# 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 2013


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_(1a)
_database_code_depnum_ccdc_archive 'CCDC 887763'
#TrackingRef 'tmastropietro.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'C36 H36 N6 O6 Zn, 0.5(C12 H12 N2 O2), 2(F6 P), O'
_chemical_formula_sum            'C42 H46 F12 N7 O8 P2 Zn'
_chemical_melting_point          ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            pink
_chemical_formula_weight         1132.17
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
_symmetry_space_group_name_Hall  '-P 1'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   12.0842(18)
_cell_length_b                   14.630(2)
_cell_length_c                   14.997(2)
_cell_angle_alpha                68.239(7)
_cell_angle_beta                 88.188(7)
_cell_angle_gamma                76.637(7)
_cell_volume                     2391.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      22.02
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1158
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            103631
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.33
_reflns_number_total             9640
_reflns_number_gt                6787
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.2000P)^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     SHELXL
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         9640
_refine_ls_number_parameters     647
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0873
_refine_ls_wR_factor_ref         0.3031
_refine_ls_wR_factor_gt          0.2660
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_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
Zn1 Zn 0.66481(4) 0.69388(4) 0.68768(4) 0.0451(3) Uani 1 1 d . . .
N1 N 0.6766(3) 0.6182(3) 0.8430(3) 0.0478(9) Uani 1 1 d . . .
N2 N 0.7543(3) 0.7812(3) 0.7393(3) 0.0463(9) Uani 1 1 d . A .
C1 C 0.6489(4) 0.5297(4) 0.8924(4) 0.0551(12) Uani 1 1 d . . .
H1 H 0.6242 0.4958 0.8582 0.066 Uiso 1 1 calc R . .
C2 C 0.6556(5) 0.4867(4) 0.9922(4) 0.0613(14) Uani 1 1 d . . .
H2 H 0.6363 0.4250 1.0235 0.074 Uiso 1 1 calc R . .
C3 C 0.6906(4) 0.5351(5) 1.0441(4) 0.0594(14) Uani 1 1 d . A .
C4 C 0.6974(7) 0.4945(6) 1.1539(5) 0.083(2) Uani 1 1 d . . .
H4A H 0.6226 0.5163 1.1748 0.100 Uiso 0.624(8) 1 calc PR A 1
H4B H 0.7155 0.4211 1.1773 0.100 Uiso 0.624(8) 1 calc PR A 1
H4C H 0.7692 0.5002 1.1760 0.100 Uiso 0.376(8) 1 d PR A 2
H4D H 0.6366 0.5368 1.1749 0.100 Uiso 0.376(8) 1 d PR A 2
O1A O 0.7702(8) 0.5213(8) 1.1940(5) 0.103(3) Uani 0.624(8) 1 d P A 1
H1A H 0.8348 0.4982 1.1817 0.155 Uiso 0.624(8) 1 calc PR A 1
O1B O 0.6889(14) 0.3917(11) 1.1982(10) 0.101(5) Uani 0.376(8) 1 d P A 2
H1B H 0.7330 0.3627 1.2460 0.152 Uiso 0.376(8) 1 calc PR A 2
C5 C 0.7230(4) 0.6279(4) 0.9924(4) 0.0536(12) Uani 1 1 d . . .
H5 H 0.7504 0.6618 1.0252 0.064 Uiso 1 1 calc R A .
C6 C 0.7132(4) 0.6662(4) 0.8941(3) 0.0456(10) Uani 1 1 d . A .
C7 C 0.7485(4) 0.7616(3) 0.8338(3) 0.0456(10) Uani 1 1 d . . .
C8 C 0.7752(4) 0.8276(4) 0.8755(4) 0.0556(13) Uani 1 1 d . A .
H8 H 0.7688 0.8140 0.9408 0.067 Uiso 1 1 calc R . .
C9 C 0.8104(4) 0.9116(4) 0.8169(4) 0.0595(13) Uani 1 1 d . . .
C10 C 0.8418(7) 0.9839(6) 0.8606(6) 0.085(2) Uani 1 1 d . A .
H10A H 0.9167 0.9935 0.8404 0.102 Uiso 0.624(8) 1 calc PR A 1
H10B H 0.7884 1.0492 0.8321 0.102 Uiso 0.624(8) 1 calc PR A 1
H10C H 0.7718 1.0213 0.8764 0.102 Uiso 0.376(8) 1 d PR A 2
H10D H 0.8866 0.9427 0.9204 0.102 Uiso 0.376(8) 1 d PR A 2
O2A O 0.8431(12) 0.9580(10) 0.9525(9) 0.145(5) Uani 0.624(8) 1 d P A 1
H2A H 0.9065 0.9236 0.9763 0.218 Uiso 0.624(8) 1 calc PR A 1
O2B O 0.8973(12) 1.0470(9) 0.8092(11) 0.090(5) Uani 0.376(8) 1 d P A 2
H2B H 0.8671 1.0753 0.7546 0.134 Uiso 0.376(8) 1 calc PR A 2
C11 C 0.8213(5) 0.9296(4) 0.7203(4) 0.0607(13) Uani 1 1 d . A .
H11 H 0.8487 0.9844 0.6804 0.073 Uiso 1 1 calc R . .
C12 C 0.7905(4) 0.8645(4) 0.6847(4) 0.0574(13) Uani 1 1 d . . .
H12 H 0.7948 0.8784 0.6191 0.069 Uiso 1 1 calc R A .
N3 N 0.4967(3) 0.7908(3) 0.6874(3) 0.0479(9) Uani 1 1 d . . .
N4 N 0.6311(3) 0.8036(3) 0.5400(3) 0.0459(9) Uani 1 1 d . . .
C13 C 0.4349(4) 0.7849(4) 0.7656(4) 0.0569(13) Uani 1 1 d . . .
H13 H 0.4678 0.7406 0.8258 0.068 Uiso 1 1 calc R . .
C14 C 0.3247(5) 0.8423(5) 0.7592(4) 0.0617(14) Uani 1 1 d . . .
H14 H 0.2857 0.8372 0.8146 0.074 Uiso 1 1 calc R . .
C15 C 0.2730(4) 0.9071(4) 0.6702(5) 0.0595(13) Uani 1 1 d . . .
C16 C 0.1505(5) 0.9687(5) 0.6573(5) 0.0773(18) Uani 1 1 d . . .
H16A H 0.1468 1.0383 0.6155 0.093 Uiso 1 1 calc R . .
H16B H 0.1034 0.9415 0.6271 0.093 Uiso 1 1 calc R . .
C17 C 0.3366(4) 0.9127(4) 0.5901(4) 0.0562(12) Uani 1 1 d . . .
H17 H 0.3041 0.9558 0.5293 0.067 Uiso 1 1 calc R . .
C18 C 0.4480(4) 0.8550(3) 0.5990(3) 0.0449(10) Uani 1 1 d . . .
C19 C 0.5211(4) 0.8567(3) 0.5162(3) 0.0454(10) Uani 1 1 d . . .
C20 C 0.4796(5) 0.9097(4) 0.4213(4) 0.0526(12) Uani 1 1 d . . .
H20 H 0.4036 0.9447 0.4066 0.063 Uiso 1 1 calc R . .
C21 C 0.5560(5) 0.9096(4) 0.3466(4) 0.0550(12) Uani 1 1 d . . .
C22 C 0.5097(7) 0.9640(5) 0.2418(4) 0.0796(19) Uani 1 1 d . . .
H22A H 0.4535 0.9318 0.2293 0.095 Uiso 1 1 calc R . .
H22B H 0.4723 1.0339 0.2308 0.095 Uiso 1 1 calc R . .
C23 C 0.6661(5) 0.8574(4) 0.3710(4) 0.0564(13) Uani 1 1 d . . .
H23 H 0.7176 0.8566 0.3236 0.068 Uiso 1 1 calc R . .
C24 C 0.7008(5) 0.8052(4) 0.4673(4) 0.0544(12) Uani 1 1 d . . .
H24 H 0.7764 0.7694 0.4829 0.065 Uiso 1 1 calc R . .
O3 O 0.1068(5) 0.9657(6) 0.7499(5) 0.139(3) Uani 1 1 d . . .
H3A H 0.1353 1.0014 0.7690 0.208 Uiso 1 1 calc R . .
O4 O 0.5939(6) 0.9618(6) 0.1808(4) 0.134(3) Uani 1 1 d . . .
H4 H 0.6201 0.9033 0.1851 0.201 Uiso 1 1 calc R . .
N5 N 0.8112(3) 0.5893(3) 0.6672(3) 0.0489(9) Uani 1 1 d . . .
N6 N 0.5915(3) 0.5862(3) 0.6563(3) 0.0453(9) Uani 1 1 d . . .
C25 C 0.9204(4) 0.5960(5) 0.6708(4) 0.0599(14) Uani 1 1 d . . .
H25 H 0.9346 0.6523 0.6789 0.072 Uiso 1 1 calc R . .
C26 C 1.0108(5) 0.5244(5) 0.6633(5) 0.0689(16) Uani 1 1 d . . .
H26 H 1.0847 0.5316 0.6673 0.083 Uiso 1 1 calc R . .
C27 C 0.9912(5) 0.4412(6) 0.6497(5) 0.0731(17) Uani 1 1 d . . .
C28 C 1.0887(6) 0.3559(8) 0.6431(8) 0.120(4) Uani 1 1 d . . .
H28A H 1.0689 0.2915 0.6766 0.143 Uiso 1 1 calc R . .
H28B H 1.0958 0.3643 0.5761 0.143 Uiso 1 1 calc R . .
C29 C 0.8796(5) 0.4312(5) 0.6463(5) 0.0651(15) Uani 1 1 d . . .
H29 H 0.8647 0.3746 0.6392 0.078 Uiso 1 1 calc R . .
