# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_2-MeCN
_database_code_depnum_ccdc_archive 'CCDC 1044954'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-09-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C60 H60 N4 O8, C H Cl3, 2(C2 H3 N)'
_chemical_formula_sum            'C65 H67 Cl3 N6 O8'
_chemical_formula_weight         1166.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 N4 O8'
_chemical_oxdiff_usercomment     tte-0270314-008
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   13.4640(6)
_cell_length_b                   13.6873(6)
_cell_length_c                   17.0771(6)
_cell_angle_alpha                107.657(4)
_cell_angle_beta                 95.015(3)
_cell_angle_gamma                95.481(3)
_cell_volume                     2962.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.5550
_cell_measurement_theta_min      2.1010
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23583
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         2.05
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -92.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470  -77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00   40.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000 -150.0000 86

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   77.0000   90.0000 42

#__ type_ start__ end____ width___ exp.time_
  4 omega  -19.00   62.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  -30.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   28.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -37.0000   60.0000 73

#__ type_ start__ end____ width___ exp.time_
  6 omega   57.00   92.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   57.0000    0.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0518737000
_diffrn_orient_matrix_UB_12      0.0194526000
_diffrn_orient_matrix_UB_13      0.0078946000
_diffrn_orient_matrix_UB_21      -0.0120249000
_diffrn_orient_matrix_UB_22      0.0503656000
_diffrn_orient_matrix_UB_23      0.0193480000
_diffrn_orient_matrix_UB_31      0.0028609000
_diffrn_orient_matrix_UB_32      -0.0096039000
_diffrn_orient_matrix_UB_33      0.0386309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                8192
_reflns_number_total             12529
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12529
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0794
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1175P)²+2.8594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2483
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: N22A(0.5) N22B(0.5)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C100(H100)
3.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
3.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C300(H30D,H30E,H30F), C200(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.4415(2) 0.7701(2) 0.95969(18) 0.0253(6) Uani 1 d . . .
C2 C 0.4931(2) 0.7132(2) 1.00134(18) 0.0259(6) Uani 1 d . . .
H2 H 0.5082 0.6474 0.9699 0.031 Uiso 1 calc . . R
C3 C 0.5240(2) 0.7472(2) 1.08648(19) 0.0280(7) Uani 1 d . . .
C4 C 0.5027(2) 0.8453(3) 1.13077(19) 0.0313(7) Uani 1 d . . .
C5 C 0.4511(3) 0.9048(3) 1.09266(19) 0.0326(7) Uani 1 d . . .
H5 H 0.4372 0.9712 1.1239 0.039 Uiso 1 calc . . R
C6 C 0.4197(2) 0.8658(2) 1.00772(19) 0.0276(7) Uani 1 d . . .
C7 C 0.5782(2) 0.6853(3) 1.13266(19) 0.0295(7) Uani 1 d . . .
H7 H 0.6348 0.7338 1.1708 0.035 Uiso 1 calc . . R
C8 C 0.5101(2) 0.6470(2) 1.18706(18) 0.0265(6) Uani 1 d . . .
C9 C 0.4087(2) 0.6102(2) 1.16045(18) 0.0264(6) Uani 1 d . . .
H9 H 0.3817 0.6099 1.1071 0.032 Uiso 1 calc . . R
C10 C 0.3454(2) 0.5740(2) 1.20825(18) 0.0249(6) Uani 1 d . . .
C11 C 0.3862(2) 0.5753(3) 1.28711(18) 0.0293(7) Uani 1 d . . .
C12 C 0.4866(2) 0.6101(3) 1.3154(2) 0.0331(7) Uani 1 d . . .
H12 H 0.5140 0.6098 1.3685 0.040 Uiso 1 calc . . R
C13 C 0.5470(2) 0.6456(3) 1.26528(19) 0.0293(7) Uani 1 d . . .
C14 C 0.2353(2) 0.5313(2) 1.17617(17) 0.0232(6) Uani 1 d . . .
H14 H 0.1982 0.5419 1.2257 0.028 Uiso 1 calc . . R
C15 C 0.1877(2) 0.5898(2) 1.12306(17) 0.0217(6) Uani 1 d . . .
C16 C 0.1535(2) 0.5458(2) 1.03848(17) 0.0215(6) Uani 1 d . . .
H16 H 0.1608 0.4753 1.0124 0.026 Uiso 1 calc . . R
C17 C 0.1094(2) 0.6001(2) 0.99075(17) 0.0220(6) Uani 1 d . . .
C18 C 0.0980(2) 0.7027(2) 1.03063(18) 0.0239(6) Uani 1 d . . .
C19 C 0.1305(2) 0.7505(2) 1.11470(17) 0.0247(6) Uani 1 d . . .
H19 H 0.1221 0.8205 1.1409 0.030 Uiso 1 calc . . R
C20 C 0.1756(2) 0.6931(2) 1.15927(17) 0.0238(6) Uani 1 d . . .
C21 C 0.0780(2) 0.5554(2) 0.89752(17) 0.0231(6) Uani 1 d . . .
H21 H 0.0061 0.5657 0.8870 0.028 Uiso 1 calc . . R
C22 C 0.1394(2) 0.6163(2) 0.85266(17) 0.0233(6) Uani 1 d . . .
C23 C 0.2412(2) 0.6501(2) 0.87798(17) 0.0240(6) Uani 1 d . . .
H23 H 0.2716 0.6347 0.9245 0.029 Uiso 1 calc . . R
C24 C 0.3010(2) 0.7049(2) 0.83915(17) 0.0236(6) Uani 1 d . . .
C25 C 0.2543(2) 0.7268(2) 0.77131(18) 0.0284(7) Uani 1 d . . .
C26 C 0.1518(2) 0.6966(2) 0.74451(18) 0.0289(7) Uani 1 d . . .
H26 H 0.1208 0.7141 0.6993 0.035 Uiso 1 calc . . R
C27 C 0.0957(2) 0.6406(2) 0.78497(17) 0.0238(6) Uani 1 d . . .
C28 C 0.4134(2) 0.7344(2) 0.86604(18) 0.0266(6) Uani 1 d . . .
H28 H 0.4349 0.7941 0.8465 0.032 Uiso 1 calc . . R
C29 C 0.6248(3) 0.5952(3) 1.0777(2) 0.0384(8) Uani 1 d . . .
H29A H 0.5716 0.5451 1.0396 0.058 Uiso 1 calc . . GR
H29B H 0.6609 0.5614 1.1125 0.058 Uiso 1 calc . . GR
H29C H 0.6719 0.6214 1.0459 0.058 Uiso 1 calc . . GR
C30 C 0.2279(2) 0.4146(2) 1.13428(19) 0.0275(6) Uani 1 d . . .
H30A H 0.1577 0.3866 1.1127 0.041 Uiso 1 calc . . GR
H30B H 0.2520 0.3818 1.1747 0.041 Uiso 1 calc . . GR
H30C H 0.2692 0.4006 1.0886 0.041 Uiso 1 calc . . GR
C31 C 0.0843(2) 0.4402(2) 0.86167(18) 0.0272(7) Uani 1 d . . .
H31A H 0.1544 0.4275 0.8692 0.041 Uiso 1 calc . . GR
H31B H 0.0594 0.4166 0.8025 0.041 Uiso 1 calc . . GR
H31C H 0.0432 0.4023 0.8903 0.041 Uiso 1 calc . . GR
C32 C 0.4683(3) 0.6442(3) 0.8203(2) 0.0359(8) Uani 1 d . . .
H32A H 0.5410 0.6633 0.8357 0.054 Uiso 1 calc . . GR
H32B H 0.4522 0.6291 0.7604 0.054 Uiso 1 calc . . GR
H32C H 0.4466 0.5828 0.8357 0.054 Uiso 1 calc . . GR
C33 C 0.5255(4) 0.9818(3) 1.2600(2) 0.0568(12) Uani 1 d . . .
H33A H 0.5612 1.0296 1.2361 0.085 Uiso 1 calc . . GR
H33B H 0.5537 0.9966 1.3179 0.085 Uiso 1 calc . . GR
H33C H 0.4540 0.9905 1.2574 0.085 Uiso 1 calc . . GR
C34 C 0.3537(3) 0.5621(4) 1.4190(2) 0.0667(15) Uani 1 d . . .
H34A H 0.4079 0.5212 1.4257 0.100 Uiso 1 calc . . GR
H34B H 0.2973 0.5443 1.4469 0.100 Uiso 1 calc . . GR
H34C H 0.3785 0.6359 1.4435 0.100 Uiso 1 calc . . GR
C35 C 0.0750(4) 0.8622(3) 1.0075(3) 0.0583(12) Uani 1 d . . .
H35A H 0.0491 0.8883 0.9633 0.087 Uiso 1 calc . . GR
H35B H 0.1482 0.8801 1.0187 0.087 Uiso 1 calc . . GR
H35C H 0.0446 0.8937 1.0578 0.087 Uiso 1 calc . . GR
C36 C 0.2727(3) 0.7981(4) 0.6606(2) 0.0535(11) Uani 1 d . . .
H36A H 0.2472 0.7317 0.6185 0.080 Uiso 1 calc . . GR
H36B H 0.3240 0.8354 0.6393 0.080 Uiso 1 calc . . GR
H36C H 0.2172 0.8393 0.6737 0.080 Uiso 1 calc . . GR
C41 C 0.3401(3) 1.0163(2) 1.0133(2) 0.0331(7) Uani 1 d . . .
H41A H 0.4009 1.0674 1.0360 0.040 Uiso 1 calc . . R
H41B H 0.3065 1.0069 1.0603 0.040 Uiso 1 calc . . R
C42 C 0.2705(3) 1.0552(3) 0.9601(2) 0.0337(7) Uani 1 d . . .
C43 C 0.2278(4) 0.9958(4) 0.8809(3) 0.0635(13) Uani 1 d . . .
H43 H 0.2445 0.9282 0.8568 0.076 Uiso 1 calc . . R
C44 C 0.1610(5) 1.0365(4) 0.8383(3) 0.0778(17) Uani 1 d . . .
H44 H 0.1327 0.9945 0.7843 0.093 Uiso 1 calc . . R
C45 C 0.1735(3) 1.1855(3) 0.9416(2) 0.0489(10) Uani 1 d . . .
H45 H 0.1550 1.2528 0.9639 0.059 Uiso 1 calc . . R
C46 C 0.2413(3) 1.1521(3) 0.9901(2) 0.0428(9) Uani 1 d . . .
H46 H 0.2678 1.1959 1.0440 0.051 Uiso 1 calc . . R
C51 C 0.6694(3) 0.7711(3) 1.3598(2) 0.0447(9) Uani 1 d . . .
H51A H 0.6495 0.7591 1.4109 0.054 Uiso 1 calc . . R
H51B H 0.6305 0.8240 1.3480 0.054 Uiso 1 calc . . R
C52 C 0.7806(3) 0.8073(3) 1.3706(2) 0.0373(8) Uani 1 d . . .
C53 C 0.8292(3) 0.8118(4) 1.3037(2) 0.0504(10) Uani 1 d . . .
H53 H 0.7935 0.7889 1.2495 0.060 Uiso 1 calc . . R
C54 C 0.9303(3) 0.8499(4) 1.3161(3) 0.0527(11) Uani 1 d . . .
H54 H 0.9625 0.8527 1.2694 0.063 Uiso 1 calc . . R
C55 C 0.9374(3) 0.8754(3) 1.4537(2) 0.0437(9) Uani 1 d . . .
H55 H 0.9751 0.8969 1.5071 0.052 Uiso 1 calc . . R
C56 C 0.8374(3) 0.8387(3) 1.4472(2) 0.0377(8) Uani 1 d . . .
H56 H 0.8078 0.8351 1.4948 0.045 Uiso 1 calc . . R
C61 C 0.2258(3) 0.8431(3) 1.2773(2) 0.0452(10) Uani 1 d . . .
H61A H 0.1606 0.8712 1.2806 0.054 Uiso 1 calc . . R
H61B H 0.2655 0.8739 1.2426 0.054 Uiso 1 calc . . R
C62 C 0.2820(3) 0.8683(2) 1.36268(19) 0.0336(8) Uani 1 d . . .
C63 C 0.3793(3) 0.8477(3) 1.3750(2) 0.0425(9) Uani 1 d . . .
H63 H 0.4133 0.8167 1.3291 0.051 Uiso 1 calc . . R
C64 C 0.4268(3) 0.8726(3) 1.4548(2) 0.0464(9) Uani 1 d . . .
H64 H 0.4941 0.8582 1.4619 0.056 Uiso 1 calc . . R
C65 C 0.2907(3) 0.9349(3) 1.5097(2) 0.0451(9) Uani 1 d . . .
H65 H 0.2582 0.9653 1.5567 0.054 Uiso 1 calc . . R
C66 C 0.2375(3) 0.9133(3) 1.4321(2) 0.0401(8) Uani 1 d . . .
H66 H 0.1707 0.9294 1.4268 0.048 Uiso 1 calc . . R
C71 C -0.0567(3) 0.6369(3) 0.69747(19) 0.0332(7) Uani 1 d . . .
H71A H -0.1234 0.5946 0.6786 0.040 Uiso 1 calc . . R
H71B H -0.0181 0.6241 0.6494 0.040 Uiso 1 calc . . R
C72 C -0.0711(3) 0.7495(3) 0.7266(2) 0.0333(7) Uani 1 d . . .
C73 C -0.0826(3) 0.7990(3) 0.8078(2) 0.0406(8) Uani 1 d . . .
H73 H -0.0775 0.7637 0.8478 0.049 Uiso 1 calc . . R
C74 C -0.1017(3) 0.9005(3) 0.8305(3) 0.0516(10) Uani 1 d . . .
H74 H -0.1113 0.9325 0.8866 0.062 Uiso 1 calc . . R
C75 C -0.0949(3) 0.9091(3) 0.7011(3) 0.0539(11) Uani 1 d . . .
H75 H -0.0980 0.9473 0.6631 0.065 Uiso 1 calc . . R
C76 C -0.0774(3) 0.8065(3) 0.6716(2) 0.0455(9) Uani 1 d . . .
H76 H -0.0698 0.7758 0.6149 0.055 Uiso 1 calc . . R
C100 C 0.3701(4) 0.2356(4) 0.3549(3) 0.0693(13) Uani 1 d . . .
H100 H 0.3193 0.2828 0.3757 0.083 Uiso 1 calc . . R
C300 C 0.0946(4) 0.6483(3) 0.3732(3) 0.0625(13) Uani 1 d . . .
H30D H 0.0532 0.5906 0.3306 0.094 Uiso 1 calc . . GR
H30E H 0.1657 0.6444 0.3662 0.094 Uiso 1 calc . . GR
H30F H 0.0763 0.7138 0.3678 0.094 Uiso 1 calc . . GR
C301 C 0.0775(4) 0.6427(4) 0.4541(3) 0.0622(12) Uani 1 d . . .
N1 N 0.1328(3) 1.1298(3) 0.8663(2) 0.0619(10) Uani 1 d . . .
N2 N 0.9846(2) 0.8827(3) 1.3904(2) 0.0512(9) Uani 1 d . . .
N3 N 0.3845(3) 0.9155(3) 1.52226(18) 0.0452(8) Uani 1 d . . .
N4 N -0.1076(3) 0.9569(3) 0.7792(2) 0.0567(9) Uani 1 d . . .
C200 C 0.1976(6) 0.4589(5) 0.6342(4) 0.104(2) Uani 1 d A . .
H20A H 0.1751 0.4051 0.6580 0.156 Uiso 1 calc . . GR
H20B H 0.1408 0.4947 0.6236 0.156 Uiso 1 calc . . GR
H20C H 0.2504 0.5086 0.6731 0.156 Uiso 1 calc . . GR
C201 C 0.2354(6) 0.4138(4) 0.5601(5) 0.097(2) Uani 1 d . . .
N22A N 0.2379(11) 0.3743(12) 0.4843(9) 0.087(4) Uani 0.50 d A 1 .
N22B N 0.2915(13) 0.3797(13) 0.5158(10) 0.100(5) Uani 0.50 d A 2 .
N302 N 0.0657(4) 0.6392(6) 0.5176(3) 0.114(2) Uani 1 d . . .
O4 O 0.53655(19) 0.87828(19) 1.21445(13) 0.0401(6) Uani 1 d . . .
O6 O 0.36792(18) 0.92088(17) 0.96612(13) 0.0343(5) Uani 1 d . . .
O11 O 0.32063(18) 0.5401(2) 1.33276(14) 0.0399(6) Uani 1 d . . .
O13 O 0.64960(16) 0.67716(19) 1.29214(13) 0.0341(5) Uani 1 d . . .
O18 O 0.05047(17) 0.75360(16) 0.98263(12) 0.0291(5) Uani 1 d . . .
O20 O 0.20980(17) 0.73456(16) 1.24276(12) 0.0296(5) Uani 1 d . . .
O25 O 0.31532(18) 0.78047(19) 0.73295(13) 0.0364(6) Uani 1 d . . .
O27 O -0.00541(16) 0.60428(16) 0.75999(13) 0.0286(5) Uani 1 d . . .
Cl1 Cl 0.35341(13) 0.19527(14) 0.24609(9) 0.0975(6) Uani 1 d . . .
Cl2 Cl 0.48850(15) 0.30227(19) 0.39122(12) 0.1272(8) Uani 1 d . . .
Cl3 Cl 0.35102(11) 0.12744(11) 0.38986(8) 0.0747(4) Uani 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 C2 1.396(4) . ?
C1 C6 1.392(4) . ?
C1 C28 1.524(4) . ?
C2 C3 1.396(4) . ?
C3 C4 1.398(5) . ?
C3 C7 1.515(4) . ?
C4 C5 1.385(5) . ?
C4 O4 1.382(4) . ?
C5 C6 1.395(4) . ?
C6 O6 1.378(4) . ?
C7 C8 1.527(4) . ?
C7 C29 1.531(5) . ?
C8 C9 1.395(4) . ?
C8 C13 1.390(4) . ?
C9 C10 1.387(4) . ?
C10 C11 1.404(4) . ?
C10 C14 1.529(4) . ?
C11 C12 1.382(5) . ?
C11 O11 1.374(4) . ?
C12 C13 1.389(5) . ?
C13 O13 1.400(4) . ?
C14 C15 1.521(4) . ?
C14 C30 1.528(4) . ?
C15 C16 1.401(4) . ?
C15 C20 1.393(4) . ?
C16 C17 1.391(4) . ?
C17 C18 1.393(4) . ?
C17 C21 1.526(4) . ?
C18 C19 1.395(4) . ?
C18 O18 1.381(3) . ?
C19 C20 1.391(4) . ?
C20 O20 1.382(3) . ?
C21 C22 1.526(4) . ?
C21 C31 1.522(4) . ?
C22 C23 1.390(4) . ?
C22 C27 1.395(4) . ?
C23 C24 1.390(4) . ?
C24 C25 1.395(4) . ?
C24 C28 1.522(4) . ?
C25 C26 1.396(5) . ?
C25 O25 1.384(4) . ?
C26 C27 1.392(4) . ?
C27 O27 1.386(4) . ?
C28 C32 1.540(4) . ?
C33 O4 1.424(5) . ?
C34 O11 1.432(4) . ?
C35 O18 1.414(4) . ?
C36 O25 1.414(4) . ?
C41 C42 1.493(5) . ?
C41 O6 1.415(4) . ?
C42 C43 1.388(5) . ?
C42 C46 1.378(5) . ?
C43 C44 1.369(6) . ?
C44 N1 1.326(6) . ?
C45 C46 1.380(5) . ?
C45 N1 1.318(5) . ?
C51 C52 1.509(5) . ?
C51 O13 1.427(4) . ?
C52 C53 1.380(5) . ?
C52 C56 1.378(5) . ?
C53 C54 1.384(5) . ?
C54 N2 1.332(5) . ?
C55 C56 1.374(5) . ?
C55 N2 1.326(5) . ?
C61 C62 1.507(4) . ?
C61 O20 1.409(4) . ?
C62 C63 1.378(5) . ?
C62 C66 1.377(5) . ?
C63 C64 1.381(5) . ?
C64 N3 1.328(5) . ?
C65 C66 1.381(5) . ?
C65 N3 1.328(5) . ?
C71 C72 1.507(5) . ?
C71 O27 1.426(4) . ?
C72 C73 1.375(5) . ?
C72 C76 1.393(5) . ?
C73 C74 1.381(5) . ?
C74 N4 1.333(5) . ?
C75 C76 1.392(6) . ?
C75 N4 1.330(5) . ?
C100 Cl1 1.758(5) . ?
C100 Cl2 1.722(5) . ?
C100 Cl3 1.761(5) . ?
C300 C301 1.445(6) . ?
C301 N302 1.124(6) . ?
C200 C201 1.393(9) . ?
C201 N22A 1.247(16) . ?
C201 N22B 1.146(16) . ?

