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

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

data_VMOP-11_sq
_database_code_depnum_ccdc_archive 'CCDC 1479717'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_audit_creation_date             2016-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H132 O100 S4 V24'
_chemical_formula_sum            'C126 H250 N10 O102 S4 V24'
_chemical_formula_weight         4888.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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'
N N 0.0061 0.0033 '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      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'x, z, y'
'z, y, x'
'-x, -z, y'
'z, -y, -x'
'-x, z, -y'
'-z, -y, x'
'x, -z, -y'
'-z, y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'z+1/2, y+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'-z+1/2, y+1/2, -x+1/2'

_cell_length_a                   21.927(5)
_cell_length_b                   21.927(5)
_cell_length_c                   21.927(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10542(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.391
_cell_measurement_theta_min      2.275
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.788
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30838
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.313
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1522
_reflns_number_total             1747
_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       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1747
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0408P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0748
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.96(5) 0.04(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 S1, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H6A(0.5) H6B(0.5) H6C(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5)
5.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
# SQUEEZE RESULTS (Version = 100616)
# 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 0.000 0.000 853 277 ' '
2 -0.134 -0.115 0.419 2068 412 ' '
3 0.500 0.500 0.500 853 277 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V1 V -0.32665(4) -0.12015(4) -0.22836(4) 0.0410(2) Uani 1 1 d . . . . .
S1 S -0.18938(7) -0.18938(7) -0.18938(7) 0.0324(7) Uani 1 6 d S TU P . .
O3 O -0.25508(19) -0.17736(13) -0.17736(13) 0.0363(10) Uani 1 2 d S T P . .
O7 O -0.1515(2) -0.1515(2) -0.1515(2) 0.051(2) Uani 1 6 d S TU P . .
O2 O -0.38200(18) -0.08491(18) -0.25805(18) 0.0659(11) Uani 1 1 d . . . . .
O6 O -0.25463(15) -0.07305(19) -0.25463(15) 0.0400(10) Uani 1 2 d S T P . .
O1 O -0.37172(19) -0.18988(15) -0.18988(15) 0.0434(11) Uani 1 2 d S T P . .
O4 O -0.29824(15) -0.1691(2) -0.29824(15) 0.0449(12) Uani 1 2 d S T P . .
O5 O -0.32807(17) -0.07456(15) -0.14772(16) 0.0556(10) Uani 1 1 d . . . . .
C2 C -0.3310(3) -0.0453(2) -0.0453(2) 0.0476(17) Uani 1 2 d S T P . .
C3 C -0.3309(3) 0.0168(2) -0.0609(2) 0.0613(15) Uani 1 1 d . . . . .
H3 H -0.3308 0.0281 -0.1017 0.074 Uiso 1 1 calc R . . . .
C1 C -0.3296(4) -0.0938(2) -0.0938(2) 0.0491(19) Uani 1 2 d S T P . .
C5 C -0.3350(3) -0.2050(6) -0.3350(3) 0.106(4) Uani 1 2 d S T P . .
H5A H -0.3658 -0.2241 -0.3105 0.160 Uiso 0.5 1 calc R . . . .
H5B H -0.3540 -0.1799 -0.3654 0.160 Uiso 0.5 1 calc R . . . .
H5C H -0.3106 -0.2357 -0.3544 0.160 Uiso 0.5 1 calc R . . . .
C6 C -0.2222(3) -0.0275(4) -0.2222(3) 0.085(3) Uani 1 2 d S T P . .
H6A H -0.1891 -0.0128 -0.2469 0.128 Uiso 0.5 1 calc R . . . .
H6B H -0.2492 0.0056 -0.2127 0.128 Uiso 0.5 1 calc R . . . .
H6C H -0.2063 -0.0445 -0.1851 0.128 Uiso 0.5 1 calc R . . . .
C4 C -0.4362(4) -0.1841(4) -0.1841(4) 0.092(3) Uani 1 2 d S T P . .
H4A H -0.4524 -0.1652 -0.2201 0.137 Uiso 0.5 1 calc R . . . .
H4B H -0.4540 -0.2238 -0.1792 0.137 Uiso 0.5 1 calc R . . . .
H4C H -0.4456 -0.1595 -0.1492 0.137 Uiso 0.5 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 3.0480(18) 18 ?
V1 O3 2.299(3) . ?
V1 O2 1.579(4) . ?
V1 O6 1.973(3) . ?
V1 O1 2.006(2) . ?
V1 O4 1.971(3) . ?
V1 O5 2.031(4) . ?
S1 O3 1.488(4) 6 ?
S1 O3 1.488(4) 5 ?
S1 O3 1.488(4) . ?
S1 O7 1.438(9) . ?
O3 V1 2.299(3) 17 ?
O6 V1 1.973(3) 18 ?
O6 C6 1.417(9) . ?
O1 V1 2.006(2) 17 ?
O1 C4 1.425(9) . ?
O4 V1 1.971(3) 18 ?
O4 C5 1.385(10) . ?
O5 C1 1.256(4) . ?
C2 C3 1.403(7) . ?
C2 C3 1.403(7) 17 ?
C2 C1 1.503(9) . ?
C3 C3 1.367(10) 23 ?
C3 H3 0.9300 . ?
C1 O5 1.256(4) 17 ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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
O3 V1 V1 82.03(8) . 18 ?
O2 V1 V1 104.59(15) . 18 ?
O2 V1 O3 172.74(18) . . ?
O2 V1 O6 103.80(19) . . ?
O2 V1 O1 99.66(19) . . ?
O2 V1 O4 100.9(2) . . ?
O2 V1 O5 96.10(18) . . ?
O6 V1 V1 39.43(10) . 18 ?
O6 V1 O3 83.18(15) . . ?
O6 V1 O1 156.33(16) . . ?
O6 V1 O5 90.50(16) . . ?
O1 V1 V1 130.21(13) . 18 ?
O1 V1 O3 73.49(13) . . ?
O1 V1 O5 90.08(16) . . ?
O4 V1 V1 39.36(10) . 18 ?
O4 V1 O3 82.28(17) . . ?
O4 V1 O6 78.75(14) . . ?
O4 V1 O1 93.91(17) . . ?
O4 V1 O5 161.64(17) . . ?
O5 V1 V1 128.78(11) . 18 ?
O5 V1 O3 81.69(15) . . ?
O3 S1 O3 108.15(18) 6 5 ?
O3 S1 O3 108.15(18) . 5 ?
O3 S1 O3 108.15(18) . 6 ?
O7 S1 O3 110.77(18) . 6 ?
O7 S1 O3 110.77(18) . 5 ?
O7 S1 O3 110.77(17) . . ?
V1 O3 V1 93.72(15) . 17 ?
S1 O3 V1 132.16(9) . 17 ?
S1 O3 V1 132.16(9) . . ?
V1 O6 V1 101.1(2) . 18 ?
C6 O6 V1 128.62(13) . 18 ?
C6 O6 V1 128.61(13) . . ?
V1 O1 V1 113.5(2) 17 . ?
C4 O1 V1 117.3(2) . . ?
C4 O1 V1 117.3(2) . 17 ?
V1 O4 V1 101.3(2) 18 . ?
C5 O4 V1 125.3(2) . 18 ?
C5 O4 V1 125.3(2) . . ?
C1 O5 V1 131.0(4) . . ?
C3 C2 C3 118.2(6) 17 . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 C1 120.9(3) 17 . ?
C2 C3 H3 119.6 . . ?
C3 C3 C2 120.9(3) 23 . ?
C3 C3 H3 119.6 23 . ?
O5 C1 O5 129.1(7) 17 . ?
O5 C1 C2 115.5(3) 17 . ?
O5 C1 C2 115.5(3) . . ?
O4 C5 H5A 109.5 . . ?
O4 C5 H5B 109.5 . . ?
O4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C4 H4A 109.5 . . ?
O1 C4 H4B 109.5 . . ?
O1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.96(5)
2 0.04(5)

####################################################################### 
# 
# 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_VMOP-12_sq
_database_code_depnum_ccdc_archive 'CCDC 1479718'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_audit_creation_date             2016-06-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H108 N6 O100 S4 V24'
_chemical_formula_sum            'C123.50 H250.50 N15.50 O101.50 S4 V24'
_chemical_formula_weight         4927.68
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
V V 0.3005 0.5294 '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'
N N 0.0061 0.0033 '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'

_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      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'x, z, y'
'z, y, x'
'-x, -z, y'
'z, -y, -x'
'-x, z, -y'
'-z, -y, x'
'x, -z, -y'
'-z, y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'z+1/2, y+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'-z+1/2, y+1/2, -x+1/2'