C30 C 0.7910(4) 0.5073(4) 0.6537(3) 0.0498(11) Uani 1 1 d . . .
C31 C 0.6684(4) 0.5049(4) 0.6499(3) 0.0458(10) Uani 1 1 d . . .
C32 C 0.6333(4) 0.4262(4) 0.6371(4) 0.0546(12) Uani 1 1 d . . .
H32 H 0.6876 0.3707 0.6345 0.065 Uiso 1 1 calc R . .
C33 C 0.5176(5) 0.4292(4) 0.6282(4) 0.0549(12) Uani 1 1 d . . .
C34 C 0.4776(6) 0.3422(5) 0.6182(5) 0.0740(17) Uani 1 1 d . . .
H34A H 0.5334 0.3099 0.5845 0.089 Uiso 1 1 calc R . .
H34B H 0.4740 0.2924 0.6819 0.089 Uiso 1 1 calc R . .
C35 C 0.4407(4) 0.5147(4) 0.6309(4) 0.0567(13) Uani 1 1 d . . .
H35 H 0.3629 0.5217 0.6222 0.068 Uiso 1 1 calc R . .
C36 C 0.4800(4) 0.5899(4) 0.6466(4) 0.0506(11) Uani 1 1 d . . .
H36 H 0.4268 0.6452 0.6506 0.061 Uiso 1 1 calc R . .
O5 O 1.1916(6) 0.3524(8) 0.6807(10) 0.217(6) Uani 1 1 d . . .
H5A H 1.2018 0.3112 0.7363 0.326 Uiso 1 1 calc R . .
O6 O 0.3709(7) 0.3717(6) 0.5688(5) 0.136(3) Uani 1 1 d . . .
H6A H 0.3212 0.3637 0.6076 0.204 Uiso 1 1 calc R . .
N7 N 0.9694(5) 0.4039(5) 1.1093(4) 0.0876(18) Uani 1 1 d . . .
C37 C 0.9430(6) 0.3124(7) 1.1376(6) 0.097(3) Uani 1 1 d . . .
H37 H 0.9346 0.2789 1.2027 0.116 Uiso 1 1 calc R . .
C38 C 0.9279(5) 0.2664(6) 1.0751(6) 0.089(2) Uani 1 1 d . . .
H38 H 0.9083 0.2042 1.0980 0.106 Uiso 1 1 calc R . .
C39 C 0.9421(6) 0.3127(6) 0.9793(6) 0.087(2) Uani 1 1 d . A .
C40 C 0.9319(9) 0.2613(8) 0.9082(9) 0.129(3) Uani 1 1 d . . .
H40A H 0.8604 0.2951 0.8702 0.155 Uiso 0.624(8) 1 calc PR A 1
H40B H 0.9928 0.2711 0.8645 0.155 Uiso 0.624(8) 1 calc PR A 1
H40C H 0.8898 0.3090 0.8489 0.155 Uiso 0.376(8) 1 d PR A 2
H40D H 0.8959 0.2049 0.9359 0.155 Uiso 0.376(8) 1 d PR A 2
O7A O 0.9361(8) 0.1648(8) 0.9469(7) 0.110(3) Uiso 0.624(8) 1 d P A 1
H7A H 0.9897 0.1336 0.9268 0.165 Uiso 0.624(8) 1 calc PR A 1
O7B O 1.068(3) 0.225(3) 0.891(3) 0.251(16) Uiso 0.376(8) 1 d P A 2
H7B H 1.0747 0.2163 0.8401 0.377 Uiso 0.376(8) 1 calc PR A 2
C41 C 0.9728(5) 0.4064(7) 0.9502(6) 0.091(2) Uani 1 1 d . . .
H41 H 0.9846 0.4394 0.8858 0.110 Uiso 1 1 calc R A .
C42 C 0.9856(5) 0.4502(5) 1.0151(5) 0.077(2) Uani 1 1 d . . .
P1 P 1.13247(16) 0.77684(13) 0.49668(13) 0.0737(5) Uani 1 1 d . . .
P2 P 0.42110(19) 0.78990(17) 1.06192(15) 0.0861(6) Uani 1 1 d . . .
F1 F 1.2627(5) 0.7766(5) 0.4865(6) 0.156(3) Uani 1 1 d . . .
F2 F 1.1079(5) 0.8938(3) 0.4803(4) 0.1103(15) Uani 1 1 d . . .
F3 F 1.0040(5) 0.7782(5) 0.5080(7) 0.182(3) Uani 1 1 d . . .
F4 F 1.1625(5) 0.6598(4) 0.5140(4) 0.1174(16) Uani 1 1 d . . .
F5 F 1.1088(6) 0.8061(6) 0.3857(5) 0.156(2) Uiso 1 1 d . . .
F6 F 1.1500(6) 0.7476(5) 0.6089(5) 0.147(2) Uiso 1 1 d . . .
F7 F 0.5308(6) 0.7388(8) 1.1261(5) 0.220(5) Uani 1 1 d . . .
F8 F 0.3497(7) 0.7856(7) 1.1494(5) 0.218(5) Uani 1 1 d . . .
F9 F 0.4220(12) 0.6876(11) 1.0765(10) 0.273(5) Uiso 1 1 d . . .
F10 F 0.4227(9) 0.9023(8) 1.0492(8) 0.223(4) Uiso 1 1 d . . .
F11 F 0.3107(5) 0.8453(7) 0.9956(5) 0.179(3) Uani 1 1 d . . .
F12 F 0.4947(7) 0.8046(9) 0.9741(5) 0.231(5) Uani 1 1 d . . .
O2W O 0.1503(18) 1.0603(17) 0.8590(15) 0.190(7) Uiso 0.50 1 d P . .
O1W O 1.2402(12) 0.2193(11) 0.8676(10) 0.121(4) Uiso 0.50 1 d P . .
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
Zn1 0.0422(4) 0.0468(4) 0.0431(4) -0.0145(3) 0.0014(2) -0.0084(2)
N1 0.046(2) 0.050(2) 0.043(2) -0.0116(18) 0.0012(16) -0.0124(17)
N2 0.048(2) 0.049(2) 0.041(2) -0.0148(18) 0.0035(16) -0.0125(17)
C1 0.055(3) 0.051(3) 0.052(3) -0.010(2) 0.004(2) -0.016(2)
C2 0.059(3) 0.056(3) 0.056(3) -0.006(3) 0.008(2) -0.018(2)
C3 0.048(3) 0.071(3) 0.046(3) -0.010(3) 0.008(2) -0.007(2)
C4 0.089(5) 0.091(5) 0.052(4) -0.009(3) 0.015(3) -0.016(4)
O1A 0.110(6) 0.148(8) 0.043(4) -0.019(5) -0.007(4) -0.043(6)
O1B 0.125(12) 0.077(9) 0.069(8) -0.002(7) 0.004(8) -0.003(8)
C5 0.045(3) 0.068(3) 0.046(3) -0.019(2) 0.005(2) -0.013(2)
C6 0.041(2) 0.046(2) 0.043(2) -0.011(2) 0.0037(18) -0.0066(19)
C7 0.043(2) 0.043(2) 0.046(3) -0.013(2) -0.0021(19) -0.0064(19)
C8 0.051(3) 0.065(3) 0.058(3) -0.033(3) 0.004(2) -0.009(2)
C9 0.049(3) 0.055(3) 0.078(4) -0.030(3) 0.004(3) -0.011(2)
C10 0.088(5) 0.082(5) 0.110(6) -0.062(5) 0.010(4) -0.022(4)
O2A 0.212(13) 0.141(10) 0.128(10) -0.081(8) 0.013(9) -0.076(9)
O2B 0.124(11) 0.067(7) 0.113(10) -0.049(7) 0.037(8) -0.065(7)
C11 0.064(3) 0.052(3) 0.064(3) -0.014(3) 0.007(3) -0.021(2)
C12 0.059(3) 0.054(3) 0.049(3) -0.004(2) 0.003(2) -0.020(2)
N3 0.044(2) 0.050(2) 0.045(2) -0.0176(18) 0.0016(16) -0.0026(17)
N4 0.045(2) 0.048(2) 0.041(2) -0.0144(17) 0.0017(16) -0.0073(16)
C13 0.050(3) 0.067(3) 0.049(3) -0.022(3) 0.007(2) -0.004(2)
C14 0.057(3) 0.071(4) 0.060(3) -0.028(3) 0.013(2) -0.016(3)
C15 0.049(3) 0.056(3) 0.079(4) -0.031(3) 0.002(3) -0.012(2)
C16 0.048(3) 0.084(4) 0.103(5) -0.045(4) 0.009(3) -0.004(3)
C17 0.051(3) 0.052(3) 0.064(3) -0.019(3) -0.002(2) -0.011(2)
C18 0.048(2) 0.040(2) 0.049(3) -0.019(2) -0.001(2) -0.0099(19)
C19 0.050(3) 0.041(2) 0.046(3) -0.016(2) 0.001(2) -0.0123(19)
C20 0.057(3) 0.047(3) 0.048(3) -0.014(2) -0.008(2) -0.004(2)
C21 0.075(3) 0.042(3) 0.047(3) -0.013(2) -0.004(2) -0.017(2)
C22 0.114(5) 0.072(4) 0.044(3) -0.013(3) -0.005(3) -0.018(4)
C23 0.071(3) 0.053(3) 0.045(3) -0.019(2) 0.012(2) -0.015(2)
C24 0.057(3) 0.056(3) 0.050(3) -0.022(2) 0.004(2) -0.010(2)
O3 0.090(4) 0.173(7) 0.122(5) -0.048(5) 0.029(3) 0.016(4)
O4 0.160(6) 0.155(6) 0.060(3) -0.021(4) 0.010(4) -0.020(5)
N5 0.041(2) 0.052(2) 0.052(2) -0.0178(19) 0.0031(17) -0.0120(17)
N6 0.044(2) 0.049(2) 0.045(2) -0.0194(18) 0.0067(16) -0.0121(16)
C25 0.039(3) 0.072(4) 0.066(3) -0.021(3) 0.004(2) -0.016(2)
C26 0.042(3) 0.087(4) 0.073(4) -0.028(3) 0.007(3) -0.010(3)
C27 0.045(3) 0.093(5) 0.080(4) -0.044(4) 0.002(3) 0.006(3)
C28 0.043(3) 0.144(8) 0.195(10) -0.111(8) 0.000(4) 0.016(4)
C29 0.048(3) 0.074(4) 0.079(4) -0.041(3) 0.001(3) -0.004(3)