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
C2 C1 C28 123.3(3) . . ?
C6 C1 C2 116.6(3) . . ?
C6 C1 C28 120.1(3) . . ?
C1 C2 C3 124.0(3) . . ?
C2 C3 C4 116.6(3) . . ?
C2 C3 C7 124.5(3) . . ?
C4 C3 C7 118.9(3) . . ?
C5 C4 C3 121.8(3) . . ?
O4 C4 C3 115.4(3) . . ?
O4 C4 C5 122.8(3) . . ?
C4 C5 C6 119.1(3) . . ?
C1 C6 C5 121.9(3) . . ?
O6 C6 C1 116.1(3) . . ?
O6 C6 C5 122.0(3) . . ?
C3 C7 C8 111.3(3) . . ?
C3 C7 C29 114.7(3) . . ?
C8 C7 C29 110.2(3) . . ?
C9 C8 C7 121.9(3) . . ?
C13 C8 C7 121.3(3) . . ?
C13 C8 C9 116.8(3) . . ?
C10 C9 C8 123.1(3) . . ?
C9 C10 C11 117.8(3) . . ?
C9 C10 C14 121.7(3) . . ?
C11 C10 C14 120.4(3) . . ?
C12 C11 C10 120.9(3) . . ?
O11 C11 C10 115.9(3) . . ?
O11 C11 C12 123.3(3) . . ?
C11 C12 C13 119.2(3) . . ?
C8 C13 O13 118.2(3) . . ?
C12 C13 C8 122.2(3) . . ?
C12 C13 O13 119.5(3) . . ?
C15 C14 C10 112.3(2) . . ?
C15 C14 C30 114.7(2) . . ?
C30 C14 C10 108.8(2) . . ?
C16 C15 C14 123.9(3) . . ?
C20 C15 C14 119.3(2) . . ?
C20 C15 C16 116.8(3) . . ?
C17 C16 C15 123.3(3) . . ?
C16 C17 C18 117.3(3) . . ?
C16 C17 C21 123.9(3) . . ?
C18 C17 C21 118.7(3) . . ?
C17 C18 C19 121.9(3) . . ?
O18 C18 C17 116.2(2) . . ?
O18 C18 C19 122.0(3) . . ?
C20 C19 C18 118.5(3) . . ?
C19 C20 C15 122.2(3) . . ?
O20 C20 C15 115.6(3) . . ?
O20 C20 C19 122.1(3) . . ?
C17 C21 C22 109.8(2) . . ?
C31 C21 C17 114.3(2) . . ?
C31 C21 C22 110.6(2) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C22 C27 117.4(3) . . ?
C27 C22 C21 121.4(3) . . ?
C24 C23 C22 123.7(3) . . ?
C23 C24 C25 116.9(3) . . ?
C23 C24 C28 121.6(3) . . ?
C25 C24 C28 121.3(3) . . ?
C24 C25 C26 121.6(3) . . ?
O25 C25 C24 116.0(3) . . ?
O25 C25 C26 122.4(3) . . ?
C27 C26 C25 119.1(3) . . ?
C26 C27 C22 121.2(3) . . ?
O27 C27 C22 116.2(3) . . ?
O27 C27 C26 122.6(3) . . ?
C1 C28 C32 113.2(3) . . ?
C24 C28 C1 113.6(2) . . ?
C24 C28 C32 108.8(3) . . ?
O6 C41 C42 109.8(3) . . ?
C43 C42 C41 123.0(3) . . ?
C46 C42 C41 120.4(3) . . ?
C46 C42 C43 116.5(3) . . ?
C44 C43 C42 118.7(4) . . ?
N1 C44 C43 125.3(4) . . ?
N1 C45 C46 124.0(4) . . ?
C42 C46 C45 119.9(3) . . ?
O13 C51 C52 107.6(3) . . ?
C53 C52 C51 120.8(3) . . ?
C56 C52 C51 121.9(3) . . ?
C56 C52 C53 117.3(3) . . ?
C52 C53 C54 119.4(4) . . ?
N2 C54 C53 123.2(4) . . ?
N2 C55 C56 124.2(3) . . ?
C55 C56 C52 119.3(3) . . ?
O20 C61 C62 107.4(3) . . ?
C63 C62 C61 122.0(3) . . ?
C66 C62 C61 120.9(3) . . ?
C66 C62 C63 117.1(3) . . ?
C62 C63 C64 119.2(3) . . ?
N3 C64 C63 124.2(4) . . ?
N3 C65 C66 123.8(3) . . ?
C62 C66 C65 119.7(4) . . ?
O27 C71 C72 113.1(3) . . ?
C73 C72 C71 121.4(3) . . ?
C73 C72 C76 117.4(3) . . ?
C76 C72 C71 121.2(3) . . ?
C72 C73 C74 119.2(4) . . ?
N4 C74 C73 124.5(4) . . ?
N4 C75 C76 124.0(4) . . ?
C75 C76 C72 118.8(4) . . ?
Cl1 C100 Cl3 109.7(3) . . ?
Cl2 C100 Cl1 109.7(3) . . ?
Cl2 C100 Cl3 111.3(3) . . ?
N302 C301 C300 178.9(6) . . ?
C45 N1 C44 115.5(4) . . ?
C55 N2 C54 116.5(3) . . ?
C65 N3 C64 116.1(3) . . ?
C75 N4 C74 115.9(4) . . ?
N22A C201 C200 159.6(11) . . ?
N22B C201 C200 159.3(13) . . ?
N22B C201 N22A 41.1(8) . . ?
C4 O4 C33 117.0(3) . . ?
C6 O6 C41 117.8(2) . . ?
C11 O11 C34 116.7(3) . . ?
C13 O13 C51 113.3(3) . . ?
C18 O18 C35 116.6(2) . . ?
C20 O20 C61 117.9(2) . . ?
C25 O25 C36 117.9(3) . . ?
C27 O27 C71 118.5(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
C1 C2 C3 C4 -1.4(4) . . . . ?
C1 C2 C3 C7 178.7(3) . . . . ?
C1 C6 O6 C41 177.0(3) . . . . ?
C2 C1 C6 C5 2.3(4) . . . . ?
C2 C1 C6 O6 -179.4(3) . . . . ?
C2 C1 C28 C24 111.1(3) . . . . ?
C2 C1 C28 C32 -13.6(4) . . . . ?
C2 C3 C4 C5 1.8(5) . . . . ?
C2 C3 C4 O4 -178.2(3) . . . . ?
C2 C3 C7 C8 -109.0(3) . . . . ?
C2 C3 C7 C29 16.9(4) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C3 C4 O4 C33 173.7(3) . . . . ?
C3 C7 C8 C9 40.0(4) . . . . ?
C3 C7 C8 C13 -141.1(3) . . . . ?
C4 C3 C7 C8 71.1(4) . . . . ?
C4 C3 C7 C29 -163.0(3) . . . . ?
C4 C5 C6 C1 -1.9(5) . . . . ?
C4 C5 C6 O6 179.9(3) . . . . ?
C5 C4 O4 C33 -6.3(5) . . . . ?
C5 C6 O6 C41 -4.8(4) . . . . ?
C6 C1 C2 C3 -0.6(4) . . . . ?
C6 C1 C28 C24 -71.9(4) . . . . ?
C6 C1 C28 C32 163.4(3) . . . . ?
C7 C3 C4 C5 -178.3(3) . . . . ?
C7 C3 C4 O4 1.7(4) . . . . ?
C7 C8 C9 C10 179.3(3) . . . . ?
C7 C8 C13 C12 -179.3(3) . . . . ?
C7 C8 C13 O13 -2.1(5) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C8 C9 C10 C14 -178.2(3) . . . . ?
C8 C13 O13 C51 112.9(3) . . . . ?
C9 C8 C13 C12 -0.4(5) . . . . ?
C9 C8 C13 O13 176.8(3) . . . . ?
C9 C10 C11 C12 -0.9(5) . . . . ?
C9 C10 C11 O11 179.2(3) . . . . ?
C9 C10 C14 C15 -36.6(4) . . . . ?
C9 C10 C14 C30 91.4(3) . . . . ?
C10 C11 C12 C13 1.0(5) . . . . ?
C10 C11 O11 C34 -166.2(4) . . . . ?
C10 C14 C15 C16 115.0(3) . . . . ?
C10 C14 C15 C20 -65.5(3) . . . . ?
C11 C10 C14 C15 144.9(3) . . . . ?
C11 C10 C14 C30 -87.1(3) . . . . ?
C11 C12 C13 C8 -0.3(5) . . . . ?
C11 C12 C13 O13 -177.5(3) . . . . ?
C12 C11 O11 C34 13.9(5) . . . . ?
C12 C13 O13 C51 -69.9(4) . . . . ?
C13 C8 C9 C10 0.4(5) . . . . ?
C14 C10 C11 C12 177.5(3) . . . . ?
C14 C10 C11 O11 -2.4(4) . . . . ?
C14 C15 C16 C17 179.6(3) . . . . ?
C14 C15 C20 C19 -178.5(3) . . . . ?
C14 C15 C20 O20 0.4(4) . . . . ?
C15 C16 C17 C18 -1.1(4) . . . . ?
C15 C16 C17 C21 175.9(3) . . . . ?
C15 C20 O20 C61 162.6(3) . . . . ?
C16 C15 C20 C19 1.0(4) . . . . ?
C16 C15 C20 O20 179.9(2) . . . . ?
C16 C17 C18 C19 1.0(4) . . . . ?
C16 C17 C18 O18 -177.6(2) . . . . ?
C16 C17 C21 C22 -116.4(3) . . . . ?
C16 C17 C21 C31 8.7(4) . . . . ?
C17 C18 C19 C20 0.0(4) . . . . ?
C17 C18 O18 C35 -153.4(3) . . . . ?
C17 C21 C22 C23 39.7(4) . . . . ?
C17 C21 C22 C27 -140.1(3) . . . . ?
C18 C17 C21 C22 60.5(3) . . . . ?
C18 C17 C21 C31 -174.4(3) . . . . ?
C18 C19 C20 C15 -1.1(4) . . . . ?
C18 C19 C20 O20 -179.9(3) . . . . ?
C19 C18 O18 C35 28.0(4) . . . . ?
C19 C20 O20 C61 -18.5(4) . . . . ?
C20 C15 C16 C17 0.1(4) . . . . ?
C21 C17 C18 C19 -176.1(3) . . . . ?
C21 C17 C18 O18 5.3(4) . . . . ?
C21 C22 C23 C24 179.4(3) . . . . ?
C21 C22 C27 C26 179.7(3) . . . . ?
C21 C22 C27 O27 -1.5(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C22 C23 C24 C28 -176.2(3) . . . . ?
C22 C27 O27 C71 172.8(3) . . . . ?
C23 C22 C27 C26 -0.1(4) . . . . ?
C23 C22 C27 O27 178.8(3) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C23 C24 C25 O25 -179.3(3) . . . . ?
C23 C24 C28 C1 -40.6(4) . . . . ?
C23 C24 C28 C32 86.5(3) . . . . ?
C24 C25 C26 C27 -2.0(5) . . . . ?
C24 C25 O25 C36 175.7(3) . . . . ?
C25 C24 C28 C1 143.0(3) . . . . ?
C25 C24 C28 C32 -89.9(3) . . . . ?
C25 C26 C27 C22 1.4(5) . . . . ?
C25 C26 C27 O27 -177.3(3) . . . . ?
C26 C25 O25 C36 -4.6(5) . . . . ?
C26 C27 O27 C71 -8.3(4) . . . . ?
C27 C22 C23 C24 -0.8(4) . . . . ?
C28 C1 C2 C3 176.5(3) . . . . ?
C28 C1 C6 C5 -174.9(3) . . . . ?
C28 C1 C6 O6 3.4(4) . . . . ?
C28 C24 C25 C26 177.6(3) . . . . ?
C28 C24 C25 O25 -2.8(4) . . . . ?
C29 C7 C8 C9 -88.4(4) . . . . ?
C29 C7 C8 C13 90.5(4) . . . . ?
C30 C14 C15 C16 -9.8(4) . . . . ?
C30 C14 C15 C20 169.7(3) . . . . ?
C31 C21 C22 C23 -87.5(3) . . . . ?
C31 C21 C22 C27 92.8(3) . . . . ?
C41 C42 C43 C44 176.9(5) . . . . ?
C41 C42 C46 C45 -177.1(3) . . . . ?
C42 C41 O6 C6 -170.5(3) . . . . ?
C42 C43 C44 N1 0.0(9) . . . . ?
C43 C42 C46 C45 -0.4(6) . . . . ?
C43 C44 N1 C45 -0.2(9) . . . . ?
C46 C42 C43 C44 0.3(7) . . . . ?
C46 C45 N1 C44 0.1(7) . . . . ?
C51 C52 C53 C54 177.0(4) . . . . ?
C51 C52 C56 C55 -177.0(4) . . . . ?
C52 C51 O13 C13 -168.5(3) . . . . ?
C52 C53 C54 N2 0.3(7) . . . . ?
C53 C52 C56 C55 2.0(6) . . . . ?
C53 C54 N2 C55 1.4(7) . . . . ?
C56 C52 C53 C54 -2.0(6) . . . . ?
C56 C55 N2 C54 -1.4(6) . . . . ?
C61 C62 C63 C64 180.0(3) . . . . ?
C61 C62 C66 C65 179.6(3) . . . . ?
C62 C61 O20 C20 -168.6(3) . . . . ?
C62 C63 C64 N3 0.4(6) . . . . ?
C63 C62 C66 C65 -0.5(5) . . . . ?
C63 C64 N3 C65 -0.3(6) . . . . ?
C66 C62 C63 C64 0.0(5) . . . . ?
C66 C65 N3 C64 -0.2(6) . . . . ?
C71 C72 C73 C74 -176.1(4) . . . . ?
C71 C72 C76 C75 177.3(4) . . . . ?
C72 C71 O27 C27 -69.6(4) . . . . ?
C72 C73 C74 N4 -1.8(7) . . . . ?
C73 C72 C76 C75 -0.1(6) . . . . ?
C73 C74 N4 C75 0.8(7) . . . . ?
C76 C72 C73 C74 1.3(6) . . . . ?
C76 C75 N4 C74 0.6(7) . . . . ?
N1 C45 C46 C42 0.3(7) . . . . ?
N2 C55 C56 C52 -0.3(6) . . . . ?
N3 C65 C66 C62 0.6(6) . . . . ?
N4 C75 C76 C72 -0.9(7) . . . . ?
O4 C4 C5 C6 179.8(3) . . . . ?
O6 C41 C42 C43 10.2(5) . . . . ?
O6 C41 C42 C46 -173.3(3) . . . . ?
O11 C11 C12 C13 -179.1(3) . . . . ?
O13 C51 C52 C53 48.4(5) . . . . ?
O13 C51 C52 C56 -132.6(4) . . . . ?
O18 C18 C19 C20 178.5(3) . . . . ?
O20 C61 C62 C63 66.9(5) . . . . ?
O20 C61 C62 C66 -113.1(4) . . . . ?
O25 C25 C26 C27 178.4(3) . . . . ?
O27 C71 C72 C73 -31.1(5) . . . . ?
O27 C71 C72 C76 151.6(3) . . . . ?



_ins_header                      
;
TITL data_2-MeCN in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  13.464050  13.687265  17.077117 107.6574  95.0148  95.4814
ZERR    2.00   0.000578   0.000552   0.000647   0.0035   0.0033   0.0034
LATT  1
SFAC C H N O
UNIT 120.00 120.00 8.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2-CHCl3
_database_code_depnum_ccdc_archive 'CCDC 1044955'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-09-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C60 H60 N4 O8, 3(C H Cl3)'
_chemical_formula_sum            'C63 H60 Cl9 D3 N4 O8'
_chemical_formula_weight         1326.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 O4 N4'
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'
D D 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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   13.5142(6)
_cell_length_b                   14.6744(7)
_cell_length_c                   17.3471(7)
_cell_angle_alpha                95.199(4)
_cell_angle_beta                 94.142(3)
_cell_angle_gamma                110.327(4)
_cell_volume                     3192.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.4850
_cell_measurement_theta_min      2.6080
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.3486
_exptl_crystal_size_mid          0.2352
_exptl_crystal_size_min          0.1686
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31467
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.90
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -60.00  -35.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470 -178.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega   21.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  -60.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega  -12.00   52.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  120.0000 64

#__ type_ start__ end____ width___ exp.time_
  4 omega  -20.00   16.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega   36.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000 -180.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega   -7.00   56.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   77.0000   60.0000 63

#__ type_ start__ end____ width___ exp.time_
  7 omega  -42.00   38.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000  150.0000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -21.00   96.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   19.0000  -30.0000 117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0494785000
_diffrn_orient_matrix_UB_12      0.0393806000
_diffrn_orient_matrix_UB_13      0.0043468000
_diffrn_orient_matrix_UB_21      0.0158324000
_diffrn_orient_matrix_UB_22      -0.0168947000
_diffrn_orient_matrix_UB_23      0.0341384000
_diffrn_orient_matrix_UB_31      0.0217506000
_diffrn_orient_matrix_UB_32      -0.0293601000
_diffrn_orient_matrix_UB_33      -0.0228573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7597
_reflns_number_total             17182
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0043(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         17182
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1888
_refine_ls_R_factor_gt           0.0995
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1480P)²+1.8200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2709
_refine_ls_wR_factor_ref         0.3386
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {D20A,D20B,D201} of C201, All C(H,H) groups
 At 1.5 times of:
  {H29A,H29B,H29C} of C29, {H30A,H30B,H30C} of C30, {H31A,H31B,H31C} of C31,
  {H32A,H32B,H32C} of C32, {H33A,H33B,H33C} of C33, {H34A,H34B,H34C} of C34,
  {H35A,H35B,H35C} of C35, {H36A,H36B,H36C} of C36
2. Restrained distances
 C201-Cl4C = C201-Cl5C
 1.79 with sigma of 0.02
 Cl7B-C301
 1.79 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl4A \\sim Cl4C \\sim Cl5A \\sim Cl5C \\sim Cl6A \\sim Cl6C: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Cl7B) = Uanis(Cl7A)
4. Others
 1*[Sof(D201)+Sof(Cl4A)+Sof(Cl5A)+Sof(Cl6A)]+1*[Sof(D20A)+Sof(Cl4B)+Sof(Cl5B)+
 Sof(Cl6B)]+1*[Sof(D20B)+Sof(Cl4C)+Sof(Cl5C)+Sof(Cl6C)]=1 with esd of 0.001
 Sof(D201)=Sof(Cl4A)=Sof(Cl5A)=Sof(Cl6A)=FVAR(1)
 Sof(D20A)=Sof(Cl4B)=Sof(Cl5B)=Sof(Cl6B)=FVAR(2)
 Sof(D20B)=Sof(Cl4C)=Sof(Cl5C)=Sof(Cl6C)=FVAR(3)
 Fixed Sof: Cl7A(0.5) Cl7B(0.5) D301(0.5) D30D(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C101(D101), C301(D301), C301(D30D),
 C201(D20A), C201(D20B), C201(D201)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.5190(3) 0.6383(3) 0.4445(2) 0.0377(8) Uani 1 d . . .
C2 C 0.4503(3) 0.6680(3) 0.4887(2) 0.0386(9) Uani 1 d . . .
H2 H 0.3950 0.6827 0.4618 0.046 Uiso 1 calc . . R
C3 C 0.4583(3) 0.6771(3) 0.5693(2) 0.0366(8) Uani 1 d . . .
C4 C 0.5402(3) 0.6539(3) 0.6075(2) 0.0399(9) Uani 1 d . . .
C5 C 0.6117(3) 0.6255(3) 0.5661(2) 0.0389(9) Uani 1 d . . .
H5 H 0.6670 0.6107 0.5928 0.047 Uiso 1 calc . . R
C6 C 0.6008(3) 0.6192(3) 0.4858(2) 0.0372(8) Uani 1 d . . .
C7 C 0.3868(3) 0.7109(3) 0.6181(2) 0.0400(9) Uani 1 d . . .
H7 H 0.3640 0.6635 0.6571 0.048 Uiso 1 calc . . R
C8 C 0.4465(3) 0.8117(3) 0.6646(2) 0.0404(9) Uani 1 d . . .
C9 C 0.5316(3) 0.8796(3) 0.6373(2) 0.0405(9) Uani 1 d . . .
H9 H 0.5537 0.8624 0.5891 0.049 Uiso 1 calc . . R
C10 C 0.5867(3) 0.9728(3) 0.6779(2) 0.0405(9) Uani 1 d . . .
C11 C 0.5512(3) 0.9960(3) 0.7474(2) 0.0439(10) Uani 1 d . . .
C12 C 0.4665(3) 0.9300(3) 0.7769(3) 0.0451(10) Uani 1 d . . .
H12 H 0.4447 0.9469 0.8253 0.054 Uiso 1 calc . . R
C13 C 0.4134(3) 0.8376(3) 0.7340(3) 0.0450(10) Uani 1 d . . .
C14 C 0.6763(3) 1.0495(3) 0.6452(3) 0.0463(10) Uani 1 d . . .
H14 H 0.7276 1.0899 0.6905 0.056 Uiso 1 calc . . R
C15 C 0.7367(3) 1.0051(3) 0.5928(3) 0.0425(9) Uani 1 d . . .
C16 C 0.7291(3) 1.0055(3) 0.5119(3) 0.0416(9) Uani 1 d . . .
H16 H 0.6829 1.0343 0.4891 0.050 Uiso 1 calc . . R
C17 C 0.7846(3) 0.9668(3) 0.4637(2) 0.0399(9) Uani 1 d . . .
C18 C 0.8502(3) 0.9223(3) 0.4979(2) 0.0405(9) Uani 1 d . . .
C19 C 0.8618(3) 0.9206(3) 0.5772(3) 0.0458(10) Uani 1 d . . .
H19 H 0.9080 0.8915 0.5997 0.055 Uiso 1 calc . . R
C20 C 0.8047(3) 0.9623(3) 0.6243(3) 0.0463(10) Uani 1 d . . .
C21 C 0.7786(3) 0.9703(3) 0.3763(2) 0.0412(9) Uani 1 d . . .
H21 H 0.8531 0.9920 0.3623 0.049 Uiso 1 calc . . R
C22 C 0.7192(3) 0.8702(3) 0.3307(2) 0.0400(9) Uani 1 d . . .
C23 C 0.6432(3) 0.7957(3) 0.3613(2) 0.0377(8) Uani 1 d . . .
H23 H 0.6266 0.8092 0.4124 0.045 Uiso 1 calc . . R
C24 C 0.5902(3) 0.7028(3) 0.3213(2) 0.0368(8) Uani 1 d . . .
C25 C 0.6142(3) 0.6848(3) 0.2463(2) 0.0393(9) Uani 1 d . . .
C26 C 0.6880(3) 0.7568(3) 0.2127(2) 0.0454(10) Uani 1 d . . .
H26 H 0.7036 0.7433 0.1613 0.054 Uiso 1 calc . . R
C27 C 0.7394(3) 0.8493(3) 0.2548(2) 0.0432(9) Uani 1 d . . .
C28 C 0.5064(3) 0.6242(3) 0.3566(2) 0.0384(9) Uani 1 d . . .
H28 H 0.5158 0.5609 0.3403 0.046 Uiso 1 calc . . R
C29 C 0.2856(3) 0.7099(3) 0.5723(3) 0.0476(10) Uani 1 d . . .
H29A H 0.3041 0.7587 0.5356 0.071 Uiso 1 calc . . GR
H29B H 0.2397 0.7256 0.6084 0.071 Uiso 1 calc . . GR
H29C H 0.2482 0.6448 0.5435 0.071 Uiso 1 calc . . GR
C30 C 0.6295(4) 1.1171(3) 0.6063(3) 0.0618(14) Uani 1 d . . .
H30A H 0.6852 1.1659 0.5833 0.093 Uiso 1 calc . . GR
H30B H 0.6005 1.1504 0.6453 0.093 Uiso 1 calc . . GR
H30C H 0.5727 1.0784 0.5655 0.093 Uiso 1 calc . . GR
C31 C 0.7310(4) 1.0437(3) 0.3507(3) 0.0530(11) Uani 1 d . . .
H31A H 0.6568 1.0234 0.3615 0.079 Uiso 1 calc . . GR
H31B H 0.7345 1.0467 0.2947 0.079 Uiso 1 calc . . GR
H31C H 0.7711 1.1085 0.3792 0.079 Uiso 1 calc . . GR
C32 C 0.3954(3) 0.6142(3) 0.3208(3) 0.0464(10) Uani 1 d . . .
H32A H 0.3416 0.5636 0.3439 0.070 Uiso 1 calc . . GR
H32B H 0.3885 0.5956 0.2644 0.070 Uiso 1 calc . . GR
H32C H 0.3851 0.6768 0.3311 0.070 Uiso 1 calc . . GR
C33 C 0.7540(3) 0.5751(3) 0.4794(3) 0.0489(10) Uani 1 d . . .
H33A H 0.7940 0.6319 0.5175 0.073 Uiso 1 calc . . GR
H33B H 0.8006 0.5649 0.4414 0.073 Uiso 1 calc . . GR
H33C H 0.7273 0.5168 0.5061 0.073 Uiso 1 calc . . GR
C34 C 0.2895(5) 0.7928(4) 0.8301(3) 0.0692(15) Uani 1 d . . .
H34A H 0.3444 0.8036 0.8736 0.104 Uiso 1 calc . . GR
H34B H 0.2252 0.7390 0.8383 0.104 Uiso 1 calc . . GR
H34C H 0.2732 0.8526 0.8273 0.104 Uiso 1 calc . . GR
C35 C 0.8927(5) 0.9341(6) 0.7391(3) 0.090(2) Uani 1 d . . .
H35A H 0.8817 0.8668 0.7176 0.135 Uiso 1 calc . . GR
H35B H 0.8889 0.9373 0.7954 0.135 Uiso 1 calc . . GR
H35C H 0.9627 0.9778 0.7288 0.135 Uiso 1 calc . . GR
C36 C 0.8301(6) 0.9121(5) 0.1465(3) 0.102(3) Uani 1 d . . .
H36A H 0.8593 0.8600 0.1379 0.153 Uiso 1 calc . . GR
H36B H 0.8798 0.9733 0.1325 0.153 Uiso 1 calc . . GR
H36C H 0.7620 0.8940 0.1141 0.153 Uiso 1 calc . . GR
C41 C 0.6319(4) 0.6568(4) 0.7310(3) 0.0538(11) Uani 1 d . . .
H41A H 0.6966 0.7102 0.7209 0.065 Uiso 1 calc . . R
H41B H 0.6408 0.5935 0.7167 0.065 Uiso 1 calc . . R
C42 C 0.6155(4) 0.6680(3) 0.8159(3) 0.0487(10) Uani 1 d . . .
C43 C 0.6737(4) 0.6390(4) 0.8690(3) 0.0635(13) Uani 1 d . . .
H43 H 0.7241 0.6114 0.8529 0.076 Uiso 1 calc . . R
C44 C 0.6587(4) 0.6500(4) 0.9462(3) 0.0661(14) Uani 1 d . . .
H44 H 0.7026 0.6317 0.9822 0.079 Uiso 1 calc . . R
C45 C 0.5290(5) 0.7097(4) 0.9214(3) 0.0729(16) Uani 1 d . . .
H45 H 0.4761 0.7331 0.9387 0.087 Uiso 1 calc . . R
C46 C 0.5410(4) 0.7036(4) 0.8429(3) 0.0615(13) Uani 1 d . . .
H46 H 0.4980 0.7239 0.8077 0.074 Uiso 1 calc . . R
C51 C 0.5508(4) 1.1411(3) 0.8236(3) 0.0558(12) Uani 1 d . . .
H51A H 0.5201 1.1096 0.8688 0.067 Uiso 1 calc . . R
H51B H 0.4917 1.1406 0.7862 0.067 Uiso 1 calc . . R
C52 C 0.6218(4) 1.2434(3) 0.8499(2) 0.0459(10) Uani 1 d . . .
C53 C 0.5846(4) 1.3037(3) 0.8969(3) 0.0502(11) Uani 1 d . . .
H53 H 0.5150 1.2792 0.9123 0.060 Uiso 1 calc . . R
C54 C 0.6489(5) 1.3981(4) 0.9206(3) 0.0641(14) Uani 1 d . . .
H54 H 0.6217 1.4373 0.9532 0.077 Uiso 1 calc . . R
C55 C 0.7819(4) 1.3816(4) 0.8553(3) 0.0571(12) Uani 1 d . . .
H55 H 0.8509 1.4081 0.8393 0.069 Uiso 1 calc . . R
C56 C 0.7227(4) 1.2846(3) 0.8295(3) 0.0492(10) Uani 1 d . . .
H56 H 0.7518 1.2465 0.7976 0.059 Uiso 1 calc . . R
C61 C 0.9649(3) 0.8312(3) 0.4746(3) 0.0477(10) Uani 1 d . . .
H61A H 0.9229 0.7803 0.5051 0.057 Uiso 1 calc . . R
H61B H 1.0277 0.8763 0.5091 0.057 Uiso 1 calc . . R
C62 C 0.9999(3) 0.7842(3) 0.4061(3) 0.0477(10) Uani 1 d . . .
C63 C 1.0690(4) 0.7358(4) 0.4182(4) 0.0694(15) Uani 1 d . . .
H63 H 1.0947 0.7313 0.4696 0.083 Uiso 1 calc . . R
C64 C 1.1009(5) 0.6934(4) 0.3545(5) 0.0815(18) Uani 1 d . . .
H64 H 1.1489 0.6603 0.3642 0.098 Uiso 1 calc . . R
C65 C 1.0024(7) 0.7422(7) 0.2716(4) 0.123(3) Uani 1 d . . .
H65 H 0.9777 0.7448 0.2195 0.148 Uiso 1 calc . . R
C66 C 0.9653(6) 0.7872(6) 0.3302(4) 0.095(2) Uani 1 d . . .
H66 H 0.9171 0.8194 0.3184 0.114 Uiso 1 calc . . R
C71 C 0.6063(4) 0.5566(3) 0.1473(2) 0.0504(11) Uani 1 d . . .
H71A H 0.6307 0.6077 0.1123 0.060 Uiso 1 calc . . R
H71B H 0.5521 0.4983 0.1165 0.060 Uiso 1 calc . . R
C72 C 0.6994(4) 0.5296(3) 0.1764(3) 0.0483(10) Uani 1 d . . .
C73 C 0.7695(5) 0.5167(4) 0.1269(3) 0.0688(15) Uani 1 d . . .
H73 H 0.7626 0.5291 0.0744 0.083 Uiso 1 calc . . R
C74 C 0.8498(5) 0.4858(5) 0.1532(4) 0.0825(18) Uani 1 d . . .
H74 H 0.8966 0.4769 0.1174 0.099 Uiso 1 calc . . R
C75 C 0.7975(4) 0.4816(4) 0.2736(3) 0.0577(12) Uani 1 d . . .
H75 H 0.8068 0.4698 0.3261 0.069 Uiso 1 calc . . R
C76 C 0.7146(4) 0.5122(4) 0.2519(3) 0.0586(12) Uani 1 d . . .
H76 H 0.6689 0.5209 0.2887 0.070 Uiso 1 calc . . R
C101 C 0.9887(4) 0.6170(4) 0.6768(3) 0.0644(14) Uani 1 d . . .
D101 H 1.0360 0.5975 0.7136 0.077 Uiso 1 calc . . R
N1 N 0.5892(4) 0.6838(4) 0.9745(2) 0.0687(12) Uani 1 d . . .
N2 N 0.7487(4) 1.4405(3) 0.9014(3) 0.0654(12) Uani 1 d . . .
N3 N 1.0693(4) 0.6960(4) 0.2818(4) 0.0878(16) Uani 1 d . . .
N4 N 0.8652(4) 0.4677(3) 0.2256(3) 0.0663(12) Uani 1 d . . .
O4 O 0.5428(2) 0.6605(2) 0.68661(17) 0.0496(7) Uani 1 d . . .
O6 O 0.6682(2) 0.5919(2) 0.44065(17) 0.0455(7) Uani 1 d . . .
O11 O 0.6082(2) 1.0882(2) 0.78789(18) 0.0527(8) Uani 1 d . . .
O13 O 0.3269(3) 0.7684(2) 0.75884(18) 0.0543(8) Uani 1 d . . .
O18 O 0.9024(2) 0.8837(2) 0.44630(18) 0.0505(8) Uani 1 d . . .
O20 O 0.8131(3) 0.9637(3) 0.70364(19) 0.0624(9) Uani 1 d . . .
O25 O 0.5587(2) 0.5916(2) 0.20785(16) 0.0455(7) Uani 1 d . . .
O27 O 0.8146(3) 0.9251(2) 0.22525(18) 0.0568(8) Uani 1 d . . .
Cl1 Cl 1.03607(15) 0.74471(12) 0.68222(12) 0.0952(6) Uani 1 d . . .
Cl2 Cl 0.99010(14) 0.56448(15) 0.58264(11) 0.0929(5) Uani 1 d . . .
Cl3 Cl 0.85915(12) 0.57279(16) 0.70330(13) 0.1049(6) Uani 1 d . . .
Cl7A Cl 0.8269(5) 1.1038(4) 0.9052(5) 0.167(2) Uani 0.50 d A 1 .
Cl7B Cl 0.7876(6) 1.1222(4) 0.9707(5) 0.167(2) Uani 0.50 d A 2 D
Cl8 Cl 0.6141(3) 0.9783(3) 0.98158(19) 0.1808(14) Uani 1 d A . .
Cl9 Cl 0.7822(2) 0.9129(2) 0.93606(14) 0.1372(9) Uani 1 d A . .
C301 C 0.7166(7) 0.9978(8) 0.9226(7) 0.176(6) Uani 1 d . . D
D301 H 0.6773 0.9732 0.8694 0.211 Uiso 0.50 calc A 1 R
D30D H 0.6919 0.9965 0.8667 0.211 Uiso 0.50 calc A 2 R
C201 C 0.9482(6) 0.6618(5) -0.0397(4) 0.0906(19) Uiso 1 d . . D
D20A H 0.8860 0.5992 -0.0528 0.109 Uiso 0.399(14) calc B 2 R
D20B H 0.8910 0.6010 -0.0662 0.109 Uiso 0.302(5) calc C 3 R
D201 H 0.8803 0.6064 -0.0589 0.109 Uiso 0.297(14) calc D 1 R
Cl4A Cl 0.9156(5) 0.7623(7) 0.0121(7) 0.085(3) Uiso 0.297(14) d B 1 .
Cl5A Cl 1.0330(13) 0.6152(13) 0.0144(9) 0.145(6) Uiso 0.297(14) d B 1 .
Cl6A Cl 0.9890(6) 0.7359(10) -0.1186(5) 0.095(3) Uiso 0.297(14) d B 1 .
Cl4B Cl 0.9151(4) 0.7397(5) 0.0343(4) 0.0741(18) Uiso 0.399(14) d B 2 .
Cl5B Cl 1.0492(5) 0.6376(6) 0.0127(4) 0.077(2) Uiso 0.399(14) d B 2 .
Cl6B Cl 0.9920(4) 0.6991(7) -0.1205(3) 0.091(2) Uiso 0.399(14) d B 2 .
Cl4C Cl 0.9488(11) 0.6881(11) 0.0557(7) 0.193(5) Uiso 0.302(5) d B 3 D
Cl5C Cl 0.9532(15) 0.7842(12) -0.0742(11) 0.253(8) Uiso 0.302(5) d B 3 D
Cl6C Cl 1.0816(16) 0.6693(15) -0.0440(13) 0.267(8) Uiso 0.302(5) d B 3 .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.401(5) . ?
C1 C6 1.395(5) . ?
C1 C28 1.510(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.406(6) . ?
C3 C7 1.507(5) . ?
C4 C5 1.395(5) . ?
C4 O4 1.364(5) . ?
C5 C6 1.382(6) . ?
C6 O6 1.380(4) . ?
C7 C8 1.534(6) . ?
C7 C29 1.526(6) . ?
C8 C9 1.381(6) . ?
C8 C13 1.381(6) . ?
C9 C10 1.402(6) . ?
C10 C11 1.387(6) . ?
C10 C14 1.523(6) . ?
C11 C12 1.384(6) . ?
C11 O11 1.393(5) . ?
C12 C13 1.403(6) . ?
C13 O13 1.382(5) . ?
C14 C15 1.513(6) . ?
C14 C30 1.528(7) . ?
C15 C16 1.401(6) . ?
C15 C20 1.388(6) . ?
C16 C17 1.373(5) . ?
C17 C18 1.401(6) . ?
C17 C21 1.519(6) . ?
C18 C19 1.376(6) . ?
C18 O18 1.378(5) . ?
C19 C20 1.402(6) . ?
C20 O20 1.371(5) . ?
C21 C22 1.519(6) . ?
C21 C31 1.516(6) . ?
C22 C23 1.391(6) . ?
C22 C27 1.392(6) . ?
C23 C24 1.390(5) . ?
C24 C25 1.387(5) . ?
C24 C28 1.519(5) . ?
C25 C26 1.383(6) . ?
C25 O25 1.389(5) . ?
C26 C27 1.398(6) . ?
C27 O27 1.387(5) . ?
C28 C32 1.534(6) . ?
C33 O6 1.404(5) . ?
C34 O13 1.431(5) . ?
C35 O20 1.415(6) . ?
C36 O27 1.403(6) . ?
C41 C42 1.507(6) . ?
C41 O4 1.401(5) . ?
C42 C43 1.360(7) . ?
C42 C46 1.376(6) . ?
C43 C44 1.373(7) . ?
C44 N1 1.310(7) . ?
C45 C46 1.381(7) . ?
C45 N1 1.350(7) . ?
C51 C52 1.481(6) . ?
C51 O11 1.411(5) . ?
C52 C53 1.393(6) . ?
C52 C56 1.373(6) . ?
C53 C54 1.361(7) . ?
C54 N2 1.356(7) . ?
C55 C56 1.381(7) . ?
C55 N2 1.336(6) . ?
C61 C62 1.507(6) . ?
C61 O18 1.417(5) . ?
C62 C63 1.372(7) . ?
C62 C66 1.375(8) . ?
C63 C64 1.387(8) . ?
C64 N3 1.310(9) . ?
C65 C66 1.379(8) . ?
C65 N3 1.316(9) . ?
C71 C72 1.512(6) . ?
C71 O25 1.417(5) . ?
C72 C73 1.372(6) . ?
C72 C76 1.371(7) . ?
C73 C74 1.378(8) . ?
C74 N4 1.323(7) . ?
C75 C76 1.385(7) . ?
C75 N4 1.334(6) . ?
C101 Cl1 1.748(6) . ?
C101 Cl2 1.746(6) . ?
C101 Cl3 1.755(5) . ?
Cl7A C301 1.810(12) . ?
Cl7B C301 1.828(12) . ?
Cl8 C301 1.740(13) . ?
Cl9 C301 1.783(12) . ?
C201 Cl4A 1.857(10) . ?
C201 Cl5A 1.780(17) . ?
C201 Cl6A 1.823(12) . ?
C201 Cl4B 1.824(8) . ?
C201 Cl5B 1.741(9) . ?
C201 Cl6B 1.627(9) . ?
C201 Cl4C 1.664(12) . ?
C201 Cl5C 1.925(14) . ?
C201 Cl6C 1.78(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
C2 C1 C28 123.2(4) . . ?
C6 C1 C2 116.8(4) . . ?
C6 C1 C28 120.1(3) . . ?
C3 C2 C1 123.7(4) . . ?
C2 C3 C4 116.9(3) . . ?
C2 C3 C7 124.7(4) . . ?
C4 C3 C7 118.4(3) . . ?
C5 C4 C3 121.5(4) . . ?
O4 C4 C3 114.8(3) . . ?
O4 C4 C5 123.7(4) . . ?
C6 C5 C4 119.1(4) . . ?
C5 C6 C1 122.1(3) . . ?
O6 C6 C1 115.3(3) . . ?
O6 C6 C5 122.6(3) . . ?
C3 C7 C8 111.6(3) . . ?
C3 C7 C29 114.0(3) . . ?
C29 C7 C8 110.6(3) . . ?
C9 C8 C7 121.3(3) . . ?
C13 C8 C7 120.1(4) . . ?
C13 C8 C9 118.6(4) . . ?
C8 C9 C10 122.6(4) . . ?
C9 C10 C14 122.4(4) . . ?
C11 C10 C9 117.1(4) . . ?
C11 C10 C14 120.3(4) . . ?
C10 C11 O11 116.4(4) . . ?
C12 C11 C10 122.0(4) . . ?
C12 C11 O11 121.5(4) . . ?
C11 C12 C13 118.9(4) . . ?
C8 C13 C12 120.8(4) . . ?
C8 C13 O13 116.9(4) . . ?
O13 C13 C12 122.3(4) . . ?
C10 C14 C30 107.9(4) . . ?
C15 C14 C10 112.9(3) . . ?
C15 C14 C30 113.8(4) . . ?
C16 C15 C14 123.1(4) . . ?
C20 C15 C14 120.3(4) . . ?
C20 C15 C16 116.6(4) . . ?
C17 C16 C15 123.8(4) . . ?
C16 C17 C18 117.5(4) . . ?
C16 C17 C21 123.5(4) . . ?
C18 C17 C21 119.0(3) . . ?
C19 C18 C17 121.4(4) . . ?
C19 C18 O18 124.0(4) . . ?
O18 C18 C17 114.6(4) . . ?
C18 C19 C20 119.1(4) . . ?
C15 C20 C19 121.6(4) . . ?
O20 C20 C15 116.2(4) . . ?
O20 C20 C19 122.2(4) . . ?
C22 C21 C17 112.2(3) . . ?
C31 C21 C17 113.0(3) . . ?
C31 C21 C22 110.0(4) . . ?
C23 C22 C21 122.8(4) . . ?
C23 C22 C27 116.9(4) . . ?
C27 C22 C21 120.4(4) . . ?
C24 C23 C22 123.6(4) . . ?
C23 C24 C28 121.8(3) . . ?
C25 C24 C23 117.5(4) . . ?
C25 C24 C28 120.7(3) . . ?
C24 C25 O25 115.8(4) . . ?
C26 C25 C24 121.2(4) . . ?
C26 C25 O25 123.0(4) . . ?
C25 C26 C27 119.5(4) . . ?
C22 C27 C26 121.2(4) . . ?
O27 C27 C22 115.8(4) . . ?
O27 C27 C26 123.0(4) . . ?
C1 C28 C24 113.6(3) . . ?
C1 C28 C32 113.2(3) . . ?
C24 C28 C32 109.8(3) . . ?
O4 C41 C42 108.4(4) . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 C46 117.3(4) . . ?
C46 C42 C41 123.1(4) . . ?
C42 C43 C44 119.0(5) . . ?
N1 C44 C43 125.6(5) . . ?
N1 C45 C46 122.9(5) . . ?
C42 C46 C45 119.8(5) . . ?
O11 C51 C52 110.0(4) . . ?
C53 C52 C51 118.9(4) . . ?
C56 C52 C51 124.3(4) . . ?
C56 C52 C53 116.7(4) . . ?
C54 C53 C52 119.3(4) . . ?
N2 C54 C53 125.0(4) . . ?
N2 C55 C56 124.4(5) . . ?
C52 C56 C55 120.1(4) . . ?
O18 C61 C62 108.5(4) . . ?
C63 C62 C61 120.0(5) . . ?
C63 C62 C66 117.3(5) . . ?
C66 C62 C61 122.8(4) . . ?
C62 C63 C64 119.2(6) . . ?
N3 C64 C63 124.4(5) . . ?
N3 C65 C66 125.5(7) . . ?
C62 C66 C65 118.3(6) . . ?
O25 C71 C72 113.5(3) . . ?
C73 C72 C71 121.0(4) . . ?
C76 C72 C71 121.8(4) . . ?
C76 C72 C73 117.1(4) . . ?
C72 C73 C74 120.2(5) . . ?
N4 C74 C73 123.6(5) . . ?
N4 C75 C76 124.3(5) . . ?
C72 C76 C75 119.0(4) . . ?
Cl1 C101 Cl3 110.9(3) . . ?
Cl2 C101 Cl1 110.5(3) . . ?
Cl2 C101 Cl3 109.4(3) . . ?
C44 N1 C45 115.3(4) . . ?
C55 N2 C54 114.4(4) . . ?
C64 N3 C65 115.4(5) . . ?
C74 N4 C75 115.9(5) . . ?
C4 O4 C41 119.2(3) . . ?
C6 O6 C33 117.6(3) . . ?
C11 O11 C51 118.1(3) . . ?
C13 O13 C34 118.6(4) . . ?
C18 O18 C61 118.7(3) . . ?
C20 O20 C35 117.9(4) . . ?
C25 O25 C71 117.4(3) . . ?
C27 O27 C36 118.4(4) . . ?
Cl7A C301 Cl7B 43.0(4) . . ?
Cl8 C301 Cl7A 134.7(9) . . ?
Cl8 C301 Cl7B 92.9(7) . . ?
Cl8 C301 Cl9 110.1(5) . . ?
Cl9 C301 Cl7A 100.6(6) . . ?
Cl9 C301 Cl7B 115.3(5) . . ?
Cl4A C201 Cl5C 51.3(7) . . ?
Cl5A C201 Cl4A 116.5(8) . . ?
Cl5A C201 Cl6A 123.7(8) . . ?
Cl5A C201 Cl4B 103.2(7) . . ?
Cl5A C201 Cl5C 138.2(9) . . ?
Cl6A C201 Cl4A 89.5(8) . . ?
Cl6A C201 Cl4B 105.5(7) . . ?
Cl6A C201 Cl5C 38.4(7) . . ?
Cl4B C201 Cl4A 16.5(3) . . ?
Cl4B C201 Cl5C 67.6(7) . . ?
Cl5B C201 Cl4A 112.1(6) . . ?
Cl5B C201 Cl5A 10.7(6) . . ?
Cl5B C201 Cl6A 115.3(6) . . ?
Cl5B C201 Cl4B 100.8(5) . . ?
Cl5B C201 Cl5C 127.6(7) . . ?
Cl5B C201 Cl6C 39.0(7) . . ?
Cl6B C201 Cl4A 106.8(8) . . ?
Cl6B C201 Cl5A 113.3(7) . . ?
Cl6B C201 Cl6A 17.3(3) . . ?
Cl6B C201 Cl4B 122.8(7) . . ?
Cl6B C201 Cl5B 107.2(5) . . ?
Cl6B C201 Cl4C 147.6(8) . . ?
Cl6B C201 Cl5C 55.6(7) . . ?
Cl6B C201 Cl6C 68.3(8) . . ?
Cl4C C201 Cl4A 51.8(7) . . ?
Cl4C C201 Cl5A 68.6(8) . . ?
Cl4C C201 Cl6A 133.8(8) . . ?
Cl4C C201 Cl4B 36.0(6) . . ?
Cl4C C201 Cl5B 68.7(6) . . ?
Cl4C C201 Cl5C 100.2(9) . . ?
Cl4C C201 Cl6C 100.4(9) . . ?
Cl6C C201 Cl4A 121.5(8) . . ?
Cl6C C201 Cl5A 46.4(9) . . ?
Cl6C C201 Cl6A 77.2(8) . . ?
Cl6C C201 Cl4B 120.6(8) . . ?
Cl6C C201 Cl5C 101.3(9) . . ?