_cell_length_a                   21.841(5)
_cell_length_b                   21.841(5)
_cell_length_c                   21.841(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     10419(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.477
_cell_measurement_theta_min      2.284
_shelx_estimated_absorpt_T_max   0.828
_shelx_estimated_absorpt_T_min   0.785
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         1.318
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1521
_reflns_number_total             1725
_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       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1725
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.059
_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)+(0.0541P)²+3.5331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0914
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.53(6) 0.47(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O6 \\sim C5: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H6B(0.5) H6A(0.5) H6C(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5) N1(0.25)
5.a Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6B,H6A,H6C), C5(H5A,H5B,H5C)
;
# SQUEEZE RESULTS (Version = 100616)
# 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 0.000 0.000 872 274 ' '
2 -0.135 -0.120 0.419 1759 384 ' '
3 0.500 0.500 0.500 872 274 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V1 V 0.32804(4) 0.22948(4) 0.12103(4) 0.0628(3) Uani 1 1 d . . . . .
S1 S 0.19070(7) 0.19070(7) 0.19070(7) 0.0425(6) Uani 1 6 d S T P . .
O3 O 0.2565(2) 0.17894(14) 0.17894(14) 0.0526(11) Uani 1 2 d S T P . .
O7 O 0.1530(2) 0.1530(2) 0.1530(2) 0.065(2) Uani 1 6 d S T P . .
O1 O 0.25585(18) 0.25585(18) 0.0737(2) 0.0652(13) Uani 1 2 d S T P . .
O5 O 0.3735(2) 0.19065(18) 0.19065(18) 0.0654(13) Uani 1 2 d S T P . .
O6 O 0.30084(16) 0.30084(16) 0.1693(2) 0.0640(13) Uani 1 2 d S TU P . .
O2 O 0.3838(2) 0.2588(2) 0.0863(2) 0.0995(14) Uani 1 1 d . . . . .
O4 O 0.3294(2) 0.1485(2) 0.07526(19) 0.0824(12) Uani 1 1 d . . . . .
C2 C 0.3333(4) 0.0452(3) 0.0452(3) 0.077(2) Uani 1 2 d S T P . .
C1 C 0.3308(4) 0.0928(3) 0.0928(3) 0.079(2) Uani 1 2 d S T P . .
C3 C 0.3341(3) 0.0616(4) -0.0164(4) 0.098(2) Uani 1 1 d . . . . .
C4 C 0.4377(4) 0.1866(5) 0.1866(5) 0.114(4) Uani 1 2 d S T P . .
H4A H 0.4534 0.2227 0.1672 0.170 Uiso 0.5 1 calc R . . . .
H4B H 0.4547 0.1830 0.2269 0.170 Uiso 0.5 1 calc R . . . .
H4C H 0.4486 0.1512 0.1629 0.170 Uiso 0.5 1 calc R . . . .
C6 C 0.2217(4) 0.2217(4) 0.0295(5) 0.123(4) Uani 1 2 d S T P . .
H6B H 0.1889 0.2465 0.0140 0.185 Uiso 0.5 1 calc R . . . .
H6A H 0.2482 0.2100 -0.0036 0.185 Uiso 0.5 1 calc R . . . .
H6C H 0.2052 0.1857 0.0484 0.185 Uiso 0.5 1 calc R . . . .
C5 C 0.3374(5) 0.3374(5) 0.2000(9) 0.168(6) Uani 1 2 d S TU P . .
H5A H 0.3137 0.3687 0.2198 0.251 Uiso 0.5 1 calc R . . . .
H5B H 0.3592 0.3142 0.2304 0.251 Uiso 0.5 1 calc R . . . .
H5C H 0.3661 0.3560 0.1724 0.251 Uiso 0.5 1 calc R . . . .
N1 N 0.3492(11) 0.1229(12) -0.0437(11) 0.093(6) Uani 0.25 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
V1 V1 3.044(2) 13 ?
V1 O3 2.294(3) . ?
V1 O1 1.971(3) . ?
V1 O5 2.004(3) . ?
V1 O6 1.973(3) . ?
V1 O2 1.571(4) . ?
V1 O4 2.031(4) . ?
S1 O3 1.482(5) 6 ?
S1 O3 1.482(5) 5 ?
S1 O3 1.482(5) . ?
S1 O7 1.427(9) . ?
O3 V1 2.294(3) 17 ?
O1 V1 1.971(3) 13 ?
O1 C6 1.429(11) . ?
O5 V1 2.004(3) 17 ?
O5 C4 1.407(11) . ?
O6 V1 1.973(3) 13 ?
O6 C5 1.314(13) . ?
O4 C1 1.277(5) . ?
C2 C1 1.469(12) . ?
C2 C3 1.393(9) . ?
C2 C3 1.393(9) 17 ?
C1 O4 1.277(5) 17 ?
C3 C3 1.396(12) 23 ?
C3 N1 1.50(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O3 V1 V1 81.86(9) . 13 ?
O1 V1 V1 39.45(12) . 13 ?
O1 V1 O3 83.38(17) . . ?
O1 V1 O5 156.57(19) . . ?
O1 V1 O4 90.43(19) . . ?
O5 V1 V1 130.49(16) . 13 ?
O5 V1 O3 73.47(15) . . ?
O5 V1 O4 89.9(2) . . ?
O6 V1 V1 39.51(12) . 13 ?
O6 V1 O3 83.13(18) . . ?
O6 V1 O1 78.96(16) . . ?
O6 V1 O5 94.5(2) . . ?
O6 V1 O4 162.69(19) . . ?
O2 V1 V1 105.1(2) . 13 ?
O2 V1 O3 172.1(2) . . ?
O2 V1 O1 104.4(2) . . ?
O2 V1 O5 98.9(2) . . ?
O2 V1 O6 99.8(2) . . ?
O2 V1 O4 96.1(2) . . ?
O4 V1 V1 128.71(14) . 13 ?
O4 V1 O3 82.08(16) . . ?
O3 S1 O3 107.8(2) . 5 ?
O3 S1 O3 107.8(2) . 6 ?
O3 S1 O3 107.8(2) 6 5 ?
O7 S1 O3 111.07(18) . 5 ?
O7 S1 O3 111.07(19) . 6 ?
O7 S1 O3 111.07(18) . . ?
V1 O3 V1 93.80(17) 17 . ?
S1 O3 V1 132.29(10) . . ?
S1 O3 V1 132.29(10) . 17 ?
V1 O1 V1 101.1(2) . 13 ?
C6 O1 V1 128.23(17) . . ?
C6 O1 V1 128.23(17) . 13 ?
V1 O5 V1 113.4(2) 17 . ?
C4 O5 V1 118.2(2) . . ?
C4 O5 V1 118.2(2) . 17 ?
V1 O6 V1 101.0(2) . 13 ?
C5 O6 V1 124.8(3) . . ?
C5 O6 V1 124.8(3) . 13 ?
C1 O4 V1 133.1(5) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 C1 120.2(4) 17 . ?
C3 C2 C3 119.7(8) 17 . ?
O4 C1 O4 124.8(9) 17 . ?
O4 C1 C2 117.6(4) 17 . ?
O4 C1 C2 117.6(4) . . ?
C2 C3 C3 120.2(4) . 23 ?
C2 C3 N1 128.0(10) . . ?
C3 C3 N1 110.4(9) 23 . ?
O5 C4 H4A 109.5 . . ?
O5 C4 H4B 109.5 . . ?
O5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C6 H6B 109.5 . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6B C6 H6A 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
O6 C5 H5A 109.5 . . ?
O6 C5 H5B 109.5 . . ?
O6 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(6)
2 0.47(6)

####################################################################### 
# 
# 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_VMOP-13_sq
_database_code_depnum_ccdc_archive 'CCDC 1479719'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_audit_creation_date             2016-06-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C168 H216 Br12 O200 S8 V48)'
_chemical_formula_sum            'C121 H152 Br6 O101 S4 V24'
_chemical_formula_weight         5052.68
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'x, z, y'
'z, y, x'
'-x, -z, y'
'z, -y, -x'
'-x, z, -y'
'-z, -y, x'
'x, -z, -y'
'-z, y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'z+1/2, y+1/2, x+1/2'
'-x+1/2, -z+1/2, y+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -z+1/2, -y+1/2'
'-z+1/2, y+1/2, -x+1/2'

_cell_length_a                   22.108(5)
_cell_length_b                   22.108(5)
_cell_length_c                   22.108(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10806(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3426
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.976
_cell_measurement_theta_min      2.256
_shelx_estimated_absorpt_T_max   0.705
_shelx_estimated_absorpt_T_min   0.641
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31352
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.974
_diffrn_reflns_theta_max         24.974
_diffrn_reflns_theta_min         1.302
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1566
_reflns_number_total             1787
_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       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 
;
 Flack x determined using 575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1787
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0567P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0925
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.97(4) 0.03(4)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C4A \\sim C4B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: Br1(0.25) H6A(0.5) H6B(0.5) H6C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
 C4A(0.15) H4AA(0.15) H4AB(0.15) H4AC(0.15) C4B(0.35) H4BA(0.35) H4BB(0.35)
 H4BC(0.35)
5.a Riding coordinates:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC)
5.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;

# SQUEEZE RESULTS (Version = 100616)
# 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 0.000 0.000 887 319 ' '
2 -0.136 -0.121 0.518 1587 457 ' '
3 0.500 0.500 0.500 887 319 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
V1 V -0.32470(4) -0.22699(4) -0.11935(5) 0.0421(3) Uani 1 1 d . . . . .
Br1 Br -0.35956(18) 0.05199(14) -0.13260(13) 0.0842(10) Uani 0.25 1 d . . . . .
O6 O -0.3802(2) -0.2552(2) -0.0835(2) 0.0656(13) Uani 1 1 d . . . . .
O2 O -0.3695(2) -0.18840(18) -0.18840(18) 0.0474(13) Uani 1 2 d S T P . .
O4 O -0.29770(17) -0.29770(17) -0.1664(2) 0.0462(14) Uani 1 2 d S T P . .
O5 O -0.25372(18) -0.25372(18) -0.0730(2) 0.0445(13) Uani 1 2 d S T P . .
O1 O -0.3253(2) -0.14682(18) -0.07443(19) 0.0546(11) Uani 1 1 d . . . . .
C2 C -0.3300(4) -0.0446(3) -0.0446(3) 0.049(2) Uani 1 2 d S T P . .
C3 C -0.3310(4) 0.0157(3) -0.0600(3) 0.071(2) Uani 1 1 d . . . . .
C6 C -0.2212(3) -0.2212(3) -0.0283(5) 0.075(3) Uani 1 2 d S T P . .
H6A H -0.2458 -0.1886 -0.0134 0.113 Uiso 0.5 1 calc R . . . .
H6B H -0.2112 -0.2479 0.0045 0.113 Uiso 0.5 1 calc R . . . .
H6C H -0.1848 -0.2052 -0.0457 0.113 Uiso 0.5 1 calc R . . . .
C1 C -0.3266(4) -0.0930(3) -0.0930(3) 0.051(2) Uani 1 2 d S T P . .
C5 C -0.4334(4) -0.1844(4) -0.1844(4) 0.084(4) Uani 1 2 d S T P . .
H5A H -0.4490 -0.1651 -0.2200 0.125 Uiso 0.5 1 calc R . . . .
H5B H -0.4503 -0.2242 -0.1809 0.125 Uiso 0.5 1 calc R . . . .
H5C H -0.4443 -0.1610 -0.1494 0.125 Uiso 0.5 1 calc R . . . .
S1 S -0.18907(7) -0.18907(7) -0.18907(7) 0.0312(7) Uani 1 6 d S T P . .
O3 O -0.2540(2) -0.17731(16) -0.17731(16) 0.0398(12) Uani 1 2 d S T P . .
O7 O -0.1513(2) -0.1513(2) -0.1513(2) 0.053(3) Uani 1 6 d S T P . .
C4A C -0.3132(19) -0.3132(19) -0.2339(17) 0.104(14) Uani 0.3 2 d S TU P A 1
H4AA H -0.2926 -0.3506 -0.2449 0.156 Uiso 0.15 1 d R . . A 1
H4AB H -0.3026 -0.2824 -0.2618 0.156 Uiso 0.15 1 d R . . A 1
H4AC H -0.3561 -0.3206 -0.2352 0.156 Uiso 0.15 1 d R . . A 1
C4B C -0.3382(5) -0.3382(5) -0.1958(9) 0.089(5) Uani 0.7 2 d S TU P A 2
H4BA H -0.3154 -0.3685 -0.2159 0.133 Uiso 0.35 1 d R . . A 2
H4BB H -0.3617 -0.3155 -0.2250 0.133 Uiso 0.35 1 d R . . A 2
H4BC H -0.3647 -0.3556 -0.1666 0.133 Uiso 0.35 1 d R . . A 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
V1 V1 3.055(2) 13 ?
V1 O6 1.588(4) . ?
V1 O2 2.010(3) . ?
V1 O4 1.971(3) . ?
V1 O5 1.965(4) . ?
V1 O1 2.032(4) . ?
V1 O3 2.301(3) . ?
Br1 Br1 2.520(6) 23 ?
Br1 C3 1.902(7) . ?
O2 V1 2.010(3) 17 ?
O2 C5 1.419(10) . ?
O4 V1 1.971(3) 13 ?
O4 C4A 1.57(4) . ?
O4 C4B 1.423(17) . ?
O5 V1 1.965(4) 13 ?
O5 C6 1.417(10) . ?
O1 C1 1.260(5) . ?
C2 C3 1.377(8) 17 ?
C2 C3 1.377(8) . ?
C2 C1 1.515(11) . ?
C3 C3 1.385(12) 23 ?
C1 O1 1.259(5) 17 ?
S1 O3 1.481(5) 6 ?
S1 O3 1.481(5) 5 ?
S1 O3 1.481(5) . ?
S1 O7 1.445(10) . ?
O3 V1 2.301(3) 17 ?

