ?
C49 C54 C53 120.6(3) . . ?
F1A C1A F3A 107.9(3) . . ?
F1A C1A F2A 105.4(3) . . ?
F3A C1A F2A 105.9(3) . . ?
F1A C1A C2A 113.2(3) . . ?
F3A C1A C2A 113.4(3) . . ?
F2A C1A C2A 110.4(3) . . ?
O2X C2A O1X 127.4(3) . . ?
O2X C2A C1A 116.7(3) . . ?
O1X C2A C1A 115.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.086


data_bs10
_database_code_depnum_ccdc_archive 'CCDC 863457'
#TrackingRef '- bs10.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        5,10,15,20-tetraphenyl-meso-anthriporphyrin
_chemical_name_common            5,10,15,20-tetraphenyl-meso-anthriporphyrin
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H35 N3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H36 Cl1 N3'
_chemical_formula_weight         767.45

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.415 0.904 0.242 158.0 20.7
2 0.585 0.096 0.758 158.0 20.7
_platon_squeeze_details          
;
The residual electron-density count was assessed as 41.4 electrons per unit cell, which is approximately consistent with nearly one molecule of dichloromethane per unit cell which yields 0.5 dichloromethane per formula unit.
;

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

_cell_length_a                   9.779(3)
_cell_length_b                   13.499(6)
_cell_length_c                   16.963(6)
_cell_angle_alpha                92.09(3)
_cell_angle_beta                 101.98(4)
_cell_angle_gamma                106.41(4)
_cell_volume                     2090.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8295
_cell_measurement_theta_min      2.7878
_cell_measurement_theta_max      36.9002

_exptl_crystal_description       plates
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Xcalibur PX with Onyx CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40404
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.1989
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         36.92
_reflns_number_total             17492
_reflns_number_gt                6447
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0953P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17492
_refine_ls_number_parameters     521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1838
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.1910
_refine_ls_wR_factor_gt          0.1637
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_restrained_S_all      0.774
_refine_ls_shift/su_max          0.000
_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
N25 N 0.77168(17) 0.63479(12) 0.13605(9) 0.0210(3) Uani 1 1 d . . .
N23 N 0.75852(18) 0.86724(12) 0.34020(10) 0.0245(4) Uani 1 1 d . . .
N24 N 0.90910(18) 0.86259(13) 0.19785(10) 0.0220(3) Uani 1 1 d . . .
H24N H 0.872(2) 0.8112(17) 0.2211(13) 0.024(6) Uiso 1 1 d . . .
C21 C 0.7119(2) 0.56396(14) 0.29663(11) 0.0202(4) Uani 1 1 d . . .
C20 C 0.6041(2) 0.47186(14) 0.15784(11) 0.0200(4) Uani 1 1 d . . .
C22 C 0.7093(2) 0.63688(14) 0.35985(11) 0.0194(4) Uani 1 1 d . . .
C1 C 0.5876(2) 0.52714(14) 0.23059(11) 0.0202(4) Uani 1 1 d . . .
C4 C 0.5837(2) 0.67037(14) 0.35565(11) 0.0203(4) Uani 1 1 d . . .
C2 C 0.4568(2) 0.55130(15) 0.23179(12) 0.0235(4) Uani 1 1 d . . .
C3 C 0.4545(2) 0.62372(15) 0.29566(11) 0.0231(4) Uani 1 1 d . . .
C10 C 0.9368(2) 1.01266(15) 0.29958(12) 0.0224(4) Uani 1 1 d . . .
C'21 C 0.8402(2) 0.53116(15) 0.30267(12) 0.0228(4) Uani 1 1 d . . .
H'21 H 0.8444 0.4841 0.2609 0.027 Uiso 1 1 calc R . .
C14 C 0.9596(2) 0.85221(15) 0.12831(11) 0.0207(4) Uani 1 1 d . . .
C17 C 0.8722(2) 0.56738(15) 0.04206(12) 0.0219(4) Uani 1 1 d . . .
