Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2004

data_global

_publ_contact_author_email       V.GIBSON@IMPERIAL.AC.UK

_publ_contact_author_name        'Prof Vernon C Gibson'
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_publ_contact_author_address     
;
Department of Chemistry
Imperial College London
Exhibition Road
London
SW7 2AZ
UNITED KINGDOM
;

_publ_section_title              
;
Magnesium and Zinc complexes of a potentially
tridentate b-diketiminate ligand
;

loop_
_publ_author_name
'Vernon C. Gibson'
'Andrew P. Dove'
'Edward L. Marshall'
'Andrew J.P. White'
'David J. Williams'

data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 224371'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C48 H62 N4 O2 Mg'
_chemical_formula_weight         751.33
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.1719(8)
_cell_length_b                   18.795(2)
_cell_length_c                   20.625(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4330.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    27
_cell_measurement_theta_min      4.50
_cell_measurement_theta_max      23.11

_exptl_crystal_description       plates
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3554
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         59.96
_reflns_number_total             3522
_reflns_number_observed          2564
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 288 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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.
;

#Results of chirality/polarity tests
_refine_ls_R_factor_obs+         0.0641
_refine_ls_wR_factor_obs+        0.1301
_refine_ls_abs_structure_Flack+  0.48(17)
_refine_ls_R_factor_obs-         0.0642
_refine_ls_wR_factor_obs-        0.1300
_refine_ls_abs_structure_Flack-  0.52(17)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+2.4988P] 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    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(17)
_refine_ls_number_reflns         3234
_refine_ls_number_parameters     505
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_obs          0.0640
_refine_ls_wR_factor_all         0.1614
_refine_ls_wR_factor_obs         0.1300
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_restrained_S_all      1.180
_refine_ls_restrained_S_obs      1.148
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mg Mg 0.6189(2) 0.02173(11) 0.43136(11) 0.0237(5) Uani 1 d . .
C1 C 0.3930(6) 0.1024(3) 0.4373(3) 0.0262(15) Uani 1 d . .
N1 N 0.4313(5) 0.0368(3) 0.4457(3) 0.0241(13) Uani 1 d . .
C2 C 0.4681(6) 0.1617(3) 0.4343(3) 0.0273(15) Uani 1 d . .
H2A H 0.4394(6) 0.2016(3) 0.4106(3) 0.033 Uiso 1 calc R .
C3 C 0.5815(6) 0.1685(3) 0.4628(3) 0.026(2) Uani 1 d . .
N3 N 0.6412(5) 0.1123(3) 0.4858(3) 0.0274(13) Uani 1 d . .
C4 C 0.2590(6) 0.1168(4) 0.4332(4) 0.034(2) Uani 1 d . .
H4A H 0.2248(6) 0.1180(4) 0.4769(4) 0.052 Uiso 1 d R .
H4B H 0.2456(6) 0.1627(4) 0.4118(4) 0.052 Uiso 1 d R .
H4C H 0.2205(6) 0.0790(4) 0.4080(4) 0.052 Uiso 1 d R .
C5 C 0.6325(7) 0.2428(3) 0.4646(4) 0.037(2) Uani 1 d . .
H5A H 0.6348(7) 0.2623(3) 0.4206(4) 0.055 Uiso 1 d R .
H5B H 0.5821(7) 0.2730(3) 0.4921(4) 0.055 Uiso 1 d R .
H5C H 0.7139(7) 0.2413(3) 0.4824(4) 0.055 Uiso 1 d R .
C6 C 0.3469(6) -0.0160(4) 0.4672(3) 0.0270(15) Uani 1 d . .
C7 C 0.2823(6) -0.0586(3) 0.4236(4) 0.030(2) Uani 1 d . .
C8 C 0.2077(7) -0.1107(4) 0.4483(4) 0.042(2) Uani 1 d . .
H8A H 0.1641(7) -0.1402(4) 0.4192(4) 0.050 Uiso 1 calc R .
C9 C 0.1951(7) -0.1209(4) 0.5143(4) 0.042(2) Uani 1 d . .
H9A H 0.1462(7) -0.1584(4) 0.5303(4) 0.050 Uiso 1 calc R .
C10 C 0.2536(7) -0.0766(5) 0.5564(4) 0.044(2) Uani 1 d . .
H10A H 0.2419(7) -0.0827(5) 0.6016(4) 0.053 Uiso 1 calc R .
C11 C 0.3292(6) -0.0234(4) 0.5350(3) 0.035(2) Uani 1 d D .
C12 C 0.2941(7) -0.0474(4) 0.3508(3) 0.030(2) Uani 1 d . .
H12A H 0.3097(7) 0.0045(4) 0.3440(3) 0.036 Uiso 1 calc R .
C13 C 0.4016(7) -0.0874(4) 0.3224(4) 0.037(2) Uani 1 d . .
H13A H 0.4059(7) -0.0788(4) 0.2756(4) 0.056 Uiso 1 calc R .
H13B H 0.3922(7) -0.1385(4) 0.3304(4) 0.056 Uiso 1 calc R .
H13C H 0.4753(7) -0.0706(4) 0.3431(4) 0.056 Uiso 1 calc R .
C14 C 0.1789(8) -0.0654(5) 0.3133(4) 0.055(2) Uani 1 d . .
H14A H 0.1918(8) -0.0571(5) 0.2669(4) 0.083 Uiso 1 calc R .
H14B H 0.1135(8) -0.0350(5) 0.3287(4) 0.083 Uiso 1 calc R .
H14C H 0.1581(8) -0.1154(5) 0.3205(4) 0.083 Uiso 1 calc R .
C15 C 0.3876(8) 0.0259(6) 0.5832(4) 0.063(3) Uani 1 d D .
H15A H 0.4583(8) 0.0512(6) 0.5645(4) 0.075 Uiso 0.60 calc PR 1
H15B H 0.4528(8) 0.0405(6) 0.5560(4) 0.075 Uiso 0.40 d PR 2
C16 C 0.2902(17) 0.0789(7) 0.6103(6) 0.058(5) Uani 0.60 d PDU 1
H16A H 0.3273(17) 0.1112(7) 0.6417(6) 0.086 Uiso 0.60 calc PR 1
H16B H 0.2262(17) 0.0519(7) 0.6316(6) 0.086 Uiso 0.60 calc PR 1
H16C H 0.2565(17) 0.1067(7) 0.5744(6) 0.086 Uiso 0.60 calc PR 1
C17 C 0.4210(14) -0.0190(10) 0.6464(6) 0.051(4) Uani 0.60 d PDU 1
H17A H 0.4591(14) 0.0123(10) 0.6784(6) 0.076 Uiso 0.60 calc PR 1
H17B H 0.4764(14) -0.0573(10) 0.6347(6) 0.076 Uiso 0.60 calc PR 1
H17C H 0.3481(14) -0.0394(10) 0.6651(6) 0.076 Uiso 0.60 calc PR 1
C16' C 0.3406(28) 0.0969(11) 0.5951(15) 0.084(12) Uiso 0.40 d PD 2
H16D H 0.2895(28) 0.1112(11) 0.5587(15) 0.126 Uiso 0.40 calc PR 2
H16E H 0.4072(28) 0.1305(11) 0.5993(15) 0.126 Uiso 0.40 calc PR 2
H16F H 0.2936(28) 0.0968(11) 0.6352(15) 0.126 Uiso 0.40 calc PR 2
C17' C 0.4647(27) 0.0015(16) 0.6359(13) 0.089(14) Uiso 0.40 d PD 2
H17D H 0.4943(27) -0.0463(16) 0.6260(13) 0.134 Uiso 0.40 calc PR 2
H17E H 0.4189(27) 0.0004(16) 0.6764(13) 0.134 Uiso 0.40 calc PR 2
H17F H 0.5325(27) 0.0342(16) 0.6405(13) 0.134 Uiso 0.40 calc PR 2
C18 C 0.7291(6) 0.1188(3) 0.5344(4) 0.030(2) Uani 1 d . .
C19 C 0.8274(6) 0.0730(4) 0.5301(3) 0.030(2) Uani 1 d . .
C20 C 0.9180(7) 0.0737(4) 0.5765(4) 0.045(2) Uani 1 d . .
H20A H 0.9837(7) 0.0418(4) 0.5734(4) 0.054 Uiso 1 calc R .
C21 C 0.9104(9) 0.1220(5) 0.6274(4) 0.052(3) Uani 1 d . .
H21A H 0.9729(9) 0.1243(5) 0.6586(4) 0.063 Uiso 1 calc R .
C22 C 0.8132(9) 0.1662(5) 0.6330(4) 0.051(2) Uani 1 d . .
H22A H 0.8079(9) 0.1979(5) 0.6688(4) 0.061 Uiso 1 calc R .
C23 C 0.7217(8) 0.1652(4) 0.5864(4) 0.039(2) Uani 1 d . .
H23A H 0.6550(8) 0.1963(4) 0.5905(4) 0.047 Uiso 1 calc R .
O24 O 0.8241(4) 0.0267(3) 0.4779(2) 0.0360(12) Uani 1 d . .
C25 C 0.9235(7) -0.0198(5) 0.4672(4) 0.051(2) Uani 1 d . .
H25A H 0.9269(7) -0.0553(5) 0.5019(4) 0.076 Uiso 1 d R .
H25B H 0.9139(7) -0.0439(5) 0.4253(4) 0.076 Uiso 1 d R .
H25C H 0.9978(7) 0.0079(5) 0.4669(4) 0.076 Uiso 1 d R .
C31 C 0.7276(6) -0.0145(4) 0.3031(3) 0.030(2) Uani 1 d . .
N31 N 0.6793(5) 0.0392(3) 0.3363(3) 0.0244(12) Uani 1 d . .
