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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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data_compound1
_database_code_depnum_ccdc_archive 'CCDC 774446'
#TrackingRef '- compound1_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H40 Al3 N3 O, 0.5(C7 H8)'
_chemical_formula_sum            'C25.50 H44 Al3 N3 O'
_chemical_formula_weight         489.58

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.5821(2)
_cell_length_b                   11.2748(3)
_cell_length_c                   14.2400(4)
_cell_angle_alpha                76.4660(13)
_cell_angle_beta                 72.5621(15)
_cell_angle_gamma                68.4506(14)
_cell_volume                     1492.83(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    38586
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             530
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51015
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6827
_reflns_number_gt                4888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_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^)+(0.0587P)^2^+0.2073P] 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         6827
_refine_ls_number_parameters     302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1181
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.94585(5) 0.75222(5) 0.17572(4) 0.02913(13) Uani 1 1 d . . .
Al2 Al 0.91973(5) 0.91880(5) 0.35053(4) 0.03154(14) Uani 1 1 d . . .
Al3 Al 0.39877(5) 1.22371(5) 0.18701(4) 0.03038(14) Uani 1 1 d . . .
O1 O 0.85899(10) 0.81469(10) 0.29522(8) 0.0252(2) Uani 1 1 d . . .
N2 N 0.90430(13) 0.58716(13) 0.19753(10) 0.0276(3) Uani 1 1 d . . .
N1 N 0.74873(13) 0.75371(12) 0.34064(9) 0.0245(3) Uani 1 1 d . . .
N3 N 0.43118(13) 1.03459(13) 0.18069(10) 0.0280(3) Uani 1 1 d . . .
C1 C 0.80042(16) 0.64712(15) 0.41495(11) 0.0270(3) Uani 1 1 d . . .
H1A H 0.7266 0.6073 0.4501 0.032 Uiso 1 1 calc R . .
H1B H 0.8222 0.6805 0.4646 0.032 Uiso 1 1 calc R . .
C2 C 0.93143(16) 0.54518(15) 0.36724(12) 0.0281(4) Uani 1 1 d . . .
H2A H 1.0101 0.5806 0.3426 0.034 Uiso 1 1 calc R . .
H2B H 0.9568 0.4696 0.4179 0.034 Uiso 1 1 calc R . .
C3 C 0.90895(16) 0.50340(15) 0.28252(12) 0.0270(3) Uani 1 1 d . . .
C4 C 0.88516(17) 0.38747(16) 0.29225(13) 0.0331(4) Uani 1 1 d . . .
H4 H 0.8897 0.3289 0.3521 0.040 Uiso 1 1 calc R . .
C5 C 0.85483(18) 0.35773(17) 0.21446(15) 0.0387(4) Uani 1 1 d . . .
H5 H 0.8380 0.2788 0.2205 0.046 Uiso 1 1 calc R . .
C6 C 0.84925(18) 0.44332(17) 0.12814(14) 0.0386(4) Uani 1 1 d . . .
H6 H 0.8280 0.4249 0.0739 0.046 Uiso 1 1 calc R . .
C7 C 0.87511(18) 0.55630(17) 0.12210(13) 0.0343(4) Uani 1 1 d . . .
H7 H 0.8723 0.6151 0.0623 0.041 Uiso 1 1 calc R . .
C8 C 0.62002(16) 0.84941(15) 0.38484(12) 0.0281(4) Uani 1 1 d . . .
H8A H 0.6384 0.8837 0.4356 0.034 Uiso 1 1 calc R . .
H8B H 0.5481 0.8070 0.4188 0.034 Uiso 1 1 calc R . .
C9 C 0.56345(17) 0.96081(16) 0.30840(13) 0.0309(4) Uani 1 1 d . . .
H9A H 0.4909 1.0305 0.3445 0.037 Uiso 1 1 calc R . .
H9B H 0.6405 0.9946 0.2688 0.037 Uiso 1 1 calc R . .
C10 C 0.50154(16) 0.93173(16) 0.23757(12) 0.0291(4) Uani 1 1 d . . .
C11 C 0.51570(18) 0.80772(17) 0.22792(14) 0.0366(4) Uani 1 1 d . . .
H11 H 0.5649 0.7364 0.2682 0.044 Uiso 1 1 calc R . .
C12 C 0.45853(18) 0.78735(18) 0.15994(14) 0.0392(4) Uani 1 1 d . . .
H12 H 0.4676 0.7025 0.1533 0.047 Uiso 1 1 calc R . .
C13 C 0.38855(19) 0.89173(18) 0.10227(14) 0.0388(4) Uani 1 1 d . . .
H13 H 0.3496 0.8803 0.0543 0.047 Uiso 1 1 calc R . .
C14 C 0.37569(17) 1.01242(18) 0.11480(13) 0.0337(4) Uani 1 1 d . . .
H14 H 0.3254 1.0842 0.0754 0.040 Uiso 1 1 calc R . .
C15 C 1.15031(19) 0.69226(19) 0.15496(16) 0.0455(5) Uani 1 1 d . . .
H15A H 1.1921 0.7273 0.0880 0.068 Uiso 1 1 calc R . .
H15B H 1.1852 0.5980 0.1623 0.068 Uiso 1 1 calc R . .
H15C H 1.1756 0.7217 0.2042 0.068 Uiso 1 1 calc R . .
C16 C 0.8564(2) 0.86432(18) 0.07066(13) 0.0421(4) Uani 1 1 d . . .
H16A H 0.7591 0.8660 0.0863 0.063 Uiso 1 1 calc R . .
H16B H 0.9066 0.8315 0.0072 0.063 Uiso 1 1 calc R . .
H16C H 0.8587 0.9517 0.0658 0.063 Uiso 1 1 calc R . .
C17 C 1.0450(3) 0.7982(2) 0.4334(2) 0.0663(7) Uani 1 1 d . . .
H17A H 0.9894 0.7663 0.4960 0.099 Uiso 1 1 calc R . .
H17B H 1.1000 0.8425 0.4475 0.099 Uiso 1 1 calc R . .
H17C H 1.1081 0.7255 0.3980 0.099 Uiso 1 1 calc R . .
C18 C 0.7625(2) 1.0449(2) 0.42814(15) 0.0488(5) Uani 1 1 d . . .
H18A H 0.7254 1.0005 0.4926 0.073 Uiso 1 1 calc R . .
H18B H 0.6887 1.0864 0.3917 0.073 Uiso 1 1 calc R . .
H18C H 0.7955 1.1103 0.4387 0.073 Uiso 1 1 calc R . .
C19 C 1.0053(2) 1.00758(19) 0.22357(17) 0.0526(6) Uani 1 1 d . . .
H19A H 1.0431 1.0673 0.2375 0.079 Uiso 1 1 calc R . .
