# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1033053'
_audit_update_record             
;
2014-11-06 deposited with the CCDC.
2014-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H45 N5 S'
_chemical_formula_sum            'C30 H45 N5 S'
_chemical_formula_weight         507.77

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   12.723(4)
_cell_length_b                   13.524(4)
_cell_length_c                   19.049(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.062(4)
_cell_angle_gamma                90.00
_cell_volume                     3227.3(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    2397
_cell_measurement_theta_min      2.216
_cell_measurement_theta_max      19.134

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21121
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5659
_reflns_number_gt                3582
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_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 F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.1262P)²+1.2901P] where P=(Fo²+2Fc²)/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         5659
_refine_ls_number_parameters     343
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2392
_refine_ls_wR_factor_gt          0.2080
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001

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
S1 S 0.59172(9) 0.35351(7) 0.26080(5) 0.0744(4) Uani 1 1 d . . .
N1 N 0.7053(2) 0.16920(18) 0.37224(13) 0.0500(6) Uani 1 1 d . . .
N2 N 0.8045(2) 0.2108(2) 0.37992(14) 0.0579(7) Uani 1 1 d . . .
N3 N 0.60397(19) 0.24615(18) 0.45297(12) 0.0471(6) Uani 1 1 d . . .
N4 N 0.6935(2) 0.2377(2) 0.50370(14) 0.0570(7) Uani 1 1 d . . .
N5 N 0.7014(2) 0.39518(18) 0.39104(13) 0.0535(7) Uani 1 1 d . . .
H5 H 0.7126 0.3742 0.4343 0.064 Uiso 1 1 calc R . .
C1 C 0.8708(3) 0.1368(2) 0.37673(17) 0.0559(8) Uani 1 1 d . A .
C2 C 0.8139(3) 0.0472(3) 0.36771(17) 0.0599(9) Uani 1 1 d . . .
H2 H 0.8430 -0.0153 0.3644 0.072 Uiso 1 1 calc R . .
C3 C 0.7082(3) 0.0685(2) 0.36475(15) 0.0503(8) Uani 1 1 d . . .
C4 C 0.9885(3) 0.1563(3) 0.3845(2) 0.0696(10) Uani 1 1 d D . .
C5 C 1.0291(9) 0.1810(8) 0.4630(5) 0.104(3) Uiso 0.50 1 d PD A 1
H5A H 1.1044 0.1942 0.4700 0.156 Uiso 0.50 1 calc PR A 1
H5B H 1.0161 0.1260 0.4922 0.156 Uiso 0.50 1 calc PR A 1
H5C H 0.9924 0.2383 0.4761 0.156 Uiso 0.50 1 calc PR A 1
C6 C 1.0466(8) 0.0608(6) 0.3696(5) 0.100(3) Uiso 0.50 1 d PD A 1
H6A H 1.1218 0.0736 0.3745 0.150 Uiso 0.50 1 calc PR A 1
H6B H 1.0197 0.0387 0.3219 0.150 Uiso 0.50 1 calc PR A 1
H6C H 1.0346 0.0107 0.4029 0.150 Uiso 0.50 1 calc PR A 1
C7 C 1.0076(11) 0.2362(9) 0.3354(6) 0.135(4) Uiso 0.50 1 d PD A 1
H7A H 1.0829 0.2485 0.3405 0.202 Uiso 0.50 1 calc PR A 1
H7B H 0.9720 0.2953 0.3464 0.202 Uiso 0.50 1 calc PR A 1
H7C H 0.9803 0.2166 0.2872 0.202 Uiso 0.50 1 calc PR A 1
C5A C 1.0457(11) 0.1250(9) 0.4566(5) 0.132(4) Uiso 0.50 1 d PD A 2
H5A1 H 1.1206 0.1381 0.4604 0.198 Uiso 0.50 1 calc PR A 2
H5A2 H 1.0350 0.0555 0.4628 0.198 Uiso 0.50 1 calc PR A 2
H5A3 H 1.0182 0.1612 0.4928 0.198 Uiso 0.50 1 calc PR A 2
C6A C 1.0347(9) 0.1057(8) 0.3249(5) 0.110(3) Uiso 0.50 1 d PD A 2
H6A1 H 1.1098 0.1192 0.3307 0.166 Uiso 0.50 1 calc PR A 2
H6A2 H 0.9996 0.1305 0.2796 0.166 Uiso 0.50 1 calc PR A 2
H6A3 H 1.0236 0.0357 0.3269 0.166 Uiso 0.50 1 calc PR A 2
C7A C 1.0125(8) 0.2690(6) 0.3750(5) 0.090(3) Uiso 0.50 1 d PD A 2
H7A1 H 1.0882 0.2788 0.3803 0.135 Uiso 0.50 1 calc PR A 2
H7A2 H 0.9851 0.3068 0.4104 0.135 Uiso 0.50 1 calc PR A 2
H7A3 H 0.9789 0.2902 0.3283 0.135 Uiso 0.50 1 calc PR A 2
C8 C 0.6139(3) 0.0002(2) 0.35426(18) 0.0603(9) Uani 1 1 d . . .
C9 C 0.5595(4) 0.0014(3) 0.4198(2) 0.0820(12) Uani 1 1 d . . .
H9A H 0.4994 -0.0426 0.4123 0.123 Uiso 1 1 calc R . .
H9B H 0.5356 0.0673 0.4274 0.123 Uiso 1 1 calc R . .
H9C H 0.6093 -0.0196 0.4609 0.123 Uiso 1 1 calc R . .
C10 C 0.5344(3) 0.0258(3) 0.2862(2) 0.0841(12) Uani 1 1 d . . .
H10A H 0.4753 -0.0193 0.2810 0.126 Uiso 1 1 calc R . .
H10B H 0.5693 0.0205 0.2456 0.126 Uiso 1 1 calc R . .
H10C H 0.5090 0.0922 0.2896 0.126 Uiso 1 1 calc R . .
C11 C 0.6544(4) -0.1056(3) 0.3456(3) 0.0944(14) Uani 1 1 d . . .
H11A H 0.5950 -0.1505 0.3386 0.142 Uiso 1 1 calc R . .
H11B H 0.7036 -0.1240 0.3876 0.142 Uiso 1 1 calc R . .
H11C H 0.6897 -0.1081 0.3050 0.142 Uiso 1 1 calc R . .
C12 C 0.6635(3) 0.2616(3) 0.56424(17) 0.0626(9) Uani 1 1 d . B .
C13 C 0.5558(3) 0.2866(3) 0.55250(18) 0.0659(9) Uani 1 1 d . . .
H13 H 0.5164 0.3056 0.5870 0.079 Uiso 1 1 calc R . .
C14 C 0.5184(3) 0.2782(2) 0.48089(16) 0.0523(8) Uani 1 1 d . D .
C15 C 0.7432(3) 0.2578(3) 0.63350(19) 0.0840(12) Uani 1 1 d D . .
C16 C 0.813(3) 0.1641(19) 0.6326(17) 0.148(11) Uiso 0.25 1 d PDU B 1
H16A H 0.8639 0.1605 0.6760 0.222 Uiso 0.25 1 calc PR B 1
H16B H 0.8497 0.1672 0.5928 0.222 Uiso 0.25 1 calc PR B 1
H16C H 0.7681 0.1065 0.6283 0.222 Uiso 0.25 1 calc PR B 1
C17 C 0.6830(17) 0.248(3) 0.6954(11) 0.115(8) Uiso 0.25 1 d PDU B 1
