Supplementary Material (ESI) for Chemical Communications
This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.
#TrackingRef 'Schulz.cif.txt'
_journal_coden_Cambridge         0182
_publ_contact_author             
;
Prof. Dr. Boese, Roland
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen, Universit\"atsstr. 7
D-45117 Essen, Germany
;
_publ_contact_author_email       roland.boese@.uni-due.de
_publ_contact_author_phone       '++49 (0)201 183 2416'
_publ_contact_author_fax         '++49 (0)201 183 2535'

_publ_section_title              
;
Reactions of a /b/-Diketiminate Zinc Hydride Complex with
Heterocumulenes
;

loop_
_publ_author_name
_publ_author_address
S.Schulz
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
T.Eisenmann
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
R.Haack
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
D.Blaser
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
R.Boese
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;

_publ_requested_coeditor_name    ?
_publ_contact_letter             
;
?
;
_publ_contact_author_name        'Prof. Dr. Boese, Roland'

data_tam_502m
_database_code_depnum_ccdc_archive 'CCDC 776239'
_ccdc_compound_id                1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H60 N4 O4 Zn2'
_chemical_formula_weight         887.74

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'
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

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

_cell_length_a                   10.4571(3)
_cell_length_b                   13.5684(4)
_cell_length_c                   17.0082(5)
_cell_angle_alpha                83.802(2)
_cell_angle_beta                 81.489(2)
_cell_angle_gamma                67.819(2)
_cell_volume                     2206.45(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.33

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
;
BRUKER AXS SMART APEX 2 Vers. 3.0-2009
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;

_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  
;
Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            22387
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.21
_diffrn_reflns_theta_max         24.45
_reflns_number_total             7210
_reflns_number_gt                6563
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_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.
Treatment of hydrogen atoms
Riding model on idealized geometrics
with the 1.2 fold (1.5 fold for methyl
groups) isotropic displacement
parameters of the equivalent Uij of the
corresponding carbon atom
Disorder
Oxygen atom O(4) and hydrogen atom HO(2)
disordered over two sites with SOF 0.5
;

