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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dcm006cu_may2016
_database_code_depnum_ccdc_archive 'CCDC 1484207'
_audit_update_record             
;
2016-06-09 deposited with the CCDC.
2016-08-29 downloaded from the CCDC.
;
_audit_creation_date             2016-06-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        'phenyl beta-aminobisulfonate'
_chemical_formula_moiety         'C44 H72 Br0.12 K9 N4 O37 S8, 0.88(Br1)'
_chemical_formula_sum            'C44 H72 Br K9 N4 O37 S8'
_chemical_formula_weight         1937.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H60 N4 O37 S17'
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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'
S S 0.3331 0.5567 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.9837(3)
_cell_length_b                   13.1145(2)
_cell_length_c                   32.7662(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.8278(19)
_cell_angle_gamma                90
_cell_volume                     7534.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22673
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      66.1150
_cell_measurement_theta_min      2.7330
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.075
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.296
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3976
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 6 -8 0.1210
0 0 21 0.0417
0 -1 -21 0.0446
12 -2 -2 0.1484
-10 -3 6 0.1119
0 8 -8 0.1401
-10 4 -1 0.1363
0 -8 8 0.0815

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.101
loop_
_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
8.0008 6.0000 -7.9974 0.0755 -0.7038 0.7201
-0.0016 0.0007 21.0010 0.9094 0.4458 0.0174
0.0015 -1.0007 -21.0009 -0.9609 -0.3405 -0.0240
12.0000 -1.9997 -1.9947 -0.0203 0.3157 1.0150
-10.0005 -3.0001 5.9962 -0.0358 0.3206 -0.8734
0.0009 7.9998 -8.0011 0.0656 -1.0128 0.0468
-9.9998 3.9997 -1.0048 0.0216 -0.5655 -0.8324
-0.0009 -7.9998 8.0011 -0.0656 1.0128 -0.0468

