# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
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data_SF6_4
_database_code_depnum_ccdc_archive 'CCDC 1542198'
_audit_update_record             
;
2017-04-05 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT082_SF6@4               
;
PROBLEM: High R1 Value ..................................       0.21 Report
RESPONSE:  poor quality data despite many efforts to grow better crystals 
and collect better data. Model contains also a lot of (disordered) solvent.
;
_vrf_PLAT084_SF6@4               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.58 Report
RESPONSE:  poor quality data despite many efforts to grow better crystals 
and collect better data. Model contains also a lot of (disordered) solvent.
;
_vrf_PLAT934_SF6@4               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         34 Check 
RESPONSE: no obvious reason (systematic absents) to omit reflections
list of mail outliers follows
 Most Disagreeable Reflections (* if suppressed or used for Rfree).
 Error/esd is calculated as sqrt(wD^2/<wD^2>) where w is given by the weight
 formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections.

     h   k   l          Fo^2          Fc^2    Error/esd  Fc/Fc(max)  Resolution(A)

     4  -2   2       1588.92         27.13       6.00       0.022       2.91
    -3  -3   4       2626.72         55.47       5.77       0.032       2.98
    -2  -5   5        835.17          7.86       5.59       0.012       2.52
    -4   3   1        367.06          4.98       5.56       0.010       3.15
    -3  -2   1       1310.63         23.22       5.54       0.021       3.55
     0  -4   6        338.53          1.95       5.46       0.006       2.63
    -7   6   1        262.72          3.24       5.46       0.008       1.75
    -2   0   5        424.38         13.64       5.34       0.016       3.14
   -14  13   2        282.54          0.04       5.25       0.001       0.85
     0  -1   2        876.33         58.96       5.22       0.033       8.17
   -13  14   1        248.31          0.18       5.08       0.002       0.87
    -6  -4   6        361.41         10.79       5.06       0.014       1.76
   -14  12   3        268.42          0.28       5.03       0.002       0.87
   -14  11   4        294.52          0.91       5.03       0.004       0.89

;
_vrf_PLAT098_SF6@4               
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -1.73 eA-3  
RESPONSE: 
The main cause to this error is limitation/inadequate modelling of disordered solvent atoms.
This is consistent with mail residual DF peaks being close to the Cl atoms of the CH2CL4 
solvent molecules
 Fourier peaks appended to .res file

              x       y       z       sof     U      Peak   Distances to nearest atoms (including eq.)

 Q1    1  -0.0148  0.8625  0.4842   1.00000  0.05    1.20   1.65 CL17  2.02 C66  2.26 CL14  2.53 H50B
 Q2    1   0.1022  0.7140  0.4929   1.00000  0.05    1.20   1.56 CL13  1.75 CL17  1.82 C65  2.18 C66
 Q3    1   0.2555  0.5469  0.5141   1.00000  0.05    1.18   1.44 CL4  1.78 CL2  2.06 C62  2.12 C61
 Q4    1   0.1849  0.9709  0.5927   1.00000  0.05    1.16   1.31 CL14  1.63 H66  1.79 C66  2.51 C45
 Q5    1   0.5733  1.1693  0.9095   1.00000  0.05    1.04   1.13 C21  1.35 C26  1.48 C22  1.76 C25
 Q6    1   0.4684  0.4936  0.5570   1.00000  0.05    1.03   1.94 CL4  2.23 C62  2.29 CL3  2.94 H62
 Q7    1   0.3402  0.9394  0.7748   1.00000  0.05    1.03   1.16 C41  1.33 C46  1.52 C42  1.72 C45
 Q8    1   0.3392  0.3925  0.6441   1.00000  0.05    0.95   1.25 CL3  2.06 H61  2.26 C62  2.34 C61
 Q9    1   0.6402  0.5110  0.7656   1.00000  0.05    0.89   1.48 CL8  2.22 CL5  2.29 C64  2.33 H11B

;
_vrf_PLAT220_SF6@4               
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        6.7 Ratio 
RESPONSE: 
moddeling of the disordered solvent molecules is poor
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C98 H132 N6 O10, F6 S, 6(C2 H2 Cl4)'
_chemical_formula_sum            'C55 H72 Cl12 F3 N3 O5 S0.50'
_chemical_formula_weight         1353.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.8587(4)
_cell_length_b                   16.6708(5)
_cell_length_c                   16.8553(6)
_cell_angle_alpha                109.455(3)
_cell_angle_beta                 102.536(3)
_cell_angle_gamma                102.194(3)
_cell_volume                     3410.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.1(4)
_cell_measurement_reflns_used    13336
_cell_measurement_theta_min      2.9360
_cell_measurement_theta_max      66.9340