_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^)+(0.0500P)^2^+6.2631P] 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         7210
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1220
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Zn1 Zn 0.36885(4) 0.46748(3) 0.29077(2) 0.01602(13) Uani 1 1 d . . .
Zn2 Zn 0.63945(4) 0.53516(3) 0.18638(3) 0.01975(13) Uani 1 1 d . . .
N1 N 0.1924(3) 0.5762(2) 0.33006(16) 0.0131(6) Uani 1 1 d . . .
N2 N 0.3418(3) 0.3380(2) 0.33750(16) 0.0141(6) Uani 1 1 d . . .
N3 N 0.6769(3) 0.6655(2) 0.16905(16) 0.0131(6) Uani 1 1 d . . .
N4 N 0.8260(3) 0.4284(2) 0.17171(16) 0.0129(6) Uani 1 1 d . . .
CO1 C 0.4376(4) 0.4829(3) 0.1110(2) 0.0210(8) Uani 1 1 d . . .
HO1 H 0.4014 0.4779 0.0539 0.025 Uiso 1 1 d R . .
CO2 C 0.5718(4) 0.5231(3) 0.3543(2) 0.0239(9) Uani 1 1 d . . .
HO2A H 0.5196 0.5159 0.4046 0.029 Uiso 0.50 1 d PR A 1
HO2B H 0.6481 0.5467 0.3522 0.029 Uiso 0.50 1 d PR A 2
O1 O 0.3738(3) 0.4574(2) 0.17151(15) 0.0254(6) Uani 1 1 d . . .
O2 O 0.5291(3) 0.5211(2) 0.10498(16) 0.0270(6) Uani 1 1 d . . .
O3 O 0.5300(3) 0.5105(2) 0.28715(14) 0.0209(5) Uani 1 1 d . B .
O4A O 0.6717(6) 0.5424(4) 0.3529(3) 0.0308(13) Uani 0.50 1 d P B 1
O4B O 0.5176(6) 0.5054(4) 0.4154(3) 0.0321(13) Uani 0.50 1 d P B 2
C1 C 0.0848(3) 0.5465(3) 0.3507(2) 0.0158(7) Uani 1 1 d . . .
C2 C 0.0942(4) 0.4398(3) 0.3577(2) 0.0192(8) Uani 1 1 d . . .
H2 H 0.0068 0.4303 0.3632 0.023 Uiso 1 1 d R . .
C3 C 0.2113(4) 0.3451(3) 0.3581(2) 0.0181(7) Uani 1 1 d . . .
C4 C -0.0580(4) 0.6298(3) 0.3700(2) 0.0251(8) Uani 1 1 d . . .
H4A H -0.0678 0.6502 0.4248 0.038 Uiso 1 1 d R . .
H4B H -0.1288 0.6007 0.3649 0.038 Uiso 1 1 d R . .
H4C H -0.0700 0.6926 0.3333 0.038 Uiso 1 1 d R . .
C5 C 0.1846(4) 0.2440(3) 0.3851(3) 0.0281(9) Uani 1 1 d . . .
H5A H 0.2308 0.1911 0.3450 0.042 Uiso 1 1 d R . .
H5B H 0.0844 0.2591 0.3918 0.042 Uiso 1 1 d R . .
H5C H 0.2218 0.2159 0.4359 0.042 Uiso 1 1 d R . .
C6 C 0.1766(3) 0.6834(3) 0.3434(2) 0.0142(7) Uani 1 1 d . . .
C7 C 0.1729(3) 0.7576(3) 0.2793(2) 0.0162(7) Uani 1 1 d . . .
C8 C 0.1506(4) 0.8619(3) 0.2960(2) 0.0192(8) Uani 1 1 d . . .
H8 H 0.1414 0.9150 0.2528 0.023 Uiso 1 1 d R . .
C9 C 0.1409(4) 0.8913(3) 0.3726(2) 0.0220(8) Uani 1 1 d . . .
C10 C 0.1541(4) 0.8139(3) 0.4343(2) 0.0200(8) Uani 1 1 d . . .
H10 H 0.1514 0.8324 0.4876 0.024 Uiso 1 1 d R . .
C11 C 0.1713(4) 0.7101(3) 0.4213(2) 0.0179(7) Uani 1 1 d . . .
C12 C 0.1972(4) 0.7276(3) 0.1946(2) 0.0207(8) Uani 1 1 d . . .
H12A H 0.2970 0.7033 0.1763 0.031 Uiso 1 1 d R . .
H12B H 0.1473 0.7896 0.1610 0.031 Uiso 1 1 d R . .
H12C H 0.1636 0.6700 0.1911 0.031 Uiso 1 1 d R . .
C13 C 0.1196(5) 1.0047(3) 0.3875(3) 0.0383(11) Uani 1 1 d . . .
H13A H 0.0661 1.0234 0.4397 0.057 Uiso 1 1 d R . .
H13B H 0.0684 1.0528 0.3459 0.057 Uiso 1 1 d R . .
H13C H 0.2099 1.0116 0.3861 0.057 Uiso 1 1 d R . .
C14 C 0.1875(4) 0.6280(3) 0.4901(2) 0.0247(8) Uani 1 1 d . . .
H14A H 0.1866 0.6601 0.5392 0.037 Uiso 1 1 d R . .
H14B H 0.2759 0.5681 0.4798 0.037 Uiso 1 1 d R . .
H14C H 0.1105 0.6023 0.4958 0.037 Uiso 1 1 d R . .
C15 C 0.4503(4) 0.2364(3) 0.3517(2) 0.0153(7) Uani 1 1 d . . .
C16 C 0.4983(4) 0.2110(3) 0.4272(2) 0.0205(8) Uani 1 1 d . . .
C17 C 0.5984(4) 0.1107(3) 0.4415(2) 0.0256(9) Uani 1 1 d . . .
H17 H 0.6318 0.0929 0.4928 0.031 Uiso 1 1 d R . .
C18 C 0.6513(4) 0.0355(3) 0.3839(2) 0.0208(8) Uani 1 1 d . . .
C19 C 0.6046(4) 0.0642(3) 0.3098(2) 0.0181(7) Uani 1 1 d . . .
H19 H 0.6413 0.0136 0.2692 0.022 Uiso 1 1 d R . .
C20 C 0.5062(4) 0.1638(3) 0.2916(2) 0.0160(7) Uani 1 1 d . . .
C21 C 0.4412(5) 0.2900(3) 0.4909(2) 0.0334(10) Uani 1 1 d . . .
H21A H 0.4511 0.3575 0.4707 0.050 Uiso 1 1 d R . .
H21B H 0.4926 0.2617 0.5372 0.050 Uiso 1 1 d R . .
H21C H 0.3427 0.3022 0.5066 0.050 Uiso 1 1 d R . .
C22 C 0.7569(4) -0.0741(3) 0.4013(3) 0.0304(9) Uani 1 1 d . . .
H22A H 0.7100 -0.1249 0.4157 0.046 Uiso 1 1 d R . .
H22B H 0.8052 -0.0712 0.4457 0.046 Uiso 1 1 d R . .
H22C H 0.8245 -0.0969 0.3541 0.046 Uiso 1 1 d R . .
C23 C 0.4627(4) 0.1919(3) 0.2094(2) 0.0262(9) Uani 1 1 d . . .
H23A H 0.5125 0.2350 0.1794 0.039 Uiso 1 1 d R . .
H23B H 0.3624 0.2327 0.2131 0.039 Uiso 1 1 d R . .
H23C H 0.4844 0.1265 0.1820 0.039 Uiso 1 1 d R . .
C31 C 0.8083(4) 0.6586(3) 0.1670(2) 0.0183(8) Uani 1 1 d . . .
C32 C 0.9237(4) 0.5634(3) 0.1731(2) 0.0206(8) Uani 1 1 d . . .
H32 H 1.0076 0.5721 0.1813 0.025 Uiso 1 1 d R . .
C33 C 0.9349(4) 0.4570(3) 0.1697(2) 0.0165(7) Uani 1 1 d . . .
C34 C 0.8371(4) 0.7609(3) 0.1557(3) 0.0290(9) Uani 1 1 d . . .
H34A H 0.8281 0.7897 0.1005 0.043 Uiso 1 1 d R . .
H34B H 0.9315 0.7464 0.1677 0.043 Uiso 1 1 d R . .
H34C H 0.7700 0.8128 0.1919 0.043 Uiso 1 1 d R . .
C35 C 1.0789(4) 0.3729(3) 0.1627(2) 0.0226(8) Uani 1 1 d . . .
H35A H 1.0837 0.3162 0.2044 0.034 Uiso 1 1 d R . .
H35B H 1.1467 0.4046 0.1688 0.034 Uiso 1 1 d R . .
H35C H 1.1001 0.3429 0.1103 0.034 Uiso 1 1 d R . .
C36 C 0.5722(3) 0.7673(3) 0.1511(2) 0.0141(7) Uani 1 1 d . . .
C37 C 0.5438(4) 0.7949(3) 0.0723(2) 0.0204(8) Uani 1 1 d . . .
C38 C 0.4408(4) 0.8922(3) 0.0543(2) 0.0243(8) Uani 1 1 d . . .
H38 H 0.4199 0.9100 0.0003 0.029 Uiso 1 1 d R . .
C39 C 0.3672(4) 0.9638(3) 0.1125(2) 0.0201(8) Uani 1 1 d . . .
C40 C 0.3992(4) 0.9347(3) 0.1898(2) 0.0183(8) Uani 1 1 d . . .
H40 H 0.3504 0.9835 0.2306 0.022 Uiso 1 1 d R . .
C41 C 0.4986(3) 0.8371(3) 0.2110(2) 0.0151(7) Uani 1 1 d . . .
C42 C 0.6254(5) 0.7196(3) 0.0076(2) 0.0318(10) Uani 1 1 d . . .
H42A H 0.7249 0.7053 0.0061 0.048 Uiso 1 1 d R . .
H42B H 0.5946 0.7519 -0.0441 0.048 Uiso 1 1 d R . .
H42C H 0.6092 0.6527 0.0188 0.048 Uiso 1 1 d R . .
C43 C 0.2545(4) 1.0684(3) 0.0924(3) 0.0299(9) Uani 1 1 d . . .
