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

####################################################################### 
# 
# 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_ss10
_database_code_depnum_ccdc_archive 'CCDC 1431843'
_audit_update_record             
;
2015-10-18 deposited with the CCDC.
2016-03-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_ss10                
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      10.55 Check
RESPONSE: This is due to that the hydrogen atoms in the water molecules were not fully found.
;
_vrf_PLAT420_ss10                
;
PROBLEM: D-H Without Acceptor        O12    -  *H122   ..     Please Check
RESPONSE: This is due to that the hydrogen atoms in the water molecule were not fully found.
;

# Added during the CSD deposition process: Monday 19th of October 2015 12:05:53 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17.09 H116.40 Br N O38'
_chemical_formula_weight         1024.56

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pmma

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

_cell_length_a                   21.0329(15)
_cell_length_b                   12.5972(9)
_cell_length_c                   12.0333(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3188.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1130
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       ' φ & ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            65480
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         29.00
_reflns_number_total             4515
_reflns_number_gt                4169
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ATOMS V.5.0'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0695P)²+5.5839P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4515
_refine_ls_number_parameters     528
_refine_ls_number_restraints     250
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1670
_refine_ls_wR_factor_gt          0.1649
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002

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
C1KA C 0.26260(14) 0.4904(2) 0.2867(2) 0.0321(6) Uani 0.0218(14) 1 d PD . 3
H1KA H 0.22115(13) 0.5000 0.2332(2) 0.050 Uiso 0.044(3) 2 d SPD . 3
H2KA H 0.28612(17) 0.56679(19) 0.2972(4) 0.050 Uiso 0.0218(14) 1 d PD . 3
H3KA H 0.2888(2) 0.4429(3) 0.2264(2) 0.050 Uiso 0.0218(14) 1 d PD . 3
H4KA H 0.2500 0.4409(4) 0.35774(19) 0.050 Uiso 0.044(3) 2 d SPD . 3
C1N C 0.5000 0.5000 0.0000 0.0321(6) Uani 0.1685(15) 4 d SPD A 4
H1N H 0.49102(19) 0.4345(2) 0.0570(3) 0.050 Uiso 0.0421(4) 1 d PD A 4
H2N H 0.54996(10) 0.5000 -0.0240(4) 0.050 Uiso 0.0842(7) 2 d SPD A 4
H3N H 0.47120(12) 0.5288(5) -0.0690(2) 0.050 Uiso 0.0421(4) 1 d PD A 4
H4N H 0.5193(2) 0.5673(2) 0.0458(3) 0.050 Uiso 0.0421(4) 1 d PD A 4
C1NA C 0.5000 0.5000 0.0000 0.0321(6) Uani 0.1079(16) 4 d SPD B 5
