# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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data_DAla-mACHC-DAla_moon200
_database_code_depnum_ccdc_archive 'CCDC 1448797'
_audit_update_record             
;
2016-01-21 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_audit_creation_date             2014-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H35 N3 O6'
_chemical_formula_sum            'C20 H35 N3 O6'
_chemical_formula_weight         413.51
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.1953(5)
_cell_length_b                   15.9688(8)
_cell_length_c                   16.3770(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2404.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0727 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.7417.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.097
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_min         2.487
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3935
_reflns_number_total             4720
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 
;
 Flack x determined using 1525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0326P)²+0.4296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0779
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5(0.025) H13(0.024) H16(0.026) H1A(0.071) H1B(0.071) H1C(0.071)
 H4(0.028) H7(0.027) H8A(0.036) H8B(0.036) H9A(0.038) H9B(0.038) H10(0.036)
 H11A(0.028) H11B(0.028) H12(0.026) H15(0.024) H20A(0.05) H20B(0.05) H20C(0.05)
 H21A(0.049) H21B(0.049) H21C(0.049) H22A(0.05) H22B(0.05) H22C(0.05)
 H24A(0.042) H24B(0.042) H24C(0.042) H26A(0.065) H26B(0.065) H26C(0.065)
 H28A(0.04) H28B(0.04) H28C(0.04)
 Fixed X: H5(0.6699) H13(0.5941) H16(0.3121) H1A(0.3471) H1B(0.311)
 H1C(0.4551) H4(0.6542) H7(0.854) H8A(1.0782) H8B(1.0818) H9A(1.0609)
 H9B(1.1935) H10(1.05) H11A(0.814) H11B(0.8058) H12(0.8443) H15(0.3907)
 H20A(0.2827) H20B(0.415) H20C(0.4209) H21A(0.6574) H21B(0.6532) H21C(0.6708)
 H22A(0.4494) H22B(0.4221) H22C(0.2971) H24A(0.4174) H24B(0.4253) H24C(0.5335)
 H26A(1.0315) H26B(1.0155) H26C(1.1678) H28A(0.3719) H28B(0.3518) H28C(0.2323)
 Fixed Y: H5(0.3934) H13(0.2) H16(0.3004) H1A(0.3063) H1B(0.2629) H1C(0.2374)
 H4(0.4318) H7(0.3245) H8A(0.3325) H8B(0.2683) H9A(0.2246) H9B(0.2028)
 H10(0.1076) H11A(0.151) H11B(0.0798) H12(0.1812) H15(0.2541) H20A(0.548)
 H20B(0.6118) H20C(0.5204) H21A(0.4902) H21B(0.5832) H21C(0.5048) H22A(0.5392)
 H22B(0.6225) H22C(0.5531) H24A(0.4408) H24B(0.4897) H24C(0.5143) H26A(0.0725)
 H26B(0.0036) H26C(0.0501) H28A(0.1418) H28B(0.1159) H28C(0.1731)
 Fixed Z: H5(0.2845) H13(0.2749) H16(0.4777) H1A(-0.0367) H1B(0.0491)
 H1C(0.0002) H4(0.1256) H7(0.3406) H8A(0.2632) H8B(0.338) H9A(0.169)
 H9B(0.2286) H10(0.3014) H11A(0.1945) H11B(0.2633) H12(0.3659) H15(0.3298)
 H20A(0.5718) H20B(0.5847) H20C(0.6247) H21A(0.5546) H21B(0.5182) H21C(0.4582)
 H22A(0.3765) H22B(0.4286) H22C(0.4217) H24A(0.2392) H24B(0.154) H24C(0.2266)
 H26A(0.1304) H26B(0.2008) H26C(0.1871) H28A(0.4665) H28B(0.3727) H28C(0.4167)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.4690(2) 0.34881(10) 0.05562(10) 0.0350(5) Uani 1 1 d . U . . .
O18 O 0.41367(17) 0.43043(9) 0.50032(9) 0.0239(4) Uani 1 1 d . U . . .
O23 O 0.49311(18) 0.26369(10) 0.16381(9) 0.0304(4) Uani 1 1 d . U . . .
O25 O 0.83673(19) 0.30914(10) 0.14758(9) 0.0290(4) Uani 1 1 d . U . . .
O27 O 0.64422(18) 0.22003(11) 0.45701(9) 0.0296(4) Uani 1 1 d . U . . .
O29 O 0.54638(19) 0.39691(9) 0.38721(9) 0.0270(4) Uani 1 1 d . U . . .
N5 N 0.6867(2) 0.37670(11) 0.23419(11) 0.0209(4) Uani 1 1 d . U . . .
H5 H 0.6699 0.3934 0.2845 0.025 Uiso 1 1 calc R . . . .
N13 N 0.6478(2) 0.20633(11) 0.31899(11) 0.0203(4) Uani 1 1 d . U . . .
H13 H 0.5941 0.2000 0.2749 0.024 Uiso 1 1 calc R . . . .
N16 N 0.3825(2) 0.30689(11) 0.44189(11) 0.0215(4) Uani 1 1 d . U . . .
H16 H 0.3121 0.3004 0.4777 0.026 Uiso 1 1 calc R . . . .
C1 C 0.3891(4) 0.28359(17) 0.01367(17) 0.0476(8) Uani 1 1 d . U . . .
H1A H 0.3471 0.3063 -0.0367 0.071 Uiso 1 1 calc GR . . . .
H1B H 0.3110 0.2629 0.0491 0.071 Uiso 1 1 calc GR . . . .
H1C H 0.4551 0.2374 0.0002 0.071 Uiso 1 1 calc GR . . . .
C3 C 0.5153(3) 0.33022(15) 0.13072(13) 0.0247(5) Uani 1 1 d . U . . .
C4 C 0.5930(3) 0.40447(14) 0.16847(14) 0.0231(5) Uani 1 1 d . U . . .
H4 H 0.6542 0.4318 0.1256 0.028 Uiso 1 1 calc R . . . .
C6 C 0.7995(3) 0.32536(14) 0.21843(13) 0.0213(5) Uani 1 1 d . U . . .
C7 C 0.8735(2) 0.28714(14) 0.29286(14) 0.0223(5) Uani 1 1 d . U . . .
H7 H 0.8540 0.3245 0.3406 0.027 Uiso 1 1 calc R . . . .
C8 C 1.0388(3) 0.27872(16) 0.28350(16) 0.0303(6) Uani 1 1 d . U . . .
H8A H 1.0782 0.3325 0.2632 0.036 Uiso 1 1 calc R . . . .
H8B H 1.0818 0.2683 0.3380 0.036 Uiso 1 1 calc R . . . .
C9 C 1.0865(3) 0.20882(16) 0.22571(16) 0.0319(6) Uani 1 1 d . U . . .
H9A H 1.0609 0.2246 0.1690 0.038 Uiso 1 1 calc R . . . .
H9B H 1.1935 0.2028 0.2286 0.038 Uiso 1 1 calc R . . . .
C10 C 1.0161(3) 0.12479(15) 0.24583(15) 0.0297(6) Uani 1 1 d . U . . .
H10 H 1.0500 0.1076 0.3014 0.036 Uiso 1 1 calc R . . . .
C11 C 0.8504(3) 0.13431(15) 0.24903(14) 0.0236(5) Uani 1 1 d . U . . .
H11A H 0.8140 0.1510 0.1945 0.028 Uiso 1 1 calc R . . . .
H11B H 0.8058 0.0798 0.2633 0.028 Uiso 1 1 calc R . . . .
C12 C 0.8059(2) 0.19975(14) 0.31172(14) 0.0215(5) Uani 1 1 d . U . . .
H12 H 0.8443 0.1812 0.3659 0.026 Uiso 1 1 calc R . . . .
C14 C 0.5818(2) 0.22169(13) 0.39057(13) 0.0199(5) Uani 1 1 d . U . . .
C15 C 0.4188(2) 0.23867(13) 0.38688(13) 0.0201(5) Uani 1 1 d . U . . .
H15 H 0.3907 0.2541 0.3298 0.024 Uiso 1 1 calc R . . . .
C17 C 0.4545(3) 0.37933(13) 0.43869(13) 0.0212(5) Uani 1 1 d . U . . .
C19 C 0.4614(3) 0.51906(14) 0.50059(14) 0.0229(5) Uani 1 1 d . U . . .
C20 C 0.3885(3) 0.55283(15) 0.57726(15) 0.0331(6) Uani 1 1 d . U . . .
H20A H 0.2827 0.5480 0.5718 0.050 Uiso 1 1 calc GR . . . .
H20B H 0.4150 0.6118 0.5847 0.050 Uiso 1 1 calc GR . . . .
