# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Eva Hevia'
_publ_contact_author_address     
;
Pure and Applied Chemistry
UNiversity of Strathclyde
Glasgow
G1 1XL
UNITED KINGDOM
;

_publ_contact_author_email       EVA.HEVIA@STRATH.AC.UK

_publ_section_title              
;
Transamination chemistry of sodium TMP-zincate:
synthesis and crystal structure of a chiral amidozincate
;
loop_
_publ_author_name
'Eva Hevia'
'David R. Armstrong'
'W Clegg'
'Sophie Dale'
'Joaquin Garcia-Alvarez'
;
R.W.Harrington
;
'Gordon W. Honeyman'
'Alan R. Kennedy'
'R. E. Mulvey'
"Charles T. O'Hara"

# Attachment 'cc.cif'

data_grem265_compound2
_database_code_depnum_ccdc_archive 'CCDC 660688'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 N3 Na Zn'
_chemical_formula_sum            'C20 H48 N3 Na Zn'
_chemical_formula_weight         418.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   27.7184(10)
_cell_length_b                   9.8386(3)
_cell_length_c                   19.6286(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.215(2)
_cell_angle_gamma                90.00
_cell_volume                     5231.7(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6042
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.10

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34146
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         27.11
_reflns_number_total             5767
_reflns_number_gt                3733
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Denzo & Collect'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    SIR
_computing_structure_refinement  SHELXL97
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97

_refine_special_details          
;
;

_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^)+(0.0306P)^2^+5.3123P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5767
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
Zn Zn 0.618112(11) 0.46250(3) -0.043627(16) 0.02712(10) Uani 1 1 d . . .
Na Na 0.63273(4) 0.23478(10) 0.09304(6) 0.0360(3) Uani 1 1 d . . .
N1 N 0.64196(7) 0.4623(2) 0.06259(10) 0.0252(5) Uani 1 1 d . . .
N2 N 0.69361(8) 0.0959(2) 0.17131(12) 0.0347(6) Uani 1 1 d . . .
N3 N 0.58275(8) 0.0604(2) 0.13566(12) 0.0335(6) Uani 1 1 d . . .
C1 C 0.61237(11) 0.2755(3) -0.09248(15) 0.0373(7) Uani 1 1 d . . .
C2 C 0.55991(13) 0.2554(4) -0.1358(2) 0.0720(12) Uani 1 1 d . . .
H2A H 0.5516 0.3305 -0.1690 0.108 Uiso 1 1 calc R . .
H2B H 0.5365 0.2537 -0.1047 0.108 Uiso 1 1 calc R . .
H2C H 0.5581 0.1693 -0.1612 0.108 Uiso 1 1 calc R . .
C3 C 0.64743(12) 0.2758(3) -0.14236(16) 0.0495(9) Uani 1 1 d . . .
H3A H 0.6815 0.2832 -0.1158 0.074 Uiso 1 1 calc R . .
H3B H 0.6399 0.3533 -0.1742 0.074 Uiso 1 1 calc R . .
H3C H 0.6435 0.1911 -0.1693 0.074 Uiso 1 1 calc R . .
C4 C 0.6259(2) 0.1515(3) -0.0456(2) 0.0606(11) Uani 1 1 d . . .
C5 C 0.60180(10) 0.6421(3) -0.09686(15) 0.0352(7) Uani 1 1 d . . .
C6 C 0.55933(11) 0.6231(3) -0.15996(16) 0.0472(8) Uani 1 1 d . . .
H6A H 0.5521 0.7098 -0.1845 0.071 Uiso 1 1 calc R . .
H6B H 0.5299 0.5916 -0.1443 0.071 Uiso 1 1 calc R . .
H6C H 0.5687 0.5555 -0.1915 0.071 Uiso 1 1 calc R . .
C7 C 0.64669(11) 0.6897(4) -0.12472(17) 0.0537(9) Uani 1 1 d . . .
H7A H 0.6387 0.7749 -0.1505 0.081 Uiso 1 1 calc R . .
H7B H 0.6553 0.6201 -0.1558 0.081 Uiso 1 1 calc R . .
H7C H 0.6747 0.7043 -0.0856 0.081 Uiso 1 1 calc R . .
C8 C 0.58699(13) 0.7569(3) -0.05295(17) 0.0513(9) Uani 1 1 d . . .
H8A H 0.6140 0.7749 -0.0130 0.077 Uiso 1 1 calc R . .
H8B H 0.5574 0.7302 -0.0363 0.077 Uiso 1 1 calc R . .
H8C H 0.5800 0.8392 -0.0814 0.077 Uiso 1 1 calc R . .
C9 C 0.55594(10) 0.4937(3) 0.06733(16) 0.0418(8) Uani 1 1 d . . .
H9A H 0.5487 0.5079 0.0168 0.063 Uiso 1 1 calc R . .
H9B H 0.5332 0.5480 0.0882 0.063 Uiso 1 1 calc R . .
H9C H 0.5519 0.3972 0.0773 0.063 Uiso 1 1 calc R . .
C10 C 0.60869(9) 0.5370(3) 0.09782(13) 0.0318(6) Uani 1 1 d . . .
H10 H 0.6117 0.6360 0.0879 0.038 Uiso 1 1 calc R . .
C11 C 0.61962(12) 0.5179(4) 0.17699(15) 0.0515(9) Uani 1 1 d . . .
H11A H 0.6191 0.4208 0.1879 0.077 Uiso 1 1 calc R . .
H11B H 0.5945 0.5653 0.1965 0.077 Uiso 1 1 calc R . .
H11C H 0.6523 0.5554 0.1973 0.077 Uiso 1 1 calc R . .
C12 C 0.70583(11) 0.6504(3) 0.08513(17) 0.0478(8) Uani 1 1 d . . .
H12A H 0.6948 0.6845 0.0375 0.072 Uiso 1 1 calc R . .
H12B H 0.7415 0.6644 0.1004 0.072 Uiso 1 1 calc R . .
H12C H 0.6886 0.6995 0.1163 0.072 Uiso 1 1 calc R . .
C13 C 0.69417(10) 0.4977(3) 0.08706(15) 0.0342(7) Uani 1 1 d . . .
H13 H 0.7046 0.4664 0.1365 0.041 Uiso 1 1 calc R . .
C14 C 0.72503(11) 0.4216(3) 0.04413(18) 0.0521(9) Uani 1 1 d . . .
H14A H 0.7184 0.3239 0.0458 0.078 Uiso 1 1 calc R . .
H14B H 0.7601 0.4387 0.0632 0.078 Uiso 1 1 calc R . .
H14C H 0.7165 0.4530 -0.0043 0.078 Uiso 1 1 calc R . .
C15 C 0.72896(12) 0.1753(4) 0.22220(17) 0.0576(10) Uani 1 1 d . . .
H15A H 0.7522 0.1137 0.2517 0.086 Uiso 1 1 calc R . .
H15B H 0.7112 0.2281 0.2513 0.086 Uiso 1 1 calc R . .
H15C H 0.7471 0.2372 0.1976 0.086 Uiso 1 1 calc R . .
C16 C 0.72060(11) 0.0183(3) 0.12796(18) 0.0508(9) Uani 1 1 d . . .
H16A H 0.7391 0.0807 0.1042 0.076 Uiso 1 1 calc R . .
H16B H 0.6972 -0.0338 0.0932 0.076 Uiso 1 1 calc R . .
H16C H 0.7436 -0.0442 0.1574 0.076 Uiso 1 1 calc R . .
C17 C 0.66545(11) 0.0039(3) 0.20767(17) 0.0454(8) Uani 1 1 d . . .
H17A H 0.6574 0.0524 0.2481 0.054 Uiso 1 1 calc R . .
H17B H 0.6865 -0.0749 0.2258 0.054 Uiso 1 1 calc R . .
C18 C 0.61841(11) -0.0470(3) 0.16214(18) 0.0473(8) Uani 1 1 d . . .
H18A H 0.6265 -0.0963 0.1221 0.057 Uiso 1 1 calc R . .
H18B H 0.6028 -0.1126 0.1891 0.057 Uiso 1 1 calc R . .
C19 C 0.56042(13) 0.1164(4) 0.19056(18) 0.0598(10) Uani 1 1 d . . .
H19A H 0.5352 0.1833 0.1704 0.090 Uiso 1 1 calc R . .
H19B H 0.5859 0.1605 0.2258 0.090 Uiso 1 1 calc R . .
H19C H 0.5451 0.0430 0.2123 0.090 Uiso 1 1 calc R . .
C20 C 0.54339(12) 0.0021(3) 0.08167(19) 0.0577(10) Uani 1 1 d . . .
H20A H 0.5268 -0.0707 0.1020 0.087 Uiso 1 1 calc R . .
H20B H 0.5577 -0.0351 0.0440 0.087 Uiso 1 1 calc R . .
H20C H 0.5194 0.0730 0.0630 0.087 Uiso 1 1 calc R . .
H4A H 0.6600(15) 0.155(4) -0.013(2) 0.091(14) Uiso 1 1 d . . .
H4B H 0.5979(11) 0.138(3) -0.0208(16) 0.052(10) Uiso 1 1 d . . .
H4C H 0.6273(13) 0.067(4) -0.0735(19) 0.084(12) Uiso 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
Zn 0.02899(17) 0.02785(17) 0.02575(17) -0.00023(16) 0.00856(12) -0.00202(15)
Na 0.0381(6) 0.0290(6) 0.0398(7) 0.0063(5) 0.0055(5) 0.0004(5)
N1 0.0251(11) 0.0271(11) 0.0235(11) -0.0002(11) 0.0056(9) -0.0003(10)
N2 0.0290(12) 0.0385(13) 0.0362(14) 0.0047(12) 0.0058(11) 0.0026(11)
N3 0.0312(12) 0.0344(14) 0.0355(14) -0.0039(11) 0.0084(11) -0.0020(10)
C1 0.0458(18) 0.0383(17) 0.0298(17) -0.0098(14) 0.0128(14) -0.0098(14)
C2 0.058(2) 0.069(3) 0.087(3) -0.037(2) 0.010(2) -0.017(2)
C3 0.065(2) 0.049(2) 0.0390(19) -0.0051(16) 0.0209(17) 0.0029(17)
C4 0.109(4) 0.0301(18) 0.048(2) -0.0103(18) 0.030(3) -0.016(2)
C5 0.0359(16) 0.0394(17) 0.0324(17) 0.0097(14) 0.0117(14) -0.0001(14)
C6 0.0407(18) 0.062(2) 0.0397(19) 0.0172(17) 0.0103(15) 0.0041(16)
C7 0.0420(19) 0.066(2) 0.054(2) 0.0265(19) 0.0121(16) -0.0033(17)
C8 0.066(2) 0.0316(17) 0.058(2) 0.0107(16) 0.0157(19) 0.0097(16)
C9 0.0340(16) 0.051(2) 0.0443(19) -0.0001(15) 0.0175(14) 0.0031(14)
C10 0.0339(15) 0.0334(15) 0.0295(15) -0.0003(14) 0.0101(12) -0.0013(14)
C11 0.056(2) 0.070(2) 0.0309(17) -0.0066(16) 0.0138(15) 0.0005(18)
C12 0.0379(17) 0.0446(19) 0.057(2) -0.0032(16) 0.0019(16) -0.0139(15)
C13 0.0314(15) 0.0387(17) 0.0307(16) 0.0007(13) 0.0029(13) -0.0014(12)
C14 0.0326(17) 0.061(2) 0.065(2) -0.0083(19) 0.0148(16) 0.0014(15)
C15 0.0444(19) 0.073(3) 0.049(2) -0.0022(19) -0.0047(17) 0.0002(18)
C16 0.0464(19) 0.0474(19) 0.064(2) 0.0054(18) 0.0243(17) 0.0073(16)
C17 0.0384(17) 0.051(2) 0.0473(19) 0.0200(15) 0.0110(15) 0.0086(14)
C18 0.0487(19) 0.0333(17) 0.064(2) 0.0096(17) 0.0217(17) -0.0013(15)
C19 0.061(2) 0.067(2) 0.058(2) -0.012(2) 0.0276(19) 0.0029(19)
C20 0.051(2) 0.065(2) 0.058(2) -0.0127(18) 0.0139(18) -0.0215(17)

_geom_special_details            
;
;