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             1404
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.7314
_exptl_crystal_size_mid          0.2505
_exptl_crystal_size_min          0.0931
_exptl_absorpt_coefficient_mu    5.037
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.36808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_reflns_number            40500
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.9542
_diffrn_reflns_theta_max         67.4065
_diffrn_measured_fraction_theta_max 0.9653
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_full 0.9711
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11834
_reflns_number_gt                8298
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11834
_refine_ls_number_parameters     676
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2377
_refine_ls_R_factor_gt           0.2093
_refine_ls_wR_factor_ref         0.5778
_refine_ls_wR_factor_gt          0.5586
_refine_ls_goodness_of_fit_ref   2.390
_refine_ls_restrained_S_all      2.390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3753(5) 0.7148(4) 0.8308(5) 0.0547(16) Uani 1 1 d . . . . .
C2 C 0.4436(5) 0.6999(4) 0.8940(5) 0.0568(16) Uani 1 1 d . . . . .
C3 C 0.5486(6) 0.7114(5) 0.8929(6) 0.0665(19) Uani 1 1 d . . . . .
H3 H 0.5952 0.7013 0.9346 0.080 Uiso 1 1 calc R U . . .
C4 C 0.5824(7) 0.7374(6) 0.8302(7) 0.080(2) Uani 1 1 d . . . . .
C5 C 0.5105(8) 0.7502(6) 0.7687(7) 0.076(2) Uani 1 1 d . . . . .
H5 H 0.5328 0.7675 0.7270 0.092 Uiso 1 1 calc R U . . .
C6 C 0.4079(6) 0.7390(5) 0.7647(6) 0.0629(18) Uani 1 1 d . . . . .
C7 C 0.3294(8) 0.7514(5) 0.6929(6) 0.074(2) Uani 1 1 d . . . . .
H7A H 0.3552 0.7431 0.6426 0.089 Uiso 1 1 calc R U . . .
H7B H 0.2646 0.7037 0.6733 0.089 Uiso 1 1 calc R U . . .
C8 C 0.6959(7) 0.7589(7) 0.8334(8) 0.089(3) Uani 1 1 d . . . . .
C9 C 0.7623(8) 0.7398(10) 0.9076(10) 0.115(4) Uani 1 1 d . . . . .
H9A H 0.8333 0.7539 0.9081 0.173 Uiso 1 1 calc R U . . .
H9B H 0.7582 0.7760 0.9638 0.173 Uiso 1 1 calc R U . . .
H9C H 0.7365 0.6778 0.8969 0.173 Uiso 1 1 calc R U . . .
C10 C 0.7413(9) 0.8596(10) 0.8481(12) 0.123(4) Uani 1 1 d . . . . .
H10A H 0.8128 0.8718 0.8499 0.185 Uiso 1 1 calc R U . . .
H10B H 0.7024 0.8703 0.8003 0.185 Uiso 1 1 calc R U . . .
H10C H 0.7365 0.8979 0.9030 0.185 Uiso 1 1 calc R U . . .
C11 C 0.7053(11) 0.6986(11) 0.7427(9) 0.115(4) Uani 1 1 d . . . . .
H11A H 0.7770 0.7124 0.7449 0.173 Uiso 1 1 calc R U . . .
H11B H 0.6787 0.6368 0.7323 0.173 Uiso 1 1 calc R U . . .
H11C H 0.6660 0.7101 0.6955 0.173 Uiso 1 1 calc R U . . .
C13 C 0.2018(7) 0.6285(6) 0.7926(8) 0.083(3) Uani 1 1 d . . . . .
C14 C 0.0170(8) 0.5699(9) 0.7866(12) 0.115(4) Uani 1 1 d . . . . .
C15 C 0.0233(10) 0.4936(10) 0.797(2) 0.254(18) Uani 1 1 d . . . . .
H15A H 0.0427 0.5051 0.8591 0.382 Uiso 1 1 calc R U . . .
H15B H -0.0430 0.4482 0.7672 0.382 Uiso 1 1 calc R U . . .
H15C H 0.0746 0.4736 0.7728 0.382 Uiso 1 1 calc R U . . .
C17 C -0.0564(10) 0.6161(12) 0.813(3) 0.242(17) Uani 1 1 d . . . . .
H17A H -0.0471 0.6682 0.7994 0.363 Uiso 1 1 calc R U . . .
H17B H -0.1261 0.5768 0.7817 0.363 Uiso 1 1 calc R U . . .
H17C H -0.0443 0.6338 0.8756 0.363 Uiso 1 1 calc R U . . .
C16 C -0.0121(18) 0.5423(17) 0.6926(18) 0.172(8) Uani 1 1 d . . . . .
H16A H -0.0187 0.5921 0.6779 0.258 Uiso 1 1 calc R U . . .
H16B H 0.0402 0.5208 0.6712 0.258 Uiso 1 1 calc R U . . .
H16C H -0.0773 0.4954 0.6656 0.258 Uiso 1 1 calc R U . . .
C21 C 0.5144(5) 1.2008(4) 0.8855(5) 0.0541(16) Uani 1 1 d . . . . .
C22 C 0.5256(7) 1.1347(6) 0.8122(7) 0.072(2) Uani 1 1 d . . . . .
C23 C 0.6246(9) 1.1236(8) 0.8159(9) 0.092(3) Uani 1 1 d . . . . .
H23 H 0.6317 1.0789 0.7689 0.111 Uiso 1 1 calc R U . . .
C24 C 0.7093(8) 1.1769(7) 0.8866(9) 0.089(3) Uani 1 1 d . . . . .
C25 C 0.7001(7) 1.2452(7) 0.9602(8) 0.085(3) Uani 1 1 d . . . . .
H25 H 0.7590 1.2820 1.0079 0.102 Uiso 1 1 calc R U . . .
C26 C 0.3950(6) 0.7426(5) 1.0388(6) 0.0641(19) Uani 1 1 d . . . . .
C27 C 0.4070(5) 0.6710(5) 0.9617(5) 0.0598(17) Uani 1 1 d . . . . .
H27A H 0.3405 0.6246 0.9311 0.072 Uiso 1 1 calc R U . . .
H27B H 0.4557 0.6443 0.9853 0.072 Uiso 1 1 calc R U . . .
C28 C 0.8206(9) 1.1668(10) 0.8942(11) 0.118(4) Uani 1 1 d . . . . .
C29 C 0.8154(16) 1.0948(16) 0.7968(16) 0.174(8) Uani 1 1 d . . . . .
H29A H 0.7865 1.1133 0.7512 0.261 Uiso 1 1 calc R U . . .
H29B H 0.8841 1.0929 0.7969 0.261 Uiso 1 1 calc R U . . .
H29C H 0.7724 1.0364 0.7857 0.261 Uiso 1 1 calc R U . . .
C30 C 0.8957(11) 1.2585(15) 0.9051(16) 0.178(9) Uani 1 1 d . . . . .
H30A H 0.8699 1.2721 0.8551 0.267 Uiso 1 1 calc R U . . .
H30B H 0.8986 1.3053 0.9583 0.267 Uiso 1 1 calc R U . . .
H30C H 0.9641 1.2534 0.9084 0.267 Uiso 1 1 calc R U . . .
C31 C 0.8641(10) 1.1484(13) 0.9737(14) 0.144(6) Uani 1 1 d . . . . .
H31A H 0.9320 1.1427 0.9757 0.215 Uiso 1 1 calc R U . . .
H31B H 0.8688 1.1968 1.0265 0.215 Uiso 1 1 calc R U . . .
H31C H 0.8192 1.0938 0.9698 0.215 Uiso 1 1 calc R U . . .
C32 C 0.3846(7) 1.2609(5) 0.8441(6) 0.067(2) Uani 1 1 d . . . . .
C33 C 0.2345(7) 1.3126(6) 0.8136(7) 0.084(3) Uani 1 1 d . . . . .
C34 C 0.2026(10) 1.2694(10) 0.7140(9) 0.120(4) Uani 1 1 d . . . . .
H34A H 0.1624 1.3007 0.6894 0.180 Uiso 1 1 calc R U . . .
H34B H 0.2635 1.2719 0.6954 0.180 Uiso 1 1 calc R U . . .
H34C H 0.1617 1.2081 0.6939 0.180 Uiso 1 1 calc R U . . .
C35 C 0.1376(10) 1.3003(10) 0.8448(11) 0.112(4) Uani 1 1 d . . . . .
H35A H 0.0924 1.3290 0.8215 0.168 Uiso 1 1 calc R U . . .
H35B H 0.1016 1.2377 0.8239 0.168 Uiso 1 1 calc R U . . .
H35C H 0.1586 1.3266 0.9083 0.168 Uiso 1 1 calc R U . . .
C36 C 0.2913(9) 1.4119(7) 0.8501(10) 0.106(4) Uani 1 1 d . . . . .
H36A H 0.2493 1.4405 0.8231 0.159 Uiso 1 1 calc R U . . .
H36B H 0.3046 1.4372 0.9130 0.159 Uiso 1 1 calc R U . . .
H36C H 0.3560 1.4207 0.8373 0.159 Uiso 1 1 calc R U . . .
C41 C 0.3748(6) 0.9146(5) 0.7178(5) 0.0581(16) Uani 1 1 d . . . . .
C42 C 0.3047(6) 0.8402(5) 0.7173(5) 0.0618(18) Uani 1 1 d . . . . .
C43 C 0.2122(6) 0.8475(6) 0.7357(6) 0.073(2) Uani 1 1 d . . . . .
H43 H 0.1656 0.7980 0.7352 0.088 Uiso 1 1 calc R U . . .
C44 C 0.1889(7) 0.9297(6) 0.7551(7) 0.078(2) Uani 1 1 d . . . . .
C45 C 0.2601(6) 1.0006(6) 0.7529(6) 0.072(2) Uani 1 1 d . . . . .
H45 H 0.2451 1.0544 0.7640 0.087 Uiso 1 1 calc R U . . .
C46 C 0.3502(6) 0.9961(5) 0.7354(5) 0.0659(19) Uani 1 1 d . . . . .
C47 C 0.4299(6) 1.0763(5) 0.7324(6) 0.0647(18) Uani 1 1 d . . . . .
H47A H 0.4542 1.0522 0.6823 0.078 Uiso 1 1 calc R U . . .
H47B H 0.3918 1.1154 0.7194 0.078 Uiso 1 1 calc R U . . .
C48 C 0.0909(7) 0.9379(8) 0.7785(9) 0.095(3) Uani 1 1 d . . . . .
C49 C 0.0139(12) 0.8504(14) 0.7543(17) 0.171(8) Uani 1 1 d . . . . .
H49A H 0.0007 0.8137 0.6931 0.256 Uiso 1 1 calc R U . . .
H49B H 0.0405 0.8212 0.7906 0.256 Uiso 1 1 calc R U . . .
H49C H -0.0497 0.8594 0.7635 0.256 Uiso 1 1 calc R U . . .
C50 C 0.0256(13) 0.9771(14) 0.7085(13) 0.143(5) Uani 1 1 d . . . . .
H50A H 0.0680 1.0349 0.7175 0.214 Uiso 1 1 calc R U . . .
H50B H 0.0104 0.9365 0.6483 0.214 Uiso 1 1 calc R U . . .
H50C H -0.0381 0.9818 0.7204 0.214 Uiso 1 1 calc R U . . .
C51 C 0.1170(16) 1.000(3) 0.8725(17) 0.29(2) Uani 1 1 d . . . . .
H51A H 0.1671 1.0553 0.8836 0.439 Uiso 1 1 calc R U . . .
H51B H 0.0552 1.0118 0.8837 0.439 Uiso 1 1 calc R U . . .
H51C H 0.1454 0.9737 0.9108 0.439 Uiso 1 1 calc R U . . .
C52 C 0.4762(8) 0.8883(7) 0.6206(7) 0.083(2) Uani 1 1 d . . . . .
C53 C 0.6058(10) 0.8586(9) 0.5460(8) 0.101(3) Uani 1 1 d . . . . .
C54 C 0.5461(13) 0.7583(12) 0.4913(11) 0.148(7) Uani 1 1 d . . . . .
H54A H 0.5680 0.7372 0.4400 0.222 Uiso 1 1 calc R U . . .
H54B H 0.5602 0.7251 0.5269 0.222 Uiso 1 1 calc R U . . .
H54C H 0.4728 0.7503 0.4731 0.222 Uiso 1 1 calc R U . . .
C55 C 0.7140(10) 0.8684(10) 0.5797(10) 0.111(4) Uani 1 1 d . . . . .
H55A H 0.7418 0.8516 0.5313 0.167 Uiso 1 1 calc R U . . .
H55B H 0.7508 0.9296 0.6188 0.167 Uiso 1 1 calc R U . . .
H55C H 0.7218 0.8307 0.6114 0.167 Uiso 1 1 calc R U . . .
C56 C 0.5875(15) 0.917(2) 0.4945(14) 0.185(11) Uani 1 1 d . . . . .
H56A H 0.6122 0.9001 0.4443 0.277 Uiso 1 1 calc R U . . .
H56B H 0.5145 0.9098 0.4747 0.277 Uiso 1 1 calc R U . . .
H56C H 0.6242 0.9789 0.5324 0.277 Uiso 1 1 calc R U . . .
C61 C 0.2280(17) 0.4465(11) 0.5642(14) 0.147(6) Uani 1 1 d . . . . .
H61 H 0.2081 0.4290 0.6098 0.176 Uiso 1 1 calc R U . . .
C62 C 0.3357(16) 0.5109(10) 0.6080(12) 0.142(6) Uani 1 1 d . . . . .
H62 H 0.3311 0.5636 0.6535 0.170 Uiso 1 1 calc R U . . .
C63 C 0.6533(11) 0.4104(9) 0.8479(10) 0.117(4) Uani 1 1 d . . . . .
H63 H 0.6243 0.3645 0.8679 0.140 Uiso 1 1 calc R U . . .
C64 C 0.6308(13) 0.3690(11) 0.7550(12) 0.135(5) Uani 1 1 d . . . . .
H64 H 0.5550 0.3462 0.7294 0.162 Uiso 1 1 calc R U . . .
C65 C 0.1656(18) 0.797(2) 0.4571(19) 0.31(3) Uani 1 1 d D . . . .
H65 H 0.2349 0.8361 0.4686 0.369 Uiso 1 1 calc R U . . .
C66 C 0.1312(16) 0.855(2) 0.5183(14) 0.235(19) Uani 1 1 d D . . . .
H66 H 0.1750 0.8674 0.5777 0.282 Uiso 1 1 calc R U . . .
N1 N 0.1149(5) 0.6388(6) 0.8093(9) 0.113(4) Uani 1 1 d . . . . .
N3 N 0.5686(6) 0.8846(6) 0.6211(6) 0.081(2) Uani 1 1 d . . . . .
N2 N 0.2970(5) 1.2656(5) 0.8538(6) 0.0763(19) Uani 1 1 d . . . . .
O3 O 0.4215(4) 1.2107(3) 0.8882(4) 0.0618(12) Uani 1 1 d . . . . .
O4 O 0.4344(5) 1.2907(4) 0.8025(5) 0.0785(16) Uani 1 1 d . . . . .
O5 O 0.4676(4) 0.9096(4) 0.7057(4) 0.0729(15) Uani 1 1 d . . . . .
O2 O 0.2182(5) 0.5636(4) 0.7486(6) 0.104(2) Uani 1 1 d . . . . .
O6 O 0.4040(5) 0.8759(6) 0.5614(5) 0.099(2) Uani 1 1 d . . . . .
Cl1 Cl 0.2179(4) 0.3497(3) 0.4801(4) 0.1609(19) Uani 1 1 d . . . . .
Cl2 Cl 0.1368(5) 0.4987(4) 0.5292(4) 0.177(2) Uani 1 1 d . . . . .
Cl3 Cl 0.4105(5) 0.4620(5) 0.6635(5) 0.208(3) Uani 1 1 d . . . . .
Cl4 Cl 0.3599(12) 0.5432(5) 0.5226(6) 0.328(8) Uani 1 1 d . . . . .
Cl5 Cl 0.5930(3) 0.4991(2) 0.8800(3) 0.1414(15) Uani 1 1 d . . . . .
Cl6 Cl 0.7890(3) 0.4596(3) 0.9099(3) 0.1412(14) Uani 1 1 d . . . . .
Cl7 Cl 0.6753(5) 0.2801(4) 0.7249(4) 0.1585(18) Uani 1 1 d . . . . .
Cl8 Cl 0.6764(3) 0.4445(3) 0.7070(3) 0.1348(14) Uani 1 1 d . . . . .
Cl12 Cl 0.1056(4) 0.7801(7) 0.3412(4) 0.229(4) Uani 1 1 d . . . . .
Cl13 Cl 0.1979(8) 0.7025(4) 0.4610(5) 0.233(4) Uani 1 1 d . . . . .
Cl14 Cl 0.1424(6) 0.9572(6) 0.5098(6) 0.213(3) Uani 1 1 d . . . . .
Cl17 Cl 0.0138(7) 0.7751(10) 0.4967(4) 0.383(11) Uani 1 1 d . . . . .
C12 C 0.2777(4) 0.7111(3) 0.8339(4) 0.0416(13) Uani 1 1 d . . . . .
S1 S 0.5000 0.0000 0.0000 0.213 Uiso 1 2 d S . P . .
F1 F 0.5260 0.0328 0.1053 0.437 Uiso 1 1 d . . . . .
F2 F 0.6338 0.0632 0.0218 0.437 Uiso 1 1 d . . . . .
F3 F 0.5540 -0.0876 -0.0040 0.437 Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C12 1.354(9) . ?
C1 C2 1.389(10) . ?
C1 C6 1.432(11) . ?
C2 C3 1.433(11) . ?
C2 C27 1.519(11) . ?
C3 C4 1.399(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(14) . ?
C4 C8 1.522(13) . ?
C5 C6 1.378(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.543(12) . ?
C7 C42 1.532(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.549(19) . ?
C8 C11 1.576(18) . ?
C8 C10 1.576(18) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 O2 1.190(12) . ?
C13 N1 1.327(13) . ?
C13 C12 1.384(10) . ?
C14 C15 1.36(2) . ?
C14 C16 1.43(3) . ?
C14 C17 1.46(3) . ?
C14 N1 1.460(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 O3 1.340(8) . ?
C21 C22 1.420(12) . ?
C21 C26 1.447(12) 2_677 ?
C22 C23 1.413(14) . ?
C22 C47 1.524(13) . ?
C23 C24 1.355(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.428(17) . ?
C24 C28 1.569(13) . ?
C25 C26 1.378(11) 2_677 ?
C25 H25 0.9300 . ?
C26 C25 1.378(11) 2_677 ?
C26 C21 1.447(12) 2_677 ?
C26 C27 1.512(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C31 1.50(2) . ?
C28 C30 1.58(3) . ?
C28 C29 1.66(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 O4 1.231(10) . ?
C32 N2 1.274(11) . ?
C32 O3 1.395(9) . ?
C33 N2 1.485(10) . ?
C33 C34 1.507(19) . ?
C33 C36 1.516(14) . ?
C33 C35 1.544(17) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C41 O5 1.361(9) . ?
C41 C42 1.401(11) . ?
C41 C46 1.421(11) . ?
C42 C43 1.404(12) . ?
C43 C44 1.422(13) . ?
C43 H43 0.9300 . ?
C44 C45 1.389(14) . ?
C44 C48 1.514(13) . ?
C45 C46 1.355(12) . ?
C45 H45 0.9300 . ?
C46 C47 1.567(11) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.48(2) . ?
C48 C51 1.49(3) . ?
C48 C50 1.72(2) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 O6 1.175(12) . ?
C52 N3 1.295(13) . ?
C52 O5 1.396(12) . ?
C53 N3 1.437(13) . ?
C53 C55 1.437(19) . ?
C53 C56 1.53(2) . ?
C53 C54 1.54(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C61 C62 1.50(3) . ?
C61 Cl1 1.711(19) . ?
C61 Cl2 1.785(18) . ?
C61 H61 0.9800 . ?
C62 Cl3 1.75(2) . ?
C62 Cl4 1.77(2) . ?
C62 H62 0.9800 . ?
C63 C64 1.42(2) . ?
C63 Cl6 1.795(15) . ?
C63 Cl5 1.835(17) . ?
C63 H63 0.9800 . ?
C64 Cl7 1.69(2) . ?
C64 Cl8 1.789(12) . ?
C64 H64 0.9800 . ?
C65 C66 1.4099(10) . ?
C65 Cl13 1.74(3) . ?
C65 Cl12 1.85(3) . ?
C65 H65 0.9800 . ?
C66 Cl14 1.73(4) . ?
C66 Cl17 1.75(2) . ?
C66 H66 0.9800 . ?
S1 F1 1.6033 2_655 ?
S1 F1 1.6033 . ?
S1 F3 1.7653 2_655 ?
S1 F3 1.7653 . ?
S1 F2 1.8179 . ?
S1 F2 1.8179 2_655 ?