C32 C 0.7345(6) -0.0853(4) 0.3248(3) 0.028(2) Uani 1 d . .
H32A H 0.7689(6) -0.1165(4) 0.2937(3) 0.034 Uiso 1 calc R .
C33 C 0.7015(6) -0.1199(4) 0.3823(4) 0.032(2) Uani 1 d . .
N33 N 0.6494(5) -0.0868(3) 0.4322(3) 0.0271(13) Uani 1 d . .
C34 C 0.7852(7) -0.0017(4) 0.2379(3) 0.039(2) Uani 1 d . .
H34A H 0.8718(7) -0.0091(4) 0.2414(3) 0.058 Uiso 1 d R .
H34B H 0.7518(7) -0.0349(4) 0.2061(3) 0.058 Uiso 1 d R .
H34C H 0.7694(7) 0.0473(4) 0.2240(3) 0.058 Uiso 1 d R .
C35 C 0.7318(8) -0.1982(4) 0.3850(4) 0.044(2) Uani 1 d . .
H35A H 0.6654(8) -0.2259(4) 0.3669(4) 0.065 Uiso 1 d R .
H35B H 0.8046(8) -0.2073(4) 0.3598(4) 0.065 Uiso 1 d R .
H35C H 0.7449(8) -0.2124(4) 0.4302(4) 0.065 Uiso 1 d R .
C36 C 0.6844(6) 0.1103(4) 0.3094(3) 0.027(2) Uani 1 d . .
C37 C 0.5823(7) 0.1398(4) 0.2798(3) 0.030(2) Uani 1 d . .
C38 C 0.5868(7) 0.2104(4) 0.2603(4) 0.040(2) Uani 1 d . .
H38A H 0.5185(7) 0.2307(4) 0.2401(4) 0.048 Uiso 1 calc R .
C39 C 0.6870(8) 0.2524(4) 0.2692(4) 0.050(2) Uani 1 d . .
H39A H 0.6868(8) 0.3012(4) 0.2573(4) 0.060 Uiso 1 calc R .
C40 C 0.7874(8) 0.2212(4) 0.2960(4) 0.042(2) Uani 1 d . .
H40A H 0.8580(8) 0.2490(4) 0.3006(4) 0.051 Uiso 1 calc R .
C41 C 0.7892(6) 0.1514(4) 0.3165(3) 0.031(2) Uani 1 d . .
C42 C 0.4727(7) 0.0949(4) 0.2658(4) 0.034(2) Uani 1 d . .
H42A H 0.4654(7) 0.0590(4) 0.3014(4) 0.041 Uiso 1 calc R .
C43 C 0.3567(7) 0.1375(5) 0.2642(4) 0.047(2) Uani 1 d . .
H43A H 0.2895(7) 0.1056(5) 0.2550(4) 0.070 Uiso 1 calc R .
H43B H 0.3618(7) 0.1739(5) 0.2303(4) 0.070 Uiso 1 calc R .
H43C H 0.3442(7) 0.1605(5) 0.3064(4) 0.070 Uiso 1 calc R .
C44 C 0.4871(9) 0.0542(5) 0.2021(5) 0.060(3) Uani 1 d . .
H44A H 0.4153(9) 0.0256(5) 0.1941(5) 0.090 Uiso 1 calc R .
H44B H 0.5570(9) 0.0228(5) 0.2050(5) 0.090 Uiso 1 calc R .
H44C H 0.4983(9) 0.0880(5) 0.1665(5) 0.090 Uiso 1 calc R .
C45 C 0.9054(6) 0.1242(4) 0.3447(4) 0.032(2) Uani 1 d . .
H45A H 0.8923(6) 0.0736(4) 0.3580(4) 0.038 Uiso 1 calc R .
C46 C 1.0070(7) 0.1250(6) 0.2961(4) 0.055(2) Uani 1 d . .
H46A H 1.0801(7) 0.1070(6) 0.3166(4) 0.083 Uiso 1 calc R .
H46B H 1.0204(7) 0.1738(6) 0.2810(4) 0.083 Uiso 1 calc R .
H46C H 0.9863(7) 0.0947(6) 0.2590(4) 0.083 Uiso 1 calc R .
C47 C 0.9415(7) 0.1654(5) 0.4049(4) 0.044(2) Uani 1 d . .
H47A H 1.0170(7) 0.1464(5) 0.4218(4) 0.066 Uiso 1 calc R .
H47B H 0.8789(7) 0.1608(5) 0.4379(4) 0.066 Uiso 1 calc R .
H47C H 0.9519(7) 0.2158(5) 0.3938(4) 0.066 Uiso 1 calc R .
C48 C 0.6232(7) -0.1270(3) 0.4897(4) 0.031(2) Uani 1 d . .
C49 C 0.5401(7) -0.1828(4) 0.4912(4) 0.035(2) Uani 1 d . .
C50 C 0.5145(7) -0.2198(4) 0.5480(4) 0.041(2) Uani 1 d . .
H50A H 0.4570(7) -0.2570(4) 0.5483(4) 0.050 Uiso 1 calc R .
C51 C 0.5750(8) -0.2009(4) 0.6043(4) 0.043(2) Uani 1 d . .
H51A H 0.5600(8) -0.2261(4) 0.6433(4) 0.052 Uiso 1 calc R .
C52 C 0.6550(8) -0.1469(4) 0.6039(4) 0.045(2) Uani 1 d . .
H52A H 0.6959(8) -0.1348(4) 0.6427(4) 0.054 Uiso 1 calc R .
C53 C 0.6779(7) -0.1092(4) 0.5478(3) 0.035(2) Uani 1 d . .
H53A H 0.7322(7) -0.0703(4) 0.5491(3) 0.042 Uiso 1 calc R .
O54 O 0.4860(5) -0.1985(3) 0.4328(3) 0.0428(13) Uani 1 d . .
C55 C 0.3997(8) -0.2548(4) 0.4316(5) 0.052(2) Uani 1 d . .
H55A H 0.3696(8) -0.2609(4) 0.3873(5) 0.078 Uiso 1 d R .
H55B H 0.4374(8) -0.2991(4) 0.4462(5) 0.078 Uiso 1 d R .
H55C H 0.3330(8) -0.2429(4) 0.4605(5) 0.078 Uiso 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
Mg 0.0232(11) 0.0199(10) 0.0281(11) -0.0012(10) 0.0025(10) 0.0007(10)
C1 0.022(3) 0.029(3) 0.027(3) -0.007(3) 0.002(3) 0.002(3)
N1 0.019(3) 0.022(3) 0.031(3) -0.004(2) 0.004(2) -0.002(2)
C2 0.034(4) 0.025(3) 0.023(3) 0.001(3) -0.002(3) 0.004(3)
C3 0.028(4) 0.024(3) 0.026(3) -0.007(3) 0.001(3) -0.004(3)
N3 0.025(3) 0.020(3) 0.037(3) 0.002(3) -0.004(3) -0.005(2)
C4 0.026(4) 0.040(4) 0.038(4) -0.003(4) -0.003(3) 0.011(3)
C5 0.048(5) 0.024(3) 0.039(4) 0.004(3) -0.004(4) 0.001(4)
C6 0.021(3) 0.023(3) 0.036(4) -0.001(3) -0.001(3) -0.001(3)
C7 0.031(4) 0.026(3) 0.034(4) -0.001(3) 0.000(3) 0.002(3)
C8 0.037(4) 0.031(4) 0.057(5) -0.002(4) 0.005(4) -0.005(4)
C9 0.036(4) 0.035(4) 0.055(5) 0.008(4) 0.009(4) -0.004(4)
C10 0.039(5) 0.052(5) 0.042(5) 0.007(4) 0.012(4) 0.003(4)
C11 0.027(4) 0.046(4) 0.031(4) 0.003(4) 0.002(3) 0.001(4)
C12 0.035(4) 0.027(3) 0.028(4) -0.004(3) -0.004(3) -0.008(3)
C13 0.037(4) 0.041(4) 0.033(4) -0.004(3) -0.003(3) -0.002(4)
C14 0.038(5) 0.074(6) 0.054(5) 0.002(5) -0.023(4) -0.007(5)
C15 0.040(5) 0.114(8) 0.034(5) -0.006(5) 0.002(4) -0.028(6)
C16 0.116(13) 0.025(6) 0.031(7) 0.005(6) -0.038(9) -0.003(9)
C17 0.036(8) 0.083(10) 0.034(7) -0.014(8) -0.002(6) 0.029(9)
C18 0.031(4) 0.022(3) 0.039(4) -0.001(3) -0.008(3) -0.003(3)
C19 0.024(4) 0.027(4) 0.038(4) 0.001(3) -0.004(3) -0.007(3)
C20 0.038(4) 0.046(4) 0.052(5) 0.013(4) -0.013(4) -0.005(4)
C21 0.065(6) 0.044(5) 0.048(5) 0.010(4) -0.031(5) -0.025(5)
C22 0.072(6) 0.042(5) 0.038(5) -0.005(4) -0.012(5) -0.021(5)
C23 0.051(5) 0.030(4) 0.036(4) 0.000(3) -0.007(4) -0.005(4)
O24 0.030(3) 0.030(3) 0.048(3) -0.006(2) -0.005(2) 0.004(2)
C25 0.038(4) 0.047(5) 0.067(6) 0.007(5) 0.008(4) 0.013(4)
C31 0.018(3) 0.038(4) 0.033(4) -0.002(3) 0.004(3) -0.003(3)
N31 0.021(3) 0.023(3) 0.030(3) 0.003(2) -0.004(2) -0.001(2)
C32 0.030(4) 0.030(4) 0.025(4) 0.000(3) 0.004(3) 0.006(3)
C33 0.027(4) 0.025(4) 0.043(4) -0.008(3) -0.006(3) 0.008(3)
N33 0.025(3) 0.024(3) 0.032(3) -0.001(3) 0.000(3) 0.004(2)
C34 0.043(5) 0.040(4) 0.033(4) -0.005(3) 0.009(4) 0.002(4)
C35 0.050(5) 0.031(4) 0.050(5) -0.004(4) 0.002(4) 0.014(4)
C36 0.028(4) 0.031(4) 0.022(3) -0.002(3) -0.002(3) -0.002(3)
C37 0.029(4) 0.037(4) 0.024(4) 0.005(3) 0.001(3) 0.004(3)
C38 0.041(5) 0.034(4) 0.046(5) 0.016(4) -0.007(4) 0.001(4)
C39 0.061(6) 0.031(4) 0.058(5) 0.013(4) -0.011(5) -0.008(4)
C40 0.041(5) 0.036(4) 0.051(5) 0.011(4) -0.002(4) -0.011(4)
C41 0.025(4) 0.034(4) 0.034(4) -0.003(3) -0.005(3) -0.006(3)
C42 0.027(4) 0.036(4) 0.040(4) 0.005(3) -0.004(3) 0.001(3)
C43 0.031(4) 0.055(5) 0.054(5) 0.014(4) -0.010(4) 0.001(4)
C44 0.053(6) 0.065(6) 0.062(6) -0.026(5) -0.004(5) 0.001(5)
C45 0.019(4) 0.036(4) 0.040(4) -0.001(3) 0.001(3) -0.004(3)
C46 0.037(5) 0.075(7) 0.054(6) 0.001(5) 0.012(4) -0.002(5)
C47 0.030(4) 0.050(5) 0.053(5) 0.005(4) 0.003(4) -0.006(4)
C48 0.033(4) 0.020(3) 0.040(4) 0.001(3) 0.008(4) 0.006(3)
C49 0.033(4) 0.031(4) 0.041(4) 0.006(3) -0.007(4) -0.002(3)
C50 0.039(4) 0.035(4) 0.051(5) 0.012(4) 0.007(4) 0.002(4)
C51 0.055(5) 0.031(4) 0.044(5) 0.002(4) 0.015(4) 0.008(4)
C52 0.051(5) 0.045(5) 0.039(5) -0.005(4) -0.003(4) 0.007(4)
C53 0.048(5) 0.028(4) 0.030(4) -0.002(3) -0.005(4) 0.004(4)
O54 0.040(3) 0.037(3) 0.051(3) 0.008(3) -0.001(3) -0.010(2)
C55 0.054(6) 0.040(4) 0.062(5) 0.016(5) -0.002(5) -0.018(4)