H20C H 0.4209 0.5204 0.6247 0.050 Uiso 1 1 calc GR . . . .
C21 C 0.6251(3) 0.52481(16) 0.50861(17) 0.0330(6) Uani 1 1 d . U . . .
H21A H 0.6574 0.4902 0.5546 0.049 Uiso 1 1 calc GR . . . .
H21B H 0.6532 0.5832 0.5182 0.049 Uiso 1 1 calc GR . . . .
H21C H 0.6708 0.5048 0.4582 0.049 Uiso 1 1 calc GR . . . .
C22 C 0.4023(3) 0.56227(16) 0.42517(15) 0.0335(6) Uani 1 1 d . U . . .
H22A H 0.4494 0.5392 0.3765 0.050 Uiso 1 1 calc GR . . . .
H22B H 0.4221 0.6225 0.4286 0.050 Uiso 1 1 calc GR . . . .
H22C H 0.2971 0.5531 0.4217 0.050 Uiso 1 1 calc GR . . . .
C24 C 0.4824(3) 0.46800(15) 0.19986(14) 0.0280(6) Uani 1 1 d . U . . .
H24A H 0.4174 0.4408 0.2392 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.4253 0.4897 0.1540 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.5335 0.5143 0.2266 0.042 Uiso 1 1 calc GR . . . .
C26 C 1.0618(3) 0.05666(17) 0.18565(18) 0.0435(7) Uani 1 1 d . U . . .
H26A H 1.0315 0.0725 0.1304 0.065 Uiso 1 1 calc GR . . . .
H26B H 1.0155 0.0036 0.2008 0.065 Uiso 1 1 calc GR . . . .
H26C H 1.1678 0.0501 0.1871 0.065 Uiso 1 1 calc GR . . . .
C28 C 0.3363(3) 0.16038(15) 0.41302(14) 0.0269(6) Uani 1 1 d . U . . .
H28A H 0.3719 0.1418 0.4665 0.040 Uiso 1 1 calc GR . . . .
H28B H 0.3518 0.1159 0.3727 0.040 Uiso 1 1 calc GR . . . .
H28C H 0.2323 0.1731 0.4167 0.040 Uiso 1 1 calc GR . . . .


_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
O2 C1 1.448(3) . ?
O2 C3 1.335(3) . ?
O18 C17 1.351(3) . ?
O18 C19 1.482(3) . ?
O23 C3 1.210(3) . ?
O25 C6 1.237(3) . ?
O27 C14 1.230(3) . ?
O29 C17 1.226(3) . ?
N5 C4 1.448(3) . ?
N5 C6 1.347(3) . ?
N13 C12 1.462(3) . ?
N13 C14 1.343(3) . ?
N16 C15 1.453(3) . ?
N16 C17 1.334(3) . ?
C3 C4 1.516(3) . ?
C4 C24 1.526(3) . ?
C6 C7 1.523(3) . ?
C7 C8 1.534(3) . ?
C7 C12 1.559(3) . ?
C8 C9 1.528(4) . ?
C9 C10 1.526(4) . ?
C10 C11 1.532(3) . ?
C10 C26 1.527(3) . ?
C11 C12 1.521(3) . ?
C14 C15 1.524(3) . ?
C15 C28 1.524(3) . ?
C19 C20 1.522(3) . ?
C19 C21 1.514(3) . ?
C19 C22 1.516(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O2 C1 116.1(2) . . ?
C17 O18 C19 119.78(17) . . ?
C6 N5 C4 120.13(18) . . ?
C14 N13 C12 122.24(19) . . ?
C17 N16 C15 120.78(18) . . ?
O2 C3 C4 110.6(2) . . ?
O23 C3 O2 123.6(2) . . ?
O23 C3 C4 125.7(2) . . ?
N5 C4 C3 110.11(18) . . ?
N5 C4 C24 110.46(18) . . ?
C3 C4 C24 110.10(19) . . ?
O25 C6 N5 121.3(2) . . ?
O25 C6 C7 122.9(2) . . ?
N5 C6 C7 115.74(19) . . ?
C6 C7 C8 113.4(2) . . ?
C6 C7 C12 109.84(18) . . ?
C8 C7 C12 109.66(19) . . ?
C9 C8 C7 114.2(2) . . ?
C10 C9 C8 112.8(2) . . ?
C9 C10 C11 110.0(2) . . ?
C9 C10 C26 111.7(2) . . ?
C26 C10 C11 111.5(2) . . ?
C12 C11 C10 111.0(2) . . ?
N13 C12 C7 110.37(18) . . ?
N13 C12 C11 111.83(19) . . ?
C11 C12 C7 111.96(18) . . ?
O27 C14 N13 123.9(2) . . ?
O27 C14 C15 119.8(2) . . ?
N13 C14 C15 116.3(2) . . ?
N16 C15 C14 109.58(18) . . ?
N16 C15 C28 109.06(18) . . ?
C28 C15 C14 109.41(19) . . ?
O29 C17 O18 124.5(2) . . ?
O29 C17 N16 124.6(2) . . ?
N16 C17 O18 110.87(19) . . ?
O18 C19 C20 102.15(18) . . ?
O18 C19 C21 110.66(19) . . ?
O18 C19 C22 109.02(19) . . ?
C21 C19 C20 110.2(2) . . ?
C21 C19 C22 113.6(2) . . ?
C22 C19 C20 110.7(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C3 C4 N5 -159.21(19) . . . . ?
O2 C3 C4 C24 78.8(2) . . . . ?
O23 C3 C4 N5 23.0(3) . . . . ?
O23 C3 C4 C24 -99.0(3) . . . . ?
O25 C6 C7 C8 38.6(3) . . . . ?
O25 C6 C7 C12 -84.5(3) . . . . ?
O27 C14 C15 N16 43.6(3) . . . . ?
O27 C14 C15 C28 -75.9(3) . . . . ?
N5 C6 C7 C8 -143.3(2) . . . . ?
N5 C6 C7 C12 93.5(2) . . . . ?
N13 C14 C15 N16 -138.64(19) . . . . ?
N13 C14 C15 C28 101.8(2) . . . . ?
C1 O2 C3 O23 -0.5(3) . . . . ?
C1 O2 C3 C4 -178.3(2) . . . . ?
C4 N5 C6 O25 9.0(3) . . . . ?
C4 N5 C6 C7 -169.06(19) . . . . ?
C6 N5 C4 C3 63.4(3) . . . . ?
C6 N5 C4 C24 -174.8(2) . . . . ?
C6 C7 C8 C9 -73.5(3) . . . . ?
C6 C7 C12 N13 -53.4(2) . . . . ?
C6 C7 C12 C11 71.9(2) . . . . ?
C7 C8 C9 C10 -51.5(3) . . . . ?
C8 C7 C12 N13 -178.71(18) . . . . ?
C8 C7 C12 C11 -53.4(2) . . . . ?
C8 C9 C10 C11 53.8(3) . . . . ?
C8 C9 C10 C26 178.2(2) . . . . ?
C9 C10 C11 C12 -57.8(3) . . . . ?
C10 C11 C12 N13 -176.75(19) . . . . ?
C10 C11 C12 C7 58.8(3) . . . . ?
C12 N13 C14 O27 -10.5(3) . . . . ?
C12 N13 C14 C15 171.92(19) . . . . ?
C12 C7 C8 C9 49.7(3) . . . . ?
C14 N13 C12 C7 -90.3(2) . . . . ?
C14 N13 C12 C11 144.4(2) . . . . ?
C15 N16 C17 O18 -173.64(18) . . . . ?
C15 N16 C17 O29 5.8(3) . . . . ?
C17 O18 C19 C20 178.29(19) . . . . ?
C17 O18 C19 C21 -64.4(3) . . . . ?
C17 O18 C19 C22 61.1(3) . . . . ?
C17 N16 C15 C14 51.5(3) . . . . ?
C17 N16 C15 C28 171.2(2) . . . . ?
C19 O18 C17 O29 10.8(3) . . . . ?
C19 O18 C17 N16 -169.82(18) . . . . ?
C26 C10 C11 C12 177.6(2) . . . . ?