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
C12 C1 C2 120.0(6) . . ?
C12 C1 C6 118.9(6) . . ?
C2 C1 C6 121.1(6) . . ?
C1 C2 C3 118.4(7) . . ?
C1 C2 C27 120.6(6) . . ?
C3 C2 C27 121.0(7) . . ?
C4 C3 C2 121.2(8) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 117.6(8) . . ?
C5 C4 C8 120.2(9) . . ?
C3 C4 C8 122.0(9) . . ?
C6 C5 C4 124.5(8) . . ?
C6 C5 H5 117.7 . . ?
C4 C5 H5 117.7 . . ?
C5 C6 C1 117.2(7) . . ?
C5 C6 C7 122.7(7) . . ?
C1 C6 C7 120.1(7) . . ?
C42 C7 C6 118.0(7) . . ?
C42 C7 H7A 107.8 . . ?
C6 C7 H7A 107.8 . . ?
C42 C7 H7B 107.8 . . ?
C6 C7 H7B 107.8 . . ?
H7A C7 H7B 107.1 . . ?
C4 C8 C9 111.3(9) . . ?
C4 C8 C11 109.7(10) . . ?
C9 C8 C11 107.7(9) . . ?
C4 C8 C10 110.7(8) . . ?
C9 C8 C10 109.6(11) . . ?
C11 C8 C10 107.7(10) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C13 N1 129.9(8) . . ?
O2 C13 C12 121.8(8) . . ?
N1 C13 C12 108.2(8) . . ?
C15 C14 C16 103(2) . . ?
C15 C14 C17 123.8(18) . . ?
C16 C14 C17 104.5(19) . . ?
C15 C14 N1 116.9(10) . . ?
C16 C14 N1 97.9(14) . . ?
C17 C14 N1 106.8(11) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C21 C22 121.8(7) . . ?
O3 C21 C26 118.7(6) . 2_677 ?
C22 C21 C26 119.4(7) . 2_677 ?
C23 C22 C21 119.1(9) . . ?
C23 C22 C47 121.9(9) . . ?
C21 C22 C47 118.9(7) . . ?
C24 C23 C22 121.3(10) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 120.4(8) . . ?
C23 C24 C28 123.2(12) . . ?
C25 C24 C28 116.4(11) . . ?
C26 C25 C24 120.8(10) 2_677 . ?
C26 C25 H25 119.6 2_677 . ?
C24 C25 H25 119.6 . . ?
C25 C26 C21 118.9(8) 2_677 2_677 ?
C25 C26 C27 121.9(8) 2_677 . ?
C21 C26 C27 119.2(6) 2_677 . ?
C26 C27 C2 117.0(6) . . ?
C26 C27 H27A 108.1 . . ?
C2 C27 H27A 108.1 . . ?
C26 C27 H27B 108.1 . . ?
C2 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C31 C28 C24 112.3(10) . . ?
C31 C28 C30 107.5(15) . . ?
C24 C28 C30 108.0(10) . . ?
C31 C28 C29 116.9(14) . . ?
C24 C28 C29 107.5(13) . . ?
C30 C28 C29 104.1(14) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O4 C32 N2 130.3(8) . . ?
O4 C32 O3 120.4(8) . . ?
N2 C32 O3 109.3(7) . . ?
N2 C33 C34 110.8(9) . . ?
N2 C33 C36 111.2(7) . . ?
C34 C33 C36 112.6(10) . . ?
N2 C33 C35 103.9(8) . . ?
C34 C33 C35 109.9(10) . . ?
C36 C33 C35 108.1(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C41 C42 119.8(6) . . ?
O5 C41 C46 120.6(7) . . ?
C42 C41 C46 119.6(7) . . ?
C41 C42 C43 119.6(7) . . ?
C41 C42 C7 118.9(7) . . ?
C43 C42 C7 121.5(7) . . ?
C42 C43 C44 120.7(8) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C45 C44 C43 117.1(8) . . ?
C45 C44 C48 122.6(8) . . ?
C43 C44 C48 120.3(8) . . ?
C46 C45 C44 123.8(8) . . ?
C46 C45 H45 118.1 . . ?
C44 C45 H45 118.1 . . ?
C45 C46 C41 119.1(7) . . ?
C45 C46 C47 123.6(7) . . ?
C41 C46 C47 117.3(6) . . ?
C22 C47 C46 120.3(7) . . ?
C22 C47 H47A 107.2 . . ?
C46 C47 H47A 107.2 . . ?
C22 C47 H47B 107.2 . . ?
C46 C47 H47B 107.2 . . ?
H47A C47 H47B 106.9 . . ?
C49 C48 C51 113.9(19) . . ?
C49 C48 C44 113.2(10) . . ?
C51 C48 C44 110.5(10) . . ?
C49 C48 C50 100.8(13) . . ?
C51 C48 C50 110.7(18) . . ?
C44 C48 C50 107.1(10) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O6 C52 N3 129.9(10) . . ?
O6 C52 O5 119.7(9) . . ?
N3 C52 O5 110.4(8) . . ?
N3 C53 C55 107.0(11) . . ?
N3 C53 C56 109.2(11) . . ?
C55 C53 C56 112.4(12) . . ?
N3 C53 C54 105.9(11) . . ?
C55 C53 C54 108.7(11) . . ?
C56 C53 C54 113.2(16) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C62 C61 Cl1 114.5(14) . . ?
C62 C61 Cl2 111.6(12) . . ?
Cl1 C61 Cl2 111.3(11) . . ?
C62 C61 H61 106.3 . . ?
Cl1 C61 H61 106.3 . . ?
Cl2 C61 H61 106.3 . . ?
C61 C62 Cl3 107.4(12) . . ?
C61 C62 Cl4 102.3(14) . . ?
Cl3 C62 Cl4 125.7(13) . . ?
C61 C62 H62 106.7 . . ?
Cl3 C62 H62 106.7 . . ?
Cl4 C62 H62 106.7 . . ?
C64 C63 Cl6 115.2(11) . . ?
C64 C63 Cl5 112.2(12) . . ?
Cl6 C63 Cl5 106.4(7) . . ?
C64 C63 H63 107.6 . . ?
Cl6 C63 H63 107.6 . . ?
Cl5 C63 H63 107.6 . . ?
C63 C64 Cl7 112.1(12) . . ?
C63 C64 Cl8 113.4(11) . . ?
Cl7 C64 Cl8 110.2(9) . . ?
C63 C64 H64 106.9 . . ?
Cl7 C64 H64 106.9 . . ?
Cl8 C64 H64 106.9 . . ?
C66 C65 Cl13 128(3) . . ?
C66 C65 Cl12 113.2(18) . . ?
Cl13 C65 Cl12 110.7(16) . . ?
C66 C65 H65 99.5 . . ?
Cl13 C65 H65 99.5 . . ?
Cl12 C65 H65 99.5 . . ?
C65 C66 Cl14 114(2) . . ?
C65 C66 Cl17 95(2) . . ?
Cl14 C66 Cl17 125.0(19) . . ?
C65 C66 H66 107.2 . . ?
Cl14 C66 H66 107.2 . . ?
Cl17 C66 H66 107.2 . . ?
C13 N1 C14 128.3(10) . . ?
C52 N3 C53 127.3(10) . . ?
C32 N2 C33 123.5(8) . . ?
C21 O3 C32 116.6(5) . . ?
C41 O5 C52 118.8(6) . . ?
C1 C12 C13 118.1(6) . . ?
F1 S1 F1 180.0 2_655 . ?
F1 S1 F3 90.7 2_655 2_655 ?
F1 S1 F3 89.3 . 2_655 ?
F1 S1 F3 89.3 2_655 . ?
F1 S1 F3 90.7 . . ?
F3 S1 F3 180.0 2_655 . ?
F1 S1 F2 93.3 2_655 . ?
F1 S1 F2 86.7 . . ?
F3 S1 F2 97.1 2_655 . ?
F3 S1 F2 82.9 . . ?
F1 S1 F2 86.7 2_655 2_655 ?
F1 S1 F2 93.3 . 2_655 ?
F3 S1 F2 82.9 2_655 2_655 ?
F3 S1 F2 97.1 . 2_655 ?
F2 S1 F2 180.0 . 2_655 ?