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
C1 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C3 C7 178.7(4) . . . . ?
C1 C6 O6 C33 177.9(3) . . . . ?
C2 C1 C6 C5 2.4(6) . . . . ?
C2 C1 C6 O6 -178.9(3) . . . . ?
C2 C1 C28 C24 108.3(4) . . . . ?
C2 C1 C28 C32 -17.8(5) . . . . ?
C2 C3 C4 C5 1.6(6) . . . . ?
C2 C3 C4 O4 -177.8(3) . . . . ?
C2 C3 C7 C8 -111.2(4) . . . . ?
C2 C3 C7 C29 15.0(6) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C3 C4 O4 C41 -168.3(4) . . . . ?
C3 C7 C8 C9 29.4(5) . . . . ?
C3 C7 C8 C13 -152.8(4) . . . . ?
C4 C3 C7 C8 68.0(4) . . . . ?
C4 C3 C7 C29 -165.7(4) . . . . ?
C4 C5 C6 C1 -1.5(6) . . . . ?
C4 C5 C6 O6 179.9(4) . . . . ?
C5 C4 O4 C41 12.4(6) . . . . ?
C5 C6 O6 C33 -3.4(6) . . . . ?
C6 C1 C2 C3 -1.3(6) . . . . ?
C6 C1 C28 C24 -73.3(4) . . . . ?
C6 C1 C28 C32 160.6(4) . . . . ?
C7 C3 C4 C5 -177.7(4) . . . . ?
C7 C3 C4 O4 2.9(5) . . . . ?
C7 C8 C9 C10 179.0(4) . . . . ?
C7 C8 C13 C12 -179.4(4) . . . . ?
C7 C8 C13 O13 1.1(6) . . . . ?
C8 C9 C10 C11 -1.0(6) . . . . ?
C8 C9 C10 C14 -176.3(4) . . . . ?
C8 C13 O13 C34 -179.4(4) . . . . ?
C9 C8 C13 C12 -1.5(6) . . . . ?
C9 C8 C13 O13 179.0(4) . . . . ?
C9 C10 C11 C12 1.2(6) . . . . ?
C9 C10 C11 O11 178.7(4) . . . . ?
C9 C10 C14 C15 -30.3(6) . . . . ?
C9 C10 C14 C30 96.4(5) . . . . ?
C10 C11 C12 C13 -1.6(6) . . . . ?
C10 C11 O11 C51 139.8(4) . . . . ?
C10 C14 C15 C16 108.6(5) . . . . ?
C10 C14 C15 C20 -72.3(5) . . . . ?
C11 C10 C14 C15 154.6(4) . . . . ?
C11 C10 C14 C30 -78.7(5) . . . . ?
C11 C12 C13 C8 1.7(6) . . . . ?
C11 C12 C13 O13 -178.8(4) . . . . ?
C12 C11 O11 C51 -42.7(6) . . . . ?
C12 C13 O13 C34 1.1(6) . . . . ?
C13 C8 C9 C10 1.2(6) . . . . ?
C14 C10 C11 C12 176.6(4) . . . . ?
C14 C10 C11 O11 -6.0(6) . . . . ?
C14 C15 C16 C17 179.0(4) . . . . ?
C14 C15 C20 C19 -180.0(4) . . . . ?
C14 C15 C20 O20 -0.4(6) . . . . ?
C15 C16 C17 C18 1.7(6) . . . . ?
C15 C16 C17 C21 -178.0(4) . . . . ?
C15 C20 O20 C35 -170.9(5) . . . . ?
C16 C15 C20 C19 -0.7(6) . . . . ?
C16 C15 C20 O20 178.9(4) . . . . ?
C16 C17 C18 C19 -2.4(6) . . . . ?
C16 C17 C18 O18 179.1(3) . . . . ?
C16 C17 C21 C22 -109.1(4) . . . . ?
C16 C17 C21 C31 16.0(6) . . . . ?
C17 C18 C19 C20 1.5(6) . . . . ?
C17 C18 O18 C61 -175.7(4) . . . . ?
C17 C21 C22 C23 25.5(5) . . . . ?
C17 C21 C22 C27 -154.7(4) . . . . ?
C18 C17 C21 C22 71.2(5) . . . . ?
C18 C17 C21 C31 -163.7(4) . . . . ?
C18 C19 C20 C15 0.1(6) . . . . ?
C18 C19 C20 O20 -179.5(4) . . . . ?
C19 C18 O18 C61 5.8(6) . . . . ?
C19 C20 O20 C35 8.7(7) . . . . ?
C20 C15 C16 C17 -0.2(6) . . . . ?
C21 C17 C18 C19 177.4(4) . . . . ?
C21 C17 C18 O18 -1.2(5) . . . . ?
C21 C22 C23 C24 -178.1(4) . . . . ?
C21 C22 C27 C26 178.1(4) . . . . ?
C21 C22 C27 O27 -0.6(6) . . . . ?
C22 C23 C24 C25 -1.0(6) . . . . ?
C22 C23 C24 C28 -179.0(4) . . . . ?
C22 C27 O27 C36 -173.3(5) . . . . ?
C23 C22 C27 C26 -2.1(6) . . . . ?
C23 C22 C27 O27 179.2(4) . . . . ?
C23 C24 C25 C26 0.0(6) . . . . ?
C23 C24 C25 O25 -179.2(3) . . . . ?
C23 C24 C28 C1 -24.9(5) . . . . ?
C23 C24 C28 C32 103.0(4) . . . . ?
C24 C25 C26 C27 -0.1(6) . . . . ?
C24 C25 O25 C71 -155.6(4) . . . . ?
C25 C24 C28 C1 157.2(4) . . . . ?
C25 C24 C28 C32 -74.9(4) . . . . ?
C25 C26 C27 C22 1.2(6) . . . . ?
C25 C26 C27 O27 179.8(4) . . . . ?
C26 C25 O25 C71 25.3(5) . . . . ?
C26 C27 O27 C36 8.1(7) . . . . ?
C27 C22 C23 C24 2.0(6) . . . . ?
C28 C1 C2 C3 177.1(4) . . . . ?
C28 C1 C6 C5 -176.1(4) . . . . ?
C28 C1 C6 O6 2.6(5) . . . . ?
C28 C24 C25 C26 177.9(4) . . . . ?
C28 C24 C25 O25 -1.2(5) . . . . ?
C29 C7 C8 C9 -98.7(4) . . . . ?
C29 C7 C8 C13 79.1(5) . . . . ?
C30 C14 C15 C16 -15.0(6) . . . . ?
C30 C14 C15 C20 164.2(4) . . . . ?
C31 C21 C22 C23 -101.3(4) . . . . ?
C31 C21 C22 C27 78.6(5) . . . . ?
C41 C42 C43 C44 179.6(5) . . . . ?
C41 C42 C46 C45 178.5(5) . . . . ?
C42 C41 O4 C4 178.7(4) . . . . ?
C42 C43 C44 N1 2.5(10) . . . . ?
C43 C42 C46 C45 0.8(8) . . . . ?
C43 C44 N1 C45 -0.4(9) . . . . ?
C46 C42 C43 C44 -2.6(8) . . . . ?
C46 C45 N1 C44 -1.5(9) . . . . ?
C51 C52 C53 C54 -179.3(5) . . . . ?
C51 C52 C56 C55 178.4(5) . . . . ?
C52 C51 O11 C11 -168.8(4) . . . . ?
C52 C53 C54 N2 0.7(8) . . . . ?
C53 C52 C56 C55 -0.2(7) . . . . ?
C53 C54 N2 C55 0.2(8) . . . . ?
C56 C52 C53 C54 -0.7(7) . . . . ?
C56 C55 N2 C54 -1.2(8) . . . . ?
C61 C62 C63 C64 -179.6(5) . . . . ?
C61 C62 C66 C65 179.8(7) . . . . ?
C62 C61 O18 C18 171.8(3) . . . . ?
C62 C63 C64 N3 -0.1(10) . . . . ?
C63 C62 C66 C65 -0.4(10) . . . . ?
C63 C64 N3 C65 -0.3(11) . . . . ?
C66 C62 C63 C64 0.5(8) . . . . ?
C66 C65 N3 C64 0.5(13) . . . . ?
C71 C72 C73 C74 -175.7(5) . . . . ?
C71 C72 C76 C75 175.9(5) . . . . ?
C72 C71 O25 C25 72.9(5) . . . . ?
C72 C73 C74 N4 -0.6(10) . . . . ?
C73 C72 C76 C75 -0.9(7) . . . . ?
C73 C74 N4 C75 -0.3(10) . . . . ?
C76 C72 C73 C74 1.1(8) . . . . ?
C76 C75 N4 C74 0.5(8) . . . . ?
N1 C45 C46 C42 1.4(9) . . . . ?
N2 C55 C56 C52 1.2(8) . . . . ?
N3 C65 C66 C62 -0.1(14) . . . . ?
N4 C75 C76 C72 0.1(8) . . . . ?
O4 C4 C5 C6 178.7(4) . . . . ?
O4 C41 C42 C43 160.9(5) . . . . ?
O4 C41 C42 C46 -16.8(7) . . . . ?
O11 C11 C12 C13 -178.9(4) . . . . ?
O11 C51 C52 C53 -170.4(4) . . . . ?
O11 C51 C52 C56 11.1(7) . . . . ?
O18 C18 C19 C20 180.0(4) . . . . ?
O18 C61 C62 C63 174.6(4) . . . . ?
O18 C61 C62 C66 -5.6(7) . . . . ?
O25 C25 C26 C27 179.0(4) . . . . ?
O25 C71 C72 C73 -164.6(5) . . . . ?
O25 C71 C72 C76 18.8(6) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-18 11 5 0.0987 -17.9948 11.0002 4.9974 -0.4354 -0.3001 -0.8286
11 2 -20 0.0814 11.0010 2.0230 -19.9963 0.5371 -0.5426 0.6369
13 -16 -10 0.1129 12.9963 -15.9974 -9.9976 -0.0304 0.1347 0.9809
-3 8 -23 0.1045 -2.9941 8.0294 -22.9976 0.0681 -0.9682 0.2248
-4 -18 5 0.0829 -4.0023 -18.0151 4.9985 -0.8857 0.4116 0.3276
18 0 2 0.0886 17.9951 -0.0020 2.0021 0.8990 0.3533 0.3457
-2 -8 -19 0.0884 -1.9973 -7.9835 -18.9983 -0.4958 -0.5453 0.6252
-2 -15 16 0.0738 -2.0043 -15.0255 15.9976 -0.6213 0.7682 0.0319
0 0 -24 0.0755 0.0042 0.0262 -23.9973 -0.1031 -0.8196 0.5478
0 19 1 0.2151 0.0024 19.0090 1.0004 0.7531 -0.2870 -0.5809
-11 5 21 0.0841 -11.0002 4.9796 20.9963 -0.2569 0.4585 -0.8654
8 -1 21 0.0752 7.9942 -1.0234 20.9986 0.4465 0.8607 -0.2760


# start Validation Reply Form
_vrf_FORMU01_2-CHCl3             
;
PROBLEM: There is a discrepancy between the atom counts in the 
_chemical_formula_sum and _chemical_formula_moiety.

RESPONSE: The discrepancy is due to the deuterium atoms of the
chloroforms which is taken into account in chemical formula.
;
# end Validation Reply Form


_ins_header                      
;
TITL 2-CHCl3 in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  13.514237  14.674417  17.347099  95.1994  94.1424 110.3270
ZERR    2.00   0.000550   0.000740   0.000733   0.0038   0.0034   0.0041
LATT  1
SFAC C H N O
UNIT 120.00 120.00 8.00 8.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1-MeOH
_database_code_depnum_ccdc_archive 'CCDC 1044956'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-09-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C60 H60 N4 O8, 3(C H4 O)'
_chemical_formula_sum            'C63 H72 N4 O11'
_chemical_formula_weight         1061.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 N4 O8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   13.4616(2)
_cell_length_b                   14.1115(3)
_cell_length_c                   15.8347(4)
_cell_angle_alpha                109.783(2)
_cell_angle_beta                 93.6810(16)
_cell_angle_gamma                99.7937(16)
_cell_volume                     2765.07(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    120
_cell_measurement_theta_max      73.9600
_cell_measurement_theta_min      4.1790
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.2812
_exptl_crystal_size_mid          0.1329
_exptl_crystal_size_min          0.1064
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19429
_diffrn_reflns_theta_full        74.33
_diffrn_reflns_theta_max         74.33
_diffrn_reflns_theta_min         3.36
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  2 omega   42.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6513 -125.0000 -120.0000 56

#__ type_ start__ end____ width___ exp.time_
  3 omega   34.00  100.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -61.0000 -180.0000 66

#__ type_ start__ end____ width___ exp.time_
  4 omega   53.00   91.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000 -120.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega   87.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   30.0000  -60.0000 91

#__ type_ start__ end____ width___ exp.time_
  6 omega  105.00  145.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   77.0000    0.0000 40

#__ type_ start__ end____ width___ exp.time_
  7 omega   94.00  154.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  125.0000  -60.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega   97.00  161.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   45.0000 -120.0000 64

#__ type_ start__ end____ width___ exp.time_
  9 omega   94.00  122.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601 -125.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 10 omega  104.00  135.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601 -151.0000   -3.0000 31

#__ type_ start__ end____ width___ exp.time_
 11 omega   49.00  103.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  150.0000 54

#__ type_ start__ end____ width___ exp.time_
 12 omega   35.00   62.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601 -125.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 13 omega   25.00  105.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000   60.0000 80

#__ type_ start__ end____ width___ exp.time_
 14 omega   34.00   86.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000   60.0000 52

#__ type_ start__ end____ width___ exp.time_
 15 omega   30.00   86.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
 16 omega   41.00  123.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -77.0000  -90.0000 82

#__ type_ start__ end____ width___ exp.time_
 17 omega  -88.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
 18 omega -116.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -19.0000  150.0000 112

