# Electronic Supplementary Material (ESI) for ChemComm.
# 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_pm3m
_database_code_depnum_ccdc_archive 'CCDC 1956286'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.42A   From C5              2.40 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Ce N11 O0 S7'
_chemical_formula_weight         987.04

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.3981(7)
_cell_length_b                   11.3981(7)
_cell_length_c                   11.3981(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1480.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0
_cell_measurement_reflns_used    21416
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      30.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_F_000             481
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.094
_exptl_absorpt_coefficient_mu    1.046
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3903
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.00
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21416
_diffrn_reflns_av_unetI/netI     0.0059
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.787
_diffrn_reflns_theta_max         30.563
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             512
_reflns_number_gt                512
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1315P)²+1.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         512
_refine_ls_number_parameters     27
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1590
_refine_ls_wR_factor_gt          0.1590
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.094
_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
Ce1 Ce 0.0000 0.0000 0.0000 0.0225(3) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.156(15) Uani 1 16 d S T P . .
C2 C 0.0000 0.106(3) 0.4155(17) 0.173(9) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.036(4) Uani 1 48 d S T P . .
C3 C 0.0000 0.229(3) 0.5000 0.173(9) Uani 1 4 d S T P . .
C4 C 0.407(2) 0.407(2) 0.5000 0.088(6) Uani 0.3332 4 d DS T P . .
C5 C 0.3026(11) 0.5000 0.5000 0.088(6) Uani 0.6664 8 d DS T P . .
S1 S 0.2630(2) 0.2630(2) 0.2630(2) 0.113(2) Uani 0.8752 6 d S T P . .
C1 C 0.1838(6) 0.1838(6) 0.1838(6) 0.075(4) Uani 0.8752 6 d S T P . .
N1 N 0.1265(6) 0.1265(6) 0.1265(6) 0.096(5) Uani 0.8752 6 d S T P . .


_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
Ce1 N1 2.497(12) . ?
Ce1 N1 2.497(12) 25 ?
Ce1 N1 2.497(12) 26 ?
Ce1 N1 2.497(12) 2 ?
Ce1 N1 2.497(12) 28 ?
Ce1 N1 2.497(12) 3 ?
Ce1 N1 2.497(12) 27 ?
Ce1 N1 2.497(12) 4 ?
N2 C2 1.55(2) 37 ?
N2 C2 1.55(2) 13_556 ?
N2 C2 1.55(2) 26_556 ?
N2 C2 1.55(2) 2 ?
N2 C2 1.55(2) 38 ?
N2 C2 1.55(2) 25_556 ?
N2 C2 1.55(2) 14_556 ?
N2 C2 1.55(2) . ?
C2 C3 1.70(3) . ?
C2 C2 1.71(5) 37 ?
C2 C2 1.71(5) 38 ?
C2 C2 1.93(4) 26_556 ?
N3 C4 1.51(3) . ?
N3 C4 1.51(3) 33_666 ?
N3 C4 1.51(3) 25_666 ?
N3 C4 1.51(3) 9 ?
N3 C4 1.51(3) 29_666 ?
N3 C4 1.51(3) 5 ?
N3 C4 1.51(3) 35_655 ?
N3 C4 1.51(3) 7_665 ?
N3 C4 1.51(3) 31_556 ?
N3 C4 1.51(3) 27_565 ?
N3 C4 1.51(3) 3_656 ?
N3 C4 1.51(3) 11_566 ?
C3 C2 1.70(3) 26_556 ?
C4 C4 1.51(3) 11_566 ?
C4 C4 1.51(3) 31_556 ?
C4 C4 1.51(3) 9 ?
C4 C4 1.51(3) 5 ?
C4 C5 1.593(10) 5 ?
C4 C5 1.593(10) . ?
C5 C4 1.593(10) 11_566 ?
C5 C4 1.593(10) 27_565 ?
C5 C4 1.593(10) 9 ?
S1 C1 1.564(13) . ?
C1 N1 1.131(16) . ?

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
N1 Ce1 N1 180.0(3) . 25 ?
N1 Ce1 N1 70.5 . 26 ?
N1 Ce1 N1 109.5 25 26 ?
N1 Ce1 N1 109.5 . 2 ?
N1 Ce1 N1 70.5 25 2 ?
N1 Ce1 N1 180.0(3) 26 2 ?
N1 Ce1 N1 70.529(1) . 28 ?
N1 Ce1 N1 109.5 25 28 ?
N1 Ce1 N1 109.5 26 28 ?
N1 Ce1 N1 70.5 2 28 ?
N1 Ce1 N1 109.5 . 3 ?
N1 Ce1 N1 70.5 25 3 ?
N1 Ce1 N1 70.5 26 3 ?
N1 Ce1 N1 109.5 2 3 ?
N1 Ce1 N1 70.5 28 3 ?
N1 Ce1 N1 70.5 . 27 ?
N1 Ce1 N1 109.5 25 27 ?
N1 Ce1 N1 109.5 26 27 ?
N1 Ce1 N1 70.5 2 27 ?
N1 Ce1 N1 109.5 28 27 ?
N1 Ce1 N1 180.0(3) 3 27 ?
N1 Ce1 N1 109.5 . 4 ?
N1 Ce1 N1 70.529(1) 25 4 ?
N1 Ce1 N1 70.5 26 4 ?
N1 Ce1 N1 109.5 2 4 ?
N1 Ce1 N1 180.0 28 4 ?
N1 Ce1 N1 109.5 3 4 ?
N1 Ce1 N1 70.5 27 4 ?
C2 N2 C2 180.0(12) 37 13_556 ?
C2 N2 C2 112.8(11) 37 26_556 ?
C2 N2 C2 67.2(11) 13_556 26_556 ?
C2 N2 C2 67.2(11) 37 2 ?
C2 N2 C2 112.8(11) 13_556 2 ?
C2 N2 C2 180.0 26_556 2 ?
C2 N2 C2 103(2) 37 38 ?
C2 N2 C2 77(2) 13_556 38 ?
C2 N2 C2 112.8(11) 26_556 38 ?
C2 N2 C2 67.2(11) 2 38 ?
C2 N2 C2 112.8(11) 37 25_556 ?
C2 N2 C2 67.2(11) 13_556 25_556 ?
C2 N2 C2 103(2) 26_556 25_556 ?
C2 N2 C2 77(2) 2 25_556 ?
C2 N2 C2 112.8(11) 38 25_556 ?
C2 N2 C2 77(2) 37 14_556 ?
C2 N2 C2 103(2) 13_556 14_556 ?
C2 N2 C2 67.2(11) 26_556 14_556 ?
C2 N2 C2 112.8(11) 2 14_556 ?
C2 N2 C2 180.0 38 14_556 ?
C2 N2 C2 67.2(11) 25_556 14_556 ?
C2 N2 C2 67.2(11) 37 . ?
C2 N2 C2 112.8(11) 13_556 . ?
C2 N2 C2 77(2) 26_556 . ?
C2 N2 C2 103(2) 2 . ?
C2 N2 C2 67.2(11) 38 . ?
C2 N2 C2 180.0 25_556 . ?
C2 N2 C2 112.8(11) 14_556 . ?
N2 C2 C3 107.1(15) . . ?
N2 C2 C2 56.4(6) . 37 ?
C3 C2 C2 125.7(5) . 37 ?
N2 C2 C2 56.4(6) . 38 ?
C3 C2 C2 125.7(5) . 38 ?
C2 C2 C2 89.999(1) 37 38 ?
N2 C2 C2 51.5(11) . 26_556 ?
C3 C2 C2 55.6(9) . 26_556 ?
C2 C2 C2 90.000(3) 37 26_556 ?
C2 C2 C2 90.000(1) 38 26_556 ?
C4 N3 C4 120.0 . 33_666 ?
C4 N3 C4 180.0 . 25_666 ?
C4 N3 C4 60.000(2) 33_666 25_666 ?
C4 N3 C4 60.000(2) . 9 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 120.000(1) 25_666 9 ?
C4 N3 C4 120.000(2) . 29_666 ?
C4 N3 C4 60.000(1) 33_666 29_666 ?
C4 N3 C4 60.000(1) 25_666 29_666 ?
C4 N3 C4 120.000(1) 9 29_666 ?
C4 N3 C4 60.000(2) . 5 ?
C4 N3 C4 120.000(2) 33_666 5 ?
C4 N3 C4 120.000(2) 25_666 5 ?
C4 N3 C4 60.000(1) 9 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 120.000(1) . 35_655 ?
C4 N3 C4 90.000(3) 33_666 35_655 ?
C4 N3 C4 60.000(2) 25_666 35_655 ?
C4 N3 C4 90.000(2) 9 35_655 ?
C4 N3 C4 120.000(1) 29_666 35_655 ?
C4 N3 C4 60.000(2) 5 35_655 ?
C4 N3 C4 120.000(2) . 7_665 ?
C4 N3 C4 120.000(2) 33_666 7_665 ?
C4 N3 C4 60.000(1) 25_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 90.000(3) 29_666 7_665 ?
C4 N3 C4 90.000(2) 5 7_665 ?
C4 N3 C4 60.000(1) 35_655 7_665 ?
C4 N3 C4 60.000(1) . 31_556 ?
C4 N3 C4 60.000(1) 33_666 31_556 ?
C4 N3 C4 120.000(2) 25_666 31_556 ?
C4 N3 C4 120.000(2) 9 31_556 ?
C4 N3 C4 90.000(2) 29_666 31_556 ?
C4 N3 C4 90.000(3) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 90.000(3) . 27_565 ?
C4 N3 C4 120.000(2) 33_666 27_565 ?
C4 N3 C4 90.000(1) 25_666 27_565 ?
C4 N3 C4 60.000(2) 9 27_565 ?
C4 N3 C4 60.000(2) 29_666 27_565 ?
C4 N3 C4 120.000(2) 5 27_565 ?
C4 N3 C4 120.000(1) 35_655 27_565 ?
C4 N3 C4 60.000(2) 7_665 27_565 ?
C4 N3 C4 120.000(2) 31_556 27_565 ?
C4 N3 C4 90.000(1) . 3_656 ?
C4 N3 C4 60.000(1) 33_666 3_656 ?
C4 N3 C4 90.000(3) 25_666 3_656 ?
C4 N3 C4 120.000(2) 9 3_656 ?
C4 N3 C4 120.000(2) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.000(2) 35_655 3_656 ?
C4 N3 C4 120.000(2) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 60.000(2) . 11_566 ?
C4 N3 C4 90.000(2) 33_666 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 90.000(4) 9 11_566 ?
C4 N3 C4 60.000(2) 29_666 11_566 ?
C4 N3 C4 120.000(2) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 120.000(2) 7_665 11_566 ?
C4 N3 C4 60.000(2) 31_556 11_566 ?
C4 N3 C4 60.000(2) 27_565 11_566 ?
C4 N3 C4 120.000(2) 3_656 11_566 ?
C2 C3 C2 68.9(18) . 26_556 ?
N3 C4 C4 60.001(4) . 11_566 ?
N3 C4 C4 60.001(4) . 31_556 ?
C4 C4 C4 60.001(1) 11_566 31_556 ?
N3 C4 C4 60.001(4) . 9 ?
C4 C4 C4 90.001(9) 11_566 9 ?
C4 C4 C4 120.003(16) 31_556 9 ?
N3 C4 C4 60.001(5) . 5 ?
C4 C4 C4 120.003(18) 11_566 5 ?
C4 C4 C4 90.002(13) 31_556 5 ?
C4 C4 C4 60.001(1) 9 5 ?
N3 C4 C5 93.1(12) . 5 ?
C4 C4 C5 121.7(7) 11_566 5 ?
C4 C4 C5 61.8(7) 31_556 5 ?
C4 C4 C5 121.7(7) 9 5 ?
C4 C4 C5 61.8(7) 5 5 ?
N3 C4 C5 93.1(12) . . ?
C4 C4 C5 61.8(7) 11_566 . ?
C4 C4 C5 121.7(7) 31_556 . ?
C4 C4 C5 61.8(7) 9 . ?
C4 C4 C5 121.7(7) 5 . ?
C5 C4 C5 174(2) 5 . ?
C4 C5 C4 56.4(14) 11_566 27_565 ?
C4 C5 C4 84(2) 11_566 9 ?
C4 C5 C4 56.4(14) 27_565 9 ?
C4 C5 C4 56.4(14) 11_566 . ?
C4 C5 C4 84(2) 27_565 . ?
C4 C5 C4 56.4(14) 9 . ?
N1 C1 S1 180.0(16) . . ?
C1 N1 Ce1 180.0(14) . . ?

_refine_diff_density_max         2.183
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.141

####################################################################### 
# 
# 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_i4mmm
_database_code_depnum_ccdc_archive 'CCDC 1956290'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Lu N11 O0 S7'
_chemical_formula_weight         1021.89

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.3929(17)
_cell_length_b                   11.3929(17)
_cell_length_c                   22.386(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2905.7(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20870
_cell_measurement_theta_min      1.819
_cell_measurement_theta_max      30.501

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    1.982
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3748
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20870
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.819
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1296
_reflns_number_gt                1296
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0806P)²+3.4381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1296
_refine_ls_number_parameters     59
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.137
_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
Lu1 Lu 0.0000 0.0000 0.0000 0.02839(15) Uani 1 16 d S T P . .
S1 S 0.25519(12) 0.25519(12) 0.13143(8) 0.0734(5) Uani 0.875 2 d S T P . .
C1 C 0.1759(4) 0.1759(4) 0.0905(3) 0.0640(16) Uani 0.875 2 d S T P . .
N1 N 0.1195(4) 0.1195(4) 0.0598(4) 0.083(2) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.106(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5806(13) -0.0530(7) 0.132(7) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1137(8) 0.152(6) Uani 1 4 d DS T P . .
C4 C -0.1039(16) 0.5817(13) 0.0000 0.132(7) Uani 0.5 2 d DS T P . .
C5 C -0.222(2) 0.5000 0.0000 0.152(6) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2543(4) 0.055(2) Uani 1 8 d DS T P . .
C6 C 0.1069(13) 0.0000 0.2134(5) 0.084(5) Uani 0.5 2 d DS T P . .
C7 C 0.1057(8) 0.0000 0.2956(4) 0.054(2) Uani 0.5 2 d DS T P . .
C8 C 0.2255(7) 0.0000 0.2553(5) 0.094(2) Uani 1 2 d DS T P . .


_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
Lu1 N1 2.345(6) 17 ?
Lu1 N1 2.345(6) 18 ?
Lu1 N1 2.345(6) 2 ?
Lu1 N1 2.345(6) 20 ?
Lu1 N1 2.345(6) 4 ?
Lu1 N1 2.345(6) 3 ?
Lu1 N1 2.345(6) 19 ?
Lu1 N1 2.345(6) . ?
S1 C1 1.572(7) . ?
C1 N1 1.140(9) . ?
N2 C2 1.500(12) 18 ?
N2 C2 1.500(12) 2_565 ?
N2 C2 1.500(12) 17_565 ?
N2 C2 1.500(12) . ?
N2 C4 1.506(14) 21_565 ?
N2 C4 1.506(14) 5 ?
N2 C4 1.506(14) 17_565 ?
N2 C4 1.506(14) . ?
C2 C3 1.640(16) . ?
C2 C4 1.676(19) 5 ?
C2 C4 1.676(19) . ?
C2 C2 1.84(3) 2_565 ?
C3 C2 1.640(16) 2_565 ?
C4 C5 1.636(16) . ?
C4 C2 1.676(19) 18 ?
C4 C4 1.86(3) 21_565 ?
C5 C4 1.636(16) 21_565 ?
N3 C7 1.519(9) 3 ?
N3 C7 1.519(9) 4 ?
N3 C7 1.519(9) 2 ?
N3 C7 1.519(9) . ?
N3 C6 1.523(11) 2 ?
N3 C6 1.523(11) 4 ?
N3 C6 1.523(11) 3 ?
N3 C6 1.523(11) . ?
C6 C8 1.645(14) . ?
C6 C6 1.72(2) 4 ?
C6 C6 1.72(2) 3 ?
C6 C7 1.841(14) . ?
C7 C8 1.637(11) . ?
C7 C7 1.703(13) 4 ?
C7 C7 1.703(13) 3 ?

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
N1 Lu1 N1 110.3(4) 17 18 ?
N1 Lu1 N1 69.7(4) 17 2 ?
N1 Lu1 N1 180.0(4) 18 2 ?
N1 Lu1 N1 71.0(2) 17 20 ?
N1 Lu1 N1 71.0(2) 18 20 ?
N1 Lu1 N1 109.0(2) 2 20 ?
N1 Lu1 N1 109.0(2) 17 4 ?
N1 Lu1 N1 109.0(2) 18 4 ?
N1 Lu1 N1 71.0(2) 2 4 ?
N1 Lu1 N1 180.0(4) 20 4 ?
N1 Lu1 N1 109.0(2) 17 3 ?
N1 Lu1 N1 109.0(2) 18 3 ?
N1 Lu1 N1 71.0(2) 2 3 ?
N1 Lu1 N1 69.7(4) 20 3 ?
N1 Lu1 N1 110.3(4) 4 3 ?
N1 Lu1 N1 71.0(2) 17 19 ?
N1 Lu1 N1 71.0(2) 18 19 ?
N1 Lu1 N1 109.0(2) 2 19 ?
N1 Lu1 N1 110.3(4) 20 19 ?
N1 Lu1 N1 69.7(4) 4 19 ?
N1 Lu1 N1 180.0(3) 3 19 ?
N1 Lu1 N1 180.0 17 . ?
N1 Lu1 N1 69.7(4) 18 . ?
N1 Lu1 N1 110.3(4) 2 . ?
N1 Lu1 N1 109.0(2) 20 . ?
N1 Lu1 N1 71.0(2) 4 . ?
N1 Lu1 N1 71.0(2) 3 . ?
N1 Lu1 N1 109.0(2) 19 . ?
N1 C1 S1 178.6(8) . . ?
C1 N1 Lu1 177.8(7) . . ?
C2 N2 C2 180.0(9) 18 2_565 ?
C2 N2 C2 75.5(14) 18 17_565 ?
C2 N2 C2 104.5(14) 2_565 17_565 ?
C2 N2 C2 104.5(14) 18 . ?
C2 N2 C2 75.5(14) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 112.2(5) 18 21_565 ?
C2 N2 C4 67.8(5) 2_565 21_565 ?
C2 N2 C4 67.8(5) 17_565 21_565 ?
C2 N2 C4 112.2(5) . 21_565 ?
C2 N2 C4 67.8(5) 18 5 ?
C2 N2 C4 112.2(5) 2_565 5 ?
C2 N2 C4 112.2(5) 17_565 5 ?
C2 N2 C4 67.8(5) . 5 ?
C4 N2 C4 180.0(9) 21_565 5 ?
C2 N2 C4 112.2(5) 18 17_565 ?
C2 N2 C4 67.8(5) 2_565 17_565 ?
C2 N2 C4 67.8(5) 17_565 17_565 ?
C2 N2 C4 112.2(5) . 17_565 ?
C4 N2 C4 103.7(14) 21_565 17_565 ?
C4 N2 C4 76.3(14) 5 17_565 ?
C2 N2 C4 67.8(5) 18 . ?
C2 N2 C4 112.2(5) 2_565 . ?
C2 N2 C4 112.2(5) 17_565 . ?
C2 N2 C4 67.8(5) . . ?
C4 N2 C4 76.3(14) 21_565 . ?
C4 N2 C4 103.7(14) 5 . ?
C4 N2 C4 180.0 17_565 . ?
N2 C2 C3 108.2(11) . . ?
N2 C2 C4 56.3(5) . 5 ?
C3 C2 C4 126.2(9) . 5 ?
N2 C2 C4 56.3(5) . . ?
C3 C2 C4 126.2(9) . . ?
C4 C2 C4 89.9(11) 5 . ?
N2 C2 C2 52.2(7) . 2_565 ?
C3 C2 C2 55.9(5) . 2_565 ?
C4 C2 C2 90.4(7) 5 2_565 ?
C4 C2 C2 90.4(7) . 2_565 ?
C2 C3 C2 68.1(11) 2_565 . ?
N2 C4 C5 107.2(12) . . ?
N2 C4 C2 55.9(6) . 18 ?
C5 C4 C2 125.2(10) . 18 ?
N2 C4 C2 55.9(6) . . ?
C5 C4 C2 125.2(10) . . ?
C2 C4 C2 90.1(11) 18 . ?
N2 C4 C4 51.8(7) . 21_565 ?
C5 C4 C4 55.3(7) . 21_565 ?
C2 C4 C4 89.6(7) 18 21_565 ?
C2 C4 C4 89.6(7) . 21_565 ?
C4 C5 C4 69.3(13) 21_565 . ?
C7 N3 C7 104.8(9) 3 4 ?
C7 N3 C7 68.2(5) 3 2 ?
C7 N3 C7 68.2(5) 4 2 ?
C7 N3 C7 68.2(5) 3 . ?
C7 N3 C7 68.2(5) 4 . ?
C7 N3 C7 104.8(9) 2 . ?
C7 N3 C6 111.5(3) 3 2 ?
C7 N3 C6 111.5(3) 4 2 ?
C7 N3 C6 74.5(6) 2 2 ?
C7 N3 C6 179.3(9) . 2 ?
C7 N3 C6 179.3(9) 3 4 ?
C7 N3 C6 74.5(6) 4 4 ?
C7 N3 C6 111.5(3) 2 4 ?
C7 N3 C6 111.5(3) . 4 ?
C6 N3 C6 68.8(6) 2 4 ?
C7 N3 C6 74.5(6) 3 3 ?
C7 N3 C6 179.3(9) 4 3 ?
C7 N3 C6 111.5(3) 2 3 ?
C7 N3 C6 111.5(3) . 3 ?
C6 N3 C6 68.8(6) 2 3 ?
C6 N3 C6 106.1(13) 4 3 ?
C7 N3 C6 111.5(3) 3 . ?
C7 N3 C6 111.5(3) 4 . ?
C7 N3 C6 179.3(9) 2 . ?
C7 N3 C6 74.5(6) . . ?
C6 N3 C6 106.1(13) 2 . ?
C6 N3 C6 68.8(6) 4 . ?
C6 N3 C6 68.8(6) 3 . ?
N3 C6 C8 108.3(7) . . ?
N3 C6 C6 55.6(3) . 4 ?
C8 C6 C6 125.5(3) . 4 ?
N3 C6 C6 55.6(3) . 3 ?
C8 C6 C6 125.5(3) . 3 ?
C6 C6 C6 89.999(1) 4 3 ?
N3 C6 C7 52.7(4) . . ?
C8 C6 C7 55.7(5) . . ?
C6 C6 C7 89.7(4) 4 . ?
C6 C6 C7 89.7(4) 3 . ?
N3 C7 C8 108.9(6) . . ?
N3 C7 C7 55.9(2) . 4 ?
C8 C7 C7 126.1(2) . 4 ?
N3 C7 C7 55.9(2) . 3 ?
C8 C7 C7 126.1(2) . 3 ?
C7 C7 C7 90.000(1) 4 3 ?
N3 C7 C6 52.8(5) . . ?
C8 C7 C6 56.1(5) . . ?
C7 C7 C6 90.3(4) 4 . ?
C7 C7 C6 90.3(4) 3 . ?
C7 C8 C6 68.3(6) . . ?

