# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011


data_global

_journal_coden_Cambridge         440
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Prof. Jong Hwa Jung'
_publ_contact_author_email       jonghwa@gnu.kr

_publ_section_title              
;
The remarkable influence of ultrasound
on porphyrin-based metallogel formation: efficient control
of H-and J-types aggregations
;
loop_
_publ_author_name
'Jong Hwa Jung'
'Youngje Cho'
'Ji Ha Lee'
J.Jaworski
'Sunhong Park'
'Shim Sung Lee'

# Attachment '- F.cif'

data_aaa
_database_code_depnum_ccdc_archive 'CCDC 843610'
#TrackingRef '- F.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H74 N8 O14 Pd'
_chemical_formula_weight         1333.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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                   7.6902(7)
_cell_length_b                   14.2290(15)
_cell_length_c                   14.8521(15)
_cell_angle_alpha                91.645(5)
_cell_angle_beta                 90.598(5)
_cell_angle_gamma                90.643(5)
_cell_volume                     1624.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9863
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      31.88

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9320
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      174(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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30654
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6226
_reflns_number_gt                5933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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^)+(0.0714P)^2^+1.8197P] 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         6226
_refine_ls_number_parameters     377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1255
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_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
Pd1 Pd 1.0000 0.5000 0.0000 0.01552(11) Uani 1 2 d S . .
O1 O 0.2130(3) -0.04011(18) -0.1445(2) 0.0547(8) Uani 1 1 d . . .
O2 O 0.0123(3) 0.06622(17) -0.10971(19) 0.0449(6) Uani 1 1 d . . .
H2A H -0.0557 0.0259 -0.1336 0.067 Uiso 1 1 calc R . .
O3 O 0.3172(3) 0.66451(19) 0.53320(16) 0.0443(6) Uani 1 1 d . . .
H3B H 0.2718 0.6743 0.5838 0.066 Uiso 1 1 calc R . .
O4 O 0.5475(3) 0.62536(18) 0.61635(14) 0.0407(6) Uani 1 1 d . . .
O11 O -0.1332(4) 0.2974(3) 0.3246(2) 0.0722(10) Uani 1 1 d . . .
O12 O 0.2196(3) 0.04819(19) 0.1790(2) 0.0493(7) Uani 1 1 d . . .
O13 O 0.4794(4) 0.1184(2) 0.5894(2) 0.0694(9) Uiso 1 1 d . . .
N1 N 0.7930(3) 0.45047(16) 0.06672(14) 0.0184(4) Uani 1 1 d . . .
N2 N 1.0549(3) 0.58895(15) 0.10485(14) 0.0178(4) Uani 1 1 d . . .
N11 N 0.0122(3) 0.2891(2) 0.19505(18) 0.0321(6) Uani 1 1 d . . .
N12 N 0.2854(4) 0.1304(2) 0.3082(2) 0.0399(7) Uani 1 1 d . . .
C1 C 0.1744(4) 0.0378(2) -0.1187(2) 0.0337(7) Uani 1 1 d . . .
C2 C 0.3046(4) 0.1138(2) -0.09590(19) 0.0262(6) Uani 1 1 d . . .
C3 C 0.2558(4) 0.2076(2) -0.08830(19) 0.0252(6) Uani 1 1 d . . .
H3A H 0.1369 0.2238 -0.0945 0.030 Uiso 1 1 calc R . .
C4 C 0.3799(3) 0.2772(2) -0.07174(18) 0.0232(6) Uani 1 1 d . . .
H4A H 0.3459 0.3411 -0.0668 0.028 Uiso 1 1 calc R . .
C5 C 0.5545(3) 0.2540(2) -0.06229(17) 0.0215(5) Uani 1 1 d . . .
C6 C 0.6025(4) 0.1597(2) -0.0689(2) 0.0273(6) Uani 1 1 d . . .
H6A H 0.7211 0.1433 -0.0615 0.033 Uiso 1 1 calc R . .
C7 C 0.4792(4) 0.0903(2) -0.0862(2) 0.0285(6) Uani 1 1 d . . .
H7A H 0.5132 0.0264 -0.0916 0.034 Uiso 1 1 calc R . .
C8 C 0.4778(4) 0.6341(2) 0.5443(2) 0.0303(7) Uani 1 1 d . . .