H19B H 0.9342 1.0556 0.1855 0.079 Uiso 1 1 calc R . .
H19C H 1.0810 0.9437 0.1849 0.079 Uiso 1 1 calc R . .
C20 C 0.5860(2) 1.24401(18) 0.15033(14) 0.0413(4) Uani 1 1 d . . .
H20A H 0.6496 1.1852 0.1027 0.062 Uiso 1 1 calc R . .
H20B H 0.6221 1.2239 0.2100 0.062 Uiso 1 1 calc R . .
H20C H 0.5792 1.3330 0.1200 0.062 Uiso 1 1 calc R . .
C21 C 0.2888(2) 1.25544(19) 0.32314(13) 0.0421(5) Uani 1 1 d . . .
H21A H 0.2332 1.3468 0.3225 0.063 Uiso 1 1 calc R . .
H21B H 0.3524 1.2323 0.3672 0.063 Uiso 1 1 calc R . .
H21C H 0.2264 1.2030 0.3473 0.063 Uiso 1 1 calc R . .
C22 C 0.2858(2) 1.31932(19) 0.08897(14) 0.0446(5) Uani 1 1 d . . .
H22A H 0.2708 1.4116 0.0831 0.067 Uiso 1 1 calc R . .
H22B H 0.1953 1.3041 0.1109 0.067 Uiso 1 1 calc R . .
H22C H 0.3352 1.2898 0.0242 0.067 Uiso 1 1 calc R . .
C23A C 0.5612(6) 0.3979(5) 0.4664(4) 0.035(2) Uiso 0.25 1 d PG A -1
H23A H 0.5981 0.3287 0.4283 0.042 Uiso 0.25 1 calc PR A -1
C24A C 0.6036(5) 0.3845(4) 0.5528(4) 0.045(2) Uiso 0.25 1 d PG A -1
H24A H 0.6694 0.3063 0.5737 0.054 Uiso 0.25 1 calc PR A -1
C25A C 0.5497(5) 0.4857(6) 0.6086(3) 0.0318(17) Uiso 0.25 1 d PG A -1
H25A H 0.5786 0.4766 0.6677 0.038 Uiso 0.25 1 calc PR A -1
C26A C 0.4533(7) 0.6002(5) 0.5780(4) 0.033(2) Uiso 0.25 1 d PG A -1
H26A H 0.4165 0.6694 0.6161 0.040 Uiso 0.25 1 calc PR A -1
C27A C 0.4110(7) 0.6135(5) 0.4916(4) 0.037(6) Uiso 0.25 1 d PG A -1
H27A H 0.3451 0.6918 0.4706 0.045 Uiso 0.25 1 calc PR A -1
C28A C 0.4649(6) 0.5124(6) 0.4358(3) 0.0409(18) Uiso 0.25 1 d PG A -1
C29A C 0.4151(11) 0.5269(11) 0.3463(7) 0.058(2) Uiso 0.25 1 d P A -1
H29A H 0.4631 0.4483 0.3150 0.087 Uiso 0.25 1 calc PR A -1
H29B H 0.4350 0.6003 0.2994 0.087 Uiso 0.25 1 calc PR A -1
H29C H 0.3141 0.5418 0.3650 0.087 Uiso 0.25 1 calc PR A -1
C23B C 0.5893(5) 0.3929(4) 0.5149(4) 0.016(3) Uiso 0.25 1 d PG B -2
H23B H 0.6395 0.3149 0.4874 0.020 Uiso 0.25 1 calc PR B -2
C24B C 0.6093(5) 0.4075(4) 0.6032(3) 0.0264(14) Uiso 0.25 1 d PG B -2
H24B H 0.6731 0.3394 0.6359 0.032 Uiso 0.25 1 calc PR B -2
C25B C 0.5359(6) 0.5215(5) 0.6435(3) 0.017(2) Uiso 0.25 1 d PG B -2
H25B H 0.5495 0.5315 0.7038 0.020 Uiso 0.25 1 calc PR B -2
C26B C 0.4425(6) 0.6211(4) 0.5956(4) 0.040(2) Uiso 0.25 1 d PG B -2
H26B H 0.3923 0.6990 0.6232 0.048 Uiso 0.25 1 calc PR B -2
C27B C 0.4226(6) 0.6065(4) 0.5073(4) 0.027(3) Uiso 0.25 1 d PG B -2
H27B H 0.3588 0.6745 0.4746 0.032 Uiso 0.25 1 calc PR B -2
C28B C 0.4960(5) 0.4924(5) 0.4670(3) 0.0285(15) Uiso 0.25 1 d PG B -2
C29B C 0.4831(12) 0.4628(11) 0.3717(8) 0.051(3) Uiso 0.25 1 d P B -2
H29D H 0.5455 0.3760 0.3597 0.076 Uiso 0.25 1 calc PR B -2
H29E H 0.5090 0.5256 0.3156 0.076 Uiso 0.25 1 calc PR B -2
H29F H 0.3863 0.4679 0.3785 0.076 Uiso 0.25 1 calc PR B -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
Al1 0.0335(3) 0.0296(3) 0.0249(3) -0.0032(2) -0.0047(2) -0.0128(2)
Al2 0.0322(3) 0.0295(3) 0.0383(3) -0.0046(2) -0.0138(2) -0.0117(2)
Al3 0.0332(3) 0.0301(3) 0.0275(3) -0.0066(2) -0.0113(2) -0.0049(2)
O1 0.0247(5) 0.0279(6) 0.0254(6) -0.0021(5) -0.0054(4) -0.0125(5)
N2 0.0274(7) 0.0281(7) 0.0280(7) -0.0061(6) -0.0089(6) -0.0063(6)
N1 0.0224(6) 0.0256(7) 0.0262(7) -0.0012(5) -0.0050(5) -0.0107(5)
N3 0.0238(7) 0.0342(8) 0.0269(7) -0.0071(6) -0.0054(5) -0.0092(6)
C1 0.0297(8) 0.0260(8) 0.0246(8) -0.0005(7) -0.0076(7) -0.0091(7)
C2 0.0297(8) 0.0254(8) 0.0295(9) -0.0003(7) -0.0117(7) -0.0074(7)
C3 0.0225(8) 0.0252(8) 0.0315(9) -0.0046(7) -0.0078(6) -0.0043(6)
C4 0.0316(9) 0.0271(9) 0.0414(10) -0.0020(8) -0.0132(8) -0.0083(7)
C5 0.0364(10) 0.0288(9) 0.0566(12) -0.0111(9) -0.0164(9) -0.0095(8)
C6 0.0406(10) 0.0360(10) 0.0459(11) -0.0156(9) -0.0183(8) -0.0074(8)
C7 0.0363(9) 0.0361(10) 0.0322(9) -0.0075(8) -0.0122(8) -0.0086(8)
C8 0.0255(8) 0.0282(8) 0.0306(9) -0.0058(7) -0.0064(7) -0.0077(7)
C9 0.0288(8) 0.0258(8) 0.0404(10) -0.0071(7) -0.0158(7) -0.0038(7)
C10 0.0221(8) 0.0305(9) 0.0353(9) -0.0068(7) -0.0067(7) -0.0079(7)
C11 0.0323(9) 0.0341(10) 0.0492(11) -0.0081(8) -0.0150(8) -0.0115(8)
C12 0.0372(10) 0.0388(10) 0.0502(11) -0.0124(9) -0.0112(8) -0.0177(8)
C13 0.0401(10) 0.0491(11) 0.0385(10) -0.0104(9) -0.0117(8) -0.0224(9)
C14 0.0328(9) 0.0411(10) 0.0315(9) -0.0049(8) -0.0114(7) -0.0138(8)
C15 0.0391(10) 0.0436(11) 0.0541(12) -0.0176(9) 0.0051(9) -0.0200(9)
C16 0.0611(12) 0.0390(10) 0.0275(10) 0.0006(8) -0.0121(9) -0.0196(9)
C17 0.0756(16) 0.0512(13) 0.0972(19) 0.0007(13) -0.0635(15) -0.0214(12)
C18 0.0527(12) 0.0578(13) 0.0481(12) -0.0255(10) -0.0072(9) -0.0243(10)
C19 0.0519(12) 0.0320(10) 0.0686(15) -0.0133(10) 0.0063(10) -0.0199(9)
C20 0.0489(11) 0.0381(10) 0.0415(11) -0.0049(8) -0.0119(9) -0.0185(9)
C21 0.0426(11) 0.0435(11) 0.0345(10) -0.0126(9) -0.0111(8) -0.0012(9)
C22 0.0535(12) 0.0385(11) 0.0388(11) -0.0102(9) -0.0221(9) 0.0005(9)