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1612
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            103432
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.343
_diffrn_reflns_theta_max         66.343
_diffrn_reflns_theta_min         2.520
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00 -35.00   1.00    4.00    --  -41.72 143.00 -36.00   26
  2  ω    -96.00 -70.00   1.00    4.00    --  -41.72 125.00 120.00   26
  3  ω    -55.00 -18.00   1.00    4.00    --  -41.72 125.00 120.00   37
  4  ω    -32.00  69.00   1.00    4.00    --   41.72 -57.00-120.00  101
  5  ω     28.00 118.00   1.00    4.00    --   41.72  38.00  30.00   90
  6  ω     65.00  90.00   1.00    4.00    --   41.72 137.00  57.00   25
  7  ω    -19.00  54.00   1.00    4.00    --   41.72 -38.00  30.00   73
  8  ω     35.00  78.00   1.00   16.00    --   92.50 -92.00 166.12   43
  9  ω     79.00 129.00   1.00   16.00    --   92.50 -93.00 122.77   50
 10  ω     14.00  40.00   1.00   16.00    --   92.50 -93.00-133.90   26
 11  ω     76.00 122.00   1.00   16.00    --   92.50 -61.00 150.00   46
 12  ω     68.00 105.00   1.00   16.00    --   92.50  77.00 120.00   37
 13  ω     65.00  90.00   1.00   16.00    --   92.50  30.00  30.00   25
 14  ω     70.00 111.00   1.00   16.00    --   92.50 -93.00  55.86   41
 15  ω     78.00 115.00   1.00   16.00    --   92.50  30.00   0.00   37
 16  ω     53.00  93.00   1.00   16.00    --   92.50 -61.00 -60.00   40
 17  ω     46.00 102.00   1.00   16.00    --   92.50 -92.00-107.00   56
 18  ω     18.00  68.00   1.00   16.00    --   92.50 -30.00 -30.00   50
 19  ω     15.00  40.00   1.00   16.00    --   92.50 -30.00-150.00   25
 20  ω     29.00  85.00   1.00   16.00    --   92.50-125.00-180.00   56
 21  ω     19.00  65.00   1.00   16.00    --   92.50 -30.00 150.00   46
 22  ω     18.00  64.00   1.00   16.00    --   92.50 -61.00 150.00   46
 23  ω     75.00 101.00   1.00   16.00    --   92.50  45.00  60.00   26
 24  ω     10.00  67.00   1.00   16.00    --   92.50 -94.00  90.00   57
 25  ω     29.00  61.00   1.00   16.00    --   92.50 -30.00 -90.00   32
 26  ω    125.00 170.00   1.00   16.00    --   92.50  77.00 120.00   45
 27  ω     89.00 132.00   1.00   16.00    --   92.50 -92.00  -3.69   43
 28  ω    106.00 167.00   1.00   16.00    --   92.50  30.00  30.00   61
 29  ω     41.00  74.00   1.00   16.00    --   92.50 -45.00-150.00   33
 30  ω     63.00 169.00   1.00   16.00    --   92.50  30.00 -30.00  106
 31  ω    129.00 168.00   1.00   16.00    --   92.50  77.00   0.00   39
 32  ω     83.00 109.00   1.00   16.00    --   92.50  77.00   0.00   26
 33  ω     85.00 111.00   1.00   16.00    --   92.50  45.00 -90.00   26
 34  ω     23.00  65.00   1.00   16.00    --   92.50 -45.00 -90.00   42
 35  ω     92.00 117.00   1.00   16.00    --   92.50 -92.00 166.12   25
 36  ω     24.00  71.00   1.00   16.00    --   92.50 -45.00 -30.00   47
 37  ω     63.00  90.00   1.00   16.00    --   92.50  61.00 120.00   27
 38  ω     50.00  79.00   1.00   16.00    --   92.50 -61.00  60.00   29
 39  ω     24.00  50.00   1.00   16.00    --   92.50-125.00-120.00   26
 40  ω     65.00  90.00   1.00   16.00    --   92.50-125.00-120.00   25
 41  ω     82.00 107.00   1.00   16.00    --   92.50 -93.00-133.90   25
 42  ω     87.00 124.00   1.00   16.00    --   92.50 -67.00 -48.43   37
 43  ω     15.00  40.00   1.00   16.00    --   92.50 -30.00-120.00   25
 44  ω     38.00  64.00   1.00   16.00    --   92.50 -45.00  60.00   26
 45  ω     41.00  66.00   1.00   16.00    --   92.50 -45.00  90.00   25
 46  ω     38.00  75.00   1.00   16.00    --   92.50 -45.00 150.00   37
 47  ω     50.00 131.00   1.00   16.00    --   92.50 -93.00 -74.81   81
 48  ω    131.00 157.00   1.00   16.00    --   92.50  45.00  60.00   26
 49  ω    150.00 176.00   1.00   16.00    --   92.50  15.00 -60.00   26
 50  ω     26.00  68.00   1.00   16.00    --   92.50 -15.00-120.00   42
 51  ω      9.00  42.00   1.00   16.00    --   92.50 -93.00 -74.81   33
 52  ω   -120.00  -8.00   1.00    4.00    --  -41.72 -77.00-150.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0140918000
_diffrn_orient_matrix_UB_12      0.0515009000
_diffrn_orient_matrix_UB_13      0.0433014000
_diffrn_orient_matrix_UB_21      0.0122779000
_diffrn_orient_matrix_UB_22      -0.1053654000
_diffrn_orient_matrix_UB_23      0.0212333000
_diffrn_orient_matrix_UB_31      0.0858303000
_diffrn_orient_matrix_UB_32      0.0066692000
_diffrn_orient_matrix_UB_33      0.0008328000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_special_details          
'multiple twinned crystal, only refelections for one individual were used for the structure solution and refinement as this gave the best refinement values.'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10366
_reflns_number_total             13155
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.81
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_diff_density_max         4.266
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.379
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.536
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         13155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.1480
_refine_ls_restrained_S_all      1.536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_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_ls_wR_factor_gt          0.3662
_refine_ls_wR_factor_ref         0.3843
_refine_special_details          
', Twin,multiple twin, multicrystal, only one individual extracted and used for structure solution'
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Br1A)
Uanis(K2) = Uanis(K2A)
3. Others
 Sof(Br1A)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
 Sof(K2A)=1-FVAR(2)
 Sof(K2)=FVAR(2)
4.a Rotating group:
 O102(H10A,H10B), O105(H10C,H10D), O100(H10E,H10F), O103(H10G,H10H), O107(H10I,
 H10J), O108(H10K,H10L)
4.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C88(H88A,H88B), C40(H40A,H40B), C19(H19A,H19B), C61(H61A,
 H61B), C62(H62A,H62B), C67(H67A,H67B), C83(H83A,H83B), C20(H20A,H20B),
 C47(H47A,H47B), C89(H89A,H89B), C41(H41A,H41B), C46(H46A,H46B), C25(H25A,H25B),
  C26(H26A,H26B), C68(H68A,H68B)
4.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C33(H33), C13(H13), C57(H57), C56(H56), C75(H75), C76(H76),
 C34(H34), C55(H55), C78(H78), C54(H54), C15(H15), C14(H14), C12(H12), C35(H35),
  C77(H77)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C60(H60A,H60B,H60C), C81(H81A,H81B,H81C), C39(H39A,H39B,
 H39C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K3 K 0.98256(11) 0.15389(14) 0.37681(7) 0.0326(5) Uani 1 1 d . . . . .
S90 S 0.42696(11) 0.86650(15) 0.37204(6) 0.0203(5) Uani 1 1 d . . . . .
S69 S 0.68001(11) 0.02383(14) 0.37505(6) 0.0203(5) Uani 1 1 d . . . . .
K6 K 0.73189(11) 0.73886(14) 0.37016(6) 0.0280(5) Uani 1 1 d . . . . .
S48 S 0.93420(11) -0.11171(16) 0.37299(7) 0.0239(5) Uani 1 1 d . . . . .
S84 S 0.58597(11) 0.39098(15) 0.42918(6) 0.0202(4) Uani 1 1 d . . . . .
S42 S 1.08940(12) 0.39760(17) 0.42850(8) 0.0299(5) Uani 1 1 d . . . . .
S27 S 1.17947(11) 0.01148(17) 0.36686(6) 0.0246(5) Uani 1 1 d . . . . .
S21 S 1.34125(12) 0.48998(17) 0.42890(7) 0.0276(5) Uani 1 1 d . . . . .
S017 S 0.84249(12) 0.52739(16) 0.41025(7) 0.0281(5) Uani 1 1 d . . . . .
O38 O 1.1777(3) 0.6166(4) 0.31161(19) 0.0235(12) Uani 1 1 d . . . . .
O17 O 1.4238(3) 0.2854(4) 0.30552(19) 0.0246(13) Uani 1 1 d . . . . .
O86 O 0.5316(3) 0.3075(4) 0.42729(18) 0.0223(12) Uani 1 1 d . . . . .
O66 O 0.7872(4) 0.5817(5) 0.4286(2) 0.0281(13) Uani 1 1 d . . . . .
O80 O 0.6744(3) 0.6002(5) 0.30741(18) 0.0234(12) Uani 1 1 d . . . . .
O24 O 1.2909(3) 0.5785(4) 0.42792(19) 0.0244(13) Uani 1 1 d . . . . .
O59 O 0.9267(3) 0.2863(5) 0.30989(19) 0.0247(13) Uani 1 1 d . . . . .
O45 O 1.0339(4) 0.3189(5) 0.4289(2) 0.0299(14) Uani 1 1 d . . . . .
O85 O 0.6622(3) 0.3544(5) 0.4286(2) 0.0263(13) Uani 1 1 d . . . . .
N31 N 1.0729(4) 0.6539(5) 0.3570(2) 0.0165(13) Uani 1 1 d . . . . .
N10 N 1.3193(4) 0.2454(5) 0.3513(2) 0.0192(14) Uani 1 1 d . . . . .
O91 O 0.4138(3) 0.9625(5) 0.34983(19) 0.0263(13) Uani 1 1 d . . . . .
O70 O 0.6641(3) -0.0720(4) 0.35212(19) 0.0237(12) Uani 1 1 d . . . . .
C53 C 0.7971(5) 0.2758(6) 0.3133(3) 0.0202(16) Uani 1 1 d . . . . .
C74 C 0.5448(5) 0.6113(6) 0.3113(3) 0.0191(16) Uani 1 1 d . . . . .
N73 N 0.5719(4) 0.6407(5) 0.3540(2) 0.0159(13) Uani 1 1 d . . . . .
O29 O 1.1161(4) 0.0747(6) 0.3722(3) 0.0428(18) Uani 1 1 d . . . . .
O71 O 0.6133(3) 0.0923(5) 0.3699(2) 0.0291(14) Uani 1 1 d . . . . .
O92 O 0.3597(3) 0.7999(5) 0.3652(2) 0.0281(13) Uani 1 1 d . . . . .
C11 C 1.2945(5) 0.2803(6) 0.3095(3) 0.0230(17) Uani 1 1 d . . . . .
O87 O 0.5874(4) 0.4593(5) 0.46458(17) 0.0264(13) Uani 1 1 d . . . . .
C79 C 0.5989(5) 0.5862(6) 0.2875(3) 0.0194(16) Uani 1 1 d . . . . .
N52 N 0.8242(4) 0.2474(5) 0.3563(2) 0.0181(14) Uani 1 1 d . . . . .
O72 O 0.7138(4) 0.0081(5) 0.41954(19) 0.0279(13) Uani 1 1 d . . . . .
O65 O 0.9121(4) 0.5037(6) 0.4403(2) 0.0398(17) Uani 1 1 d . . . . .
C36 C 1.0806(6) 0.5625(7) 0.2505(3) 0.029(2) Uani 1 1 d . . . . .
H36 H 1.1180 0.5456 0.2352 0.035 Uiso 1 1 calc R . . . .
O30 O 1.1568(4) -0.0725(5) 0.3386(2) 0.0337(15) Uani 1 1 d . . . . .
O22 O 1.4179(4) 0.5187(6) 0.4298(2) 0.0414(18) Uani 1 1 d . . . . .
O50 O 0.9146(4) -0.0242(5) 0.3459(2) 0.0354(16) Uani 1 1 d . . . . .
C32 C 1.0469(5) 0.6213(6) 0.3145(3) 0.0187(16) Uani 1 1 d . . . . .
C33 C 0.9707(5) 0.6061(6) 0.2956(3) 0.0242(18) Uani 1 1 d . . . . .
H33 H 0.9325 0.6185 0.3109 0.029 Uiso 1 1 calc R . . . .
C13 C 1.1958(5) 0.3277(7) 0.2490(3) 0.0282(19) Uani 1 1 d . . . . .
H13 H 1.1432 0.3327 0.2360 0.034 Uiso 1 1 calc R . . . .
C37 C 1.1034(5) 0.5991(6) 0.2910(2) 0.0187(16) Uani 1 1 d . . . . .
C57 C 0.8280(5) 0.3350(7) 0.2491(3) 0.0268(19) Uani 1 1 d . . . . .
H57 H 0.8650 0.3542 0.2339 0.032 Uiso 1 1 calc R . . . .
O93 O 0.4584(4) 0.8798(5) 0.4168(2) 0.0350(15) Uani 1 1 d . . . . .
O49 O 0.8689(4) -0.1696(5) 0.3772(3) 0.0434(19) Uani 1 1 d . . . . .
C82 C 0.6072(4) 0.5573(7) 0.3812(3) 0.0209(17) Uani 1 1 d . . . . .
H82A H 0.6270 0.5846 0.4097 0.025 Uiso 1 1 calc R . . . .
H82B H 0.6512 0.5312 0.3708 0.025 Uiso 1 1 calc R . . . .
C56 C 0.7523(6) 0.3424(7) 0.2305(3) 0.0283(19) Uani 1 1 d . . . . .
H56 H 0.7371 0.3654 0.2024 0.034 Uiso 1 1 calc R . . . .
C58 C 0.8514(5) 0.3001(6) 0.2896(3) 0.0231(17) Uani 1 1 d . . . . .
C75 C 0.4671(5) 0.6020(6) 0.2921(3) 0.0233(17) Uani 1 1 d . . . . .
H75 H 0.4296 0.6158 0.3077 0.028 Uiso 1 1 calc R . . . .
C76 C 0.4444(5) 0.5731(6) 0.2505(3) 0.0256(18) Uani 1 1 d . . . . .
H76 H 0.3917 0.5716 0.2374 0.031 Uiso 1 1 calc R . . . .
C34 C 0.9498(5) 0.5723(6) 0.2538(3) 0.0264(19) Uani 1 1 d . . . . .
H34 H 0.8974 0.5648 0.2406 0.032 Uiso 1 1 calc R . . . .
C88 C 0.5169(5) 0.6979(6) 0.3730(3) 0.0214(17) Uani 1 1 d . . . . .
H88A H 0.5389 0.7080 0.4032 0.026 Uiso 1 1 calc R . . . .
H88B H 0.4695 0.6576 0.3702 0.026 Uiso 1 1 calc R . . . .
C55 C 0.6976(5) 0.3164(6) 0.2525(3) 0.0257(19) Uani 1 1 d . . . . .
H55 H 0.6449 0.3197 0.2394 0.031 Uiso 1 1 calc R . . . .
O44 O 1.0973(4) 0.4605(6) 0.4674(2) 0.0406(17) Uani 1 1 d . . . . .
C16 C 1.3496(5) 0.3038(6) 0.2860(3) 0.0225(17) Uani 1 1 d . . . . .
C78 C 0.5734(6) 0.5524(7) 0.2462(3) 0.0268(19) Uani 1 1 d . . . . .
H78 H 0.6100 0.5334 0.2307 0.032 Uiso 1 1 calc R . . . .
C40 C 1.1066(4) 0.5708(6) 0.3849(3) 0.0189(16) Uani 1 1 d . . . . .
H40A H 1.1269 0.5990 0.4132 0.023 Uiso 1 1 calc R . . A .
H40B H 1.1501 0.5421 0.3747 0.023 Uiso 1 1 calc R . . A .
C54 C 0.7206(5) 0.2854(6) 0.2943(3) 0.0234(17) Uani 1 1 d . . . . .
H54 H 0.6831 0.2706 0.3099 0.028 Uiso 1 1 calc R . . . .
C15 C 1.3267(5) 0.3420(6) 0.2453(3) 0.0250(18) Uani 1 1 d . . . . .
H15 H 1.3641 0.3600 0.2302 0.030 Uiso 1 1 calc R . . . .
O23 O 1.3376(4) 0.4177(6) 0.4624(2) 0.0360(15) Uani 1 1 d . . . . .
