# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_A'
_database_code_depnum_ccdc_archive 'CCDC 1859014'
loop_
_audit_author_name
_audit_author_address
'kai chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2019-05-28 deposited with the CCDC.	2019-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H119 Mo12 N24 O104 P'
_chemical_formula_weight         3734.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'

_cell_length_a                   18.0014(11)
_cell_length_b                   18.0014(11)
_cell_length_c                   29.4043(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     8251.9(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4623
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.38

_exptl_crystal_description       lump
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_F_000             5562
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.481
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24940
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.478
_diffrn_reflns_theta_max         25.986
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1991
_reflns_number_gt                1685
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+342.9695P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1991
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.1984
_refine_ls_wR_factor_gt          0.1915
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_restrained_S_all      1.261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.0973(6) 0.0486(3) 0.8863(5) 0.078(4) Uani 1 2 d S T P . .
O4 O 0.0956(3) -0.0956(3) 0.8555(3) 0.051(2) Uani 1 2 d S T P . .
O5 O 0.2352(11) 0.1176(6) 0.9898(4) 0.094(5) Uani 1 2 d S T P . .
O6 O 0.2886(6) 0.000000 1.000000 0.108(6) Uani 1 2 d S T P . .
O7 O 0.1662(5) -0.0210(5) 0.9380(3) 0.080(3) Uani 1 1 d . . . . .
O8 O -0.0464(4) -0.0929(9) 1.0175(5) 0.052(3) Uani 0.7 2 d S T P . .
O9 O 0.000000 0.000000 0.9462(11) 0.035(7) Uani 0.5 6 d S T P . .
Mo1 Mo 0.06601(4) -0.06601(4) 0.90117(4) 0.0381(3) Uani 1 2 d S T P . .
Mo2 Mo 0.19682(7) 0.000000 1.000000 0.079 Uani 1 2 d S T P . .
P1 P 0.000000 0.000000 1.000000 0.0310(16) Uani 1 12 d S T P . .
C1 C 0.4465(6) 0.1103(6) 0.8983(3) 0.041(2) Uani 1 1 d . . . . .
C2 C 0.3608(5) 0.0778(5) 0.8334(3) 0.0352(19) Uani 1 1 d . . . . .
C3 C 0.3537(9) 0.1769(4) 0.8931(4) 0.039(3) Uani 1 2 d S T P . .
H3A H 0.361640 0.180817 0.925856 0.046 Uiso 1 2 calc R U P . .
H3B H 0.292563 0.146282 0.887086 0.046 Uiso 1 2 calc R U P . .
C4 C 0.5086(5) 0.0173(9) 0.8924(4) 0.041(3) Uani 1 2 d S T P . .
H4A H 0.511879 0.023763 0.925189 0.049 Uiso 1 2 calc R U P . .
H4B H 0.478181 -0.043641 0.885672 0.049 Uiso 1 2 calc R U P . .
N1 N 0.4604(5) 0.0550(5) 0.8743(2) 0.0356(16) Uani 1 1 d . . . . .
N2 N 0.3914(5) 0.1288(5) 0.8743(2) 0.0330(15) Uani 1 1 d . . . . .
O1 O 0.4772(5) 0.1428(4) 0.93486(19) 0.0471(17) Uani 1 1 d . . . . .
O2 O 0.2724(4) 0.0271(5) 0.8374(2) 0.0510(17) Uani 1 1 d . . . . .
H2 H 0.250861 0.015166 0.811932 0.077 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 Mo1 1.899(4) . ?
O3 Mo1 1.899(4) 2 ?
O4 Mo1 1.629(9) . ?
O5 Mo2 1.894(5) . ?
O5 Mo2 1.894(5) 21_557 ?
O6 Mo2 1.653(12) . ?
O7 Mo2 1.887(7) . ?
O7 Mo1 1.903(8) . ?
O8 P1 1.537(14) . ?
O8 O8 1.78(2) 20_557 ?
O8 O8 1.78(2) 21_557 ?
O8 O9 1.80(2) 19_557 ?
O8 Mo2 2.455(10) 3 ?
O8 Mo2 2.455(10) 20_557 ?
O8 Mo1 2.468(15) 20_557 ?