_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
Al1 O1 1.8397(11) . ?
Al1 C16 1.9535(18) . ?
Al1 C15 1.9650(19) . ?
Al1 N2 2.0004(14) . ?
Al2 O1 1.9240(11) . ?
Al2 C17 1.965(2) . ?
Al2 C18 1.976(2) . ?
Al2 C19 1.982(2) . ?
Al3 C22 1.9722(18) . ?
Al3 C21 1.9765(18) . ?
Al3 C20 1.9772(19) . ?
Al3 N3 2.0510(14) . ?
O1 N1 1.4769(15) . ?
N2 C7 1.350(2) . ?
N2 C3 1.351(2) . ?
N1 C1 1.460(2) . ?
N1 C8 1.463(2) . ?
N3 C14 1.355(2) . ?
N3 C10 1.357(2) . ?
C1 C2 1.528(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.501(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.388(2) . ?
C4 C5 1.382(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.376(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.523(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.504(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.386(2) . ?
C11 C12 1.383(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.371(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.366(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A C24A 1.3900 . ?
C23A C28A 1.3900 . ?
C23A H23A 0.9500 . ?
C24A C25A 1.3900 . ?
C24A H24A 0.9500 . ?
C25A C26A 1.3900 . ?
C25A H25A 0.9500 . ?
C26A C27A 1.3900 . ?
C26A H26A 0.9500 . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A C29A 1.473(11) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C23B C24B 1.3900 . ?
C23B C28B 1.3900 . ?
C23B H23B 0.9500 . ?
C24B C25B 1.3900 . ?
C24B H24B 0.9500 . ?
C25B C26B 1.3900 . ?
C25B H25B 0.9500 . ?
C26B C27B 1.3900 . ?
C26B H26B 0.9500 . ?
C27B C28B 1.3900 . ?
C27B H27B 0.9500 . ?
C28B C29B 1.526(11) . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?

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
O1 Al1 C16 110.71(7) . . ?
O1 Al1 C15 111.30(7) . . ?
C16 Al1 C15 120.66(9) . . ?
O1 Al1 N2 103.56(5) . . ?
C16 Al1 N2 106.43(7) . . ?
C15 Al1 N2 102.26(7) . . ?
O1 Al2 C17 106.10(7) . . ?
O1 Al2 C18 112.81(7) . . ?
C17 Al2 C18 111.45(11) . . ?
O1 Al2 C19 97.74(7) . . ?
C17 Al2 C19 117.61(11) . . ?
C18 Al2 C19 110.35(9) . . ?
C22 Al3 C21 110.78(8) . . ?
C22 Al3 C20 113.54(9) . . ?
C21 Al3 C20 115.46(8) . . ?
C22 Al3 N3 103.56(7) . . ?
C21 Al3 N3 106.10(7) . . ?
C20 Al3 N3 106.27(7) . . ?
N1 O1 Al1 104.47(8) . . ?
N1 O1 Al2 129.64(8) . . ?
Al1 O1 Al2 125.47(6) . . ?
C7 N2 C3 118.65(14) . . ?
C7 N2 Al1 118.10(12) . . ?
C3 N2 Al1 123.20(11) . . ?
C1 N1 C8 111.89(12) . . ?
C1 N1 O1 107.08(11) . . ?
C8 N1 O1 109.30(11) . . ?
C14 N3 C10 118.23(14) . . ?
C14 N3 Al3 116.44(11) . . ?
C10 N3 Al3 125.32(11) . . ?
N1 C1 C2 111.36(13) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C1 111.44(13) . . ?
C3 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 120.91(15) . . ?
N2 C3 C2 117.08(14) . . ?
C4 C3 C2 121.89(15) . . ?
C5 C4 C3 119.66(16) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 119.46(16) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 118.48(16) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
N2 C7 C6 122.84(17) . . ?
N2 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N1 C8 C9 112.75(13) . . ?
N1 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 116.71(14) . . ?
C10 C9 H9A 108.1 . . ?
C8 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
C8 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
N3 C10 C11 120.46(15) . . ?
N3 C10 C9 116.39(14) . . ?
C11 C10 C9 123.14(15) . . ?
C12 C11 C10 120.31(17) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 118.85(17) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C14 C13 C12 119.01(16) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
N3 C14 C13 123.13(17) . . ?
N3 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
Al1 C15 H15A 109.5 . . ?
Al1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Al1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Al1 C16 H16A 109.5 . . ?
Al1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Al1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Al2 C17 H17A 109.5 . . ?
Al2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Al2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Al2 C18 H18A 109.5 . . ?
Al2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Al2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Al2 C19 H19A 109.5 . . ?
Al2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Al2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Al3 C20 H20A 109.5 . . ?
Al3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Al3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Al3 C21 H21A 109.5 . . ?
Al3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Al3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Al3 C22 H22A 109.5 . . ?
Al3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Al3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24A C23A C28A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C28A C23A H23A 120.0 . . ?
C23A C24A C25A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C28A C27A C26A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C27A C28A C23A 120.0 . . ?
C27A C28A C29A 119.1(6) . . ?
C23A C28A C29A 120.8(6) . . ?
C28A C29A H29A 109.5 . . ?
C28A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C28A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C24B C23B C28B 120.0 . . ?
C24B C23B H23B 120.0 . . ?
C28B C23B H23B 120.0 . . ?
C25B C24B C23B 120.0 . . ?
C25B C24B H24B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C24B C25B C26B 120.0 . . ?
C24B C25B H25B 120.0 . . ?
C26B C25B H25B 120.0 . . ?
C27B C26B C25B 120.0 . . ?
C27B C26B H26B 120.0 . . ?
C25B C26B H26B 120.0 . . ?
C26B C27B C28B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C28B C27B H27B 120.0 . . ?
C27B C28B C23B 120.0 . . ?
C27B C28B C29B 125.5(6) . . ?
C23B C28B C29B 114.5(6) . . ?
C28B C29B H29D 109.5 . . ?
C28B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.046


data_compound2
_database_code_depnum_ccdc_archive 'CCDC 774447'
#TrackingRef '- compound1_3.cif'



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H40 Ga3 N3 O, 0.5 (C7 H8)'
_chemical_formula_sum            'C25.50 H44 Ga3 N3 O'
_chemical_formula_weight         617.80

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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.62000(10)
_cell_length_b                   11.34720(10)
_cell_length_c                   14.2438(2)
_cell_angle_alpha                75.9478(7)
_cell_angle_beta                 72.4010(7)
_cell_angle_gamma                68.0061(8)
_cell_volume                     1500.68(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    39482
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      30.034