H43A H 0.1635 1.0626 0.1084 0.045 Uiso 1 1 d R . .
H43B H 0.2651 1.0858 0.0350 0.045 Uiso 1 1 d R . .
H43C H 0.2612 1.1249 0.1211 0.045 Uiso 1 1 d R . .
C44 C 0.5236(4) 0.8073(3) 0.2968(2) 0.0223(8) Uani 1 1 d . . .
H44A H 0.4956 0.8722 0.3258 0.033 Uiso 1 1 d R . .
H44B H 0.6225 0.7657 0.2998 0.033 Uiso 1 1 d R . .
H44C H 0.4686 0.7647 0.3205 0.033 Uiso 1 1 d R . .
C45 C 0.8456(3) 0.3212(3) 0.1556(2) 0.0145(7) Uani 1 1 d . . .
C46 C 0.8433(3) 0.2459(3) 0.2181(2) 0.0164(7) Uani 1 1 d . . .
C47 C 0.8552(4) 0.1451(3) 0.1995(2) 0.0210(8) Uani 1 1 d . . .
H47 H 0.8569 0.0922 0.2420 0.025 Uiso 1 1 d R . .
C48 C 0.8644(4) 0.1186(3) 0.1223(2) 0.0232(8) Uani 1 1 d . . .
C49 C 0.8645(4) 0.1956(3) 0.0613(2) 0.0230(8) Uani 1 1 d . . .
H49A H 0.8707 0.1783 0.0072 0.028 Uiso 1 1 d R . .
C50 C 0.8566(4) 0.2968(3) 0.0762(2) 0.0183(7) Uani 1 1 d . . .
C52 C 0.8718(5) 0.0092(3) 0.1049(3) 0.0384(11) Uani 1 1 d . . .
H52A H 0.9310 -0.0448 0.1405 0.058 Uiso 1 1 d R . .
H52B H 0.9111 -0.0052 0.0495 0.058 Uiso 1 1 d R . .
H52C H 0.7782 0.0068 0.1134 0.058 Uiso 1 1 d R . .
C51 C 0.8262(4) 0.2720(3) 0.3034(2) 0.0237(8) Uani 1 1 d . . .
H51A H 0.8644 0.3268 0.3073 0.035 Uiso 1 1 d R . .
H51B H 0.8755 0.2077 0.3352 0.035 Uiso 1 1 d R . .
H51C H 0.7271 0.2985 0.3235 0.035 Uiso 1 1 d R . .
C53 C 0.8612(5) 0.3778(3) 0.0086(2) 0.0282(9) Uani 1 1 d . . .
H53A H 0.9494 0.3889 0.0046 0.042 Uiso 1 1 d R . .
H53B H 0.7837 0.4454 0.0191 0.042 Uiso 1 1 d R . .
H53C H 0.8536 0.3519 -0.0414 0.042 Uiso 1 1 d 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
Zn1 0.0122(2) 0.0103(2) 0.0247(2) -0.00024(16) 0.00076(16) -0.00436(17)
Zn2 0.0108(2) 0.0108(2) 0.0372(3) -0.00095(18) -0.00021(17) -0.00453(17)
N1 0.0173(15) 0.0098(14) 0.0119(14) -0.0007(11) -0.0008(11) -0.0049(12)
N2 0.0176(15) 0.0105(14) 0.0132(14) 0.0003(11) 0.0003(11) -0.0050(12)
N3 0.0140(14) 0.0108(14) 0.0133(14) 0.0010(11) -0.0005(11) -0.0039(12)
N4 0.0140(14) 0.0115(14) 0.0130(14) -0.0010(11) -0.0020(11) -0.0043(12)
CO1 0.0188(19) 0.0187(19) 0.027(2) -0.0014(15) -0.0055(15) -0.0078(16)
CO2 0.022(2) 0.019(2) 0.033(2) -0.0063(16) -0.0094(17) -0.0054(17)
O1 0.0306(15) 0.0285(15) 0.0200(14) -0.0013(11) -0.0005(11) -0.0150(13)
O2 0.0239(14) 0.0315(15) 0.0274(15) 0.0009(12) -0.0021(11) -0.0134(13)
O3 0.0201(13) 0.0246(14) 0.0203(13) -0.0021(11) -0.0043(10) -0.0098(11)
O4A 0.031(3) 0.026(3) 0.036(3) -0.001(2) 0.007(2) -0.016(3)
O4B 0.041(3) 0.032(3) 0.011(3) 0.001(2) 0.004(2) -0.002(3)
C1 0.0147(17) 0.0156(18) 0.0149(17) -0.0017(14) 0.0022(13) -0.0044(15)
C2 0.0150(17) 0.0182(19) 0.0250(19) 0.0009(15) 0.0021(14) -0.0089(15)
C3 0.0202(19) 0.0146(18) 0.0204(18) -0.0012(14) 0.0009(14) -0.0084(15)
C4 0.0149(18) 0.019(2) 0.040(2) -0.0041(17) 0.0030(16) -0.0055(16)
C5 0.022(2) 0.019(2) 0.043(2) 0.0021(17) 0.0019(17) -0.0102(17)
C6 0.0120(16) 0.0108(17) 0.0184(18) -0.0015(13) -0.0006(13) -0.0029(14)
C7 0.0107(16) 0.0144(18) 0.0224(18) 0.0004(14) -0.0019(14) -0.0038(14)
C8 0.0156(18) 0.0145(18) 0.027(2) 0.0036(15) -0.0033(15) -0.0058(15)
C9 0.0172(18) 0.0143(19) 0.035(2) -0.0066(16) -0.0009(15) -0.0056(15)
C10 0.0161(18) 0.023(2) 0.0210(19) -0.0096(15) -0.0015(14) -0.0046(16)
C11 0.0159(17) 0.0178(19) 0.0183(18) -0.0011(14) -0.0026(14) -0.0042(15)
C12 0.0247(19) 0.0187(19) 0.0206(19) 0.0037(15) -0.0054(15) -0.0103(16)
C13 0.050(3) 0.021(2) 0.044(3) -0.0092(19) -0.002(2) -0.014(2)
C14 0.032(2) 0.025(2) 0.0131(18) -0.0004(15) -0.0025(15) -0.0065(18)
C15 0.0172(18) 0.0111(17) 0.0160(17) 0.0025(13) 0.0005(14) -0.0052(15)
C16 0.028(2) 0.0162(19) 0.0160(18) 0.0008(14) -0.0035(15) -0.0075(16)
C17 0.032(2) 0.023(2) 0.0201(19) 0.0063(16) -0.0101(16) -0.0074(18)
C18 0.0221(19) 0.0141(18) 0.0237(19) 0.0034(15) -0.0027(15) -0.0050(16)
C19 0.0193(18) 0.0157(18) 0.0183(18) -0.0039(14) 0.0004(14) -0.0054(15)
C20 0.0173(18) 0.0134(17) 0.0172(18) -0.0005(14) -0.0010(14) -0.0060(15)
C21 0.050(3) 0.024(2) 0.020(2) -0.0016(17) -0.0068(18) -0.006(2)
C22 0.032(2) 0.017(2) 0.035(2) 0.0035(17) -0.0094(18) 0.0003(18)
C23 0.039(2) 0.017(2) 0.0184(19) -0.0034(15) -0.0080(17) -0.0032(17)
C31 0.0189(18) 0.0149(18) 0.0217(19) 0.0005(14) 0.0003(14) -0.0083(15)
C32 0.0151(18) 0.0173(19) 0.030(2) -0.0004(15) -0.0003(15) -0.0077(15)
C33 0.0162(17) 0.0162(18) 0.0154(17) -0.0006(14) 0.0024(13) -0.0056(15)
C34 0.0177(19) 0.018(2) 0.052(3) -0.0002(18) -0.0009(18) -0.0087(17)
C35 0.0144(18) 0.0182(19) 0.033(2) -0.0014(16) 0.0005(15) -0.0045(16)
C36 0.0151(17) 0.0109(17) 0.0162(17) 0.0005(13) 0.0005(13) -0.0060(14)
C37 0.028(2) 0.0175(19) 0.0149(18) 0.0003(14) -0.0012(15) -0.0076(16)
C38 0.032(2) 0.021(2) 0.0183(19) 0.0074(15) -0.0097(16) -0.0084(17)
C39 0.0182(18) 0.0163(19) 0.0247(19) 0.0047(15) -0.0028(15) -0.0066(15)
C40 0.0174(18) 0.0140(18) 0.0222(19) -0.0022(14) 0.0022(14) -0.0055(15)
C41 0.0134(17) 0.0141(17) 0.0189(18) 0.0000(14) -0.0017(13) -0.0066(14)
C42 0.051(3) 0.024(2) 0.0152(19) -0.0010(16) -0.0046(18) -0.008(2)
C43 0.027(2) 0.024(2) 0.034(2) 0.0068(17) -0.0078(17) -0.0034(18)
C44 0.028(2) 0.0179(19) 0.0178(19) -0.0039(15) -0.0047(15) -0.0031(16)
C45 0.0117(16) 0.0114(17) 0.0186(18) -0.0025(13) -0.0025(13) -0.0016(14)
C46 0.0129(17) 0.0150(18) 0.0203(18) 0.0006(14) -0.0027(14) -0.0040(14)
C47 0.0161(18) 0.0137(18) 0.031(2) 0.0037(15) -0.0013(15) -0.0047(15)
C48 0.0184(19) 0.0162(19) 0.035(2) -0.0086(16) -0.0001(16) -0.0060(16)
C49 0.0211(19) 0.021(2) 0.023(2) -0.0097(16) -0.0025(15) -0.0022(16)
C50 0.0194(18) 0.0153(18) 0.0177(18) -0.0044(14) -0.0020(14) -0.0025(15)
C52 0.047(3) 0.021(2) 0.050(3) -0.013(2) 0.001(2) -0.015(2)
C51 0.031(2) 0.0189(19) 0.0181(19) 0.0040(15) -0.0021(15) -0.0077(17)
C53 0.043(2) 0.022(2) 0.0134(18) -0.0026(15) -0.0031(16) -0.0057(19)