_refine_diff_density_max         1.297
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.161



####################################################################### 
# 
# 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_CO2_4
_database_code_depnum_ccdc_archive 'CCDC 1542197'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_CO2@4               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.887 Note  
RESPONSE: weakly/poorly diffracting crystal 
(best we could obtain from numerous crystallization efforts)
;
_vrf_PLAT082_CO2@4               
;
PROBLEM: High R1 Value ..................................       0.21 Report
RESPONSE: poor quality data despite many efforts to grow better crystals 
and collect better data. Model contains also a lot of (disordered) solvent.
;
_vrf_PLAT084_CO2@4               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.57 Report
RESPONSE: poor quality data despite many efforts to grow better crystals 
and collect better data. Model contains also a lot of (disordered) solvent.
;
_vrf_PLAT934_CO2@4               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         26 Check 
RESPONSE: no obvious reason (systematic absents) to omit reflections
list of mail outliers follows
 Most Disagreeable Reflections (* if suppressed or used for Rfree).
 Error/esd is calculated as sqrt(wD^2/<wD^2>) where w is given by the weight
 formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections.

     h   k   l          Fo^2          Fc^2    Error/esd  Fc/Fc(max)  Resolution(A)

     4  -2   2       2159.47          0.21       7.37       0.002       2.92
     3  -1   1       5082.10        111.12       6.96       0.045       4.10
     0   1   2       2413.90         82.25       6.65       0.038       5.85
    -1  -6   1       1036.86          8.62       6.64       0.012       2.45
    -2   4   2        386.41          0.59       6.57       0.003       3.11
     2  -1   2       3868.17        141.08       6.50       0.050       4.70
    -2  -2   5        747.63          8.79       6.47       0.013       3.20
    -4  -1   1        712.28         27.76       6.38       0.022       3.14
    -3  -3   2       1019.74          6.08       6.32       0.010       3.16
    -2   0   4        719.36          4.37       6.21       0.009       3.80

;
_vrf_PLAT097_shelx               
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.72 eA-3  
RESPONSE: The main cause to this error is limitation/inadequate modelling of disordered solvent atoms.
This is consistent with mail residual DF peaks being close to the Cl atoms of the CH2CL4 
solvent molecules
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96H144N6O12,4(C2H2Cl4),C O2,8(H2O)'
_chemical_formula_sum            'C105 H162 Cl16 N6 O22'
_chemical_formula_weight         2428


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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.8689(9)
_cell_length_b                   16.6934(13)
_cell_length_c                   16.8118(12)
_cell_angle_alpha                109.746(7)
_cell_angle_beta                 102.230(6)
_cell_angle_gamma                102.209(6)
_cell_volume                     3406.5(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    149.95(10)
_cell_measurement_reflns_used    6938
_cell_measurement_theta_min      2.9520
_cell_measurement_theta_max      24.3440