C30 0.046(3) 0.055(3) 0.043(3) -0.016(2) 0.0009(19) -0.008(2)
C31 0.043(2) 0.048(3) 0.044(2) -0.016(2) 0.0003(19) -0.0069(19)
C32 0.055(3) 0.051(3) 0.059(3) -0.024(2) 0.008(2) -0.010(2)
C33 0.068(3) 0.060(3) 0.045(3) -0.023(2) 0.013(2) -0.028(3)
C34 0.075(4) 0.081(4) 0.081(4) -0.039(4) 0.007(3) -0.033(3)
C35 0.049(3) 0.069(3) 0.057(3) -0.025(3) 0.003(2) -0.018(2)
C36 0.040(2) 0.057(3) 0.055(3) -0.023(2) 0.003(2) -0.011(2)
O5 0.083(5) 0.211(9) 0.390(16) -0.195(11) -0.043(7) 0.049(5)
O6 0.156(6) 0.136(6) 0.134(6) -0.040(4) -0.021(5) -0.082(5)
N7 0.069(3) 0.099(4) 0.066(3) -0.001(3) 0.001(3) -0.017(3)
C37 0.071(4) 0.095(6) 0.077(5) 0.016(4) 0.010(4) -0.011(4)
C38 0.050(3) 0.089(5) 0.100(6) -0.011(4) 0.014(3) -0.008(3)
C39 0.060(4) 0.091(5) 0.088(5) -0.010(4) 0.009(3) -0.015(3)
C40 0.114(7) 0.115(8) 0.139(9) -0.024(7) 0.021(6) -0.035(6)
C41 0.054(4) 0.111(6) 0.074(5) -0.002(4) 0.011(3) -0.009(4)
C42 0.038(3) 0.100(5) 0.061(4) 0.000(4) 0.002(2) -0.004(3)
P1 0.0810(11) 0.0659(10) 0.0703(11) -0.0180(8) 0.0019(8) -0.0224(8)
P2 0.0942(13) 0.0846(13) 0.0716(11) -0.0308(10) -0.0024(10) -0.0024(10)
F1 0.094(4) 0.131(5) 0.254(8) -0.079(5) 0.029(4) -0.041(3)
F2 0.125(4) 0.069(2) 0.122(4) -0.023(3) 0.010(3) -0.015(2)
F3 0.089(4) 0.137(5) 0.287(10) -0.031(6) 0.033(5) -0.044(3)
F4 0.164(5) 0.078(3) 0.119(4) -0.043(3) 0.011(3) -0.034(3)
F7 0.139(6) 0.330(12) 0.116(5) -0.074(6) -0.041(4) 0.075(7)
F8 0.186(7) 0.259(9) 0.095(4) 0.003(5) 0.036(4) 0.045(7)
F11 0.100(4) 0.288(10) 0.110(4) -0.049(5) -0.016(3) -0.009(5)
F12 0.157(6) 0.354(13) 0.110(5) -0.082(7) 0.024(4) 0.066(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
Zn1 N5 2.151(4) . ?
Zn1 N6 2.169(4) . ?
Zn1 N1 2.169(4) . ?
Zn1 N4 2.183(4) . ?
Zn1 N3 2.191(4) . ?
Zn1 N2 2.197(4) . ?
N1 C1 1.346(6) . ?
N1 C6 1.358(6) . ?
N2 C7 1.341(6) . ?
N2 C12 1.352(6) . ?
C1 C2 1.388(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(9) . ?
C2 H2 0.9300 . ?
C3 C5 1.430(8) . ?
C3 C4 1.527(8) . ?
C4 O1A 1.287(11) . ?
C4 O1B 1.428(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9699 . ?
O1A H4C 0.4819 . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
C5 C6 1.367(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.505(7) . ?
C7 C8 1.424(7) . ?
C8 C9 1.371(8) . ?
C8 H8 0.9300 . ?
C9 C11 1.381(8) . ?
C9 C10 1.552(8) . ?
C10 O2B 1.274(13) . ?
C10 O2A 1.287(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9701 . ?
C10 H10D 0.9700 . ?
O2A H10C 1.3473 . ?
O2A H10D 0.7527 . ?
O2A H2A 0.8200 . ?
O2B H2B 0.8200 . ?
C11 C12 1.372(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
N3 C13 1.356(6) . ?
N3 C18 1.363(6) . ?
N4 C24 1.352(6) . ?
N4 C19 1.359(6) . ?
C13 C14 1.385(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(8) . ?
C14 H14 0.9300 . ?
C15 C17 1.393(8) . ?
C15 C16 1.521(7) . ?
C16 O3 1.459(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.395(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.497(7) . ?
C19 C20 1.387(7) . ?
C20 C21 1.429(8) . ?
C20 H20 0.9300 . ?
C21 C23 1.357(8) . ?
C21 C22 1.530(8) . ?
C22 O4 1.350(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.385(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
O3 H3A 0.8200 . ?
O4 H4 0.8200 . ?
N5 C25 1.350(6) . ?
N5 C30 1.364(7) . ?
N6 C36 1.347(6) . ?
N6 C31 1.363(6) . ?
C25 C26 1.361(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.379(10) . ?
C26 H26 0.9300 . ?
C27 C29 1.395(8) . ?
C27 C28 1.536(9) . ?
C28 O5 1.364(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.388(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.494(7) . ?
C31 C32 1.392(7) . ?
C32 C33 1.397(7) . ?
C32 H32 0.9300 . ?
C33 C35 1.388(8) . ?
C33 C34 1.519(8) . ?
C34 O6 1.401(9) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.390(8) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
O5 H5A 0.8200 . ?
O6 H6A 0.8200 . ?
N7 C42 1.351(8) . ?
N7 C37 1.358(11) . ?
C37 C38 1.378(12) . ?
C37 H37 0.9300 . ?
C38 C39 1.368(11) . ?
C38 H38 0.9300 . ?
C39 C41 1.409(12) . ?
C39 C40 1.539(14) . ?
C40 O7A 1.300(13) . ?
C40 O7B 1.66(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
C40 H40D 0.9700 . ?
O7A H40D 0.6389 . ?
O7A H7A 0.8200 . ?
O7B H7B 0.8200 . ?
C41 C42 1.379(11) . ?
C41 H41 0.9300 . ?
C42 C42 1.478(15) 2_767 ?
P1 F3 1.553(6) . ?
P1 F5 1.575(8) . ?
P1 F1 1.576(6) . ?
P1 F6 1.583(7) . ?
P1 F4 1.587(5) . ?
P1 F2 1.592(5) . ?
P2 F9 1.428(14) . ?
P2 F7 1.527(7) . ?
P2 F8 1.537(7) . ?
P2 F12 1.541(7) . ?
P2 F11 1.553(6) . ?
P2 F10 1.588(11) . ?
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
N5 Zn1 N6 76.56(15) . . ?
N5 Zn1 N1 94.16(16) . . ?
N6 Zn1 N1 96.55(15) . . ?
N5 Zn1 N4 99.07(15) . . ?
N6 Zn1 N4 92.70(15) . . ?
N1 Zn1 N4 165.33(15) . . ?
N5 Zn1 N3 167.58(15) . . ?
N6 Zn1 N3 92.39(15) . . ?
N1 Zn1 N3 92.72(15) . . ?
N4 Zn1 N3 75.49(15) . . ?
N5 Zn1 N2 98.40(15) . . ?
N6 Zn1 N2 170.59(14) . . ?
N1 Zn1 N2 75.72(15) . . ?
N4 Zn1 N2 95.97(15) . . ?
N3 Zn1 N2 93.31(15) . . ?
C1 N1 C6 117.7(4) . . ?
C1 N1 Zn1 125.9(4) . . ?
C6 N1 Zn1 116.4(3) . . ?
C7 N2 C12 117.6(4) . . ?
C7 N2 Zn1 114.0(3) . . ?
C12 N2 Zn1 126.6(3) . . ?
N1 C1 C2 122.9(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C5 117.8(5) . . ?
C2 C3 C4 123.1(6) . . ?
C5 C3 C4 119.0(6) . . ?
O1A C4 O1B 116.4(9) . . ?
O1A C4 C3 116.3(7) . . ?
O1B C4 C3 114.2(9) . . ?
O1A C4 H4A 108.2 . . ?
O1B C4 H4A 89.5 . . ?
C3 C4 H4A 108.2 . . ?
O1A C4 H4B 108.2 . . ?
O1B C4 H4B 17.9 . . ?
C3 C4 H4B 108.2 . . ?
H4A C4 H4B 107.4 . . ?
O1A C4 H4C 18.7 . . ?
O1B C4 H4C 108.8 . . ?
C3 C4 H4C 108.7 . . ?
H4A C4 H4C 126.4 . . ?
H4B C4 H4C 96.3 . . ?
O1A C4 H4D 88.9 . . ?
O1B C4 H4D 108.7 . . ?
C3 C4 H4D 108.7 . . ?
H4A C4 H4D 22.4 . . ?
H4B C4 H4D 125.9 . . ?
H4C C4 H4D 107.6 . . ?
C4 O1A H4C 40.1 . . ?