_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 N2 1.950(3) . ?
Zn1 N1 1.954(3) . ?
Zn1 O3 1.971(2) . ?
Zn1 O1 2.039(3) . ?
Zn2 N3 1.935(3) . ?
Zn2 N4 1.941(3) . ?
Zn2 O3 1.986(2) . ?
Zn2 O2 1.995(3) . ?
N1 C1 1.321(4) . ?
N1 C6 1.440(4) . ?
N2 C3 1.326(4) . ?
N2 C15 1.440(4) . ?
N3 C31 1.337(4) . ?
N3 C36 1.437(4) . ?
N4 C33 1.330(4) . ?
N4 C45 1.441(4) . ?
CO1 O1 1.233(4) . ?
CO1 O2 1.236(4) . ?
CO2 O4B 1.154(7) . ?
CO2 O4A 1.165(7) . ?
CO2 O3 1.332(5) . ?
C1 C2 1.407(5) . ?
C1 C4 1.509(5) . ?
C2 C3 1.401(5) . ?
C3 C5 1.512(5) . ?
C6 C7 1.397(5) . ?
C6 C11 1.398(5) . ?
C7 C8 1.399(5) . ?
C7 C12 1.498(5) . ?
C8 C9 1.383(5) . ?
C9 C10 1.384(5) . ?
C9 C13 1.514(5) . ?
C10 C11 1.389(5) . ?
C11 C14 1.508(5) . ?
C15 C20 1.401(5) . ?
C15 C16 1.409(5) . ?
C16 C17 1.391(5) . ?
C16 C21 1.502(5) . ?
C17 C18 1.392(5) . ?
C18 C19 1.382(5) . ?
C18 C22 1.510(5) . ?
C19 C20 1.391(5) . ?
C20 C23 1.500(5) . ?
C31 C32 1.402(5) . ?
C31 C34 1.515(5) . ?
C32 C33 1.410(5) . ?
C33 C35 1.504(5) . ?
C36 C37 1.397(5) . ?
C36 C41 1.396(5) . ?
C37 C38 1.391(5) . ?
C37 C42 1.514(5) . ?
C38 C39 1.391(5) . ?
C39 C40 1.383(5) . ?
C39 C43 1.508(5) . ?
C40 C41 1.390(5) . ?
C41 C44 1.505(5) . ?
C45 C46 1.396(5) . ?
C45 C50 1.401(5) . ?
C46 C47 1.393(5) . ?
C46 C51 1.501(5) . ?
C47 C48 1.378(5) . ?
C48 C49 1.391(5) . ?
C48 C52 1.516(5) . ?
C49 C50 1.394(5) . ?
C50 C53 1.511(5) . ?