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.4000
_exptl_crystal_size_min          0.0500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.18
_exptl_crystal_F_000             1898
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.38
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.87785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.95(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20920
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.973
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.719
_diffrn_measured_fraction_theta_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.719
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.719
_diffrn_reflns_point_group_measured_fraction_full 0.887
_reflns_number_total             12207
_reflns_number_gt                7139
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12207
_refine_ls_number_parameters     673
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.2631
_refine_ls_R_factor_gt           0.2137
_refine_ls_wR_factor_ref         0.5728
_refine_ls_wR_factor_gt          0.5386
_refine_ls_goodness_of_fit_ref   2.065
_refine_ls_restrained_S_all      2.055
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0139(6) 0.2013(5) 0.8867(5) 0.0444(17) Uani 1 1 d . . . . .
C2 C 0.1048(6) 0.2574(6) 0.9588(6) 0.055(2) Uani 1 1 d . . . . .
C3 C 0.1998(6) 0.2451(7) 0.9589(7) 0.066(2) Uani 1 1 d . . . . .
H3 H 0.2583 0.2830 1.0066 0.079 Uiso 1 1 calc R U . . .
C4 C 0.2099(8) 0.1754(7) 0.8873(8) 0.075(3) Uani 1 1 d . . . . .
C5 C 0.1197(8) 0.1219(7) 0.8138(7) 0.068(2) Uani 1 1 d . . . . .
H5 H 0.1258 0.0782 0.7649 0.082 Uiso 1 1 calc R U . . .
C6 C 0.0244(7) 0.1323(6) 0.8122(6) 0.058(2) Uani 1 1 d . . . . .
C7 C 0.3146(8) 0.1625(9) 0.8862(10) 0.094(4) Uani 1 1 d . . . . .
C8 C 0.3127(12) 0.0938(13) 0.7991(13) 0.143(7) Uani 1 1 d . . . . .
H8A H 0.3811 0.0889 0.8028 0.214 Uiso 1 1 calc R U . . .
H8B H 0.2659 0.0368 0.7873 0.214 Uiso 1 1 calc R U . . .
H8C H 0.2899 0.1122 0.7519 0.214 Uiso 1 1 calc R U . . .
C9 C 0.3525(13) 0.1436(13) 0.9700(15) 0.145(7) Uani 1 1 d . . . . .
H9A H 0.3508 0.1906 1.0214 0.218 Uiso 1 1 calc R U . . .
H9B H 0.3079 0.0875 0.9630 0.218 Uiso 1 1 calc R U . . .
H9C H 0.4221 0.1409 0.9774 0.218 Uiso 1 1 calc R U . . .
C10 C 0.3962(11) 0.2580(13) 0.913(2) 0.189(11) Uani 1 1 d . . . . .
H10A H 0.3948 0.2992 0.9687 0.283 Uiso 1 1 calc R U . . .
H10B H 0.4645 0.2522 0.9195 0.283 Uiso 1 1 calc R U . . .
H10C H 0.3783 0.2799 0.8681 0.283 Uiso 1 1 calc R U . . .
C11 C -0.0694(7) 0.0757(5) 0.7333(6) 0.055(2) Uani 1 1 d . . . . .
H11A H -0.0451 0.0531 0.6826 0.066 Uiso 1 1 calc R U . . .
H11B H -0.1079 0.1150 0.7220 0.066 Uiso 1 1 calc R U . . .
C12 C -0.1165(7) 0.2604(5) 0.8412(5) 0.054(2) Uani 1 1 d . . . . .
C13 C -0.2673(8) 0.3114(7) 0.8124(8) 0.079(3) Uani 1 1 d . . . . .
C14 C -0.2989(10) 0.2672(10) 0.7119(8) 0.102(4) Uani 1 1 d . . . . .
H14A H -0.3398 0.2977 0.6870 0.153 Uiso 1 1 calc R U . . .
H14B H -0.2380 0.2702 0.6931 0.153 Uiso 1 1 calc R U . . .
H14C H -0.3390 0.2057 0.6920 0.153 Uiso 1 1 calc R U . . .
C15 C -0.3665(10) 0.2950(10) 0.8401(11) 0.104(4) Uani 1 1 d . . . . .
H15A H -0.4113 0.3244 0.8179 0.156 Uiso 1 1 calc R U . . .
H15B H -0.4017 0.2319 0.8159 0.156 Uiso 1 1 calc R U . . .
H15C H -0.3482 0.3185 0.9037 0.156 Uiso 1 1 calc R U . . .
C16 C -0.2086(8) 0.4084(6) 0.8442(9) 0.090(4) Uani 1 1 d . . . . .
H16A H -0.2513 0.4374 0.8189 0.135 Uiso 1 1 calc R U . . .
H16B H -0.1897 0.4360 0.9078 0.135 Uiso 1 1 calc R U . . .
H16C H -0.1470 0.4140 0.8264 0.135 Uiso 1 1 calc R U . . .
C21 C -0.1235(6) -0.0850(5) 0.7181(4) 0.0444(17) Uani 1 1 d . . . . .
C22 C -0.1494(6) -0.0071(6) 0.7343(6) 0.059(2) Uani 1 1 d . . . . .
C23 C -0.2397(7) -0.0010(7) 0.7543(6) 0.071(3) Uani 1 1 d . . . . .
H23 H -0.2535 0.0534 0.7671 0.086 Uiso 1 1 calc R U . . .
C24 C -0.3093(8) -0.0700(7) 0.7560(7) 0.072(3) Uani 1 1 d . . . . .
C25 C -0.2870(7) -0.1530(7) 0.7370(6) 0.066(2) Uani 1 1 d . . . . .
H25 H -0.3342 -0.2012 0.7377 0.079 Uiso 1 1 calc R U . . .
C26 C -0.1976(7) -0.1638(8) 0.7176(6) 0.070(3) Uani 1 1 d . . . . .
C27 C -0.4099(9) -0.0640(9) 0.7807(10) 0.096(4) Uani 1 1 d . . . . .
C28 C -0.3789(13) 0.0036(17) 0.8759(13) 0.164(8) Uani 1 1 d . . . . .
H28A H -0.3274 0.0566 0.8838 0.247 Uiso 1 1 calc R U . . .
H28B H -0.4386 0.0186 0.8885 0.247 Uiso 1 1 calc R U . . .
H28C H -0.3508 -0.0217 0.9155 0.247 Uiso 1 1 calc R U . . .
C29 C -0.4781(13) -0.0191(13) 0.7125(13) 0.146(7) Uani 1 1 d . . . . .
H29A H -0.4992 -0.0601 0.6514 0.219 Uiso 1 1 calc R U . . .
H29B H -0.5382 -0.0104 0.7294 0.219 Uiso 1 1 calc R U . . .
H29C H -0.4335 0.0371 0.7199 0.219 Uiso 1 1 calc R U . . .
C30 C -0.4907(15) -0.1517(15) 0.757(2) 0.202(12) Uani 1 1 d . . . . .
H30A H -0.5045 -0.1893 0.6954 0.304 Uiso 1 1 calc R U . . .
H30B H -0.4655 -0.1810 0.7933 0.304 Uiso 1 1 calc R U . . .
H30C H -0.5533 -0.1408 0.7663 0.304 Uiso 1 1 calc R U . . .
C31 C -0.1712(7) -0.2481(6) 0.6965(6) 0.061(2) Uani 1 1 d . . . . .
H31A H -0.1457 -0.2566 0.6457 0.073 Uiso 1 1 calc R U . . .
H31B H -0.2356 -0.2960 0.6769 0.073 Uiso 1 1 calc R U . . .
C32 C -0.0243(9) -0.1143(7) 0.6206(6) 0.070(2) Uani 1 1 d . . . . .
C33 C 0.1015(10) -0.1439(10) 0.5434(8) 0.097(4) Uani 1 1 d . . . . .
C34 C 0.0892(16) -0.0886(17) 0.4935(13) 0.160(9) Uani 1 1 d . . . . .
H34A H 0.1126 -0.1091 0.4426 0.240 Uiso 1 1 calc R U . . .
H34B H 0.0174 -0.0925 0.4744 0.240 Uiso 1 1 calc R U . . .
H34C H 0.1295 -0.0275 0.5307 0.240 Uiso 1 1 calc R U . . .
C35 C 0.0469(11) -0.2459(8) 0.4882(9) 0.101(4) Uani 1 1 d . . . . .
H35A H 0.0694 -0.2651 0.4367 0.151 Uiso 1 1 calc R U . . .
H35B H 0.0644 -0.2781 0.5240 0.151 Uiso 1 1 calc R U . . .
H35C H -0.0269 -0.2573 0.4701 0.151 Uiso 1 1 calc R U . . .
C36 C 0.2204(9) -0.1310(10) 0.5808(10) 0.098(4) Uani 1 1 d . . . . .
H36A H 0.2483 -0.1489 0.5324 0.148 Uiso 1 1 calc R U . . .
H36B H 0.2562 -0.0692 0.6188 0.148 Uiso 1 1 calc R U . . .
H36C H 0.2292 -0.1671 0.6142 0.148 Uiso 1 1 calc R U . . .
C41 C -0.1271(5) -0.2869(4) 0.8298(5) 0.0398(16) Uani 1 1 d . . . . .
C42 C -0.0923(6) -0.2625(5) 0.7668(5) 0.0491(18) Uani 1 1 d . . . . .
C43 C 0.0096(8) -0.2502(6) 0.7692(7) 0.065(2) Uani 1 1 d . . . . .
H43 H 0.0309 -0.2319 0.7275 0.078 Uiso 1 1 calc R U . . .
C44 C 0.0833(7) -0.2636(6) 0.8305(6) 0.063(2) Uani 1 1 d . . . . .
C45 C -0.0553(6) -0.3015(5) 0.8956(5) 0.0493(19) Uani 1 1 d . . . . .
C46 C 0.0462(7) -0.2904(6) 0.8924(6) 0.055(2) Uani 1 1 d . . . . .
H46 H 0.0921 -0.3013 0.9336 0.066 Uiso 1 1 calc R U . . .
C47 C 0.1950(7) -0.2457(7) 0.8316(7) 0.074(3) Uani 1 1 d . . . . .
C48 C 0.2585(10) -0.2651(10) 0.9030(10) 0.101(4) Uani 1 1 d . . . . .
H48A H 0.3290 -0.2532 0.9022 0.152 Uiso 1 1 calc R U . . .
H48B H 0.2561 -0.2278 0.9599 0.152 Uiso 1 1 calc R U . . .
H48C H 0.2308 -0.3268 0.8927 0.152 Uiso 1 1 calc R U . . .
C49 C 0.2359(10) -0.1423(11) 0.8443(13) 0.124(5) Uani 1 1 d . . . . .
H49A H 0.1928 -0.1335 0.7972 0.186 Uiso 1 1 calc R U . . .
H49B H 0.2328 -0.1037 0.9003 0.186 Uiso 1 1 calc R U . . .
H49C H 0.3062 -0.1284 0.8430 0.186 Uiso 1 1 calc R U . . .
C50 C 0.2061(10) -0.3027(9) 0.7407(8) 0.091(3) Uani 1 1 d . . . . .
H50A H 0.1660 -0.2911 0.6942 0.137 Uiso 1 1 calc R U . . .
H50B H 0.2777 -0.2870 0.7431 0.137 Uiso 1 1 calc R U . . .
H50C H 0.1815 -0.3651 0.7289 0.137 Uiso 1 1 calc R U . . .
C51 C 0.0932(6) 0.3300(5) 1.0374(5) 0.0498(18) Uani 1 1 d . . . . .
H51A H 0.1601 0.3757 1.0685 0.060 Uiso 1 1 calc R U . . .
H51B H 0.0457 0.3577 1.0142 0.060 Uiso 1 1 calc R U . . .
C52 C -0.2980(7) -0.3720(6) 0.7946(7) 0.066(2) Uani 1 1 d . . . . .
C53 C -0.4836(8) -0.4316(8) 0.7877(11) 0.093(4) Uani 1 1 d . . . . .
C54 C -0.5154(18) -0.4491(14) 0.6986(15) 0.164(8) Uani 1 1 d . . . . .
H54A H -0.5175 -0.3948 0.6912 0.246 Uiso 1 1 calc R U . . .
H54B H -0.4676 -0.4725 0.6712 0.246 Uiso 1 1 calc R U . . .
H54C H -0.5833 -0.4922 0.6711 0.246 Uiso 1 1 calc R U . . .
C55 C -0.4750(10) -0.5016(11) 0.814(2) 0.196(13) Uani 1 1 d . . . . .
H55A H -0.4522 -0.4792 0.8773 0.294 Uiso 1 1 calc R U . . .
H55B H -0.5413 -0.5467 0.7907 0.294 Uiso 1 1 calc R U . . .
H55C H -0.4257 -0.5271 0.7908 0.294 Uiso 1 1 calc R U . . .
C56 C -0.5553(12) -0.3829(13) 0.8305(13) 0.133(6) Uani 1 1 d . . . . .
H56A H -0.5600 -0.3352 0.8116 0.199 Uiso 1 1 calc R U . . .
H56B H -0.6232 -0.4247 0.8122 0.199 Uiso 1 1 calc R U . . .
H56C H -0.5271 -0.3589 0.8940 0.199 Uiso 1 1 calc R U . . .
C61 C 0.8713(10) 0.6283(10) 0.2456(9) 0.099(4) Uani 1 1 d . . . . .
H61 H 0.9470 0.6502 0.2706 0.119 Uiso 1 1 calc R U . . .
C62 C 0.8448(10) 0.5885(9) 0.1488(9) 0.102(4) Uani 1 1 d . . . . .
H62 H 0.8733 0.6353 0.1299 0.122 Uiso 1 1 calc R U . . .
C63 C 0.8297(13) 0.5076(10) 0.6007(11) 0.109(4) Uani 1 1 d . . . . .
H63 H 0.8260 0.5616 0.6455 0.131 Uiso 1 1 calc R U . . .
C64 C 0.7276(13) 0.4477(10) 0.5661(10) 0.107(4) Uani 1 1 d . . . . .
H64 H 0.7106 0.4334 0.6144 0.129 Uiso 1 1 calc R U . . .
N1 N -0.2042(6) 0.2634(5) 0.8498(6) 0.067(2) Uani 1 1 d . . . . .
H1 H -0.2291 0.2358 0.8794 0.081 Uiso 1 1 calc R U . . .
N2 N 0.0671(7) -0.1154(6) 0.6209(6) 0.071(2) Uani 1 1 d . . . . .
H2 H 0.1127 -0.0975 0.6718 0.085 Uiso 1 1 calc R U . . .
N3 N -0.3855(5) -0.3616(5) 0.8154(8) 0.096(3) Uani 1 1 d . . . . .
H3A H -0.3826 -0.3084 0.8483 0.115 Uiso 1 1 calc R U . . .
O1 O -0.0781(4) 0.2108(4) 0.8882(4) 0.0527(14) Uani 1 1 d . U . . .
O2 O -0.0674(5) 0.2895(4) 0.8018(5) 0.0703(17) Uani 1 1 d . U . . .
O3 O -0.0315(5) -0.0915(5) 0.7063(4) 0.0679(17) Uani 1 1 d . U . . .
O4 O -0.0971(6) -0.1281(7) 0.5615(5) 0.099(3) Uani 1 1 d . U . . .
O5 O -0.2223(4) -0.2899(3) 0.8368(4) 0.0544(14) Uani 1 1 d . U . . .
O6 O -0.2824(5) -0.4379(5) 0.7517(5) 0.080(2) Uani 1 1 d . U . . .
O10 O 0.5170(7) 0.7715(9) 0.4969(4) 0.197(8) Uani 1 1 d . U . . .
O9 O 0.6045(4) 0.7780(7) 0.3411(4) 0.101(3) Uani 1 1 d . U . . .
O8 O 0.6982(6) 0.7014(4) 0.4602(5) 0.095(3) Uani 1 1 d . U . . .
O11 O 0.6452(7) 0.9557(6) 0.5115(6) 0.107(3) Uani 1 1 d . U . . .
Cl1 Cl 0.7122(3) 0.5398(3) 0.0888(3) 0.1170(13) Uani 1 1 d . U . . .
Cl2 Cl 0.9083(3) 0.5007(2) 0.1163(3) 0.1243(14) Uani 1 1 d . U . . .
Cl3 Cl 0.8251(4) 0.7193(3) 0.2742(3) 0.1367(16) Uani 1 1 d . U . . .
Cl4 Cl 0.8233(3) 0.5551(3) 0.2916(3) 0.1204(14) Uani 1 1 d . U . . .
Cl5 Cl 0.8665(9) 0.5416(4) 0.5232(5) 0.255(5) Uani 1 1 d . U . . .
Cl6 Cl 0.9141(4) 0.4636(4) 0.6640(4) 0.170(2) Uani 1 1 d . U . . .
Cl7 Cl 0.7176(4) 0.3481(3) 0.4816(3) 0.1422(17) Uani 1 1 d . U . . .
Cl8 Cl 0.6378(4) 0.4987(4) 0.5297(3) 0.152(2) Uani 1 1 d . U . . .
C65 C 0.0000 0.0000 1.0000 0.077(4) Uani 1 2 d S U P . .
O7 O 0.027(2) 0.0321(15) 1.0971(13) 0.269(11) Uani 1 1 d . U . . .
H1OO H 0.5514 0.8094 0.5501 0.060 Uiso 1 1 d . . . . .
H10P H 0.4582 0.7449 0.4989 0.060 Uiso 1 1 d . . . . .
H90 H 0.5581 0.7292 0.3023 0.050 Uiso 1 1 d . . . . .
H9P H 0.6529 0.7879 0.3187 0.050 Uiso 1 1 d . . . . .
H8O H 0.7176 0.6548 0.4550 0.050 Uiso 1 1 d . . . . .
H8P H 0.7545 0.7463 0.4858 0.050 Uiso 1 1 d . . . . .
H110 H 0.6507 1.0115 0.5258 0.050 Uiso 1 1 d . . . . .
H11P H 0.7069 0.9534 0.5282 0.050 Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.322(9) . ?
C1 C2 1.422(12) . ?
C1 C6 1.445(12) . ?
C2 C3 1.375(11) . ?
C2 C51 1.528(12) . ?
C3 C4 1.420(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.421(16) . ?
C4 C7 1.515(13) . ?
C5 C6 1.365(13) . ?
C5 H5 0.9300 . ?
C6 C11 1.499(13) . ?
C7 C8 1.52(2) . ?
C7 C9 1.55(2) . ?
C7 C10 1.60(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C22 1.586(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.188(10) . ?
C12 N1 1.264(11) . ?
C12 O1 1.430(9) . ?
C13 N1 1.485(11) . ?
C13 C16 1.498(15) . ?
C13 C14 1.515(18) . ?
C13 C15 1.544(18) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 O3 1.353(10) . ?
C21 C22 1.375(12) . ?
C21 C26 1.485(14) . ?
C22 C23 1.380(13) . ?
C23 C24 1.350(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.429(14) . ?
C24 C27 1.550(15) . ?
C25 C26 1.379(13) . ?
C25 H25 0.9300 . ?
C26 C31 1.475(13) . ?
C27 C28 1.52(2) . ?
C27 C30 1.51(2) . ?
C27 C29 1.79(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C42 1.552(11) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 O4 1.175(11) . ?
C32 N2 1.271(13) . ?
C32 O3 1.392(12) . ?
C33 N2 1.446(13) . ?
C33 C34 1.45(2) . ?
C33 C35 1.557(19) . ?
C33 C36 1.576(17) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C41 O5 1.341(9) . ?
C41 C42 1.395(11) . ?
C41 C45 1.447(10) . ?
C42 C43 1.374(13) . ?
C43 C44 1.402(13) . ?
C43 H43 0.9300 . ?
C44 C46 1.412(13) . ?
C44 C47 1.510(13) . ?
C45 C46 1.394(12) . ?
C45 C51 1.510(12) 2_557 ?
C46 H46 0.9300 . ?
C47 C48 1.502(17) . ?
C47 C50 1.564(16) . ?
C47 C49 1.623(19) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C45 1.510(12) 2_557 ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 O6 1.187(11) . ?
C52 N3 1.361(14) . ?
C52 O5 1.379(10) . ?
C53 C55 1.40(2) . ?
C53 C54 1.38(2) . ?
C53 N3 1.457(13) . ?
C53 C56 1.55(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C61 C62 1.462(19) . ?
C61 Cl3 1.732(15) . ?
C61 Cl4 1.745(13) . ?
C61 H61 0.9800 . ?
C62 Cl1 1.757(13) . ?
C62 Cl2 1.852(16) . ?
C62 H62 0.9800 . ?
C63 C64 1.41(2) . ?
C63 Cl5 1.714(17) . ?
C63 Cl6 1.845(16) . ?
C63 H63 0.9800 . ?
C64 Cl7 1.740(14) . ?
C64 Cl8 1.768(15) . ?
C64 H64 0.9800 . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
N3 H3A 0.8600 . ?
O10 H1OO 0.8585 . ?
O10 H10P 0.8547 . ?
O9 H90 0.8624 . ?
O9 H9P 0.8509 . ?
O8 H8O 0.8596 . ?
O8 H8P 0.8654 . ?
O11 H110 0.8612 . ?
O11 H11P 0.8557 . ?
C65 O7 1.47(2) 2_557 ?
C65 O7 1.47(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
O1 C1 C2 121.1(7) . . ?
O1 C1 C6 120.8(7) . . ?
C2 C1 C6 118.1(7) . . ?
C3 C2 C1 121.2(8) . . ?
C3 C2 C51 120.9(8) . . ?
C1 C2 C51 117.9(6) . . ?
C2 C3 C4 120.9(9) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 117.7(8) . . ?
C5 C4 C7 120.9(10) . . ?
C3 C4 C7 121.3(11) . . ?
C6 C5 C4 122.4(9) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C1 119.6(9) . . ?
C5 C6 C11 121.3(8) . . ?
C1 C6 C11 119.0(7) . . ?
C8 C7 C4 113.7(12) . . ?
C8 C7 C9 115.9(13) . . ?
C4 C7 C9 104.6(10) . . ?
C8 C7 C10 112.4(14) . . ?
C4 C7 C10 108.3(10) . . ?
C9 C7 C10 100.8(15) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C22 120.4(7) . . ?
C6 C11 H11A 107.2 . . ?
C22 C11 H11A 107.2 . . ?
C6 C11 H11B 107.2 . . ?
C22 C11 H11B 107.2 . . ?
H11A C11 H11B 106.9 . . ?
O2 C12 N1 131.1(8) . . ?
O2 C12 O1 120.2(8) . . ?
N1 C12 O1 108.8(7) . . ?
N1 C13 C16 111.5(8) . . ?
N1 C13 C14 108.7(9) . . ?
C16 C13 C14 110.1(10) . . ?
N1 C13 C15 105.0(9) . . ?
C16 C13 C15 113.6(10) . . ?
C14 C13 C15 107.7(10) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C21 C22 122.7(7) . . ?
O3 C21 C26 118.7(7) . . ?
C22 C21 C26 118.6(7) . . ?
C23 C22 C21 120.7(9) . . ?
C23 C22 C11 121.8(8) . . ?
C21 C22 C11 117.5(7) . . ?
C24 C23 C22 123.3(9) . . ?
C24 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C23 C24 C25 117.9(9) . . ?
C23 C24 C27 124.2(9) . . ?
C25 C24 C27 117.9(10) . . ?
C26 C25 C24 122.1(10) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C25 C26 C31 124.4(10) . . ?
C25 C26 C21 117.4(9) . . ?
C31 C26 C21 118.2(8) . . ?
C28 C27 C30 116.3(16) . . ?
C28 C27 C24 107.9(10) . . ?
C30 C27 C24 116.3(11) . . ?
C28 C27 C29 106.8(13) . . ?
C30 C27 C29 100.9(15) . . ?
C24 C27 C29 107.6(11) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 C42 121.3(8) . . ?
C26 C31 H31A 107.0 . . ?
C42 C31 H31A 107.0 . . ?
C26 C31 H31B 107.0 . . ?
C42 C31 H31B 107.0 . . ?
H31A C31 H31B 106.7 . . ?
O4 C32 N2 130.0(10) . . ?
O4 C32 O3 119.9(9) . . ?
N2 C32 O3 110.1(8) . . ?
N2 C33 C34 111.5(12) . . ?
N2 C33 C35 109.2(11) . . ?
C34 C33 C35 114.6(14) . . ?
N2 C33 C36 105.1(10) . . ?
C34 C33 C36 109.0(12) . . ?
C35 C33 C36 107.0(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C41 C42 122.5(6) . . ?
O5 C41 C45 118.2(7) . . ?
C42 C41 C45 119.0(7) . . ?
C43 C42 C41 120.1(7) . . ?
C43 C42 C31 121.9(7) . . ?
C41 C42 C31 118.0(7) . . ?
C42 C43 C44 124.0(8) . . ?
C42 C43 H43 118.0 . . ?
C44 C43 H43 118.0 . . ?
C43 C44 C46 115.2(8) . . ?
C43 C44 C47 121.3(8) . . ?
C46 C44 C47 123.4(8) . . ?
C46 C45 C41 117.8(7) . . ?
C46 C45 C51 123.0(7) . 2_557 ?
C41 C45 C51 119.2(7) . 2_557 ?
C45 C46 C44 123.9(7) . . ?
C45 C46 H46 118.1 . . ?
C44 C46 H46 118.1 . . ?
C48 C47 C44 111.3(9) . . ?
C48 C47 C50 108.4(9) . . ?
C44 C47 C50 112.1(9) . . ?
C48 C47 C49 112.9(11) . . ?
C44 C47 C49 106.4(8) . . ?
C50 C47 C49 105.7(10) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C45 C51 C2 117.2(6) 2_557 . ?
C45 C51 H51A 108.0 2_557 . ?
C2 C51 H51A 108.0 . . ?
C45 C51 H51B 108.0 2_557 . ?
C2 C51 H51B 108.0 . . ?
H51A C51 H51B 107.3 . . ?
O6 C52 N3 129.4(9) . . ?
O6 C52 O5 122.7(9) . . ?
N3 C52 O5 107.9(8) . . ?
C55 C53 C54 119.1(19) . . ?
C55 C53 N3 113.7(10) . . ?
C54 C53 N3 99.6(13) . . ?
C55 C53 C56 111.1(15) . . ?
C54 C53 C56 107.1(14) . . ?
N3 C53 C56 104.8(11) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C62 C61 Cl3 107.7(10) . . ?
C62 C61 Cl4 114.5(10) . . ?
Cl3 C61 Cl4 110.1(8) . . ?
C62 C61 H61 108.1 . . ?
Cl3 C61 H61 108.1 . . ?
Cl4 C61 H61 108.1 . . ?
C61 C62 Cl1 116.6(10) . . ?
C61 C62 Cl2 109.1(10) . . ?
Cl1 C62 Cl2 107.4(7) . . ?
C61 C62 H62 107.9 . . ?
Cl1 C62 H62 107.9 . . ?
Cl2 C62 H62 107.9 . . ?
C64 C63 Cl5 112.0(13) . . ?
C64 C63 Cl6 108.7(10) . . ?
Cl5 C63 Cl6 120.2(10) . . ?
C64 C63 H63 104.9 . . ?
Cl5 C63 H63 104.9 . . ?
Cl6 C63 H63 104.9 . . ?
C63 C64 Cl7 111.7(11) . . ?
C63 C64 Cl8 110.7(11) . . ?
Cl7 C64 Cl8 111.2(8) . . ?
C63 C64 H64 107.7 . . ?
Cl7 C64 H64 107.7 . . ?
Cl8 C64 H64 107.7 . . ?
C12 N1 C13 124.6(9) . . ?
C12 N1 H1 117.7 . . ?
C13 N1 H1 117.7 . . ?
C32 N2 C33 125.9(10) . . ?
C32 N2 H2 117.0 . . ?
C33 N2 H2 117.0 . . ?
C52 N3 C53 126.6(9) . . ?
C52 N3 H3A 116.7 . . ?
C53 N3 H3A 116.7 . . ?
C1 O1 C12 117.0(6) . . ?
C21 O3 C32 117.7(7) . . ?
C41 O5 C52 117.3(6) . . ?
H1OO O10 H10P 106.5 . . ?
H90 O9 H9P 106.5 . . ?
H8O O8 H8P 105.5 . . ?
H110 O11 H11P 106.2 . . ?
O7 C65 O7 179.999(11) 2_557 . ?