C9 C 0.5650(4) 0.6120(2) 0.45696(19) 0.0256(6) Uani 1 1 d . . .
C10 C 0.7344(4) 0.5793(2) 0.45819(19) 0.0289(6) Uani 1 1 d . . .
H10A H 0.7931 0.5719 0.5141 0.035 Uiso 1 1 calc R . .
C11 C 0.8183(4) 0.5574(2) 0.37811(19) 0.0258(6) Uani 1 1 d . . .
H11A H 0.9342 0.5349 0.3796 0.031 Uiso 1 1 calc R . .
C12 C 0.7340(3) 0.56806(19) 0.29547(18) 0.0215(5) Uani 1 1 d . . .
C13 C 0.5632(4) 0.6006(2) 0.29516(19) 0.0266(6) Uani 1 1 d . . .
H13A H 0.5042 0.6085 0.2394 0.032 Uiso 1 1 calc R . .
C14 C 0.4791(4) 0.6216(2) 0.3752(2) 0.0291(6) Uani 1 1 d . . .
H14A H 0.3623 0.6425 0.3741 0.035 Uiso 1 1 calc R . .
C15 C 0.8119(3) 0.34553(19) -0.11024(17) 0.0196(5) Uani 1 1 d . . .
C16 C 0.6888(3) 0.32964(19) -0.04442(18) 0.0203(5) Uani 1 1 d . . .
C17 C 0.6821(3) 0.37908(19) 0.03778(17) 0.0199(5) Uani 1 1 d . . .
C18 C 0.5602(4) 0.3600(2) 0.10758(19) 0.0268(6) Uani 1 1 d . . .
H18A H 0.4700 0.3137 0.1049 0.032 Uiso 1 1 calc R . .
C19 C 0.5965(4) 0.4193(2) 0.17734(19) 0.0256(6) Uani 1 1 d . . .
H19A H 0.5368 0.4226 0.2330 0.031 Uiso 1 1 calc R . .
C20 C 0.7414(3) 0.47653(19) 0.15248(17) 0.0199(5) Uani 1 1 d . . .
C21 C 0.8196(3) 0.54573(19) 0.20796(17) 0.0196(5) Uani 1 1 d . . .
C22 C 0.9661(3) 0.59768(19) 0.18520(17) 0.0196(5) Uani 1 1 d . . .
C23 C 1.0468(4) 0.6703(2) 0.24043(18) 0.0243(6) Uani 1 1 d . . .
H23A H 1.0108 0.6904 0.2988 0.029 Uiso 1 1 calc R . .
C24 C 1.1817(4) 0.7046(2) 0.19534(18) 0.0239(6) Uani 1 1 d . . .
H24A H 1.2592 0.7532 0.2159 0.029 Uiso 1 1 calc R . .
C101 C 0.0327(5) 0.2460(3) 0.1063(2) 0.0443(9) Uani 1 1 d . . .
H10I H -0.0627 0.2010 0.0942 0.066 Uiso 1 1 calc R . .
H10J H 0.1439 0.2131 0.1037 0.066 Uiso 1 1 calc R . .
H10K H 0.0307 0.2947 0.0610 0.066 Uiso 1 1 calc R . .
C102 C 0.1426(5) 0.3579(3) 0.2234(3) 0.0466(9) Uani 1 1 d . . .
H10L H 0.1158 0.3822 0.2841 0.070 Uiso 1 1 calc R . .
H10M H 0.1432 0.4099 0.1815 0.070 Uiso 1 1 calc R . .
H10N H 0.2571 0.3285 0.2240 0.070 Uiso 1 1 calc R . .
C103 C -0.1153(5) 0.2651(3) 0.2480(3) 0.0452(9) Uani 1 1 d . . .
H10W H -0.1985 0.2201 0.2256 0.054 Uiso 1 1 calc R . .
C104 C 0.4641(5) 0.1473(3) 0.2834(3) 0.0522(10) Uiso 1 1 d . . .
H10O H 0.4852 0.1187 0.2238 0.078 Uiso 1 1 calc R . .
H10P H 0.5417 0.1194 0.3278 0.078 Uiso 1 1 calc R . .