H17A H 0.7330 0.2452 0.7393 0.173 Uiso 0.25 1 calc PR B 1
H17B H 0.6408 0.1890 0.6898 0.173 Uiso 0.25 1 calc PR B 1
H17C H 0.6371 0.3045 0.6961 0.173 Uiso 0.25 1 calc PR B 1
C18 C 0.811(2) 0.3488(17) 0.6358(16) 0.121(10) Uiso 0.25 1 d PD B 1
H18A H 0.8636 0.3485 0.6787 0.182 Uiso 0.25 1 calc PR B 1
H18B H 0.7671 0.4065 0.6350 0.182 Uiso 0.25 1 calc PR B 1
H18C H 0.8466 0.3495 0.5952 0.182 Uiso 0.25 1 calc PR B 1
C16A C 0.736(2) 0.1554(12) 0.6664(14) 0.082(6) Uiso 0.25 1 d PDU B 2
H16D H 0.7859 0.1508 0.7102 0.123 Uiso 0.25 1 calc PR B 2
H16E H 0.7514 0.1057 0.6338 0.123 Uiso 0.25 1 calc PR B 2
H16F H 0.6647 0.1454 0.6759 0.123 Uiso 0.25 1 calc PR B 2
C17A C 0.712(2) 0.3381(17) 0.6871(11) 0.075(5) Uiso 0.25 1 d PDU C 2
H17D H 0.7630 0.3357 0.7309 0.112 Uiso 0.25 1 calc PR C 2
H17E H 0.6422 0.3246 0.6966 0.112 Uiso 0.25 1 calc PR C 2
H17F H 0.7137 0.4027 0.6663 0.112 Uiso 0.25 1 calc PR C 2
C18A C 0.8563(12) 0.280(2) 0.6238(10) 0.071(5) Uiso 0.25 1 d PDU B 2
H18D H 0.9031 0.2756 0.6691 0.107 Uiso 0.25 1 calc PR B 2
H18E H 0.8597 0.3449 0.6045 0.107 Uiso 0.25 1 calc PR B 2
H18F H 0.8780 0.2321 0.5917 0.107 Uiso 0.25 1 calc PR B 2
C16B C 0.709(2) 0.1811(19) 0.6839(12) 0.097(7) Uiso 0.25 1 d PDU B 3
H16G H 0.7607 0.1788 0.7271 0.146 Uiso 0.25 1 calc PR B 3
H16H H 0.7042 0.1174 0.6615 0.146 Uiso 0.25 1 calc PR B 3
H16I H 0.6406 0.1990 0.6948 0.146 Uiso 0.25 1 calc PR B 3
C17B C 0.750(2) 0.3597(11) 0.6703(13) 0.094(7) Uiso 0.25 1 d PDU B 3
H17G H 0.8005 0.3569 0.7139 0.142 Uiso 0.25 1 calc PR B 3
H17H H 0.6808 0.3771 0.6807 0.142 Uiso 0.25 1 calc PR B 3
H17I H 0.7718 0.4086 0.6394 0.142 Uiso 0.25 1 calc PR B 3
C18B C 0.8557(13) 0.230(2) 0.6189(11) 0.093(6) Uiso 0.25 1 d PDU B 3
H18G H 0.9051 0.2274 0.6632 0.140 Uiso 0.25 1 calc PR B 3
H18H H 0.8790 0.2788 0.5884 0.140 Uiso 0.25 1 calc PR B 3
H18I H 0.8527 0.1665 0.5961 0.140 Uiso 0.25 1 calc PR B 3
C16D C 0.769(3) 0.1481(10) 0.6484(15) 0.095(7) Uiso 0.25 1 d PDU B 4
H16J H 0.8198 0.1419 0.6919 0.143 Uiso 0.25 1 calc PR B 4
H16K H 0.7987 0.1205 0.6097 0.143 Uiso 0.25 1 calc PR B 4
H16L H 0.7049 0.1132 0.6530 0.143 Uiso 0.25 1 calc PR B 4
C17D C 0.6890(17) 0.303(2) 0.6922(10) 0.087(6) Uiso 0.25 1 d PDU B 4
H17J H 0.7376 0.3008 0.7368 0.130 Uiso 0.25 1 calc PR B 4
H17K H 0.6263 0.2649 0.6962 0.130 Uiso 0.25 1 calc PR B 4
H17L H 0.6691 0.3697 0.6803 0.130 Uiso 0.25 1 calc PR B 4
C18D C 0.8411(18) 0.317(2) 0.6254(12) 0.083(6) Uiso 0.25 1 d PD B 4
H18J H 0.8919 0.3139 0.6690 0.124 Uiso 0.25 1 calc PR B 4
H18K H 0.8212 0.3845 0.6149 0.124 Uiso 0.25 1 calc PR B 4
H18L H 0.8723 0.2898 0.5873 0.124 Uiso 0.25 1 calc PR B 4
C19 C 0.4078(3) 0.3030(3) 0.44144(18) 0.0642(9) Uani 1 1 d D . .
C20 C 0.3391(7) 0.3400(7) 0.4927(4) 0.079(3) Uiso 0.50 1 d PDU D 1
H20A H 0.2692 0.3556 0.4670 0.119 Uiso 0.50 1 calc PR D 1
H20B H 0.3707 0.3983 0.5163 0.119 Uiso 0.50 1 calc PR D 1
H20C H 0.3335 0.2898 0.5274 0.119 Uiso 0.50 1 calc PR D 1
C21 C 0.4043(7) 0.3805(6) 0.3834(4) 0.080(2) Uiso 0.50 1 d PDU D 1
H21A H 0.3316 0.3922 0.3614 0.119 Uiso 0.50 1 calc PR D 1
H21B H 0.4439 0.3573 0.3481 0.119 Uiso 0.50 1 calc PR D 1
H21C H 0.4354 0.4409 0.4039 0.119 Uiso 0.50 1 calc PR D 1
C22 C 0.3551(7) 0.2050(6) 0.4027(4) 0.076(2) Uiso 0.50 1 d PDU D 1
H22A H 0.2847 0.2200 0.3776 0.114 Uiso 0.50 1 calc PR D 1
H22B H 0.3509 0.1549 0.4377 0.114 Uiso 0.50 1 calc PR D 1
H22C H 0.3983 0.1817 0.3695 0.114 Uiso 0.50 1 calc PR D 1
C20A C 0.3304(6) 0.2934(6) 0.4952(4) 0.067(2) Uiso 0.50 1 d PDU D 2
H20D H 0.2592 0.3091 0.4718 0.100 Uiso 0.50 1 calc PR D 2
H20E H 0.3516 0.3383 0.5341 0.100 Uiso 0.50 1 calc PR D 2
H20F H 0.3322 0.2269 0.5130 0.100 Uiso 0.50 1 calc PR D 2
C21A C 0.4128(8) 0.4142(6) 0.4192(5) 0.097(3) Uiso 0.50 1 d PDU D 2
H21D H 0.3442 0.4344 0.3938 0.146 Uiso 0.50 1 calc PR D 2
H21E H 0.4653 0.4220 0.3890 0.146 Uiso 0.50 1 calc PR D 2
H21F H 0.4319 0.4543 0.4611 0.146 Uiso 0.50 1 calc PR D 2
C22A C 0.3650(8) 0.2444(7) 0.3769(4) 0.086(3) Uiso 0.50 1 d PDU D 2
H22D H 0.2948 0.2675 0.3570 0.129 Uiso 0.50 1 calc PR D 2
H22E H 0.3616 0.1759 0.3895 0.129 Uiso 0.50 1 calc PR D 2
H22F H 0.4110 0.2519 0.3423 0.129 Uiso 0.50 1 calc PR D 2
C23 C 0.6186(2) 0.2361(2) 0.37841(15) 0.0472(7) Uani 1 1 d . . .
H23 H 0.5528 0.2087 0.3508 0.057 Uiso 1 1 calc R . .
C24 C 0.6410(2) 0.3354(2) 0.34502(16) 0.0491(8) Uani 1 1 d . . .
C25 C 0.7502(3) 0.4863(2) 0.38150(16) 0.0520(8) Uani 1 1 d . . .
C26 C 0.7121(3) 0.5530(2) 0.32785(18) 0.0657(10) Uani 1 1 d . . .
H26 H 0.6508 0.5390 0.2950 0.079 Uiso 1 1 calc R . .
C27 C 0.7666(4) 0.6407(3) 0.3238(2) 0.0763(11) Uani 1 1 d . . .
H27 H 0.7420 0.6855 0.2876 0.092 Uiso 1 1 calc R . .
C28 C 0.8553(4) 0.6621(3) 0.3719(2) 0.0801(12) Uani 1 1 d . . .
H28 H 0.8910 0.7216 0.3686 0.096 Uiso 1 1 calc R . .
C29 C 0.8923(4) 0.5974(3) 0.4247(3) 0.0872(13) Uani 1 1 d . . .
H29 H 0.9528 0.6126 0.4579 0.105 Uiso 1 1 calc R . .
C30 C 0.8402(3) 0.5090(3) 0.4292(2) 0.0712(10) Uani 1 1 d . . .
H30 H 0.8666 0.4643 0.4650 0.085 Uiso 1 1 calc R . .


