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

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

data_240708b
_database_code_depnum_ccdc_archive 'CCDC 1426675'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;

#==============================================================================


# 6. CRYSTALLOGRAPHY

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C56 H47 Gd O36 S8, Gd H16 O8, C8 H15 N2, 2(C25 H22 O P), H2 O'
_chemical_formula_sum            'C114 H124 Gd2 N2 O47 P2 S8'
_chemical_formula_weight         2907.06

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'
P P 0.2955 0.4335 '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'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_H-M_alt        'P n n n'
_space_group_name_Hall           '-P 2ab 2bc'

_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+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   12.3714(3)
_cell_length_b                   13.3655(2)
_cell_length_c                   37.5272(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6205.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19125
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      67.1
_diffrn_orient_matrix_UB_11      0.1156757524
_diffrn_orient_matrix_UB_12      -0.0358365188
_diffrn_orient_matrix_UB_13      -0.0084310237
_diffrn_orient_matrix_UB_21      -0.0371449830
_diffrn_orient_matrix_UB_22      -0.0335649320
_diffrn_orient_matrix_UB_23      -0.0373773306
_diffrn_orient_matrix_UB_31      0.0277513618
_diffrn_orient_matrix_UB_32      0.1042469470
_diffrn_orient_matrix_UB_33      -0.0149338914