_refine_diff_density_max         1.720
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.183



####################################################################### 
# 
# 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_C2H4Cl2_4
_database_code_depnum_ccdc_archive 'CCDC 1542196'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_C2H4Cl2@4           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.855 Note  
RESPONSE: poorly diffracting crystal 
(best we could obtain from numerous crystallization efforts)
;
# end Validation Reply Form

_audit_creation_date             2017-04-06
_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C2H4Cl2), C96H144N6O12'
_chemical_formula_sum            'C104 H138 Cl8 N6 O12'
_chemical_formula_weight         1947.8
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.7784(9)
_cell_length_b                   14.3195(7)
_cell_length_c                   16.9560(8)
_cell_angle_alpha                97.571(4)
_cell_angle_beta                 109.693(5)
_cell_angle_gamma                114.255(5)
_cell_volume                     2725.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3116
_cell_measurement_temperature    149.8
_cell_measurement_theta_max      62.3786
_cell_measurement_theta_min      3.5638
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.35
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.033
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9569
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        62.470
_diffrn_reflns_theta_max         62.470
_diffrn_reflns_theta_min         3.567
_diffrn_ambient_temperature      149.8
_diffrn_detector_area_resol_mean 5.1856
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -28.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -1.1041   38.0000    0.0000 103

#__ type_ start__ end____ width___ exp.time_
  2 omega -117.00  -13.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   77.0000   30.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega -171.00    5.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000    0.0000    0.0000 176