#__ type_ start__ end____ width___ exp.time_
 19 omega -107.00  -69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513 -151.0000   -3.0000 38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0082375000
_diffrn_orient_matrix_UB_12      -0.0037056000
_diffrn_orient_matrix_UB_13      -0.0986022000
_diffrn_orient_matrix_UB_21      0.0134257000
_diffrn_orient_matrix_UB_22      -0.1124741000
_diffrn_orient_matrix_UB_23      -0.0323052000
_diffrn_orient_matrix_UB_31      -0.1160844000
_diffrn_orient_matrix_UB_32      -0.0371782000
_diffrn_orient_matrix_UB_33      -0.0105613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                9560
_reflns_number_total             10886
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         10886
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0880P)²+1.1880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1524
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C100(H10A,H10B,H10C), C200(H20A,H20B,H20C), C300(H30D,H30E,H30F)
2.e Idealised tetrahedral OH refined as rotating group:
 O100(H100), O200(H200), O300(H300)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.28044(11) 0.66258(11) 0.56973(10) 0.0195(3) Uani 1 d . . .
C2 C 0.37053(11) 0.73007(11) 0.61637(10) 0.0191(3) Uani 1 d . . .
H2 H 0.4305 0.7214 0.5915 0.023 Uiso 1 calc . . R
C3 C 0.37506(11) 0.81014(11) 0.69865(10) 0.0184(3) Uani 1 d . . .
C4 C 0.28390(12) 0.82052(11) 0.73476(10) 0.0202(3) Uani 1 d . . .
C5 C 0.19162(12) 0.75560(12) 0.69025(10) 0.0220(3) Uani 1 d . . .
H5 H 0.1317 0.7643 0.7153 0.026 Uiso 1 calc . . R
C6 C 0.19035(11) 0.67723(11) 0.60744(10) 0.0211(3) Uani 1 d . . .
C7 C 0.47262(11) 0.88474(11) 0.75046(10) 0.0191(3) Uani 1 d . . .
H7 H 0.4780 0.8833 0.8120 0.023 Uiso 1 calc . . R
C8 C 0.46964(11) 0.99490(11) 0.75851(10) 0.0186(3) Uani 1 d . . .
C9 C 0.42555(11) 1.01835(11) 0.68825(10) 0.0194(3) Uani 1 d . . .
H9 H 0.3953 0.9646 0.6353 0.023 Uiso 1 calc . . R
C10 C 0.42461(11) 1.11864(11) 0.69341(10) 0.0195(3) Uani 1 d . . .
C11 C 0.47112(12) 1.19813(11) 0.77379(10) 0.0211(3) Uani 1 d . . .
C12 C 0.51458(12) 1.17797(11) 0.84621(10) 0.0219(3) Uani 1 d . . .
H12 H 0.5439 1.2317 0.8995 0.026 Uiso 1 calc . . R
C13 C 0.51380(11) 1.07625(11) 0.83806(10) 0.0198(3) Uani 1 d . . .
C14 C 0.37639(12) 1.14371(11) 0.61591(10) 0.0213(3) Uani 1 d . . .
H14 H 0.3501 1.2064 0.6432 0.026 Uiso 1 calc . . R
C15 C 0.28600(11) 1.05925(11) 0.56215(10) 0.0200(3) Uani 1 d . . .
C16 C 0.28674(11) 0.98815(11) 0.47584(10) 0.0199(3) Uani 1 d . . .
H16 H 0.3450 0.9947 0.4480 0.024 Uiso 1 calc . . R
C17 C 0.20477(11) 0.90771(11) 0.42898(10) 0.0195(3) Uani 1 d . . .
C18 C 0.11892(11) 0.89911(11) 0.47342(10) 0.0208(3) Uani 1 d . . .
C19 C 0.11342(12) 0.96930(12) 0.55865(11) 0.0230(3) Uani 1 d . . .
H19 H 0.0550 0.9629 0.5863 0.028 Uiso 1 calc . . R
C20 C 0.19649(12) 1.04932(11) 0.60212(10) 0.0218(3) Uani 1 d . . .
C21 C 0.20358(11) 0.83255(11) 0.33351(10) 0.0203(3) Uani 1 d . . .
H21 H 0.1398 0.8305 0.2988 0.024 Uiso 1 calc . . R
C22 C 0.20259(11) 0.72277(11) 0.32939(10) 0.0204(3) Uani 1 d . . .
C23 C 0.23857(11) 0.69932(11) 0.40261(10) 0.0199(3) Uani 1 d . . .
H23 H 0.2655 0.7533 0.4564 0.024 Uiso 1 calc . . R
C24 C 0.23648(11) 0.59886(11) 0.39973(10) 0.0199(3) Uani 1 d . . .
C25 C 0.19576(12) 0.51903(11) 0.31780(10) 0.0220(3) Uani 1 d . . .
C26 C 0.16045(12) 0.53900(12) 0.24231(10) 0.0245(3) Uani 1 d . . .
H26 H 0.1346 0.4850 0.1882 0.029 Uiso 1 calc . . R
C27 C 0.16406(12) 0.64027(12) 0.24809(10) 0.0235(3) Uani 1 d . . .
C28 C 0.27675(11) 0.57490(11) 0.48077(10) 0.0205(3) Uani 1 d . . .
H28 H 0.2285 0.5156 0.4829 0.025 Uiso 1 calc . . R
C29 C 0.56924(12) 0.85666(12) 0.71154(11) 0.0238(3) Uani 1 d . . .
H29A H 0.5678 0.8598 0.6519 0.036 Uiso 1 calc . . GR
H29B H 0.5728 0.7882 0.7085 0.036 Uiso 1 calc . . GR
H29C H 0.6277 0.9043 0.7498 0.036 Uiso 1 calc . . GR
C30 C 0.45714(13) 1.16845(13) 0.55832(11) 0.0282(3) Uani 1 d . . .
H30A H 0.4263 1.1867 0.5112 0.042 Uiso 1 calc . . GR
H30B H 0.4861 1.1092 0.5318 0.042 Uiso 1 calc . . GR
H30C H 0.5096 1.2250 0.5958 0.042 Uiso 1 calc . . GR
C31 C 0.28962(12) 0.86707(12) 0.28507(11) 0.0258(3) Uani 1 d . . .
H31A H 0.3537 0.8660 0.3147 0.039 Uiso 1 calc . . GR
H31B H 0.2888 0.9357 0.2870 0.039 Uiso 1 calc . . GR
H31C H 0.2803 0.8213 0.2232 0.039 Uiso 1 calc . . GR
C32 C 0.37922(13) 0.54202(13) 0.46734(11) 0.0269(3) Uani 1 d . . .
H32A H 0.4046 0.5298 0.5200 0.040 Uiso 1 calc . . GR
H32B H 0.4268 0.5955 0.4584 0.040 Uiso 1 calc . . GR
H32C H 0.3704 0.4801 0.4153 0.040 Uiso 1 calc . . GR
C33 C 0.01251(12) 0.61421(13) 0.59998(12) 0.0278(3) Uani 1 d . . .
H33A H 0.0219 0.6008 0.6552 0.042 Uiso 1 calc . . GR
H33B H -0.0423 0.5631 0.5594 0.042 Uiso 1 calc . . GR
H33C H -0.0033 0.6811 0.6131 0.042 Uiso 1 calc . . GR
C34 C 0.57828(16) 1.12566(13) 0.99400(11) 0.0334(4) Uani 1 d . . .
H34A H 0.5974 1.0950 1.0366 0.050 Uiso 1 calc . . GR
H34B H 0.5192 1.1541 1.0100 0.050 Uiso 1 calc . . GR
H34C H 0.6333 1.1793 0.9951 0.050 Uiso 1 calc . . GR
C35 C 0.10402(14) 1.12230(14) 0.72403(12) 0.0311(4) Uani 1 d . . .
H35A H 0.1129 1.1806 0.7793 0.047 Uiso 1 calc . . GR
H35B H 0.0855 1.0602 0.7366 0.047 Uiso 1 calc . . GR
H35C H 0.0512 1.1261 0.6823 0.047 Uiso 1 calc . . GR
C36 C 0.09388(18) 0.58318(15) 0.09229(12) 0.0396(4) Uani 1 d . . .
H36A H 0.0359 0.5373 0.0987 0.059 Uiso 1 calc . . GR
H36B H 0.1472 0.5464 0.0741 0.059 Uiso 1 calc . . GR
H36C H 0.0751 0.6107 0.0472 0.059 Uiso 1 calc . . GR
C41 C 0.20463(14) 0.93822(15) 0.84379(14) 0.0380(4) Uani 1 d . . .
H41A H 0.1597 0.8928 0.8656 0.046 Uiso 1 calc . . R
H41B H 0.1676 0.9461 0.7928 0.046 Uiso 1 calc . . R
C42 C 0.24208(13) 1.04099(13) 0.91779(12) 0.0314(4) Uani 1 d . . .
C43 C 0.24925(16) 1.04882(17) 1.00737(15) 0.0416(4) Uani 1 d . . .
H43 H 0.2298 0.9911 1.0230 0.050 Uiso 1 calc . . R
C44 C 0.28642(17) 1.1457(2) 1.07395(14) 0.0478(5) Uani 1 d . . .
H44 H 0.2944 1.1537 1.1349 0.057 Uiso 1 calc . . R
C45 C 0.31093(15) 1.22873(16) 1.04699(16) 0.0446(5) Uani 1 d . . .
H45 H 0.3327 1.2934 1.0917 0.054 Uiso 1 calc . . R
C46 C 0.27471(14) 1.12862(15) 0.89887(13) 0.0340(4) Uani 1 d . . .
H46 H 0.2753 1.1220 0.8385 0.041 Uiso 1 calc . . R
C51 C 0.52301(18) 1.37973(13) 0.85299(13) 0.0387(4) Uani 1 d . . .
H51A H 0.5946 1.3775 0.8598 0.046 Uiso 1 calc . . R
H51B H 0.4953 1.3768 0.9074 0.046 Uiso 1 calc . . R
C52 C 0.50904(14) 1.47632(12) 0.83727(12) 0.0307(4) Uani 1 d . . .
C53 C 0.54971(15) 1.50325(14) 0.76858(13) 0.0359(4) Uani 1 d . . .
H53 H 0.5905 1.4638 0.7327 0.043 Uiso 1 calc . . R
C54 C 0.52892(17) 1.58969(14) 0.75392(14) 0.0401(4) Uani 1 d . . .
H54 H 0.5538 1.6084 0.7071 0.048 Uiso 1 calc . . R
C55 C 0.47029(16) 1.64719(14) 0.81072(15) 0.0396(4) Uani 1 d . . .
H55 H 0.4570 1.7056 0.8011 0.048 Uiso 1 calc . . R
C56 C 0.45038(15) 1.53866(13) 0.88973(12) 0.0338(4) Uani 1 d . . .
H56 H 0.4224 1.5202 0.9355 0.041 Uiso 1 calc . . R
C61 C -0.04110(12) 0.79508(12) 0.47366(11) 0.0262(3) Uani 1 d . . .
H61A H -0.0791 0.8498 0.4887 0.031 Uiso 1 calc . . R
H61B H -0.0147 0.7886 0.5295 0.031 Uiso 1 calc . . R
C62 C -0.10903(12) 0.69567(12) 0.41393(11) 0.0257(3) Uani 1 d . . .
C63 C -0.21326(13) 0.67976(14) 0.41633(12) 0.0311(4) Uani 1 d . . .
H63 H -0.2420 0.7314 0.4536 0.037 Uiso 1 calc . . R
C64 C -0.27408(14) 0.58616(15) 0.36263(14) 0.0367(4) Uani 1 d . . .
H64 H -0.3439 0.5734 0.3641 0.044 Uiso 1 calc . . R
C65 C -0.22838(15) 0.51198(15) 0.30676(14) 0.0366(4) Uani 1 d . . .
H65 H -0.2693 0.4491 0.2710 0.044 Uiso 1 calc . . R
C66 C -0.07066(13) 0.61641(14) 0.35540(13) 0.0318(4) Uani 1 d . . .
H66 H -0.0009 0.6266 0.3534 0.038 Uiso 1 calc . . R
C71 C 0.14636(14) 0.33849(12) 0.23536(11) 0.0280(3) Uani 1 d . . .
H71A H 0.1869 0.3385 0.1869 0.034 Uiso 1 calc . . R
H71B H 0.0790 0.3471 0.2178 0.034 Uiso 1 calc . . R
C72 C 0.13915(13) 0.23865(13) 0.25167(12) 0.0286(3) Uani 1 d . . .
C73 C 0.18907(14) 0.22920(14) 0.32627(13) 0.0333(4) Uani 1 d . . .
H73 H 0.2285 0.2868 0.3714 0.040 Uiso 1 calc . . R
C74 C 0.17976(15) 0.13281(16) 0.33316(15) 0.0382(4) Uani 1 d . . .
H74 H 0.2121 0.1247 0.3832 0.046 Uiso 1 calc . . R
C75 C 0.12137(15) 0.04901(15) 0.26394(17) 0.0437(5) Uani 1 d . . .
H75 H 0.1162 -0.0156 0.2685 0.052 Uiso 1 calc . . R
C76 C 0.08076(15) 0.14957(15) 0.18594(15) 0.0384(4) Uani 1 d . . .
H76 H 0.0462 0.1560 0.1361 0.046 Uiso 1 calc . . R
C100 C -0.0196(2) -0.20477(19) 0.03537(19) 0.0536(6) Uani 1 d . . .
H10A H -0.0264 -0.2655 -0.0175 0.080 Uiso 1 calc . . GR
H10B H -0.0858 -0.1918 0.0480 0.080 Uiso 1 calc . . GR
H10C H 0.0143 -0.2147 0.0860 0.080 Uiso 1 calc . . GR
C200 C 0.82787(16) 0.31317(16) 0.10102(14) 0.0396(4) Uani 1 d . . .
H20A H 0.8388 0.2543 0.0528 0.059 Uiso 1 calc . . GR
H20B H 0.7912 0.3526 0.0764 0.059 Uiso 1 calc . . GR
H20C H 0.7892 0.2908 0.1421 0.059 Uiso 1 calc . . GR
C300 C 0.2089(3) 0.4049(2) 0.8911(3) 0.0760(9) Uani 1 d . . .
H30D H 0.1426 0.3662 0.8902 0.114 Uiso 1 calc . . GR
H30E H 0.2390 0.3681 0.8397 0.114 Uiso 1 calc . . GR
H30F H 0.2030 0.4707 0.8886 0.114 Uiso 1 calc . . GR
N1 N 0.30556(13) 1.22260(13) 0.96171(13) 0.0412(4) Uani 1 d . . .
N2 N 0.43153(13) 1.62426(12) 0.87838(12) 0.0385(4) Uani 1 d . . .
N3 N -0.12852(12) 0.52620(12) 0.30166(11) 0.0361(3) Uani 1 d . . .
N4 N 0.07167(14) 0.05568(13) 0.19050(14) 0.0460(4) Uani 1 d . . .
O4 O 0.29184(8) 0.89730(8) 0.81762(7) 0.0238(2) Uani 1 d . . .
O6 O 0.10345(8) 0.61065(9) 0.55877(8) 0.0268(2) Uani 1 d . . .
O11 O 0.46991(9) 1.29611(8) 0.77563(7) 0.0264(2) Uani 1 d . . .
O13 O 0.55597(9) 1.04970(8) 0.90586(7) 0.0247(2) Uani 1 d . . .
O18 O 0.04027(8) 0.81837(9) 0.42630(7) 0.0245(2) Uani 1 d . . .
O20 O 0.19692(9) 1.12235(9) 0.68518(8) 0.0268(2) Uani 1 d . . .
O25 O 0.19248(9) 0.42049(8) 0.31686(8) 0.0257(2) Uani 1 d . . .
O27 O 0.12871(10) 0.66549(9) 0.17701(8) 0.0303(3) Uani 1 d . . .
O100 O 0.03823(16) -0.11963(13) 0.02000(13) 0.0601(5) Uani 1 d . . .
H100 H 0.0465 -0.0684 0.0660 0.090 Uiso 1 calc . . GR
O200 O 0.92227(11) 0.37452(13) 0.14755(11) 0.0495(4) Uani 1 d . . .
H200 H 0.9132 0.4186 0.1941 0.074 Uiso 1 calc . . GR
O300 O 0.2715(2) 0.41894(16) 0.97237(16) 0.0808(7) Uani 1 d . . .
H300 H 0.2862 0.3641 0.9697 0.121 Uiso 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
C1 C2 1.392(2) . ?
C1 C6 1.402(2) . ?
C1 C28 1.5192(19) . ?
C2 C3 1.396(2) . ?
C3 C4 1.396(2) . ?
C3 C7 1.5208(19) . ?
C4 C5 1.394(2) . ?
C4 O4 1.3737(18) . ?
C5 C6 1.397(2) . ?
C6 O6 1.3657(18) . ?
C7 C8 1.5238(19) . ?
C7 C29 1.530(2) . ?
C8 C9 1.390(2) . ?
C8 C13 1.397(2) . ?
C9 C10 1.392(2) . ?
C10 C11 1.401(2) . ?
C10 C14 1.5238(19) . ?
C11 C12 1.389(2) . ?
C11 O11 1.3760(18) . ?
C12 C13 1.395(2) . ?
C13 O13 1.3718(18) . ?
C14 C15 1.521(2) . ?
C14 C30 1.533(2) . ?
C15 C16 1.397(2) . ?
C15 C20 1.405(2) . ?
C16 C17 1.398(2) . ?
C17 C18 1.400(2) . ?
C17 C21 1.522(2) . ?
C18 C19 1.393(2) . ?
C18 O18 1.3742(18) . ?
C19 C20 1.395(2) . ?
C20 O20 1.3680(19) . ?
C21 C22 1.526(2) . ?
C21 C31 1.530(2) . ?
C22 C23 1.390(2) . ?
C22 C27 1.406(2) . ?
C23 C24 1.398(2) . ?
C24 C25 1.401(2) . ?
C24 C28 1.524(2) . ?
C25 C26 1.391(2) . ?
C25 O25 1.3787(18) . ?
C26 C27 1.393(2) . ?
C27 O27 1.3711(19) . ?
C28 C32 1.534(2) . ?
C33 O6 1.4242(19) . ?
C34 O13 1.4182(19) . ?
C35 O20 1.429(2) . ?
C36 O27 1.431(2) . ?
C41 C42 1.502(2) . ?
C41 O4 1.419(2) . ?
C42 C43 1.381(3) . ?
C42 C46 1.377(3) . ?
C43 C44 1.398(3) . ?
C44 C45 1.375(4) . ?
C45 N1 1.320(3) . ?
C46 N1 1.337(3) . ?
C51 C52 1.505(2) . ?
C51 O11 1.423(2) . ?
C52 C53 1.383(3) . ?
C52 C56 1.383(3) . ?
C53 C54 1.385(3) . ?
C54 C55 1.380(3) . ?
C55 N2 1.332(3) . ?
C56 N2 1.342(2) . ?
C61 C62 1.501(2) . ?
C61 O18 1.4212(19) . ?
C62 C63 1.388(2) . ?
C62 C66 1.390(3) . ?
C63 C64 1.386(3) . ?
C64 C65 1.385(3) . ?
C65 N3 1.337(3) . ?
C66 N3 1.340(2) . ?
C71 C72 1.505(2) . ?
C71 O25 1.4255(19) . ?
C72 C73 1.378(3) . ?
C72 C76 1.398(3) . ?
C73 C74 1.386(3) . ?
C74 C75 1.383(3) . ?
C75 N4 1.343(3) . ?
C76 N4 1.336(3) . ?
C100 O100 1.419(3) . ?
C200 O200 1.407(2) . ?
C300 O300 1.427(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.87(13) . . ?
C2 C1 C28 122.62(13) . . ?
C6 C1 C28 119.52(13) . . ?
C1 C2 C3 123.15(14) . . ?
C2 C3 C4 117.09(13) . . ?
C2 C3 C7 123.92(13) . . ?
C4 C3 C7 118.99(13) . . ?
C5 C4 C3 121.94(14) . . ?
O4 C4 C3 115.51(13) . . ?
O4 C4 C5 122.54(14) . . ?
C4 C5 C6 119.08(14) . . ?
C5 C6 C1 120.86(14) . . ?
O6 C6 C1 116.04(13) . . ?
O6 C6 C5 123.10(14) . . ?
C3 C7 C8 111.86(11) . . ?
C3 C7 C29 114.20(12) . . ?
C8 C7 C29 109.13(12) . . ?
C9 C8 C7 122.21(13) . . ?
C9 C8 C13 117.97(13) . . ?
C13 C8 C7 119.81(13) . . ?
C8 C9 C10 123.04(13) . . ?
C9 C10 C11 117.23(13) . . ?
C9 C10 C14 122.70(13) . . ?
C11 C10 C14 120.06(13) . . ?
C12 C11 C10 121.56(13) . . ?
O11 C11 C10 115.41(13) . . ?
O11 C11 C12 123.03(13) . . ?
C11 C12 C13 119.25(14) . . ?
C12 C13 C8 120.93(13) . . ?
O13 C13 C8 116.09(13) . . ?
O13 C13 C12 122.98(13) . . ?
C10 C14 C30 110.35(13) . . ?
C15 C14 C10 110.99(11) . . ?
C15 C14 C30 114.03(13) . . ?
C16 C15 C14 124.22(14) . . ?
C16 C15 C20 117.23(13) . . ?
C20 C15 C14 118.52(13) . . ?
C15 C16 C17 123.64(14) . . ?
C16 C17 C18 116.70(14) . . ?
C16 C17 C21 123.88(13) . . ?
C18 C17 C21 119.41(13) . . ?
C19 C18 C17 121.91(14) . . ?
O18 C18 C17 115.37(13) . . ?
O18 C18 C19 122.70(14) . . ?
C18 C19 C20 119.29(14) . . ?
C19 C20 C15 121.15(14) . . ?
O20 C20 C15 115.78(14) . . ?
O20 C20 C19 123.07(14) . . ?
C17 C21 C22 113.28(12) . . ?
C17 C21 C31 113.27(12) . . ?
C22 C21 C31 110.06(12) . . ?
C23 C22 C21 123.20(13) . . ?
C23 C22 C27 117.45(13) . . ?
C27 C22 C21 119.34(13) . . ?
C22 C23 C24 123.51(13) . . ?
C23 C24 C25 117.04(13) . . ?
C23 C24 C28 122.64(13) . . ?
C25 C24 C28 120.32(13) . . ?
C26 C25 C24 121.41(14) . . ?
O25 C25 C24 116.16(13) . . ?
O25 C25 C26 122.43(14) . . ?
C25 C26 C27 119.68(14) . . ?
C26 C27 C22 120.89(14) . . ?
O27 C27 C22 116.28(13) . . ?
O27 C27 C26 122.81(14) . . ?
C1 C28 C24 112.23(12) . . ?
C1 C28 C32 112.87(12) . . ?
C24 C28 C32 110.67(12) . . ?
O4 C41 C42 106.73(14) . . ?
C43 C42 C41 120.24(18) . . ?
C46 C42 C41 121.58(18) . . ?
C46 C42 C43 118.10(17) . . ?
C42 C43 C44 118.3(2) . . ?
C45 C44 C43 118.3(2) . . ?
N1 C45 C44 124.21(19) . . ?
N1 C46 C42 124.24(18) . . ?
O11 C51 C52 106.30(13) . . ?
C53 C52 C51 121.91(17) . . ?
C53 C52 C56 118.06(16) . . ?
C56 C52 C51 119.97(17) . . ?
C52 C53 C54 119.20(18) . . ?
C55 C54 C53 118.11(19) . . ?
N2 C55 C54 124.08(17) . . ?
N2 C56 C52 123.78(18) . . ?
O18 C61 C62 108.28(13) . . ?
C63 C62 C61 120.44(16) . . ?
C63 C62 C66 117.70(16) . . ?
C66 C62 C61 121.86(15) . . ?
C64 C63 C62 119.40(18) . . ?
C65 C64 C63 118.43(17) . . ?
N3 C65 C64 123.34(17) . . ?
N3 C66 C62 123.72(17) . . ?
O25 C71 C72 108.41(13) . . ?
C73 C72 C71 123.93(16) . . ?
C73 C72 C76 117.98(16) . . ?
C76 C72 C71 118.06(16) . . ?
C72 C73 C74 119.20(18) . . ?
C75 C74 C73 118.53(19) . . ?
N4 C75 C74 123.70(18) . . ?
N4 C76 C72 123.9(2) . . ?
C45 N1 C46 116.60(18) . . ?
C55 N2 C56 116.73(17) . . ?
C65 N3 C66 117.37(17) . . ?
C76 N4 C75 116.66(18) . . ?
C4 O4 C41 118.73(13) . . ?
C6 O6 C33 117.74(12) . . ?
C11 O11 C51 117.54(12) . . ?
C13 O13 C34 117.52(12) . . ?
C18 O18 C61 117.70(12) . . ?
C20 O20 C35 117.80(13) . . ?
C25 O25 C71 116.69(12) . . ?
C27 O27 C36 117.25(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O200 H200 N3 0.82 2.05 2.860(2) 172.3 1_655
O300 H300 N1 0.82 2.02 2.836(3) 173.6 1_545

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
C1 C2 C3 C4 0.7(2) . . . . ?
C1 C2 C3 C7 -179.86(13) . . . . ?
C1 C6 O6 C33 172.01(14) . . . . ?
C2 C1 C6 C5 -1.5(2) . . . . ?
C2 C1 C6 O6 178.80(12) . . . . ?
C2 C1 C28 C24 -103.19(16) . . . . ?
C2 C1 C28 C32 22.70(19) . . . . ?
C2 C3 C4 C5 -1.3(2) . . . . ?
C2 C3 C4 O4 177.32(12) . . . . ?
C2 C3 C7 C8 116.80(15) . . . . ?
C2 C3 C7 C29 -7.77(19) . . . . ?
C3 C4 C5 C6 0.6(2) . . . . ?
C3 C4 O4 C41 157.17(15) . . . . ?
C3 C7 C8 C9 -38.36(19) . . . . ?
C3 C7 C8 C13 142.75(14) . . . . ?
C4 C3 C7 C8 -63.76(16) . . . . ?
C4 C3 C7 C29 171.67(12) . . . . ?
C4 C5 C6 C1 0.9(2) . . . . ?
C4 C5 C6 O6 -179.43(13) . . . . ?
C5 C4 O4 C41 -24.2(2) . . . . ?
C5 C6 O6 C33 -7.7(2) . . . . ?
C6 C1 C2 C3 0.7(2) . . . . ?
C6 C1 C28 C24 76.88(16) . . . . ?
C6 C1 C28 C32 -157.23(14) . . . . ?
C7 C3 C4 C5 179.18(13) . . . . ?
C7 C3 C4 O4 -2.16(18) . . . . ?
C7 C8 C9 C10 -178.15(13) . . . . ?
C7 C8 C13 C12 178.22(13) . . . . ?
C7 C8 C13 O13 -1.4(2) . . . . ?
C8 C9 C10 C11 0.2(2) . . . . ?
C8 C9 C10 C14 179.79(14) . . . . ?
C8 C13 O13 C34 -164.57(15) . . . . ?
C9 C8 C13 C12 -0.7(2) . . . . ?
C9 C8 C13 O13 179.67(13) . . . . ?
C9 C10 C11 C12 -1.3(2) . . . . ?
C9 C10 C11 O11 179.04(13) . . . . ?
C9 C10 C14 C15 31.8(2) . . . . ?
C9 C10 C14 C30 -95.62(16) . . . . ?
C10 C11 C12 C13 1.4(2) . . . . ?
C10 C11 O11 C51 -175.26(16) . . . . ?
C10 C14 C15 C16 -106.48(16) . . . . ?
C10 C14 C15 C20 71.55(17) . . . . ?
C11 C10 C14 C15 -148.68(14) . . . . ?
C11 C10 C14 C30 83.92(17) . . . . ?
C11 C12 C13 C8 -0.3(2) . . . . ?
C11 C12 C13 O13 179.28(14) . . . . ?
C12 C11 O11 C51 5.1(2) . . . . ?
C12 C13 O13 C34 15.8(2) . . . . ?
C13 C8 C9 C10 0.8(2) . . . . ?
C14 C10 C11 C12 179.12(14) . . . . ?
C14 C10 C11 O11 -0.5(2) . . . . ?
C14 C15 C16 C17 176.71(13) . . . . ?
C14 C15 C20 C19 -175.77(13) . . . . ?
C14 C15 C20 O20 4.14(19) . . . . ?
C15 C16 C17 C18 -1.0(2) . . . . ?
C15 C16 C17 C21 177.53(13) . . . . ?
C15 C20 O20 C35 173.19(13) . . . . ?
C16 C15 C20 C19 2.4(2) . . . . ?
C16 C15 C20 O20 -177.69(12) . . . . ?
C16 C17 C18 C19 2.4(2) . . . . ?
C16 C17 C18 O18 -178.98(12) . . . . ?
C16 C17 C21 C22 113.11(15) . . . . ?
C16 C17 C21 C31 -13.1(2) . . . . ?
C17 C18 C19 C20 -1.4(2) . . . . ?
C17 C18 O18 C61 169.30(13) . . . . ?
C17 C21 C22 C23 -23.9(2) . . . . ?
C17 C21 C22 C27 156.31(14) . . . . ?
C18 C17 C21 C22 -68.40(17) . . . . ?
C18 C17 C21 C31 165.34(13) . . . . ?
C18 C19 C20 C15 -1.1(2) . . . . ?
C18 C19 C20 O20 179.01(13) . . . . ?
C19 C18 O18 C61 -12.1(2) . . . . ?
C19 C20 O20 C35 -6.9(2) . . . . ?
C20 C15 C16 C17 -1.3(2) . . . . ?
C21 C17 C18 C19 -176.18(13) . . . . ?
C21 C17 C18 O18 2.43(19) . . . . ?
C21 C22 C23 C24 178.99(13) . . . . ?
C21 C22 C27 C26 -178.94(14) . . . . ?
C21 C22 C27 O27 -0.5(2) . . . . ?
C22 C23 C24 C25 0.1(2) . . . . ?
C22 C23 C24 C28 179.75(14) . . . . ?
C22 C27 O27 C36 176.93(16) . . . . ?
C23 C22 C27 C26 1.3(2) . . . . ?
C23 C22 C27 O27 179.77(13) . . . . ?
C23 C24 C25 C26 1.0(2) . . . . ?
C23 C24 C25 O25 -178.73(13) . . . . ?
C23 C24 C28 C1 21.8(2) . . . . ?
C23 C24 C28 C32 -105.28(16) . . . . ?
C24 C25 C26 C27 -0.9(2) . . . . ?
C24 C25 O25 C71 176.82(13) . . . . ?
C25 C24 C28 C1 -158.61(14) . . . . ?
C25 C24 C28 C32 74.31(17) . . . . ?
C25 C26 C27 C22 -0.2(2) . . . . ?
C25 C26 C27 O27 -178.63(15) . . . . ?
C26 C25 O25 C71 -2.9(2) . . . . ?
C26 C27 O27 C36 -4.6(2) . . . . ?
C27 C22 C23 C24 -1.3(2) . . . . ?
C28 C1 C2 C3 -179.23(13) . . . . ?
C28 C1 C6 C5 178.42(13) . . . . ?
C28 C1 C6 O6 -1.3(2) . . . . ?
C28 C24 C25 C26 -178.65(14) . . . . ?
C28 C24 C25 O25 1.7(2) . . . . ?
C29 C7 C8 C9 88.99(16) . . . . ?
C29 C7 C8 C13 -89.90(16) . . . . ?
C30 C14 C15 C16 18.9(2) . . . . ?
C30 C14 C15 C20 -163.08(13) . . . . ?
C31 C21 C22 C23 104.01(16) . . . . ?
C31 C21 C22 C27 -75.75(17) . . . . ?
C41 C42 C43 C44 178.74(18) . . . . ?
C41 C42 C46 N1 177.64(17) . . . . ?
C42 C41 O4 C4 -160.55(14) . . . . ?
C42 C43 C44 C45 2.0(3) . . . . ?
C42 C46 N1 C45 4.8(3) . . . . ?
C43 C42 C46 N1 -5.5(3) . . . . ?
C43 C44 C45 N1 -2.8(3) . . . . ?
C44 C45 N1 C46 -0.5(3) . . . . ?
C46 C42 C43 C44 1.8(3) . . . . ?
C51 C52 C53 C54 175.99(18) . . . . ?
C51 C52 C56 N2 -177.90(17) . . . . ?
C52 C51 O11 C11 -179.88(15) . . . . ?
C52 C53 C54 C55 1.8(3) . . . . ?
C52 C56 N2 C55 1.8(3) . . . . ?
C53 C52 C56 N2 -0.7(3) . . . . ?
C53 C54 C55 N2 -0.7(3) . . . . ?
C54 C55 N2 C56 -1.1(3) . . . . ?
C56 C52 C53 C54 -1.1(3) . . . . ?
C61 C62 C63 C64 -178.00(16) . . . . ?
C61 C62 C66 N3 179.33(17) . . . . ?
C62 C61 O18 C18 -171.35(12) . . . . ?
C62 C63 C64 C65 -1.2(3) . . . . ?
C62 C66 N3 C65 -1.4(3) . . . . ?
C63 C62 C66 N3 0.0(3) . . . . ?
C63 C64 C65 N3 -0.3(3) . . . . ?
C64 C65 N3 C66 1.6(3) . . . . ?
C66 C62 C63 C64 1.4(3) . . . . ?
C71 C72 C73 C74 -177.90(16) . . . . ?
C71 C72 C76 N4 177.12(18) . . . . ?
C72 C71 O25 C25 -173.37(13) . . . . ?
C72 C73 C74 C75 0.8(3) . . . . ?
C72 C76 N4 C75 0.9(3) . . . . ?
C73 C72 C76 N4 -1.0(3) . . . . ?
C73 C74 C75 N4 -0.9(3) . . . . ?
C74 C75 N4 C76 0.1(3) . . . . ?
C76 C72 C73 C74 0.1(3) . . . . ?
O4 C4 C5 C6 -178.00(13) . . . . ?
O4 C41 C42 C43 -92.8(2) . . . . ?
O4 C41 C42 C46 84.0(2) . . . . ?
O11 C11 C12 C13 -179.03(14) . . . . ?
O11 C51 C52 C53 -65.8(2) . . . . ?
O11 C51 C52 C56 111.28(19) . . . . ?
O18 C18 C19 C20 -179.94(13) . . . . ?
O18 C61 C62 C63 -145.90(15) . . . . ?
O18 C61 C62 C66 34.8(2) . . . . ?
O25 C25 C26 C27 178.76(14) . . . . ?
O25 C71 C72 C73 -12.8(2) . . . . ?
O25 C71 C72 C76 169.21(15) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 7 2 0.0415 -4.9434 6.9658 2.1359 -0.1957 -0.9188 0.2923
4 6 1 0.1078 4.0567 5.9649 0.9856 -0.1527 -0.6483 -0.7031
8 -3 -2 0.0978 7.9734 -2.9847 -2.1522 0.1576 0.5123 -0.7919
4 -7 8 0.0643 4.0688 -7.0396 7.9024 -0.7866 0.5911 -0.2941
6 5 -5 0.1352 5.9785 5.0110 -5.0669 0.4318 -0.3197 -0.8268
3 7 -7 0.1146 2.9586 7.0227 -7.0093 0.6407 -0.5237 -0.5305
2 -2 -8 0.0542 1.8903 -1.9352 -8.0646 0.7868 0.5036 -0.0623
-4 6 -8 0.0566 -4.0748 6.0433 -7.9100 0.7911 -0.4789 0.3319
2 -1 9 0.0441 2.1130 -1.0666 8.9816 -0.8991 -0.1418 -0.3005
4 2 -9 0.1173 3.9055 2.0548 -9.0676 0.8543 0.1142 -0.4340
1 -2 -9 0.0575 0.8755 -1.9263 -9.0513 0.8924 0.5208 0.0656
0 -8 0 0.0907 -0.0475 -7.9704 -0.0610 0.0359 0.8978 0.3025
-8 0 2 0.1248 -7.9912 -0.0043 2.1294 -0.1441 -0.1756 0.9053
-5 -4 8 0.1010 -4.9322 -4.0386 8.0657 -0.7397 0.1275 0.6375
3 -3 -8 0.0625 2.8865 -2.9328 -8.0878 0.7846 0.6299 -0.1406
7 -7 2 0.0610 6.9986 -6.9986 1.8419 -0.2133 0.8216 -0.5717
-3 5 6 0.0348 -2.9001 4.9405 6.0985 -0.5957 -0.7916 0.0886
3 -3 -8 0.0628 2.8865 -2.9328 -8.0878 0.7846 0.6299 -0.1406