####################################################################### 
# 
# 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/access/V1 
# 
# 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_DAla-ACHC_5mer_moon116
_database_code_depnum_ccdc_archive 'CCDC 1448798'
_audit_update_record             
;
2016-01-21 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_audit_creation_date             2014-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C29 H49 N5 O8'
_chemical_formula_sum            'C29 H49 N5 O8'
_chemical_formula_weight         595.73
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.7107(7)
_cell_length_b                   17.8054(12)
_cell_length_c                   18.6925(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3232.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.9523.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.840
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            200536
_diffrn_reflns_point_group_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.328
_diffrn_reflns_theta_min         2.179
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.825
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5036
_reflns_number_total             5268
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details 
;
 Flack x determined using 2117 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.06(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+0.8190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0686
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H1A(0.059) H1B(0.059) H1C(0.059) H4(0.035) H7(0.028) H8A(0.035)
 H8B(0.035) H9A(0.04) H9B(0.04) H10A(0.043) H10B(0.043) H11A(0.035) H11B(0.035)
 H12(0.028) H15(0.026) H18(0.028) H19A(0.036) H19B(0.036) H20A(0.045)
 H20B(0.045) H21A(0.041) H21B(0.041) H22A(0.036) H22B(0.036) H23(0.028)
 H26(0.032) H31A(0.086) H31B(0.086) H31C(0.086) H32A(0.075) H32B(0.075)
 H32C(0.075) H33A(0.066) H33B(0.066) H33C(0.066) H35A(0.065) H35B(0.065)
 H35C(0.065) H38A(0.052) H38B(0.052) H38C(0.052) H41A(0.059) H41B(0.059)
 H41C(0.059) H5(0.034) H13(0.026) H16(0.026) H24(0.028) H27(0.039)
 Fixed X: H1A(1.0383) H1B(1.058) H1C(1.1897) H4(1.0568) H7(0.672) H8A(0.854)
 H8B(0.7027) H9A(0.9096) H9B(0.852) H10A(0.634) H10B(0.75) H11A(0.7512)
 H11B(0.5981) H12(0.5345) H15(0.3757) H18(0.7241) H19A(0.5697) H19B(0.5443)
 H20A(0.6988) H20B(0.7985) H21A(0.8903) H21B(0.7483) H22A(0.9058) H22B(0.927)
 H23(0.7821) H26(0.518) H31A(0.0509) H31B(-0.0503) H31C(-0.0071) H32A(0.2906)
 H32B(0.1424) H32C(0.2379) H33A(0.0672) H33B(0.0365) H33C(0.1871) H35A(0.8761)
 H35B(1.0407) H35C(0.9641) H38A(0.5214) H38B(0.3612) H38C(0.4166) H41A(0.7143)
 H41B(0.744) H41C(0.6359) H5(0.7956) H13(0.6144) H16(0.6561) H24(0.6233)
 H27(0.4694)
 Fixed Y: H1A(0.8705) H1B(0.8536) H1C(0.8672) H4(1.086) H7(1.1423) H8A(1.1867)
 H8B(1.1891) H9A(1.0796) H9B(1.1419) H10A(1.0827) H10B(1.0235) H11A(0.9714)
 H11B(0.968) H12(1.0747) H15(0.9388) H18(0.8128) H19A(0.7275) H19B(0.6883)
 H20A(0.6139) H20B(0.6844) H21A(0.6101) H21B(0.6146) H22A(0.7014) H22B(0.7398)
 H23(0.8169) H26(0.6848) H31A(0.7875) H31B(0.8573) H31C(0.8052) H32A(0.9392)
 H32B(0.9407) H32C(0.8678) H33A(0.9187) H33B(0.9721) H33C(0.9702) H35A(1.0968)
 H35B(1.0952) H35C(1.1657) H38A(1.0345) H38B(1.0414) H38C(0.97) H41A(0.7611)
 H41B(0.6844) H41C(0.6857) H5(1.131) H13(0.9525) H16(0.9209) H24(0.692)
 H27(0.7987)
 Fixed Z: H1A(0.5749) H1B(0.6584) H1C(0.6086) H4(0.6802) H7(0.7773) H8A(0.856)
 H8B(0.8896) H9A(0.9223) H9B(0.9764) H10A(0.9782) H10B(1.0014) H11A(0.8848)
 H11B(0.9166) H12(0.8524) H15(0.6786) H18(0.5934) H19A(0.5427) H19B(0.6186)
 H20A(0.5529) H20B(0.5403) H21A(0.6326) H21B(0.6761) H22A(0.7251) H22B(0.6485)
 H23(0.7132) H26(0.8536) H31A(0.8205) H31B(0.8327) H31C(0.8988) H32A(0.8134)
 H32B(0.776) H32C(0.7693) H33A(0.9622) H33B(0.8952) H33C(0.9299) H35A(0.559)
 H35B(0.5544) H35C(0.5896) H38A(0.5825) H38B(0.6015) H38C(0.5582) H41A(0.9422)
 H41B(0.9003) H41C(0.9649) H5(0.6832) H13(0.7762) H16(0.6654) H24(0.7481)
 H27(0.9486)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0939(3) 0.88173(13) 0.61737(14) 0.0394(6) Uani 1 1 d . . . . .
H1A H 1.0383 0.8705 0.5749 0.059 Uiso 1 1 calc GR . . . .
H1B H 1.0580 0.8536 0.6584 0.059 Uiso 1 1 calc GR . . . .
H1C H 1.1897 0.8672 0.6086 0.059 Uiso 1 1 calc GR . . . .
C3 C 0.9618(2) 0.98836(12) 0.64501(10) 0.0248(5) Uani 1 1 d . . . . .
C4 C 0.9678(2) 1.07284(12) 0.65639(11) 0.0288(5) Uani 1 1 d . . . . .
H4 H 1.0568 1.0860 0.6802 0.035 Uiso 1 1 calc R . . . .
C6 C 0.8396(2) 1.07250(11) 0.76808(11) 0.0230(4) Uani 1 1 d . . . . .
C7 C 0.7227(2) 1.10779(11) 0.81027(11) 0.0236(4) Uani 1 1 d . . . . .
H7 H 0.6720 1.1423 0.7773 0.028 Uiso 1 1 calc R . . . .
C8 C 0.7769(2) 1.15513(12) 0.87311(12) 0.0291(5) Uani 1 1 d . . . . .
H8A H 0.8540 1.1867 0.8560 0.035 Uiso 1 1 calc R . . . .
H8B H 0.7027 1.1891 0.8896 0.035 Uiso 1 1 calc R . . . .
C9 C 0.8265(2) 1.10826(13) 0.93636(12) 0.0334(5) Uani 1 1 d . . . . .
H9A H 0.9096 1.0796 0.9223 0.040 Uiso 1 1 calc R . . . .
H9B H 0.8520 1.1419 0.9764 0.040 Uiso 1 1 calc R . . . .
C10 C 0.7149(3) 1.05398(14) 0.96108(12) 0.0357(5) Uani 1 1 d . . . . .
H10A H 0.6340 1.0827 0.9782 0.043 Uiso 1 1 calc R . . . .
H10B H 0.7500 1.0235 1.0014 0.043 Uiso 1 1 calc R . . . .
C11 C 0.6716(2) 1.00232(12) 0.89990(11) 0.0291(5) Uani 1 1 d . . . . .
H11A H 0.7512 0.9714 0.8848 0.035 Uiso 1 1 calc R . . . .
H11B H 0.5981 0.9680 0.9166 0.035 Uiso 1 1 calc R . . . .
C12 C 0.6195(2) 1.04781(10) 0.83653(11) 0.0230(4) Uani 1 1 d . . . . .
H12 H 0.5345 1.0747 0.8524 0.028 Uiso 1 1 calc R . . . .
C14 C 0.4943(2) 1.02028(10) 0.72649(11) 0.0218(4) Uani 1 1 d . . . . .
C15 C 0.4631(2) 0.96538(11) 0.66595(11) 0.0220(4) Uani 1 1 d . . . . .
H15 H 0.3757 0.9388 0.6786 0.026 Uiso 1 1 calc R . . . .
C17 C 0.5379(2) 0.83732(11) 0.64027(11) 0.0234(4) Uani 1 1 d . . . . .
C18 C 0.6603(2) 0.78582(11) 0.62656(11) 0.0232(4) Uani 1 1 d . . . . .
H18 H 0.7241 0.8128 0.5934 0.028 Uiso 1 1 calc R . . . .
C19 C 0.6138(2) 0.71418(11) 0.58875(12) 0.0303(5) Uani 1 1 d . . . . .
H19A H 0.5697 0.7275 0.5427 0.036 Uiso 1 1 calc R . . . .
H19B H 0.5443 0.6883 0.6186 0.036 Uiso 1 1 calc R . . . .
C20 C 0.7340(3) 0.66087(13) 0.57461(13) 0.0379(6) Uani 1 1 d . . . . .
H20A H 0.6988 0.6139 0.5529 0.045 Uiso 1 1 calc R . . . .
H20B H 0.7985 0.6844 0.5403 0.045 Uiso 1 1 calc R . . . .
C21 C 0.8101(2) 0.64247(12) 0.64341(13) 0.0339(5) Uani 1 1 d . . . . .