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_F_000             2968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    9.105
_shelx_estimated_absorpt_T_min   0.239
_shelx_estimated_absorpt_T_max   0.307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61212
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            80713
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         3.510
_diffrn_reflns_theta_max         67.208
_diffrn_reflns_theta_full        67.208
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5560
_reflns_number_gt                3999
_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       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_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)+(0.1500P)²+36.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5560
_refine_ls_number_parameters     423
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.1027
_refine_ls_wR_factor_ref         0.2968
_refine_ls_wR_factor_gt          0.2818
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.090
_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
Gd1 Gd 0.7500 0.2500 0.2500 0.0704(4) Uani 1 4 d DS T P . .
Gd2 Gd 0.7500 0.7500 0.2500 0.0665(4) Uani 1 4 d DS T P . .
O01W O 0.6189(10) 0.3659(8) 0.2698(3) 0.125(3) Uani 1 1 d D . . . .
H01A H 0.576(10) 0.401(10) 0.2572(6) 0.188 Uiso 1 1 d D U . . .
H01B H 0.607(11) 0.385(11) 0.2911(7) 0.188 Uiso 1 1 d D U . . .
O02W O 0.5989(10) 0.8157(6) 0.2808(3) 0.116(3) Uani 1 1 d D . . . .
H02A H 0.573(10) 0.873(5) 0.277(2) 0.173 Uiso 1 1 d D U . . .
H02B H 0.589(10) 0.807(9) 0.3030(9) 0.173 Uiso 1 1 d D U . . .
O03W O 0.6888(9) 0.6197(6) 0.2872(2) 0.102(3) Uani 1 1 d D . . . .
H03A H 0.635(7) 0.583(8) 0.2817(16) 0.153 Uiso 1 1 d D U . . .
H03B H 0.684(11) 0.626(8) 0.3097(5) 0.153 Uiso 1 1 d D U . . .
O04W O 0.2500 0.7500 0.2500 0.078(4) Uani 1 4 d DS T P . .
H04A H 0.216(10) 0.7111(7) 0.264(3) 0.117 Uiso 0.5 1 d D U P . .
O1 O 0.3891(7) 0.1962(9) 0.4429(3) 0.123(3) Uani 1 1 d . U . . .
H1 H 0.3266 0.1718 0.4422 0.184 Uiso 1 1 calc R U . . .
C11 C 0.4441(8) 0.1688(11) 0.4132(3) 0.080(3) Uani 1 1 d . U . . .
C12 C 0.5116(8) 0.2428(9) 0.3983(3) 0.078(3) Uani 1 1 d . . . . .
C13 C 0.5746(8) 0.2168(8) 0.3693(3) 0.070(2) Uani 1 1 d . . . . .
H13 H 0.6210 0.2649 0.3586 0.085 Uiso 1 1 calc R U . . .
C14 C 0.5695(7) 0.1192(6) 0.3558(2) 0.064(2) Uani 1 1 d D . . . .
C15 C 0.4997(8) 0.0503(8) 0.3704(3) 0.074(3) Uani 1 1 d . . . . .
H15 H 0.4953 -0.0147 0.3602 0.088 Uiso 1 1 calc R U . . .
C16 C 0.4367(8) 0.0730(10) 0.3991(3) 0.085(4) Uani 1 1 d . . . . .
S1 S 0.6520(2) 0.0848(2) 0.32014(8) 0.0853(8) Uani 1 1 d D . . . .
O11 O 0.6989(10) 0.1751(7) 0.3050(3) 0.093(2) Uiso 0.5 1 d D . P A 1
O12 O 0.7334(8) 0.0150(9) 0.3342(3) 0.093(2) Uiso 0.5 1 d D . P A 1
O13 O 0.5813(9) 0.0324(9) 0.2941(3) 0.093(2) Uiso 0.5 1 d D . P A 1
O14 O 0.6517(10) 0.1743(7) 0.2962(3) 0.093(2) Uiso 0.5 1 d D . P A 2
O15 O 0.7598(7) 0.0659(10) 0.3342(3) 0.093(2) Uiso 0.5 1 d D . P A 2
O16 O 0.6018(10) 0.0000(7) 0.3024(3) 0.093(2) Uiso 0.5 1 d D . P A 2
C10 C 0.5194(9) 0.3503(10) 0.4114(4) 0.099(4) Uani 1 1 d . U . . .
H10A H 0.5932 0.3754 0.4064 0.119 Uiso 1 1 calc R U . . .
H10B H 0.5091 0.3508 0.4375 0.119 Uiso 1 1 calc R U . . .
O2 O 0.3114(7) 0.3818(7) 0.4412(3) 0.110(3) Uani 1 1 d . U . . .
H2 H 0.3351 0.3231 0.4397 0.165 Uiso 0.75 1 calc R U P . .
C21 C 0.3344(10) 0.4315(10) 0.4113(4) 0.094(4) Uani 1 1 d . U . . .
C22 C 0.2544(8) 0.4974(8) 0.3949(4) 0.086(4) Uani 1 1 d . U . . .
C23 C 0.2778(10) 0.5468(11) 0.3644(4) 0.096(4) Uani 1 1 d . U . . .
H23 H 0.2253 0.5891 0.3537 0.115 Uiso 1 1 calc R U . . .
C24 C 0.3772(8) 0.5355(9) 0.3491(4) 0.093(3) Uani 1 1 d D U . . .
C25 C 0.4542(11) 0.4759(10) 0.3643(4) 0.094(4) Uani 1 1 d . U . . .
H25 H 0.5232 0.4714 0.3534 0.113 Uiso 1 1 calc R U . . .
C26 C 0.4357(8) 0.4239(9) 0.3941(3) 0.084(3) Uani 1 1 d . U . . .
S2 S 0.4067(4) 0.6010(4) 0.30995(16) 0.154(2) Uani 1 1 d D . . . .
O21 O 0.4605(10) 0.6994(8) 0.3198(3) 0.149(3) Uiso 0.75 1 d D . P B 1
O22 O 0.4841(10) 0.5419(10) 0.2875(3) 0.149(3) Uiso 0.75 1 d D . P B 1
O23 O 0.3063(10) 0.6228(10) 0.2894(3) 0.149(3) Uiso 0.75 1 d D . P B 1
O24 O 0.400(3) 0.7109(8) 0.3162(5) 0.149(3) Uiso 0.25 1 d D . P B 2
O25 O 0.5176(15) 0.573(2) 0.2971(6) 0.149(3) Uiso 0.25 1 d D . P B 2
O26 O 0.326(2) 0.571(2) 0.2817(4) 0.149(3) Uiso 0.25 1 d D . P B 2
C20 C 0.1425(11) 0.4996(10) 0.4146(4) 0.108(4) Uani 1 1 d . U . . .
H20A H 0.1537 0.4837 0.4401 0.129 Uiso 1 1 calc R U . . .
H20B H 0.1120 0.5680 0.4131 0.129 Uiso 1 1 calc R U . . .
P1 P 0.7500 0.2500 0.51142(7) 0.0363(5) Uani 1 2 d S T P . .
C31 C 0.6306(6) 0.2344(5) 0.53765(19) 0.0427(16) Uani 1 1 d . . . . .
C32 C 0.5429(6) 0.1877(6) 0.5224(2) 0.0500(18) Uani 1 1 d . . . . .
H32 H 0.5487 0.1597 0.4992 0.060 Uiso 1 1 calc R U . . .
C33 C 0.4461(7) 0.1818(7) 0.5408(3) 0.061(2) Uani 1 1 d . . . . .
H33 H 0.3853 0.1510 0.5300 0.073 Uiso 1 1 calc R U . . .
C34 C 0.4373(8) 0.2204(7) 0.5750(3) 0.070(3) Uani 1 1 d . . . . .
H34A H 0.3714 0.2132 0.5878 0.084 Uiso 0.5 1 calc R U P C 2
C37 C 0.3379(19) 0.2503(19) 0.6319(5) 0.086(7) Uani 0.5 1 d . . P D 1
H37A H 0.2728 0.2213 0.6426 0.130 Uiso 0.5 1 calc R U P D 1
H37B H 0.3332 0.3234 0.6327 0.130 Uiso 0.5 1 calc R U P D 1
H37C H 0.4017 0.2282 0.6452 0.130 Uiso 0.5 1 calc R U P D 1
O37 O 0.3468(10) 0.2175(9) 0.5952(3) 0.063(3) Uani 0.5 1 d . . P D 1
C35 C 0.5240(10) 0.2696(7) 0.5908(3) 0.078(3) Uani 1 1 d . . . . .
H35 H 0.5178 0.2975 0.6140 0.093 Uiso 1 1 calc R U . . .
C36 C 0.6198(8) 0.2767(6) 0.5717(2) 0.062(2) Uani 1 1 d . . . . .
H36 H 0.6795 0.3110 0.5820 0.074 Uiso 1 1 calc R U . . .
C41 C 0.7301(5) 0.3595(5) 0.48447(19) 0.0369(14) Uani 1 1 d . . . . .
C42 C 0.6656(6) 0.4366(5) 0.49764(19) 0.0421(16) Uani 1 1 d . . . . .
H42 H 0.6307 0.4297 0.5201 0.050 Uiso 1 1 calc R U . . .
C43 C 0.6525(7) 0.5236(5) 0.4778(2) 0.0470(17) Uani 1 1 d . . . . .
H43 H 0.6077 0.5757 0.4866 0.056 Uiso 1 1 calc R U . . .
C44 C 0.7038(7) 0.5350(6) 0.4456(2) 0.0523(19) Uani 1 1 d . . . . .
H44 H 0.6944 0.5947 0.4323 0.063 Uiso 1 1 calc R U . . .
C45 C 0.7695(6) 0.4588(6) 0.4326(2) 0.0492(18) Uani 1 1 d . . . . .
H45 H 0.8052 0.4669 0.4104 0.059 Uiso 1 1 calc R U . . .
C46 C 0.7833(5) 0.3714(5) 0.45182(19) 0.0409(15) Uani 1 1 d . . . . .
H46 H 0.8285 0.3197 0.4429 0.049 Uiso 1 1 calc R U . . .
C1 C 0.267(2) 0.226(2) 0.3395(7) 0.078(3) Uiso 0.25 1 d D . P E -1
H1A H 0.3420 0.2272 0.3482 0.117 Uiso 0.25 1 calc R U P E -1
H1B H 0.2495 0.1589 0.3310 0.117 Uiso 0.25 1 calc R U P E -1
H1C H 0.2182 0.2448 0.3589 0.117 Uiso 0.25 1 calc R U P E -1
N1 N 0.2560(16) 0.2970(15) 0.3105(5) 0.078(3) Uiso 0.25 1 d D . P E -1
C2 C 0.3276(16) 0.3085(15) 0.2836(5) 0.078(3) Uiso 0.25 1 d D . P E -1
H2A H 0.3930 0.2724 0.2804 0.094 Uiso 0.25 1 calc R U P E -1
N2 N 0.2894(18) 0.3792(13) 0.2627(5) 0.078(3) Uiso 0.25 1 d D . P E -1
C3 C 0.192(2) 0.4156(17) 0.2755(7) 0.078(3) Uiso 0.25 1 d D . P E -1
H3A H 0.1477 0.4665 0.2654 0.094 Uiso 0.25 1 calc R U P E -1
C4 C 0.1722(16) 0.361(2) 0.3065(6) 0.078(3) Uiso 0.25 1 d D . P E -1
H4A H 0.1116 0.3675 0.3218 0.094 Uiso 0.25 1 calc R U P E -1
C5 C 0.344(3) 0.415(2) 0.2298(6) 0.078(3) Uiso 0.25 1 d D . P E -1
H5A H 0.4205 0.4286 0.2354 0.094 Uiso 0.25 1 calc R U P E -1
H5B H 0.3102 0.4790 0.2226 0.094 Uiso 0.25 1 calc R U P E -1
C6 C 0.3392(19) 0.344(3) 0.1988(6) 0.078(3) Uiso 0.25 1 d D . P E -1
H6A H 0.3925 0.2897 0.2024 0.094 Uiso 0.25 1 calc R U P E -1
H6B H 0.3586 0.3801 0.1767 0.094 Uiso 0.25 1 calc R U P E -1
C7 C 0.228(2) 0.300(3) 0.1949(9) 0.078(3) Uiso 0.25 1 d D . P E -1
H7A H 0.1741 0.3542 0.1945 0.094 Uiso 0.25 1 calc R U P E -1
H7B H 0.2127 0.2566 0.2157 0.094 Uiso 0.25 1 calc R U P E -1
C8 C 0.217(3) 0.238(4) 0.1608(9) 0.078(3) Uiso 0.25 1 d D . P E -1
H8A H 0.1430 0.2115 0.1590 0.117 Uiso 0.25 1 calc R U P E -1
H8B H 0.2681 0.1816 0.1615 0.117 Uiso 0.25 1 calc R U P E -1
H8C H 0.2324 0.2797 0.1401 0.117 Uiso 0.25 1 calc R U P E -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O14 2.346(9) . ?
Gd1 O14 2.346(9) 2_655 ?
Gd1 O14 2.346(9) 4 ?
Gd1 O14 2.346(9) 3_655 ?
Gd1 O01W 2.363(9) 4 ?
Gd1 O01W 2.363(9) 3_655 ?
Gd1 O01W 2.363(9) 2_655 ?
Gd1 O01W 2.363(9) . ?
Gd1 O11 2.381(9) 2_655 ?
Gd1 O11 2.381(9) 3_655 ?
Gd1 O11 2.381(9) 4 ?
Gd1 O11 2.381(9) . ?
Gd2 O03W 2.357(8) 2_665 ?
Gd2 O03W 2.357(8) 3_655 ?
Gd2 O03W 2.357(8) 4_565 ?
Gd2 O03W 2.357(8) . ?
Gd2 O02W 2.367(9) . ?
Gd2 O02W 2.367(9) 4_565 ?
Gd2 O02W 2.367(9) 2_665 ?
Gd2 O02W 2.367(9) 3_655 ?
O01W H01A 0.850(5) . ?
O01W H01B 0.850(5) . ?
O02W H02A 0.850(5) . ?
O02W H02B 0.850(5) . ?
O03W H03A 0.850(5) . ?
O03W H03B 0.850(5) . ?
O04W H04A 0.850(4) . ?
O1 C11 1.356(14) . ?
O1 H1 0.8400 . ?