_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
Mg N3 2.054(6) . ?
Mg N33 2.068(6) . ?
Mg N31 2.099(6) . ?
Mg N1 2.135(6) . ?
Mg O24 2.486(5) . ?
C1 N1 1.316(8) . ?
C1 C2 1.397(10) . ?
C1 C4 1.523(9) . ?
N1 C6 1.440(8) . ?
C2 C3 1.403(9) . ?
C3 N3 1.335(9) . ?
C3 C5 1.509(9) . ?
N3 C18 1.410(9) . ?
C6 C7 1.404(10) . ?
C6 C11 1.419(9) . ?
C7 C8 1.383(10) . ?
C7 C12 1.521(9) . ?
C8 C9 1.382(11) . ?
C9 C10 1.369(11) . ?
C10 C11 1.382(11) . ?
C11 C15 1.507(11) . ?
C12 C13 1.533(10) . ?
C12 C14 1.539(10) . ?
C15 C16' 1.45(2) . ?
C15 C17' 1.46(2) . ?
C15 C16 1.58(2) . ?
C15 C17 1.597(14) . ?
C18 C23 1.385(10) . ?
C18 C19 1.398(10) . ?
C19 O24 1.385(8) . ?
C19 C20 1.394(10) . ?
C20 C21 1.390(12) . ?
C21 C22 1.372(13) . ?
C22 C23 1.404(11) . ?
O24 C25 1.431(9) . ?
C31 N31 1.333(9) . ?
C31 C32 1.406(10) . ?
C31 C34 1.510(9) . ?
N31 C36 1.448(8) . ?
C32 C33 1.402(10) . ?
C33 N33 1.337(9) . ?
C33 C35 1.511(9) . ?
N33 C48 1.437(9) . ?
C36 C37 1.407(10) . ?
C36 C41 1.411(10) . ?
C37 C38 1.388(10) . ?
C37 C42 1.515(10) . ?
C38 C39 1.381(11) . ?
C39 C40 1.382(12) . ?
C40 C41 1.380(10) . ?
C41 C45 1.512(10) . ?
C42 C43 1.524(10) . ?
C42 C44 1.529(11) . ?
C45 C46 1.516(10) . ?
C45 C47 1.517(11) . ?
C48 C53 1.386(10) . ?
C48 C49 1.401(10) . ?
C49 O54 1.380(9) . ?
C49 C50 1.391(10) . ?
C50 C51 1.389(12) . ?
C51 C52 1.352(11) . ?
C52 C53 1.381(11) . ?
O54 C55 1.432(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Mg N33 142.5(3) . . ?
N3 Mg N31 110.0(2) . . ?
N33 Mg N31 96.2(2) . . ?
N3 Mg N1 86.2(2) . . ?
N33 Mg N1 107.0(2) . . ?
N31 Mg N1 115.1(2) . . ?
N3 Mg O24 69.3(2) . . ?
N33 Mg O24 83.2(2) . . ?
N31 Mg O24 93.3(2) . . ?
N1 Mg O24 147.8(2) . . ?
N1 C1 C2 123.9(6) . . ?
N1 C1 C4 119.6(6) . . ?
C2 C1 C4 116.4(6) . . ?
C1 N1 C6 118.3(6) . . ?
C1 N1 Mg 115.2(4) . . ?
C6 N1 Mg 126.4(4) . . ?
C1 C2 C3 126.6(6) . . ?
N3 C3 C2 121.8(6) . . ?
N3 C3 C5 122.3(6) . . ?
C2 C3 C5 115.8(6) . . ?
N3 C3 Mg 41.0(3) . . ?
C2 C3 Mg 87.1(4) . . ?
C5 C3 Mg 147.3(5) . . ?
C3 N3 C18 122.1(6) . . ?
C3 N3 Mg 113.7(4) . . ?
C18 N3 Mg 123.0(4) . . ?
C7 C6 C11 120.3(7) . . ?
C7 C6 N1 122.2(6) . . ?
C11 C6 N1 117.5(6) . . ?
C8 C7 C6 118.5(7) . . ?
C8 C7 C12 120.9(7) . . ?
C6 C7 C12 120.5(6) . . ?
C9 C8 C7 121.5(8) . . ?
C10 C9 C8 119.5(7) . . ?
C9 C10 C11 122.0(8) . . ?
C10 C11 C6 118.0(7) . . ?
C10 C11 C15 119.9(7) . . ?
C6 C11 C15 122.0(7) . . ?
C7 C12 C13 112.1(6) . . ?
C7 C12 C14 113.1(7) . . ?
C13 C12 C14 110.8(6) . . ?
C16' C15 C17' 112.0(16) . . ?
C16' C15 C11 121.2(13) . . ?
C17' C15 C11 123.7(14) . . ?
C11 C15 C16 108.9(8) . . ?
C11 C15 C17 108.4(9) . . ?
C16 C15 C17 101.9(8) . . ?
C23 C18 C19 119.0(7) . . ?
C23 C18 N3 124.4(7) . . ?
C19 C18 N3 116.6(6) . . ?
O24 C19 C20 124.0(7) . . ?
O24 C19 C18 114.6(6) . . ?
C20 C19 C18 121.4(7) . . ?
C21 C20 C19 118.8(8) . . ?
C22 C21 C20 120.4(8) . . ?
C21 C22 C23 120.7(8) . . ?
C18 C23 C22 119.7(8) . . ?
C19 O24 C25 118.9(6) . . ?
C19 O24 Mg 110.4(4) . . ?
C25 O24 Mg 129.3(5) . . ?
N31 C31 C32 125.1(6) . . ?
N31 C31 C34 120.6(6) . . ?
C32 C31 C34 114.2(6) . . ?
C31 N31 C36 119.1(6) . . ?
C31 N31 Mg 119.4(4) . . ?
C36 N31 Mg 121.0(4) . . ?
C33 C32 C31 133.9(6) . . ?
N33 C33 C32 123.3(6) . . ?
N33 C33 C35 121.5(7) . . ?
C32 C33 C35 115.1(6) . . ?
C33 N33 C48 118.6(5) . . ?
C33 N33 Mg 121.7(5) . . ?
C48 N33 Mg 119.5(4) . . ?
C37 C36 C41 120.1(6) . . ?
C37 C36 N31 119.8(6) . . ?
C41 C36 N31 119.9(6) . . ?
C38 C37 C36 118.2(7) . . ?
C38 C37 C42 120.4(7) . . ?
C36 C37 C42 121.2(6) . . ?
C39 C38 C37 122.5(8) . . ?
C38 C39 C40 118.0(7) . . ?
C41 C40 C39 122.5(8) . . ?
C40 C41 C36 118.5(7) . . ?
C40 C41 C45 116.9(7) . . ?
C36 C41 C45 124.6(6) . . ?
C37 C42 C43 113.5(6) . . ?
C37 C42 C44 110.9(6) . . ?
C43 C42 C44 109.6(7) . . ?
C41 C45 C46 112.6(6) . . ?
C41 C45 C47 111.7(6) . . ?
C46 C45 C47 109.7(6) . . ?
C53 C48 C49 117.1(7) . . ?
C53 C48 N33 119.8(6) . . ?
C49 C48 N33 123.1(7) . . ?
O54 C49 C50 122.6(7) . . ?
O54 C49 C48 115.6(6) . . ?
C50 C49 C48 121.9(7) . . ?
C51 C50 C49 118.4(7) . . ?
C52 C51 C50 120.6(8) . . ?
C51 C52 C53 120.8(8) . . ?
C52 C53 C48 121.2(7) . . ?
C49 O54 C55 117.9(6) . . ?