C14 C 1.2505(6) 0.3540(7) 0.2270(3) 0.032(2) Uani 1 1 d . . . . .
H14 H 1.2355 0.3802 0.1994 0.039 Uiso 1 1 calc R . . . .
C19 C 1.3555(5) 0.3265(7) 0.3798(3) 0.0218(17) Uani 1 1 d . . . . .
H19A H 1.4013 0.3506 0.3706 0.026 Uiso 1 1 calc R . . . .
H19B H 1.3729 0.2970 0.4081 0.026 Uiso 1 1 calc R . . . .
C18 C 1.4814(5) 0.3071(7) 0.2832(3) 0.0288(19) Uani 1 1 d . . . . .
H18A H 1.4719 0.2673 0.2572 0.043 Uiso 1 1 calc GR . . . .
H18B H 1.5314 0.2890 0.3005 0.043 Uiso 1 1 calc GR . . . .
H18C H 1.4805 0.3800 0.2765 0.043 Uiso 1 1 calc GR . . . .
C61 C 0.8579(5) 0.3330(7) 0.3829(3) 0.0235(17) Uani 1 1 d . . . . .
H61A H 0.8956 0.3674 0.3697 0.028 Uiso 1 1 calc R . . . .
H61B H 0.8858 0.3058 0.4102 0.028 Uiso 1 1 calc R . . . .
C62 C 0.7998(5) 0.4119(6) 0.3906(3) 0.0234(17) Uani 1 1 d . . . . .
H62A H 0.7715 0.3836 0.4106 0.028 Uiso 1 1 calc R . . . .
H62B H 0.7626 0.4252 0.3639 0.028 Uiso 1 1 calc R . . . .
O43 O 1.1630(5) 0.3652(7) 0.4242(3) 0.060(3) Uani 1 1 d . . . . .
C67 C 0.7698(5) 0.1914(6) 0.3758(3) 0.0230(17) Uani 1 1 d . . . . .
H67A H 0.7229 0.2324 0.3736 0.028 Uiso 1 1 calc R . . . .
H67B H 0.7927 0.1806 0.4059 0.028 Uiso 1 1 calc R . . . .
C83 C 0.5531(5) 0.4676(6) 0.3840(3) 0.0219(17) Uani 1 1 d . . . . .
H83A H 0.5481 0.4246 0.3587 0.026 Uiso 1 1 calc R . . . .
H83B H 0.5020 0.4947 0.3845 0.026 Uiso 1 1 calc R . . . .
C12 C 1.2177(5) 0.2944(6) 0.2897(3) 0.0246(18) Uani 1 1 d . . . . .
H12 H 1.1795 0.2806 0.3048 0.029 Uiso 1 1 calc R . . . .
C20 C 1.3041(5) 0.4197(7) 0.3829(3) 0.0279(19) Uani 1 1 d . . . . .
H20A H 1.2519 0.3962 0.3831 0.033 Uiso 1 1 calc R . . . .
H20B H 1.3011 0.4640 0.3581 0.033 Uiso 1 1 calc R . . . .
C35 C 1.0050(6) 0.5502(7) 0.2322(3) 0.030(2) Uani 1 1 d . . . . .
H35 H 0.9906 0.5261 0.2042 0.036 Uiso 1 1 calc R . . . .
C77 C 0.4989(5) 0.5459(6) 0.2278(3) 0.0266(18) Uani 1 1 d . . . . .
H77 H 0.4833 0.5233 0.1996 0.032 Uiso 1 1 calc R . . . .
C47 C 0.9944(5) -0.1890(6) 0.3503(3) 0.0208(17) Uani 1 1 d . . . . .
H47A H 0.9679 -0.2064 0.3213 0.025 Uiso 1 1 calc R . . . .
H47B H 1.0410 -0.1502 0.3490 0.025 Uiso 1 1 calc R . . . .
O28 O 1.2247(4) -0.0303(7) 0.4067(2) 0.0459(19) Uani 1 1 d . . . . .
C89 C 0.4978(5) 0.8021(6) 0.3519(3) 0.0201(16) Uani 1 1 d . . . . .
H89A H 0.4794 0.7923 0.3214 0.024 Uiso 1 1 calc R . . . .
H89B H 0.5445 0.8443 0.3566 0.024 Uiso 1 1 calc R . . . .
C60 C 0.9833(5) 0.3104(7) 0.2869(3) 0.0286(19) Uani 1 1 d . . . . .
H60A H 1.0339 0.2927 0.3037 0.043 Uiso 1 1 calc GR . . . .
H60B H 0.9815 0.3835 0.2807 0.043 Uiso 1 1 calc GR . . . .
H60C H 0.9734 0.2716 0.2607 0.043 Uiso 1 1 calc GR . . . .
C41 C 1.0506(5) 0.4838(7) 0.3882(3) 0.0246(18) Uani 1 1 d . . . . .
H41A H 1.0374 0.4467 0.3613 0.030 Uiso 1 1 calc R . . . .
H41B H 1.0030 0.5132 0.3937 0.030 Uiso 1 1 calc R . . . .
C81 C 0.7309(5) 0.5805(7) 0.2833(3) 0.0250(18) Uani 1 1 d . . . . .
H81A H 0.7207 0.6235 0.2582 0.037 Uiso 1 1 calc GR . . . .
H81B H 0.7287 0.5086 0.2750 0.037 Uiso 1 1 calc GR . . . .
H81C H 0.7818 0.5961 0.3002 0.037 Uiso 1 1 calc GR . . . .
C46 C 1.0170(5) -0.2869(6) 0.3748(2) 0.0193(16) Uani 1 1 d . . . . .
H46A H 1.0398 -0.2701 0.4044 0.023 Uiso 1 1 calc R . . . .
H46B H 0.9710 -0.3290 0.3741 0.023 Uiso 1 1 calc R . . . .
C39 C 1.2353(5) 0.5920(7) 0.2900(3) 0.0261(18) Uani 1 1 d . . . . .
H39A H 1.2365 0.5180 0.2859 0.039 Uiso 1 1 calc GR . . B .
H39B H 1.2849 0.6149 0.3064 0.039 Uiso 1 1 calc GR . . B .
H39C H 1.2245 0.6260 0.2627 0.039 Uiso 1 1 calc GR . . B .
C25 C 1.2633(5) 0.1863(7) 0.3687(3) 0.0260(18) Uani 1 1 d . . . . .
H25A H 1.2166 0.2276 0.3670 0.031 Uiso 1 1 calc R . . . .
H25B H 1.2851 0.1712 0.3985 0.031 Uiso 1 1 calc R . . . .
C26 C 1.2428(5) 0.0879(6) 0.3452(3) 0.0243(17) Uani 1 1 d . . . . .
H26A H 1.2900 0.0487 0.3456 0.029 Uiso 1 1 calc R . . . .
H26B H 1.2188 0.1035 0.3157 0.029 Uiso 1 1 calc R . . . .
O64 O 0.8568(4) 0.5812(6) 0.3737(2) 0.0391(16) Uani 1 1 d . . . . .
C68 C 0.7494(5) 0.0884(6) 0.3545(2) 0.0175(15) Uani 1 1 d . . . . .
H68A H 0.7959 0.0458 0.3583 0.021 Uiso 1 1 calc R . . . .
H68B H 0.7300 0.0991 0.3241 0.021 Uiso 1 1 calc R . . . .
O51 O 0.9810(5) -0.0803(7) 0.4138(3) 0.054(2) Uani 1 1 d . . . . .
K8 K 0.51795(11) 0.62959(15) 0.49576(6) 0.0278(5) Uani 1 1 d . . . . .
K9 K 0.47396(10) 1.14992(14) 0.37135(6) 0.0258(4) Uani 1 1 d . . . . .
K4 K 0.97991(14) 0.3777(2) 0.50377(8) 0.0494(6) Uani 1 1 d . . . . .
K2 K 1.2247(5) 0.7558(10) 0.3858(10) 0.025(2) Uani 0.75(11) 1 d . . P C 1
K5 K 0.75420(11) 0.47665(16) 0.49671(6) 0.0289(5) Uani 1 1 d . . . . .
K1 K 1.11727(15) -0.0085(2) 0.45770(7) 0.0461(6) Uani 1 1 d . . . . .
K7 K 0.65270(12) 0.15463(15) 0.46598(6) 0.0331(5) Uani 1 1 d . . . . .
Br1 Br 0.83086(7) 0.24484(9) 0.51400(4) 0.0351(4) Uani 0.883(3) 1 d . . P D 1
O102 O 1.1014(4) 0.2592(6) 0.5334(3) 0.047(2) Uani 1 1 d . . . . .
H10A H 1.0998 0.2380 0.5585 0.070 Uiso 1 1 d GR . . . .
H10B H 1.1431 0.2942 0.5346 0.070 Uiso 1 1 d GR . . . .
O104 O 0.3854(4) 0.7487(5) 0.4662(2) 0.0323(15) Uani 1 1 d . . . . .
O105 O 0.6957(6) 0.8043(7) 0.4438(3) 0.062(2) Uani 1 1 d . . . . .
H10C H 0.6798 0.7526 0.4564 0.094 Uiso 1 1 d GR . . . .
H10D H 0.6596 0.8502 0.4381 0.094 Uiso 1 1 d GR . . . .
O100 O 1.1309(5) 0.0022(8) 0.5398(3) 0.059(2) Uani 1 1 d . . . . .
H10E H 1.0909 -0.0262 0.5466 0.088 Uiso 1 1 d GR . . . .
H10F H 1.1338 0.0664 0.5479 0.088 Uiso 1 1 d GR . . . .
O101 O 0.9966(7) 0.1243(7) 0.4621(4) 0.074(3) Uani 1 1 d . . . . .
O103 O 0.5699(5) 0.8220(8) 0.4862(3) 0.068(3) Uani 1 1 d . . . . .
H10G H 0.5670 0.8643 0.5087 0.102 Uiso 1 1 d GR . . . .
H10H H 0.5418 0.8536 0.4622 0.102 Uiso 1 1 d GR . . . .
O106 O 0.4998(6) 1.0764(7) 0.4503(3) 0.066(3) Uani 1 1 d . . . . .
O107 O 1.1918(7) 0.1892(9) 0.4776(4) 0.089(4) Uani 1 1 d . . . . .
H10I H 1.2430 0.1900 0.4731 0.134 Uiso 1 1 d GR . . . .
H10J H 1.1961 0.2093 0.5064 0.134 Uiso 1 1 d GR . . . .
O108 O 1.3168(10) 0.0190(12) 0.4818(4) 0.135(7) Uani 1 1 d . . . . .
H10K H 1.3068 0.0832 0.4967 0.203 Uiso 1 1 d GR . . . .
H10L H 1.2704 0.0121 0.4582 0.203 Uiso 1 1 d GR . . . .
Br1A Br 0.8061(6) 0.2165(8) 0.5279(3) 0.0351(4) Uani 0.117(3) 1 d . . P D 2
K2A K 1.2259(19) 0.749(3) 0.3765(14) 0.025(2) Uani 0.25(11) 1 d . . P C 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
K3 O59 2.802(6) . ?
K3 O45 2.783(7) . ?
K3 O29 2.651(7) . ?
K3 N52 3.036(7) . ?
K3 O50 2.725(7) . ?
K3 O101 2.777(12) . ?
S90 O91 1.447(6) . ?
S90 O92 1.469(6) . ?
S90 O93 1.460(7) . ?
S90 C89 1.773(8) . ?
S69 O70 1.460(6) . ?
S69 O71 1.478(6) . ?
S69 O72 1.464(7) . ?
S69 C68 1.762(8) . ?
S69 K7 3.565(3) . ?
K6 O66 2.838(6) . ?
K6 O80 2.767(6) . ?
K6 O70 2.769(6) 1_565 ?
K6 O49 2.704(7) 1_565 ?
K6 O64 3.036(8) . ?
K6 O105 2.770(9) . ?
S48 O50 1.445(7) . ?
S48 O49 1.430(7) . ?
S48 C47 1.763(8) . ?
S48 O51 1.473(8) . ?
S84 O86 1.460(6) . ?
S84 O85 1.457(6) . ?
S84 O87 1.461(6) . ?
S84 C83 1.778(8) . ?
S84 K8 3.414(3) 3_666 ?
S84 K5 3.513(3) . ?
S84 K7 3.444(3) . ?
S42 O45 1.438(6) . ?
S42 O44 1.497(8) . ?
S42 O43 1.428(8) . ?
S42 C41 1.760(9) . ?
S42 K4 3.491(3) . ?
S42 K5 3.684(3) 3_766 ?
S27 O29 1.451(7) . ?
S27 O30 1.438(7) . ?
S27 O28 1.481(8) . ?
S27 C26 1.778(9) . ?
S27 K2 3.473(11) 1_545 ?
S27 K1 3.414(3) . ?
S27 K2A 3.54(3) 1_545 ?
S21 O24 1.468(6) . ?
S21 O22 1.423(8) . ?
S21 O23 1.464(7) . ?
S21 C20 1.768(9) . ?
S21 K8 3.491(3) 3_766 ?
S21 K5 3.307(3) 3_766 ?
S017 O66 1.457(7) . ?
S017 O65 1.444(7) . ?
S017 C62 1.755(8) . ?
S017 O64 1.461(7) . ?
S017 K5 3.604(3) . ?
O38 C37 1.377(10) . ?
O38 C39 1.416(10) . ?
O38 K2 3.01(3) . ?
O38 K2A 2.73(4) . ?
O17 C16 1.367(11) . ?
O17 C18 1.423(11) . ?
O17 K9 2.786(6) 1_645 ?
O86 K8 2.971(6) 3_666 ?
O86 K9 2.804(6) 1_545 ?
O86 K7 3.024(6) . ?
O66 K5 2.797(7) . ?
O80 C79 1.382(10) . ?
O80 C81 1.444(10) . ?
O24 K2 2.829(12) . ?
O24 K5 2.858(6) 3_766 ?
O24 K2A 2.89(4) . ?
O59 C58 1.382(11) . ?
O59 C60 1.429(10) . ?
O45 K4 2.936(7) . ?
O85 K5 2.941(7) . ?
O85 K7 2.914(6) . ?
N31 C32 1.433(11) . ?
N31 C40 1.465(10) . ?
N31 C46 1.488(10) 1_565 ?
N31 K2 2.998(13) . ?
N31 K2A 2.96(3) . ?
N10 C11 1.418(11) . ?
N10 C19 1.470(10) . ?
N10 C25 1.482(11) . ?
N10 K9 2.987(7) 1_645 ?
O91 K9 2.715(7) . ?
O70 K6 2.769(6) 1_545 ?
C53 N52 1.433(11) . ?
C53 C58 1.412(12) . ?
C53 C54 1.385(12) . ?
C74 N73 1.429(11) . ?
C74 C79 1.414(12) . ?
C74 C75 1.406(12) . ?
N73 C82 1.463(10) . ?
N73 C88 1.485(10) . ?
O29 K1 3.002(9) . ?
O71 K9 2.628(6) 1_545 ?
O71 K7 3.178(7) . ?
O92 K2 2.723(18) 1_455 ?
O92 K2A 2.60(4) 1_455 ?
C11 C16 1.416(13) . ?
C11 C12 1.402(13) . ?
O87 K8 2.856(6) . ?
O87 K8 2.781(6) 3_666 ?
O87 K5 2.959(6) . ?
C79 C78 1.402(12) . ?
N52 C61 1.468(11) . ?
N52 C67 1.477(10) . ?
O72 K7 2.821(7) . ?
O65 K4 2.723(8) . ?
O65 K4 2.823(7) 3_766 ?
C36 H36 0.9500 . ?
C36 C37 1.384(13) . ?
C36 C35 1.367(15) . ?
O30 K2 2.849(13) 1_545 ?
O30 K2A 2.81(3) 1_545 ?
O22 K8 2.880(7) 1_655 ?
O22 K8 3.132(9) 3_766 ?
C32 C33 1.387(12) . ?
C32 C37 1.434(11) . ?
C33 H33 0.9500 . ?
C33 C34 1.408(13) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(15) . ?
C13 C12 1.373(13) . ?
C57 H57 0.9500 . ?
C57 C56 1.366(14) . ?
C57 C58 1.379(13) . ?
O49 K6 2.705(7) 1_545 ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.541(11) . ?
C56 H56 0.9500 . ?
C56 C55 1.386(14) . ?
C75 H75 0.9500 . ?
C75 C76 1.385(13) . ?
C76 H76 0.9500 . ?
C76 C77 1.402(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.373(14) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.535(11) . ?
C55 H55 0.9500 . ?
C55 C54 1.400(13) . ?
O44 K4 2.858(8) . ?
O44 K4 2.812(8) 3_766 ?
O44 K5 2.794(7) 3_766 ?
C16 C15 1.397(12) . ?
C78 H78 0.9500 . ?
C78 C77 1.345(14) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.543(11) . ?
C40 K2 3.220(12) . ?
C40 K2A 3.23(3) . ?
C54 H54 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.376(14) . ?
O23 K8 2.726(7) 3_766 ?
O23 K5 2.723(7) 3_766 ?
C14 H14 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.549(12) . ?
C19 K9 3.200(8) 1_645 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.531(12) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
O43 K5 3.395(12) 3_766 ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.527(11) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C12 H12 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C35 H35 0.9500 . ?
C77 H77 0.9500 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C46 1.522(11) . ?
O28 K2 2.89(2) 1_545 ?
O28 K1 2.836(8) . ?
O28 K2A 3.06(4) 1_545 ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C46 N31 1.488(10) 1_545 ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 K2A 3.54(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
O51 K1 2.719(9) . ?
K8 O87 2.781(6) 3_666 ?
K8 O22 2.880(7) 1_455 ?
K8 O23 2.726(7) 3_766 ?
K8 O104 2.835(7) . ?
K8 O103 2.734(9) . ?
K9 O17 2.786(6) 1_465 ?
K9 O71 2.628(6) 1_565 ?
K9 O106 2.704(9) . ?
K4 O65 2.823(7) 3_766 ?
K4 O44 2.812(8) 3_766 ?
K4 O102 2.681(8) . ?
K4 H10A 3.0832 . ?
K4 H10B 3.0848 . ?
K2 O92 2.723(18) 1_655 ?
K2 O30 2.849(13) 1_565 ?
K2 O28 2.89(2) 1_565 ?
K5 O24 2.858(6) 3_766 ?
K5 O44 2.794(7) 3_766 ?
K5 O23 2.723(7) 3_766 ?
K1 O100 2.650(8) . ?
K1 H10E 3.0631 . ?
K1 H10F 3.0658 . ?
K1 O101 2.811(11) . ?
K1 O107 2.925(13) . ?
K1 H10L 2.7641 . ?
K7 O104 2.773(7) 3_666 ?
K7 O106 2.873(11) 1_545 ?
K7 O108 2.828(13) 3_756 ?
Br1 K2 3.64(3) 3_766 ?
Br1 K1 3.309(3) 3_756 ?
O102 H10A 0.8728 . ?
O102 H10B 0.8723 . ?
O104 K7 2.773(7) 3_666 ?
O105 H10C 0.8743 . ?
O105 H10D 0.8748 . ?
O100 H10E 0.8813 . ?
O100 H10F 0.8806 . ?
O103 H10G 0.9339 . ?
O103 H10H 0.9325 . ?
O106 K7 2.873(11) 1_565 ?
O107 H10I 0.9647 . ?
O107 H10J 0.9666 . ?
O108 K7 2.828(13) 3_756 ?
O108 H10K 1.0087 . ?
O108 H10L 1.0075 . ?
Br1A K1 3.044(9) 3_756 ?
Br1A K2A 3.34(5) 3_766 ?
K2A S27 3.54(3) 1_565 ?
K2A O92 2.60(4) 1_655 ?
K2A O30 2.81(3) 1_565 ?
K2A O28 3.06(4) 1_565 ?
K2A K1 4.83(4) 1_565 ?
K2A Br1A 3.34(5) 3_766 ?