H21A H 0.8903 0.6101 0.6326 0.041 Uiso 1 1 calc R . . . .
H21B H 0.7483 0.6146 0.6761 0.041 Uiso 1 1 calc R . . . .
C22 C 0.8590(2) 0.71449(12) 0.67973(13) 0.0300(5) Uani 1 1 d . . . . .
H22A H 0.9058 0.7014 0.7251 0.036 Uiso 1 1 calc R . . . .
H22B H 0.9270 0.7398 0.6485 0.036 Uiso 1 1 calc R . . . .
C23 C 0.7412(2) 0.76875(11) 0.69560(11) 0.0237(4) Uani 1 1 d . . . . .
H23 H 0.7821 0.8169 0.7132 0.028 Uiso 1 1 calc R . . . .
C25 C 0.6206(2) 0.77731(11) 0.81060(11) 0.0251(5) Uani 1 1 d . . . . .
C26 C 0.5586(2) 0.73248(11) 0.87236(11) 0.0268(5) Uani 1 1 d . . . . .
H26 H 0.5180 0.6848 0.8536 0.032 Uiso 1 1 calc R . . . .
C28 C 0.3267(2) 0.78206(11) 0.87746(11) 0.0258(5) Uani 1 1 d . . . . .
C30 C 0.1461(2) 0.87733(12) 0.86784(11) 0.0296(5) Uani 1 1 d . . . . .
C31 C 0.0244(3) 0.82753(16) 0.85373(19) 0.0573(8) Uani 1 1 d . . . . .
H31A H 0.0509 0.7875 0.8205 0.086 Uiso 1 1 calc GR . . . .
H31B H -0.0503 0.8573 0.8327 0.086 Uiso 1 1 calc GR . . . .
H31C H -0.0071 0.8052 0.8988 0.086 Uiso 1 1 calc GR . . . .
C32 C 0.2098(3) 0.90902(16) 0.80079(14) 0.0500(7) Uani 1 1 d . . . . .
H32A H 0.2906 0.9392 0.8134 0.075 Uiso 1 1 calc GR . . . .
H32B H 0.1424 0.9407 0.7760 0.075 Uiso 1 1 calc GR . . . .
H32C H 0.2379 0.8678 0.7693 0.075 Uiso 1 1 calc GR . . . .
C33 C 0.1057(3) 0.94014(14) 0.91826(13) 0.0438(6) Uani 1 1 d . . . . .
H33A H 0.0672 0.9187 0.9622 0.066 Uiso 1 1 calc GR . . . .
H33B H 0.0365 0.9721 0.8952 0.066 Uiso 1 1 calc GR . . . .
H33C H 0.1871 0.9702 0.9299 0.066 Uiso 1 1 calc GR . . . .
C35 C 0.9616(3) 1.11103(14) 0.58332(13) 0.0435(6) Uani 1 1 d . . . . .
H35A H 0.8761 1.0968 0.5590 0.065 Uiso 1 1 calc GR . . . .
H35B H 1.0407 1.0952 0.5544 0.065 Uiso 1 1 calc GR . . . .
H35C H 0.9641 1.1657 0.5896 0.065 Uiso 1 1 calc GR . . . .
C38 C 0.4384(3) 1.00648(13) 0.59581(12) 0.0349(5) Uani 1 1 d . . . . .
H38A H 0.5214 1.0345 0.5825 0.052 Uiso 1 1 calc GR . . . .
H38B H 0.3612 1.0414 0.6015 0.052 Uiso 1 1 calc GR . . . .
H38C H 0.4166 0.9700 0.5582 0.052 Uiso 1 1 calc GR . . . .
C41 C 0.6733(3) 0.71431(14) 0.92458(13) 0.0396(6) Uani 1 1 d . . . . .
H41A H 0.7143 0.7611 0.9422 0.059 Uiso 1 1 calc GR . . . .
H41B H 0.7440 0.6844 0.9003 0.059 Uiso 1 1 calc GR . . . .
H41C H 0.6359 0.6857 0.9649 0.059 Uiso 1 1 calc GR . . . .
N5 N 0.85493(19) 1.09834(10) 0.70050(9) 0.0279(4) Uani 1 1 d . . . . .
H5 H 0.7956 1.1310 0.6832 0.034 Uiso 1 1 calc R . . . .
N13 N 0.58026(17) 0.99825(9) 0.77775(9) 0.0219(4) Uani 1 1 d . . . . .
H13 H 0.6144 0.9525 0.7762 0.026 Uiso 1 1 calc R . . . .
N16 N 0.56947(16) 0.90858(9) 0.65821(9) 0.0214(4) Uani 1 1 d . . . . .
H16 H 0.6561 0.9209 0.6654 0.026 Uiso 1 1 calc R . . . .
N24 N 0.65445(18) 0.73818(9) 0.75244(9) 0.0236(4) Uani 1 1 d . . . . .
H24 H 0.6233 0.6920 0.7481 0.028 Uiso 1 1 calc R . . . .
N27 N 0.4521(2) 0.77617(10) 0.90770(10) 0.0323(4) Uani 1 1 d . . . . .
H27 H 0.4694 0.7987 0.9486 0.039 Uiso 1 1 calc R . . . .
O2 O 1.08723(15) 0.96148(8) 0.63245(8) 0.0323(4) Uani 1 1 d . . . . .
O29 O 0.25508(17) 0.83809(8) 0.90831(8) 0.0312(4) Uani 1 1 d . . . . .
O34 O 0.85911(15) 0.95087(8) 0.64357(8) 0.0322(4) Uani 1 1 d . . . . .
O36 O 0.91639(16) 1.02407(8) 0.79157(8) 0.0299(3) Uani 1 1 d . . . . .
O37 O 0.43750(16) 1.08266(7) 0.72686(8) 0.0305(4) Uani 1 1 d . . . . .
O39 O 0.41951(16) 0.81564(8) 0.63567(11) 0.0455(5) Uani 1 1 d . . . . .
O40 O 0.64409(19) 0.84476(8) 0.81834(8) 0.0367(4) Uani 1 1 d . . . . .
O42 O 0.28442(17) 0.74115(9) 0.83083(10) 0.0438(4) Uani 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
C1 O2 1.449(3) . ?
C3 C4 1.520(3) . ?
C3 O2 1.330(3) . ?
C3 O34 1.200(3) . ?
C4 C35 1.527(3) . ?
C4 N5 1.445(3) . ?
C6 C7 1.518(3) . ?
C6 N5 1.353(3) . ?
C6 O36 1.222(2) . ?
C7 C8 1.539(3) . ?
C7 C12 1.544(3) . ?
C8 C9 1.525(3) . ?
C9 C10 1.524(3) . ?
C10 C11 1.527(3) . ?
C11 C12 1.521(3) . ?
C12 N13 1.460(3) . ?
C14 C15 1.526(3) . ?
C14 N13 1.330(3) . ?
C14 O37 1.240(2) . ?
C15 C38 1.521(3) . ?
C15 N16 1.453(2) . ?
C17 C18 1.523(3) . ?
C17 N16 1.348(3) . ?
C17 O39 1.216(3) . ?
C18 C19 1.526(3) . ?
C18 C23 1.541(3) . ?
C19 C20 1.527(3) . ?
C20 C21 1.519(3) . ?
C21 C22 1.527(3) . ?
C22 C23 1.526(3) . ?
C23 N24 1.461(3) . ?
C25 C26 1.527(3) . ?
C25 N24 1.332(3) . ?
C25 O40 1.231(2) . ?
C26 C41 1.516(3) . ?
C26 N27 1.453(3) . ?
C28 N27 1.347(3) . ?
C28 O29 1.346(3) . ?
C28 O42 1.208(3) . ?
C30 C31 1.501(4) . ?
C30 C32 1.507(3) . ?
C30 C33 1.514(3) . ?
C30 O29 1.477(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C3 C4 110.19(18) . . ?
O34 C3 C4 125.9(2) . . ?
O34 C3 O2 123.84(19) . . ?
C3 C4 C35 108.30(17) . . ?
N5 C4 C3 111.18(17) . . ?
N5 C4 C35 109.90(19) . . ?
N5 C6 C7 115.26(18) . . ?
O36 C6 C7 124.19(18) . . ?
O36 C6 N5 120.55(19) . . ?
C6 C7 C8 111.55(17) . . ?
C6 C7 C12 111.33(16) . . ?
C8 C7 C12 110.99(17) . . ?
C9 C8 C7 113.58(17) . . ?
C10 C9 C8 110.93(19) . . ?
C9 C10 C11 110.54(18) . . ?
C12 C11 C10 110.73(17) . . ?