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 Zn1 N1 100.83(11) . . ?
N2 Zn1 O3 129.93(11) . . ?
N1 Zn1 O3 113.58(11) . . ?
N2 Zn1 O1 103.71(11) . . ?
N1 Zn1 O1 109.07(11) . . ?
O3 Zn1 O1 98.24(10) . . ?
N3 Zn2 N4 101.33(11) . . ?
N3 Zn2 O3 119.16(11) . . ?
N4 Zn2 O3 113.20(11) . . ?
N3 Zn2 O2 112.34(11) . . ?
N4 Zn2 O2 109.21(11) . . ?
O3 Zn2 O2 101.69(10) . . ?
C1 N1 C6 118.7(3) . . ?
C1 N1 Zn1 117.5(2) . . ?
C6 N1 Zn1 123.7(2) . . ?
C3 N2 C15 117.6(3) . . ?
C3 N2 Zn1 116.6(2) . . ?
C15 N2 Zn1 125.9(2) . . ?
C31 N3 C36 118.8(3) . . ?
C31 N3 Zn2 118.2(2) . . ?
C36 N3 Zn2 122.8(2) . . ?
C33 N4 C45 120.5(3) . . ?
C33 N4 Zn2 119.5(2) . . ?
C45 N4 Zn2 119.7(2) . . ?
O1 CO1 O2 129.1(4) . . ?
O4B CO2 O4A 118.4(5) . . ?
O4B CO2 O3 120.6(5) . . ?
O4A CO2 O3 120.7(5) . . ?
CO1 O1 Zn1 135.1(2) . . ?
CO1 O2 Zn2 130.8(2) . . ?
CO2 O3 Zn1 120.3(2) . . ?
CO2 O3 Zn2 116.5(2) . . ?
Zn1 O3 Zn2 123.25(12) . . ?
N1 C1 C2 124.0(3) . . ?
N1 C1 C4 119.6(3) . . ?
C2 C1 C4 116.4(3) . . ?
C3 C2 C1 130.0(3) . . ?
N2 C3 C2 125.2(3) . . ?
N2 C3 C5 118.4(3) . . ?
C2 C3 C5 116.4(3) . . ?
C7 C6 C11 120.8(3) . . ?
C7 C6 N1 120.4(3) . . ?
C11 C6 N1 118.7(3) . . ?
C6 C7 C8 117.9(3) . . ?
C6 C7 C12 122.1(3) . . ?
C8 C7 C12 119.9(3) . . ?
C9 C8 C7 122.2(3) . . ?
C8 C9 C10 118.2(3) . . ?
C8 C9 C13 120.2(4) . . ?
C10 C9 C13 121.6(4) . . ?
C9 C10 C11 121.9(3) . . ?
C10 C11 C6 118.7(3) . . ?
C10 C11 C14 120.1(3) . . ?
C6 C11 C14 121.2(3) . . ?
C20 C15 C16 120.6(3) . . ?
C20 C15 N2 120.5(3) . . ?
C16 C15 N2 118.9(3) . . ?
C17 C16 C15 118.4(3) . . ?
C17 C16 C21 120.9(3) . . ?
C15 C16 C21 120.7(3) . . ?
C16 C17 C18 122.0(3) . . ?
C19 C18 C17 118.0(3) . . ?
C19 C18 C22 120.8(3) . . ?
C17 C18 C22 121.3(3) . . ?
C18 C19 C20 122.6(3) . . ?
C19 C20 C15 118.2(3) . . ?
C19 C20 C23 120.3(3) . . ?
C15 C20 C23 121.4(3) . . ?
N3 C31 C32 125.2(3) . . ?
N3 C31 C34 118.2(3) . . ?
C32 C31 C34 116.6(3) . . ?
C31 C32 C33 130.0(3) . . ?
N4 C33 C32 123.5(3) . . ?
N4 C33 C35 119.2(3) . . ?
C32 C33 C35 117.3(3) . . ?
C37 C36 C41 120.3(3) . . ?
C37 C36 N3 118.5(3) . . ?
C41 C36 N3 121.2(3) . . ?
C38 C37 C36 119.2(3) . . ?
C38 C37 C42 120.7(3) . . ?
C36 C37 C42 120.1(3) . . ?
C37 C38 C39 121.7(3) . . ?
C40 C39 C38 117.6(3) . . ?
C40 C39 C43 121.2(3) . . ?
C38 C39 C43 121.2(3) . . ?
C39 C40 C41 122.7(3) . . ?
C40 C41 C36 118.4(3) . . ?
C40 C41 C44 120.3(3) . . ?
C36 C41 C44 121.2(3) . . ?
C46 C45 C50 120.9(3) . . ?
C46 C45 N4 120.4(3) . . ?
C50 C45 N4 118.5(3) . . ?
C47 C46 C45 118.3(3) . . ?
C47 C46 C51 120.1(3) . . ?
C45 C46 C51 121.7(3) . . ?
C48 C47 C46 122.4(3) . . ?
C47 C48 C49 118.1(3) . . ?
C47 C48 C52 120.7(4) . . ?
C49 C48 C52 121.2(4) . . ?
C48 C49 C50 121.9(3) . . ?
C49 C50 C45 118.3(3) . . ?
C49 C50 C53 120.8(3) . . ?
C45 C50 C53 120.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        24.45
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.906
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.084
_vrf_PLAT312_tam_502m            
;
PROBLEM: Strange C-O-H Geometry (C-O .LT. 1.25 Ang) ..... O4A/O4B
RESPONSE:
Oxygen atom O(4) and hydrogen atom HO(2)
disordered over two sites with SOF 0.5
;