_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
S1 C24 1.636(3) . ?
N1 N2 1.366(4) . ?
N1 C3 1.371(4) . ?
N1 C23 1.447(4) . ?
N2 C1 1.317(4) . ?
N3 C14 1.363(4) . ?
N3 N4 1.364(3) . ?
N3 C23 1.471(4) . ?
N4 C12 1.317(4) . ?
N5 C24 1.333(4) . ?
N5 C25 1.406(4) . ?
C1 C2 1.406(5) . ?
C1 C4 1.502(5) . ?
C2 C3 1.366(4) . ?
C3 C8 1.499(4) . ?
C4 C7 1.477(10) . ?
C4 C5A 1.499(10) . ?
C4 C6A 1.529(9) . ?
C4 C5 1.532(9) . ?
C4 C6 1.539(9) . ?
C4 C7A 1.571(8) . ?
C8 C11 1.539(5) . ?
C8 C10 1.538(5) . ?
C8 C9 1.530(5) . ?
C12 C13 1.391(5) . ?
C12 C15 1.518(5) . ?
C13 C14 1.369(4) . ?
C14 C19 1.513(5) . ?
C15 C18 1.500(14) . ?
C15 C18D 1.510(13) . ?
C15 C18A 1.511(13) . ?
C15 C17 1.519(14) . ?
C15 C16B 1.527(13) . ?
C15 C17D 1.537(13) . ?
C15 C17B 1.542(13) . ?
C15 C16A 1.531(13) . ?
C15 C16D 1.537(13) . ?
C15 C18B 1.552(13) . ?
C15 C16 1.549(15) . ?
C19 C22A 1.484(8) . ?
C19 C20 1.505(8) . ?
C19 C21 1.519(8) . ?
C19 C20A 1.545(7) . ?
C19 C21A 1.567(9) . ?
C19 C22 1.605(8) . ?
C23 C24 1.535(4) . ?
C25 C30 1.367(5) . ?
C25 C26 1.386(4) . ?
C26 C27 1.382(5) . ?
C27 C28 1.356(6) . ?
C28 C29 1.355(6) . ?
C29 C30 1.376(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C3 112.2(2) . . ?
N2 N1 C23 115.9(2) . . ?
C3 N1 C23 131.7(3) . . ?
C1 N2 N1 105.7(3) . . ?
C14 N3 N4 112.1(2) . . ?
C14 N3 C23 130.6(3) . . ?
N4 N3 C23 116.4(2) . . ?
C12 N4 N3 105.4(3) . . ?
C24 N5 C25 131.5(3) . . ?
N2 C1 C2 109.9(3) . . ?
N2 C1 C4 119.8(3) . . ?
C2 C1 C4 130.3(3) . . ?
C3 C2 C1 107.8(3) . . ?
C2 C3 N1 104.4(3) . . ?
C2 C3 C8 129.4(3) . . ?
N1 C3 C8 126.2(3) . . ?
C7 C4 C1 109.7(6) . . ?
C7 C4 C5A 132.9(8) . . ?
C1 C4 C5A 110.9(6) . . ?
C7 C4 C6A 74.3(6) . . ?
C1 C4 C6A 110.7(5) . . ?
C5A C4 C6A 111.5(7) . . ?
C7 C4 C5 113.3(7) . . ?
C1 C4 C5 107.2(5) . . ?
C5A C4 C5 30.7(5) . . ?
C6A C4 C5 135.7(6) . . ?
C7 C4 C6 111.0(7) . . ?
C1 C4 C6 109.7(5) . . ?
C5A C4 C6 76.1(6) . . ?
C6A C4 C6 39.4(4) . . ?
C5 C4 C6 105.8(6) . . ?
C7 C4 C7A 32.9(5) . . ?
C1 C4 C7A 111.7(4) . . ?
C5A C4 C7A 107.9(6) . . ?
C6A C4 C7A 103.9(6) . . ?
C5 C4 C7A 82.1(5) . . ?
C6 C4 C7A 133.1(6) . . ?
C3 C8 C11 108.2(3) . . ?
C3 C8 C10 111.5(3) . . ?
C11 C8 C10 107.6(3) . . ?
C3 C8 C9 110.5(3) . . ?
C11 C8 C9 107.8(3) . . ?
C10 C8 C9 111.1(3) . . ?
N4 C12 C13 110.3(3) . . ?
N4 C12 C15 120.1(3) . . ?
C13 C12 C15 129.6(3) . . ?
C14 C13 C12 107.5(3) . . ?
N3 C14 C13 104.7(3) . . ?
N3 C14 C19 127.9(3) . . ?
C13 C14 C19 127.4(3) . . ?
C18 C15 C18D 24.1(12) . . ?
C18 C15 C18A 44.5(12) . . ?
C18D C15 C18A 20.7(11) . . ?
C18 C15 C12 107.0(11) . . ?
C18D C15 C12 109.3(10) . . ?
C18A C15 C12 113.1(8) . . ?
C18 C15 C17 114.4(12) . . ?
C18D C15 C17 131.3(14) . . ?
C18A C15 C17 137.0(12) . . ?
C12 C15 C17 109.1(10) . . ?
C18 C15 C16B 139.9(13) . . ?
C18D C15 C16B 138.9(13) . . ?
C18A C15 C16B 126.2(12) . . ?
C12 C15 C16B 110.4(9) . . ?
C17 C15 C16B 38.4(10) . . ?
C18 C15 C17D 89.2(12) . . ?
C18D C15 C17D 110.4(11) . . ?
C18A C15 C17D 124.8(12) . . ?
C12 C15 C17D 107.6(9) . . ?
C17 C15 C17D 28.1(11) . . ?
C16B C15 C17D 66.2(11) . . ?
C18 C15 C17B 43.0(10) . . ?
C18D C15 C17B 66.0(11) . . ?
C18A C15 C17B 84.6(11) . . ?
C12 C15 C17B 109.9(8) . . ?
C17 C15 C17B 73.6(11) . . ?
C16B C15 C17B 108.6(10) . . ?
C17D C15 C17B 46.6(11) . . ?
C18 C15 C16A 143.8(14) . . ?
C18D C15 C16A 129.3(13) . . ?
C18A C15 C16A 110.9(10) . . ?
C12 C15 C16A 107.8(9) . . ?
C17 C15 C16A 61.9(12) . . ?
C16B C15 C16A 23.4(10) . . ?
C17D C15 C16A 89.4(12) . . ?
C17B C15 C16A 128.6(11) . . ?
C18 C15 C16D 133.0(14) . . ?
C18D C15 C16D 112.1(11) . . ?
C18A C15 C16D 91.9(12) . . ?
C12 C15 C16D 106.4(10) . . ?
C17 C15 C16D 84.0(12) . . ?
C16B C15 C16D 45.8(12) . . ?
C17D C15 C16D 110.8(11) . . ?
C17B C15 C16D 141.9(13) . . ?
C16A C15 C16D 22.6(11) . . ?
C18 C15 C18B 70.0(11) . . ?
C18D C15 C18B 46.1(11) . . ?
C18A C15 C18B 25.5(9) . . ?
C12 C15 C18B 110.4(8) . . ?
C17 C15 C18B 136.4(12) . . ?
C16B C15 C18B 108.7(10) . . ?
C17D C15 C18B 140.5(12) . . ?
C17B C15 C18B 108.7(10) . . ?
C16A C15 C18B 88.9(11) . . ?
C16D C15 C18B 67.9(11) . . ?
C18 C15 C16 110.1(12) . . ?
C18D C15 C16 87.0(14) . . ?
C18A C15 C16 66.4(13) . . ?
C12 C15 C16 108.3(12) . . ?
C17 C15 C16 107.8(11) . . ?
C16B C15 C16 71.2(12) . . ?
C17D C15 C16 131.3(14) . . ?
C17B C15 C16 138.7(14) . . ?
C16A C15 C16 48.8(13) . . ?
C16D C15 C16 26.7(13) . . ?
C18B C15 C16 41.5(11) . . ?
C22A C19 C14 117.9(4) . . ?
C22A C19 C20 123.0(6) . . ?
C14 C19 C20 110.3(4) . . ?
C22A C19 C21 78.8(5) . . ?
C14 C19 C21 114.9(4) . . ?
C20 C19 C21 107.3(5) . . ?
C22A C19 C20A 108.7(5) . . ?
C14 C19 C20A 107.3(4) . . ?
C20 C19 C20A 24.3(4) . . ?
C21 C19 C20A 126.9(5) . . ?
C22A C19 C21A 108.3(5) . . ?
C14 C19 C21A 105.6(4) . . ?
C20 C19 C21A 85.0(5) . . ?
C21 C19 C21A 30.5(4) . . ?
C20A C19 C21A 108.7(5) . . ?
C22A C19 C22 27.8(4) . . ?
C14 C19 C22 108.8(4) . . ?
C20 C19 C22 109.3(5) . . ?
C21 C19 C22 106.1(5) . . ?
C20A C19 C22 88.4(5) . . ?
C21A C19 C22 134.5(5) . . ?
N1 C23 N3 111.3(2) . . ?
N1 C23 C24 108.3(2) . . ?
N3 C23 C24 112.5(2) . . ?
N5 C24 C23 112.7(3) . . ?
N5 C24 S1 129.3(2) . . ?
C23 C24 S1 118.0(2) . . ?
C30 C25 C26 119.2(3) . . ?
C30 C25 N5 116.7(3) . . ?
C26 C25 N5 124.1(3) . . ?
C27 C26 C25 119.1(4) . . ?
C28 C27 C26 120.8(4) . . ?
C27 C28 C29 120.2(4) . . ?
C28 C29 C30 119.9(4) . . ?
C25 C30 C29 120.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.047