O9 P1 1.58(3) . ?
O9 Mo1 2.448(17) 3 ?
O9 Mo1 2.448(17) 2 ?
O9 Mo1 2.448(17) . ?
C1 O1 1.216(11) . ?
C1 N1 1.343(12) . ?
C1 N2 1.388(11) . ?
C2 O2 1.388(11) . ?
C2 N1 1.431(11) 18_546 ?
C2 N2 1.444(11) . ?
C2 C2 1.570(16) 18_546 ?
C3 N2 1.450(9) . ?
C3 N2 1.450(9) 23 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.445(10) 22_655 ?
C4 N1 1.445(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O2 H2 0.8200 . ?

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
Mo1 O3 Mo1 139.7(7) . 2 ?
Mo2 O5 Mo2 138.6(8) . 21_557 ?
Mo2 O7 Mo1 139.1(5) . . ?
P1 O8 O8 54.7(3) . 20_557 ?
P1 O8 O8 54.7(3) . 21_557 ?
O8 O8 O8 89.8(12) 20_557 21_557 ?
P1 O8 O9 55.9(10) . 19_557 ?
O8 O8 O9 90.9(8) 20_557 19_557 ?
O8 O8 O9 90.9(8) 21_557 19_557 ?
P1 O8 Mo2 123.5(5) . 3 ?
O8 O8 Mo2 68.8(3) 20_557 3 ?
O8 O8 Mo2 131.1(11) 21_557 3 ?
O9 O8 Mo2 131.0(4) 19_557 3 ?
P1 O8 Mo2 123.5(5) . 20_557 ?
O8 O8 Mo2 131.1(11) 20_557 20_557 ?
O8 O8 Mo2 68.8(3) 21_557 20_557 ?
O9 O8 Mo2 131.0(4) 19_557 20_557 ?
Mo2 O8 Mo2 92.4(5) 3 20_557 ?
P1 O8 Mo1 123.9(8) . 20_557 ?
O8 O8 Mo1 131.4(8) 20_557 20_557 ?
O8 O8 Mo1 131.4(9) 21_557 20_557 ?
O9 O8 Mo1 67.9(9) 19_557 20_557 ?
Mo2 O8 Mo1 92.3(4) 3 20_557 ?
Mo2 O8 Mo1 92.3(4) 20_557 20_557 ?
P1 O9 O8 53.6(9) . 19_557 ?
P1 O9 O8 53.6(9) . 21_557 ?
O8 O9 O8 88.4(14) 19_557 21_557 ?
P1 O9 O8 53.6(9) . 20_557 ?
O8 O9 O8 88.4(14) 19_557 20_557 ?
O8 O9 O8 88.4(14) 21_557 20_557 ?
P1 O9 Mo1 122.8(6) . 3 ?
O8 O9 Mo1 131.26(12) 19_557 3 ?
O8 O9 Mo1 131.27(12) 21_557 3 ?
O8 O9 Mo1 69.2(5) 20_557 3 ?
P1 O9 Mo1 122.8(6) . 2 ?
O8 O9 Mo1 69.2(5) 19_557 2 ?
O8 O9 Mo1 131.26(12) 21_557 2 ?
O8 O9 Mo1 131.27(12) 20_557 2 ?
Mo1 O9 Mo1 93.5(9) 3 2 ?
P1 O9 Mo1 122.8(6) . . ?
O8 O9 Mo1 131.27(12) 19_557 . ?
O8 O9 Mo1 69.2(5) 21_557 . ?
O8 O9 Mo1 131.27(12) 20_557 . ?
Mo1 O9 Mo1 93.5(9) 3 . ?
Mo1 O9 Mo1 93.5(9) 2 . ?
O4 Mo1 O3 101.4(5) . 3 ?
O4 Mo1 O3 101.4(5) . . ?
O3 Mo1 O3 87.5(6) 3 . ?
O4 Mo1 O7 102.4(4) . . ?
O3 Mo1 O7 156.2(5) 3 . ?
O3 Mo1 O7 88.0(5) . . ?
O4 Mo1 O7 102.4(4) . 24 ?
O3 Mo1 O7 88.0(5) 3 24 ?
O3 Mo1 O7 156.2(5) . 24 ?
