# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_rgtm29m
_database_code_depnum_ccdc_archive 'CCDC 1902619'
loop_
_audit_author_name
_audit_author_address
'Rakesh Ganguly'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H50 N10 Na2 Ni O24 S2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1031.55

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1407(3)
_cell_length_b                   8.7295(3)
_cell_length_c                   15.6983(5)
_cell_angle_alpha                78.8978(11)
_cell_angle_beta                 79.5625(10)
_cell_angle_gamma                88.0006(11)
_cell_volume                     1076.60(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    408
_cell_measurement_theta_min      2.3568
_cell_measurement_theta_max      29.7054
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538

_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.96

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            24096
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_full        31.11
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
;

_reflns_number_total             6860
_reflns_number_gt                5782
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0920
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.037
_refine_ls_number_reflns         6860
_refine_ls_number_parameters     335
_refine_ls_number_restraints     48
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)²+0.8396P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.432
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2018)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2018)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2018)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2018)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.5 0.5 1.0 0.00983(7) Uani d . P S 1.0 . .
Na Na1 0.63474(8) 0.01399(7) 0.57720(4) 0.01438(13) Uani d . . D 1.0 . .
C C1 0.39992(19) 0.18131(17) 0.94847(10) 0.0111(3) Uani d . . . 1.0 . .
C C2 0.52518(18) 0.27532(17) 0.88801(10) 0.0107(3) Uani d . . . 1.0 . .
C C3 0.7322(2) 0.31234(19) 0.74913(10) 0.0154(3) Uani d . . . 1.0 . .
H H3A 0.774127 0.255176 0.70165 0.023 Uiso calc U . R 1.0 . .
H H3B 0.824259 0.331689 0.778165 0.023 Uiso calc U . R 1.0 . .
H H3C 0.68464 0.412167 0.724408 0.023 Uiso calc U . R 1.0 . .
C C4 0.5594(2) 0.07924(18) 0.79518(10) 0.0132(3) Uani d . . . 1.0 . .
C C5 0.4004(2) -0.16252(19) 0.83632(11) 0.0179(3) Uani d . . . 1.0 . .
H H5A 0.35626 -0.234853 0.891014 0.027 Uiso calc U . R 1.0 . .
H H5B 0.501072 -0.207201 0.805816 0.027 Uiso calc U . R 1.0 . .
H H5C 0.316026 -0.1451 0.798162 0.027 Uiso calc U . R 1.0 . .
C C6 0.35858(19) 0.02920(18) 0.93426(10) 0.0121(3) Uani d . . . 1.0 . .
C C7 0.16862(19) 0.39615(18) 1.09811(10) 0.0115(3) Uani d . . . 1.0 . .
C C8 0.08109(19) 0.53577(18) 1.08060(10) 0.0132(3) Uani d . . . 1.0 . .
H H8 0.117435 0.610265 1.028391 0.016 Uiso calc U . R 1.0 . .
C C9 -0.05950(19) 0.56498(18) 1.14005(10) 0.0135(3) Uani d . . . 1.0 . .
H H9 -0.120855 0.65892 1.128318 0.016 Uiso calc U . R 1.0 . .
C C10 -0.10989(19) 0.45588(18) 1.21685(10) 0.0119(3) Uani d . . . 1.0 . .
C C11 -0.0192(2) 0.31940(18) 1.23534(10) 0.0146(3) Uani d . . . 1.0 . .
H H11 -0.052699 0.247048 1.288803 0.018 Uiso calc U . R 1.0 . .
C C12 0.1200(2) 0.28884(18) 1.17573(10) 0.0141(3) Uani d . . . 1.0 . .
H H12 0.181769 0.195239 1.187876 0.017 Uiso calc U . R 1.0 . .
N N1 0.31241(16) 0.36541(15) 1.03438(8) 0.0110(2) Uani d . . . 1.0 . .
N N2 0.29508(16) 0.23088(15) 1.01391(8) 0.0113(2) Uani d . . . 1.0 . .
N N3 0.56367(17) 0.41123(16) 0.90076(9) 0.0132(2) Uani d . . . 1.0 . .
H H3 0.626(3) 0.462(3) 0.8560(15) 0.02 Uiso d U . . 1.0 . .
N N4 0.60267(16) 0.21950(15) 0.81378(8) 0.0119(2) Uani d . . . 1.0 . .
N N5 0.44227(17) -0.01286(15) 0.85728(9) 0.0134(2) Uani d . . . 1.0 . .
O O3 -0.43278(14) 0.43147(14) 1.26200(8) 0.0161(2) Uani d . . . 1.0 . .
O O4 -0.26989(15) 0.40167(15) 1.37757(8) 0.0194(2) Uani d . . . 1.0 . .
O O5 -0.30039(15) 0.65790(13) 1.28845(8) 0.0186(2) Uani d . . . 1.0 . .
O O6 0.25501(15) -0.06093(13) 0.98452(8) 0.0162(2) Uani d . . . 1.0 . .
O O7 0.62432(16) 0.03546(14) 0.72779(8) 0.0186(2) Uani d . . . 1.0 . .
O O8A 0.6979(12) -0.2510(9) 0.6152(9) 0.0297(18) Uani d U P D 0.41(2) A 1
H H8AA 0.60833 -0.326765 0.633091 0.045 Uiso d U P R 0.41(2) A 1
H H8AB 0.749785 -0.276456 0.666483 0.045 Uiso d U P R 0.41(2) A 1
O O9A 0.4923(12) 0.2513(10) 0.5565(7) 0.0272(15) Uani d U P D 0.41(2) A 1
H H9AA 0.551228 0.319893 0.514665 0.041 Uiso d U P R 0.41(2) A 1
H H9AB 0.483216 0.293312 0.603867 0.041 Uiso d U P R 0.41(2) A 1