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
O6 V1 V1 105.60(17) . 13 ?
O6 V1 O2 99.5(2) . . ?
O6 V1 O4 100.7(2) . . ?
O6 V1 O5 103.8(2) . . ?
O6 V1 O1 95.3(2) . . ?
O6 V1 O3 172.0(2) . . ?
O2 V1 V1 130.44(16) . 13 ?
O2 V1 O1 89.9(2) . . ?
O2 V1 O3 73.10(16) . . ?
O4 V1 V1 39.18(12) . 13 ?
O4 V1 O2 94.9(2) . . ?
O4 V1 O1 162.2(2) . . ?
O4 V1 O3 83.0(2) . . ?
O5 V1 V1 38.99(13) . 13 ?
O5 V1 O2 156.5(2) . . ?
O5 V1 O4 78.17(17) . . ?
O5 V1 O1 90.74(19) . . ?
O5 V1 O3 83.75(19) . . ?
O1 V1 V1 128.44(13) . 13 ?
O1 V1 O3 81.98(18) . . ?
O3 V1 V1 81.77(10) . 13 ?
C3 Br1 Br1 72.6(2) . 23 ?
V1 O2 V1 113.7(2) . 17 ?
C5 O2 V1 118.0(2) . 17 ?
C5 O2 V1 118.0(2) . . ?
V1 O4 V1 101.6(2) . 13 ?
C4A O4 V1 127.6(5) . 13 ?
C4A O4 V1 127.6(5) . . ?
C4B O4 V1 123.3(4) . 13 ?
C4B O4 V1 123.3(4) . . ?
V1 O5 V1 102.0(3) 13 . ?
C6 O5 V1 128.02(16) . 13 ?
C6 O5 V1 128.02(16) . . ?
C1 O1 V1 131.7(5) . . ?
C3 C2 C3 118.7(8) . 17 ?
C3 C2 C1 120.6(4) . . ?
C3 C2 C1 120.6(4) 17 . ?
C2 C3 Br1 128.5(5) . . ?
C2 C3 C3 120.6(4) . 23 ?
C3 C3 Br1 107.4(2) 23 . ?
O1 C1 O1 127.9(8) 17 . ?
O1 C1 C2 116.0(4) 17 . ?
O1 C1 C2 116.0(4) . . ?
O3 S1 O3 108.0(2) . 5 ?
O3 S1 O3 108.0(2) . 6 ?
O3 S1 O3 108.0(2) 6 5 ?
O7 S1 O3 110.9(2) . . ?
O7 S1 O3 110.9(2) . 6 ?
O7 S1 O3 110.9(2) . 5 ?
V1 O3 V1 93.99(18) . 17 ?
S1 O3 V1 132.25(10) . . ?
S1 O3 V1 132.25(10) . 17 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.97(4)
2 0.03(4)

####################################################################### 
# 
# 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_VMOP-14_sq
_database_code_depnum_ccdc_archive 'CCDC 1479720'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_audit_creation_date             2016-06-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H120 O100 S4 V24'
_chemical_formula_sum            'C106.50 H221.50 N8.50 O100.50 S4 V24'
_chemical_formula_weight         4580.21
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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'
N N 0.0061 0.0033 '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      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   21.848(5)
_cell_length_b                   21.848(5)
_cell_length_c                   19.081(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     9108(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4594
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.419
_cell_measurement_theta_min      2.341
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.761
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.318
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5561
_reflns_number_total             8051
_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       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 
;
 Flack x determined using 2077 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      0.914
_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)+(0.0523P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0975
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-O13
 1.35 with sigma of 0.01
3. Rigid bond restraints
 O13, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11A \\sim C14A \\sim C11B \\sim C14B \\sim C12 \\sim C13 \\sim
C15 \\sim C16 \\sim C17 \\sim C18: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14A) = Uanis(C14B)
5. Others
 Fixed Sof: C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C14A(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C11B(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C14B(0.5)
 H14D(0.5) H14E(0.5) H14F(0.5)
6.a Riding coordinates:
 C11A(H11A,H11B,H11C), C14A(H14A,H14B,H14C), C11B(H11D,H11E,H11F), C14B(H14D,
 H14E,H14F)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;

# SQUEEZE RESULTS (Version = 100616)
# 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 -0.031 -0.012 -0.005 2709 781 ' '
2 0.500 0.500 0.000 205 26 ' '
3 0.000 0.000 0.500 205 26 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.1941(4) 0.0070(3) -0.2767(4) 0.0447(16) Uani 1 1 d . U . . .
C2 C 0.1798(3) -0.0541(3) -0.3051(4) 0.0464(16) Uani 1 1 d . U . . .
C3 C 0.1333(3) -0.0906(3) -0.2751(4) 0.0452(16) Uani 1 1 d . U . . .
H3 H 0.1125 -0.0770 -0.2355 0.054 Uiso 1 1 calc R . . . .
C4 C 0.1184(3) -0.1471(3) -0.3046(4) 0.0437(15) Uani 1 1 d . U . . .
C5 C 0.1507(3) -0.1667(3) -0.3642(4) 0.0460(16) Uani 1 1 d . U . . .
H5 H 0.1414 -0.2045 -0.3838 0.055 Uiso 1 1 calc R . . . .
C6 C 0.1943(3) -0.1324(3) -0.3933(3) 0.0423(15) Uani 1 1 d . U . . .
C7 C 0.2100(3) -0.0770(3) -0.3638(4) 0.0464(16) Uani 1 1 d . U . . .
H7 H 0.2416 -0.0544 -0.3835 0.056 Uiso 1 1 calc R . . . .
C8 C -0.0653(3) 0.1844(4) -0.2760(4) 0.0497(19) Uani 1 1 d . U . . .
C9 C 0.0358(5) 0.0572(6) -0.2085(7) 0.119(4) Uani 1 1 d . U . . .
H9A H -0.0064 0.0693 -0.2092 0.178 Uiso 1 1 calc R . . . .
H9B H 0.0480 0.0445 -0.2546 0.178 Uiso 1 1 calc R . . . .
H9C H 0.0411 0.0239 -0.1763 0.178 Uiso 1 1 calc R . . . .
C10 C 0.1523(4) 0.2254(4) -0.5390(4) 0.0461(18) Uani 1 1 d . U . . .
C11A C 0.1488(14) 0.3354(12) -0.2708(19) 0.087(6) Uani 0.5 1 d . U P A 1
H11A H 0.1322 0.3387 -0.2243 0.131 Uiso 0.5 1 d R . P A 1
H11B H 0.1821 0.3067 -0.2706 0.131 Uiso 0.5 1 d R . P A 1
H11C H 0.1634 0.3747 -0.2858 0.131 Uiso 0.5 1 d R . P A 1
C14A C 0.2455(12) 0.0895(15) -0.4498(17) 0.116(6) Uani 0.5 1 d . U P B 1
H14A H 0.2501 0.0511 -0.4261 0.173 Uiso 0.5 1 d R . P B 1
H14B H 0.2052 0.0921 -0.4696 0.173 Uiso 0.5 1 d R . P B 1
H14C H 0.2754 0.0926 -0.4865 0.173 Uiso 0.5 1 d R . P B 1
C11B C 0.1309(15) 0.3608(12) -0.276(2) 0.105(8) Uani 0.5 1 d . U P A 2
H11D H 0.1130 0.3576 -0.2303 0.157 Uiso 0.5 1 d R . P A 2
H11E H 0.1727 0.3474 -0.2743 0.157 Uiso 0.5 1 d R . P A 2
H11F H 0.1294 0.4026 -0.2914 0.157 Uiso 0.5 1 d R . P A 2
C14B C 0.2061(12) 0.0858(15) -0.4503(17) 0.116(6) Uani 0.5 1 d . U P B 2
H14D H 0.2136 0.0448 -0.4344 0.173 Uiso 0.5 1 d R . P B 2