_refine_diff_density_max         0.280
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.057

#===END

data_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 224372'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C48 H62 N4 O2 Li2'
_chemical_formula_weight         740.90
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   20.8408(6)
_cell_length_b                   8.5688(4)
_cell_length_c                   26.0002(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.256(3)
_cell_angle_gamma                90.00
_cell_volume                     4457.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    28
_cell_measurement_theta_min      11.24
_cell_measurement_theta_max      24.97

_exptl_crystal_description       'platy prisms'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6784
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         60.00
_reflns_number_total             6579
_reflns_number_observed          4792
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 593 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+1.4022P] 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    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00110(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5986
_refine_ls_number_parameters     506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_obs          0.0551
_refine_ls_wR_factor_all         0.1528
_refine_ls_wR_factor_obs         0.1303
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.084
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Li1 Li 0.2170(2) -0.0866(5) 0.4058(2) 0.0377(9) Uani 1 d . .
Li2 Li 0.2788(2) -0.0506(5) 0.3418(2) 0.0368(9) Uani 1 d . .
C1 C 0.11998(11) 0.1188(3) 0.42109(9) 0.0352(5) Uani 1 d . .
N1 N 0.14593(9) -0.0167(2) 0.43638(7) 0.0333(5) Uani 1 d . .
C2 C 0.13479(11) 0.2033(3) 0.37781(9) 0.0344(5) Uani 1 d . .
H2A H 0.13209(11) 0.3138(3) 0.37931(9) 0.041 Uiso 1 calc R .
C3 C 0.15214(11) 0.1438(3) 0.33519(9) 0.0351(5) Uani 1 d . .
N3 N 0.17524(9) -0.0062(2) 0.33202(7) 0.0325(4) Uani 1 d . .
C4 C 0.07000(14) 0.1964(4) 0.44494(11) 0.0488(7) Uani 1 d . .
H4A H 0.02646(14) 0.2014(4) 0.41799(11) 0.073 Uiso 1 d R .
H4B H 0.08519(14) 0.3022(4) 0.45650(11) 0.073 Uiso 1 d R .
H4C H 0.06586(14) 0.1359(4) 0.47584(11) 0.073 Uiso 1 d R .
C5 C 0.1495(2) 0.2529(3) 0.28881(12) 0.0515(7) Uani 1 d . .
H5A H 0.1344(2) 0.1951(3) 0.25503(12) 0.077 Uiso 1 d R .
H5B H 0.1941(2) 0.2959(3) 0.29244(12) 0.077 Uiso 1 d R .
H5C H 0.1182(2) 0.3382(3) 0.28895(12) 0.077 Uiso 1 d R .
C6 C 0.12282(12) -0.1138(3) 0.47182(9) 0.0356(5) Uani 1 d . .
C7 C 0.16515(13) -0.1383(3) 0.52424(10) 0.0423(6) Uani 1 d . .
C8 C 0.14556(15) -0.2444(4) 0.55686(11) 0.0537(7) Uani 1 d . .
H8A H 0.17313(15) -0.2601(4) 0.59233(11) 0.064 Uiso 1 calc R .
C9 C 0.0871(2) -0.3277(4) 0.53929(12) 0.0561(8) Uani 1 d . .
H9A H 0.0748(2) -0.4008(4) 0.56231(12) 0.067 Uiso 1 calc R .
C10 C 0.04658(14) -0.3046(4) 0.48812(11) 0.0491(7) Uani 1 d . .
H10A H 0.00643(14) -0.3631(4) 0.47616(11) 0.059 Uiso 1 calc R .
C11 C 0.06277(12) -0.1980(3) 0.45351(10) 0.0392(6) Uani 1 d . .
C12 C 0.23024(14) -0.0465(4) 0.54253(10) 0.0521(7) Uani 1 d . .
H12A H 0.24868(14) -0.0370(4) 0.51105(10) 0.062 Uiso 1 calc R .
C13 C 0.2828(2) -0.1288(6) 0.58696(14) 0.0833(12) Uani 1 d . .
H13A H 0.3235(2) -0.0653(6) 0.59723(14) 0.125 Uiso 1 calc R .
H13B H 0.2930(2) -0.2308(6) 0.57414(14) 0.125 Uiso 1 calc R .
H13C H 0.2656(2) -0.1432(6) 0.61808(14) 0.125 Uiso 1 calc R .
C14 C 0.2184(2) 0.1182(5) 0.55993(13) 0.0675(9) Uani 1 d . .
H14A H 0.2611(2) 0.1739(5) 0.57142(13) 0.101 Uiso 1 calc R .
H14B H 0.1983(2) 0.1129(5) 0.58978(13) 0.101 Uiso 1 calc R .
H14C H 0.1881(2) 0.1736(5) 0.52981(13) 0.101 Uiso 1 calc R .
C15 C 0.01713(13) -0.1785(3) 0.39690(10) 0.0453(6) Uani 1 d . .
H15A H 0.03341(13) -0.0867(3) 0.38035(10) 0.054 Uiso 1 calc R .
C16 C -0.05478(14) -0.1452(5) 0.39723(13) 0.0651(9) Uani 1 d . .
H16A H -0.08293(14) -0.1332(5) 0.36033(13) 0.098 Uiso 1 calc R .
H16B H -0.05610(14) -0.0489(5) 0.41724(13) 0.098 Uiso 1 calc R .
H16C H -0.07143(14) -0.2322(5) 0.41434(13) 0.098 Uiso 1 calc R .
C17 C 0.0202(2) -0.3215(5) 0.36282(13) 0.0724(10) Uani 1 d . .
H17A H -0.0095(2) -0.3063(5) 0.32661(13) 0.109 Uiso 1 calc R .
H17B H 0.0060(2) -0.4139(5) 0.37897(13) 0.109 Uiso 1 calc R .
H17C H 0.0662(2) -0.3363(5) 0.36097(13) 0.109 Uiso 1 calc R .
C18 C 0.14237(12) -0.0952(3) 0.28778(9) 0.0349(5) Uani 1 d . .
C19 C 0.17543(13) -0.2217(3) 0.27224(11) 0.0430(6) Uani 1 d . .
C20 C 0.1445(2) -0.3216(4) 0.23153(13) 0.0590(8) Uani 1 d . .
H20A H 0.1685(2) -0.4063(4) 0.22223(13) 0.071 Uiso 1 calc R .
C21 C 0.0778(2) -0.2974(4) 0.20411(13) 0.0675(9) Uani 1 d . .
H21A H 0.0558(2) -0.3660(4) 0.17599(13) 0.081 Uiso 1 calc R .
C22 C 0.0438(2) -0.1751(4) 0.21761(13) 0.0616(9) Uani 1 d . .
H22A H -0.0017(2) -0.1579(4) 0.19844(13) 0.074 Uiso 1 calc R .
C23 C 0.07516(13) -0.0756(3) 0.25912(10) 0.0453(6) Uani 1 d . .
H23A H 0.05047(13) 0.0078(3) 0.26832(10) 0.054 Uiso 1 calc R .
O24 O 0.24213(9) -0.2349(2) 0.30154(9) 0.0582(6) Uani 1 d . .
C25 C 0.2797(2) -0.3594(5) 0.2878(2) 0.115(2) Uani 1 d . .
H25A H 0.3273(2) -0.3445(5) 0.3060(2) 0.172 Uiso 1 d R .
H25B H 0.2730(2) -0.3602(5) 0.2489(2) 0.172 Uiso 1 d R .
H25C H 0.2647(2) -0.4589(5) 0.2989(2) 0.172 Uiso 1 d R .
C31 C 0.37148(12) 0.1818(3) 0.34678(9) 0.0356(5) Uani 1 d . .
N31 N 0.34820(10) 0.0576(2) 0.31939(8) 0.0350(5) Uani 1 d . .
C32 C 0.35731(12) 0.2180(3) 0.39672(10) 0.0364(5) Uani 1 d . .
H32A H 0.35788(12) 0.3254(3) 0.40595(10) 0.044 Uiso 1 calc R .
C33 C 0.34320(11) 0.1153(3) 0.43215(9) 0.0357(5) Uani 1 d . .
N33 N 0.32133(9) -0.0352(2) 0.42053(7) 0.0326(4) Uani 1 d . .
C34 C 0.41787(15) 0.2938(4) 0.33053(11) 0.0505(7) Uani 1 d . .
H34A H 0.46394(15) 0.2733(4) 0.35175(11) 0.076 Uiso 1 d R .
H34B H 0.40565(15) 0.4011(4) 0.33686(11) 0.076 Uiso 1 d R .
H34C H 0.41426(15) 0.2800(4) 0.29241(11) 0.076 Uiso 1 d R .
C35 C 0.3488(2) 0.1764(3) 0.48818(11) 0.0509(7) Uani 1 d . .
H35A H 0.3076(2) 0.2317(3) 0.48816(11) 0.076 Uiso 1 d R .
H35B H 0.3868(2) 0.2481(3) 0.49915(11) 0.076 Uiso 1 d R .
H35C H 0.3555(2) 0.0887(3) 0.51334(11) 0.076 Uiso 1 d R .
C36 C 0.37193(12) 0.0067(3) 0.27566(10) 0.0393(6) Uani 1 d . .
C37 C 0.32934(13) 0.0214(3) 0.22344(10) 0.0452(6) Uani 1 d . .
C38 C 0.3505(2) -0.0377(5) 0.18146(12) 0.0650(9) Uani 1 d . .
H38A H 0.3232(2) -0.0243(5) 0.14576(12) 0.078 Uiso 1 calc R .
C39 C 0.4103(2) -0.1156(6) 0.19049(15) 0.0814(12) Uani 1 d . .
H39A H 0.4237(2) -0.1571(6) 0.16120(15) 0.098 Uiso 1 calc R .
C40 C 0.4507(2) -0.1334(5) 0.24172(14) 0.0739(11) Uani 1 d . .
H40A H 0.4917(2) -0.1882(5) 0.24740(14) 0.089 Uiso 1 calc R .
C41 C 0.43320(13) -0.0733(4) 0.28559(12) 0.0509(7) Uani 1 d . .
C42 C 0.26291(14) 0.1054(3) 0.21378(10) 0.0467(7) Uani 1 d . .
H42A H 0.24772(14) 0.0919(3) 0.24674(10) 0.056 Uiso 1 calc R .
C43 C 0.2081(2) 0.0411(4) 0.16702(12) 0.0625(8) Uani 1 d . .
H43A H 0.1669(2) 0.1006(4) 0.16319(12) 0.094 Uiso 1 calc R .
H43B H 0.2002(2) -0.0689(4) 0.17366(12) 0.094 Uiso 1 calc R .
H43C H 0.2219(2) 0.0499(4) 0.13405(12) 0.094 Uiso 1 calc R .
C44 C 0.2715(2) 0.2804(4) 0.20653(12) 0.0627(8) Uani 1 d . .
H44A H 0.2282(2) 0.3326(4) 0.20036(12) 0.094 Uiso 1 calc R .
H44B H 0.2890(2) 0.2978(4) 0.17572(12) 0.094 Uiso 1 calc R .
H44C H 0.3029(2) 0.3231(4) 0.23887(12) 0.094 Uiso 1 calc R .
C45 C 0.47801(14) -0.0991(4) 0.34195(13) 0.0572(8) Uani 1 d . .
H45A H 0.46680(14) -0.0166(4) 0.36526(13) 0.069 Uiso 1 calc R .
C46 C 0.5517(2) -0.0828(7) 0.3459(2) 0.114(2) Uani 1 d . .
H46A H 0.5597(2) 0.0186(7) 0.3314(2) 0.171 Uiso 1 calc R .
H46B H 0.5651(2) -0.1664(7) 0.3254(2) 0.171 Uiso 1 calc R .
H46C H 0.5779(2) -0.0901(7) 0.3836(2) 0.171 Uiso 1 calc R .
C47 C 0.4653(2) -0.2539(5) 0.3640(2) 0.0858(12) Uani 1 d . .
H47A H 0.4176(2) -0.2638(5) 0.3614(2) 0.129 Uiso 1 calc R .
H47B H 0.4914(2) -0.2615(5) 0.4017(2) 0.129 Uiso 1 calc R .
H47C H 0.4786(2) -0.3378(5) 0.3435(2) 0.129 Uiso 1 calc R .
C48 C 0.35313(12) -0.1490(3) 0.45743(10) 0.0372(6) Uani 1 d . .
C49 C 0.31886(13) -0.2861(3) 0.46285(12) 0.0484(7) Uani 1 d . .
C50 C 0.3484(2) -0.4032(4) 0.4973(2) 0.0738(11) Uani 1 d . .
H50A H 0.3236(2) -0.4936(4) 0.5007(2) 0.089 Uiso 1 calc R .
C51 C 0.4150(2) -0.3891(4) 0.5272(2) 0.0821(12) Uani 1 d . .
H51A H 0.4356(2) -0.4693(4) 0.5515(2) 0.099 Uiso 1 calc R .
C52 C 0.4504(2) -0.2599(4) 0.52158(14) 0.0701(10) Uani 1 d . .
H52A H 0.4961(2) -0.2512(4) 0.54119(14) 0.084 Uiso 1 calc R .
C53 C 0.41985(13) -0.1410(4) 0.48730(11) 0.0512(7) Uani 1 d . .
H53A H 0.44523(13) -0.0512(4) 0.48409(11) 0.061 Uiso 1 calc R .