O O8B 0.6713(8) -0.2599(6) 0.5909(4) 0.0197(9) Uani d U P D 0.59(2) A 2
H H8BA 0.624033 -0.314283 0.646191 0.029 Uiso d U P R 0.59(2) A 2
H H8BB 0.781528 -0.290743 0.587365 0.029 Uiso d U P R 0.59(2) A 2
O O9B 0.5419(13) 0.2733(8) 0.5617(4) 0.0315(14) Uani d U P D 0.59(2) A 2
H H9BA 0.607003 0.335652 0.581327 0.047 Uiso d U P R 0.59(2) A 2
H H9BB 0.442219 0.27926 0.597027 0.047 Uiso d U P R 0.59(2) A 2
O O10 0.92291(16) 0.08891(17) 0.56005(9) 0.0226(3) Uani d . . D 1.0 . .
H H10 0.954487 0.076774 0.612437 0.034 Uiso d U . DR 1.0 . .
H H10A 0.949996 0.194834 0.526123 0.034 Uiso d U P DR 0.53(3) B 1
H H10B 0.950219 0.012867 0.532032 0.038(17) Uiso d . P DR 0.47(3) B 2
O O11 0.65282(16) 0.07064(15) 0.41778(8) 0.0173(2) Uani d . . . 1.0 . .
H H11A 0.716(3) 0.028(3) 0.3824(16) 0.026 Uiso d U . . 1.0 . .
H H11B 0.678(3) 0.161(3) 0.4019(16) 0.026 Uiso d U . . 1.0 . .
O O12 0.00154(17) 0.96984(16) 0.12519(8) 0.0226(3) Uani d . . G 1.0 . .
H H12A 0.097126 0.966673 0.090213 0.034 Uiso d U . G 1.0 . .
H H12B -0.067753 1.027867 0.096881 0.034 Uiso d U . G 1.0 . .
O O13 0.88771(16) 0.91464(15) 0.30393(8) 0.0177(2) Uani d . . . 1.0 . .
H H13A 0.930(3) 0.942(3) 0.2523(17) 0.027 Uiso d U . . 1.0 . .
H H13B 0.842(3) 0.829(3) 0.3075(16) 0.027 Uiso d U . . 1.0 . .
O O14 1.00511(17) 0.37761(17) 0.45723(9) 0.0256(3) Uani d . . DG 1.0 . .
H H14 0.916492 0.395945 0.433147 0.038 Uiso d U . DG 1.0 . .
H H14A 1.019875 0.462665 0.47608 0.038 Uiso d U P DG 0.53(3) B 1
H H14B 0.973968 0.275804 0.501926 0.038 Uiso d U P DG 0.47(3) B 2
S S1 -0.29246(5) 0.49008(4) 1.29172(2) 0.01173(8) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N3 2_667 1.8548(12) ?
Ni1 N3 . 1.8548(12) ?
Ni1 N1 2_667 1.8937(13) ?
Ni1 N1 . 1.8937(13) ?
Na1 O9A . 2.335(8) ?
Na1 O8A . 2.338(7) ?
Na1 O9B . 2.343(5) ?
Na1 O8B . 2.372(5) ?
Na1 O7 . 2.3933(13) ?
Na1 O10 . 2.4112(14) ?
Na1 O11 . 2.4339(14) ?
Na1 O11 2_656 2.4624(14) ?
Na1 Na1 2_656 3.5970(13) ?
C1 N2 . 1.3412(18) ?
C1 C2 . 1.422(2) ?
C1 C6 . 1.449(2) ?
C2 N3 . 1.299(2) ?
C2 N4 . 1.3871(18) ?
C3 N4 . 1.468(2) ?
C4 O7 . 1.2181(18) ?
C4 N4 . 1.3834(19) ?
C4 N5 . 1.386(2) ?
C5 N5 . 1.4726(19) ?
C6 O6 . 1.232(2) ?
C6 N5 . 1.3836(19) ?
C7 C12 . 1.389(2) ?
C7 C8 . 1.396(2) ?
C7 N1 . 1.4493(18) ?
C8 C9 . 1.389(2) ?
C9 C10 . 1.391(2) ?
C10 C11 . 1.390(2) ?
C10 S1 . 1.7751(15) ?
C11 C12 . 1.387(2) ?
N1 N2 . 1.2944(17) ?
O3 S1 . 1.4526(12) ?
O4 S1 . 1.4577(13) ?
O5 S1 . 1.4555(12) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Ni1 N3 2_667 . 180.0 ?
N3 Ni1 N1 2_667 2_667 89.16(6) ?
N3 Ni1 N1 . 2_667 90.84(6) ?
N3 Ni1 N1 2_667 . 90.84(6) ?
N3 Ni1 N1 . . 89.16(6) ?
N1 Ni1 N1 2_667 . 180.0 ?
O9A Na1 O8A . . 163.1(3) ?
O9B Na1 O8B . . 168.2(2) ?
O9A Na1 O7 . . 88.5(3) ?
O8A Na1 O7 . . 88.8(4) ?
O9B Na1 O7 . . 83.81(17) ?
O8B Na1 O7 . . 99.24(16) ?
O9A Na1 O10 . . 104.0(3) ?
O8A Na1 O10 . . 92.3(3) ?
O9B Na1 O10 . . 92.8(3) ?
O8B Na1 O10 . . 98.89(16) ?
O7 Na1 O10 . . 84.06(5) ?
O9A Na1 O11 . . 78.4(3) ?
O8A Na1 O11 . . 106.4(4) ?
O9B Na1 O11 . . 81.56(16) ?
O8B Na1 O11 . . 96.37(16) ?
O7 Na1 O11 . . 164.02(5) ?
O10 Na1 O11 . . 90.25(5) ?
O9A Na1 O11 . 2_656 77.8(2) ?
O8A Na1 O11 . 2_656 86.4(3) ?
O9B Na1 O11 . 2_656 89.3(3) ?
O8B Na1 O11 . 2_656 78.95(16) ?
O7 Na1 O11 . 2_656 100.80(5) ?
O10 Na1 O11 . 2_656 174.92(5) ?
O11 Na1 O11 . 2_656 85.45(5) ?
O9A Na1 Na1 . 2_656 73.7(3) ?
O8A Na1 Na1 . 2_656 98.5(4) ?
O7 Na1 Na1 . 2_656 141.15(5) ?
O10 Na1 Na1 . 2_656 133.22(4) ?
O11 Na1 Na1 . 2_656 43.03(3) ?
O11 Na1 Na1 2_656 2_656 42.41(3) ?
N2 C1 C2 . . 124.47(13) ?
N2 C1 C6 . . 114.04(14) ?
C2 C1 C6 . . 120.78(13) ?
N3 C2 N4 . . 120.76(14) ?
N3 C2 C1 . . 121.05(13) ?
N4 C2 C1 . . 118.17(13) ?
O7 C4 N4 . . 121.60(15) ?
O7 C4 N5 . . 120.72(14) ?
N4 C4 N5 . . 117.66(13) ?
O6 C6 N5 . . 119.42(14) ?
O6 C6 C1 . . 124.81(13) ?
N5 C6 C1 . . 115.77(14) ?
C12 C7 C8 . . 120.70(13) ?
C12 C7 N1 . . 120.35(13) ?
C8 C7 N1 . . 118.94(14) ?
C9 C8 C7 . . 119.55(15) ?
C8 C9 C10 . . 119.61(14) ?
C11 C10 C9 . . 120.61(14) ?
C11 C10 S1 . . 119.53(12) ?
C9 C10 S1 . . 119.86(11) ?
C12 C11 C10 . . 119.99(15) ?
C11 C12 C7 . . 119.49(14) ?
N2 N1 C7 . . 109.47(12) ?
N2 N1 Ni1 . . 128.20(10) ?
C7 N1 Ni1 . . 122.04(9) ?
N1 N2 C1 . . 122.03(13) ?
C2 N3 Ni1 . . 128.87(12) ?
C4 N4 C2 . . 122.70(14) ?
C4 N4 C3 . . 116.94(12) ?
C2 N4 C3 . . 120.32(13) ?
C6 N5 C4 . . 124.72(13) ?
C6 N5 C5 . . 118.74(14) ?
C4 N5 C5 . . 116.47(12) ?
C4 O7 Na1 . . 152.35(11) ?
Na1 O11 Na1 . 2_656 94.55(5) ?
O3 S1 O5 . . 112.80(7) ?
O3 S1 O4 . . 111.44(8) ?
O5 S1 O4 . . 113.04(7) ?
O3 S1 C10 . . 106.93(7) ?
O5 S1 C10 . . 106.30(7) ?
O4 S1 C10 . . 105.73(7) ?