_refine_diff_density_max         0.978
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_i4mmm_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956288'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_i4mmm               
;
PROBLEM: Check Calcd Resid. Dens.  0.73A   From Ow1             2.32 eA-3
RESPONSE: This residual density is near the water molecule of crystallization and is not associated with the main structural residue.  It is likely that the water of crystallization may be disordered.
;
_vrf_PLAT306_i4mmm               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        Ow1 Check
RESPONSE: We have not included any of the H-atoms in any of the models.
;
_vrf_PLAT975_i4mmm_2             
;
PROBLEM: Check Calcd Resid. Dens.  0.47A   From C5              1.69 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Gd N11 O S7'
_chemical_formula_weight         1020.17

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.418(2)
_cell_length_b                   11.418(2)
_cell_length_c                   22.504(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2934.1(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21830
_cell_measurement_theta_min      1.810
_cell_measurement_theta_max      32.961

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             990
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    1.412
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3244
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24130
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.810
_diffrn_reflns_theta_max         32.961
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1592
_reflns_number_gt                1575
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1305P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1592
_refine_ls_number_parameters     59
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1738
_refine_ls_wR_factor_gt          0.1727
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_restrained_S_all      1.295
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.0000 0.0000 0.0000 0.02853(19) Uani 1 16 d S T P . .
S1 S 0.25747(16) 0.25747(16) 0.13219(11) 0.0746(7) Uani 0.875 2 d S T P . .
C1 C 0.1803(5) 0.1803(5) 0.0916(4) 0.0611(18) Uani 0.875 2 d S T P . .
N1 N 0.1227(5) 0.1227(5) 0.0611(5) 0.091(3) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.080(5) Uani 1 8 d S T P . .
C2 C 0.0000 0.580(2) -0.0561(16) 0.126(8) Uani 0.5 2 d S T P . .
C3 C 0.0000 0.5000 -0.1097(14) 0.163(10) Uani 1 4 d S T P . .
C4 C -0.095(3) 0.582(2) 0.0000 0.126(8) Uani 0.5 2 d S T P . .
C5 C -0.209(5) 0.5000 0.0000 0.24(2) Uani 1 4 d S T P . .
N3 N 0.0000 0.0000 0.2515(5) 0.054(2) Uani 1 8 d S T P . .
C6 C 0.110(2) 0.0000 0.2125(7) 0.073(3) Uani 0.5 2 d S T P . .
C7 C 0.105(2) 0.0000 0.2933(7) 0.073(3) Uani 0.5 2 d S T P . .
C8 C 0.2236(12) 0.0000 0.2553(8) 0.110(4) Uani 1 2 d S T P . .
OW1 O -0.5000 0.5000 0.0000 0.0124(8) Uani 1 16 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 N1 2.412(8) 17 ?
Gd1 N1 2.412(8) 18 ?
Gd1 N1 2.412(8) 2 ?
Gd1 N1 2.412(8) 20 ?
Gd1 N1 2.412(8) 4 ?
Gd1 N1 2.412(8) 3 ?
Gd1 N1 2.412(8) 19 ?
Gd1 N1 2.412(8) . ?
S1 C1 1.545(7) . ?
C1 N1 1.156(10) . ?
N2 C4 1.43(3) . ?
N2 C4 1.43(3) 21_565 ?
N2 C4 1.43(3) 5 ?
N2 C4 1.43(3) 17_565 ?
N2 C2 1.56(2) 2_565 ?
N2 C2 1.56(2) 18 ?
N2 C2 1.56(2) 17_565 ?
N2 C2 1.56(2) . ?
C2 C3 1.52(3) . ?
C2 C4 1.66(3) . ?
C2 C4 1.66(3) 5 ?
C2 C2 1.84(5) 2_565 ?
C3 C2 1.52(3) 2_565 ?
C4 C5 1.60(4) . ?
C4 C2 1.66(3) 18 ?
C4 C4 1.87(5) 21_565 ?
C5 C4 1.60(4) 21_565 ?
N3 C7 1.52(2) 3 ?
N3 C7 1.52(2) 4 ?
N3 C7 1.52(2) 2 ?
N3 C7 1.52(2) . ?
N3 C6 1.53(2) . ?
N3 C6 1.53(2) 4 ?
N3 C6 1.53(2) 2 ?
N3 C6 1.53(2) 3 ?
C6 C8 1.62(3) . ?
C6 C6 1.77(3) 4 ?
C6 C6 1.77(3) 3 ?
C6 C7 1.821(19) . ?
C7 C8 1.60(2) . ?
C7 C7 1.69(3) 4 ?
C7 C7 1.69(3) 3 ?

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
N1 Gd1 N1 110.5(6) 17 18 ?
N1 Gd1 N1 69.5(6) 17 2 ?
N1 Gd1 N1 180.0(6) 18 2 ?
N1 Gd1 N1 71.1(3) 17 20 ?
N1 Gd1 N1 71.1(3) 18 20 ?
N1 Gd1 N1 108.9(3) 2 20 ?
N1 Gd1 N1 108.9(3) 17 4 ?
N1 Gd1 N1 108.9(3) 18 4 ?
N1 Gd1 N1 71.1(3) 2 4 ?
N1 Gd1 N1 180.0(6) 20 4 ?
N1 Gd1 N1 108.9(3) 17 3 ?
N1 Gd1 N1 108.9(3) 18 3 ?
N1 Gd1 N1 71.1(3) 2 3 ?
N1 Gd1 N1 69.5(6) 20 3 ?
N1 Gd1 N1 110.5(6) 4 3 ?
N1 Gd1 N1 71.1(3) 17 19 ?
N1 Gd1 N1 71.1(3) 18 19 ?
N1 Gd1 N1 108.9(3) 2 19 ?
N1 Gd1 N1 110.5(6) 20 19 ?
N1 Gd1 N1 69.5(6) 4 19 ?
N1 Gd1 N1 180.0(4) 3 19 ?
N1 Gd1 N1 180.0 17 . ?
N1 Gd1 N1 69.5(6) 18 . ?
N1 Gd1 N1 110.5(6) 2 . ?
N1 Gd1 N1 108.9(3) 20 . ?
N1 Gd1 N1 71.1(3) 4 . ?
N1 Gd1 N1 71.1(3) 3 . ?
N1 Gd1 N1 108.9(3) 19 . ?
N1 C1 S1 179.7(11) . . ?
C1 N1 Gd1 178.2(10) . . ?
C4 N2 C4 81(3) . 21_565 ?
C4 N2 C4 99(3) . 5 ?
C4 N2 C4 180.0(14) 21_565 5 ?
C4 N2 C4 180.0 . 17_565 ?
C4 N2 C4 99(3) 21_565 17_565 ?
C4 N2 C4 81(3) 5 17_565 ?
C4 N2 C2 112.6(9) . 2_565 ?
C4 N2 C2 67.4(9) 21_565 2_565 ?
C4 N2 C2 112.6(9) 5 2_565 ?
C4 N2 C2 67.4(9) 17_565 2_565 ?
C4 N2 C2 67.4(9) . 18 ?
C4 N2 C2 112.6(9) 21_565 18 ?
C4 N2 C2 67.4(9) 5 18 ?
C4 N2 C2 112.6(9) 17_565 18 ?
C2 N2 C2 180.0(15) 2_565 18 ?
C4 N2 C2 112.6(9) . 17_565 ?
C4 N2 C2 67.4(9) 21_565 17_565 ?
C4 N2 C2 112.6(9) 5 17_565 ?
C4 N2 C2 67.4(9) 17_565 17_565 ?
C2 N2 C2 108(3) 2_565 17_565 ?
C2 N2 C2 72(3) 18 17_565 ?
C4 N2 C2 67.4(9) . . ?
C4 N2 C2 112.6(9) 21_565 . ?
C4 N2 C2 67.4(9) 5 . ?
C4 N2 C2 112.6(9) 17_565 . ?
C2 N2 C2 72(3) 2_565 . ?
C2 N2 C2 108(3) 18 . ?
C2 N2 C2 180.0 17_565 . ?
C3 C2 N2 106.7(18) . . ?
C3 C2 C4 127.5(17) . . ?
N2 C2 C4 52.5(13) . . ?
C3 C2 C4 127.5(17) . 5 ?
N2 C2 C4 52.5(13) . 5 ?
C4 C2 C4 81(3) . 5 ?
C3 C2 C2 52.7(10) . 2_565 ?
N2 C2 C2 53.9(13) . 2_565 ?
C4 C2 C2 90.5(12) . 2_565 ?
C4 C2 C2 90.5(12) 5 2_565 ?
C2 C3 C2 74.6(19) . 2_565 ?
N2 C4 C5 104(2) . . ?
N2 C4 C2 60.0(13) . 18 ?
C5 C4 C2 121.7(17) . 18 ?
N2 C4 C2 60.0(13) . . ?
C5 C4 C2 121.7(17) . . ?
C2 C4 C2 99(3) 18 . ?
N2 C4 C4 49.3(13) . 21_565 ?
C5 C4 C4 54.4(13) . 21_565 ?
C2 C4 C4 89.5(12) 18 21_565 ?
C2 C4 C4 89.5(12) . 21_565 ?
C4 C5 C4 71(3) 21_565 . ?
C7 N3 C7 103.6(15) 3 4 ?
C7 N3 C7 67.5(8) 3 2 ?
C7 N3 C7 67.5(8) 4 2 ?
C7 N3 C7 67.5(8) 3 . ?
C7 N3 C7 67.5(8) 4 . ?
C7 N3 C7 103.6(15) 2 . ?
C7 N3 C6 110.8(5) 3 . ?
C7 N3 C6 110.8(5) 4 . ?
C7 N3 C6 176.9(13) 2 . ?
C7 N3 C6 73.3(9) . . ?
C7 N3 C6 176.9(13) 3 4 ?
C7 N3 C6 73.3(9) 4 4 ?
C7 N3 C6 110.8(5) 2 4 ?
C7 N3 C6 110.8(5) . 4 ?
C6 N3 C6 70.7(8) . 4 ?
C7 N3 C6 110.8(5) 3 2 ?
C7 N3 C6 110.8(5) 4 2 ?
C7 N3 C6 73.3(9) 2 2 ?
C7 N3 C6 176.9(13) . 2 ?
C6 N3 C6 109.8(16) . 2 ?
C6 N3 C6 70.7(8) 4 2 ?
C7 N3 C6 73.3(9) 3 3 ?
C7 N3 C6 176.9(13) 4 3 ?
C7 N3 C6 110.8(5) 2 3 ?
C7 N3 C6 110.8(5) . 3 ?
C6 N3 C6 70.7(8) . 3 ?
C6 N3 C6 109.8(16) 4 3 ?
C6 N3 C6 70.7(8) 2 3 ?
N3 C6 C8 108.4(10) . . ?
N3 C6 C6 54.6(4) . 4 ?
C8 C6 C6 124.6(4) . 4 ?
N3 C6 C6 54.6(4) . 3 ?
C8 C6 C6 124.6(4) . 3 ?
C6 C6 C6 89.998(1) 4 3 ?
N3 C6 C7 53.2(10) . . ?
C8 C6 C7 55.2(11) . . ?
C6 C6 C7 88.8(8) 4 . ?
C6 C6 C7 88.8(8) 3 . ?
N3 C7 C8 109.6(11) . . ?
N3 C7 C7 56.2(4) . 4 ?
C8 C7 C7 126.7(4) . 4 ?
N3 C7 C7 56.2(4) . 3 ?
C8 C7 C7 126.7(4) . 3 ?
C7 C7 C7 90.000(1) 4 3 ?
N3 C7 C6 53.5(10) . . ?
C8 C7 C6 56.0(11) . . ?
C7 C7 C6 91.2(8) 4 . ?
C7 C7 C6 91.2(8) 3 . ?
C7 C8 C6 68.7(9) . . ?

_refine_diff_density_max         2.434
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.207

####################################################################### 
# 
# 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_pm3m_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956293'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.40A   From C5              2.72 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
_vrf_PLAT971_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.40A   From C5              2.72 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
_vrf_PLAT972_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.19A   From C5             -2.70 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 O0 Pr S7'
_chemical_formula_weight         987.79

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.4242(9)
_cell_length_b                   11.4242(9)
_cell_length_c                   11.4242(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1491.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25892
_cell_measurement_theta_min      1.783
_cell_measurement_theta_max      33.087

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_F_000             572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.098
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3635
_exptl_absorpt_correction_T_max  0.4353
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25892
_diffrn_reflns_av_unetI/netI     0.0064
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.783
_diffrn_reflns_theta_max         33.087
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             626
_reflns_number_gt                626
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1315P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         626
_refine_ls_number_parameters     29
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1448
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.053
_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
Pr1 Pr 0.0000 0.0000 0.0000 0.0179(2) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.149(13) Uani 1 16 d S T P . .
C2 C 0.0000 0.106(2) 0.4162(12) 0.160(12) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.029(2) Uani 1 48 d S T P . .
C3 C 0.0000 0.228(2) 0.5000 0.155(7) Uani 1 4 d S T P . .
C4 C 0.4056(17) 0.4056(17) 0.5000 0.076(5) Uani 0.3332 4 d DS T P . .
C5 C 0.3007(11) 0.5000 0.5000 0.076(5) Uani 0.6664 8 d DS T P . .
S1 S 0.26238(16) 0.26238(16) 0.26238(16) 0.0931(14) Uani 0.875 6 d S T P . .
C1 C 0.1835(5) 0.1835(5) 0.1835(5) 0.061(3) Uani 0.875 6 d S T P . .
N1 N 0.1260(5) 0.1260(5) 0.1260(5) 0.078(3) Uani 0.875 6 d S T P . .


_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
Pr1 N1 2.493(9) 25 ?
Pr1 N1 2.493(9) 28 ?
Pr1 N1 2.493(9) 4 ?
Pr1 N1 2.493(9) 27 ?
Pr1 N1 2.493(9) 3 ?
Pr1 N1 2.493(9) 2 ?
Pr1 N1 2.493(9) 26 ?
Pr1 N1 2.493(9) . ?
N2 C2 1.55(2) 37 ?
N2 C2 1.55(2) 13_556 ?
N2 C2 1.55(2) 26_556 ?
N2 C2 1.55(2) 2 ?
N2 C2 1.55(2) 38 ?
N2 C2 1.55(2) 25_556 ?
N2 C2 1.55(2) 14_556 ?
N2 C2 1.55(2) . ?
C2 C2 1.72(4) 37 ?
C2 C2 1.72(4) 38 ?
C2 C3 1.69(3) . ?
C2 C2 1.91(3) 26_556 ?
N3 C4 1.53(3) . ?
N3 C4 1.53(3) 33_666 ?
N3 C4 1.53(3) 25_666 ?
N3 C4 1.53(3) 9 ?
N3 C4 1.53(3) 29_666 ?
N3 C4 1.53(3) 5 ?
N3 C4 1.53(3) 35_655 ?
N3 C4 1.53(3) 7_665 ?
N3 C4 1.53(3) 31_556 ?
N3 C4 1.53(3) 27_565 ?
N3 C4 1.53(3) 3_656 ?
N3 C4 1.53(3) 11_566 ?
C3 C2 1.69(3) 26_556 ?
C4 C4 1.53(3) 11_566 ?
C4 C4 1.53(3) 31_556 ?
C4 C4 1.53(3) 9 ?
C4 C4 1.53(3) 5 ?
C4 C5 1.612(9) . ?
C4 C5 1.612(9) 5 ?
C5 C4 1.612(9) 11_566 ?
C5 C4 1.612(9) 27_565 ?
C5 C4 1.612(9) 9 ?
S1 C1 1.561(11) . ?
C1 N1 1.138(12) . ?

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
N1 Pr1 N1 109.471(1) 25 28 ?
N1 Pr1 N1 70.529(1) 25 4 ?
N1 Pr1 N1 180.0(4) 28 4 ?
N1 Pr1 N1 109.5 25 27 ?
N1 Pr1 N1 109.5 28 27 ?
N1 Pr1 N1 70.5 4 27 ?
N1 Pr1 N1 70.5 25 3 ?
N1 Pr1 N1 70.5 28 3 ?
N1 Pr1 N1 109.5 4 3 ?
N1 Pr1 N1 180.0(6) 27 3 ?
N1 Pr1 N1 70.5 25 2 ?
N1 Pr1 N1 70.5 28 2 ?
N1 Pr1 N1 109.5 4 2 ?
N1 Pr1 N1 70.5 27 2 ?
N1 Pr1 N1 109.5 3 2 ?
N1 Pr1 N1 109.5 25 26 ?
N1 Pr1 N1 109.5 28 26 ?
N1 Pr1 N1 70.5 4 26 ?
N1 Pr1 N1 109.5 27 26 ?
N1 Pr1 N1 70.5 3 26 ?
N1 Pr1 N1 180.0(6) 2 26 ?
N1 Pr1 N1 180.0(6) 25 . ?
N1 Pr1 N1 70.529(1) 28 . ?
N1 Pr1 N1 109.5 4 . ?
N1 Pr1 N1 70.5 27 . ?
N1 Pr1 N1 109.5 3 . ?
N1 Pr1 N1 109.5 2 . ?
N1 Pr1 N1 70.529(1) 26 . ?
C2 N2 C2 180.0(8) 37 13_556 ?
C2 N2 C2 112.5(9) 37 26_556 ?
C2 N2 C2 67.5(9) 13_556 26_556 ?
C2 N2 C2 67.5(9) 37 2 ?
C2 N2 C2 112.5(9) 13_556 2 ?
C2 N2 C2 180.0 26_556 2 ?
C2 N2 C2 103.5(17) 37 38 ?
C2 N2 C2 76.5(17) 13_556 38 ?
C2 N2 C2 112.5(9) 26_556 38 ?
C2 N2 C2 67.5(9) 2 38 ?
C2 N2 C2 112.5(9) 37 25_556 ?
C2 N2 C2 67.5(9) 13_556 25_556 ?
C2 N2 C2 103.5(17) 26_556 25_556 ?
C2 N2 C2 76.5(17) 2 25_556 ?
C2 N2 C2 112.5(9) 38 25_556 ?
C2 N2 C2 76.5(17) 37 14_556 ?
C2 N2 C2 103.5(17) 13_556 14_556 ?
C2 N2 C2 67.5(9) 26_556 14_556 ?
C2 N2 C2 112.5(9) 2 14_556 ?
C2 N2 C2 180.0 38 14_556 ?
C2 N2 C2 67.5(9) 25_556 14_556 ?
C2 N2 C2 67.5(9) 37 . ?
C2 N2 C2 112.5(9) 13_556 . ?
C2 N2 C2 76.5(17) 26_556 . ?
C2 N2 C2 103.5(17) 2 . ?
C2 N2 C2 67.5(9) 38 . ?
C2 N2 C2 180.0 25_556 . ?
C2 N2 C2 112.5(9) 14_556 . ?
N2 C2 C2 56.3(5) . 37 ?
N2 C2 C2 56.3(5) . 38 ?
C2 C2 C2 90.000(2) 37 38 ?
N2 C2 C3 107.2(11) . . ?
C2 C2 C3 125.6(3) 37 . ?
C2 C2 C3 125.6(3) 38 . ?
N2 C2 C2 51.8(9) . 26_556 ?
C2 C2 C2 89.999(2) 37 26_556 ?
C2 C2 C2 89.999(1) 38 26_556 ?
C3 C2 C2 55.4(7) . 26_556 ?
C4 N3 C4 120.0 . 33_666 ?
C4 N3 C4 180.0 . 25_666 ?
C4 N3 C4 60.000(1) 33_666 25_666 ?
C4 N3 C4 60.000(2) . 9 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 120.0 25_666 9 ?
C4 N3 C4 120.000(1) . 29_666 ?
C4 N3 C4 60.0 33_666 29_666 ?
C4 N3 C4 60.0 25_666 29_666 ?
C4 N3 C4 120.0 9 29_666 ?
C4 N3 C4 60.000(1) . 5 ?
C4 N3 C4 120.000(2) 33_666 5 ?
C4 N3 C4 120.000(2) 25_666 5 ?
C4 N3 C4 60.000(1) 9 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 120.0 . 35_655 ?
C4 N3 C4 90.000(3) 33_666 35_655 ?
C4 N3 C4 60.000(2) 25_666 35_655 ?
C4 N3 C4 90.000(1) 9 35_655 ?
C4 N3 C4 120.000(2) 29_666 35_655 ?
C4 N3 C4 60.000(1) 5 35_655 ?
C4 N3 C4 120.000(2) . 7_665 ?
C4 N3 C4 120.000(1) 33_666 7_665 ?
C4 N3 C4 60.0 25_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 90.000(3) 29_666 7_665 ?
C4 N3 C4 90.000(1) 5 7_665 ?
C4 N3 C4 60.0 35_655 7_665 ?
C4 N3 C4 60.0 . 31_556 ?
C4 N3 C4 60.0 33_666 31_556 ?
C4 N3 C4 120.000(1) 25_666 31_556 ?
C4 N3 C4 120.000(2) 9 31_556 ?
C4 N3 C4 90.000(1) 29_666 31_556 ?
C4 N3 C4 90.000(3) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 90.000(3) . 27_565 ?
C4 N3 C4 120.000(1) 33_666 27_565 ?
C4 N3 C4 90.0 25_666 27_565 ?
C4 N3 C4 60.000(1) 9 27_565 ?
C4 N3 C4 60.000(1) 29_666 27_565 ?
C4 N3 C4 120.000(1) 5 27_565 ?
C4 N3 C4 120.000(1) 35_655 27_565 ?
C4 N3 C4 60.000(1) 7_665 27_565 ?
C4 N3 C4 120.000(1) 31_556 27_565 ?
C4 N3 C4 90.0 . 3_656 ?
C4 N3 C4 60.000(1) 33_666 3_656 ?
C4 N3 C4 90.000(3) 25_666 3_656 ?
C4 N3 C4 120.000(1) 9 3_656 ?
C4 N3 C4 120.000(2) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.000(1) 35_655 3_656 ?
C4 N3 C4 120.000(2) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 60.000(2) . 11_566 ?
C4 N3 C4 90.000(1) 33_666 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 90.000(3) 9 11_566 ?
C4 N3 C4 60.000(1) 29_666 11_566 ?
C4 N3 C4 120.000(2) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 120.000(2) 7_665 11_566 ?
C4 N3 C4 60.000(1) 31_556 11_566 ?
C4 N3 C4 60.000(2) 27_565 11_566 ?
C4 N3 C4 120.000(2) 3_656 11_566 ?
C2 C3 C2 69.2(13) 26_556 . ?
N3 C4 C4 60.000(3) . 11_566 ?
N3 C4 C4 60.000(4) . 31_556 ?
C4 C4 C4 60.0 11_566 31_556 ?
N3 C4 C4 60.000(3) . 9 ?
C4 C4 C4 90.000(5) 11_566 9 ?
C4 C4 C4 120.000(13) 31_556 9 ?
N3 C4 C4 60.000(4) . 5 ?
C4 C4 C4 120.000(14) 11_566 5 ?
C4 C4 C4 90.000(10) 31_556 5 ?
C4 C4 C4 60.000(1) 9 5 ?
N3 C4 C5 93.0(10) . . ?
C4 C4 C5 61.8(6) 11_566 . ?
C4 C4 C5 121.7(5) 31_556 . ?
C4 C4 C5 61.8(6) 9 . ?
C4 C4 C5 121.7(5) 5 . ?
N3 C4 C5 93.0(10) . 5 ?
C4 C4 C5 121.7(5) 11_566 5 ?
C4 C4 C5 61.8(6) 31_556 5 ?
C4 C4 C5 121.7(5) 9 5 ?
C4 C4 C5 61.8(6) 5 5 ?
C5 C4 C5 174.0(19) . 5 ?
C4 C5 C4 56.5(11) 11_566 27_565 ?
C4 C5 C4 84.0(19) 11_566 9 ?
C4 C5 C4 56.5(11) 27_565 9 ?
C4 C5 C4 56.5(11) 11_566 . ?
C4 C5 C4 84.0(19) 27_565 . ?
C4 C5 C4 56.5(11) 9 . ?
N1 C1 S1 180.0(13) . . ?
C1 N1 Pr1 180.0(11) . . ?