#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
_shelx_title                     ' JA_36 in P2(1)/n'
_shelx_refln_list_code           4
_shelx_F_calc_maximum            157.43
_reflns_d_resolution_high        0.8409

_shelx_F_squared_multiplier      1.000

_chemical_properties_physical    Heat-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1033054'
_audit_update_record             
;
2014-11-06 deposited with the CCDC.
2014-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H45 N5 O'
_chemical_formula_sum            'C30 H45 N5 O'
_chemical_formula_weight         491.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   12.6909(10)
_cell_length_b                   13.2006(11)
_cell_length_c                   18.4966(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.329(3)
_cell_angle_gamma                90.00
_cell_volume                     3048.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    1015
_cell_measurement_theta_min      2.245
_cell_measurement_theta_max      16.678

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17758
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.1041
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5291
_reflns_number_gt                2554
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_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 F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0903P)²+0.4117P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5291
_refine_ls_number_parameters     337
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.2195
_refine_ls_wR_factor_gt          0.1714
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.7790(2) 0.1704(2) 0.12977(16) 0.0373(8) Uani 1 1 d . . .
N2 N 0.6792(2) 0.2105(2) 0.12510(17) 0.0416(8) Uani 1 1 d . . .
N3 N 0.8802(2) 0.2503(2) 0.04682(15) 0.0333(7) Uani 1 1 d . . .
N4 N 0.7928(2) 0.2367(2) -0.00682(16) 0.0386(8) Uani 1 1 d . . .
N5 N 0.7777(3) 0.4076(2) 0.1030(2) 0.0397(9) Uani 1 1 d . . .
O1 O 0.8565(2) 0.36212(19) 0.21896(14) 0.0500(8) Uani 1 1 d . . .
C1 C 0.6151(3) 0.1320(3) 0.1285(2) 0.0408(10) Uani 1 1 d . . .
C2 C 0.6741(3) 0.0416(3) 0.1342(2) 0.0440(10) Uani 1 1 d . . .
H2 H 0.6468 -0.0234 0.1369 0.053 Uiso 1 1 calc R . .
C3 C 0.7784(3) 0.0664(3) 0.1349(2) 0.0380(9) Uani 1 1 d . . .
C4 C 0.4962(3) 0.1491(3) 0.1249(2) 0.0527(12) Uani 1 1 d . . .
C5 C 0.4579(4) 0.0864(5) 0.1829(3) 0.116(3) Uani 1 1 d . . .
H5A H 0.4992 0.1026 0.2302 0.174 Uiso 1 1 calc R . .
H5B H 0.4662 0.0158 0.1728 0.174 Uiso 1 1 calc R . .
H5C H 0.3837 0.1007 0.1828 0.174 Uiso 1 1 calc R . .
C6 C 0.4730(4) 0.2601(4) 0.1387(4) 0.102(2) Uani 1 1 d . . .
H6A H 0.3977 0.2688 0.1379 0.153 Uiso 1 1 calc R . .
H6B H 0.4946 0.3012 0.1011 0.153 Uiso 1 1 calc R . .
H6C H 0.5122 0.2801 0.1858 0.153 Uiso 1 1 calc R . .
C7 C 0.4371(4) 0.1208(5) 0.0501(3) 0.107(2) Uani 1 1 d . . .
H7A H 0.4462 0.0498 0.0420 0.160 Uiso 1 1 calc R . .
H7B H 0.4648 0.1591 0.0136 0.160 Uiso 1 1 calc R . .
H7C H 0.3623 0.1356 0.0469 0.160 Uiso 1 1 calc R . .
C8 C 0.8753(3) -0.0028(3) 0.1424(2) 0.0426(10) Uani 1 1 d . . .
C9 C 0.8378(4) -0.1119(3) 0.1494(3) 0.0668(14) Uani 1 1 d . . .
H9A H 0.8065 -0.1181 0.1928 0.100 Uiso 1 1 calc R . .
H9B H 0.8979 -0.1569 0.1530 0.100 Uiso 1 1 calc R . .
H9C H 0.7855 -0.1291 0.1070 0.100 Uiso 1 1 calc R . .
C10 C 0.9569(3) 0.0219(3) 0.2123(2) 0.0582(12) Uani 1 1 d . . .
H10A H 0.9793 0.0912 0.2106 0.087 Uiso 1 1 calc R . .
H10B H 1.0179 -0.0218 0.2152 0.087 Uiso 1 1 calc R . .
H10C H 0.9243 0.0118 0.2547 0.087 Uiso 1 1 calc R . .
C11 C 0.9274(3) 0.0038(3) 0.0737(2) 0.0576(12) Uani 1 1 d . . .
H11A H 0.8744 -0.0086 0.0307 0.086 Uiso 1 1 calc R . .
H11B H 0.9832 -0.0460 0.0769 0.086 Uiso 1 1 calc R . .
H11C H 0.9574 0.0701 0.0707 0.086 Uiso 1 1 calc R . .
C12 C 0.8260(3) 0.2604(3) -0.0684(2) 0.0446(10) Uani 1 1 d . A .
C13 C 0.9327(3) 0.2919(3) -0.0539(2) 0.0490(11) Uani 1 1 d . . .
H13 H 0.9729 0.3127 -0.0885 0.059 Uiso 1 1 calc R . .
C14 C 0.9673(3) 0.2867(3) 0.0203(2) 0.0374(9) Uani 1 1 d . . .
C15 C 0.7517(3) 0.2519(4) -0.1414(2) 0.0575(12) Uani 1 1 d D . .
C16 C 0.6503(7) 0.1911(8) -0.1320(6) 0.067(3) Uiso 0.50 1 d PDU A 1
H16A H 0.6029 0.1862 -0.1786 0.101 Uiso 0.50 1 calc PR A 1
H16B H 0.6145 0.2251 -0.0975 0.101 Uiso 0.50 1 calc PR A 1
H16C H 0.6709 0.1243 -0.1143 0.101 Uiso 0.50 1 calc PR A 1
C17 C 0.7195(10) 0.3587(7) -0.1685(7) 0.088(4) Uiso 0.50 1 d PDU A 1
H17A H 0.6721 0.3549 -0.2151 0.132 Uiso 0.50 1 calc PR A 1
H17B H 0.7823 0.3964 -0.1738 0.132 Uiso 0.50 1 calc PR A 1
H17C H 0.6837 0.3920 -0.1336 0.132 Uiso 0.50 1 calc PR A 1
C18 C 0.8078(8) 0.2011(8) -0.1979(6) 0.072(3) Uiso 0.50 1 d PDU A 1
H18A H 0.7595 0.1970 -0.2441 0.108 Uiso 0.50 1 calc PR A 1
H18B H 0.8299 0.1342 -0.1814 0.108 Uiso 0.50 1 calc PR A 1
H18C H 0.8695 0.2402 -0.2038 0.108 Uiso 0.50 1 calc PR A 1
C16A C 0.6375(8) 0.2455(8) -0.1348(6) 0.079(3) Uiso 0.50 1 d PDU A 2
H16D H 0.5942 0.2417 -0.1829 0.118 Uiso 0.50 1 calc PR A 2
H16E H 0.6181 0.3046 -0.1099 0.118 Uiso 0.50 1 calc PR A 2
H16F H 0.6262 0.1861 -0.1072 0.118 Uiso 0.50 1 calc PR A 2