_ins_header                      
;
TITL 1-MeOH in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  13.461605  14.111470  15.834693 109.7829  93.6810  99.7937
ZERR    2.00   0.000222   0.000324   0.000372   0.0021   0.0016   0.0016
LATT  1
SFAC C H N O
UNIT 120.00 120.00 8.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2-EtOH
_database_code_depnum_ccdc_archive 'CCDC 1044957'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C60 H60 N4 O8, C H Cl3, C2 H6 O'
_chemical_formula_sum            'C63 H67 Cl3 N4 O9'
_chemical_formula_weight         1130.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 N4 O8'
_chemical_oxdiff_usercomment     tte-270314-006
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.1236(4)
_cell_length_b                   32.8276(8)
_cell_length_c                   13.3088(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.373(3)
_cell_angle_gamma                90.00
_cell_volume                     5728.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6527
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.2010
_cell_measurement_theta_min      2.2820
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27084
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         1.99
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0431256000
_diffrn_orient_matrix_UB_12      0.0065990000
_diffrn_orient_matrix_UB_13      0.0259978000
_diffrn_orient_matrix_UB_21      0.0320913000
_diffrn_orient_matrix_UB_22      0.0050270000
_diffrn_orient_matrix_UB_23      0.0423887000
_diffrn_orient_matrix_UB_31      0.0062182000
_diffrn_orient_matrix_UB_32      0.0199519000
_diffrn_orient_matrix_UB_33      -0.0192414000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7140
_reflns_number_total             12119
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         12119
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1184P)²+3.9918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2186
_refine_ls_wR_factor_ref         0.2609
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C201-C20A = C201-C20B
 1.54 with sigma of 0.01
 O202-C201
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C20B) = Uanis(C20A)
4. Others
 Fixed Sof: H20A(0.5) H20B(0.5) H20C(0.5) H20D(0.5) C20A(0.5) H20E(0.5)
 H20F(0.5) H20G(0.5) C20B(0.5) H20H(0.5) H20I(0.5) H20J(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C100(H100)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B), C201(H20A,
 H20B), C201(H20C,H20D)
5.c Me refined with riding coordinates:
 C20A(H20E,H20F,H20G), C20B(H20H,H20I,H20J)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
5.e Tetrahedral OH refined with riding coordinates:
 O202(H202)
5.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.2868(2) 0.48490(10) 0.4642(2) 0.0368(7) Uani 1 1 d . . .
C2 C 0.2105(2) 0.51229(10) 0.4855(2) 0.0384(7) Uani 1 1 d . . .
H2 H 0.1532 0.5024 0.5195 0.046 Uiso 1 1 calc . . R
C3 C 0.2125(2) 0.55334(10) 0.4599(2) 0.0378(7) Uani 1 1 d . . .
C4 C 0.2979(3) 0.56724(10) 0.4102(3) 0.0407(8) Uani 1 1 d . . .
C5 C 0.3767(3) 0.54102(10) 0.3870(2) 0.0404(8) Uani 1 1 d . . .
H5 H 0.4342 0.5509 0.3535 0.048 Uiso 1 1 calc . . R
C6 C 0.3703(3) 0.49995(10) 0.4135(2) 0.0388(7) Uani 1 1 d . . .
C7 C 0.1281(3) 0.58299(10) 0.4833(2) 0.0404(8) Uani 1 1 d . . .
H7 H 0.1615 0.6086 0.5089 0.048 Uiso 1 1 calc . . R
C8 C 0.0637(2) 0.59424(10) 0.3897(2) 0.0382(7) Uani 1 1 d . . .
C9 C 0.0468(2) 0.56699(10) 0.3104(2) 0.0371(7) Uani 1 1 d . . .
H9 H 0.0793 0.5411 0.3144 0.044 Uiso 1 1 calc . . R
C10 C -0.0149(2) 0.57562(10) 0.2260(2) 0.0363(7) Uani 1 1 d . . .
C11 C -0.0630(3) 0.61358(10) 0.2218(2) 0.0400(8) Uani 1 1 d . . .
C12 C -0.0475(3) 0.64191(10) 0.2982(3) 0.0418(8) Uani 1 1 d . . .
H12 H -0.0797 0.6678 0.2941 0.050 Uiso 1 1 calc . . R
C13 C 0.0156(3) 0.63194(10) 0.3809(2) 0.0399(8) Uani 1 1 d . . .
C14 C -0.0353(3) 0.54460(10) 0.1425(2) 0.0388(7) Uani 1 1 d . . .
H14 H -0.0455 0.5602 0.0782 0.047 Uiso 1 1 calc . . R
C15 C 0.0550(3) 0.51559(10) 0.1293(2) 0.0376(7) Uani 1 1 d . . .
C16 C 0.0497(3) 0.47419(10) 0.1466(2) 0.0384(7) Uani 1 1 d . . .
H16 H -0.0127 0.4633 0.1682 0.046 Uiso 1 1 calc . . R
C17 C 0.1313(3) 0.44746(10) 0.1340(2) 0.0386(8) Uani 1 1 d . . .
C18 C 0.2218(3) 0.46450(10) 0.1021(2) 0.0395(8) Uani 1 1 d . . .
C19 C 0.2306(3) 0.50598(10) 0.0845(2) 0.0415(8) Uani 1 1 d . . .
H19 H 0.2933 0.5169 0.0636 0.050 Uiso 1 1 calc . . R
C20 C 0.1482(3) 0.53135(10) 0.0974(2) 0.0385(7) Uani 1 1 d . . .
C21 C 0.1253(3) 0.40208(10) 0.1555(3) 0.0421(8) Uani 1 1 d . . .
H21 H 0.1600 0.3879 0.0998 0.051 Uiso 1 1 calc . . R
C22 C 0.1848(3) 0.39095(10) 0.2533(3) 0.0421(8) Uani 1 1 d . . .
C23 C 0.2068(3) 0.41916(10) 0.3289(2) 0.0406(8) Uani 1 1 d . . .
H23 H 0.1818 0.4461 0.3203 0.049 Uiso 1 1 calc . . R
C24 C 0.2637(3) 0.40994(10) 0.4168(2) 0.0408(8) Uani 1 1 d . . .
C25 C 0.2968(3) 0.36989(11) 0.4289(3) 0.0469(9) Uani 1 1 d . . .
C26 C 0.2759(3) 0.34077(11) 0.3551(3) 0.0536(10) Uani 1 1 d . . .
H26 H 0.2998 0.3137 0.3642 0.064 Uiso 1 1 calc . . R
C27 C 0.2202(3) 0.35125(10) 0.2684(3) 0.0481(9) Uani 1 1 d . . .
C28 C 0.2866(3) 0.44080(10) 0.4996(2) 0.0384(7) Uani 1 1 d . . .
H28 H 0.3569 0.4348 0.5275 0.046 Uiso 1 1 calc . . R
C29 C 0.0590(3) 0.56779(12) 0.5654(3) 0.0482(9) Uani 1 1 d . . .
H29A H 0.0100 0.5892 0.5813 0.072 Uiso 1 1 calc . . GR
H29B H 0.1006 0.5610 0.6259 0.072 Uiso 1 1 calc . . GR
H29C H 0.0221 0.5435 0.5415 0.072 Uiso 1 1 calc . . GR
C30 C -0.1345(3) 0.52234(11) 0.1605(3) 0.0461(8) Uani 1 1 d . . .
H30A H -0.1283 0.5076 0.2245 0.069 Uiso 1 1 calc . . GR
H30B H -0.1489 0.5030 0.1057 0.069 Uiso 1 1 calc . . GR
H30C H -0.1904 0.5421 0.1630 0.069 Uiso 1 1 calc . . GR
C31 C 0.0158(3) 0.38586(11) 0.1544(3) 0.0515(9) Uani 1 1 d . . .
H31A H -0.0207 0.3984 0.2092 0.077 Uiso 1 1 calc . . GR
H31B H 0.0170 0.3562 0.1632 0.077 Uiso 1 1 calc . . GR
H31C H -0.0190 0.3926 0.0899 0.077 Uiso 1 1 calc . . GR
C32 C 0.2138(3) 0.43376(11) 0.5853(3) 0.0478(9) Uani 1 1 d . . .
H32A H 0.2308 0.4526 0.6406 0.072 Uiso 1 1 calc . . GR
H32B H 0.2207 0.4057 0.6095 0.072 Uiso 1 1 calc . . GR
H32C H 0.1434 0.4385 0.5606 0.072 Uiso 1 1 calc . . GR
C33 C 0.3879(3) 0.62487(12) 0.3491(4) 0.0618(11) Uani 1 1 d . . .
H33A H 0.3990 0.6128 0.2831 0.093 Uiso 1 1 calc . . GR
H33B H 0.4465 0.6189 0.3947 0.093 Uiso 1 1 calc . . GR
H33C H 0.3801 0.6544 0.3421 0.093 Uiso 1 1 calc . . GR
C34 C -0.1583(5) 0.66113(13) 0.1197(4) 0.0847(17) Uani 1 1 d . . .
H34A H -0.1967 0.6624 0.0551 0.127 Uiso 1 1 calc . . GR
H34B H -0.0991 0.6793 0.1180 0.127 Uiso 1 1 calc . . GR
H34C H -0.2022 0.6696 0.1736 0.127 Uiso 1 1 calc . . GR
C35 C 0.3893(3) 0.44277(14) 0.1500(3) 0.0628(11) Uani 1 1 d . . .
H35A H 0.4369 0.4204 0.1388 0.094 Uiso 1 1 calc . . GR
H35B H 0.3682 0.4421 0.2197 0.094 Uiso 1 1 calc . . GR
H35C H 0.4228 0.4688 0.1370 0.094 Uiso 1 1 calc . . GR
C36 C 0.3670(5) 0.32103(14) 0.5439(4) 0.0908(19) Uani 1 1 d . . .
H36A H 0.4089 0.3075 0.4946 0.136 Uiso 1 1 calc . . GR
H36B H 0.3009 0.3072 0.5462 0.136 Uiso 1 1 calc . . GR
H36C H 0.4017 0.3198 0.6104 0.136 Uiso 1 1 calc . . GR
C41 C 0.5309(3) 0.48536(10) 0.3421(2) 0.0404(8) Uani 1 1 d . . .
H41A H 0.5721 0.5043 0.3851 0.048 Uiso 1 1 calc . . R
H41B H 0.5083 0.5000 0.2801 0.048 Uiso 1 1 calc . . R
C42 C 0.5941(3) 0.44901(10) 0.3156(3) 0.0415(8) Uani 1 1 d . . .
C43 C 0.5786(3) 0.41078(12) 0.3533(3) 0.0562(10) Uani 1 1 d . . .
H43 H 0.5257 0.4059 0.3984 0.067 Uiso 1 1 calc . . R
C44 C 0.6417(4) 0.37924(14) 0.3245(4) 0.0748(13) Uani 1 1 d . . .
H44 H 0.6304 0.3529 0.3517 0.090 Uiso 1 1 calc . . R
C45 C 0.7301(3) 0.42088(14) 0.2259(4) 0.0635(11) Uani 1 1 d . . .
H45 H 0.7836 0.4251 0.1811 0.076 Uiso 1 1 calc . . R
C46 C 0.6718(3) 0.45407(12) 0.2497(3) 0.0502(9) Uani 1 1 d . . .
H46 H 0.6848 0.4800 0.2213 0.060 Uiso 1 1 calc . . R
C51 C -0.0422(3) 0.67896(16) 0.5033(4) 0.0749(14) Uani 1 1 d . . .
H51A H -0.0899 0.6583 0.5280 0.090 Uiso 1 1 calc . . R
H51B H -0.0801 0.6972 0.4556 0.090 Uiso 1 1 calc . . R
C52 C 0.0046(4) 0.70334(14) 0.5906(3) 0.0671(12) Uani 1 1 d . . .
C53 C 0.0732(4) 0.68507(14) 0.6571(3) 0.0656(12) Uani 1 1 d . . .
H53 H 0.0877 0.6569 0.6501 0.079 Uiso 1 1 calc . . R
C54 C 0.1206(5) 0.70650(17) 0.7327(4) 0.0877(17) Uani 1 1 d . . .
H54 H 0.1666 0.6925 0.7777 0.105 Uiso 1 1 calc . . R
C55 C 0.0376(8) 0.76350(18) 0.6885(6) 0.141(3) Uani 1 1 d . . .
H55 H 0.0213 0.7911 0.7017 0.170 Uiso 1 1 calc . . R
C56 C -0.0138(7) 0.74319(18) 0.6056(5) 0.128(3) Uani 1 1 d . . .
H56 H -0.0601 0.7576 0.5619 0.153 Uiso 1 1 calc . . R
C61 C 0.2439(3) 0.59230(11) 0.0741(3) 0.0560(10) Uani 1 1 d . . .
H61A H 0.2771 0.5858 0.0106 0.067 Uiso 1 1 calc . . R
H61B H 0.2896 0.5835 0.1312 0.067 Uiso 1 1 calc . . R
C62 C 0.2232(3) 0.63713(11) 0.0805(3) 0.0508(9) Uani 1 1 d . . .
C63 C 0.2419(4) 0.66335(13) 0.0029(4) 0.0703(12) Uani 1 1 d . . .
H63 H 0.2698 0.6536 -0.0574 0.084 Uiso 1 1 calc . . R
C64 C 0.2192(5) 0.70426(15) 0.0144(4) 0.0866(16) Uani 1 1 d . . .
H64 H 0.2333 0.7221 -0.0395 0.104 Uiso 1 1 calc . . R
C65 C 0.1612(4) 0.69473(14) 0.1682(4) 0.0717(13) Uani 1 1 d . . .
H65 H 0.1318 0.7054 0.2267 0.086 Uiso 1 1 calc . . R
C66 C 0.1819(3) 0.65357(13) 0.1657(4) 0.0631(11) Uani 1 1 d . . .
H66 H 0.1681 0.6367 0.2215 0.076 Uiso 1 1 calc . . R
C71 C 0.2319(5) 0.28343(12) 0.2036(4) 0.0783(15) Uani 1 1 d . . .
H71A H 0.2046 0.2715 0.2653 0.094 Uiso 1 1 calc . . R
H71B H 0.3073 0.2826 0.2095 0.094 Uiso 1 1 calc . . R
C72 C 0.1944(4) 0.25977(12) 0.1134(3) 0.0598(11) Uani 1 1 d . . .
C73 C 0.0993(4) 0.26599(13) 0.0705(4) 0.0684(12) Uani 1 1 d . . .
H73 H 0.0558 0.2860 0.0973 0.082 Uiso 1 1 calc . . R
C74 C 0.0665(4) 0.24329(14) -0.0110(4) 0.0796(14) Uani 1 1 d . . .
H74 H 0.0009 0.2488 -0.0409 0.096 Uiso 1 1 calc . . R
C75 C 0.2136(5) 0.20671(18) -0.0038(5) 0.0961(19) Uani 1 1 d . . .
H75 H 0.2529 0.1845 -0.0268 0.115 Uiso 1 1 calc . . R
C76 C 0.2528(4) 0.22936(15) 0.0743(4) 0.0820(15) Uani 1 1 d . . .
H76 H 0.3197 0.2242 0.1013 0.098 Uiso 1 1 calc . . R
N1 N 0.7172(3) 0.38350(12) 0.2609(3) 0.0756(11) Uani 1 1 d . . .
N2 N 0.1061(6) 0.74524(16) 0.7463(4) 0.120(2) Uani 1 1 d . . .
N3 N 0.1795(3) 0.72017(11) 0.0946(4) 0.0765(11) Uani 1 1 d . . .
N4 N 0.1226(4) 0.21387(15) -0.0503(4) 0.0989(16) Uani 1 1 d . . .
O4 O 0.29855(19) 0.60819(7) 0.3886(2) 0.0499(6) Uani 1 1 d . . .
O6 O 0.44446(17) 0.47202(7) 0.39420(18) 0.0430(6) Uani 1 1 d . . .
O11 O -0.1249(2) 0.62089(7) 0.13737(18) 0.0494(6) Uani 1 1 d . . .
O13 O 0.03833(18) 0.66022(7) 0.45620(19) 0.0492(6) Uani 1 1 d . . .
O18 O 0.30203(18) 0.43845(7) 0.08364(18) 0.0468(6) Uani 1 1 d . . .
O20 O 0.14882(19) 0.57232(7) 0.07753(19) 0.0469(6) Uani 1 1 d . . .
O25 O 0.3520(2) 0.36127(8) 0.5163(2) 0.0603(8) Uani 1 1 d . . .
O27 O 0.1980(2) 0.32422(7) 0.1916(2) 0.0597(8) Uani 1 1 d . . .
C100 C 0.5954(4) 0.59305(19) 0.1050(4) 0.0894(17) Uani 1 1 d . . .
H100 H 0.6601 0.5898 0.0687 0.107 Uiso 1 1 calc . . R
Cl1 Cl 0.52565(14) 0.54708(6) 0.09571(13) 0.1183(6) Uani 1 1 d . . .
Cl2 Cl 0.62553(12) 0.60381(8) 0.23043(12) 0.1415(9) Uani 1 1 d . . .
Cl3 Cl 0.52428(18) 0.63187(6) 0.04829(15) 0.1368(8) Uani 1 1 d . . .
C201 C 0.3934(11) 0.7359(4) 0.7837(8) 0.205(6) Uani 1 1 d . . D
H20A H 0.3966 0.7471 0.7149 0.246 Uiso 0.50 1 calc A 1 R
H20B H 0.3522 0.7107 0.7757 0.246 Uiso 0.50 1 calc A 1 R
H20C H 0.4429 0.7534 0.7499 0.246 Uiso 0.50 1 calc A 2 R
H20D H 0.3533 0.7218 0.7295 0.246 Uiso 0.50 1 calc A 2 R
C20A C 0.4990(11) 0.7192(9) 0.802(2) 0.230(11) Uani 0.50 1 d B 1 D
H20E H 0.5127 0.6987 0.7507 0.345 Uiso 0.50 1 calc B 1 R
H20F H 0.5045 0.7067 0.8687 0.345 Uiso 0.50 1 calc B 1 R
H20G H 0.5486 0.7414 0.7981 0.345 Uiso 0.50 1 calc B 1 R
C20B C 0.4566(13) 0.7030(7) 0.837(2) 0.230(11) Uani 0.50 1 d B 2 D
H20H H 0.4494 0.6774 0.7991 0.345 Uiso 0.50 1 calc B 2 R
H20I H 0.4327 0.6991 0.9049 0.345 Uiso 0.50 1 calc B 2 R
H20J H 0.5284 0.7112 0.8405 0.345 Uiso 0.50 1 calc B 2 R
O202 O 0.3218(5) 0.76389(17) 0.8306(4) 0.148(2) Uani 1 1 d B . D
H202 H 0.2637 0.7613 0.8026 0.222 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
C1 C2 1.384(5) . ?
C1 C6 1.400(5) . ?
C1 C28 1.523(5) . ?
C2 C3 1.390(5) . ?
C3 C4 1.401(5) . ?
C3 C7 1.517(5) . ?
C4 C5 1.390(5) . ?
C4 O4 1.374(4) . ?
C5 C6 1.397(5) . ?
C6 O6 1.369(4) . ?
C7 C8 1.522(4) . ?
C7 C29 1.532(5) . ?
C8 C9 1.395(4) . ?
C8 C13 1.392(5) . ?
C9 C10 1.386(4) . ?
C10 C11 1.397(5) . ?
C10 C14 1.524(4) . ?
C11 C12 1.387(5) . ?
C11 O11 1.380(4) . ?
C12 C13 1.389(5) . ?
C13 O13 1.389(4) . ?
C14 C15 1.536(5) . ?
C14 C30 1.521(5) . ?
C15 C16 1.380(5) . ?
C15 C20 1.409(5) . ?
C16 C17 1.400(5) . ?
C17 C18 1.394(5) . ?
C17 C21 1.520(5) . ?
C18 C19 1.387(5) . ?
C18 O18 1.387(4) . ?
C19 C20 1.382(5) . ?
C20 O20 1.371(4) . ?
C21 C22 1.533(5) . ?
C21 C31 1.533(5) . ?
C22 C23 1.389(5) . ?
C22 C27 1.396(5) . ?
C23 C24 1.396(4) . ?
C24 C25 1.392(5) . ?
C24 C28 1.517(5) . ?
C25 C26 1.390(5) . ?
C25 O25 1.375(4) . ?
C26 C27 1.383(5) . ?
C27 O27 1.376(4) . ?
C28 C32 1.535(5) . ?
C33 O4 1.415(5) . ?
C34 O11 1.408(5) . ?
C35 O18 1.423(4) . ?
C36 O25 1.383(5) . ?
C41 C42 1.504(5) . ?
C41 O6 1.423(4) . ?
C42 C43 1.370(5) . ?
C42 C46 1.382(5) . ?
C43 C44 1.389(6) . ?
C44 N1 1.337(6) . ?
C45 C46 1.375(5) . ?
C45 N1 1.326(6) . ?
C51 C52 1.520(6) . ?
C51 O13 1.394(5) . ?
C52 C53 1.374(6) . ?
C52 C56 1.347(7) . ?
C53 C54 1.357(6) . ?
C54 N2 1.300(7) . ?
C55 C56 1.434(9) . ?
C55 N2 1.305(9) . ?
C61 C62 1.500(5) . ?
C61 O20 1.412(5) . ?
C62 C63 1.374(6) . ?
C62 C66 1.387(6) . ?
C63 C64 1.386(6) . ?
C64 N3 1.314(7) . ?
C65 C66 1.379(6) . ?
C65 N3 1.317(6) . ?
C71 C72 1.496(6) . ?
C71 O27 1.418(5) . ?
C72 C73 1.366(6) . ?
C72 C76 1.374(6) . ?
C73 C74 1.371(7) . ?
C74 N4 1.334(6) . ?
C75 C76 1.361(7) . ?
C75 N4 1.342(7) . ?
C100 Cl1 1.767(7) . ?
C100 Cl2 1.736(5) . ?
C100 Cl3 1.734(5) . ?
C201 C20A 1.499(10) . ?
C201 C20B 1.518(10) . ?
C201 O202 1.472(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
C2 C1 C6 117.2(3) . . ?
C2 C1 C28 122.9(3) . . ?
C6 C1 C28 119.8(3) . . ?
C1 C2 C3 123.9(3) . . ?
C2 C3 C4 117.1(3) . . ?
C2 C3 C7 123.4(3) . . ?
C4 C3 C7 119.6(3) . . ?
C5 C4 C3 121.3(3) . . ?
O4 C4 C3 115.4(3) . . ?
O4 C4 C5 123.2(3) . . ?
C4 C5 C6 119.3(3) . . ?
C5 C6 C1 121.2(3) . . ?
O6 C6 C1 115.5(3) . . ?
O6 C6 C5 123.3(3) . . ?
C3 C7 C8 111.9(3) . . ?
C3 C7 C29 113.4(3) . . ?
C8 C7 C29 109.7(3) . . ?
C9 C8 C7 122.0(3) . . ?
C13 C8 C7 121.3(3) . . ?
C13 C8 C9 116.7(3) . . ?
C10 C9 C8 123.5(3) . . ?
C9 C10 C11 117.6(3) . . ?
C9 C10 C14 122.3(3) . . ?
C11 C10 C14 120.1(3) . . ?
C12 C11 C10 121.1(3) . . ?
O11 C11 C10 116.0(3) . . ?
O11 C11 C12 122.9(3) . . ?
C11 C12 C13 119.2(3) . . ?
C12 C13 C8 122.0(3) . . ?
C12 C13 O13 121.2(3) . . ?
O13 C13 C8 116.8(3) . . ?
C10 C14 C15 112.6(3) . . ?
C30 C14 C10 109.4(3) . . ?
C30 C14 C15 112.9(3) . . ?
C16 C15 C14 123.2(3) . . ?
C16 C15 C20 117.5(3) . . ?
C20 C15 C14 119.3(3) . . ?
C15 C16 C17 123.6(3) . . ?
C16 C17 C21 123.1(3) . . ?
C18 C17 C16 116.7(3) . . ?
C18 C17 C21 120.1(3) . . ?
C19 C18 C17 121.6(3) . . ?
O18 C18 C17 118.0(3) . . ?
O18 C18 C19 120.4(3) . . ?
C20 C19 C18 119.9(3) . . ?
C19 C20 C15 120.7(3) . . ?
O20 C20 C15 115.5(3) . . ?
O20 C20 C19 123.8(3) . . ?
C17 C21 C22 111.4(3) . . ?
C17 C21 C31 113.2(3) . . ?
C22 C21 C31 111.7(3) . . ?
C23 C22 C21 122.6(3) . . ?
C23 C22 C27 117.3(3) . . ?
C27 C22 C21 120.0(3) . . ?
C22 C23 C24 123.5(3) . . ?
C23 C24 C28 123.2(3) . . ?
C25 C24 C23 117.1(3) . . ?
C25 C24 C28 119.7(3) . . ?
C26 C25 C24 121.1(3) . . ?
O25 C25 C24 116.3(3) . . ?
O25 C25 C26 122.6(3) . . ?
C27 C26 C25 120.0(3) . . ?
C26 C27 C22 121.0(3) . . ?
O27 C27 C22 115.8(3) . . ?
O27 C27 C26 123.2(3) . . ?
C1 C28 C32 112.5(3) . . ?
C24 C28 C1 114.4(3) . . ?
C24 C28 C32 109.2(3) . . ?
O6 C41 C42 109.2(3) . . ?
C43 C42 C41 123.3(3) . . ?
C43 C42 C46 117.9(3) . . ?
C46 C42 C41 118.8(3) . . ?
C42 C43 C44 118.8(4) . . ?
N1 C44 C43 124.2(4) . . ?
N1 C45 C46 124.9(4) . . ?
C45 C46 C42 118.8(4) . . ?
O13 C51 C52 106.6(3) . . ?
C53 C52 C51 119.7(4) . . ?
C56 C52 C51 123.7(5) . . ?
C56 C52 C53 116.5(5) . . ?
C54 C53 C52 121.3(5) . . ?
N2 C54 C53 123.0(5) . . ?
N2 C55 C56 122.1(6) . . ?
C52 C56 C55 118.9(6) . . ?
O20 C61 C62 106.9(3) . . ?
C63 C62 C61 122.3(4) . . ?
C63 C62 C66 117.3(4) . . ?
C66 C62 C61 120.4(4) . . ?
C62 C63 C64 118.5(5) . . ?
N3 C64 C63 124.7(5) . . ?
N3 C65 C66 124.1(5) . . ?
C65 C66 C62 119.0(4) . . ?
O27 C71 C72 108.0(3) . . ?
C73 C72 C71 121.4(4) . . ?
C73 C72 C76 117.7(4) . . ?
C76 C72 C71 120.7(4) . . ?
C72 C73 C74 120.0(4) . . ?
N4 C74 C73 122.9(5) . . ?
N4 C75 C76 123.9(5) . . ?
C75 C76 C72 119.1(5) . . ?
C45 N1 C44 115.3(4) . . ?
C54 N2 C55 117.9(5) . . ?
C64 N3 C65 116.3(4) . . ?
C74 N4 C75 116.2(4) . . ?
C4 O4 C33 117.9(3) . . ?
C6 O6 C41 118.2(3) . . ?
C11 O11 C34 117.9(3) . . ?
C13 O13 C51 118.4(3) . . ?
C18 O18 C35 115.2(3) . . ?
C20 O20 C61 118.3(3) . . ?
C25 O25 C36 119.0(3) . . ?
C27 O27 C71 118.0(3) . . ?
Cl2 C100 Cl1 109.7(3) . . ?
Cl3 C100 Cl1 109.2(3) . . ?
Cl3 C100 Cl2 111.5(3) . . ?
C20A C201 C20B 35.2(12) . . ?
O202 C201 C20A 139.6(16) . . ?
O202 C201 C20B 126.4(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O202 H202 N2 0.84 2.23 3.064(9) 170.0 .