H17 H 0.9351 0.5659 0.0065 0.026 Uiso 1 1 calc R . .
C46 C 0.5036(2) 0.74057(15) 0.47315(12) 0.0229(4) Uani 1 1 d . . .
C9 C 0.8516(2) 0.96316(15) 0.35484(12) 0.0222(4) Uani 1 1 d . . .
C28 C 0.9422(2) 1.19867(15) 0.32920(12) 0.0244(4) Uani 1 1 d . . .
H28 H 0.8393 1.1756 0.3244 0.029 Uiso 1 1 calc R . .
C15 C 0.9512(2) 0.76337(14) 0.08139(11) 0.0201(4) Uani 1 1 d . . .
C16 C 0.8672(2) 0.65916(15) 0.08847(11) 0.0199(4) Uani 1 1 d . . .
C5 C 0.5938(2) 0.75845(15) 0.41238(11) 0.0208(4) Uani 1 1 d . . .
C19 C 0.7068(2) 0.52697(14) 0.11881(11) 0.0191(4) Uani 1 1 d . . .
C39 C 0.5170(2) 0.36407(15) 0.12954(12) 0.0227(4) Uani 1 1 d . . .
C6 C 0.6929(2) 0.85220(15) 0.40713(12) 0.0231(4) Uani 1 1 d . . .
C13 C 1.0313(2) 0.95624(14) 0.11243(12) 0.0218(4) Uani 1 1 d . . .
H13 H 1.0741 0.9740 0.0675 0.026 Uiso 1 1 calc R . .
C"22 C 0.9530(2) 0.63667(16) 0.43053(12) 0.0265(4) Uani 1 1 d . . .
H"22 H 1.0338 0.6600 0.4758 0.032 Uiso 1 1 calc R . .
C27 C 1.0164(2) 1.12627(15) 0.32003(12) 0.0234(4) Uani 1 1 d . . .
C7 C 0.7545(2) 0.94507(15) 0.46515(12) 0.0233(4) Uani 1 1 d . . .
H7 H 0.7298 0.9554 0.5155 0.028 Uiso 1 1 calc R . .
C"21 C 0.9567(2) 0.56609(15) 0.36719(13) 0.0261(4) Uani 1 1 d . . .
H"21 H 1.0407 0.5432 0.3699 0.031 Uiso 1 1 calc R . .
C18 C 0.7709(2) 0.48531(15) 0.05914(12) 0.0230(4) Uani 1 1 d . . .
H18 H 0.7461 0.4151 0.0372 0.028 Uiso 1 1 calc R . .
C8 C 0.8530(2) 1.01323(16) 0.43331(12) 0.0246(4) Uani 1 1 d . . .
H8 H 0.9120 1.0806 0.4571 0.029 Uiso 1 1 calc R . .
C40 C 0.4653(2) 0.32997(16) 0.04649(13) 0.0262(4) Uani 1 1 d . . .
H40 H 0.4826 0.3782 0.0076 0.031 Uiso 1 1 calc R . .
C'22 C 0.8334(2) 0.67069(15) 0.42607(12) 0.0231(4) Uani 1 1 d . . .
H'22 H 0.8328 0.7185 0.4684 0.028 Uiso 1 1 calc R . .
C12 C 1.0274(2) 1.02426(15) 0.17190(12) 0.0234(4) Uani 1 1 d . . .
H12 H 1.0669 1.0976 0.1755 0.028 Uiso 1 1 calc R . .
C33 C 1.0331(2) 0.77520(15) 0.01530(12) 0.0233(4) Uani 1 1 d . . .
C38 C 0.9606(2) 0.73880(15) -0.06466(12) 0.0260(4) Uani 1 1 d . . .
H38 H 0.8570 0.7113 -0.0782 0.031 Uiso 1 1 calc R . .
C29 C 1.0162(2) 1.30386(16) 0.34521(13) 0.0295(5) Uani 1 1 d . . .