H1NA H 0.49108(19) 0.5657(2) 0.0568(3) 0.050 Uiso 0.0270(4) 1 d PD B 5
H2NA H 0.54993(10) 0.5000 -0.0242(4) 0.050 Uiso 0.0539(8) 2 d SPD B 5
H3NA H 0.47107(12) 0.4718(5) -0.0691(2) 0.050 Uiso 0.0270(4) 1 d PD B 5
H4NA H 0.5184(2) 0.4323(2) 0.0463(3) 0.050 Uiso 0.0270(4) 1 d PD B 5
C1NB C 0.5000 0.5000 0.0000 0.0321(6) Uani 0.1086(16) 4 d SPD C 6
H1NB H 0.50892(19) 0.5657(2) -0.0568(3) 0.050 Uiso 0.0271(4) 1 d PD C 6
H2NB H 0.45007(10) 0.5000 0.0242(4) 0.050 Uiso 0.0543(8) 2 d SPD C 6
H3NB H 0.52893(12) 0.4718(5) 0.0691(2) 0.050 Uiso 0.0271(4) 1 d PD C 6
H4NB H 0.4816(2) 0.4323(2) -0.0463(3) 0.050 Uiso 0.0271(4) 1 d PD C 6
C1NC C 0.5000 0.5000 0.0000 0.0321(6) Uani 0.1094(17) 4 d SPD D 7
H1NC H 0.50892(19) 0.4343(2) -0.0568(3) 0.050 Uiso 0.0274(4) 1 d PD D 7
H2NC H 0.45007(10) 0.5000 0.0242(4) 0.050 Uiso 0.0547(8) 2 d SPD D 7
H3NC H 0.52893(12) 0.5282(5) 0.0691(2) 0.050 Uiso 0.0274(4) 1 d PD D 7
H4NC H 0.4816(2) 0.5677(2) -0.0463(3) 0.050 Uiso 0.0274(4) 1 d PD D 7
C1Q C 0.5000 0.5000 0.5000 0.0321(6) Uani 0.3704(15) 4 d SPD E 8
H1Q H 0.50924(19) 0.58038(17) 0.4706(7) 0.050 Uiso 0.0926(4) 1 d PD E 8
H2Q H 0.54374(13) 0.4538(2) 0.4965(4) 0.050 Uiso 0.0926(4) 1 d PD E 8
H3Q H 0.4924(2) 0.5281(4) 0.5846(2) 0.050 Uiso 0.0926(4) 1 d PD E 8
H4Q H 0.45519(13) 0.4718(3) 0.4655(3) 0.050 Uiso 0.0926(4) 1 d PD E 8
C1QA C 0.5000 0.5000 0.5000 0.0321(6) Uani 0.0272(16) 4 d SPD F 9
H1QA H 0.5074(2) 0.41870(17) 0.4718(8) 0.050 Uiso 0.0068(4) 1 d PD F 9
H2QA H 0.54422(13) 0.5445(2) 0.4920(4) 0.050 Uiso 0.0068(4) 1 d PD F 9
H3QA H 0.4928(2) 0.4779(4) 0.58666(19) 0.050 Uiso 0.0068(4) 1 d PD F 9
H4QA H 0.45560(13) 0.5303(3) 0.4657(3) 0.050 Uiso 0.0068(4) 1 d PD F 9
C1QB C 0.5000 0.5000 0.5000 0.0321(6) Uani 0.0379(16) 4 d SPD G 10
H1QB H 0.4926(2) 0.41871(17) 0.5282(8) 0.050 Uiso 0.0095(4) 1 d PD G 10
H2QB H 0.45579(13) 0.5445(2) 0.5079(4) 0.050 Uiso 0.0095(4) 1 d PD G 10
H3QB H 0.5072(2) 0.4779(4) 0.41334(19) 0.050 Uiso 0.0095(4) 1 d PD G 10
H4QB H 0.54440(13) 0.5303(3) 0.5343(3) 0.050 Uiso 0.0095(4) 1 d PD G 10
C1R C 0.49221(13) 0.4874(2) 0.4981(2) 0.0321(6) Uani 0.0145(4) 1 d PD H 12
H1R H 0.4797(2) 0.5625(2) 0.5372(3) 0.050 Uiso 0.0145(4) 1 d PD H 12
H2R H 0.53097(16) 0.5000 0.4394(2) 0.050 Uiso 0.0290(9) 2 d SPD H 12
H3R H 0.50889(19) 0.4386(4) 0.5670(2) 0.050 Uiso 0.0145(4) 1 d PD H 12
H4R H 0.44976(14) 0.4516(3) 0.4620(3) 0.050 Uiso 0.0145(4) 1 d PD H 12
C1RB C 0.50822(13) 0.5127(2) 0.5033(2) 0.0321(6) Uani 0.0007(5) 1 d PD I 14
H1RB H 0.5206(2) 0.4377(2) 0.4637(3) 0.050 Uiso 0.0007(5) 1 d PD I 14
H2RB H 0.46923(16) 0.5000 0.5615(2) 0.050 Uiso 0.0015(9) 2 d SPD I 14
H3RB H 0.49154(19) 0.5604(4) 0.4336(2) 0.050 Uiso 0.0007(5) 1 d PD I 14
H4RB H 0.55087(14) 0.5487(3) 0.5383(3) 0.050 Uiso 0.0007(5) 1 d PD I 14
Br1 Br 0.7500 0.0000 0.469483(13) 0.02831(4) Uani 1 4 d S . .