C11 C16 1.388(17) . ?
C11 C12 1.409(16) . ?
C12 C13 1.382(15) . ?
C12 C10 1.522(16) . ?
C13 C14 1.401(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(12) . ?
C14 S1 1.744(11) . ?
C15 C16 1.364(16) . ?
C15 H15 0.9500 . ?
C16 C20 1.497(16) 2 ?
S1 O16 1.454(8) . ?
S1 O11 1.454(8) . ?
S1 O15 1.456(8) . ?
S1 O12 1.471(8) . ?
S1 O13 1.487(8) . ?
S1 O14 1.497(8) . ?
C10 C26 1.568(17) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O2 C21 1.334(17) . ?
O2 H2 0.8400 . ?
C21 C26 1.413(17) . ?
C21 C22 1.461(18) . ?
C22 C23 1.35(2) . ?
C22 C20 1.570(17) . ?
C23 C24 1.366(17) . ?
C23 H23 0.9500 . ?
C24 C25 1.367(18) . ?
C24 S2 1.747(17) . ?
C25 C26 1.337(18) . ?
C25 H25 0.9500 . ?
S2 O24 1.490(10) . ?
S2 O23 1.491(10) . ?
S2 O22 1.502(10) . ?
S2 O25 1.503(10) . ?
S2 O26 1.514(10) . ?
S2 O21 1.519(10) . ?
C20 C16 1.497(16) 2 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
P1 C31 1.788(8) 2_655 ?
P1 C31 1.788(8) . ?
P1 C41 1.796(7) 2_655 ?
P1 C41 1.796(7) . ?
C31 C32 1.377(11) . ?
C31 C36 1.405(12) . ?
C32 C33 1.385(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.387(14) . ?
C33 H33 0.9500 . ?
C34 O37 1.353(14) . ?
C34 C35 1.390(16) . ?
C34 H34A 0.9500 . ?
C37 O37 1.45(2) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C35 C36 1.388(13) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.394(10) . ?
C41 C46 1.400(10) . ?
C42 C43 1.390(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.372(12) . ?
C43 H43 0.9500 . ?
C44 C45 1.392(13) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(11) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C1 N1 1.449(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 C2 1.351(5) . ?
N1 C4 1.354(5) . ?
C2 N2 1.316(5) . ?
C2 H2A 0.9500 . ?
N2 C3 1.390(5) . ?
N2 C5 1.484(5) . ?
C3 C4 1.392(5) . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C5 C6 1.503(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.503(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.530(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
O14 Gd1 O14 84.8(6) . 2_655 ?
O14 Gd1 O14 117.6(6) . 4 ?
O14 Gd1 O14 128.9(5) 2_655 4 ?
O14 Gd1 O14 128.9(5) . 3_655 ?
O14 Gd1 O14 117.6(6) 2_655 3_655 ?
O14 Gd1 O14 84.8(6) 4 3_655 ?
O14 Gd1 O01W 66.1(4) . 4 ?
O14 Gd1 O01W 150.6(4) 2_655 4 ?
O14 Gd1 O01W 72.2(4) 4 4 ?
O14 Gd1 O01W 80.8(4) 3_655 4 ?
O14 Gd1 O01W 150.6(4) . 3_655 ?
O14 Gd1 O01W 66.1(4) 2_655 3_655 ?
O14 Gd1 O01W 80.8(4) 4 3_655 ?
O14 Gd1 O01W 72.2(4) 3_655 3_655 ?
O01W Gd1 O01W 143.3(5) 4 3_655 ?
O14 Gd1 O01W 80.8(4) . 2_655 ?
O14 Gd1 O01W 72.2(4) 2_655 2_655 ?
O14 Gd1 O01W 150.6(4) 4 2_655 ?
O14 Gd1 O01W 66.1(4) 3_655 2_655 ?
O01W Gd1 O01W 98.1(6) 4 2_655 ?
O01W Gd1 O01W 93.3(6) 3_655 2_655 ?
O14 Gd1 O01W 72.2(4) . . ?
O14 Gd1 O01W 80.8(4) 2_655 . ?
O14 Gd1 O01W 66.1(4) 4 . ?
O14 Gd1 O01W 150.6(4) 3_655 . ?
O01W Gd1 O01W 93.3(6) 4 . ?
O01W Gd1 O01W 98.1(6) 3_655 . ?
O01W Gd1 O01W 143.3(5) 2_655 . ?
O01W Gd1 O11 137.0(4) 4 2_655 ?
O01W Gd1 O11 79.4(4) 3_655 2_655 ?
O01W Gd1 O11 79.6(4) 2_655 2_655 ?
O01W Gd1 O11 68.5(4) . 2_655 ?
O01W Gd1 O11 68.5(4) 4 3_655 ?
O01W Gd1 O11 79.6(4) 3_655 3_655 ?
O01W Gd1 O11 79.4(4) 2_655 3_655 ?
O01W Gd1 O11 137.0(4) . 3_655 ?
O11 Gd1 O11 149.2(6) 2_655 3_655 ?
O01W Gd1 O11 79.6(4) 4 4 ?
O01W Gd1 O11 68.5(4) 3_655 4 ?
O01W Gd1 O11 137.0(4) 2_655 4 ?
O01W Gd1 O11 79.4(4) . 4 ?
O11 Gd1 O11 130.3(5) 2_655 4 ?
O11 Gd1 O11 59.6(6) 3_655 4 ?
O01W Gd1 O11 79.4(4) 4 . ?
O01W Gd1 O11 137.0(4) 3_655 . ?
O01W Gd1 O11 68.5(4) 2_655 . ?
O01W Gd1 O11 79.6(4) . . ?
O11 Gd1 O11 59.6(6) 2_655 . ?
O11 Gd1 O11 130.3(5) 3_655 . ?
O11 Gd1 O11 149.2(6) 4 . ?
O03W Gd2 O03W 142.5(5) 2_665 3_655 ?
O03W Gd2 O03W 84.7(5) 2_665 4_565 ?
O03W Gd2 O03W 107.4(4) 3_655 4_565 ?
O03W Gd2 O03W 107.4(4) 2_665 . ?
O03W Gd2 O03W 84.7(5) 3_655 . ?
O03W Gd2 O03W 142.5(5) 4_565 . ?
O03W Gd2 O02W 72.0(4) 2_665 . ?
O03W Gd2 O02W 144.8(4) 3_655 . ?
O03W Gd2 O02W 76.2(3) 4_565 . ?
O03W Gd2 O02W 74.4(3) . . ?
O03W Gd2 O02W 144.8(4) 2_665 4_565 ?
O03W Gd2 O02W 72.0(4) 3_655 4_565 ?
O03W Gd2 O02W 74.4(3) 4_565 4_565 ?
O03W Gd2 O02W 76.2(3) . 4_565 ?
O02W Gd2 O02W 75.6(6) . 4_565 ?
O03W Gd2 O02W 74.4(3) 2_665 2_665 ?
O03W Gd2 O02W 76.2(3) 3_655 2_665 ?
O03W Gd2 O02W 144.8(4) 4_565 2_665 ?
O03W Gd2 O02W 72.0(4) . 2_665 ?
O02W Gd2 O02W 121.5(6) . 2_665 ?
O02W Gd2 O02W 136.5(4) 4_565 2_665 ?
O03W Gd2 O02W 76.2(3) 2_665 3_655 ?
O03W Gd2 O02W 74.4(3) 3_655 3_655 ?
O03W Gd2 O02W 72.0(4) 4_565 3_655 ?
O03W Gd2 O02W 144.8(4) . 3_655 ?
O02W Gd2 O02W 136.5(4) . 3_655 ?
O02W Gd2 O02W 121.5(6) 4_565 3_655 ?
O02W Gd2 O02W 75.6(6) 2_665 3_655 ?
Gd1 O01W H01A 127.8(11) . . ?
Gd1 O01W H01B 127.7(11) . . ?
H01A O01W H01B 104.4(13) . . ?
Gd2 O02W H02A 123(5) . . ?
Gd2 O02W H02B 123(5) . . ?
H02A O02W H02B 104.5(13) . . ?
Gd2 O03W H03A 122(4) . . ?
Gd2 O03W H03B 122(4) . . ?
H03A O03W H03B 104.4(13) . . ?
C11 O1 H1 109.5 . . ?
O1 C11 C16 121.9(12) . . ?
O1 C11 C12 115.7(13) . . ?
C16 C11 C12 122.4(10) . . ?
C13 C12 C11 118.1(10) . . ?
C13 C12 C10 117.0(11) . . ?
C11 C12 C10 124.9(11) . . ?
C12 C13 C14 119.5(10) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.4(10) . . ?
C15 C14 S1 119.8(8) . . ?
C13 C14 S1 119.8(7) . . ?
C16 C15 C14 121.7(11) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C11 117.9(10) . . ?
C15 C16 C20 122.4(13) . 2 ?
C11 C16 C20 119.6(12) . 2 ?
O16 S1 O15 115.0(5) . . ?
O11 S1 O12 113.2(5) . . ?
O11 S1 O13 111.7(5) . . ?
O12 S1 O13 109.9(5) . . ?
O16 S1 O14 110.3(5) . . ?
O15 S1 O14 111.0(5) . . ?
O16 S1 C14 107.8(5) . . ?
O11 S1 C14 108.2(5) . . ?
O15 S1 C14 107.7(5) . . ?
O12 S1 C14 107.0(5) . . ?
O13 S1 C14 106.4(5) . . ?
O14 S1 C14 104.4(4) . . ?
S1 O11 Gd1 142.5(7) . . ?
S1 O14 Gd1 141.9(7) . . ?
C12 C10 C26 114.6(8) . . ?
C12 C10 H10A 108.6 . . ?
C26 C10 H10A 108.6 . . ?
C12 C10 H10B 108.6 . . ?
C26 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C21 O2 H2 109.5 . . ?
O2 C21 C26 122.5(13) . . ?
O2 C21 C22 120.6(12) . . ?
C26 C21 C22 116.9(14) . . ?
C23 C22 C21 120.4(12) . . ?
C23 C22 C20 125.3(12) . . ?
C21 C22 C20 114.2(15) . . ?
C22 C23 C24 119.7(14) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 121.0(16) . . ?
C23 C24 S2 119.1(11) . . ?
C25 C24 S2 119.9(10) . . ?
C26 C25 C24 122.3(13) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C25 C26 C21 119.8(12) . . ?
C25 C26 C10 123.9(11) . . ?
C21 C26 C10 116.3(13) . . ?
O23 S2 O22 110.0(6) . . ?
O24 S2 O25 110.4(7) . . ?
O24 S2 O26 109.3(7) . . ?
O25 S2 O26 108.3(7) . . ?
O23 S2 O21 108.8(6) . . ?
O22 S2 O21 108.2(6) . . ?
O24 S2 C24 110.4(7) . . ?
O23 S2 C24 111.1(6) . . ?
O22 S2 C24 110.0(6) . . ?
O25 S2 C24 109.6(6) . . ?
O26 S2 C24 108.7(6) . . ?
O21 S2 C24 108.7(5) . . ?
C16 C20 C22 112.4(8) 2 . ?
C16 C20 H20A 109.1 2 . ?
C22 C20 H20A 109.1 . . ?
C16 C20 H20B 109.1 2 . ?
C22 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C31 P1 C31 113.2(5) 2_655 . ?
C31 P1 C41 107.0(3) 2_655 2_655 ?
C31 P1 C41 109.2(3) . 2_655 ?
C31 P1 C41 109.2(3) 2_655 . ?
C31 P1 C41 107.0(3) . . ?
C41 P1 C41 111.5(5) 2_655 . ?
C32 C31 C36 119.1(8) . . ?
C32 C31 P1 118.3(6) . . ?
C36 C31 P1 122.2(7) . . ?
C31 C32 C33 119.9(8) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C34 120.6(9) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
O37 C34 C33 124.9(11) . . ?
O37 C34 C35 114.4(10) . . ?
C33 C34 C35 120.7(8) . . ?
C33 C34 H34A 119.7 . . ?
C35 C34 H34A 119.7 . . ?
O37 C37 H37A 109.5 . . ?
O37 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O37 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 O37 C37 125.9(14) . . ?
C36 C35 C34 118.1(10) . . ?
C36 C35 H35 121.0 . . ?
C34 C35 H35 121.0 . . ?
C35 C36 C31 121.5(9) . . ?
C35 C36 H36 119.2 . . ?
C31 C36 H36 119.2 . . ?
C42 C41 C46 119.7(6) . . ?
C42 C41 P1 118.8(5) . . ?
C46 C41 P1 121.4(5) . . ?
C43 C42 C41 119.7(7) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 120.7(7) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C43 C44 C45 119.8(7) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 120.5(7) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C41 119.6(7) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 N1 C4 110.3(5) . . ?
C2 N1 C1 125.0(4) . . ?
C4 N1 C1 124.8(4) . . ?
N2 C2 N1 107.0(3) . . ?
N2 C2 H2A 126.5 . . ?
N1 C2 H2A 126.5 . . ?
C2 N2 C3 110.9(5) . . ?
C2 N2 C5 124.3(19) . . ?
C3 N2 C5 124.8(18) . . ?
N2 C3 C4 104.9(5) . . ?
N2 C3 H3A 127.6 . . ?
C4 C3 H3A 127.6 . . ?
N1 C4 C3 106.9(5) . . ?
N1 C4 H4A 126.5 . . ?
C3 C4 H4A 126.5 . . ?
N2 C5 C6 115.1(6) . . ?
N2 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 C7 111.1(5) . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 112.3(5) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
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 . . ?