O54 O 0.25262(9) -0.2896(2) 0.43192(9) 0.0593(6) Uani 1 d . .
C55 C 0.2166(2) -0.4316(4) 0.4304(2) 0.113(2) Uani 1 d . .
H55A H 0.1723(2) -0.4216(4) 0.4047(2) 0.169 Uiso 1 d R .
H55B H 0.2118(2) -0.4540(4) 0.4661(2) 0.169 Uiso 1 d R .
H55C H 0.2411(2) -0.5170(4) 0.4192(2) 0.169 Uiso 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
Li1 0.030(2) 0.047(2) 0.034(2) 0.004(2) 0.007(2) -0.001(2)
Li2 0.032(2) 0.042(2) 0.036(2) -0.003(2) 0.009(2) -0.004(2)
C1 0.0309(12) 0.0415(14) 0.0306(11) -0.0068(10) 0.0043(9) -0.0036(10)
N1 0.0294(10) 0.0407(11) 0.0281(9) 0.0014(9) 0.0051(8) -0.0041(9)
C2 0.0316(12) 0.0327(12) 0.0384(12) -0.0019(10) 0.0087(10) -0.0031(10)
C3 0.0252(11) 0.0402(13) 0.0384(13) 0.0033(11) 0.0064(9) 0.0008(10)
N3 0.0280(9) 0.0373(11) 0.0305(10) -0.0011(8) 0.0052(8) 0.0018(8)
C4 0.053(2) 0.054(2) 0.0437(14) -0.0063(13) 0.0203(12) 0.0051(13)
C5 0.060(2) 0.049(2) 0.052(2) 0.0161(13) 0.0263(14) 0.0102(14)
C6 0.0328(12) 0.0435(14) 0.0307(12) 0.0027(10) 0.0092(10) -0.0020(11)
C7 0.0391(13) 0.054(2) 0.0306(12) 0.0041(12) 0.0051(10) -0.0043(12)
C8 0.053(2) 0.069(2) 0.0354(13) 0.0155(14) 0.0067(12) -0.0015(15)
C9 0.056(2) 0.064(2) 0.049(2) 0.0185(14) 0.0163(13) -0.0068(15)
C10 0.0386(14) 0.057(2) 0.052(2) 0.0085(13) 0.0136(12) -0.0097(12)
C11 0.0326(12) 0.0471(14) 0.0376(13) 0.0033(11) 0.0094(10) -0.0020(11)
C12 0.0427(14) 0.075(2) 0.0331(13) 0.0040(13) 0.0024(11) -0.0115(14)
C13 0.052(2) 0.120(3) 0.059(2) 0.024(2) -0.015(2) -0.016(2)
C14 0.066(2) 0.084(2) 0.051(2) -0.023(2) 0.0137(15) -0.025(2)
C15 0.0348(13) 0.056(2) 0.0396(13) 0.0045(12) 0.0017(11) -0.0132(12)
C16 0.0363(15) 0.086(2) 0.065(2) 0.018(2) 0.0013(13) -0.004(2)
C17 0.077(2) 0.083(3) 0.047(2) -0.010(2) 0.002(2) -0.006(2)
C18 0.0303(12) 0.0393(13) 0.0332(12) 0.0034(10) 0.0057(10) -0.0049(10)
C19 0.0350(13) 0.0430(14) 0.0469(14) -0.0065(12) 0.0048(11) -0.0061(11)
C20 0.059(2) 0.047(2) 0.064(2) -0.0191(15) 0.0053(15) -0.0104(14)
C21 0.065(2) 0.061(2) 0.058(2) -0.013(2) -0.013(2) -0.016(2)
C22 0.043(2) 0.069(2) 0.056(2) 0.004(2) -0.0128(13) -0.009(2)
C23 0.0327(13) 0.054(2) 0.0427(14) 0.0047(12) 0.0002(11) -0.0038(12)
O24 0.0321(10) 0.0456(11) 0.0873(15) -0.0262(10) 0.0009(9) 0.0039(8)
C25 0.050(2) 0.073(3) 0.197(5) -0.069(3) -0.003(3) 0.016(2)
C31 0.0321(12) 0.0384(13) 0.0352(12) 0.0015(11) 0.0075(10) -0.0018(10)
N31 0.0331(10) 0.0399(11) 0.0320(10) -0.0047(9) 0.0093(8) -0.0018(9)
C32 0.0357(12) 0.0330(12) 0.0399(13) -0.0042(10) 0.0097(10) -0.0038(10)
C33 0.0288(11) 0.0391(13) 0.0371(13) -0.0066(11) 0.0057(10) -0.0039(10)
N33 0.0279(9) 0.0330(10) 0.0338(10) -0.0032(8) 0.0038(8) -0.0041(8)
C34 0.052(2) 0.051(2) 0.050(2) -0.0022(13) 0.0182(13) -0.0154(13)
C35 0.067(2) 0.048(2) 0.0396(14) -0.0124(12) 0.0182(13) -0.0164(14)
C36 0.0359(13) 0.0441(14) 0.0396(13) -0.0054(11) 0.0136(11) -0.0027(11)
C37 0.0436(14) 0.054(2) 0.0398(14) -0.0050(12) 0.0144(11) 0.0006(12)
C38 0.064(2) 0.091(3) 0.043(2) -0.011(2) 0.0214(14) 0.011(2)
C39 0.069(2) 0.118(3) 0.066(2) -0.027(2) 0.034(2) 0.018(2)
C40 0.046(2) 0.103(3) 0.076(2) -0.023(2) 0.024(2) 0.017(2)
C41 0.0367(14) 0.059(2) 0.058(2) -0.0075(14) 0.0141(12) 0.0025(13)
C42 0.050(2) 0.057(2) 0.0315(12) -0.0017(12) 0.0086(11) 0.0107(13)
C43 0.055(2) 0.078(2) 0.049(2) -0.009(2) 0.0055(14) 0.005(2)
C44 0.076(2) 0.057(2) 0.049(2) -0.0020(14) 0.0069(15) 0.011(2)
C45 0.0392(15) 0.064(2) 0.063(2) -0.006(2) 0.0047(13) 0.0089(14)
C46 0.043(2) 0.169(5) 0.114(3) 0.043(4) -0.006(2) -0.027(3)
C47 0.078(3) 0.093(3) 0.078(2) 0.013(2) 0.007(2) -0.017(2)
C48 0.0302(12) 0.0390(13) 0.0377(13) -0.0062(11) 0.0017(10) 0.0013(10)
C49 0.0372(14) 0.0383(14) 0.060(2) -0.0008(13) -0.0029(12) 0.0020(12)
C50 0.068(2) 0.038(2) 0.098(3) 0.013(2) -0.007(2) 0.0020(15)
C51 0.070(2) 0.058(2) 0.094(3) 0.021(2) -0.018(2) 0.017(2)
C52 0.045(2) 0.070(2) 0.075(2) 0.003(2) -0.016(2) 0.010(2)
C53 0.0334(14) 0.055(2) 0.056(2) 0.0003(14) -0.0035(12) 0.0006(12)
O54 0.0365(10) 0.0346(10) 0.092(2) 0.0059(10) -0.0071(10) -0.0074(8)
C55 0.056(2) 0.046(2) 0.202(5) 0.016(3) -0.019(3) -0.022(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O54 1.938(5) . ?
Li1 N1 1.959(4) . ?
Li1 N3 1.995(4) . ?
Li1 N33 2.146(4) . ?
Li2 O24 1.930(4) . ?
Li2 N31 1.941(4) . ?
Li2 N33 1.993(4) . ?
Li2 N3 2.134(4) . ?
C1 N1 1.295(3) . ?
C1 C2 1.443(3) . ?
C1 C4 1.508(4) . ?
N1 C6 1.422(3) . ?
C2 C3 1.357(3) . ?
C3 N3 1.383(3) . ?
C3 C5 1.514(4) . ?
N3 C18 1.390(3) . ?
C6 C11 1.407(4) . ?
C6 C7 1.417(3) . ?
C7 C8 1.380(4) . ?
C7 C12 1.524(4) . ?
C8 C9 1.375(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.388(4) . ?
C11 C15 1.522(3) . ?
C12 C14 1.523(5) . ?
C12 C13 1.524(4) . ?
C15 C17 1.524(5) . ?
C15 C16 1.528(4) . ?
C18 C23 1.400(3) . ?
C18 C19 1.403(4) . ?
C19 C20 1.374(4) . ?
C19 O24 1.390(3) . ?
C20 C21 1.390(5) . ?
C21 C22 1.365(5) . ?
C22 C23 1.387(4) . ?
O24 C25 1.427(4) . ?
C31 N31 1.297(3) . ?
C31 C32 1.444(3) . ?
C31 C34 1.504(4) . ?
N31 C36 1.429(3) . ?
C32 C33 1.365(4) . ?
C33 N33 1.372(3) . ?
C33 C35 1.521(3) . ?
N33 C48 1.398(3) . ?
C36 C37 1.404(4) . ?
C36 C41 1.408(4) . ?
C37 C38 1.382(4) . ?
C37 C42 1.518(4) . ?
C38 C39 1.376(5) . ?
C39 C40 1.370(5) . ?
C40 C41 1.390(4) . ?
C41 C45 1.517(4) . ?
C42 C43 1.520(4) . ?
C42 C44 1.528(4) . ?
C45 C47 1.499(5) . ?
C45 C46 1.516(5) . ?
C48 C53 1.392(4) . ?
C48 C49 1.402(4) . ?
C49 C50 1.370(4) . ?
C49 O54 1.390(3) . ?
C50 C51 1.394(5) . ?
C51 C52 1.360(5) . ?
C52 C53 1.386(5) . ?
O54 C55 1.424(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
O54 Li1 N1 113.1(2) . . ?
O54 Li1 N3 131.9(2) . . ?
N1 Li1 N3 96.3(2) . . ?
O54 Li1 N33 81.5(2) . . ?
N1 Li1 N33 135.1(2) . . ?
N3 Li1 N33 104.3(2) . . ?
O24 Li2 N31 116.2(2) . . ?
O24 Li2 N33 127.3(2) . . ?
N31 Li2 N33 97.0(2) . . ?
O24 Li2 N3 81.3(2) . . ?
N31 Li2 N3 133.8(2) . . ?
N33 Li2 N3 104.8(2) . . ?
N1 C1 C2 121.8(2) . . ?
N1 C1 C4 123.1(2) . . ?
C2 C1 C4 115.0(2) . . ?
C1 N1 C6 122.4(2) . . ?
C1 N1 Li1 116.6(2) . . ?
C6 N1 Li1 121.0(2) . . ?
C3 C2 C1 127.8(2) . . ?
C2 C3 N3 125.0(2) . . ?
C2 C3 C5 117.4(2) . . ?
N3 C3 C5 117.5(2) . . ?
C2 C3 Li1 85.3(2) . . ?
N3 C3 Li1 42.73(14) . . ?
C5 C3 Li1 150.2(2) . . ?
C3 N3 C18 117.4(2) . . ?
C3 N3 Li1 109.2(2) . . ?
C18 N3 Li1 126.0(2) . . ?
C3 N3 Li2 121.0(2) . . ?
C18 N3 Li2 104.4(2) . . ?
Li1 N3 Li2 70.7(2) . . ?
C11 C6 C7 120.3(2) . . ?
C11 C6 N1 120.8(2) . . ?
C7 C6 N1 118.5(2) . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 C12 122.6(2) . . ?
C6 C7 C12 118.9(2) . . ?
C9 C8 C7 121.6(2) . . ?
C8 C9 C10 119.6(3) . . ?
C9 C10 C11 121.8(3) . . ?
C10 C11 C6 118.2(2) . . ?
C10 C11 C15 120.0(2) . . ?
C6 C11 C15 121.8(2) . . ?
C7 C12 C14 111.5(3) . . ?
C7 C12 C13 112.7(3) . . ?
C14 C12 C13 110.2(3) . . ?
C11 C15 C17 110.9(2) . . ?
C11 C15 C16 111.3(2) . . ?
C17 C15 C16 110.8(3) . . ?
N3 C18 C23 124.2(2) . . ?
N3 C18 C19 119.6(2) . . ?
C23 C18 C19 116.0(2) . . ?
C20 C19 O24 123.5(3) . . ?
C20 C19 C18 122.8(3) . . ?
O24 C19 C18 113.7(2) . . ?
C19 C20 C21 119.2(3) . . ?
C22 C21 C20 120.0(3) . . ?
C21 C22 C23 120.4(3) . . ?
C22 C23 C18 121.6(3) . . ?
C19 O24 C25 117.3(2) . . ?
C19 O24 Li2 114.4(2) . . ?
C25 O24 Li2 125.9(2) . . ?
N31 C31 C32 122.1(2) . . ?
N31 C31 C34 122.7(2) . . ?
C32 C31 C34 115.1(2) . . ?
N31 C31 Li2 39.72(14) . . ?
C32 C31 Li2 83.1(2) . . ?
C34 C31 Li2 161.2(2) . . ?
C31 N31 C36 121.9(2) . . ?
C31 N31 Li2 115.0(2) . . ?
C36 N31 Li2 123.1(2) . . ?
C33 C32 C31 127.3(2) . . ?
C32 C33 N33 125.3(2) . . ?
C32 C33 C35 116.8(2) . . ?
N33 C33 C35 117.8(2) . . ?
C32 C33 Li2 84.5(2) . . ?
N33 C33 Li2 43.46(14) . . ?
C35 C33 Li2 152.0(2) . . ?
C33 N33 C48 116.1(2) . . ?
C33 N33 Li2 108.3(2) . . ?
C48 N33 Li2 130.3(2) . . ?
C33 N33 Li1 119.3(2) . . ?
C48 N33 Li1 103.9(2) . . ?
Li2 N33 Li1 70.5(2) . . ?
C37 C36 C41 121.1(2) . . ?
C37 C36 N31 118.4(2) . . ?
C41 C36 N31 120.1(2) . . ?
C38 C37 C36 118.4(3) . . ?
C38 C37 C42 121.4(3) . . ?
C36 C37 C42 120.2(2) . . ?
C39 C38 C37 121.1(3) . . ?
C40 C39 C38 120.1(3) . . ?
C39 C40 C41 121.7(3) . . ?
C40 C41 C36 117.6(3) . . ?
C40 C41 C45 120.4(3) . . ?
C36 C41 C45 121.9(3) . . ?
C37 C42 C43 114.0(2) . . ?
C37 C42 C44 110.7(3) . . ?
C43 C42 C44 110.2(3) . . ?
C47 C45 C46 109.8(3) . . ?
C47 C45 C41 111.8(3) . . ?
C46 C45 C41 113.0(3) . . ?
C53 C48 N33 123.8(2) . . ?
C53 C48 C49 116.3(2) . . ?
N33 C48 C49 119.8(2) . . ?
C50 C49 O54 123.6(3) . . ?
C50 C49 C48 122.0(3) . . ?
O54 C49 C48 114.3(2) . . ?
C49 C50 C51 119.8(3) . . ?
C52 C51 C50 119.7(3) . . ?
C51 C52 C53 120.2(3) . . ?
C52 C53 C48 122.0(3) . . ?
C49 O54 C55 117.7(2) . . ?
C49 O54 Li1 113.9(2) . . ?
C55 O54 Li1 127.6(2) . . ?