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
C1 C2 C3 C4 -0.3(5) . . . . ?
C1 C2 C3 C7 179.8(3) . . . . ?
C1 C6 O6 C41 179.5(3) . . . . ?
C2 C1 C6 C5 0.9(4) . . . . ?
C2 C1 C6 O6 179.7(3) . . . . ?
C2 C1 C28 C24 107.9(4) . . . . ?
C2 C1 C28 C32 -17.4(4) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C2 C3 C4 O4 -178.3(3) . . . . ?
C2 C3 C7 C8 -106.0(4) . . . . ?
C2 C3 C7 C29 18.7(4) . . . . ?
C3 C4 C5 C6 0.3(5) . . . . ?
C3 C4 O4 C33 172.8(3) . . . . ?
C3 C7 C8 C9 31.6(5) . . . . ?
C3 C7 C8 C13 -150.8(3) . . . . ?
C4 C3 C7 C8 74.0(4) . . . . ?
C4 C3 C7 C29 -161.2(3) . . . . ?
C4 C5 C6 C1 -0.9(5) . . . . ?
C4 C5 C6 O6 -179.6(3) . . . . ?
C5 C4 O4 C33 -5.8(5) . . . . ?
C5 C6 O6 C41 -1.8(4) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
C6 C1 C28 C24 -76.5(4) . . . . ?
C6 C1 C28 C32 158.2(3) . . . . ?
C7 C3 C4 C5 -179.7(3) . . . . ?
C7 C3 C4 O4 1.7(4) . . . . ?
C7 C8 C9 C10 177.2(3) . . . . ?
C7 C8 C13 C12 -176.8(3) . . . . ?
C7 C8 C13 O13 6.9(5) . . . . ?
C8 C9 C10 C11 -0.7(5) . . . . ?
C8 C9 C10 C14 -177.5(3) . . . . ?
C8 C13 O13 C51 -128.6(4) . . . . ?
C9 C8 C13 C12 1.0(5) . . . . ?
C9 C8 C13 O13 -175.3(3) . . . . ?
C9 C10 C11 C12 1.5(5) . . . . ?
C9 C10 C11 O11 -179.1(3) . . . . ?
C9 C10 C14 C15 -31.3(5) . . . . ?
C9 C10 C14 C30 95.1(4) . . . . ?
C10 C11 C12 C13 -1.1(5) . . . . ?
C10 C11 O11 C34 -167.4(4) . . . . ?
C10 C14 C15 C16 115.6(3) . . . . ?
C10 C14 C15 C20 -64.8(4) . . . . ?
C11 C10 C14 C15 152.0(3) . . . . ?
C11 C10 C14 C30 -81.6(4) . . . . ?
C11 C12 C13 C8 -0.2(5) . . . . ?
C11 C12 C13 O13 176.0(3) . . . . ?
C12 C11 O11 C34 12.0(6) . . . . ?
C12 C13 O13 C51 55.0(5) . . . . ?
C13 C8 C9 C10 -0.6(5) . . . . ?
C14 C10 C11 C12 178.4(3) . . . . ?
C14 C10 C11 O11 -2.2(5) . . . . ?
C14 C15 C16 C17 179.4(3) . . . . ?
C14 C15 C20 C19 -179.7(3) . . . . ?
C14 C15 C20 O20 -1.9(4) . . . . ?
C15 C16 C17 C18 -0.1(4) . . . . ?
C15 C16 C17 C21 178.6(3) . . . . ?
C15 C20 O20 C61 161.8(3) . . . . ?
C16 C15 C20 C19 -0.2(4) . . . . ?
C16 C15 C20 O20 177.7(3) . . . . ?
C16 C17 C18 C19 0.5(4) . . . . ?
C16 C17 C18 O18 -176.5(3) . . . . ?
C16 C17 C21 C22 -105.8(3) . . . . ?
C16 C17 C21 C31 21.1(4) . . . . ?
C17 C18 C19 C20 -0.8(5) . . . . ?
C17 C18 O18 C35 -113.9(4) . . . . ?
C17 C21 C22 C23 22.4(5) . . . . ?
C17 C21 C22 C27 -156.7(3) . . . . ?
C18 C17 C21 C22 72.8(4) . . . . ?
C18 C17 C21 C31 -160.3(3) . . . . ?
C18 C19 C20 C15 0.6(5) . . . . ?
C18 C19 C20 O20 -177.0(3) . . . . ?
C19 C18 O18 C35 69.0(4) . . . . ?
C19 C20 O20 C61 -20.4(5) . . . . ?
C20 C15 C16 C17 -0.1(4) . . . . ?
C21 C17 C18 C19 -178.2(3) . . . . ?
C21 C17 C18 O18 4.8(4) . . . . ?
C21 C22 C23 C24 -177.7(3) . . . . ?
C21 C22 C27 C26 178.5(4) . . . . ?
C21 C22 C27 O27 -0.1(5) . . . . ?
C22 C23 C24 C25 -1.9(6) . . . . ?
C22 C23 C24 C28 -179.3(3) . . . . ?
C22 C27 O27 C71 -179.7(4) . . . . ?
C23 C22 C27 C26 -0.6(6) . . . . ?
C23 C22 C27 O27 -179.3(3) . . . . ?
C23 C24 C25 C26 1.5(6) . . . . ?
C23 C24 C25 O25 -179.4(3) . . . . ?
C23 C24 C28 C1 -26.3(5) . . . . ?
C23 C24 C28 C32 100.8(4) . . . . ?
C24 C25 C26 C27 -0.8(6) . . . . ?
C24 C25 O25 C36 165.3(4) . . . . ?
C25 C24 C28 C1 156.3(3) . . . . ?
C25 C24 C28 C32 -76.6(4) . . . . ?
C25 C26 C27 C22 0.4(6) . . . . ?
C25 C26 C27 O27 178.9(4) . . . . ?
C26 C25 O25 C36 -15.7(6) . . . . ?
C26 C27 O27 C71 1.8(6) . . . . ?
C27 C22 C23 C24 1.4(6) . . . . ?
C28 C1 C2 C3 175.4(3) . . . . ?
C28 C1 C6 C5 -174.9(3) . . . . ?
C28 C1 C6 O6 3.9(4) . . . . ?
C28 C24 C25 C26 179.1(4) . . . . ?
C28 C24 C25 O25 -1.9(5) . . . . ?
C29 C7 C8 C9 -95.2(4) . . . . ?
C29 C7 C8 C13 82.5(4) . . . . ?
C30 C14 C15 C16 -8.8(4) . . . . ?
C30 C14 C15 C20 170.7(3) . . . . ?
C31 C21 C22 C23 -105.3(4) . . . . ?
C31 C21 C22 C27 75.5(4) . . . . ?
C41 C42 C43 C44 -179.7(4) . . . . ?
C41 C42 C46 C45 179.6(3) . . . . ?
C42 C41 O6 C6 -171.7(3) . . . . ?
C42 C43 C44 N1 -0.5(7) . . . . ?
C43 C42 C46 C45 -0.6(5) . . . . ?
C43 C44 N1 C45 0.5(7) . . . . ?
C46 C42 C43 C44 0.5(6) . . . . ?
C46 C45 N1 C44 -0.6(7) . . . . ?
C51 C52 C53 C54 176.4(5) . . . . ?
C51 C52 C56 C55 -177.7(7) . . . . ?
C52 C51 O13 C13 172.2(4) . . . . ?
C52 C53 C54 N2 -1.1(9) . . . . ?
C53 C52 C56 C55 -0.5(10) . . . . ?
C53 C54 N2 C55 4.7(11) . . . . ?
C56 C52 C53 C54 -1.0(8) . . . . ?
C56 C55 N2 C54 -6.1(13) . . . . ?
C61 C62 C63 C64 179.1(4) . . . . ?
C61 C62 C66 C65 -178.3(4) . . . . ?
C62 C61 O20 C20 -164.4(3) . . . . ?
C62 C63 C64 N3 -0.8(9) . . . . ?
C63 C62 C66 C65 0.5(6) . . . . ?
C63 C64 N3 C65 0.2(8) . . . . ?
C66 C62 C63 C64 0.4(7) . . . . ?
C66 C65 N3 C64 0.7(8) . . . . ?
C71 C72 C73 C74 -178.8(5) . . . . ?
C71 C72 C76 C75 175.8(6) . . . . ?
C72 C71 O27 C27 177.2(4) . . . . ?
C72 C73 C74 N4 2.1(8) . . . . ?
C73 C72 C76 C75 -0.7(8) . . . . ?
C73 C74 N4 C75 1.5(9) . . . . ?
C76 C72 C73 C74 -2.4(7) . . . . ?
C76 C75 N4 C74 -4.8(10) . . . . ?
N1 C45 C46 C42 0.7(7) . . . . ?
N2 C55 C56 C52 4.1(14) . . . . ?
N3 C65 C66 C62 -1.1(7) . . . . ?
N4 C75 C76 C72 4.5(10) . . . . ?
O4 C4 C5 C6 178.8(3) . . . . ?
O6 C41 C42 C43 -11.0(4) . . . . ?
O6 C41 C42 C46 168.8(3) . . . . ?
O11 C11 C12 C13 179.6(3) . . . . ?
O13 C51 C52 C53 -50.1(7) . . . . ?
O13 C51 C52 C56 127.1(6) . . . . ?
O18 C18 C19 C20 176.2(3) . . . . ?
O20 C61 C62 C63 -115.3(4) . . . . ?
O20 C61 C62 C66 63.4(5) . . . . ?
O25 C25 C26 C27 -179.8(4) . . . . ?
O27 C71 C72 C73 -39.5(7) . . . . ?
O27 C71 C72 C76 144.2(5) . . . . ?


# start Validation Reply Form
_vrf_PLAT241_2-EtOH              
;
PROBLEM:High Ueq as Compared to Neighbors for .....

RESPONSE: There was not enough electron density to build a chemically
reasonable disorder for the pyridine rings and thus the Ueq values are
larger compared to neighboring atoms.
;
# end Validation Reply Form

_ins_header                      
;
TITL 2-EtOH in P2/n 
REM P2/n (#13 in standard setting)
CELL 0.71073  13.123622  32.827605  13.308841  90.0000  92.3728  90.0000
ZERR    4.00   0.000387   0.000803   0.000371   0.0000   0.0026   0.0000
LATT  1
SYMM -x+1/2, y,-z+1/2 
SFAC C H N O
UNIT 240.00 240.00 16.00 32.00
TREF
HKLF 4
END
;
####################################################################### 
# 
# 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_1-B
_database_code_depnum_ccdc_archive 'CCDC 1044958'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C60 H60 N4 O8, 1.5(C6 F4 I2), C H Cl3'
_chemical_formula_sum            'C70 H60 Cl3 D F6 I3 N4 O8'
_chemical_formula_weight         1688.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 O4 N4'
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'
D D 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   13.0454(3)
_cell_length_b                   13.7948(5)
_cell_length_c                   20.6219(7)
_cell_angle_alpha                88.043(3)
_cell_angle_beta                 82.996(2)
_cell_angle_gamma                84.693(2)
_cell_volume                     3666.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11508
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.2070
_cell_measurement_theta_min      2.4520
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 
CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric 
absorption correction using a multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta
Cryst. A51, 887-897) Empirical absorption correction using spherical
harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.1496
_exptl_crystal_size_mid          0.1269
_exptl_crystal_size_min          0.0279
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30106
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         1.96
_diffrn_ambient_temperature      170.15(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000   90.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega   53.00   81.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408 -126.0000   17.0000 28

#__ type_ start__ end____ width___ exp.time_
  3 omega   21.00   64.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega   46.00  100.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408 -178.0000  120.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   34.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  150.0000 31

#__ type_ start__ end____ width___ exp.time_
  6 omega  -34.00   38.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000  -60.0000 72