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
Zn N1 2.050(2) . ?
Zn C5 2.054(3) . ?
Zn C1 2.065(3) . ?
Na N1 2.345(2) . ?
Na N2 2.445(2) . ?
Na N3 2.460(2) . ?
Na C4 2.809(4) . ?
N1 C10 1.462(3) . ?
N1 C13 1.467(3) . ?
N2 C16 1.462(4) . ?
N2 C15 1.468(4) . ?
N2 C17 1.474(4) . ?
N3 C19 1.459(4) . ?
N3 C18 1.465(4) . ?
N3 C20 1.467(4) . ?
C1 C3 1.518(4) . ?
C1 C4 1.526(5) . ?
C1 C2 1.534(4) . ?
C5 C8 1.528(4) . ?
C5 C6 1.529(4) . ?
C5 C7 1.534(4) . ?
C9 C10 1.519(4) . ?
C10 C11 1.531(4) . ?
C12 C13 1.538(4) . ?
C13 C14 1.519(4) . ?
C17 C18 1.502(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
N1 Zn C5 120.47(10) . . ?
N1 Zn C1 116.62(10) . . ?
C5 Zn C1 122.90(11) . . ?
N1 Na N2 126.56(8) . . ?
N1 Na N3 148.42(9) . . ?
N2 Na N3 76.12(8) . . ?
N1 Na C4 91.15(9) . . ?
N2 Na C4 110.01(12) . . ?
N3 Na C4 101.45(10) . . ?
C10 N1 Zn 112.37(15) . . ?
C13 N1 Zn 114.60(16) . . ?
C10 N1 Na 104.22(15) . . ?
C13 N1 Na 107.25(15) . . ?
Zn N1 Na 103.36(9) . . ?
C16 N2 C15 108.9(2) . . ?
C16 N2 C17 110.5(2) . . ?
C15 N2 C17 110.1(2) . . ?
C16 N2 Na 107.25(18) . . ?
C15 N2 Na 113.76(19) . . ?
C17 N2 Na 106.35(16) . . ?
C19 N3 C18 111.7(2) . . ?
C19 N3 C20 108.3(2) . . ?
C18 N3 C20 108.5(2) . . ?
C19 N3 Na 110.20(19) . . ?
C18 N3 Na 103.73(16) . . ?
C20 N3 Na 114.41(19) . . ?
C3 C1 C4 106.4(3) . . ?
C3 C1 C2 107.7(3) . . ?
C4 C1 C2 108.3(3) . . ?
C3 C1 Zn 107.50(19) . . ?
C4 C1 Zn 116.6(2) . . ?
C2 C1 Zn 110.0(2) . . ?
C1 C4 Na 108.0(2) . . ?
C8 C5 C6 107.1(2) . . ?
C8 C5 C7 108.1(3) . . ?
C6 C5 C7 107.0(2) . . ?
C8 C5 Zn 113.91(19) . . ?
C6 C5 Zn 110.8(2) . . ?
C7 C5 Zn 109.61(19) . . ?
N1 C10 C9 108.9(2) . . ?
N1 C10 C11 114.2(2) . . ?
C9 C10 C11 109.4(2) . . ?
N1 C10 Na 48.11(12) . . ?
C9 C10 Na 84.99(16) . . ?
C11 C10 Na 85.07(18) . . ?
N1 C13 C14 109.5(2) . . ?
N1 C13 C12 114.9(2) . . ?
C14 C13 C12 108.8(2) . . ?
N1 C13 Na 46.00(12) . . ?
C14 C13 Na 89.31(17) . . ?
C12 C13 Na 158.69(19) . . ?
N2 C17 C18 113.5(2) . . ?
N3 C18 C17 113.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.11
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.066

#===END

data_rem335_compound3
_database_code_depnum_ccdc_archive 'CCDC 660908'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 N4 Na +, C14 H36 N Si2 Zn -'
_chemical_formula_sum            'C26 H68 N5 Na Si2 Zn'
_chemical_formula_weight         595.39

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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                   9.3269(12)
_cell_length_b                   10.649(2)
_cell_length_c                   19.8598(12)
_cell_angle_alpha                81.740(10)
_cell_angle_beta                 78.079(10)
_cell_angle_gamma                83.872(12)
_cell_volume                     1904.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    324
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.44
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SHELXTL'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29550
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.43
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8621
_reflns_number_gt                6320
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Nonius COLLECT'
_computing_cell_refinement       DIRAX
_computing_data_reduction        EvalCCD
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
Restraints: 'rigid bond' (DELU) and similarity (SIMU) restraints for
the disordered TMEDA ligand, to control the displacement parameters
of overlapping components; also geometrical similarity restraints
(SAME) for these components. Such restraints are often required for
disorder components that interpenetrate each other, since the
electron density of the disordered atoms strongly overlap and can
not be resolved satisfactorily in free refinement. Restraints are
gentler and more flexible than rigid constraints.
;