data_tam_519m
_database_code_depnum_ccdc_archive 'CCDC 776240'
#TrackingRef 'Schulz.cif.txt'

_ccdc_compound_id                2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 N4 Zn, 0.5 C6 H14'
_chemical_formula_sum            'C33 H51 N4 Zn'
_chemical_formula_weight         569.15

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   12.9606(16)
_cell_length_b                   13.4781(17)
_cell_length_c                   18.614(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.476(5)
_cell_angle_gamma                90.00
_cell_volume                     3186.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6486
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      23.67

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1228
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
;
BRUKER AXS SMART APEX 2 Vers. 3.0-2009
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;

_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  
;
Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            21158
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         23.93
_reflns_number_total             4760
_reflns_number_gt                3327
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_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.
Treatment of hydrogen atoms
Riding model on idealized geometrics
with the 1.2 fold (1.5 fold for methyl
groups) isotropic displacement
parameters of the equivalent Uij of the
corresponding carbon atom
Hydrogen atom position H(24) taken from
a Fourier-map and also refined as riding
group with the 1.2 fold isotropic
displacement parameters of the
equivalent Uij of the corresponding
carbon atom.
;

_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^)+(0.0391P)^2^+9.9605P] 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         4760
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1343
_refine_ls_wR_factor_gt          0.1162
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 0.67488(4) 0.54193(4) 0.17349(3) 0.02022(18) Uani 1 1 d . . .
N1 N 0.6031(3) 0.4361(2) 0.2175(2) 0.0197(9) Uani 1 1 d . . .
N2 N 0.7920(3) 0.4608(3) 0.1529(2) 0.0203(9) Uani 1 1 d . . .
N3 N 0.6914(3) 0.6843(3) 0.2084(2) 0.0205(9) Uani 1 1 d . . .
N4 N 0.5914(3) 0.6449(3) 0.1000(2) 0.0219(9) Uani 1 1 d . . .
C1 C 0.6239(4) 0.3406(3) 0.2069(3) 0.0218(11) Uani 1 1 d . . .
C2 C 0.7039(4) 0.3086(3) 0.1720(3) 0.0233(12) Uani 1 1 d . . .
H2A H 0.7025 0.2396 0.1601 0.028 Uiso 1 1 d R . .
C3 C 0.7853(4) 0.3623(3) 0.1518(3) 0.0233(11) Uani 1 1 d . . .
C4 C 0.5607(4) 0.2622(3) 0.2367(3) 0.0253(12) Uani 1 1 d . . .
H4A H 0.5843 0.2579 0.2897 0.038 Uiso 1 1 d R . .
H4B H 0.5714 0.1985 0.2145 0.038 Uiso 1 1 d R . .
H4C H 0.4859 0.2794 0.2253 0.038 Uiso 1 1 d R . .
C5 C 0.8726(4) 0.3034(3) 0.1289(3) 0.0287(12) Uani 1 1 d . . .
H5A H 0.8941 0.3356 0.0873 0.043 Uiso 1 1 d R . .
H5B H 0.8470 0.2367 0.1150 0.043 Uiso 1 1 d R . .
H5C H 0.9330 0.2994 0.1695 0.043 Uiso 1 1 d R . .
C6 C 0.5313(3) 0.4609(3) 0.2637(2) 0.0189(10) Uani 1 1 d . . .
C7 C 0.4260(4) 0.4794(3) 0.2338(3) 0.0200(11) Uani 1 1 d . . .
C8 C 0.3581(4) 0.5053(3) 0.2802(3) 0.0211(11) Uani 1 1 d . . .
H8A H 0.2857 0.5180 0.2595 0.025 Uiso 1 1 d R . .
C9 C 0.3929(4) 0.5138(3) 0.3555(3) 0.0234(12) Uani 1 1 d . . .
C10 C 0.4989(4) 0.4961(3) 0.3842(3) 0.0226(11) Uani 1 1 d . . .
H10A H 0.5236 0.5027 0.4358 0.027 Uiso 1 1 d R . .
C11 C 0.5685(3) 0.4688(3) 0.3397(3) 0.0200(11) Uani 1 1 d . . .
C12 C 0.3855(4) 0.4690(3) 0.1526(3) 0.0261(11) Uani 1 1 d . . .
H12A H 0.4274 0.5104 0.1262 0.039 Uiso 1 1 d R . .
H12B H 0.3118 0.4897 0.1405 0.039 Uiso 1 1 d R . .
H12C H 0.3911 0.3998 0.1384 0.039 Uiso 1 1 d R . .
C13 C 0.3200(4) 0.5408(4) 0.4053(3) 0.0306(12) Uani 1 1 d . . .
H13A H 0.2480 0.5482 0.3778 0.046 Uiso 1 1 d R . .
H13B H 0.3435 0.6032 0.4296 0.046 Uiso 1 1 d R . .
H13C H 0.3220 0.4888 0.4420 0.046 Uiso 1 1 d R . .
C14 C 0.6826(4) 0.4484(4) 0.3724(3) 0.0284(12) Uani 1 1 d . . .
H14A H 0.6987 0.3788 0.3653 0.043 Uiso 1 1 d R . .
H14B H 0.6954 0.4633 0.4246 0.043 Uiso 1 1 d R . .
H14C H 0.7275 0.4902 0.3486 0.043 Uiso 1 1 d R . .
C15 C 0.8875(4) 0.5103(3) 0.1452(3) 0.0213(11) Uani 1 1 d . . .
C16 C 0.9651(4) 0.5258(3) 0.2081(3) 0.0229(11) Uani 1 1 d . . .
C17 C 1.0524(4) 0.5826(3) 0.2012(3) 0.0263(12) Uani 1 1 d . . .
H17A H 1.1052 0.5948 0.2440 0.032 Uiso 1 1 d R . .
C18 C 1.0650(4) 0.6229(3) 0.1351(3) 0.0261(12) Uani 1 1 d . . .
C19 C 0.9867(4) 0.6040(3) 0.0737(3) 0.0270(12) Uani 1 1 d . . .
H19A H 0.9958 0.6292 0.0274 0.032 Uiso 1 1 d R . .
C20 C 0.8978(4) 0.5488(3) 0.0777(3) 0.0237(11) Uani 1 1 d . . .
C21 C 0.9546(4) 0.4844(4) 0.2810(3) 0.0336(13) Uani 1 1 d . . .