_refine_diff_density_max         2.489
_refine_diff_density_min         -2.440
_refine_diff_density_rms         0.146

####################################################################### 
# 
# 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_i4mmm_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1956294'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 O0 S7 Tb'
_chemical_formula_weight         1005.84

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.3933(6)
_cell_length_b                   11.3933(6)
_cell_length_c                   22.4759(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2917.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25720
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      33.13

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    1.494
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3680
_exptl_absorpt_correction_T_max  0.4353
_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  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25720
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.812
_diffrn_reflns_theta_max         33.129
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1580
_reflns_number_gt                1573
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1134P)²+2.2976P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1580
_refine_ls_number_parameters     58
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.003
_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
Tb1 Tb 0.0000 0.0000 0.0000 0.02958(15) Uani 1 16 d S T P . .
S1 S 0.25752(12) 0.25752(12) 0.13167(8) 0.0731(5) Uani 0.875 2 d S T P . .
C1 C 0.1792(4) 0.1792(4) 0.0912(3) 0.0645(15) Uani 0.875 2 d S T P . .
N1 N 0.1221(4) 0.1221(4) 0.0604(4) 0.095(3) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.097(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5795(12) -0.0531(7) 0.132(7) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1134(7) 0.151(5) Uani 1 4 d DS T P . .
C4 C -0.1053(16) 0.5801(12) 0.0000 0.132(7) Uani 0.5 2 d DS T P . .
C5 C -0.225(2) 0.5000 0.0000 0.151(5) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2519(4) 0.057(2) Uani 1 8 d DS T P . .
C6 C 0.1080(13) 0.0000 0.2116(5) 0.089(5) Uani 0.5 2 d DS T P . .
C7 C 0.1049(8) 0.0000 0.2934(4) 0.0536(19) Uani 0.5 2 d DS T P . .
C8 C 0.2256(8) 0.0000 0.2540(6) 0.101(3) Uani 1 2 d DS T P . .


_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
Tb1 N1 2.391(7) 17 ?
Tb1 N1 2.391(7) 20 ?
Tb1 N1 2.391(7) 4 ?
Tb1 N1 2.391(7) 19 ?
Tb1 N1 2.391(7) 3 ?
Tb1 N1 2.391(7) 2 ?
Tb1 N1 2.391(7) 18 ?
Tb1 N1 2.391(7) . ?
S1 C1 1.557(6) . ?
C1 N1 1.150(8) . ?
N2 C2 1.499(12) 18 ?
N2 C2 1.499(12) 2_565 ?
N2 C2 1.499(12) 17_565 ?
N2 C2 1.499(12) . ?
N2 C4 1.507(14) 21_565 ?
N2 C4 1.507(14) 5 ?
N2 C4 1.507(14) 17_565 ?
N2 C4 1.507(14) . ?
C2 C3 1.630(15) . ?
C2 C4 1.693(19) 5 ?
C2 C4 1.693(19) . ?
C2 C2 1.81(3) 2_565 ?
C3 C2 1.630(15) 2_565 ?
C4 C5 1.637(16) . ?
C4 C2 1.693(19) 18 ?
C4 C4 1.82(3) 21_565 ?
C5 C4 1.637(16) 21_565 ?
N3 C7 1.516(9) 3 ?
N3 C7 1.516(9) 4 ?
N3 C7 1.516(9) 2 ?
N3 C7 1.516(9) . ?
N3 C6 1.528(11) 2 ?
N3 C6 1.528(11) 4 ?
N3 C6 1.528(11) 3 ?
N3 C6 1.528(11) . ?
C6 C8 1.643(14) . ?
C6 C6 1.74(2) 4 ?
C6 C6 1.74(2) 3 ?
C6 C7 1.839(13) . ?
C7 C8 1.636(11) . ?
C7 C7 1.690(13) 4 ?
C7 C7 1.690(13) 3 ?

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
N1 Tb1 N1 71.2(2) 17 20 ?
N1 Tb1 N1 108.8(2) 17 4 ?
N1 Tb1 N1 180.0(5) 20 4 ?
N1 Tb1 N1 71.2(2) 17 19 ?
N1 Tb1 N1 110.8(4) 20 19 ?
N1 Tb1 N1 69.2(4) 4 19 ?
N1 Tb1 N1 108.8(2) 17 3 ?
N1 Tb1 N1 69.2(4) 20 3 ?
N1 Tb1 N1 110.8(4) 4 3 ?
N1 Tb1 N1 180.0(5) 19 3 ?
N1 Tb1 N1 69.2(4) 17 2 ?
N1 Tb1 N1 108.8(2) 20 2 ?
N1 Tb1 N1 71.2(2) 4 2 ?
N1 Tb1 N1 108.8(2) 19 2 ?
N1 Tb1 N1 71.2(2) 3 2 ?
N1 Tb1 N1 110.8(4) 17 18 ?
N1 Tb1 N1 71.2(2) 20 18 ?
N1 Tb1 N1 108.8(2) 4 18 ?
N1 Tb1 N1 71.2(2) 19 18 ?
N1 Tb1 N1 108.8(2) 3 18 ?
N1 Tb1 N1 180.0(5) 2 18 ?
N1 Tb1 N1 180.0 17 . ?
N1 Tb1 N1 108.8(2) 20 . ?
N1 Tb1 N1 71.2(2) 4 . ?
N1 Tb1 N1 108.8(2) 19 . ?
N1 Tb1 N1 71.2(2) 3 . ?
N1 Tb1 N1 110.8(4) 2 . ?
N1 Tb1 N1 69.2(4) 18 . ?
N1 C1 S1 178.9(8) . . ?
C1 N1 Tb1 177.7(8) . . ?
C2 N2 C2 180.0(9) 18 2_565 ?
C2 N2 C2 74.4(13) 18 17_565 ?
C2 N2 C2 105.6(13) 2_565 17_565 ?
C2 N2 C2 105.6(13) 18 . ?
C2 N2 C2 74.4(13) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 111.5(5) 18 21_565 ?
C2 N2 C4 68.5(5) 2_565 21_565 ?
C2 N2 C4 68.5(5) 17_565 21_565 ?
C2 N2 C4 111.5(5) . 21_565 ?
C2 N2 C4 68.5(5) 18 5 ?
C2 N2 C4 111.5(5) 2_565 5 ?
C2 N2 C4 111.5(5) 17_565 5 ?
C2 N2 C4 68.5(5) . 5 ?
C4 N2 C4 180.0 21_565 5 ?
C2 N2 C4 111.5(5) 18 17_565 ?
C2 N2 C4 68.5(5) 2_565 17_565 ?
C2 N2 C4 68.5(5) 17_565 17_565 ?
C2 N2 C4 111.5(5) . 17_565 ?
C4 N2 C4 105.5(14) 21_565 17_565 ?
C4 N2 C4 74.5(14) 5 17_565 ?
C2 N2 C4 68.5(5) 18 . ?
C2 N2 C4 111.5(5) 2_565 . ?
C2 N2 C4 111.5(5) 17_565 . ?
C2 N2 C4 68.5(5) . . ?
C4 N2 C4 74.5(14) 21_565 . ?
C4 N2 C4 105.5(14) 5 . ?
C4 N2 C4 180.0 17_565 . ?
N2 C2 C3 109.1(10) . . ?
N2 C2 C4 56.0(5) . 5 ?
C3 C2 C4 126.1(8) . 5 ?
N2 C2 C4 56.0(5) . . ?
C3 C2 C4 126.1(8) . . ?
C4 C2 C4 90.3(10) 5 . ?
N2 C2 C2 52.8(7) . 2_565 ?
C3 C2 C2 56.2(5) . 2_565 ?
C4 C2 C2 90.2(7) 5 2_565 ?
C4 C2 C2 90.2(7) . 2_565 ?
C2 C3 C2 67.5(10) . 2_565 ?
N2 C4 C5 108.9(11) . . ?
N2 C4 C2 55.5(5) . 18 ?
C5 C4 C2 125.9(9) . 18 ?
N2 C4 C2 55.5(5) . . ?
C5 C4 C2 125.9(9) . . ?
C2 C4 C2 89.7(10) 18 . ?
N2 C4 C4 52.8(7) . 21_565 ?
C5 C4 C4 56.1(6) . 21_565 ?
C2 C4 C4 89.8(7) 18 21_565 ?
C2 C4 C4 89.8(7) . 21_565 ?
C4 C5 C4 67.7(13) . 21_565 ?
C7 N3 C7 104.0(9) 3 4 ?
C7 N3 C7 67.7(5) 3 2 ?
C7 N3 C7 67.7(5) 4 2 ?
C7 N3 C7 67.7(5) 3 . ?
C7 N3 C7 67.7(5) 4 . ?
C7 N3 C7 104.0(9) 2 . ?
C7 N3 C6 111.4(3) 3 2 ?
C7 N3 C6 111.4(3) 4 2 ?
C7 N3 C6 74.3(6) 2 2 ?
C7 N3 C6 178.4(9) . 2 ?
C7 N3 C6 178.3(9) 3 4 ?
C7 N3 C6 74.3(6) 4 4 ?
C7 N3 C6 111.4(3) 2 4 ?
C7 N3 C6 111.4(3) . 4 ?
C6 N3 C6 69.4(7) 2 4 ?
C7 N3 C6 74.3(6) 3 3 ?
C7 N3 C6 178.3(9) 4 3 ?
C7 N3 C6 111.4(3) 2 3 ?
C7 N3 C6 111.4(3) . 3 ?
C6 N3 C6 69.4(7) 2 3 ?
C6 N3 C6 107.3(13) 4 3 ?
C7 N3 C6 111.4(3) 3 . ?
C7 N3 C6 111.4(3) 4 . ?
C7 N3 C6 178.4(9) 2 . ?
C7 N3 C6 74.3(6) . . ?
C6 N3 C6 107.3(13) 2 . ?
C6 N3 C6 69.4(7) 4 . ?
C6 N3 C6 69.4(7) 3 . ?
N3 C6 C8 108.3(7) . . ?
N3 C6 C6 55.3(3) . 4 ?
C8 C6 C6 125.2(3) . 4 ?
N3 C6 C6 55.3(3) . 3 ?
C8 C6 C6 125.2(3) . 3 ?
C6 C6 C6 90.002(2) 4 3 ?
N3 C6 C7 52.5(5) . . ?
C8 C6 C7 55.7(5) . . ?
C6 C6 C7 89.2(4) 4 . ?
C6 C6 C7 89.2(4) 3 . ?
N3 C7 C8 109.2(6) . . ?
N3 C7 C7 56.1(2) . 4 ?
C8 C7 C7 126.5(3) . 4 ?
N3 C7 C7 56.1(2) . 3 ?
C8 C7 C7 126.5(3) . 3 ?
C7 C7 C7 89.999(1) 4 3 ?
N3 C7 C6 53.1(5) . . ?
C8 C7 C6 56.1(5) . . ?
C7 C7 C6 90.8(4) 4 . ?
C7 C7 C6 90.8(4) 3 . ?
C7 C8 C6 68.2(5) . . ?

_refine_diff_density_max         1.031
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.127

####################################################################### 
# 
# 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_i4mmm_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1956289'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_i4mmm               
;
PROBLEM: Check Calcd Resid. Dens.  3.17A   From C5              5.32 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Eu N11 S7'
_chemical_formula_weight         998.89

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.3876(5)
_cell_length_b                   11.3876(5)
_cell_length_c                   22.5539(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2924.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25799
_cell_measurement_theta_min      1.806
_cell_measurement_theta_max      33.198

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.033
_exptl_absorpt_coefficient_mu    1.359
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3978
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25799
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.806
_diffrn_reflns_theta_max         33.198
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1605
_reflns_number_gt                1589
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1227P)²+2.9324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1605
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1513
_refine_ls_wR_factor_gt          0.1489
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Eu1 Eu 0.0000 0.0000 0.0000 0.02888(17) Uani 1 16 d S T P . .
S1 S 0.25909(13) 0.25909(13) 0.13197(8) 0.0770(6) Uani 0.875 2 d S T P . .
C1 C 0.1806(4) 0.1806(4) 0.0914(4) 0.0651(16) Uani 0.875 2 d S T P . .
N1 N 0.1237(5) 0.1237(5) 0.0607(4) 0.099(3) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.081(3) Uani 1 8 d S T P . .
C2 C 0.0000 0.5786(16) -0.0524(12) 0.145(9) Uani 0.5 2 d S T P . .
C3 C 0.0000 0.5000 -0.1134(8) 0.146(7) Uani 1 4 d S T P . .
C4 C -0.101(3) 0.5798(16) 0.0000 0.145(9) Uani 0.5 2 d S T P . .
C5 C -0.222(3) 0.5000 0.0000 0.171(11) Uani 1 4 d S T P . .
N3 N 0.0000 0.0000 0.2515(6) 0.081(3) Uani 1 8 d S T P . .
C6 C 0.109(2) 0.0000 0.2110(6) 0.093(6) Uani 0.5 2 d S T P . .
C7 C 0.1051(10) 0.0000 0.2924(5) 0.054(2) Uani 0.5 2 d S T P . .
C8 C 0.2267(9) 0.0000 0.2533(7) 0.100(3) Uani 1 2 d S T P . .


_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
Eu1 N1 2.417(7) 17 ?
Eu1 N1 2.417(7) 18 ?
Eu1 N1 2.417(7) 2 ?
Eu1 N1 2.417(7) 20 ?
Eu1 N1 2.417(7) 4 ?
Eu1 N1 2.417(7) 3 ?
Eu1 N1 2.417(7) 19 ?
Eu1 N1 2.417(7) . ?
S1 C1 1.561(7) . ?
C1 N1 1.148(9) . ?
N2 C4 1.47(3) 21_565 ?
N2 C4 1.47(3) 5 ?
N2 C4 1.47(3) 17_565 ?
N2 C4 1.47(3) . ?
N2 C2 1.482(19) 2_565 ?
N2 C2 1.482(19) 18 ?
N2 C2 1.482(19) 17_565 ?
N2 C2 1.482(19) . ?
C2 C3 1.64(3) . ?
C2 C4 1.65(3) 5 ?
C2 C4 1.65(3) . ?
C2 C2 1.79(4) 2_565 ?
C3 C2 1.64(3) 2_565 ?
C4 C2 1.65(3) 18 ?
C4 C5 1.65(4) . ?
C4 C4 1.82(4) 21_565 ?
C5 C4 1.65(4) 21_565 ?
N3 C7 1.511(13) 3 ?
N3 C7 1.511(13) 4 ?
N3 C7 1.511(13) 2 ?
N3 C7 1.511(13) . ?
N3 C6 1.543(18) . ?
N3 C6 1.543(18) 4 ?
N3 C6 1.543(18) 2 ?
N3 C6 1.543(18) 3 ?
C6 C8 1.64(3) . ?
C6 C6 1.76(3) 4 ?
C6 C6 1.76(3) 3 ?
C6 C7 1.836(15) . ?
C7 C8 1.642(15) . ?
C7 C7 1.692(17) 4 ?
C7 C7 1.692(17) 3 ?

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
N1 Eu1 N1 111.0(5) 17 18 ?
N1 Eu1 N1 69.0(5) 17 2 ?
N1 Eu1 N1 180.0(5) 18 2 ?
N1 Eu1 N1 71.3(2) 17 20 ?
N1 Eu1 N1 71.3(2) 18 20 ?
N1 Eu1 N1 108.7(2) 2 20 ?
N1 Eu1 N1 108.7(2) 17 4 ?
N1 Eu1 N1 108.7(2) 18 4 ?
N1 Eu1 N1 71.3(2) 2 4 ?
N1 Eu1 N1 180.0(5) 20 4 ?
N1 Eu1 N1 108.7(2) 17 3 ?
N1 Eu1 N1 108.7(2) 18 3 ?
N1 Eu1 N1 71.3(2) 2 3 ?
N1 Eu1 N1 69.0(5) 20 3 ?
N1 Eu1 N1 111.0(5) 4 3 ?
N1 Eu1 N1 71.3(2) 17 19 ?
N1 Eu1 N1 71.3(2) 18 19 ?
N1 Eu1 N1 108.7(2) 2 19 ?
N1 Eu1 N1 111.0(5) 20 19 ?
N1 Eu1 N1 69.0(5) 4 19 ?
N1 Eu1 N1 180.0(4) 3 19 ?
N1 Eu1 N1 180.0 17 . ?
N1 Eu1 N1 69.0(5) 18 . ?
N1 Eu1 N1 111.0(5) 2 . ?
N1 Eu1 N1 108.7(2) 20 . ?
N1 Eu1 N1 71.3(2) 4 . ?
N1 Eu1 N1 71.3(2) 3 . ?
N1 Eu1 N1 108.7(2) 19 . ?
N1 C1 S1 178.9(9) . . ?
C1 N1 Eu1 177.5(9) . . ?
C4 N2 C4 180.0(11) 21_565 5 ?
C4 N2 C4 103(2) 21_565 17_565 ?
C4 N2 C4 77(2) 5 17_565 ?
C4 N2 C4 77(2) 21_565 . ?
C4 N2 C4 103(2) 5 . ?
C4 N2 C4 180.0 17_565 . ?
C4 N2 C2 68.0(7) 21_565 2_565 ?
C4 N2 C2 112.0(7) 5 2_565 ?
C4 N2 C2 68.0(7) 17_565 2_565 ?
C4 N2 C2 112.0(7) . 2_565 ?
C4 N2 C2 112.0(7) 21_565 18 ?
C4 N2 C2 68.0(7) 5 18 ?
C4 N2 C2 112.0(7) 17_565 18 ?
C4 N2 C2 68.0(7) . 18 ?
C2 N2 C2 180.0(12) 2_565 18 ?
C4 N2 C2 68.0(7) 21_565 17_565 ?
C4 N2 C2 112.0(7) 5 17_565 ?
C4 N2 C2 68.0(7) 17_565 17_565 ?
C4 N2 C2 112.0(7) . 17_565 ?
C2 N2 C2 106(2) 2_565 17_565 ?
C2 N2 C2 74(2) 18 17_565 ?
C4 N2 C2 112.0(7) 21_565 . ?
C4 N2 C2 68.0(7) 5 . ?
C4 N2 C2 112.0(7) 17_565 . ?
C4 N2 C2 68.0(7) . . ?
C2 N2 C2 74(2) 2_565 . ?
C2 N2 C2 106(2) 18 . ?
C2 N2 C2 180.0 17_565 . ?
N2 C2 C3 109.9(13) . . ?
N2 C2 C4 55.5(11) . 5 ?
C3 C2 C4 127.3(13) . 5 ?
N2 C2 C4 55.5(11) . . ?
C3 C2 C4 127.3(13) . . ?
C4 C2 C4 88(2) 5 . ?
N2 C2 C2 52.9(10) . 2_565 ?
C3 C2 C2 57.0(6) . 2_565 ?
C4 C2 C2 90.5(9) 5 2_565 ?
C4 C2 C2 90.5(9) . 2_565 ?
C2 C3 C2 66.0(12) . 2_565 ?
N2 C4 C2 56.5(12) . 18 ?
N2 C4 C2 56.5(12) . . ?
C2 C4 C2 92(2) 18 . ?
N2 C4 C5 108.3(14) . . ?
C2 C4 C5 125.3(13) 18 . ?
C2 C4 C5 125.3(13) . . ?
N2 C4 C4 51.7(11) . 21_565 ?
C2 C4 C4 89.5(9) 18 21_565 ?
C2 C4 C4 89.5(9) . 21_565 ?
C5 C4 C4 56.6(10) . 21_565 ?
C4 C5 C4 66.8(19) 21_565 . ?
C7 N3 C7 104.7(12) 3 4 ?
C7 N3 C7 68.1(6) 3 2 ?
C7 N3 C7 68.1(6) 4 2 ?
C7 N3 C7 68.1(6) 3 . ?
C7 N3 C7 68.1(6) 4 . ?
C7 N3 C7 104.7(12) 2 . ?
C7 N3 C6 111.2(4) 3 . ?
C7 N3 C6 111.2(4) 4 . ?
C7 N3 C6 178.7(13) 2 . ?
C7 N3 C6 73.9(8) . . ?
C7 N3 C6 178.7(13) 3 4 ?
C7 N3 C6 73.9(8) 4 4 ?
C7 N3 C6 111.2(4) 2 4 ?
C7 N3 C6 111.2(4) . 4 ?
C6 N3 C6 69.5(9) . 4 ?
C7 N3 C6 111.2(4) 3 2 ?
C7 N3 C6 111.2(4) 4 2 ?
C7 N3 C6 73.9(8) 2 2 ?
C7 N3 C6 178.7(13) . 2 ?
C6 N3 C6 107.4(18) . 2 ?
C6 N3 C6 69.5(9) 4 2 ?
C7 N3 C6 73.9(8) 3 3 ?
C7 N3 C6 178.7(13) 4 3 ?
C7 N3 C6 111.2(4) 2 3 ?
C7 N3 C6 111.2(4) . 3 ?
C6 N3 C6 69.5(9) . 3 ?
C6 N3 C6 107.4(18) 4 3 ?
C6 N3 C6 69.5(9) 2 3 ?
N3 C6 C8 108.2(10) . . ?
N3 C6 C6 55.3(5) . 4 ?
C8 C6 C6 125.2(3) . 4 ?
N3 C6 C6 55.3(5) . 3 ?
C8 C6 C6 125.2(3) . 3 ?
C6 C6 C6 90.002(1) 4 3 ?
N3 C6 C7 52.2(7) . . ?
C8 C6 C7 56.0(8) . . ?
C6 C6 C7 89.0(6) 4 . ?
C6 C6 C7 89.0(6) 3 . ?
N3 C7 C8 109.9(8) . . ?
N3 C7 C7 55.9(3) . 4 ?
C8 C7 C7 126.6(3) . 4 ?
N3 C7 C7 55.9(3) . 3 ?
C8 C7 C7 126.6(3) . 3 ?
C7 C7 C7 89.999(1) 4 3 ?
N3 C7 C6 53.8(9) . . ?
C8 C7 C6 56.1(10) . . ?
C7 C7 C6 91.0(6) 4 . ?
C7 C7 C6 91.0(6) 3 . ?
C7 C8 C6 67.9(6) . . ?

_refine_diff_density_max         4.928
_refine_diff_density_min         -1.769
_refine_diff_density_rms         0.150

####################################################################### 
# 
# 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_pm3m_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1956291'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.19A   From C5             -2.51 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 La N11 O0 S7'
_chemical_formula_weight         985.83

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.4263(5)
_cell_length_b                   11.4263(5)
_cell_length_c                   11.4263(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1491.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25943
_cell_measurement_theta_min      1.782
_cell_measurement_theta_max      33.08

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_F_000             480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.128
_exptl_absorpt_coefficient_mu    0.991
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3127
_exptl_absorpt_correction_T_max  0.4351
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25943
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.782
_diffrn_reflns_theta_max         33.080
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             625
_reflns_number_gt                625
_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 APEX III'
_computing_cell_refinement       'BRUKER APEX III'
_computing_data_reduction        'BRUKER APEX III'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1315P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         625
_refine_ls_number_parameters     29
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.189
_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
La1 La 0.0000 0.0000 0.0000 0.0210(2) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.199(18) Uani 1 16 d S T P . .
C2 C 0.0000 0.108(3) 0.4161(11) 0.181(14) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.034(2) Uani 1 48 d S T P . .
C3 C 0.0000 0.230(2) 0.5000 0.157(5) Uani 1 4 d S T P . .
C4 C 0.4066(14) 0.4066(14) 0.5000 0.078(5) Uani 0.3332 4 d DS T P . .
C5 C 0.3001(11) 0.5000 0.5000 0.078(5) Uani 0.6664 8 d DS T P . .
S1 S 0.26339(16) 0.26339(16) 0.26339(16) 0.1061(16) Uani 0.875 6 d S T P . .
C1 C 0.1848(5) 0.1848(5) 0.1848(5) 0.070(3) Uani 0.875 6 d S T P . .
N1 N 0.1274(5) 0.1274(5) 0.1274(5) 0.089(4) Uani 0.875 6 d S T P . .