O7 Mo1 O7 86.7(5) . 24 ?
O4 Mo1 O9 157.2(8) . . ?
O3 Mo1 O9 63.2(6) 3 . ?
O3 Mo1 O9 63.2(6) . . ?
O7 Mo1 O9 94.1(6) . . ?
O7 Mo1 O9 94.1(6) 24 . ?
O4 Mo1 O8 159.9(5) . 21_557 ?
O3 Mo1 O8 93.1(5) 3 21_557 ?
O3 Mo1 O8 93.1(5) . 21_557 ?
O7 Mo1 O8 63.9(3) . 21_557 ?
O7 Mo1 O8 63.9(3) 24 21_557 ?
O9 Mo1 O8 42.9(7) . 21_557 ?
O6 Mo2 O7 101.1(3) . 4_557 ?
O6 Mo2 O7 101.1(3) . . ?
O7 Mo2 O7 157.8(6) 4_557 . ?
O6 Mo2 O5 101.2(5) . . ?
O7 Mo2 O5 87.0(4) 4_557 . ?
O7 Mo2 O5 88.7(5) . . ?
O6 Mo2 O5 101.2(5) . 20_557 ?
O7 Mo2 O5 88.7(5) 4_557 20_557 ?
O7 Mo2 O5 87.0(4) . 20_557 ?
O5 Mo2 O5 157.6(10) . 20_557 ?
O6 Mo2 O8 158.8(3) . 21_557 ?
O7 Mo2 O8 94.2(5) 4_557 21_557 ?
O7 Mo2 O8 64.4(5) . 21_557 ?
O5 Mo2 O8 94.1(6) . 21_557 ?
O5 Mo2 O8 64.3(5) 20_557 21_557 ?
O6 Mo2 O8 158.8(3) . 2 ?
O7 Mo2 O8 64.4(5) 4_557 2 ?
O7 Mo2 O8 94.2(5) . 2 ?
O5 Mo2 O8 64.3(5) . 2 ?
O5 Mo2 O8 94.1(6) 20_557 2 ?
O8 Mo2 O8 42.4(6) 21_557 2 ?
O8 P1 O8 180.0 20_557 2 ?
O8 P1 O8 109.4(5) 20_557 19_557 ?
O8 P1 O8 70.6(6) 2 19_557 ?
O8 P1 O8 109.4(6) 20_557 21_557 ?
O8 P1 O8 70.6(6) 2 21_557 ?
O8 P1 O8 109.4(6) 19_557 21_557 ?
O8 P1 O8 70.6(6) 20_557 3 ?
O8 P1 O8 109.4(6) 2 3 ?
O8 P1 O8 70.6(6) 19_557 3 ?
O8 P1 O8 180.0(10) 21_557 3 ?
O8 P1 O8 70.6(6) 20_557 . ?
O8 P1 O8 109.4(5) 2 . ?
O8 P1 O8 180.0(10) 19_557 . ?
O8 P1 O8 70.6(6) 21_557 . ?
O8 P1 O8 109.4(6) 3 . ?
O8 P1 O9 70.5(5) 20_557 . ?
O8 P1 O9 109.5(5) 2 . ?
O8 P1 O9 70.5(5) 19_557 . ?
O8 P1 O9 70.5(5) 21_557 . ?
O8 P1 O9 109.5(5) 3 . ?
O8 P1 O9 109.5(5) . . ?
O8 P1 O9 109.5(5) 20_557 19_557 ?
O8 P1 O9 70.5(5) 2 19_557 ?
O8 P1 O9 109.5(5) 19_557 19_557 ?
O8 P1 O9 109.5(5) 21_557 19_557 ?
O8 P1 O9 70.5(5) 3 19_557 ?
O8 P1 O9 70.5(5) . 19_557 ?
O9 P1 O9 180.0 . 19_557 ?
O1 C1 N1 127.8(9) . . ?
O1 C1 N2 122.8(9) . . ?
N1 C1 N2 109.3(8) . . ?
O2 C2 N1 113.9(7) . 18_546 ?
O2 C2 N2 107.2(7) . . ?
N1 C2 N2 113.9(7) 18_546 . ?
O2 C2 C2 115.1(5) . 18_546 ?