_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^)+(0.0265P)^2^+1.1320P] 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         8621
_refine_ls_number_parameters     393
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.002
_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
Zn Zn 0.23123(3) 0.78151(2) 0.226324(13) 0.02699(8) Uani 1 1 d . . .
C1 C 0.2555(3) 0.6102(2) 0.28658(11) 0.0348(5) Uani 1 1 d . . .
C2 C 0.3214(4) 0.6255(3) 0.34866(14) 0.0636(8) Uani 1 1 d . . .
H2A H 0.3291 0.5432 0.3774 0.095 Uiso 1 1 calc R . .
H2B H 0.2582 0.6869 0.3761 0.095 Uiso 1 1 calc R . .
H2C H 0.4195 0.6564 0.3324 0.095 Uiso 1 1 calc R . .
C3 C 0.1068(3) 0.5541(3) 0.31217(16) 0.0622(8) Uani 1 1 d . . .
H3A H 0.0638 0.5447 0.2723 0.093 Uiso 1 1 calc R . .
H3B H 0.0409 0.6111 0.3415 0.093 Uiso 1 1 calc R . .
H3C H 0.1205 0.4706 0.3391 0.093 Uiso 1 1 calc R . .
C4 C 0.3585(3) 0.5155(2) 0.24504(14) 0.0494(6) Uani 1 1 d . . .
H4A H 0.4563 0.5474 0.2304 0.074 Uiso 1 1 calc R . .
H4B H 0.3200 0.5050 0.2040 0.074 Uiso 1 1 calc R . .
H4C H 0.3653 0.4332 0.2740 0.074 Uiso 1 1 calc R . .
C5 C 0.1619(2) 0.8140(2) 0.13353(12) 0.0318(5) Uani 1 1 d . . .
C6 C 0.0609(3) 0.7139(2) 0.12741(15) 0.0507(7) Uani 1 1 d . . .
H6A H -0.0287 0.7196 0.1631 0.076 Uiso 1 1 calc R . .
H6B H 0.1117 0.6289 0.1338 0.076 Uiso 1 1 calc R . .
H6C H 0.0349 0.7291 0.0814 0.076 Uiso 1 1 calc R . .
C7 C 0.2966(3) 0.8055(3) 0.07517(13) 0.0477(6) Uani 1 1 d . . .
H7A H 0.2655 0.8226 0.0303 0.072 Uiso 1 1 calc R . .
H7B H 0.3468 0.7199 0.0798 0.072 Uiso 1 1 calc R . .
H7C H 0.3638 0.8684 0.0779 0.072 Uiso 1 1 calc R . .
C8 C 0.0814(3) 0.9451(2) 0.12138(14) 0.0455(6) Uani 1 1 d . . .
H8A H 0.1437 1.0107 0.1260 0.068 Uiso 1 1 calc R . .
H8B H -0.0104 0.9505 0.1557 0.068 Uiso 1 1 calc R . .
H8C H 0.0592 0.9584 0.0746 0.068 Uiso 1 1 calc R . .
N1 N 0.29028(19) 0.93403(16) 0.26172(9) 0.0300(4) Uani 1 1 d . . .
Si1 Si 0.15024(7) 1.01353(6) 0.31059(3) 0.03523(15) Uani 1 1 d . . .
C9 C 0.1126(4) 1.1825(3) 0.27188(17) 0.0679(9) Uani 1 1 d . . .
H9A H 0.1935 1.2324 0.2740 0.102 Uiso 1 1 calc R . .
H9B H 0.0206 1.2191 0.2981 0.102 Uiso 1 1 calc R . .
H9C H 0.1039 1.1840 0.2234 0.102 Uiso 1 1 calc R . .
C10 C 0.1759(4) 1.0192(4) 0.40117(15) 0.0758(10) Uani 1 1 d . . .
H10A H 0.1905 0.9323 0.4241 0.114 Uiso 1 1 calc R . .
H10B H 0.0885 1.0629 0.4271 0.114 Uiso 1 1 calc R . .
H10C H 0.2621 1.0654 0.3997 0.114 Uiso 1 1 calc R . .
C11 C -0.0240(3) 0.9332(3) 0.32239(18) 0.0714(9) Uani 1 1 d . . .
H11A H -0.0494 0.9318 0.2770 0.107 Uiso 1 1 calc R . .
H11B H -0.1036 0.9800 0.3515 0.107 Uiso 1 1 calc R . .
H11C H -0.0102 0.8458 0.3448 0.107 Uiso 1 1 calc R . .
Si2 Si 0.46023(7) 0.98093(6) 0.22737(3) 0.03103(14) Uani 1 1 d . . .
C12 C 0.4693(3) 1.0940(3) 0.14487(14) 0.0576(8) Uani 1 1 d . . .
H12A H 0.4260 1.0572 0.1120 0.086 Uiso 1 1 calc R . .
H12B H 0.5721 1.1086 0.1246 0.086 Uiso 1 1 calc R . .
H12C H 0.4145 1.1750 0.1551 0.086 Uiso 1 1 calc R . .
C13 C 0.5914(3) 0.8401(3) 0.20569(15) 0.0512(7) Uani 1 1 d . . .
H13A H 0.6015 0.7840 0.2484 0.077 Uiso 1 1 calc R . .
H13B H 0.6875 0.8691 0.1825 0.077 Uiso 1 1 calc R . .
H13C H 0.5537 0.7933 0.1748 0.077 Uiso 1 1 calc R . .
C14 C 0.5398(3) 1.0665(3) 0.28627(14) 0.0521(7) Uani 1 1 d . . .
H14A H 0.4829 1.1483 0.2925 0.078 Uiso 1 1 calc R . .
H14B H 0.6423 1.0813 0.2655 0.078 Uiso 1 1 calc R . .
H14C H 0.5355 1.0143 0.3314 0.078 Uiso 1 1 calc R . .
Na1 Na 1.0000 0.5000 0.0000 0.0445(4) Uani 1 2 d S . .
N2 N 0.75587(18) 0.62051(16) 0.00866(9) 0.0291(4) Uani 1 1 d D . .
C15 C 0.6626(2) 0.5616(2) 0.07197(12) 0.0355(5) Uani 1 1 d D . .
H15A H 0.5586 0.5777 0.0670 0.043 Uiso 1 1 calc R . .
H15B H 0.6740 0.6035 0.1117 0.043 Uiso 1 1 calc R . .
C16 C 0.6968(2) 0.4201(2) 0.08809(12) 0.0328(5) Uani 1 1 d D . .
H16A H 0.6237 0.3873 0.1287 0.039 Uiso 1 1 calc R . .
H16B H 0.6867 0.3781 0.0482 0.039 Uiso 1 1 calc R . .
N3 N 0.84531(18) 0.38554(15) 0.10292(8) 0.0276(4) Uani 1 1 d D . .
C17 C 0.7059(3) 0.5941(2) -0.05290(13) 0.0491(6) Uani 1 1 d D . .
H17A H 0.7117 0.5019 -0.0537 0.074 Uiso 1 1 calc R . .
H17B H 0.7687 0.6335 -0.0948 0.074 Uiso 1 1 calc R . .
H17C H 0.6040 0.6293 -0.0513 0.074 Uiso 1 1 calc R . .
C18 C 0.7449(2) 0.7587(2) 0.00938(13) 0.0393(5) Uani 1 1 d D . .
H18A H 0.8035 0.7987 -0.0336 0.059 Uiso 1 1 calc R . .
H18B H 0.7821 0.7778 0.0492 0.059 Uiso 1 1 calc R . .
H18C H 0.6419 0.7921 0.0130 0.059 Uiso 1 1 calc R . .
C19 C 0.8746(3) 0.2465(2) 0.10803(12) 0.0387(5) Uani 1 1 d D . .
H19A H 0.8017 0.2065 0.1455 0.058 Uiso 1 1 calc R . .
H19B H 0.9733 0.2227 0.1179 0.058 Uiso 1 1 calc R . .
H19C H 0.8683 0.2178 0.0641 0.058 Uiso 1 1 calc R . .
C20 C 0.8552(3) 0.4256(2) 0.16907(13) 0.0499(6) Uani 1 1 d D . .
H20A H 0.8383 0.5184 0.1663 0.075 Uiso 1 1 calc R . .
H20B H 0.9531 0.3989 0.1792 0.075 Uiso 1 1 calc R . .
H20C H 0.7807 0.3862 0.2060 0.075 Uiso 1 1 calc R . .
Na2 Na 0.5000 0.5000 0.5000 0.0578(4) Uani 1 2 d S . .
N4 N 0.3202(3) 0.6533(2) 0.56340(11) 0.0559(6) Uani 1 1 d DU . .
C21 C 0.3834(5) 0.7767(4) 0.5461(3) 0.0785(13) Uani 0.838(10) 1 d PDU A 1
H21A H 0.3582 0.8179 0.5017 0.094 Uiso 0.838(10) 1 calc PR A 1
H21B H 0.3363 0.8311 0.5823 0.094 Uiso 0.838(10) 1 calc PR A 1
C22 C 0.5414(4) 0.7727(4) 0.5399(3) 0.0704(12) Uani 0.838(10) 1 d PDU A 1
H22A H 0.5664 0.7353 0.5851 0.085 Uiso 0.838(10) 1 calc PR A 1
H22B H 0.5708 0.8611 0.5304 0.085 Uiso 0.838(10) 1 calc PR A 1
N5 N 0.6299(3) 0.6987(2) 0.48468(12) 0.0584(6) Uani 1 1 d DU . .
C23 C 0.1720(5) 0.6701(8) 0.5456(4) 0.0682(16) Uani 0.838(10) 1 d PDU A 1
H23A H 0.1108 0.7339 0.5721 0.102 Uiso 0.838(10) 1 calc PR A 1
H23B H 0.1267 0.5889 0.5571 0.102 Uiso 0.838(10) 1 calc PR A 1
H23C H 0.1807 0.6987 0.4959 0.102 Uiso 0.838(10) 1 calc PR A 1
C24 C 0.3029(9) 0.6075(8) 0.6377(2) 0.096(2) Uani 0.838(10) 1 d PDU A 1
H24A H 0.3998 0.5934 0.6506 0.144 Uiso 0.838(10) 1 calc PR A 1
H24B H 0.2552 0.5275 0.6476 0.144 Uiso 0.838(10) 1 calc PR A 1
H24C H 0.2422 0.6712 0.6644 0.144 Uiso 0.838(10) 1 calc PR A 1
C25 C 0.6253(8) 0.7670(7) 0.4155(3) 0.096(2) Uani 0.838(10) 1 d PDU A 1
H25A H 0.5234 0.7794 0.4087 0.144 Uiso 0.838(10) 1 calc PR A 1
H25B H 0.6846 0.7173 0.3803 0.144 Uiso 0.838(10) 1 calc PR A 1
H25C H 0.6649 0.8501 0.4114 0.144 Uiso 0.838(10) 1 calc PR A 1
C26 C 0.7822(5) 0.6838(7) 0.4938(3) 0.0582(13) Uani 0.838(10) 1 d PDU A 1
H26A H 0.7871 0.6414 0.5405 0.087 Uiso 0.838(10) 1 calc PR A 1
H26B H 0.8206 0.7677 0.4875 0.087 Uiso 0.838(10) 1 calc PR A 1
H26C H 0.8413 0.6321 0.4594 0.087 Uiso 0.838(10) 1 calc PR A 1
C21X C 0.3656(13) 0.7761(12) 0.5263(12) 0.067(3) Uani 0.162(10) 1 d PDU A 2
H21C H 0.3221 0.7915 0.4841 0.081 Uiso 0.162(10) 1 calc PR A 2
H21D H 0.3184 0.8421 0.5560 0.081 Uiso 0.162(10) 1 calc PR A 2
C22X C 0.5196(13) 0.7998(11) 0.5047(14) 0.076(3) Uani 0.162(10) 1 d PDU A 2
H22C H 0.5270 0.8681 0.4649 0.092 Uiso 0.162(10) 1 calc PR A 2
H22D H 0.5482 0.8350 0.5431 0.092 Uiso 0.162(10) 1 calc PR A 2
C23X C 0.166(2) 0.644(4) 0.559(2) 0.055(5) Uani 0.162(10) 1 d PDU A 2
H23D H 0.1322 0.5637 0.5847 0.082 Uiso 0.162(10) 1 calc PR A 2
H23E H 0.1588 0.6467 0.5100 0.082 Uiso 0.162(10) 1 calc PR A 2
H23F H 0.1046 0.7155 0.5784 0.082 Uiso 0.162(10) 1 calc PR A 2
C24X C 0.332(4) 0.643(3) 0.6363(7) 0.062(5) Uani 0.162(10) 1 d PDU A 2
H24D H 0.3029 0.5604 0.6602 0.094 Uiso 0.162(10) 1 calc PR A 2
H24E H 0.2682 0.7112 0.6583 0.094 Uiso 0.162(10) 1 calc PR A 2
H24F H 0.4345 0.6521 0.6392 0.094 Uiso 0.162(10) 1 calc PR A 2
C25X C 0.670(3) 0.706(2) 0.4079(4) 0.056(4) Uani 0.162(10) 1 d PDU A 2
H25D H 0.5823 0.6990 0.3892 0.084 Uiso 0.162(10) 1 calc PR A 2
H25E H 0.7438 0.6366 0.3951 0.084 Uiso 0.162(10) 1 calc PR A 2
H25F H 0.7105 0.7879 0.3887 0.084 Uiso 0.162(10) 1 calc PR A 2
C26X C 0.7643(19) 0.698(4) 0.5110(15) 0.057(5) Uani 0.162(10) 1 d PDU A 2
H26D H 0.8306 0.6242 0.4976 0.086 Uiso 0.162(10) 1 calc PR A 2
H26E H 0.7407 0.6935 0.5617 0.086 Uiso 0.162(10) 1 calc PR A 2
H26F H 0.8124 0.7763 0.4914 0.086 Uiso 0.162(10) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.02625(13) 0.02078(12) 0.03232(14) -0.00407(9) -0.00130(9) -0.00221(9)
C1 0.0440(13) 0.0267(11) 0.0320(12) -0.0003(9) -0.0032(10) -0.0070(9)
C2 0.109(3) 0.0419(16) 0.0417(16) 0.0076(12) -0.0213(16) -0.0169(16)
C3 0.0569(18) 0.0418(16) 0.076(2) 0.0099(14) 0.0081(15) -0.0142(13)
C4 0.0612(17) 0.0293(13) 0.0523(16) -0.0004(11) -0.0074(13) 0.0065(11)
C5 0.0269(11) 0.0280(11) 0.0436(13) -0.0090(9) -0.0123(9) 0.0008(9)
C6 0.0418(15) 0.0410(14) 0.0770(19) -0.0135(13) -0.0248(13) -0.0046(11)
C7 0.0401(14) 0.0625(17) 0.0447(15) -0.0207(13) -0.0100(11) -0.0009(12)
C8 0.0489(15) 0.0330(13) 0.0560(16) -0.0019(11) -0.0200(12) 0.0044(11)
N1 0.0325(10) 0.0218(9) 0.0361(10) -0.0068(7) -0.0048(8) -0.0043(7)
Si1 0.0395(4) 0.0294(3) 0.0355(3) -0.0090(3) -0.0051(3) 0.0054(3)
C9 0.082(2) 0.0398(16) 0.072(2) -0.0073(14) -0.0066(17) 0.0262(15)
C10 0.081(2) 0.103(3) 0.0417(17) -0.0257(17) -0.0121(15) 0.023(2)
C11 0.0409(16) 0.083(2) 0.086(2) -0.0354(19) 0.0164(15) -0.0068(15)
Si2 0.0334(3) 0.0284(3) 0.0332(3) -0.0017(2) -0.0092(3) -0.0086(2)
C12 0.0620(18) 0.0627(18) 0.0515(17) 0.0154(14) -0.0207(14) -0.0315(15)
C13 0.0346(14) 0.0543(16) 0.0599(17) -0.0138(13) 0.0057(12) -0.0024(12)
C14 0.0545(17) 0.0542(17) 0.0565(17) -0.0109(13) -0.0243(13) -0.0129(13)
Na1 0.0214(6) 0.0485(8) 0.0461(8) 0.0231(6) 0.0075(5) 0.0101(5)
N2 0.0243(9) 0.0258(9) 0.0337(10) 0.0006(7) -0.0027(7) 0.0022(7)
C15 0.0237(11) 0.0321(12) 0.0436(13) -0.0011(10) 0.0046(9) 0.0037(9)
C16 0.0238(11) 0.0311(12) 0.0397(13) -0.0013(9) 0.0004(9) -0.0027(9)
N3 0.0255(9) 0.0268(9) 0.0277(9) 0.0018(7) -0.0024(7) -0.0021(7)
C17 0.0574(17) 0.0436(15) 0.0485(16) -0.0058(12) -0.0203(13) 0.0058(12)
C18 0.0321(12) 0.0294(12) 0.0524(15) 0.0021(10) -0.0058(11) 0.0007(9)
C19 0.0405(13) 0.0297(12) 0.0427(14) 0.0001(10) -0.0069(10) 0.0031(10)
C20 0.0656(18) 0.0438(15) 0.0445(15) -0.0049(12) -0.0162(13) -0.0129(13)
Na2 0.0465(8) 0.0444(8) 0.0749(10) -0.0272(7) 0.0272(7) -0.0196(7)
N4 0.0567(13) 0.0638(14) 0.0425(12) -0.0184(11) 0.0031(10) 0.0079(11)
C21 0.090(2) 0.057(2) 0.097(3) -0.0369(19) -0.027(2) 0.0073(18)
C22 0.087(2) 0.042(2) 0.098(3) -0.0247(19) -0.047(2) 0.0054(17)
N5 0.0624(14) 0.0477(13) 0.0658(15) 0.0042(11) -0.0120(11) -0.0242(11)
C23 0.061(2) 0.090(4) 0.047(4) -0.009(3) -0.004(2) 0.009(2)
C24 0.074(4) 0.152(6) 0.046(2) -0.005(3) -0.007(2) 0.043(4)
C25 0.105(5) 0.104(5) 0.091(3) 0.040(3) -0.054(3) -0.063(4)
C26 0.065(2) 0.058(3) 0.051(3) 0.003(2) -0.0097(19) -0.021(2)
C21X 0.074(4) 0.053(5) 0.081(6) -0.019(5) -0.028(5) 0.006(4)
C22X 0.081(4) 0.050(4) 0.098(5) -0.003(5) -0.023(5) -0.005(3)
C23X 0.058(6) 0.075(11) 0.025(10) -0.007(9) 0.002(6) 0.006(7)
C24X 0.075(11) 0.070(10) 0.052(5) -0.039(6) -0.011(8) -0.009(9)
C25X 0.043(9) 0.052(10) 0.078(4) 0.011(7) -0.030(6) -0.020(7)
C26X 0.064(7) 0.057(10) 0.055(10) -0.021(10) -0.007(8) -0.015(7)

_geom_special_details            
;
;