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
O59 K3 N52 54.60(17) . . ?
O45 K3 O59 90.60(19) . . ?
O45 K3 N52 89.38(19) . . ?
O29 K3 O59 111.7(2) . . ?
O29 K3 O45 99.1(2) . . ?
O29 K3 N52 164.3(2) . . ?
O29 K3 O50 88.9(2) . . ?
O29 K3 O101 97.0(3) . . ?
O50 K3 O59 100.8(2) . . ?
O50 K3 O45 162.7(2) . . ?
O50 K3 N52 86.71(19) . . ?
O50 K3 O101 100.8(3) . . ?
O101 K3 O59 144.2(3) . . ?
O101 K3 O45 63.1(3) . . ?
O101 K3 N52 98.7(3) . . ?
O91 S90 O92 113.8(4) . . ?
O91 S90 O93 112.6(4) . . ?
O91 S90 C89 106.2(4) . . ?
O92 S90 C89 107.1(4) . . ?
O93 S90 O92 110.3(4) . . ?
O93 S90 C89 106.3(4) . . ?
O70 S69 O71 113.7(4) . . ?
O70 S69 O72 112.4(4) . . ?
O70 S69 C68 107.0(4) . . ?
O70 S69 K7 142.8(3) . . ?
O71 S69 C68 106.9(4) . . ?
O71 S69 K7 62.9(3) . . ?
O72 S69 O71 110.3(4) . . ?
O72 S69 C68 106.0(4) . . ?
O72 S69 K7 48.7(3) . . ?
C68 S69 K7 109.2(3) . . ?
O66 K6 O64 48.26(18) . . ?
O80 K6 O66 92.38(18) . . ?
O80 K6 O70 110.83(18) . 1_565 ?
O80 K6 O64 74.47(19) . . ?
O80 K6 O105 136.8(3) . . ?
O70 K6 O66 150.01(19) 1_565 . ?
O70 K6 O64 154.83(19) 1_565 . ?
O70 K6 O105 74.4(2) 1_565 . ?
O49 K6 O66 95.1(2) 1_565 . ?
O49 K6 O80 122.6(2) 1_565 . ?
O49 K6 O70 88.29(19) 1_565 1_565 ?
O49 K6 O64 69.3(2) 1_565 . ?
O49 K6 O105 100.0(3) 1_565 . ?
O105 K6 O66 75.7(2) . . ?
O105 K6 O64 119.5(2) . . ?
O50 S48 K3 43.5(3) . . ?
O50 S48 C47 106.6(4) . . ?
O50 S48 O51 110.4(5) . . ?
O49 S48 K3 135.2(3) . . ?
O49 S48 O50 112.8(4) . . ?
O49 S48 C47 109.3(4) . . ?
O49 S48 O51 112.1(5) . . ?
C47 S48 K3 114.0(3) . . ?
O51 S48 K3 67.1(4) . . ?
O51 S48 C47 105.3(4) . . ?
O86 S84 O87 112.8(4) . . ?
O86 S84 C83 107.0(4) . . ?
O86 S84 K8 60.2(2) . 3_666 ?
O86 S84 K5 137.9(2) . . ?
O86 S84 K7 61.2(2) . . ?
O85 S84 O86 112.1(4) . . ?
O85 S84 O87 111.2(4) . . ?
O85 S84 C83 108.3(4) . . ?
O85 S84 K8 130.6(3) . 3_666 ?
O85 S84 K5 55.4(3) . . ?
O85 S84 K7 56.8(2) . . ?
O87 S84 C83 105.0(4) . . ?
O87 S84 K8 52.6(3) . 3_666 ?
O87 S84 K5 56.1(3) . . ?
O87 S84 K7 109.3(3) . . ?
C83 S84 K8 120.7(3) . 3_666 ?
C83 S84 K5 115.1(3) . . ?
C83 S84 K7 145.7(3) . . ?
K8 S84 K5 95.98(7) 3_666 . ?
K8 S84 K7 83.15(6) 3_666 . ?
K7 S84 K5 83.27(6) . . ?
O45 S42 O44 108.8(4) . . ?
O45 S42 C41 107.9(4) . . ?
O45 S42 K4 55.9(3) . . ?
O45 S42 K5 138.1(3) . 3_766 ?
O44 S42 C41 103.4(4) . . ?
O44 S42 K4 53.2(3) . . ?
O44 S42 K5 43.4(3) . 3_766 ?
O43 S42 O45 116.6(5) . . ?
O43 S42 O44 109.5(6) . . ?
O43 S42 C41 109.8(5) . . ?
O43 S42 K4 136.9(4) . . ?
O43 S42 K5 67.1(5) . 3_766 ?
C41 S42 K4 112.7(3) . . ?
C41 S42 K5 109.2(3) . 3_766 ?
K4 S42 K5 91.75(8) . 3_766 ?
O29 S27 O28 113.5(5) . . ?
O29 S27 C26 108.4(4) . . ?
O29 S27 K2 133.5(5) . 1_545 ?
O29 S27 K1 61.4(3) . . ?
O29 S27 K2A 136.1(7) . 1_545 ?
O30 S27 O29 113.4(4) . . ?
O30 S27 O28 107.8(5) . . ?
O30 S27 C26 106.9(4) . . ?
O30 S27 K2 53.0(6) . 1_545 ?
O30 S27 K1 113.7(3) . . ?
O30 S27 K2A 48.8(8) . 1_545 ?
O28 S27 C26 106.5(4) . . ?
O28 S27 K2 54.9(6) . 1_545 ?
O28 S27 K1 55.0(3) . . ?
O28 S27 K2A 59.2(8) . 1_545 ?
C26 S27 K2 118.0(4) . 1_545 ?
C26 S27 K1 138.9(3) . . ?
C26 S27 K2A 115.1(7) . 1_545 ?
K1 S27 K2 83.1(5) . 1_545 ?
K1 S27 K2A 87.9(7) . 1_545 ?
O24 S21 C20 106.2(4) . . ?
O24 S21 K8 135.9(3) . 3_766 ?
O24 S21 K5 59.5(3) . 3_766 ?
O22 S21 O24 112.4(4) . . ?
O22 S21 O23 111.1(5) . . ?
O22 S21 C20 109.7(4) . . ?
O22 S21 K8 63.7(3) . 3_766 ?
O22 S21 K5 127.5(3) . 3_766 ?
O23 S21 O24 113.4(4) . . ?
O23 S21 C20 103.4(4) . . ?
O23 S21 K8 47.5(3) . 3_766 ?
O23 S21 K5 54.2(3) . 3_766 ?
C20 S21 K8 116.5(3) . 3_766 ?
C20 S21 K5 122.6(3) . 3_766 ?
K5 S21 K8 87.25(7) 3_766 3_766 ?
K6 S017 K5 97.39(7) . . ?
O66 S017 K6 51.9(3) . . ?
O66 S017 C62 106.9(4) . . ?
O66 S017 O64 111.2(4) . . ?
O66 S017 K5 46.0(3) . . ?
O65 S017 K6 139.6(3) . . ?
O65 S017 O66 113.0(4) . . ?
O65 S017 C62 107.9(4) . . ?
O65 S017 O64 112.3(5) . . ?
O65 S017 K5 83.7(3) . . ?
C62 S017 K6 112.4(3) . . ?
C62 S017 K5 84.1(3) . . ?
O64 S017 K6 59.8(3) . . ?
O64 S017 C62 104.9(4) . . ?
O64 S017 K5 157.2(3) . . ?
C37 O38 C39 117.0(7) . . ?
C37 O38 K2 124.5(5) . . ?
C37 O38 K2A 126.4(9) . . ?
C39 O38 K2 115.9(6) . . ?
C39 O38 K2A 113.1(9) . . ?
C16 O17 C18 118.1(7) . . ?
C16 O17 K9 126.1(5) . 1_645 ?
C18 O17 K9 112.2(5) . 1_645 ?
S84 O86 K8 94.6(3) . 3_666 ?
S84 O86 K9 136.7(3) . 1_545 ?
S84 O86 K7 93.8(3) . . ?
K8 O86 K7 98.75(17) 3_666 . ?
K9 O86 K8 128.5(2) 1_545 3_666 ?
K9 O86 K7 84.99(16) 1_545 . ?
S017 O66 K6 104.2(3) . . ?
S017 O66 K5 111.9(3) . . ?
K5 O66 K6 142.3(2) . . ?
C79 O80 K6 127.2(5) . . ?
C79 O80 C81 117.1(6) . . ?
C81 O80 K6 109.4(5) . . ?
S21 O24 K2 148.4(7) . . ?
S21 O24 K5 94.2(3) . 3_766 ?
S21 O24 K2A 142.5(10) . . ?
K2 O24 K5 117.4(7) . 3_766 ?
K5 O24 K2A 123.0(9) 3_766 . ?
C58 O59 K3 126.9(5) . . ?
C58 O59 C60 117.0(7) . . ?
C60 O59 K3 112.0(5) . . ?
K3 O45 K4 126.2(2) . . ?
S42 O45 K3 133.6(4) . . ?
S42 O45 K4 100.2(3) . . ?
S84 O85 K5 100.5(3) . . ?
S84 O85 K7 98.4(3) . . ?
K7 O85 K5 104.3(2) . . ?
C32 N31 C40 112.7(6) . . ?
C32 N31 C46 115.8(6) . 1_565 ?
C32 N31 K2 121.1(8) . . ?
C32 N31 K2A 115.0(10) . . ?
C40 N31 C46 111.4(6) . 1_565 ?
C40 N31 K2 85.0(5) . . ?
C40 N31 K2A 86.7(8) . . ?
C46 N31 K2 106.9(7) 1_565 . ?
C46 N31 K2A 111.8(9) 1_565 . ?
C11 N10 C19 112.4(7) . . ?
C11 N10 C25 116.4(7) . . ?
C11 N10 K9 115.2(5) . 1_645 ?
C19 N10 C25 112.1(6) . . ?
C19 N10 K9 84.5(4) . 1_645 ?
C25 N10 K9 112.0(5) . 1_645 ?
S90 O91 K9 130.2(4) . . ?
S69 O70 K6 129.4(3) . 1_545 ?
C58 C53 N52 118.3(7) . . ?
C54 C53 N52 123.5(8) . . ?
C54 C53 C58 118.1(8) . . ?
C79 C74 N73 118.4(7) . . ?
C75 C74 N73 123.5(7) . . ?
C75 C74 C79 118.0(8) . . ?
C74 N73 K6 112.5(5) . . ?
C74 N73 C82 113.7(6) . . ?
C74 N73 C88 115.7(6) . . ?
C82 N73 K6 86.9(4) . . ?
C82 N73 C88 111.2(6) . . ?
C88 N73 K6 113.6(5) . . ?
K3 O29 K1 84.7(2) . . ?
S27 O29 K3 167.5(5) . . ?
S27 O29 K1 93.5(4) . . ?
S69 O71 K9 157.8(4) . 1_545 ?
S69 O71 K7 92.6(3) . . ?
K9 O71 K7 84.92(18) 1_545 . ?
S90 O92 K2 146.9(7) . 1_455 ?
S90 O92 K2A 152.5(10) . 1_455 ?
C16 C11 N10 119.1(8) . . ?
C12 C11 N10 123.8(8) . . ?
C12 C11 C16 117.1(8) . . ?
S84 O87 K8 102.7(3) . 3_666 ?
S84 O87 K8 146.2(4) . . ?
S84 O87 K5 99.7(3) . . ?
K8 O87 K8 76.29(16) 3_666 . ?
K8 O87 K5 127.5(2) 3_666 . ?
K8 O87 K5 107.6(2) . . ?
O80 C79 C74 115.7(7) . . ?
O80 C79 C78 125.0(7) . . ?
C78 C79 C74 119.3(8) . . ?
C53 N52 K3 114.8(5) . . ?
C53 N52 C61 112.9(6) . . ?
C53 N52 C67 116.2(6) . . ?
C61 N52 K3 86.2(4) . . ?
C61 N52 C67 110.5(6) . . ?
C67 N52 K3 112.4(5) . . ?
S69 O72 K7 108.4(3) . . ?
S017 O65 K4 145.5(5) . . ?
S017 O65 K4 133.8(4) . 3_766 ?
K4 O65 K4 73.2(2) . 3_766 ?
C37 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C35 C36 C37 121.0(8) . . ?
S27 O30 K2 103.2(7) . 1_545 ?
S27 O30 K2A 108.5(10) . 1_545 ?
S21 O22 K8 92.3(4) . 3_766 ?
S21 O22 K8 126.2(4) . 1_655 ?
K8 O22 K8 70.66(18) 1_655 3_766 ?
S48 O50 K3 115.1(4) . . ?
N31 C32 C37 117.8(7) . . ?
C33 C32 N31 123.5(7) . . ?
C33 C32 C37 118.6(8) . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.2(8) . . ?
C34 C33 H33 119.9 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(8) . . ?
O38 C37 C36 125.3(8) . . ?
O38 C37 C32 115.4(7) . . ?
C36 C37 C32 119.4(8) . . ?
C56 C57 H57 119.5 . . ?
C56 C57 C58 120.9(8) . . ?
C58 C57 H57 119.5 . . ?
S48 O49 K6 168.3(5) . 1_545 ?
K6 C82 H82A 74.6 . . ?
K6 C82 H82B 66.5 . . ?
N73 C82 K6 67.2(4) . . ?
N73 C82 H82A 108.7 . . ?
N73 C82 H82B 108.7 . . ?
N73 C82 C83 114.4(6) . . ?
H82A C82 H82B 107.6 . . ?
C83 C82 K6 175.0(6) . . ?
C83 C82 H82A 108.7 . . ?
C83 C82 H82B 108.7 . . ?
C57 C56 H56 119.9 . . ?
C57 C56 C55 120.2(8) . . ?
C55 C56 H56 119.9 . . ?
O59 C58 C53 115.4(8) . . ?
C57 C58 O59 124.3(8) . . ?
C57 C58 C53 120.3(8) . . ?
C74 C75 H75 119.6 . . ?
C76 C75 C74 120.7(8) . . ?
C76 C75 H75 119.6 . . ?
C75 C76 H76 119.8 . . ?
C75 C76 C77 120.3(8) . . ?
C77 C76 H76 119.8 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0(8) . . ?
C35 C34 H34 120.0 . . ?
N73 C88 H88A 109.4 . . ?
N73 C88 H88B 109.4 . . ?
N73 C88 C89 111.4(6) . . ?
H88A C88 H88B 108.0 . . ?
C89 C88 H88A 109.4 . . ?
C89 C88 H88B 109.4 . . ?
C56 C55 H55 120.3 . . ?
C56 C55 C54 119.4(8) . . ?
C54 C55 H55 120.3 . . ?
S42 O44 K4 137.8(4) . 3_766 ?
S42 O44 K4 101.9(3) . . ?
S42 O44 K5 114.9(4) . 3_766 ?
K4 O44 K4 71.4(2) 3_766 . ?
K5 O44 K4 97.6(2) 3_766 3_766 ?
K5 O44 K4 131.4(3) 3_766 . ?
O17 C16 C11 115.8(7) . . ?
O17 C16 C15 124.0(8) . . ?
C15 C16 C11 120.2(8) . . ?
C79 C78 H78 118.9 . . ?
C77 C78 C79 122.2(8) . . ?
C77 C78 H78 118.9 . . ?
N31 C40 H40A 108.7 . . ?
N31 C40 H40B 108.7 . . ?
N31 C40 C41 114.0(6) . . ?
N31 C40 K2 68.1(5) . . ?
N31 C40 K2A 66.4(7) . . ?
H40A C40 H40B 107.6 . . ?
C41 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C41 C40 K2 175.4(8) . . ?
C41 C40 K2A 178.6(10) . . ?
K2 C40 H40A 66.7 . . ?
K2 C40 H40B 73.8 . . ?
C53 C54 C55 121.0(8) . . ?
C53 C54 H54 119.5 . . ?
C55 C54 H54 119.5 . . ?
C16 C15 H15 119.7 . . ?
C14 C15 C16 120.7(9) . . ?
C14 C15 H15 119.7 . . ?
S21 O23 K8 109.1(4) . 3_766 ?
S21 O23 K5 100.0(3) . 3_766 ?
K5 O23 K8 118.9(2) 3_766 3_766 ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.9(9) . . ?
C15 C14 H14 120.1 . . ?
N10 C19 H19A 108.5 . . ?
N10 C19 H19B 108.5 . . ?
N10 C19 C20 115.2(7) . . ?
N10 C19 K9 68.3(4) . 1_645 ?
H19A C19 H19B 107.5 . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C20 C19 K9 174.2(6) . 1_645 ?
K9 C19 H19A 65.8 1_645 . ?
K9 C19 H19B 73.8 1_645 . ?
O17 C18 H18A 109.5 . . ?
O17 C18 H18B 109.5 . . ?