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
O1 C11 C12 C13 176.0(9) . . . . ?
C16 C11 C12 C13 -2.0(14) . . . . ?
O1 C11 C12 C10 -4.9(14) . . . . ?
C16 C11 C12 C10 177.1(9) . . . . ?
C11 C12 C13 C14 0.0(14) . . . . ?
C10 C12 C13 C14 -179.1(8) . . . . ?
C12 C13 C14 C15 2.2(13) . . . . ?
C12 C13 C14 S1 -177.9(7) . . . . ?
C13 C14 C15 C16 -2.6(13) . . . . ?
S1 C14 C15 C16 177.5(7) . . . . ?
C14 C15 C16 C11 0.6(13) . . . . ?
C14 C15 C16 C20 177.8(9) . . . 2 ?
O1 C11 C16 C15 -176.2(8) . . . . ?
C12 C11 C16 C15 1.6(14) . . . . ?
O1 C11 C16 C20 6.5(14) . . . 2 ?
C12 C11 C16 C20 -175.6(9) . . . 2 ?
C15 C14 S1 O16 23.3(9) . . . . ?
C13 C14 S1 O16 -156.7(8) . . . . ?
C15 C14 S1 O11 167.7(8) . . . . ?
C13 C14 S1 O11 -12.3(9) . . . . ?
C15 C14 S1 O15 -101.4(9) . . . . ?
C13 C14 S1 O15 78.7(9) . . . . ?
C15 C14 S1 O12 -70.0(8) . . . . ?
C13 C14 S1 O12 110.0(8) . . . . ?
C15 C14 S1 O13 47.5(9) . . . . ?
C13 C14 S1 O13 -132.5(8) . . . . ?
C15 C14 S1 O14 140.6(8) . . . . ?
C13 C14 S1 O14 -39.4(9) . . . . ?
O12 S1 O11 Gd1 98.7(12) . . . . ?
O13 S1 O11 Gd1 -26.0(14) . . . . ?
C14 S1 O11 Gd1 -142.8(10) . . . . ?
O16 S1 O14 Gd1 -84.7(13) . . . . ?
O15 S1 O14 Gd1 44.0(14) . . . . ?
C14 S1 O14 Gd1 159.7(10) . . . . ?
C13 C12 C10 C26 91.1(13) . . . . ?
C11 C12 C10 C26 -88.0(14) . . . . ?
O2 C21 C22 C23 -179.3(10) . . . . ?
C26 C21 C22 C23 0.8(14) . . . . ?
O2 C21 C22 C20 -2.0(13) . . . . ?
C26 C21 C22 C20 178.0(8) . . . . ?
C21 C22 C23 C24 -0.5(16) . . . . ?
C20 C22 C23 C24 -177.4(10) . . . . ?
C22 C23 C24 C25 -0.8(18) . . . . ?
C22 C23 C24 S2 -179.3(8) . . . . ?
C23 C24 C25 C26 1.9(18) . . . . ?
S2 C24 C25 C26 -179.6(8) . . . . ?
C24 C25 C26 C21 -1.6(17) . . . . ?
C24 C25 C26 C10 176.6(10) . . . . ?
O2 C21 C26 C25 -179.7(10) . . . . ?
C22 C21 C26 C25 0.3(14) . . . . ?
O2 C21 C26 C10 2.0(14) . . . . ?
C22 C21 C26 C10 -178.0(8) . . . . ?
C12 C10 C26 C25 -90.0(15) . . . . ?
C12 C10 C26 C21 88.2(13) . . . . ?
C23 C24 S2 O24 61.0(17) . . . . ?
C25 C24 S2 O24 -117.4(17) . . . . ?
C23 C24 S2 O23 -26.8(11) . . . . ?
C25 C24 S2 O23 154.7(10) . . . . ?
C23 C24 S2 O22 -148.8(10) . . . . ?
C25 C24 S2 O22 32.7(11) . . . . ?
C23 C24 S2 O25 -177.1(17) . . . . ?
C25 C24 S2 O25 4.4(17) . . . . ?
C23 C24 S2 O26 -58.9(17) . . . . ?
C25 C24 S2 O26 122.7(17) . . . . ?
C23 C24 S2 O21 92.9(10) . . . . ?
C25 C24 S2 O21 -85.6(10) . . . . ?
C23 C22 C20 C16 83.0(16) . . . 2 ?
C21 C22 C20 C16 -94.1(14) . . . 2 ?
C31 P1 C31 C32 -157.4(6) 2_655 . . . ?
C41 P1 C31 C32 -38.4(6) 2_655 . . . ?
C41 P1 C31 C32 82.3(6) . . . . ?
C31 P1 C31 C36 29.1(6) 2_655 . . . ?
C41 P1 C31 C36 148.1(6) 2_655 . . . ?
C41 P1 C31 C36 -91.1(7) . . . . ?
C36 C31 C32 C33 -0.9(11) . . . . ?
P1 C31 C32 C33 -174.6(5) . . . . ?
C31 C32 C33 C34 -1.5(12) . . . . ?
C32 C33 C34 O37 -179.4(10) . . . . ?
C32 C33 C34 C35 2.8(13) . . . . ?
C33 C34 O37 C37 174.9(15) . . . . ?
C35 C34 O37 C37 -7(2) . . . . ?
O37 C34 C35 C36 -179.5(9) . . . . ?
C33 C34 C35 C36 -1.5(14) . . . . ?
C34 C35 C36 C31 -1.0(14) . . . . ?
C32 C31 C36 C35 2.2(12) . . . . ?
P1 C31 C36 C35 175.7(7) . . . . ?
C31 P1 C41 C42 -92.3(6) 2_655 . . . ?
C31 P1 C41 C42 30.4(6) . . . . ?
C41 P1 C41 C42 149.7(6) 2_655 . . . ?
C31 P1 C41 C46 83.6(6) 2_655 . . . ?
C31 P1 C41 C46 -153.6(6) . . . . ?
C41 P1 C41 C46 -34.4(5) 2_655 . . . ?
C46 C41 C42 C43 1.6(10) . . . . ?
P1 C41 C42 C43 177.6(5) . . . . ?
C41 C42 C43 C44 -1.0(11) . . . . ?
C42 C43 C44 C45 0.1(12) . . . . ?
C43 C44 C45 C46 0.3(12) . . . . ?
C44 C45 C46 C41 0.3(11) . . . . ?
C42 C41 C46 C45 -1.3(10) . . . . ?
P1 C41 C46 C45 -177.1(5) . . . . ?
C4 N1 C2 N2 0.0(4) . . . . ?
C1 N1 C2 N2 -180.0(3) . . . . ?
N1 C2 N2 C3 0.0(5) . . . . ?
N1 C2 N2 C5 -179.9(5) . . . . ?
C2 N2 C3 C4 0.1(7) . . . . ?
C5 N2 C3 C4 179.9(6) . . . . ?
C2 N1 C4 C3 0.0(5) . . . . ?
C1 N1 C4 C3 -180.0(3) . . . . ?
N2 C3 C4 N1 -0.1(7) . . . . ?
C2 N2 C5 C6 73(2) . . . . ?
C3 N2 C5 C6 -107(2) . . . . ?
N2 C5 C6 C7 44(3) . . . . ?
C5 C6 C7 C8 173(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O01W H01A O13 0.850(5) 2.13(7) 2.797(16) 136(9) 4
O01W H01A O22 0.850(5) 2.48(4) 2.958(14) 117(3) .
O01W H01B O15 0.850(5) 2.40(12) 2.986(17) 127(12) 2_655
O02W H02A O13 0.850(5) 2.23(10) 2.947(14) 143(14) 1_565
O02W H02A O16 0.850(5) 1.98(12) 2.594(12) 128(13) 1_565
O03W H03A O22 0.850(5) 1.96(6) 2.738(16) 152(12) .
O03W H03A O25 0.850(5) 1.57(9) 2.24(2) 134(11) .
O03W H03B O12 0.850(5) 2.34(14) 2.699(14) 106(11) 2_655
O03W H03B O15 0.850(5) 2.82(13) 3.110(15) 102(10) 2_655
O04W H04A O23 0.850(4) 1.89(13) 2.358(11) 113(11) .
O04W H04A O24 0.850(4) 2.64(3) 3.14(3) 119.0(11) 2_565
O1 H1 O2 0.84 1.85 2.691(14) 179.5 2
O2 H2 O1 0.84 1.83 2.661(15) 172.2 .
C37 H37C O21 0.98 2.36 3.16(3) 138.0 5_666
C35 H35 O21 0.95 2.50 3.386(18) 155.3 5_666

_refine_diff_density_max         1.051
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_080808e
_database_code_depnum_ccdc_archive 'CCDC 1426676'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;

#==============================================================================


# 6. CRYSTALLOGRAPHY

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C28 H21 O16 S4, C28 H22 O16 S4, 4(C25 H22 O P), 0.5(C22 H32 N4), 24(H2 O)'
_chemical_formula_sum            'C167 H195 N2 O60 P4 S8'
_chemical_formula_weight         3570.60

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'
P P 0.2955 0.4335 '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'

_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                   17.4699(8)
_cell_length_b                   18.0265(7)
_cell_length_c                   23.3461(9)
_cell_angle_alpha                102.788(3)
_cell_angle_beta                 96.123(3)
_cell_angle_gamma                118.576(4)
_cell_volume                     6099.4(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7877
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      62.0