#__ type_ start__ end____ width___ exp.time_
  7 omega  -17.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   19.0000  -90.0000 113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0154223000
_diffrn_orient_matrix_UB_12      -0.0407473000
_diffrn_orient_matrix_UB_13      0.0194468000
_diffrn_orient_matrix_UB_21      -0.0012833000
_diffrn_orient_matrix_UB_22      0.0273975000
_diffrn_orient_matrix_UB_23      0.0286199000
_diffrn_orient_matrix_UB_31      -0.0527768000
_diffrn_orient_matrix_UB_32      0.0160340000
_diffrn_orient_matrix_UB_33      -0.0020670000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                12295
_reflns_number_total             15519
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.31 
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.31 
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.31
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         15519
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0397
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0354P)²+2.1253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0935
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C300(D300)
2.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
C1 C 0.5187(2) 0.7118(2) 0.47905(15) 0.0199(6) Uani 1 d . . .
C2 C 0.4645(2) 0.7908(2) 0.51148(15) 0.0215(6) Uani 1 d . . .
H2 H 0.4489 0.8469 0.4870 0.026 Uiso 1 calc . . R
C3 C 0.4320(2) 0.7912(2) 0.57809(15) 0.0210(6) Uani 1 d . . .
C4 C 0.4542(2) 0.7055(2) 0.61381(15) 0.0229(7) Uani 1 d . . .
C5 C 0.5110(2) 0.6251(2) 0.58346(16) 0.0235(7) Uani 1 d . . .
H5 H 0.5264 0.5688 0.6078 0.028 Uiso 1 calc . . R
C6 C 0.5442(2) 0.6291(2) 0.51729(15) 0.0209(6) Uani 1 d . . .
C7 C 0.3776(2) 0.8799(2) 0.61366(16) 0.0236(7) Uani 1 d . . .
H7 H 0.3208 0.8572 0.6442 0.028 Uiso 1 calc . . R
C8 C 0.4499(2) 0.9254(2) 0.65392(15) 0.0210(6) Uani 1 d . . .
C9 C 0.5573(2) 0.9204(2) 0.63666(16) 0.0225(7) Uani 1 d . . .
H9 H 0.5857 0.8863 0.5996 0.027 Uiso 1 calc . . R
C10 C 0.6236(2) 0.9642(2) 0.67235(15) 0.0212(6) Uani 1 d . . .
C11 C 0.5799(2) 1.0163(2) 0.72710(16) 0.0232(7) Uani 1 d . . .
C12 C 0.4732(2) 1.0227(2) 0.74589(16) 0.0241(7) Uani 1 d . . .
H12 H 0.4449 1.0563 0.7831 0.029 Uiso 1 calc . . R
C13 C 0.4096(2) 0.9788(2) 0.70889(16) 0.0225(7) Uani 1 d . . .
C14 C 0.7413(2) 0.9581(2) 0.65297(16) 0.0234(7) Uani 1 d . . .
H14 H 0.7730 0.9590 0.6936 0.028 Uiso 1 calc . . R
C15 C 0.7821(2) 0.8627(2) 0.62021(15) 0.0203(6) Uani 1 d . . .
C16 C 0.8242(2) 0.8547(2) 0.55500(15) 0.0219(6) Uani 1 d . . .
H16 H 0.8261 0.9113 0.5292 0.026 Uiso 1 calc . . R
C17 C 0.8637(2) 0.7671(2) 0.52598(15) 0.0198(6) Uani 1 d . . .
C18 C 0.8586(2) 0.6826(2) 0.56556(16) 0.0233(7) Uani 1 d . . .
C19 C 0.8172(2) 0.6873(2) 0.63060(16) 0.0267(7) Uani 1 d . . .
H19 H 0.8143 0.6306 0.6562 0.032 Uiso 1 calc . . R
C20 C 0.7801(2) 0.7759(2) 0.65751(15) 0.0240(7) Uani 1 d . . .
C21 C 0.9124(2) 0.7607(2) 0.45528(15) 0.0217(6) Uani 1 d . . .
H21 H 0.9733 0.7132 0.4541 0.026 Uiso 1 calc . . R
C22 C 0.8402(2) 0.7243(2) 0.41057(15) 0.0219(6) Uani 1 d . . .
C23 C 0.7330(2) 0.7320(2) 0.42636(15) 0.0197(6) Uani 1 d . . .
H23 H 0.7054 0.7583 0.4663 0.024 Uiso 1 calc . . R
C24 C 0.6650(2) 0.7025(2) 0.38553(15) 0.0203(6) Uani 1 d . . .
C25 C 0.7069(2) 0.6661(2) 0.32492(15) 0.0232(7) Uani 1 d . . .
C26 C 0.8137(2) 0.6565(2) 0.30692(16) 0.0261(7) Uani 1 d . . .
H26 H 0.8411 0.6314 0.2666 0.031 Uiso 1 calc . . R
C27 C 0.8785(2) 0.6848(2) 0.34999(16) 0.0232(7) Uani 1 d . . .
C28 C 0.5485(2) 0.7107(2) 0.40583(15) 0.0201(6) Uani 1 d . . .
H28 H 0.5220 0.6529 0.3899 0.024 Uiso 1 calc . . R
C29 C 0.3297(3) 0.9574(3) 0.56863(18) 0.0361(8) Uani 1 d . . .
H29A H 0.3837 0.9837 0.5393 0.054 Uiso 1 calc . . GR
H29B H 0.2922 1.0087 0.5945 0.054 Uiso 1 calc . . GR
H29C H 0.2832 0.9285 0.5439 0.054 Uiso 1 calc . . GR
C30 C 0.7718(2) 1.0483(2) 0.61273(17) 0.0304(8) Uani 1 d . . .
H30A H 0.8452 1.0422 0.5995 0.046 Uiso 1 calc . . GR
H30B H 0.7536 1.1052 0.6387 0.046 Uiso 1 calc . . GR
H30C H 0.7358 1.0543 0.5747 0.046 Uiso 1 calc . . GR
C31 C 0.9502(2) 0.8579(2) 0.42784(17) 0.0297(7) Uani 1 d . . .
H31A H 0.8916 0.9044 0.4242 0.045 Uiso 1 calc . . GR
H31B H 0.9886 0.8481 0.3855 0.045 Uiso 1 calc . . GR
H31C H 0.9940 0.8819 0.4567 0.045 Uiso 1 calc . . GR
C32 C 0.4986(2) 0.7996(2) 0.37051(17) 0.0300(7) Uani 1 d . . .
H32A H 0.4251 0.8055 0.3833 0.045 Uiso 1 calc . . GR
H32B H 0.5123 0.7914 0.3241 0.045 Uiso 1 calc . . GR
H32C H 0.5274 0.8573 0.3821 0.045 Uiso 1 calc . . GR
C33 C 0.4164(3) 0.6141(3) 0.71286(19) 0.0436(9) Uani 1 d . . .
H33A H 0.3823 0.5700 0.6896 0.065 Uiso 1 calc . . GR
H33B H 0.3802 0.6226 0.7560 0.065 Uiso 1 calc . . GR
H33C H 0.4865 0.5879 0.7160 0.065 Uiso 1 calc . . GR
C34 C 0.6074(3) 1.1088(3) 0.8186(2) 0.0498(11) Uani 1 d . . .
H34A H 0.5608 1.1637 0.8084 0.075 Uiso 1 calc . . GR
H34B H 0.6636 1.1310 0.8384 0.075 Uiso 1 calc . . GR
H34C H 0.5709 1.0652 0.8483 0.075 Uiso 1 calc . . GR
C35 C 0.9172(3) 0.5138(3) 0.57687(19) 0.0382(9) Uani 1 d . . .
H35A H 0.9606 0.5295 0.6087 0.057 Uiso 1 calc . . GR
H35B H 0.9513 0.4610 0.5510 0.057 Uiso 1 calc . . GR
H35C H 0.8526 0.4949 0.5987 0.057 Uiso 1 calc . . GR
C36 C 0.6746(3) 0.6153(4) 0.22013(18) 0.0501(11) Uani 1 d . . .
H36A H 0.7116 0.6674 0.1996 0.075 Uiso 1 calc . . GR
H36B H 0.6176 0.6053 0.1965 0.075 Uiso 1 calc . . GR
H36C H 0.7205 0.5568 0.2201 0.075 Uiso 1 calc . . GR
C41 C 0.6556(2) 0.4831(2) 0.52370(16) 0.0280(7) Uani 1 d . . .
H41A H 0.6065 0.4448 0.5500 0.034 Uiso 1 calc . . R
H41B H 0.6924 0.5166 0.5530 0.034 Uiso 1 calc . . R
C42 C 0.7316(2) 0.4167(2) 0.48068(17) 0.0277(7) Uani 1 d . . .
C43 C 0.7623(3) 0.3241(3) 0.5041(2) 0.0368(8) Uani 1 d . . .
H43 H 0.7347 0.3020 0.5451 0.044 Uiso 1 calc . . R
C44 C 0.8346(3) 0.2658(3) 0.4652(2) 0.0457(10) Uani 1 d . . .
H44 H 0.8565 0.2035 0.4796 0.055 Uiso 1 calc . . R
C45 C 0.8737(3) 0.3005(3) 0.4052(2) 0.0535(11) Uani 1 d . . .
H45 H 0.9226 0.2604 0.3796 0.064 Uiso 1 calc . . R
C46 C 0.7760(3) 0.4448(3) 0.42012(19) 0.0419(9) Uani 1 d . . .
H46 H 0.7564 0.5072 0.4049 0.050 Uiso 1 calc . . R
C51 C 0.2531(2) 1.0659(3) 0.75617(19) 0.0335(8) Uani 1 d . . .
H51A H 0.2738 1.1237 0.7317 0.040 Uiso 1 calc . . R
H51B H 0.2727 1.0690 0.7999 0.040 Uiso 1 calc . . R
C52 C 0.1379(2) 1.0624(3) 0.75959(17) 0.0294(7) Uani 1 d . . .
C53 C 0.0923(2) 0.9934(3) 0.72728(18) 0.0357(8) Uani 1 d . . .
H53 H 0.1333 0.9464 0.7021 0.043 Uiso 1 calc . . R
C54 C -0.0148(3) 0.9957(3) 0.7332(2) 0.0417(9) Uani 1 d . . .
H54 H -0.0466 0.9500 0.7123 0.050 Uiso 1 calc . . R
C55 C -0.0731(3) 1.0658(3) 0.7699(2) 0.0419(10) Uani 1 d . . .
H55 H -0.1450 1.0668 0.7733 0.050 Uiso 1 calc . . R
C56 C 0.0721(2) 1.1291(3) 0.79599(19) 0.0383(9) Uani 1 d . . .
H56 H 0.1017 1.1745 0.8185 0.046 Uiso 1 calc . . R
C61 C 0.6536(3) 0.7423(3) 0.74764(18) 0.0361(8) Uani 1 d . . .
H61A H 0.6681 0.6730 0.7556 0.043 Uiso 1 calc . . R
H61B H 0.6044 0.7515 0.7159 0.043 Uiso 1 calc . . R
C62 C 0.6095(3) 0.7911(3) 0.81008(17) 0.0330(8) Uani 1 d . . .
C63 C 0.6726(3) 0.8214(4) 0.8538(2) 0.0563(12) Uani 1 d . . .
H63 H 0.7444 0.8130 0.8447 0.068 Uiso 1 calc . . R
C64 C 0.6271(4) 0.8638(4) 0.9105(2) 0.0724(16) Uani 1 d . . .
H64 H 0.6677 0.8842 0.9407 0.087 Uiso 1 calc . . R
C65 C 0.5203(4) 0.8758(4) 0.9224(2) 0.0609(13) Uani 1 d . . .
H65 H 0.4904 0.9040 0.9614 0.073 Uiso 1 calc . . R
C66 C 0.5034(3) 0.8084(3) 0.82697(19) 0.0365(9) Uani 1 d . . .
H66 H 0.4605 0.7898 0.7977 0.044 Uiso 1 calc . . R
C71 C 1.0298(2) 0.6268(3) 0.27788(16) 0.0283(7) Uani 1 d . . .
H71A H 1.0066 0.6617 0.2399 0.034 Uiso 1 calc . . R
H71B H 1.0088 0.5611 0.2784 0.034 Uiso 1 calc . . R
C72 C 1.1454(2) 0.6242(3) 0.27508(16) 0.0284(7) Uani 1 d . . .
C73 C 1.1917(3) 0.6971(3) 0.3011(2) 0.0448(10) Uani 1 d . . .
H73 H 1.1519 0.7486 0.3224 0.054 Uiso 1 calc . . R
C74 C 1.2986(3) 0.6922(4) 0.2950(2) 0.0599(14) Uani 1 d . . .
H74 H 1.3317 0.7403 0.3125 0.072 Uiso 1 calc . . R
C75 C 1.3557(3) 0.6159(3) 0.2630(2) 0.0487(11) Uani 1 d . . .
H75 H 1.4276 0.6126 0.2601 0.058 Uiso 1 calc . . R
C76 C 1.2086(2) 0.5514(3) 0.24226(18) 0.0348(8) Uani 1 d . . .
H76 H 1.1775 0.5029 0.2236 0.042 Uiso 1 calc . . R
C101 C 0.4375(2) 0.5957(3) 0.94283(16) 0.0295(7) Uani 1 d . . .
C102 C 0.3340(3) 0.5876(4) 0.9405(2) 0.0547(13) Uani 1 d . . .
C103 C 0.2583(3) 0.6297(4) 0.9866(2) 0.0539(12) Uani 1 d . . .
C104 C 0.2844(3) 0.6839(3) 1.03577(18) 0.0330(8) Uani 1 d . . .
C105 C 0.3879(3) 0.6921(3) 1.03761(19) 0.0382(9) Uani 1 d . . .
C106 C 0.4630(3) 0.6490(3) 0.99220(19) 0.0361(8) Uani 1 d . . .
C201 C 0.0992(3) 0.9662(3) 0.9710(2) 0.0442(10) Uani 1 d . . .
C202 C 0.0131(3) 0.9575(3) 0.9406(2) 0.0475(10) Uani 1 d . . .
C203 C 0.0846(3) 1.0095(3) 1.0307(2) 0.0482(10) Uani 1 d . . .
C300 C 1.0833(4) 0.6512(4) 0.7724(3) 0.0760(16) Uani 1 d . . .
D300 H 1.1126 0.6245 0.7300 0.091 Uiso 1 calc . . R
N1 N 0.8452(3) 0.3892(3) 0.38155(19) 0.0590(10) Uani 1 d . . .
N2 N -0.0319(2) 1.1335(3) 0.80132(17) 0.0443(8) Uani 1 d . . .
N3 N 0.4586(2) 0.8493(2) 0.88163(17) 0.0456(8) Uani 1 d . . .
N4 N 1.3120(2) 0.5468(3) 0.23590(18) 0.0466(9) Uani 1 d . . .
O4 O 0.41686(17) 0.70561(17) 0.67893(11) 0.0311(5) Uani 1 d . . .
O6 O 0.60174(15) 0.55213(15) 0.48471(11) 0.0243(5) Uani 1 d . . .
O11 O 0.64732(16) 1.05926(18) 0.76016(12) 0.0329(6) Uani 1 d . . .
O13 O 0.30312(15) 0.98251(17) 0.72547(12) 0.0307(5) Uani 1 d . . .
O18 O 0.89807(18) 0.59696(16) 0.53548(12) 0.0326(5) Uani 1 d . . .
O20 O 0.74710(16) 0.78462(18) 0.72338(11) 0.0321(5) Uani 1 d . . .
O25 O 0.63674(16) 0.63962(18) 0.28505(11) 0.0307(5) Uani 1 d . . .
O27 O 0.98561(15) 0.67487(17) 0.33611(11) 0.0299(5) Uani 1 d . . .
F102 F 0.3043(2) 0.5370(3) 0.89285(17) 0.1227(17) Uani 1 d . . .
F103 F 0.15950(18) 0.6198(3) 0.98154(17) 0.1291(18) Uani 1 d . . .
F105 F 0.41848(18) 0.7418(2) 1.08522(15) 0.0832(11) Uani 1 d . . .
F106 F 0.56241(17) 0.6583(2) 0.99800(14) 0.0744(9) Uani 1 d . . .
F202 F 0.02123(19) 0.9148(2) 0.88209(12) 0.0636(7) Uani 1 d . . .
F203 F 0.16625(18) 1.0204(2) 1.06357(13) 0.0633(7) Uani 1 d . . .
Cl1 Cl 1.07418(12) 0.55395(12) 0.83027(7) 0.0880(5) Uani 1 d . . .
Cl2 Cl 1.16197(12) 0.73655(14) 0.79296(12) 0.1204(7) Uani 1 d . . .
Cl3 Cl 0.95705(9) 0.70622(12) 0.76502(7) 0.0787(4) Uani 1 d . . .
I104 I 0.170832(17) 0.752787(18) 1.104522(12) 0.03681(7) Uani 1 d . . .
I201 I 0.24821(2) 0.91426(2) 0.927803(14) 0.04942(8) Uani 1 d . . .
I101 I 0.550074(16) 0.535670(17) 0.870774(11) 0.03229(7) Uani 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 C2 1.388(4) . ?
C1 C6 1.402(4) . ?
C1 C28 1.513(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.397(4) . ?
C3 C7 1.521(4) . ?
C4 C5 1.398(4) . ?
C4 O4 1.372(4) . ?
C5 C6 1.381(4) . ?
C6 O6 1.386(4) . ?
C7 C8 1.520(4) . ?
C7 C29 1.532(5) . ?
C8 C9 1.399(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.391(4) . ?
C10 C11 1.392(4) . ?
C10 C14 1.534(4) . ?
C11 C12 1.394(4) . ?
C11 O11 1.364(4) . ?
C12 C13 1.384(4) . ?
C13 O13 1.386(3) . ?
C14 C15 1.522(4) . ?
C14 C30 1.529(5) . ?
C15 C16 1.393(4) . ?
C15 C20 1.401(4) . ?
C16 C17 1.394(4) . ?
C17 C18 1.401(4) . ?
C17 C21 1.520(4) . ?
C18 C19 1.385(4) . ?
C18 O18 1.381(4) . ?
C19 C20 1.381(4) . ?
C20 O20 1.380(4) . ?
C21 C22 1.523(4) . ?
C21 C31 1.537(4) . ?
C22 C23 1.391(4) . ?
C22 C27 1.397(4) . ?
C23 C24 1.391(4) . ?
C24 C25 1.392(4) . ?
C24 C28 1.521(4) . ?
C25 C26 1.392(4) . ?
C25 O25 1.383(4) . ?
C26 C27 1.388(4) . ?
C27 O27 1.386(3) . ?
C28 C32 1.538(4) . ?
C33 O4 1.422(4) . ?
C34 O11 1.424(4) . ?
C35 O18 1.428(4) . ?
C36 O25 1.410(4) . ?
C41 C42 1.510(4) . ?
C41 O6 1.417(4) . ?
C42 C43 1.392(5) . ?
C42 C46 1.370(5) . ?
C43 C44 1.378(5) . ?
C44 C45 1.367(6) . ?
C45 N1 1.340(6) . ?
C46 N1 1.332(5) . ?
C51 C52 1.502(4) . ?
C51 O13 1.400(4) . ?
C52 C53 1.396(5) . ?
C52 C56 1.375(5) . ?
C53 C54 1.385(5) . ?
C54 C55 1.365(5) . ?
C55 N2 1.342(5) . ?
C56 N2 1.343(4) . ?
C61 C62 1.500(5) . ?
C61 O20 1.428(4) . ?
C62 C63 1.391(6) . ?
C62 C66 1.385(5) . ?
C63 C64 1.369(6) . ?
C64 C65 1.381(6) . ?
C65 N3 1.315(6) . ?
C66 N3 1.324(5) . ?
C71 C72 1.499(4) . ?
C71 O27 1.424(4) . ?
C72 C73 1.376(5) . ?
C72 C76 1.380(5) . ?
C73 C74 1.381(5) . ?
C74 C75 1.371(6) . ?
C75 N4 1.327(5) . ?
C76 N4 1.335(4) . ?
C101 C102 1.372(5) . ?
C101 C106 1.366(5) . ?
C101 I101 2.092(3) . ?
C102 C103 1.386(5) . ?
C102 F102 1.339(5) . ?
C103 C104 1.373(5) . ?
C103 F103 1.326(4) . ?
C104 C105 1.370(5) . ?
C104 I104 2.104(3) . ?
C105 C106 1.377(5) . ?
C105 F105 1.336(4) . ?
C106 F106 1.335(4) . ?
C201 C202 1.368(6) . ?
C201 C203 1.369(6) . ?
C201 I201 2.110(4) . ?
C202 C203 1.382(5) 2_577 ?
C202 F202 1.349(5) . ?
C203 C202 1.382(5) 2_577 ?
C203 F203 1.354(5) . ?
C300 Cl1 1.767(6) . ?
C300 Cl2 1.728(6) . ?
C300 Cl3 1.770(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
C2 C1 C6 116.9(3) . . ?
C2 C1 C28 123.4(3) . . ?
C6 C1 C28 119.7(3) . . ?
C3 C2 C1 124.1(3) . . ?
C2 C3 C4 117.1(3) . . ?
C2 C3 C7 123.6(3) . . ?
C4 C3 C7 119.2(3) . . ?
C3 C4 C5 120.7(3) . . ?
O4 C4 C3 116.3(3) . . ?
O4 C4 C5 123.0(3) . . ?
C6 C5 C4 120.0(3) . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 O6 122.6(3) . . ?
O6 C6 C1 116.3(3) . . ?
C3 C7 C29 113.9(3) . . ?
C8 C7 C3 111.2(2) . . ?
C8 C7 C29 109.8(3) . . ?
C9 C8 C7 122.7(3) . . ?
C13 C8 C7 120.1(2) . . ?
C13 C8 C9 117.1(3) . . ?
C10 C9 C8 123.0(3) . . ?
C9 C10 C11 117.9(3) . . ?
C9 C10 C14 122.5(3) . . ?
C11 C10 C14 119.5(3) . . ?
C10 C11 C12 120.7(3) . . ?
O11 C11 C10 116.1(3) . . ?
O11 C11 C12 123.2(3) . . ?
C13 C12 C11 119.7(3) . . ?
C12 C13 C8 121.6(3) . . ?
C12 C13 O13 122.2(3) . . ?
O13 C13 C8 116.2(3) . . ?
C15 C14 C10 112.0(2) . . ?
C15 C14 C30 113.6(3) . . ?
C30 C14 C10 110.6(3) . . ?
C16 C15 C14 124.6(3) . . ?
C16 C15 C20 116.4(3) . . ?
C20 C15 C14 118.9(3) . . ?
C15 C16 C17 124.1(3) . . ?
C16 C17 C18 116.9(3) . . ?
C16 C17 C21 123.0(3) . . ?
C18 C17 C21 120.1(3) . . ?
C19 C18 C17 120.9(3) . . ?
O18 C18 C17 115.6(3) . . ?
O18 C18 C19 123.5(3) . . ?
C20 C19 C18 120.2(3) . . ?
C19 C20 C15 121.5(3) . . ?
O20 C20 C15 116.5(3) . . ?
O20 C20 C19 121.8(3) . . ?
C17 C21 C22 112.7(2) . . ?
C17 C21 C31 112.6(3) . . ?
C22 C21 C31 109.4(3) . . ?
C23 C22 C21 122.2(3) . . ?
C23 C22 C27 116.5(3) . . ?
C27 C22 C21 121.3(3) . . ?
C24 C23 C22 123.5(3) . . ?
C23 C24 C25 117.8(3) . . ?
C23 C24 C28 121.3(3) . . ?
C25 C24 C28 120.9(3) . . ?
C24 C25 C26 120.9(3) . . ?
O25 C25 C24 116.2(3) . . ?
O25 C25 C26 122.9(3) . . ?
C27 C26 C25 119.1(3) . . ?
C26 C27 C22 122.1(3) . . ?
O27 C27 C22 115.6(3) . . ?
O27 C27 C26 122.3(3) . . ?
C1 C28 C24 113.7(2) . . ?
C1 C28 C32 112.6(3) . . ?
C24 C28 C32 109.0(2) . . ?
O6 C41 C42 110.0(3) . . ?
C43 C42 C41 119.2(3) . . ?
C46 C42 C41 123.0(3) . . ?
C46 C42 C43 117.7(3) . . ?
C44 C43 C42 118.4(4) . . ?
C45 C44 C43 119.3(4) . . ?
N1 C45 C44 123.3(4) . . ?
N1 C46 C42 124.7(4) . . ?
O13 C51 C52 109.2(3) . . ?
C53 C52 C51 123.1(3) . . ?
C56 C52 C51 119.9(3) . . ?
C56 C52 C53 117.0(3) . . ?
C54 C53 C52 119.1(3) . . ?
C55 C54 C53 119.3(4) . . ?
N2 C55 C54 123.2(3) . . ?
N2 C56 C52 124.7(4) . . ?
O20 C61 C62 108.2(3) . . ?
C63 C62 C61 121.9(3) . . ?
C66 C62 C61 121.4(3) . . ?
C66 C62 C63 116.7(3) . . ?
C64 C63 C62 118.9(4) . . ?
C63 C64 C65 119.2(4) . . ?
N3 C65 C64 123.4(4) . . ?
N3 C66 C62 125.0(4) . . ?
O27 C71 C72 107.6(3) . . ?
C73 C72 C71 121.4(3) . . ?
C73 C72 C76 118.0(3) . . ?
C76 C72 C71 120.4(3) . . ?
C72 C73 C74 118.6(3) . . ?
C75 C74 C73 119.6(4) . . ?
N4 C75 C74 122.4(3) . . ?
N4 C76 C72 123.5(3) . . ?
C102 C101 I101 121.2(3) . . ?
C106 C101 C102 116.9(3) . . ?
C106 C101 I101 121.8(2) . . ?
C101 C102 C103 121.9(4) . . ?
F102 C102 C101 119.7(3) . . ?
F102 C102 C103 118.4(3) . . ?
C104 C103 C102 120.8(4) . . ?
F103 C103 C102 119.1(4) . . ?
F103 C103 C104 120.1(3) . . ?
C103 C104 I104 121.6(3) . . ?
C105 C104 C103 117.0(3) . . ?
C105 C104 I104 121.4(3) . . ?
C104 C105 C106 122.1(3) . . ?
F105 C105 C104 119.8(3) . . ?
F105 C105 C106 118.1(3) . . ?
C101 C106 C105 121.3(3) . . ?
F106 C106 C101 120.0(3) . . ?
F106 C106 C105 118.7(3) . . ?
C202 C201 C203 117.3(4) . . ?
C202 C201 I201 121.1(3) . . ?
C203 C201 I201 121.5(3) . . ?
C201 C202 C203 121.1(4) . 2_577 ?
F202 C202 C201 120.8(4) . . ?
F202 C202 C203 118.2(4) . 2_577 ?
C201 C203 C202 121.6(4) . 2_577 ?
F203 C203 C201 120.5(4) . . ?
F203 C203 C202 117.9(4) . 2_577 ?
Cl1 C300 Cl3 108.8(3) . . ?
Cl2 C300 Cl1 112.4(3) . . ?
Cl2 C300 Cl3 110.4(3) . . ?
C46 N1 C45 116.5(4) . . ?
C55 N2 C56 116.8(3) . . ?
C65 N3 C66 116.9(3) . . ?
C75 N4 C76 117.8(3) . . ?
C4 O4 C33 117.4(3) . . ?
C6 O6 C41 116.4(2) . . ?
C11 O11 C34 118.3(2) . . ?
C13 O13 C51 117.9(2) . . ?
C18 O18 C35 117.1(3) . . ?
C20 O20 C61 116.9(3) . . ?
C25 O25 C36 117.8(2) . . ?
C27 O27 C71 118.3(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
C1 C2 C3 C4 -1.3(4) . . . . ?
C1 C2 C3 C7 176.7(3) . . . . ?
C1 C6 O6 C41 160.3(3) . . . . ?
C2 C1 C6 C5 3.8(4) . . . . ?
C2 C1 C6 O6 -177.6(2) . . . . ?
C2 C1 C28 C24 116.1(3) . . . . ?
C2 C1 C28 C32 -8.5(4) . . . . ?
C2 C3 C4 C5 2.8(4) . . . . ?
C2 C3 C4 O4 -176.7(2) . . . . ?
C2 C3 C7 C8 -105.7(3) . . . . ?
C2 C3 C7 C29 19.0(4) . . . . ?
C3 C4 C5 C6 -1.1(4) . . . . ?
C3 C4 O4 C33 165.5(3) . . . . ?
C3 C7 C8 C9 29.4(4) . . . . ?
C3 C7 C8 C13 -153.8(3) . . . . ?
C4 C3 C7 C8 72.2(3) . . . . ?
C4 C3 C7 C29 -163.0(3) . . . . ?
C4 C5 C6 C1 -2.3(4) . . . . ?
C4 C5 C6 O6 179.2(3) . . . . ?
C5 C4 O4 C33 -14.1(4) . . . . ?
C5 C6 O6 C41 -21.1(4) . . . . ?
C6 C1 C2 C3 -2.0(4) . . . . ?
C6 C1 C28 C24 -65.4(3) . . . . ?
C6 C1 C28 C32 170.0(3) . . . . ?
C7 C3 C4 C5 -175.2(3) . . . . ?
C7 C3 C4 O4 5.3(4) . . . . ?
C7 C8 C9 C10 178.2(3) . . . . ?
C7 C8 C13 C12 -178.8(3) . . . . ?
C7 C8 C13 O13 3.4(4) . . . . ?
C8 C9 C10 C11 -1.0(5) . . . . ?
C8 C9 C10 C14 179.9(3) . . . . ?
C8 C13 O13 C51 -149.5(3) . . . . ?
C9 C8 C13 C12 -1.8(5) . . . . ?
C9 C8 C13 O13 -179.6(3) . . . . ?
C9 C10 C11 C12 1.1(5) . . . . ?
C9 C10 C11 O11 -179.1(3) . . . . ?
C9 C10 C14 C15 -32.0(4) . . . . ?
C9 C10 C14 C30 95.7(4) . . . . ?
C10 C11 C12 C13 -1.6(5) . . . . ?
C10 C11 O11 C34 -176.5(3) . . . . ?
C10 C14 C15 C16 113.2(3) . . . . ?
C10 C14 C15 C20 -68.2(3) . . . . ?
C11 C10 C14 C15 148.9(3) . . . . ?
C11 C10 C14 C30 -83.3(4) . . . . ?
C11 C12 C13 C8 2.0(5) . . . . ?
C11 C12 C13 O13 179.7(3) . . . . ?
C12 C11 O11 C34 3.3(5) . . . . ?
C12 C13 O13 C51 32.7(4) . . . . ?
C13 C8 C9 C10 1.3(5) . . . . ?
C14 C10 C11 C12 -179.8(3) . . . . ?
C14 C10 C11 O11 0.1(4) . . . . ?
C14 C15 C16 C17 178.3(3) . . . . ?
C14 C15 C20 C19 -179.3(3) . . . . ?
C14 C15 C20 O20 -4.3(4) . . . . ?
C15 C16 C17 C18 0.9(4) . . . . ?
C15 C16 C17 C21 -178.0(3) . . . . ?
C15 C20 O20 C61 115.8(3) . . . . ?
C16 C15 C20 C19 -0.6(4) . . . . ?
C16 C15 C20 O20 174.4(2) . . . . ?
C16 C17 C18 C19 -0.7(4) . . . . ?
C16 C17 C18 O18 179.8(3) . . . . ?
C16 C17 C21 C22 -102.9(3) . . . . ?
C16 C17 C21 C31 21.4(4) . . . . ?
C17 C18 C19 C20 -0.1(5) . . . . ?
C17 C18 O18 C35 165.4(3) . . . . ?
C17 C21 C22 C23 22.8(4) . . . . ?
C17 C21 C22 C27 -159.8(3) . . . . ?
C18 C17 C21 C22 78.2(3) . . . . ?
C18 C17 C21 C31 -157.4(3) . . . . ?
C18 C19 C20 C15 0.8(5) . . . . ?
C18 C19 C20 O20 -173.9(3) . . . . ?
C19 C18 O18 C35 -14.0(4) . . . . ?
C19 C20 O20 C61 -69.2(4) . . . . ?
C20 C15 C16 C17 -0.3(4) . . . . ?
C21 C17 C18 C19 178.2(3) . . . . ?
C21 C17 C18 O18 -1.2(4) . . . . ?
C21 C22 C23 C24 177.7(3) . . . . ?
C21 C22 C27 C26 -176.2(3) . . . . ?
C21 C22 C27 O27 4.5(4) . . . . ?
C22 C23 C24 C25 -2.0(5) . . . . ?
C22 C23 C24 C28 178.7(3) . . . . ?
C22 C27 O27 C71 174.3(3) . . . . ?
C23 C22 C27 C26 1.3(5) . . . . ?
C23 C22 C27 O27 -178.0(3) . . . . ?
C23 C24 C25 C26 2.2(5) . . . . ?
C23 C24 C25 O25 -178.6(3) . . . . ?
C23 C24 C28 C1 -24.0(4) . . . . ?
C23 C24 C28 C32 102.5(3) . . . . ?
C24 C25 C26 C27 -0.8(5) . . . . ?
C24 C25 O25 C36 171.4(3) . . . . ?
C25 C24 C28 C1 156.7(3) . . . . ?
C25 C24 C28 C32 -76.7(4) . . . . ?
C25 C26 C27 C22 -1.1(5) . . . . ?
C25 C26 C27 O27 178.2(3) . . . . ?
C26 C25 O25 C36 -9.4(5) . . . . ?
C26 C27 O27 C71 -5.1(5) . . . . ?
C27 C22 C23 C24 0.2(5) . . . . ?
C28 C1 C2 C3 176.6(3) . . . . ?
C28 C1 C6 C5 -174.9(3) . . . . ?
C28 C1 C6 O6 3.8(4) . . . . ?
C28 C24 C25 C26 -178.5(3) . . . . ?
C28 C24 C25 O25 0.7(4) . . . . ?
C29 C7 C8 C9 -97.6(3) . . . . ?
C29 C7 C8 C13 79.2(4) . . . . ?
C30 C14 C15 C16 -12.9(4) . . . . ?
C30 C14 C15 C20 165.6(3) . . . . ?
C31 C21 C22 C23 -103.3(3) . . . . ?
C31 C21 C22 C27 74.1(4) . . . . ?
C41 C42 C43 C44 -177.6(3) . . . . ?
C41 C42 C46 N1 178.2(4) . . . . ?
C42 C41 O6 C6 -168.1(2) . . . . ?
C42 C43 C44 C45 0.1(6) . . . . ?
C42 C46 N1 C45 -1.4(7) . . . . ?
C43 C42 C46 N1 1.2(6) . . . . ?
C43 C44 C45 N1 -0.3(7) . . . . ?
C44 C45 N1 C46 0.9(7) . . . . ?
C46 C42 C43 C44 -0.5(5) . . . . ?
C51 C52 C53 C54 -179.9(4) . . . . ?
C51 C52 C56 N2 178.7(4) . . . . ?
C52 C51 O13 C13 170.6(3) . . . . ?
C52 C53 C54 C55 0.5(6) . . . . ?
C52 C56 N2 C55 1.8(6) . . . . ?
C53 C52 C56 N2 -1.5(6) . . . . ?
C53 C54 C55 N2 -0.3(7) . . . . ?
C54 C55 N2 C56 -0.8(6) . . . . ?
C56 C52 C53 C54 0.3(6) . . . . ?
C61 C62 C63 C64 -178.7(5) . . . . ?
C61 C62 C66 N3 178.7(3) . . . . ?
C62 C61 O20 C20 -158.0(3) . . . . ?
C62 C63 C64 C65 -0.4(8) . . . . ?
C62 C66 N3 C65 0.4(6) . . . . ?
C63 C62 C66 N3 -1.4(6) . . . . ?
C63 C64 C65 N3 -0.6(9) . . . . ?
C64 C65 N3 C66 0.7(7) . . . . ?
C66 C62 C63 C64 1.4(7) . . . . ?
C71 C72 C73 C74 -177.8(4) . . . . ?
C71 C72 C76 N4 177.5(4) . . . . ?
C72 C71 O27 C27 -179.1(3) . . . . ?
C72 C73 C74 C75 0.5(7) . . . . ?
C72 C76 N4 C75 0.3(6) . . . . ?
C73 C72 C76 N4 1.7(6) . . . . ?
C73 C74 C75 N4 1.6(8) . . . . ?
C74 C75 N4 C76 -2.0(7) . . . . ?
C76 C72 C73 C74 -2.0(6) . . . . ?
C101 C102 C103 C104 1.9(8) . . . . ?
C101 C102 C103 F103 179.6(5) . . . . ?
C102 C101 C106 C105 0.3(6) . . . . ?
C102 C101 C106 F106 178.8(4) . . . . ?
C102 C103 C104 C105 -1.5(7) . . . . ?
C102 C103 C104 I104 177.8(4) . . . . ?
C103 C104 C105 C106 0.6(6) . . . . ?
C103 C104 C105 F105 -178.3(4) . . . . ?
C104 C105 C106 C101 0.0(6) . . . . ?
C104 C105 C106 F106 -178.5(4) . . . . ?
C106 C101 C102 C103 -1.2(7) . . . . ?
C106 C101 C102 F102 179.4(5) . . . . ?
C202 C201 C203 C202 0.4(7) . . . 2_577 ?
C202 C201 C203 F203 179.9(4) . . . . ?
C203 C201 C202 C203 -0.4(7) . . . 2_577 ?
C203 C201 C202 F202 -179.3(4) . . . . ?
O4 C4 C5 C6 178.4(3) . . . . ?
O6 C41 C42 C43 -155.3(3) . . . . ?
O6 C41 C42 C46 27.8(4) . . . . ?
O11 C11 C12 C13 178.6(3) . . . . ?
O13 C51 C52 C53 -9.3(5) . . . . ?
O13 C51 C52 C56 170.6(3) . . . . ?
O18 C18 C19 C20 179.3(3) . . . . ?
O20 C61 C62 C63 -35.2(5) . . . . ?
O20 C61 C62 C66 144.7(3) . . . . ?
O25 C25 C26 C27 -179.9(3) . . . . ?
O27 C71 C72 C73 -31.5(5) . . . . ?
O27 C71 C72 C76 152.8(3) . . . . ?
F102 C102 C103 C104 -178.7(5) . . . . ?
F102 C102 C103 F103 -1.0(8) . . . . ?
F103 C103 C104 C105 -179.2(5) . . . . ?
F103 C103 C104 I104 0.1(7) . . . . ?
F105 C105 C106 C101 178.9(4) . . . . ?
F105 C105 C106 F106 0.4(6) . . . . ?
I104 C104 C105 C106 -178.7(3) . . . . ?
I104 C104 C105 F105 2.4(5) . . . . ?
I201 C201 C202 C203 179.2(3) . . . 2_577 ?
I201 C201 C202 F202 0.4(6) . . . . ?
I201 C201 C203 C202 -179.2(3) . . . 2_577 ?
I201 C201 C203 F203 0.3(6) . . . . ?
I101 C101 C102 C103 -177.8(4) . . . . ?
I101 C101 C102 F102 2.8(7) . . . . ?
I101 C101 C106 C105 176.9(3) . . . . ?
I101 C101 C106 F106 -4.7(5) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4 18 -7 0.0632 -4.0000 18.0000 -6.9998 -0.8079 0.2980 0.5142
2 19 -7 0.0708 1.9999 19.0000 -6.9997 -0.9412 0.3177 0.2136
-18 -5 -2 0.0543 -17.9999 -5.0000 -2.0004 0.4424 -0.1711 0.8739
0 3 28 0.0164 0.0000 3.0000 28.0012 0.4223 0.8836 -0.0098
0 -3 -28 0.0115 -0.0000 -3.0000 -28.0012 -0.4223 -0.8836 0.0098
-1 19 -1 0.0639 -1.0000 19.0000 -0.9995 -0.7782 0.4932 0.3595
1 -19 2 0.0624 1.0000 -19.0000 1.9995 0.7977 -0.4646 -0.3616
14 14 3 0.0712 13.9999 14.0000 3.0006 -0.7280 0.4515 -0.5206
16 -8 5 0.0717 15.9999 -8.0000 5.0001 0.1765 -0.0966 -0.9830



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 379 105 ' '
2 0.039 0.925 0.590 12 1 ' '
3 0.961 0.075 0.410 12 1 ' '
_platon_squeeze_details          
;

;

# start Validation Reply Form
_vrf_PLAT250_1-B                 
;
PROBLEM:Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.9 Note

RESPONSE: There was not enough electron density to build a chemically
reasonable disorder for 1,4-diiodotetrafluorobenzene what causes
fluorine atoms to have larger U(i,j) than average.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_FORMU01_1-B                 
;
PROBLEM: There is a discrepancy between the atom counts in the 
_chemical_formula_sum and _chemical_formula_moiety.