C4 O1A H1A 109.5 . . ?
H4C O1A H1A 69.5 . . ?
C4 O1B H1B 109.5 . . ?
C6 C5 C3 119.1(5) . . ?
C6 C5 H5 120.4 . . ?
C3 C5 H5 120.4 . . ?
N1 C6 C5 122.6(5) . . ?
N1 C6 C7 114.5(4) . . ?
C5 C6 C7 122.8(5) . . ?
N2 C7 C8 121.7(5) . . ?
N2 C7 C6 116.9(4) . . ?
C8 C7 C6 121.4(4) . . ?
C9 C8 C7 118.4(5) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C11 120.0(5) . . ?
C8 C9 C10 119.6(6) . . ?
C11 C9 C10 120.4(6) . . ?
O2B C10 O2A 121.1(10) . . ?
O2B C10 C9 117.0(8) . . ?
O2A C10 C9 118.3(8) . . ?
O2B C10 H10A 34.9 . . ?
O2A C10 H10A 107.7 . . ?
C9 C10 H10A 107.7 . . ?
O2B C10 H10B 72.3 . . ?
O2A C10 H10B 107.7 . . ?
C9 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
O2B C10 H10C 108.4 . . ?
O2A C10 H10C 71.7 . . ?
C9 C10 H10C 108.0 . . ?
H10A C10 H10C 138.8 . . ?
H10B C10 H10C 41.7 . . ?
O2B C10 H10D 107.8 . . ?
O2A C10 H10D 35.6 . . ?
C9 C10 H10D 108.0 . . ?
H10A C10 H10D 80.2 . . ?
H10B C10 H10D 139.0 . . ?
H10C C10 H10D 107.3 . . ?
C10 O2A H10C 43.1 . . ?
C10 O2A H10D 48.5 . . ?
H10C O2A H10D 91.7 . . ?
C10 O2A H2A 109.5 . . ?
H10C O2A H2A 151.5 . . ?
H10D O2A H2A 61.3 . . ?
C10 O2B H2B 109.5 . . ?
C12 C11 C9 118.2(5) . . ?
C12 C11 H11 120.9 . . ?
C9 C11 H11 120.9 . . ?
N2 C12 C11 123.9(5) . . ?
N2 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
C13 N3 C18 118.7(4) . . ?
C13 N3 Zn1 125.6(3) . . ?
C18 N3 Zn1 115.5(3) . . ?
C24 N4 C19 117.5(4) . . ?
C24 N4 Zn1 125.3(3) . . ?
C19 N4 Zn1 115.1(3) . . ?
N3 C13 C14 122.6(5) . . ?
N3 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C15 C14 C13 119.8(5) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C17 117.4(5) . . ?
C14 C15 C16 122.7(6) . . ?
C17 C15 C16 119.9(5) . . ?
O3 C16 C15 110.7(6) . . ?
O3 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C15 C17 C18 121.5(5) . . ?
C15 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
N3 C18 C17 120.1(5) . . ?
N3 C18 C19 115.6(4) . . ?
C17 C18 C19 124.3(4) . . ?
N4 C19 C20 122.1(4) . . ?
N4 C19 C18 115.6(4) . . ?
C20 C19 C18 122.2(4) . . ?
C19 C20 C21 118.6(5) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
C23 C21 C20 119.0(5) . . ?
C23 C21 C22 122.1(5) . . ?
C20 C21 C22 118.9(5) . . ?
O4 C22 C21 111.3(6) . . ?
O4 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
O4 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C21 C23 C24 119.0(5) . . ?
C21 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
N4 C24 C23 123.8(5) . . ?
N4 C24 H24 118.1 . . ?
C23 C24 H24 118.1 . . ?
C16 O3 H3A 109.5 . . ?
C22 O4 H4 109.5 . . ?
C25 N5 C30 117.9(4) . . ?
C25 N5 Zn1 125.6(4) . . ?
C30 N5 Zn1 116.4(3) . . ?
C36 N6 C31 117.8(4) . . ?
C36 N6 Zn1 127.0(3) . . ?
C31 N6 Zn1 115.1(3) . . ?
N5 C25 C26 123.4(6) . . ?
N5 C25 H25 118.3 . . ?
C26 C25 H25 118.3 . . ?
C25 C26 C27 119.1(5) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C26 C27 C29 119.2(5) . . ?
C26 C27 C28 122.3(6) . . ?
C29 C27 C28 118.5(7) . . ?
O5 C28 C27 114.1(7) . . ?
O5 C28 H28A 108.7 . . ?
C27 C28 H28A 108.7 . . ?
O5 C28 H28B 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C27 118.9(6) . . ?
C30 C29 H29 120.6 . . ?
C27 C29 H29 120.6 . . ?
N5 C30 C29 121.5(5) . . ?
N5 C30 C31 115.1(4) . . ?
C29 C30 C31 123.3(5) . . ?
N6 C31 C32 121.3(4) . . ?
N6 C31 C30 116.2(4) . . ?
C32 C31 C30 122.4(4) . . ?
C31 C32 C33 120.9(5) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C35 C33 C32 116.9(5) . . ?
C35 C33 C34 121.4(5) . . ?
C32 C33 C34 121.7(5) . . ?
O6 C34 C33 113.8(6) . . ?
O6 C34 H34A 108.8 . . ?
C33 C34 H34A 108.8 . . ?
O6 C34 H34B 108.8 . . ?
C33 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C33 C35 C36 120.0(5) . . ?
C33 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
N6 C36 C35 123.0(5) . . ?
N6 C36 H36 118.5 . . ?
C35 C36 H36 118.5 . . ?
C28 O5 H5A 109.5 . . ?
C34 O6 H6A 109.5 . . ?
C42 N7 C37 117.8(8) . . ?
N7 C37 C38 123.5(7) . . ?
N7 C37 H37 118.3 . . ?
C38 C37 H37 118.3 . . ?
C39 C38 C37 119.6(8) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 C41 116.9(9) . . ?
C38 C39 C40 121.0(8) . . ?
C41 C39 C40 121.9(8) . . ?
O7A C40 C39 115.4(10) . . ?
O7A C40 O7B 85.2(15) . . ?
C39 C40 O7B 99.5(15) . . ?
O7A C40 H40A 108.4 . . ?
C39 C40 H40A 108.4 . . ?
O7B C40 H40A 138.6 . . ?
O7A C40 H40B 108.4 . . ?
C39 C40 H40B 108.4 . . ?
O7B C40 H40B 32.9 . . ?
H40A C40 H40B 107.5 . . ?
O7A C40 H40C 126.4 . . ?
C39 C40 H40C 111.5 . . ?
O7B C40 H40C 111.3 . . ?
H40A C40 H40C 29.8 . . ?
H40B C40 H40C 78.7 . . ?
O7A C40 H40D 28.2 . . ?
C39 C40 H40D 111.8 . . ?
O7B C40 H40D 113.1 . . ?
H40A C40 H40D 84.4 . . ?
H40B C40 H40D 131.6 . . ?
H40C C40 H40D 109.4 . . ?
C40 O7A H40D 45.8 . . ?
C40 O7A H7A 109.5 . . ?
H40D O7A H7A 145.0 . . ?
C40 O7B H7B 109.5 . . ?
C42 C41 C39 121.5(7) . . ?
C42 C41 H41 119.2 . . ?
C39 C41 H41 119.2 . . ?
N7 C42 C41 120.6(7) . . ?
N7 C42 C42 117.4(9) . 2_767 ?
C41 C42 C42 121.9(8) . 2_767 ?
F3 P1 F5 87.4(5) . . ?
F3 P1 F1 178.9(5) . . ?
F5 P1 F1 93.4(4) . . ?
F3 P1 F6 89.8(4) . . ?
F5 P1 F6 177.2(4) . . ?
F1 P1 F6 89.4(4) . . ?
F3 P1 F4 91.2(4) . . ?
F5 P1 F4 91.0(3) . . ?
F1 P1 F4 89.5(3) . . ?
F6 P1 F4 89.1(3) . . ?
F3 P1 F2 91.1(3) . . ?
F5 P1 F2 89.9(4) . . ?
F1 P1 F2 88.2(3) . . ?
F6 P1 F2 90.2(3) . . ?
F4 P1 F2 177.6(3) . . ?
F9 P2 F7 82.2(7) . . ?
F9 P2 F8 91.8(7) . . ?
F7 P2 F8 91.5(4) . . ?
F9 P2 F12 94.0(7) . . ?
F7 P2 F12 88.1(4) . . ?
F8 P2 F12 174.1(7) . . ?
F9 P2 F11 99.7(7) . . ?
F7 P2 F11 178.0(6) . . ?
F8 P2 F11 89.0(4) . . ?
F12 P2 F11 91.2(4) . . ?
F9 P2 F10 178.0(7) . . ?
F7 P2 F10 96.0(6) . . ?
F8 P2 F10 87.4(6) . . ?
F12 P2 F10 86.8(6) . . ?
F11 P2 F10 82.1(5) . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.33
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.152


data_(2)
_database_code_depnum_ccdc_archive 'CCDC 887764'
#TrackingRef 'tmastropietro.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 N6 O6 Zn, 2(F6 P)'
_chemical_formula_sum            'C36 H36 F12 N6 O6 P2 Zn'
_chemical_formula_weight         1004.02
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.354(3)
_cell_length_b                   13.202(4)
_cell_length_c                   15.056(5)
_cell_angle_alpha                76.794(13)
_cell_angle_beta                 76.652(13)
_cell_angle_gamma                83.772(13)
_cell_volume                     2134.0(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9694
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.24
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9421
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69588
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         26.15
_reflns_number_total             8353
_reflns_number_gt                6545
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.0479P)^2^+8.9784P] 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     SHELXL
_refine_ls_extinction_coef       0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4250
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1142
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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
Zn1 Zn 0.70426(3) 0.68098(3) 0.70452(2) 0.03723(13) Uani 1 1 d . . .