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.972
#         
#_exptl_crystal_F_000              1879
#
#  In consideration of disordered solvent density removed
#  by program SQUEEZE, the F(000), formula weight, density
#  will have slightly different values.
#
_exptl_crystal_F_000             1921
#
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.459
_shelx_estimated_absorpt_T_min   0.560
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75265
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            36795
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.903
_diffrn_reflns_theta_max         62.246
_diffrn_reflns_theta_full        62.246
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             18492
_reflns_number_gt                7102
_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       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
Residual electron density in the crystal which could not be interpreted
as chemically reasonable moieties was effectively removed by use
of the program Squeeze.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1500P)²+20.0000P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00167(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         18492
_refine_ls_number_parameters     1112
_refine_ls_number_restraints     326
_refine_ls_R_factor_all          0.2438
_refine_ls_R_factor_gt           0.1719
_refine_ls_wR_factor_ref         0.4396
_refine_ls_wR_factor_gt          0.4089
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.027
_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
O1 O 0.2548(4) 0.2299(5) 0.4149(4) 0.112(2) Uani 1 1 d . . . . .
C11 C 0.2847(7) 0.1926(7) 0.3746(6) 0.104(3) Uani 1 1 d . . . . .
C12 C 0.3555(8) 0.2462(7) 0.3530(6) 0.114(3) Uani 1 1 d . . . . .
C13 C 0.3889(8) 0.2053(9) 0.3132(7) 0.144(5) Uani 1 1 d . . . . .
H13 H 0.4378 0.2413 0.2983 0.173 Uiso 1 1 calc R U . . .
C14 C 0.3533(8) 0.1156(8) 0.2951(6) 0.152(5) Uani 1 1 d D . . . .
C15 C 0.2829(10) 0.0647(8) 0.3163(7) 0.146(5) Uani 1 1 d . . . . .
H15 H 0.2579 0.0022 0.3038 0.175 Uiso 1 1 calc R U . . .
C16 C 0.2459(7) 0.1008(8) 0.3557(6) 0.116(4) Uani 1 1 d . . . . .
S1 S 0.4016(3) 0.0658(3) 0.2491(3) 0.205(2) Uani 1 1 d D U . . .
O11 O 0.3286(8) -0.0219(8) 0.2147(7) 0.209(4) Uiso 0.6667 1 d D . P A 1
O12 O 0.4415(11) 0.1221(10) 0.2131(7) 0.209(4) Uiso 0.6667 1 d D . P A 1
O13 O 0.4670(9) 0.0644(11) 0.2922(6) 0.209(4) Uiso 0.6667 1 d D . P A 1
O14 O 0.3725(18) -0.0186(11) 0.2593(12) 0.209(4) Uiso 0.3333 1 d D . P A 2
O15 O 0.3651(17) 0.0567(19) 0.1877(5) 0.209(4) Uiso 0.3333 1 d D . P A 2
O16 O 0.4972(8) 0.1262(13) 0.2693(11) 0.209(4) Uiso 0.3333 1 d D . P A 2
C1 C 0.3968(7) 0.3454(6) 0.3695(5) 0.114(3) Uani 1 1 d . . . . .
H1A H 0.4571 0.3720 0.3610 0.136 Uiso 1 1 calc R U . . .
H1B H 0.4050 0.3700 0.4135 0.136 Uiso 1 1 calc R U . . .
O2 O 0.2682(5) 0.3765(5) 0.4133(4) 0.127(2) Uani 1 1 d . . . . .
C21 C 0.2792(8) 0.3868(6) 0.3590(5) 0.096(3) Uani 1 1 d . . . . .
C22 C 0.2279(8) 0.4127(7) 0.3279(6) 0.105(3) Uani 1 1 d . . . . .
C23 C 0.2379(8) 0.4198(7) 0.2727(7) 0.123(4) Uani 1 1 d . . . . .
H23 H 0.2029 0.4369 0.2514 0.147 Uiso 1 1 calc R U . . .
C24 C 0.2974(8) 0.4030(8) 0.2454(6) 0.129(4) Uani 1 1 d D . . . .
C25 C 0.3478(8) 0.3781(7) 0.2775(7) 0.131(4) Uani 1 1 d . . . . .
H25 H 0.3884 0.3653 0.2599 0.157 Uiso 1 1 calc R U . . .
C26 C 0.3398(7) 0.3715(6) 0.3347(6) 0.100(3) Uani 1 1 d . . . . .
S2 S 0.3126(4) 0.4164(4) 0.1732(2) 0.215(2) Uani 1 1 d D . . . .
O21 O 0.3471(15) 0.5087(9) 0.1811(8) 0.223(5) Uiso 0.5 1 d D . P B 1
O22 O 0.3771(13) 0.3914(15) 0.1606(8) 0.223(5) Uiso 0.5 1 d D . P B 1
O23 O 0.2267(9) 0.3592(14) 0.1321(6) 0.223(5) Uiso 0.5 1 d D . P B 1
O24 O 0.2503(13) 0.4412(16) 0.1536(8) 0.223(5) Uiso 0.5 1 d D . P B 2
O25 O 0.4043(9) 0.4842(13) 0.1835(7) 0.223(5) Uiso 0.5 1 d D . P B 2
O26 O 0.2916(16) 0.3315(10) 0.1358(7) 0.223(5) Uiso 0.5 1 d D . P B 2
C2 C 0.1564(9) 0.4282(8) 0.3530(6) 0.136(4) Uani 1 1 d . . . . .
H2A H 0.1772 0.4525 0.3978 0.163 Uiso 1 1 calc R U . . .
H2B H 0.1521 0.4736 0.3380 0.163 Uiso 1 1 calc R U . . .
O3 O 0.1033(5) 0.2879(5) 0.4080(4) 0.122(2) Uani 1 1 d . . . . .
C31 C 0.0444(9) 0.2814(9) 0.3648(6) 0.116(4) Uani 1 1 d . . . . .
C32 C -0.0467(9) 0.2027(10) 0.3458(6) 0.127(4) Uani 1 1 d . . . . .
C33 C -0.1119(11) 0.1954(11) 0.3019(7) 0.151(5) Uani 1 1 d . U . . .
H33 H -0.1715 0.1455 0.2907 0.181 Uiso 1 1 calc R U . . .
C34 C -0.0896(8) 0.2623(9) 0.2740(5) 0.143(5) Uani 1 1 d D . . . .
C35 C -0.0041(11) 0.3377(10) 0.2917(6) 0.146(5) Uani 1 1 d . . . . .
H35 H 0.0081 0.3833 0.2737 0.176 Uiso 1 1 calc R U . . .
C36 C 0.0661(10) 0.3484(10) 0.3366(6) 0.126(4) Uani 1 1 d . . . . .
S3 S -0.1754(3) 0.2563(4) 0.2207(3) 0.214(2) Uani 1 1 d D . . . .
O31 O -0.1288(11) 0.3038(11) 0.1794(7) 0.196(4) Uiso 0.5 1 d D . P C 1
O32 O -0.2366(10) 0.1598(8) 0.1882(7) 0.196(4) Uiso 0.5 1 d D . P C 1
O33 O -0.2176(11) 0.2972(12) 0.2550(6) 0.196(4) Uiso 0.5 1 d D . P C 1
O34 O -0.2550(8) 0.2250(12) 0.2480(7) 0.196(4) Uiso 0.5 1 d D . P C 2
O35 O -0.1423(11) 0.3488(8) 0.2210(8) 0.196(4) Uiso 0.5 1 d D . P C 2
O36 O -0.1910(11) 0.1951(11) 0.1631(5) 0.196(4) Uiso 0.5 1 d D . P C 2
C3 C -0.0679(8) 0.1293(10) 0.3717(7) 0.148(5) Uani 1 1 d . . . . .
H3A H -0.1339 0.0922 0.3651 0.178 Uiso 1 1 calc R U . . .
H3B H -0.0409 0.1545 0.4160 0.178 Uiso 1 1 calc R U . . .
O4 O 0.0879(5) 0.1379(6) 0.4301(4) 0.159(3) Uani 1 1 d . . . . .
C41 C 0.0447(9) 0.0791(8) 0.3717(5) 0.118(4) Uani 1 1 d . . . . .
C42 C 0.0780(8) 0.0291(8) 0.3443(6) 0.113(3) Uani 1 1 d . . . . .
C43 C 0.0303(9) -0.0321(7) 0.2889(6) 0.117(4) Uani 1 1 d . . . . .
H43 H 0.0512 -0.0688 0.2698 0.141 Uiso 1 1 calc R U . . .
C44 C -0.0459(7) -0.0409(6) 0.2608(5) 0.112(3) Uani 1 1 d D . . . .
C45 C -0.0798(8) 0.0067(8) 0.2878(5) 0.120(4) Uani 1 1 d . . . . .
H45 H -0.1364 -0.0044 0.2681 0.144 Uiso 1 1 calc R U . . .
C46 C -0.0333(8) 0.0721(8) 0.3439(6) 0.119(4) Uani 1 1 d . . . . .
S4 S -0.1131(2) -0.1256(2) 0.18883(15) 0.1376(12) Uani 1 1 d D . . . .
O41 O -0.1290(8) -0.0791(7) 0.1491(4) 0.141(2) Uiso 0.5 1 d D . P D 1
O42 O -0.0595(7) -0.1628(8) 0.1685(5) 0.141(2) Uiso 0.5 1 d D . P D 1
O43 O -0.1958(6) -0.1891(7) 0.2010(5) 0.141(2) Uiso 0.5 1 d D . P D 1
O44 O -0.0480(7) -0.1318(8) 0.1558(5) 0.141(2) Uiso 0.5 1 d D . P D 2
O45 O -0.1677(7) -0.2074(6) 0.2030(5) 0.141(2) Uiso 0.5 1 d D . P D 2
O46 O -0.1652(8) -0.0955(8) 0.1593(5) 0.141(2) Uiso 0.5 1 d D . P D 2
C4 C 0.1675(9) 0.0422(8) 0.3777(6) 0.136(4) Uani 1 1 d . U . . .
H4A H 0.1786 0.0692 0.4218 0.163 Uiso 1 1 calc R U . . .
H4B H 0.1621 -0.0164 0.3710 0.163 Uiso 1 1 calc R U . . .
P1A P 0.02935(16) 0.25019(15) 0.60781(12) 0.0909(8) Uani 1 1 d . . . . .
O1A O 0.1159(4) 0.5777(4) 0.5451(3) 0.0982(18) Uani 1 1 d . . . . .
C11A C 0.0546(6) 0.3511(6) 0.5920(5) 0.087(2) Uani 1 1 d . . . . .
C12A C 0.0504(6) 0.3514(6) 0.5328(5) 0.091(3) Uani 1 1 d . . . . .
H12A H 0.0325 0.2984 0.5014 0.109 Uiso 1 1 calc R U . . .
C13A C 0.0724(6) 0.4299(6) 0.5185(4) 0.088(3) Uani 1 1 d . . . . .
H13A H 0.0704 0.4305 0.4778 0.106 Uiso 1 1 calc R U . . .
C14A C 0.0969(5) 0.5058(6) 0.5642(5) 0.079(2) Uani 1 1 d . . . . .
C15A C 0.0992(5) 0.5035(6) 0.6226(5) 0.084(3) Uani 1 1 d . . . . .
H15A H 0.1148 0.5556 0.6540 0.101 Uiso 1 1 calc R U . . .
C16A C 0.0798(5) 0.4287(6) 0.6364(4) 0.080(2) Uani 1 1 d . . . . .
H16A H 0.0834 0.4295 0.6775 0.096 Uiso 1 1 calc R U . . .
C17A C 0.1421(7) 0.6604(6) 0.5903(5) 0.113(3) Uani 1 1 d . . . . .
H17A H 0.1537 0.7062 0.5706 0.169 Uiso 1 1 calc R U . . .
H17B H 0.0935 0.6519 0.6105 0.169 Uiso 1 1 calc R U . . .
H17C H 0.1967 0.6792 0.6203 0.169 Uiso 1 1 calc R U . . .
C21A C -0.0042(8) 0.2502(7) 0.6767(5) 0.098(3) Uani 1 1 d . . . . .
C22A C 0.0600(9) 0.3017(8) 0.7327(6) 0.127(4) Uani 1 1 d . . . . .
H22A H 0.1220 0.3366 0.7340 0.152 Uiso 1 1 calc R U . . .
C23A C 0.0316(13) 0.3007(10) 0.7860(6) 0.147(5) Uani 1 1 d . . . . .
H23A H 0.0746 0.3326 0.8241 0.176 Uiso 1 1 calc R U . . .
C24A C -0.0571(15) 0.2544(12) 0.7839(9) 0.153(6) Uani 1 1 d . . . . .
H24A H -0.0758 0.2569 0.8207 0.184 Uiso 1 1 calc R U . . .
C25A C -0.1209(10) 0.2038(9) 0.7296(8) 0.126(4) Uani 1 1 d . . . . .
H25A H -0.1829 0.1707 0.7289 0.151 Uiso 1 1 calc R U . . .
C26A C -0.0937(8) 0.2018(7) 0.6770(6) 0.104(3) Uani 1 1 d . . . . .
H26A H -0.1375 0.1661 0.6396 0.125 Uiso 1 1 calc R U . . .
C31A C -0.0598(6) 0.1597(6) 0.5477(5) 0.094(3) Uani 1 1 d . . . . .
C32A C -0.1318(7) 0.1650(6) 0.5237(5) 0.103(3) Uani 1 1 d . . . . .
H32A H -0.1326 0.2179 0.5391 0.124 Uiso 1 1 calc R U . . .
C33A C -0.2068(7) 0.0911(7) 0.4750(5) 0.110(3) Uani 1 1 d . . . . .
H33A H -0.2552 0.0955 0.4569 0.132 Uiso 1 1 calc R U . . .
C34A C -0.2039(8) 0.0152(7) 0.4568(5) 0.113(3) Uani 1 1 d . . . . .
H34A H -0.2531 -0.0360 0.4272 0.136 Uiso 1 1 calc R U . . .
C35A C -0.1290(8) 0.0121(7) 0.4814(5) 0.114(3) Uani 1 1 d . . . . .
H35A H -0.1271 -0.0403 0.4664 0.137 Uiso 1 1 calc R U . . .
C36A C -0.0599(7) 0.0814(6) 0.5257(5) 0.102(3) Uani 1 1 d . . . . .
H36A H -0.0107 0.0769 0.5421 0.122 Uiso 1 1 calc R U . . .
C41A C 0.1258(6) 0.2394(6) 0.6112(5) 0.083(2) Uani 1 1 d . . . . .
C42A C 0.1740(6) 0.2575(5) 0.5686(5) 0.092(3) Uani 1 1 d . . . . .
H42A H 0.1574 0.2792 0.5388 0.111 Uiso 1 1 calc R U . . .
C43A C 0.2469(7) 0.2452(6) 0.5674(5) 0.100(3) Uani 1 1 d . . . . .
H43A H 0.2793 0.2575 0.5372 0.120 Uiso 1 1 calc R U . . .
C44A C 0.2711(7) 0.2144(6) 0.6116(6) 0.102(3) Uani 1 1 d . . . . .
H44A H 0.3224 0.2085 0.6123 0.123 Uiso 1 1 calc R U . . .
C45A C 0.2229(7) 0.1920(7) 0.6547(5) 0.108(3) Uani 1 1 d . . . . .
H45A H 0.2394 0.1697 0.6839 0.129 Uiso 1 1 calc R U . . .
C46A C 0.1471(6) 0.2037(6) 0.6536(5) 0.104(3) Uani 1 1 d . . . . .
H46A H 0.1113 0.1872 0.6816 0.125 Uiso 1 1 calc R U . . .
P1B P 0.40641(15) 0.70535(17) 0.48443(15) 0.1024(9) Uani 1 1 d . . . . .
O2B O 0.5854(6) 0.5439(5) 0.3502(6) 0.169(4) Uani 1 1 d . . . . .
C11B C 0.4560(6) 0.6545(6) 0.4418(6) 0.094(3) Uani 1 1 d . . . . .
C12B C 0.5070(6) 0.6268(7) 0.4713(5) 0.105(3) Uani 1 1 d . . . . .
H12B H 0.5134 0.6343 0.5134 0.126 Uiso 1 1 calc R U . . .
C13B C 0.5489(6) 0.5877(7) 0.4385(6) 0.107(3) Uani 1 1 d . . . . .
H13B H 0.5835 0.5688 0.4583 0.128 Uiso 1 1 calc R U . . .
C14B C 0.5392(7) 0.5777(7) 0.3791(7) 0.103(3) Uani 1 1 d . U . . .
C15B C 0.4900(8) 0.6030(7) 0.3487(5) 0.113(3) Uani 1 1 d . . . . .
H15B H 0.4851 0.5959 0.3067 0.135 Uiso 1 1 calc R U . . .
C16B C 0.4466(7) 0.6400(6) 0.3808(6) 0.105(3) Uani 1 1 d . . . . .
H16B H 0.4097 0.6553 0.3596 0.127 Uiso 1 1 calc R U . . .
C17B C 0.5908(12) 0.5404(12) 0.2842(8) 0.186(7) Uani 1 1 d . . . . .
H17D H 0.6267 0.5141 0.2721 0.278 Uiso 1 1 calc R U . . .
H17E H 0.5300 0.5040 0.2574 0.278 Uiso 1 1 calc R U . . .
H17F H 0.6190 0.6007 0.2812 0.278 Uiso 1 1 calc R U . . .
C21B C 0.3081(6) 0.6906(6) 0.4390(5) 0.098(3) Uani 1 1 d . . . . .
C22B C 0.3172(7) 0.7315(7) 0.3963(6) 0.123(4) Uani 1 1 d . . . . .
H22B H 0.3756 0.7730 0.3939 0.148 Uiso 1 1 calc R U . . .
C23B C 0.2394(9) 0.7130(9) 0.3543(7) 0.146(5) Uani 1 1 d . . . . .
H23B H 0.2448 0.7390 0.3226 0.175 Uiso 1 1 calc R U . . .
C24B C 0.1555(7) 0.6552(7) 0.3622(6) 0.119(4) Uani 1 1 d . . . . .
H24B H 0.1026 0.6383 0.3335 0.142 Uiso 1 1 calc R U . . .
C25B C 0.1477(6) 0.6227(6) 0.4098(5) 0.093(3) Uani 1 1 d . . . . .
H25B H 0.0903 0.5892 0.4171 0.112 Uiso 1 1 calc R U . . .
C26B C 0.2243(6) 0.6390(5) 0.4473(5) 0.091(3) Uani 1 1 d . . . . .
H26B H 0.2190 0.6140 0.4796 0.109 Uiso 1 1 calc R U . . .
C31B C 0.3761(6) 0.6551(8) 0.5403(6) 0.099(3) Uani 1 1 d . . . . .
C32B C 0.3329(6) 0.5640(7) 0.5276(6) 0.098(3) Uani 1 1 d . . . . .
H32B H 0.3207 0.5275 0.4876 0.118 Uiso 1 1 calc R U . . .
C33B C 0.3075(7) 0.5258(9) 0.5716(9) 0.121(4) Uani 1 1 d . . . . .
H33B H 0.2783 0.4630 0.5615 0.145 Uiso 1 1 calc R U . . .
C34B C 0.3227(9) 0.5756(15) 0.6308(9) 0.138(5) Uani 1 1 d . . . . .
H34B H 0.3056 0.5476 0.6611 0.165 Uiso 1 1 calc R U . . .
C35B C 0.3615(10) 0.6633(16) 0.6442(7) 0.147(5) Uani 1 1 d . . . . .
H35B H 0.3703 0.6985 0.6839 0.176 Uiso 1 1 calc R U . . .
C36B C 0.3898(7) 0.7041(9) 0.5989(9) 0.131(4) Uani 1 1 d . . . . .
H36B H 0.4191 0.7670 0.6092 0.157 Uiso 1 1 calc R U . . .
C41B C 0.4836(7) 0.8218(7) 0.5153(5) 0.115(3) Uani 1 1 d . U . . .
C42B C 0.5756(6) 0.8607(7) 0.5206(5) 0.115(3) Uani 1 1 d . . . . .
H42B H 0.5988 0.8242 0.5059 0.138 Uiso 1 1 calc R U . . .
C43B C 0.6345(7) 0.9520(8) 0.5467(6) 0.132(4) Uani 1 1 d . . . . .
H43B H 0.6965 0.9772 0.5473 0.158 Uiso 1 1 calc R U . . .