H10Q H 0.4864 0.2151 0.2820 0.078 Uiso 1 1 calc R . .
C105 C 0.2279(6) 0.1670(3) 0.3949(3) 0.0549(10) Uiso 1 1 d . . .
H10R H 0.1051 0.1504 0.4030 0.082 Uiso 1 1 calc R . .
H10S H 0.2421 0.2355 0.3974 0.082 Uiso 1 1 calc R . .
H10T H 0.2977 0.1396 0.4429 0.082 Uiso 1 1 calc R . .
C106 C 0.1793(4) 0.0815(2) 0.2531(3) 0.0411(8) Uani 1 1 d . . .
H10U H 0.0633 0.0714 0.2724 0.049 Uiso 1 1 calc R . .
C107 C 0.7441(8) 0.0920(4) 0.5131(4) 0.0811(15) Uiso 1 1 d . . .
H10F H 0.8705 0.0895 0.5214 0.122 Uiso 1 1 calc R . .
H10G H 0.7156 0.1407 0.4701 0.122 Uiso 1 1 calc R . .
H10H H 0.7007 0.0309 0.4898 0.122 Uiso 1 1 calc R . .
C108 C 0.6615(7) 0.1146(4) 0.6007(4) 0.0717(13) Uiso 1 1 d . . .
H10D H 0.6910 0.0659 0.6445 0.086 Uiso 1 1 calc R . .
H10E H 0.7062 0.1759 0.6248 0.086 Uiso 1 1 calc R . .
C109 C 0.3904(7) 0.1298(4) 0.6704(4) 0.0697(13) Uiso 1 1 d . . .
H10B H 0.4299 0.1886 0.7020 0.084 Uiso 1 1 calc R . .
H10C H 0.4159 0.0766 0.7098 0.084 Uiso 1 1 calc R . .
C110 C 0.2007(8) 0.1337(5) 0.6523(5) 0.0958(19) Uiso 1 1 d . . .
H11B H 0.1390 0.1418 0.7093 0.144 Uiso 1 1 calc R . .
H11C H 0.1618 0.0751 0.6218 0.144 Uiso 1 1 calc R . .
H11D H 0.1759 0.1869 0.6138 0.144 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
Pd1 0.01526(15) 0.01958(16) 0.01167(15) -0.00046(10) 0.00284(9) -0.00158(10)
O1 0.0321(13) 0.0332(14) 0.097(2) -0.0214(14) 0.0017(13) -0.0079(10)
O2 0.0233(11) 0.0387(13) 0.0714(18) -0.0165(12) 0.0001(11) -0.0075(9)
O3 0.0481(14) 0.0554(16) 0.0302(12) 0.0035(11) 0.0208(10) 0.0142(12)
O4 0.0496(14) 0.0539(15) 0.0178(11) -0.0085(10) 0.0111(10) -0.0106(11)
O11 0.0604(19) 0.118(3) 0.0401(16) 0.0130(17) 0.0265(14) 0.0354(19)
O12 0.0309(12) 0.0453(15) 0.0701(19) -0.0174(14) -0.0063(12) -0.0056(10)
N1 0.0187(10) 0.0223(11) 0.0141(10) -0.0007(8) 0.0027(8) -0.0015(8)
N2 0.0179(10) 0.0203(11) 0.0152(10) -0.0005(8) 0.0022(8) -0.0022(8)
N11 0.0281(13) 0.0395(15) 0.0289(13) 0.0016(11) 0.0068(10) 0.0056(11)
N12 0.0334(14) 0.0341(15) 0.0519(18) 0.0020(13) -0.0061(13) -0.0051(12)
C1 0.0258(15) 0.0324(17) 0.0425(18) -0.0046(14) 0.0017(13) -0.0061(12)
C2 0.0250(14) 0.0279(15) 0.0256(14) -0.0013(12) 0.0026(11) -0.0045(11)
C3 0.0204(13) 0.0312(15) 0.0239(14) -0.0016(11) 0.0013(10) -0.0016(11)
C4 0.0238(13) 0.0245(14) 0.0212(13) 0.0002(11) 0.0018(10) -0.0003(11)
C5 0.0218(13) 0.0269(14) 0.0155(12) -0.0012(10) 0.0028(10) -0.0062(11)
C6 0.0206(13) 0.0296(15) 0.0314(15) -0.0033(12) 0.0014(11) -0.0002(11)