# start Validation Reply Form
_vrf_PLAT420_rgtm29m             
;
PROBLEM: D-H Without Acceptor       O9B      --H9BA     .     Please Check 
RESPONSE: The aqua oxygen atom is disordered and the H-atoms are at the 
caluulated positions.
The H3 of Nitrogen atom is at the postion found by the difference map.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_rgtm31a
_database_code_depnum_ccdc_archive 'CCDC 1902621'
loop_
_audit_author_name
_audit_author_address
'Rakesh Ganguly'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H36 K2 N10 O15.25 S2'
_chemical_formula_weight         850.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   35.2528(6)
_cell_length_b                   15.7804(3)
_cell_length_c                   13.0890(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.9540(10)
_cell_angle_gamma                90
_cell_volume                     6844.3(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      30.89

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             3536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59393
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.341
_diffrn_reflns_theta_max         30.987
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10864
_reflns_number_gt                7663
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0341P)²+14.0119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10864
_refine_ls_number_parameters     602
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.0960
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_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
S1 S 0.06175(9) 0.53099(15) 0.3854(2) 0.0157(4) Uani 0.5 1 d D . P A 1
O1 O 0.0429(2) 0.4960(5) 0.4590(5) 0.0287(17) Uani 0.5 1 d D . P A 1
O2 O 0.05973(15) 0.6234(3) 0.3822(4) 0.0294(11) Uani 0.5 1 d D . P A 1
O3 O 0.0482(2) 0.4907(4) 0.2805(5) 0.0198(10) Uani 0.5 1 d D . P A 1
S1A S 0.05906(9) 0.51044(16) 0.3623(2) 0.0160(4) Uani 0.5 1 d D . P A 2
O1A O 0.0384(2) 0.4788(5) 0.4339(5) 0.0202(12) Uani 0.5 1 d D . P A 2
O2A O 0.05429(14) 0.6017(3) 0.3463(3) 0.0211(9) Uani 0.5 1 d D . P A 2
O3A O 0.0472(2) 0.4659(4) 0.2578(5) 0.0200(10) Uani 0.5 1 d D . P A 2
C1 C 0.11273(6) 0.49839(14) 0.43508(18) 0.0234(4) Uani 1 1 d . . . . .
C2 C 0.14105(6) 0.56282(14) 0.46160(18) 0.0241(4) Uani 1 1 d . . . . .
H2 H 0.132472 0.620097 0.448525 0.029 Uiso 1 1 calc R U . . .
C3 C 0.18199(6) 0.54439(13) 0.50726(17) 0.0203(4) Uani 1 1 d . . . . .
H3 H 0.201271 0.588934 0.525966 0.024 Uiso 1 1 calc R U . . .
C4 C 0.19455(6) 0.46047(13) 0.52540(16) 0.0177(4) Uani 1 1 d . . . . .
C5 C 0.16600(6) 0.39540(13) 0.49855(17) 0.0204(4) Uani 1 1 d . . . . .
H5 H 0.174617 0.338090 0.510702 0.025 Uiso 1 1 calc R U . . .
C6 C 0.12501(6) 0.41382(14) 0.45414(17) 0.0230(4) Uani 1 1 d . . . . .
H6 H 0.105612 0.369500 0.436964 0.028 Uiso 1 1 calc R U . . .
C7 C 0.30120(6) 0.47822(12) 0.63082(15) 0.0150(3) Uani 1 1 d . . . . .
C8 C 0.32674(6) 0.55126(12) 0.63995(15) 0.0164(4) Uani 1 1 d . . . . .
C9 C 0.38599(6) 0.45941(13) 0.71427(15) 0.0175(4) Uani 1 1 d . . . . .
C10 C 0.31898(6) 0.39814(12) 0.66505(15) 0.0158(4) Uani 1 1 d . . . . .
C11 C 0.39574(6) 0.60931(14) 0.69373(19) 0.0249(4) Uani 1 1 d . . . . .
H11A H 0.416597 0.607893 0.765958 0.037 Uiso 1 1 calc R U . . .
H11B H 0.380574 0.662457 0.684843 0.037 Uiso 1 1 calc R U . . .
H11C H 0.408467 0.605540 0.637998 0.037 Uiso 1 1 calc R U . . .
C12 C 0.37873(6) 0.30766(14) 0.74145(19) 0.0250(4) Uani 1 1 d . . . . .
H12A H 0.370891 0.287099 0.802048 0.037 Uiso 1 1 calc R U . . .
H12B H 0.408166 0.312921 0.765074 0.037 Uiso 1 1 calc R U . . .
H12C H 0.369504 0.267492 0.680866 0.037 Uiso 1 1 calc R U . . .
C13 C -0.40186(6) 0.36603(12) 0.01966(15) 0.0163(4) Uani 1 1 d . . . . .
C14 C -0.36663(6) 0.31810(13) 0.04604(16) 0.0192(4) Uani 1 1 d . . . . .
H14 H -0.368313 0.258169 0.039138 0.023 Uiso 1 1 calc R U . . .
C15 C -0.32927(6) 0.35693(12) 0.08215(16) 0.0187(4) Uani 1 1 d . . . . .
H15 H -0.305308 0.324103 0.099516 0.022 Uiso 1 1 calc R U . . .
C16 C -0.32714(6) 0.44516(12) 0.09283(15) 0.0154(4) Uani 1 1 d . . . . .
C17 C -0.36240(6) 0.49314(12) 0.06536(15) 0.0159(4) Uani 1 1 d . . . . .
H17 H -0.360786 0.553118 0.071521 0.019 Uiso 1 1 calc R U . . .
C18 C -0.40012(6) 0.45357(12) 0.02883(15) 0.0162(4) Uani 1 1 d . . . . .
H18 H -0.424181 0.486141 0.010571 0.019 Uiso 1 1 calc R U . . .
C19 C -0.22178(6) 0.48190(12) 0.19857(15) 0.0160(4) Uani 1 1 d . . . . .
C20 C -0.18849(6) 0.42411(12) 0.23747(16) 0.0177(4) Uani 1 1 d . . . . .
C21 C -0.14236(6) 0.54646(12) 0.27852(16) 0.0170(4) Uani 1 1 d . . . . .
C22 C -0.21467(6) 0.56993(12) 0.19649(15) 0.0160(4) Uani 1 1 d . . . . .
C23 C -0.11546(6) 0.40347(13) 0.32228(19) 0.0243(4) Uani 1 1 d . . . . .
H23A H -0.108641 0.377444 0.262794 0.036 Uiso 1 1 calc R U . . .
H23B H -0.122330 0.359083 0.365355 0.036 Uiso 1 1 calc R U . . .
H23C H -0.092270 0.435874 0.368773 0.036 Uiso 1 1 calc R U . . .
C24 C -0.16789(6) 0.68948(13) 0.22449(19) 0.0231(4) Uani 1 1 d . . . . .
H24A H -0.178470 0.705805 0.147677 0.035 Uiso 1 1 calc R U . . .
H24B H -0.138739 0.699876 0.253336 0.035 Uiso 1 1 calc R U . . .
H24C H -0.181191 0.723089 0.265456 0.035 Uiso 1 1 calc R U . . .