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             638
_exptl_absorpt_coefficient_mu    2.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4987
_exptl_absorpt_correction_T_max  0.7042
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            60220
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         30.00
_reflns_number_total             8716
_reflns_number_gt                7334
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_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^)+(0.0361P)^2^+0.3934P] 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         8716
_refine_ls_number_parameters     302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0727
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.961080(19) 0.748496(17) 0.168801(12) 0.02274(5) Uani 1 1 d . . .
Ga2 Ga 0.92497(2) 0.926591(18) 0.350024(14) 0.02651(5) Uani 1 1 d . . .
Ga3 Ga 0.396821(19) 1.230907(17) 0.186186(12) 0.02380(5) Uani 1 1 d . . .
O1 O 0.86074(11) 0.81298(10) 0.29359(8) 0.0198(2) Uani 1 1 d . . .
N2 N 0.91075(14) 0.58129(12) 0.19755(9) 0.0218(3) Uani 1 1 d . . .
N1 N 0.75256(13) 0.75268(12) 0.33971(9) 0.0196(2) Uani 1 1 d . . .
N3 N 0.43324(14) 1.03367(13) 0.18003(10) 0.0225(3) Uani 1 1 d . . .
C1 C 0.80416(17) 0.64760(14) 0.41572(11) 0.0220(3) Uani 1 1 d . . .
H1A H 0.7303 0.6088 0.4523 0.026 Uiso 1 1 calc R . .
H1B H 0.8268 0.6817 0.4640 0.026 Uiso 1 1 calc R . .
C2 C 0.93493(17) 0.54422(15) 0.36852(11) 0.0220(3) Uani 1 1 d . . .
H2A H 1.0137 0.5789 0.3422 0.026 Uiso 1 1 calc R . .
H2B H 0.9608 0.4694 0.4200 0.026 Uiso 1 1 calc R . .
C3 C 0.91052(15) 0.50155(14) 0.28555(11) 0.0208(3) Uani 1 1 d . . .
C4 C 0.88095(18) 0.38845(16) 0.29899(13) 0.0274(3) Uani 1 1 d . . .
H4 H 0.8822 0.3326 0.3606 0.033 Uiso 1 1 calc R . .
C5 C 0.84961(19) 0.35722(17) 0.22245(14) 0.0328(4) Uani 1 1 d . . .
H5 H 0.8292 0.2800 0.2311 0.039 Uiso 1 1 calc R . .
C6 C 0.8484(2) 0.43951(18) 0.13342(14) 0.0329(4) Uani 1 1 d . . .
H6 H 0.8262 0.4206 0.0802 0.040 Uiso 1 1 calc R . .
C7 C 0.88025(18) 0.55020(16) 0.12348(12) 0.0275(3) Uani 1 1 d . . .
H7 H 0.8806 0.6065 0.0620 0.033 Uiso 1 1 calc R . .
C8 C 0.62397(16) 0.84927(15) 0.38392(12) 0.0235(3) Uani 1 1 d . . .
H8A H 0.6428 0.8833 0.4342 0.028 Uiso 1 1 calc R . .
H8B H 0.5518 0.8078 0.4184 0.028 Uiso 1 1 calc R . .
C9 C 0.56816(18) 0.96031(15) 0.30632(13) 0.0259(3) Uani 1 1 d . . .
H9A H 0.4960 1.0305 0.3417 0.031 Uiso 1 1 calc R . .
H9B H 0.6456 0.9929 0.2663 0.031 Uiso 1 1 calc R . .
C10 C 0.50582(16) 0.93164(16) 0.23583(12) 0.0242(3) Uani 1 1 d . . .
C11 C 0.52245(19) 0.80697(17) 0.22621(14) 0.0315(4) Uani 1 1 d . . .
H11 H 0.5736 0.7357 0.2659 0.038 Uiso 1 1 calc R . .
C12 C 0.46457(19) 0.78687(18) 0.15902(15) 0.0340(4) Uani 1 1 d . . .
H12 H 0.4755 0.7021 0.1522 0.041 Uiso 1 1 calc R . .
C13 C 0.39092(19) 0.89131(18) 0.10204(13) 0.0318(4) Uani 1 1 d . . .
H13 H 0.3508 0.8800 0.0550 0.038 Uiso 1 1 calc R . .
C14 C 0.37670(18) 1.01261(17) 0.11486(12) 0.0279(3) Uani 1 1 d . . .
H14 H 0.3249 1.0847 0.0762 0.034 Uiso 1 1 calc R . .
C15 C 1.16391(18) 0.68379(18) 0.15941(15) 0.0348(4) Uani 1 1 d . . .
H15A H 1.2133 0.7068 0.0911 0.052 Uiso 1 1 calc R . .
H15B H 1.1946 0.5901 0.1774 0.052 Uiso 1 1 calc R . .
H15C H 1.1847 0.7223 0.2051 0.052 Uiso 1 1 calc R . .
C16 C 0.8666(2) 0.86022(18) 0.06459(13) 0.0359(4) Uani 1 1 d . . .
H16A H 0.7704 0.8593 0.0813 0.054 Uiso 1 1 calc R . .
H16B H 0.9166 0.8290 0.0006 0.054 Uiso 1 1 calc R . .
H16C H 0.8656 0.9482 0.0598 0.054 Uiso 1 1 calc R . .
C17 C 1.0517(3) 0.8005(2) 0.4319(2) 0.0633(8) Uani 1 1 d . . .
H17A H 0.9966 0.7757 0.4975 0.095 Uiso 1 1 calc R . .
H17B H 1.1158 0.8391 0.4397 0.095 Uiso 1 1 calc R . .
H17C H 1.1055 0.7242 0.3989 0.095 Uiso 1 1 calc R . .
C18 C 0.7608(2) 1.0517(2) 0.42683(16) 0.0441(5) Uani 1 1 d . . .
H18A H 0.7269 1.0076 0.4926 0.066 Uiso 1 1 calc R . .
H18B H 0.6862 1.0878 0.3908 0.066 Uiso 1 1 calc R . .
H18C H 0.7889 1.1211 0.4348 0.066 Uiso 1 1 calc R . .
C19 C 1.0048(2) 1.01085(18) 0.21744(15) 0.0385(4) Uani 1 1 d . . .
H19A H 1.0476 1.0691 0.2263 0.058 Uiso 1 1 calc R . .
H19B H 0.9302 1.0598 0.1823 0.058 Uiso 1 1 calc R . .
H19C H 1.0758 0.9452 0.1784 0.058 Uiso 1 1 calc R . .
C20 C 0.5868(2) 1.24631(19) 0.14667(14) 0.0358(4) Uani 1 1 d . . .
H20A H 0.6487 1.1853 0.1007 0.054 Uiso 1 1 calc R . .
H20B H 0.6235 1.2273 0.2060 0.054 Uiso 1 1 calc R . .
H20C H 0.5820 1.3339 0.1138 0.054 Uiso 1 1 calc R . .
C21 C 0.2878(2) 1.25473(19) 0.32478(13) 0.0358(4) Uani 1 1 d . . .
H21A H 0.2269 1.3443 0.3261 0.054 Uiso 1 1 calc R . .
H21B H 0.3521 1.2338 0.3679 0.054 Uiso 1 1 calc R . .
H21C H 0.2307 1.1979 0.3487 0.054 Uiso 1 1 calc R . .
C22 C 0.2802(2) 1.32266(19) 0.08744(14) 0.0376(4) Uani 1 1 d . . .
H22A H 0.2605 1.4154 0.0812 0.056 Uiso 1 1 calc R . .
H22B H 0.1922 1.3036 0.1099 0.056 Uiso 1 1 calc R . .
H22C H 0.3307 1.2941 0.0226 0.056 Uiso 1 1 calc R . .
C23A C 0.5626(7) 0.3933(5) 0.4778(5) 0.046(3) Uiso 0.25 1 d PG A -1
H23A H 0.5991 0.3206 0.4441 0.055 Uiso 0.25 1 calc PR A -1
C24A C 0.5996(7) 0.3857(5) 0.5653(5) 0.049(2) Uiso 0.25 1 d PG A -1
H24A H 0.6614 0.3077 0.5913 0.059 Uiso 0.25 1 calc PR A -1
C25A C 0.5463(7) 0.4920(7) 0.6148(4) 0.035(2) Uiso 0.25 1 d PG A -1
H25A H 0.5715 0.4868 0.6745 0.042 Uiso 0.25 1 calc PR A -1
C26A C 0.4559(8) 0.6060(5) 0.5767(5) 0.043(2) Uiso 0.25 1 d PG A -1
H26A H 0.4194 0.6787 0.6105 0.051 Uiso 0.25 1 calc PR A -1
C27A C 0.4189(7) 0.6136(5) 0.4893(5) 0.030(3) Uiso 0.25 1 d PG A -1
H27A H 0.3571 0.6915 0.4633 0.036 Uiso 0.25 1 calc PR A -1
C28A C 0.4723(7) 0.5073(6) 0.4398(4) 0.0395(18) Uiso 0.25 1 d PG A -1
C29A C 0.4255(13) 0.5235(13) 0.3533(8) 0.055(3) Uiso 0.25 1 d P A -1
H29A H 0.4730 0.4454 0.3220 0.083 Uiso 0.25 1 calc PR A -1
H29B H 0.4468 0.5964 0.3066 0.083 Uiso 0.25 1 calc PR A -1
H29C H 0.3244 0.5399 0.3713 0.083 Uiso 0.25 1 calc PR A -1
C23B C 0.5858(5) 0.3927(3) 0.5216(3) 0.016(2) Uiso 0.25 1 d PG B -2
H23B H 0.6323 0.3139 0.4955 0.020 Uiso 0.25 1 calc PR B -2
C24B C 0.6085(5) 0.4065(4) 0.6089(3) 0.0213(11) Uiso 0.25 1 d PG B -2
H24B H 0.6706 0.3370 0.6424 0.026 Uiso 0.25 1 calc PR B -2
C25B C 0.5405(6) 0.5219(5) 0.6470(3) 0.0222(17) Uiso 0.25 1 d PG B -2
H25B H 0.5560 0.5313 0.7067 0.027 Uiso 0.25 1 calc PR B -2
C26B C 0.4497(6) 0.6236(4) 0.5979(4) 0.0266(14) Uiso 0.25 1 d PG B -2
H26B H 0.4032 0.7024 0.6240 0.032 Uiso 0.25 1 calc PR B -2
C27B C 0.4269(5) 0.6098(4) 0.5107(4) 0.018(2) Uiso 0.25 1 d PG B -2
H27B H 0.3649 0.6792 0.4771 0.021 Uiso 0.25 1 calc PR B -2
C28B C 0.4950(5) 0.4944(4) 0.4725(3) 0.0189(11) Uiso 0.25 1 d PG B -2
C29B C 0.4786(10) 0.4671(10) 0.3726(7) 0.0361(19) Uiso 0.25 1 d P B -2
H29D H 0.5400 0.3804 0.3598 0.054 Uiso 0.25 1 calc PR B -2
H29E H 0.5043 0.5302 0.3167 0.054 Uiso 0.25 1 calc PR B -2
H29F H 0.3814 0.4738 0.3801 0.054 Uiso 0.25 1 calc PR B -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
Ga1 0.02715(10) 0.02321(9) 0.01843(8) -0.00187(6) -0.00411(7) -0.01053(7)
Ga2 0.03086(10) 0.02593(9) 0.02941(10) -0.00248(7) -0.01333(8) -0.01268(8)
Ga3 0.02666(10) 0.02382(9) 0.02068(8) -0.00535(6) -0.00872(7) -0.00418(7)
O1 0.0210(5) 0.0217(5) 0.0192(5) -0.0024(4) -0.0045(4) -0.0101(4)
N2 0.0234(7) 0.0214(6) 0.0215(6) -0.0031(5) -0.0077(5) -0.0063(5)
N1 0.0187(6) 0.0190(6) 0.0211(6) -0.0009(5) -0.0050(5) -0.0071(5)
N3 0.0190(6) 0.0271(7) 0.0228(6) -0.0062(5) -0.0050(5) -0.0075(5)
C1 0.0243(8) 0.0214(7) 0.0182(6) -0.0004(5) -0.0047(6) -0.0070(6)
C2 0.0237(8) 0.0212(7) 0.0213(7) -0.0009(5) -0.0098(6) -0.0055(6)
C3 0.0174(7) 0.0196(7) 0.0237(7) -0.0032(5) -0.0062(6) -0.0033(6)
C4 0.0281(8) 0.0213(7) 0.0326(8) -0.0006(6) -0.0112(7) -0.0067(6)
C5 0.0344(9) 0.0240(8) 0.0466(10) -0.0090(7) -0.0149(8) -0.0104(7)
C6 0.0371(10) 0.0314(9) 0.0384(9) -0.0114(7) -0.0180(8) -0.0090(8)
C7 0.0333(9) 0.0276(8) 0.0235(7) -0.0051(6) -0.0109(7) -0.0080(7)
C8 0.0196(7) 0.0231(7) 0.0278(7) -0.0060(6) -0.0068(6) -0.0045(6)
C9 0.0257(8) 0.0203(7) 0.0352(8) -0.0057(6) -0.0156(7) -0.0036(6)
C10 0.0185(7) 0.0261(8) 0.0299(8) -0.0079(6) -0.0072(6) -0.0060(6)
C11 0.0304(9) 0.0253(8) 0.0451(10) -0.0079(7) -0.0166(8) -0.0084(7)
C12 0.0334(10) 0.0309(9) 0.0469(10) -0.0121(8) -0.0128(8) -0.0139(8)
C13 0.0330(9) 0.0399(10) 0.0324(9) -0.0086(7) -0.0109(7) -0.0184(8)
C14 0.0280(8) 0.0338(9) 0.0264(8) -0.0055(7) -0.0097(7) -0.0116(7)
C15 0.0261(9) 0.0316(9) 0.0446(10) -0.0119(8) 0.0024(8) -0.0118(7)
C16 0.0529(12) 0.0322(9) 0.0229(8) 0.0039(7) -0.0136(8) -0.0154(9)
C17 0.0800(18) 0.0509(14) 0.0862(19) 0.0134(13) -0.0668(16) -0.0288(13)
C18 0.0490(12) 0.0518(12) 0.0422(11) -0.0272(10) 0.0009(9) -0.0248(10)
C19 0.0405(11) 0.0255(8) 0.0468(11) -0.0066(8) 0.0020(9) -0.0166(8)
C20 0.0415(11) 0.0359(10) 0.0360(9) -0.0053(8) -0.0084(8) -0.0197(8)
C21 0.0361(10) 0.0373(10) 0.0262(8) -0.0114(7) -0.0067(7) 0.0003(8)
C22 0.0479(12) 0.0316(9) 0.0321(9) -0.0081(7) -0.0237(9) 0.0019(8)