O17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
K3 C61 H61A 76.0 . . ?
K3 C61 H61B 65.3 . . ?
N52 C61 K3 67.3(4) . . ?
N52 C61 H61A 108.8 . . ?
N52 C61 H61B 108.8 . . ?
N52 C61 C62 114.0(7) . . ?
H61A C61 H61B 107.6 . . ?
C62 C61 K3 173.7(6) . . ?
C62 C61 H61A 108.8 . . ?
C62 C61 H61B 108.8 . . ?
S017 C62 H62A 109.1 . . ?
S017 C62 H62B 109.1 . . ?
C61 C62 S017 112.6(6) . . ?
C61 C62 H62A 109.1 . . ?
C61 C62 H62B 109.1 . . ?
H62A C62 H62B 107.8 . . ?
S42 O43 K5 90.1(5) . 3_766 ?
N52 C67 H67A 109.5 . . ?
N52 C67 H67B 109.5 . . ?
N52 C67 C68 110.9(7) . . ?
H67A C67 H67B 108.1 . . ?
C68 C67 H67A 109.5 . . ?
C68 C67 H67B 109.5 . . ?
S84 C83 H83A 109.1 . . ?
S84 C83 H83B 109.1 . . ?
C82 C83 S84 112.6(6) . . ?
C82 C83 H83A 109.1 . . ?
C82 C83 H83B 109.1 . . ?
H83A C83 H83B 107.8 . . ?
C11 C12 H12 118.9 . . ?
C13 C12 C11 122.1(8) . . ?
C13 C12 H12 118.9 . . ?
S21 C20 H20A 109.6 . . ?
S21 C20 H20B 109.6 . . ?
C19 C20 S21 110.4(6) . . ?
C19 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C36 C35 C34 120.8(8) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C76 C77 H77 120.3 . . ?
C78 C77 C76 119.3(8) . . ?
C78 C77 H77 120.3 . . ?
S48 C47 H47A 109.1 . . ?
S48 C47 H47B 109.1 . . ?
H47A C47 H47B 107.9 . . ?
C46 C47 S48 112.3(6) . . ?
C46 C47 H47A 109.1 . . ?
C46 C47 H47B 109.1 . . ?
S27 O28 K2 100.3(6) . 1_545 ?
S27 O28 K1 99.7(4) . . ?
S27 O28 K2A 96.2(8) . 1_545 ?
K1 O28 K2 105.9(5) . 1_545 ?
K1 O28 K2A 109.9(8) . 1_545 ?
S90 C89 H89A 109.4 . . ?
S90 C89 H89B 109.4 . . ?
C88 C89 S90 111.4(6) . . ?
C88 C89 H89A 109.4 . . ?
C88 C89 H89B 109.4 . . ?
H89A C89 H89B 108.0 . . ?
O59 C60 H60A 109.5 . . ?
O59 C60 H60B 109.5 . . ?
O59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
S42 C41 H41A 109.3 . . ?
S42 C41 H41B 109.3 . . ?
C40 C41 S42 111.8(6) . . ?
C40 C41 H41A 109.3 . . ?
C40 C41 H41B 109.3 . . ?
H41A C41 H41B 107.9 . . ?
K6 C81 H81A 107.8 . . ?
K6 C81 H81B 141.6 . . ?
K6 C81 H81C 65.3 . . ?
O80 C81 K6 47.8(4) . . ?
O80 C81 H81A 109.5 . . ?
O80 C81 H81B 109.5 . . ?
O80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N31 C46 C47 110.9(6) 1_545 . ?
N31 C46 H46A 109.5 1_545 . ?
N31 C46 H46B 109.5 1_545 . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 108.0 . . ?
O38 C39 H39A 109.5 . . ?
O38 C39 H39B 109.5 . . ?
O38 C39 H39C 109.5 . . ?
O38 C39 K2A 45.3(7) . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
K2A C39 H39A 133.7 . . ?
K2A C39 H39B 65.3 . . ?
K2A C39 H39C 115.5 . . ?
N10 C25 H25A 109.4 . . ?
N10 C25 H25B 109.4 . . ?
N10 C25 C26 111.3(7) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
S27 C26 H26A 109.0 . . ?
S27 C26 H26B 109.0 . . ?
C25 C26 S27 112.7(6) . . ?
C25 C26 H26A 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
S017 O64 K6 95.6(3) . . ?
S69 C68 H68A 109.3 . . ?
S69 C68 H68B 109.3 . . ?
C67 C68 S69 111.6(6) . . ?
C67 C68 H68A 109.3 . . ?
C67 C68 H68B 109.3 . . ?
H68A C68 H68B 108.0 . . ?
S48 O51 K3 88.6(4) . . ?
S48 O51 K1 147.5(5) . . ?
K1 O51 K3 78.0(2) . . ?
O87 K8 O87 103.71(16) 3_666 . ?
O87 K8 O22 76.2(2) 3_666 1_455 ?
O87 K8 O22 65.60(18) . 1_455 ?
O87 K8 O104 77.39(19) 3_666 . ?
O23 K8 O87 110.0(2) 3_766 3_666 ?
O23 K8 O87 63.76(19) 3_766 . ?
O23 K8 O22 129.0(2) 3_766 1_455 ?
O23 K8 O104 158.8(2) 3_766 . ?
O23 K8 O103 87.5(3) 3_766 . ?
O104 K8 O87 135.24(18) . . ?
O104 K8 O22 71.57(19) . 1_455 ?
O103 K8 O87 119.5(3) . . ?
O103 K8 O87 136.6(3) . 3_666 ?
O103 K8 O22 123.5(3) . 1_455 ?
O103 K8 O104 74.7(2) . . ?
O91 K9 O17 109.54(19) . 1_465 ?
O71 K9 O17 108.4(2) 1_565 1_465 ?
O71 K9 O91 93.52(19) 1_565 . ?
O71 K9 O106 87.3(3) 1_565 . ?
O106 K9 O17 157.8(3) . 1_465 ?
O106 K9 O91 84.2(2) . . ?
O45 K4 H10A 90.7 . . ?
O45 K4 H10B 73.4 . . ?
O65 K4 O45 112.3(2) 3_766 . ?
O65 K4 O45 72.3(2) . . ?
O65 K4 O65 106.8(2) . 3_766 ?
O65 K4 O44 68.2(2) . 3_766 ?
O65 K4 O44 72.4(2) . . ?
O65 K4 O44 66.2(2) 3_766 . ?
O65 K4 H10A 70.0 3_766 . ?
O65 K4 H10A 160.3 . . ?
O65 K4 H10B 61.0 3_766 . ?
O65 K4 H10B 134.3 . . ?
O44 K4 O45 48.63(19) . . ?
O44 K4 O45 139.4(2) 3_766 . ?
O44 K4 O65 71.7(2) 3_766 3_766 ?
O44 K4 O44 108.6(2) 3_766 . ?
O44 K4 H10A 125.9 3_766 . ?
O44 K4 H10A 89.0 . . ?
O44 K4 H10B 62.3 . . ?
O44 K4 H10B 131.5 3_766 . ?
O102 K4 O45 75.9(2) . . ?
O102 K4 O65 72.3(2) . 3_766 ?
O102 K4 O65 145.0(3) . . ?
O102 K4 O44 137.6(2) . 3_766 ?
O102 K4 O44 75.7(3) . . ?
O102 K4 H10A 15.5 . . ?
O102 K4 H10B 15.5 . . ?
H10A K4 H10B 26.7 . . ?
O24 K2 O38 84.7(5) . . ?
O24 K2 N31 92.4(3) . . ?
O24 K2 O30 176.4(13) . 1_565 ?
O24 K2 O28 134.8(11) . 1_565 ?
N31 K2 O38 53.3(4) . . ?
O92 K2 O38 92.0(10) 1_655 . ?
O92 K2 O24 89.6(4) 1_655 . ?
O92 K2 N31 144.7(13) 1_655 . ?
O92 K2 O30 89.8(5) 1_655 1_565 ?
O92 K2 O28 84.2(3) 1_655 1_565 ?
O30 K2 O38 91.8(8) 1_565 . ?
O30 K2 N31 86.0(4) 1_565 . ?
O30 K2 O28 48.6(3) 1_565 1_565 ?
O28 K2 O38 140.1(8) 1_565 . ?
O28 K2 N31 117.4(5) 1_565 . ?
O66 K5 O24 164.90(18) . 3_766 ?
O66 K5 O85 81.15(18) . . ?
O66 K5 O87 97.59(18) . . ?
O24 K5 O85 107.35(18) 3_766 . ?
O24 K5 O87 80.11(17) 3_766 . ?
O85 K5 O87 48.16(16) . . ?
O44 K5 O66 80.7(2) 3_766 . ?
O44 K5 O24 97.99(19) 3_766 3_766 ?
O44 K5 O85 143.6(2) 3_766 . ?
O44 K5 O87 166.3(2) 3_766 . ?
O23 K5 O66 113.6(2) 3_766 . ?
O23 K5 O24 52.03(18) 3_766 3_766 ?
O23 K5 O85 110.5(2) 3_766 . ?
O23 K5 O87 62.41(19) 3_766 . ?
O23 K5 O44 105.7(2) 3_766 3_766 ?
O29 K1 H10E 160.8 . . ?
O29 K1 H10F 139.6 . . ?
O29 K1 H10L 76.7 . . ?
O28 K1 O29 49.6(2) . . ?
O28 K1 H10E 145.3 . . ?
O28 K1 H10F 131.9 . . ?
O28 K1 O107 83.2(4) . . ?
O28 K1 H10L 37.3 . . ?
O51 K1 O29 79.3(2) . . ?
O51 K1 O28 107.8(2) . . ?
O51 K1 H10E 99.5 . . ?
O51 K1 H10F 120.2 . . ?
O51 K1 O101 68.1(3) . . ?
O51 K1 O107 137.7(3) . . ?
O51 K1 H10L 144.8 . . ?
O100 K1 O29 155.2(3) . . ?
O100 K1 O28 133.0(3) . . ?
O100 K1 O51 115.1(3) . . ?
O100 K1 H10E 15.7 . . ?
O100 K1 H10F 15.7 . . ?
O100 K1 O101 79.2(3) . . ?
O100 K1 O107 78.0(4) . . ?
O100 K1 H10L 97.0 . . ?
H10E K1 H10F 27.1 . . ?
H10E K1 H10L 111.5 . . ?
H10F K1 H10L 94.6 . . ?
O101 K1 O29 88.7(3) . . ?
O101 K1 O28 136.7(3) . . ?
O101 K1 H10E 73.4 . . ?
O101 K1 H10F 70.3 . . ?
O101 K1 O107 76.1(3) . . ?
O101 K1 H10L 135.9 . . ?
O107 K1 O29 78.1(3) . . ?
O107 K1 H10E 90.9 . . ?
O107 K1 H10F 63.9 . . ?
O107 K1 H10L 60.3 . . ?
O85 K7 O86 48.06(16) . . ?
O72 K7 O86 123.79(18) . . ?
O72 K7 O85 108.64(18) . . ?
O72 K7 O106 97.6(2) . 1_545 ?
O72 K7 O108 74.4(4) . 3_756 ?
O104 K7 O86 75.50(19) 3_666 . ?
O104 K7 O85 88.49(18) 3_666 . ?
O104 K7 O72 159.8(2) 3_666 . ?
O104 K7 O106 84.8(2) 3_666 1_545 ?
O104 K7 O108 86.2(4) 3_666 3_756 ?
O106 K7 O86 65.8(2) 1_545 . ?
O106 K7 O85 112.9(2) 1_545 . ?
O108 K7 O86 144.3(4) 3_756 . ?
O108 K7 O85 163.1(3) 3_756 . ?
O108 K7 O106 82.5(4) 3_756 1_545 ?
K4 Br1 K2 119.2(2) . 3_766 ?
K4 Br1 K5 79.30(7) . . ?
K4 Br1 K1 109.92(7) . 3_756 ?
K4 Br1 K7 146.49(7) . . ?
K5 Br1 K2 88.26(18) . 3_766 ?
K5 Br1 K7 85.88(5) . . ?
K1 Br1 K2 82.04(19) 3_756 3_766 ?
K1 Br1 K5 169.03(8) 3_756 . ?
K1 Br1 K7 88.97(6) 3_756 . ?
K7 Br1 K2 89.9(2) . 3_766 ?
K4 O102 H10A 109.4 . . ?
K4 O102 H10B 109.6 . . ?
H10A O102 H10B 109.3 . . ?
K7 O104 K8 108.5(2) 3_666 . ?
K6 O105 H10C 109.6 . . ?
K6 O105 H10D 109.5 . . ?
H10C O105 H10D 109.3 . . ?
K1 O100 H10E 109.8 . . ?
K1 O100 H10F 110.0 . . ?
H10E O100 H10F 108.9 . . ?
K3 O101 K1 86.2(3) . . ?
K8 O103 H10G 112.1 . . ?
K8 O103 H10H 111.8 . . ?
H10G O103 H10H 106.7 . . ?
K9 O106 K7 89.8(3) . 1_565 ?
K1 O107 H10I 112.4 . . ?
K1 O107 H10J 113.1 . . ?
H10I O107 H10J 105.9 . . ?
K7 O108 H10K 114.3 3_756 . ?
K7 O108 H10L 114.1 3_756 . ?
H10K O108 H10L 103.9 . . ?
K1 Br1A K5 165.1(5) 3_756 . ?
K1 Br1A K7 99.8(3) 3_756 . ?
K1 Br1A K2A 98.2(7) 3_756 3_766 ?
K7 Br1A K5 85.8(2) . . ?
K7 Br1A K2A 109.3(7) . 3_766 ?
K2A Br1A K5 92.9(6) 3_766 . ?
S27 K2A C39 123.1(12) 1_565 . ?
S27 K2A K1 45.0(5) 1_565 1_565 ?
O38 K2A S27 121.3(13) . 1_565 ?
O38 K2A O24 88.8(10) . . ?
O38 K2A N31 56.3(7) . . ?
O38 K2A O30 98.8(13) . 1_565 ?
O38 K2A C40 60.2(7) . . ?
O38 K2A O28 145.9(14) . 1_565 ?
O38 K2A C39 21.6(4) . . ?
O38 K2A K1 138.6(10) . 1_565 ?
O38 K2A Br1A 136.5(12) . 3_766 ?
O24 K2A S27 149.6(16) . 1_565 ?
O24 K2A N31 92.1(10) . . ?
O24 K2A C40 65.1(7) . . ?
O24 K2A O28 125.1(15) . 1_565 ?
O24 K2A C39 86.0(10) . . ?
O24 K2A K1 110.5(12) . 1_565 ?
O24 K2A Br1A 71.9(10) . 3_766 ?
N31 K2A S27 101.6(9) . 1_565 ?
N31 K2A C40 27.0(3) . . ?
N31 K2A O28 113.3(12) . 1_565 ?
N31 K2A C39 77.8(9) . . ?
N31 K2A K1 85.8(9) . 1_565 ?
N31 K2A Br1A 85.1(10) . 3_766 ?
O92 K2A S27 86.9(9) 1_655 1_565 ?
O92 K2A O38 101.2(15) 1_655 . ?
O92 K2A O24 90.8(10) 1_655 . ?
O92 K2A N31 157.2(19) 1_655 . ?
O92 K2A O30 93.2(11) 1_655 1_565 ?
O92 K2A C40 148.3(14) 1_655 . ?
O92 K2A O28 82.9(10) 1_655 1_565 ?
O92 K2A C39 79.9(11) 1_655 . ?
O92 K2A K1 114.2(11) 1_655 1_565 ?
O92 K2A Br1A 117.2(14) 1_655 3_766 ?
O30 K2A S27 22.7(3) 1_565 1_565 ?
O30 K2A O24 170.6(19) 1_565 . ?
O30 K2A N31 87.5(10) 1_565 . ?
O30 K2A C40 113.8(11) 1_565 . ?
O30 K2A O28 47.2(6) 1_565 1_565 ?
O30 K2A C39 103.0(13) 1_565 . ?
O30 K2A K1 60.1(8) 1_565 1_565 ?
O30 K2A Br1A 98.7(12) 1_565 3_766 ?
C40 K2A S27 124.4(11) . 1_565 ?
C40 K2A C39 78.3(9) . . ?
C40 K2A K1 94.2(9) . 1_565 ?
C40 K2A Br1A 76.2(9) . 3_766 ?
O28 K2A S27 24.6(3) 1_565 1_565 ?
O28 K2A C40 127.3(13) 1_565 . ?
O28 K2A C39 144.5(13) 1_565 . ?
O28 K2A K1 33.5(5) 1_565 1_565 ?
O28 K2A Br1A 63.5(9) 1_565 3_766 ?
C39 K2A K1 157.2(10) . 1_565 ?
Br1A K2A S27 82.3(9) 3_766 1_565 ?
Br1A K2A C39 151.6(11) 3_766 . ?
Br1A K2A K1 38.6(5) 3_766 1_565 ?