K1 K -0.02875(2) 0.60532(3) 0.39523(4) 0.02151(10) Uani 1 1 d D . . . .
K2 K -0.0089(2) 0.6583(2) 0.7715(6) 0.0183(9) Uani 0.332(17) 1 d D U P A 1
K2A K 0.000000 0.6541(4) 0.750000 0.027(4) Uani 0.34(3) 2 d DS TU P A 2
K3 K 0.500000 0.46670(4) 0.750000 0.02534(14) Uani 1 2 d DS T P . .
N1 N 0.23565(5) 0.43405(11) 0.57169(13) 0.0173(3) Uani 1 1 d . . . . .
N2 N 0.26070(5) 0.49566(10) 0.58674(13) 0.0160(3) Uani 1 1 d . . . . .
N3 N 0.36011(5) 0.39116(10) 0.70587(13) 0.0170(3) Uani 1 1 d . . . . .
N4 N 0.36815(5) 0.53744(11) 0.68234(13) 0.0176(3) Uani 1 1 d . . . . .
N5 N 0.29676(5) 0.32952(10) 0.65824(14) 0.0200(3) Uani 1 1 d . . . . .
H5A H 0.308457 0.280268 0.679798 0.024 Uiso 1 1 calc R U . . .
H5B H 0.270265 0.333082 0.632137 0.024 Uiso 1 1 calc R U . . .
N6 N -0.29027(5) 0.49105(10) 0.12798(13) 0.0171(3) Uani 1 1 d . . . . .
N7 N -0.25901(5) 0.44373(10) 0.16497(13) 0.0166(3) Uani 1 1 d . . . . .
N8 N -0.24421(5) 0.62485(11) 0.15885(14) 0.0201(3) Uani 1 1 d . . . . .
H8A H -0.238802 0.679286 0.158695 0.024 Uiso 1 1 calc R U . . .
H8B H -0.269384 0.607188 0.133812 0.024 Uiso 1 1 calc R U . . .
N9 N -0.15017(5) 0.46052(10) 0.27715(14) 0.0185(3) Uani 1 1 d . . . . .
N10 N -0.17576(5) 0.59912(10) 0.23499(13) 0.0169(3) Uani 1 1 d . . . . .
O4 O -0.48001(4) 0.37170(10) -0.06279(14) 0.0295(4) Uani 1 1 d . . . . .
O5 O -0.44540(5) 0.25134(12) -0.10493(15) 0.0375(4) Uani 1 1 d . . . . .
O6 O -0.44904(5) 0.26661(11) 0.07457(14) 0.0351(4) Uani 1 1 d . . . . .
O7 O 0.31396(4) 0.62379(9) 0.61200(12) 0.0220(3) Uani 1 1 d . . . . .
O8 O 0.42239(4) 0.45093(10) 0.74871(12) 0.0232(3) Uani 1 1 d . . . . .
O9 O -0.19173(4) 0.34619(9) 0.23964(13) 0.0227(3) Uani 1 1 d . . . . .
O10 O -0.10852(4) 0.57540(9) 0.31473(12) 0.0210(3) Uani 1 1 d . . . . .
O11 O -0.01894(12) 0.7553(2) 0.2517(4) 0.0521(11) Uani 0.5 1 d . . P A -1
O12 O 0.02874(17) 0.6764(4) 0.5917(4) 0.0650(16) Uani 0.5 1 d D U P A 1
O12A O 0.03805(15) 0.7039(3) 0.5637(4) 0.0476(13) Uani 0.5 1 d D U P A 2
O13 O 0.5225(4) 0.5899(5) 0.9164(7) 0.0304(18) Uani 0.5 1 d D U P B 1
H130 H 0.5070(14) 0.602(3) 0.946(5) 0.046 Uiso 0.5 1 d D U P C 1
H131 H 0.5348(17) 0.632(2) 0.916(6) 0.046 Uiso 0.5 1 d D U P D 1
O13A O 0.5177(6) 0.6034(7) 0.8894(11) 0.037(3) Uani 0.35 1 d D U P B 2
O13B O 0.5016(4) 0.6235(7) 0.8384(11) 0.030(3) Uani 0.15 1 d D U P B 3
O14 O 0.07463(11) 0.7548(2) 0.4700(3) 0.0316(8) Uani 0.5 1 d . . P . .
H140 H 0.0960(10) 0.763(2) 0.489(3) 0.047 Uiso 1 1 d D U . . .
H141 H 0.0665(9) 0.718(2) 0.430(3) 0.047 Uiso 1 1 d D U . . .
O15 O 0.16544(7) 0.77844(12) 0.54595(19) 0.0456(5) Uani 1 1 d D . . . .
H150 H 0.1724(10) 0.805(2) 0.504(2) 0.068 Uiso 1 1 d D U . . .
H151 H 0.1840(8) 0.749(2) 0.579(3) 0.068 Uiso 1 1 d D U . . .
O16 O 0.74781(5) 0.80263(10) 0.15200(16) 0.0312(4) Uani 1 1 d D . . . .
H160 H 0.7425(9) 0.8256(18) 0.200(2) 0.047 Uiso 1 1 d D U . . .
H161 H 0.7638(8) 0.8317(17) 0.137(2) 0.047 Uiso 1 1 d D U . . .
O17 O 0.9409(3) 0.8572(7) 0.9616(9) 0.072(3) Uani 0.25 1 d . . P . .
S2 S -0.44810(2) 0.30963(3) -0.02258(4) 0.01917(11) 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
S1 O3 1.438(5) . ?
S1 O1 1.455(8) . ?
S1 O2 1.460(5) . ?
S1 C1 1.767(4) . ?
S1 K1 3.443(3) . ?
S1 K1 3.647(3) 2 ?
S1 K2 3.742(6) 5_566 ?
O1 K1 2.662(8) 5_566 ?
O1 K1 2.934(9) . ?
O2 K1 3.194(5) . ?
O2 K1 3.429(5) 2 ?
O3 K2 2.697(7) 5_566 ?
O3 K1 2.820(7) 2 ?
O3 K2 3.072(9) 6_565 ?
S1A O2A 1.457(5) . ?
S1A O1A 1.458(7) . ?
S1A O3A 1.467(5) . ?
S1A C1 1.815(4) . ?
S1A K2A 3.339(6) 5_566 ?
S1A K1 3.506(3) 2 ?
S1A K1 3.594(3) . ?
O1A K1 2.719(7) 5_566 ?
O1A K1 3.004(8) . ?
O1A K2A 3.131(8) 5_566 ?
O2A K1 2.978(4) 2 ?
O2A K1 3.203(5) . ?
O3A K2A 2.500(8) 5_566 ?
O3A K1 2.897(8) 2 ?
C1 C2 1.383(3) . ?
C1 C6 1.399(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(3) . ?
C4 N1 1.428(2) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N2 1.373(2) . ?
C7 C10 1.414(3) . ?
C7 C8 1.442(3) . ?
C8 O7 1.239(2) . ?
C8 N4 1.391(2) . ?
C9 O8 1.214(2) . ?
C9 N4 1.381(3) . ?
C9 N3 1.391(3) . ?
C10 N5 1.322(2) . ?
C10 N3 1.368(2) . ?
C11 N4 1.468(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.475(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.386(3) . ?
C13 C14 1.393(3) . ?
C13 S2 1.772(2) . ?
C14 C15 1.382(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(3) . ?
C16 N6 1.420(2) . ?
C17 C18 1.397(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 N7 1.373(2) . ?
C19 C22 1.414(3) . ?
C19 C20 1.435(3) . ?
C20 O9 1.236(2) . ?
C20 N9 1.395(2) . ?
C21 O10 1.212(2) . ?
C21 N9 1.383(3) . ?
C21 N10 1.394(2) . ?
C22 N8 1.314(2) . ?
C22 N10 1.370(2) . ?
C23 N9 1.471(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N10 1.468(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
K1 O10 2.6867(14) . ?
K1 O6 2.7310(17) 4_455 ?
K1 O12 2.902(6) . ?
K1 O12A 3.047(5) . ?
K1 O11 3.113(5) . ?
K2 K2 0.976(17) 2_556 ?
K2 O12 2.152(11) 2_556 ?
K2 O5 2.666(6) 4_455 ?
K2 O5 2.703(6) 3_556 ?
K2 O12 3.085(10) . ?
K2 S2 3.690(6) 3_556 ?
K2A O5 2.678(4) 3_556 ?
K2A O5 2.678(4) 4_455 ?
K2A O12A 3.255(5) . ?
K2A O12A 3.255(5) 2_556 ?
K3 O13B 2.724(10) . ?
K3 O13B 2.724(10) 2_656 ?
K3 O8 2.7417(14) . ?
K3 O8 2.7417(14) 2_656 ?
K3 O4 2.7514(17) 2 ?
K3 O4 2.7514(17) 1_656 ?
K3 O13A 2.755(11) . ?
K3 O13A 2.755(11) 2_656 ?
K3 O13 2.823(7) 2_656 ?