O1 O 0.55679(2) 0.19685(4) 0.44091(4) 0.02143(11) Uani 1 1 d D . .
H11 H 0.5693(16) 0.1264(13) 0.426(3) 0.050 Uiso 0.25 1 d PD . .
H12 H 0.5191(8) 0.182(3) 0.484(2) 0.050 Uiso 0.25 1 d PD . .
H13 H 0.561(2) 0.228(2) 0.3726(14) 0.050 Uiso 0.25 1 d PD . .
H14 H 0.5818(11) 0.2453(18) 0.482(2) 0.046 Uiso 0.25 1 d PD . .
O2 O 0.61810(3) 0.5000 0.25790(5) 0.02114(16) Uani 1 2 d SD . .
H21 H 0.6565(8) 0.5000 0.3017(19) 0.055 Uiso 0.50 2 d SPD . .
H22 H 0.6306(14) 0.5000 0.3346(12) 0.055 Uiso 0.50 2 d SPD . .
H23 H 0.6472(9) 0.5000 0.1973(15) 0.053 Uiso 0.50 2 d SPD . .
H24 H 0.5908(11) 0.4414(15) 0.266(3) 0.050 Uiso 0.25 1 d PD . .
O3 O 0.35877(2) 0.31942(4) 0.43719(4) 0.02203(11) Uani 1 1 d D . .
H31 H 0.3965(9) 0.276(2) 0.451(3) 0.059 Uiso 0.25 1 d PD . .
H32 H 0.3203(9) 0.277(2) 0.417(3) 0.053 Uiso 0.25 1 d PD . .
H34 H 0.3943(9) 0.278(2) 0.464(3) 0.050 Uiso 0.25 1 d PD . .
O4 O 0.54287(2) 0.31947(4) 0.25230(4) 0.02220(12) Uani 1 1 d D . .
H41 H 0.5459(17) 0.2771(19) 0.3200(14) 0.035 Uiso 0.25 1 d PD . .
H42 H 0.5004(8) 0.350(2) 0.252(3) 0.031 Uiso 0.25 1 d PD . .
H43 H 0.5474(19) 0.277(2) 0.1820(15) 0.050 Uiso 0.25 1 d PD . .
H44 H 0.546(2) 0.279(2) 0.3220(15) 0.057 Uiso 0.25 1 d PD . .
O5 O 0.2500 0.21388(6) 0.38048(6) 0.02679(18) Uani 1 2 d SD . .
H51 H 0.2500 0.1471(13) 0.4188(19) 0.050 Uiso 0.50 2 d SPD . .
H52 H 0.2500 0.183(2) 0.3089(13) 0.051 Uiso 0.50 2 d SPD . .
O6 O 0.57668(4) 0.0000 0.14433(6) 0.02945(19) Uani 1 2 d SD . .
H61 H 0.5823(16) 0.0000 0.213(3) 0.050 Uiso 0.50 2 d SP . .
H62 H 0.5592(14) 0.0689(13) 0.122(3) 0.050 Uiso 0.25 1 d PD . .
O7 O 0.41992(2) 0.39120(4) 0.24999(4) 0.02221(12) Uani 1 1 d D . .
H71 H 0.4099(17) 0.371(3) 0.1767(13) 0.050 Uiso 0.25 1 d PD . .
H72 H 0.4085(15) 0.4627(12) 0.249(3) 0.037 Uiso 0.25 1 d PD . .
H73 H 0.4586(8) 0.355(2) 0.252(3) 0.049 Uiso 0.25 1 d PD . .
H74 H 0.4045(15) 0.363(3) 0.3161(15) 0.056 Uiso 0.25 1 d PD . .
O8 O 0.36044(2) 0.32749(4) 0.05802(4) 0.02404(12) Uani 1 1 d D . .
H81 H 0.3285(9) 0.311(3) 0.1128(17) 0.046 Uiso 0.25 1 d PD . .
H82 H 0.3924(10) 0.2812(19) 0.023(2) 0.050 Uiso 0.25 1 d PD . .
H83 H 0.3514(18) 0.3838(15) 0.0090(19) 0.050 Uiso 0.25 1 d PD . .