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
Zn C1 2.052(2) . ?
Zn C5 2.048(2) . ?
Zn N1 2.0284(17) . ?
C1 C2 1.522(4) . ?
C1 C3 1.528(3) . ?
C1 C4 1.525(3) . ?
C5 C6 1.529(3) . ?
C5 C7 1.527(3) . ?
C5 C8 1.525(3) . ?
N1 Si1 1.6855(18) . ?
N1 Si2 1.6888(18) . ?
Si1 C9 1.879(3) . ?
Si1 C10 1.873(3) . ?
Si1 C11 1.874(3) . ?
Si2 C12 1.881(3) . ?
Si2 C13 1.873(3) . ?
Si2 C14 1.887(2) . ?
Na1 N2 2.4777(16) . ?
Na1 N3 2.4873(16) . ?
N2 C15 1.473(3) . ?
N2 C17 1.467(3) . ?
N2 C18 1.466(3) . ?
C15 C16 1.508(3) . ?
C16 N3 1.473(3) . ?
N3 C19 1.469(3) . ?
N3 C20 1.461(3) . ?
Na2 N4 2.489(2) . ?
Na2 N5 2.500(2) . ?
N4 C21 1.464(4) . ?
N4 C23 1.483(4) . ?
N4 C24 1.467(4) . ?
N4 C21X 1.465(8) . ?
N4 C23X 1.474(8) . ?
N4 C24X 1.464(8) . ?
C21 C22 1.450(5) . ?
C22 N5 1.497(4) . ?
N5 C25 1.466(4) . ?
N5 C26 1.458(4) . ?
N5 C22X 1.446(8) . ?
N5 C25X 1.487(8) . ?
N5 C26X 1.454(8) . ?
C21X C22X 1.450(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zn C5 127.40(9) . . ?
C1 Zn N1 115.65(8) . . ?
C5 Zn N1 116.91(8) . . ?
Zn C1 C2 110.91(15) . . ?
Zn C1 C3 110.22(17) . . ?
Zn C1 C4 110.60(15) . . ?
C2 C1 C3 109.3(2) . . ?
C2 C1 C4 107.5(2) . . ?
C3 C1 C4 108.2(2) . . ?
Zn C5 C6 111.63(16) . . ?
Zn C5 C7 108.43(15) . . ?
Zn C5 C8 113.10(16) . . ?
C6 C5 C7 107.6(2) . . ?
C6 C5 C8 108.17(19) . . ?
C7 C5 C8 107.7(2) . . ?
Zn N1 Si1 114.06(9) . . ?
Zn N1 Si2 116.95(9) . . ?
Si1 N1 Si2 127.88(10) . . ?
N1 Si1 C9 113.20(12) . . ?
N1 Si1 C10 114.07(12) . . ?
N1 Si1 C11 110.75(11) . . ?
C9 Si1 C10 106.92(16) . . ?
C9 Si1 C11 107.04(16) . . ?
C10 Si1 C11 104.24(16) . . ?
N1 Si2 C12 113.71(11) . . ?
N1 Si2 C13 110.30(10) . . ?
N1 Si2 C14 114.09(11) . . ?
C12 Si2 C13 106.42(14) . . ?
C12 Si2 C14 104.63(13) . . ?
C13 Si2 C14 107.15(13) . . ?
N2 Na1 N3 75.86(5) . . ?
N2 Na1 N3 104.14(5) . 2_765 ?
Na1 N2 C15 106.22(12) . . ?
Na1 N2 C17 103.05(13) . . ?
Na1 N2 C18 119.35(13) . . ?
C15 N2 C17 110.03(18) . . ?
C15 N2 C18 109.22(17) . . ?
C17 N2 C18 108.66(17) . . ?
N2 C15 C16 114.26(17) . . ?
C15 C16 N3 113.50(17) . . ?
Na1 N3 C16 101.55(11) . . ?
Na1 N3 C19 113.26(13) . . ?
Na1 N3 C20 114.33(14) . . ?
C16 N3 C19 108.91(16) . . ?
C16 N3 C20 110.30(18) . . ?
C19 N3 C20 108.24(17) . . ?
N4 Na2 N5 75.06(8) . . ?
N4 Na2 N5 104.94(8) . 2_666 ?
Na2 N4 C21 106.3(2) . . ?
Na2 N4 C23 115.8(4) . . ?
Na2 N4 C24 107.5(3) . . ?
Na2 N4 C21X 102.1(7) . . ?
Na2 N4 C23X 114.5(19) . . ?
Na2 N4 C24X 111.7(16) . . ?
C21 N4 C23 107.7(4) . . ?
C21 N4 C24 111.9(4) . . ?
C23 N4 C24 107.8(3) . . ?
C21X N4 C23X 108.1(11) . . ?
C21X N4 C24X 110.5(11) . . ?
C23X N4 C24X 109.6(12) . . ?
N4 C21 C22 115.7(3) . . ?
C21 C22 N5 115.1(3) . . ?
Na2 N5 C22 103.53(19) . . ?
Na2 N5 C25 109.1(3) . . ?
Na2 N5 C26 116.9(3) . . ?
Na2 N5 C22X 107.0(5) . . ?
Na2 N5 C25X 94.8(10) . . ?
Na2 N5 C26X 120.4(18) . . ?
C22 N5 C25 110.9(4) . . ?
C22 N5 C26 108.1(3) . . ?
C25 N5 C26 108.2(3) . . ?
C22X N5 C25X 110.3(10) . . ?
C22X N5 C26X 114.5(12) . . ?
C25X N5 C26X 107.9(11) . . ?
N4 C21X C22X 121.3(10) . . ?
N5 C22X C21X 121.0(11) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054

#===END

data_rem332_compound_4
_database_code_depnum_ccdc_archive 'CCDC 660909'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H53 N4 Na Zn'
_chemical_formula_sum            'C22 H53 N4 Na Zn'
_chemical_formula_weight         462.04

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'
Na Na 0.0362 0.0249 '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   'C 2/c'

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

_cell_length_a                   10.8591(9)
_cell_length_b                   18.6245(16)
_cell_length_c                   14.1986(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5662(13)
_cell_angle_gamma                90.00
_cell_volume                     2822.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10781
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      28.65

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.44
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7807
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         22.49
_reflns_number_total             1852
_reflns_number_gt                1784
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_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 and local programs'

_refine_special_details          
;
Restraints: 'rigid bond' (DELU) and similarity (SIMU) restraints for
all C atoms, many of which have been resolved as disordered and others
may be disordered also, to control the displacement parameters
of overlapping components; also geometrical similarity restraints
(SADI) for C-C bond lengths in disordered groups.
Such restraints are often required for
disorder components that interpenetrate each other, since the
electron density of the disordered atoms strongly overlap and can
not be resolved satisfactorily in free refinement. Restraints are
gentler and more flexible than rigid constraints.
;

_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^)+(0.0299P)^2^+14.3536P] 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         1852
_refine_ls_number_parameters     179
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1239
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.178
_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
Zn Zn 0.5000 0.62965(4) 0.7500 0.0320(3) Uani 1 2 d S . .
Na Na 0.5000 0.79244(12) 0.7500 0.0360(6) Uani 1 2 d S . .
N1 N 0.4486(4) 0.8989(2) 0.6442(3) 0.0594(12) Uani 1 1 d . A .
N2 N 0.6157(3) 0.69535(19) 0.6937(3) 0.0398(9) Uani 1 1 d . A .
C1 C 0.4534(8) 0.9608(3) 0.7084(5) 0.104(3) Uani 1 1 d U . .
H1A H 0.4646 1.0044 0.6712 0.124 Uiso 1 1 calc R A .
H1B H 0.3710 0.9648 0.7284 0.124 Uiso 1 1 calc R . .
C2 C 0.3265(6) 0.8985(4) 0.5831(5) 0.084(2) Uani 1 1 d U . .
H2A H 0.2615 0.8981 0.6227 0.126 Uiso 1 1 calc R A .
H2B H 0.3182 0.8556 0.5425 0.126 Uiso 1 1 calc R . .
H2C H 0.3171 0.9415 0.5427 0.126 Uiso 1 1 calc R . .
C3 C 0.5434(7) 0.9006(4) 0.5834(5) 0.097(2) Uani 1 1 d U . .
H3A H 0.6270 0.9005 0.6236 0.145 Uiso 1 1 calc R A .
H3B H 0.5329 0.9442 0.5440 0.145 Uiso 1 1 calc R . .
H3C H 0.5340 0.8583 0.5417 0.145 Uiso 1 1 calc R . .
C4 C 0.7375(11) 0.7147(6) 0.7666(10) 0.040(3) Uani 0.536(13) 1 d PDU A 1
H4 H 0.7058 0.7329 0.8240 0.048 Uiso 0.536(13) 1 calc PR A 1
C4A C 0.7418(15) 0.6903(9) 0.7287(10) 0.053(4) Uani 0.464(13) 1 d PDU A 2
H4A H 0.7760 0.6450 0.7059 0.063 Uiso 0.464(13) 1 calc PR A 2
C5 C 0.8199(11) 0.6511(6) 0.8047(9) 0.067(4) Uani 0.536(13) 1 d PDU A 1
H5A H 0.7677 0.6127 0.8236 0.100 Uiso 0.536(13) 1 calc PR A 1
H5B H 0.8817 0.6662 0.8604 0.100 Uiso 0.536(13) 1 calc PR A 1
H5C H 0.8634 0.6334 0.7546 0.100 Uiso 0.536(13) 1 calc PR A 1
C5A C 0.7558(11) 0.6895(8) 0.8373(9) 0.061(4) Uani 0.464(13) 1 d PDU A 2
H5A1 H 0.7120 0.6476 0.8570 0.092 Uiso 0.464(13) 1 calc PR A 2
H5A2 H 0.7196 0.7334 0.8586 0.092 Uiso 0.464(13) 1 calc PR A 2
H5A3 H 0.8449 0.6868 0.8663 0.092 Uiso 0.464(13) 1 calc PR A 2
C6 C 0.8138(19) 0.7770(8) 0.7384(11) 0.061(4) Uani 0.536(13) 1 d PDU A 1
H6A H 0.7579 0.8174 0.7166 0.092 Uiso 0.536(13) 1 calc PR A 1
H6B H 0.8565 0.7619 0.6867 0.092 Uiso 0.536(13) 1 calc PR A 1
H6C H 0.8760 0.7919 0.7940 0.092 Uiso 0.536(13) 1 calc PR A 1
C6A C 0.8134(18) 0.7548(11) 0.7014(17) 0.088(8) Uani 0.464(13) 1 d PDU A 2
H6A1 H 0.8002 0.7589 0.6315 0.132 Uiso 0.464(13) 1 calc PR A 2
H6A2 H 0.9030 0.7487 0.7268 0.132 Uiso 0.464(13) 1 calc PR A 2
H6A3 H 0.7832 0.7985 0.7283 0.132 Uiso 0.464(13) 1 calc PR A 2
C7 C 0.6151(7) 0.6909(3) 0.5912(4) 0.0758(18) Uani 1 1 d DU . .
H7A H 0.6424 0.7397 0.5738 0.091 Uiso 0.50 1 calc PR A 1
H7B H 0.6478 0.7378 0.5719 0.091 Uiso 0.50 1 d PR A 2
C8 C 0.4826(8) 0.6847(4) 0.5387(4) 0.112(3) Uani 1 1 d DU A .
H8A H 0.4818 0.6824 0.4697 0.168 Uiso 1 1 calc R . .
H8B H 0.4346 0.7265 0.5530 0.168 Uiso 1 1 calc R . .
H8C H 0.4449 0.6409 0.5592 0.168 Uiso 1 1 calc R . .
C9 C 0.723(2) 0.6396(9) 0.5732(15) 0.091(5) Uani 0.536(13) 1 d PU A 1
H9A H 0.8014 0.6534 0.6151 0.137 Uiso 0.536(13) 1 calc PR A 1
H9B H 0.7326 0.6432 0.5061 0.137 Uiso 0.536(13) 1 calc PR A 1
H9C H 0.7018 0.5900 0.5872 0.137 Uiso 0.536(13) 1 calc PR A 1
C9A C 0.668(3) 0.6213(13) 0.544(2) 0.118(8) Uani 0.464(13) 1 d PU A 2
H9D H 0.7574 0.6156 0.5696 0.178 Uiso 0.464(13) 1 calc PR A 2
H9E H 0.6557 0.6275 0.4741 0.178 Uiso 0.464(13) 1 calc PR A 2
H9F H 0.6226 0.5784 0.5586 0.178 Uiso 0.464(13) 1 calc PR A 2
C10 C 0.5000 0.5199(4) 0.7500 0.068(2) Uani 1 2 d SDU . .
C11 C 0.566(2) 0.4889(7) 0.8413(12) 0.123(6) Uani 0.50 1 d PDU A -1
H11A H 0.6539 0.5046 0.8530 0.184 Uiso 0.50 1 calc PR A -1
H11B H 0.5629 0.4364 0.8374 0.184 Uiso 0.50 1 calc PR A -1
H11C H 0.5260 0.5051 0.8939 0.184 Uiso 0.50 1 calc PR A -1
C12 C 0.555(2) 0.4896(7) 0.6649(15) 0.130(6) Uani 0.50 1 d PDU A -1
H12A H 0.5106 0.5104 0.6049 0.196 Uiso 0.50 1 calc PR A -1
H12B H 0.5458 0.4373 0.6628 0.196 Uiso 0.50 1 calc PR A -1
H12C H 0.6443 0.5020 0.6734 0.196 Uiso 0.50 1 calc PR A -1
C13 C 0.3645(10) 0.4957(7) 0.7271(14) 0.090(4) Uani 0.50 1 d PDU A -1
H13A H 0.3238 0.5167 0.6660 0.135 Uiso 0.50 1 calc PR A -1
H13B H 0.3209 0.5114 0.7781 0.135 Uiso 0.50 1 calc PR A -1
H13C H 0.3612 0.4432 0.7223 0.135 Uiso 0.50 1 calc PR A -1