C17A C 0.7641(10) 0.3478(8) -0.1895(7) 0.094(4) Uiso 0.50 1 d PDU A 2
H17D H 0.7165 0.3421 -0.2359 0.141 Uiso 0.50 1 calc PR A 2
H17E H 0.8366 0.3524 -0.1975 0.141 Uiso 0.50 1 calc PR A 2
H17F H 0.7466 0.4075 -0.1645 0.141 Uiso 0.50 1 calc PR A 2
C18A C 0.7862(9) 0.1576(8) -0.1815(7) 0.087(4) Uiso 0.50 1 d PDU A 2
H18D H 0.7404 0.1506 -0.2286 0.130 Uiso 0.50 1 calc PR A 2
H18E H 0.7806 0.0982 -0.1526 0.130 Uiso 0.50 1 calc PR A 2
H18F H 0.8590 0.1657 -0.1883 0.130 Uiso 0.50 1 calc PR A 2
C19 C 1.0757(3) 0.3128(3) 0.0642(2) 0.0453(11) Uani 1 1 d . . .
C20 C 1.0694(4) 0.3933(3) 0.1235(2) 0.0643(13) Uani 1 1 d . . .
H20A H 1.0299 0.4509 0.1015 0.096 Uiso 1 1 calc R . .
H20B H 1.1405 0.4140 0.1455 0.096 Uiso 1 1 calc R . .
H20C H 1.0339 0.3652 0.1606 0.096 Uiso 1 1 calc R . .
C21 C 1.1327(3) 0.2189(3) 0.1004(3) 0.0624(13) Uani 1 1 d . . .
H21A H 1.0950 0.1939 0.1373 0.094 Uiso 1 1 calc R . .
H21B H 1.2047 0.2363 0.1227 0.094 Uiso 1 1 calc R . .
H21C H 1.1343 0.1675 0.0639 0.094 Uiso 1 1 calc R . .
C22 C 1.1453(3) 0.3567(4) 0.0119(3) 0.0790(17) Uani 1 1 d . . .
H22A H 1.1522 0.3076 -0.0253 0.119 Uiso 1 1 calc R . .
H22B H 1.2149 0.3730 0.0391 0.119 Uiso 1 1 calc R . .
H22C H 1.1122 0.4169 -0.0109 0.119 Uiso 1 1 calc R . .
C23 C 0.8625(3) 0.2426(3) 0.12322(19) 0.0346(9) Uani 1 1 d . . .
H23 H 0.9292 0.2194 0.1540 0.041 Uiso 1 1 calc R . .
C24 C 0.8306(3) 0.3439(3) 0.1539(2) 0.0368(9) Uani 1 1 d . . .
C25 C 0.7303(3) 0.5007(3) 0.1156(2) 0.0392(9) Uani 1 1 d . . .
C26 C 0.7740(3) 0.5636(3) 0.1731(2) 0.0445(10) Uani 1 1 d . . .
H26 H 0.8353 0.5442 0.2056 0.053 Uiso 1 1 calc R . .
C27 C 0.7257(4) 0.6557(3) 0.1819(2) 0.0499(11) Uani 1 1 d . . .
H27 H 0.7548 0.6978 0.2207 0.060 Uiso 1 1 calc R . .
C28 C 0.6365(4) 0.6856(3) 0.1348(2) 0.0556(12) Uani 1 1 d . . .
H28 H 0.6046 0.7475 0.1414 0.067 Uiso 1 1 calc R . .
C29 C 0.5938(4) 0.6237(3) 0.0776(3) 0.0651(13) Uani 1 1 d . . .
H29 H 0.5329 0.6440 0.0451 0.078 Uiso 1 1 calc R . .
C30 C 0.6404(3) 0.5313(3) 0.0678(2) 0.0537(12) Uani 1 1 d . . .
H30 H 0.6107 0.4898 0.0288 0.064 Uiso 1 1 calc R . .
H5 H 0.759(3) 0.384(3) 0.065(2) 0.032(12) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.362(4) . ?
N1 C3 1.377(4) . ?
N1 C23 1.446(4) . ?
N2 C1 1.325(5) . ?
N3 N4 1.361(4) . ?
N3 C14 1.374(4) . ?
N3 C23 1.474(4) . ?
N4 C12 1.320(4) . ?
N5 C24 1.349(5) . ?
N5 C25 1.406(5) . ?
O1 C24 1.213(4) . ?
C1 C2 1.403(5) . ?
C1 C4 1.515(5) . ?
C2 C3 1.362(5) . ?
C3 C8 1.517(5) . ?
C4 C7 1.497(6) . ?
C4 C5 1.504(6) . ?
C4 C6 1.525(6) . ?
C8 C9 1.529(5) . ?
C8 C11 1.537(5) . ?
C8 C10 1.539(5) . ?
C12 C13 1.395(5) . ?
C12 C15 1.507(5) . ?
C13 C14 1.366(5) . ?
C14 C19 1.506(5) . ?
C15 C16A 1.479(10) . ?
C15 C18 1.521(9) . ?
C15 C17 1.527(10) . ?
C15 C16 1.553(9) . ?
C15 C18A 1.552(10) . ?
C15 C17A 1.571(10) . ?
C19 C21 1.528(6) . ?
C19 C22 1.536(5) . ?
C19 C20 1.540(6) . ?
C23 C24 1.535(5) . ?
C25 C30 1.373(5) . ?
C25 C26 1.385(5) . ?
C26 C27 1.384(5) . ?
C27 C28 1.357(6) . ?
C28 C29 1.369(6) . ?
C29 C30 1.381(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C3 112.0(3) . . ?
N2 N1 C23 115.3(3) . . ?
C3 N1 C23 132.5(3) . . ?
C1 N2 N1 105.4(3) . . ?
N4 N3 C14 112.9(3) . . ?
N4 N3 C23 116.5(3) . . ?
C14 N3 C23 129.6(3) . . ?
C12 N4 N3 104.7(3) . . ?
C24 N5 C25 127.2(4) . . ?
N2 C1 C2 110.2(3) . . ?
N2 C1 C4 119.8(4) . . ?
C2 C1 C4 130.0(4) . . ?
C3 C2 C1 107.5(3) . . ?
C2 C3 N1 104.8(3) . . ?
C2 C3 C8 128.8(4) . . ?
N1 C3 C8 126.3(3) . . ?
C7 C4 C5 110.5(5) . . ?
C7 C4 C1 109.5(4) . . ?
C5 C4 C1 109.5(4) . . ?
C7 C4 C6 108.3(4) . . ?
C5 C4 C6 108.2(4) . . ?
C1 C4 C6 110.8(4) . . ?
C3 C8 C9 108.4(3) . . ?
C3 C8 C11 110.6(3) . . ?
C9 C8 C11 108.0(3) . . ?
C3 C8 C10 111.2(3) . . ?
C9 C8 C10 107.5(3) . . ?
C11 C8 C10 111.0(3) . . ?
N4 C12 C13 110.7(3) . . ?
N4 C12 C15 120.7(4) . . ?
C13 C12 C15 128.6(4) . . ?
C14 C13 C12 107.8(4) . . ?
C13 C14 N3 103.9(3) . . ?
C13 C14 C19 129.0(3) . . ?
N3 C14 C19 127.1(3) . . ?
C16A C15 C12 113.2(5) . . ?
C16A C15 C18 128.2(7) . . ?
C12 C15 C18 110.7(5) . . ?
C16A C15 C17 82.6(6) . . ?
C12 C15 C17 108.2(6) . . ?
C18 C15 C17 108.2(6) . . ?
C16A C15 C16 28.0(5) . . ?
C12 C15 C16 109.6(5) . . ?
C18 C15 C16 110.4(6) . . ?
C17 C15 C16 109.6(6) . . ?
C16A C15 C18A 111.0(7) . . ?
C12 C15 C18A 107.7(5) . . ?
C18 C15 C18A 27.3(5) . . ?
C17 C15 C18A 131.8(7) . . ?
C16 C15 C18A 87.1(6) . . ?
C16A C15 C17A 107.0(7) . . ?
C12 C15 C17A 109.8(6) . . ?
C18 C15 C17A 82.0(6) . . ?
C17 C15 C17A 28.2(5) . . ?
C16 C15 C17A 130.5(7) . . ?
C18A C15 C17A 108.1(6) . . ?
C14 C19 C21 111.5(3) . . ?
C14 C19 C22 108.6(3) . . ?
C21 C19 C22 107.6(4) . . ?
C14 C19 C20 112.5(3) . . ?
C21 C19 C20 109.2(3) . . ?
C22 C19 C20 107.3(4) . . ?
N1 C23 N3 111.4(3) . . ?
N1 C23 C24 107.3(3) . . ?
N3 C23 C24 113.0(3) . . ?
O1 C24 N5 125.5(4) . . ?
O1 C24 C23 119.8(3) . . ?
N5 C24 C23 114.6(3) . . ?
C30 C25 C26 119.3(4) . . ?
C30 C25 N5 118.9(4) . . ?
C26 C25 N5 121.8(4) . . ?
C27 C26 C25 119.5(4) . . ?
C28 C27 C26 121.1(4) . . ?
C27 C28 C29 119.4(4) . . ?
C28 C29 C30 120.6(4) . . ?
C25 C30 C29 120.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.054