H29 H 0.9636 1.3520 0.3510 0.035 Uiso 1 1 calc R . .
C11 C 0.9537(2) 0.96711(15) 0.22881(12) 0.0229(4) Uani 1 1 d . . .
C32 C 1.1693(2) 1.16279(16) 0.32991(12) 0.0269(4) Uani 1 1 d . . .
H32 H 1.2229 1.1147 0.3263 0.032 Uiso 1 1 calc R . .
C23 C 0.3674(2) 0.61766(17) 0.55119(12) 0.0282(4) Uani 1 1 d . . .
H23 H 0.3338 0.5488 0.5649 0.034 Uiso 1 1 calc R . .
C45 C 0.4534(2) 0.63886(16) 0.49485(12) 0.0254(4) Uani 1 1 d . . .
H45 H 0.4790 0.5842 0.4705 0.031 Uiso 1 1 calc R . .
C26 C 0.4602(2) 0.81839(17) 0.50788(13) 0.0296(5) Uani 1 1 d . . .
H26 H 0.4875 0.8866 0.4919 0.036 Uiso 1 1 calc R . .
C'3 C 0.3226(2) 0.65198(18) 0.29219(13) 0.0311(5) Uani 1 1 d . . .
H'3 H 0.3192 0.6999 0.3337 0.037 Uiso 1 1 calc R . .
C44 C 0.4833(2) 0.29228(16) 0.18531(14) 0.0301(5) Uani 1 1 d . . .
H44 H 0.5120 0.3144 0.2417 0.036 Uiso 1 1 calc R . .
C30 C 1.1663(2) 1.33928(17) 0.35277(13) 0.0314(5) Uani 1 1 d . . .
H30 H 1.2167 1.4114 0.3633 0.038 Uiso 1 1 calc R . .
C'2 C 0.3282(2) 0.51268(18) 0.16829(13) 0.0322(5) Uani 1 1 d . . .
H'2 H 0.3285 0.4664 0.1249 0.039 Uiso 1 1 calc R . .
C41 C 0.3894(2) 0.22646(17) 0.02063(15) 0.0327(5) Uani 1 1 d . . .
H41 H 0.3558 0.2042 -0.0356 0.039 Uiso 1 1 calc R . .
C25 C 0.3765(3) 0.79635(19) 0.56621(15) 0.0388(6) Uani 1 1 d . . .
H25 H 0.3512 0.8505 0.5914 0.047 Uiso 1 1 calc R . .
C"3 C 0.2025(2) 0.6118(2) 0.23089(14) 0.0400(6) Uani 1 1 d . . .
H"3 H 0.1164 0.6315 0.2300 0.048 Uiso 1 1 calc R . .
C37 C 1.0390(3) 0.74247(17) -0.12495(14) 0.0332(5) Uani 1 1 d . . .
H37 H 0.9887 0.7158 -0.1791 0.040 Uiso 1 1 calc R . .
C31 C 1.2424(2) 1.26807(17) 0.34485(12) 0.0303(5) Uani 1 1 d . . .
H31 H 1.3452 1.2917 0.3497 0.036 Uiso 1 1 calc R . .
C36 C 1.1892(3) 0.78456(18) -0.10652(15) 0.0393(6) Uani 1 1 d . . .
H36 H 1.2422 0.7868 -0.1478 0.047 Uiso 1 1 calc R . .
C"2 C 0.2053(2) 0.5408(2) 0.16866(14) 0.0400(6) Uani 1 1 d . . .
H"2 H 0.1203 0.5123 0.1265 0.048 Uiso 1 1 calc R . .
C34 C 1.1855(2) 0.81777(19) 0.03294(15) 0.0381(6) Uani 1 1 d . . .
H34 H 1.2372 0.8431 0.0871 0.046 Uiso 1 1 calc R . .
C24 C 0.3304(2) 0.69685(18) 0.58740(13) 0.0336(5) Uani 1 1 d . . .