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
K3 S48 O49 K6 69(3) . . . 1_545 ?
K3 S48 C47 C46 136.5(5) . . . . ?
K3 S48 O51 K1 -64.9(9) . . . . ?
K3 O59 C58 C53 24.6(10) . . . . ?
K3 O59 C58 C57 -155.3(6) . . . . ?
K3 N52 C61 C62 -173.3(7) . . . . ?
K3 N52 C67 C68 -71.5(7) . . . . ?
K6 S017 O66 K5 169.2(4) . . . . ?
K6 S017 O65 K4 135.5(5) . . . . ?
K6 S017 O65 K4 2.0(9) . . . 3_766 ?
K6 S017 C62 C61 142.9(5) . . . . ?
K6 O80 C79 C74 -27.9(9) . . . . ?
K6 O80 C79 C78 150.3(7) . . . . ?
K6 N73 C82 C83 -174.9(6) . . . . ?
K6 N73 C88 C89 67.1(7) . . . . ?
S48 C47 C46 N31 -175.2(5) . . . 1_545 ?
O17 C16 C15 C14 176.9(8) . . . . ?
O86 S84 O85 K5 -133.8(3) . . . . ?
O86 S84 O85 K7 -27.5(4) . . . . ?
O86 S84 O87 K8 -83.0(7) . . . . ?
O86 S84 O87 K8 1.3(4) . . . 3_666 ?
O86 S84 O87 K5 133.4(3) . . . . ?
O86 S84 C83 C82 -178.0(6) . . . . ?
O66 S017 O65 K4 77.8(8) . . . . ?
O66 S017 O65 K4 -55.7(7) . . . 3_766 ?
O66 S017 C62 C61 -162.0(6) . . . . ?
O66 S017 O64 K6 -7.8(4) . . . . ?
O80 C79 C78 C77 -176.0(8) . . . . ?
O24 S21 O22 K8 63.9(6) . . . 1_655 ?
O24 S21 O22 K8 131.5(3) . . . 3_766 ?
O24 S21 O23 K8 -131.6(3) . . . 3_766 ?
O24 S21 O23 K5 -6.1(4) . . . 3_766 ?
O24 S21 C20 C19 177.5(6) . . . . ?
O45 S42 O44 K4 -6.0(4) . . . . ?
O45 S42 O44 K4 -81.4(6) . . . 3_766 ?
O45 S42 O44 K5 141.6(4) . . . 3_766 ?
O45 S42 O43 K5 -133.8(4) . . . 3_766 ?
O45 S42 C41 C40 -179.2(6) . . . . ?
O85 S84 O86 K8 125.3(3) . . . 3_666 ?
O85 S84 O86 K9 -60.5(6) . . . 1_545 ?
O85 S84 O86 K7 26.2(4) . . . . ?
O85 S84 O87 K8 -125.7(3) . . . 3_666 ?
O85 S84 O87 K8 150.1(6) . . . . ?
O85 S84 O87 K5 6.5(4) . . . . ?
O85 S84 C83 C82 -56.9(7) . . . . ?
N31 C32 C33 C34 -178.9(8) . . . . ?
N31 C32 C37 O38 -3.0(10) . . . . ?
N31 C32 C37 C36 176.7(7) . . . . ?
N31 C40 C41 S42 -169.9(6) . . . . ?
N10 C11 C16 O17 3.3(11) . . . . ?
N10 C11 C16 C15 -177.5(7) . . . . ?
N10 C11 C12 C13 -179.6(8) . . . . ?
N10 C19 C20 S21 161.1(6) . . . . ?
N10 C25 C26 S27 176.9(6) . . . . ?
O91 S90 O92 K2 -80.3(10) . . . 1_455 ?
O91 S90 O92 K2A -74(2) . . . 1_455 ?
O91 S90 C89 C88 -179.8(6) . . . . ?
O70 S69 O71 K9 55.9(11) . . . 1_545 ?
O70 S69 O71 K7 138.8(3) . . . . ?
O70 S69 O72 K7 -141.7(3) . . . . ?
O70 S69 C68 C67 179.1(6) . . . . ?
C53 N52 C61 K3 -115.4(6) . . . . ?
C53 N52 C61 C62 71.4(9) . . . . ?
C53 N52 C67 C68 63.7(9) . . . . ?
C74 N73 C82 K6 113.2(6) . . . . ?
C74 N73 C82 C83 -61.6(9) . . . . ?
C74 N73 C88 C89 -65.2(9) . . . . ?
C74 C79 C78 C77 2.2(13) . . . . ?
C74 C75 C76 C77 4.2(12) . . . . ?
N73 C74 C79 O80 -4.8(10) . . . . ?
N73 C74 C79 C78 176.9(7) . . . . ?
N73 C74 C75 C76 -179.9(7) . . . . ?
N73 C82 C83 S84 -159.9(6) . . . . ?
N73 C88 C89 S90 175.8(5) . . . . ?
O29 S27 O30 K2 -127.9(6) . . . 1_545 ?
O29 S27 O30 K2A -131.7(9) . . . 1_545 ?
O29 S27 O28 K2 127.8(6) . . . 1_545 ?
O29 S27 O28 K1 19.6(5) . . . . ?
O29 S27 O28 K2A 131.0(8) . . . 1_545 ?
O29 S27 C26 C25 50.0(8) . . . . ?
O71 S69 O70 K6 -151.4(4) . . . 1_545 ?
O71 S69 O72 K7 -13.6(4) . . . . ?
O71 S69 C68 C67 56.9(7) . . . . ?
O92 S90 O91 K9 146.9(4) . . . . ?
O92 S90 C89 C88 -57.9(7) . . . . ?
C11 N10 C19 C20 59.9(9) . . . . ?
C11 N10 C19 K9 -115.1(6) . . . 1_645 ?
C11 N10 C25 C26 63.9(9) . . . . ?
C11 C16 C15 C14 -2.3(13) . . . . ?
O87 S84 O86 K8 -1.2(4) . . . 3_666 ?
O87 S84 O86 K9 173.0(4) . . . 1_545 ?
O87 S84 O86 K7 -100.3(3) . . . . ?
O87 S84 O85 K5 -6.5(4) . . . . ?
O87 S84 O85 K7 99.8(3) . . . . ?
O87 S84 C83 C82 61.9(7) . . . . ?
C79 O80 C81 K6 154.1(8) . . . . ?
C79 C74 N73 K6 27.7(8) . . . . ?
C79 C74 N73 C82 -69.1(9) . . . . ?
C79 C74 N73 C88 160.5(7) . . . . ?
C79 C74 C75 C76 -2.5(11) . . . . ?
C79 C78 C77 C76 -0.5(13) . . . . ?
N52 C53 C58 O59 4.8(11) . . . . ?
N52 C53 C58 C57 -175.3(7) . . . . ?
N52 C53 C54 C55 178.1(7) . . . . ?
N52 C61 C62 S017 -164.3(6) . . . . ?
N52 C67 C68 S69 -176.2(6) . . . . ?
O72 S69 O70 K6 -25.1(5) . . . 1_545 ?
O72 S69 O71 K9 -71.5(11) . . . 1_545 ?
O72 S69 O71 K7 11.4(3) . . . . ?
O72 S69 C68 C67 -60.7(7) . . . . ?
O65 S017 O66 K6 135.9(4) . . . . ?
O65 S017 O66 K5 -54.9(5) . . . . ?
O65 S017 C62 C61 -40.1(8) . . . . ?
O65 S017 O64 K6 -135.6(3) . . . . ?
O30 S27 O29 K3 24(3) . . . . ?
O30 S27 O29 K1 105.2(4) . . . . ?
O30 S27 O28 K2 1.4(6) . . . 1_545 ?
O30 S27 O28 K1 -106.8(4) . . . . ?
O30 S27 O28 K2A 4.6(8) . . . 1_545 ?
O30 S27 C26 C25 172.5(6) . . . . ?
O22 S21 O24 K2 61.6(10) . . . . ?
O22 S21 O24 K5 -121.4(4) . . . 3_766 ?
O22 S21 O24 K2A 65.9(13) . . . . ?
O22 S21 O23 K8 -3.8(5) . . . 3_766 ?
O22 S21 O23 K5 121.7(4) . . . 3_766 ?
O22 S21 C20 C19 55.8(8) . . . . ?
O50 S48 O49 K6 23(3) . . . 1_545 ?
O50 S48 C47 C46 -177.7(6) . . . . ?
O50 S48 O51 K3 -4.7(4) . . . . ?
O50 S48 O51 K1 -69.6(9) . . . . ?
C32 N31 C40 C41 -62.8(9) . . . . ?
C32 N31 C40 K2 121.7(8) . . . . ?
C32 N31 C40 K2A 115.8(10) . . . . ?
C32 C33 C34 C35 2.7(13) . . . . ?
C33 C32 C37 O38 179.6(7) . . . . ?
C33 C32 C37 C36 -0.6(12) . . . . ?
C33 C34 C35 C36 -1.3(13) . . . . ?
C37 O38 C39 K2A 160.6(11) . . . . ?
C37 C36 C35 C34 -1.1(14) . . . . ?
C37 C32 C33 C34 -1.8(12) . . . . ?
C57 C56 C55 C54 1.8(13) . . . . ?
O93 S90 O91 K9 20.4(6) . . . . ?
O93 S90 O92 K2 47.4(10) . . . 1_455 ?
O93 S90 O92 K2A 54(2) . . . 1_455 ?
O93 S90 C89 C88 60.0(7) . . . . ?
O49 S48 O50 K3 132.5(4) . . . . ?
O49 S48 C47 C46 -55.5(7) . . . . ?
O49 S48 O51 K3 -131.3(3) . . . . ?
O49 S48 O51 K1 163.8(8) . . . . ?
C82 N73 C88 C89 163.2(7) . . . . ?
C56 C57 C58 O59 177.0(8) . . . . ?
C56 C57 C58 C53 -3.0(13) . . . . ?
C56 C55 C54 C53 -2.9(13) . . . . ?
C58 C53 N52 K3 -26.6(9) . . . . ?
C58 C53 N52 C61 70.1(9) . . . . ?
C58 C53 N52 C67 -160.7(7) . . . . ?
C58 C53 C54 C55 1.2(12) . . . . ?
C58 C57 C56 C55 1.2(13) . . . . ?
C75 C74 N73 K6 -154.9(6) . . . . ?
C75 C74 N73 C82 108.4(8) . . . . ?
C75 C74 N73 C88 -22.1(10) . . . . ?
C75 C74 C79 O80 177.7(7) . . . . ?
C75 C74 C79 C78 -0.6(12) . . . . ?
C75 C76 C77 C78 -2.7(12) . . . . ?
C88 N73 C82 K6 -114.1(6) . . . . ?
C88 N73 C82 C83 71.0(9) . . . . ?
O44 S42 O45 K3 -174.9(5) . . . . ?
O44 S42 O45 K4 5.8(4) . . . . ?
O44 S42 O43 K5 -9.7(4) . . . 3_766 ?
O44 S42 C41 C40 65.7(7) . . . . ?
C16 C11 C12 C13 1.2(13) . . . . ?
C16 C15 C14 C13 -0.1(13) . . . . ?
C40 N31 C32 C33 104.3(9) . . . . ?
C40 N31 C32 C37 -72.9(9) . . . . ?
C54 C53 N52 K3 156.6(6) . . . . ?
C54 C53 N52 C61 -106.8(9) . . . . ?
C54 C53 N52 C67 22.4(11) . . . . ?
C54 C53 C58 O59 -178.2(7) . . . . ?
C54 C53 C58 C57 1.8(12) . . . . ?
O23 S21 O24 K2 -171.3(9) . . . . ?
O23 S21 O24 K5 5.7(4) . . . 3_766 ?
O23 S21 O24 K2A -167.0(13) . . . . ?
O23 S21 O22 K8 3.1(4) . . . 3_766 ?
O23 S21 O22 K8 -64.5(6) . . . 1_655 ?
O23 S21 C20 C19 -62.9(7) . . . . ?
C14 C13 C12 C11 -3.7(13) . . . . ?
C19 N10 C11 C16 71.1(9) . . . . ?
C19 N10 C11 C12 -108.0(9) . . . . ?
C19 N10 C25 C26 -164.7(7) . . . . ?
C18 O17 C16 C11 179.6(7) . . . . ?
C18 O17 C16 C15 0.4(12) . . . . ?
C61 N52 C67 C68 -165.9(7) . . . . ?
C62 S017 O66 K6 -105.5(4) . . . . ?
C62 S017 O66 K5 63.7(4) . . . . ?
C62 S017 O65 K4 -173.8(5) . . . 3_766 ?
C62 S017 O65 K4 -40.3(8) . . . . ?
C62 S017 O64 K6 107.5(4) . . . . ?
O43 S42 O45 K3 -50.4(7) . . . . ?
O43 S42 O45 K4 130.3(5) . . . . ?
O43 S42 O44 K4 150.1(6) . . . 3_766 ?
O43 S42 O44 K4 -134.5(4) . . . . ?
O43 S42 O44 K5 13.1(5) . . . 3_766 ?
O43 S42 C41 C40 -51.1(8) . . . . ?
C67 N52 C61 K3 112.5(6) . . . . ?
C67 N52 C61 C62 -60.7(9) . . . . ?
C83 S84 O86 K8 -116.1(3) . . . 3_666 ?
C83 S84 O86 K9 58.1(6) . . . 1_545 ?
C83 S84 O86 K7 144.8(3) . . . . ?
C83 S84 O85 K5 108.3(3) . . . . ?
C83 S84 O85 K7 -145.4(3) . . . . ?
C83 S84 O87 K8 33.2(7) . . . . ?
C83 S84 O87 K8 117.4(3) . . . 3_666 ?
C83 S84 O87 K5 -110.4(3) . . . . ?
C12 C11 C16 O17 -177.5(7) . . . . ?
C12 C11 C16 C15 1.7(12) . . . . ?
C12 C13 C14 C15 3.1(13) . . . . ?
C20 S21 O24 K2 -58.4(10) . . . . ?
C20 S21 O24 K5 118.7(4) . . . 3_766 ?
C20 S21 O24 K2A -54.1(13) . . . . ?
C20 S21 O22 K8 -110.6(4) . . . 3_766 ?
C20 S21 O22 K8 -178.2(4) . . . 1_655 ?
C20 S21 O23 K8 113.9(4) . . . 3_766 ?
C20 S21 O23 K5 -120.7(4) . . . 3_766 ?
C35 C36 C37 O38 -178.2(8) . . . . ?
C35 C36 C37 C32 2.1(13) . . . . ?
C47 S48 O50 K3 -107.5(4) . . . . ?
C47 S48 O49 K6 -96(2) . . . 1_545 ?
C47 S48 O51 K3 110.0(3) . . . . ?
C47 S48 O51 K1 45.2(10) . . . . ?
O28 S27 O29 K3 -100(2) . . . . ?
O28 S27 O29 K1 -18.2(5) . . . . ?
O28 S27 O30 K2 -1.4(6) . . . 1_545 ?
O28 S27 O30 K2A -5.3(9) . . . 1_545 ?
O28 S27 C26 C25 -72.5(7) . . . . ?
C89 S90 O91 K9 -95.5(5) . . . . ?
C89 S90 O92 K2 162.6(9) . . . 1_455 ?
C89 S90 O92 K2A 169(2) . . . 1_455 ?
C60 O59 C58 C53 -179.8(7) . . . . ?
C60 O59 C58 C57 0.3(12) . . . . ?
C41 S42 O45 K3 73.6(6) . . . . ?
C41 S42 O45 K4 -105.7(4) . . . . ?
C41 S42 O44 K4 33.1(7) . . . 3_766 ?
C41 S42 O44 K4 108.5(4) . . . . ?
C41 S42 O44 K5 -103.9(4) . . . 3_766 ?
C41 S42 O43 K5 103.1(4) . . . 3_766 ?
C81 O80 C79 C74 -176.8(7) . . . . ?
C81 O80 C79 C78 1.4(12) . . . . ?
C46 N31 C32 C33 -25.6(11) 1_565 . . . ?
C46 N31 C32 C37 157.2(7) 1_565 . . . ?
C46 N31 C40 C41 69.3(9) 1_565 . . . ?
C46 N31 C40 K2 -106.2(8) 1_565 . . . ?
C46 N31 C40 K2A -112.1(10) 1_565 . . . ?
C39 O38 C37 C36 -2.1(11) . . . . ?
C39 O38 C37 C32 177.7(7) . . . . ?
C25 N10 C11 C16 -157.6(7) . . . . ?
C25 N10 C11 C12 23.2(11) . . . . ?
C25 N10 C19 C20 -73.4(9) . . . . ?
C25 N10 C19 K9 111.6(6) . . . 1_645 ?
C26 S27 O29 K3 142(2) . . . . ?
C26 S27 O29 K1 -136.3(3) . . . . ?
C26 S27 O30 K2 112.7(6) . . . 1_545 ?
C26 S27 O30 K2A 108.9(9) . . . 1_545 ?
C26 S27 O28 K2 -113.0(5) . . . 1_545 ?
C26 S27 O28 K1 138.8(3) . . . . ?
C26 S27 O28 K2A -109.8(8) . . . 1_545 ?
O64 S017 O66 K6 8.6(5) . . . . ?
O64 S017 O66 K5 177.7(4) . . . . ?
O64 S017 O65 K4 -155.4(7) . . . . ?
O64 S017 O65 K4 71.1(7) . . . 3_766 ?
O64 S017 C62 C61 79.8(7) . . . . ?
C68 S69 O70 K6 90.9(5) . . . 1_545 ?
C68 S69 O71 K9 173.7(10) . . . 1_545 ?
C68 S69 O71 K7 -103.4(3) . . . . ?
C68 S69 O72 K7 101.8(3) . . . . ?
O51 S48 O50 K3 6.3(5) . . . . ?
O51 S48 O49 K6 148(2) . . . 1_545 ?
O51 S48 C47 C46 65.1(7) . . . . ?
K8 S84 O86 K9 174.2(5) 3_666 . . 1_545 ?
K8 S84 O86 K7 -99.1(2) 3_666 . . . ?
K8 S84 O85 K5 -64.8(3) 3_666 . . . ?
K8 S84 O85 K7 41.5(4) 3_666 . . . ?
K8 S84 O87 K8 -84.3(6) 3_666 . . . ?
K8 S84 O87 K5 132.1(3) 3_666 . . . ?
K8 S84 C83 C82 117.0(5) 3_666 . . . ?
K8 S21 O24 K2 136.3(8) 3_766 . . . ?
K8 S21 O24 K5 -46.7(4) 3_766 . . 3_766 ?
K8 S21 O24 K2A 140.6(12) 3_766 . . . ?
K8 S21 O22 K8 -67.6(4) 3_766 . . 1_655 ?
K8 S21 O23 K5 125.5(4) 3_766 . . 3_766 ?
K8 S21 C20 C19 -13.9(8) 3_766 . . . ?
K9 O17 C16 C11 22.8(10) 1_645 . . . ?
K9 O17 C16 C15 -156.4(6) 1_645 . . . ?
K9 N10 C11 C16 -23.5(9) 1_645 . . . ?
K9 N10 C11 C12 157.4(7) 1_645 . . . ?
K9 N10 C19 C20 175.0(7) 1_645 . . . ?
K9 N10 C25 C26 -71.6(7) 1_645 . . . ?
K4 S42 O45 K3 179.3(6) . . . . ?
K4 S42 O44 K4 -75.4(5) . . . 3_766 ?
K4 S42 O44 K5 147.6(5) . . . 3_766 ?
K4 S42 O43 K5 -66.3(5) . . . 3_766 ?
K4 S42 C41 C40 121.1(6) . . . . ?
K2 S27 O29 K3 -37(3) 1_545 . . . ?
K2 S27 O29 K1 44.9(8) 1_545 . . . ?
K2 S27 O28 K1 -108.2(5) 1_545 . . . ?
K2 S27 C26 C25 -131.0(8) 1_545 . . . ?
K2 O38 C37 C36 159.0(7) . . . . ?
K2 O38 C37 C32 -21.2(10) . . . . ?
K2 N31 C32 C33 -157.6(7) . . . . ?
K2 N31 C32 C37 25.2(9) . . . . ?
K2 N31 C40 C41 175.5(9) . . . . ?
K5 S84 O86 K8 62.9(4) . . . 3_666 ?
K5 S84 O86 K9 -122.9(4) . . . 1_545 ?
K5 S84 O86 K7 -36.2(4) . . . . ?
K5 S84 O85 K7 106.3(3) . . . . ?
K5 S84 O87 K8 -132.1(3) . . . 3_666 ?
K5 S84 O87 K8 143.6(7) . . . . ?
K5 S84 C83 C82 2.7(7) . . . . ?
K5 S42 O45 K3 -135.1(3) 3_766 . . . ?
K5 S42 O45 K4 45.5(5) 3_766 . . . ?
K5 S42 O44 K4 -147.6(5) 3_766 . . . ?
K5 S42 O44 K4 137.0(8) 3_766 . . 3_766 ?
K5 S42 C41 C40 20.7(7) 3_766 . . . ?
K5 S21 O24 K2 -177.0(10) 3_766 . . . ?
K5 S21 O24 K2A -172.8(13) 3_766 . . . ?
K5 S21 O22 K8 -4.1(7) 3_766 . . 1_655 ?
K5 S21 O22 K8 63.5(3) 3_766 . . 3_766 ?
K5 S21 O23 K8 -125.5(4) 3_766 . . 3_766 ?
K5 S21 C20 C19 -118.7(6) 3_766 . . . ?
K5 S017 O66 K6 -169.2(4) . . . . ?
K5 S017 O65 K4 -92.1(5) . . . 3_766 ?
K5 S017 O65 K4 41.4(7) . . . . ?
K5 S017 C62 C61 -121.5(6) . . . . ?
K5 S017 O64 K6 -3.5(9) . . . . ?
K1 S27 O29 K3 -82(2) . . . . ?
K1 S27 O30 K2 -60.3(5) . . . 1_545 ?
K1 S27 O30 K2A -64.1(9) . . . 1_545 ?
K1 S27 O28 K2 108.2(5) . . . 1_545 ?
K1 S27 O28 K2A 111.5(8) . . . 1_545 ?
K1 S27 C26 C25 -17.3(9) . . . . ?
K7 S69 O70 K6 -75.5(6) . . . 1_545 ?
K7 S69 O71 K9 -82.9(10) . . . 1_545 ?
K7 S69 C68 C67 -9.6(6) . . . . ?
K7 S84 O86 K8 99.1(2) . . . 3_666 ?
K7 S84 O86 K9 -86.7(4) . . . 1_545 ?
K7 S84 O85 K5 -106.3(3) . . . . ?
K7 S84 O87 K8 -149.0(5) . . . . ?
K7 S84 O87 K8 -64.7(2) . . . 3_666 ?
K7 S84 O87 K5 67.4(2) . . . . ?
K7 S84 C83 C82 -114.4(6) . . . . ?
K2A S27 O29 K3 -30(3) 1_545 . . . ?
K2A S27 O29 K1 51.1(11) 1_545 . . . ?
K2A S27 O28 K1 -111.5(8) 1_545 . . . ?
K2A S27 C26 C25 -135.7(9) 1_545 . . . ?
K2A O38 C37 C36 155.6(12) . . . . ?
K2A O38 C37 C32 -24.6(13) . . . . ?
K2A N31 C32 C33 -158.5(10) . . . . ?
K2A N31 C32 C37 24.3(11) . . . . ?
K2A N31 C40 C41 -178.6(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2014-06-17
_olex2_submission_original_sample_id dcm006Cu
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.784