#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
_shelx_title                     ' JA_ORG2 in P2(1)/n'
_shelx_refln_list_code           4
_shelx_F_calc_maximum            263.25
_reflns_d_resolution_high        0.8410

_shelx_F_squared_multiplier      1.000

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_14
_database_code_depnum_ccdc_archive 'CCDC 1033055'
_audit_update_record             
;
2014-11-06 deposited with the CCDC.
2014-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H56 Al N5 S'
_chemical_formula_sum            'C38 H56 Al N5 S'
_chemical_formula_weight         641.92

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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/n

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

_cell_length_a                   16.770(13)
_cell_length_b                   11.023(9)
_cell_length_c                   22.285(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.369(19)
_cell_angle_gamma                90.00
_cell_volume                     3862(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    317
_cell_measurement_theta_min      2.256
_cell_measurement_theta_max      13.139

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20770
_diffrn_reflns_av_R_equivalents  0.2168
_diffrn_reflns_av_sigmaI/netI    0.2792
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6771
_reflns_number_gt                1669
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_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 F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.1167P)²+0.0000P] where P=(Fo²+2Fc²)/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         6771
_refine_ls_number_parameters     454
_refine_ls_number_restraints     382
_refine_ls_R_factor_all          0.2980
_refine_ls_R_factor_gt           0.0725
_refine_ls_wR_factor_ref         0.2864
_refine_ls_wR_factor_gt          0.1648
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_restrained_S_all      0.790
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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
Al1 Al 0.59504(14) 0.2202(2) 0.39827(11) 0.0726(8) Uani 1 1 d DU . .
S1 S 0.77098(13) -0.10341(19) 0.43436(10) 0.0740(7) Uani 1 1 d U A .
N1 N 0.7812(4) 0.2304(5) 0.4305(3) 0.0547(16) Uani 1 1 d U . .
N2 N 0.7061(4) 0.2937(6) 0.4007(3) 0.0609(17) Uani 1 1 d U A .
N3 N 0.7732(4) 0.3127(6) 0.5335(3) 0.0625(17) Uani 1 1 d U A .
N4 N 0.7675(3) 0.1868(6) 0.5317(3) 0.0566(16) Uani 1 1 d U . .
N5 N 0.6431(4) 0.0600(5) 0.4099(3) 0.0580(16) Uani 1 1 d U A .
C1 C 0.7295(6) 0.3935(8) 0.3775(3) 0.066(2) Uani 1 1 d U . .
C2 C 0.8172(6) 0.3931(7) 0.3917(3) 0.069(2) Uani 1 1 d U A .
H2 H 0.8482 0.4521 0.3797 0.082 Uiso 1 1 calc R . .
C3 C 0.8499(5) 0.2913(7) 0.4264(3) 0.058(2) Uani 1 1 d U A .
C4 C 0.6700(6) 0.4941(8) 0.3389(4) 0.093(3) Uani 1 1 d U A .
C5 C 0.6001(7) 0.5184(9) 0.3689(5) 0.134(4) Uani 1 1 d U . .
H5A H 0.5569 0.5700 0.3410 0.200 Uiso 1 1 calc R A .
H5B H 0.6254 0.5574 0.4097 0.200 Uiso 1 1 calc R . .
H5C H 0.5751 0.4428 0.3745 0.200 Uiso 1 1 calc R . .
C6 C 0.6288(6) 0.4550(8) 0.2691(4) 0.110(3) Uani 1 1 d U . .
H6A H 0.6716 0.4489 0.2498 0.165 Uiso 1 1 calc R A .
H6B H 0.5871 0.5140 0.2464 0.165 Uiso 1 1 calc R . .
H6C H 0.6018 0.3776 0.2673 0.165 Uiso 1 1 calc R . .
C7 C 0.7207(7) 0.6112(8) 0.3418(4) 0.130(4) Uani 1 1 d U . .
H7A H 0.7625 0.5978 0.3220 0.195 Uiso 1 1 calc R A .
H7B H 0.7486 0.6344 0.3857 0.195 Uiso 1 1 calc R . .
H7C H 0.6828 0.6747 0.3195 0.195 Uiso 1 1 calc R . .
C8 C 0.9412(5) 0.2482(7) 0.4534(4) 0.067(2) Uani 1 1 d U . .
C9 C 0.9523(5) 0.1241(7) 0.4275(4) 0.084(3) Uani 1 1 d U A .
H9A H 0.9141 0.0673 0.4359 0.125 Uiso 1 1 calc R . .
H9B H 1.0098 0.0971 0.4480 0.125 Uiso 1 1 calc R . .
H9C H 0.9400 0.1296 0.3822 0.125 Uiso 1 1 calc R . .
C10 C 0.9745(5) 0.2495(7) 0.5270(3) 0.084(3) Uani 1 1 d U A .
H10A H 0.9459 0.1880 0.5424 0.126 Uiso 1 1 calc R . .
H10B H 0.9639 0.3275 0.5419 0.126 Uiso 1 1 calc R . .
H10C H 1.0346 0.2337 0.5427 0.126 Uiso 1 1 calc R . .
C11 C 0.9965(5) 0.3385(8) 0.4319(4) 0.099(3) Uani 1 1 d U A .
H11A H 1.0540 0.3095 0.4455 0.148 Uiso 1 1 calc R . .
H11B H 0.9952 0.4165 0.4508 0.148 Uiso 1 1 calc R . .
H11C H 0.9746 0.3457 0.3862 0.148 Uiso 1 1 calc R . .
C12 C 0.7665(4) 0.1398(7) 0.5895(4) 0.059(2) Uani 1 1 d U A .
C13 C 0.7681(4) 0.2406(8) 0.6260(4) 0.066(2) Uani 1 1 d U . .
H13 H 0.7662 0.2403 0.6672 0.080 Uiso 1 1 calc R A .
C14 C 0.7729(4) 0.3434(8) 0.5913(4) 0.059(2) Uani 1 1 d U A .
C15 C 0.7679(5) 0.0068(7) 0.6085(4) 0.062(2) Uani 1 1 d U . .