K3 O13 2.823(7) . ?
N1 N2 1.283(2) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 N7 1.282(2) . ?
N8 H8A 0.8800 . ?
N8 H8B 0.8800 . ?
O4 S2 1.4482(16) . ?
O5 S2 1.4448(17) . ?
O6 S2 1.4517(17) . ?
O13 H130 0.80(2) . ?
O13 H131 0.80(2) . ?
O14 H140 0.72(3) . ?
O14 H141 0.77(3) . ?
O15 H150 0.791(18) . ?
O15 H151 0.798(18) . ?
O16 H160 0.797(17) . ?
O16 H161 0.798(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
O3 S1 O1 112.7(4) . . ?
O3 S1 O2 114.7(4) . . ?
O1 S1 O2 111.7(4) . . ?
O3 S1 C1 100.8(3) . . ?
O1 S1 C1 106.5(4) . . ?
O2 S1 C1 109.6(3) . . ?
O3 S1 K1 100.2(3) . . ?
O1 S1 K1 57.7(4) . . ?
O2 S1 K1 67.9(2) . . ?
C1 S1 K1 157.64(16) . . ?
O3 S1 K1 45.0(3) . 2 ?
O1 S1 K1 136.8(3) . 2 ?
O2 S1 K1 69.8(2) . 2 ?
C1 S1 K1 113.54(15) . 2 ?
K1 S1 K1 86.97(7) . 2 ?
O3 S1 K2 35.2(3) . 5_566 ?
O1 S1 K2 78.8(3) . 5_566 ?
O2 S1 K2 140.5(3) . 5_566 ?
C1 S1 K2 102.90(16) . 5_566 ?
K1 S1 K2 89.90(14) . 5_566 ?
K1 S1 K2 77.06(11) 2 5_566 ?
S1 O1 K1 160.5(5) . 5_566 ?
S1 O1 K1 97.6(4) . . ?
K1 O1 K1 101.8(3) 5_566 . ?
S1 O2 K1 87.0(2) . . ?
S1 O2 K1 86.6(2) . 2 ?
K1 O2 K1 94.88(12) . 2 ?
S1 O3 K2 127.0(4) . 5_566 ?
S1 O3 K1 113.8(4) . 2 ?
K2 O3 K1 113.1(2) 5_566 2 ?
S1 O3 K2 112.0(4) . 6_565 ?
K2 O3 K2 18.0(3) 5_566 6_565 ?
K1 O3 K2 119.1(2) 2 6_565 ?
O2A S1A O1A 111.9(4) . . ?
O2A S1A O3A 111.0(4) . . ?
O1A S1A O3A 112.9(4) . . ?
O2A S1A C1 103.2(2) . . ?
O1A S1A C1 106.7(3) . . ?
O3A S1A C1 110.7(3) . . ?
C1 S1A K2A 122.10(15) . 5_566 ?
C1 S1A K1 118.06(15) . 2 ?
O2A S1A K1 62.8(2) . . ?
O1A S1A K1 54.9(3) . . ?
O3A S1A K1 109.2(3) . . ?
C1 S1A K1 140.10(12) . . ?
K2A S1A K1 86.76(9) 5_566 . ?
K1 S1A K1 86.85(7) 2 . ?
S1A O1A K1 101.6(4) . . ?
K1 O1A K1 98.7(2) 5_566 . ?
K1 O1A K2A 99.4(2) 5_566 5_566 ?
K1 O1A K2A 101.9(2) . 5_566 ?
S1A O2A K1 93.3(2) . . ?
K1 O2A K1 104.24(13) 2 . ?
C2 C1 C6 120.23(19) . . ?
C2 C1 S1 115.77(18) . . ?
C6 C1 S1 123.89(18) . . ?
C2 C1 S1A 126.05(18) . . ?
C6 C1 S1A 113.41(18) . . ?
C1 C2 C3 120.5(2) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.80(18) . . ?
C3 C4 N1 124.62(18) . . ?
C5 C4 N1 115.58(17) . . ?
C6 C5 C4 120.53(19) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C1 C6 H6 120.4 . . ?
N2 C7 C10 126.68(17) . . ?
N2 C7 C8 113.88(16) . . ?
C10 C7 C8 119.43(17) . . ?
O7 C8 N4 119.29(18) . . ?
O7 C8 C7 124.07(18) . . ?
N4 C8 C7 116.63(17) . . ?
O8 C9 N4 121.69(19) . . ?
O8 C9 N3 121.72(19) . . ?
N4 C9 N3 116.59(17) . . ?
N5 C10 N3 119.02(17) . . ?
N5 C10 C7 121.50(17) . . ?
N3 C10 C7 119.47(17) . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 120.67(18) . . ?
C18 C13 S2 122.43(15) . . ?
C14 C13 S2 116.88(15) . . ?
C15 C14 C13 120.61(18) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.21(18) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 120.15(18) . . ?
C17 C16 N6 116.33(17) . . ?
C15 C16 N6 123.49(17) . . ?
C16 C17 C18 120.41(18) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 118.94(18) . . ?
C13 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
N7 C19 C22 125.54(17) . . ?
N7 C19 C20 114.30(17) . . ?
C22 C19 C20 120.16(17) . . ?
O9 C20 N9 119.11(18) . . ?
O9 C20 C19 124.70(18) . . ?
N9 C20 C19 116.17(17) . . ?
O10 C21 N9 122.64(18) . . ?
O10 C21 N10 121.08(18) . . ?
N9 C21 N10 116.28(16) . . ?
N8 C22 N10 118.81(17) . . ?
N8 C22 C19 122.16(18) . . ?
N10 C22 C19 119.03(17) . . ?
N9 C23 H23A 109.5 . . ?
N9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N9 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N10 C24 H24A 109.5 . . ?
N10 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N10 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 K1 O10 75.47(16) 5_566 . ?
O1 K1 O1A 8.7(2) 5_566 5_566 ?
O10 K1 O1A 80.16(15) . 5_566 ?
O1 K1 O6 108.84(18) 5_566 4_455 ?
O10 K1 O6 84.68(5) . 4_455 ?
O1 K1 O3 98.43(18) 5_566 2 ?
O10 K1 O3 68.71(14) . 2 ?
O6 K1 O3 135.54(11) 4_455 2 ?
O1 K1 O3A 89.23(18) 5_566 2 ?
O10 K1 O3A 68.72(14) . 2 ?
O6 K1 O3A 143.16(12) 4_455 2 ?
O3 K1 O3A 9.64(10) 2 2 ?
O1 K1 O12 80.92(19) 5_566 . ?
O10 K1 O12 137.44(12) . . ?
O6 K1 O12 70.08(12) 4_455 . ?
O3 K1 O12 150.74(17) 2 . ?
O1 K1 O1 78.2(3) 5_566 . ?
O10 K1 O1 133.78(15) . . ?
O6 K1 O1 140.19(14) 4_455 . ?
O3 K1 O1 78.53(17) 2 . ?
O12 K1 O1 72.68(17) . . ?
O1 K1 O2A 133.37(17) 5_566 2 ?
O10 K1 O2A 71.55(10) . 2 ?
O6 K1 O2A 100.00(9) 4_455 2 ?
O3 K1 O2A 38.80(12) 2 2 ?
O12 K1 O2A 144.56(16) . 2 ?
O1 K1 O2A 102.13(16) . 2 ?
O10 K1 O1A 127.46(14) . . ?
O1A K1 O1A 81.3(2) 5_566 . ?
O6 K1 O1A 147.47(14) 4_455 . ?
O3A K1 O1A 65.79(17) 2 . ?
O2A K1 O1A 95.84(15) 2 . ?
O10 K1 O12A 145.14(12) . . ?
O1A K1 O12A 86.36(16) 5_566 . ?
O6 K1 O12A 66.94(12) 4_455 . ?
O3A K1 O12A 145.51(18) 2 . ?
O2A K1 O12A 131.08(13) 2 . ?
O1A K1 O12A 81.22(17) . . ?
O1 K1 O11 167.18(19) 5_566 . ?
O10 K1 O11 102.35(8) . . ?
O6 K1 O11 58.35(9) 4_455 . ?
O3 K1 O11 92.37(12) 2 . ?
O12 K1 O11 93.03(15) . . ?
O1 K1 O11 110.91(18) . . ?
K2 K2 O12 159.4(9) 2_556 2_556 ?
K2 K2 O5 81.7(7) 2_556 4_455 ?
O12 K2 O5 109.3(3) 2_556 4_455 ?
K2 K2 O3 103.3(4) 2_556 5_566 ?
O12 K2 O3 92.3(3) 2_556 5_566 ?
O5 K2 O3 99.1(3) 4_455 5_566 ?
K2 K2 O5 77.4(6) 2_556 3_556 ?
O12 K2 O5 82.4(3) 2_556 3_556 ?
O5 K2 O5 109.65(17) 4_455 3_556 ?
O3 K2 O5 150.9(3) 5_566 3_556 ?
K2 K2 O3 58.7(4) 2_556 6_566 ?