H24 H 0.2731 0.6826 0.6269 0.040 Uiso 1 1 calc R . .
C43 C 0.4081(2) 0.18876(17) 0.15875(17) 0.0401(6) Uani 1 1 d . . .
H43 H 0.3877 0.1402 0.1971 0.048 Uiso 1 1 calc R . .
C42 C 0.3626(2) 0.15603(18) 0.07670(16) 0.0370(6) Uani 1 1 d . . .
H42 H 0.3130 0.0849 0.0589 0.044 Uiso 1 1 calc R . .
C35 C 1.2620(3) 0.8232(2) -0.02841(17) 0.0463(7) Uani 1 1 d . . .
H35 H 1.3651 0.8539 -0.0160 0.056 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N25 0.0196(8) 0.0227(8) 0.0211(8) 0.0023(6) 0.0073(6) 0.0048(6)
N23 0.0296(9) 0.0225(8) 0.0272(9) 0.0062(7) 0.0170(7) 0.0087(7)
N24 0.0259(9) 0.0188(8) 0.0243(9) 0.0048(7) 0.0126(7) 0.0063(7)
C21 0.0214(9) 0.0186(9) 0.0226(10) 0.0042(7) 0.0080(8) 0.0064(7)
C20 0.0194(9) 0.0204(9) 0.0205(9) 0.0000(7) 0.0051(7) 0.0065(7)
C22 0.0200(9) 0.0181(9) 0.0215(9) 0.0045(7) 0.0087(8) 0.0048(7)
C1 0.0217(9) 0.0176(9) 0.0226(10) 0.0048(7) 0.0089(8) 0.0048(7)
C4 0.0220(9) 0.0220(9) 0.0195(9) 0.0044(7) 0.0102(8) 0.0063(7)
C2 0.0200(9) 0.0276(10) 0.0236(10) 0.0023(8) 0.0073(8) 0.0066(8)
C3 0.0216(9) 0.0313(11) 0.0210(10) 0.0039(8) 0.0099(8) 0.0115(8)
C10 0.0243(10) 0.0208(9) 0.0252(10) 0.0054(8) 0.0116(8) 0.0070(7)
C'21 0.0234(10) 0.0218(9) 0.0267(10) 0.0036(8) 0.0100(8) 0.0087(8)
C14 0.0185(9) 0.0250(10) 0.0207(10) 0.0056(8) 0.0079(7) 0.0071(7)
C17 0.0241(10) 0.0235(10) 0.0222(10) 0.0040(8) 0.0091(8) 0.0104(8)
C46 0.0204(9) 0.0272(10) 0.0230(10) 0.0073(8) 0.0089(8) 0.0066(8)
C9 0.0222(9) 0.0225(10) 0.0272(10) 0.0059(8) 0.0124(8) 0.0094(8)
C28 0.0283(10) 0.0236(10) 0.0250(10) 0.0025(8) 0.0143(8) 0.0075(8)
C15 0.0176(9) 0.0213(9) 0.0223(10) 0.0029(7) 0.0064(7) 0.0060(7)
C16 0.0194(9) 0.0253(10) 0.0170(9) 0.0034(7) 0.0051(7) 0.0089(7)
C5 0.0203(9) 0.0254(10) 0.0207(10) 0.0051(8) 0.0087(8) 0.0099(8)
C19 0.0204(9) 0.0188(9) 0.0194(9) 0.0025(7) 0.0051(7) 0.0071(7)
C39 0.0179(9) 0.0224(10) 0.0303(11) 0.0017(8) 0.0092(8) 0.0071(7)
C6 0.0247(10) 0.0256(10) 0.0253(10) 0.0062(8) 0.0129(8) 0.0118(8)
C13 0.0215(9) 0.0225(9) 0.0240(10) 0.0046(8) 0.0113(8) 0.0056(7)
C"22 0.0231(10) 0.0277(11) 0.0244(11) -0.0036(8) -0.0001(8) 0.0058(8)
C27 0.0267(10) 0.0253(10) 0.0198(10) 0.0027(8) 0.0113(8) 0.0061(8)