_refine_diff_density_max         0.211
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.037

#===END

data_Compound_7
_database_code_depnum_ccdc_archive 'CCDC 224373'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C30 H49 N3 O Si2 Zn'
_chemical_formula_weight         589.27
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.407(2)
_cell_length_b                   18.2361(15)
_cell_length_c                   16.251(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.289(14)
_cell_angle_gamma                90.00
_cell_volume                     3275.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    39
_cell_measurement_theta_min      10.56
_cell_measurement_theta_max      27.94

_exptl_crystal_description       blocks
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.43
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.3427
_exptl_absorpt_correction_T_max  0.7651

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5132
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.71
_diffrn_reflns_theta_max         59.97
_reflns_number_total             4859
_reflns_number_observed          4456
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 84 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.9085P] 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    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00018(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4775
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_obs          0.0355
_refine_ls_wR_factor_all         0.1059
_refine_ls_wR_factor_obs         0.0896
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_restrained_S_all      1.280
_refine_ls_restrained_S_obs      1.132
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn Zn 0.85229(3) 0.18602(2) 0.74521(2) 0.02361(12) Uani 1 d . .
C1 C 0.8124(2) 0.23918(13) 0.90139(15) 0.0249(5) Uani 1 d . .
N1 N 0.7740(2) 0.19075(11) 0.83927(12) 0.0232(4) Uani 1 d . .
C2 C 0.8916(2) 0.29718(13) 0.89836(15) 0.0258(5) Uani 1 d . .
H2A H 0.9213(2) 0.32249(13) 0.95044(15) 0.031 Uiso 1 calc R .
C3 C 0.9336(2) 0.32335(13) 0.82976(15) 0.0234(5) Uani 1 d . .
N3 N 0.9243(2) 0.28478(11) 0.75918(12) 0.0243(4) Uani 1 d . .
C4 C 0.7656(3) 0.2347(2) 0.9805(2) 0.0382(7) Uani 1 d . .
H4A H 0.8062(3) 0.2717(2) 1.0214(2) 0.057 Uiso 1 d R .
H4B H 0.7820(3) 0.1858(2) 1.0056(2) 0.057 Uiso 1 d R .
H4C H 0.6782(3) 0.2437(2) 0.9656(2) 0.057 Uiso 1 d R .
C5 C 0.9849(3) 0.40013(14) 0.8392(2) 0.0352(6) Uani 1 d . .
H5A H 1.0735(3) 0.39771(14) 0.8528(2) 0.053 Uiso 1 d R .
H5B H 0.9594(3) 0.42544(14) 0.8851(2) 0.053 Uiso 1 d R .
H5C H 0.9552(3) 0.42705(14) 0.7860(2) 0.053 Uiso 1 d R .
C6 C 0.6712(2) 0.14486(13) 0.83962(15) 0.0234(5) Uani 1 d . .
C7 C 0.6879(2) 0.07116(13) 0.86363(15) 0.0252(5) Uani 1 d . .
C8 C 0.5856(2) 0.02690(15) 0.8551(2) 0.0322(6) Uani 1 d . .
H8A H 0.5951(2) -0.02328(15) 0.8711(2) 0.039 Uiso 1 calc R .
C9 C 0.4714(2) 0.05478(15) 0.8240(2) 0.0363(6) Uani 1 d . .
H9A H 0.4030(2) 0.02360(15) 0.8169(2) 0.044 Uiso 1 calc R .
C10 C 0.4562(2) 0.1280(2) 0.8031(2) 0.0352(6) Uani 1 d . .
H10A H 0.3767(2) 0.1469(2) 0.7826(2) 0.042 Uiso 1 calc R .
C11 C 0.5542(2) 0.17481(14) 0.8113(2) 0.0282(6) Uani 1 d . .
C12 C 0.8115(2) 0.03796(14) 0.9010(2) 0.0320(6) Uani 1 d . .
H12A H 0.8737(2) 0.07662(14) 0.9011(2) 0.038 Uiso 1 calc R .
C13 C 0.8375(3) -0.0265(2) 0.8484(2) 0.0443(7) Uani 1 d . .
H13A H 0.9179(3) -0.0465(2) 0.8745(2) 0.066 Uiso 1 calc R .
H13B H 0.8349(3) -0.0098(2) 0.7906(2) 0.066 Uiso 1 calc R .
H13C H 0.7764(3) -0.0647(2) 0.8462(2) 0.066 Uiso 1 calc R .
C14 C 0.8227(3) 0.0144(2) 0.9933(2) 0.0451(7) Uani 1 d . .
H14A H 0.9029(3) -0.0069(2) 1.0166(2) 0.068 Uiso 1 calc R .
H14B H 0.7604(3) -0.0221(2) 0.9950(2) 0.068 Uiso 1 calc R .
H14C H 0.8119(3) 0.0572(2) 1.0271(2) 0.068 Uiso 1 calc R .
C15 C 0.5323(2) 0.25582(15) 0.7905(2) 0.0365(6) Uani 1 d . .
H15A H 0.6114(2) 0.28209(15) 0.8096(2) 0.044 Uiso 1 calc R .
C16 C 0.4449(4) 0.2883(2) 0.8377(3) 0.0799(13) Uani 1 d . .
H16A H 0.4760(4) 0.2802(2) 0.8988(3) 0.120 Uiso 1 calc R .
H16B H 0.3657(4) 0.2646(2) 0.8183(3) 0.120 Uiso 1 calc R .
H16C H 0.4365(4) 0.3411(2) 0.8264(3) 0.120 Uiso 1 calc R .
C17 C 0.4857(5) 0.2679(2) 0.6966(2) 0.0865(14) Uani 1 d . .
H17A H 0.5427(5) 0.2468(2) 0.6668(2) 0.130 Uiso 1 calc R .
H17B H 0.4775(5) 0.3206(2) 0.6849(2) 0.130 Uiso 1 calc R .
H17C H 0.4067(5) 0.2442(2) 0.6769(2) 0.130 Uiso 1 calc R .
C18 C 0.9630(2) 0.31322(13) 0.6888(2) 0.0254(5) Uani 1 d . .
C19 C 0.8807(2) 0.31152(13) 0.6091(2) 0.0292(6) Uani 1 d . .
C20 C 0.9143(3) 0.33689(15) 0.5379(2) 0.0377(7) Uani 1 d . .
H20A H 0.8578(3) 0.33623(15) 0.4841(2) 0.045 Uiso 1 calc R .
C21 C 1.0299(3) 0.3631(2) 0.5450(2) 0.0409(7) Uani 1 d . .
H21A H 1.0522(3) 0.3812(2) 0.4962(2) 0.049 Uiso 1 calc R .
C22 C 1.1128(3) 0.3632(2) 0.6223(2) 0.0401(7) Uani 1 d . .
H22A H 1.1926(3) 0.3807(2) 0.6268(2) 0.048 Uiso 1 calc R .
C23 C 1.0800(2) 0.33774(14) 0.6938(2) 0.0326(6) Uani 1 d . .
H23A H 1.1382(2) 0.33703(14) 0.7469(2) 0.039 Uiso 1 calc R .
O24 O 0.7688(2) 0.28350(10) 0.60851(11) 0.0351(4) Uani 1 d . .
C25 C 0.6764(3) 0.2891(2) 0.5307(2) 0.0479(8) Uani 1 d . .
H25A H 0.6014(3) 0.2673(2) 0.5384(2) 0.072 Uiso 1 calc R .
H25B H 0.7024(3) 0.2630(2) 0.4855(2) 0.072 Uiso 1 calc R .
H25C H 0.6625(3) 0.3409(2) 0.5151(2) 0.072 Uiso 1 calc R .
N26 N 0.9010(2) 0.10806(11) 0.68437(12) 0.0260(5) Uani 1 d . .
Si27 Si 0.79964(6) 0.07010(4) 0.59976(5) 0.0333(2) Uani 1 d . .
C28 C 0.8225(3) 0.1042(2) 0.4961(2) 0.0649(11) Uani 1 d . .
H28A H 0.9046(3) 0.0920(2) 0.4920(2) 0.097 Uiso 1 calc R .
H28B H 0.8114(3) 0.1575(2) 0.4928(2) 0.097 Uiso 1 calc R .
H28C H 0.7636(3) 0.0809(2) 0.4493(2) 0.097 Uiso 1 calc R .
C29 C 0.6430(2) 0.0935(2) 0.6071(2) 0.0427(7) Uani 1 d . .
H29A H 0.6350(2) 0.1468(2) 0.6105(2) 0.064 Uiso 1 calc R .
H29B H 0.6273(2) 0.0707(2) 0.6580(2) 0.064 Uiso 1 calc R .
H29C H 0.5844(2) 0.0751(2) 0.5566(2) 0.064 Uiso 1 calc R .
C30 C 0.8088(3) -0.0322(2) 0.5934(2) 0.0601(10) Uani 1 d . .
H30A H 0.8901(3) -0.0464(2) 0.5895(2) 0.090 Uiso 1 calc R .
H30B H 0.7491(3) -0.0496(2) 0.5430(2) 0.090 Uiso 1 calc R .
H30C H 0.7920(3) -0.0540(2) 0.6444(2) 0.090 Uiso 1 calc R .
Si31 Si 1.05451(6) 0.09536(4) 0.71039(4) 0.0296(2) Uani 1 d . .
C32 C 1.1197(2) 0.1376(2) 0.8166(2) 0.0394(7) Uani 1 d . .
H32A H 1.0982(2) 0.1897(2) 0.8148(2) 0.059 Uiso 1 calc R .
H32B H 1.2079(2) 0.1325(2) 0.8310(2) 0.059 Uiso 1 calc R .
H32C H 1.0871(2) 0.1128(2) 0.8596(2) 0.059 Uiso 1 calc R .
C33 C 1.1301(3) 0.1372(2) 0.6317(2) 0.0514(8) Uani 1 d . .
H33A H 1.1082(3) 0.1891(2) 0.6241(2) 0.077 Uiso 1 calc R .
H33B H 1.1037(3) 0.1117(2) 0.5772(2) 0.077 Uiso 1 calc R .
H33C H 1.2181(3) 0.1326(2) 0.6526(2) 0.077 Uiso 1 calc R .
C34 C 1.1006(3) -0.0029(2) 0.7211(3) 0.0602(9) Uani 1 d . .
H34A H 1.0687(3) -0.0281(2) 0.6669(3) 0.090 Uiso 1 calc R .
H34B H 1.0683(3) -0.0260(2) 0.7652(3) 0.090 Uiso 1 calc R .
H34C H 1.1891(3) -0.0063(2) 0.7367(3) 0.090 Uiso 1 calc R .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.0240(2) 0.0233(2) 0.0240(2) -0.00362(13) 0.00667(13) -0.00372(13)
C1 0.0233(12) 0.0272(13) 0.0228(12) 0.0007(10) 0.0030(10) 0.0003(10)
N1 0.0220(10) 0.0246(11) 0.0232(10) -0.0010(8) 0.0056(8) -0.0038(8)
C2 0.0263(13) 0.0277(13) 0.0210(12) -0.0033(10) 0.0013(10) -0.0030(10)
C3 0.0200(12) 0.0227(12) 0.0254(12) 0.0003(10) 0.0019(10) -0.0016(9)
N3 0.0250(10) 0.0230(11) 0.0249(11) 0.0018(9) 0.0062(8) -0.0010(8)
C4 0.046(2) 0.044(2) 0.0275(14) -0.0068(12) 0.0151(12) -0.0134(13)
C5 0.043(2) 0.0277(14) 0.0362(15) -0.0060(12) 0.0122(12) -0.0100(12)
C6 0.0225(12) 0.0248(13) 0.0237(12) -0.0018(10) 0.0070(10) -0.0039(10)
C7 0.0261(13) 0.0251(13) 0.0254(12) -0.0018(10) 0.0082(10) -0.0008(10)
C8 0.0318(14) 0.0257(14) 0.0393(15) -0.0015(11) 0.0095(12) -0.0035(11)
C9 0.0273(14) 0.033(2) 0.048(2) -0.0015(13) 0.0079(12) -0.0092(12)
C10 0.0228(13) 0.038(2) 0.043(2) 0.0014(12) 0.0046(11) -0.0009(11)
C11 0.0260(13) 0.0292(14) 0.0283(13) 0.0025(11) 0.0050(10) -0.0007(10)
C12 0.0258(13) 0.0289(14) 0.0414(15) 0.0038(12) 0.0086(11) 0.0026(11)
C13 0.046(2) 0.040(2) 0.051(2) 0.0029(14) 0.0188(14) 0.0130(14)
C14 0.038(2) 0.053(2) 0.041(2) 0.0062(14) 0.0048(13) 0.0082(14)
C15 0.0287(14) 0.0315(15) 0.048(2) 0.0094(13) 0.0063(12) 0.0023(11)
C16 0.107(3) 0.041(2) 0.112(3) 0.016(2) 0.064(3) 0.026(2)
C17 0.145(4) 0.058(2) 0.054(2) 0.026(2) 0.021(3) 0.026(3)
C18 0.0315(14) 0.0187(12) 0.0281(13) 0.0009(10) 0.0113(11) 0.0004(10)
C19 0.0372(15) 0.0210(13) 0.0305(14) 0.0008(10) 0.0106(11) 0.0000(11)
C20 0.055(2) 0.0316(15) 0.0296(14) 0.0029(12) 0.0164(13) 0.0062(13)
C21 0.059(2) 0.031(2) 0.042(2) 0.0059(12) 0.0315(15) 0.0045(13)
C22 0.043(2) 0.033(2) 0.054(2) 0.0004(13) 0.0294(15) -0.0012(12)
C23 0.0322(14) 0.0285(14) 0.0388(15) -0.0016(11) 0.0120(12) -0.0006(11)
O24 0.0336(10) 0.0408(11) 0.0271(9) 0.0048(8) 0.0006(8) -0.0067(8)
C25 0.048(2) 0.053(2) 0.034(2) 0.0048(14) -0.0056(13) -0.0053(15)
N26 0.0267(11) 0.0252(11) 0.0265(11) -0.0044(9) 0.0071(9) -0.0032(9)
Si27 0.0314(4) 0.0381(4) 0.0296(4) -0.0109(3) 0.0058(3) -0.0088(3)
C28 0.057(2) 0.106(3) 0.031(2) -0.007(2) 0.0083(15) -0.016(2)
C29 0.033(2) 0.047(2) 0.044(2) -0.0031(14) 0.0021(13) -0.0067(13)
C30 0.051(2) 0.046(2) 0.079(2) -0.031(2) 0.009(2) -0.012(2)
Si31 0.0273(4) 0.0303(4) 0.0313(4) -0.0066(3) 0.0076(3) -0.0012(3)
C32 0.0286(14) 0.051(2) 0.036(2) -0.0048(13) 0.0019(12) 0.0003(12)
C33 0.039(2) 0.075(2) 0.044(2) -0.007(2) 0.0179(14) -0.009(2)
C34 0.042(2) 0.043(2) 0.091(3) -0.012(2) 0.007(2) 0.0081(15)