C11 C12 C7 113.58(18) . . ?
N13 C12 C7 110.37(16) . . ?
N13 C12 C11 110.55(15) . . ?
N13 C14 C15 118.03(16) . . ?
O37 C14 C15 119.32(18) . . ?
O37 C14 N13 122.64(18) . . ?
C38 C15 C14 111.26(16) . . ?
N16 C15 C14 112.26(16) . . ?
N16 C15 C38 111.19(17) . . ?
N16 C17 C18 115.57(17) . . ?
O39 C17 C18 122.33(18) . . ?
O39 C17 N16 122.10(19) . . ?
C17 C18 C19 110.52(17) . . ?
C17 C18 C23 112.07(17) . . ?
C19 C18 C23 111.94(16) . . ?
C18 C19 C20 111.94(18) . . ?
C21 C20 C19 111.06(18) . . ?
C20 C21 C22 110.28(18) . . ?
C23 C22 C21 112.64(18) . . ?
C22 C23 C18 110.13(17) . . ?
N24 C23 C18 112.86(16) . . ?
N24 C23 C22 109.73(16) . . ?
N24 C25 C26 116.16(17) . . ?
O40 C25 C26 119.61(18) . . ?
O40 C25 N24 124.1(2) . . ?
C41 C26 C25 107.97(18) . . ?
N27 C26 C25 110.15(17) . . ?
N27 C26 C41 110.16(18) . . ?
O29 C28 N27 110.18(18) . . ?
O42 C28 N27 124.3(2) . . ?
O42 C28 O29 125.5(2) . . ?
C31 C30 C32 113.5(2) . . ?
C31 C30 C33 110.0(2) . . ?
C32 C30 C33 110.3(2) . . ?
O29 C30 C31 112.01(19) . . ?
O29 C30 C32 107.97(19) . . ?
O29 C30 C33 102.50(17) . . ?
C6 N5 C4 120.64(18) . . ?
C14 N13 C12 121.87(16) . . ?
C17 N16 C15 121.24(17) . . ?
C25 N24 C23 122.74(17) . . ?
C28 N27 C26 119.64(17) . . ?
C3 O2 C1 115.31(17) . . ?
C28 O29 C30 120.10(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C4 N5 C6 60.6(3) . . . . ?
C4 C3 O2 C1 -177.22(18) . . . . ?
C6 C7 C8 C9 -75.9(2) . . . . ?
C6 C7 C12 C11 75.8(2) . . . . ?
C6 C7 C12 N13 -49.0(2) . . . . ?
C7 C6 N5 C4 175.96(17) . . . . ?
C7 C8 C9 C10 -54.1(2) . . . . ?
C7 C12 N13 C14 -74.7(2) . . . . ?
C8 C7 C12 C11 -49.1(2) . . . . ?
C8 C7 C12 N13 -173.94(16) . . . . ?
C8 C9 C10 C11 58.0(2) . . . . ?
C9 C10 C11 C12 -58.2(3) . . . . ?
C10 C11 C12 C7 54.4(2) . . . . ?
C10 C11 C12 N13 179.12(17) . . . . ?
C11 C12 N13 C14 158.76(18) . . . . ?
C12 C7 C8 C9 48.8(2) . . . . ?
C14 C15 N16 C17 143.54(18) . . . . ?
C15 C14 N13 C12 178.02(17) . . . . ?
C17 C18 C19 C20 -179.59(18) . . . . ?
C17 C18 C23 C22 177.68(16) . . . . ?
C17 C18 C23 N24 54.7(2) . . . . ?
C18 C17 N16 C15 173.97(17) . . . . ?
C18 C19 C20 C21 55.5(3) . . . . ?
C18 C23 N24 C25 -108.4(2) . . . . ?
C19 C18 C23 C22 52.9(2) . . . . ?
C19 C18 C23 N24 -70.2(2) . . . . ?
C19 C20 C21 C22 -56.3(3) . . . . ?
C20 C21 C22 C23 57.1(3) . . . . ?
C21 C22 C23 C18 -54.9(2) . . . . ?
C21 C22 C23 N24 69.9(2) . . . . ?
C22 C23 N24 C25 128.4(2) . . . . ?
C23 C18 C19 C20 -53.9(2) . . . . ?
C25 C26 N27 C28 77.8(2) . . . . ?
C26 C25 N24 C23 -166.23(17) . . . . ?
C31 C30 O29 C28 68.5(3) . . . . ?
C32 C30 O29 C28 -57.2(2) . . . . ?
C33 C30 O29 C28 -173.69(19) . . . . ?
C35 C4 N5 C6 -179.55(19) . . . . ?
C38 C15 N16 C17 -91.1(2) . . . . ?
C41 C26 N27 C28 -163.17(19) . . . . ?
N5 C6 C7 C8 -113.3(2) . . . . ?
N5 C6 C7 C12 122.16(19) . . . . ?
N13 C14 C15 C38 -147.25(18) . . . . ?
N13 C14 C15 N16 -21.9(2) . . . . ?
N16 C17 C18 C19 -165.48(17) . . . . ?
N16 C17 C18 C23 68.9(2) . . . . ?
N24 C25 C26 C41 96.5(2) . . . . ?
N24 C25 C26 N27 -143.20(19) . . . . ?
N27 C28 O29 C30 153.54(18) . . . . ?
O2 C3 C4 C35 85.5(2) . . . . ?
O2 C3 C4 N5 -153.65(18) . . . . ?
O29 C28 N27 C26 -165.22(17) . . . . ?
O34 C3 C4 C35 -90.8(3) . . . . ?
O34 C3 C4 N5 30.0(3) . . . . ?
O34 C3 O2 C1 -0.8(3) . . . . ?
O36 C6 C7 C8 66.8(2) . . . . ?
O36 C6 C7 C12 -57.8(3) . . . . ?
O36 C6 N5 C4 -4.1(3) . . . . ?
O37 C14 C15 C38 33.9(3) . . . . ?
O37 C14 C15 N16 159.28(17) . . . . ?
O37 C14 N13 C12 -3.2(3) . . . . ?
O39 C17 C18 C19 14.8(3) . . . . ?
O39 C17 C18 C23 -110.8(2) . . . . ?
O39 C17 N16 C15 -6.3(3) . . . . ?
O40 C25 C26 C41 -79.1(2) . . . . ?
O40 C25 C26 N27 41.2(3) . . . . ?
O40 C25 N24 C23 9.1(3) . . . . ?
O42 C28 N27 C26 16.8(3) . . . . ?
O42 C28 O29 C30 -28.5(3) . . . . ?