N1 C2 C2 103.5(8) 18_546 18_546 ?
N2 C2 C2 102.9(7) . 18_546 ?
N2 C3 N2 112.3(10) . 23 ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3A 109.2 23 . ?
N2 C3 H3B 109.2 . . ?
N2 C3 H3B 109.2 23 . ?
H3A C3 H3B 107.9 . . ?
N1 C4 N1 113.5(10) 22_655 . ?
N1 C4 H4A 108.9 22_655 . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 22_655 . ?
N1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C1 N1 C2 112.8(7) . 18_546 ?
C1 N1 C4 122.3(8) . . ?
C2 N1 C4 124.2(8) 18_546 . ?
C1 N2 C2 111.2(7) . . ?
C1 N2 C3 123.5(8) . . ?
C2 N2 C3 123.7(8) . . ?
C2 O2 H2 109.5 . . ?

_refine_diff_density_max         1.964
_refine_diff_density_min         -3.200
_refine_diff_density_rms         0.195



####################################################################### 
# 
# 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_A
_database_code_depnum_ccdc_archive 'CCDC 1859015'
loop_
_audit_author_name
_audit_author_address
'kai chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2019-05-28 deposited with the CCDC.	2019-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 N24 O64 P W12'
_chemical_formula_weight         4066.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'

_cell_length_a                   18.096(4)
_cell_length_b                   18.096(4)
_cell_length_c                   29.247(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     8294(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7274
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.48

_exptl_crystal_description       lump
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_F_000             5505
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    12.536
_shelx_estimated_absorpt_T_min   0.199
_shelx_estimated_absorpt_T_max   0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2314
_exptl_absorpt_correction_T_max  0.3581
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24340
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.474
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.009
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1798
_reflns_number_gt                1684
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+2100.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1798
_refine_ls_number_parameters     121
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1465
_refine_ls_wR_factor_gt          0.1440
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1418(9) 0.4779(10) 0.0637(4) 0.047(4) Uani 1 1 d . . . . .
O3 O -0.0580(8) 0.3635(8) 0.1708(5) 0.041(3) Uani 1 1 d . . . . .
H3 H -0.070024 0.327712 0.190914 0.062 Uiso 1 1 d R U . . .
N1 N 0.0539(9) 0.4596(9) 0.1253(5) 0.030(3) Uani 1 1 d . . . . .
N2 N 0.1305(10) 0.3939(10) 0.1260(4) 0.032(3) Uani 1 1 d . . . . .
C1 C 0.1082(13) 0.4467(11) 0.1011(7) 0.041(5) Uani 1 1 d . . . . .
C2 C 0.0294(10) 0.4124(11) 0.1668(5) 0.029(4) Uani 1 1 d . . . . .
C5 C 0.1802(9) 0.3604(17) 0.1066(9) 0.033(6) Uani 1 2 d S T P . .
H5A H 0.186104 0.372210 0.074042 0.040 Uiso 1 2 calc R U P . .
H5B H 0.149465 0.298932 0.110404 0.040 Uiso 1 2 calc R U P . .
C6 C 0.0181(17) 0.5091(8) 0.1075(9) 0.035(6) Uani 1 2 d S T P . .
H6A H 0.025335 0.512667 0.074515 0.042 Uiso 1 2 calc R U P . .
H6B H -0.042696 0.478651 0.113636 0.042 Uiso 1 2 calc R U P . .
W1 W 0.19647(5) 0.19647(5) 0.000000 0.0306(3) Uani 1 2 d S T P . .
W2 W 0.13116(7) 0.06558(3) 0.09971(3) 0.0300(3) Uani 1 2 d S T P . .
O5 O 0.1930(14) 0.0965(7) 0.1455(6) 0.046(5) Uani 1 2 d S T P A .
O6 O 0.2906(10) 0.2906(10) 0.000000 0.053(5) Uani 1 2 d S T P . .
O7 O 0.1160(9) 0.2319(18) 0.0103(6) 0.063(7) Uani 1 2 d S T P . .
O8 O 0.0488(8) 0.0976(17) 0.1172(9) 0.071(6) Uani 1 2 d S TU P A .
O9 O 0.1845(12) 0.1646(10) 0.0630(4) 0.061(5) Uani 1 1 d . . . . .