_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
La1 N1 2.520(9) 25 ?
La1 N1 2.520(9) 28 ?
La1 N1 2.520(9) 4 ?
La1 N1 2.520(9) 27 ?
La1 N1 2.520(9) 3 ?
La1 N1 2.520(9) 2 ?
La1 N1 2.520(9) 26 ?
La1 N1 2.521(9) . ?
N2 C2 1.57(2) 37 ?
N2 C2 1.57(2) 13_556 ?
N2 C2 1.57(2) 26_556 ?
N2 C2 1.57(2) 2 ?
N2 C2 1.57(2) 38 ?
N2 C2 1.57(2) 25_556 ?
N2 C2 1.57(2) 14_556 ?
N2 C2 1.57(2) . ?
C2 C2 1.75(4) 37 ?
C2 C2 1.75(4) 38 ?
C2 C3 1.69(3) . ?
C2 C2 1.92(3) 26_556 ?
N3 C4 1.51(2) . ?
N3 C4 1.51(2) 33_666 ?
N3 C4 1.51(2) 25_666 ?
N3 C4 1.51(2) 9 ?
N3 C4 1.51(2) 29_666 ?
N3 C4 1.51(2) 5 ?
N3 C4 1.51(2) 35_655 ?
N3 C4 1.51(2) 7_665 ?
N3 C4 1.51(2) 31_556 ?
N3 C4 1.51(2) 27_565 ?
N3 C4 1.51(2) 3_656 ?
N3 C4 1.51(2) 11_566 ?
C3 C2 1.69(3) 26_556 ?
C4 C4 1.51(2) 11_566 ?
C4 C4 1.51(2) 31_556 ?
C4 C4 1.51(2) 9 ?
C4 C4 1.51(2) 5 ?
C4 C5 1.618(9) . ?
C4 C5 1.618(9) 5 ?
C5 C4 1.618(9) 11_566 ?
C5 C4 1.618(9) 27_565 ?
C5 C4 1.618(9) 9 ?
S1 C1 1.555(10) . ?
C1 N1 1.137(12) . ?

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
N1 La1 N1 109.471(1) 25 28 ?
N1 La1 N1 70.529(1) 25 4 ?
N1 La1 N1 180.0(2) 28 4 ?
N1 La1 N1 109.5 25 27 ?
N1 La1 N1 109.5 28 27 ?
N1 La1 N1 70.5 4 27 ?
N1 La1 N1 70.5 25 3 ?
N1 La1 N1 70.5 28 3 ?
N1 La1 N1 109.5 4 3 ?
N1 La1 N1 180.0(2) 27 3 ?
N1 La1 N1 70.5 25 2 ?
N1 La1 N1 70.5 28 2 ?
N1 La1 N1 109.5 4 2 ?
N1 La1 N1 70.5 27 2 ?
N1 La1 N1 109.5 3 2 ?
N1 La1 N1 109.5 25 26 ?
N1 La1 N1 109.5 28 26 ?
N1 La1 N1 70.5 4 26 ?
N1 La1 N1 109.5 27 26 ?
N1 La1 N1 70.5 3 26 ?
N1 La1 N1 180.0(4) 2 26 ?
N1 La1 N1 180.0(6) 25 . ?
N1 La1 N1 70.529(1) 28 . ?
N1 La1 N1 109.5 4 . ?
N1 La1 N1 70.5 27 . ?
N1 La1 N1 109.5 3 . ?
N1 La1 N1 109.5 2 . ?
N1 La1 N1 70.5 26 . ?
C2 N2 C2 180.0(7) 37 13_556 ?
C2 N2 C2 112.0(9) 37 26_556 ?
C2 N2 C2 68.0(9) 13_556 26_556 ?
C2 N2 C2 68.0(9) 37 2 ?
C2 N2 C2 112.0(9) 13_556 2 ?
C2 N2 C2 180.0 26_556 2 ?
C2 N2 C2 104.5(17) 37 38 ?
C2 N2 C2 75.5(17) 13_556 38 ?
C2 N2 C2 112.0(9) 26_556 38 ?
C2 N2 C2 68.0(9) 2 38 ?
C2 N2 C2 112.0(9) 37 25_556 ?
C2 N2 C2 68.0(9) 13_556 25_556 ?
C2 N2 C2 104.5(17) 26_556 25_556 ?
C2 N2 C2 75.5(17) 2 25_556 ?
C2 N2 C2 112.0(9) 38 25_556 ?
C2 N2 C2 75.5(17) 37 14_556 ?
C2 N2 C2 104.5(17) 13_556 14_556 ?
C2 N2 C2 68.0(9) 26_556 14_556 ?
C2 N2 C2 112.0(9) 2 14_556 ?
C2 N2 C2 180.0 38 14_556 ?
C2 N2 C2 68.0(9) 25_556 14_556 ?
C2 N2 C2 68.0(9) 37 . ?
C2 N2 C2 112.0(9) 13_556 . ?
C2 N2 C2 75.5(17) 26_556 . ?
C2 N2 C2 104.5(17) 2 . ?
C2 N2 C2 68.0(9) 38 . ?
C2 N2 C2 180.0 25_556 . ?
C2 N2 C2 112.0(9) 14_556 . ?
N2 C2 C2 56.0(4) . 37 ?
N2 C2 C2 56.0(4) . 38 ?
C2 C2 C2 90.000(1) 37 38 ?
N2 C2 C3 107.7(10) . . ?
C2 C2 C3 125.7(3) 37 . ?
C2 C2 C3 125.7(3) 38 . ?
N2 C2 C2 52.2(9) . 26_556 ?
C2 C2 C2 89.999(1) 37 26_556 ?
C2 C2 C2 89.999(1) 38 26_556 ?
C3 C2 C2 55.5(6) . 26_556 ?
C4 N3 C4 120.0 . 33_666 ?
C4 N3 C4 180.0 . 25_666 ?
C4 N3 C4 60.000(1) 33_666 25_666 ?
C4 N3 C4 60.000(1) . 9 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 120.0 25_666 9 ?
C4 N3 C4 120.000(1) . 29_666 ?
C4 N3 C4 60.0 33_666 29_666 ?
C4 N3 C4 60.0 25_666 29_666 ?
C4 N3 C4 120.0 9 29_666 ?
C4 N3 C4 60.000(1) . 5 ?
C4 N3 C4 120.000(1) 33_666 5 ?
C4 N3 C4 120.000(1) 25_666 5 ?
C4 N3 C4 60.000(1) 9 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 120.0 . 35_655 ?
C4 N3 C4 90.000(2) 33_666 35_655 ?
C4 N3 C4 60.000(1) 25_666 35_655 ?
C4 N3 C4 90.000(1) 9 35_655 ?
C4 N3 C4 120.000(1) 29_666 35_655 ?
C4 N3 C4 60.000(1) 5 35_655 ?
C4 N3 C4 120.000(1) . 7_665 ?
C4 N3 C4 120.000(1) 33_666 7_665 ?
C4 N3 C4 60.0 25_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 90.000(3) 29_666 7_665 ?
C4 N3 C4 90.000(1) 5 7_665 ?
C4 N3 C4 60.0 35_655 7_665 ?
C4 N3 C4 60.0 . 31_556 ?
C4 N3 C4 60.0 33_666 31_556 ?
C4 N3 C4 120.000(1) 25_666 31_556 ?
C4 N3 C4 120.000(1) 9 31_556 ?
C4 N3 C4 90.000(1) 29_666 31_556 ?
C4 N3 C4 90.000(3) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 90.000(2) . 27_565 ?
C4 N3 C4 120.000(1) 33_666 27_565 ?
C4 N3 C4 90.0 25_666 27_565 ?
C4 N3 C4 60.000(1) 9 27_565 ?
C4 N3 C4 60.000(1) 29_666 27_565 ?
C4 N3 C4 120.000(1) 5 27_565 ?
C4 N3 C4 120.000(1) 35_655 27_565 ?
C4 N3 C4 60.000(1) 7_665 27_565 ?
C4 N3 C4 120.000(1) 31_556 27_565 ?
C4 N3 C4 90.0 . 3_656 ?
C4 N3 C4 60.0 33_666 3_656 ?
C4 N3 C4 90.000(2) 25_666 3_656 ?
C4 N3 C4 120.000(1) 9 3_656 ?
C4 N3 C4 120.000(1) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.0 35_655 3_656 ?
C4 N3 C4 120.000(1) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 60.000(1) . 11_566 ?
C4 N3 C4 90.000(1) 33_666 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 90.000(2) 9 11_566 ?
C4 N3 C4 60.000(1) 29_666 11_566 ?
C4 N3 C4 120.000(1) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 120.000(1) 7_665 11_566 ?
C4 N3 C4 60.000(1) 31_556 11_566 ?
C4 N3 C4 60.000(1) 27_565 11_566 ?
C4 N3 C4 120.000(1) 3_656 11_566 ?
C2 C3 C2 69.0(13) 26_556 . ?
N3 C4 C4 60.000(3) . 11_566 ?
N3 C4 C4 60.000(3) . 31_556 ?
C4 C4 C4 60.000(1) 11_566 31_556 ?
N3 C4 C4 60.000(3) . 9 ?
C4 C4 C4 90.000(6) 11_566 9 ?
C4 C4 C4 120.000(12) 31_556 9 ?
N3 C4 C4 60.000(4) . 5 ?
C4 C4 C4 120.000(12) 11_566 5 ?
C4 C4 C4 90.000(9) 31_556 5 ?
C4 C4 C4 60.000(1) 9 5 ?
N3 C4 C5 93.8(8) . . ?
C4 C4 C5 62.2(5) 11_566 . ?
C4 C4 C5 122.1(4) 31_556 . ?
C4 C4 C5 62.2(5) 9 . ?
C4 C4 C5 122.1(4) 5 . ?
N3 C4 C5 93.8(8) . 5 ?
C4 C4 C5 122.1(4) 11_566 5 ?
C4 C4 C5 62.2(5) 31_556 5 ?
C4 C4 C5 122.1(4) 9 5 ?
C4 C4 C5 62.2(5) 5 5 ?
C5 C4 C5 172.5(16) . 5 ?
C4 C5 C4 55.6(10) 11_566 27_565 ?
C4 C5 C4 82.5(16) 11_566 9 ?
C4 C5 C4 55.6(10) 27_565 9 ?
C4 C5 C4 55.6(10) 11_566 . ?
C4 C5 C4 82.5(16) 27_565 . ?
C4 C5 C4 55.6(10) 9 . ?
N1 C1 S1 180.0(12) . . ?
C1 N1 La1 180.0(10) . . ?

_refine_diff_density_max         2.140
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.145

####################################################################### 
# 
# 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_rew
_database_code_depnum_ccdc_archive 'CCDC 1956287'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_DIFF003_rew                 
;
PROBLEM: _diffrn_measurement_device_type is missing
RESPONSE: BRUKER APEX II
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 Am N11 S7'
_chemical_formula_weight         1089.92

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'
N N 0.0061 0.0033 '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'
Am Am -7.8990 4.5130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.3641(18)
_cell_length_b                   11.3641(18)
_cell_length_c                   11.3641(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1467.6(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25900
_cell_measurement_theta_min      1.792
_cell_measurement_theta_max      33.101

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_F_000             518
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.587
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25900
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.792
_diffrn_reflns_theta_max         33.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             609
_reflns_number_gt                601
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0823P)²+1.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         609
_refine_ls_number_parameters     28
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.1121
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.004
_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
Am1 Am 0.0000 0.0000 0.0000 0.0260(2) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.142(14) Uani 1 16 d S T P . .
C2 C 0.0000 0.110(3) 0.418(2) 0.170(10) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.040(4) Uani 1 48 d S T P . .
C3 C 0.0000 0.232(2) 0.5000 0.170(10) Uani 1 4 d S T P . .
C4 C 0.4048(16) 0.4048(16) 0.5000 0.062(7) Uani 0.3333 4 d DS T P . .
C5 C 0.298(2) 0.5000 0.5000 0.116(13) Uani 0.6666 8 d DS T P . .
S1 S 0.2620(2) 0.2620(2) 0.2620(2) 0.111(2) Uani 0.875 6 d S T P . .
C1 C 0.1828(7) 0.1828(7) 0.1828(7) 0.073(4) Uani 0.875 6 d S T P . .
N1 N 0.1258(7) 0.1258(7) 0.1258(7) 0.088(4) Uani 0.875 6 d S T P . .


_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
Am1 N1 2.475(13) 25 ?
Am1 N1 2.475(13) 28 ?
Am1 N1 2.475(13) 4 ?
Am1 N1 2.475(13) 27 ?
Am1 N1 2.475(13) 3 ?
Am1 N1 2.475(13) 26 ?
Am1 N1 2.475(13) 2 ?
Am1 N1 2.475(13) . ?
Am1 C1 3.598(14) 25 ?
Am1 C1 3.598(14) 4 ?
Am1 C1 3.598(14) 28 ?
Am1 C1 3.598(14) 27 ?
N2 C2 1.56(3) 37 ?
N2 C2 1.56(3) 13_556 ?
N2 C2 1.56(3) 26_556 ?
N2 C2 1.56(3) 2 ?
N2 C2 1.56(3) 38 ?
N2 C2 1.56(3) 25_556 ?
N2 C2 1.56(3) 14_556 ?
N2 C2 1.56(3) . ?
C2 C3 1.67(4) . ?
C2 C2 1.77(4) 37 ?
C2 C2 1.77(4) 38 ?
C2 C2 1.86(6) 26_556 ?
N3 C4 1.53(3) . ?
N3 C4 1.53(3) 33_666 ?
N3 C4 1.53(3) 25_666 ?
N3 C4 1.53(3) 9 ?
N3 C4 1.53(3) 29_666 ?
N3 C4 1.53(3) 5 ?
N3 C4 1.53(3) 35_655 ?
N3 C4 1.53(3) 7_665 ?
N3 C4 1.53(3) 31_556 ?
N3 C4 1.53(3) 27_565 ?
N3 C4 1.53(3) 3_656 ?
N3 C4 1.53(3) 11_566 ?
C3 C2 1.67(4) 26_556 ?
C4 C4 1.53(3) 11_566 ?
C4 C4 1.53(3) 31_556 ?
C4 C4 1.53(3) 9 ?
C4 C4 1.53(3) 5 ?
C4 C5 1.624(18) 5 ?
C4 C5 1.624(18) . ?
C5 C4 1.624(18) 11_566 ?
C5 C4 1.624(18) 27_565 ?
C5 C4 1.624(18) 9 ?
S1 C1 1.559(14) . ?
C1 N1 1.123(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Am1 N1 109.5 25 28 ?
N1 Am1 N1 70.5 25 4 ?
N1 Am1 N1 180.0(6) 28 4 ?
N1 Am1 N1 109.5 25 27 ?
N1 Am1 N1 109.5 28 27 ?
N1 Am1 N1 70.5 4 27 ?
N1 Am1 N1 70.5 25 3 ?
N1 Am1 N1 70.5 28 3 ?
N1 Am1 N1 109.5 4 3 ?
N1 Am1 N1 180.0(9) 27 3 ?
N1 Am1 N1 109.5 25 26 ?
N1 Am1 N1 109.5 28 26 ?
N1 Am1 N1 70.5 4 26 ?
N1 Am1 N1 109.5 27 26 ?
N1 Am1 N1 70.5 3 26 ?
N1 Am1 N1 70.5 25 2 ?
N1 Am1 N1 70.5 28 2 ?
N1 Am1 N1 109.5 4 2 ?
N1 Am1 N1 70.5 27 2 ?
N1 Am1 N1 109.5 3 2 ?
N1 Am1 N1 180.0(9) 26 2 ?
N1 Am1 N1 180.0(9) 25 . ?
N1 Am1 N1 70.5 28 . ?
N1 Am1 N1 109.5 4 . ?
N1 Am1 N1 70.5 27 . ?
N1 Am1 N1 109.5 3 . ?
N1 Am1 N1 70.5 26 . ?
N1 Am1 N1 109.5 2 . ?
N1 Am1 C1 0.0(4) 25 25 ?
N1 Am1 C1 109.5 28 25 ?
N1 Am1 C1 70.5 4 25 ?
N1 Am1 C1 109.5 27 25 ?
N1 Am1 C1 70.5 3 25 ?
N1 Am1 C1 109.471(1) 26 25 ?
N1 Am1 C1 70.529(1) 2 25 ?
N1 Am1 C1 180.0(4) . 25 ?
N1 Am1 C1 70.5 25 4 ?
N1 Am1 C1 180.0(4) 28 4 ?
N1 Am1 C1 0.0(6) 4 4 ?
N1 Am1 C1 70.5 27 4 ?
N1 Am1 C1 109.5 3 4 ?
N1 Am1 C1 70.5 26 4 ?
N1 Am1 C1 109.5 2 4 ?
N1 Am1 C1 109.5 . 4 ?
C1 Am1 C1 70.529(1) 25 4 ?
N1 Am1 C1 109.5 25 28 ?
N1 Am1 C1 0.00(16) 28 28 ?
N1 Am1 C1 180.0(4) 4 28 ?
N1 Am1 C1 109.5 27 28 ?
N1 Am1 C1 70.5 3 28 ?
N1 Am1 C1 109.5 26 28 ?
N1 Am1 C1 70.5 2 28 ?
N1 Am1 C1 70.5 . 28 ?
C1 Am1 C1 109.471(1) 25 28 ?
C1 Am1 C1 180.0 4 28 ?
N1 Am1 C1 109.471(1) 25 27 ?
N1 Am1 C1 109.5 28 27 ?
N1 Am1 C1 70.5 4 27 ?
N1 Am1 C1 0.00(18) 27 27 ?
N1 Am1 C1 180.0(4) 3 27 ?
N1 Am1 C1 109.5 26 27 ?
N1 Am1 C1 70.5 2 27 ?
N1 Am1 C1 70.529(1) . 27 ?
C1 Am1 C1 109.471(1) 25 27 ?
C1 Am1 C1 70.5 4 27 ?
C1 Am1 C1 109.5 28 27 ?
C2 N2 C2 180.0(16) 37 13_556 ?
C2 N2 C2 110.8(12) 37 26_556 ?
C2 N2 C2 69.2(12) 13_556 26_556 ?
C2 N2 C2 69.2(12) 37 2 ?
C2 N2 C2 110.8(12) 13_556 2 ?
C2 N2 C2 180.0 26_556 2 ?
C2 N2 C2 107(2) 37 38 ?
C2 N2 C2 73(2) 13_556 38 ?
C2 N2 C2 110.8(12) 26_556 38 ?
C2 N2 C2 69.2(12) 2 38 ?
C2 N2 C2 110.8(12) 37 25_556 ?
C2 N2 C2 69.2(12) 13_556 25_556 ?
C2 N2 C2 107(2) 26_556 25_556 ?
C2 N2 C2 73(2) 2 25_556 ?
C2 N2 C2 110.8(12) 38 25_556 ?
C2 N2 C2 73(2) 37 14_556 ?
C2 N2 C2 107(2) 13_556 14_556 ?
C2 N2 C2 69.2(12) 26_556 14_556 ?
C2 N2 C2 110.8(12) 2 14_556 ?
C2 N2 C2 180.0 38 14_556 ?
C2 N2 C2 69.2(12) 25_556 14_556 ?
C2 N2 C2 69.2(12) 37 . ?
C2 N2 C2 110.8(12) 13_556 . ?
C2 N2 C2 73(2) 26_556 . ?
C2 N2 C2 107(2) 2 . ?
C2 N2 C2 69.2(12) 38 . ?
C2 N2 C2 180.0 25_556 . ?
C2 N2 C2 110.8(12) 14_556 . ?
N2 C2 C3 109.5(18) . . ?
N2 C2 C2 55.4(6) . 37 ?
C3 C2 C2 125.9(5) . 37 ?
N2 C2 C2 55.4(6) . 38 ?
C3 C2 C2 125.9(5) . 38 ?
C2 C2 C2 89.999(1) 37 38 ?
N2 C2 C2 53.4(12) . 26_556 ?
C3 C2 C2 56.1(11) . 26_556 ?
C2 C2 C2 90.000(3) 37 26_556 ?
C2 C2 C2 90.000(1) 38 26_556 ?
C4 N3 C4 120.0 . 33_666 ?
C4 N3 C4 180.0(9) . 25_666 ?
C4 N3 C4 60.000(2) 33_666 25_666 ?
C4 N3 C4 60.000(1) . 9 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 120.000(1) 25_666 9 ?
C4 N3 C4 120.000(1) . 29_666 ?
C4 N3 C4 60.0 33_666 29_666 ?
C4 N3 C4 60.0 25_666 29_666 ?
C4 N3 C4 120.0 9 29_666 ?
C4 N3 C4 60.000(1) . 5 ?
C4 N3 C4 120.000(2) 33_666 5 ?
C4 N3 C4 120.000(2) 25_666 5 ?
C4 N3 C4 60.000(2) 9 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 120.0 . 35_655 ?
C4 N3 C4 90.000(3) 33_666 35_655 ?
C4 N3 C4 60.000(2) 25_666 35_655 ?
C4 N3 C4 90.000(2) 9 35_655 ?
C4 N3 C4 120.000(2) 29_666 35_655 ?
C4 N3 C4 60.000(2) 5 35_655 ?
C4 N3 C4 120.000(1) . 7_665 ?
C4 N3 C4 120.000(2) 33_666 7_665 ?
C4 N3 C4 60.0 25_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 90.000(2) 29_666 7_665 ?
C4 N3 C4 90.000(1) 5 7_665 ?
C4 N3 C4 60.000(1) 35_655 7_665 ?
C4 N3 C4 60.0 . 31_556 ?
C4 N3 C4 60.0 33_666 31_556 ?
C4 N3 C4 120.000(2) 25_666 31_556 ?
C4 N3 C4 120.000(2) 9 31_556 ?
C4 N3 C4 90.000(2) 29_666 31_556 ?
C4 N3 C4 90.000(3) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 90.000(3) . 27_565 ?
C4 N3 C4 120.000(1) 33_666 27_565 ?
C4 N3 C4 90.000(1) 25_666 27_565 ?
C4 N3 C4 60.000(1) 9 27_565 ?
C4 N3 C4 60.000(1) 29_666 27_565 ?
C4 N3 C4 120.000(2) 5 27_565 ?
C4 N3 C4 120.000(1) 35_655 27_565 ?
C4 N3 C4 60.000(1) 7_665 27_565 ?
C4 N3 C4 120.000(2) 31_556 27_565 ?
C4 N3 C4 90.000(1) . 3_656 ?
C4 N3 C4 60.0 33_666 3_656 ?
C4 N3 C4 90.000(3) 25_666 3_656 ?
C4 N3 C4 120.000(1) 9 3_656 ?
C4 N3 C4 120.000(1) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.000(1) 35_655 3_656 ?
C4 N3 C4 120.000(1) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 60.000(2) . 11_566 ?
C4 N3 C4 90.000(1) 33_666 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 90.000(3) 9 11_566 ?
C4 N3 C4 60.000(1) 29_666 11_566 ?
C4 N3 C4 120.000(2) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 120.000(2) 7_665 11_566 ?
C4 N3 C4 60.000(2) 31_556 11_566 ?
C4 N3 C4 60.000(2) 27_565 11_566 ?
C4 N3 C4 120.000(2) 3_656 11_566 ?
C2 C3 C2 68(2) . 26_556 ?
N3 C4 C4 60.000(3) . 11_566 ?
N3 C4 C4 60.000(4) . 31_556 ?
C4 C4 C4 60.000(1) 11_566 31_556 ?
N3 C4 C4 60.000(2) . 9 ?
C4 C4 C4 90.000(7) 11_566 9 ?
C4 C4 C4 120.000(13) 31_556 9 ?
N3 C4 C4 60.000(4) . 5 ?
C4 C4 C4 120.000(14) 11_566 5 ?
C4 C4 C4 90.000(11) 31_556 5 ?
C4 C4 C4 60.000(1) 9 5 ?
N3 C4 C5 93.2(10) . 5 ?
C4 C4 C5 121.8(6) 11_566 5 ?
C4 C4 C5 61.9(6) 31_556 5 ?
C4 C4 C5 121.8(6) 9 5 ?
C4 C4 C5 61.9(6) 5 5 ?
N3 C4 C5 93.2(10) . . ?
C4 C4 C5 61.9(6) 11_566 . ?
C4 C4 C5 121.8(6) 31_556 . ?
C4 C4 C5 61.9(6) 9 . ?
C4 C4 C5 121.8(6) 5 . ?
C5 C4 C5 174(2) 5 . ?
C4 C5 C4 56.2(12) 11_566 27_565 ?
C4 C5 C4 84(2) 11_566 9 ?
C4 C5 C4 56.2(12) 27_565 9 ?
C4 C5 C4 56.2(12) 11_566 . ?
C4 C5 C4 84(2) 27_565 . ?
C4 C5 C4 56.2(12) 9 . ?
N1 C1 S1 180.0(18) . . ?
N1 C1 Am1 0.0(11) . . ?
S1 C1 Am1 180.0(10) . . ?
C1 N1 Am1 180.0(16) . . ?