N1 N 0.7898(2) 0.54117(19) 0.78877(17) 0.0383(6) Uani 1 1 d . . .
N2 N 0.5528(2) 0.59465(19) 0.79454(18) 0.0393(6) Uani 1 1 d . . .
N3 N 0.6783(2) 0.7991(2) 0.78462(18) 0.0412(6) Uani 1 1 d . . .
N4 N 0.5846(2) 0.80119(18) 0.63608(17) 0.0375(5) Uani 1 1 d . . .
N5 N 0.8756(2) 0.73403(19) 0.61270(18) 0.0395(6) Uani 1 1 d . . .
N6 N 0.7352(2) 0.59284(19) 0.59402(17) 0.0379(5) Uani 1 1 d . . .
O1 O 0.9066(2) 0.22693(19) 0.85516(19) 0.0601(7) Uani 1 1 d . . .
O2 O 0.2848(2) 0.41711(19) 0.98245(17) 0.0550(6) Uani 1 1 d . . .
O3 O 0.6204(3) 1.0466(2) 0.9204(2) 0.0677(7) Uani 1 1 d . . .
O4 O 0.2927(2) 0.99616(19) 0.56284(19) 0.0567(6) Uani 1 1 d . . .
O5 O 1.1779(3) 0.8493(2) 0.4141(2) 0.0734(8) Uani 1 1 d . . .
O6 O 0.8301(2) 0.43173(19) 0.37832(17) 0.0524(6) Uani 1 1 d . . .
C1 C 0.9103(3) 0.5121(3) 0.7734(2) 0.0448(7) Uani 1 1 d . . .
H1 H 0.9647 0.5640 0.7459 0.054 Uiso 1 1 calc R . .
C2 C 0.9579(3) 0.4099(3) 0.7960(2) 0.0458(7) Uani 1 1 d . . .
H2 H 1.0413 0.3947 0.7855 0.055 Uiso 1 1 calc R . .
C3 C 0.8766(3) 0.3303(3) 0.8350(2) 0.0446(7) Uani 1 1 d . . .
C4 C 0.7513(3) 0.3596(2) 0.8531(2) 0.0455(7) Uani 1 1 d . . .
H4 H 0.6951 0.3093 0.8806 0.055 Uiso 1 1 calc R . .
C5 C 0.7121(3) 0.4642(2) 0.8298(2) 0.0368(6) Uani 1 1 d . . .
C6 C 0.5793(3) 0.4996(2) 0.8467(2) 0.0356(6) Uani 1 1 d . . .
C7 C 0.4906(3) 0.4402(2) 0.9100(2) 0.0398(7) Uani 1 1 d . . .
H7 H 0.5116 0.3760 0.9451 0.048 Uiso 1 1 calc R . .
C8 C 0.3689(3) 0.4782(2) 0.9205(2) 0.0396(7) Uani 1 1 d . . .
C9 C 0.3413(3) 0.5772(3) 0.8684(2) 0.0449(7) Uani 1 1 d . . .
H9 H 0.2618 0.6053 0.8748 0.054 Uiso 1 1 calc R . .
C10 C 0.4347(3) 0.6314(2) 0.8077(2) 0.0459(8) Uani 1 1 d . . .
H10 H 0.4162 0.6970 0.7737 0.055 Uiso 1 1 calc R . .
C11 C 1.0343(4) 0.1917(3) 0.8423(3) 0.0749(13) Uani 1 1 d . . .
H11A H 1.0414 0.1170 0.8593 0.112 Uiso 1 1 calc R . .
H11B H 1.0720 0.2205 0.8811 0.112 Uiso 1 1 calc R . .
H11C H 1.0736 0.2143 0.7781 0.112 Uiso 1 1 calc R . .
C12 C 0.1583(3) 0.4485(4) 0.9835(3) 0.0666(11) Uani 1 1 d . . .
H12A H 0.1082 0.3994 1.0300 0.100 Uiso 1 1 calc R . .
H12B H 0.1420 0.4506 0.9233 0.100 Uiso 1 1 calc R . .
H12C H 0.1407 0.5164 0.9981 0.100 Uiso 1 1 calc R . .
C13 C 0.7332(3) 0.7966(3) 0.8562(2) 0.0516(8) Uani 1 1 d . . .
H13 H 0.7847 0.7391 0.8726 0.062 Uiso 1 1 calc R . .
C14 C 0.7166(3) 0.8750(3) 0.9061(2) 0.0546(9) Uani 1 1 d . . .
H14 H 0.7552 0.8697 0.9553 0.066 Uiso 1 1 calc R . .
C15 C 0.6406(3) 0.9622(3) 0.8808(2) 0.0469(8) Uani 1 1 d . . .
C16 C 0.5804(3) 0.9652(2) 0.8071(2) 0.0430(7) Uani 1 1 d . . .
H16 H 0.5280 1.0217 0.7898 0.052 Uiso 1 1 calc R . .
C17 C 0.6010(3) 0.8825(2) 0.7614(2) 0.0350(6) Uani 1 1 d . . .
C18 C 0.5402(3) 0.8787(2) 0.6826(2) 0.0350(6) Uani 1 1 d . . .
C19 C 0.4428(3) 0.9478(2) 0.6620(2) 0.0391(7) Uani 1 1 d . . .
H19 H 0.4140 0.9997 0.6956 0.047 Uiso 1 1 calc R . .
C20 C 0.3893(3) 0.9367(2) 0.5892(2) 0.0418(7) Uani 1 1 d . . .
C21 C 0.4378(3) 0.8589(2) 0.5393(2) 0.0436(7) Uani 1 1 d . . .
H21 H 0.4062 0.8514 0.4896 0.052 Uiso 1 1 calc R . .
C22 C 0.5333(3) 0.7936(2) 0.5650(2) 0.0415(7) Uani 1 1 d . . .
H22 H 0.5640 0.7416 0.5319 0.050 Uiso 1 1 calc R . .
C23 C 0.6833(4) 1.0481(4) 0.9944(3) 0.0756(12) Uani 1 1 d . . .
H23A H 0.6608 1.1120 1.0160 0.113 Uiso 1 1 calc R . .
H23B H 0.7693 1.0434 0.9705 0.113 Uiso 1 1 calc R . .
H23C H 0.6611 0.9901 1.0452 0.113 Uiso 1 1 calc R . .
C24 C 0.2346(4) 1.0738(3) 0.6151(3) 0.0678(11) Uani 1 1 d . . .
H24A H 0.1683 1.1094 0.5886 0.102 Uiso 1 1 calc R . .
H24B H 0.2922 1.1231 0.6124 0.102 Uiso 1 1 calc R . .
H24C H 0.2046 1.0406 0.6790 0.102 Uiso 1 1 calc R . .
C25 C 0.9411(3) 0.8102(3) 0.6228(3) 0.0490(8) Uani 1 1 d . . .
H25 H 0.9167 0.8375 0.6763 0.059 Uiso 1 1 calc R . .
C26 C 1.0417(3) 0.8487(3) 0.5572(3) 0.0549(9) Uani 1 1 d . . .
H26 H 1.0846 0.8997 0.5673 0.066 Uiso 1 1 calc R . .
C27 C 1.0777(3) 0.8098(3) 0.4759(2) 0.0482(8) Uani 1 1 d . . .
C28 C 1.0120(3) 0.7309(2) 0.4643(2) 0.0409(7) Uani 1 1 d . . .
H28 H 1.0343 0.7030 0.4109 0.049 Uiso 1 1 calc R . .
C29 C 0.9124(3) 0.6953(2) 0.5346(2) 0.0346(6) Uani 1 1 d . . .
C30 C 0.8375(2) 0.6108(2) 0.5269(2) 0.0331(6) Uani 1 1 d . . .
C31 C 0.8699(3) 0.5556(2) 0.4562(2) 0.0376(6) Uani 1 1 d . . .
H31 H 0.9417 0.5681 0.4119 0.045 Uiso 1 1 calc R . .
C32 C 0.7930(3) 0.4800(2) 0.4516(2) 0.0394(7) Uani 1 1 d . . .
C33 C 0.6886(3) 0.4612(2) 0.5203(2) 0.0450(7) Uani 1 1 d . . .
H33 H 0.6366 0.4115 0.5201 0.054 Uiso 1 1 calc R . .
C34 C 0.6637(3) 0.5191(2) 0.5898(2) 0.0456(7) Uani 1 1 d . . .
H34 H 0.5938 0.5063 0.6361 0.055 Uiso 1 1 calc R . .
C35 C 1.2140(4) 0.8155(4) 0.3260(3) 0.0865(15) Uani 1 1 d . . .
H35A H 1.2856 0.8492 0.2894 0.130 Uiso 1 1 calc R . .
H35B H 1.1498 0.8335 0.2925 0.130 Uiso 1 1 calc R . .
H35C H 1.2307 0.7413 0.3377 0.130 Uiso 1 1 calc R . .
C36 C 0.7490(4) 0.3609(3) 0.3657(3) 0.0646(10) Uani 1 1 d . . .
H36A H 0.7855 0.3322 0.3119 0.097 Uiso 1 1 calc R . .
H36B H 0.6737 0.3982 0.3567 0.097 Uiso 1 1 calc R . .
H36C H 0.7340 0.3056 0.4200 0.097 Uiso 1 1 calc R . .
P1 P 0.39072(9) 0.28911(8) 0.72459(8) 0.0554(3) Uani 1 1 d . . .
P2 P 0.09806(10) 0.83612(9) 0.85494(8) 0.0621(3) Uani 1 1 d . . .
F1 F 0.4787(4) 0.2478(6) 0.6449(4) 0.221(3) Uani 1 1 d . . .