C7 0.0284(10) 0.0247(10) 0.0229(10) 0.0050(8) 0.0122(8) 0.0124(8)
C"21 0.0228(10) 0.0252(10) 0.0315(11) 0.0020(8) 0.0072(9) 0.0086(8)
C18 0.0269(10) 0.0236(10) 0.0208(10) 0.0004(8) 0.0077(8) 0.0097(8)
C8 0.0287(10) 0.0241(10) 0.0238(10) 0.0044(8) 0.0095(8) 0.0098(8)
C40 0.0196(9) 0.0266(10) 0.0326(12) -0.0027(9) 0.0067(8) 0.0075(8)
C'22 0.0214(9) 0.0225(10) 0.0231(10) -0.0025(8) 0.0041(8) 0.0042(7)
C12 0.0240(10) 0.0225(10) 0.0269(11) 0.0044(8) 0.0114(8) 0.0074(8)
C33 0.0228(9) 0.0209(9) 0.0296(11) 0.0023(8) 0.0135(8) 0.0061(7)
C38 0.0292(11) 0.0250(10) 0.0283(11) 0.0084(8) 0.0134(9) 0.0093(8)
C29 0.0351(12) 0.0261(11) 0.0307(12) 0.0006(9) 0.0170(10) 0.0080(9)
C11 0.0232(10) 0.0212(9) 0.0271(10) 0.0040(8) 0.0111(8) 0.0068(7)
C32 0.0269(10) 0.0309(11) 0.0246(11) 0.0001(8) 0.0093(8) 0.0090(8)
C23 0.0233(10) 0.0336(11) 0.0259(11) 0.0077(9) 0.0090(9) 0.0025(8)
C45 0.0295(10) 0.0262(10) 0.0212(10) 0.0050(8) 0.0088(8) 0.0066(8)
C26 0.0324(11) 0.0318(11) 0.0338(12) 0.0094(9) 0.0190(9) 0.0148(9)
C'3 0.0244(10) 0.0482(14) 0.0258(11) 0.0007(10) 0.0098(9) 0.0164(10)
C44 0.0274(11) 0.0292(11) 0.0361(12) 0.0061(9) 0.0144(9) 0.0069(9)
C30 0.0342(12) 0.0265(11) 0.0303(12) -0.0036(9) 0.0120(10) 0.0015(9)
C'2 0.0260(11) 0.0434(13) 0.0279(11) -0.0067(10) 0.0040(9) 0.0141(9)
C41 0.0176(10) 0.0358(12) 0.0426(13) -0.0127(10) 0.0047(9) 0.0081(9)
C25 0.0457(14) 0.0445(14) 0.0421(14) 0.0107(11) 0.0301(12) 0.0232(11)
C"3 0.0243(11) 0.0691(17) 0.0321(13) -0.0037(12) 0.0056(10) 0.0240(11)
C37 0.0467(13) 0.0301(11) 0.0339(12) 0.0100(9) 0.0239(11) 0.0177(10)
C31 0.0246(10) 0.0353(12) 0.0266(11) -0.0030(9) 0.0073(9) 0.0017(9)
C36 0.0494(14) 0.0352(12) 0.0484(15) 0.0093(11) 0.0367(12) 0.0174(11)
C"2 0.0265(11) 0.0657(17) 0.0285(12) -0.0050(11) 0.0019(9) 0.0192(11)
C34 0.0248(11) 0.0441(14) 0.0452(14) -0.0087(11) 0.0167(10) 0.0054(10)
C24 0.0272(11) 0.0488(14) 0.0315(12) 0.0107(10) 0.0174(9) 0.0133(10)
C43 0.0323(12) 0.0266(12) 0.0641(18) 0.0105(11) 0.0238(12) 0.0026(9)
C42 0.0215(10) 0.0282(12) 0.0602(17) -0.0046(11) 0.0130(11) 0.0040(8)
C35 0.0303(12) 0.0476(15) 0.0647(18) -0.0042(13) 0.0298(13) 0.0050(11)

_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
N25 C16 1.338(2) . ?