_refine_diff_density_max         1.952
_refine_diff_density_min         -2.582
_refine_diff_density_rms         0.154

####################################################################### 
# 
# 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_pm3m_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1956292'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.40A   From C5              2.81 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
_vrf_PLAT972_pm3m                
;
PROBLEM: Check Calcd Resid. Dens.  0.19A   From C5             -2.68 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 Nd O0 S7'
_chemical_formula_weight         991.16

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.3976(4)
_cell_length_b                   11.3976(4)
_cell_length_c                   11.3976(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1480.61(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25898
_cell_measurement_theta_min      1.787
_cell_measurement_theta_max      33.133

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_F_000             483
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    1.154
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3853
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25898
_diffrn_reflns_av_unetI/netI     0.0044
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.787
_diffrn_reflns_theta_max         33.113
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             625
_reflns_number_gt                625
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1244P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         625
_refine_ls_number_parameters     29
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1414
_refine_ls_wR_factor_gt          0.1414
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      1.001
_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
Nd1 Nd 0.0000 0.0000 0.0000 0.0180(2) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.141(13) Uani 1 16 d S T P . .
C2 C 0.0000 0.104(2) 0.4165(13) 0.158(12) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.028(3) Uani 1 48 d S T P . .
C3 C 0.0000 0.228(2) 0.5000 0.155(7) Uani 1 4 d S T P . .
C4 C 0.4053(18) 0.4053(18) 0.5000 0.076(5) Uani 0.3332 4 d DS T P . .
C5 C 0.3003(11) 0.5000 0.5000 0.076(5) Uani 0.6664 8 d DS T P . .
S1 S 0.26218(17) 0.26218(17) 0.26218(17) 0.0946(14) Uani 0.875 6 d S T P . .
C1 C 0.1831(5) 0.1831(5) 0.1831(5) 0.063(3) Uani 0.875 6 d S T P . .
N1 N 0.1253(5) 0.1253(5) 0.1253(5) 0.080(4) Uani 0.875 6 d S T P . .


_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
Nd1 N1 2.473(10) . ?
Nd1 N1 2.473(10) 25 ?
Nd1 N1 2.473(10) 28 ?
Nd1 N1 2.473(10) 2 ?
Nd1 N1 2.473(10) 26 ?
Nd1 N1 2.473(10) 3 ?
Nd1 N1 2.473(10) 27 ?
Nd1 N1 2.473(10) 4 ?
N2 C2 1.52(2) . ?
N2 C2 1.52(2) 37 ?
N2 C2 1.52(2) 13_556 ?
N2 C2 1.52(2) 2 ?
N2 C2 1.52(2) 26_556 ?
N2 C2 1.52(2) 38 ?
N2 C2 1.52(2) 25_556 ?
N2 C2 1.52(2) 14_556 ?
C2 C2 1.68(4) 37 ?
C2 C2 1.68(4) 38 ?
C2 C3 1.70(3) . ?
C2 C2 1.90(3) 26_556 ?
N3 C4 1.53(3) 33_666 ?
N3 C4 1.53(3) 9 ?
N3 C4 1.53(3) 25_666 ?
N3 C4 1.53(3) 29_666 ?
N3 C4 1.53(3) 5 ?
N3 C4 1.53(3) 35_655 ?
N3 C4 1.53(3) 27_565 ?
N3 C4 1.53(3) 7_665 ?
N3 C4 1.53(3) 31_556 ?
N3 C4 1.53(3) 3_656 ?
N3 C4 1.53(3) 11_566 ?
N3 C4 1.53(3) . ?
C3 C2 1.70(3) 26_556 ?
C4 C4 1.53(3) 11_566 ?
C4 C4 1.53(3) 31_556 ?
C4 C4 1.53(3) 9 ?
C4 C4 1.53(3) 5 ?
C4 C5 1.612(9) 5 ?
C4 C5 1.612(9) . ?
C5 C4 1.612(9) 27_565 ?
C5 C4 1.612(9) 11_566 ?
C5 C4 1.612(9) 9 ?
S1 C1 1.561(11) . ?
C1 N1 1.141(13) . ?

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
N1 Nd1 N1 180.0(4) . 25 ?
N1 Nd1 N1 70.5 . 28 ?
N1 Nd1 N1 109.5 25 28 ?
N1 Nd1 N1 109.5 . 2 ?
N1 Nd1 N1 70.5 25 2 ?
N1 Nd1 N1 70.5 28 2 ?
N1 Nd1 N1 70.5 . 26 ?
N1 Nd1 N1 109.5 25 26 ?
N1 Nd1 N1 109.5 28 26 ?
N1 Nd1 N1 180.0(6) 2 26 ?
N1 Nd1 N1 109.5 . 3 ?
N1 Nd1 N1 70.5 25 3 ?
N1 Nd1 N1 70.5 28 3 ?
N1 Nd1 N1 109.5 2 3 ?
N1 Nd1 N1 70.5 26 3 ?
N1 Nd1 N1 70.5 . 27 ?
N1 Nd1 N1 109.5 25 27 ?
N1 Nd1 N1 109.5 28 27 ?
N1 Nd1 N1 70.5 2 27 ?
N1 Nd1 N1 109.5 26 27 ?
N1 Nd1 N1 180.0(6) 3 27 ?
N1 Nd1 N1 109.5 . 4 ?
N1 Nd1 N1 70.5 25 4 ?
N1 Nd1 N1 180.0(4) 28 4 ?
N1 Nd1 N1 109.5 2 4 ?
N1 Nd1 N1 70.5 26 4 ?
N1 Nd1 N1 109.5 3 4 ?
N1 Nd1 N1 70.5 27 4 ?
C2 N2 C2 67.0(10) . 37 ?
C2 N2 C2 113.0(10) . 13_556 ?
C2 N2 C2 180.0(8) 37 13_556 ?
C2 N2 C2 102.6(18) . 2 ?
C2 N2 C2 67.0(10) 37 2 ?
C2 N2 C2 113.0(10) 13_556 2 ?
C2 N2 C2 77.4(18) . 26_556 ?
C2 N2 C2 113.0(10) 37 26_556 ?
C2 N2 C2 67.0(10) 13_556 26_556 ?
C2 N2 C2 180.0(8) 2 26_556 ?
C2 N2 C2 67.0(10) . 38 ?
C2 N2 C2 102.6(18) 37 38 ?
C2 N2 C2 77.4(18) 13_556 38 ?
C2 N2 C2 67.0(10) 2 38 ?
C2 N2 C2 113.0(10) 26_556 38 ?
C2 N2 C2 180.0 . 25_556 ?
C2 N2 C2 113.0(10) 37 25_556 ?
C2 N2 C2 67.0(10) 13_556 25_556 ?
C2 N2 C2 77.4(18) 2 25_556 ?
C2 N2 C2 102.6(18) 26_556 25_556 ?
C2 N2 C2 113.0(10) 38 25_556 ?
C2 N2 C2 113.0(10) . 14_556 ?
C2 N2 C2 77.4(18) 37 14_556 ?
C2 N2 C2 102.6(18) 13_556 14_556 ?
C2 N2 C2 113.0(10) 2 14_556 ?
C2 N2 C2 67.0(10) 26_556 14_556 ?
C2 N2 C2 180.0(13) 38 14_556 ?
C2 N2 C2 67.0(10) 25_556 14_556 ?
N2 C2 C2 56.5(5) . 37 ?
N2 C2 C2 56.5(5) . 38 ?
C2 C2 C2 90.001(1) 37 38 ?
N2 C2 C3 107.2(11) . . ?
C2 C2 C3 125.9(3) 37 . ?
C2 C2 C3 125.9(3) 38 . ?
N2 C2 C2 51.3(9) . 26_556 ?
C2 C2 C2 90.001(2) 37 26_556 ?
C2 C2 C2 90.001(1) 38 26_556 ?
C3 C2 C2 55.9(7) . 26_556 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 60.000(1) 33_666 25_666 ?
C4 N3 C4 120.000(1) 9 25_666 ?
C4 N3 C4 60.0 33_666 29_666 ?
C4 N3 C4 120.0 9 29_666 ?
C4 N3 C4 60.0 25_666 29_666 ?
C4 N3 C4 120.000(2) 33_666 5 ?
C4 N3 C4 60.000(1) 9 5 ?
C4 N3 C4 120.000(2) 25_666 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 90.000(3) 33_666 35_655 ?
C4 N3 C4 90.000(1) 9 35_655 ?
C4 N3 C4 60.000(2) 25_666 35_655 ?
C4 N3 C4 120.000(2) 29_666 35_655 ?
C4 N3 C4 60.000(2) 5 35_655 ?
C4 N3 C4 120.000(1) 33_666 27_565 ?
C4 N3 C4 60.0 9 27_565 ?
C4 N3 C4 90.0 25_666 27_565 ?
C4 N3 C4 60.000(1) 29_666 27_565 ?
C4 N3 C4 120.000(1) 5 27_565 ?
C4 N3 C4 120.0 35_655 27_565 ?
C4 N3 C4 120.000(2) 33_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 60.0 25_666 7_665 ?
C4 N3 C4 90.000(3) 29_666 7_665 ?
C4 N3 C4 90.000(1) 5 7_665 ?
C4 N3 C4 60.0 35_655 7_665 ?
C4 N3 C4 60.0 27_565 7_665 ?
C4 N3 C4 60.0 33_666 31_556 ?
C4 N3 C4 120.000(2) 9 31_556 ?
C4 N3 C4 120.000(1) 25_666 31_556 ?
C4 N3 C4 90.000(1) 29_666 31_556 ?
C4 N3 C4 90.000(3) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 120.000(1) 27_565 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 60.0 33_666 3_656 ?
C4 N3 C4 120.000(1) 9 3_656 ?
C4 N3 C4 90.000(3) 25_666 3_656 ?
C4 N3 C4 120.000(2) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.0 35_655 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 120.000(2) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 90.000(1) 33_666 11_566 ?
C4 N3 C4 90.000(3) 9 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 60.000(1) 29_666 11_566 ?
C4 N3 C4 120.000(2) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 60.000(1) 27_565 11_566 ?
C4 N3 C4 120.000(2) 7_665 11_566 ?
C4 N3 C4 60.000(1) 31_556 11_566 ?
C4 N3 C4 120.000(1) 3_656 11_566 ?
C4 N3 C4 120.000(2) 33_666 . ?
C4 N3 C4 60.000(2) 9 . ?
C4 N3 C4 180.0 25_666 . ?
C4 N3 C4 120.000(2) 29_666 . ?
C4 N3 C4 60.000(1) 5 . ?
C4 N3 C4 120.000(2) 35_655 . ?
C4 N3 C4 90.000(3) 27_565 . ?
C4 N3 C4 120.000(1) 7_665 . ?
C4 N3 C4 60.000(2) 31_556 . ?
C4 N3 C4 90.000(3) 3_656 . ?
C4 N3 C4 60.000(2) 11_566 . ?
C2 C3 C2 68.1(13) 26_556 . ?
C4 C4 C4 59.999(1) 11_566 31_556 ?
C4 C4 C4 89.999(8) 11_566 9 ?
C4 C4 C4 119.998(13) 31_556 9 ?
C4 C4 C4 119.998(14) 11_566 5 ?
C4 C4 C4 89.999(12) 31_556 5 ?
C4 C4 C4 59.999(1) 9 5 ?
C4 C4 N3 59.999(4) 11_566 . ?
C4 C4 N3 59.999(3) 31_556 . ?
C4 C4 N3 59.999(4) 9 . ?
C4 C4 N3 59.999(3) 5 . ?
C4 C4 C5 121.7(6) 11_566 5 ?
C4 C4 C5 61.7(6) 31_556 5 ?
C4 C4 C5 121.7(6) 9 5 ?
C4 C4 C5 61.7(6) 5 5 ?
N3 C4 C5 92.9(10) . 5 ?
C4 C4 C5 61.7(6) 11_566 . ?
C4 C4 C5 121.7(6) 31_556 . ?
C4 C4 C5 61.7(6) 9 . ?
C4 C4 C5 121.7(6) 5 . ?
N3 C4 C5 92.9(10) . . ?
C5 C4 C5 174(2) 5 . ?
C4 C5 C4 84(2) . 27_565 ?
C4 C5 C4 56.6(12) . 11_566 ?
C4 C5 C4 56.6(12) 27_565 11_566 ?
C4 C5 C4 56.6(12) . 9 ?
C4 C5 C4 56.6(12) 27_565 9 ?
C4 C5 C4 84(2) 11_566 9 ?
N1 C1 S1 180.0(13) . . ?
C1 N1 Nd1 180.0(11) . . ?

_refine_diff_density_max         2.573
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.144

####################################################################### 
# 
# 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_i4mmm_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1956295'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Ho N11 O0 S7'
_chemical_formula_weight         1011.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.4039(4)
_cell_length_b                   11.4039(4)
_cell_length_c                   22.5714(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2935.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25910
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      33.09

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.044
_exptl_absorpt_coefficient_mu    1.628
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3733
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25910
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.804
_diffrn_reflns_theta_max         33.092
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1615
_reflns_number_gt                1615
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1043P)²+2.4878P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1615
_refine_ls_number_parameters     58
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1151
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.006
_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
Ho1 Ho 0.0000 0.0000 0.0000 0.02695(12) Uani 1 16 d S T P . .
S1 S 0.25627(11) 0.25627(11) 0.13194(7) 0.0720(5) Uani 0.875 2 d S T P . .
C1 C 0.1782(3) 0.1782(3) 0.0917(3) 0.0582(12) Uani 0.875 2 d S T P . .
N1 N 0.1210(3) 0.1210(3) 0.0612(3) 0.0746(16) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.102(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5801(11) -0.0524(7) 0.131(6) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1123(7) 0.150(5) Uani 1 4 d DS T P . .
C4 C -0.1054(15) 0.5809(12) 0.0000 0.131(6) Uani 0.5 2 d DS T P . .
C5 C -0.2238(19) 0.5000 0.0000 0.150(5) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2533(3) 0.0528(16) Uani 1 8 d DS T P . .
C6 C 0.1081(11) 0.0000 0.2132(4) 0.084(5) Uani 0.5 2 d DS T P . .
C7 C 0.1056(7) 0.0000 0.2944(3) 0.0494(16) Uani 0.5 2 d DS T P . .
C8 C 0.2259(6) 0.0000 0.2551(5) 0.091(2) Uani 1 2 d DS T P . .


_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
Ho1 N1 2.391(5) . ?
Ho1 N1 2.391(5) 17 ?
Ho1 N1 2.391(5) 20 ?
Ho1 N1 2.391(5) 2 ?
Ho1 N1 2.391(5) 18 ?
Ho1 N1 2.391(5) 3 ?
Ho1 N1 2.391(5) 19 ?
Ho1 N1 2.391(5) 4 ?
S1 C1 1.551(6) . ?
C1 N1 1.152(7) . ?
N2 C2 1.495(12) 18 ?
N2 C2 1.495(12) 2_565 ?
N2 C2 1.495(12) 17_565 ?
N2 C2 1.495(12) . ?
N2 C4 1.515(14) 21_565 ?
N2 C4 1.515(14) 5 ?
N2 C4 1.515(14) 17_565 ?
N2 C4 1.515(14) . ?
C2 C3 1.632(14) . ?
C2 C4 1.687(18) 5 ?
C2 C4 1.687(18) . ?
C2 C2 1.83(3) 2_565 ?
C3 C2 1.632(14) 2_565 ?
C4 C5 1.635(16) . ?
C4 C2 1.687(18) 18 ?
C4 C4 1.85(3) 21_565 ?
C5 C4 1.635(16) 21_565 ?
N3 C7 1.519(8) 3 ?
N3 C7 1.519(8) 4 ?
N3 C7 1.519(8) 2 ?
N3 C7 1.519(8) . ?
N3 C6 1.529(10) 2 ?
N3 C6 1.529(10) 4 ?
N3 C6 1.529(10) 3 ?
N3 C6 1.529(10) . ?
C6 C8 1.643(13) . ?
C6 C6 1.743(19) 4 ?
C6 C6 1.743(19) 3 ?
C6 C7 1.832(11) . ?
C7 C8 1.634(10) . ?
C7 C7 1.702(12) 4 ?
C7 C7 1.702(12) 3 ?

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
N1 Ho1 N1 180.0 . 17 ?
N1 Ho1 N1 109.48(16) . 20 ?
N1 Ho1 N1 70.52(16) 17 20 ?
N1 Ho1 N1 109.4(3) . 2 ?
N1 Ho1 N1 70.6(3) 17 2 ?
N1 Ho1 N1 109.48(16) 20 2 ?
N1 Ho1 N1 70.6(3) . 18 ?
N1 Ho1 N1 109.4(3) 17 18 ?
N1 Ho1 N1 70.52(16) 20 18 ?
N1 Ho1 N1 180.0(4) 2 18 ?
N1 Ho1 N1 70.52(16) . 3 ?
N1 Ho1 N1 109.48(16) 17 3 ?
N1 Ho1 N1 70.6(3) 20 3 ?
N1 Ho1 N1 70.52(16) 2 3 ?
N1 Ho1 N1 109.48(16) 18 3 ?
N1 Ho1 N1 109.48(16) . 19 ?
N1 Ho1 N1 70.52(16) 17 19 ?
N1 Ho1 N1 109.4(3) 20 19 ?
N1 Ho1 N1 109.48(16) 2 19 ?
N1 Ho1 N1 70.52(16) 18 19 ?
N1 Ho1 N1 180.0(3) 3 19 ?
N1 Ho1 N1 70.52(16) . 4 ?
N1 Ho1 N1 109.48(16) 17 4 ?
N1 Ho1 N1 180.0(4) 20 4 ?
N1 Ho1 N1 70.52(16) 2 4 ?
N1 Ho1 N1 109.48(16) 18 4 ?
N1 Ho1 N1 109.4(3) 3 4 ?
N1 Ho1 N1 70.6(3) 19 4 ?
N1 C1 S1 179.0(7) . . ?
C1 N1 Ho1 178.5(6) . . ?
C2 N2 C2 180.0(8) 18 2_565 ?
C2 N2 C2 75.3(13) 18 17_565 ?
C2 N2 C2 104.7(13) 2_565 17_565 ?
C2 N2 C2 104.7(13) 18 . ?
C2 N2 C2 75.3(13) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 111.9(5) 18 21_565 ?
C2 N2 C4 68.1(5) 2_565 21_565 ?
C2 N2 C4 68.1(5) 17_565 21_565 ?
C2 N2 C4 111.9(5) . 21_565 ?
C2 N2 C4 68.1(5) 18 5 ?
C2 N2 C4 111.9(5) 2_565 5 ?
C2 N2 C4 111.9(5) 17_565 5 ?
C2 N2 C4 68.1(5) . 5 ?
C4 N2 C4 180.0(8) 21_565 5 ?
C2 N2 C4 111.9(5) 18 17_565 ?
C2 N2 C4 68.1(5) 2_565 17_565 ?
C2 N2 C4 68.1(5) 17_565 17_565 ?
C2 N2 C4 111.9(5) . 17_565 ?
C4 N2 C4 105.0(13) 21_565 17_565 ?
C4 N2 C4 75.0(13) 5 17_565 ?
C2 N2 C4 68.1(5) 18 . ?
C2 N2 C4 111.9(5) 2_565 . ?
C2 N2 C4 111.9(5) 17_565 . ?
C2 N2 C4 68.1(5) . . ?
C4 N2 C4 75.0(13) 21_565 . ?
C4 N2 C4 105.0(13) 5 . ?
C4 N2 C4 180.0(8) 17_565 . ?
N2 C2 C3 108.3(10) . . ?
N2 C2 C4 56.5(5) . 5 ?
C3 C2 C4 125.8(8) . 5 ?
N2 C2 C4 56.5(5) . . ?
C3 C2 C4 125.8(8) . . ?
C4 C2 C4 90.9(10) 5 . ?
N2 C2 C2 52.3(6) . 2_565 ?
C3 C2 C2 55.9(5) . 2_565 ?
C4 C2 C2 90.3(6) 5 2_565 ?
C4 C2 C2 90.3(6) . 2_565 ?
C2 C3 C2 68.1(9) . 2_565 ?
N2 C4 C5 108.1(11) . . ?
N2 C4 C2 55.4(5) . 18 ?
C5 C4 C2 125.8(9) . 18 ?
N2 C4 C2 55.4(5) . . ?
C5 C4 C2 125.8(9) . . ?
C2 C4 C2 89.1(10) 18 . ?
N2 C4 C4 52.5(6) . 21_565 ?
C5 C4 C4 55.7(6) . 21_565 ?
C2 C4 C4 89.7(6) 18 21_565 ?
C2 C4 C4 89.7(6) . 21_565 ?
C4 C5 C4 68.7(12) . 21_565 ?
C7 N3 C7 104.8(8) 3 4 ?
C7 N3 C7 68.2(4) 3 2 ?
C7 N3 C7 68.2(4) 4 2 ?
C7 N3 C7 68.2(4) 3 . ?
C7 N3 C7 68.2(4) 4 . ?
C7 N3 C7 104.8(8) 2 . ?
C7 N3 C6 111.2(3) 3 2 ?
C7 N3 C6 111.2(3) 4 2 ?
C7 N3 C6 73.9(6) 2 2 ?
C7 N3 C6 178.7(8) . 2 ?
C7 N3 C6 178.7(8) 3 4 ?
C7 N3 C6 73.9(6) 4 4 ?
C7 N3 C6 111.2(3) 2 4 ?
C7 N3 C6 111.2(3) . 4 ?
C6 N3 C6 69.5(6) 2 4 ?
C7 N3 C6 73.9(6) 3 3 ?
C7 N3 C6 178.7(8) 4 3 ?
C7 N3 C6 111.2(3) 2 3 ?
C7 N3 C6 111.2(3) . 3 ?
C6 N3 C6 69.5(6) 2 3 ?
C6 N3 C6 107.4(11) 4 3 ?
C7 N3 C6 111.2(3) 3 . ?
C7 N3 C6 111.2(3) 4 . ?
C7 N3 C6 178.7(8) 2 . ?
C7 N3 C6 73.9(6) . . ?
C6 N3 C6 107.4(11) 2 . ?
C6 N3 C6 69.5(6) 4 . ?
C6 N3 C6 69.5(6) 3 . ?
N3 C6 C8 108.6(6) . . ?
N3 C6 C6 55.3(3) . 4 ?
C8 C6 C6 125.3(2) . 4 ?
N3 C6 C6 55.3(3) . 3 ?
C8 C6 C6 125.3(2) . 3 ?
C6 C6 C6 90.001(1) 4 3 ?
N3 C6 C7 52.8(4) . . ?
C8 C6 C7 55.8(4) . . ?
C6 C6 C7 89.4(3) 4 . ?
C6 C6 C7 89.4(3) 3 . ?
N3 C7 C8 109.5(6) . . ?
N3 C7 C7 55.9(2) . 4 ?
C8 C7 C7 126.4(2) . 4 ?
N3 C7 C7 55.9(2) . 3 ?
C8 C7 C7 126.4(2) . 3 ?
C7 C7 C7 90.000(1) 4 3 ?
N3 C7 C6 53.3(5) . . ?
C8 C7 C6 56.2(5) . . ?
C7 C7 C6 90.6(3) 4 . ?
C7 C7 C6 90.6(3) 3 . ?
C7 C8 C6 68.0(5) . . ?