_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
Ga1 O1 1.9320(11) . ?
Ga1 C16 1.9624(17) . ?
Ga1 C15 1.9713(18) . ?
Ga1 N2 2.0744(13) . ?
Ga2 C17 1.978(2) . ?
Ga2 C19 1.9902(19) . ?
Ga2 C18 2.000(2) . ?
Ga2 O1 2.0656(10) . ?
Ga3 C20 1.9872(19) . ?
Ga3 C21 1.9882(18) . ?
Ga3 C22 1.9929(17) . ?
Ga3 N3 2.1431(14) . ?
O1 N1 1.4608(16) . ?
N2 C7 1.347(2) . ?
N2 C3 1.3560(19) . ?
N1 C1 1.4617(19) . ?
N1 C8 1.469(2) . ?
N3 C10 1.350(2) . ?
N3 C14 1.353(2) . ?
C1 C2 1.535(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.502(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.389(2) . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.523(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.508(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.394(2) . ?
C11 C12 1.383(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A C24A 1.3900 . ?
C23A C28A 1.3900 . ?
C23A H23A 0.9500 . ?
C24A C25A 1.3900 . ?
C24A H24A 0.9500 . ?
C25A C26A 1.3900 . ?
C25A H25A 0.9500 . ?
C26A C27A 1.3900 . ?
C26A H26A 0.9500 . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A C29A 1.410(12) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C23B C24B 1.3900 . ?
C23B C28B 1.3900 . ?
C23B H23B 0.9500 . ?
C24B C25B 1.3900 . ?
C24B H24B 0.9500 . ?
C25B C26B 1.3900 . ?
C25B H25B 0.9500 . ?
C26B C27B 1.3900 . ?
C26B H26B 0.9500 . ?
C27B C28B 1.3900 . ?
C27B H27B 0.9500 . ?
C28B C29B 1.598(11) . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?