P1 P 0.000000 0.000000 0.000000 0.015(3) Uani 1 12 d S T P . .
O11 O 0.000000 0.000000 0.0567(14) 0.027(11) Uani 0.6 6 d S T P A 1
O11' O 0.0906(19) 0.0453(10) 0.0169(10) 0.017(2) Uani 0.468 2 d S TU P 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
O1 C1 1.24(2) . ?
O3 C2 1.38(2) . ?
O3 H3 0.8199 . ?
N1 C1 1.32(2) . ?
N1 C2 1.42(2) . ?
N1 C6 1.441(18) . ?
N2 C1 1.41(2) . ?
N2 C5 1.429(19) . ?
N2 C2 1.44(2) 10_455 ?
C2 C2 1.56(4) 10_455 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
W1 O6 1.703(18) . ?
W1 O7 1.887(9) . ?
W1 O7 1.887(9) 20 ?
W1 O9 1.910(12) . ?
W1 O9 1.910(12) 4 ?
W1 O11' 2.48(2) 21 ?
W1 O11' 2.48(2) . ?
W2 O5 1.653(18) . ?
W2 O9 1.888(14) 23 ?
W2 O9 1.888(15) . ?
W2 O8 1.919(10) 3 ?
W2 O8 1.919(10) . ?
W2 O11 2.41(2) . ?
W2 O11' 2.50(3) . ?
P1 O11' 1.50(3) . ?
P1 O11' 1.50(3) 19 ?
P1 O11' 1.50(3) 21 ?
P1 O11' 1.50(3) 3 ?
P1 O11' 1.50(3) 20 ?
P1 O11' 1.50(3) 2 ?
P1 O11 1.66(4) 19 ?
P1 O11 1.66(4) . ?
O11' O11' 1.73(4) 20 ?
O11' O11' 1.73(4) 21 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O3 H3 109.6 . . ?
C1 N1 C2 112.8(15) . . ?
C1 N1 C6 121.3(18) . . ?
C2 N1 C6 125.5(17) . . ?
C1 N2 C5 122.5(16) . . ?
C1 N2 C2 110.0(15) . 10_455 ?
C5 N2 C2 125.6(17) . 10_455 ?
O1 C1 N1 129(2) . . ?
O1 C1 N2 121.2(18) . . ?
N1 C1 N2 109.5(16) . . ?
O3 C2 N1 111.9(14) . . ?
O3 C2 N2 107.3(13) . 10_455 ?
N1 C2 N2 114.3(14) . 10_455 ?
O3 C2 C2 116.0(10) . 10_455 ?
N1 C2 C2 104.3(14) . 10_455 ?
N2 C2 C2 102.9(15) 10_455 10_455 ?
N2 C5 N2 115(2) . 24 ?
N2 C5 H5A 108.6 . . ?
N2 C5 H5A 108.6 24 . ?
N2 C5 H5B 108.6 . . ?
N2 C5 H5B 108.6 24 . ?
H5A C5 H5B 107.6 . . ?
N1 C6 N1 115.6(19) 23_565 . ?
N1 C6 H6A 108.4 23_565 . ?
N1 C6 H6A 108.4 . . ?
N1 C6 H6B 108.4 23_565 . ?
N1 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
O6 W1 O7 102.5(8) . . ?
O6 W1 O7 102.5(8) . 20 ?
O7 W1 O7 155.1(16) . 20 ?
O6 W1 O9 102.0(6) . . ?
O7 W1 O9 87.6(8) . . ?
O7 W1 O9 87.2(7) 20 . ?
O6 W1 O9 102.0(6) . 4 ?
O7 W1 O9 87.2(7) . 4 ?
O7 W1 O9 87.6(8) 20 4 ?
O9 W1 O9 156.0(11) . 4 ?
O6 W1 O11' 159.6(6) . 21 ?
O7 W1 O11' 63.5(9) . 21 ?
O7 W1 O11' 92.4(10) 20 21 ?
O9 W1 O11' 92.5(9) . 21 ?
O9 W1 O11' 64.3(8) 4 21 ?
O6 W1 O11' 159.6(6) . . ?
O7 W1 O11' 92.4(10) . . ?