H14E H 0.1631 0.0942 -0.4483 0.173 Uiso 0.5 1 d R . P B 2
H14F H 0.2202 0.0900 -0.4977 0.173 Uiso 0.5 1 d R . P B 2
C12 C 0.2443(5) 0.3595(4) -0.4297(6) 0.095(3) Uani 1 1 d . U . . .
H12A H 0.2868 0.3497 -0.4240 0.143 Uiso 1 1 calc R . . . .
H12B H 0.2368 0.3722 -0.4770 0.143 Uiso 1 1 calc R . . . .
H12C H 0.2335 0.3920 -0.3982 0.143 Uiso 1 1 calc R . . . .
C13 C 0.2916(5) 0.2594(5) -0.2787(5) 0.095(3) Uani 1 1 d . U . . .
H13A H 0.2963 0.2441 -0.2318 0.143 Uiso 1 1 calc R . . . .
H13B H 0.3311 0.2693 -0.2976 0.143 Uiso 1 1 calc R . . . .
H13C H 0.2666 0.2956 -0.2780 0.143 Uiso 1 1 calc R . . . .
C15 C 0.2933(5) 0.1376(5) -0.1499(6) 0.110(4) Uani 1 1 d . U . . .
H15A H 0.2763 0.1403 -0.1036 0.165 Uiso 1 1 calc R . . . .
H15B H 0.3192 0.1022 -0.1529 0.165 Uiso 1 1 calc R . . . .
H15C H 0.3169 0.1737 -0.1595 0.165 Uiso 1 1 calc R . . . .
C16 C 0.0171(6) 0.3194(5) -0.1490(7) 0.119(4) Uani 1 1 d . U . . .
H16A H 0.0125 0.3592 -0.1696 0.178 Uiso 1 1 calc R . . . .
H16B H -0.0199 0.3085 -0.1250 0.178 Uiso 1 1 calc R . . . .
H16C H 0.0505 0.3200 -0.1163 0.178 Uiso 1 1 calc R . . . .
C17 C 0.1662(5) 0.2356(5) -0.1182(6) 0.107(4) Uani 1 1 d . U . . .
H17A H 0.1455 0.2742 -0.1155 0.160 Uiso 1 1 calc R . . . .
H17B H 0.1717 0.2194 -0.0719 0.160 Uiso 1 1 calc R . . . .
H17C H 0.2054 0.2412 -0.1400 0.160 Uiso 1 1 calc R . . . .
C18 C 0.0019(6) 0.2374(6) -0.4467(7) 0.144(5) Uani 1 1 d D U . . .
H18A H 0.0154 0.2412 -0.4943 0.216 Uiso 1 1 calc R . . . .
H18B H 0.0114 0.1971 -0.4297 0.216 Uiso 1 1 calc R . . . .
H18C H -0.0415 0.2439 -0.4444 0.216 Uiso 1 1 calc R . . . .
O1 O 0.2640(2) 0.2153(2) -0.3200(3) 0.0561(13) Uani 1 1 d . . . . .
O2 O 0.2078(2) 0.3064(2) -0.4143(3) 0.0599(14) Uani 1 1 d . . . . .
O3 O 0.1032(3) 0.3240(2) -0.3183(3) 0.0621(14) Uani 1 1 d . . . . .
O4 O 0.0293(3) 0.2757(2) -0.2025(3) 0.0612(15) Uani 1 1 d . . . . .
O5 O 0.0691(2) 0.2006(2) -0.2912(2) 0.0484(12) Uani 1 1 d . . . . .
O6 O 0.1592(2) 0.1384(2) -0.2907(2) 0.0458(12) Uani 1 1 d . . . . .
O8 O 0.1439(2) 0.2123(2) -0.3821(2) 0.0495(12) Uani 1 1 d . . . . .
O7 O 0.0819(3) 0.1216(2) -0.3782(3) 0.0639(15) Uani 1 1 d . . . . .
O9 O 0.1700(3) 0.0850(2) -0.0990(3) 0.0642(15) Uani 1 1 d . . . . .
O10 O 0.3100(3) 0.2379(3) -0.4497(3) 0.0772(17) Uani 1 1 d . . . . .
O11 O 0.1659(2) 0.0243(2) -0.2229(3) 0.0491(13) Uani 1 1 d . . . . .
O12 O 0.2343(2) 0.0368(2) -0.3072(3) 0.0529(12) Uani 1 1 d . . . . .
O13 O 0.0311(2) 0.2803(2) -0.4059(3) 0.0599(14) Uani 1 1 d D U . . .
O14 O 0.1178(2) 0.2650(2) -0.5142(3) 0.0519(13) Uani 1 1 d . . . . .
O15 O 0.2023(2) 0.2085(2) -0.5133(3) 0.0550(13) Uani 1 1 d . . . . .
O16 O -0.0524(2) 0.2334(2) -0.3084(3) 0.0540(13) Uani 1 1 d . . . . .
O17 O -0.0390(2) 0.1651(2) -0.2229(3) 0.0524(13) Uani 1 1 d . . . . .
O18 O 0.2444(3) 0.1325(2) -0.2004(3) 0.0630(15) Uani 1 1 d . . . . .
O19 O 0.2469(2) 0.1332(2) -0.4043(3) 0.0559(14) Uani 1 1 d . . . . .
O20 O 0.3343(2) 0.1121(3) -0.2993(3) 0.0760(17) Uani 1 1 d . . . . .
O21 O 0.1085(3) 0.3759(2) -0.4531(3) 0.0769(18) Uani 1 1 d . . . . .
O22 O -0.0191(3) 0.3533(2) -0.2994(3) 0.0792(18) Uani 1 1 d . . . . .
O23 O 0.0159(3) 0.1911(3) -0.0974(3) 0.0707(16) Uani 1 1 d . . . . .
O24 O 0.0700(2) 0.1042(2) -0.1883(2) 0.0494(12) Uani 1 1 d . . . . .
O25 O 0.1305(2) 0.1938(2) -0.1589(2) 0.0601(14) Uani 1 1 d . . . . .
V1 V 0.26333(6) 0.12593(6) -0.30314(7) 0.0512(4) Uani 1 1 d . . . . .
V2 V 0.24370(6) 0.22235(6) -0.41976(7) 0.0499(3) Uani 1 1 d . . . . .
V3 V 0.15814(6) 0.10916(6) -0.17646(7) 0.0493(3) Uani 1 1 d . . . . .
V4 V 0.02007(6) 0.29228(6) -0.30421(7) 0.0548(4) Uani 1 1 d . . . . .
V5 V 0.11680(6) 0.30992(6) -0.42056(7) 0.0539(4) Uani 1 1 d . . . . .
V6 V 0.04112(6) 0.18871(6) -0.17601(7) 0.0508(4) Uani 1 1 d . . . . .
S1 S 0.11280(8) 0.16705(8) -0.33705(9) 0.0431(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.474(10) . ?
C1 O11 1.255(8) . ?
C1 O12 1.238(8) . ?
C2 C3 1.413(10) . ?
C2 C7 1.393(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(9) . ?
C4 C5 1.404(10) . ?
C4 C8 1.519(10) 2 ?
C5 H5 0.9300 . ?
C5 C6 1.333(10) . ?
C6 C7 1.379(9) . ?
C6 C10 1.522(10) 3_554 ?
C7 H7 0.9300 . ?
C8 C4 1.519(10) 2 ?
C8 O16 1.269(8) . ?
C8 O17 1.239(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 O24 1.326(12) . ?
C10 C6 1.522(10) 4_554 ?
C10 O14 1.240(9) . ?
C10 O15 1.254(9) . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9599 . ?
C11A H11C 0.9601 . ?
C11A O3 1.37(3) . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9601 . ?
C14A O19 1.29(3) . ?
C11B H11D 0.9601 . ?
C11B H11E 0.9599 . ?
C11B H11F 0.9600 . ?
C11B O3 1.29(3) . ?
C14B H14D 0.9599 . ?
C14B H14E 0.9599 . ?
C14B H14F 0.9600 . ?
C14B O19 1.62(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 O2 1.437(9) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 O1 1.383(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 O18 1.442(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 O4 1.423(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 O25 1.430(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 O13 1.375(9) . ?
O1 V1 1.979(5) . ?
O1 V2 1.961(5) . ?
O2 V2 1.998(6) . ?
O2 V5 1.994(5) . ?
O3 V4 1.962(5) . ?
O3 V5 1.998(6) . ?
O4 V4 1.985(5) . ?
O4 V6 1.983(5) . ?
O5 V4 2.285(5) . ?
O5 V6 2.296(5) . ?
O5 S1 1.488(5) . ?
O6 V1 2.305(5) . ?
O6 V3 2.272(5) . ?
O6 S1 1.483(5) . ?
O8 V2 2.307(5) . ?
O8 V5 2.332(5) . ?
O8 S1 1.475(5) . ?
O7 S1 1.435(5) . ?
O9 V3 1.591(5) . ?
O10 V2 1.593(6) . ?
O11 V3 2.062(5) . ?
O12 V1 2.050(5) . ?
O13 V4 1.973(6) . ?
O13 V5 2.000(5) . ?
O14 V5 2.039(5) . ?
O15 V2 2.023(5) . ?
O16 V4 2.041(5) . ?
O17 V6 2.032(5) . ?
O18 V1 2.008(5) . ?
O18 V3 2.006(6) . ?
O19 V1 1.970(5) . ?
O19 V2 1.972(5) . ?
O20 V1 1.581(5) . ?
O21 V5 1.579(5) . ?
O22 V4 1.587(5) . ?
O23 V6 1.599(6) . ?
O24 V3 1.942(5) . ?
O24 V6 1.966(5) . ?
O25 V3 1.974(5) . ?
O25 V6 1.983(5) . ?
V1 V2 3.0942(19) . ?
V3 V6 3.091(2) . ?
V4 V5 3.0892(19) . ?