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
Zn 0.0316(4) 0.0267(4) 0.0372(4) 0.000 0.0052(3) 0.000
Na 0.0388(13) 0.0333(13) 0.0352(13) 0.000 0.0044(10) 0.000
N1 0.077(3) 0.048(3) 0.051(3) 0.010(2) 0.005(2) 0.010(2)
N2 0.034(2) 0.040(2) 0.048(2) 0.0064(18) 0.0155(18) 0.0032(17)
C1 0.152(7) 0.041(3) 0.099(5) 0.008(3) -0.026(5) 0.012(4)
C2 0.085(5) 0.093(5) 0.071(4) 0.016(4) 0.005(4) 0.035(4)
C3 0.095(5) 0.094(5) 0.105(5) 0.056(4) 0.027(4) 0.022(4)
C4 0.025(5) 0.048(7) 0.044(8) -0.003(6) 0.002(5) 0.000(5)
C4A 0.042(8) 0.055(10) 0.064(9) 0.006(7) 0.017(8) -0.003(7)
C5 0.058(7) 0.061(7) 0.074(8) 0.010(6) -0.009(6) 0.010(5)
C5A 0.035(7) 0.074(10) 0.063(8) 0.013(7) -0.023(6) -0.013(6)
C6 0.068(9) 0.050(6) 0.068(10) -0.010(6) 0.016(8) -0.014(6)
C6A 0.025(8) 0.119(17) 0.109(15) 0.035(12) -0.016(9) -0.041(10)
C7 0.136(5) 0.049(3) 0.057(4) 0.009(3) 0.057(4) 0.016(3)
C8 0.185(7) 0.109(6) 0.031(3) 0.001(4) -0.012(4) 0.002(6)
C9 0.188(13) 0.041(10) 0.064(11) -0.014(7) 0.070(10) 0.020(10)
C9A 0.218(19) 0.060(13) 0.11(2) -0.040(10) 0.104(16) -0.008(13)
C10 0.071(5) 0.030(4) 0.115(6) 0.000 0.050(5) 0.000
C11 0.157(14) 0.036(8) 0.163(11) 0.034(9) -0.002(11) 0.010(10)
C12 0.190(16) 0.044(8) 0.191(13) -0.038(10) 0.125(14) -0.014(11)
C13 0.102(8) 0.041(7) 0.133(12) -0.012(8) 0.034(7) -0.034(7)

_geom_special_details            
;
;

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
Zn N2 2.020(4) . ?
Zn N2 2.020(3) 2_656 ?
Zn C10 2.044(7) . ?
Na N1 2.489(4) . ?
Na N1 2.489(4) 2_656 ?
Na N2 2.419(4) . ?
Na N2 2.419(4) 2_656 ?
Na C4 2.929(11) . ?
Na C4 2.929(11) 2_656 ?
N1 C1 1.463(8) . ?
N1 C2 1.445(7) . ?
N1 C3 1.461(8) . ?
N2 C4 1.565(13) . ?
N2 C4A 1.372(16) . ?
N2 C7 1.457(6) . ?
C1 C1 1.408(12) 2_656 ?
C4 C5 1.524(11) . ?
C4 C6 1.521(11) . ?
C4A C5A 1.521(12) . ?
C4A C6A 1.520(12) . ?
C7 C8 1.498(9) . ?
C7 C9 1.568(19) . ?
C7 C9A 1.62(2) . ?
C10 C11 1.480(11) . ?
C10 C12 1.550(11) . ?
C10 C13 1.516(10) . ?

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 Zn N2 105.4(2) . 2_656 ?
N2 Zn C10 127.28(10) . . ?
N2 Zn C10 127.28(10) 2_656 . ?
N1 Na N1 74.3(2) . 2_656 ?
N1 Na N2 117.97(14) . . ?
N1 Na N2 136.25(14) . 2_656 ?
N1 Na N2 136.24(14) 2_656 . ?
N1 Na N2 117.97(14) 2_656 2_656 ?
N1 Na C4 122.6(3) . . ?
N1 Na C4 104.4(3) 2_656 . ?
N1 Na C4 104.4(3) . 2_656 ?
N1 Na C4 122.6(3) 2_656 2_656 ?
N2 Na N2 83.26(18) . 2_656 ?
N2 Na C4 32.3(3) . . ?
N2 Na C4 96.1(3) 2_656 . ?
N2 Na C4 96.1(3) . 2_656 ?
N2 Na C4 32.3(3) 2_656 2_656 ?
C4 Na C4 120.8(5) . 2_656 ?
Na N1 C1 105.8(3) . . ?
Na N1 C2 116.0(4) . . ?
Na N1 C3 105.6(3) . . ?
C1 N1 C2 107.6(5) . . ?
C1 N1 C3 113.8(6) . . ?
C2 N1 C3 108.3(5) . . ?
Zn N2 Na 85.65(13) . . ?
Zn N2 C4 113.0(5) . . ?
Zn N2 C4A 117.8(6) . . ?
Zn N2 C7 118.1(4) . . ?
Na N2 C4 92.1(4) . . ?
Na N2 C4A 118.4(8) . . ?
Na N2 C7 117.7(3) . . ?
C4 N2 C7 121.4(6) . . ?
C4A N2 C7 100.3(7) . . ?
N1 C1 C1 117.4(5) . 2_656 ?
Na C4 N2 55.6(3) . . ?
Na C4 C5 149.8(9) . . ?
Na C4 C6 96.6(9) . . ?
N2 C4 C5 115.2(9) . . ?
N2 C4 C6 115.9(10) . . ?
C5 C4 C6 112.0(12) . . ?
N2 C4A C5A 106.0(11) . . ?
N2 C4A C6A 112.1(13) . . ?
C5A C4A C6A 107.8(14) . . ?
N2 C7 C8 109.2(5) . . ?
N2 C7 C9 109.3(9) . . ?
N2 C7 C9A 121.7(13) . . ?
C8 C7 C9 123.2(9) . . ?
C8 C7 C9A 96.4(12) . . ?
Zn C10 C11 113.0(6) . . ?
Zn C10 C12 111.3(6) . . ?
Zn C10 C13 107.3(6) . . ?
C11 C10 C12 110.2(10) . . ?
C11 C10 C13 111.6(9) . . ?
C12 C10 C13 102.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        22.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.063

#===END

data_grem204_compound5
_database_code_depnum_ccdc_archive 'CCDC 660910'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H50 N3 Na Zn'
_chemical_formula_sum            'C29 H50 N3 Na Zn'
_chemical_formula_weight         529.08
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   8.9412(2)
_cell_length_b                   17.3511(6)
_cell_length_c                   20.8700(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.524(2)
_cell_angle_gamma                90.00
_cell_volume                     3202.00(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5854
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      25.03

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Nonious KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42285
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.03
_reflns_number_total             11301
_reflns_number_gt                8844
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'DENZO & COLLECT'
_computing_cell_refinement       'DENZO & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    SIR
_computing_structure_refinement  SHELXL97
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97

_refine_special_details          
;
Restraint: to fix the "floating origin" along the polar b axis.
;