F2 F 0.3617(5) 0.1720(3) 0.7694(4) 0.1598(19) Uani 1 1 d . . .
F3 F 0.2816(3) 0.2940(2) 0.6733(3) 0.1092(11) Uani 1 1 d . . .
F4 F 0.2995(4) 0.3257(4) 0.8055(3) 0.176(2) Uani 1 1 d . . .
F5 F 0.4150(4) 0.4055(3) 0.6819(4) 0.187(2) Uani 1 1 d . . .
F6 F 0.4994(3) 0.2851(4) 0.7734(3) 0.1495(18) Uani 1 1 d . . .
F7 F 0.2074(3) 0.8128(2) 0.7730(2) 0.0961(9) Uani 1 1 d . . .
F8 F 0.0399(4) 0.7343(3) 0.8460(3) 0.1318(14) Uani 1 1 d . . .
F9 F 0.0264(3) 0.9066(3) 0.7805(2) 0.0978(9) Uani 1 1 d . . .
F10 F -0.0111(4) 0.8562(5) 0.9357(3) 0.186(3) Uani 1 1 d . . .
F11 F 0.1603(4) 0.9372(3) 0.8579(3) 0.1363(16) Uani 1 1 d . . .
F12 F 0.1699(3) 0.7664(3) 0.9297(2) 0.1154(12) 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
Zn1 0.0367(2) 0.0353(2) 0.0382(2) -0.00855(14) -0.00426(14) -0.00220(14)
N1 0.0356(13) 0.0401(13) 0.0369(13) -0.0079(11) -0.0045(10) 0.0003(10)
N2 0.0346(13) 0.0370(13) 0.0415(14) -0.0048(11) -0.0021(10) -0.0016(10)
N3 0.0438(14) 0.0404(14) 0.0412(14) -0.0090(11) -0.0140(11) 0.0011(11)
N4 0.0444(14) 0.0341(12) 0.0338(13) -0.0066(10) -0.0075(10) -0.0041(10)
N5 0.0385(13) 0.0400(13) 0.0410(14) -0.0109(11) -0.0065(11) -0.0060(11)
N6 0.0354(13) 0.0368(13) 0.0413(14) -0.0124(11) -0.0012(10) -0.0077(10)
O1 0.0490(14) 0.0473(13) 0.0743(17) -0.0076(12) -0.0073(12) 0.0150(11)
O2 0.0368(12) 0.0618(15) 0.0531(14) 0.0058(11) 0.0016(10) -0.0076(10)
O3 0.094(2) 0.0603(16) 0.0652(17) -0.0314(13) -0.0331(15) -0.0008(14)
O4 0.0553(14) 0.0511(14) 0.0729(17) -0.0148(12) -0.0338(13) 0.0046(11)
O5 0.0628(17) 0.094(2) 0.0631(17) -0.0160(15) 0.0076(13) -0.0497(16)
O6 0.0517(13) 0.0592(14) 0.0538(14) -0.0311(12) -0.0037(11) -0.0113(11)
C1 0.0323(15) 0.0525(19) 0.0464(18) -0.0068(15) -0.0050(13) -0.0045(13)
C2 0.0339(15) 0.0562(19) 0.0442(18) -0.0115(15) -0.0052(13) 0.0060(14)
C3 0.0453(17) 0.0471(18) 0.0372(16) -0.0088(14) -0.0060(13) 0.0094(14)
C4 0.0410(16) 0.0408(17) 0.0483(18) -0.0043(14) -0.0028(14) -0.0003(13)
C5 0.0354(15) 0.0406(16) 0.0323(15) -0.0091(12) -0.0034(11) 0.0016(12)
C6 0.0364(15) 0.0368(15) 0.0334(15) -0.0089(12) -0.0063(11) -0.0004(12)
C7 0.0395(16) 0.0407(16) 0.0357(16) -0.0046(12) -0.0057(12) 0.0003(12)
C8 0.0377(15) 0.0458(17) 0.0334(15) -0.0087(13) -0.0018(12) -0.0054(13)
C9 0.0324(15) 0.0468(18) 0.0498(18) -0.0085(14) -0.0009(13) 0.0023(13)
C10 0.0369(16) 0.0384(16) 0.056(2) -0.0032(14) -0.0054(14) 0.0025(13)
C11 0.057(2) 0.068(3) 0.087(3) -0.011(2) -0.007(2) 0.027(2)
C12 0.0381(18) 0.085(3) 0.064(2) 0.005(2) -0.0022(16) -0.0107(18)
C13 0.057(2) 0.054(2) 0.0471(19) -0.0101(16) -0.0223(16) 0.0073(16)
C14 0.062(2) 0.066(2) 0.0435(19) -0.0146(17) -0.0237(16) -0.0004(18)
C15 0.0514(19) 0.0523(19) 0.0408(17) -0.0143(15) -0.0097(14) -0.0092(15)
C16 0.0464(17) 0.0424(17) 0.0427(17) -0.0106(13) -0.0134(14) -0.0003(13)
C17 0.0360(15) 0.0358(15) 0.0326(15) -0.0050(12) -0.0060(11) -0.0065(12)
C18 0.0358(15) 0.0323(14) 0.0350(15) -0.0030(12) -0.0052(12) -0.0076(11)
C19 0.0410(16) 0.0324(14) 0.0441(17) -0.0075(12) -0.0099(13) -0.0031(12)
C20 0.0419(17) 0.0368(15) 0.0463(18) 0.0005(13) -0.0151(14) -0.0086(13)
C21 0.0493(18) 0.0452(17) 0.0399(17) -0.0060(14) -0.0149(14) -0.0127(14)
C22 0.0505(18) 0.0390(16) 0.0356(16) -0.0080(13) -0.0085(13) -0.0068(13)
C23 0.093(3) 0.083(3) 0.069(3) -0.035(2) -0.032(2) -0.009(2)
C24 0.060(2) 0.057(2) 0.090(3) -0.018(2) -0.029(2) 0.0133(18)
C25 0.0484(18) 0.0497(19) 0.054(2) -0.0192(16) -0.0078(15) -0.0129(15)
C26 0.055(2) 0.054(2) 0.063(2) -0.0175(17) -0.0144(17) -0.0210(16)
C27 0.0412(17) 0.0543(19) 0.0492(19) -0.0073(15) -0.0071(14) -0.0171(15)
C28 0.0369(15) 0.0446(17) 0.0412(17) -0.0071(13) -0.0070(13) -0.0090(13)
C29 0.0352(14) 0.0318(14) 0.0375(15) -0.0047(12) -0.0117(12) -0.0030(11)
C30 0.0307(14) 0.0308(14) 0.0374(15) -0.0038(11) -0.0095(11) -0.0020(11)
C31 0.0327(14) 0.0410(16) 0.0380(16) -0.0096(13) -0.0026(12) -0.0057(12)
C32 0.0391(16) 0.0390(16) 0.0427(17) -0.0138(13) -0.0099(13) -0.0004(12)
C33 0.0424(17) 0.0415(17) 0.0528(19) -0.0135(14) -0.0047(14) -0.0141(13)
C34 0.0404(16) 0.0448(17) 0.0509(19) -0.0159(14) 0.0021(14) -0.0126(13)
C35 0.079(3) 0.114(4) 0.061(3) -0.018(3) 0.013(2) -0.047(3)
C36 0.063(2) 0.068(2) 0.079(3) -0.041(2) -0.020(2) -0.0086(19)
P1 0.0501(5) 0.0531(5) 0.0688(6) -0.0242(5) -0.0146(4) 0.0006(4)
P2 0.0575(6) 0.0721(7) 0.0617(6) -0.0279(5) -0.0152(5) 0.0100(5)
F1 0.099(3) 0.427(9) 0.208(5) -0.247(6) 0.008(3) -0.019(4)
F2 0.220(5) 0.070(2) 0.211(5) 0.007(2) -0.128(4) -0.004(2)
F3 0.095(2) 0.093(2) 0.152(3) -0.008(2) -0.070(2) -0.0036(16)
F4 0.112(3) 0.246(6) 0.201(5) -0.162(5) 0.035(3) -0.040(3)
F5 0.150(4) 0.094(3) 0.304(7) 0.044(3) -0.081(4) -0.062(3)
F6 0.114(3) 0.188(4) 0.211(4) -0.130(4) -0.102(3) 0.043(3)
F7 0.0837(18) 0.101(2) 0.098(2) -0.0401(17) 0.0141(15) -0.0090(15)
F8 0.140(3) 0.113(3) 0.140(3) -0.007(2) -0.017(2) -0.071(2)
F9 0.102(2) 0.108(2) 0.098(2) -0.0234(17) -0.0558(17) 0.0071(17)
F10 0.138(3) 0.310(7) 0.081(2) -0.060(3) -0.003(2) 0.112(4)
F11 0.169(3) 0.086(2) 0.214(4) -0.077(2) -0.131(3) 0.027(2)
F12 0.141(3) 0.118(2) 0.094(2) -0.0362(18) -0.055(2) 0.060(2)
_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
Zn1 N3 2.137(3) . ?
Zn1 N2 2.176(2) . ?
Zn1 N6 2.184(3) . ?
Zn1 N5 2.190(3) . ?
Zn1 N4 2.204(3) . ?
Zn1 N1 2.251(3) . ?
N1 C5 1.360(4) . ?
N1 C1 1.362(4) . ?
N2 C10 1.361(4) . ?
N2 C6 1.363(4) . ?
N3 C13 1.355(4) . ?
N3 C17 1.365(4) . ?
N4 C18 1.358(4) . ?
N4 C22 1.359(4) . ?
N5 C29 1.349(4) . ?
N5 C25 1.368(4) . ?
N6 C34 1.354(4) . ?
N6 C30 1.354(4) . ?
O1 C3 1.353(4) . ?
O1 C11 1.456(4) . ?