O12 K2 O3 117.7(3) 2_556 6_566 ?
O5 K2 O3 131.2(3) 4_455 6_566 ?
O3 K2 O3 67.4(3) 5_566 6_566 ?
O5 K2 O3 89.7(2) 3_556 6_566 ?
K2 K2 O12 14.2(6) 2_556 . ?
O12 K2 O12 165.7(3) 2_556 . ?
O5 K2 O12 67.8(2) 4_455 . ?
O3 K2 O12 101.9(3) 5_566 . ?
O5 K2 O12 85.5(2) 3_556 . ?
O3 K2 O12 69.7(2) 6_566 . ?
K2 K2 S2 95.4(6) 2_556 3_556 ?
O12 K2 S2 65.1(2) 2_556 3_556 ?
O5 K2 S2 106.22(12) 4_455 3_556 ?
O3 K2 S2 150.4(3) 5_566 3_556 ?
O5 K2 S2 19.25(7) 3_556 3_556 ?
O3 K2 S2 105.0(2) 6_566 3_556 ?
O12 K2 S2 101.8(2) . 3_556 ?
K2 K2 S1 88.9(5) 2_556 5_566 ?
O12 K2 S1 108.7(3) 2_556 5_566 ?
O5 K2 S1 86.67(18) 4_455 5_566 ?
O3 K2 S1 17.88(15) 5_566 5_566 ?
O5 K2 S1 156.5(3) 3_556 5_566 ?
O3 K2 S1 66.84(17) 6_566 5_566 ?
O12 K2 S1 85.3(2) . 5_566 ?
S2 K2 S1 166.85(18) 3_556 5_566 ?
K2 K2 K1 124.4(8) 2_556 2_556 ?
O12 K2 K1 40.3(2) 2_556 2_556 ?
O5 K2 K1 148.2(3) 4_455 2_556 ?
O3 K2 K1 92.4(2) 5_566 2_556 ?
O5 K2 K1 65.30(15) 3_556 2_556 ?
O3 K2 K1 80.60(16) 6_566 2_556 ?
O12 K2 K1 138.4(2) . 2_556 ?
S2 K2 K1 57.99(10) 3_556 2_556 ?
S1 K2 K1 109.49(13) 5_566 2_556 ?
K2 K2 K1 114.08(15) 2_556 6_566 ?
O12 K2 K1 72.3(2) 2_556 6_566 ?
O5 K2 K1 131.54(19) 4_455 6_566 ?
O3 K2 K1 34.30(16) 5_566 6_566 ?
O5 K2 K1 118.34(18) 3_556 6_566 ?
O3 K2 K1 58.06(12) 6_566 6_566 ?
O12 K2 K1 120.6(2) . 6_566 ?
S2 K2 K1 116.62(16) 3_556 6_566 ?
S1 K2 K1 50.54(7) 5_566 6_566 ?
K1 K2 K1 59.03(8) 2_556 6_566 ?
K2 K2 K1 46.0(7) 2_556 . ?
O12 K2 K1 154.2(3) 2_556 . ?
O5 K2 K1 54.66(14) 4_455 . ?
O3 K2 K1 72.9(2) 5_566 . ?
O5 K2 K1 120.6(2) 3_556 . ?
O3 K2 K1 76.72(19) 6_566 . ?
O12 K2 K1 35.32(14) . . ?
S2 K2 K1 134.94(18) 3_556 . ?
S1 K2 K1 55.07(11) 5_566 . ?
K1 K2 K1 156.39(13) 2_556 . ?
K1 K2 K1 102.51(10) 6_566 . ?
O5 K2A O5 110.1(3) 3_556 4_455 ?
O5 K2A O1A 161.19(17) 3_556 5_566 ?
O5 K2A O1A 79.70(15) 4_455 5_566 ?
O5 K2A O1A 79.70(15) 3_556 6_566 ?
O5 K2A O1A 161.19(17) 4_455 6_566 ?
O3A K2A O12A 126.2(2) 5_566 . ?
O3A K2A O12A 76.96(16) 6_566 . ?
O5 K2A O12A 90.72(15) 3_556 . ?
O5 K2A O12A 73.19(13) 4_455 . ?
O1A K2A O12A 76.47(17) 5_566 . ?
O1A K2A O12A 123.9(2) 6_566 . ?
O5 K2A O12A 73.19(13) 3_556 2_556 ?
O5 K2A O12A 90.72(15) 4_455 2_556 ?
O5 K2A S1A 161.29(19) 3_556 5_566 ?
O5 K2A S1A 86.80(8) 4_455 5_566 ?
O5 K2A S1A 86.80(8) 3_556 6_566 ?
O5 K2A S1A 161.29(19) 4_455 6_566 ?
O3A K2A K1 85.14(16) 5_566 . ?
O3A K2A K1 79.85(17) 6_566 . ?
O5 K2A K1 133.53(11) 3_556 . ?
O5 K2A K1 60.57(4) 4_455 . ?
O1A K2A K1 36.90(14) 5_566 . ?
O1A K2A K1 124.7(2) 6_566 . ?
O12A K2A K1 42.99(9) . . ?
O12A K2A K1 144.56(9) 2_556 . ?
S1A K2A K1 61.46(7) 5_566 . ?
S1A K2A K1 102.11(13) 6_566 . ?
O5 K2A K1 60.57(4) 3_556 2_556 ?
O5 K2A K1 133.53(11) 4_455 2_556 ?
K1 K2A K1 160.16(18) . 2_556 ?
O13B K3 O8 87.8(3) . . ?
O13B K3 O8 101.7(3) 2_656 . ?
O8 K3 O8 169.58(7) . 2_656 ?
O8 K3 O4 89.62(5) . 2 ?
O8 K3 O4 84.71(5) 2_656 2 ?
O8 K3 O4 84.71(5) . 1_656 ?
O8 K3 O4 89.62(5) 2_656 1_656 ?
O4 K3 O4 113.96(7) 2 1_656 ?
O8 K3 O13A 94.3(4) . . ?
O8 K3 O13A 93.8(4) 2_656 . ?
O4 K3 O13A 161.3(3) 2 . ?
O4 K3 O13A 84.6(3) 1_656 . ?
O8 K3 O13A 93.8(4) . 2_656 ?
O8 K3 O13A 94.3(4) 2_656 2_656 ?
O4 K3 O13A 84.6(3) 2 2_656 ?
O4 K3 O13A 161.3(3) 1_656 2_656 ?
O8 K3 O13 92.4(3) . 2_656 ?
O8 K3 O13 94.8(3) 2_656 2_656 ?
O4 K3 O13 76.64(19) 2 2_656 ?
O4 K3 O13 168.9(2) 1_656 2_656 ?
O8 K3 O13 94.8(3) . . ?
O8 K3 O13 92.4(3) 2_656 . ?
O4 K3 O13 168.9(2) 2 . ?
O4 K3 O13 76.64(19) 1_656 . ?
O13 K3 O13 93.0(4) 2_656 . ?
O8 K3 K2 89.58(10) . 4_546 ?
O8 K3 K2 80.01(10) 2_656 4_546 ?
O4 K3 K2 53.73(9) 2 4_546 ?
O4 K3 K2 60.47(10) 1_656 4_546 ?
O13 K3 K2 130.3(2) 2_656 4_546 ?
O13 K3 K2 136.3(2) . 4_546 ?
O8 K3 K2 80.01(10) . 3_545 ?
O8 K3 K2 89.58(10) 2_656 3_545 ?
O4 K3 K2 60.47(10) 2 3_545 ?
O4 K3 K2 53.73(9) 1_656 3_545 ?
O13 K3 K2 136.3(2) 2_656 3_545 ?
O13 K3 K2 130.3(2) . 3_545 ?
K2 K3 K2 11.5(2) 4_546 3_545 ?
N2 N1 C4 112.92(16) . . ?
N1 N2 C7 118.39(16) . . ?
C10 N3 C9 123.20(17) . . ?
C10 N3 C12 119.58(17) . . ?
C9 N3 C12 117.21(16) . . ?
C9 N4 C8 124.63(17) . . ?
C9 N4 C11 116.14(16) . . ?
C8 N4 C11 119.23(17) . . ?
C10 N5 H5A 120.0 . . ?
C10 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N7 N6 C16 113.53(16) . . ?
N6 N7 C19 118.05(16) . . ?
C22 N8 H8A 120.0 . . ?
C22 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C21 N9 C20 124.89(16) . . ?
C21 N9 C23 117.41(16) . . ?
C20 N9 C23 117.69(16) . . ?
C22 N10 C21 123.37(16) . . ?
C22 N10 C24 119.33(16) . . ?
C21 N10 C24 117.19(16) . . ?
S2 O4 K3 128.56(10) . 1_454 ?
S2 O5 K2 141.75(19) . 4_445 ?
S2 O5 K2A 132.79(11) . 3_444 ?
K2 O5 K2A 10.57(18) 4_445 3_444 ?
S2 O5 K2 122.7(2) . 3_444 ?
K2 O5 K2 20.9(4) 4_445 3_444 ?
S2 O6 K1 130.99(10) . 4_445 ?
C9 O8 K3 156.74(14) . . ?
C21 O10 K1 167.92(14) . . ?
K2 O12 K1 111.0(3) 2_556 . ?
K2 O12 K2 6.4(3) 2_556 . ?
K1 O12 K2 106.7(2) . . ?
K1 O12A K2A 90.27(13) . . ?
K3 O13 H130 119(4) . . ?
K3 O13 H131 125(5) . . ?
H130 O13 H131 106(3) . . ?
H140 O14 H141 118(3) . . ?
H150 O15 H151 107(3) . . ?
H160 O16 H161 107(2) . . ?
O5 S2 O4 113.60(11) . . ?
O5 S2 O6 112.51(12) . . ?
O4 S2 O6 112.80(11) . . ?
O5 S2 C13 105.34(10) . . ?
O4 S2 C13 106.95(9) . . ?
O6 S2 C13 104.78(9) . . ?
O5 S2 K2 38.08(15) . 3_444 ?
O4 S2 K2 89.24(11) . 3_444 ?
O6 S2 K2 98.97(13) . 3_444 ?
C13 S2 K2 142.75(15) . 3_444 ?