N25 C19 1.406(2) . ?
N23 C9 1.335(3) . ?
N23 C6 1.410(2) . ?
N24 C14 1.387(2) . ?
N24 C11 1.400(3) . ?
C21 C1 1.426(3) . ?
C21 C'21 1.431(3) . ?
C21 C22 1.438(3) . ?
C20 C19 1.375(3) . ?
C20 C39 1.467(3) . ?
C20 C1 1.480(3) . ?
C22 C4 1.414(3) . ?
C22 C'22 1.424(3) . ?
C1 C2 1.410(3) . ?
C4 C3 1.414(3) . ?
C4 C5 1.470(3) . ?
C2 C'2 1.428(3) . ?
C2 C3 1.440(3) . ?
C3 C'3 1.436(3) . ?
C10 C11 1.390(3) . ?
C10 C9 1.441(3) . ?
C10 C27 1.501(3) . ?
C'21 C"21 1.363(3) . ?
C14 C15 1.388(3) . ?
C14 C13 1.444(3) . ?
C17 C18 1.347(3) . ?
C17 C16 1.461(3) . ?
C46 C26 1.393(3) . ?
C46 C45 1.412(3) . ?
C46 C5 1.475(3) . ?
C9 C8 1.466(3) . ?
C28 C29 1.387(3) . ?
C28 C27 1.394(3) . ?
C15 C16 1.438(3) . ?
C15 C33 1.496(3) . ?
C5 C6 1.378(3) . ?
C19 C18 1.468(3) . ?
C39 C44 1.399(3) . ?
C39 C40 1.406(3) . ?
C6 C7 1.463(3) . ?
C13 C12 1.353(3) . ?
C"22 C'22 1.361(3) . ?
C"22 C"21 1.423(3) . ?
C27 C32 1.407(3) . ?
C7 C8 1.349(3) . ?
C40 C41 1.389(3) . ?
C12 C11 1.441(3) . ?
C33 C38 1.393(3) . ?
C33 C34 1.400(3) . ?
C38 C37 1.394(3) . ?
C29 C30 1.386(3) . ?
C32 C31 1.385(3) . ?
C23 C24 1.383(3) . ?
C23 C45 1.386(3) . ?
C26 C25 1.399(3) . ?
C'3 C"3 1.359(3) . ?
C44 C43 1.390(3) . ?
C30 C31 1.390(3) . ?
C'2 C"2 1.360(3) . ?
C41 C42 1.380(3) . ?
C25 C24 1.377(3) . ?
C"3 C"2 1.409(3) . ?
C37 C36 1.380(3) . ?
C36 C35 1.372(4) . ?
C34 C35 1.395(3) . ?
C43 C42 1.385(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 N25 C19 104.82(15) . . ?
C9 N23 C6 105.75(16) . . ?
C14 N24 C11 110.03(16) . . ?
C1 C21 C'21 122.47(17) . . ?
C1 C21 C22 119.26(16) . . ?
C'21 C21 C22 118.27(17) . . ?
C19 C20 C39 121.94(16) . . ?
C19 C20 C1 116.16(16) . . ?
C39 C20 C1 121.90(16) . . ?
C4 C22 C'22 122.27(17) . . ?
C4 C22 C21 119.51(17) . . ?
C'22 C22 C21 118.20(16) . . ?
C2 C1 C21 120.61(17) . . ?
C2 C1 C20 120.94(17) . . ?
C21 C1 C20 118.20(16) . . ?
C3 C4 C22 120.68(16) . . ?
C3 C4 C5 121.06(16) . . ?
C22 C4 C5 118.17(17) . . ?
C1 C2 C'2 122.30(17) . . ?
C1 C2 C3 119.44(17) . . ?