O2 C8 1.357(4) . ?
O2 C12 1.449(4) . ?
O3 C15 1.354(4) . ?
O3 C23 1.459(5) . ?
O4 C20 1.359(4) . ?
O4 C24 1.445(5) . ?
O5 C27 1.360(4) . ?
O5 C35 1.451(5) . ?
O6 C32 1.360(4) . ?
O6 C36 1.452(4) . ?
C1 C2 1.395(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.407(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.413(4) . ?
C4 C5 1.395(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.509(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.404(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(5) . ?
C9 C10 1.375(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.386(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.422(5) . ?
C16 C17 1.391(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.518(4) . ?
C18 C19 1.400(4) . ?
C19 C20 1.411(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.401(5) . ?
C21 C22 1.381(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.393(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.409(4) . ?
C28 C29 1.399(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.514(4) . ?
C30 C31 1.384(4) . ?
C31 C32 1.419(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.384(4) . ?
C33 C34 1.393(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
P1 F1 1.537(4) . ?
P1 F4 1.539(3) . ?
P1 F5 1.552(4) . ?
P1 F6 1.567(3) . ?
P1 F2 1.576(4) . ?
P1 F3 1.592(3) . ?
P2 F10 1.570(3) . ?
P2 F11 1.590(3) . ?
P2 F7 1.594(3) . ?
P2 F9 1.601(3) . ?
P2 F12 1.602(3) . ?
P2 F8 1.606(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
N3 Zn1 N2 93.61(10) . . ?
N3 Zn1 N6 166.01(10) . . ?
N2 Zn1 N6 96.22(9) . . ?
N3 Zn1 N5 96.19(10) . . ?
N2 Zn1 N5 167.51(9) . . ?
N6 Zn1 N5 75.59(9) . . ?
N3 Zn1 N4 76.33(10) . . ?
N2 Zn1 N4 93.03(9) . . ?
N6 Zn1 N4 93.19(10) . . ?
N5 Zn1 N4 96.78(10) . . ?
N3 Zn1 N1 105.47(10) . . ?
N2 Zn1 N1 74.90(9) . . ?
N6 Zn1 N1 86.74(10) . . ?
N5 Zn1 N1 94.98(9) . . ?
N4 Zn1 N1 167.84(9) . . ?
C5 N1 C1 116.7(3) . . ?
C5 N1 Zn1 113.05(19) . . ?
C1 N1 Zn1 125.1(2) . . ?
C10 N2 C6 117.5(2) . . ?
C10 N2 Zn1 125.0(2) . . ?
C6 N2 Zn1 117.33(19) . . ?
C13 N3 C17 118.2(3) . . ?
C13 N3 Zn1 124.6(2) . . ?
C17 N3 Zn1 117.1(2) . . ?
C18 N4 C22 117.6(3) . . ?
C18 N4 Zn1 114.97(19) . . ?
C22 N4 Zn1 126.0(2) . . ?
C29 N5 C25 117.5(3) . . ?
C29 N5 Zn1 116.45(19) . . ?
C25 N5 Zn1 125.7(2) . . ?
C34 N6 C30 117.9(3) . . ?
C34 N6 Zn1 125.4(2) . . ?
C30 N6 Zn1 116.61(19) . . ?
C3 O1 C11 118.9(3) . . ?
C8 O2 C12 117.5(3) . . ?
C15 O3 C23 118.2(3) . . ?
C20 O4 C24 118.8(3) . . ?
C27 O5 C35 118.3(3) . . ?
C32 O6 C36 117.7(3) . . ?
N1 C1 C2 124.5(3) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C1 C2 C3 118.3(3) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
O1 C3 C2 126.1(3) . . ?
O1 C3 C4 116.1(3) . . ?
C2 C3 C4 117.8(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 122.7(3) . . ?
N1 C5 C6 115.2(3) . . ?
C4 C5 C6 122.1(3) . . ?
N2 C6 C7 122.3(3) . . ?
N2 C6 C5 114.9(2) . . ?
C7 C6 C5 122.9(3) . . ?
C6 C7 C8 119.3(3) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
O2 C8 C7 117.4(3) . . ?
O2 C8 C9 123.9(3) . . ?
C7 C8 C9 118.6(3) . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N2 C10 C9 123.9(3) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
O1 C11 H11A 109.5 . . ?
O1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 123.6(3) . . ?
N3 C13 H13 118.2 . . ?
C14 C13 H13 118.2 . . ?
C13 C14 C15 118.5(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
O3 C15 C14 124.9(3) . . ?
O3 C15 C16 116.4(3) . . ?
C14 C15 C16 118.7(3) . . ?
C17 C16 C15 119.1(3) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N3 C17 C16 121.9(3) . . ?
N3 C17 C18 115.4(3) . . ?
C16 C17 C18 122.7(3) . . ?
N4 C18 C19 122.9(3) . . ?
N4 C18 C17 114.9(2) . . ?
C19 C18 C17 122.2(3) . . ?
C18 C19 C20 118.4(3) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
O4 C20 C21 116.3(3) . . ?
O4 C20 C19 125.1(3) . . ?
C21 C20 C19 118.6(3) . . ?
C22 C21 C20 119.0(3) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
N4 C22 C21 123.4(3) . . ?
N4 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
O3 C23 H23A 109.5 . . ?
O3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 C26 123.3(3) . . ?
N5 C25 H25 118.4 . . ?
C26 C25 H25 118.4 . . ?
C25 C26 C27 118.9(3) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
O5 C27 C26 116.7(3) . . ?
O5 C27 C28 124.5(3) . . ?
C26 C27 C28 118.8(3) . . ?
C29 C28 C27 118.6(3) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
N5 C29 C28 122.9(3) . . ?
N5 C29 C30 115.6(2) . . ?
C28 C29 C30 121.5(3) . . ?
N6 C30 C31 121.8(3) . . ?
N6 C30 C29 115.4(2) . . ?
C31 C30 C29 122.8(2) . . ?
C30 C31 C32 119.7(3) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
O6 C32 C33 125.7(3) . . ?
O6 C32 C31 115.7(3) . . ?
C33 C32 C31 118.6(3) . . ?
C32 C33 C34 117.9(3) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
N6 C34 C33 124.0(3) . . ?
N6 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O6 C36 H36A 109.5 . . ?
O6 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O6 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F1 P1 F4 177.3(3) . . ?
F1 P1 F5 95.0(4) . . ?
F4 P1 F5 87.5(3) . . ?
F1 P1 F6 88.8(2) . . ?
F4 P1 F6 92.4(2) . . ?
F5 P1 F6 87.2(3) . . ?
F1 P1 F2 86.6(4) . . ?
F4 P1 F2 90.9(3) . . ?
F5 P1 F2 178.1(3) . . ?
F6 P1 F2 93.8(3) . . ?
F1 P1 F3 90.6(2) . . ?
F4 P1 F3 88.3(2) . . ?
F5 P1 F3 92.2(2) . . ?
F6 P1 F3 179.0(3) . . ?
F2 P1 F3 86.80(19) . . ?
F10 P2 F11 91.6(3) . . ?
F10 P2 F7 178.4(3) . . ?
F11 P2 F7 90.0(2) . . ?
F10 P2 F9 89.4(2) . . ?
F11 P2 F9 88.96(18) . . ?
F7 P2 F9 90.75(18) . . ?
F10 P2 F12 90.4(2) . . ?
F11 P2 F12 90.6(2) . . ?
F7 P2 F12 89.43(18) . . ?
F9 P2 F12 179.6(2) . . ?
F10 P2 F8 91.5(3) . . ?
F11 P2 F8 176.7(2) . . ?
F7 P2 F8 86.91(19) . . ?
F9 P2 F8 90.0(2) . . ?
F12 P2 F8 90.4(2) . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        26.15
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.078


data_(L1)
_database_code_depnum_ccdc_archive 'CCDC 887765'
#TrackingRef 'tmastropietro.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 N2 O2'
_chemical_formula_sum            'C12 H12 N2 O2'
_chemical_formula_weight         216.24
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'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
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                   7.507(5)
_cell_length_b                   12.063(8)
_cell_length_c                   16.970(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.79(2)
_cell_angle_gamma                90.00
_cell_volume                     1526.0(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3755
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      24.30
_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15114
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2649
_reflns_number_gt                1804
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker-Nonius X8 APEX'
_computing_cell_refinement       'Bruker-Nonius X8 APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.0766P)^2^+0.2814P] 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         2649
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1437
_refine_ls_wR_factor_gt          0.1244
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.5404(2) 0.24432(14) 0.89516(9) 0.0379(4) Uani 1 1 d . . .
N2 N 0.4058(2) 0.11146(14) 1.06939(10) 0.0439(5) Uani 1 1 d . . .
N3 N 0.4236(2) 0.43663(15) 0.08689(10) 0.0423(5) Uani 1 1 d . . .
O1 O -0.1170(2) 0.20256(12) 0.86095(9) 0.0479(4) Uani 1 1 d . . .
H1A H -0.2199 0.2143 0.8706 0.072 Uiso 1 1 calc R . .
O2 O 1.0307(2) 0.00762(13) 1.18606(8) 0.0525(5) Uani 1 1 d . . .
H2A H 1.0470 -0.0583 1.1774 0.079 Uiso 1 1 calc R . .
O3 O 1.0623(2) 0.36204(18) 0.06860(9) 0.0663(6) Uani 1 1 d . . .
H3 H 1.1617 0.3910 0.0717 0.100 Uiso 1 1 calc R . .
C1 C 0.4634(3) 0.29784(17) 0.83152(12) 0.0420(5) Uani 1 1 d . . .
H1 H 0.5365 0.3228 0.7946 0.050 Uiso 1 1 calc R . .
C2 C 0.2844(3) 0.31830(17) 0.81703(12) 0.0407(5) Uani 1 1 d . . .