C44B C 0.6037(11) 1.0057(11) 0.5715(7) 0.166(5) Uani 1 1 d . U . . .
H44B H 0.6445 1.0677 0.5900 0.200 Uiso 1 1 calc R U . . .
C45B C 0.5129(12) 0.9696(11) 0.5697(8) 0.180(6) Uani 1 1 d . U . . .
H45B H 0.4919 1.0055 0.5898 0.216 Uiso 1 1 calc R U . . .
C46B C 0.4510(10) 0.8769(10) 0.5370(7) 0.167(5) Uani 1 1 d . U . . .
H46B H 0.3880 0.8533 0.5302 0.201 Uiso 1 1 calc R U . . .
C01D C -0.1665(14) -0.2936(12) 0.0606(8) 0.203(6) Uiso 0.25 1 d D . P E 1
C02D C -0.1006(15) -0.3157(16) 0.0586(11) 0.203(6) Uiso 0.25 1 d D . P E 1
H02A H -0.1167 -0.3761 0.0500 0.243 Uiso 0.25 1 calc R U P E 1
C03D C -0.0116(15) -0.2496(12) 0.0692(11) 0.203(6) Uiso 0.25 1 d D . P E 1
H03A H 0.0329 -0.2654 0.0677 0.243 Uiso 0.25 1 calc R U P E 1
C04D C 0.0142(14) -0.1603(12) 0.0819(9) 0.203(6) Uiso 0.25 1 d D . P E 1
C05D C -0.0535(15) -0.1398(14) 0.0836(15) 0.203(6) Uiso 0.25 1 d D . P E 1
H05A H -0.0374 -0.0795 0.0921 0.243 Uiso 0.25 1 calc R U P E 1
C06D C -0.1441(16) -0.2052(13) 0.0732(15) 0.203(6) Uiso 0.25 1 d D . P E 1
H06A H -0.1890 -0.1899 0.0746 0.243 Uiso 0.25 1 calc R U P E 1
C07D C -0.2659(15) -0.3678(14) 0.0487(12) 0.203(6) Uiso 0.25 1 d D . P E 1
H07A H -0.2780 -0.3751 0.0882 0.243 Uiso 0.25 1 calc R U P E 1
H07B H -0.3043 -0.3470 0.0326 0.243 Uiso 0.25 1 calc R U P E 1
N08D N -0.2949(12) -0.4554(13) 0.0073(9) 0.203(6) Uiso 0.25 1 d D . P E 1
C09D C -0.255(2) -0.4671(16) -0.0396(14) 0.203(6) Uiso 0.25 1 d D . P E 1
H09A H -0.2073 -0.4215 -0.0497 0.243 Uiso 0.25 1 calc R U P E 1
C10D C -0.298(2) -0.5546(16) -0.0681(14) 0.203(6) Uiso 0.25 1 d D . P E 1
H10A H -0.2853 -0.5829 -0.1022 0.243 Uiso 0.25 1 calc R U P E 1
N11D N -0.3631(17) -0.5959(13) -0.0384(13) 0.203(6) Uiso 0.25 1 d D . P E 1
C12D C -0.3590(17) -0.5341(13) 0.0064(13) 0.203(6) Uiso 0.25 1 d D . P E 1
H12C H -0.3965 -0.5447 0.0339 0.243 Uiso 0.25 1 calc R U P E 1
C13D C -0.423(2) -0.6921(14) -0.0565(19) 0.203(6) Uiso 0.25 1 d D . P E 1
H13C H -0.4856 -0.7043 -0.0625 0.243 Uiso 0.25 1 calc R U P E 1
H13D H -0.4122 -0.7119 -0.0219 0.243 Uiso 0.25 1 calc R U P E 1
C14D C -0.419(4) -0.7510(17) -0.1128(18) 0.203(6) Uiso 0.25 1 d D . P E 1
H14A H -0.4554 -0.7524 -0.1491 0.243 Uiso 0.25 1 calc R U P E 1
H14B H -0.3563 -0.7245 -0.1162 0.243 Uiso 0.25 1 calc R U P E 1
C15D C -0.454(5) -0.846(2) -0.1120(18) 0.203(6) Uiso 0.25 1 d D . P E 1
H15C H -0.5011 -0.8619 -0.0889 0.243 Uiso 0.25 1 calc R U P E 1
H15D H -0.4043 -0.8490 -0.0906 0.243 Uiso 0.25 1 calc R U P E 1
C16D C -0.494(4) -0.914(2) -0.175(2) 0.203(6) Uiso 0.25 1 d D . P E 1
H16C H -0.5151 -0.9736 -0.1717 0.304 Uiso 0.25 1 calc R U P E 1
H16D H -0.5445 -0.9125 -0.1964 0.304 Uiso 0.25 1 calc R U P E 1
H16E H -0.4476 -0.8996 -0.1981 0.304 Uiso 0.25 1 calc R U P E 1
C17D C 0.1124(15) -0.0883(14) 0.0934(12) 0.203(6) Uiso 0.25 1 d D . P E 1
H17G H 0.1494 -0.1086 0.1122 0.243 Uiso 0.25 1 calc R U P E 1
H17H H 0.1252 -0.0856 0.0534 0.243 Uiso 0.25 1 calc R U P E 1
N18D N 0.1452(13) 0.0024(13) 0.1306(9) 0.203(6) Uiso 0.25 1 d D . P E 1
C19D C 0.2244(18) 0.0754(15) 0.1306(16) 0.203(6) Uiso 0.25 1 d D . P E 1
H19A H 0.2654 0.0750 0.1070 0.243 Uiso 0.25 1 calc R U P E 1
C20D C 0.233(2) 0.1470(15) 0.1700(17) 0.203(6) Uiso 0.25 1 d D . P E 1
H20A H 0.2804 0.2068 0.1796 0.243 Uiso 0.25 1 calc R U P E 1
N21D N 0.1583(19) 0.1172(17) 0.1940(12) 0.203(6) Uiso 0.25 1 d D . P E 1
C22D C 0.1080(17) 0.0307(17) 0.1693(11) 0.203(6) Uiso 0.25 1 d D . P E 1
H22C H 0.0527 -0.0062 0.1780 0.243 Uiso 0.25 1 calc R U P E 1
C23D C 0.143(3) 0.176(2) 0.2389(16) 0.203(6) Uiso 0.25 1 d D . P E 1
H23C H 0.1944 0.2371 0.2478 0.243 Uiso 0.25 1 calc R U P E 1
H23D H 0.1450 0.1597 0.2766 0.243 Uiso 0.25 1 calc R U P E 1
C24D C 0.057(3) 0.179(4) 0.2253(17) 0.203(6) Uiso 0.25 1 d D . P E 1
H24C H 0.0054 0.1208 0.2232 0.243 Uiso 0.25 1 calc R U P E 1
H24D H 0.0604 0.2249 0.2593 0.243 Uiso 0.25 1 calc R U P E 1
C25D C 0.041(3) 0.199(4) 0.167(3) 0.203(6) Uiso 0.25 1 d D . P E 1
H25C H 0.0794 0.1883 0.1413 0.243 Uiso 0.25 1 calc R U P E 1
H25D H 0.0602 0.2621 0.1763 0.243 Uiso 0.25 1 calc R U P E 1
C26D C -0.057(3) 0.142(4) 0.131(2) 0.203(6) Uiso 0.25 1 d D . P E 1
H26C H -0.0634 0.1570 0.0934 0.304 Uiso 0.25 1 calc R U P E 1
H26D H -0.0755 0.0786 0.1201 0.304 Uiso 0.25 1 calc R U P E 1
H26E H -0.0948 0.1525 0.1551 0.304 Uiso 0.25 1 calc R U P E 1
O01W O 0.4425(3) 0.1380(3) 0.6566(3) 0.0826(17) Uani 1 1 d . . . . .
O02W O -0.3494(13) 0.1275(13) 0.3247(9) 0.173(7) Uiso 0.5 1 d . . P . .
O03W O 0.259(2) 0.708(2) 0.1938(14) 0.184(11) Uiso 0.3333 1 d . . P . .
O04W O 0.3168(18) 0.0138(17) 0.6896(12) 0.150(8) Uiso 0.3333 1 d . . P . .
O05W O -0.2778(16) -0.3797(16) 0.1747(11) 0.137(8) Uiso 0.3333 1 d . . P . .
O06W O 0.243(3) 0.822(3) 0.140(2) 0.207(17) Uiso 0.25 1 d . . P . .
O07W O -0.292(3) -0.042(3) 0.178(2) 0.216(18) Uiso 0.25 1 d . . P . .
O08W O -0.200(3) 0.274(3) 0.056(2) 0.223(19) Uiso 0.25 1 d . . P . .
O09W O 0.483(4) 0.530(4) 0.016(3) 0.27(3) Uiso 0.25 1 d . . P . .
O10W O -0.101(4) 0.491(3) 0.097(2) 0.154(17) Uiso 0.1667 1 d . . P . .
O11W O 0.522(4) 0.710(4) 0.232(3) 0.19(2) Uiso 0.1667 1 d . . P . .
O12W O 0.422(5) 0.823(5) -0.068(4) 0.23(3) Uiso 0.1667 1 d . . P . .
O13W O 0.3758(15) -0.1355(15) 0.2902(10) 0.193(8) Uiso 0.5 1 d . . P F 1
O14W O -0.0716(15) 0.4930(14) 0.2206(9) 0.159(7) Uiso 0.5 1 d . . P G 1
O15W O -0.412(2) -0.102(2) 0.0658(14) 0.130(9) Uiso 0.25 1 d . . P H 1
O16W O 0.512(2) 0.295(2) 0.2083(16) 0.151(11) Uiso 0.25 1 d . . P I 1
O17W O -0.223(3) -0.508(3) 0.1650(19) 0.178(14) Uiso 0.25 1 d . . P J 1
O18W O -0.278(4) -0.207(4) 0.042(2) 0.23(2) Uiso 0.25 1 d . . P K 1
O19W O 0.439(4) 0.622(4) -0.048(2) 0.156(18) Uiso 0.1667 1 d . . P L 1
O20W O -0.473(4) -0.445(4) 0.132(3) 0.18(2) Uiso 0.1667 1 d . . P M 1
O21W O 0.4471(7) 0.7515(7) 0.0219(5) 0.141(3) Uiso 0.75 1 d . . P N 2
O22W O 0.1138(15) 0.1599(15) 0.2194(10) 0.254(8) Uiso 0.75 1 d . . P O 2
O23W O -0.4310(13) -0.1694(13) 0.0926(9) 0.170(7) Uiso 0.5 1 d . . P P 2
O24W O 0.0475(16) 0.0634(16) 0.1469(11) 0.199(8) Uiso 0.5 1 d . . P Q 2
O25W O -0.3436(17) -0.6122(17) -0.0112(12) 0.222(10) Uiso 0.5 1 d . . P R 2
O26W O 0.360(3) 0.646(3) 0.242(2) 0.206(17) Uiso 0.25 1 d . . P S 2
O27W O 0.587(4) 0.205(4) 0.201(2) 0.23(2) Uiso 0.25 1 d . . P T 2
O28W O -0.290(3) -0.587(3) 0.233(2) 0.189(15) Uiso 0.25 1 d . . P U 2
O29W O -0.112(3) -0.417(3) -0.115(2) 0.209(17) Uiso 0.25 1 d . . P V 2
O30W O -0.202(3) -0.249(3) -0.0208(19) 0.184(15) Uiso 0.25 1 d . . P W 2
O31W O -0.121(3) -0.543(3) -0.2045(19) 0.186(15) Uiso 0.25 1 d . . P X 2
O32W O -0.029(3) -0.067(3) 0.0158(17) 0.171(13) Uiso 0.25 1 d . . P Y 2
O33W O -0.014(3) 0.527(2) 0.2217(15) 0.134(11) Uiso 0.25 1 d . . P Z 2
O34W O 0.465(3) 0.347(3) 0.117(2) 0.148(16) Uiso 0.1667 1 d . . P A 2
O35W O 0.0273(13) 0.1356(12) 0.1768(9) 0.152(6) Uiso 0.5 1 d . . P B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C11 1.330(13) . ?
C11 C12 1.387(15) . ?
C11 C16 1.391(14) . ?
C12 C13 1.405(16) . ?
C12 C1 1.504(14) . ?
C13 C14 1.364(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.360(18) . ?
C14 S1 1.779(14) . ?
C15 C16 1.397(17) . ?
C15 H15 0.9500 . ?
C16 C4 1.503(15) . ?
S1 O12 1.431(10) . ?
S1 O16 1.435(10) . ?
S1 O11 1.436(10) . ?
S1 O14 1.440(10) . ?
S1 O15 1.446(10) . ?
S1 O13 1.451(10) . ?
C1 C26 1.523(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
O2 C21 1.341(12) . ?
C21 C26 1.362(14) . ?
C21 C22 1.400(14) . ?
C22 C23 1.344(15) . ?
C22 C2 1.549(15) . ?
C23 C24 1.391(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(16) . ?
C24 S2 1.783(14) . ?
C25 C26 1.384(16) . ?
C25 H25 0.9500 . ?
S2 O23 1.419(11) . ?
S2 O25 1.426(11) . ?
S2 O24 1.430(11) . ?
S2 O26 1.430(11) . ?
S2 O21 1.431(11) . ?
S2 O22 1.434(11) . ?
C2 C36 1.470(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C31 1.305(14) . ?
C31 C36 1.415(17) . ?
C31 C32 1.468(17) . ?
C32 C33 1.382(18) . ?
C32 C3 1.480(17) . ?
C33 C34 1.409(18) . ?
C33 H33 0.9500 . ?
C34 C35 1.388(17) . ?
C34 S3 1.787(13) . ?
C35 C36 1.431(17) . ?
C35 H35 0.9500 . ?
S3 O36 1.439(10) . ?
S3 O33 1.454(10) . ?
S3 O35 1.479(10) . ?
S3 O31 1.480(10) . ?
S3 O32 1.485(10) . ?
S3 O34 1.503(10) . ?
C3 C46 1.495(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4 C41 1.387(13) . ?
C41 C42 1.373(16) . ?
C41 C46 1.380(16) . ?
C42 C43 1.359(15) . ?
C42 C4 1.553(16) . ?
C43 C44 1.339(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.345(14) . ?
C44 S4 1.806(11) . ?
C45 C46 1.393(15) . ?
C45 H45 0.9500 . ?
S4 O46 1.449(8) . ?
S4 O42 1.453(8) . ?
S4 O43 1.458(8) . ?
S4 O45 1.460(8) . ?
S4 O41 1.467(8) . ?
S4 O44 1.474(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
P1A C21A 1.769(11) . ?
P1A C31A 1.773(10) . ?
P1A C41A 1.782(10) . ?
P1A C11A 1.789(10) . ?
O1A C14A 1.366(10) . ?
O1A C17A 1.446(11) . ?
C11A C16A 1.378(11) . ?
C11A C12A 1.379(12) . ?
C12A C13A 1.405(12) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.375(12) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.371(12) . ?
C15A C16A 1.346(11) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C21A C26A 1.380(14) . ?
C21A C22A 1.409(15) . ?
C22A C23A 1.389(16) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.352(19) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.376(19) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.363(15) . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?
C31A C32A 1.377(13) . ?
C31A C36A 1.388(12) . ?
C32A C33A 1.457(13) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.368(13) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.402(14) . ?
C34A H34A 0.9500 . ?
C35A C36A 1.344(13) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C41A C42A 1.366(12) . ?
C41A C46A 1.402(13) . ?
C42A C43A 1.396(13) . ?
C42A H42A 0.9500 . ?
C43A C44A 1.391(14) . ?
C43A H43A 0.9500 . ?
C44A C45A 1.385(14) . ?
C44A H44A 0.9500 . ?
C45A C46A 1.435(13) . ?
C45A H45A 0.9500 . ?
C46A H46A 0.9500 . ?
P1B C31B 1.736(12) . ?
P1B C11B 1.765(11) . ?
P1B C41B 1.777(11) . ?
P1B C21B 1.788(10) . ?
O2B C14B 1.372(13) . ?
O2B C17B 1.542(16) . ?
C11B C16B 1.366(14) . ?
C11B C12B 1.404(13) . ?
C12B C13B 1.410(14) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.340(14) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.356(15) . ?
C15B C16B 1.401(14) . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C21B C22B 1.346(14) . ?
C21B C26B 1.372(12) . ?
C22B C23B 1.433(15) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.396(15) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.357(14) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.381(12) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C31B C36B 1.379(17) . ?
C31B C32B 1.380(13) . ?
C32B C33B 1.357(15) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.390(18) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.329(19) . ?
C34B H34B 0.9500 . ?
C35B C36B 1.418(18) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C41B C42B 1.389(13) . ?
C41B C46B 1.396(15) . ?
C42B C43B 1.393(14) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.371(17) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.388(19) . ?
C44B H44B 0.9500 . ?
C45B C46B 1.440(19) . ?
C45B H45B 0.9500 . ?
C46B H46B 0.9500 . ?
C01D C02D 1.389(10) . ?
C01D C06D 1.395(10) . ?
C01D C07D 1.547(9) . ?
C02D C03D 1.383(10) . ?
C02D H02A 0.9500 . ?
C03D C04D 1.396(10) . ?
C03D H03A 0.9500 . ?
C04D C05D 1.399(10) . ?
C04D C17D 1.522(9) . ?
C05D C06D 1.400(10) . ?
C05D H05A 0.9500 . ?
C06D H06A 0.9500 . ?
C07D N08D 1.462(8) . ?
C07D H07A 0.9900 . ?
C07D H07B 0.9900 . ?
N08D C12D 1.315(9) . ?
N08D C09D 1.386(9) . ?
C09D C10D 1.339(10) . ?
C09D H09A 0.9500 . ?
C10D N11D 1.388(9) . ?
C10D H10A 0.9500 . ?
N11D C12D 1.317(9) . ?
N11D C13D 1.458(8) . ?
C12D H12C 0.9500 . ?
C13D C14D 1.526(10) . ?
C13D H13C 0.9900 . ?
C13D H13D 0.9900 . ?
C14D C15D 1.524(10) . ?
C14D H14A 0.9900 . ?
C14D H14B 0.9900 . ?
C15D C16D 1.526(10) . ?
C15D H15C 0.9900 . ?
C15D H15D 0.9900 . ?
C16D H16C 0.9800 . ?
C16D H16D 0.9800 . ?
C16D H16E 0.9800 . ?
C17D N18D 1.457(8) . ?
C17D H17G 0.9900 . ?
C17D H17H 0.9900 . ?
N18D C22D 1.318(9) . ?
N18D C19D 1.380(9) . ?
C19D C20D 1.343(10) . ?
C19D H19A 0.9500 . ?
C20D N21D 1.382(9) . ?
C20D H20A 0.9500 . ?
N21D C22D 1.311(9) . ?
N21D C23D 1.459(8) . ?
C22D H22C 0.9500 . ?
C23D C24D 1.520(10) . ?
C23D H23C 0.9900 . ?
C23D H23D 0.9900 . ?
C24D C25D 1.520(10) . ?
C24D H24C 0.9900 . ?
C24D H24D 0.9900 . ?
C25D C26D 1.528(10) . ?
C25D H25C 0.9900 . ?
C25D H25D 0.9900 . ?
C26D H26C 0.9800 . ?
C26D H26D 0.9800 . ?
C26D H26E 0.9800 . ?
O09W O09W 1.56(10) 2_665 ?