O9 O 0.55605(2) 0.20123(4) 0.06069(4) 0.02309(12) Uani 1 1 d D . .
H91 H 0.5849(10) 0.243(2) 0.016(2) 0.050 Uiso 0.25 1 d PD . .
H92 H 0.560(2) 0.1290(12) 0.083(3) 0.050 Uiso 0.25 1 d PD . .
H93 H 0.554(2) 0.239(2) 0.1310(14) 0.050 Uiso 0.25 1 d PD . .
H94 H 0.5183(8) 0.198(3) 0.017(2) 0.050 Uiso 0.25 1 d PD . .
O10 O 0.2500 0.27821(7) 0.16203(7) 0.0343(2) Uani 1 2 d SD . .
H101 H 0.2500 0.265(3) 0.2387(12) 0.050 Uiso 0.50 2 d SPD . .
H102 H 0.2500 0.2213(14) 0.2138(16) 0.045 Uiso 0.50 2 d SPD . .
H103 H 0.2913(8) 0.291(4) 0.134(3) 0.059 Uiso 0.25 1 d PD . .
O11 O 0.68385(3) 0.5000 0.06088(6) 0.02185(16) Uani 1 2 d SD . .
H111 H 0.7280(6) 0.5000 0.064(2) 0.030(7) Uiso 0.50 2 d SPD . .
H112 H 0.6538(9) 0.5000 0.1165(15) 0.056 Uiso 0.50 2 d SPD . .
H113 H 0.6805(17) 0.472(2) 0.1346(13) 0.050 Uiso 0.25 1 d PD . .
H114 H 0.6636(13) 0.4347(14) 0.062(4) 0.053 Uiso 0.25 1 d PD . .
O12 O 0.31631(3) 0.5000 0.54414(5) 0.01990(15) Uani 1 2 d SD . .
H121 H 0.3434(10) 0.5000 0.6041(15) 0.059 Uiso 0.50 2 d SPD . .
H122 H 0.2730(7) 0.5000 0.551(2) 0.050 Uiso 0.50 2 d SPD . .
H124 H 0.3349(14) 0.5574(15) 0.506(2) 0.050 Uiso 0.25 1 d PD . .
O13 O 0.60329(4) 0.0000 0.37407(6) 0.02616(18) Uani 1 2 d SD . .
H131 H 0.6441(7) 0.0000 0.378(3) 0.050 Uiso 0.50 2 d SPD . .
H132 H 0.5917(17) 0.0666(14) 0.409(2) 0.050 Uiso 0.25 1 d PD . .
H133 H 0.6444(7) 0.0000 0.379(3) 0.058 Uiso 0.50 2 d SPD . .
N1 N 0.7503(6) 0.0021(6) -0.00133(10) 0.0162(2) Uani 1 4 d SU J -1
C1A C 0.72441(11) -0.09348(19) 0.06902(19) 0.0151(4) Uani 0.25 1 d PU J -1
H1A1 H 0.6863 -0.0699 0.1070 0.035 Uiso 0.25 1 calc PR J -1
H1A2 H 0.7119 -0.1491 0.0178 0.030 Uiso 0.25 1 calc PR J -1
C2A C 0.76786(10) -0.14172(19) 0.15409(19) 0.0159(5) Uani 0.25 1 d PU J -1
H2A1 H 0.7867 -0.0865 0.1995 0.032 Uiso 0.25 1 calc PR J -1
H2A2 H 0.8018 -0.1805 0.1176 0.035(10) Uiso 0.25 1 calc PR J -1
C3A C 0.72931(11) -0.21564(19) 0.2254(2) 0.0182(5) Uani 0.25 1 d PU J -1
H3A1 H 0.7086 -0.2686 0.1793 0.048 Uiso 0.25 1 calc PR J -1
H3A2 H 0.6967 -0.1761 0.2647 0.014(7) Uiso 0.25 1 calc PR J -1
C4A C 0.77356(14) -0.2693(2) 0.3079(2) 0.0254(6) Uani 0.25 1 d PU J -1
H4A1 H 0.8041 -0.3116 0.2684 0.057 Uiso 0.25 1 calc PR J -1
H4A2 H 0.7492 -0.3140 0.3566 0.032(7) Uiso 0.50 2 calc SPR J -1
H4A3 H 0.7953 -0.2163 0.3508 0.037 Uiso 0.25 1 calc PR J -1
C1B C 0.80336(10) -0.0488(2) -0.07232(18) 0.0150(5) Uani 0.25 1 d PU J -1
H1B1 H 0.7862 -0.1089 -0.1127 0.030 Uiso 0.25 1 calc PR J -1