_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
Zn N26 1.892(2) . ?
Zn N1 1.953(2) . ?
Zn N3 1.969(2) . ?
C1 N1 1.331(3) . ?
C1 C2 1.400(3) . ?
C1 C4 1.510(3) . ?
N1 C6 1.441(3) . ?
C2 C3 1.401(3) . ?
C3 N3 1.327(3) . ?
C3 C5 1.511(3) . ?
N3 C18 1.421(3) . ?
C6 C7 1.399(3) . ?
C6 C11 1.411(3) . ?
C7 C8 1.398(3) . ?
C7 C12 1.517(3) . ?
C8 C9 1.373(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.386(4) . ?
C11 C15 1.522(4) . ?
C12 C13 1.526(4) . ?
C12 C14 1.534(4) . ?
C15 C17 1.503(5) . ?
C15 C16 1.521(4) . ?
C18 C23 1.391(4) . ?
C18 C19 1.400(4) . ?
C19 O24 1.372(3) . ?
C19 C20 1.386(4) . ?
C20 C21 1.380(4) . ?
C21 C22 1.374(4) . ?
C22 C23 1.385(4) . ?
O24 C25 1.436(3) . ?
N26 Si27 1.709(2) . ?
N26 Si31 1.713(2) . ?
Si27 C29 1.870(3) . ?
Si27 C30 1.872(3) . ?
Si27 C28 1.873(3) . ?
Si31 C34 1.864(3) . ?
Si31 C32 1.868(3) . ?
Si31 C33 1.872(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
N26 Zn N1 133.80(9) . . ?
N26 Zn N3 125.42(8) . . ?
N1 Zn N3 97.34(8) . . ?
N1 C1 C2 124.7(2) . . ?
N1 C1 C4 119.3(2) . . ?
C2 C1 C4 116.0(2) . . ?
C1 N1 C6 119.8(2) . . ?
C1 N1 Zn 119.6(2) . . ?
C6 N1 Zn 120.46(15) . . ?
C1 C2 C3 129.5(2) . . ?
N3 C3 C2 122.5(2) . . ?
N3 C3 C5 121.7(2) . . ?
C2 C3 C5 115.8(2) . . ?
C3 N3 C18 121.9(2) . . ?
C3 N3 Zn 121.7(2) . . ?
C18 N3 Zn 116.4(2) . . ?
C7 C6 C11 121.0(2) . . ?
C7 C6 N1 120.3(2) . . ?
C11 C6 N1 118.6(2) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 C12 118.7(2) . . ?
C6 C7 C12 123.0(2) . . ?
C9 C8 C7 121.0(2) . . ?
C8 C9 C10 120.0(2) . . ?
C9 C10 C11 121.5(2) . . ?
C10 C11 C6 118.0(2) . . ?
C10 C11 C15 119.5(2) . . ?
C6 C11 C15 122.6(2) . . ?
C7 C12 C13 111.9(2) . . ?
C7 C12 C14 110.4(2) . . ?
C13 C12 C14 110.6(2) . . ?
C17 C15 C16 110.1(3) . . ?
C17 C15 C11 111.4(3) . . ?
C16 C15 C11 111.0(2) . . ?
C23 C18 C19 118.4(2) . . ?
C23 C18 N3 123.7(2) . . ?
C19 C18 N3 117.8(2) . . ?
O24 C19 C20 124.5(2) . . ?
O24 C19 C18 115.2(2) . . ?
C20 C19 C18 120.3(2) . . ?
C21 C20 C19 120.1(3) . . ?
C22 C21 C20 120.3(3) . . ?
C21 C22 C23 119.9(3) . . ?
C22 C23 C18 120.9(3) . . ?
C19 O24 C25 117.3(2) . . ?
Si27 N26 Si31 126.23(12) . . ?
Si27 N26 Zn 119.83(11) . . ?
Si31 N26 Zn 112.75(11) . . ?
N26 Si27 C29 108.89(12) . . ?
N26 Si27 C30 114.34(14) . . ?
C29 Si27 C30 107.31(15) . . ?
N26 Si27 C28 111.85(14) . . ?
C29 Si27 C28 109.2(2) . . ?
C30 Si27 C28 105.0(2) . . ?
N26 Si31 C34 113.63(13) . . ?
N26 Si31 C32 108.78(11) . . ?
C34 Si31 C32 105.8(2) . . ?
N26 Si31 C33 113.06(13) . . ?
C34 Si31 C33 106.7(2) . . ?
C32 Si31 C33 108.51(14) . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.051

#===END

data_Compound_8
_database_code_depnum_ccdc_archive 'CCDC 224374'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H36 N2 O Zn'
_chemical_formula_weight         457.94

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.6145(16)
_cell_length_b                   16.025(3)
_cell_length_c                   13.905(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.273(12)
_cell_angle_gamma                90.00
_cell_volume                     2528.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    24
_cell_measurement_theta_min      4.90
_cell_measurement_theta_max      12.43