_solvent_exptl_crystal_recrystallization_method 'methanol and water'
####################################################################### 
# 
# 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_dcm004_new
_database_code_depnum_ccdc_archive 'CCDC 1484351'
_audit_update_record             
;
2016-06-09 deposited with the CCDC.
2016-08-29 downloaded from the CCDC.
;
_audit_creation_date             2016-06-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        'phenyl beta-aminobisulfonate'
_chemical_formula_moiety         '0.25(C40 H68 K8 N4 O32 S8)'
_chemical_formula_sum            'C10 H17 K2 N O8 S2'
_chemical_formula_weight         421.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H8 N1 S2 O6 K2'
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'
K K 0.2009 0.2494 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   8.2498(3)
_cell_length_b                   22.5592(7)
_cell_length_c                   8.7439(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1627.33(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.7190
_cell_measurement_theta_min      3.8600
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.3155
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.1822
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.778
_diffrn_reflns_theta_min         3.395
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -33.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   77.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
  2 omega   34.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695 -149.0000 -158.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega    0.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000    0.0000 73

#__ type_ start__ end____ width___ exp.time_
  4 omega   -9.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000 -150.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega  -51.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000 -150.0000 81

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  123.0000   85.0000 32

#__ type_ start__ end____ width___ exp.time_
  7 omega  -35.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   38.0000  -60.0000 102

#__ type_ start__ end____ width___ exp.time_
  8 omega   -4.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000  150.0000 56

#__ type_ start__ end____ width___ exp.time_
  9 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000  -30.0000 44