C16 C 0.8486(4) -0.0577(7) 0.6066(4) 0.075(2) Uani 1 1 d U A .
H16A H 0.8471 -0.0619 0.5632 0.113 Uiso 1 1 calc R . .
H16B H 0.8509 -0.1383 0.6235 0.113 Uiso 1 1 calc R . .
H16C H 0.8980 -0.0132 0.6320 0.113 Uiso 1 1 calc R . .
C17 C 0.7689(5) 0.0026(7) 0.6787(3) 0.088(3) Uani 1 1 d U A .
H17A H 0.7715 -0.0803 0.6925 0.132 Uiso 1 1 calc R . .
H17B H 0.7180 0.0396 0.6806 0.132 Uiso 1 1 calc R . .
H17C H 0.8177 0.0457 0.7061 0.132 Uiso 1 1 calc R . .
C18 C 0.6870(4) -0.0597(6) 0.5680(3) 0.071(2) Uani 1 1 d U A .
H18A H 0.6879 -0.0718 0.5256 0.106 Uiso 1 1 calc R . .
H18B H 0.6382 -0.0122 0.5660 0.106 Uiso 1 1 calc R . .
H18C H 0.6843 -0.1369 0.5872 0.106 Uiso 1 1 calc R . .
C19 C 0.7789(5) 0.4736(8) 0.6126(4) 0.076(2) Uani 1 1 d U . .
C20 C 0.7594(6) 0.5582(8) 0.5554(4) 0.123(4) Uani 1 1 d U A .
H20A H 0.7974 0.5412 0.5327 0.184 Uiso 1 1 calc R . .
H20B H 0.7667 0.6408 0.5700 0.184 Uiso 1 1 calc R . .
H20C H 0.7018 0.5460 0.5274 0.184 Uiso 1 1 calc R . .
C21 C 0.8701(6) 0.4999(8) 0.6571(5) 0.137(4) Uani 1 1 d U A .
H21A H 0.8818 0.4553 0.6962 0.205 Uiso 1 1 calc R . .
H21B H 0.8763 0.5851 0.6664 0.205 Uiso 1 1 calc R . .
H21C H 0.9092 0.4757 0.6365 0.205 Uiso 1 1 calc R . .
C22 C 0.7179(7) 0.4988(9) 0.6482(5) 0.136(4) Uani 1 1 d U A .
H22A H 0.6621 0.4707 0.6231 0.204 Uiso 1 1 calc R . .
H22B H 0.7160 0.5845 0.6553 0.204 Uiso 1 1 calc R . .
H22C H 0.7372 0.4573 0.6886 0.204 Uiso 1 1 calc R . .
C23 C 0.7827(4) 0.1318(6) 0.4748(3) 0.0536(19) Uani 1 1 d U A .
H23 H 0.8407 0.0994 0.4902 0.064 Uiso 1 1 calc R . .
C24 C 0.7244(5) 0.0289(6) 0.4381(3) 0.0547(19) Uani 1 1 d U . .
C25 C 0.5838(5) -0.0349(7) 0.3740(4) 0.061(2) Uani 1 1 d U . .
C26 C 0.5280(5) -0.0841(8) 0.3990(4) 0.075(2) Uani 1 1 d U A .
H26 H 0.5306 -0.0616 0.4399 0.090 Uiso 1 1 calc R . .
C27 C 0.4664(5) -0.1686(8) 0.3642(5) 0.082(3) Uani 1 1 d U . .
H27 H 0.4279 -0.2007 0.3816 0.098 Uiso 1 1 calc R A .
C28 C 0.4636(5) -0.2030(7) 0.3050(5) 0.081(3) Uani 1 1 d U A .
H28 H 0.4227 -0.2590 0.2824 0.097 Uiso 1 1 calc R . .
C29 C 0.5202(5) -0.1572(8) 0.2768(4) 0.068(2) Uani 1 1 d U . .
C30 C 0.5818(5) -0.0701(8) 0.3122(4) 0.068(2) Uani 1 1 d U A .
C31 C 0.6390(5) -0.0216(8) 0.2843(4) 0.085(3) Uani 1 1 d U . .
H31 H 0.6792 0.0358 0.3064 0.102 Uiso 1 1 calc R A .
C32 C 0.6350(5) -0.0593(9) 0.2249(4) 0.096(3) Uani 1 1 d U A .
H32 H 0.6727 -0.0275 0.2066 0.116 Uiso 1 1 calc R . .
C33 C 0.5754(7) -0.1443(10) 0.1916(5) 0.104(4) Uani 1 1 d U . .
H33 H 0.5743 -0.1698 0.1515 0.124 Uiso 1 1 calc R A .
C34 C 0.5196(6) -0.1904(9) 0.2156(5) 0.097(3) Uani 1 1 d U A .
H34 H 0.4794 -0.2458 0.1915 0.116 Uiso 1 1 calc R . .
C35 C 0.5039(16) 0.217(5) 0.3138(14) 0.106(8) Uani 0.50 1 d PDU A 1
H35A H 0.5265 0.2591 0.2849 0.128 Uiso 0.50 1 calc PR A 1
H35B H 0.4975 0.1329 0.3005 0.128 Uiso 0.50 1 calc PR A 1
C36 C 0.4173(14) 0.264(2) 0.2994(14) 0.138(9) Uani 0.50 1 d PDU A 1
H36A H 0.3926 0.2817 0.2545 0.206 Uiso 0.50 1 calc PR A 1
H36B H 0.4192 0.3367 0.3236 0.206 Uiso 0.50 1 calc PR A 1
H36C H 0.3834 0.2041 0.3107 0.206 Uiso 0.50 1 calc PR A 1
C37 C 0.569(3) 0.279(4) 0.4732(17) 0.102(10) Uani 0.50 1 d PDU A 1
H37A H 0.5572 0.2049 0.4925 0.123 Uiso 0.50 1 calc PR A 1
H37B H 0.6230 0.3077 0.5023 0.123 Uiso 0.50 1 calc PR A 1
C38 C 0.5108(19) 0.361(3) 0.4807(15) 0.132(11) Uani 0.50 1 d PDU A 1
H38A H 0.5174 0.3662 0.5252 0.198 Uiso 0.50 1 calc PR A 1
H38B H 0.4542 0.3342 0.4566 0.198 Uiso 0.50 1 calc PR A 1
H38C H 0.5206 0.4389 0.4656 0.198 Uiso 0.50 1 calc PR A 1
C35A C 0.5083(16) 0.235(5) 0.3112(13) 0.100(7) Uani 0.50 1 d PDU A 2
H35C H 0.5000 0.3196 0.2996 0.120 Uiso 0.50 1 calc PR A 2
H35D H 0.5293 0.1947 0.2808 0.120 Uiso 0.50 1 calc PR A 2
C36A C 0.4254(12) 0.1804(18) 0.3064(12) 0.098(7) Uani 0.50 1 d PDU A 2
H36D H 0.3904 0.1726 0.2622 0.147 Uiso 0.50 1 calc PR A 2
H36E H 0.3976 0.2317 0.3278 0.147 Uiso 0.50 1 calc PR A 2
H36F H 0.4347 0.1017 0.3262 0.147 Uiso 0.50 1 calc PR A 2
C37A C 0.551(3) 0.241(4) 0.4702(16) 0.093(9) Uani 0.50 1 d PDU A 2
H37C H 0.5384 0.1606 0.4819 0.112 Uiso 0.50 1 calc PR A 2
H37D H 0.5982 0.2718 0.5064 0.112 Uiso 0.50 1 calc PR A 2
C38A C 0.4819(16) 0.313(3) 0.4639(14) 0.110(8) Uani 0.50 1 d PDU A 2
H38D H 0.4697 0.3110 0.5028 0.164 Uiso 0.50 1 calc PR A 2
H38E H 0.4337 0.2837 0.4292 0.164 Uiso 0.50 1 calc PR A 2
H38F H 0.4940 0.3951 0.4552 0.164 Uiso 0.50 1 calc PR A 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
Al1 N5 1.921(6) . ?
Al1 C35 1.97(2) . ?
Al1 C35A 1.98(2) . ?
Al1 C37A 1.99(2) . ?
Al1 C37 1.98(2) . ?
Al1 N2 2.015(7) . ?
S1 C24 1.669(7) . ?
N1 C3 1.364(8) . ?
N1 N2 1.389(7) . ?
N1 C23 1.463(8) . ?
N2 C1 1.332(9) . ?
N3 C14 1.333(8) . ?