_refine_diff_density_max         1.017
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.123

####################################################################### 
# 
# 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_i4mmm_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1956296'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 O0 S7 Tm'
_chemical_formula_weight         1015.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.3875(10)
_cell_length_b                   11.3875(10)
_cell_length_c                   22.478(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2914.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25512
_cell_measurement_theta_min      1.812
_cell_measurement_theta_max      33.060

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    1.804
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3622
_exptl_absorpt_correction_T_max  0.4351
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25512
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.812
_diffrn_reflns_theta_max         33.060
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1582
_reflns_number_gt                1581
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0987P)²+1.7293P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1582
_refine_ls_number_parameters     59
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_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
Tm1 Tm 0.0000 0.0000 0.0000 0.02591(12) Uani 1 16 d S T P . .
S1 S 0.25587(11) 0.25587(11) 0.13164(7) 0.0704(5) Uani 0.875 2 d S T P . .
C1 C 0.1773(4) 0.1773(4) 0.0913(3) 0.0587(13) Uani 0.875 2 d S T P . .
N1 N 0.1202(4) 0.1202(4) 0.0603(3) 0.0763(18) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.103(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5795(12) -0.0528(7) 0.126(6) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1132(7) 0.150(6) Uani 1 4 d DS T P . .
C4 C -0.1046(15) 0.5814(12) 0.0000 0.126(6) Uani 0.5 2 d DS T P . .
C5 C -0.2223(19) 0.5000 0.0000 0.150(6) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2536(4) 0.0501(16) Uani 1 8 d DS T P . .
C6 C 0.1076(12) 0.0000 0.2131(4) 0.080(5) Uani 0.5 2 d DS T P . .
C7 C 0.1053(7) 0.0000 0.2948(4) 0.0482(17) Uani 0.5 2 d DS T P . .
C8 C 0.2256(7) 0.0000 0.2552(5) 0.089(2) Uani 1 2 d DS T P . .


_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
Tm1 N1 2.364(6) 17 ?
Tm1 N1 2.364(6) 20 ?
Tm1 N1 2.364(6) 4 ?
Tm1 N1 2.364(6) 2 ?
Tm1 N1 2.364(6) 18 ?
Tm1 N1 2.364(6) 3 ?
Tm1 N1 2.364(6) 19 ?
Tm1 N1 2.364(6) . ?
S1 C1 1.557(6) . ?
C1 N1 1.152(7) . ?
N2 C2 1.493(12) . ?
N2 C2 1.493(12) 18 ?
N2 C2 1.493(12) 2_565 ?
N2 C2 1.493(12) 17_565 ?
N2 C4 1.509(14) . ?
N2 C4 1.509(14) 21_565 ?
N2 C4 1.509(14) 5 ?
N2 C4 1.509(14) 17_565 ?
C2 C3 1.631(15) . ?
C2 C4 1.682(18) 5 ?
C2 C4 1.682(18) . ?
C2 C2 1.81(3) 2_565 ?
C3 C2 1.631(15) 2_565 ?
C4 C5 1.629(16) . ?
C4 C2 1.682(18) 18 ?
C4 C4 1.85(3) 21_565 ?
C5 C4 1.629(16) 21_565 ?
N3 C7 1.516(8) . ?
N3 C7 1.516(8) 3 ?
N3 C7 1.516(8) 4 ?
N3 C7 1.516(8) 2 ?
N3 C6 1.527(10) 2 ?
N3 C6 1.527(10) 4 ?
N3 C6 1.527(10) 3 ?
N3 C6 1.527(10) . ?
C6 C8 1.644(14) . ?
C6 C6 1.733(19) 4 ?
C6 C6 1.733(19) 3 ?
C6 C7 1.837(12) . ?
C7 C8 1.634(10) . ?
C7 C7 1.697(12) 4 ?
C7 C7 1.697(12) 3 ?

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
N1 Tm1 N1 70.79(18) 17 20 ?
N1 Tm1 N1 109.21(18) 17 4 ?
N1 Tm1 N1 180.0(4) 20 4 ?
N1 Tm1 N1 70.0(4) 17 2 ?
N1 Tm1 N1 109.21(18) 20 2 ?
N1 Tm1 N1 70.79(18) 4 2 ?
N1 Tm1 N1 110.0(4) 17 18 ?
N1 Tm1 N1 70.79(18) 20 18 ?
N1 Tm1 N1 109.21(18) 4 18 ?
N1 Tm1 N1 180.0(3) 2 18 ?
N1 Tm1 N1 109.21(18) 17 3 ?
N1 Tm1 N1 70.0(4) 20 3 ?
N1 Tm1 N1 110.0(4) 4 3 ?
N1 Tm1 N1 70.79(18) 2 3 ?
N1 Tm1 N1 109.21(18) 18 3 ?
N1 Tm1 N1 70.79(18) 17 19 ?
N1 Tm1 N1 110.0(4) 20 19 ?
N1 Tm1 N1 70.0(4) 4 19 ?
N1 Tm1 N1 109.21(18) 2 19 ?
N1 Tm1 N1 70.79(18) 18 19 ?
N1 Tm1 N1 180.0(3) 3 19 ?
N1 Tm1 N1 180.0 17 . ?
N1 Tm1 N1 109.21(18) 20 . ?
N1 Tm1 N1 70.79(18) 4 . ?
N1 Tm1 N1 110.0(4) 2 . ?
N1 Tm1 N1 70.0(4) 18 . ?
N1 Tm1 N1 70.79(18) 3 . ?
N1 Tm1 N1 109.21(18) 19 . ?
N1 C1 S1 178.5(7) . . ?
C1 N1 Tm1 177.8(6) . . ?
C2 N2 C2 105.4(13) . 18 ?
C2 N2 C2 74.6(13) . 2_565 ?
C2 N2 C2 180.0(8) 18 2_565 ?
C2 N2 C2 180.0 . 17_565 ?
C2 N2 C2 74.6(13) 18 17_565 ?
C2 N2 C2 105.4(13) 2_565 17_565 ?
C2 N2 C4 68.1(5) . . ?
C2 N2 C4 68.1(5) 18 . ?
C2 N2 C4 111.9(5) 2_565 . ?
C2 N2 C4 111.9(5) 17_565 . ?
C2 N2 C4 111.9(5) . 21_565 ?
C2 N2 C4 111.9(5) 18 21_565 ?
C2 N2 C4 68.1(5) 2_565 21_565 ?
C2 N2 C4 68.1(5) 17_565 21_565 ?
C4 N2 C4 75.8(13) . 21_565 ?
C2 N2 C4 68.1(5) . 5 ?
C2 N2 C4 68.1(5) 18 5 ?
C2 N2 C4 111.9(5) 2_565 5 ?
C2 N2 C4 111.9(5) 17_565 5 ?
C4 N2 C4 104.2(13) . 5 ?
C4 N2 C4 180.0(8) 21_565 5 ?
C2 N2 C4 111.9(5) . 17_565 ?
C2 N2 C4 111.9(5) 18 17_565 ?
C2 N2 C4 68.1(5) 2_565 17_565 ?
C2 N2 C4 68.1(5) 17_565 17_565 ?
C4 N2 C4 180.0 . 17_565 ?
C4 N2 C4 104.2(13) 21_565 17_565 ?
C4 N2 C4 75.8(13) 5 17_565 ?
N2 C2 C3 109.0(10) . . ?
N2 C2 C4 56.4(5) . 5 ?
C3 C2 C4 126.5(8) . 5 ?
N2 C2 C4 56.4(5) . . ?
C3 C2 C4 126.5(8) . . ?
C4 C2 C4 90.1(10) 5 . ?
N2 C2 C2 52.7(6) . 2_565 ?
C3 C2 C2 56.3(5) . 2_565 ?
C4 C2 C2 90.7(6) 5 2_565 ?
C4 C2 C2 90.7(6) . 2_565 ?
C2 C3 C2 67.4(10) 2_565 . ?
N2 C4 C5 107.5(11) . . ?
N2 C4 C2 55.5(5) . . ?
C5 C4 C2 125.1(9) . . ?
N2 C4 C2 55.5(5) . 18 ?
C5 C4 C2 125.1(9) . 18 ?
C2 C4 C2 89.8(10) . 18 ?
N2 C4 C4 52.1(6) . 21_565 ?
C5 C4 C4 55.3(6) . 21_565 ?
C2 C4 C4 89.3(6) . 21_565 ?
C2 C4 C4 89.3(6) 18 21_565 ?
C4 C5 C4 69.3(12) . 21_565 ?
C7 N3 C7 68.1(4) . 3 ?
C7 N3 C7 68.1(4) . 4 ?
C7 N3 C7 104.6(8) 3 4 ?
C7 N3 C7 104.6(8) . 2 ?
C7 N3 C7 68.1(4) 3 2 ?
C7 N3 C7 68.1(4) 4 2 ?
C7 N3 C6 178.9(8) . 2 ?
C7 N3 C6 111.4(3) 3 2 ?
C7 N3 C6 111.4(3) 4 2 ?
C7 N3 C6 74.3(6) 2 2 ?
C7 N3 C6 111.4(3) . 4 ?
C7 N3 C6 178.9(8) 3 4 ?
C7 N3 C6 74.3(6) 4 4 ?
C7 N3 C6 111.4(3) 2 4 ?
C6 N3 C6 69.2(6) 2 4 ?
C7 N3 C6 111.4(3) . 3 ?
C7 N3 C6 74.3(6) 3 3 ?
C7 N3 C6 178.9(8) 4 3 ?
C7 N3 C6 111.4(3) 2 3 ?
C6 N3 C6 69.2(6) 2 3 ?
C6 N3 C6 106.8(11) 4 3 ?
C7 N3 C6 74.3(6) . . ?
C7 N3 C6 111.4(3) 3 . ?
C7 N3 C6 111.4(3) 4 . ?
C7 N3 C6 178.9(8) 2 . ?
C6 N3 C6 106.8(11) 2 . ?
C6 N3 C6 69.2(6) 4 . ?
C6 N3 C6 69.2(6) 3 . ?
N3 C6 C8 108.2(6) . . ?
N3 C6 C6 55.4(3) . 4 ?
C8 C6 C6 125.3(2) . 4 ?
N3 C6 C6 55.4(3) . 3 ?
C8 C6 C6 125.3(2) . 3 ?
C6 C6 C6 89.999(1) 4 3 ?
N3 C6 C7 52.6(4) . . ?
C8 C6 C7 55.6(5) . . ?
C6 C6 C7 89.4(3) 4 . ?
C6 C6 C7 89.4(3) 3 . ?
N3 C7 C8 109.3(6) . . ?
N3 C7 C7 56.0(2) . 4 ?
C8 C7 C7 126.4(2) . 4 ?
N3 C7 C7 56.0(2) . 3 ?
C8 C7 C7 126.4(2) . 3 ?
C7 C7 C7 90.000(1) 4 3 ?
N3 C7 C6 53.1(5) . . ?
C8 C7 C6 56.2(5) . . ?
C7 C7 C6 90.6(3) 4 . ?
C7 C7 C6 90.6(3) 3 . ?
C7 C8 C6 68.2(5) . . ?

_refine_diff_density_max         0.966
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.125

####################################################################### 
# 
# 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_i4mmm_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1956297'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Dy N11 O0 S7'
_chemical_formula_weight         1009.42

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.4134(6)
_cell_length_b                   11.4134(6)
_cell_length_c                   22.6144(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2945.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21181
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      30.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_F_000             978
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.547
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3837
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21181
_diffrn_reflns_av_unetI/netI     0.0070
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.801
_diffrn_reflns_theta_max         30.465
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1310
_reflns_number_gt                1310
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0985P)²+2.5740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1310
_refine_ls_number_parameters     58
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1132
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.033
_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
Dy1 Dy 0.0000 0.0000 0.0000 0.02758(16) Uani 1 16 d S T P . .
S1 S 0.25638(12) 0.25638(12) 0.13203(8) 0.0734(5) Uani 0.875 2 d S T P . .
C1 C 0.1779(4) 0.1779(4) 0.0916(3) 0.0608(13) Uani 0.875 2 d S T P . .
N1 N 0.1215(4) 0.1215(4) 0.0615(3) 0.0799(18) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.104(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5799(12) -0.0528(7) 0.133(6) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1124(7) 0.147(5) Uani 1 4 d DS T P . .
C4 C -0.1058(15) 0.5805(12) 0.0000 0.133(6) Uani 0.5 2 d DS T P . .
C5 C -0.2240(18) 0.5000 0.0000 0.147(5) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2534(4) 0.0547(19) Uani 1 8 d DS T P . .
C6 C 0.1081(12) 0.0000 0.2133(4) 0.086(5) Uani 0.5 2 d DS T P . .
C7 C 0.1060(8) 0.0000 0.2942(3) 0.0519(19) Uani 0.5 2 d DS T P . .
C8 C 0.2259(7) 0.0000 0.2548(5) 0.092(2) Uani 1 2 d DS T P . .


_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
Dy1 N1 2.403(6) . ?
Dy1 N1 2.404(6) 17 ?
Dy1 N1 2.404(6) 20 ?
Dy1 N1 2.404(6) 2 ?
Dy1 N1 2.404(6) 18 ?
Dy1 N1 2.404(6) 3 ?
Dy1 N1 2.404(6) 19 ?
Dy1 N1 2.404(6) 4 ?
S1 C1 1.563(6) . ?
C1 N1 1.136(7) . ?
N2 C2 1.502(12) 18 ?
N2 C2 1.502(12) 2_565 ?
N2 C2 1.502(12) 17_565 ?
N2 C2 1.502(12) . ?
N2 C4 1.518(14) 21_565 ?
N2 C4 1.518(14) 5 ?
N2 C4 1.518(14) 17_565 ?
N2 C4 1.518(14) . ?
C2 C3 1.628(14) . ?
C2 C4 1.698(18) 5 ?
C2 C4 1.698(18) . ?
C2 C2 1.82(3) 2_565 ?
C3 C2 1.628(14) 2_565 ?
C4 C5 1.632(15) . ?
C4 C2 1.698(18) 18 ?
C4 C4 1.84(3) 21_565 ?
C5 C4 1.632(15) 21_565 ?
N3 C7 1.520(9) 3 ?
N3 C7 1.520(9) . ?
N3 C7 1.520(9) 4 ?
N3 C7 1.520(9) 2 ?
N3 C6 1.531(10) 2 ?
N3 C6 1.531(10) 4 ?
N3 C6 1.531(10) 3 ?
N3 C6 1.531(10) . ?
C6 C8 1.640(13) . ?
C6 C6 1.745(19) 4 ?
C6 C6 1.745(19) 3 ?
C6 C7 1.828(11) . ?
C7 C8 1.633(10) . ?
C7 C7 1.710(12) 4 ?
C7 C7 1.710(12) 3 ?

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
N1 Dy1 N1 180.0 . 17 ?
N1 Dy1 N1 109.55(16) . 20 ?
N1 Dy1 N1 70.45(16) 17 20 ?
N1 Dy1 N1 109.3(3) . 2 ?
N1 Dy1 N1 70.7(3) 17 2 ?
N1 Dy1 N1 109.55(16) 20 2 ?
N1 Dy1 N1 70.7(3) . 18 ?
N1 Dy1 N1 109.3(3) 17 18 ?
N1 Dy1 N1 70.45(16) 20 18 ?
N1 Dy1 N1 180.0(4) 2 18 ?
N1 Dy1 N1 70.45(16) . 3 ?
N1 Dy1 N1 109.55(16) 17 3 ?
N1 Dy1 N1 70.7(3) 20 3 ?
N1 Dy1 N1 70.45(16) 2 3 ?
N1 Dy1 N1 109.55(16) 18 3 ?
N1 Dy1 N1 109.55(16) . 19 ?
N1 Dy1 N1 70.45(16) 17 19 ?
N1 Dy1 N1 109.3(3) 20 19 ?
N1 Dy1 N1 109.55(16) 2 19 ?
N1 Dy1 N1 70.45(16) 18 19 ?
N1 Dy1 N1 180.0(3) 3 19 ?
N1 Dy1 N1 70.45(16) . 4 ?
N1 Dy1 N1 109.55(16) 17 4 ?
N1 Dy1 N1 180.0(4) 20 4 ?
N1 Dy1 N1 70.45(16) 2 4 ?
N1 Dy1 N1 109.55(16) 18 4 ?
N1 Dy1 N1 109.3(3) 3 4 ?
N1 Dy1 N1 70.7(3) 19 4 ?
N1 C1 S1 179.1(7) . . ?
C1 N1 Dy1 178.6(6) . . ?
C2 N2 C2 180.0(8) 18 2_565 ?
C2 N2 C2 74.8(13) 18 17_565 ?
C2 N2 C2 105.2(13) 2_565 17_565 ?
C2 N2 C2 105.2(13) 18 . ?
C2 N2 C2 74.8(13) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 111.6(5) 18 21_565 ?
C2 N2 C4 68.4(5) 2_565 21_565 ?
C2 N2 C4 68.4(5) 17_565 21_565 ?
C2 N2 C4 111.6(5) . 21_565 ?
C2 N2 C4 68.4(5) 18 5 ?
C2 N2 C4 111.6(5) 2_565 5 ?
C2 N2 C4 111.6(5) 17_565 5 ?
C2 N2 C4 68.4(5) . 5 ?
C4 N2 C4 180.0(8) 21_565 5 ?
C2 N2 C4 111.6(5) 18 17_565 ?
C2 N2 C4 68.4(5) 2_565 17_565 ?
C2 N2 C4 68.4(5) 17_565 17_565 ?
C2 N2 C4 111.6(5) . 17_565 ?
C4 N2 C4 105.5(13) 21_565 17_565 ?
C4 N2 C4 74.5(13) 5 17_565 ?
C2 N2 C4 68.4(5) 18 . ?
C2 N2 C4 111.6(5) 2_565 . ?
C2 N2 C4 111.6(5) 17_565 . ?
C2 N2 C4 68.4(5) . . ?
C4 N2 C4 74.5(13) 21_565 . ?
C4 N2 C4 105.5(13) 5 . ?
C4 N2 C4 180.0 17_565 . ?
N2 C2 C3 108.5(10) . . ?
N2 C2 C4 56.2(5) . 5 ?
C3 C2 C4 125.8(8) . 5 ?
N2 C2 C4 56.2(5) . . ?
C3 C2 C4 125.8(8) . . ?
C4 C2 C4 90.7(10) 5 . ?
N2 C2 C2 52.6(7) . 2_565 ?
C3 C2 C2 55.9(5) . 2_565 ?
C4 C2 C2 90.2(7) 5 2_565 ?
C4 C2 C2 90.2(7) . 2_565 ?
C2 C3 C2 68.1(10) . 2_565 ?
N2 C4 C5 108.5(11) . . ?
N2 C4 C2 55.3(5) . 18 ?
C5 C4 C2 125.8(9) . 18 ?
N2 C4 C2 55.3(5) . . ?
C5 C4 C2 125.8(9) . . ?
C2 C4 C2 89.3(10) 18 . ?
N2 C4 C4 52.7(6) . 21_565 ?
C5 C4 C4 55.7(6) . 21_565 ?
C2 C4 C4 89.8(7) 18 21_565 ?
C2 C4 C4 89.8(7) . 21_565 ?
C4 C5 C4 68.6(12) . 21_565 ?
C7 N3 C7 68.4(4) 3 . ?
C7 N3 C7 105.4(9) 3 4 ?
C7 N3 C7 68.4(4) . 4 ?
C7 N3 C7 68.4(4) 3 2 ?
C7 N3 C7 105.4(9) . 2 ?
C7 N3 C7 68.4(4) 4 2 ?
C7 N3 C6 111.0(3) 3 2 ?
C7 N3 C6 179.0(8) . 2 ?
C7 N3 C6 111.0(3) 4 2 ?
C7 N3 C6 73.6(6) 2 2 ?
C7 N3 C6 179.0(8) 3 4 ?
C7 N3 C6 111.0(3) . 4 ?
C7 N3 C6 73.6(6) 4 4 ?
C7 N3 C6 111.0(3) 2 4 ?
C6 N3 C6 69.5(6) 2 4 ?
C7 N3 C6 73.6(6) 3 3 ?
C7 N3 C6 111.0(3) . 3 ?
C7 N3 C6 179.0(8) 4 3 ?
C7 N3 C6 111.0(3) 2 3 ?
C6 N3 C6 69.5(6) 2 3 ?
C6 N3 C6 107.4(11) 4 3 ?
C7 N3 C6 111.0(3) 3 . ?
C7 N3 C6 73.6(6) . . ?
C7 N3 C6 111.0(3) 4 . ?
C7 N3 C6 179.0(8) 2 . ?
C6 N3 C6 107.4(11) 2 . ?
C6 N3 C6 69.5(6) 4 . ?
C6 N3 C6 69.5(6) 3 . ?
N3 C6 C8 108.8(6) . . ?
N3 C6 C6 55.3(3) . 4 ?
C8 C6 C6 125.4(2) . 4 ?
N3 C6 C6 55.3(3) . 3 ?
C8 C6 C6 125.4(2) . 3 ?
C6 C6 C6 89.998(1) 4 3 ?
N3 C6 C7 52.9(4) . . ?
C8 C6 C7 55.9(5) . . ?
C6 C6 C7 89.5(4) 4 . ?
C6 C6 C7 89.5(4) 3 . ?
N3 C7 C8 109.7(6) . . ?
N3 C7 C7 55.8(2) . 4 ?
C8 C7 C7 126.4(2) . 4 ?
N3 C7 C7 55.8(2) . 3 ?
C8 C7 C7 126.4(2) . 3 ?
C7 C7 C7 90.001(1) 4 3 ?
N3 C7 C6 53.5(5) . . ?
C8 C7 C6 56.2(5) . . ?
C7 C7 C6 90.5(4) 4 . ?
C7 C7 C6 90.5(4) 3 . ?
C7 C8 C6 67.9(5) . . ?

_refine_diff_density_max         0.906
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.117

####################################################################### 
# 
# 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_i4mmm_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 1956299'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Er N11 O0 S7'
_chemical_formula_weight         1014.18

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.4093(6)
_cell_length_b                   11.4093(6)
_cell_length_c                   22.5770(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2938.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21183
_cell_measurement_theta_min      1.804
_cell_measurement_theta_max      30.552

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             982
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.707
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3721
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21183
_diffrn_reflns_av_unetI/netI     0.0082
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.804
_diffrn_reflns_theta_max         30.552
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1317
_reflns_number_gt                1316
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0941P)²+2.4335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1317
_refine_ls_number_parameters     57
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.092
_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
Er1 Er 0.0000 0.0000 0.0000 0.02739(16) Uani 1 16 d S T P . .
S1 S 0.25546(12) 0.25546(12) 0.13194(8) 0.0723(5) Uani 0.875 2 d S T P . .
C1 C 0.1769(4) 0.1769(4) 0.0914(3) 0.0597(14) Uani 0.875 2 d S T P . .
N1 N 0.1202(4) 0.1202(4) 0.0613(3) 0.0749(18) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.108(6) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5811(12) -0.0524(8) 0.129(6) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1117(8) 0.144(6) Uani 1 4 d DS T P . .
C4 C -0.1050(16) 0.5819(13) 0.0000 0.129(6) Uani 0.5 2 d DS T P . .
C5 C -0.222(2) 0.5000 0.0000 0.160(9) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2539(4) 0.0537(19) Uani 1 8 d DS T P . .
C6 C 0.1073(10) 0.0000 0.2131(4) 0.0610(17) Uani 0.5 2 d DS T P . .
C7 C 0.1052(10) 0.0000 0.2952(4) 0.0610(17) Uani 0.5 2 d DS T P . .
C8 C 0.2252(7) 0.0000 0.2552(5) 0.090(2) Uani 1 2 d DS T P . .


_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
Er1 N1 2.384(6) . ?
Er1 N1 2.384(6) 17 ?
Er1 N1 2.384(6) 20 ?
Er1 N1 2.384(6) 2 ?
Er1 N1 2.384(6) 18 ?
Er1 N1 2.384(6) 3 ?
Er1 N1 2.384(6) 19 ?
Er1 N1 2.384(6) 4 ?
S1 C1 1.564(6) . ?
C1 N1 1.139(8) . ?
N2 C2 1.503(12) 18 ?
N2 C2 1.503(12) 2_565 ?
N2 C2 1.503(12) 17_565 ?
N2 C2 1.503(12) . ?
N2 C4 1.519(14) 21_565 ?
N2 C4 1.519(14) 5 ?
N2 C4 1.519(14) 17_565 ?
N2 C4 1.519(14) . ?
C2 C3 1.628(15) . ?
C2 C4 1.684(19) 5 ?
C2 C4 1.684(19) . ?
C2 C2 1.85(3) 2_565 ?
C3 C2 1.628(15) 2_565 ?
C4 C5 1.631(16) . ?
C4 C2 1.684(19) 18 ?
C4 C4 1.87(3) 21_565 ?
C5 C4 1.631(16) 21_565 ?
N3 C7 1.520(11) 3 ?
N3 C7 1.520(11) 4 ?
N3 C7 1.520(11) 2 ?
N3 C7 1.520(11) . ?
N3 C6 1.531(10) 2 ?
N3 C6 1.531(10) 4 ?
N3 C6 1.531(10) 3 ?
N3 C6 1.531(10) . ?
C6 C8 1.647(12) . ?
C6 C6 1.731(16) 4 ?
C6 C6 1.731(16) 3 ?
C6 C7 1.853(12) . ?
C7 C8 1.640(12) . ?
C7 C7 1.697(16) 4 ?
C7 C7 1.697(16) 3 ?