H21A H 0.8879 0.5061 0.2929 0.050 Uiso 1 1 d R . .
H21B H 1.0130 0.5076 0.3187 0.050 Uiso 1 1 d R . .
H21C H 0.9559 0.4122 0.2787 0.050 Uiso 1 1 d R . .
C22 C 1.1587(4) 0.6868(4) 0.1303(3) 0.0382(14) Uani 1 1 d . . .
H22A H 1.1524 0.7497 0.1550 0.057 Uiso 1 1 d R . .
H22B H 1.1604 0.6991 0.0790 0.057 Uiso 1 1 d R . .
H22C H 1.2236 0.6535 0.1538 0.057 Uiso 1 1 d R . .
C23 C 0.8128(4) 0.5330(4) 0.0106(3) 0.0298(12) Uani 1 1 d . . .
H23A H 0.8344 0.5634 -0.0317 0.045 Uiso 1 1 d R . .
H23B H 0.7471 0.5633 0.0180 0.045 Uiso 1 1 d R . .
H23C H 0.8020 0.4621 0.0020 0.045 Uiso 1 1 d R . .
C24 C 0.6286(4) 0.7139(3) 0.1478(3) 0.0216(11) Uani 1 1 d . . .
H24 H 0.6038 0.7850 0.1408 0.026 Uiso 1 1 d R . .
C25 C 0.7428(4) 0.7563(3) 0.2617(3) 0.0265(12) Uani 1 1 d . . .
H25A H 0.6972 0.8124 0.2604 0.032 Uiso 1 1 d R . .
C26 C 0.8457(4) 0.7919(4) 0.2443(3) 0.0447(16) Uani 1 1 d . . .
H26A H 0.8917 0.7348 0.2431 0.067 Uiso 1 1 d R . .
H26B H 0.8796 0.8382 0.2819 0.067 Uiso 1 1 d R . .
H26C H 0.8327 0.8248 0.1968 0.067 Uiso 1 1 d R . .
C27 C 0.7591(5) 0.7119(4) 0.3384(3) 0.0439(16) Uani 1 1 d . . .
H27A H 0.6919 0.6882 0.3482 0.066 Uiso 1 1 d R . .
H27B H 0.7881 0.7620 0.3747 0.066 Uiso 1 1 d R . .
H27C H 0.8084 0.6566 0.3413 0.066 Uiso 1 1 d R . .
C28 C 0.5190(4) 0.6694(4) 0.0309(3) 0.0281(12) Uani 1 1 d . . .
H28A H 0.5048 0.6094 0.0035 0.034 Uiso 1 1 d R . .
C29 C 0.4142(4) 0.7089(4) 0.0430(3) 0.0370(14) Uani 1 1 d . . .
H29A H 0.3856 0.6655 0.0762 0.056 Uiso 1 1 d R . .
H29B H 0.3647 0.7129 -0.0037 0.056 Uiso 1 1 d R . .
H29C H 0.4254 0.7750 0.0645 0.056 Uiso 1 1 d R . .
C30 C 0.5667(4) 0.7417(4) -0.0164(3) 0.0360(13) Uani 1 1 d . . .
H30A H 0.5777 0.8052 0.0092 0.054 Uiso 1 1 d R . .
H30B H 0.5184 0.7508 -0.0632 0.054 Uiso 1 1 d R . .
H30C H 0.6341 0.7167 -0.0248 0.054 Uiso 1 1 d R . .
C31 C 0.9457(5) 0.5187(6) 0.5016(4) 0.077(2) Uani 1 1 d . . .
H31A H 0.8995 0.5069 0.4557 0.093 Uiso 1 1 d R . .
H31B H 0.9195 0.4838 0.5390 0.093 Uiso 1 1 d R . .
C32 C 0.9486(7) 0.6280(6) 0.5207(5) 0.093(3) Uani 1 1 d . . .
H32A H 0.9659 0.6635 0.4802 0.111 Uiso 1 1 d R . .
H32B H 1.0023 0.6401 0.5629 0.111 Uiso 1 1 d R . .
C33 C 0.8445(7) 0.6650(6) 0.5338(5) 0.097(3) Uani 1 1 d . . .
H33A H 0.7887 0.6373 0.4963 0.145 Uiso 1 1 d R . .
H33B H 0.8407 0.7372 0.5322 0.145 Uiso 1 1 d R . .
H33C H 0.8358 0.6418 0.5819 0.145 Uiso 1 1 d 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
Zn1 0.0224(3) 0.0150(3) 0.0242(3) 0.0012(3) 0.0070(2) 0.0011(3)
N1 0.025(2) 0.015(2) 0.020(2) -0.0014(16) 0.0052(18) 0.0007(16)
N2 0.022(2) 0.0180(19) 0.021(2) -0.0011(18) 0.0051(17) 0.0003(18)
N3 0.026(2) 0.0143(19) 0.021(2) -0.0030(18) 0.0050(19) 0.0023(17)
N4 0.026(2) 0.021(2) 0.018(2) 0.0017(18) 0.0053(19) -0.0002(18)
C1 0.025(3) 0.020(2) 0.019(3) 0.003(2) 0.003(2) -0.002(2)
C2 0.031(3) 0.013(2) 0.025(3) -0.004(2) 0.003(2) 0.001(2)
C3 0.027(3) 0.022(3) 0.020(3) -0.001(2) 0.001(2) 0.007(2)
C4 0.032(3) 0.017(2) 0.029(3) 0.003(2) 0.013(2) 0.002(2)
C5 0.029(3) 0.021(3) 0.038(3) -0.002(2) 0.011(3) 0.002(2)
C6 0.030(3) 0.009(2) 0.020(3) 0.001(2) 0.009(2) -0.003(2)
C7 0.025(3) 0.010(2) 0.025(3) 0.0006(19) 0.004(2) -0.0024(19)
C8 0.022(3) 0.013(2) 0.028(3) 0.003(2) 0.004(2) -0.001(2)
C9 0.028(3) 0.014(2) 0.031(3) 0.001(2) 0.011(2) -0.001(2)
C10 0.032(3) 0.019(2) 0.019(3) 0.002(2) 0.008(2) -0.004(2)
C11 0.024(2) 0.013(2) 0.023(3) 0.002(2) 0.007(2) -0.002(2)
C12 0.029(3) 0.025(3) 0.025(3) 0.001(2) 0.005(2) 0.001(2)
C13 0.038(3) 0.025(3) 0.033(3) -0.003(2) 0.017(3) 0.004(3)
C14 0.028(3) 0.035(3) 0.023(3) 0.000(2) 0.006(2) -0.003(2)
C15 0.019(3) 0.018(2) 0.028(3) -0.002(2) 0.009(2) 0.005(2)
C16 0.021(3) 0.025(3) 0.025(3) -0.002(2) 0.009(2) 0.005(2)
C17 0.018(3) 0.029(3) 0.031(3) -0.007(2) 0.004(2) 0.005(2)
C18 0.021(3) 0.026(3) 0.033(3) -0.005(2) 0.009(2) 0.001(2)
C19 0.029(3) 0.026(3) 0.028(3) 0.008(2) 0.011(3) 0.001(2)
C20 0.026(3) 0.019(2) 0.028(3) -0.001(2) 0.009(2) 0.004(2)
C21 0.028(3) 0.044(3) 0.028(3) -0.002(2) 0.005(2) 0.004(3)
C22 0.031(3) 0.035(3) 0.051(4) -0.003(3) 0.013(3) -0.005(3)
C23 0.031(3) 0.034(3) 0.025(3) 0.006(2) 0.008(2) 0.000(3)
C24 0.023(3) 0.016(2) 0.028(3) 0.004(2) 0.010(2) -0.001(2)
C25 0.030(3) 0.018(2) 0.029(3) -0.003(2) 0.000(2) 0.006(2)
C26 0.032(3) 0.039(3) 0.062(4) -0.012(3) 0.006(3) -0.009(3)
C27 0.068(4) 0.027(3) 0.031(4) -0.008(2) -0.004(3) 0.005(3)
C28 0.034(3) 0.024(3) 0.026(3) 0.003(2) 0.006(2) 0.001(2)
C29 0.035(3) 0.041(3) 0.034(3) 0.007(3) 0.006(3) 0.002(3)
C30 0.040(3) 0.038(3) 0.029(3) 0.004(3) 0.004(3) 0.003(3)
C31 0.065(5) 0.108(7) 0.048(5) -0.006(4) -0.013(4) -0.004(5)
C32 0.101(7) 0.067(5) 0.095(7) -0.008(5) -0.019(6) 0.020(5)
C33 0.114(8) 0.085(6) 0.088(7) 0.013(5) 0.014(6) -0.024(6)