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
O11 C1 C2 118.0(7) . . ?
O12 C1 C2 117.0(7) . . ?
O12 C1 O11 125.0(7) . . ?
C3 C2 C1 121.0(7) . . ?
C7 C2 C1 121.4(7) . . ?
C7 C2 C3 117.6(7) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(7) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 118.6(7) . . ?
C3 C4 C8 120.5(6) . 2 ?
C5 C4 C8 120.7(7) . 2 ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.7(7) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 120.0(7) . . ?
C5 C6 C10 120.9(7) . 3_554 ?
C7 C6 C10 119.1(7) . 3_554 ?
C2 C7 H7 119.1 . . ?
C6 C7 C2 121.7(7) . . ?
C6 C7 H7 119.1 . . ?
O16 C8 C4 116.6(7) . 2 ?
O17 C8 C4 117.8(7) . 2 ?
O17 C8 O16 125.7(7) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O24 C9 H9A 109.5 . . ?
O24 C9 H9B 109.5 . . ?
O24 C9 H9C 109.5 . . ?
O14 C10 C6 117.5(7) . 4_554 ?
O14 C10 O15 125.8(7) . . ?
O15 C10 C6 116.7(7) . 4_554 ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
O3 C11A H11A 110.4 . . ?
O3 C11A H11B 115.8 . . ?
O3 C11A H11C 101.8 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
O19 C14A H14A 109.1 . . ?
O19 C14A H14B 104.1 . . ?
O19 C14A H14C 115.0 . . ?
H11D C11B H11E 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
O3 C11B H11D 109.4 . . ?
O3 C11B H11E 106.3 . . ?
O3 C11B H11F 112.7 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
O19 C14B H14D 109.4 . . ?
O19 C14B H14E 113.2 . . ?
O19 C14B H14F 105.8 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O18 C15 H15A 109.5 . . ?
O18 C15 H15B 109.5 . . ?
O18 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O25 C17 H17A 109.5 . . ?
O25 C17 H17B 109.5 . . ?
O25 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O13 C18 H18A 109.5 . . ?
O13 C18 H18B 109.5 . . ?
O13 C18 H18C 109.5 . . ?
C13 O1 V1 126.8(6) . . ?
C13 O1 V2 126.7(5) . . ?
V2 O1 V1 103.5(2) . . ?
C12 O2 V2 120.9(5) . . ?
C12 O2 V5 120.5(5) . . ?
V5 O2 V2 115.1(2) . . ?
C11A O3 V4 130.3(15) . . ?
C11A O3 V5 124.5(15) . . ?
C11B O3 V4 124.7(16) . . ?
C11B O3 V5 129.5(16) . . ?
V4 O3 V5 102.5(2) . . ?
C16 O4 V4 124.0(6) . . ?
C16 O4 V6 119.0(6) . . ?
V6 O4 V4 115.9(2) . . ?
V4 O5 V6 94.48(18) . . ?
S1 O5 V4 131.9(3) . . ?
S1 O5 V6 132.7(3) . . ?
V3 O6 V1 94.30(17) . . ?
S1 O6 V1 131.5(3) . . ?
S1 O6 V3 133.2(3) . . ?
V2 O8 V5 93.12(16) . . ?
S1 O8 V2 132.9(3) . . ?
S1 O8 V5 132.8(3) . . ?
C1 O11 V3 131.5(5) . . ?
C1 O12 V1 134.6(5) . . ?
C18 O13 V4 126.1(7) . . ?
C18 O13 V5 125.2(7) . . ?
V4 O13 V5 102.1(2) . . ?
C10 O14 V5 132.6(5) . . ?
C10 O15 V2 133.7(5) . . ?
C8 O16 V4 133.2(5) . . ?
C8 O17 V6 132.3(5) . . ?
C15 O18 V1 120.4(6) . . ?
C15 O18 V3 124.3(6) . . ?
V1 O18 V3 113.4(2) . . ?
C14A O19 V1 127.2(16) . . ?
C14A O19 V2 129.0(16) . . ?
C14B O19 V1 125.3(13) . . ?
C14B O19 V2 122.0(13) . . ?
V1 O19 V2 103.4(2) . . ?
C9 O24 V3 129.5(6) . . ?
C9 O24 V6 125.5(6) . . ?
V3 O24 V6 104.6(2) . . ?
C17 O25 V3 121.6(6) . . ?
C17 O25 V6 131.5(6) . . ?
V3 O25 V6 102.7(2) . . ?
O1 V1 O6 84.68(19) . . ?
O1 V1 O12 159.0(2) . . ?
O1 V1 O18 95.1(2) . . ?
O1 V1 V2 38.04(15) . . ?
O6 V1 V2 81.75(12) . . ?
O12 V1 O6 79.08(19) . . ?
O12 V1 V2 125.23(15) . . ?
O18 V1 O6 71.81(19) . . ?
O18 V1 O12 92.4(2) . . ?
O18 V1 V2 128.65(16) . . ?
O19 V1 O1 76.3(2) . . ?
O19 V1 O6 84.94(19) . . ?
O19 V1 O12 89.0(2) . . ?
O19 V1 O18 156.0(2) . . ?
O19 V1 V2 38.31(15) . . ?
O20 V1 O1 100.9(3) . . ?
O20 V1 O6 170.4(2) . . ?
O20 V1 O12 97.1(3) . . ?
O20 V1 O18 99.8(3) . . ?
O20 V1 O19 103.8(3) . . ?
O20 V1 V2 107.4(2) . . ?
O1 V2 O2 96.3(2) . . ?
O1 V2 O8 84.49(19) . . ?
O1 V2 O15 161.0(2) . . ?
O1 V2 O19 76.7(2) . . ?
O1 V2 V1 38.46(14) . . ?
O2 V2 O8 72.57(18) . . ?
O2 V2 O15 90.5(2) . . ?
O2 V2 V1 129.93(17) . . ?
O8 V2 V1 80.91(13) . . ?
O10 V2 O1 99.1(3) . . ?
O10 V2 O2 100.3(3) . . ?
O10 V2 O8 172.4(3) . . ?
O10 V2 O15 97.0(3) . . ?
O10 V2 O19 103.4(3) . . ?
O10 V2 V1 106.1(2) . . ?
O15 V2 O8 80.67(18) . . ?
O15 V2 V1 126.47(16) . . ?
O19 V2 O2 156.0(2) . . ?
O19 V2 O8 83.86(19) . . ?
O19 V2 O15 90.0(2) . . ?
O19 V2 V1 38.26(15) . . ?
O6 V3 V6 81.51(13) . . ?
O9 V3 O6 169.5(2) . . ?
O9 V3 O11 95.0(2) . . ?
O9 V3 O18 98.2(3) . . ?
O9 V3 O24 104.6(3) . . ?
O9 V3 O25 101.7(2) . . ?
O9 V3 V6 108.6(2) . . ?
O11 V3 O6 80.80(18) . . ?
O11 V3 V6 125.08(15) . . ?
O18 V3 O6 72.58(18) . . ?
O18 V3 O11 93.1(2) . . ?
O18 V3 V6 129.40(16) . . ?
O24 V3 O6 85.04(18) . . ?
O24 V3 O11 88.9(2) . . ?
O24 V3 O18 156.9(2) . . ?
O24 V3 O25 76.7(2) . . ?
O24 V3 V6 37.99(14) . . ?
O25 V3 O6 84.38(18) . . ?
O25 V3 O11 160.1(2) . . ?
O25 V3 O18 95.0(2) . . ?
O25 V3 V6 38.73(15) . . ?
O3 V4 O4 95.9(2) . . ?
O3 V4 O5 83.8(2) . . ?
O3 V4 O13 78.4(2) . . ?
O3 V4 O16 159.2(2) . . ?
O3 V4 V5 39.16(17) . . ?
O4 V4 O5 71.69(19) . . ?
O4 V4 O16 90.2(2) . . ?
O4 V4 V5 130.97(17) . . ?
O5 V4 V5 82.36(12) . . ?
O13 V4 O4 157.7(2) . . ?
O13 V4 O5 86.2(2) . . ?
O13 V4 O16 88.4(2) . . ?
O13 V4 V5 39.28(15) . . ?
O16 V4 O5 79.36(18) . . ?
O16 V4 V5 125.52(16) . . ?
O22 V4 O3 102.2(3) . . ?
O22 V4 O4 98.7(3) . . ?
O22 V4 O5 169.4(3) . . ?
O22 V4 O13 103.6(3) . . ?
O22 V4 O16 96.5(3) . . ?
O22 V4 V5 107.8(2) . . ?
O2 V5 O3 95.5(2) . . ?
O2 V5 O8 72.09(18) . . ?
O2 V5 O13 155.8(2) . . ?
O2 V5 O14 91.3(2) . . ?
O2 V5 V4 129.35(17) . . ?
O3 V5 O8 82.58(19) . . ?
O3 V5 O13 76.9(2) . . ?
O3 V5 O14 158.7(2) . . ?
O3 V5 V4 38.31(15) . . ?
O8 V5 V4 80.38(12) . . ?
O13 V5 O8 84.08(19) . . ?
O13 V5 O14 88.6(2) . . ?
O13 V5 V4 38.66(16) . . ?
O14 V5 O8 80.37(18) . . ?
O14 V5 V4 125.23(15) . . ?
O21 V5 O2 100.0(3) . . ?
O21 V5 O3 103.1(3) . . ?
O21 V5 O8 170.9(2) . . ?
O21 V5 O13 104.1(3) . . ?
O21 V5 O14 95.5(3) . . ?
O21 V5 V4 108.5(2) . . ?
O4 V6 O5 71.49(19) . . ?
O4 V6 O17 91.1(2) . . ?
O4 V6 O25 96.7(2) . . ?
O4 V6 V3 130.19(17) . . ?
O5 V6 V3 80.83(13) . . ?
O17 V6 O5 80.57(19) . . ?
O17 V6 V3 124.61(15) . . ?
O23 V6 O4 99.4(3) . . ?
O23 V6 O5 170.5(2) . . ?
O23 V6 O17 97.2(3) . . ?
O23 V6 O24 104.7(3) . . ?
O23 V6 O25 100.5(3) . . ?
O23 V6 V3 107.8(2) . . ?
O24 V6 O4 155.7(2) . . ?
O24 V6 O5 84.61(18) . . ?
O24 V6 O17 89.1(2) . . ?
O24 V6 O25 75.9(2) . . ?
O24 V6 V3 37.45(15) . . ?
O25 V6 O5 83.66(19) . . ?
O25 V6 O17 159.2(2) . . ?
O25 V6 V3 38.52(14) . . ?
O6 S1 O5 107.2(3) . . ?
O8 S1 O5 108.0(3) . . ?
O8 S1 O6 108.4(3) . . ?
O7 S1 O5 111.1(3) . . ?
O7 S1 O6 110.9(3) . . ?
O7 S1 O8 111.2(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_VMOP-15_sq
_database_code_depnum_ccdc_archive 'CCDC 1479721'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_audit_creation_date             2016-06-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C144 H168 O100 S4 V24'
_chemical_formula_sum            'C183.50 H280.50 N9.50 O101.50 S4 V24'
_chemical_formula_weight         5594.46
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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'
N N 0.0061 0.0033 '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      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   28.983(5)
_cell_length_b                   28.983(5)
_cell_length_c                   25.744(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     21625(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5219
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.508
_cell_measurement_theta_min      2.221
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.877
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             5752
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.1292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60011
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         0.993
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7332
_reflns_number_total             17997
_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       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 
;
 Flack x determined using 2632 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         17997
_refine_ls_number_restraints     976
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      0.761
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0501P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1150
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C22A = O7-C22B
 1.35 with sigma of 0.01
 O12-C33A = O12-C33B
 1.35 with sigma of 0.01
3. Rigid bond restraints
 S1, O4
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O13, C1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C8, C13
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C17, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 V1, O19
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C17, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C13
\\sim C10 \\sim C11 \\sim C12 \\sim C21 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C28 \\sim C22A \\sim C23A \\sim C24A \\sim
C25A \\sim C26A \\sim C33A \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim
C26B \\sim C33B \\sim C27 \\sim C9 \\sim C29 \\sim C30 \\sim C31A \\sim C32A
\\sim C31B \\sim C32B \\sim C34 \\sim C35 \\sim C36: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03
Uanis(C3) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C22A) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C33B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
Uanis(C22A) = Uanis(C22B)
5. Others
 Fixed Sof: C22A(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23A(0.5) H23A(0.5)
 C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5) C26A(0.5) H26A(0.5) C33A(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
 C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5) C26B(0.5)
 H26B(0.5) C33B(0.5) H33D(0.5) H33E(0.5) H33F(0.5) C31A(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32A(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C31B(0.5)
 H31D(0.5) H31E(0.5) H31F(0.5) C32B(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
6.a Riding coordinates:
 C22A(H22A,H22B,H22C), C33A(H33A,H33B,H33C), C22B(H22D,H22E,H22F), C33B(H33D,
 H33E,H33F), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C31B(H31D,H31E,H31F),
 C32B(H32D,H32E,H32F)
6.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C13(H13), C10(H10), C12(H12), C15(H15), C16(H16),
 C18(H18), C19(H19), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C23B(H23B),
  C24B(H24B), C25B(H25B), C26B(H26B), C9(H9)
;