O7 W1 O11' 63.5(9) 20 . ?
O9 W1 O11' 64.3(8) . . ?
O9 W1 O11' 92.5(9) 4 . ?
O11' W1 O11' 40.8(12) 21 . ?
O5 W2 O9 101.6(7) . 23 ?
O5 W2 O9 101.6(7) . . ?
O9 W2 O9 87.8(8) 23 . ?
O5 W2 O8 100.2(9) . 3 ?
O9 W2 O8 88.3(9) 23 3 ?
O9 W2 O8 158.1(9) . 3 ?
O5 W2 O8 100.2(9) . . ?
O9 W2 O8 158.1(9) 23 . ?
O9 W2 O8 88.3(9) . . ?
O8 W2 O8 87.3(16) 3 . ?
O5 W2 O11 157.3(11) . . ?
O9 W2 O11 94.6(8) 23 . ?
O9 W2 O11 94.6(8) . . ?
O8 W2 O11 64.2(9) 3 . ?
O8 W2 O11 64.2(9) . . ?
O5 W2 O11' 158.8(10) . . ?
O9 W2 O11' 64.0(6) 23 . ?
O9 W2 O11' 64.0(6) . . ?
O8 W2 O11' 95.0(9) 3 . ?
O8 W2 O11' 95.0(9) . . ?
W1 O7 W1 140.9(15) 21 . ?
W2 O8 W2 136.1(14) 2 . ?
W2 O9 W1 139.7(9) . . ?
O11' P1 O11' 70.2(11) . 21 ?
O11' P1 O11' 109.8(11) 19 21 ?
O11' P1 O11' 109.8(11) . 3 ?
O11' P1 O11' 70.2(11) 19 3 ?
O11' P1 O11' 180(3) 21 3 ?
O11' P1 O11' 70.2(11) . 20 ?
O11' P1 O11' 109.8(11) 19 20 ?
O11' P1 O11' 109.8(11) 21 20 ?
O11' P1 O11' 70.2(11) 3 20 ?
O11 P1 O11 180.0 19 . ?
P1 O11 W2 121.5(8) . . ?
P1 O11 W2 121.5(8) . 3 ?
W2 O11 W2 95.2(11) . 3 ?
P1 O11 W2 121.5(8) . 2 ?
W2 O11 W2 95.2(11) . 2 ?
W2 O11 W2 95.2(11) 3 2 ?
P1 O11' O11' 54.9(5) . 20 ?
P1 O11' O11' 54.9(5) . 21 ?
O11' O11' O11' 91(2) 20 21 ?
P1 O11' W1 124.5(9) . 20 ?
O11' O11' W1 69.6(6) 20 20 ?
O11' O11' W1 132(2) 21 20 ?
P1 O11' W1 124.5(9) . . ?
O11' O11' W1 132(2) 20 . ?
O11' O11' W1 69.6(6) 21 . ?
W1 O11' W1 91.5(10) 20 . ?
P1 O11' W2 123.9(16) . . ?
O11' O11' W2 131.0(17) 20 . ?
O11' O11' W2 131.0(17) 21 . ?
W1 O11' W2 91.3(8) 20 . ?
W1 O11' W2 91.3(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 O1 -179.9(19) . . . . ?
C6 N1 C1 O1 7(3) . . . . ?
C2 N1 C1 N2 -4(2) . . . . ?
C6 N1 C1 N2 -177.8(15) . . . . ?
C5 N2 C1 O1 -12(3) . . . . ?
C2 N2 C1 O1 -176.8(17) 10_455 . . . ?
C5 N2 C1 N1 172.4(17) . . . . ?
C2 N2 C1 N1 7(2) 10_455 . . . ?
C1 N1 C2 O3 -126.0(16) . . . . ?
C6 N1 C2 O3 47(2) . . . . ?
C1 N1 C2 N2 111.8(17) . . . 10_455 ?
C6 N1 C2 N2 -75(2) . . . 10_455 ?
C1 N1 C2 C2 0.1(16) . . . 10_455 ?
C6 N1 C2 C2 173.1(14) . . . 10_455 ?
C1 N2 C5 N2 112(2) . . . 24 ?
C2 N2 C5 N2 -85(3) 10_455 . . 24 ?