H2 H 0.2373 0.3558 0.7714 0.049 Uiso 1 1 calc R . .
C3 C 0.1732(3) 0.28224(16) 0.87155(12) 0.0363(5) Uani 1 1 d . . .
C4 C 0.2511(3) 0.22700(16) 0.93855(12) 0.0377(5) Uani 1 1 d . . .
H4 H 0.1805 0.2018 0.9763 0.045 Uiso 1 1 calc R . .
C5 C 0.4334(3) 0.20966(15) 0.94887(11) 0.0330(5) Uani 1 1 d . . .
C6 C 0.5191(3) 0.15091(16) 1.02033(11) 0.0351(5) Uani 1 1 d . . .
C7 C 0.7013(3) 0.13709(17) 1.03466(11) 0.0380(5) Uani 1 1 d . . .
H7 H 0.7752 0.1666 0.9997 0.046 Uiso 1 1 calc R . .
C8 C 0.7758(3) 0.07927(16) 1.10118(11) 0.0375(5) Uani 1 1 d . . .
C9 C 0.6583(3) 0.03879(17) 1.15131(12) 0.0435(6) Uani 1 1 d . . .
H9 H 0.7015 -0.0003 1.1968 0.052 Uiso 1 1 calc R . .
C10 C 0.4787(3) 0.05669(19) 1.13346(13) 0.0475(6) Uani 1 1 d . . .
H10 H 0.4025 0.0290 1.1681 0.057 Uiso 1 1 calc R . .
C11 C -0.0238(3) 0.30364(18) 0.86036(14) 0.0451(6) Uani 1 1 d . . .
H11B H -0.0560 0.3510 0.9026 0.054 Uiso 1 1 calc R . .
H11A H -0.0566 0.3413 0.8103 0.054 Uiso 1 1 calc R . .
C12 C 0.9727(3) 0.0618(2) 1.11434(13) 0.0489(6) Uani 1 1 d . . .
H12B H 1.0086 0.0184 1.0708 0.059 Uiso 1 1 calc R . .
H12A H 1.0321 0.1332 1.1139 0.059 Uiso 1 1 calc R . .
C13 C 0.4940(3) 0.38634(19) 0.15332(12) 0.0477(6) Uani 1 1 d . . .
H13 H 0.4160 0.3622 0.1884 0.057 Uiso 1 1 calc R . .
C14 C 0.6711(3) 0.36817(18) 0.17299(12) 0.0425(6) Uani 1 1 d . . .
H14 H 0.7126 0.3343 0.2209 0.051 Uiso 1 1 calc R . .
C15 C 0.7905(3) 0.40060(16) 0.12081(11) 0.0361(5) Uani 1 1 d . . .
C16 C 0.7206(3) 0.45303(16) 0.05158(11) 0.0368(5) Uani 1 1 d . . .
H16 H 0.7963 0.4761 0.0152 0.044 Uiso 1 1 calc R . .
C17 C 0.5392(3) 0.47098(16) 0.03663(11) 0.0340(5) Uani 1 1 d . . .
C18 C 0.9865(3) 0.38153(19) 0.13878(12) 0.0445(6) Uani 1 1 d . . .
H18B H 1.0424 0.4459 0.1656 0.053 Uiso 1 1 calc R . .
H18A H 1.0078 0.3182 0.1739 0.053 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
N1 0.0379(11) 0.0454(10) 0.0304(9) 0.0026(8) 0.0038(8) 0.0028(8)
N2 0.0428(12) 0.0535(11) 0.0359(10) 0.0056(8) 0.0069(8) 0.0015(9)
N3 0.0419(12) 0.0575(11) 0.0276(9) 0.0055(8) 0.0043(8) 0.0000(9)
O1 0.0351(9) 0.0566(10) 0.0527(10) -0.0031(7) 0.0077(8) 0.0016(7)
O2 0.0625(12) 0.0611(10) 0.0308(8) 0.0035(7) -0.0078(7) 0.0102(9)
O3 0.0451(11) 0.1131(15) 0.0415(9) -0.0046(9) 0.0081(8) 0.0043(10)
C1 0.0415(14) 0.0541(13) 0.0314(11) 0.0051(10) 0.0083(10) 0.0006(11)
C2 0.0428(14) 0.0469(12) 0.0316(11) 0.0034(9) 0.0012(10) 0.0050(10)
C3 0.0359(13) 0.0409(11) 0.0316(11) -0.0044(9) 0.0022(9) 0.0021(10)
C4 0.0381(13) 0.0439(11) 0.0317(11) 0.0001(9) 0.0066(9) 0.0003(10)
C5 0.0333(12) 0.0381(11) 0.0273(10) -0.0027(8) 0.0026(9) -0.0003(9)
C6 0.0378(13) 0.0395(11) 0.0279(10) -0.0026(8) 0.0033(9) 0.0018(10)
C7 0.0409(14) 0.0456(12) 0.0279(10) 0.0022(9) 0.0051(9) 0.0013(10)
C8 0.0437(14) 0.0402(11) 0.0274(11) -0.0023(9) -0.0002(9) 0.0009(10)
C9 0.0528(16) 0.0490(13) 0.0285(11) 0.0043(9) 0.0040(11) 0.0009(11)
C10 0.0491(16) 0.0596(14) 0.0352(12) 0.0082(10) 0.0115(11) -0.0030(12)
C11 0.0402(14) 0.0496(13) 0.0452(13) 0.0049(10) 0.0036(11) 0.0053(11)
C12 0.0495(16) 0.0600(14) 0.0361(12) 0.0103(10) 0.0004(11) 0.0082(12)
C13 0.0459(15) 0.0686(15) 0.0292(12) 0.0091(10) 0.0073(10) -0.0027(12)
C14 0.0485(15) 0.0530(13) 0.0251(10) 0.0065(9) 0.0009(10) 0.0002(11)
C15 0.0428(14) 0.0395(11) 0.0254(10) -0.0014(8) 0.0020(9) -0.0002(10)
C16 0.0424(14) 0.0429(11) 0.0259(11) 0.0012(9) 0.0066(9) -0.0009(10)
C17 0.0373(13) 0.0404(11) 0.0242(10) -0.0032(8) 0.0034(9) -0.0013(9)
C18 0.0463(15) 0.0547(13) 0.0323(11) 0.0035(10) 0.0031(10) 0.0039(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
N1 C1 1.331(3) . ?
N1 C5 1.351(3) . ?
N2 C10 1.333(3) . ?
N2 C6 1.346(3) . ?
N3 C13 1.333(3) . ?
N3 C17 1.352(3) . ?
O1 C11 1.406(3) . ?
O1 H1A 0.8200 . ?
O2 C12 1.405(3) . ?
O2 H2A 0.8200 . ?
O3 C18 1.399(2) . ?
O3 H3 0.8200 . ?
C1 C2 1.360(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(3) . ?
C3 C11 1.491(3) . ?
C4 C5 1.375(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.484(3) . ?
C6 C7 1.371(3) . ?
C7 C8 1.387(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(3) . ?
C8 C12 1.483(3) . ?
C9 C10 1.363(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11B 0.9700 . ?
C11 H11A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12A 0.9700 . ?
C13 C14 1.350(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.389(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(3) . ?
C15 C18 1.485(3) . ?
C16 C17 1.372(3) . ?
C16 H16 0.9300 . ?
C17 C17 1.486(4) 3_665 ?
C18 H18B 0.9700 . ?
C18 H18A 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C5 117.48(19) . . ?
C10 N2 C6 116.8(2) . . ?
C13 N3 C17 116.9(2) . . ?
C11 O1 H1A 109.5 . . ?
C12 O2 H2A 109.5 . . ?
C18 O3 H3 109.5 . . ?
N1 C1 C2 124.09(19) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C1 C2 C3 118.8(2) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 118.0(2) . . ?
C4 C3 C11 120.25(19) . . ?
C2 C3 C11 121.77(19) . . ?
C5 C4 C3 119.66(19) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 121.98(18) . . ?
N1 C5 C6 117.65(19) . . ?
C4 C5 C6 120.37(18) . . ?
N2 C6 C7 122.54(19) . . ?
N2 C6 C5 115.44(19) . . ?
C7 C6 C5 122.02(18) . . ?
C6 C7 C8 120.24(19) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 116.9(2) . . ?
C9 C8 C12 123.6(2) . . ?
C7 C8 C12 119.52(19) . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N2 C10 C9 124.0(2) . . ?
N2 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
O1 C11 C3 109.63(17) . . ?
O1 C11 H11B 109.7 . . ?
C3 C11 H11B 109.7 . . ?
O1 C11 H11A 109.7 . . ?
C3 C11 H11A 109.7 . . ?
H11B C11 H11A 108.2 . . ?
O2 C12 C8 113.45(19) . . ?
O2 C12 H12B 108.9 . . ?
C8 C12 H12B 108.9 . . ?
O2 C12 H12A 108.9 . . ?
C8 C12 H12A 108.9 . . ?
H12B C12 H12A 107.7 . . ?
N3 C13 C14 124.3(2) . . ?
N3 C13 H13 117.9 . . ?
C14 C13 H13 117.9 . . ?
C13 C14 C15 119.2(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 117.5(2) . . ?
C16 C15 C18 120.87(18) . . ?
C14 C15 C18 121.60(19) . . ?
C17 C16 C15 119.89(19) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
N3 C17 C16 122.12(19) . . ?
N3 C17 C17 116.8(2) . 3_665 ?
C16 C17 C17 121.0(2) . 3_665 ?
O3 C18 C15 110.13(17) . . ?
O3 C18 H18B 109.6 . . ?
C15 C18 H18B 109.6 . . ?
O3 C18 H18A 109.6 . . ?
C15 C18 H18A 109.6 . . ?
H18B C18 H18A 108.1 . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.053
#===END