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
O1 Ga1 C16 108.45(7) . . ?
O1 Ga1 C15 110.39(7) . . ?
C16 Ga1 C15 126.44(9) . . ?
O1 Ga1 N2 99.27(5) . . ?
C16 Ga1 N2 105.57(7) . . ?
C15 Ga1 N2 103.00(7) . . ?
C17 Ga2 C19 119.59(11) . . ?
C17 Ga2 C18 113.85(12) . . ?
C19 Ga2 C18 111.84(9) . . ?
C17 Ga2 O1 103.41(8) . . ?
C19 Ga2 O1 95.00(7) . . ?
C18 Ga2 O1 110.75(7) . . ?
C20 Ga3 C21 117.47(8) . . ?
C20 Ga3 C22 114.92(9) . . ?
C21 Ga3 C22 111.91(8) . . ?
C20 Ga3 N3 104.20(7) . . ?
C21 Ga3 N3 104.04(7) . . ?
C22 Ga3 N3 101.98(7) . . ?
N1 O1 Ga1 107.35(8) . . ?
N1 O1 Ga2 129.99(8) . . ?
Ga1 O1 Ga2 122.16(5) . . ?
C7 N2 C3 119.14(14) . . ?
C7 N2 Ga1 117.55(11) . . ?
C3 N2 Ga1 123.29(10) . . ?
O1 N1 C1 107.24(11) . . ?
O1 N1 C8 108.80(11) . . ?
C1 N1 C8 111.18(12) . . ?
C10 N3 C14 118.75(14) . . ?
C10 N3 Ga3 125.29(10) . . ?
C14 N3 Ga3 115.96(11) . . ?
N1 C1 C2 110.91(12) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C1 111.29(12) . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 120.57(14) . . ?
N2 C3 C2 117.46(13) . . ?
C4 C3 C2 121.87(14) . . ?
C5 C4 C3 119.92(16) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.26(16) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 118.51(15) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
N2 C7 C6 122.59(15) . . ?
N2 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
N1 C8 C9 112.29(13) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C8 116.73(13) . . ?
C10 C9 H9A 108.1 . . ?
C8 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
C8 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
N3 C10 C11 120.53(15) . . ?
N3 C10 C9 116.63(14) . . ?
C11 C10 C9 122.82(15) . . ?
C12 C11 C10 120.09(17) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 119.15(16) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 118.50(15) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
N3 C14 C13 122.97(16) . . ?
N3 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
Ga1 C15 H15A 109.5 . . ?
Ga1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Ga1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Ga1 C16 H16A 109.5 . . ?
Ga1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Ga1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Ga2 C17 H17A 109.5 . . ?
Ga2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Ga2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Ga2 C18 H18A 109.5 . . ?
Ga2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Ga2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Ga2 C19 H19A 109.5 . . ?
Ga2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Ga2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Ga3 C20 H20A 109.5 . . ?
Ga3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Ga3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Ga3 C21 H21A 109.5 . . ?
Ga3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Ga3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Ga3 C22 H22A 109.5 . . ?
Ga3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Ga3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24A C23A C28A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C28A C23A H23A 120.0 . . ?
C23A C24A C25A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C26A C27A C28A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C27A C28A C23A 120.0 . . ?
C27A C28A C29A 115.7(7) . . ?
C23A C28A C29A 124.2(7) . . ?
C28A C29A H29A 109.5 . . ?
C28A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C28A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C24B C23B C28B 120.0 . . ?
C24B C23B H23B 120.0 . . ?
C28B C23B H23B 120.0 . . ?
C25B C24B C23B 120.0 . . ?
C25B C24B H24B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C26B C25B C24B 120.0 . . ?
C26B C25B H25B 120.0 . . ?
C24B C25B H25B 120.0 . . ?
C25B C26B C27B 120.0 . . ?
C25B C26B H26B 120.0 . . ?
C27B C26B H26B 120.0 . . ?
C28B C27B C26B 120.0 . . ?
C28B C27B H27B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C27B C28B C23B 120.0 . . ?
C27B C28B C29B 124.7(5) . . ?
C23B C28B C29B 115.3(5) . . ?
C28B C29B H29D 109.5 . . ?
C28B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.071


data_compound3
_database_code_depnum_ccdc_archive 'CCDC 774448'
#TrackingRef '- compound1_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H40 In3 N3 O'
_chemical_formula_sum            'C22 H40 In3 N3 O'
_chemical_formula_weight         707.03

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'
In In -0.7276 1.3100 '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'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   37.505(5)
_cell_length_b                   8.0398(18)
_cell_length_c                   18.7351(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.012(12)
_cell_angle_gamma                90.00
_cell_volume                     5635.4(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    218
_cell_measurement_theta_min      4.301
_cell_measurement_theta_max      21.075

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5269
_exptl_absorpt_correction_T_max  0.6400
_exptl_absorpt_process_details   
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'

_exptl_special_details           
;