# SQUEEZE RESULTS (Version = 100616)
# 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 -0.013 -0.005 -0.001 13513 3200 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.0458(3) 0.2551(3) 0.4875(4) 0.081(2) Uani 1 1 d . U . . .
C2 C 0.0053(3) 0.2759(3) 0.5101(3) 0.0809(19) Uani 1 1 d . U . . .
C3 C 0.2170(3) 0.1433(3) 0.4776(4) 0.121(3) Uani 1 1 d . U . . .
H3A H 0.2468 0.1399 0.4934 0.182 Uiso 1 1 calc R . . . .
H3B H 0.2043 0.1134 0.4705 0.182 Uiso 1 1 calc R . . . .
H3C H 0.2200 0.1602 0.4457 0.182 Uiso 1 1 calc R . . . .
C4 C -0.0181(3) 0.3081(2) 0.4815(3) 0.0846(19) Uani 1 1 d . U . . .
H4 H -0.0071 0.3155 0.4487 0.102 Uiso 1 1 calc R . . . .
C5 C -0.0089(3) 0.2665(3) 0.5579(3) 0.084(2) Uani 1 1 d . U . . .
H5 H 0.0066 0.2453 0.5787 0.100 Uiso 1 1 calc R . . . .
C6 C -0.0461(3) 0.2885(3) 0.5749(3) 0.0858(18) Uani 1 1 d . U . . .
H6 H -0.0563 0.2798 0.6078 0.103 Uiso 1 1 calc R . . . .
C7 C -0.0713(3) 0.3214(3) 0.5516(3) 0.0769(17) Uani 1 1 d . U . . .
C8 C -0.1144(3) 0.3461(3) 0.5755(3) 0.0851(18) Uani 1 1 d . U . . .
C13 C -0.1278(3) 0.3911(2) 0.5529(3) 0.0839(17) Uani 1 1 d . U . . .
H13 H -0.1113 0.4045 0.5259 0.101 Uiso 1 1 calc R . . . .
C10 C -0.1357(2) 0.3283(3) 0.6174(3) 0.0792(17) Uani 1 1 d . U . . .
H10 H -0.1264 0.2999 0.6304 0.095 Uiso 1 1 calc R . . . .
C11 C -0.1712(3) 0.3520(3) 0.6411(3) 0.0783(17) Uani 1 1 d . U . . .
C12 C -0.1839(2) 0.3923(3) 0.6196(3) 0.0842(17) Uani 1 1 d . U . . .
H12 H -0.2070 0.4089 0.6362 0.101 Uiso 1 1 calc R . . . .
C21 C -0.1649(3) 0.4117(3) 0.5734(3) 0.0817(16) Uani 1 1 d . U . . .
C14 C -0.1944(3) 0.3346(2) 0.6872(3) 0.0773(17) Uani 1 1 d . U . . .
C15 C -0.1727(3) 0.3010(3) 0.7168(3) 0.0888(19) Uani 1 1 d . U . . .
H15 H -0.1430 0.2914 0.7083 0.107 Uiso 1 1 calc R . . . .
C16 C -0.1949(3) 0.2819(3) 0.7587(3) 0.0869(19) Uani 1 1 d . U . . .
H16 H -0.1809 0.2574 0.7759 0.104 Uiso 1 1 calc R . . . .
C17 C -0.2368(3) 0.2973(3) 0.7764(3) 0.0853(19) Uani 1 1 d . U . . .
C18 C -0.2585(3) 0.3312(3) 0.7460(3) 0.089(2) Uani 1 1 d . U . . .
H18 H -0.2879 0.3411 0.7553 0.107 Uiso 1 1 calc R . . . .
C19 C -0.2388(3) 0.3496(3) 0.7045(3) 0.0867(18) Uani 1 1 d . U . . .
H19 H -0.2541 0.3728 0.6863 0.104 Uiso 1 1 calc R . . . .
C20 C -0.2583(3) 0.2790(3) 0.8264(4) 0.089(2) Uani 1 1 d . U . . .
C28 C -0.1779(3) 0.4563(3) 0.5524(3) 0.0884(17) Uani 1 1 d . U . . .
C22A C 0.1221(7) 0.1652(7) 0.3915(8) 0.134(5) Uani 0.5 1 d D U P A 1
H22A H 0.1258 0.1773 0.3570 0.201 Uiso 0.5 1 d R . P A 1
H22B H 0.1421 0.1392 0.3961 0.201 Uiso 0.5 1 d R . P A 1
H22C H 0.0906 0.1559 0.3965 0.201 Uiso 0.5 1 d R . P A 1
C23A C -0.1689(6) 0.5247(6) 0.5016(7) 0.096(3) Uani 0.5 1 d . U P B 1
H23A H -0.1487 0.5432 0.4829 0.115 Uiso 0.5 1 calc R . P B 1
C24A C -0.1492(6) 0.4795(5) 0.5225(7) 0.090(2) Uani 0.5 1 d . U P B 1
H24A H -0.1196 0.4692 0.5147 0.108 Uiso 0.5 1 calc R . P B 1
C25A C -0.2083(6) 0.4855(6) 0.5796(7) 0.093(2) Uani 0.5 1 d . U P B 1
H25A H -0.2186 0.4770 0.6124 0.112 Uiso 0.5 1 calc R . P B 1
C26A C -0.2233(6) 0.5271(6) 0.5579(7) 0.093(3) Uani 0.5 1 d . U P B 1
H26A H -0.2417 0.5466 0.5779 0.112 Uiso 0.5 1 calc R . P B 1
C33A C 0.2864(7) 0.3658(5) 0.6027(8) 0.136(5) Uani 0.5 1 d D U P C 1
H33A H 0.2676 0.3846 0.5804 0.204 Uiso 0.5 1 d R . P C 1
H33B H 0.2795 0.3730 0.6383 0.204 Uiso 0.5 1 d R . P C 1
H33C H 0.3184 0.3719 0.5959 0.204 Uiso 0.5 1 d R . P C 1
C22B C 0.0993(6) 0.1688(7) 0.3958(8) 0.134(5) Uani 0.5 1 d D U P A 2
H22D H 0.1025 0.1772 0.3599 0.201 Uiso 0.5 1 d R . P A 2
H22E H 0.1083 0.1372 0.4004 0.201 Uiso 0.5 1 d R . P A 2
H22F H 0.0677 0.1726 0.4062 0.201 Uiso 0.5 1 d R . P A 2
C23B C -0.1889(5) 0.5045(5) 0.4756(7) 0.093(3) Uani 0.5 1 d . U P B 2
H23B H -0.1830 0.5116 0.4410 0.111 Uiso 0.5 1 calc R . P B 2
C24B C -0.1750(5) 0.4594(6) 0.4932(7) 0.094(2) Uani 0.5 1 d . U P B 2
H24B H -0.1656 0.4355 0.4716 0.113 Uiso 0.5 1 calc R . P B 2
C25B C -0.2262(6) 0.4711(6) 0.5583(7) 0.090(2) Uani 0.5 1 d . U P B 2
H25B H -0.2448 0.4539 0.5805 0.108 Uiso 0.5 1 calc R . P B 2
C26B C -0.2479(6) 0.5117(5) 0.5312(7) 0.096(3) Uani 0.5 1 d . U P B 2
H26B H -0.2794 0.5177 0.5297 0.115 Uiso 0.5 1 calc R . P B 2
C33B C 0.2647(7) 0.3532(6) 0.6123(7) 0.136(5) Uani 0.5 1 d D U P C 2
H33D H 0.2639 0.3829 0.5958 0.204 Uiso 0.5 1 d R . P C 2
H33E H 0.2354 0.3470 0.6282 0.204 Uiso 0.5 1 d R . P C 2
H33F H 0.2884 0.3530 0.6384 0.204 Uiso 0.5 1 d R . P C 2
C27 C -0.2117(3) 0.5407(3) 0.5072(3) 0.0839(18) Uani 1 1 d . U . . .
C9 C -0.0566(2) 0.3298(2) 0.4988(3) 0.0837(18) Uani 1 1 d . U . . .
H9 H -0.0731 0.3495 0.4773 0.100 Uiso 1 1 calc R . . . .
C29 C 0.3073(4) 0.3366(4) 0.3797(4) 0.164(4) Uani 1 1 d . U . . .
H29A H 0.2919 0.3332 0.3469 0.247 Uiso 1 1 calc R . . . .
H29B H 0.3203 0.3669 0.3822 0.247 Uiso 1 1 calc R . . . .
H29C H 0.3315 0.3140 0.3823 0.247 Uiso 1 1 calc R . . . .
C30 C 0.2313(4) 0.4131(3) 0.4866(4) 0.098(3) Uani 1 1 d . U . . .
C31A C 0.2211(17) 0.2446(18) 0.3839(15) 0.120(9) Uani 0.5 1 d . U P D 1
H31A H 0.2484 0.2623 0.3769 0.180 Uiso 0.5 1 d R . P D 1
H31B H 0.2259 0.2259 0.4143 0.180 Uiso 0.5 1 d R . P D 1
H31C H 0.2144 0.2251 0.3548 0.180 Uiso 0.5 1 d R . P D 1
C32A C 0.1063(17) 0.3619(16) 0.4527(11) 0.118(8) Uani 0.5 1 d . U P E 1
H32A H 0.0756 0.3496 0.4503 0.177 Uiso 0.5 1 d R . P E 1
H32B H 0.1156 0.3628 0.4884 0.177 Uiso 0.5 1 d R . P E 1
H32C H 0.1068 0.3926 0.4386 0.177 Uiso 0.5 1 d R . P E 1
C31B C 0.2282(16) 0.2430(16) 0.3690(16) 0.115(9) Uani 0.5 1 d . U P D 2
H31D H 0.2589 0.2554 0.3690 0.172 Uiso 0.5 1 d R . P D 2
H31E H 0.2287 0.2124 0.3833 0.172 Uiso 0.5 1 d R . P D 2
H31F H 0.2168 0.2419 0.3340 0.172 Uiso 0.5 1 d R . P D 2
C32B C 0.1046(17) 0.3698(16) 0.4274(11) 0.118(8) Uani 0.5 1 d . U P E 2
H32D H 0.0729 0.3613 0.4327 0.177 Uiso 0.5 1 d R . P E 2
H32E H 0.1151 0.3880 0.4562 0.177 Uiso 0.5 1 d R . P E 2
H32F H 0.1073 0.3874 0.3960 0.177 Uiso 0.5 1 d R . P E 2
C34 C 0.3254(3) 0.2392(3) 0.4775(4) 0.135(4) Uani 1 1 d . U . . .
H34A H 0.3233 0.2080 0.4896 0.202 Uiso 1 1 calc R . . . .
H34B H 0.3161 0.2407 0.4418 0.202 Uiso 1 1 calc R . . . .
H34C H 0.3567 0.2497 0.4806 0.202 Uiso 1 1 calc R . . . .