C1 N1 C6 N1 -104(2) . . . 23_565 ?
C2 N1 C6 N1 84(3) . . . 23_565 ?
O6 W1 O7 W1 155.0(18) . . . 21 ?
O7 W1 O7 W1 -25.0(18) 20 . . 21 ?
O9 W1 O7 W1 -103(2) . . . 21 ?
O9 W1 O7 W1 53(2) 4 . . 21 ?
O11' W1 O7 W1 -9.2(18) 21 . . 21 ?
O11' W1 O7 W1 -39(2) . . . 21 ?
O5 W2 O9 W1 154.0(14) . . . . ?
O9 W2 O9 W1 52.6(18) 23 . . . ?
O8 W2 O9 W1 -27(3) 3 . . . ?
O8 W2 O9 W1 -105.8(16) . . . . ?
O11 W2 O9 W1 -41.9(15) . . . . ?
O11' W2 O9 W1 -9.4(13) . . . . ?
O11' P1 O11' O11' -121(3) 21 . . 20 ?
O11' P1 O11' O11' 59(3) 3 . . 20 ?
O11' P1 O11' O11' 180.000(0) 2 . . 20 ?
O11' P1 O11' O11' 180.000(0) 3 . . 21 ?
O11' P1 O11' O11' 121(3) 20 . . 21 ?
O11' P1 O11' O11' -59(3) 2 . . 21 ?
O11' P1 O11' W1 -121(3) 21 . . 20 ?
O11' P1 O11' W1 59(3) 3 . . 20 ?
O11' P1 O11' W1 0.001(3) 20 . . 20 ?
O11' P1 O11' W1 180.001(3) 2 . . 20 ?
O11' P1 O11' W1 -0.001(3) 21 . . . ?
O11' P1 O11' W1 179.999(3) 3 . . . ?
O11' P1 O11' W1 121(3) 20 . . . ?
O11' P1 O11' W1 -59(3) 2 . . . ?
O11' P1 O11' W2 119.6(14) 21 . . . ?
O11' P1 O11' W2 -60.4(14) 3 . . . ?
O11' P1 O11' W2 -119.6(13) 20 . . . ?
O11' P1 O11' W2 60.4(13) 2 . . . ?

_refine_diff_density_max         3.621
_refine_diff_density_min         -2.053
_refine_diff_density_rms         0.323



####################################################################### 
# 
# 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_B
_database_code_depnum_ccdc_archive 'CCDC 1859016'
loop_
_audit_author_name
_audit_author_address
'kai chen'
;NanJing University of information Science and technology
China
;
_audit_update_record             
;
2019-05-28 deposited with the CCDC.	2019-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H77 Cl3 N24 O43'
_chemical_formula_weight         1640.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   22.317(3)
_cell_length_b                   22.317(3)
_cell_length_c                   22.272(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9606(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5006
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      24.66

_exptl_crystal_description       lump
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_F_000             5136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.273
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24938
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.825
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        24.993
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1889
_reflns_number_gt                1515
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1331P)²+13.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1889
_refine_ls_number_parameters     133
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.2292
_refine_ls_wR_factor_gt          0.2093
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.333333 0.41988(8) -0.083333 0.0754(6) Uani 1 2 d S T P . .
C1 C 0.11158(16) 0.20422(16) -0.08527(13) 0.0280(7) Uani 1 1 d . . . . .
C2 C 0.10375(16) 0.26309(15) -0.00063(12) 0.0244(7) Uani 1 1 d . . . . .
C3 C 0.17299(15) 0.26006(15) 0.00215(13) 0.0252(7) Uani 1 1 d . . . . .
C4 C 0.10529(16) 0.20614(16) 0.08674(14) 0.0267(7) Uani 1 1 d . . . . .
C5 C 0.22997(16) 0.22148(16) -0.07670(13) 0.0282(7) Uani 1 1 d . . . . .
H5A H 0.227655 0.219350 -0.120190 0.034 Uiso 1 1 calc R U . . .
H5B H 0.273095 0.262417 -0.065751 0.034 Uiso 1 1 calc R U . . .
C6 C 0.21664(16) 0.20831(16) 0.08036(13) 0.0282(7) Uani 1 1 d . . . . .