;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            63464
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         30.00
_reflns_number_total             8223
_reflns_number_gt                7106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        
'EVALCCD (Duisenberg,1998,Thesis.Utrecht University.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_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^)+(0.0089P)^2^+9.0144P] 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         8223
_refine_ls_number_parameters     270
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0371
_refine_ls_wR_factor_gt          0.0343
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.183623(3) 0.016403(14) 0.252728(6) 0.01397(3) Uani 1 1 d . . .
In2 In 0.210868(3) -0.155511(14) 0.438707(6) 0.01405(3) Uani 1 1 d . . .
In3 In 0.041690(3) 0.342050(16) 0.367743(6) 0.01894(3) Uani 1 1 d . . .
O1 O 0.17002(3) -0.03896(14) 0.35952(6) 0.0148(2) Uani 1 1 d . . .
N1 N 0.13130(3) -0.03055(17) 0.35923(7) 0.0139(2) Uani 1 1 d . . .
N2 N 0.12928(4) -0.08381(18) 0.20138(7) 0.0164(3) Uani 1 1 d . . .
N3 N 0.08662(4) 0.41262(18) 0.45970(7) 0.0173(3) Uani 1 1 d . . .
C1 C 0.11803(4) -0.2008(2) 0.36318(9) 0.0173(3) Uani 1 1 d . . .
H1A H 0.0921 -0.1993 0.3698 0.021 Uiso 1 1 calc R . .
H1B H 0.1302 -0.2582 0.4048 0.021 Uiso 1 1 calc R . .
C2 C 0.12489(5) -0.2952(2) 0.29442(9) 0.0189(3) Uani 1 1 d . . .
H2A H 0.1510 -0.3089 0.2911 0.023 Uiso 1 1 calc R . .
H2B H 0.1141 -0.4074 0.2961 0.023 Uiso 1 1 calc R . .
C3 C 0.10933(4) -0.2041(2) 0.22925(9) 0.0175(3) Uani 1 1 d . . .
C4 C 0.07503(5) -0.2385(2) 0.19970(10) 0.0223(4) Uani 1 1 d . . .
H4 H 0.0611 -0.3225 0.2200 0.027 Uiso 1 1 calc R . .
C5 C 0.06124(5) -0.1500(2) 0.14051(10) 0.0242(4) Uani 1 1 d . . .
H5 H 0.0378 -0.1719 0.1203 0.029 Uiso 1 1 calc R . .
C6 C 0.08210(5) -0.0294(2) 0.11140(9) 0.0216(3) Uani 1 1 d . . .
H6 H 0.0735 0.0313 0.0702 0.026 Uiso 1 1 calc R . .
C7 C 0.11576(4) 0.0007(2) 0.14370(8) 0.0194(3) Uani 1 1 d . . .
H7 H 0.1300 0.0848 0.1243 0.023 Uiso 1 1 calc R . .
C8 C 0.12215(4) 0.0678(2) 0.42086(8) 0.0148(3) Uani 1 1 d . . .
H8A H 0.1338 0.0193 0.4652 0.018 Uiso 1 1 calc R . .
H8B H 0.0960 0.0652 0.4247 0.018 Uiso 1 1 calc R . .
C9 C 0.13447(4) 0.2480(2) 0.41303(9) 0.0163(3) Uani 1 1 d . . .
H9A H 0.1609 0.2519 0.4165 0.020 Uiso 1 1 calc R . .
H9B H 0.1259 0.2904 0.3653 0.020 Uiso 1 1 calc R . .
C10 C 0.12056(4) 0.3571(2) 0.46977(8) 0.0161(3) Uani 1 1 d . . .
C11 C 0.14170(5) 0.3955(2) 0.53175(9) 0.0235(4) Uani 1 1 d . . .
H11 H 0.1655 0.3553 0.5380 0.028 Uiso 1 1 calc R . .
C12 C 0.12777(6) 0.4924(3) 0.58406(10) 0.0301(4) Uani 1 1 d . . .
H12 H 0.1418 0.5185 0.6267 0.036 Uiso 1 1 calc R . .
C13 C 0.09324(6) 0.5508(2) 0.57360(10) 0.0289(4) Uani 1 1 d . . .
H13 H 0.0832 0.6185 0.6086 0.035 Uiso 1 1 calc R . .
C14 C 0.07366(5) 0.5085(2) 0.51107(9) 0.0239(4) Uani 1 1 d . . .
H14 H 0.0499 0.5489 0.5038 0.029 Uiso 1 1 calc R . .
C15 C 0.17547(5) 0.2789(2) 0.23996(9) 0.0194(3) Uani 1 1 d . . .
H15A H 0.1498 0.3025 0.2344 0.029 Uiso 1 1 calc R . .
H15B H 0.1868 0.3172 0.1974 0.029 Uiso 1 1 calc R . .
H15C H 0.1861 0.3371 0.2822 0.029 Uiso 1 1 calc R . .
C16 C 0.22088(5) -0.1692(2) 0.22377(10) 0.0266(4) Uani 1 1 d . . .
H16A H 0.2316 -0.1355 0.1798 0.040 Uiso 1 1 calc R . .
H16B H 0.2084 -0.2755 0.2159 0.040 Uiso 1 1 calc R . .
H16C H 0.2397 -0.1817 0.2624 0.040 Uiso 1 1 calc R . .
C17 C 0.20971(5) -0.4126(2) 0.40079(10) 0.0230(4) Uani 1 1 d . . .
H17A H 0.2263 -0.4799 0.4316 0.035 Uiso 1 1 calc R . .
H17B H 0.2169 -0.4162 0.3515 0.035 Uiso 1 1 calc R . .
H17C H 0.1854 -0.4571 0.4023 0.035 Uiso 1 1 calc R . .
C18 C 0.19061(5) -0.1199(2) 0.54439(9) 0.0230(4) Uani 1 1 d . . .
H18A H 0.2088 -0.1551 0.5814 0.035 Uiso 1 1 calc R . .
H18B H 0.1689 -0.1867 0.5480 0.035 Uiso 1 1 calc R . .
H18C H 0.1850 -0.0022 0.5511 0.035 Uiso 1 1 calc R . .
C19 C 0.25226(5) 0.0159(3) 0.40896(10) 0.0262(4) Uani 1 1 d . . .
H19A H 0.2470 0.1279 0.4261 0.039 Uiso 1 1 calc R . .
H19B H 0.2529 0.0176 0.3568 0.039 Uiso 1 1 calc R . .
H19C H 0.2755 -0.0205 0.4307 0.039 Uiso 1 1 calc R . .
C20 C 0.06534(5) 0.2680(2) 0.26978(9) 0.0239(4) Uani 1 1 d . . .
H20A H 0.0463 0.2448 0.2325 0.036 Uiso 1 1 calc R . .
H20B H 0.0798 0.1678 0.2788 0.036 Uiso 1 1 calc R . .
H20C H 0.0805 0.3581 0.2539 0.036 Uiso 1 1 calc R . .
C21 C 0.01526(5) 0.5840(3) 0.36471(12) 0.0337(5) Uani 1 1 d . . .
H21A H 0.0013 0.5971 0.3189 0.051 Uiso 1 1 calc R . .
H21B H 0.0333 0.6722 0.3699 0.051 Uiso 1 1 calc R . .
H21C H -0.0006 0.5913 0.4039 0.051 Uiso 1 1 calc R . .
C22 C 0.01594(6) 0.1520(3) 0.42884(12) 0.0390(5) Uani 1 1 d . . .
H22A H 0.0194 0.1776 0.4800 0.059 Uiso 1 1 calc R . .
H22B H 0.0265 0.0433 0.4196 0.059 Uiso 1 1 calc R . .
H22C H -0.0097 0.1494 0.4145 0.059 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
In1 0.01101(5) 0.01764(6) 0.01338(5) -0.00092(4) 0.00160(3) 0.00017(4)
In2 0.01196(5) 0.01606(6) 0.01411(5) 0.00258(4) 0.00084(4) 0.00061(4)
In3 0.01490(5) 0.02280(6) 0.01912(6) 0.00143(5) 0.00120(4) 0.00182(4)
O1 0.0098(5) 0.0195(6) 0.0152(5) 0.0014(4) 0.0014(4) 0.0027(4)
N1 0.0103(5) 0.0145(6) 0.0169(6) -0.0013(5) 0.0017(5) 0.0001(5)
N2 0.0147(6) 0.0192(7) 0.0153(6) -0.0041(5) 0.0009(5) -0.0009(5)
N3 0.0196(7) 0.0157(7) 0.0169(6) -0.0018(5) 0.0037(5) 0.0002(5)
C1 0.0177(7) 0.0146(8) 0.0197(7) 0.0020(6) 0.0015(6) -0.0020(6)
C2 0.0204(8) 0.0137(8) 0.0222(8) -0.0013(6) -0.0011(6) -0.0007(6)
C3 0.0178(7) 0.0141(8) 0.0206(8) -0.0053(6) 0.0018(6) 0.0002(6)
C4 0.0195(8) 0.0182(8) 0.0289(9) -0.0017(7) -0.0007(7) -0.0046(7)
C5 0.0177(8) 0.0255(9) 0.0286(9) -0.0047(7) -0.0048(7) -0.0037(7)
C6 0.0203(8) 0.0268(9) 0.0170(7) -0.0024(7) -0.0027(6) -0.0012(7)
C7 0.0173(7) 0.0264(9) 0.0147(7) -0.0011(7) 0.0019(6) -0.0021(7)
C8 0.0142(7) 0.0152(8) 0.0153(7) 0.0005(6) 0.0029(6) 0.0014(6)
C9 0.0144(7) 0.0177(8) 0.0171(7) -0.0014(6) 0.0031(6) 0.0000(6)
C10 0.0180(7) 0.0142(8) 0.0163(7) -0.0011(6) 0.0030(6) -0.0033(6)
C11 0.0226(8) 0.0260(9) 0.0214(8) -0.0029(7) -0.0023(7) -0.0068(7)
C12 0.0400(11) 0.0311(11) 0.0188(8) -0.0057(8) -0.0005(7) -0.0119(9)
C13 0.0441(11) 0.0233(10) 0.0205(8) -0.0083(7) 0.0106(8) -0.0045(8)
C14 0.0290(9) 0.0197(9) 0.0241(8) -0.0018(7) 0.0092(7) 0.0038(7)
C15 0.0220(8) 0.0190(8) 0.0175(8) 0.0024(6) 0.0032(6) -0.0007(7)
C16 0.0231(9) 0.0315(10) 0.0262(9) -0.0025(8) 0.0084(7) 0.0088(8)
C17 0.0253(9) 0.0179(9) 0.0255(9) 0.0009(7) -0.0010(7) 0.0023(7)
C18 0.0222(8) 0.0312(10) 0.0160(8) 0.0037(7) 0.0039(6) 0.0049(7)
C19 0.0208(8) 0.0304(10) 0.0274(9) 0.0074(8) 0.0015(7) -0.0067(7)
C20 0.0252(9) 0.0272(10) 0.0187(8) -0.0023(7) -0.0021(7) 0.0016(7)
C21 0.0282(10) 0.0374(12) 0.0357(11) 0.0040(9) 0.0025(8) 0.0164(9)
C22 0.0307(10) 0.0490(14) 0.0374(11) 0.0088(10) 0.0020(9) -0.0164(10)