C35 C 0.3014(3) 0.1581(3) 0.5812(4) 0.149(4) Uani 1 1 d . U . . .
H35A H 0.2877 0.1281 0.5774 0.223 Uiso 1 1 calc R . . . .
H35B H 0.3241 0.1626 0.5546 0.223 Uiso 1 1 calc R . . . .
H35C H 0.3158 0.1604 0.6147 0.223 Uiso 1 1 calc R . . . .
C36 C 0.1083(3) 0.2051(3) 0.6189(4) 0.148(4) Uani 1 1 d . U . . .
H36A H 0.0774 0.2104 0.6066 0.223 Uiso 1 1 calc R . . . .
H36B H 0.1080 0.1811 0.6446 0.223 Uiso 1 1 calc R . . . .
H36C H 0.1202 0.2329 0.6339 0.223 Uiso 1 1 calc R . . . .
O1 O 0.20908(16) 0.25418(16) 0.55825(18) 0.0785(14) Uani 1 1 d . . . . .
O2 O 0.15086(13) 0.25625(14) 0.49483(19) 0.0686(12) Uani 1 1 d . . . . .
O3 O 0.15318(17) 0.31442(16) 0.56055(18) 0.0886(16) Uani 1 1 d . . . . .
O4 O 0.21199(16) 0.31226(14) 0.4941(2) 0.0793(14) Uani 1 1 d . U . . .
O5 O 0.27189(17) 0.32914(17) 0.4249(2) 0.0964(17) Uani 1 1 d . . . . .
O6 O 0.19282(18) 0.27200(18) 0.3944(2) 0.0920(18) Uani 1 1 d . . . . .
O7 O 0.12772(15) 0.19948(15) 0.42715(17) 0.0736(14) Uani 1 1 d D . . . .
O8 O 0.18793(16) 0.16704(15) 0.5111(2) 0.0887(16) Uani 1 1 d . . . . .
O9 O 0.26863(17) 0.19050(17) 0.5771(2) 0.0989(18) Uani 1 1 d . . . . .
O10 O 0.29814(17) 0.26587(16) 0.5059(2) 0.0946(17) Uani 1 1 d . . . . .
O11 O 0.13564(16) 0.19201(15) 0.5782(2) 0.0822(15) Uani 1 1 d . . . . .
O12 O 0.28049(17) 0.32315(16) 0.57372(19) 0.0889(16) Uani 1 1 d D . . . .
O13 O 0.06314(16) 0.22326(17) 0.5107(2) 0.0851(15) Uani 1 1 d . U . . .
O14 O 0.2058(2) 0.3597(2) 0.3516(2) 0.122(2) Uani 1 1 d . . . . .
O15 O 0.20333(19) 0.40042(17) 0.4470(2) 0.0933(16) Uani 1 1 d . . . . .
O16 O 0.2632(2) 0.39656(19) 0.5071(2) 0.102(2) Uani 1 1 d . . . . .
O17 O 0.34169(16) 0.35177(19) 0.4935(2) 0.120(2) Uani 1 1 d . . . . .
O18 O 0.33703(16) 0.25006(18) 0.6048(2) 0.110(2) Uani 1 1 d . . . . .
O19 O 0.20085(18) 0.12531(17) 0.6032(2) 0.116(2) Uani 1 1 d . U . . .
O20 O 0.09923(15) 0.13562(16) 0.4977(2) 0.0966(16) Uani 1 1 d . . . . .
O22 O 0.06536(16) 0.27339(17) 0.4479(2) 0.0852(15) Uani 1 1 d . . . . .
O23 O 0.10562(17) 0.26433(17) 0.3522(2) 0.0951(16) Uani 1 1 d . . . . .
O24 O -0.29166(17) 0.30202(18) 0.84422(19) 0.0866(16) Uani 1 1 d . . . . .
O25 O -0.23768(17) 0.24385(19) 0.84614(19) 0.0871(15) Uani 1 1 d . . . . .
O21 O 0.13681(16) 0.33311(16) 0.4201(2) 0.0890(15) Uani 1 1 d . . . . .
V1 V 0.20040(4) 0.17794(4) 0.58560(6) 0.0831(4) Uani 1 1 d . U . . .
V2 V 0.28876(4) 0.33282(4) 0.49860(6) 0.0875(4) Uani 1 1 d . . . . .
V3 V 0.12344(4) 0.18498(4) 0.50236(6) 0.0783(4) Uani 1 1 d . . . . .
V4 V 0.12614(4) 0.26600(4) 0.41011(6) 0.0813(4) Uani 1 1 d . . . . .
V5 V 0.28621(4) 0.25659(4) 0.58323(6) 0.0841(4) Uani 1 1 d . . . . .
V6 V 0.20466(5) 0.33851(5) 0.40929(6) 0.0881(4) Uani 1 1 d . . . . .
S1 S 0.18039(7) 0.28539(7) 0.52824(8) 0.0703(6) Uani 1 1 d . 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
C1 C2 1.442(10) . ?
C1 O13 1.209(8) . ?
C1 O22 1.281(9) . ?
C2 C4 1.369(9) . ?
C2 C5 1.327(9) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 O8 1.390(8) . ?
C4 H4 0.9300 . ?
C4 C9 1.354(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.329(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.343(9) . ?
C7 C8 1.565(10) . ?
C7 C9 1.445(10) . ?
C8 C13 1.481(9) . ?
C8 C10 1.345(9) . ?
C13 H13 0.9300 . ?
C13 C21 1.336(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.379(9) . ?
C11 C12 1.345(9) . ?
C11 C14 1.453(9) . ?
C12 H12 0.9300 . ?
C12 C21 1.425(9) . ?
C21 C28 1.451(10) . ?
C14 C15 1.388(9) . ?
C14 C19 1.430(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.373(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.373(9) . ?
C17 C18 1.405(10) . ?
C17 C20 1.524(11) . ?
C18 H18 0.9300 . ?
C18 C19 1.323(9) . ?
C19 H19 0.9300 . ?
C20 O24 1.262(9) . ?
C20 O25 1.286(9) . ?
C28 C24A 1.317(15) . ?
C28 C25A 1.408(17) . ?
C28 C24B 1.528(18) . ?
C28 C25B 1.471(17) . ?
C22A H22A 0.9601 . ?
C22A H22B 0.9599 . ?
C22A H22C 0.9601 . ?
C22A O7 1.362(12) . ?
C23A H23A 0.9300 . ?
C23A C24A 1.528(19) . ?
C23A C27 1.332(15) . ?
C24A H24A 0.9300 . ?
C25A H25A 0.9300 . ?
C25A C26A 1.40(2) . ?
C26A H26A 0.9300 . ?
C26A C27 1.404(16) . ?
C33A H33A 0.9602 . ?
C33A H33B 0.9600 . ?
C33A H33C 0.9600 . ?
C33A O12 1.455(12) . ?
C22B H22D 0.9598 . ?
C22B H22E 0.9601 . ?
C22B H22F 0.9603 . ?
C22B O7 1.457(12) . ?
C23B H23B 0.9300 . ?
C23B C24B 1.441(19) . ?
C23B C27 1.485(17) . ?
C24B H24B 0.9300 . ?
C25B H25B 0.9300 . ?
C25B C26B 1.51(2) . ?
C26B H26B 0.9300 . ?
C26B C27 1.479(17) . ?
C33B H33D 0.9598 . ?
C33B H33E 0.9601 . ?
C33B H33F 0.9601 . ?
C33B O12 1.398(12) . ?
C27 C30 1.548(11) 2_565 ?
C9 H9 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 O5 1.566(10) . ?
C30 C27 1.548(11) 2_565 ?
C30 O15 1.355(10) . ?
C30 O16 1.165(11) . ?
C31A H31A 0.9600 . ?
C31A H31B 0.9601 . ?
C31A H31C 0.9601 . ?
C31A O6 1.17(4) . ?
C32A H32A 0.9601 . ?
C32A H32B 0.9599 . ?
C32A H32C 0.9600 . ?
C32A O21 1.48(5) . ?
C31B H31D 0.9600 . ?
C31B H31E 0.9599 . ?
C31B H31F 0.9600 . ?
C31B O6 1.48(4) . ?
C32B H32D 0.9600 . ?
C32B H32E 0.9600 . ?
C32B H32F 0.9601 . ?
C32B O21 1.43(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C34 O10 1.325(8) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C35 O9 1.340(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C36 O11 1.367(9) . ?
O1 V1 2.333(5) . ?
O1 V5 2.327(5) . ?
O1 S1 1.451(5) . ?
O2 V3 2.222(4) . ?
O2 V4 2.313(5) . ?
O2 S1 1.478(4) . ?
O3 S1 1.422(4) . ?
O4 V2 2.306(5) . ?
O4 V6 2.323(5) . ?
O4 S1 1.489(5) . ?
O5 V2 1.963(5) . ?
O5 V6 2.008(5) . ?
O6 V4 1.982(5) . ?
O6 V6 1.996(5) . ?
O7 V3 1.985(5) . ?
O7 V4 1.978(5) . ?
O8 V1 1.976(5) . ?
O8 V3 1.953(5) . ?
O9 V1 2.023(5) . ?
O9 V5 1.989(5) . ?
O10 V2 1.968(5) . ?
O10 V5 2.038(6) . ?
O11 V1 1.930(5) . ?
O11 V3 1.995(5) . ?
O12 V2 1.969(5) . ?
O12 V5 1.951(5) . ?
O13 V3 2.081(5) . ?
O14 V6 1.608(6) . ?
O15 V6 2.040(6) . ?
O16 V2 2.003(5) . ?
O17 V2 1.635(5) . ?
O18 V5 1.585(5) . ?
O19 V1 1.591(5) . ?
O20 V3 1.598(5) . ?
O22 V4 2.024(5) . ?
O23 V4 1.605(5) . ?
O24 V1 2.011(5) 7_456 ?
O25 V5 2.023(5) 7_456 ?
O21 V4 1.986(5) . ?
O21 V6 1.992(5) . ?
V1 O24 2.012(5) 8_556 ?
V1 V3 3.100(2) . ?
V2 V5 3.103(2) . ?
V4 V6 3.0977(19) . ?
V5 O25 2.023(5) 8_556 ?