C'2 C2 C3 118.09(17) . . ?
C4 C3 C'3 122.18(17) . . ?
C4 C3 C2 119.58(16) . . ?
C'3 C3 C2 118.06(18) . . ?
C11 C10 C9 127.31(18) . . ?
C11 C10 C27 115.89(16) . . ?
C9 C10 C27 116.81(16) . . ?
C"21 C'21 C21 121.35(18) . . ?
N24 C14 C15 129.95(17) . . ?
N24 C14 C13 106.14(16) . . ?
C15 C14 C13 123.89(16) . . ?
C18 C17 C16 107.18(16) . . ?
C26 C46 C45 118.16(17) . . ?
C26 C46 C5 123.22(17) . . ?
C45 C46 C5 118.56(17) . . ?
N23 C9 C10 124.38(18) . . ?
N23 C9 C8 111.53(16) . . ?
C10 C9 C8 124.06(18) . . ?
C29 C28 C27 121.01(19) . . ?
C14 C15 C16 126.20(16) . . ?
C14 C15 C33 118.13(16) . . ?
C16 C15 C33 115.65(16) . . ?
N25 C16 C15 124.25(17) . . ?
N25 C16 C17 111.90(16) . . ?
C15 C16 C17 123.81(16) . . ?
C6 C5 C4 117.09(16) . . ?
C6 C5 C46 124.19(17) . . ?
C4 C5 C46 118.66(16) . . ?
C20 C19 N25 122.31(16) . . ?
C20 C19 C18 127.21(17) . . ?
N25 C19 C18 110.39(15) . . ?
C44 C39 C40 118.28(18) . . ?
C44 C39 C20 120.29(18) . . ?
C40 C39 C20 121.43(18) . . ?
C5 C6 N23 120.55(17) . . ?
C5 C6 C7 130.00(17) . . ?
N23 C6 C7 109.33(16) . . ?
C12 C13 C14 108.92(16) . . ?
C'22 C"22 C"21 119.79(18) . . ?
C28 C27 C32 118.00(18) . . ?
C28 C27 C10 121.54(17) . . ?
C32 C27 C10 120.46(17) . . ?
C8 C7 C6 106.69(17) . . ?
C'21 C"21 C"22 120.37(18) . . ?
C17 C18 C19 105.63(16) . . ?
C7 C8 C9 106.67(18) . . ?
C41 C40 C39 120.7(2) . . ?
C"22 C'22 C22 122.01(18) . . ?
C13 C12 C11 108.74(17) . . ?
C38 C33 C34 118.34(18) . . ?
C38 C33 C15 120.78(17) . . ?
C34 C33 C15 120.78(19) . . ?
C33 C38 C37 120.5(2) . . ?
C30 C29 C28 120.5(2) . . ?
C10 C11 N24 130.04(17) . . ?
C10 C11 C12 123.92(17) . . ?
N24 C11 C12 106.03(16) . . ?
C31 C32 C27 120.70(19) . . ?
C24 C23 C45 120.0(2) . . ?
C23 C45 C46 120.90(19) . . ?
C46 C26 C25 120.2(2) . . ?
C"3 C'3 C3 121.45(19) . . ?
C43 C44 C39 120.4(2) . . ?
C29 C30 C31 119.3(2) . . ?
C"2 C'2 C2 121.4(2) . . ?
C42 C41 C40 120.0(2) . . ?
C24 C25 C26 120.6(2) . . ?
C'3 C"3 C"2 120.2(2) . . ?
C36 C37 C38 120.4(2) . . ?
C32 C31 C30 120.5(2) . . ?
C35 C36 C37 119.8(2) . . ?
C'2 C"2 C"3 120.7(2) . . ?
C35 C34 C33 120.4(2) . . ?
C25 C24 C23 119.99(19) . . ?
C42 C43 C44 120.3(2) . . ?
C41 C42 C43 120.2(2) . . ?
C36 C35 C34 120.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.828
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.071