C7 0.0271(14) 0.0235(14) 0.0347(16) -0.0013(12) 0.0021(12) -0.0012(11)
C8 0.0409(17) 0.0251(15) 0.0250(15) -0.0018(12) 0.0136(13) -0.0058(12)
C9 0.0325(15) 0.0240(14) 0.0202(14) -0.0026(11) 0.0093(11) -0.0044(11)
C10 0.0319(15) 0.0381(17) 0.0167(13) -0.0011(12) 0.0019(11) -0.0050(12)
C11 0.0246(13) 0.0335(16) 0.0191(13) -0.0011(11) 0.0022(11) -0.0004(11)
C12 0.0242(13) 0.0232(14) 0.0170(13) -0.0020(10) 0.0056(10) -0.0046(10)
C13 0.0274(14) 0.0347(16) 0.0178(13) 0.0003(11) 0.0033(11) 0.0040(12)
C14 0.0275(14) 0.0328(16) 0.0271(15) -0.0004(12) 0.0077(11) 0.0038(12)
C15 0.0192(12) 0.0225(13) 0.0169(12) -0.0013(10) -0.0001(9) -0.0008(10)
C16 0.0182(12) 0.0234(13) 0.0191(13) -0.0007(10) -0.0003(10) -0.0016(10)
C17 0.0195(12) 0.0236(13) 0.0167(12) 0.0008(10) 0.0032(10) -0.0029(10)
C18 0.0231(13) 0.0347(16) 0.0226(14) -0.0015(12) 0.0065(11) -0.0100(11)
C19 0.0244(13) 0.0338(16) 0.0186(13) -0.0011(11) 0.0069(10) -0.0054(11)
C20 0.0184(12) 0.0246(14) 0.0169(12) 0.0022(10) 0.0038(9) 0.0005(10)
C21 0.0190(12) 0.0241(13) 0.0158(12) 0.0015(10) 0.0027(9) 0.0007(10)
C22 0.0198(12) 0.0239(13) 0.0149(12) -0.0013(10) 0.0021(9) 0.0016(10)
C23 0.0253(13) 0.0294(15) 0.0177(13) -0.0056(11) 0.0036(10) -0.0035(11)
C24 0.0246(13) 0.0273(14) 0.0193(13) -0.0051(11) 0.0006(10) -0.0044(11)
C101 0.054(2) 0.046(2) 0.0337(18) 0.0010(16) 0.0067(15) 0.0154(17)
C102 0.0365(18) 0.052(2) 0.051(2) 0.0035(18) -0.0022(16) 0.0004(16)
C103 0.0332(17) 0.059(2) 0.044(2) 0.0142(18) 0.0128(15) 0.0106(16)
C106 0.0300(16) 0.0330(18) 0.060(2) 0.0055(17) -0.0041(15) -0.0036(13)

_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 N1 2.015(2) 2_765 ?
Pd1 N1 2.015(2) . ?
Pd1 N2 2.016(2) . ?
Pd1 N2 2.016(2) 2_765 ?
O1 C1 1.204(4) . ?
O2 C1 1.321(4) . ?
O3 C8 1.323(4) . ?
O4 C8 1.202(4) . ?
O11 C103 1.225(5) . ?
O12 C106 1.230(5) . ?
O13 C109 1.397(6) . ?
O13 C108 1.411(6) . ?
N1 C17 1.375(3) . ?
N1 C20 1.380(3) . ?
N2 C15 1.378(3) 2_765 ?
N2 C22 1.384(3) . ?
N11 C103 1.311(4) . ?
N11 C102 1.445(5) . ?
N11 C101 1.449(4) . ?
N12 C106 1.326(5) . ?
N12 C104 1.445(5) . ?
N12 C105 1.451(5) . ?
C1 C2 1.494(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.394(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.392(4) . ?
C5 C6 1.398(4) . ?
C5 C16 1.499(4) . ?
C6 C7 1.379(4) . ?
C8 C9 1.494(4) . ?
C9 C14 1.387(4) . ?
C9 C10 1.388(4) . ?
C10 C11 1.389(4) . ?
C11 C12 1.395(4) . ?
C12 C13 1.397(4) . ?