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
O13 C1 C2 117.2(9) . . ?
O13 C1 O22 121.7(8) . . ?
O22 C1 C2 120.6(8) . . ?
C4 C2 C1 118.2(8) . . ?
C5 C2 C1 122.7(8) . . ?
C5 C2 C4 119.0(8) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O8 C3 H3A 109.5 . . ?
O8 C3 H3B 109.5 . . ?
O8 C3 H3C 109.5 . . ?
C2 C4 H4 118.4 . . ?
C9 C4 C2 123.2(8) . . ?
C9 C4 H4 118.4 . . ?
C2 C5 H5 121.4 . . ?
C2 C5 C6 117.3(8) . . ?
C6 C5 H5 121.4 . . ?
C5 C6 H6 115.3 . . ?
C5 C6 C7 129.5(8) . . ?
C7 C6 H6 115.3 . . ?
C6 C7 C8 125.7(8) . . ?
C6 C7 C9 112.3(7) . . ?
C9 C7 C8 121.9(7) . . ?
C13 C8 C7 117.3(7) . . ?
C10 C8 C7 120.4(7) . . ?
C10 C8 C13 122.1(8) . . ?
C8 C13 H13 121.7 . . ?
C21 C13 C8 116.7(8) . . ?
C21 C13 H13 121.7 . . ?
C8 C10 H10 119.7 . . ?
C8 C10 C11 120.5(8) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C14 122.3(7) . . ?
C12 C11 C10 116.9(8) . . ?
C12 C11 C14 120.8(7) . . ?
C11 C12 H12 117.2 . . ?
C11 C12 C21 125.5(8) . . ?
C21 C12 H12 117.2 . . ?
C13 C21 C12 117.6(7) . . ?
C13 C21 C28 117.3(7) . . ?
C12 C21 C28 124.1(7) . . ?
C15 C14 C11 118.8(7) . . ?
C15 C14 C19 116.8(7) . . ?
C19 C14 C11 124.4(7) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.1(8) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 118.5 . . ?
C17 C16 C15 123.0(8) . . ?
C17 C16 H16 118.5 . . ?
C16 C17 C18 116.0(8) . . ?
C16 C17 C20 121.9(8) . . ?
C18 C17 C20 122.2(8) . . ?
C17 C18 H18 118.7 . . ?
C19 C18 C17 122.7(8) . . ?
C19 C18 H18 118.7 . . ?
C14 C19 H19 119.4 . . ?
C18 C19 C14 121.1(8) . . ?
C18 C19 H19 119.4 . . ?
O24 C20 C17 115.8(8) . . ?
O25 C20 C17 114.8(8) . . ?
O25 C20 O24 129.1(8) . . ?
C21 C28 C24B 114.2(9) . . ?
C21 C28 C25B 117.9(9) . . ?
C24A C28 C21 120.5(10) . . ?
C24A C28 C25A 112.3(12) . . ?
C25A C28 C21 120.9(10) . . ?
C25B C28 C24B 97.9(10) . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
O7 C22A H22A 110.2 . . ?
O7 C22A H22B 114.7 . . ?
O7 C22A H22C 103.3 . . ?
C24A C23A H23A 116.2 . . ?
C27 C23A H23A 116.2 . . ?
C27 C23A C24A 127.6(14) . . ?
C28 C24A C23A 114.0(14) . . ?
C28 C24A H24A 123.0 . . ?
C23A C24A H24A 123.0 . . ?
C28 C25A H25A 119.5 . . ?
C28 C25A C26A 121.0(16) . . ?
C26A C25A H25A 119.5 . . ?
C25A C26A H26A 118.7 . . ?
C27 C26A C25A 122.6(15) . . ?
C27 C26A H26A 118.7 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
O12 C33A H33A 96.2 . . ?
O12 C33A H33B 130.5 . . ?
O12 C33A H33C 100.1 . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O7 C22B H22D 109.0 . . ?
O7 C22B H22E 111.1 . . ?
O7 C22B H22F 108.3 . . ?
C24B C23B H23B 116.8 . . ?
C24B C23B C27 126.4(15) . . ?
C27 C23B H23B 116.8 . . ?
C28 C24B H24B 124.7 . . ?
C23B C24B C28 110.7(14) . . ?
C23B C24B H24B 124.7 . . ?
C28 C25B H25B 117.4 . . ?
C28 C25B C26B 125.2(14) . . ?
C26B C25B H25B 117.4 . . ?
C25B C26B H26B 125.0 . . ?
C27 C26B C25B 110.0(14) . . ?
C27 C26B H26B 125.0 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
O12 C33B H33D 104.6 . . ?
O12 C33B H33E 118.4 . . ?
O12 C33B H33F 105.1 . . ?
C23A C27 C26A 102.9(12) . . ?
C23A C27 C30 127.4(10) . 2_565 ?
C26A C27 C30 118.2(10) . 2_565 ?
C23B C27 C26B 98.2(10) . . ?
C23B C27 C30 126.1(10) . 2_565 ?
C30 C27 C26B 112.0(9) 2_565 . ?
C4 C9 C7 118.3(7) . . ?
C4 C9 H9 120.8 . . ?
C7 C9 H9 120.8 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O5 C29 H29A 109.5 . . ?
O5 C29 H29B 109.5 . . ?
O5 C29 H29C 109.5 . . ?
O15 C30 C27 105.8(9) . 2_565 ?
O16 C30 C27 119.4(9) . 2_565 ?
O16 C30 O15 134.8(9) . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
O6 C31A H31A 105.0 . . ?
O6 C31A H31B 107.3 . . ?
O6 C31A H31C 115.9 . . ?
H32A C32A H32B 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
O21 C32A H32A 108.1 . . ?
O21 C32A H32B 113.0 . . ?
O21 C32A H32C 107.4 . . ?
H31D C31B H31E 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
O6 C31B H31D 115.5 . . ?
O6 C31B H31E 111.3 . . ?
O6 C31B H31F 101.2 . . ?
H32D C32B H32E 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
O21 C32B H32D 117.0 . . ?
O21 C32B H32E 107.7 . . ?
O21 C32B H32F 103.4 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O10 C34 H34A 109.5 . . ?
O10 C34 H34B 109.5 . . ?
O10 C34 H34C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O9 C35 H35A 109.5 . . ?
O9 C35 H35B 109.5 . . ?
O9 C35 H35C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O11 C36 H36A 109.5 . . ?
O11 C36 H36B 109.5 . . ?
O11 C36 H36C 109.5 . . ?
V1 O1 V5 92.80(17) . . ?
S1 O1 V1 133.6(3) . . ?
S1 O1 V5 132.7(3) . . ?
V3 O2 V4 94.88(17) . . ?
S1 O2 V3 133.4(3) . . ?
S1 O2 V4 131.2(3) . . ?
V2 O4 V6 92.9(2) . . ?
S1 O4 V2 134.4(3) . . ?
S1 O4 V6 132.0(3) . . ?
C29 O5 V2 123.2(5) . . ?
C29 O5 V6 118.0(5) . . ?
V2 O5 V6 115.3(2) . . ?
C31A O6 V4 132(3) . . ?
C31A O6 V6 125(3) . . ?
C31B O6 V4 135.8(19) . . ?
C31B O6 V6 121.0(19) . . ?
V4 O6 V6 102.3(2) . . ?
C22A O7 V3 119.7(11) . . ?
C22A O7 V4 123.9(11) . . ?
C22B O7 V3 112.1(10) . . ?
C22B O7 V4 117.3(10) . . ?
V4 O7 V3 114.9(2) . . ?
C3 O8 V1 124.8(5) . . ?
C3 O8 V3 129.9(5) . . ?
V3 O8 V1 104.2(2) . . ?
C35 O9 V1 123.9(6) . . ?
C35 O9 V5 119.2(6) . . ?
V5 O9 V1 114.5(2) . . ?
C34 O10 V2 127.2(5) . . ?
C34 O10 V5 124.2(5) . . ?
V2 O10 V5 101.5(2) . . ?
C36 O11 V1 123.2(5) . . ?
C36 O11 V3 132.5(5) . . ?
V1 O11 V3 104.3(2) . . ?
C33A O12 V2 111.7(9) . . ?
C33A O12 V5 140.0(10) . . ?
C33B O12 V2 130.5(10) . . ?
C33B O12 V5 123.7(10) . . ?
V5 O12 V2 104.7(2) . . ?
C1 O13 V3 134.8(6) . . ?
C30 O15 V6 125.8(6) . . ?
C30 O16 V2 128.5(7) . . ?
C1 O22 V4 136.4(5) . . ?
C20 O24 V1 130.1(5) . 7_456 ?
C20 O25 V5 131.2(6) . 7_456 ?
C32A O21 V4 122.2(19) . . ?
C32A O21 V6 128.8(19) . . ?
C32B O21 V4 130(2) . . ?
C32B O21 V6 127(2) . . ?
V6 O21 V4 102.3(2) . . ?
O1 V1 V3 78.86(12) . . ?
O8 V1 O1 83.02(18) . . ?
O8 V1 O9 95.9(2) . . ?
O8 V1 O24 159.2(2) . 8_556 ?
O8 V1 V3 37.67(14) . . ?
O9 V1 O1 72.02(19) . . ?
O9 V1 V3 128.06(17) . . ?
O11 V1 O1 82.83(18) . . ?
O11 V1 O8 76.1(2) . . ?
O11 V1 O9 154.4(2) . . ?
O11 V1 O24 87.8(2) . 8_556 ?
O11 V1 V3 38.58(15) . . ?
O19 V1 O1 173.2(2) . . ?
O19 V1 O8 97.2(3) . . ?
O19 V1 O9 101.3(2) . . ?
O19 V1 O11 103.8(2) . . ?
O19 V1 O24 99.4(3) . 8_556 ?
O19 V1 V3 105.4(2) . . ?
O24 V1 O1 81.94(18) 8_556 . ?
O24 V1 O9 93.0(2) 8_556 . ?
O24 V1 V3 124.54(15) 8_556 . ?
O4 V2 V5 80.10(13) . . ?
O5 V2 O4 72.40(19) . . ?
O5 V2 O10 94.2(2) . . ?
O5 V2 O12 155.8(2) . . ?
O5 V2 O16 93.6(2) . . ?
O5 V2 V5 129.36(16) . . ?
O10 V2 O4 83.30(18) . . ?
O10 V2 O16 161.8(2) . . ?
O10 V2 V5 40.05(16) . . ?
O12 V2 O4 84.0(2) . . ?
O12 V2 O10 77.4(2) . . ?
O12 V2 O16 88.8(2) . . ?
O12 V2 V5 37.46(14) . . ?
O16 V2 O4 83.5(2) . . ?
O16 V2 V5 124.84(19) . . ?
O17 V2 O4 171.1(3) . . ?
O17 V2 O5 100.0(3) . . ?
O17 V2 O10 102.1(2) . . ?
O17 V2 O12 104.0(3) . . ?
O17 V2 O16 92.7(3) . . ?
O17 V2 V5 108.6(2) . . ?
O2 V3 V1 82.19(12) . . ?
O7 V3 O2 72.28(18) . . ?
O7 V3 O11 157.22(19) . . ?
O7 V3 O13 92.3(2) . . ?
O7 V3 V1 130.02(14) . . ?
O8 V3 O2 85.14(18) . . ?
O8 V3 O7 96.3(2) . . ?
O8 V3 O11 75.2(2) . . ?
O8 V3 O13 159.0(2) . . ?
O8 V3 V1 38.18(15) . . ?
O11 V3 O2 85.82(19) . . ?
O11 V3 O13 89.6(2) . . ?
O11 V3 V1 37.11(14) . . ?
O13 V3 O2 79.27(17) . . ?
O13 V3 V1 124.58(16) . . ?
O20 V3 O2 169.4(2) . . ?
O20 V3 O7 98.3(2) . . ?
O20 V3 O8 101.0(2) . . ?
O20 V3 O11 104.0(2) . . ?
O20 V3 O13 96.7(2) . . ?
O20 V3 V1 108.0(2) . . ?
O2 V4 V6 82.05(11) . . ?
O6 V4 O2 84.35(19) . . ?
O6 V4 O22 159.7(2) . . ?
O6 V4 O21 77.8(2) . . ?
O6 V4 V6 39.01(15) . . ?
O7 V4 O2 70.40(17) . . ?
O7 V4 O6 96.2(2) . . ?
O7 V4 O22 91.0(2) . . ?
O7 V4 O21 157.3(2) . . ?
O7 V4 V6 130.23(14) . . ?
O22 V4 O2 80.16(18) . . ?
O22 V4 V6 124.82(15) . . ?
O23 V4 O2 170.5(2) . . ?
O23 V4 O6 100.0(2) . . ?
O23 V4 O7 100.7(2) . . ?
O23 V4 O22 97.3(2) . . ?
O23 V4 O21 102.0(2) . . ?
O23 V4 V6 106.64(18) . . ?
O21 V4 O2 87.12(18) . . ?
O21 V4 O22 88.3(2) . . ?
O21 V4 V6 38.93(14) . . ?
O1 V5 V2 81.39(13) . . ?
O9 V5 O1 72.71(18) . . ?
O9 V5 O10 95.3(2) . . ?
O9 V5 O25 92.3(2) . 8_556 ?
O9 V5 V2 129.47(18) . . ?
O10 V5 O1 84.09(19) . . ?
O10 V5 V2 38.42(13) . . ?
O12 V5 O1 85.04(18) . . ?
O12 V5 O9 157.0(2) . . ?
O12 V5 O10 76.2(2) . . ?
O12 V5 O25 89.7(2) . 8_556 ?
O12 V5 V2 37.85(15) . . ?
O18 V5 O1 170.3(3) . . ?
O18 V5 O9 98.7(2) . . ?
O18 V5 O10 101.5(3) . . ?
O18 V5 O12 103.9(2) . . ?
O18 V5 O25 95.5(3) . 8_556 ?
O18 V5 V2 108.0(2) . . ?
O25 V5 O1 80.62(19) 8_556 . ?
O25 V5 O10 160.1(2) 8_556 . ?
O25 V5 V2 125.64(14) 8_556 . ?
O4 V6 V4 80.71(12) . . ?
O5 V6 O4 71.3(2) . . ?
O5 V6 O15 92.4(2) . . ?
O5 V6 V4 128.30(15) . . ?
O6 V6 O4 83.13(19) . . ?
O6 V6 O5 94.3(2) . . ?
O6 V6 O15 159.7(2) . . ?
O6 V6 V4 38.71(16) . . ?
O14 V6 O4 172.8(3) . . ?
O14 V6 O5 102.5(3) . . ?
O14 V6 O6 101.2(3) . . ?
O14 V6 O15 95.9(3) . . ?
O14 V6 O21 100.3(3) . . ?
O14 V6 V4 106.3(2) . . ?
O15 V6 O4 80.9(2) . . ?
O15 V6 V4 125.42(15) . . ?
O21 V6 O4 86.19(19) . . ?
O21 V6 O5 156.9(2) . . ?
O21 V6 O6 77.4(2) . . ?
O21 V6 O15 89.1(2) . . ?
O21 V6 V4 38.79(13) . . ?
O1 S1 O2 106.6(3) . . ?
O1 S1 O4 106.7(3) . . ?
O3 S1 O1 112.0(3) . . ?
O3 S1 O2 110.9(3) . . ?
O3 S1 O4 112.1(3) . . ?
O4 S1 O2 108.2(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