H6A H 0.260439 0.250844 0.075398 0.034 Uiso 1 1 calc DR U . . .
H6B H 0.208131 0.199908 0.123082 0.034 Uiso 1 1 calc R U . . .
N1 N 0.07000(13) 0.22187(13) -0.05387(11) 0.0266(6) Uani 1 1 d . . . . .
N2 N 0.17354(13) 0.22924(14) -0.05473(11) 0.0281(6) Uani 1 1 d . . . . .
N3 N 0.07010(14) 0.23152(14) 0.05484(11) 0.0281(6) Uani 1 1 d . . . . .
N4 N 0.16184(13) 0.21718(13) 0.05402(11) 0.0271(6) Uani 1 1 d . . . . .
O1 O 0.09745(12) 0.17328(14) -0.13268(10) 0.0387(6) Uani 1 1 d . . . . .
O2 O 0.08841(12) 0.17752(13) 0.13548(10) 0.0372(6) Uani 1 1 d . . . . .
O3 O 0.11188(13) 0.32862(12) -0.00375(11) 0.0367(6) Uani 1 1 d . . . . .
H3 H 0.131123 0.347081 -0.035343 0.055 Uiso 1 1 calc R U . . .
O4 O 0.23222(12) 0.32357(12) 0.01195(11) 0.0383(6) Uani 1 1 d . . . . .
H4 H 0.266510 0.319476 0.007789 0.057 Uiso 1 1 calc DR 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 O1 1.214(4) . ?
C1 N1 1.368(4) . ?
C1 N2 1.384(4) . ?
C2 O3 1.382(4) . ?
C2 N3 1.434(4) . ?
C2 N1 1.458(4) . ?
C2 C3 1.581(4) . ?
C3 O4 1.389(4) . ?
C3 N2 1.445(4) . ?
C3 N4 1.440(4) . ?
C4 O2 1.220(4) . ?
C4 N4 1.369(4) . ?
C4 N3 1.374(4) . ?
C5 N3 1.443(4) 20 ?
C5 N2 1.440(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.447(4) 20 ?
C6 N4 1.456(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
O3 H3 0.8200 . ?
O4 H4 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 126.0(3) . . ?
O1 C1 N2 125.5(3) . . ?
N1 C1 N2 108.5(2) . . ?
O3 C2 N3 108.8(2) . . ?
O3 C2 N1 112.3(2) . . ?
N3 C2 N1 114.3(2) . . ?
O3 C2 C3 115.7(2) . . ?
N3 C2 C3 103.2(2) . . ?
N1 C2 C3 102.3(2) . . ?
O4 C3 N2 113.1(2) . . ?
O4 C3 N4 108.2(2) . . ?
N2 C3 N4 115.3(2) . . ?
O4 C3 C2 114.5(2) . . ?
N2 C3 C2 103.1(2) . . ?
N4 C3 C2 102.2(2) . . ?
O2 C4 N4 125.7(3) . . ?
O2 C4 N3 125.8(3) . . ?
N4 C4 N3 108.4(3) . . ?
N3 C5 N2 115.2(2) 20 . ?
N3 C5 H5A 108.5 20 . ?
N2 C5 H5A 108.5 . . ?
N3 C5 H5B 108.5 20 . ?
N2 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N1 C6 N4 113.1(2) 20 . ?
N1 C6 H6A 109.0 20 . ?
N4 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 20 . ?
N4 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C1 N1 C6 121.5(2) . 21 ?
C1 N1 C2 112.7(2) . . ?
C6 N1 C2 123.6(2) 21 . ?
C1 N2 C3 112.2(2) . . ?
C1 N2 C5 122.8(2) . . ?
C3 N2 C5 124.9(2) . . ?
C4 N3 C2 112.4(2) . . ?
C4 N3 C5 123.4(3) . 21 ?
C2 N3 C5 124.1(2) . 21 ?
C4 N4 C3 112.6(2) . . ?
C4 N4 C6 121.5(3) . . ?
C3 N4 C6 122.4(2) . . ?
C2 O3 H3 109.5 . . ?
C3 O4 H4 109.5 . . ?

_refine_diff_density_max         0.972
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.084