_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
In1 C16 2.1404(18) . ?
In1 C15 2.1437(18) . ?
In1 O1 2.1457(11) . ?
In1 N2 2.3353(14) . ?
In2 C19 2.1775(18) . ?
In2 C17 2.1853(19) . ?
In2 C18 2.1886(17) . ?
In2 O1 2.2600(11) . ?
In3 C22 2.175(2) . ?
In3 C20 2.1764(18) . ?
In3 C21 2.182(2) . ?
In3 N3 2.3923(14) . ?
O1 N1 1.4536(16) . ?
N1 C8 1.460(2) . ?
N1 C1 1.460(2) . ?
N2 C7 1.345(2) . ?
N2 C3 1.350(2) . ?
N3 C10 1.350(2) . ?
N3 C14 1.350(2) . ?
C1 C2 1.532(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.506(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.392(2) . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.530(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.500(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.394(2) . ?
C11 C12 1.383(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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 In1 C15 138.49(7) . . ?
C16 In1 O1 107.08(6) . . ?
C15 In1 O1 105.48(5) . . ?
C16 In1 N2 102.79(7) . . ?
C15 In1 N2 100.38(6) . . ?
O1 In1 N2 93.15(5) . . ?
C19 In2 C17 120.93(7) . . ?
C19 In2 C18 116.59(7) . . ?
C17 In2 C18 114.67(7) . . ?
C19 In2 O1 91.84(6) . . ?
C17 In2 O1 100.47(6) . . ?
C18 In2 O1 106.11(5) . . ?
C22 In3 C20 118.28(9) . . ?
C22 In3 C21 114.98(9) . . ?
C20 In3 C21 115.65(8) . . ?
C22 In3 N3 95.96(7) . . ?
C20 In3 N3 111.35(6) . . ?
C21 In3 N3 95.92(7) . . ?
N1 O1 In1 106.83(8) . . ?
N1 O1 In2 130.76(8) . . ?
In1 O1 In2 120.24(5) . . ?
O1 N1 C8 108.19(11) . . ?
O1 N1 C1 107.47(12) . . ?
C8 N1 C1 111.59(12) . . ?
C7 N2 C3 118.96(14) . . ?
C7 N2 In1 115.21(11) . . ?
C3 N2 In1 125.40(11) . . ?
C10 N3 C14 118.18(15) . . ?
C10 N3 In3 129.21(11) . . ?
C14 N3 In3 112.23(11) . . ?
N1 C1 C2 110.11(13) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
C3 C2 C1 111.23(14) . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 120.69(16) . . ?
N2 C3 C2 117.91(14) . . ?
C4 C3 C2 121.36(15) . . ?
C5 C4 C3 119.89(17) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 119.07(16) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 118.35(16) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
N2 C7 C6 123.01(16) . . ?
N2 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
N1 C8 C9 110.34(13) . . ?
N1 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
N1 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.30(13) . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N3 C10 C11 121.27(15) . . ?
N3 C10 C9 117.77(14) . . ?
C11 C10 C9 120.93(15) . . ?
C12 C11 C10 119.61(17) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C13 C12 C11 119.27(17) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 118.34(17) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
N3 C14 C13 123.32(18) . . ?
N3 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
In1 C15 H15A 109.5 . . ?
In1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
In1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
In1 C16 H16A 109.5 . . ?
In1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
In1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
In2 C17 H17A 109.5 . . ?
In2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
In2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
In2 C18 H18A 109.5 . . ?
In2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
In2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
In2 C19 H19A 109.5 . . ?
In2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
In2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
In3 C20 H20A 109.5 . . ?
In3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
In3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
In3 C21 H21A 109.5 . . ?
In3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
In3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
In3 C22 H22A 109.5 . . ?
In3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
In3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.087


#===END