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
N1 Er1 N1 180.0 . 17 ?
N1 Er1 N1 109.73(17) . 20 ?
N1 Er1 N1 70.27(17) 17 20 ?
N1 Er1 N1 109.0(3) . 2 ?
N1 Er1 N1 71.0(3) 17 2 ?
N1 Er1 N1 109.73(17) 20 2 ?
N1 Er1 N1 71.0(3) . 18 ?
N1 Er1 N1 109.0(3) 17 18 ?
N1 Er1 N1 70.27(17) 20 18 ?
N1 Er1 N1 180.0(4) 2 18 ?
N1 Er1 N1 70.27(17) . 3 ?
N1 Er1 N1 109.73(17) 17 3 ?
N1 Er1 N1 71.0(3) 20 3 ?
N1 Er1 N1 70.27(17) 2 3 ?
N1 Er1 N1 109.73(17) 18 3 ?
N1 Er1 N1 109.73(17) . 19 ?
N1 Er1 N1 70.27(17) 17 19 ?
N1 Er1 N1 109.0(3) 20 19 ?
N1 Er1 N1 109.73(17) 2 19 ?
N1 Er1 N1 70.27(17) 18 19 ?
N1 Er1 N1 180.0(3) 3 19 ?
N1 Er1 N1 70.27(17) . 4 ?
N1 Er1 N1 109.73(17) 17 4 ?
N1 Er1 N1 180.0(4) 20 4 ?
N1 Er1 N1 70.27(17) 2 4 ?
N1 Er1 N1 109.73(17) 18 4 ?
N1 Er1 N1 109.0(3) 3 4 ?
N1 Er1 N1 71.0(3) 19 4 ?
N1 C1 S1 179.2(7) . . ?
C1 N1 Er1 178.9(6) . . ?
C2 N2 C2 180.0(9) 18 2_565 ?
C2 N2 C2 76.0(14) 18 17_565 ?
C2 N2 C2 104.0(14) 2_565 17_565 ?
C2 N2 C2 104.0(14) 18 . ?
C2 N2 C2 76.0(14) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 112.3(5) 18 21_565 ?
C2 N2 C4 67.7(5) 2_565 21_565 ?
C2 N2 C4 67.7(5) 17_565 21_565 ?
C2 N2 C4 112.3(5) . 21_565 ?
C2 N2 C4 67.7(5) 18 5 ?
C2 N2 C4 112.3(5) 2_565 5 ?
C2 N2 C4 112.3(5) 17_565 5 ?
C2 N2 C4 67.7(5) . 5 ?
C4 N2 C4 180.0(9) 21_565 5 ?
C2 N2 C4 112.3(5) 18 17_565 ?
C2 N2 C4 67.7(5) 2_565 17_565 ?
C2 N2 C4 67.7(5) 17_565 17_565 ?
C2 N2 C4 112.3(5) . 17_565 ?
C4 N2 C4 104.1(14) 21_565 17_565 ?
C4 N2 C4 75.9(14) 5 17_565 ?
C2 N2 C4 67.7(5) 18 . ?
C2 N2 C4 112.3(5) 2_565 . ?
C2 N2 C4 112.3(5) 17_565 . ?
C2 N2 C4 67.7(5) . . ?
C4 N2 C4 75.9(14) 21_565 . ?
C4 N2 C4 104.1(14) 5 . ?
C4 N2 C4 180.0 17_565 . ?
N2 C2 C3 107.3(11) . . ?
N2 C2 C4 56.6(5) . 5 ?
C3 C2 C4 125.5(9) . 5 ?
N2 C2 C4 56.6(5) . . ?
C3 C2 C4 125.5(9) . . ?
C4 C2 C4 90.7(11) 5 . ?
N2 C2 C2 52.0(7) . 2_565 ?
C3 C2 C2 55.3(5) . 2_565 ?
C4 C2 C2 90.3(7) 5 2_565 ?
C4 C2 C2 90.3(7) . 2_565 ?
C2 C3 C2 69.3(11) 2_565 . ?
N2 C4 C5 107.1(12) . . ?
N2 C4 C2 55.7(5) . . ?
C5 C4 C2 125.5(10) . . ?
N2 C4 C2 55.7(5) . 18 ?
C5 C4 C2 125.5(10) . 18 ?
C2 C4 C2 89.3(11) . 18 ?
N2 C4 C4 52.1(7) . 21_565 ?
C5 C4 C4 55.1(7) . 21_565 ?
C2 C4 C4 89.7(7) . 21_565 ?
C2 C4 C4 89.7(7) 18 21_565 ?
C4 C5 C4 69.9(13) . 21_565 ?
C7 N3 C7 104.3(9) 3 4 ?
C7 N3 C7 67.9(5) 3 2 ?
C7 N3 C7 67.9(5) 4 2 ?
C7 N3 C7 67.9(5) 3 . ?
C7 N3 C7 67.9(5) 4 . ?
C7 N3 C7 104.3(9) 2 . ?
C7 N3 C6 111.6(3) 3 2 ?
C7 N3 C6 111.6(3) 4 2 ?
C7 N3 C6 74.8(5) 2 2 ?
C7 N3 C6 179.1(8) . 2 ?
C7 N3 C6 179.1(8) 3 4 ?
C7 N3 C6 74.8(5) 4 4 ?
C7 N3 C6 111.6(3) 2 4 ?
C7 N3 C6 111.6(3) . 4 ?
C6 N3 C6 68.9(5) 2 4 ?
C7 N3 C6 74.8(5) 3 3 ?
C7 N3 C6 179.1(8) 4 3 ?
C7 N3 C6 111.6(3) 2 3 ?
C7 N3 C6 111.6(3) . 3 ?
C6 N3 C6 68.9(5) 2 3 ?
C6 N3 C6 106.2(10) 4 3 ?
C7 N3 C6 111.6(3) 3 . ?
C7 N3 C6 111.6(3) 4 . ?
C7 N3 C6 179.1(8) 2 . ?
C7 N3 C6 74.8(5) . . ?
C6 N3 C6 106.2(10) 2 . ?
C6 N3 C6 68.8(5) 4 . ?
C6 N3 C6 68.8(5) 3 . ?
N3 C6 C8 107.9(6) . . ?
N3 C6 C6 55.6(3) . 4 ?
C8 C6 C6 125.3(2) . 4 ?
N3 C6 C6 55.6(3) . 3 ?
C8 C6 C6 125.3(2) . 3 ?
C6 C6 C6 90.000(1) 4 3 ?
N3 C6 C7 52.3(4) . . ?
C8 C6 C7 55.5(5) . . ?
C6 C6 C7 89.5(3) 4 . ?
C6 C6 C7 89.5(3) 3 . ?
N3 C7 C8 108.8(6) . . ?
N3 C7 C7 56.1(2) . 4 ?
C8 C7 C7 126.2(3) . 4 ?
N3 C7 C7 56.1(2) . 3 ?
C8 C7 C7 126.2(3) . 3 ?
C7 C7 C7 90.001(1) 4 3 ?
N3 C7 C6 52.9(5) . . ?
C8 C7 C6 55.9(5) . . ?
C7 C7 C6 90.5(3) 4 . ?
C7 C7 C6 90.5(3) 3 . ?
C7 C8 C6 68.6(6) . . ?

_refine_diff_density_max         0.944
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.123

####################################################################### 
# 
# 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_pm3m_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1956301'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 O0 S7 Sm'
_chemical_formula_weight         997.27

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   11.3772(6)
_cell_length_b                   11.3772(6)
_cell_length_c                   11.3772(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1472.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25736
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      33.06

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_F_000             485
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    1.276
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3960
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25736
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.790
_diffrn_reflns_theta_max         33.058
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             615
_reflns_number_gt                615
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0964P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         615
_refine_ls_number_parameters     32
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1136
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Sm1 Sm 0.0000 0.0000 0.0000 0.01734(19) Uani 1 48 d S T P . .
N2 N 0.0000 0.0000 0.5000 0.141(11) Uani 1 16 d S T P . .
C2 C 0.0000 0.100(2) 0.4152(12) 0.157(10) Uani 0.5 2 d S T P . .
N3 N 0.5000 0.5000 0.5000 0.030(2) Uani 1 48 d S T P . .
C3 C 0.0000 0.220(2) 0.5000 0.175(8) Uani 1 4 d S T P . .
C4 C 0.4063(9) 0.4063(9) 0.5000 0.054(5) Uani 0.3332 4 d S T P . .
C5 C 0.2742(12) 0.5000 0.5000 0.059(3) Uani 0.6664 8 d S T P . .
S1 S 0.26174(15) 0.26174(15) 0.26174(15) 0.0981(13) Uani 0.875 6 d S T P . .
C1 C 0.1823(5) 0.1823(5) 0.1823(5) 0.064(3) Uani 0.875 6 d S T P . .
N1 N 0.1244(4) 0.1244(4) 0.1244(4) 0.080(3) Uani 0.875 6 d S T P . .


_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
Sm1 N1 2.452(8) . ?
Sm1 N1 2.452(8) 25 ?
Sm1 N1 2.452(8) 28 ?
Sm1 N1 2.452(8) 2 ?
Sm1 N1 2.452(8) 26 ?
Sm1 N1 2.452(8) 3 ?
Sm1 N1 2.452(8) 27 ?
Sm1 N1 2.452(8) 4 ?
N2 C2 1.490(18) 37 ?
N2 C2 1.490(18) 13_556 ?
N2 C2 1.490(18) 26_556 ?
N2 C2 1.490(18) 2 ?
N2 C2 1.490(18) 38 ?
N2 C2 1.490(18) 25_556 ?
N2 C2 1.490(18) 14_556 ?
N2 C2 1.490(18) . ?
C2 C2 1.61(3) 37 ?
C2 C2 1.61(3) 38 ?
C2 C3 1.67(2) . ?
C2 C2 1.93(3) 26_556 ?
N3 C4 1.508(15) 33_666 ?
N3 C4 1.508(15) . ?
N3 C4 1.508(15) 25_666 ?
N3 C4 1.508(15) 9 ?
N3 C4 1.508(14) 29_666 ?
N3 C4 1.508(14) 5 ?
N3 C4 1.508(15) 35_655 ?
N3 C4 1.508(14) 7_665 ?
N3 C4 1.508(14) 31_556 ?
N3 C4 1.508(14) 27_565 ?
N3 C4 1.508(15) 3_656 ?
N3 C4 1.508(15) 11_566 ?
C3 C2 1.67(2) 26_556 ?
C4 C4 1.508(14) 11_566 ?
C4 C4 1.508(14) 31_556 ?
C4 C4 1.508(14) 9 ?
C4 C4 1.508(14) 5 ?
C4 C5 1.843(11) . ?
C4 C5 1.843(11) 5 ?
C5 C4 1.843(11) 27_565 ?
C5 C4 1.843(11) 11_566 ?
C5 C4 1.843(11) 9 ?
S1 C1 1.566(10) . ?
C1 N1 1.140(11) . ?

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
N1 Sm1 N1 180.0(4) . 25 ?
N1 Sm1 N1 70.529(1) . 28 ?
N1 Sm1 N1 109.471(1) 25 28 ?
N1 Sm1 N1 109.5 . 2 ?
N1 Sm1 N1 70.529(1) 25 2 ?
N1 Sm1 N1 70.5 28 2 ?
N1 Sm1 N1 70.5 . 26 ?
N1 Sm1 N1 109.5 25 26 ?
N1 Sm1 N1 109.5 28 26 ?
N1 Sm1 N1 180.0(6) 2 26 ?
N1 Sm1 N1 109.5 . 3 ?
N1 Sm1 N1 70.529(1) 25 3 ?
N1 Sm1 N1 70.5 28 3 ?
N1 Sm1 N1 109.5 2 3 ?
N1 Sm1 N1 70.5 26 3 ?
N1 Sm1 N1 70.5 . 27 ?
N1 Sm1 N1 109.5 25 27 ?
N1 Sm1 N1 109.5 28 27 ?
N1 Sm1 N1 70.5 2 27 ?
N1 Sm1 N1 109.5 26 27 ?
N1 Sm1 N1 180.0(6) 3 27 ?
N1 Sm1 N1 109.471(1) . 4 ?
N1 Sm1 N1 70.529(1) 25 4 ?
N1 Sm1 N1 180.0(4) 28 4 ?
N1 Sm1 N1 109.5 2 4 ?
N1 Sm1 N1 70.5 26 4 ?
N1 Sm1 N1 109.5 3 4 ?
N1 Sm1 N1 70.5 27 4 ?
C2 N2 C2 180.0(8) 37 13_556 ?
C2 N2 C2 114.8(9) 37 26_556 ?
C2 N2 C2 65.2(9) 13_556 26_556 ?
C2 N2 C2 65.2(9) 37 2 ?
C2 N2 C2 114.8(9) 13_556 2 ?
C2 N2 C2 180.0 26_556 2 ?
C2 N2 C2 99.3(17) 37 38 ?
C2 N2 C2 80.7(17) 13_556 38 ?
C2 N2 C2 114.8(9) 26_556 38 ?
C2 N2 C2 65.2(9) 2 38 ?
C2 N2 C2 114.8(9) 37 25_556 ?
C2 N2 C2 65.2(9) 13_556 25_556 ?
C2 N2 C2 99.3(17) 26_556 25_556 ?
C2 N2 C2 80.7(17) 2 25_556 ?
C2 N2 C2 114.8(9) 38 25_556 ?
C2 N2 C2 80.7(17) 37 14_556 ?
C2 N2 C2 99.3(17) 13_556 14_556 ?
C2 N2 C2 65.2(9) 26_556 14_556 ?
C2 N2 C2 114.8(9) 2 14_556 ?
C2 N2 C2 180.0 38 14_556 ?
C2 N2 C2 65.2(9) 25_556 14_556 ?
C2 N2 C2 65.2(9) 37 . ?
C2 N2 C2 114.8(9) 13_556 . ?
C2 N2 C2 80.7(17) 26_556 . ?
C2 N2 C2 99.3(17) 2 . ?
C2 N2 C2 65.2(9) 38 . ?
C2 N2 C2 180.0 25_556 . ?
C2 N2 C2 114.8(9) 14_556 . ?
N2 C2 C2 57.4(5) . 37 ?
N2 C2 C2 57.4(5) . 38 ?
C2 C2 C2 90.0 37 38 ?
N2 C2 C3 104.4(11) . . ?
C2 C2 C3 125.3(3) 37 . ?
C2 C2 C3 125.3(3) 38 . ?
N2 C2 C2 49.6(8) . 26_556 ?
C2 C2 C2 90.000(2) 37 26_556 ?
C2 C2 C2 90.000(1) 38 26_556 ?
C3 C2 C2 54.7(6) . 26_556 ?
C4 N3 C4 120.000(1) 33_666 . ?
C4 N3 C4 60.000(1) 33_666 25_666 ?
C4 N3 C4 180.0(6) . 25_666 ?
C4 N3 C4 180.0 33_666 9 ?
C4 N3 C4 60.000(1) . 9 ?
C4 N3 C4 120.0 25_666 9 ?
C4 N3 C4 60.0 33_666 29_666 ?
C4 N3 C4 120.0 . 29_666 ?
C4 N3 C4 60.0 25_666 29_666 ?
C4 N3 C4 120.0 9 29_666 ?
C4 N3 C4 120.000(1) 33_666 5 ?
C4 N3 C4 60.000(1) . 5 ?
C4 N3 C4 120.000(1) 25_666 5 ?
C4 N3 C4 60.000(1) 9 5 ?
C4 N3 C4 180.0 29_666 5 ?
C4 N3 C4 90.000(2) 33_666 35_655 ?
C4 N3 C4 120.0 . 35_655 ?
C4 N3 C4 60.000(1) 25_666 35_655 ?
C4 N3 C4 90.000(1) 9 35_655 ?
C4 N3 C4 120.000(1) 29_666 35_655 ?
C4 N3 C4 60.000(1) 5 35_655 ?
C4 N3 C4 120.000(1) 33_666 7_665 ?
C4 N3 C4 120.000(1) . 7_665 ?
C4 N3 C4 60.0 25_666 7_665 ?
C4 N3 C4 60.0 9 7_665 ?
C4 N3 C4 90.000(1) 29_666 7_665 ?
C4 N3 C4 90.000(1) 5 7_665 ?
C4 N3 C4 60.0 35_655 7_665 ?
C4 N3 C4 60.0 33_666 31_556 ?
C4 N3 C4 60.0 . 31_556 ?
C4 N3 C4 120.000(1) 25_666 31_556 ?
C4 N3 C4 120.000(1) 9 31_556 ?
C4 N3 C4 90.000(1) 29_666 31_556 ?
C4 N3 C4 90.000(2) 5 31_556 ?
C4 N3 C4 120.000(1) 35_655 31_556 ?
C4 N3 C4 180.0 7_665 31_556 ?
C4 N3 C4 120.0 33_666 27_565 ?
C4 N3 C4 90.000(2) . 27_565 ?
C4 N3 C4 90.0 25_666 27_565 ?
C4 N3 C4 60.0 9 27_565 ?
C4 N3 C4 60.000(1) 29_666 27_565 ?
C4 N3 C4 120.000(1) 5 27_565 ?
C4 N3 C4 120.0 35_655 27_565 ?
C4 N3 C4 60.0 7_665 27_565 ?
C4 N3 C4 120.000(1) 31_556 27_565 ?
C4 N3 C4 60.0 33_666 3_656 ?
C4 N3 C4 90.0 . 3_656 ?
C4 N3 C4 90.000(1) 25_666 3_656 ?
C4 N3 C4 120.0 9 3_656 ?
C4 N3 C4 120.000(1) 29_666 3_656 ?
C4 N3 C4 60.0 5 3_656 ?
C4 N3 C4 60.0 35_655 3_656 ?
C4 N3 C4 120.000(1) 7_665 3_656 ?
C4 N3 C4 60.0 31_556 3_656 ?
C4 N3 C4 180.0 27_565 3_656 ?
C4 N3 C4 90.000(1) 33_666 11_566 ?
C4 N3 C4 60.000(1) . 11_566 ?
C4 N3 C4 120.0 25_666 11_566 ?
C4 N3 C4 90.000(2) 9 11_566 ?
C4 N3 C4 60.000(1) 29_666 11_566 ?
C4 N3 C4 120.000(1) 5 11_566 ?
C4 N3 C4 180.0 35_655 11_566 ?
C4 N3 C4 120.000(1) 7_665 11_566 ?
C4 N3 C4 60.000(1) 31_556 11_566 ?
C4 N3 C4 60.000(1) 27_565 11_566 ?
C4 N3 C4 120.000(1) 3_656 11_566 ?
C2 C3 C2 70.5(13) . 26_556 ?
C4 C4 N3 60.000(2) 11_566 . ?
C4 C4 C4 60.0 11_566 31_556 ?
N3 C4 C4 60.000(2) . 31_556 ?
C4 C4 C4 90.000(4) 11_566 9 ?
N3 C4 C4 60.000(2) . 9 ?
C4 C4 C4 120.000(7) 31_556 9 ?
C4 C4 C4 120.000(8) 11_566 5 ?
N3 C4 C4 60.000(2) . 5 ?
C4 C4 C4 90.000(6) 31_556 5 ?
C4 C4 C4 60.0 9 5 ?
C4 C4 C5 65.9(3) 11_566 . ?
N3 C4 C5 99.7(5) . . ?
C4 C4 C5 125.2(2) 31_556 . ?
C4 C4 C5 65.9(3) 9 . ?
C4 C4 C5 125.2(2) 5 . ?
C4 C4 C5 125.2(2) 11_566 5 ?
N3 C4 C5 99.7(5) . 5 ?
C4 C4 C5 65.9(3) 31_556 5 ?
C4 C4 C5 125.2(2) 9 5 ?
C4 C4 C5 65.9(3) 5 5 ?
C5 C4 C5 160.7(10) . 5 ?
C4 C5 C4 48.3(6) 27_565 11_566 ?
C4 C5 C4 70.7(10) 27_565 . ?
C4 C5 C4 48.3(6) 11_566 . ?
C4 C5 C4 48.3(6) 27_565 9 ?
C4 C5 C4 70.7(10) 11_566 9 ?
C4 C5 C4 48.3(6) . 9 ?
N1 C1 S1 180.0(11) . . ?
C1 N1 Sm1 180.0(10) . . ?

_refine_diff_density_max         1.383
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_i4mmm_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 1956298'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_i4mmm               
;
PROBLEM: Check Calcd Resid. Dens.  0.07A   From N3              3.06 eA-3
RESPONSE: There is considerable disorder associated with the tetraethylammonium cations in all of the structures published.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 N11 O0 S7 Yb'
_chemical_formula_weight         1019.96

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   11.3736(4)
_cell_length_b                   11.3736(4)
_cell_length_c                   22.4950(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2909.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25655
_cell_measurement_theta_min      1.811
_cell_measurement_theta_max      33.115

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             986
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.081
_exptl_absorpt_coefficient_mu    1.889
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3785
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25655
_diffrn_reflns_av_unetI/netI     0.0075
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.811
_diffrn_reflns_theta_max         33.115
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1600
_reflns_number_gt                1600
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1075P)²+1.5155P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1600
_refine_ls_number_parameters     56
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1261
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.002
_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
Yb1 Yb 0.0000 0.0000 0.0000 0.02583(13) Uani 1 16 d S T P . .
S1 S 0.25728(11) 0.25728(11) 0.13178(7) 0.0670(5) Uani 0.875 2 d S T P . .
C1 C 0.1785(4) 0.1785(4) 0.0914(3) 0.0544(13) Uani 0.875 2 d S T P . .
N1 N 0.1214(4) 0.1214(4) 0.0603(3) 0.0712(18) Uani 0.875 2 d S T P . .
N2 N 0.0000 0.5000 0.0000 0.078(3) Uani 1 8 d DS T P . .
C2 C 0.0000 0.5806(12) -0.0527(8) 0.124(7) Uani 0.5 2 d DS T P . .
C3 C 0.0000 0.5000 -0.1120(8) 0.164(7) Uani 1 4 d DS T P . .
C4 C -0.1027(17) 0.5835(13) 0.0000 0.124(7) Uani 0.5 2 d DS T P . .
C5 C -0.217(2) 0.5000 0.0000 0.164(7) Uani 1 4 d DS T P . .
N3 N 0.0000 0.0000 0.2524(5) 0.078(3) Uani 1 8 d DS T P . .
C6 C 0.1085(12) 0.0000 0.2119(5) 0.076(5) Uani 0.5 2 d DS T P . .
C7 C 0.1056(8) 0.0000 0.2936(3) 0.0437(16) Uani 0.5 2 d DS T P . .
C8 C 0.2261(7) 0.0000 0.2541(6) 0.084(2) Uani 1 2 d DS T P . .