#__ type_ start__ end____ width___ exp.time_
 10 omega  -26.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   86.0000   76.1730 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0422405000
_diffrn_orient_matrix_UB_12      0.0221314000
_diffrn_orient_matrix_UB_13      -0.0416327000
_diffrn_orient_matrix_UB_21      -0.0338245000
_diffrn_orient_matrix_UB_22      0.0221626000
_diffrn_orient_matrix_UB_23      0.0478907000
_diffrn_orient_matrix_UB_31      0.0667827000
_diffrn_orient_matrix_UB_32      -0.0027726000
_diffrn_orient_matrix_UB_33      0.0505579000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1812
_reflns_number_total             2066
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2066
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0270P)²+0.8504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0606
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.16470(4) 0.48260(2) 0.80588(3) 0.01653(9) Uani 1 1 d . . . . .
S1 S 0.03001(4) 0.40286(2) 0.49481(4) 0.01224(9) Uani 1 1 d . . . . .
N5 N 0.2585(2) 0.2500 0.38466(18) 0.0147(3) Uani 1 2 d S T P . .
O1 O -0.06305(12) 0.41598(4) 0.63213(11) 0.0175(2) Uani 1 1 d . . . . .
O91 O 0.11323(14) 0.44378(5) 1.09935(12) 0.0210(2) Uani 1 1 d . . . . .
O90 O 0.06724(12) 0.58992(4) 0.64491(11) 0.0171(2) Uani 1 1 d . . . . .
O2 O 0.18186(12) 0.43530(4) 0.48768(11) 0.0190(2) Uani 1 1 d . . . . .
C4 C 0.17103(17) 0.30516(6) 0.35963(16) 0.0150(3) Uani 1 1 d . . . . .
C9 C 0.6949(3) 0.2500 0.6348(2) 0.0196(4) Uani 1 2 d S T P . .
C7 C 0.47361(17) 0.30328(6) 0.51752(15) 0.0163(3) Uani 1 1 d . . . . .
C3 C 0.08052(18) 0.32665(6) 0.50261(15) 0.0161(3) Uani 1 1 d . . . . .
C6 C 0.3983(2) 0.2500 0.4736(2) 0.0134(4) Uani 1 2 d S T P . .
C8 C 0.61988(18) 0.30276(6) 0.59482(16) 0.0193(3) Uani 1 1 d . . . . .
H4A H 0.0954(19) 0.2979(7) 0.2783(18) 0.015(4) Uiso 1 1 d . . . . .
H8 H 0.669(2) 0.3400(8) 0.623(2) 0.025(4) Uiso 1 1 d . . . . .
H7 H 0.426(2) 0.3396(8) 0.4945(18) 0.021(4) Uiso 1 1 d . . . . .
H4B H 0.249(2) 0.3352(7) 0.3230(17) 0.017(4) Uiso 1 1 d . . . . .
H9 H 0.798(3) 0.2500 0.684(3) 0.019(6) Uiso 1 2 d S T P . .
H3A H 0.148(2) 0.3219(8) 0.594(2) 0.028(5) Uiso 1 1 d . . . . .
H3B H -0.020(2) 0.3058(8) 0.5186(18) 0.022(4) Uiso 1 1 d . . . . .
H91A H 0.203(3) 0.4288(9) 1.107(2) 0.032(5) Uiso 1 1 d . . . . .
H91B H 0.063(3) 0.4253(10) 1.160(3) 0.039(6) 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
K1 K1 4.23906(19) 6_557 ?
K1 K1 4.4188(6) 5_567 ?
K1 K1 4.23911(19) 6_657 ?
K1 S1 3.4452(4) . ?
K1 O1 2.7563(10) 6_657 ?
K1 O1 2.8455(10) . ?
K1 O91 2.7445(11) . ?
K1 O91 3.0621(12) 2_564 ?
K1 O91 2.9500(12) 5_567 ?
K1 O90 2.9136(10) . ?
K1 O2 2.9833(10) . ?
K1 O2 2.7494(10) 2_565 ?
K1 H91A 2.91(2) . ?
S1 O1 1.4556(10) . ?
S1 O90 1.4707(10) 5_566 ?
S1 O2 1.4522(10) . ?
S1 C3 1.7704(14) . ?
N5 C4 1.4551(15) . ?
N5 C4 1.4551(15) 8_565 ?
N5 C6 1.391(3) . ?
O1 K1 2.7563(10) 6_557 ?
O91 K1 3.0621(11) 2_565 ?
O91 K1 2.9500(12) 5_567 ?
O91 H91A 0.82(2) . ?
O91 H91B 0.79(2) . ?
O90 S1 1.4707(10) 5_566 ?
O2 K1 2.7495(10) 2_564 ?
C4 C3 1.5348(19) . ?
C4 H4A 0.960(16) . ?
C4 H4B 0.989(17) . ?
C9 C8 1.3860(18) 8_565 ?
C9 C8 1.3861(18) . ?
C9 H9 0.95(2) . ?
C7 C6 1.4066(17) . ?
C7 C8 1.383(2) . ?
C7 H7 0.930(18) . ?
C3 H3A 0.978(19) . ?
C3 H3B 0.964(18) . ?
C6 C7 1.4067(17) 8_565 ?
C8 H8 0.965(18) . ?

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
K1 K1 K1 65.082(7) 6_557 5_567 ?
K1 K1 K1 140.854(13) 6_657 5_567 ?
K1 K1 K1 153.344(15) 6_557 6_657 ?
K1 K1 H91A 95.9(4) 6_657 . ?
K1 K1 H91A 108.3(4) 6_557 . ?
K1 K1 H91A 56.4(4) 5_567 . ?
S1 K1 K1 97.576(11) . 6_657 ?
S1 K1 K1 120.063(12) . 5_567 ?
S1 K1 K1 60.274(9) . 6_557 ?
S1 K1 H91A 122.0(4) . . ?
O1 K1 K1 41.62(2) 6_657 6_657 ?
O1 K1 K1 40.04(2) . 6_557 ?
O1 K1 K1 121.29(2) . 6_657 ?
O1 K1 K1 116.55(2) 6_657 5_567 ?
O1 K1 K1 146.95(2) 6_657 6_557 ?
O1 K1 K1 95.62(2) . 5_567 ?
O1 K1 S1 24.46(2) . . ?
O1 K1 S1 97.66(2) 6_657 . ?
O1 K1 O1 110.79(3) 6_657 . ?
O1 K1 O91 86.22(3) . 5_567 ?
O1 K1 O91 111.51(3) . 2_564 ?
O1 K1 O91 152.27(3) 6_657 5_567 ?
O1 K1 O91 85.65(3) 6_657 2_564 ?
O1 K1 O90 89.93(3) . . ?
O1 K1 O90 140.62(3) 6_657 . ?
O1 K1 O2 87.12(3) 6_657 . ?
O1 K1 O2 49.04(3) . . ?
O1 K1 H91A 60.5(4) 6_657 . ?
O1 K1 H91A 109.5(4) . . ?
O91 K1 K1 111.48(3) . 6_657 ?
O91 K1 K1 136.44(2) 2_564 5_567 ?
O91 K1 K1 37.45(2) 5_567 5_567 ?
O91 K1 K1 116.50(2) 2_564 6_557 ?
O91 K1 K1 93.73(3) . 6_557 ?
O91 K1 K1 40.82(2) . 5_567 ?
O91 K1 K1 46.25(2) 5_567 6_557 ?
O91 K1 K1 44.10(2) 2_564 6_657 ?
O91 K1 K1 145.19(2) 5_567 6_657 ?
O91 K1 S1 121.44(3) . . ?
O91 K1 S1 90.61(2) 2_564 . ?
O91 K1 S1 105.37(2) 5_567 . ?
O91 K1 O1 103.21(3) . . ?
O91 K1 O1 76.60(3) . 6_657 ?
O91 K1 O91 144.80(3) . 2_564 ?
O91 K1 O91 108.99(4) 5_567 2_564 ?
O91 K1 O91 78.27(3) . 5_567 ?
O91 K1 O90 132.39(3) . . ?
O91 K1 O2 75.26(3) . 2_565 ?
O91 K1 O2 139.93(3) . . ?
O91 K1 O2 120.02(3) 5_567 . ?
O91 K1 H91A 133.9(4) 2_564 . ?
O91 K1 H91A 16.2(4) . . ?
O91 K1 H91A 93.7(4) 5_567 . ?
O90 K1 K1 67.67(2) . 6_557 ?
O90 K1 K1 93.08(2) . 5_567 ?
O90 K1 K1 99.04(2) . 6_657 ?
O90 K1 S1 87.91(2) . . ?
O90 K1 O91 55.22(3) . 2_564 ?
O90 K1 O91 56.86(3) . 5_567 ?
O90 K1 O2 81.94(3) . . ?
O90 K1 H91A 144.3(4) . . ?
O2 K1 K1 74.86(2) . 6_657 ?
O2 K1 K1 80.28(2) . 6_557 ?
O2 K1 K1 144.02(2) . 5_567 ?
O2 K1 K1 125.54(2) 2_565 6_557 ?
O2 K1 K1 73.70(2) 2_565 5_567 ?
O2 K1 K1 71.66(2) 2_565 6_657 ?
O2 K1 S1 24.80(2) . . ?
O2 K1 S1 163.08(2) 2_565 . ?
O2 K1 O1 83.02(3) 2_565 6_657 ?
O2 K1 O1 165.57(3) 2_565 . ?
O2 K1 O91 79.41(3) 2_565 5_567 ?
O2 K1 O91 72.55(3) 2_565 2_564 ?
O2 K1 O91 67.39(3) . 2_564 ?
O2 K1 O90 81.18(3) 2_565 . ?
O2 K1 O2 139.32(2) 2_565 . ?
O2 K1 H91A 73.1(4) 2_565 . ?
O2 K1 H91A 133.5(4) . . ?
O1 S1 K1 54.03(4) . . ?
O1 S1 O90 112.03(6) . 5_566 ?
O1 S1 C3 106.85(6) . . ?
O90 S1 K1 140.71(4) 5_566 . ?
O90 S1 C3 105.54(6) 5_566 . ?
O2 S1 K1 59.50(4) . . ?
O2 S1 O1 112.82(6) . . ?
O2 S1 O90 112.28(6) . 5_566 ?
O2 S1 C3 106.74(7) . . ?
C3 S1 K1 113.63(5) . . ?
C4 N5 C4 117.55(16) . 8_565 ?
C6 N5 C4 119.70(8) . 8_565 ?
C6 N5 C4 119.70(8) . . ?
K1 O1 K1 98.34(3) 6_557 . ?
S1 O1 K1 101.51(5) . . ?
S1 O1 K1 134.66(6) . 6_557 ?
K1 O91 K1 101.73(3) . 5_567 ?
K1 O91 K1 106.60(4) . 2_565 ?
K1 O91 K1 89.65(3) 5_567 2_565 ?
K1 O91 H91A 156.2(14) 5_567 . ?
K1 O91 H91A 68.6(14) 2_565 . ?
K1 O91 H91A 93.8(14) . . ?
K1 O91 H91B 151.4(16) . . ?
K1 O91 H91B 101.4(16) 2_565 . ?
K1 O91 H91B 72.7(15) 5_567 . ?
H91A O91 H91B 101(2) . . ?
S1 O90 K1 130.08(5) 5_566 . ?
K1 O2 K1 108.67(3) 2_564 . ?
S1 O2 K1 95.70(5) . . ?
S1 O2 K1 139.60(6) . 2_564 ?
N5 C4 C3 112.89(12) . . ?
N5 C4 H4A 106.8(9) . . ?
N5 C4 H4B 108.2(10) . . ?
C3 C4 H4A 109.9(9) . . ?
C3 C4 H4B 111.4(9) . . ?
H4A C4 H4B 107.4(13) . . ?
C8 C9 C8 118.34(19) 8_565 . ?
C8 C9 H9 120.79(10) 8_565 . ?
C8 C9 H9 120.79(11) . . ?
C6 C7 H7 120.5(11) . . ?
C8 C7 C6 120.78(14) . . ?
C8 C7 H7 118.7(11) . . ?
S1 C3 H3A 105.7(11) . . ?
S1 C3 H3B 106.0(11) . . ?
C4 C3 S1 112.94(9) . . ?
C4 C3 H3A 110.6(11) . . ?
C4 C3 H3B 112.6(10) . . ?
H3A C3 H3B 108.7(14) . . ?
N5 C6 C7 121.27(9) . . ?
N5 C6 C7 121.26(9) . 8_565 ?
C7 C6 C7 117.41(18) . 8_565 ?
C9 C8 H8 119.7(11) . . ?
C7 C8 C9 121.31(14) . . ?
C7 C8 H8 119.0(10) . . ?

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
K1 S1 O1 K1 114.17(8) . . . 6_557 ?
K1 S1 O2 K1 -127.85(10) . . . 2_564 ?
K1 S1 C3 C4 -125.91(9) . . . . ?
N5 C4 C3 S1 160.85(10) . . . . ?
O1 S1 O2 K1 -118.75(9) . . . 2_564 ?
O1 S1 O2 K1 9.10(6) . . . . ?
O1 S1 C3 C4 176.59(10) . . . . ?
O90 S1 O1 K1 -23.40(10) 5_566 . . 6_557 ?
O90 S1 O1 K1 -137.56(5) 5_566 . . . ?
O90 S1 O2 K1 136.84(5) 5_566 . . . ?
O90 S1 O2 K1 8.99(11) 5_566 . . 2_564 ?
O90 S1 C3 C4 57.18(12) 5_566 . . . ?
O2 S1 O1 K1 104.48(8) . . . 6_557 ?
O2 S1 O1 K1 -9.69(6) . . . . ?
O2 S1 C3 C4 -62.45(12) . . . . ?
C4 N5 C4 C3 87.99(17) 8_565 . . . ?
C4 N5 C6 C7 -171.25(14) 8_565 . . . ?
C4 N5 C6 C7 -11.5(2) . . . . ?
C4 N5 C6 C7 171.25(14) . . . 8_565 ?
C4 N5 C6 C7 11.5(2) 8_565 . . 8_565 ?
C3 S1 O1 K1 107.31(6) . . . . ?
C3 S1 O1 K1 -138.52(8) . . . 6_557 ?
C3 S1 O2 K1 124.18(9) . . . 2_564 ?
C3 S1 O2 K1 -107.97(5) . . . . ?
C6 N5 C4 C3 -72.20(18) . . . . ?
C6 C7 C8 C9 -1.6(2) . . . . ?
C8 C9 C8 C7 0.2(3) 8_565 . . . ?
C8 C7 C6 N5 -174.48(15) . . . . ?
C8 C7 C6 C7 2.9(3) . . . 8_565 ?

_shelx_SHELXL_version_number     2014/7
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
-2 -31 1 0.0985 -1.9973 -30.9929 0.9968 -0.8118 -0.5716 0.0029
2 31 -1 0.0985 1.9973 30.9929 -0.9968 0.8118 0.5716 -0.0029
9 9 7 0.0940 9.0027 8.9988 7.0010 0.2880 0.2302 0.9302
-9 -9 -7 0.0940 -9.0027 -8.9988 -7.0010 -0.2880 -0.2302 -0.9302
6 -2 -10 0.0911 6.0011 -1.9998 -10.0044 0.6257 -0.7264 -0.0995
-6 2 10 0.0911 -6.0011 1.9998 10.0044 -0.6257 0.7264 0.0995

_olex2_date_sample_data_collection 18/06/2014
_olex2_date_sample_submission    03/06/2014
_olex2_submission_original_sample_id DCM004
_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'acetone, methanol and water'