_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 N1 1.968(4) . ?
Zn1 N2 1.970(4) . ?
Zn1 N3 2.024(3) . ?
Zn1 N4 2.092(4) . ?
Zn1 C24 2.417(5) . ?
N1 C1 1.338(5) . ?
N1 C6 1.427(6) . ?
N2 C3 1.330(6) . ?
N2 C15 1.438(6) . ?
N3 C24 1.314(6) . ?
N3 C25 1.452(6) . ?
N4 C24 1.311(6) . ?
N4 C28 1.471(6) . ?
C1 C2 1.398(7) . ?
C1 C4 1.507(6) . ?
C2 C3 1.392(7) . ?
C3 C5 1.512(6) . ?
C6 C7 1.390(6) . ?
C6 C11 1.405(6) . ?
C7 C8 1.395(6) . ?
C7 C12 1.505(7) . ?
C8 C9 1.389(7) . ?
C9 C10 1.392(7) . ?
C9 C13 1.495(6) . ?
C10 C11 1.389(6) . ?
C11 C14 1.508(6) . ?
C15 C20 1.390(7) . ?
C15 C16 1.398(7) . ?
C16 C17 1.394(7) . ?
C16 C21 1.498(7) . ?
C17 C18 1.385(7) . ?
C18 C19 1.392(7) . ?
C18 C22 1.505(7) . ?
C19 C20 1.387(7) . ?
C20 C23 1.507(7) . ?
C25 C26 1.511(7) . ?
C25 C27 1.524(7) . ?
C28 C29 1.517(7) . ?
C28 C30 1.524(7) . ?
C31 C31 1.508(14) 3_766 ?
C31 C32 1.513(10) . ?
C32 C33 1.503(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
N1 Zn1 N2 97.19(15) . . ?
N1 Zn1 N3 125.59(15) . . ?
N2 Zn1 N3 123.56(15) . . ?
N1 Zn1 N4 121.80(15) . . ?
N2 Zn1 N4 124.02(15) . . ?
N3 Zn1 N4 65.72(15) . . ?
N1 Zn1 C24 131.12(15) . . ?
N2 Zn1 C24 131.63(15) . . ?
N3 Zn1 C24 32.92(15) . . ?
N4 Zn1 C24 32.79(15) . . ?
C1 N1 C6 119.3(4) . . ?
C1 N1 Zn1 120.7(3) . . ?
C6 N1 Zn1 120.0(3) . . ?
C3 N2 C15 121.1(4) . . ?
C3 N2 Zn1 120.4(3) . . ?
C15 N2 Zn1 118.3(3) . . ?
C24 N3 C25 120.4(4) . . ?
C24 N3 Zn1 90.2(3) . . ?
C25 N3 Zn1 149.1(3) . . ?
C24 N4 C28 121.3(4) . . ?
C24 N4 Zn1 87.4(3) . . ?
C28 N4 Zn1 151.3(3) . . ?
N1 C1 C2 123.7(4) . . ?
N1 C1 C4 118.7(4) . . ?
C2 C1 C4 117.5(4) . . ?
C3 C2 C1 129.6(4) . . ?
N2 C3 C2 124.5(4) . . ?
N2 C3 C5 118.6(4) . . ?
C2 C3 C5 116.9(4) . . ?
C7 C6 C11 120.2(4) . . ?
C7 C6 N1 120.4(4) . . ?
C11 C6 N1 119.4(4) . . ?
C6 C7 C8 119.1(4) . . ?
C6 C7 C12 120.3(4) . . ?
C8 C7 C12 120.6(4) . . ?
C9 C8 C7 121.9(4) . . ?
C8 C9 C10 118.1(4) . . ?
C8 C9 C13 121.9(4) . . ?
C10 C9 C13 120.0(4) . . ?
C11 C10 C9 121.6(5) . . ?
C10 C11 C6 119.1(4) . . ?
C10 C11 C14 120.6(4) . . ?
C6 C11 C14 120.3(4) . . ?
C20 C15 C16 121.2(4) . . ?
C20 C15 N2 120.1(4) . . ?
C16 C15 N2 118.4(4) . . ?
C17 C16 C15 117.9(4) . . ?
C17 C16 C21 120.6(4) . . ?
C15 C16 C21 121.5(4) . . ?
C18 C17 C16 122.6(5) . . ?
C17 C18 C19 117.5(4) . . ?
C17 C18 C22 121.0(5) . . ?
C19 C18 C22 121.5(5) . . ?
C20 C19 C18 122.2(5) . . ?
C19 C20 C15 118.6(4) . . ?
C19 C20 C23 120.7(4) . . ?
C15 C20 C23 120.7(4) . . ?
N4 C24 N3 116.7(4) . . ?
N4 C24 Zn1 59.8(2) . . ?
N3 C24 Zn1 56.8(2) . . ?
N3 C25 C26 111.7(4) . . ?
N3 C25 C27 109.7(4) . . ?
C26 C25 C27 111.2(5) . . ?
N4 C28 C29 112.5(4) . . ?
N4 C28 C30 112.8(4) . . ?
C29 C28 C30 109.8(4) . . ?
C31 C31 C32 110.8(8) 3_766 . ?
C33 C32 C31 112.3(8) . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        23.93
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.083