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 C11 C12 119.4(10) . . ?
O1 C11 C16 119.7(12) . . ?
C12 C11 C16 121.0(13) . . ?
C11 C12 C13 118.0(11) . . ?
C11 C12 C1 123.2(11) . . ?
C13 C12 C1 118.8(12) . . ?
C14 C13 C12 122.1(13) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C14 C13 118.4(14) . . ?
C15 C14 S1 120.0(10) . . ?
C13 C14 S1 121.4(11) . . ?
C14 C15 C16 122.6(12) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C11 C16 C15 117.8(12) . . ?
C11 C16 C4 121.1(13) . . ?
C15 C16 C4 121.0(12) . . ?
O12 S1 O11 114.2(6) . . ?
O16 S1 O14 113.7(7) . . ?
O16 S1 O15 112.9(7) . . ?
O14 S1 O15 112.8(7) . . ?
O12 S1 O13 113.4(6) . . ?
O11 S1 O13 112.5(6) . . ?
O12 S1 C14 105.8(6) . . ?
O16 S1 C14 106.0(6) . . ?
O11 S1 C14 105.5(6) . . ?
O14 S1 C14 105.4(6) . . ?
O15 S1 C14 105.1(6) . . ?
O13 S1 C14 104.3(6) . . ?
C12 C1 C26 112.7(8) . . ?
C12 C1 H1A 109.1 . . ?
C26 C1 H1A 109.1 . . ?
C12 C1 H1B 109.1 . . ?
C26 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
O2 C21 C26 119.5(11) . . ?
O2 C21 C22 119.5(11) . . ?
C26 C21 C22 121.0(11) . . ?
C23 C22 C21 118.4(12) . . ?
C23 C22 C2 118.9(12) . . ?
C21 C22 C2 122.6(12) . . ?
C22 C23 C24 122.9(12) . . ?
C22 C23 H23 118.5 . . ?
C24 C23 H23 118.5 . . ?
C25 C24 C23 117.3(12) . . ?
C25 C24 S2 120.4(11) . . ?
C23 C24 S2 122.2(11) . . ?
C26 C25 C24 121.1(13) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C21 C26 C25 119.3(11) . . ?
C21 C26 C1 120.6(12) . . ?
C25 C26 C1 120.1(12) . . ?
O25 S2 O24 113.3(7) . . ?
O25 S2 O26 113.2(7) . . ?
O24 S2 O26 112.8(7) . . ?
O23 S2 O21 113.8(7) . . ?
O23 S2 O22 113.3(7) . . ?
O21 S2 O22 112.0(7) . . ?
O23 S2 C24 106.0(6) . . ?
O25 S2 C24 106.0(6) . . ?
O24 S2 C24 105.2(6) . . ?
O26 S2 C24 105.4(6) . . ?
O21 S2 C24 105.6(6) . . ?
O22 S2 C24 105.2(6) . . ?
C36 C2 C22 114.8(9) . . ?
C36 C2 H2A 108.6 . . ?
C22 C2 H2A 108.6 . . ?
C36 C2 H2B 108.6 . . ?
C22 C2 H2B 108.6 . . ?
H2A C2 H2B 107.5 . . ?
O3 C31 C36 121.7(13) . . ?
O3 C31 C32 118.6(14) . . ?
C36 C31 C32 119.7(14) . . ?
C33 C32 C31 120.2(16) . . ?
C33 C32 C3 119.8(14) . . ?
C31 C32 C3 119.9(13) . . ?
C32 C33 C34 119.7(15) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 121.0(13) . . ?
C35 C34 S3 119.0(11) . . ?
C33 C34 S3 119.6(11) . . ?
C34 C35 C36 121.5(15) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C31 C36 C35 117.8(14) . . ?
C31 C36 C2 122.3(13) . . ?
C35 C36 C2 119.9(15) . . ?
O36 S3 O35 115.1(6) . . ?
O33 S3 O31 113.7(6) . . ?
O33 S3 O32 113.9(6) . . ?
O31 S3 O32 110.9(6) . . ?
O36 S3 O34 113.3(6) . . ?
O35 S3 O34 109.6(6) . . ?
O36 S3 C34 108.3(6) . . ?
O33 S3 C34 107.2(6) . . ?
O35 S3 C34 105.5(6) . . ?
O31 S3 C34 105.5(6) . . ?
O32 S3 C34 104.7(6) . . ?
O34 S3 C34 104.0(6) . . ?
C32 C3 C46 112.1(11) . . ?
C32 C3 H3A 109.2 . . ?
C46 C3 H3A 109.2 . . ?
C32 C3 H3B 109.2 . . ?
C46 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C42 C41 C46 122.4(12) . . ?
C42 C41 O4 120.6(13) . . ?
C46 C41 O4 117.0(14) . . ?
C43 C42 C41 118.7(12) . . ?
C43 C42 C4 121.7(13) . . ?
C41 C42 C4 119.6(12) . . ?
C44 C43 C42 120.3(12) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 121.3(11) . . ?
C43 C44 S4 121.0(9) . . ?
C45 C44 S4 117.4(8) . . ?
C44 C45 C46 121.2(12) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C41 C46 C45 115.8(13) . . ?
C41 C46 C3 123.1(13) . . ?
C45 C46 C3 121.0(13) . . ?
O42 S4 O43 113.7(5) . . ?
O46 S4 O45 113.9(5) . . ?
O42 S4 O41 112.6(5) . . ?
O43 S4 O41 112.4(5) . . ?
O46 S4 O44 112.7(5) . . ?
O45 S4 O44 111.4(5) . . ?
O46 S4 C44 106.8(5) . . ?
O42 S4 C44 106.1(5) . . ?
O43 S4 C44 105.8(5) . . ?
O45 S4 C44 105.9(5) . . ?
O41 S4 C44 105.5(5) . . ?
O44 S4 C44 105.3(5) . . ?
C16 C4 C42 111.7(9) . . ?
C16 C4 H4A 109.3 . . ?
C42 C4 H4A 109.3 . . ?
C16 C4 H4B 109.3 . . ?
C42 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C21A P1A C31A 109.4(5) . . ?
C21A P1A C41A 111.0(5) . . ?
C31A P1A C41A 108.7(4) . . ?
C21A P1A C11A 110.1(4) . . ?
C31A P1A C11A 108.4(5) . . ?
C41A P1A C11A 109.2(4) . . ?
C14A O1A C17A 117.9(8) . . ?
C16A C11A C12A 118.6(9) . . ?
C16A C11A P1A 123.1(8) . . ?
C12A C11A P1A 118.3(7) . . ?
C11A C12A C13A 120.3(9) . . ?
C11A C12A H12A 119.9 . . ?
C13A C12A H12A 119.9 . . ?
C14A C13A C12A 119.2(9) . . ?
C14A C13A H13A 120.4 . . ?
C12A C13A H13A 120.4 . . ?
O1A C14A C15A 126.3(9) . . ?
O1A C14A C13A 114.2(9) . . ?
C15A C14A C13A 119.5(9) . . ?
C16A C15A C14A 121.3(9) . . ?
C16A C15A H15A 119.4 . . ?
C14A C15A H15A 119.4 . . ?
C15A C16A C11A 121.2(9) . . ?
C15A C16A H16A 119.4 . . ?
C11A C16A H16A 119.4 . . ?
O1A C17A H17A 109.5 . . ?
O1A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
O1A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C26A C21A C22A 118.3(11) . . ?
C26A C21A P1A 121.2(10) . . ?
C22A C21A P1A 120.5(9) . . ?
C23A C22A C21A 119.2(13) . . ?
C23A C22A H22A 120.4 . . ?
C21A C22A H22A 120.4 . . ?
C24A C23A C22A 120.2(15) . . ?
C24A C23A H23A 119.9 . . ?
C22A C23A H23A 119.9 . . ?
C23A C24A C25A 121.4(15) . . ?
C23A C24A H24A 119.3 . . ?
C25A C24A H24A 119.3 . . ?
C26A C25A C24A 118.9(14) . . ?
C26A C25A H25A 120.5 . . ?
C24A C25A H25A 120.5 . . ?
C25A C26A C21A 121.9(12) . . ?
C25A C26A H26A 119.1 . . ?
C21A C26A H26A 119.1 . . ?
C32A C31A C36A 118.9(9) . . ?
C32A C31A P1A 120.1(7) . . ?
C36A C31A P1A 120.9(8) . . ?
C31A C32A C33A 121.4(9) . . ?
C31A C32A H32A 119.3 . . ?
C33A C32A H32A 119.3 . . ?
C34A C33A C32A 116.5(10) . . ?
C34A C33A H33A 121.7 . . ?
C32A C33A H33A 121.7 . . ?
C33A C34A C35A 120.8(10) . . ?
C33A C34A H34A 119.6 . . ?
C35A C34A H34A 119.6 . . ?
C36A C35A C34A 121.6(10) . . ?
C36A C35A H35A 119.2 . . ?
C34A C35A H35A 119.2 . . ?
C35A C36A C31A 120.6(10) . . ?
C35A C36A H36A 119.7 . . ?
C31A C36A H36A 119.7 . . ?
C42A C41A C46A 119.6(9) . . ?
C42A C41A P1A 119.9(8) . . ?
C46A C41A P1A 120.2(8) . . ?
C41A C42A C43A 121.9(10) . . ?
C41A C42A H42A 119.1 . . ?
C43A C42A H42A 119.1 . . ?
C44A C43A C42A 118.4(10) . . ?
C44A C43A H43A 120.8 . . ?
C42A C43A H43A 120.8 . . ?
C45A C44A C43A 122.2(10) . . ?
C45A C44A H44A 118.9 . . ?
C43A C44A H44A 118.9 . . ?
C44A C45A C46A 117.7(11) . . ?
C44A C45A H45A 121.1 . . ?
C46A C45A H45A 121.1 . . ?
C41A C46A C45A 120.0(10) . . ?
C41A C46A H46A 120.0 . . ?
C45A C46A H46A 120.0 . . ?
C31B P1B C11B 107.0(5) . . ?
C31B P1B C41B 112.2(6) . . ?
C11B P1B C41B 109.9(5) . . ?
C31B P1B C21B 108.8(5) . . ?
C11B P1B C21B 112.1(5) . . ?
C41B P1B C21B 106.9(5) . . ?
C14B O2B C17B 122.2(11) . . ?
C16B C11B C12B 117.7(10) . . ?
C16B C11B P1B 123.2(8) . . ?
C12B C11B P1B 119.1(10) . . ?
C11B C12B C13B 120.2(11) . . ?
C11B C12B H12B 119.9 . . ?
C13B C12B H12B 119.9 . . ?
C14B C13B C12B 119.1(10) . . ?
C14B C13B H13B 120.4 . . ?
C12B C13B H13B 120.4 . . ?
C13B C14B C15B 122.6(11) . . ?
C13B C14B O2B 116.7(12) . . ?
C15B C14B O2B 120.7(13) . . ?
C14B C15B C16B 118.4(11) . . ?
C14B C15B H15B 120.8 . . ?
C16B C15B H15B 120.8 . . ?
C11B C16B C15B 121.9(10) . . ?
C11B C16B H16B 119.1 . . ?
C15B C16B H16B 119.1 . . ?
O2B C17B H17D 109.5 . . ?
O2B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
O2B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C22B C21B C26B 120.0(9) . . ?
C22B C21B P1B 118.9(8) . . ?
C26B C21B P1B 121.1(8) . . ?
C21B C22B C23B 120.4(10) . . ?
C21B C22B H22B 119.8 . . ?
C23B C22B H22B 119.8 . . ?
C24B C23B C22B 117.1(12) . . ?
C24B C23B H23B 121.5 . . ?
C22B C23B H23B 121.5 . . ?
C25B C24B C23B 121.6(11) . . ?
C25B C24B H24B 119.2 . . ?
C23B C24B H24B 119.2 . . ?
C24B C25B C26B 119.0(10) . . ?
C24B C25B H25B 120.5 . . ?
C26B C25B H25B 120.5 . . ?
C21B C26B C25B 121.3(10) . . ?
C21B C26B H26B 119.4 . . ?
C25B C26B H26B 119.4 . . ?
C36B C31B C32B 116.7(11) . . ?
C36B C31B P1B 121.4(11) . . ?
C32B C31B P1B 121.8(11) . . ?
C33B C32B C31B 120.9(12) . . ?
C33B C32B H32B 119.5 . . ?
C31B C32B H32B 119.5 . . ?
C32B C33B C34B 122.1(14) . . ?
C32B C33B H33B 118.9 . . ?
C34B C33B H33B 118.9 . . ?
C35B C34B C33B 118.6(17) . . ?
C35B C34B H34B 120.7 . . ?
C33B C34B H34B 120.7 . . ?
C34B C35B C36B 119.7(17) . . ?
C34B C35B H35B 120.1 . . ?
C36B C35B H35B 120.1 . . ?
C31B C36B C35B 121.9(14) . . ?
C31B C36B H36B 119.1 . . ?
C35B C36B H36B 119.1 . . ?
C42B C41B C46B 118.0(11) . . ?
C42B C41B P1B 123.2(9) . . ?
C46B C41B P1B 118.7(10) . . ?
C41B C42B C43B 121.7(11) . . ?
C41B C42B H42B 119.1 . . ?
C43B C42B H42B 119.1 . . ?
C44B C43B C42B 120.5(12) . . ?
C44B C43B H43B 119.8 . . ?
C42B C43B H43B 119.8 . . ?
C43B C44B C45B 120.1(15) . . ?
C43B C44B H44B 120.0 . . ?
C45B C44B H44B 120.0 . . ?
C44B C45B C46B 119.1(15) . . ?
C44B C45B H45B 120.5 . . ?
C46B C45B H45B 120.5 . . ?
C41B C46B C45B 120.0(14) . . ?
C41B C46B H46B 120.0 . . ?
C45B C46B H46B 120.0 . . ?
C02D C01D C06D 120.8(16) . . ?
C02D C01D C07D 119.5(10) . . ?
C06D C01D C07D 119.7(10) . . ?
C03D C02D C01D 119.8(18) . . ?
C03D C02D H02A 120.1 . . ?
C01D C02D H02A 120.1 . . ?
C02D C03D C04D 121.6(14) . . ?
C02D C03D H03A 119.2 . . ?
C04D C03D H03A 119.2 . . ?
C03D C04D C05D 117.4(12) . . ?
C03D C04D C17D 121.0(9) . . ?
C05D C04D C17D 121.5(8) . . ?
C04D C05D C06D 122.3(14) . . ?
C04D C05D H05A 118.9 . . ?
C06D C05D H05A 118.9 . . ?
C01D C06D C05D 118.1(18) . . ?
C01D C06D H06A 121.0 . . ?
C05D C06D H06A 121.0 . . ?
N08D C07D C01D 117.6(8) . . ?
N08D C07D H07A 107.9 . . ?
C01D C07D H07A 107.9 . . ?
N08D C07D H07B 107.9 . . ?
C01D C07D H07B 107.9 . . ?
H07A C07D H07B 107.2 . . ?
C12D N08D C09D 108.2(9) . . ?
C12D N08D C07D 129.0(9) . . ?
C09D N08D C07D 122.8(8) . . ?
C10D C09D N08D 107.1(10) . . ?
C10D C09D H09A 126.4 . . ?
N08D C09D H09A 126.4 . . ?
C09D C10D N11D 106.9(10) . . ?
C09D C10D H10A 126.6 . . ?
N11D C10D H10A 126.6 . . ?
C12D N11D C10D 108.2(9) . . ?
C12D N11D C13D 128.9(9) . . ?
C10D N11D C13D 122.9(8) . . ?
N08D C12D N11D 109.6(10) . . ?
N08D C12D H12C 125.2 . . ?
N11D C12D H12C 125.2 . . ?
N11D C13D C14D 119.7(11) . . ?
N11D C13D H13C 107.4 . . ?
C14D C13D H13C 107.4 . . ?
N11D C13D H13D 107.4 . . ?
C14D C13D H13D 107.4 . . ?
H13C C13D H13D 106.9 . . ?
C15D C14D C13D 113.3(11) . . ?
C15D C14D H14A 108.9 . . ?
C13D C14D H14A 108.9 . . ?
C15D C14D H14B 108.9 . . ?
C13D C14D H14B 108.9 . . ?
H14A C14D H14B 107.7 . . ?
C14D C15D C16D 113.3(11) . . ?
C14D C15D H15C 108.9 . . ?
C16D C15D H15C 108.9 . . ?
C14D C15D H15D 108.9 . . ?
C16D C15D H15D 108.9 . . ?
H15C C15D H15D 107.7 . . ?
C15D C16D H16C 109.5 . . ?
C15D C16D H16D 109.5 . . ?
H16C C16D H16D 109.5 . . ?
C15D C16D H16E 109.5 . . ?
H16C C16D H16E 109.5 . . ?
H16D C16D H16E 109.5 . . ?
N18D C17D C04D 120.4(9) . . ?
N18D C17D H17G 107.2 . . ?
C04D C17D H17G 107.2 . . ?
N18D C17D H17H 107.2 . . ?
C04D C17D H17H 107.2 . . ?
H17G C17D H17H 106.9 . . ?
C22D N18D C19D 107.7(9) . . ?
C22D N18D C17D 128.4(8) . . ?
C19D N18D C17D 123.8(8) . . ?
C20D C19D N18D 107.2(10) . . ?
C20D C19D H19A 126.4 . . ?
N18D C19D H19A 126.4 . . ?
C19D C20D N21D 107.0(10) . . ?
C19D C20D H20A 126.5 . . ?
N21D C20D H20A 126.5 . . ?
C22D N21D C20D 107.9(9) . . ?
C22D N21D C23D 128.7(9) . . ?
C20D N21D C23D 123.4(8) . . ?
N21D C22D N18D 110.2(10) . . ?
N21D C22D H22C 124.9 . . ?
N18D C22D H22C 124.9 . . ?
N21D C23D C24D 120.0(11) . . ?
N21D C23D H23C 107.3 . . ?
C24D C23D H23C 107.3 . . ?
N21D C23D H23D 107.3 . . ?
C24D C23D H23D 107.3 . . ?
H23C C23D H23D 106.9 . . ?
C25D C24D C23D 114.1(11) . . ?
C25D C24D H24C 108.7 . . ?
C23D C24D H24C 108.7 . . ?
C25D C24D H24D 108.7 . . ?
C23D C24D H24D 108.7 . . ?
H24C C24D H24D 107.6 . . ?
C24D C25D C26D 112.9(11) . . ?
C24D C25D H25C 109.0 . . ?
C26D C25D H25C 109.0 . . ?
C24D C25D H25D 109.0 . . ?
C26D C25D H25D 109.0 . . ?
H25C C25D H25D 107.8 . . ?
C25D C26D H26C 109.5 . . ?
C25D C26D H26D 109.5 . . ?
H26C C26D H26D 109.5 . . ?
C25D C26D H26E 109.5 . . ?
H26C C26D H26E 109.5 . . ?
H26D C26D H26E 109.5 . . ?