H1B2 H 0.8368 -0.0747 -0.0239 0.030 Uiso 0.25 1 calc PR J -1
C2B C 0.83303(10) 0.03528(18) -0.15930(18) 0.0139(4) Uani 0.25 1 d PU J -1
H2B1 H 0.8010 0.0564 -0.2130 0.050 Uiso 0.25 1 calc PR J -1
H2B2 H 0.8474 0.0982 -0.1203 0.054 Uiso 0.25 1 calc PR J -1
C3B C 0.88930(11) -0.01817(19) -0.2190(2) 0.0236(6) Uani 0.25 1 d PU J -1
H3B1 H 0.9208 -0.0390 -0.1643 0.024(9) Uiso 0.25 1 calc PR J -1
H3B2 H 0.8744 -0.0820 -0.2559 0.075(18) Uiso 0.25 1 calc PR J -1
C4B C 0.92041(14) 0.0550(2) -0.3048(2) 0.0292(6) Uani 0.25 1 d PU J -1
H4B1 H 0.8884 0.0827 -0.3537 0.054 Uiso 0.25 1 calc PR J -1
H4B2 H 0.9510 0.0155 -0.3471 0.026(8) Uiso 0.25 1 calc PR J -1
H4B3 H 0.9413 0.1125 -0.2673 0.050 Uiso 0.25 1 calc PR J -1
C1C C 0.77841(13) 0.0830(2) 0.0635(2) 0.0193(5) Uani 0.25 1 d PU J -1
H1C1 H 0.7922 0.1398 0.0147 0.047 Uiso 0.25 1 calc PR J -1
H1C2 H 0.8158 0.0545 0.1000 0.017(7) Uiso 0.25 1 calc PR J -1
C2C C 0.73359(11) 0.1297(2) 0.1527(2) 0.0229(6) Uani 0.25 1 d PU J -1
H2C1 H 0.7248 0.0763 0.2087 0.016(7) Uiso 0.25 1 calc PR J -1
H2C2 H 0.6936 0.1500 0.1186 0.038 Uiso 0.25 1 calc PR J -1
C3C C 0.76566(13) 0.2309(3) 0.2097(3) 0.0319(7) Uani 0.25 1 d PU J -1
H3C1 H 0.8059 0.2089 0.2418 0.050 Uiso 0.25 1 calc PR J -1
H3C2 H 0.7751 0.2822 0.1519 0.051 Uiso 0.25 1 calc PR J -1
C4C C 0.72784(17) 0.2860(3) 0.2984(3) 0.0387(8) Uani 0.25 1 d PU J -1
H4C1 H 0.6882 0.3099 0.2679 0.050 Uiso 0.25 1 calc PR J -1
H4C2 H 0.7514 0.3458 0.3258 0.051 Uiso 0.50 2 calc SPR J -1
H4C3 H 0.7198 0.2374 0.3583 0.015(7) Uiso 0.25 1 calc PR J -1
C1D C 0.69639(13) 0.0392(2) -0.0778(2) 0.0238(6) Uani 0.25 1 d PU J -1
H1D1 H 0.6619 0.0599 -0.0290 0.050 Uiso 0.25 1 calc PR J -1
H1D2 H 0.7115 0.1041 -0.1123 0.050 Uiso 0.25 1 calc PR J -1
C2D C 0.66819(14) -0.0202(2) -0.1636(2) 0.0293(7) Uani 0.25 1 d PU J -1
H2D1 H 0.6503 -0.0845 -0.1322 0.045 Uiso 0.25 1 calc PR J -1
H2D2 H 0.7010 -0.0410 -0.2160 0.035(10) Uiso 0.25 1 calc PR J -1
C3D C 0.61721(15) 0.0373(3) -0.2250(3) 0.0311(6) Uani 0.25 1 d PU J -1
H3D1 H 0.6353 0.1001 -0.2594 0.023(9) Uiso 0.25 1 calc PR J -1
H3D2 H 0.5851 0.0606 -0.1725 0.014(7) Uiso 0.25 1 calc PR J -1
C4D C 0.58611(15) -0.0296(2) -0.3132(3) 0.0325(7) Uani 0.25 1 d PU J -1
H4D1 H 0.6162 -0.0440 -0.3713 0.041 Uiso 0.25 1 calc PR J -1
H4D2 H 0.5503 0.0079 -0.3435 0.080(14) Uiso 0.25 1 calc PR J -1
H4D3 H 0.5720 -0.0952 -0.2812 0.047 Uiso 0.25 1 calc PR J -1


_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
C1KA C1KA 0.530(6) 8_655 ?