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257  -61.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  5 omega   18.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257 -126.0000  120.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0113631000
_diffrn_orient_matrix_UB_12      -0.0468253000
_diffrn_orient_matrix_UB_13      0.0773391000
_diffrn_orient_matrix_UB_21      0.0932832000
_diffrn_orient_matrix_UB_22      0.1136652000
_diffrn_orient_matrix_UB_23      0.0652387000
_diffrn_orient_matrix_UB_31      -0.0983582000
_diffrn_orient_matrix_UB_32      0.0185291000
_diffrn_orient_matrix_UB_33      0.0099567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5252
_reflns_number_total             7431
_reflns_odcompleteness_completeness 90.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     9
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1316
_refine_ls_wR_factor_ref         0.4171
_refine_ls_wR_factor_gt          0.3837
_refine_ls_goodness_of_fit_ref   1.649
_refine_ls_restrained_S_all      1.611
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O21 O 0.8161(3) 0.3372(3) 0.6373(3) 0.0372(10) Uani 1 1 d . U . . .
O41 O 0.4861(4) 0.2209(3) 0.3270(2) 0.0390(10) Uani 1 1 d . U . . .
O42 O 0.5247(4) 0.3139(4) 0.2327(3) 0.0518(12) Uani 1 1 d . U . . .
O1 O 0.5551(4) 0.1490(4) 0.7893(3) 0.0543(13) Uani 1 1 d . U . . .
O2 O 0.6699(5) 0.2513(5) 0.9340(3) 0.0613(14) Uani 1 1 d . U . . .
O22 O 0.9253(5) 0.5137(4) 0.7152(5) 0.087(2) Uani 1 1 d . U . . .
N1 N 0.4822(6) 0.2143(5) 0.8644(4) 0.0619(17) Uani 1 1 d . U . . .
H1 H 0.4219 0.1811 0.8138 0.074 Uiso 1 1 calc R U . . .
N21 N 1.0081(4) 0.4146(4) 0.6877(4) 0.0468(13) Uani 1 1 d . U . . .
H21 H 0.9904 0.3491 0.6655 0.056 Uiso 1 1 calc R U . . .
N41 N 0.3719(5) 0.2883(5) 0.2689(3) 0.0473(14) Uani 1 1 d . U . . .
H41 H 0.3473 0.2708 0.3078 0.057 Uiso 1 1 calc R U . . .
C41 C 0.5822(5) 0.2034(4) 0.3400(3) 0.0300(12) Uani 1 1 d . U . . .
C42 C 0.6871(5) 0.2700(5) 0.4166(4) 0.0347(13) Uani 1 1 d . U . . .
C24 C 0.7100(5) 0.3368(4) 0.6223(4) 0.0344(13) Uani 1 1 d . U . . .
C23 C 0.6655(5) 0.3213(4) 0.6843(4) 0.0353(14) Uani 1 1 d . U . . .
C25 C 0.6472(5) 0.3459(4) 0.5418(4) 0.0348(13) Uani 1 1 d . U . . .
C31 C 0.7005(5) 0.3690(5) 0.4774(4) 0.0370(14) Uani 1 1 d . U . . .
H31A H 0.7840 0.4205 0.5105 0.044 Uiso 1 1 calc R U . . .
H31B H 0.6644 0.4030 0.4407 0.044 Uiso 1 1 calc R U . . .
C46 C 0.5704(5) 0.1190(5) 0.2806(4) 0.0396(14) Uani 1 1 d . U . . .
C52 C 0.4648(5) 0.2787(5) 0.2706(4) 0.0378(14) Uani 1 1 d . U . . .
C43 C 0.7784(5) 0.2482(5) 0.4325(4) 0.0388(14) Uani 1 1 d . U . . .
H43 H 0.8480 0.2917 0.4836 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4850(6) 0.3125(5) 0.5826(4) 0.0404(14) Uani 1 1 d . U . . .
C32 C 0.9201(6) 0.4323(5) 0.6833(4) 0.0424(15) Uani 1 1 d . U . . .
C26 C 0.5378(6) 0.3351(5) 0.5250(4) 0.0391(14) Uani 1 1 d . U . . .
H26 H 0.4967 0.3432 0.4727 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7396(5) 0.3213(5) 0.7747(3) 0.0364(14) Uani 1 1 d . U . . .
H11A H 0.8205 0.3774 0.7946 0.044 Uiso 1 1 calc R U . . .
H11B H 0.7112 0.3404 0.8160 0.044 Uiso 1 1 calc R U . . .
C45 C 0.6662(6) 0.1020(5) 0.2995(4) 0.0445(16) Uani 1 1 d . U . . .
H45 H 0.6602 0.0463 0.2596 0.053 Uiso 1 1 calc R U . . .
C44 C 0.7725(6) 0.1649(5) 0.3763(4) 0.0424(15) Uani 1 1 d . U . . .
C51 C 0.4579(6) 0.0491(5) 0.1966(4) 0.0450(16) Uani 1 1 d . U . . .
H51A H 0.4757 0.0129 0.1555 0.054 Uiso 1 1 calc R U . . .
H51B H 0.4317 0.0956 0.1702 0.054 Uiso 1 1 calc R U . . .
C22 C 0.5540(5) 0.3087(5) 0.6632(4) 0.0370(14) Uani 1 1 d . U . . .
H22 H 0.5233 0.2972 0.7043 0.044 Uiso 1 1 calc R U . . .
C1 C 0.8297(6) 0.0998(6) 0.7773(5) 0.0530(18) Uani 1 1 d . U . . .
C4 C 0.6436(6) 0.1343(5) 0.7870(4) 0.0423(16) Uani 1 1 d . U . . .
C27 C 0.3615(6) 0.2955(5) 0.5567(4) 0.0470(16) Uani 1 1 d . U . . .
C7 C 0.9380(6) 0.0916(6) 0.7798(5) 0.0477(16) Uani 1 1 d . U . . .
C53 C 0.3079(6) 0.3274(6) 0.2039(4) 0.0497(17) Uani 1 1 d . U . . .
C47 C 0.8771(7) 0.1432(7) 0.3947(5) 0.0574(19) Uani 1 1 d . U . . .
C33 C 1.1331(6) 0.4960(6) 0.7268(5) 0.0526(18) Uani 1 1 d . U . . .
C13 C 0.4679(7) 0.2690(7) 0.9351(5) 0.062(2) Uani 1 1 d . U . . .
C28 C 0.3221(6) 0.2758(7) 0.6318(5) 0.061(2) Uani 1 1 d . U . . .
H28A H 0.2434 0.2653 0.6135 0.092 Uiso 1 1 calc R U . . .
H28B H 0.3237 0.2128 0.6442 0.092 Uiso 1 1 calc R U . . .
H28C H 0.3749 0.3372 0.6840 0.092 Uiso 1 1 calc R U . . .
C3 C 0.6459(6) 0.0377(6) 0.7915(4) 0.0479(16) Uani 1 1 d . U . . .
C56 C 0.2482(7) 0.2491(7) 0.1126(5) 0.064(2) Uani 1 1 d . U . . .
H56A H 0.2073 0.2751 0.0713 0.095 Uiso 1 1 calc R U . . .
H56B H 0.3064 0.2422 0.0971 0.095 Uiso 1 1 calc R U . . .
H56C H 0.1928 0.1800 0.1111 0.095 Uiso 1 1 calc R U . . .
C30 C 0.2754(6) 0.1977(7) 0.4747(5) 0.069(2) Uani 1 1 d . U . . .
H30A H 0.1969 0.1872 0.4585 0.104 Uiso 1 1 calc R U . . .
H30B H 0.2968 0.2094 0.4271 0.104 Uiso 1 1 calc R U . . .
H30C H 0.2779 0.1349 0.4867 0.104 Uiso 1 1 calc R U . . .
C5 C 0.7399(6) 0.2172(6) 0.7789(4) 0.0499(17) Uani 1 1 d . U . . .
C6 C 0.8301(6) 0.1983(6) 0.7760(4) 0.0512(17) Uani 1 1 d . U . . .
H6 H 0.8938 0.2533 0.7730 0.061 Uiso 1 1 calc R U . . .
C12 C 0.5759(7) 0.2111(6) 0.8705(4) 0.0573(19) Uani 1 1 d . U . . .
C2 C 0.7384(6) 0.0230(6) 0.7886(4) 0.0507(17) Uani 1 1 d . U . . .
H2 H 0.7388 -0.0406 0.7943 0.061 Uiso 1 1 calc R U . . .
C29 C 0.3538(7) 0.3959(7) 0.5392(6) 0.064(2) Uani 1 1 d . U . . .
H29A H 0.2745 0.3829 0.5229 0.096 Uiso 1 1 calc R U . . .
H29B H 0.4067 0.4569 0.5917 0.096 Uiso 1 1 calc R U . . .
H29C H 0.3755 0.4102 0.4921 0.096 Uiso 1 1 calc R U . . .
C15 C 0.5540(10) 0.3904(9) 0.9644(7) 0.093(3) Uani 1 1 d . U . . .
H15A H 0.5457 0.4276 1.0110 0.139 Uiso 1 1 calc R U . . .
H15B H 0.6335 0.4024 0.9852 0.139 Uiso 1 1 calc R U . . .
H15C H 0.5367 0.4171 0.9152 0.139 Uiso 1 1 calc R U . . .
C55 C 0.3949(8) 0.4388(7) 0.2062(7) 0.085(3) Uani 1 1 d . U . . .
H55A H 0.3531 0.4635 0.1641 0.127 Uiso 1 1 calc R U . . .
H55B H 0.4317 0.4891 0.2642 0.127 Uiso 1 1 calc R U . . .
H55C H 0.4544 0.4334 0.1915 0.127 Uiso 1 1 calc R U . . .
C16 C 0.4897(11) 0.2273(9) 1.0126(7) 0.098(3) Uani 1 1 d . U . . .
H16A H 0.4794 0.2653 1.0575 0.146 Uiso 1 1 calc R U . . .
H16B H 0.4347 0.1516 0.9939 0.146 Uiso 1 1 calc R U . . .
H16C H 0.5688 0.2383 1.0359 0.146 Uiso 1 1 calc R U . . .
C54 C 0.2194(9) 0.3357(10) 0.2332(6) 0.087(3) Uani 1 1 d . U . . .
H54A H 0.1749 0.3607 0.1937 0.130 Uiso 1 1 calc R U . . .
H54B H 0.1669 0.2660 0.2329 0.130 Uiso 1 1 calc R U . . .
H54C H 0.2600 0.3856 0.2918 0.130 Uiso 1 1 calc R U . . .
C8 C 0.9136(9) -0.0249(8) 0.7704(7) 0.082(3) Uani 1 1 d . U . . .
H8A H 0.8495 -0.0718 0.7140 0.123 Uiso 1 1 calc R U . . .
H8B H 0.9830 -0.0291 0.7752 0.123 Uiso 1 1 calc R U . . .
H8C H 0.8931 -0.0466 0.8163 0.123 Uiso 1 1 calc R U . . .
C01H C 1.1414(11) 0.8434(10) 0.9790(8) 0.098(3) Uani 1 1 d D U . . .
C10 C 0.9648(12) 0.1170(11) 0.7038(10) 0.110(4) Uani 1 1 d . U . . .
H10A H 0.8957 0.0721 0.6493 0.165 Uiso 1 1 calc R U . . .
H10B H 0.9881 0.1915 0.7092 0.165 Uiso 1 1 calc R U . . .
H10C H 1.0279 0.1037 0.7043 0.165 Uiso 1 1 calc R U . . .
C9 C 1.0376(10) 0.1555(14) 0.8687(9) 0.159(8) Uani 1 1 d . U . . .
H9A H 1.0125 0.1339 0.9128 0.238 Uiso 1 1 calc R U . . .
H9B H 1.1023 0.1430 0.8729 0.238 Uiso 1 1 calc R U . . .
H9C H 1.0625 0.2308 0.8778 0.238 Uiso 1 1 calc R U . . .
C14 C 0.3452(10) 0.2495(14) 0.8941(9) 0.135(6) Uani 1 1 d . U . . .
H14A H 0.3294 0.2836 0.9373 0.203 Uiso 1 1 calc R U . . .
H14B H 0.3351 0.2790 0.8461 0.203 Uiso 1 1 calc R U . . .
H14C H 0.2914 0.1733 0.8722 0.203 Uiso 1 1 calc R U . . .
C36 C 1.1492(10) 0.5812(14) 0.6841(13) 0.160(8) Uani 1 1 d . U . . .
H36A H 1.2312 0.6345 0.7099 0.240 Uiso 1 1 calc R U . . .
H36B H 1.1226 0.5499 0.6221 0.240 Uiso 1 1 calc R U . . .
H36C H 1.1041 0.6147 0.6925 0.240 Uiso 1 1 calc R U . . .
C35 C 1.1982(10) 0.4377(11) 0.7117(13) 0.147(7) Uani 1 1 d . U . . .
H35A H 1.2811 0.4880 0.7363 0.221 Uiso 1 1 calc R U . . .
H35B H 1.1857 0.3824 0.7396 0.221 Uiso 1 1 calc R U . . .
H35C H 1.1693 0.4055 0.6495 0.221 Uiso 1 1 calc R U . . .
C34 C 1.1759(10) 0.5351(15) 0.8242(8) 0.149(7) Uani 1 1 d . U . . .
H34A H 1.2579 0.5887 0.8509 0.224 Uiso 1 1 calc R U . . .
H34B H 1.1312 0.5663 0.8375 0.224 Uiso 1 1 calc R U . . .
H34C H 1.1662 0.4757 0.8471 0.224 Uiso 1 1 calc R U . . .
C48 C 0.9626(13) 0.2204(18) 0.3666(15) 0.194(10) Uani 1 1 d . U . . .
H48A H 0.9229 0.2107 0.3051 0.292 Uiso 1 1 calc R U . . .
H48B H 0.9918 0.2932 0.4006 0.292 Uiso 1 1 calc R U . . .
H48C H 1.0274 0.2063 0.3764 0.292 Uiso 1 1 calc R U . . .
Cl01 Cl 0.8900(2) 0.5724(2) 0.98681(16) 0.0856(8) Uani 1 1 d D U . . .
Cl02 Cl 1.1213(4) 0.9563(3) 0.9728(3) 0.1314(13) Uani 1 1 d . U . . .
Cl00 Cl 1.3051(5) 0.9000(5) 0.9137(4) 0.184(2) Uani 1 1 d D U . . .
C01P C 1.1719(14) 0.8053(11) 0.9134(10) 0.133(5) Uani 1 1 d D U . . .
C01Q C 1.0113(10) 0.5505(7) 0.9881(8) 0.188(10) Uani 1 1 d D U . . .
C50 C 0.9382(16) 0.159(2) 0.4879(8) 0.209(11) Uani 1 1 d . U . . .
H50A H 0.9664 0.2313 0.5217 0.314 Uiso 1 1 calc R U . . .
H50B H 0.8849 0.1090 0.5061 0.314 Uiso 1 1 calc R U . . .
H50C H 1.0039 0.1460 0.4976 0.314 Uiso 1 1 calc R U . . .
C49 C 0.8365(13) 0.0310(12) 0.3470(19) 0.250(15) Uani 1 1 d . U . . .
H49A H 0.7954 0.0173 0.2848 0.375 Uiso 1 1 calc R U . . .
H49B H 0.9033 0.0198 0.3582 0.375 Uiso 1 1 calc R U . . .
H49C H 0.7843 -0.0172 0.3667 0.375 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6350(8) 0.0285(7) 0.4917(7) 0.112(2) Uani 0.5 1 d D U P A 1
C0AA C 0.5462(16) -0.0357(14) 0.5408(12) 0.087(6) Uani 0.5 1 d D U P A 1
C1AA C 0.5340(17) -0.0127(18) 0.4543(10) 0.088(6) Uani 0.5 1 d D U P B 2
Cl2 Cl 0.6515(7) 0.0342(8) 0.5571(5) 0.125(3) Uani 0.5 1 d D U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O21 C32 1.371(8) . ?
O21 C24 1.395(7) . ?
O41 C52 1.381(7) . ?
O41 C41 1.398(7) . ?
O42 C52 1.204(7) . ?
O1 C4 1.331(8) . ?
O1 C12 1.404(9) . ?
O2 C12 1.206(9) . ?
O22 C32 1.180(8) . ?
N1 C12 1.280(10) . ?
N1 C13 1.459(9) . ?
N1 H1 0.8600 . ?
N21 C32 1.319(8) . ?
N21 C33 1.464(9) . ?
N21 H21 0.8600 . ?
N41 C52 1.333(8) . ?
N41 C53 1.490(8) . ?
N41 H41 0.8600 . ?
C41 C46 1.382(8) . ?
C41 C42 1.400(8) . ?
C42 C43 1.368(9) . ?
C42 C31 1.541(8) . ?
C24 C23 1.383(8) . ?
C24 C25 1.404(8) . ?
C23 C22 1.381(9) . ?
C23 C11 1.529(8) . ?
C25 C26 1.372(9) . ?
C25 C31 1.510(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C46 C45 1.380(9) . ?
C46 C51 1.515(9) . ?
C43 C44 1.380(9) . ?
C43 H43 0.9300 . ?
C21 C26 1.398(9) . ?
C21 C22 1.400(9) . ?
C21 C27 1.509(9) . ?
C26 H26 0.9300 . ?
C11 C5 1.503(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C45 C44 1.405(9) . ?
C45 H45 0.9300 . ?
C44 C47 1.536(9) . ?
C51 C3 1.558(9) 2_656 ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C22 H22 0.9300 . ?
C1 C2 1.382(10) . ?
C1 C6 1.412(11) . ?
C1 C7 1.530(10) . ?
C4 C3 1.407(9) . ?
C4 C5 1.436(10) . ?
C27 C30 1.520(10) . ?
C27 C29 1.543(10) . ?
C27 C28 1.559(10) . ?
C7 C9 1.484(13) . ?
C7 C10 1.506(13) . ?
C7 C8 1.534(12) . ?
C53 C56 1.501(10) . ?
C53 C54 1.503(12) . ?
C53 C55 1.538(11) . ?
C47 C50 1.454(15) . ?
C47 C49 1.470(16) . ?
C47 C48 1.511(14) . ?
C33 C36 1.477(14) . ?
C33 C34 1.489(14) . ?
C33 C35 1.511(14) . ?
C13 C14 1.480(14) . ?
C13 C16 1.504(14) . ?
C13 C15 1.535(14) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C3 C2 1.391(10) . ?
C3 C51 1.558(9) 2_656 ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C5 C6 1.391(10) . ?
C6 H6 0.9300 . ?
C2 H2 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C01H C01P 1.435(14) . ?
C01H Cl02 1.758(11) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
Cl01 C01Q 1.816(12) . ?
Cl00 C01P 1.775(14) . ?
C01Q C01Q 1.488(16) 2_767 ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
Cl1 C0AA 1.732(13) . ?
C1AA C0AA 1.544(7) 2_656 ?
C1AA Cl2 1.735(14) . ?