_refine_diff_density_max         0.826
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.082



# start Validation Reply Form

_vrf_PLAT430_rgtm31a             
;
PROBLEM: Short Inter D...A Contact  O13A     ..O17      .       2.09 Ang.  
RESPONSE: The aquo O atom is disorderd and the e-density difference map
could not locate the H-atoms in accepetable positions and are not
included.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_rgtm30t2
_database_code_depnum_ccdc_archive 'CCDC 1902620'
loop_
_audit_author_name
_audit_author_address
'Rakesh Ganguly'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            rgtm30m
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H18 N5 Na O8 S'
_chemical_formula_iupac          ?
_chemical_formula_weight         415.36

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.7666(7)
_cell_length_b                   10.5350(9)
_cell_length_c                   20.5005(17)
_cell_angle_alpha                90
_cell_angle_beta                 90.853(3)
_cell_angle_gamma                90
_cell_volume                     1677.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9961
_cell_measurement_theta_min      3.2539
_cell_measurement_theta_max      27.8317
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864

_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_T_max  0.74

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            3993
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_full        27.94
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27

_refine_special_details          
;

Refined as a 2-component twin.
;

_reflns_number_total             3993
_reflns_number_gt                3491
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1392
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.067
_refine_ls_number_reflns         3993
_refine_ls_number_parameters     293
_refine_ls_number_restraints     346
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0311P)²+4.9699P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Na Na 0.0362 0.0249 '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'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2018)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2018)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2018)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.1862(6) 0.4225(4) 0.53262(18) 0.0128(8) Uani d . . . 1.0 . .
C C2 0.2234(6) 0.5191(4) 0.57861(17) 0.0140(8) Uani d . . . 1.0 . .
C C3 0.2314(6) 0.5942(4) 0.69267(18) 0.0169(9) Uani d . . . 1.0 . .
H H3A 0.350659 0.620903 0.685714 0.025 Uiso calc U . R 1.0 . .
H H3B 0.221924 0.556353 0.736129 0.025 Uiso calc U . R 1.0 . .
H H3C 0.155198 0.668141 0.689332 0.025 Uiso calc U . R 1.0 . .
C C4 0.0965(5) 0.3922(4) 0.66454(18) 0.0145(8) Uani d . . . 1.0 . .
C C6 -0.0513(6) 0.1936(4) 0.6383(2) 0.0201(9) Uani d . . . 1.0 . .
H H6A -0.083474 0.203341 0.684101 0.03 Uiso calc U . R 1.0 . .
H H6B 0.018742 0.116868 0.633492 0.03 Uiso calc U . R 1.0 . .
H H6C -0.155599 0.186318 0.611093 0.03 Uiso calc U . R 1.0 . .
C C7 0.0963(6) 0.3112(4) 0.55269(18) 0.0136(8) Uani d . . . 1.0 . .
C C8 0.3215(5) 0.5171(4) 0.37551(18) 0.0110(7) Uani d . . . 1.0 . .
C C9 0.2542(6) 0.4223(3) 0.33497(18) 0.0127(8) Uani d . . . 1.0 . .
H H9 0.187503 0.355619 0.352876 0.015 Uiso calc U . R 1.0 . .
C C10 0.2851(5) 0.4256(4) 0.26831(18) 0.0129(8) Uani d . . . 1.0 . .
H H10 0.240089 0.360992 0.240558 0.016 Uiso calc U . R 1.0 . .
C C11 0.3823(5) 0.5241(4) 0.24254(18) 0.0104(7) Uani d . . . 1.0 . .
C C12 0.4485(6) 0.6197(3) 0.28231(18) 0.0132(8) Uani d . . . 1.0 . .
H H12 0.513912 0.686889 0.264194 0.016 Uiso calc U . R 1.0 . .
C C13 0.4178(5) 0.6158(3) 0.34922(18) 0.0136(7) Uani d . . . 1.0 . .
H H13 0.4626 0.680606 0.376883 0.016 Uiso calc U . R 1.0 . .
N N1 0.2949(4) 0.5233(3) 0.44413(16) 0.0122(6) Uani d . . . 1.0 . .
N N2 0.2230(4) 0.4245(3) 0.46690(15) 0.0111(7) Uani d . . . 1.0 . .
N N3 0.3003(5) 0.6256(3) 0.56246(16) 0.0149(7) Uani d . . . 1.0 . .
H H3D 0.323887 0.682958 0.592489 0.018 Uiso calc U . R 1.0 . .
H H3E 0.328253 0.639427 0.521628 0.018 Uiso calc U . R 1.0 . .
N N4 0.1812(5) 0.5000(3) 0.64284(15) 0.0137(7) Uani d . . . 1.0 . .
N N5 0.0483(5) 0.3048(3) 0.61781(15) 0.0146(7) Uani d . . . 1.0 . .
Na Na1 0.7500(2) 0.64392(15) 0.06255(7) 0.0158(4) Uani d . . D 1.0 . .
O O1 0.0670(4) 0.3763(3) 0.72205(13) 0.0202(7) Uani d . . . 1.0 . .
O O2 0.0571(4) 0.2217(2) 0.51598(13) 0.0160(6) Uani d . . . 1.0 . .
O O3 0.6036(5) 0.5479(4) 0.15023(16) 0.0302(9) Uani d U P D 0.934(4) A 1
O O4 0.3214(5) 0.6351(4) 0.13260(17) 0.0308(10) Uani d U P D 0.934(4) A 1
O O5 0.3591(6) 0.4098(4) 0.13113(17) 0.0373(12) Uani d U P D 0.934(4) A 1