_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^)+(0.0149P)^2^+3.5949P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(10)
_refine_ls_number_reflns         11301
_refine_ls_number_parameters     678
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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 0.14282(5) 1.11344(3) 0.52098(2) 0.02958(11) Uani 1 1 d . A .
Na1 Na 0.11311(17) 0.99526(9) 0.37119(8) 0.0367(4) Uani 1 1 d . . .
N1 N 0.2474(3) 1.08739(17) 0.44169(16) 0.0272(8) Uani 1 1 d . . .
N2 N -0.0825(4) 0.9492(2) 0.28147(18) 0.0423(9) Uani 1 1 d . . .
N3 N 0.2343(4) 0.8872(2) 0.32570(17) 0.0382(9) Uani 1 1 d . . .
C1 C 0.1503(5) 1.2146(2) 0.4053(2) 0.0370(11) Uani 1 1 d . . .
H1A H 0.0599 1.1885 0.3833 0.056 Uiso 1 1 calc R . .
H1B H 0.1716 1.2600 0.3803 0.056 Uiso 1 1 calc R . .
H1C H 0.1331 1.2306 0.4487 0.056 Uiso 1 1 calc R . .
C2 C 0.2843(4) 1.1598(2) 0.4112(2) 0.0315(10) Uani 1 1 d . . .
H2 H 0.3695 1.1844 0.4405 0.038 Uiso 1 1 calc R . .
C3 C 0.3372(5) 1.1467(2) 0.3464(2) 0.0394(11) Uani 1 1 d . . .
C4 C 0.2367(6) 1.1311(3) 0.2907(2) 0.0497(13) Uani 1 1 d . . .
H4 H 0.1312 1.1293 0.2924 0.060 Uiso 1 1 calc R . .
C5 C 0.2914(7) 1.1180(3) 0.2314(2) 0.0708(16) Uani 1 1 d . . .
H5 H 0.2236 1.1077 0.1928 0.085 Uiso 1 1 calc R . .
C6 C 0.4474(8) 1.1206(4) 0.2309(3) 0.0782(19) Uani 1 1 d . . .
H6 H 0.4851 1.1122 0.1913 0.094 Uiso 1 1 calc R . .
C7 C 0.5460(8) 1.1345(3) 0.2849(4) 0.0792(19) Uani 1 1 d . . .
H7 H 0.6517 1.1351 0.2835 0.095 Uiso 1 1 calc R . .
C8 C 0.4919(6) 1.1477(3) 0.3416(3) 0.0567(14) Uani 1 1 d . . .
H8 H 0.5620 1.1581 0.3795 0.068 Uiso 1 1 calc R . .
C9 C 0.3882(4) 1.0437(2) 0.4609(2) 0.0301(10) Uani 1 1 d . . .
H9A H 0.4605 1.0769 0.4889 0.036 Uiso 1 1 calc R . .
H9B H 0.4334 1.0318 0.4215 0.036 Uiso 1 1 calc R . .
C10 C 0.3696(4) 0.9699(2) 0.49606(19) 0.0306(10) Uani 1 1 d . . .
C11 C 0.2335(5) 0.9450(2) 0.5140(2) 0.0332(10) Uani 1 1 d . . .
H11 H 0.1449 0.9751 0.5025 0.040 Uiso 1 1 calc R . .
C12 C 0.2249(5) 0.8774(3) 0.5483(2) 0.0401(11) Uani 1 1 d . . .
H12 H 0.1307 0.8619 0.5600 0.048 Uiso 1 1 calc R . .
C13 C 0.3508(5) 0.8324(3) 0.5657(2) 0.0437(11) Uani 1 1 d . . .
H13 H 0.3447 0.7863 0.5897 0.052 Uiso 1 1 calc R . .
C14 C 0.4859(5) 0.8554(2) 0.5476(2) 0.0429(12) Uani 1 1 d . . .
H14 H 0.5735 0.8244 0.5586 0.051 Uiso 1 1 calc R . .
C15 C 0.4954(5) 0.9229(2) 0.5137(2) 0.0361(11) Uani 1 1 d . . .
H15 H 0.5900 0.9378 0.5021 0.043 Uiso 1 1 calc R . .
C16 C -0.0816(5) 1.0870(2) 0.5104(2) 0.0357(11) Uani 1 1 d . . .
C17 C -0.1424(4) 1.0441(3) 0.4472(2) 0.0387(11) Uani 1 1 d . . .
H17A H -0.0928 0.9937 0.4470 0.058 Uiso 1 1 calc R . .
H17B H -0.1211 1.0744 0.4100 0.058 Uiso 1 1 calc R . .
H17C H -0.2518 1.0368 0.4446 0.058 Uiso 1 1 calc R . .
C18 C -0.1678(5) 1.1636(3) 0.5085(3) 0.0569(15) Uani 1 1 d . . .
H18A H -0.2766 1.1533 0.5038 0.085 Uiso 1 1 calc R . .
H18B H -0.1457 1.1944 0.4717 0.085 Uiso 1 1 calc R . .
H18C H -0.1360 1.1919 0.5488 0.085 Uiso 1 1 calc R . .
C19 C -0.1209(5) 1.0390(3) 0.5673(2) 0.0493(14) Uani 1 1 d . . .
H19A H -0.2310 1.0351 0.5645 0.074 Uiso 1 1 calc R . .
H19B H -0.0790 1.0639 0.6082 0.074 Uiso 1 1 calc R . .
H19C H -0.0777 0.9872 0.5656 0.074 Uiso 1 1 calc R . .
C20 C 0.2688(5) 1.1680(3) 0.5973(2) 0.0401(11) Uani 1 1 d . . .
C21 C 0.3686(12) 1.2310(6) 0.5792(4) 0.074(3) Uani 0.601(6) 1 d P A 1
H21A H 0.4143 1.2583 0.6184 0.111 Uiso 0.601(6) 1 calc PR A 1
H21B H 0.3084 1.2672 0.5499 0.111 Uiso 0.601(6) 1 calc PR A 1
H21C H 0.4485 1.2088 0.5575 0.111 Uiso 0.601(6) 1 calc PR A 1
C22 C 0.1643(9) 1.2010(6) 0.6420(4) 0.053(3) Uani 0.601(6) 1 d P A 1
H22A H 0.0970 1.1604 0.6535 0.079 Uiso 0.601(6) 1 calc PR A 1
H22B H 0.1037 1.2428 0.6196 0.079 Uiso 0.601(6) 1 calc PR A 1
H22C H 0.2249 1.2212 0.6814 0.079 Uiso 0.601(6) 1 calc PR A 1
C23 C 0.3668(10) 1.1088(6) 0.6366(4) 0.065(3) Uani 0.601(6) 1 d P A 1
H23A H 0.4253 1.1338 0.6744 0.098 Uiso 0.601(6) 1 calc PR A 1
H23B H 0.4361 1.0857 0.6098 0.098 Uiso 0.601(6) 1 calc PR A 1
H23C H 0.3027 1.0686 0.6511 0.098 Uiso 0.601(6) 1 calc PR A 1
C24 C -0.2298(5) 0.9337(3) 0.3005(2) 0.0532(14) Uani 1 1 d . . .
H24A H -0.2760 0.9823 0.3114 0.080 Uiso 1 1 calc R . .
H24B H -0.2174 0.8996 0.3384 0.080 Uiso 1 1 calc R . .
H24C H -0.2951 0.9087 0.2646 0.080 Uiso 1 1 calc R . .
C25 C -0.0995(6) 1.0041(4) 0.2283(3) 0.0682(16) Uani 1 1 d . . .
H25A H -0.1680 0.9828 0.1915 0.102 Uiso 1 1 calc R . .
H25B H -0.0006 1.0142 0.2151 0.102 Uiso 1 1 calc R . .
H25C H -0.1416 1.0524 0.2423 0.102 Uiso 1 1 calc R . .
C26 C -0.0197(6) 0.8749(3) 0.2620(3) 0.0604(15) Uani 1 1 d . . .
H26A H -0.0458 0.8341 0.2917 0.072 Uiso 1 1 calc R . .
H26B H -0.0701 0.8617 0.2179 0.072 Uiso 1 1 calc R . .
C27 C 0.1432(6) 0.8735(3) 0.2622(2) 0.0601(15) Uani 1 1 d . . .
H27A H 0.1692 0.9131 0.2315 0.072 Uiso 1 1 calc R . .
H27B H 0.1712 0.8226 0.2460 0.072 Uiso 1 1 calc R . .
C28 C 0.2362(5) 0.8193(3) 0.3670(2) 0.0470(12) Uani 1 1 d . . .
H28A H 0.1342 0.8098 0.3771 0.070 Uiso 1 1 calc R . .
H28B H 0.3057 0.8280 0.4073 0.070 Uiso 1 1 calc R . .
H28C H 0.2700 0.7745 0.3444 0.070 Uiso 1 1 calc R . .
C29 C 0.3914(5) 0.9040(3) 0.3155(3) 0.0597(15) Uani 1 1 d . . .
H29A H 0.4541 0.9133 0.3574 0.090 Uiso 1 1 calc R . .
H29B H 0.3922 0.9499 0.2881 0.090 Uiso 1 1 calc R . .
H29C H 0.4318 0.8600 0.2941 0.090 Uiso 1 1 calc R . .
Zn1A Zn 0.58088(8) 1.33252(3) -0.02676(3) 0.05759(19) Uani 1 1 d . . .
Na1A Na 0.74865(19) 1.41005(10) 0.13728(8) 0.0443(4) Uani 1 1 d . . .
N1A N 0.5651(4) 1.3306(2) 0.07079(16) 0.0390(9) Uani 1 1 d . A .
N2A N 0.9452(4) 1.5102(2) 0.1743(2) 0.0527(11) Uani 1 1 d . A .
N3A N 0.8988(4) 1.3564(2) 0.23558(18) 0.0428(10) Uani 1 1 d . A .
C1A C 0.3167(12) 1.3983(7) 0.0355(5) 0.066(3) Uani 0.601(6) 1 d P A 1
H1A1 H 0.3677 1.4470 0.0289 0.099 Uiso 0.601(6) 1 calc PR A 1
H1A2 H 0.2202 1.4090 0.0507 0.099 Uiso 0.601(6) 1 calc PR A 1
H1A3 H 0.2979 1.3699 -0.0054 0.099 Uiso 0.601(6) 1 calc PR A 1
C2A C 0.4130(5) 1.3518(3) 0.0842(2) 0.0595(15) Uani 1 1 d . . .
H2A H 0.3584 1.3016 0.0850 0.071 Uiso 1 1 calc R A 1
C3A C 0.4218(5) 1.3830(3) 0.1532(2) 0.0461(13) Uani 1 1 d . A .
C4A C 0.4580(5) 1.4580(3) 0.1696(2) 0.0445(12) Uani 1 1 d . A .
H4A H 0.4733 1.4930 0.1362 0.053 Uiso 1 1 calc R . .
C5A C 0.4733(5) 1.4851(3) 0.2325(3) 0.0487(13) Uani 1 1 d . . .
H5A H 0.4999 1.5373 0.2418 0.058 Uiso 1 1 calc R A .
C6A C 0.4496(5) 1.4353(3) 0.2817(3) 0.0514(14) Uani 1 1 d . A .
H6A H 0.4602 1.4530 0.3253 0.062 Uiso 1 1 calc R . .
C7A C 0.4102(5) 1.3597(3) 0.2672(3) 0.0503(14) Uani 1 1 d . . .
H7A H 0.3924 1.3254 0.3007 0.060 Uiso 1 1 calc R A .
C8A C 0.3966(4) 1.3338(3) 0.2035(3) 0.0490(12) Uani 1 1 d . A .
H8A H 0.3697 1.2816 0.1940 0.059 Uiso 1 1 calc R . .
C9A C 0.5945(17) 1.2582(10) 0.1016(8) 0.034(4) Uani 0.601(6) 1 d P A 1
H9A1 H 0.5131 1.2210 0.0862 0.041 Uiso 0.601(6) 1 calc PR A 1
H9A2 H 0.6017 1.2635 0.1492 0.041 Uiso 0.601(6) 1 calc PR A 1
C10A C 0.7610(18) 1.2286(11) 0.0811(8) 0.033(4) Uani 0.601(6) 1 d P A 1
C11A C 0.8504(13) 1.2769(7) 0.0528(6) 0.032(3) Uani 0.601(6) 1 d P A 1
H11A H 0.8198 1.3287 0.0439 0.039 Uiso 0.601(6) 1 calc PR A 1
C12A C 0.9876(10) 1.2508(6) 0.0367(5) 0.043(2) Uani 0.601(6) 1 d P A 1
H12A H 1.0517 1.2840 0.0169 0.052 Uiso 0.601(6) 1 calc PR A 1
C13A C 1.0288(11) 1.1721(8) 0.0512(5) 0.050(3) Uani 0.601(6) 1 d P A 1
H13A H 1.1222 1.1535 0.0408 0.060 Uiso 0.601(6) 1 calc PR A 1
C14A C 0.9359(12) 1.1216(7) 0.0801(5) 0.058(3) Uani 0.601(6) 1 d P A 1
H14A H 0.9627 1.0693 0.0892 0.070 Uiso 0.601(6) 1 calc PR A 1
C15A C 0.8003(10) 1.1537(5) 0.0949(4) 0.037(2) Uiso 0.601(6) 1 d P A 1
H15A H 0.7340 1.1222 0.1151 0.045 Uiso 0.601(6) 1 calc PR A 1
C16A C 0.6473(12) 1.4350(6) -0.0542(5) 0.060(3) Uiso 0.601(6) 1 d P A 1
C17A C 0.7023(12) 1.4904(6) 0.0014(5) 0.071(3) Uiso 0.601(6) 1 d P A 1
H17D H 0.7981 1.4717 0.0252 0.107 Uiso 0.601(6) 1 calc PR A 1
H17E H 0.6266 1.4934 0.0308 0.107 Uiso 0.601(6) 1 calc PR A 1
H17F H 0.7174 1.5418 -0.0162 0.107 Uiso 0.601(6) 1 calc PR A 1
C18A C 0.7690(14) 1.4247(7) -0.0946(7) 0.093(4) Uiso 0.601(6) 1 d P A 1
H18D H 0.7276 1.3995 -0.1354 0.139 Uiso 0.601(6) 1 calc PR A 1
H18E H 0.8496 1.3927 -0.0713 0.139 Uiso 0.601(6) 1 calc PR A 1
H18F H 0.8103 1.4752 -0.1038 0.139 Uiso 0.601(6) 1 calc PR A 1
C19A C 0.5170(16) 1.4808(8) -0.0944(7) 0.121(5) Uiso 0.601(6) 1 d P A 1
H19D H 0.5540 1.5318 -0.1050 0.182 Uiso 0.601(6) 1 calc PR A 1
H19E H 0.4338 1.4869 -0.0690 0.182 Uiso 0.601(6) 1 calc PR A 1
H19F H 0.4809 1.4529 -0.1345 0.182 Uiso 0.601(6) 1 calc PR A 1
C20A C 0.4923(7) 1.2463(4) -0.0848(3) 0.0697(17) Uani 1 1 d . A .
C21A C 0.4219(13) 1.1771(7) -0.0502(5) 0.081(3) Uiso 0.601(6) 1 d P A 1
H21D H 0.3774 1.1398 -0.0827 0.122 Uiso 0.601(6) 1 calc PR A 1
H21E H 0.3433 1.1967 -0.0263 0.122 Uiso 0.601(6) 1 calc PR A 1
H21F H 0.5013 1.1520 -0.0199 0.122 Uiso 0.601(6) 1 calc PR A 1
C22A C 0.3724(15) 1.2743(8) -0.1364(7) 0.103(4) Uiso 0.601(6) 1 d P A 1
H22D H 0.3553 1.2359 -0.1712 0.154 Uiso 0.601(6) 1 calc PR A 1