RESPONSE: The discrepancy is due to the deuterium atom of the
chloroform which is taken into account in chemical formula.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT605_1-B                 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        381 A**3

RESPONSE: The electron density peaks were suitable for highly disordered
chloroform molecule. Even with numerous attemps to model the solvent 
molecule a reasonable model could not be build. Thus the SQUEEZE option 
in PLATON was used to remove the electron density.
;
# end Validation Reply Form

_ins_header                      
;
TITL 1-B
REM P-1 (#2 in standard setting)
CELL 0.71073  13.045385  13.794779  20.621891  88.0431  82.9962  84.6929
ZERR    3.00   0.000315   0.000453   0.000732   0.0028   0.0024   0.0023
LATT  1
SFAC C H N O
UNIT 180.00 180.00 12.00 12.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2-B
_database_code_depnum_ccdc_archive 'CCDC 1044959'
_audit_update_record             
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-09-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C6 F4 I2, C H Cl3, C30 H30 N2 O4'
_chemical_formula_sum            'C37 H31 Cl3 F4 I2 N2 O4'
_chemical_formula_weight         1003.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 N4 O8 I2 F4'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y+1/2, z'
3 'x+1/2, -y, -z+1/2'
4 '-x, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y-1/2, -z'
7 '-x-1/2, y, z-1/2'
8 'x, -y-1/2, z-1/2'

_cell_length_a                   11.07141(13)
_cell_length_b                   44.2970(7)
_cell_length_c                   15.7761(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7737.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19694
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.1630
_cell_measurement_theta_min      2.2840
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.3092
_exptl_crystal_size_mid          0.0883
_exptl_crystal_size_min          0.0615
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66818
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         1.84
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -85.00    7.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470  -77.0000  -30.0000 184

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   47.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470   77.0000   90.0000 190

#__ type_ start__ end____ width___ exp.time_
  3 omega    2.00   92.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   57.0000 -150.0000 180

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   65.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  -90.0000 132

#__ type_ start__ end____ width___ exp.time_
  5 omega  -42.00  -16.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00  -11.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000   60.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0104215000
_diffrn_orient_matrix_UB_12      -0.0134079000
_diffrn_orient_matrix_UB_13      0.0234844000
_diffrn_orient_matrix_UB_21      0.0028923000
_diffrn_orient_matrix_UB_22      -0.0085551000
_diffrn_orient_matrix_UB_23      -0.0379369000
_diffrn_orient_matrix_UB_31      0.0631588000
_diffrn_orient_matrix_UB_32      -0.0018072000
_diffrn_orient_matrix_UB_33      0.0055997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                8275
_reflns_number_total             11088
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0250P)²+17.6680P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1055
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C201(H201)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C5(H5), C12(H12), C43(H43), C45(H45), C46(H46), C44(H44),
 C53(H53), C54(H54), C56(H56), C55(H55)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
I101 I 0.51693(2) 0.516741(6) 0.65020(2) 0.04508(8) Uani 1 d . . .
I104 I 0.00295(2) 0.606496(6) 0.71391(2) 0.04197(8) Uani 1 d . . .
Cl1 Cl 0.25394(17) 0.43073(4) 0.62242(13) 0.0984(6) Uani 1 d . . .
Cl2 Cl 0.20900(11) 0.43541(4) 0.44374(12) 0.0907(6) Uani 1 d . . .
Cl3 Cl 0.43141(13) 0.41018(3) 0.50158(14) 0.0918(6) Uani 1 d . . .
F103 F 0.2864(2) 0.61733(5) 0.74865(19) 0.0547(7) Uani 1 d . . .
F106 F 0.2346(2) 0.50667(5) 0.6063(2) 0.0591(8) Uani 1 d . . .
F102 F 0.4795(2) 0.58280(6) 0.7264(2) 0.0562(7) Uani 1 d . . .
F105 F 0.0403(2) 0.54083(6) 0.63091(19) 0.0553(7) Uani 1 d . . .
O11 O 0.2952(2) 0.18805(5) 0.47758(19) 0.0380(6) Uani 1 d . . .
O6 O 0.4270(2) 0.23357(5) 0.66359(17) 0.0336(6) Uani 1 d . . .
O4 O 0.7040(3) 0.31609(6) 0.70647(18) 0.0449(7) Uani 1 d . . .
N1 N 0.1997(3) 0.14313(8) 0.7559(3) 0.0484(9) Uani 1 d . . .
C16 C 0.4258(3) 0.24958(9) 0.3970(3) 0.0371(8) Uani 1 d . . .
H16A H 0.3882 0.2691 0.3957 0.056 Uiso 1 calc . . GR
H16B H 0.3775 0.2355 0.3655 0.056 Uiso 1 calc . . GR
H16C H 0.5048 0.2508 0.3721 0.056 Uiso 1 calc . . GR
N2 N 0.7143(3) 0.47816(8) 0.6203(3) 0.0492(9) Uani 1 d . . .
C1 C 0.5054(3) 0.26036(7) 0.5453(2) 0.0225(6) Uani 1 d . . .
C15 C 0.6354(3) 0.34755(8) 0.4654(3) 0.0354(9) Uani 1 d . . .
H15A H 0.6796 0.3651 0.4477 0.053 Uiso 1 calc . . GR
H15B H 0.5565 0.3535 0.4844 0.053 Uiso 1 calc . . GR
H15C H 0.6277 0.3338 0.4187 0.053 Uiso 1 calc . . GR
C7 C 0.7032(3) 0.33192(7) 0.5385(2) 0.0266(7) Uani 1 d . . .
H7 H 0.7028 0.3463 0.5858 0.032 Uiso 1 calc . . R
C13 C 0.9160(3) 0.35062(7) 0.5152(2) 0.0274(7) Uani 1 d . . .
C14 C 0.4367(3) 0.23892(7) 0.4887(2) 0.0259(7) Uani 1 d . . .
H14 H 0.3545 0.2376 0.5113 0.031 Uiso 1 calc . . R
C9 C 0.8853(3) 0.29767(7) 0.5056(2) 0.0236(6) Uani 1 d . . .
H9 H 0.8337 0.2811 0.5057 0.028 Uiso 1 calc . . R
C51 C 0.9392(3) 0.40343(7) 0.5466(3) 0.0345(8) Uani 1 d . . .
H51A H 0.9866 0.4086 0.4971 0.041 Uiso 1 calc . . R
H51B H 0.9940 0.3986 0.5926 0.041 Uiso 1 calc . . R
C11 C 0.4157(3) 0.18224(7) 0.4903(2) 0.0288(7) Uani 1 d . . .
C2 C 0.5723(3) 0.28500(7) 0.5171(2) 0.0243(7) Uani 1 d . . .
H2 H 0.5733 0.2890 0.4592 0.029 Uiso 1 calc . . R
C102 C 0.3714(3) 0.57219(9) 0.7007(3) 0.0406(9) Uani 1 d . . .
C41 C 0.4802(3) 0.20783(8) 0.7031(2) 0.0290(7) Uani 1 d . . .
H41A H 0.5202 0.2137 0.7553 0.035 Uiso 1 calc . . R
H41B H 0.5396 0.1988 0.6658 0.035 Uiso 1 calc . . R
C18 C 0.2130(3) 0.16363(9) 0.4872(4) 0.0528(13) Uani 1 d . . .
H18A H 0.2256 0.1492 0.4426 0.079 Uiso 1 calc . . GR
H18B H 0.1317 0.1711 0.4845 0.079 Uiso 1 calc . . GR
H18C H 0.2261 0.1541 0.5411 0.079 Uiso 1 calc . . GR
C5 C 0.5709(3) 0.27314(8) 0.6880(2) 0.0319(8) Uani 1 d . . .
H5 H 0.5709 0.2690 0.7457 0.038 Uiso 1 calc . . R
C103 C 0.2709(3) 0.58994(8) 0.7126(3) 0.0386(9) Uani 1 d . . .
C6 C 0.5044(3) 0.25534(7) 0.6325(2) 0.0262(7) Uani 1 d . . .
C8 C 0.8361(3) 0.32622(7) 0.5174(2) 0.0245(7) Uani 1 d . . .
C10 C 0.4910(3) 0.20731(7) 0.4935(2) 0.0227(6) Uani 1 d . . .
C12 C 1.0386(3) 0.34674(7) 0.5014(2) 0.0299(7) Uani 1 d . . .
H12 H 1.0898 0.3634 0.4994 0.036 Uiso 1 calc . . R
C43 C 0.4088(3) 0.15643(8) 0.7455(3) 0.0393(9) Uani 1 d . . .
H43 H 0.4890 0.1504 0.7501 0.047 Uiso 1 calc . . R
C4 C 0.6377(3) 0.29736(8) 0.6563(2) 0.0307(7) Uani 1 d . . .
C104 C 0.1575(3) 0.58017(8) 0.6904(3) 0.0362(9) Uani 1 d . . .
C3 C 0.6376(3) 0.30398(7) 0.5700(2) 0.0248(7) Uani 1 d . . .
C42 C 0.3811(3) 0.18562(7) 0.7217(2) 0.0308(7) Uani 1 d . . .
C17 C 0.6909(5) 0.31261(11) 0.7963(3) 0.0580(13) Uani 1 d . . .
H17A H 0.6066 0.3120 0.8106 0.087 Uiso 1 calc . . GR
H17B H 0.7283 0.3294 0.8246 0.087 Uiso 1 calc . . GR
H17C H 0.7288 0.2942 0.8139 0.087 Uiso 1 calc . . GR
C45 C 0.1743(4) 0.17121(10) 0.7314(4) 0.0582(14) Uani 1 d . . .
H45 H 0.0934 0.1765 0.7254 0.070 Uiso 1 calc . . R
C46 C 0.2605(4) 0.19306(9) 0.7142(3) 0.0463(11) Uani 1 d . . .
H46 H 0.2374 0.2124 0.6978 0.056 Uiso 1 calc . . R
C105 C 0.1486(3) 0.55187(9) 0.6542(3) 0.0405(9) Uani 1 d . . .
C106 C 0.2492(4) 0.53412(8) 0.6419(3) 0.0423(10) Uani 1 d . . .
C201 C 0.3187(4) 0.43696(10) 0.5231(4) 0.0602(14) Uani 1 d . . .
H201 H 0.3554 0.4571 0.5227 0.072 Uiso 1 calc . . R
C44 C 0.3165(4) 0.13624(9) 0.7625(3) 0.0479(11) Uani 1 d . . .
H44 H 0.3370 0.1168 0.7795 0.058 Uiso 1 calc . . R
C52 C 0.8592(3) 0.42936(8) 0.5711(3) 0.0338(8) Uani 1 d . . .
C101 C 0.3628(3) 0.54372(8) 0.6650(3) 0.0376(9) Uani 1 d . . .
C53 C 0.7358(3) 0.42646(9) 0.5789(3) 0.0477(11) Uani 1 d . . .
H53 H 0.6984 0.4081 0.5677 0.057 Uiso 1 calc . . R
C54 C 0.6688(4) 0.45102(9) 0.6035(3) 0.0538(13) Uani 1 d . . .
H54 H 0.5858 0.4485 0.6088 0.065 Uiso 1 calc . . R
C56 C 0.9087(3) 0.45736(8) 0.5893(3) 0.0434(10) Uani 1 d . . .
H56 H 0.9916 0.4604 0.5854 0.052 Uiso 1 calc . . R
C55 C 0.8336(4) 0.48079(9) 0.6133(3) 0.0504(12) Uani 1 d . . .
H55 H 0.8684 0.4994 0.6252 0.060 Uiso 1 calc . . R
O13 O 0.8639(2) 0.37840(5) 0.52876(19) 0.0373(6) Uani 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
I101 C101 2.097(3) . ?
I104 C104 2.104(3) . ?
Cl1 C201 1.745(6) . ?
Cl2 C201 1.746(5) . ?
Cl3 C201 1.755(5) . ?
F103 C103 1.351(4) . ?
F106 C106 1.349(4) . ?
F102 C102 1.348(4) . ?
F105 C105 1.346(4) . ?
O11 C11 1.373(4) . ?
O11 C18 1.422(4) . ?
O6 C41 1.427(4) . ?
O6 C6 1.381(4) . ?
O4 C4 1.361(4) . ?
O4 C17 1.433(5) . ?
N1 C45 1.333(5) . ?
N1 C44 1.332(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C14 1.526(5) . ?
N2 C54 1.330(5) . ?
N2 C55 1.331(5) . ?
C1 C14 1.510(4) . ?
C1 C2 1.392(4) . ?
C1 C6 1.393(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C7 1.540(5) . ?
C7 H7 0.9800 . ?
C7 C8 1.530(4) . ?
C7 C3 1.519(4) . ?
C13 C8 1.397(4) . ?
C13 C12 1.385(4) . ?
C13 O13 1.376(4) . ?
C14 H14 0.9800 . ?
C14 C10 1.526(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.389(4) . ?
C9 C10 1.400(4) 2_655 ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51 C52 1.501(5) . ?
C51 O13 1.416(4) . ?
C11 C10 1.389(4) . ?
C11 C12 1.391(4) 2_655 ?
C2 H2 0.9300 . ?
C2 C3 1.388(5) . ?
C102 C103 1.376(5) . ?
C102 C101 1.384(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.502(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C6 1.389(5) . ?
C5 C4 1.396(5) . ?
C103 C104 1.374(5) . ?
C10 C9 1.400(4) 2_655 ?
C12 C11 1.391(4) 2_655 ?
C12 H12 0.9300 . ?
C43 H43 0.9300 . ?
C43 C42 1.381(5) . ?
C43 C44 1.385(5) . ?
C4 C3 1.392(5) . ?
C104 C105 1.381(5) . ?
C42 C46 1.381(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C45 H45 0.9300 . ?
C45 C46 1.386(5) . ?
C46 H46 0.9300 . ?
C105 C106 1.377(5) . ?
C106 C101 1.376(5) . ?
C201 H201 0.9800 . ?
C44 H44 0.9300 . ?
C52 C53 1.378(5) . ?
C52 C56 1.385(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.373(5) . ?
C54 H54 0.9300 . ?
C56 H56 0.9300 . ?
C56 C55 1.382(5) . ?
C55 H55 0.9300 . ?

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
C11 O11 C18 117.6(3) . . ?
C6 O6 C41 117.2(3) . . ?
C4 O4 C17 117.1(3) . . ?
C44 N1 C45 116.2(3) . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
C54 N2 C55 116.0(3) . . ?
C2 C1 C14 124.9(3) . . ?
C2 C1 C6 116.4(3) . . ?
C6 C1 C14 118.7(3) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
C15 C7 H7 106.1 . . ?
C8 C7 C15 112.4(3) . . ?
C8 C7 H7 106.1 . . ?
C3 C7 C15 112.2(3) . . ?
C3 C7 H7 106.1 . . ?
C3 C7 C8 113.4(3) . . ?
C12 C13 C8 121.9(3) . . ?
O13 C13 C8 115.0(3) . . ?
O13 C13 C12 123.1(3) . . ?
C16 C14 H14 106.9 . . ?
C1 C14 C16 114.0(3) . . ?
C1 C14 H14 106.9 . . ?
C1 C14 C10 110.4(3) . . ?
C10 C14 C16 111.3(3) . . ?
C10 C14 H14 106.9 . . ?
C8 C9 H9 118.5 . . ?
C8 C9 C10 123.0(3) . 2_655 ?
C10 C9 H9 118.5 2_655 . ?
H51A C51 H51B 108.5 . . ?
C52 C51 H51A 110.2 . . ?
C52 C51 H51B 110.2 . . ?
O13 C51 H51A 110.2 . . ?
O13 C51 H51B 110.2 . . ?
O13 C51 C52 107.6(3) . . ?
O11 C11 C10 116.0(3) . . ?
O11 C11 C12 123.0(3) . 2_655 ?
C10 C11 C12 121.0(3) . 2_655 ?
C1 C2 H2 118.0 . . ?
C3 C2 C1 124.0(3) . . ?
C3 C2 H2 118.0 . . ?
F102 C102 C103 118.5(3) . . ?
F102 C102 C101 120.1(3) . . ?
C103 C102 C101 121.3(4) . . ?
O6 C41 H41A 110.1 . . ?
O6 C41 H41B 110.1 . . ?
O6 C41 C42 107.9(3) . . ?
H41A C41 H41B 108.4 . . ?
C42 C41 H41A 110.1 . . ?
C42 C41 H41B 110.1 . . ?
O11 C18 H18A 109.5 . . ?
O11 C18 H18B 109.5 . . ?
O11 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C6 C5 H5 120.3 . . ?
C6 C5 C4 119.4(3) . . ?
C4 C5 H5 120.3 . . ?
F103 C103 C102 117.9(3) . . ?
F103 C103 C104 120.4(3) . . ?
C104 C103 C102 121.7(3) . . ?
O6 C6 C1 117.8(3) . . ?
O6 C6 C5 120.1(3) . . ?
C5 C6 C1 121.8(3) . . ?
C13 C8 C7 119.1(3) . . ?
C9 C8 C7 123.8(3) . . ?
C9 C8 C13 116.9(3) . . ?
C9 C10 C14 122.4(3) 2_655 . ?
C11 C10 C14 119.7(3) . . ?
C11 C10 C9 117.8(3) . 2_655 ?
C13 C12 C11 119.4(3) . 2_655 ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 2_655 . ?
C42 C43 H43 120.2 . . ?
C42 C43 C44 119.6(4) . . ?
C44 C43 H43 120.2 . . ?
O4 C4 C5 123.1(3) . . ?
O4 C4 C3 116.2(3) . . ?
C3 C4 C5 120.8(3) . . ?
C103 C104 I104 121.6(3) . . ?
C103 C104 C105 117.1(3) . . ?
C105 C104 I104 121.2(3) . . ?
C2 C3 C7 123.1(3) . . ?
C2 C3 C4 117.5(3) . . ?
C4 C3 C7 119.4(3) . . ?
C43 C42 C41 120.3(3) . . ?
C43 C42 C46 117.5(3) . . ?
C46 C42 C41 122.2(3) . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C45 H45 117.9 . . ?
N1 C45 C46 124.3(4) . . ?
C46 C45 H45 117.9 . . ?
C42 C46 C45 118.8(4) . . ?
C42 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
F105 C105 C104 120.4(3) . . ?
F105 C105 C106 118.3(3) . . ?
C106 C105 C104 121.3(4) . . ?
F106 C106 C105 118.4(4) . . ?
F106 C106 C101 119.9(3) . . ?
C101 C106 C105 121.7(3) . . ?
Cl1 C201 Cl2 110.6(3) . . ?
Cl1 C201 Cl3 111.0(3) . . ?
Cl1 C201 H201 108.6 . . ?
Cl2 C201 Cl3 109.2(3) . . ?
Cl2 C201 H201 108.6 . . ?
Cl3 C201 H201 108.6 . . ?
N1 C44 C43 123.6(4) . . ?
N1 C44 H44 118.2 . . ?
C43 C44 H44 118.2 . . ?
C53 C52 C51 122.4(3) . . ?
C53 C52 C56 117.2(3) . . ?
C56 C52 C51 120.4(3) . . ?
C102 C101 I101 120.5(3) . . ?
C106 C101 I101 122.5(3) . . ?
C106 C101 C102 116.9(3) . . ?
C52 C53 H53 120.4 . . ?
C54 C53 C52 119.2(4) . . ?
C54 C53 H53 120.4 . . ?
N2 C54 C53 124.6(4) . . ?
N2 C54 H54 117.7 . . ?
C53 C54 H54 117.7 . . ?
C52 C56 H56 120.3 . . ?
C55 C56 C52 119.4(4) . . ?
C55 C56 H56 120.3 . . ?
N2 C55 C56 123.6(4) . . ?
N2 C55 H55 118.2 . . ?
C56 C55 H55 118.2 . . ?
C13 O13 C51 119.0(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
I104 C104 C105 F105 1.8(6) . . . . ?
I104 C104 C105 C106 -177.4(3) . . . . ?
F103 C103 C104 I104 -1.6(6) . . . . ?
F103 C103 C104 C105 -179.7(4) . . . . ?
F106 C106 C101 I101 -1.7(6) . . . . ?
F106 C106 C101 C102 179.6(4) . . . . ?
F102 C102 C103 F103 0.8(6) . . . . ?
F102 C102 C103 C104 -177.9(4) . . . . ?
F102 C102 C101 I101 0.0(6) . . . . ?
F102 C102 C101 C106 178.7(4) . . . . ?
F105 C105 C106 F106 0.7(7) . . . . ?
F105 C105 C106 C101 -179.2(4) . . . . ?
O11 C11 C10 C14 3.9(5) . . . . ?
O11 C11 C10 C9 -179.4(3) . . . 2_655 ?
O6 C41 C42 C43 168.0(3) . . . . ?
O6 C41 C42 C46 -10.6(5) . . . . ?
O4 C4 C3 C7 -3.5(5) . . . . ?
O4 C4 C3 C2 179.0(3) . . . . ?
N1 C45 C46 C42 0.7(8) . . . . ?
C16 C14 C10 C9 94.4(4) . . . 2_655 ?
C16 C14 C10 C11 -89.0(4) . . . . ?
C1 C14 C10 C9 -33.2(4) . . . 2_655 ?
C1 C14 C10 C11 143.4(3) . . . . ?
C1 C2 C3 C7 -175.9(3) . . . . ?
C1 C2 C3 C4 1.5(5) . . . . ?
C15 C7 C8 C13 72.4(4) . . . . ?
C15 C7 C8 C9 -112.0(4) . . . . ?
C15 C7 C3 C2 34.6(4) . . . . ?
C15 C7 C3 C4 -142.7(3) . . . . ?
C14 C1 C2 C3 -178.2(3) . . . . ?
C14 C1 C6 O6 -9.0(4) . . . . ?
C14 C1 C6 C5 176.4(3) . . . . ?
C51 C52 C53 C54 178.5(4) . . . . ?
C51 C52 C56 C55 -178.8(4) . . . . ?
C2 C1 C14 C16 -11.0(4) . . . . ?
C2 C1 C14 C10 115.1(3) . . . . ?
C2 C1 C6 O6 171.8(3) . . . . ?
C2 C1 C6 C5 -2.8(5) . . . . ?
C102 C103 C104 I104 177.1(3) . . . . ?
C102 C103 C104 C105 -1.0(7) . . . . ?
C41 O6 C6 C1 115.8(3) . . . . ?
C41 O6 C6 C5 -69.5(4) . . . . ?
C41 C42 C46 C45 179.2(4) . . . . ?
C18 O11 C11 C10 -170.3(4) . . . . ?
C18 O11 C11 C12 8.4(6) . . . 2_655 ?
C5 C4 C3 C7 175.2(3) . . . . ?
C5 C4 C3 C2 -2.3(5) . . . . ?
C103 C102 C101 I101 -178.5(3) . . . . ?
C103 C102 C101 C106 0.2(7) . . . . ?
C103 C104 C105 F105 179.9(4) . . . . ?
C103 C104 C105 C106 0.7(7) . . . . ?
C6 O6 C41 C42 -172.9(3) . . . . ?
C6 C1 C14 C16 169.9(3) . . . . ?
C6 C1 C14 C10 -64.0(4) . . . . ?
C6 C1 C2 C3 1.0(5) . . . . ?
C6 C5 C4 O4 179.2(3) . . . . ?
C6 C5 C4 C3 0.5(5) . . . . ?
C8 C7 C3 C2 -94.0(4) . . . . ?
C8 C7 C3 C4 88.7(4) . . . . ?
C8 C13 C12 C11 -0.8(6) . . . 2_655 ?
C8 C13 O13 C51 165.9(3) . . . . ?
C10 C9 C8 C7 -174.4(3) 2_655 . . . ?
C10 C9 C8 C13 1.3(5) 2_655 . . . ?
C12 C13 C8 C7 176.2(3) . . . . ?
C12 C13 C8 C9 0.3(5) . . . . ?
C12 C13 O13 C51 -13.3(6) . . . . ?
C12 C11 C10 C14 -174.9(3) 2_655 . . . ?
C12 C11 C10 C9 1.8(5) 2_655 . . 2_655 ?
C43 C42 C46 C45 0.6(7) . . . . ?
C4 C5 C6 O6 -172.4(3) . . . . ?
C4 C5 C6 C1 2.1(5) . . . . ?
C104 C105 C106 F106 179.9(4) . . . . ?
C104 C105 C106 C101 0.0(7) . . . . ?
C3 C7 C8 C13 -159.0(3) . . . . ?
C3 C7 C8 C9 16.6(5) . . . . ?
C42 C43 C44 N1 1.2(7) . . . . ?
C17 O4 C4 C5 -8.0(6) . . . . ?
C17 O4 C4 C3 170.7(4) . . . . ?
C45 N1 C44 C43 0.0(8) . . . . ?
C105 C106 C101 I101 178.2(4) . . . . ?
C105 C106 C101 C102 -0.5(7) . . . . ?
C44 N1 C45 C46 -1.0(8) . . . . ?
C44 C43 C42 C41 180.0(4) . . . . ?
C44 C43 C42 C46 -1.4(6) . . . . ?
C52 C51 O13 C13 -171.8(3) . . . . ?
C52 C53 C54 N2 0.5(8) . . . . ?
C52 C56 C55 N2 0.1(8) . . . . ?
C101 C102 C103 F103 179.3(4) . . . . ?
C101 C102 C103 C104 0.6(7) . . . . ?
C53 C52 C56 C55 -0.6(7) . . . . ?
C54 N2 C55 C56 0.7(8) . . . . ?
C56 C52 C53 C54 0.3(7) . . . . ?
C55 N2 C54 C53 -1.0(8) . . . . ?
O13 C13 C8 C7 -3.0(5) . . . . ?
O13 C13 C8 C9 -178.8(3) . . . . ?
O13 C13 C12 C11 178.3(3) . . . 2_655 ?
O13 C51 C52 C53 4.1(6) . . . . ?
O13 C51 C52 C56 -177.7(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -3 22 0.0411 -1.0003 -3.0067 22.0002 0.5674 -0.8118 0.0654
0 3 -22 0.0380 0.0003 3.0064 -22.0002 -0.5570 0.8089 -0.1286
15 -7 -1 0.1415 15.0001 -6.9963 -1.0001 -0.0860 0.1412 0.9544
-14 5 10 0.1173 -14.0003 4.9939 10.0001 0.3138 -0.4626 -0.8373
0 -62 2 0.0413 0.0002 -61.9981 1.9994 0.8782 0.4545 0.1233
-1 62 3 0.0132 -1.0003 61.9964 3.0006 -0.7503 -0.6471 -0.1584
0 -62 -1 0.0364 0.0003 -61.9972 -1.0006 0.8078 0.5684 0.1065



_ins_header                      
;
TITL 2-B in Pccn 
REM Pccn (#56, found as Pbnb in a-cb setting)
CELL 0.71073  11.071412  44.297018  15.776135  90.0000  90.0000  90.0000
ZERR    8.00   0.000133   0.000678   0.000378   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y,-z+1/2 
SFAC C H N O F I
UNIT 480.00 480.00 32.00 64.00 32.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'

#===END 