C1KA C1KA 0.583(6) 2_565 ?
N1 C1C 1.414(8) . ?
N1 C1D 1.533(10) . ?
N1 C1B 1.545(10) . ?
N1 C1A 1.569(8) . ?
C1A C2A 1.501(3) . ?
C2A C3A 1.504(3) . ?
C3A C4A 1.520(4) . ?
C1B C2B 1.614(3) . ?
C2B C3B 1.539(3) . ?
C3B C4B 1.530(4) . ?
C1C C2C 1.544(4) . ?
C2C C3C 1.598(4) . ?
C3C C4C 1.501(5) . ?
C1D C2D 1.406(4) . ?
C2D C3D 1.490(4) . ?
C3D C4D 1.505(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
C1KA C1KA C1KA 24.6(5) 8_655 2_565 ?
C1C N1 C1D 114.9(6) . . ?
C1C N1 C1B 107.5(8) . . ?
C1D N1 C1B 109.20(16) . . ?
C1C N1 C1A 113.60(16) . . ?
C1D N1 C1A 107.6(7) . . ?
C1B N1 C1A 103.3(5) . . ?
C2A C1A N1 117.9(4) . . ?
C1A C2A C3A 108.15(18) . . ?
C2A C3A C4A 108.5(2) . . ?
N1 C1B C2B 111.5(3) . . ?
C3B C2B C1B 108.23(18) . . ?
C4B C3B C2B 112.3(2) . . ?
N1 C1C C2C 113.7(5) . . ?
C1C C2C C3C 110.1(2) . . ?
C4C C3C C2C 116.8(2) . . ?
C2D C1D N1 126.2(3) . . ?
C1D C2D C3D 114.1(2) . . ?
C2D C3D C4D 113.0(3) . . ?

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
C1C N1 C1A C2A -49.4(8) . . . . ?
C1D N1 C1A C2A -177.8(3) . . . . ?
C1B N1 C1A C2A 66.8(4) . . . . ?
N1 C1A C2A C3A 168.9(3) . . . . ?
C1A C2A C3A C4A 177.0(2) . . . . ?
C1C N1 C1B C2B -64.1(4) . . . . ?
C1D N1 C1B C2B 61.2(6) . . . . ?
C1A N1 C1B C2B 175.4(3) . . . . ?
N1 C1B C2B C3B 174.9(4) . . . . ?
C1B C2B C3B C4B 179.32(19) . . . . ?
C1D N1 C1C C2C 67.3(5) . . . . ?
C1B N1 C1C C2C -170.8(3) . . . . ?
C1A N1 C1C C2C -57.1(8) . . . . ?
N1 C1C C2C C3C -171.9(4) . . . . ?
C1C C2C C3C C4C 179.8(3) . . . . ?
C1C N1 C1D C2D 168.3(4) . . . . ?
C1B N1 C1D C2D 47.4(7) . . . . ?
C1A N1 C1D C2D -64.1(5) . . . . ?
N1 C1D C2D C3D -179.3(5) . . . . ?
C1D C2D C3D C4D -177.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.096