H22E H 0.4042 1.3231 -0.1538 0.154 Uiso 0.601(6) 1 calc PR A 1
H22F H 0.2786 1.2822 -0.1183 0.154 Uiso 0.601(6) 1 calc PR A 1
C23A C 0.6273(15) 1.2020(8) -0.1125(6) 0.103(4) Uiso 0.601(6) 1 d P A 1
H23D H 0.7003 1.1831 -0.0762 0.154 Uiso 0.601(6) 1 calc PR A 1
H23E H 0.6778 1.2376 -0.1388 0.154 Uiso 0.601(6) 1 calc PR A 1
H23F H 0.5859 1.1584 -0.1392 0.154 Uiso 0.601(6) 1 calc PR A 1
C24A C 0.8550(7) 1.5702(4) 0.2001(4) 0.088(2) Uani 1 1 d . . .
H24D H 0.7894 1.5466 0.2283 0.132 Uiso 1 1 calc R A .
H24E H 0.7928 1.5968 0.1642 0.132 Uiso 1 1 calc R . .
H24F H 0.9226 1.6075 0.2251 0.132 Uiso 1 1 calc R . .
C25A C 1.0369(7) 1.5454(4) 0.1298(3) 0.087(2) Uani 1 1 d . . .
H25D H 1.1143 1.5784 0.1542 0.131 Uiso 1 1 calc R A .
H25E H 0.9721 1.5765 0.0978 0.131 Uiso 1 1 calc R . .
H25F H 1.0860 1.5049 0.1077 0.131 Uiso 1 1 calc R . .
C26A C 1.0483(6) 1.4753(3) 0.2276(3) 0.0628(15) Uani 1 1 d . . .
H26C H 1.0978 1.5171 0.2554 0.075 Uiso 1 1 calc R A .
H26D H 1.1283 1.4472 0.2092 0.075 Uiso 1 1 calc R . .
C27A C 0.9758(6) 1.4211(3) 0.2692(3) 0.0612(15) Uani 1 1 d . A .
H27C H 1.0547 1.4011 0.3035 0.073 Uiso 1 1 calc R . .
H27D H 0.9022 1.4503 0.2907 0.073 Uiso 1 1 calc R . .
C28A C 0.8077(5) 1.3189(4) 0.2800(2) 0.0727(19) Uani 1 1 d . . .
H28D H 0.8745 1.3002 0.3183 0.109 Uiso 1 1 calc R A .
H28E H 0.7523 1.2754 0.2579 0.109 Uiso 1 1 calc R . .
H28F H 0.7358 1.3561 0.2932 0.109 Uiso 1 1 calc R . .
C29A C 1.0058(5) 1.3006(3) 0.2172(2) 0.0514(13) Uani 1 1 d . . .
H29D H 1.0619 1.3235 0.1851 0.077 Uiso 1 1 calc R A .
H29E H 0.9510 1.2550 0.1986 0.077 Uiso 1 1 calc R . .
H29F H 1.0766 1.2855 0.2556 0.077 Uiso 1 1 calc R . .
C21B C 0.2567(17) 1.2557(8) 0.5869(7) 0.058(4) Uiso 0.399(6) 1 d P A 2
H21J H 0.1506 1.2714 0.5834 0.087 Uiso 0.399(6) 1 calc PR A 2
H21K H 0.2959 1.2693 0.5470 0.087 Uiso 0.399(6) 1 calc PR A 2
H21L H 0.3160 1.2821 0.6237 0.087 Uiso 0.399(6) 1 calc PR A 2
C23B C 0.4457(14) 1.1475(8) 0.6065(7) 0.053(4) Uiso 0.399(6) 1 d P A 2
H23J H 0.4990 1.1774 0.6427 0.080 Uiso 0.399(6) 1 calc PR A 2
H23K H 0.4865 1.1603 0.5667 0.080 Uiso 0.399(6) 1 calc PR A 2
H23L H 0.4595 1.0924 0.6157 0.080 Uiso 0.399(6) 1 calc PR A 2
C22B C 0.2122(17) 1.1480(10) 0.6596(7) 0.071(5) Uiso 0.399(6) 1 d P A 2
H22J H 0.2133 1.0919 0.6651 0.107 Uiso 0.399(6) 1 calc PR A 2
H22K H 0.1087 1.1672 0.6582 0.107 Uiso 0.399(6) 1 calc PR A 2
H22L H 0.2778 1.1719 0.6960 0.107 Uiso 0.399(6) 1 calc PR A 2
C17C C 0.8096(17) 1.4698(9) 0.0060(7) 0.065(4) Uiso 0.399(6) 1 d P A 2
H17G H 0.8971 1.4446 0.0312 0.097 Uiso 0.399(6) 1 calc PR A 2
H17H H 0.7320 1.4790 0.0337 0.097 Uiso 0.399(6) 1 calc PR A 2
H17I H 0.8410 1.5191 -0.0107 0.097 Uiso 0.399(6) 1 calc PR A 2
C18C C 0.650(2) 1.4690(10) -0.1016(9) 0.089(6) Uiso 0.399(6) 1 d P A 2
H18G H 0.7159 1.5062 -0.1189 0.133 Uiso 0.399(6) 1 calc PR A 2
H18H H 0.5737 1.4966 -0.0812 0.133 Uiso 0.399(6) 1 calc PR A 2
H18I H 0.5994 1.4368 -0.1369 0.133 Uiso 0.399(6) 1 calc PR A 2
C19C C 0.8659(17) 1.3867(10) -0.0843(7) 0.070(5) Uiso 0.399(6) 1 d P A 2
H19G H 0.8212 1.3565 -0.1220 0.105 Uiso 0.399(6) 1 calc PR A 2
H19H H 0.9321 1.3535 -0.0544 0.105 Uiso 0.399(6) 1 calc PR A 2
H19I H 0.9250 1.4293 -0.0985 0.105 Uiso 0.399(6) 1 calc PR A 2
C16C C 0.7447(18) 1.4178(9) -0.0510(8) 0.063(4) Uiso 0.399(6) 1 d P A 2
C13D C 0.982(3) 1.1347(15) 0.0513(11) 0.080(9) Uiso 0.399(6) 1 d P A 2
H13D H 1.0649 1.1053 0.0413 0.096 Uiso 0.399(6) 1 calc PR A 2
C12D C 0.987(2) 1.2119(13) 0.0421(10) 0.052(6) Uiso 0.399(6) 1 d P A 2
H12D H 1.0696 1.2374 0.0273 0.062 Uiso 0.399(6) 1 calc PR A 2
C15D C 0.7448(17) 1.1339(9) 0.0884(7) 0.056(4) Uiso 0.399(6) 1 d P A 2
H15D H 0.6670 1.1064 0.1050 0.067 Uiso 0.399(6) 1 calc PR A 2
C14D C 0.867(2) 1.0955(14) 0.0738(10) 0.093(9) Uiso 0.399(6) 1 d P A 2
H14D H 0.8738 1.0412 0.0791 0.111 Uiso 0.399(6) 1 calc PR A 2
C11D C 0.858(3) 1.2506(11) 0.0565(11) 0.045(7) Uiso 0.399(6) 1 d P A 2
H11D H 0.8549 1.3049 0.0508 0.054 Uiso 0.399(6) 1 calc PR A 2
C21E C 0.333(2) 1.2260(12) -0.0569(9) 0.103(6) Uiso 0.399(6) 1 d P A 2
H21G H 0.2983 1.1744 -0.0714 0.154 Uiso 0.399(6) 1 calc PR A 2
H21H H 0.2555 1.2640 -0.0733 0.154 Uiso 0.399(6) 1 calc PR A 2
H21I H 0.3503 1.2276 -0.0094 0.154 Uiso 0.399(6) 1 calc PR A 2
C23E C 0.562(2) 1.1807(13) -0.0839(11) 0.116(7) Uiso 0.399(6) 1 d P A 2
H23G H 0.5141 1.1487 -0.1200 0.174 Uiso 0.399(6) 1 calc PR A 2
H23H H 0.5559 1.1544 -0.0428 0.174 Uiso 0.399(6) 1 calc PR A 2
H23I H 0.6681 1.1894 -0.0883 0.174 Uiso 0.399(6) 1 calc PR A 2
C22E C 0.443(2) 1.2777(10) -0.1529(8) 0.071(5) Uiso 0.399(6) 1 d P A 2
H22G H 0.5332 1.2912 -0.1724 0.107 Uiso 0.399(6) 1 calc PR A 2
H22H H 0.3809 1.3237 -0.1507 0.107 Uiso 0.399(6) 1 calc PR A 2
H22I H 0.3850 1.2384 -0.1794 0.107 Uiso 0.399(6) 1 calc PR A 2
C1D C 0.376(2) 1.4283(10) 0.0327(10) 0.063(6) Uiso 0.399(6) 1 d P A 2
H1D1 H 0.3519 1.4094 -0.0119 0.094 Uiso 0.399(6) 1 calc PR A 2
H1D2 H 0.4658 1.4616 0.0361 0.094 Uiso 0.399(6) 1 calc PR A 2
H1D3 H 0.2907 1.4577 0.0442 0.094 Uiso 0.399(6) 1 calc PR A 2
C10D C 0.732(3) 1.2152(16) 0.0791(14) 0.025(7) Uiso 0.399(6) 1 d P A 2
C9D C 0.622(3) 1.2517(16) 0.0955(12) 0.026(6) Uiso 0.399(6) 1 d P A 2
H9D1 H 0.6442 1.2566 0.1432 0.032 Uiso 0.399(6) 1 calc PR A 2
H9D2 H 0.5341 1.2167 0.0865 0.032 Uiso 0.399(6) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0268(2) 0.0282(3) 0.0331(3) -0.0016(3) 0.00249(18) 0.0004(2)
Na1 0.0315(9) 0.0348(10) 0.0430(11) -0.0039(8) 0.0029(8) -0.0014(7)
N1 0.0227(17) 0.026(2) 0.033(2) 0.0026(15) 0.0026(14) 0.0028(13)
N2 0.034(2) 0.050(3) 0.041(2) -0.002(2) 0.0027(17) -0.0036(18)
N3 0.038(2) 0.042(2) 0.035(2) 0.0046(18) 0.0067(17) 0.0063(17)
C1 0.043(3) 0.033(3) 0.036(3) 0.005(2) 0.007(2) 0.005(2)
C2 0.035(2) 0.023(2) 0.036(3) 0.003(2) 0.0030(19) -0.0024(18)
C3 0.050(3) 0.024(2) 0.047(3) 0.003(2) 0.014(2) 0.000(2)
C4 0.081(3) 0.033(3) 0.036(3) 0.010(2) 0.015(3) -0.006(2)
C5 0.131(5) 0.037(3) 0.047(3) -0.005(3) 0.021(3) -0.014(4)
C6 0.125(5) 0.047(4) 0.080(5) 0.007(4) 0.071(4) -0.004(4)
C7 0.094(5) 0.057(4) 0.100(5) 0.006(4) 0.056(4) -0.001(3)
C8 0.061(3) 0.036(3) 0.080(4) 0.007(3) 0.033(3) -0.001(2)
C9 0.025(2) 0.026(2) 0.039(3) -0.003(2) 0.0031(18) 0.0017(18)
C10 0.036(2) 0.023(2) 0.031(2) -0.0035(19) -0.0012(19) 0.0035(19)
C11 0.035(2) 0.024(2) 0.039(3) 0.000(2) 0.002(2) 0.0021(19)
C12 0.047(3) 0.034(3) 0.040(3) 0.000(2) 0.007(2) 0.000(2)
C13 0.065(3) 0.025(2) 0.039(3) 0.004(2) 0.001(2) 0.004(3)
C14 0.050(3) 0.032(3) 0.043(3) -0.003(2) -0.005(2) 0.018(2)
C15 0.029(2) 0.033(3) 0.044(3) -0.006(2) -0.0035(19) 0.0046(19)
C16 0.031(2) 0.040(3) 0.035(3) -0.010(2) 0.0011(19) 0.0012(18)
C17 0.021(2) 0.049(3) 0.045(3) -0.004(2) 0.004(2) -0.001(2)
C18 0.033(3) 0.050(3) 0.087(4) -0.017(3) 0.007(3) 0.006(2)
C19 0.035(3) 0.068(4) 0.047(3) -0.006(3) 0.012(2) -0.014(2)
C20 0.039(3) 0.047(3) 0.033(3) -0.005(2) 0.003(2) -0.006(2)
C21 0.085(8) 0.086(8) 0.047(6) -0.022(5) 0.000(5) -0.062(7)
C22 0.047(5) 0.065(7) 0.046(5) -0.039(5) 0.005(4) -0.002(4)
C23 0.087(6) 0.056(6) 0.042(5) -0.008(5) -0.025(4) 0.027(6)
C24 0.049(3) 0.060(4) 0.049(3) -0.003(3) 0.000(2) -0.013(3)
C25 0.059(4) 0.081(4) 0.063(4) 0.018(3) 0.005(3) -0.012(3)
C26 0.062(4) 0.062(4) 0.054(4) -0.023(3) -0.004(3) -0.003(3)
C27 0.069(4) 0.068(4) 0.041(3) -0.009(3) 0.000(3) 0.025(3)
C28 0.053(3) 0.035(3) 0.051(3) 0.010(2) 0.002(2) 0.000(2)
C29 0.054(3) 0.052(3) 0.079(4) 0.002(3) 0.032(3) 0.001(3)
Zn1A 0.0963(5) 0.0430(4) 0.0309(3) 0.0012(3) 0.0009(3) -0.0080(4)
Na1A 0.0458(10) 0.0480(11) 0.0367(11) -0.0006(9) -0.0019(8) 0.0080(8)
N1A 0.047(2) 0.039(2) 0.032(2) 0.007(2) 0.0065(16) 0.0064(19)
N2A 0.049(3) 0.053(3) 0.056(3) 0.005(2) 0.006(2) 0.005(2)
N3A 0.035(2) 0.057(3) 0.036(2) 0.005(2) 0.0029(17) 0.0095(19)
C1A 0.050(7) 0.069(8) 0.067(7) -0.013(6) -0.027(6) 0.035(6)
C2A 0.052(3) 0.067(4) 0.056(3) -0.010(3) -0.004(3) 0.023(3)
C3A 0.029(2) 0.054(3) 0.054(3) -0.007(3) 0.001(2) 0.018(2)
C4A 0.041(3) 0.053(3) 0.042(3) 0.002(3) 0.012(2) 0.011(2)
C5A 0.041(3) 0.049(3) 0.057(4) -0.001(3) 0.012(2) 0.005(2)
C6A 0.035(3) 0.071(4) 0.048(3) 0.008(3) 0.006(2) 0.009(3)
C7A 0.030(3) 0.059(4) 0.063(4) 0.017(3) 0.012(2) 0.009(2)
C8A 0.025(2) 0.048(3) 0.074(4) 0.005(3) 0.006(2) 0.006(2)
C9A 0.023(7) 0.047(8) 0.038(7) 0.002(4) 0.020(5) 0.011(5)
C10A 0.023(8) 0.044(9) 0.027(6) 0.002(5) -0.006(5) -0.004(6)
C11A 0.038(6) 0.026(6) 0.032(5) -0.006(5) 0.002(3) 0.009(5)
C12A 0.050(6) 0.035(6) 0.048(6) -0.011(5) 0.019(4) 0.006(5)
C13A 0.050(6) 0.043(7) 0.061(7) 0.001(6) 0.021(5) 0.028(6)
C14A 0.042(6) 0.057(7) 0.078(8) 0.038(6) 0.016(6) 0.030(6)
C20A 0.086(4) 0.071(4) 0.045(4) -0.002(3) -0.014(3) -0.011(3)
C24A 0.064(4) 0.071(4) 0.127(6) -0.009(4) 0.006(4) 0.026(3)
C25A 0.086(5) 0.094(5) 0.082(5) 0.022(4) 0.013(4) -0.009(4)
C26A 0.053(3) 0.068(4) 0.061(4) 0.005(3) -0.011(3) -0.002(3)
C27A 0.060(3) 0.064(4) 0.054(4) 0.003(3) -0.011(3) 0.016(3)
C28A 0.048(3) 0.118(6) 0.052(3) 0.032(4) 0.008(3) 0.018(3)
C29A 0.047(3) 0.064(4) 0.041(3) 0.000(3) 0.000(2) 0.012(3)