####################################################################### 
# 
# 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/access/V1 
# 
# 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_DAla-mACHC-DAla-ACHC-DAla_moon214
_database_code_depnum_ccdc_archive 'CCDC 1448799'
_audit_update_record             
;
2016-01-21 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_audit_creation_date             2014-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C H Cl3, C30 H51 N5 O8'
_chemical_formula_sum            'C31 H52 Cl3 N5 O8'
_chemical_formula_weight         729.12
_chemical_absolute_configuration rm
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.5052(17)
_cell_length_b                   17.583(3)
_cell_length_c                   23.471(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3922.8(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.44
_cell_measurement_theta_min      3.14
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.7637.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16765
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.338
_diffrn_reflns_theta_min         3.140
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                6826
_reflns_number_total             7221
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 2850 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.053(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0682
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1348P)²+1.8496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1943
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5(0.04) H13(0.039) H16(0.038) H24(0.04) H27(0.034) H1A(0.165)
 H1B(0.165) H1C(0.165) H4(0.043) H7(0.047) H8A(0.061) H8B(0.061) H9A(0.06)
 H9B(0.06) H10(0.058) H11A(0.047) H11B(0.047) H12(0.043) H15(0.04) H18(0.044)
 H19A(0.056) H19B(0.056) H20A(0.065) H20B(0.065) H21A(0.065) H21B(0.065)
 H22A(0.052) H22B(0.052) H23(0.041) H26(0.035) H31A(0.134) H31B(0.134)
 H31C(0.134) H32A(0.082) H32B(0.082) H32C(0.082) H33A(0.167) H33B(0.167)
 H33C(0.167) H35A(0.064) H35B(0.064) H35C(0.064) H37A(0.1) H37B(0.1) H37C(0.1)
 H39A(0.071) H39B(0.071) H39C(0.071) H42A(0.061) H42B(0.061) H42C(0.061)
 H44(0.049) H48(0.341)
 Fixed X: H5(-0.9743) H13(-0.7078) H16(-0.7646) H24(-0.7648) H27(-0.4076) H1A(-
 1.1294) H1B(-0.9741) H1C(-1.0291) H4(-1.1267) H7(-0.7981) H8A(-0.6554) H8B(-
 0.8004) H9A(-0.7062) H9B(-0.5984) H10(-0.4472) H11A(-0.6483) H11B(-0.4999)
 H12(-0.5707) H15(-0.7716) H18(-0.9458) H19A(-1.1823) H19B(-1.1678) H20A(-
 1.3301) H20B(-1.2066) H21A(-1.2405) H21B(-1.2189) H22A(-1.0024) H22B(-1.0101)
 H23(-0.984) H26(-0.5429) H31A(-0.6676) H31B(-0.6001) H31C(-0.6003) H32A(-
 0.3367) H32B(-0.3416) H32C(-0.2407) H33A(-0.3396) H33B(-0.4165) H33C(-0.5058)
 H35A(-1.2492) H35B(-1.2796) H35C(-1.1713) H37A(-0.4199) H37B(-0.3654) H37C(-
 0.5144) H39A(-0.6067) H39B(-0.5243) H39C(-0.5268) H42A(-0.4171) H42B(-0.5688)
 H42C(-0.5431) H44(-1.0917) H48(-1.0797)
 Fixed Y: H5(-1.1373) H13(-1.1429) H16(-0.8908) H24(-0.944) H27(-0.7787) H1A(-
 1.2516) H1B(-1.2651) H1C(-1.1805) H4(-1.252) H7(-1.1669) H8A(-1.2496) H8B(-
 1.2942) H9A(-1.3709) H9B(-1.3724) H10(-1.2868) H11A(-1.2821) H11B(-1.239) H12(-
 1.1661) H15(-1.0286) H18(-0.8388) H19A(-0.8337) H19B(-0.8893) H20A(-0.9361)
 H20B(-0.9956) H21A(-0.9882) H21B(-0.8979) H22A(-1.0066) H22B(-0.9571) H23(-
 0.8438) H26(-0.9074) H31A(-0.6812) H31B(-0.6102) H31C(-0.6125) H32A(-0.5957)
 H32B(-0.59) H32C(-0.6507) H33A(-0.7691) H33B(-0.7139) H33C(-0.7755) H35A(-
 1.1411) H35B(-1.1579) H35C(-1.0924) H37A(-1.4177) H37B(-1.3625) H37C(-1.4041)
 H39A(-0.9399) H39B(-1.0149) H39C(-0.9416) H42A(-0.8604) H42B(-0.8919) H42C(-
 0.8023) H44(-0.9132) H48(-0.8951)
 Fixed Z: H5(-0.5944) H13(-0.6692) H16(-0.6495) H24(-0.512) H27(-0.5267) H1A(-
 0.8313) H1B(-0.8069) H1C(-0.8185) H4(-0.6424) H7(-0.5326) H8A(-0.4848) H8B(-
 0.4928) H9A(-0.5632) H9B(-0.5108) H10(-0.5573) H11A(-0.648) H11B(-0.6488) H12(-
 0.5682) H15(-0.6985) H18(-0.6045) H19A(-0.586) H19B(-0.6396) H20A(-0.5703)
 H20B(-0.5834) H21A(-0.4851) H21B(-0.4865) H22A(-0.5118) H22B(-0.4544) H23(-
 0.5072) H26(-0.5273) H31A(-0.6678) H31B(-0.7005) H31C(-0.6323) H32A(-0.6308)
 H32B(-0.6988) H32C(-0.6686) H33A(-0.7067) H33B(-0.7511) H33C(-0.7164) H35A(-
 0.612) H35B(-0.6779) H35C(-0.6602) H37A(-0.5812) H37B(-0.6308) H37C(-0.6367)
 H39A(-0.7307) H39B(-0.7111) H39C(-0.6707) H42A(-0.4456) H42B(-0.4277) H42C(-
 0.4332) H44(-0.8505) H48(-0.8395)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl45 Cl -0.9656(7) -0.9100(5) -0.7663(3) 0.095(2) Uani 0.361(8) 1 d . . P A 1
Cl46 Cl -1.2605(7) -0.9319(4) -0.7680(3) 0.0846(19) Uani 0.361(8) 1 d . . P A 1
Cl47 Cl -1.0484(13) -1.0435(4) -0.8059(6) 0.159(6) Uani 0.361(8) 1 d . . P A 1
Cl49 Cl -0.9006(9) -0.9470(9) -0.8016(6) 0.261(7) Uani 0.639(8) 1 d . . P A 2
Cl50 Cl -1.180(2) -0.9209(10) -0.7621(6) 0.326(9) Uani 0.639(8) 1 d . . P A 2
Cl51 Cl -1.1344(8) -1.0073(3) -0.8557(2) 0.145(3) Uani 0.639(8) 1 d . . P A 2
O2 O -1.1105(4) -1.2277(3) -0.74807(16) 0.0660(12) Uani 1 1 d . . . . .
O29 O -0.4330(3) -0.72078(16) -0.61236(11) 0.0349(6) Uani 1 1 d . . . . .
O34 O -0.8995(4) -1.1868(2) -0.72015(12) 0.0473(8) Uani 1 1 d . . . . .
O36 O -0.9152(4) -1.30519(18) -0.60176(17) 0.0569(9) Uani 1 1 d . . . . .
O38 O -0.6411(4) -1.03238(17) -0.57413(14) 0.0487(8) Uani 1 1 d . . . . .
O40 O -0.9682(3) -1.01782(15) -0.62066(13) 0.0383(6) Uani 1 1 d . . . . .
O41 O -0.7609(3) -0.77169(15) -0.51380(12) 0.0356(6) Uani 1 1 d . . . . .
O43 O -0.6091(3) -0.80688(16) -0.62502(11) 0.0368(6) Uani 1 1 d . . . . .
N5 N -0.9808(4) -1.18358(18) -0.60846(13) 0.0335(7) Uani 1 1 d . . . . .
H5 H -0.9743 -1.1373 -0.5944 0.040 Uiso 1 1 calc R . . . .
N13 N -0.6814(4) -1.12960(18) -0.63465(14) 0.0328(7) Uani 1 1 d . . . . .
H13 H -0.7078 -1.1429 -0.6692 0.039 Uiso 1 1 calc R . . . .
N16 N -0.7949(4) -0.93796(18) -0.64644(14) 0.0319(7) Uani 1 1 d . . . . .
H16 H -0.7646 -0.8908 -0.6495 0.038 Uiso 1 1 calc R . . . .
N24 N -0.8022(4) -0.89861(18) -0.51654(15) 0.0333(7) Uani 1 1 d . . . . .
H24 H -0.7648 -0.9440 -0.5120 0.040 Uiso 1 1 calc R . . . .
N27 N -0.4816(3) -0.79955(17) -0.54300(13) 0.0285(6) Uani 1 1 d . . . . .
H27 H -0.4076 -0.7787 -0.5267 0.034 Uiso 1 1 calc R . . . .
C1 C -1.0564(8) -1.2315(6) -0.8059(3) 0.110(4) Uani 1 1 d . . . . .
H1A H -1.1294 -1.2516 -0.8313 0.165 Uiso 1 1 calc GR . . . .
H1B H -0.9741 -1.2651 -0.8069 0.165 Uiso 1 1 calc GR . . . .
H1C H -1.0291 -1.1805 -0.8185 0.165 Uiso 1 1 calc GR . . . .
C3 C -1.0183(5) -1.2040(3) -0.70944(19) 0.0433(10) Uani 1 1 d . . . . .
C4 C -1.0867(5) -1.2007(2) -0.65100(18) 0.0360(9) Uani 1 1 d . . . . .
H4 H -1.1267 -1.2520 -0.6424 0.043 Uiso 1 1 calc R . . . .
C6 C -0.8925(5) -1.2382(2) -0.59035(17) 0.0373(9) Uani 1 1 d . . . . .
C7 C -0.7682(5) -1.2123(2) -0.55526(17) 0.0396(10) Uani 1 1 d . . . . .
H7 H -0.7981 -1.1669 -0.5326 0.047 Uiso 1 1 calc R . . . .
C8 C -0.7177(6) -1.2737(3) -0.51334(19) 0.0506(12) Uani 1 1 d . . . . .
H8A H -0.6554 -1.2496 -0.4848 0.061 Uiso 1 1 calc R . . . .
H8B H -0.8004 -1.2942 -0.4928 0.061 Uiso 1 1 calc R . . . .
C9 C -0.6387(6) -1.3397(3) -0.5411(2) 0.0501(12) Uani 1 1 d . . . . .
H9A H -0.7062 -1.3709 -0.5632 0.060 Uiso 1 1 calc R . . . .
H9B H -0.5984 -1.3724 -0.5108 0.060 Uiso 1 1 calc R . . . .