N3 N4 1.391(7) . ?
N4 C12 1.394(8) . ?
N4 C23 1.504(8) . ?
N5 C24 1.333(8) . ?
N5 C25 1.473(9) . ?
C1 C2 1.392(10) . ?
C1 C4 1.539(10) . ?
C2 C3 1.364(9) . ?
C3 C8 1.513(10) . ?
C4 C6 1.527(11) . ?
C4 C5 1.561(12) . ?
C4 C7 1.536(11) . ?
C8 C9 1.521(9) . ?
C8 C10 1.537(9) . ?
C8 C11 1.547(9) . ?
C12 C13 1.372(9) . ?
C12 C15 1.523(10) . ?
C13 C14 1.389(9) . ?
C14 C19 1.504(10) . ?
C15 C18 1.529(9) . ?
C15 C16 1.542(9) . ?
C15 C17 1.559(10) . ?
C19 C21 1.533(11) . ?
C19 C22 1.521(11) . ?
C19 C20 1.521(11) . ?
C23 C24 1.534(9) . ?
C25 C26 1.358(9) . ?
C25 C30 1.419(10) . ?
C26 C27 1.407(10) . ?
C27 C28 1.357(10) . ?
C28 C29 1.402(10) . ?
C29 C34 1.410(11) . ?
C29 C30 1.430(10) . ?
C30 C31 1.418(10) . ?
C31 C32 1.367(10) . ?
C32 C33 1.383(12) . ?
C33 C34 1.329(12) . ?
C35 C36 1.47(3) . ?
C37 C38 1.38(2) . ?
C35A C36A 1.48(3) . ?
C37A C38A 1.38(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Al1 C35 105.3(17) . . ?
N5 Al1 C35A 109.6(18) . . ?
C35 Al1 C35A 6(3) . . ?
N5 Al1 C37A 104.5(13) . . ?
C35 Al1 C37A 113.0(17) . . ?
C35A Al1 C37A 115.3(17) . . ?
N5 Al1 C37 113.1(14) . . ?
C35 Al1 C37 119.0(17) . . ?
C35A Al1 C37 119.8(19) . . ?
C37A Al1 C37 14(3) . . ?
N5 Al1 N2 91.5(3) . . ?
C35 Al1 N2 115.8(12) . . ?
C35A Al1 N2 110.5(10) . . ?
C37A Al1 N2 121.8(14) . . ?
C37 Al1 N2 108.8(13) . . ?
C3 N1 N2 111.5(6) . . ?
C3 N1 C23 126.5(6) . . ?
N2 N1 C23 119.7(6) . . ?
C1 N2 N1 105.1(6) . . ?
C1 N2 Al1 135.8(6) . . ?
N1 N2 Al1 119.1(5) . . ?
C14 N3 N4 105.0(6) . . ?
N3 N4 C12 111.5(6) . . ?
N3 N4 C23 113.4(6) . . ?
C12 N4 C23 133.5(7) . . ?
C24 N5 C25 117.4(6) . . ?
C24 N5 Al1 127.8(5) . . ?
C25 N5 Al1 114.1(4) . . ?
N2 C1 C2 109.8(7) . . ?
N2 C1 C4 126.2(8) . . ?
C2 C1 C4 124.0(9) . . ?
C3 C2 C1 108.5(7) . . ?
N1 C3 C2 105.1(7) . . ?
N1 C3 C8 125.4(7) . . ?
C2 C3 C8 129.5(8) . . ?
C1 C4 C6 110.0(7) . . ?
C1 C4 C5 108.8(8) . . ?
C6 C4 C5 110.1(8) . . ?
C1 C4 C7 109.8(8) . . ?
C6 C4 C7 109.1(8) . . ?
C5 C4 C7 109.0(8) . . ?
C3 C8 C9 111.8(6) . . ?
C3 C8 C10 111.4(6) . . ?
C9 C8 C10 111.5(7) . . ?
C3 C8 C11 107.9(7) . . ?
C9 C8 C11 107.1(6) . . ?
C10 C8 C11 106.8(6) . . ?
C13 C12 N4 104.0(7) . . ?
C13 C12 C15 128.3(8) . . ?
N4 C12 C15 127.6(7) . . ?
C12 C13 C14 108.9(7) . . ?
N3 C14 C13 110.5(7) . . ?
N3 C14 C19 121.7(8) . . ?
C13 C14 C19 127.8(8) . . ?
C12 C15 C18 111.9(6) . . ?
C12 C15 C16 111.5(6) . . ?
C18 C15 C16 111.7(6) . . ?
C12 C15 C17 107.6(6) . . ?
C18 C15 C17 105.9(6) . . ?
C16 C15 C17 108.1(6) . . ?
C14 C19 C21 109.0(7) . . ?
C14 C19 C22 110.8(7) . . ?
C21 C19 C22 109.2(8) . . ?
C14 C19 C20 110.5(7) . . ?
C21 C19 C20 107.5(8) . . ?
C22 C19 C20 109.7(8) . . ?
N1 C23 N4 107.5(6) . . ?
N1 C23 C24 109.3(5) . . ?
N4 C23 C24 119.0(6) . . ?
N5 C24 C23 114.7(6) . . ?
N5 C24 S1 128.4(5) . . ?
C23 C24 S1 116.8(5) . . ?
C26 C25 C30 120.2(7) . . ?
C26 C25 N5 119.4(7) . . ?
C30 C25 N5 120.3(7) . . ?
C25 C26 C27 121.1(8) . . ?
C28 C27 C26 119.4(8) . . ?
C27 C28 C29 122.4(8) . . ?
C28 C29 C34 124.3(9) . . ?
C28 C29 C30 117.8(8) . . ?
C34 C29 C30 117.9(9) . . ?
C25 C30 C31 122.2(8) . . ?
C25 C30 C29 119.1(8) . . ?
C31 C30 C29 118.7(8) . . ?
C32 C31 C30 119.9(8) . . ?
C31 C32 C33 120.5(9) . . ?
C34 C33 C32 121.5(10) . . ?
C33 C34 C29 121.4(10) . . ?
C36 C35 Al1 126(3) . . ?
C38 C37 Al1 134(3) . . ?
C36A C35A Al1 113(2) . . ?
C38A C37A Al1 121(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.049


#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
_shelx_title                     ' JA_26 in P2/n'
_shelx_refln_list_code           4
_shelx_F_calc_maximum            273.34
_reflns_d_resolution_high        0.8409


_shelx_F_squared_multiplier      1.000




# start Validation Reply Form
_vrf_PLAT026_14                  
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         25 %    
RESPONSE: 
For this alert and related: 
Only crystals of low quality and very weakly diffracting 
could be grown but we considered that the data were of sufficient quality 
to determine the molecular structure.
;
_vrf_RINTA01_14                  
;
PROBLEM:  The value of Rint is greater than 0.18     Rint given   0.217
RESPONSE: For this alert and related: Quality of the data was poor due 
to the crystal quality and also the crystal is thin and very weakly 
diffracting, so that a large proportion of essentially unobserved 
reflections were used in the refinement.
;
_vrf_PLAT340_14                  
;
PROBLEM:  Low Bond Precision on  C-C Bonds ...............     0.0126 Ang.  
RESPONSE: This alert can be due to the poor quality of the data and to the 
disorder show in the ethyl groups
;
# end Validation Reply Form