O O3A 0.513(4) 0.660(3) 0.1362(19) 0.025(4) Uani d U P D 0.066(4) A 2
O O4A 0.266(5) 0.522(4) 0.122(2) 0.028(5) Uani d U P D 0.066(4) A 2
O O5A 0.543(6) 0.433(4) 0.145(2) 0.028(5) Uani d U P D 0.066(4) A 2
O O6 0.5185(4) 0.6785(3) -0.01079(14) 0.0177(6) Uani d . . D 1.0 . .
H H6O 0.550(6) 0.659(4) -0.0444(16) 0.027 Uiso d U . D 1.0 . .
H H6OA 0.434(5) 0.642(4) -0.006(2) 0.027 Uiso d U . D 1.0 . .
O O7 0.7951(4) 0.4535(3) 0.00187(14) 0.0184(6) Uani d . . D 1.0 . .
H H7OA 0.797(7) 0.463(5) -0.0349(13) 0.028 Uiso d U . D 1.0 . .
H H7O 0.864(6) 0.403(4) 0.009(2) 0.028 Uiso d U . D 1.0 . .
O O8 0.9620(5) 0.6418(3) 0.14096(15) 0.0215(7) Uani d . . D 1.0 . .
H H8O 1.060(3) 0.635(5) 0.140(3) 0.032 Uiso d U . D 1.0 . .
H H8OA 0.939(7) 0.629(5) 0.1767(15) 0.032 Uiso d U . D 1.0 . .
S S1 0.42187(13) 0.52907(9) 0.15766(5) 0.0116(2) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N2 . 1.382(5) ?
C1 C2 . 1.414(5) ?
C1 C7 . 1.429(6) ?
C2 N3 . 1.316(5) ?
C2 N4 . 1.376(5) ?
C3 N4 . 1.473(5) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 O1 . 1.216(5) ?
C4 N5 . 1.376(5) ?
C4 N4 . 1.390(5) ?
C6 N5 . 1.469(5) ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C6 H6C . 0.98 ?
C7 O2 . 1.241(5) ?
C7 N5 . 1.393(5) ?
C8 C13 . 1.394(5) ?
C8 C9 . 1.396(5) ?
C8 N1 . 1.426(5) ?
C9 C10 . 1.391(5) ?
C9 H9 . 0.95 ?
C10 C11 . 1.393(5) ?
C10 H10 . 0.95 ?
C11 C12 . 1.389(5) ?
C11 S1 . 1.772(4) ?
C12 C13 . 1.396(5) ?
C12 H12 . 0.95 ?
C13 H13 . 0.95 ?
N1 N2 . 1.274(4) ?
N2 Na1 2_645 3.025(3) ?
N3 H3D . 0.88 ?
N3 H3E . 0.88 ?
Na1 O8 . 2.284(4) ?
Na1 O6 . 2.355(4) ?
Na1 O2 2_655 2.363(3) ?
Na1 O3 . 2.368(4) ?
Na1 O7 . 2.390(3) ?
Na1 O3A . 2.402(19) ?
Na1 H6O . 2.67(5) ?
O3 S1 . 1.435(4) ?
O4 S1 . 1.453(4) ?
O5 S1 . 1.451(4) ?
O3A S1 . 1.61(3) ?
O4A S1 . 1.40(4) ?
O5A S1 . 1.41(4) ?
O6 H6O . 0.76(2) ?
O6 H6OA . 0.77(2) ?
O7 H7OA . 0.76(2) ?
O7 H7O . 0.76(2) ?
O8 H8O . 0.76(3) ?
O8 H8OA . 0.77(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 C1 C2 . . 126.6(4) ?
N2 C1 C7 . . 113.7(3) ?
C2 C1 C7 . . 119.7(3) ?
N3 C2 N4 . . 118.7(3) ?
N3 C2 C1 . . 122.3(3) ?
N4 C2 C1 . . 118.9(4) ?
N4 C3 H3A . . 109.5 ?
N4 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
N4 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
O1 C4 N5 . . 122.0(4) ?
O1 C4 N4 . . 121.3(4) ?
N5 C4 N4 . . 116.7(3) ?
N5 C6 H6A . . 109.5 ?
N5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
N5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
O2 C7 N5 . . 118.5(4) ?
O2 C7 C1 . . 124.4(3) ?
N5 C7 C1 . . 117.0(3) ?
C13 C8 C9 . . 120.1(3) ?
C13 C8 N1 . . 115.7(3) ?
C9 C8 N1 . . 124.2(4) ?
C10 C9 C8 . . 119.9(4) ?
C10 C9 H9 . . 120.0 ?
C8 C9 H9 . . 120.0 ?
C9 C10 C11 . . 119.5(3) ?
C9 C10 H10 . . 120.2 ?
C11 C10 H10 . . 120.2 ?
C12 C11 C10 . . 121.1(3) ?
C12 C11 S1 . . 119.1(3) ?
C10 C11 S1 . . 119.8(3) ?
C11 C12 C13 . . 119.2(4) ?
C11 C12 H12 . . 120.4 ?
C13 C12 H12 . . 120.4 ?
C8 C13 C12 . . 120.1(3) ?
C8 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
N2 N1 C8 . . 113.2(3) ?
N1 N2 C1 . . 117.9(3) ?
N1 N2 Na1 . 2_645 133.9(2) ?
C1 N2 Na1 . 2_645 101.3(2) ?
C2 N3 H3D . . 120.0 ?
C2 N3 H3E . . 120.0 ?
H3D N3 H3E . . 120.0 ?
C2 N4 C4 . . 123.1(3) ?
C2 N4 C3 . . 120.0(3) ?
C4 N4 C3 . . 116.8(3) ?
C4 N5 C7 . . 124.1(3) ?
C4 N5 C6 . . 118.2(3) ?
C7 N5 C6 . . 117.6(3) ?
O8 Na1 O6 . . 170.54(13) ?
O8 Na1 O2 . 2_655 91.43(13) ?
O6 Na1 O2 . 2_655 89.84(11) ?
O8 Na1 O3 . . 79.10(13) ?
O6 Na1 O3 . . 100.38(13) ?
O2 Na1 O3 2_655 . 169.12(14) ?
O8 Na1 O7 . . 104.39(13) ?
O6 Na1 O7 . . 85.07(11) ?
O2 Na1 O7 2_655 . 80.61(11) ?
O3 Na1 O7 . . 96.45(13) ?
O8 Na1 O3A . . 96.3(11) ?
O6 Na1 O3A . . 78.8(11) ?
O2 Na1 O3A 2_655 . 154.6(9) ?
O7 Na1 O3A . . 120.3(9) ?
O8 Na1 N2 . 2_655 95.64(12) ?
O6 Na1 N2 . 2_655 77.06(10) ?
O2 Na1 N2 2_655 2_655 58.56(9) ?
O3 Na1 N2 . 2_655 127.20(13) ?
O7 Na1 N2 . 2_655 134.87(11) ?
O8 Na1 H6O . . 169.2(8) ?
O6 Na1 H6O . . 15.9(7) ?
O2 Na1 H6O 2_655 . 77.8(8) ?
O3 Na1 H6O . . 111.5(9) ?
O7 Na1 H6O . . 73.1(9) ?
O3A Na1 H6O . . 94.0(13) ?
N2 Na1 H6O 2_655 . 79.7(10) ?
C7 O2 Na1 . 2_645 121.6(3) ?
S1 O3 Na1 . . 128.6(2) ?
S1 O3A Na1 . . 117.2(16) ?
Na1 O6 H6O . . 107.(4) ?
Na1 O6 H6OA . . 119.(4) ?
H6O O6 H6OA . . 105.(4) ?
Na1 O7 H7OA . . 114.(4) ?
Na1 O7 H7O . . 126.(4) ?
H7OA O7 H7O . . 106.(4) ?
Na1 O8 H8O . . 133.(4) ?
Na1 O8 H8OA . . 120.(4) ?
H8O O8 H8OA . . 105.(4) ?
O4A S1 O5A . . 116.(2) ?
O3 S1 O5 . . 113.9(2) ?
O3 S1 O4 . . 112.3(2) ?
O5 S1 O4 . . 111.0(3) ?
O4A S1 O3A . . 107.(2) ?
O5A S1 O3A . . 105.1(19) ?
O4A S1 C11 . . 110.1(18) ?
O5A S1 C11 . . 106.9(18) ?
O3 S1 C11 . . 107.05(19) ?
O5 S1 C11 . . 106.28(19) ?
O4 S1 C11 . . 105.66(19) ?
O3A S1 C11 . . 112.1(13) ?