C12 C21 1.491(3) . ?
C13 C14 1.386(4) . ?
C15 N2 1.378(3) 2_765 ?
C15 C16 1.389(4) . ?
C15 C24 1.435(4) 2_765 ?
C16 C17 1.393(4) . ?
C17 C18 1.435(4) . ?
C18 C19 1.342(4) . ?
C19 C20 1.431(4) . ?
C20 C21 1.393(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.432(4) . ?
C23 C24 1.336(4) . ?
C24 C15 1.435(4) 2_765 ?
C107 C108 1.483(7) . ?
C109 C110 1.483(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N1 180.0 2_765 . ?
N1 Pd1 N2 90.32(9) 2_765 . ?
N1 Pd1 N2 89.68(9) . . ?
N1 Pd1 N2 89.68(9) 2_765 2_765 ?
N1 Pd1 N2 90.32(9) . 2_765 ?
N2 Pd1 N2 179.999(1) . 2_765 ?
C109 O13 C108 113.4(4) . . ?
C17 N1 C20 106.4(2) . . ?
C17 N1 Pd1 126.39(17) . . ?
C20 N1 Pd1 127.07(18) . . ?
C15 N2 C22 106.0(2) 2_765 . ?
C15 N2 Pd1 126.60(17) 2_765 . ?
C22 N2 Pd1 127.37(18) . . ?
C103 N11 C102 121.6(3) . . ?
C103 N11 C101 121.8(3) . . ?
C102 N11 C101 116.5(3) . . ?
C106 N12 C104 120.3(3) . . ?
C106 N12 C105 121.6(3) . . ?
C104 N12 C105 118.0(3) . . ?
O1 C1 O2 123.7(3) . . ?
O1 C1 C2 123.6(3) . . ?
O2 C1 C2 112.7(3) . . ?
C3 C2 C7 119.7(3) . . ?
C3 C2 C1 121.2(3) . . ?
C7 C2 C1 119.0(3) . . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 C5 120.3(3) . . ?
C4 C5 C6 119.3(2) . . ?
C4 C5 C16 120.2(3) . . ?
C6 C5 C16 120.5(2) . . ?
C7 C6 C5 120.5(3) . . ?
C6 C7 C2 120.0(3) . . ?
O4 C8 O3 124.3(3) . . ?
O4 C8 C9 123.1(3) . . ?
O3 C8 C9 112.5(3) . . ?
C14 C9 C10 119.6(3) . . ?
C14 C9 C8 121.4(3) . . ?
C10 C9 C8 119.0(3) . . ?
C9 C10 C11 120.3(3) . . ?
C10 C11 C12 120.6(3) . . ?
C11 C12 C13 118.6(2) . . ?
C11 C12 C21 122.3(2) . . ?
C13 C12 C21 119.1(2) . . ?
C14 C13 C12 120.8(3) . . ?
C13 C14 C9 120.2(3) . . ?
N2 C15 C16 126.0(2) 2_765 . ?
N2 C15 C24 109.5(2) 2_765 2_765 ?
C16 C15 C24 124.5(3) . 2_765 ?
C15 C16 C17 124.3(3) . . ?
C15 C16 C5 118.2(2) . . ?
C17 C16 C5 117.5(2) . . ?
N1 C17 C16 126.3(2) . . ?
N1 C17 C18 109.2(2) . . ?
C16 C17 C18 124.5(3) . . ?
C19 C18 C17 107.6(2) . . ?
C18 C19 C20 107.5(2) . . ?
N1 C20 C21 126.0(2) . . ?
N1 C20 C19 109.3(2) . . ?
C21 C20 C19 124.7(2) . . ?
C22 C21 C20 124.4(2) . . ?
C22 C21 C12 118.4(2) . . ?
C20 C21 C12 117.1(2) . . ?
N2 C22 C21 125.5(2) . . ?
N2 C22 C23 109.2(2) . . ?
C21 C22 C23 125.4(2) . . ?
C24 C23 C22 107.9(2) . . ?
C23 C24 C15 107.5(2) . 2_765 ?
O11 C103 N11 123.7(4) . . ?
O12 C106 N12 125.0(3) . . ?
O13 C108 C107 109.8(5) . . ?
O13 C109 C110 109.8(5) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.092