_exptl_crystal_description       plates
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_type   'Lamina [1 0 -1]'
_exptl_absorpt_correction_T_min  0.7903
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      183(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 P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        15.45
_diffrn_reflns_number            4355
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4139
_reflns_number_gt                2627
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4139
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1170
_refine_ls_wR_factor_gt          0.1032
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.945
_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
Zn Zn 0.83772(5) 0.36899(3) 0.61087(4) 0.03446(15) Uani 1 1 d . . .
C1 C 0.8395(4) 0.5249(3) 0.7175(3) 0.0307(9) Uani 1 1 d . . .
N1 N 0.8470(4) 0.4424(2) 0.7249(2) 0.0321(8) Uani 1 1 d . . .
C2 C 0.8240(4) 0.5695(3) 0.6284(3) 0.0313(10) Uani 1 1 d . . .
H2A H 0.8244 0.6286 0.6340 0.038 Uiso 1 1 calc R . .
C3 C 0.8080(4) 0.5380(3) 0.5328(3) 0.0301(9) Uani 1 1 d . . .
N3 N 0.8148(3) 0.4573(2) 0.5118(2) 0.0312(8) Uani 1 1 d . . .
C4 C 0.8465(5) 0.5763(3) 0.8097(3) 0.0463(12) Uani 1 1 d . . .
H4A H 0.7817 0.5607 0.8412 0.069 Uiso 1 1 calc R . .
H4B H 0.8403 0.6357 0.7924 0.069 Uiso 1 1 calc R . .
H4C H 0.9219 0.5658 0.8552 0.069 Uiso 1 1 calc R . .
C5 C 0.7854(5) 0.6008(3) 0.4502(3) 0.0470(12) Uani 1 1 d . . .
H5A H 0.8478 0.5968 0.4127 0.071 Uiso 1 1 calc R . .
H5B H 0.7848 0.6571 0.4776 0.071 Uiso 1 1 calc R . .
H5C H 0.7090 0.5893 0.4066 0.071 Uiso 1 1 calc R . .
C6 C 0.8581(4) 0.4023(3) 0.8192(3) 0.0323(10) Uani 1 1 d . . .
C7 C 0.9713(4) 0.3832(3) 0.8737(3) 0.0365(10) Uani 1 1 d . . .
C8 C 0.9806(5) 0.3358(3) 0.9593(3) 0.0404(11) Uani 1 1 d . . .
H8A H 1.0563 0.3214 0.9966 0.048 Uiso 1 1 calc R . .
C9 C 0.8813(5) 0.3096(3) 0.9904(3) 0.0445(12) Uani 1 1 d . . .
H9A H 0.8892 0.2778 1.0491 0.053 Uiso 1 1 calc R . .
C10 C 0.7692(5) 0.3296(3) 0.9359(3) 0.0454(12) Uani 1 1 d . . .
H10A H 0.7013 0.3111 0.9577 0.054 Uiso 1 1 calc R . .
C11 C 0.7560(4) 0.3765(3) 0.8499(3) 0.0375(10) Uani 1 1 d . . .
C12 C 1.0832(5) 0.4112(3) 0.8423(3) 0.0449(12) Uani 1 1 d . . .
H12A H 1.0597 0.4527 0.7880 0.054 Uiso 1 1 calc R . .
C13 C 1.1416(6) 0.3377(4) 0.8009(4) 0.0595(15) Uani 1 1 d . . .
H13A H 1.2130 0.3571 0.7808 0.089 Uiso 1 1 calc R . .
H13B H 1.0868 0.3145 0.7438 0.089 Uiso 1 1 calc R . .
H13C H 1.1625 0.2946 0.8516 0.089 Uiso 1 1 calc R . .
C14 C 1.1703(5) 0.4541(4) 0.9249(4) 0.0508(13) Uani 1 1 d . . .
H14A H 1.1316 0.5014 0.9496 0.076 Uiso 1 1 calc R . .
H14B H 1.2379 0.4742 0.8997 0.076 Uiso 1 1 calc R . .
H14C H 1.1974 0.4144 0.9784 0.076 Uiso 1 1 calc R . .
C15 C 0.6330(5) 0.3977(3) 0.7915(4) 0.0479(13) Uani 1 1 d . . .
H15A H 0.6421 0.4395 0.7402 0.057 Uiso 1 1 calc R . .
C16 C 0.5572(6) 0.4373(5) 0.8554(5) 0.075(2) Uani 1 1 d . . .
H16A H 0.5975 0.4866 0.8885 0.113 Uiso 1 1 calc R . .
H16B H 0.5439 0.3970 0.9049 0.113 Uiso 1 1 calc R . .
H16C H 0.4814 0.4541 0.8143 0.113 Uiso 1 1 calc R . .
C17 C 0.5748(6) 0.3212(5) 0.7387(6) 0.088(2) Uani 1 1 d . . .
H17A H 0.6254 0.2977 0.6974 0.131 Uiso 1 1 calc R . .
H17B H 0.4986 0.3367 0.6973 0.131 Uiso 1 1 calc R . .
H17C H 0.5627 0.2795 0.7872 0.131 Uiso 1 1 calc R . .
C18 C 0.7853(4) 0.4304(3) 0.4119(3) 0.0301(9) Uani 1 1 d . . .
C19 C 0.6683(4) 0.4146(3) 0.3676(3) 0.0385(11) Uani 1 1 d . . .
C20 C 0.6388(5) 0.3838(3) 0.2715(4) 0.0498(13) Uani 1 1 d . . .
H20A H 0.5587 0.3743 0.2407 0.060 Uiso 1 1 calc R . .
C21 C 0.7277(5) 0.3674(4) 0.2215(3) 0.0535(13) Uani 1 1 d . . .
H21A H 0.7081 0.3461 0.1563 0.064 Uiso 1 1 calc R . .
C22 C 0.8428(5) 0.3814(4) 0.2648(4) 0.0576(15) Uani 1 1 d . . .
H22A H 0.9029 0.3700 0.2297 0.069 Uiso 1 1 calc R . .
C23 C 0.8722(5) 0.4123(3) 0.3600(4) 0.0457(12) Uani 1 1 d . . .
H23A H 0.9526 0.4213 0.3901 0.055 Uiso 1 1 calc R . .
O24 O 0.5899(3) 0.4315(3) 0.4249(3) 0.0707(13) Uani 1 1 d . . .
C25 C 0.4720(5) 0.4073(5) 0.3923(5) 0.074(2) Uani 1 1 d . . .
H25A H 0.4266 0.4239 0.4410 0.111 Uiso 1 1 calc R . .
H25B H 0.4679 0.3466 0.3837 0.111 Uiso 1 1 calc R . .
H25C H 0.4393 0.4345 0.3293 0.111 Uiso 1 1 calc R . .
C26 C 0.8500(5) 0.2480(3) 0.6010(4) 0.0502(13) Uani 1 1 d . . .
H26A H 0.8763 0.2251 0.6682 0.060 Uiso 1 1 calc R . .
H26B H 0.7703 0.2254 0.5740 0.060 Uiso 1 1 calc R . .
C27 C 0.9333(6) 0.2159(4) 0.5375(4) 0.0649(16) Uani 1 1 d . . .
H27A H 0.9326 0.1548 0.5371 0.097 Uiso 1 1 calc R . .
H27B H 1.0134 0.2358 0.5647 0.097 Uiso 1 1 calc R . .
H27C H 0.9073 0.2367 0.4701 0.097 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.0425(3) 0.0322(2) 0.0278(2) -0.0003(3) 0.00539(18) 0.0010(3)
C1 0.029(2) 0.030(2) 0.033(2) -0.0026(17) 0.0076(18) -0.0018(18)
N1 0.039(2) 0.033(2) 0.0244(17) 0.0018(14) 0.0077(15) -0.0027(17)
C2 0.025(2) 0.031(2) 0.038(2) 0.0036(17) 0.0073(18) -0.0002(19)
C3 0.023(2) 0.038(2) 0.031(2) 0.0039(18) 0.0097(17) 0.0016(19)
N3 0.0234(19) 0.042(2) 0.0276(17) 0.0027(15) 0.0047(14) 0.0009(17)
C4 0.065(4) 0.041(3) 0.035(2) 0.001(2) 0.013(2) -0.004(3)
C5 0.058(3) 0.046(3) 0.037(2) 0.011(2) 0.010(2) 0.001(2)
C6 0.046(3) 0.027(2) 0.0237(19) 0.0000(16) 0.0081(19) 0.000(2)
C7 0.049(3) 0.030(2) 0.031(2) -0.0011(17) 0.0082(19) -0.002(2)
C8 0.049(3) 0.039(2) 0.030(2) 0.0005(18) 0.003(2) -0.002(2)
C9 0.068(4) 0.038(2) 0.029(2) 0.0062(19) 0.015(2) -0.005(3)
C10 0.066(4) 0.040(3) 0.035(2) 0.001(2) 0.023(2) -0.009(3)
C11 0.047(3) 0.033(2) 0.035(2) -0.003(2) 0.0117(19) -0.004(2)
C12 0.050(3) 0.050(3) 0.035(2) 0.011(2) 0.011(2) -0.002(3)
C13 0.058(4) 0.074(4) 0.051(3) -0.010(3) 0.021(3) -0.004(3)
C14 0.051(3) 0.053(3) 0.048(3) 0.001(2) 0.010(3) -0.005(3)
C15 0.045(3) 0.047(3) 0.052(3) 0.010(2) 0.013(2) 0.003(2)
C16 0.061(4) 0.081(5) 0.092(5) 0.019(4) 0.036(4) 0.022(4)
C17 0.061(4) 0.077(5) 0.109(6) -0.016(4) -0.017(4) -0.004(4)
C18 0.028(2) 0.037(2) 0.0262(19) 0.0032(17) 0.0073(17) 0.0010(19)
C19 0.028(2) 0.044(3) 0.043(3) 0.001(2) 0.005(2) 0.001(2)
C20 0.046(3) 0.053(3) 0.043(3) -0.006(2) -0.006(2) -0.008(3)
C21 0.076(4) 0.055(3) 0.030(2) -0.008(2) 0.010(2) -0.015(3)
C22 0.057(3) 0.080(4) 0.043(3) -0.013(3) 0.029(2) -0.007(3)
C23 0.036(3) 0.061(3) 0.042(3) 0.000(2) 0.012(2) -0.006(2)
O24 0.0265(19) 0.110(4) 0.078(3) -0.032(3) 0.0158(19) -0.002(2)
C25 0.032(3) 0.105(5) 0.084(5) 0.007(4) 0.010(3) -0.009(3)
C26 0.058(3) 0.040(2) 0.050(3) 0.000(2) 0.005(2) 0.001(3)
C27 0.081(5) 0.057(3) 0.059(3) -0.010(3) 0.022(3) 0.009(3)

_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
Zn C26 1.951(5) . ?
Zn N3 1.954(4) . ?
Zn N1 1.959(4) . ?
C1 N1 1.328(6) . ?
C1 C2 1.408(6) . ?
C1 C4 1.511(6) . ?
N1 C6 1.441(5) . ?
C2 C3 1.396(6) . ?
C3 N3 1.332(6) . ?
C3 C5 1.507(6) . ?
N3 C18 1.425(5) . ?
C6 C7 1.405(7) . ?
C6 C11 1.406(7) . ?
C7 C8 1.396(6) . ?
C7 C12 1.523(7) . ?
C8 C9 1.380(7) . ?
C9 C10 1.398(8) . ?
C10 C11 1.393(6) . ?
C11 C15 1.524(7) . ?
C12 C14 1.524(7) . ?
C12 C13 1.531(8) . ?
C15 C17 1.513(8) . ?
C15 C16 1.517(8) . ?
C18 C23 1.390(7) . ?
C18 C19 1.391(7) . ?
C19 O24 1.359(6) . ?
C19 C20 1.397(7) . ?
C20 C21 1.387(8) . ?
C21 C22 1.363(8) . ?
C22 C23 1.387(7) . ?
O24 C25 1.402(7) . ?
C26 C27 1.531(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
C26 Zn N3 132.15(19) . . ?
C26 Zn N1 131.44(19) . . ?
N3 Zn N1 96.40(15) . . ?
N1 C1 C2 124.5(4) . . ?
N1 C1 C4 119.1(4) . . ?
C2 C1 C4 116.4(4) . . ?
C1 N1 C6 120.4(4) . . ?
C1 N1 Zn 123.0(3) . . ?
C6 N1 Zn 116.5(3) . . ?
C3 C2 C1 128.4(4) . . ?
N3 C3 C2 123.9(4) . . ?
N3 C3 C5 119.3(4) . . ?
C2 C3 C5 116.8(4) . . ?
C3 N3 C18 119.7(3) . . ?
C3 N3 Zn 123.7(3) . . ?
C18 N3 Zn 115.9(3) . . ?
C7 C6 C11 121.7(4) . . ?
C7 C6 N1 118.8(4) . . ?
C11 C6 N1 119.3(4) . . ?
C8 C7 C6 118.2(5) . . ?
C8 C7 C12 119.2(4) . . ?
C6 C7 C12 122.6(4) . . ?
C9 C8 C7 121.0(5) . . ?
C8 C9 C10 120.3(4) . . ?
C11 C10 C9 120.6(5) . . ?
C10 C11 C6 118.3(5) . . ?
C10 C11 C15 119.9(5) . . ?
C6 C11 C15 121.9(4) . . ?
C7 C12 C14 112.8(4) . . ?
C7 C12 C13 110.8(4) . . ?
C14 C12 C13 110.7(5) . . ?
C17 C15 C16 111.6(6) . . ?
C17 C15 C11 110.4(5) . . ?
C16 C15 C11 112.0(5) . . ?
C23 C18 C19 118.8(4) . . ?
C23 C18 N3 121.3(4) . . ?
C19 C18 N3 119.7(4) . . ?
O24 C19 C18 114.7(4) . . ?
O24 C19 C20 124.9(5) . . ?
C18 C19 C20 120.4(5) . . ?
C21 C20 C19 119.3(5) . . ?
C22 C21 C20 120.8(4) . . ?
C21 C22 C23 120.0(5) . . ?
C22 C23 C18 120.8(5) . . ?
C19 O24 C25 119.0(5) . . ?
C27 C26 Zn 116.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.929
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.067

#===END