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
C32 O21 C24 118.9(5) . . ?
C52 O41 C41 117.6(4) . . ?
C4 O1 C12 116.4(5) . . ?
C12 N1 C13 126.2(6) . . ?
C12 N1 H1 116.9 . . ?
C13 N1 H1 116.9 . . ?
C32 N21 C33 126.2(6) . . ?
C32 N21 H21 116.9 . . ?
C33 N21 H21 116.9 . . ?
C52 N41 C53 124.3(5) . . ?
C52 N41 H41 117.8 . . ?
C53 N41 H41 117.8 . . ?
C46 C41 O41 120.1(5) . . ?
C46 C41 C42 121.9(5) . . ?
O41 C41 C42 118.0(5) . . ?
C43 C42 C41 118.0(5) . . ?
C43 C42 C31 121.6(5) . . ?
C41 C42 C31 120.3(5) . . ?
C23 C24 O21 119.6(5) . . ?
C23 C24 C25 121.4(5) . . ?
O21 C24 C25 118.9(5) . . ?
C22 C23 C24 118.3(5) . . ?
C22 C23 C11 121.1(5) . . ?
C24 C23 C11 120.7(5) . . ?
C26 C25 C24 117.8(5) . . ?
C26 C25 C31 121.8(5) . . ?
C24 C25 C31 120.4(5) . . ?
C25 C31 C42 115.5(5) . . ?
C25 C31 H31A 108.4 . . ?
C42 C31 H31A 108.4 . . ?
C25 C31 H31B 108.4 . . ?
C42 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C45 C46 C41 117.5(5) . . ?
C45 C46 C51 121.0(6) . . ?
C41 C46 C51 121.5(6) . . ?
O42 C52 N41 128.8(6) . . ?
O42 C52 O41 123.0(5) . . ?
N41 C52 O41 108.2(5) . . ?
C42 C43 C44 123.2(6) . . ?
C42 C43 H43 118.4 . . ?
C44 C43 H43 118.4 . . ?
C26 C21 C22 116.0(6) . . ?
C26 C21 C27 120.0(6) . . ?
C22 C21 C27 124.0(5) . . ?
O22 C32 N21 127.9(6) . . ?
O22 C32 O21 123.4(6) . . ?
N21 C32 O21 108.7(5) . . ?
C25 C26 C21 123.4(5) . . ?
C25 C26 H26 118.3 . . ?
C21 C26 H26 118.3 . . ?
C5 C11 C23 116.2(5) . . ?
C5 C11 H11A 108.2 . . ?
C23 C11 H11A 108.2 . . ?
C5 C11 H11B 108.2 . . ?
C23 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C46 C45 C44 123.0(6) . . ?
C46 C45 H45 118.5 . . ?
C44 C45 H45 118.5 . . ?
C43 C44 C45 116.4(6) . . ?
C43 C44 C47 122.3(6) . . ?
C45 C44 C47 121.3(6) . . ?
C46 C51 C3 115.3(5) . 2_656 ?
C46 C51 H51A 108.4 . . ?
C3 C51 H51A 108.4 2_656 . ?
C46 C51 H51B 108.4 . . ?
C3 C51 H51B 108.4 2_656 . ?
H51A C51 H51B 107.5 . . ?
C23 C22 C21 122.9(5) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C2 C1 C6 116.8(7) . . ?
C2 C1 C7 124.5(7) . . ?
C6 C1 C7 118.1(6) . . ?
O1 C4 C3 121.7(6) . . ?
O1 C4 C5 120.5(6) . . ?
C3 C4 C5 117.8(6) . . ?
C21 C27 C30 109.8(5) . . ?
C21 C27 C29 111.2(6) . . ?
C30 C27 C29 109.8(6) . . ?
C21 C27 C28 111.4(6) . . ?
C30 C27 C28 108.3(6) . . ?
C29 C27 C28 106.4(6) . . ?
C9 C7 C10 115.3(10) . . ?
C9 C7 C1 109.3(6) . . ?
C10 C7 C1 112.2(7) . . ?
C9 C7 C8 104.4(9) . . ?
C10 C7 C8 105.7(7) . . ?
C1 C7 C8 109.5(6) . . ?
N41 C53 C56 110.2(6) . . ?
N41 C53 C54 105.3(6) . . ?
C56 C53 C54 111.4(7) . . ?
N41 C53 C55 109.9(6) . . ?
C56 C53 C55 109.7(7) . . ?
C54 C53 C55 110.3(8) . . ?
C50 C47 C49 106.7(15) . . ?
C50 C47 C48 109.0(14) . . ?
C49 C47 C48 110.2(15) . . ?
C50 C47 C44 111.4(6) . . ?
C49 C47 C44 110.9(7) . . ?
C48 C47 C44 108.6(7) . . ?
N21 C33 C36 109.7(7) . . ?
N21 C33 C34 108.5(7) . . ?
C36 C33 C34 114.8(12) . . ?
N21 C33 C35 106.4(7) . . ?
C36 C33 C35 111.3(11) . . ?
C34 C33 C35 105.9(11) . . ?
N1 C13 C14 104.9(8) . . ?
N1 C13 C16 112.2(7) . . ?
C14 C13 C16 111.7(9) . . ?
N1 C13 C15 108.4(7) . . ?
C14 C13 C15 109.4(10) . . ?
C16 C13 C15 110.1(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 C51 122.2(6) . 2_656 ?
C4 C3 C51 116.5(6) . 2_656 ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C5 C4 118.7(6) . . ?
C6 C5 C11 122.7(6) . . ?
C4 C5 C11 118.6(6) . . ?
C5 C6 C1 123.2(7) . . ?
C5 C6 H6 118.4 . . ?
C1 C6 H6 118.4 . . ?
O2 C12 N1 128.6(7) . . ?
O2 C12 O1 121.6(7) . . ?
N1 C12 O1 109.8(6) . . ?
C1 C2 C3 122.1(7) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C01P C01H Cl02 115.4(9) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C01H C01P Cl00 115.3(11) . . ?
C01Q C01Q Cl01 104.9(10) 2_767 . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

_refine_diff_density_max         1.523
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.103