C10 C -0.5194(6) -1.3135(3) -0.5810(2) 0.0482(11) Uani 1 1 d . . . . .
H10 H -0.4472 -1.2868 -0.5573 0.058 Uiso 1 1 calc R . . . .
C11 C -0.5771(5) -1.2568(2) -0.62383(19) 0.0391(9) Uani 1 1 d . . . . .
H11A H -0.6483 -1.2821 -0.6480 0.047 Uiso 1 1 calc R . . . .
H11B H -0.4999 -1.2390 -0.6488 0.047 Uiso 1 1 calc R . . . .
C12 C -0.6443(5) -1.1882(2) -0.59377(18) 0.0359(9) Uani 1 1 d . . . . .
H12 H -0.5707 -1.1661 -0.5682 0.043 Uiso 1 1 calc R . . . .
C14 C -0.6765(4) -1.0558(2) -0.62091(17) 0.0337(8) Uani 1 1 d . . . . .
C15 C -0.7133(4) -1.0010(2) -0.66962(17) 0.0335(8) Uani 1 1 d . . . . .
H15 H -0.7716 -1.0286 -0.6985 0.040 Uiso 1 1 calc R . . . .
C17 C -0.9169(4) -0.9535(2) -0.62036(16) 0.0323(8) Uani 1 1 d . . . . .
C18 C -0.9870(4) -0.8872(2) -0.58950(19) 0.0364(9) Uani 1 1 d . . . . .
H18 H -0.9458 -0.8388 -0.6045 0.044 Uiso 1 1 calc R . . . .
C19 C -1.1476(5) -0.8842(3) -0.5984(2) 0.0467(11) Uani 1 1 d . . . . .
H19A H -1.1823 -0.8337 -0.5860 0.056 Uiso 1 1 calc R . . . .
H19B H -1.1678 -0.8893 -0.6396 0.056 Uiso 1 1 calc R . . . .
C20 C -1.2278(5) -0.9454(3) -0.5664(3) 0.0539(13) Uani 1 1 d . . . . .
H20A H -1.3301 -0.9361 -0.5703 0.065 Uiso 1 1 calc R . . . .
H20B H -1.2066 -0.9956 -0.5834 0.065 Uiso 1 1 calc R . . . .
C21 C -1.1893(5) -0.9463(3) -0.5043(3) 0.0546(14) Uani 1 1 d . . . . .
H21A H -1.2405 -0.9882 -0.4851 0.065 Uiso 1 1 calc R . . . .
H21B H -1.2189 -0.8979 -0.4865 0.065 Uiso 1 1 calc R . . . .
C22 C -1.0321(5) -0.9571(2) -0.4957(2) 0.0431(10) Uani 1 1 d . . . . .
H22A H -1.0024 -1.0066 -0.5118 0.052 Uiso 1 1 calc R . . . .
H22B H -1.0101 -0.9571 -0.4544 0.052 Uiso 1 1 calc R . . . .
C23 C -0.9527(4) -0.8925(2) -0.52518(18) 0.0346(8) Uani 1 1 d . . . . .
H23 H -0.9840 -0.8438 -0.5072 0.041 Uiso 1 1 calc R . . . .
C25 C -0.7183(4) -0.8376(2) -0.51530(14) 0.0282(7) Uani 1 1 d . . . . .
C26 C -0.5615(4) -0.8555(2) -0.51164(15) 0.0289(7) Uani 1 1 d . . . . .
H26 H -0.5429 -0.9074 -0.5273 0.035 Uiso 1 1 calc R . . . .
C28 C -0.5162(4) -0.7783(2) -0.59608(15) 0.0284(7) Uani 1 1 d . . . . .
C30 C -0.4500(6) -0.6833(3) -0.66773(18) 0.0472(11) Uani 1 1 d . . . . .
C31 C -0.5922(8) -0.6432(4) -0.6670(4) 0.089(3) Uani 1 1 d . . . . .
H31A H -0.6676 -0.6812 -0.6678 0.134 Uiso 1 1 calc GR . . . .
H31B H -0.6001 -0.6102 -0.7005 0.134 Uiso 1 1 calc GR . . . .
H31C H -0.6003 -0.6125 -0.6323 0.134 Uiso 1 1 calc GR . . . .
C32 C -0.3317(6) -0.6247(3) -0.6664(2) 0.0545(13) Uani 1 1 d . . . . .
H32A H -0.3367 -0.5957 -0.6308 0.082 Uiso 1 1 calc GR . . . .
H32B H -0.3416 -0.5900 -0.6988 0.082 Uiso 1 1 calc GR . . . .
H32C H -0.2407 -0.6507 -0.6686 0.082 Uiso 1 1 calc GR . . . .
C33 C -0.4258(12) -0.7404(5) -0.7146(3) 0.111(4) Uani 1 1 d . . . . .
H33A H -0.3396 -0.7691 -0.7067 0.167 Uiso 1 1 calc GR . . . .
H33B H -0.4165 -0.7139 -0.7511 0.167 Uiso 1 1 calc GR . . . .
H33C H -0.5058 -0.7755 -0.7164 0.167 Uiso 1 1 calc GR . . . .
C35 C -1.2077(5) -1.1428(3) -0.65018(19) 0.0424(10) Uani 1 1 d . . . . .
H35A H -1.2492 -1.1411 -0.6120 0.064 Uiso 1 1 calc GR . . . .
H35B H -1.2796 -1.1579 -0.6779 0.064 Uiso 1 1 calc GR . . . .
H35C H -1.1713 -1.0924 -0.6602 0.064 Uiso 1 1 calc GR . . . .
C37 C -0.4485(7) -1.3804(3) -0.6100(3) 0.0664(16) Uani 1 1 d . . . . .
H37A H -0.4199 -1.4177 -0.5812 0.100 Uiso 1 1 calc GR . . . .
H37B H -0.3654 -1.3625 -0.6308 0.100 Uiso 1 1 calc GR . . . .
H37C H -0.5144 -1.4041 -0.6367 0.100 Uiso 1 1 calc GR . . . .
C39 C -0.5811(5) -0.9718(3) -0.6980(2) 0.0473(11) Uani 1 1 d . . . . .
H39A H -0.6067 -0.9399 -0.7307 0.071 Uiso 1 1 calc GR . . . .
H39B H -0.5243 -1.0149 -0.7111 0.071 Uiso 1 1 calc GR . . . .
H39C H -0.5268 -0.9416 -0.6707 0.071 Uiso 1 1 calc GR . . . .
C42 C -0.5188(5) -0.8522(3) -0.44893(17) 0.0405(9) Uani 1 1 d . . . . .
H42A H -0.4171 -0.8604 -0.4456 0.061 Uiso 1 1 calc GR . . . .
H42B H -0.5688 -0.8919 -0.4277 0.061 Uiso 1 1 calc GR . . . .
H42C H -0.5431 -0.8023 -0.4332 0.061 Uiso 1 1 calc GR . . . .
C44 C -1.0913(13) -0.9367(9) -0.8117(8) 0.041(4) Uani 0.361(8) 1 d . . P A 1
H44 H -1.0917 -0.9132 -0.8505 0.049 Uiso 0.361(8) 1 calc R . P A 1
C48 C -1.0731(18) -0.9414(10) -0.8149(6) 0.28(3) Uani 0.639(8) 1 d . . P A 2
H48 H -1.0797 -0.8951 -0.8395 0.341 Uiso 0.639(8) 1 calc R . P 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
Cl45 C44 1.669(15) . ?
Cl46 C44 1.910(17) . ?
Cl47 C44 1.926(19) . ?
Cl49 C48 1.672(17) . ?
Cl50 C48 1.643(16) . ?
Cl51 C48 1.613(15) . ?
O2 C1 1.453(8) . ?
O2 C3 1.329(6) . ?
O29 C28 1.340(5) . ?
O29 C30 1.466(5) . ?
O34 C3 1.195(6) . ?
O36 C6 1.227(5) . ?
O38 C14 1.220(5) . ?
O40 C17 1.232(5) . ?
O41 C25 1.228(5) . ?
O43 C28 1.222(5) . ?
N5 C4 1.450(5) . ?
N5 C6 1.345(6) . ?
N13 C12 1.451(5) . ?
N13 C14 1.339(5) . ?
N16 C15 1.458(5) . ?
N16 C17 1.340(5) . ?
N24 C23 1.449(6) . ?
N24 C25 1.338(5) . ?
N27 C26 1.445(5) . ?
N27 C28 1.342(5) . ?
C3 C4 1.519(6) . ?
C4 C35 1.536(6) . ?
C6 C7 1.510(6) . ?
C7 C8 1.537(6) . ?