_geom_special_details            
;
;

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 C16 2.038(4) . ?
Zn1 C20 2.043(4) . ?
Zn1 N1 2.068(3) . ?
Na1 N1 2.374(4) . ?
Na1 N3 2.428(4) . ?
Na1 N2 2.497(4) . ?
N1 C2 1.468(5) . ?
N1 C9 1.474(5) . ?
N2 C25 1.454(6) . ?
N2 C24 1.456(6) . ?
N2 C26 1.487(6) . ?
N3 C28 1.459(5) . ?
N3 C27 1.469(6) . ?
N3 C29 1.481(6) . ?
C1 C2 1.521(5) . ?
C2 C3 1.514(6) . ?
C3 C4 1.386(6) . ?
C3 C8 1.402(6) . ?
C4 C5 1.416(7) . ?
C5 C6 1.397(8) . ?
C6 C7 1.346(8) . ?
C7 C8 1.362(7) . ?
C9 C10 1.497(6) . ?
C10 C15 1.394(5) . ?
C10 C11 1.394(6) . ?
C11 C12 1.382(6) . ?
C12 C13 1.374(6) . ?
C13 C14 1.377(6) . ?
C14 C15 1.378(6) . ?
C16 C18 1.533(6) . ?
C16 C19 1.534(6) . ?
C16 C17 1.541(6) . ?
C20 C21 1.495(9) . ?
C20 C22B 1.502(15) . ?
C20 C23 1.510(9) . ?
C20 C22 1.525(9) . ?
C20 C21B 1.538(14) . ?
C20 C23B 1.605(13) . ?
C26 C27 1.456(7) . ?
Zn1A C16A 1.986(10) . ?
Zn1A C20A 2.012(6) . ?
Zn1A N1A 2.062(3) . ?
Zn1A C16C 2.193(16) . ?
Na1A N1A 2.418(4) . ?
Na1A N3A 2.462(4) . ?
Na1A N2A 2.511(5) . ?
Na1A C4A 2.902(5) . ?
N1A C9A 1.417(17) . ?
N1A C2A 1.475(6) . ?
N1A C9D 1.52(3) . ?
N2A C25A 1.460(7) . ?
N2A C26A 1.466(6) . ?
N2A C24A 1.467(7) . ?
N3A C27A 1.443(6) . ?
N3A C29A 1.453(5) . ?
N3A C28A 1.472(6) . ?
C1A C2A 1.472(10) . ?
C2A C3A 1.529(7) . ?
C3A C4A 1.372(7) . ?
C3A C8A 1.397(7) . ?
C4A C5A 1.380(6) . ?
C5A C6A 1.384(7) . ?
C6A C7A 1.380(7) . ?
C7A C8A 1.392(7) . ?
C9A C10A 1.69(2) . ?
C10A C11A 1.35(2) . ?
C10A C15A 1.367(19) . ?
C11A C12A 1.395(15) . ?
C12A C13A 1.435(15) . ?
C13A C14A 1.404(18) . ?
C14A C15A 1.410(13) . ?
C16A C18A 1.482(16) . ?
C16A C17A 1.532(13) . ?
C16A C19A 1.550(16) . ?
C20A C23E 1.30(2) . ?
C20A C22A 1.484(13) . ?
C20A C22E 1.524(16) . ?
C20A C21A 1.580(12) . ?
C20A C23A 1.608(14) . ?
C20A C21E 1.656(18) . ?
C26A C27A 1.490(7) . ?
C17C C16C 1.54(2) . ?
C18C C16C 1.54(2) . ?
C19C C16C 1.47(2) . ?
C13D C12D 1.35(3) . ?
C13D C14D 1.37(3) . ?
C12D C11D 1.40(3) . ?
C15D C14D 1.36(3) . ?
C15D C10D 1.43(3) . ?
C11D C10D 1.43(3) . ?
C10D C9D 1.26(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 Zn1 C20 127.53(17) . . ?
C16 Zn1 N1 114.73(15) . . ?
C20 Zn1 N1 117.61(15) . . ?
N1 Na1 N3 123.24(13) . . ?
N1 Na1 N2 156.05(14) . . ?
N3 Na1 N2 76.30(13) . . ?
C2 N1 C9 108.7(3) . . ?
C2 N1 Zn1 108.5(2) . . ?
C9 N1 Zn1 111.4(2) . . ?
C2 N1 Na1 115.6(2) . . ?
C9 N1 Na1 98.9(2) . . ?
Zn1 N1 Na1 113.34(14) . . ?
C25 N2 C24 109.5(4) . . ?
C25 N2 C26 111.2(4) . . ?
C24 N2 C26 107.9(4) . . ?
C25 N2 Na1 110.2(3) . . ?
C24 N2 Na1 114.6(3) . . ?
C26 N2 Na1 103.4(3) . . ?
C28 N3 C27 111.0(4) . . ?
C28 N3 C29 108.4(4) . . ?
C27 N3 C29 108.2(4) . . ?
C28 N3 Na1 111.0(3) . . ?
C27 N3 Na1 105.0(3) . . ?
C29 N3 Na1 113.1(3) . . ?
N1 C2 C3 112.3(3) . . ?
N1 C2 C1 110.2(3) . . ?
C3 C2 C1 111.7(4) . . ?
C4 C3 C8 117.8(5) . . ?
C4 C3 C2 121.9(4) . . ?
C8 C3 C2 120.3(4) . . ?
C3 C4 C5 120.0(5) . . ?
C6 C5 C4 118.4(5) . . ?
C7 C6 C5 122.1(5) . . ?
C6 C7 C8 119.0(6) . . ?
C7 C8 C3 122.8(6) . . ?
N1 C9 C10 114.9(3) . . ?
C15 C10 C11 116.7(4) . . ?
C15 C10 C9 119.1(4) . . ?
C11 C10 C9 124.2(4) . . ?
C12 C11 C10 121.3(4) . . ?
C13 C12 C11 120.9(4) . . ?
C12 C13 C14 118.7(4) . . ?
C13 C14 C15 120.7(4) . . ?
C14 C15 C10 121.7(4) . . ?
C18 C16 C19 108.6(4) . . ?
C18 C16 C17 106.6(4) . . ?
C19 C16 C17 107.9(4) . . ?
C18 C16 Zn1 106.9(3) . . ?
C19 C16 Zn1 111.9(3) . . ?
C17 C16 Zn1 114.7(3) . . ?
C21 C20 C23 108.3(7) . . ?
C21 C20 C22 108.8(6) . . ?
C23 C20 C22 106.5(6) . . ?
C22B C20 C21B 109.0(9) . . ?
C22B C20 C23B 107.3(8) . . ?
C21B C20 C23B 106.5(8) . . ?
C21 C20 Zn1 115.0(4) . . ?
C22B C20 Zn1 110.5(7) . . ?
C23 C20 Zn1 108.5(4) . . ?
C22 C20 Zn1 109.5(4) . . ?
C21B C20 Zn1 109.2(6) . . ?
C23B C20 Zn1 114.2(5) . . ?
C27 C26 N2 115.6(4) . . ?
C26 C27 N3 114.8(4) . . ?
C16A Zn1A C20A 126.9(3) . . ?
C16A Zn1A N1A 111.5(3) . . ?
C20A Zn1A N1A 120.3(2) . . ?
C20A Zn1A C16C 125.4(5) . . ?
N1A Zn1A C16C 112.6(4) . . ?
N1A Na1A N3A 120.17(15) . . ?
N1A Na1A N2A 162.97(15) . . ?
N3A Na1A N2A 74.61(14) . . ?
C9A N1A C2A 104.5(7) . . ?
C2A N1A C9D 115.6(9) . . ?
C9A N1A Zn1A 115.3(7) . . ?
C2A N1A Zn1A 112.5(3) . . ?
C9D N1A Zn1A 106.3(9) . . ?
C9A N1A Na1A 100.4(7) . . ?
C2A N1A Na1A 108.3(3) . . ?
C9D N1A Na1A 98.8(10) . . ?
Zn1A N1A Na1A 114.67(16) . . ?
C25A N2A C26A 107.8(4) . . ?
C25A N2A C24A 109.1(5) . . ?
C26A N2A C24A 109.4(5) . . ?
C25A N2A Na1A 121.8(4) . . ?
C26A N2A Na1A 106.3(3) . . ?
C24A N2A Na1A 101.9(3) . . ?
C27A N3A C29A 111.2(4) . . ?
C27A N3A C28A 107.9(4) . . ?
C29A N3A C28A 108.6(4) . . ?
C27A N3A Na1A 105.8(3) . . ?
C29A N3A Na1A 109.3(3) . . ?
C28A N3A Na1A 114.0(3) . . ?
C1A C2A N1A 117.9(6) . . ?
C1A C2A C3A 113.5(6) . . ?
N1A C2A C3A 110.3(4) . . ?
N1A C2A C1D 99.8(8) . . ?
C3A C2A C1D 107.3(8) . . ?
C4A C3A C8A 116.8(5) . . ?
C4A C3A C2A 123.2(5) . . ?
C8A C3A C2A 120.0(5) . . ?
C3A C4A C5A 123.1(5) . . ?
C4A C5A C6A 119.3(5) . . ?
C7A C6A C5A 119.5(5) . . ?
C6A C7A C8A 120.0(5) . . ?
C7A C8A C3A 121.3(5) . . ?
N1A C9A C10A 105.4(11) . . ?
C11A C10A C15A 122.1(14) . . ?
C11A C10A C9A 121.5(13) . . ?
C15A C10A C9A 116.4(13) . . ?
C10A C11A C12A 120.1(13) . . ?
C11A C12A C13A 117.8(10) . . ?
C14A C13A C12A 122.3(8) . . ?
C13A C14A C15A 115.5(9) . . ?
C10A C15A C14A 122.2(11) . . ?
C18A C16A C17A 109.0(9) . . ?
C18A C16A C19A 108.1(10) . . ?
C17A C16A C19A 102.6(9) . . ?
C18A C16A Zn1A 109.4(8) . . ?
C17A C16A Zn1A 114.8(7) . . ?
C19A C16A Zn1A 112.5(8) . . ?
C23E C20A C22E 113.4(13) . . ?
C22A C20A C21A 106.7(8) . . ?
C22A C20A C23A 113.3(8) . . ?
C21A C20A C23A 99.9(8) . . ?
C23E C20A C21E 104.2(13) . . ?
C22E C20A C21E 105.2(10) . . ?
C23E C20A Zn1A 119.9(11) . . ?
C22A C20A Zn1A 111.8(7) . . ?
C22E C20A Zn1A 109.2(7) . . ?
C21A C20A Zn1A 115.9(5) . . ?
C23A C20A Zn1A 108.8(6) . . ?
C21E C20A Zn1A 103.2(7) . . ?
N2A C26A C27A 115.1(4) . . ?
N3A C27A C26A 115.2(4) . . ?
C19C C16C C18C 105.0(14) . . ?
C19C C16C C17C 111.1(13) . . ?
C18C C16C C17C 107.4(13) . . ?
C19C C16C Zn1A 115.1(10) . . ?
C18C C16C Zn1A 103.3(11) . . ?
C17C C16C Zn1A 113.9(11) . . ?
C12D C13D C14D 126(2) . . ?
C13D C12D C11D 113.3(19) . . ?
C14D C15D C10D 120.5(18) . . ?
C15D C14D C13D 120(2) . . ?
C12D C11D C10D 126(2) . . ?
C9D C10D C11D 124(2) . . ?
C9D C10D C15D 121(2) . . ?
C11D C10D C15D 115(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.055

#===END