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 126 13 ' '
2 0.500 0.000 0.000 265 27 ' '
3 0.363 0.269 0.856 11 1 ' '
4 0.637 0.730 0.144 11 1 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_refine_diff_density_max         1.017
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_aac4_g3
_database_code_depnum_ccdc_archive 'CCDC 1426677'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;

#==============================================================================


# 6. CRYSTALLOGRAPHY

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H22 O P, I'
_chemical_formula_sum            'C25 H22 I O P'
_chemical_formula_weight         496.29

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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                   10.4708(6)
_cell_length_b                   10.5478(6)
_cell_length_c                   11.0342(6)
_cell_angle_alpha                72.783(5)
_cell_angle_beta                 75.786(5)
_cell_angle_gamma                70.243(5)
_cell_volume                     1081.09(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3602
_cell_measurement_theta_min      4.231
_cell_measurement_theta_max      67.037
_diffrn_orient_matrix_UB_11      -0.1439616
_diffrn_orient_matrix_UB_12      -0.0027210
_diffrn_orient_matrix_UB_13      0.0762718
_diffrn_orient_matrix_UB_21      -0.0081435
_diffrn_orient_matrix_UB_22      -0.0950361
_diffrn_orient_matrix_UB_23      -0.0786100
_diffrn_orient_matrix_UB_31      0.0656166
_diffrn_orient_matrix_UB_32      -0.1281931
_diffrn_orient_matrix_UB_33      0.0997110

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    12.422
_shelx_estimated_absorpt_T_min   0.317
_shelx_estimated_absorpt_T_max   0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6863
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            8211
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.251
_diffrn_reflns_theta_max         67.155
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             3805
_reflns_number_gt                3428
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 The higest residual peak of 1.26 e/A3
 located at  0.2511  0.1373  0.1397  [  0.90 A from I1 ]
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²+1.6000P] 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         3805
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
I1 I 0.24120(3) 1.05205(3) 0.17886(3) 0.03645(12) Uani 1 1 d . . . . .
P1 P 0.27098(10) 0.53613(10) 0.33731(10) 0.0236(2) Uani 1 1 d . . . . .
O1 O 0.3492(4) -0.0189(4) 0.6979(3) 0.0431(8) Uani 1 1 d . . . . .
C11 C 0.2890(4) 0.3688(4) 0.4458(4) 0.0258(8) Uani 1 1 d . . . . .
C12 C 0.2893(4) 0.3563(4) 0.5740(4) 0.0289(9) Uani 1 1 d . . . . .
H12 H 0.2748 0.4368 0.6035 0.035 Uiso 1 1 calc R U . . .
C13 C 0.3104(5) 0.2277(5) 0.6606(4) 0.0325(9) Uani 1 1 d . . . . .
H13 H 0.3112 0.2206 0.7483 0.039 Uiso 1 1 calc R U . . .
C14 C 0.3303(4) 0.1096(4) 0.6183(4) 0.0310(9) Uani 1 1 d . . . . .
C15 C 0.3277(5) 0.1216(5) 0.4886(5) 0.0338(10) Uani 1 1 d . . . . .
H15 H 0.3393 0.0414 0.4597 0.041 Uiso 1 1 calc R U . . .
C16 C 0.3082(4) 0.2493(4) 0.4031(4) 0.0291(9) Uani 1 1 d . . . . .
H16 H 0.3077 0.2566 0.3153 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3540(6) -0.0347(6) 0.8349(6) 0.0503(13) Uani 1 1 d . . . . .
H17A H 0.3701 -0.1326 0.8798 0.075 Uiso 1 1 calc R U . . .
H17B H 0.2663 0.0197 0.8748 0.075 Uiso 1 1 calc R U . . .
H17C H 0.4287 -0.0016 0.8407 0.075 Uiso 1 1 calc R U . . .
C21 C 0.4289(4) 0.5424(4) 0.2283(4) 0.0264(8) Uani 1 1 d . . . . .
C22 C 0.5226(4) 0.4219(5) 0.1960(4) 0.0327(9) Uani 1 1 d . . . . .
H22 H 0.5074 0.3341 0.2365 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6379(5) 0.4323(6) 0.1041(5) 0.0405(11) Uani 1 1 d . . . . .
H23 H 0.7018 0.3508 0.0817 0.049 Uiso 1 1 calc R U . . .
C24 C 0.6610(5) 0.5580(6) 0.0452(5) 0.0390(11) Uani 1 1 d . . . . .
H24 H 0.7406 0.5629 -0.0177 0.047 Uiso 1 1 calc R U . . .
C25 C 0.5694(5) 0.6781(5) 0.0762(4) 0.0358(10) Uani 1 1 d . . . . .
H25 H 0.5859 0.7652 0.0346 0.043 Uiso 1 1 calc R U . . .
C26 C 0.4530(4) 0.6707(5) 0.1688(4) 0.0324(9) Uani 1 1 d . . . . .
H26 H 0.3903 0.7526 0.1913 0.039 Uiso 1 1 calc R U . . .
C31 C 0.1378(4) 0.5808(4) 0.2431(4) 0.0258(8) Uani 1 1 d . . . . .
C32 C 0.1110(4) 0.7111(5) 0.1585(4) 0.0300(9) Uani 1 1 d . . . . .
H32 H 0.1583 0.7746 0.1561 0.036 Uiso 1 1 calc R U . . .
C33 C 0.0147(4) 0.7476(5) 0.0779(4) 0.0346(10) Uani 1 1 d . . . . .
H33 H -0.0031 0.8357 0.0193 0.042 Uiso 1 1 calc R U . . .
C34 C -0.0550(4) 0.6554(5) 0.0832(5) 0.0354(10) Uani 1 1 d . . . . .
H34 H -0.1201 0.6806 0.0274 0.043 Uiso 1 1 calc R U . . .
C35 C -0.0316(4) 0.5275(5) 0.1681(5) 0.0338(10) Uani 1 1 d . . . . .
H35 H -0.0812 0.4657 0.1713 0.041 Uiso 1 1 calc R U . . .
C36 C 0.0649(4) 0.4890(5) 0.2493(4) 0.0301(9) Uani 1 1 d . . . . .
H36 H 0.0811 0.4012 0.3083 0.036 Uiso 1 1 calc R U . . .
C41 C 0.2276(4) 0.6622(4) 0.4298(4) 0.0253(8) Uani 1 1 d . . . . .
C42 C 0.0889(4) 0.7281(4) 0.4700(4) 0.0307(9) Uani 1 1 d . . . . .
H42 H 0.0186 0.7129 0.4404 0.037 Uiso 1 1 calc R U . . .
C43 C 0.0546(5) 0.8151(5) 0.5526(5) 0.0370(10) Uani 1 1 d . . . . .
H43 H -0.0393 0.8588 0.5806 0.044 Uiso 1 1 calc R U . . .
C44 C 0.1560(5) 0.8381(5) 0.5941(5) 0.0387(11) Uani 1 1 d . . . . .
H44 H 0.1316 0.8983 0.6506 0.046 Uiso 1 1 calc R U . . .
C45 C 0.2939(5) 0.7751(5) 0.5551(4) 0.0362(10) Uani 1 1 d . . . . .
H45 H 0.3631 0.7921 0.5847 0.043 Uiso 1 1 calc R U . . .
C46 C 0.3303(5) 0.6867(4) 0.4721(4) 0.0316(9) Uani 1 1 d . . . . .
H46 H 0.4244 0.6435 0.4446 0.038 Uiso 1 1 calc R U . . .


_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
P1 C41 1.783(4) . ?
P1 C11 1.794(4) . ?
P1 C31 1.796(4) . ?
P1 C21 1.799(4) . ?
O1 C14 1.359(6) . ?
O1 C17 1.483(7) . ?
C11 C12 1.382(6) . ?
C11 C16 1.409(6) . ?
C12 C13 1.391(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.405(7) . ?
C15 C16 1.379(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 C26 1.396(6) . ?
C21 C22 1.400(6) . ?
C22 C23 1.385(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.367(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.394(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.395(6) . ?
C31 C36 1.400(6) . ?
C32 C33 1.390(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.378(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.396(6) . ?
C41 C42 1.404(6) . ?
C42 C43 1.384(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.370(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.388(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.395(7) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?

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
C41 P1 C11 108.27(19) . . ?
C41 P1 C31 108.19(19) . . ?
C11 P1 C31 112.36(19) . . ?
C41 P1 C21 109.33(19) . . ?
C11 P1 C21 110.77(19) . . ?
C31 P1 C21 107.86(19) . . ?
C14 O1 C17 118.5(4) . . ?
C12 C11 C16 119.2(4) . . ?
C12 C11 P1 118.9(3) . . ?
C16 C11 P1 121.9(3) . . ?
C11 C12 C13 121.1(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 119.7(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
O1 C14 C13 122.9(4) . . ?
O1 C14 C15 117.4(4) . . ?
C13 C14 C15 119.6(4) . . ?
C16 C15 C14 120.2(4) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 120.1(4) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 C22 119.9(4) . . ?
C26 C21 P1 119.1(3) . . ?
C22 C21 P1 120.8(3) . . ?
C23 C22 C21 119.1(4) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 C22 121.0(5) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 120.6(4) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C26 119.7(4) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C25 C26 C21 119.7(4) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
C32 C31 C36 120.0(4) . . ?
C32 C31 P1 117.4(3) . . ?
C36 C31 P1 122.5(3) . . ?
C33 C32 C31 119.7(4) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C35 C34 C33 121.1(4) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 C36 119.9(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 119.4(4) . . ?
C35 C36 H36 120.3 . . ?
C31 C36 H36 120.3 . . ?
C46 C41 C42 119.6(4) . . ?
C46 C41 P1 120.3(3) . . ?
C42 C41 P1 119.9(3) . . ?
C43 C42 C41 120.1(4) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C44 C43 C42 119.9(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 121.2(4) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C44 C45 C46 119.6(4) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C41 119.6(4) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C16 H16 I1 0.95 3.30 3.979(4) 130.5 1_545
C17 H17C I1 0.98 3.28 4.147(6) 149.0 2_666
C26 H26 I1 0.95 2.99 3.901(5) 161.0 .
C44 H44 O1 0.95 2.90 3.449(6) 117.8 1_565
C45 H45 O1 0.95 2.60 3.296(6) 130.7 1_565

_refine_diff_density_max         1.260
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.122

_shelxl_version_number           2014-3