C7 C12 1.544(7) . ?
C8 C9 1.529(7) . ?
C9 C10 1.541(8) . ?
C10 C11 1.518(6) . ?
C10 C37 1.517(7) . ?
C11 C12 1.536(5) . ?
C14 C15 1.535(6) . ?
C15 C39 1.513(6) . ?
C17 C18 1.526(5) . ?
C18 C19 1.541(6) . ?
C18 C23 1.547(6) . ?
C19 C20 1.518(7) . ?
C20 C21 1.502(9) . ?
C21 C22 1.520(7) . ?
C22 C23 1.530(5) . ?
C25 C26 1.526(6) . ?
C26 C42 1.528(5) . ?
C30 C31 1.524(10) . ?
C30 C32 1.525(6) . ?
C30 C33 1.508(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O2 C1 114.7(5) . . ?
C28 O29 C30 121.8(3) . . ?
C6 N5 C4 120.2(3) . . ?
C14 N13 C12 121.4(3) . . ?
C17 N16 C15 118.4(3) . . ?
C25 N24 C23 122.1(3) . . ?
C28 N27 C26 122.2(3) . . ?
O2 C3 C4 110.2(4) . . ?
O34 C3 O2 124.0(4) . . ?
O34 C3 C4 125.8(4) . . ?
N5 C4 C3 109.4(4) . . ?
N5 C4 C35 111.9(3) . . ?
C3 C4 C35 110.9(4) . . ?
O36 C6 N5 120.4(4) . . ?
O36 C6 C7 123.1(4) . . ?
N5 C6 C7 116.4(3) . . ?
C6 C7 C8 112.4(4) . . ?
C6 C7 C12 111.1(3) . . ?
C8 C7 C12 109.2(4) . . ?
C9 C8 C7 114.5(4) . . ?
C8 C9 C10 113.1(4) . . ?
C11 C10 C9 109.5(4) . . ?
C37 C10 C9 111.5(4) . . ?
C37 C10 C11 111.9(4) . . ?
C10 C11 C12 111.2(4) . . ?
N13 C12 C7 113.3(4) . . ?
N13 C12 C11 110.8(3) . . ?
C11 C12 C7 111.8(3) . . ?
O38 C14 N13 123.6(4) . . ?
O38 C14 C15 121.5(4) . . ?
N13 C14 C15 114.9(3) . . ?
N16 C15 C14 108.7(3) . . ?
N16 C15 C39 110.3(3) . . ?
C39 C15 C14 110.6(4) . . ?
O40 C17 N16 121.8(4) . . ?
O40 C17 C18 122.1(4) . . ?
N16 C17 C18 116.1(3) . . ?
C17 C18 C19 113.2(4) . . ?
C17 C18 C23 109.0(3) . . ?
C19 C18 C23 110.1(4) . . ?
C20 C19 C18 114.0(4) . . ?
C21 C20 C19 111.5(4) . . ?
C20 C21 C22 111.7(4) . . ?
C21 C22 C23 109.4(4) . . ?
N24 C23 C18 110.4(3) . . ?
N24 C23 C22 111.6(4) . . ?
C22 C23 C18 112.5(3) . . ?
O41 C25 N24 124.1(4) . . ?
O41 C25 C26 121.1(3) . . ?
N24 C25 C26 114.7(3) . . ?
N27 C26 C25 110.1(3) . . ?
N27 C26 C42 109.0(3) . . ?
C25 C26 C42 107.8(3) . . ?
O29 C28 N27 109.3(3) . . ?
O43 C28 O29 125.3(3) . . ?
O43 C28 N27 125.4(3) . . ?
O29 C30 C31 107.2(5) . . ?
O29 C30 C32 101.8(3) . . ?
O29 C30 C33 109.2(5) . . ?
C31 C30 C32 110.0(5) . . ?
C33 C30 C31 116.8(7) . . ?
C33 C30 C32 110.7(5) . . ?
Cl45 C44 Cl46 104.3(10) . . ?
Cl45 C44 Cl47 94.5(9) . . ?
Cl46 C44 Cl47 100.6(9) . . ?
Cl50 C48 Cl49 118.7(12) . . ?
Cl51 C48 Cl49 115.0(13) . . ?
Cl51 C48 Cl50 112.4(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C3 C4 N5 173.2(4) . . . . ?
O2 C3 C4 C35 -62.8(5) . . . . ?
O34 C3 C4 N5 -7.9(6) . . . . ?
O34 C3 C4 C35 116.1(5) . . . . ?
O36 C6 C7 C8 -27.4(6) . . . . ?
O36 C6 C7 C12 95.4(5) . . . . ?
O38 C14 C15 N16 -40.7(5) . . . . ?
O38 C14 C15 C39 80.6(5) . . . . ?
O40 C17 C18 C19 -42.8(6) . . . . ?
O40 C17 C18 C23 80.0(5) . . . . ?
O41 C25 C26 N27 -38.2(5) . . . . ?
O41 C25 C26 C42 80.6(4) . . . . ?
N5 C6 C7 C8 151.7(4) . . . . ?
N5 C6 C7 C12 -85.5(4) . . . . ?
N13 C14 C15 N16 141.7(4) . . . . ?
N13 C14 C15 C39 -97.1(4) . . . . ?
N16 C17 C18 C19 138.2(4) . . . . ?
N16 C17 C18 C23 -99.0(4) . . . . ?
N24 C25 C26 N27 145.8(3) . . . . ?
N24 C25 C26 C42 -95.4(4) . . . . ?
C1 O2 C3 O34 0.0(8) . . . . ?
C1 O2 C3 C4 178.9(6) . . . . ?
C4 N5 C6 O36 -12.7(6) . . . . ?
C4 N5 C6 C7 168.2(4) . . . . ?
C6 N5 C4 C3 -77.5(5) . . . . ?
C6 N5 C4 C35 159.1(4) . . . . ?
C6 C7 C8 C9 73.8(6) . . . . ?
C6 C7 C12 N13 56.0(4) . . . . ?
C6 C7 C12 C11 -70.1(4) . . . . ?
C7 C8 C9 C10 50.5(6) . . . . ?
C8 C7 C12 N13 -179.4(3) . . . . ?
C8 C7 C12 C11 54.5(4) . . . . ?
C8 C9 C10 C11 -52.7(5) . . . . ?
C8 C9 C10 C37 -177.1(5) . . . . ?
C9 C10 C11 C12 57.7(5) . . . . ?
C10 C11 C12 N13 172.1(4) . . . . ?
C10 C11 C12 C7 -60.5(5) . . . . ?
C12 N13 C14 O38 0.1(7) . . . . ?
C12 N13 C14 C15 177.7(4) . . . . ?
C12 C7 C8 C9 -50.1(6) . . . . ?
C14 N13 C12 C7 86.0(5) . . . . ?
C14 N13 C12 C11 -147.4(4) . . . . ?
C15 N16 C17 O40 -7.5(6) . . . . ?
C15 N16 C17 C18 171.4(3) . . . . ?
C17 N16 C15 C14 -59.5(4) . . . . ?
C17 N16 C15 C39 179.1(4) . . . . ?
C17 C18 C19 C20 72.9(5) . . . . ?
C17 C18 C23 N24 52.8(4) . . . . ?
C17 C18 C23 C22 -72.6(4) . . . . ?
C18 C19 C20 C21 52.2(5) . . . . ?
C19 C18 C23 N24 177.6(3) . . . . ?
C19 C18 C23 C22 52.1(4) . . . . ?
C19 C20 C21 C22 -56.7(5) . . . . ?
C20 C21 C22 C23 59.0(5) . . . . ?
C21 C22 C23 N24 178.0(4) . . . . ?
C21 C22 C23 C18 -57.2(5) . . . . ?
C23 N24 C25 O41 9.9(6) . . . . ?
C23 N24 C25 C26 -174.3(3) . . . . ?
C23 C18 C19 C20 -49.4(5) . . . . ?
C25 N24 C23 C18 83.7(4) . . . . ?
C25 N24 C23 C22 -150.4(3) . . . . ?
C26 N27 C28 O29 174.0(3) . . . . ?
C26 N27 C28 O43 -6.0(6) . . . . ?
C28 O29 C30 C31 65.7(5) . . . . ?
C28 O29 C30 C32 -178.8(4) . . . . ?
C28 O29 C30 C33 -61.8(6) . . . . ?
C28 N27 C26 C25 -47.8(4) . . . . ?
C28 N27 C26 C42 -165.9(3) . . . . ?
C30 O29 C28 O43 2.6(6) . . . . ?
C30 O29 C28 N27 -177.4(4) . . . . ?
C37 C10 C11 C12 -178.2(4) . . . . ?