_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
Yb1 N1 2.378(6) . ?
Yb1 N1 2.378(6) 17 ?
Yb1 N1 2.378(6) 20 ?
Yb1 N1 2.378(6) 2 ?
Yb1 N1 2.378(6) 18 ?
Yb1 N1 2.378(6) 3 ?
Yb1 N1 2.378(6) 19 ?
Yb1 N1 2.378(6) 4 ?
S1 C1 1.558(6) . ?
C1 N1 1.156(8) . ?
N2 C2 1.498(12) 18 ?
N2 C2 1.498(12) 2_565 ?
N2 C2 1.498(12) 17_565 ?
N2 C2 1.498(12) . ?
N2 C4 1.505(15) . ?
N2 C4 1.505(15) 21_565 ?
N2 C4 1.505(15) 5 ?
N2 C4 1.505(15) 17_565 ?
C2 C3 1.620(15) . ?
C2 C4 1.66(2) . ?
C2 C4 1.66(2) 5 ?
C2 C2 1.83(3) 2_565 ?
C3 C2 1.620(15) 2_565 ?
C4 C5 1.612(17) . ?
C4 C2 1.66(2) 18 ?
C4 C4 1.90(3) 21_565 ?
C5 C4 1.612(17) 21_565 ?
N3 C7 1.516(9) 3 ?
N3 C7 1.516(9) 4 ?
N3 C7 1.516(9) 2 ?
N3 C7 1.517(9) . ?
N3 C6 1.533(11) 2 ?
N3 C6 1.533(11) 4 ?
N3 C6 1.533(11) 3 ?
N3 C6 1.533(11) . ?
C6 C8 1.640(14) . ?
C6 C6 1.74(2) 4 ?
C6 C6 1.74(2) 3 ?
C6 C7 1.836(12) . ?
C7 C8 1.633(11) . ?
C7 C7 1.698(12) 4 ?
C7 C7 1.698(12) 3 ?

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
N1 Yb1 N1 180.0 . 17 ?
N1 Yb1 N1 109.01(19) . 20 ?
N1 Yb1 N1 70.99(19) 17 20 ?
N1 Yb1 N1 110.4(4) . 2 ?
N1 Yb1 N1 69.6(4) 17 2 ?
N1 Yb1 N1 109.01(19) 20 2 ?
N1 Yb1 N1 69.6(4) . 18 ?
N1 Yb1 N1 110.4(4) 17 18 ?
N1 Yb1 N1 70.99(19) 20 18 ?
N1 Yb1 N1 180.0(4) 2 18 ?
N1 Yb1 N1 70.99(19) . 3 ?
N1 Yb1 N1 109.01(19) 17 3 ?
N1 Yb1 N1 69.6(4) 20 3 ?
N1 Yb1 N1 70.99(19) 2 3 ?
N1 Yb1 N1 109.01(19) 18 3 ?
N1 Yb1 N1 109.01(19) . 19 ?
N1 Yb1 N1 70.99(19) 17 19 ?
N1 Yb1 N1 110.4(4) 20 19 ?
N1 Yb1 N1 109.01(19) 2 19 ?
N1 Yb1 N1 70.99(19) 18 19 ?
N1 Yb1 N1 180.0(3) 3 19 ?
N1 Yb1 N1 70.99(19) . 4 ?
N1 Yb1 N1 109.01(19) 17 4 ?
N1 Yb1 N1 180.0(4) 20 4 ?
N1 Yb1 N1 70.99(19) 2 4 ?
N1 Yb1 N1 109.01(19) 18 4 ?
N1 Yb1 N1 110.4(4) 3 4 ?
N1 Yb1 N1 69.6(4) 19 4 ?
N1 C1 S1 178.3(7) . . ?
C1 N1 Yb1 177.5(7) . . ?
C2 N2 C2 180.0(9) 18 2_565 ?
C2 N2 C2 75.5(14) 18 17_565 ?
C2 N2 C2 104.5(14) 2_565 17_565 ?
C2 N2 C2 104.5(14) 18 . ?
C2 N2 C2 75.5(14) 2_565 . ?
C2 N2 C2 180.0 17_565 . ?
C2 N2 C4 67.3(6) 18 . ?
C2 N2 C4 112.7(6) 2_565 . ?
C2 N2 C4 112.7(6) 17_565 . ?
C2 N2 C4 67.3(6) . . ?
C2 N2 C4 112.7(6) 18 21_565 ?
C2 N2 C4 67.3(6) 2_565 21_565 ?
C2 N2 C4 67.3(6) 17_565 21_565 ?
C2 N2 C4 112.7(6) . 21_565 ?
C4 N2 C4 78.3(15) . 21_565 ?
C2 N2 C4 67.3(6) 18 5 ?
C2 N2 C4 112.7(6) 2_565 5 ?
C2 N2 C4 112.7(6) 17_565 5 ?
C2 N2 C4 67.3(6) . 5 ?
C4 N2 C4 101.7(15) . 5 ?
C4 N2 C4 180.0(8) 21_565 5 ?
C2 N2 C4 112.7(6) 18 17_565 ?
C2 N2 C4 67.3(5) 2_565 17_565 ?
C2 N2 C4 67.3(5) 17_565 17_565 ?
C2 N2 C4 112.7(6) . 17_565 ?
C4 N2 C4 180.0 . 17_565 ?
C4 N2 C4 101.7(15) 21_565 17_565 ?
C4 N2 C4 78.3(15) 5 17_565 ?
N2 C2 C3 107.8(11) . . ?
N2 C2 C4 56.6(5) . . ?
C3 C2 C4 126.7(9) . . ?
N2 C2 C4 56.6(5) . 5 ?
C3 C2 C4 126.7(9) . 5 ?
C4 C2 C4 89.1(11) . 5 ?
N2 C2 C2 52.3(7) . 2_565 ?
C3 C2 C2 55.5(5) . 2_565 ?
C4 C2 C2 91.1(7) . 2_565 ?
C4 C2 C2 91.1(7) 5 2_565 ?
C2 C3 C2 69.0(11) . 2_565 ?
N2 C4 C5 104.8(12) . . ?
N2 C4 C2 56.2(6) . 18 ?
C5 C4 C2 123.7(10) . 18 ?
N2 C4 C2 56.2(6) . . ?
C5 C4 C2 123.7(10) . . ?
C2 C4 C2 90.8(11) 18 . ?
N2 C4 C4 50.9(7) . 21_565 ?
C5 C4 C4 53.9(7) . 21_565 ?
C2 C4 C4 88.9(7) 18 21_565 ?
C2 C4 C4 88.9(7) . 21_565 ?
C4 C5 C4 72.2(14) 21_565 . ?
C7 N3 C7 104.7(10) 3 4 ?
C7 N3 C7 68.1(5) 3 2 ?
C7 N3 C7 68.1(5) 4 2 ?
C7 N3 C7 68.1(5) 3 . ?
C7 N3 C7 68.1(5) 4 . ?
C7 N3 C7 104.7(10) 2 . ?
C7 N3 C6 111.3(3) 3 2 ?
C7 N3 C6 111.3(3) 4 2 ?
C7 N3 C6 74.0(6) 2 2 ?
C7 N3 C6 178.8(10) . 2 ?
C7 N3 C6 178.8(10) 3 4 ?
C7 N3 C6 74.0(6) 4 4 ?
C7 N3 C6 111.3(3) 2 4 ?
C7 N3 C6 111.3(3) . 4 ?
C6 N3 C6 69.4(7) 2 4 ?
C7 N3 C6 74.0(6) 3 3 ?
C7 N3 C6 178.8(10) 4 3 ?
C7 N3 C6 111.3(3) 2 3 ?
C7 N3 C6 111.3(3) . 3 ?
C6 N3 C6 69.4(7) 2 3 ?
C6 N3 C6 107.2(13) 4 3 ?
C7 N3 C6 111.3(3) 3 . ?
C7 N3 C6 111.3(3) 4 . ?
C7 N3 C6 178.8(10) 2 . ?
C7 N3 C6 74.0(6) . . ?
C6 N3 C6 107.2(13) 2 . ?
C6 N3 C6 69.4(7) 4 . ?
C6 N3 C6 69.4(7) 3 . ?
N3 C6 C8 108.2(7) . . ?
N3 C6 C6 55.3(3) . 4 ?
C8 C6 C6 125.2(2) . 4 ?
N3 C6 C6 55.3(3) . 3 ?
C8 C6 C6 125.2(2) . 3 ?
C6 C6 C6 90.000(1) 4 3 ?
N3 C6 C7 52.6(5) . . ?
C8 C6 C7 55.7(5) . . ?
C6 C6 C7 89.3(4) 4 . ?
C6 C6 C7 89.3(4) 3 . ?
N3 C7 C8 109.5(6) . . ?
N3 C7 C7 55.9(3) . 4 ?
C8 C7 C7 126.4(2) . 4 ?
N3 C7 C7 55.9(3) . 3 ?
C8 C7 C7 126.4(2) . 3 ?
C7 C7 C7 90.000(1) 4 3 ?
N3 C7 C6 53.4(5) . . ?
C8 C7 C6 56.1(5) . . ?
C7 C7 C6 90.7(4) 4 . ?
C7 C7 C6 90.7(4) 3 . ?
C7 C8 C6 68.3(5) . . ?

_refine_diff_density_max         2.921
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.163

####################################################################### 
# 
# 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_rew_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956300'
loop_
_audit_author_name
_audit_author_address
'Richard Wilson'
;Argonne National Laboratory
United States of America
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_rew                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O1 Check
RESPONSE: We have not assigned any of the H-atoms in these structures
;
_vrf_PLAT975_rew                 
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From C5              1.79 eA-3
RESPONSE: This residual density is near the terminal methyl group of the tetraethylammonium cations.  There is considerable disorder about these groups.  We have looked into this but have modeled the data by constraining the thermal parameters of the carbon atoms rather than splitting the positions.
;
# Added during the CSD deposition process: Thursday 26 September 2019 08:26 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H0 Cm N11 O3 S7'
_chemical_formula_weight         1142.92

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'
Cm Cm -7.3248 4.6980 '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      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'z, x, y'
'z, -y, x'
'z, -x, -y'
'-x, y, -z'
'y, x, -z'
'y, z, x'
'-y, -x, -z'
'-y, z, -x'
'-y, x, z'
'-y, -z, x'
'-x, z, y'
'-x, -y, z'
'-x, -z, -y'
'-z, y, x'
'-z, -x, y'
'-z, -y, -x'
'-z, x, -y'
'y, -x, z'
'y, -z, -x'
'-x, -y, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'-z, -x, -y'
'-z, y, -x'
'-z, x, y'
'x, -y, z'
'-y, -x, z'
'-y, -z, -x'
'y, x, z'
'y, -z, x'
'y, -x, -z'
'y, z, -x'
'x, -z, -y'
'x, y, -z'
'x, z, y'
'z, -y, -x'
'z, x, -y'
'z, y, x'
'z, -x, y'
'-y, x, -z'
'-y, z, x'

_cell_length_a                   11.3752(11)
_cell_length_b                   11.3752(11)
_cell_length_c                   11.3752(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1471.9(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19756
_cell_measurement_theta_min      1.790
_cell_measurement_theta_max      30.631

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             543
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.125
_exptl_absorpt_coefficient_mu    1.670
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19756
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.790
_diffrn_reflns_theta_max         30.631
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             513
_reflns_number_gt                513
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1035P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         513
_refine_ls_number_parameters     33
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1500
_refine_ls_goodness_of_fit_ref   1.476
_refine_ls_restrained_S_all      1.476
_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
Cm1 Cm 0.0000 0.0000 0.0000 0.0155(3) Uani 1 48 d S T P . .
S1 S 0.2610(3) 0.2610(3) 0.2610(3) 0.090(3) Uani 0.8752 6 d S T P . .
N1 N 0.1256(10) 0.1256(10) 0.1256(10) 0.078(7) Uani 0.8752 6 d S T P . .
C1 C 0.1822(11) 0.1822(11) 0.1822(11) 0.070(7) Uani 0.8752 6 d S T P . .
N2 N 0.5000 0.5000 0.5000 0.026(5) Uani 1 48 d S T P . .
C2 C 0.409(2) 0.5000 0.409(2) 0.043(8) Uani 0.3333 4 d S T P . .
C3 C 0.5000 0.5000 0.276(2) 0.060(8) Uani 0.6666 8 d S T P . .
O1 O 0.5000 0.5000 0.0000 0.072(8) Uani 1 16 d S T P . .
N3 N 0.0000 0.0000 0.5000 0.119(13) Uani 1 16 d DS TU P . .
C4 C 0.0798(15) 0.0000 0.4019(14) 0.132(13) Uani 0.5 2 d DS TU P . .
C5 C 0.173(3) 0.0000 0.5000 0.182(14) Uani 1 4 d DS TU P . .


_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
Cm1 N1 2.475(19) 25 ?
Cm1 N1 2.475(19) 28 ?
Cm1 N1 2.475(19) 4 ?
Cm1 N1 2.475(19) 27 ?
Cm1 N1 2.475(19) 2 ?
Cm1 N1 2.475(19) 26 ?
Cm1 N1 2.475(19) 3 ?
Cm1 N1 2.475(19) . ?
Cm1 C1 3.59(2) . ?
Cm1 C1 3.59(2) 25 ?
Cm1 C1 3.59(2) 28 ?
Cm1 C1 3.59(2) 4 ?
S1 C1 1.55(2) . ?
N1 C1 1.12(3) . ?
N2 C2 1.46(3) . ?
N2 C2 1.46(3) 35_666 ?
N2 C2 1.46(3) 25_666 ?
N2 C2 1.46(3) 11 ?
N2 C2 1.46(3) 28_665 ?
N2 C2 1.46(3) 4_556 ?
N2 C2 1.46(3) 2_565 ?
N2 C2 1.46(3) 27_655 ?
N2 C2 1.46(3) 3_566 ?
N2 C2 1.46(3) 10_556 ?
N2 C2 1.46(3) 34_665 ?
N2 C2 1.46(3) 26_656 ?
C2 C2 1.46(3) 34_665 ?
C2 C2 1.46(3) 2_565 ?
C2 C2 1.46(3) 11 ?
C2 C2 1.46(3) 4_556 ?
C2 C3 1.84(2) . ?
C2 C3 1.84(2) 5_556 ?
C3 C2 1.84(2) 34_665 ?
C3 C2 1.84(2) 27_655 ?
C3 C2 1.84(2) 11 ?
N3 C4 1.439(10) . ?
N3 C4 1.439(10) 34 ?
N3 C4 1.439(10) 10_556 ?
N3 C4 1.439(10) 3_556 ?
N3 C4 1.439(10) 27 ?
N3 C4 1.439(10) 36 ?
N3 C4 1.439(10) 25_556 ?
N3 C4 1.439(10) 12_556 ?
C4 C4 1.28(2) 34 ?
C4 C4 1.28(2) 36 ?
C4 C5 1.543(10) . ?
C4 C4 1.82(3) 27 ?
C5 C4 1.543(10) 3_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cm1 N1 70.5 25 28 ?
N1 Cm1 N1 109.5 25 4 ?
N1 Cm1 N1 180.0(8) 28 4 ?
N1 Cm1 N1 109.5 25 27 ?
N1 Cm1 N1 70.5 28 27 ?
N1 Cm1 N1 109.5 4 27 ?
N1 Cm1 N1 109.5 25 2 ?
N1 Cm1 N1 70.529(1) 28 2 ?
N1 Cm1 N1 109.471(1) 4 2 ?
N1 Cm1 N1 109.5 27 2 ?
N1 Cm1 N1 70.5 25 26 ?
N1 Cm1 N1 109.471(1) 28 26 ?
N1 Cm1 N1 70.529(1) 4 26 ?
N1 Cm1 N1 70.5 27 26 ?
N1 Cm1 N1 180.0(4) 2 26 ?
N1 Cm1 N1 70.5 25 3 ?
N1 Cm1 N1 109.5 28 3 ?
N1 Cm1 N1 70.5 4 3 ?
N1 Cm1 N1 180.0(4) 27 3 ?
N1 Cm1 N1 70.5 2 3 ?
N1 Cm1 N1 109.5 26 3 ?
N1 Cm1 N1 180.0(8) 25 . ?
N1 Cm1 N1 109.5 28 . ?
N1 Cm1 N1 70.5 4 . ?
N1 Cm1 N1 70.5 27 . ?
N1 Cm1 N1 70.5 2 . ?
N1 Cm1 N1 109.5 26 . ?
N1 Cm1 N1 109.5 3 . ?
N1 Cm1 C1 180.0(8) 25 . ?
N1 Cm1 C1 109.5 28 . ?
N1 Cm1 C1 70.5 4 . ?
N1 Cm1 C1 70.5 27 . ?
N1 Cm1 C1 70.5 2 . ?
N1 Cm1 C1 109.5 26 . ?
N1 Cm1 C1 109.5 3 . ?
N1 Cm1 C1 0.0(2) . . ?
N1 Cm1 C1 0.0(8) 25 25 ?
N1 Cm1 C1 70.5 28 25 ?
N1 Cm1 C1 109.5 4 25 ?
N1 Cm1 C1 109.5 27 25 ?
N1 Cm1 C1 109.5 2 25 ?
N1 Cm1 C1 70.5 26 25 ?
N1 Cm1 C1 70.5 3 25 ?
N1 Cm1 C1 180.0(5) . 25 ?
C1 Cm1 C1 180.0(6) . 25 ?
N1 Cm1 C1 70.5 25 28 ?
N1 Cm1 C1 0.0(7) 28 28 ?
N1 Cm1 C1 180.0(5) 4 28 ?
N1 Cm1 C1 70.529(1) 27 28 ?
N1 Cm1 C1 70.5 2 28 ?
N1 Cm1 C1 109.5 26 28 ?
N1 Cm1 C1 109.471(1) 3 28 ?
N1 Cm1 C1 109.5 . 28 ?
C1 Cm1 C1 109.471(1) . 28 ?
C1 Cm1 C1 70.5 25 28 ?
N1 Cm1 C1 109.5 25 4 ?
N1 Cm1 C1 180.0(5) 28 4 ?
N1 Cm1 C1 0.0(3) 4 4 ?
N1 Cm1 C1 109.471(1) 27 4 ?
N1 Cm1 C1 109.5 2 4 ?
N1 Cm1 C1 70.5 26 4 ?
N1 Cm1 C1 70.529(1) 3 4 ?
N1 Cm1 C1 70.5 . 4 ?
C1 Cm1 C1 70.5 . 4 ?
C1 Cm1 C1 109.471(1) 25 4 ?
C1 Cm1 C1 180.0(6) 28 4 ?
C1 N1 Cm1 180(2) . . ?
N1 C1 S1 180(3) . . ?
N1 C1 Cm1 0.0(17) . . ?
S1 C1 Cm1 180.0(16) . . ?
C2 N2 C2 120.000(1) . 35_666 ?
C2 N2 C2 180.0 . 25_666 ?
C2 N2 C2 60.000(2) 35_666 25_666 ?
C2 N2 C2 60.000(2) . 11 ?
C2 N2 C2 180.0 35_666 11 ?
C2 N2 C2 120.000(2) 25_666 11 ?
C2 N2 C2 120.000(2) . 28_665 ?
C2 N2 C2 60.000(2) 35_666 28_665 ?
C2 N2 C2 60.000(2) 25_666 28_665 ?
C2 N2 C2 120.000(2) 11 28_665 ?
C2 N2 C2 60.000(2) . 4_556 ?
C2 N2 C2 120.000(2) 35_666 4_556 ?
C2 N2 C2 120.000(2) 25_666 4_556 ?
C2 N2 C2 60.000(2) 11 4_556 ?
C2 N2 C2 180.0 28_665 4_556 ?
C2 N2 C2 60.000(2) . 2_565 ?
C2 N2 C2 60.000(2) 35_666 2_565 ?
C2 N2 C2 120.000(2) 25_666 2_565 ?
C2 N2 C2 120.000(2) 11 2_565 ?
C2 N2 C2 90.000(1) 28_665 2_565 ?
C2 N2 C2 90.000(3) 4_556 2_565 ?
C2 N2 C2 90.000(2) . 27_655 ?
C2 N2 C2 120.000(2) 35_666 27_655 ?
C2 N2 C2 90.000(4) 25_666 27_655 ?
C2 N2 C2 60.000(2) 11 27_655 ?
C2 N2 C2 60.000(2) 28_665 27_655 ?
C2 N2 C2 120.0 4_556 27_655 ?
C2 N2 C2 120.000(2) 2_565 27_655 ?
C2 N2 C2 90.000(3) . 3_566 ?
C2 N2 C2 60.000(2) 35_666 3_566 ?
C2 N2 C2 90.000(2) 25_666 3_566 ?
C2 N2 C2 120.000(2) 11 3_566 ?
C2 N2 C2 120.0 28_665 3_566 ?
C2 N2 C2 60.000(2) 4_556 3_566 ?
C2 N2 C2 60.000(2) 2_565 3_566 ?
C2 N2 C2 180.0 27_655 3_566 ?
C2 N2 C2 120.000(2) . 10_556 ?
C2 N2 C2 90.000(2) 35_666 10_556 ?
C2 N2 C2 60.0 25_666 10_556 ?
C2 N2 C2 90.000(3) 11 10_556 ?
C2 N2 C2 120.000(2) 28_665 10_556 ?
C2 N2 C2 60.0 4_556 10_556 ?
C2 N2 C2 120.000(2) 2_565 10_556 ?
C2 N2 C2 120.000(2) 27_655 10_556 ?
C2 N2 C2 60.000(2) 3_566 10_556 ?
C2 N2 C2 60.0 . 34_665 ?
C2 N2 C2 90.000(4) 35_666 34_665 ?
C2 N2 C2 120.000(2) 25_666 34_665 ?
C2 N2 C2 90.000(2) 11 34_665 ?
C2 N2 C2 60.0 28_665 34_665 ?
C2 N2 C2 120.000(2) 4_556 34_665 ?
C2 N2 C2 60.000(1) 2_565 34_665 ?
C2 N2 C2 60.000(1) 27_655 34_665 ?
C2 N2 C2 120.000(1) 3_566 34_665 ?
C2 N2 C2 180.0 10_556 34_665 ?
C2 N2 C2 120.000(1) . 26_656 ?
C2 N2 C2 120.000(2) 35_666 26_656 ?
C2 N2 C2 60.000(1) 25_666 26_656 ?
C2 N2 C2 60.000(1) 11 26_656 ?
C2 N2 C2 90.000(4) 28_665 26_656 ?
C2 N2 C2 90.0 4_556 26_656 ?
C2 N2 C2 180.0 2_565 26_656 ?
C2 N2 C2 60.000(1) 27_655 26_656 ?
C2 N2 C2 120.000(1) 3_566 26_656 ?
C2 N2 C2 60.000(1) 10_556 26_656 ?
C2 N2 C2 120.000(2) 34_665 26_656 ?
N2 C2 C2 60.000(4) . 34_665 ?
N2 C2 C2 60.000(2) . 2_565 ?
C2 C2 C2 60.000(2) 34_665 2_565 ?
N2 C2 C2 60.000(2) . 11 ?
C2 C2 C2 90.000(13) 34_665 11 ?
C2 C2 C2 120.000(12) 2_565 11 ?
N2 C2 C2 60.000(1) . 4_556 ?
C2 C2 C2 120.000(8) 34_665 4_556 ?
C2 C2 C2 90.000(2) 2_565 4_556 ?
C2 C2 C2 60.000(3) 11 4_556 ?
N2 C2 C3 100.8(11) . . ?
C2 C2 C3 66.6(7) 34_665 . ?
C2 C2 C3 125.8(5) 2_565 . ?
C2 C2 C3 66.6(7) 11 . ?
C2 C2 C3 125.8(5) 4_556 . ?
N2 C2 C3 100.8(11) . 5_556 ?
C2 C2 C3 125.8(5) 34_665 5_556 ?
C2 C2 C3 66.6(7) 2_565 5_556 ?
C2 C2 C3 125.8(5) 11 5_556 ?
C2 C2 C3 66.6(7) 4_556 5_556 ?
C3 C2 C3 158(2) . 5_556 ?
C2 C3 C2 46.9(14) 34_665 27_655 ?
C2 C3 C2 68(2) 34_665 11 ?
C2 C3 C2 46.9(14) 27_655 11 ?
C2 C3 C2 46.9(14) 34_665 . ?
C2 C3 C2 68(2) 27_655 . ?
C2 C3 C2 46.9(14) 11 . ?
C4 N3 C4 53.0(10) . 34 ?
C4 N3 C4 127.0(10) . 10_556 ?
C4 N3 C4 180.0 34 10_556 ?
C4 N3 C4 101.8(17) . 3_556 ?
C4 N3 C4 127.0(10) 34 3_556 ?
C4 N3 C4 53.0(10) 10_556 3_556 ?
C4 N3 C4 78.2(17) . 27 ?
C4 N3 C4 53.0(10) 34 27 ?
C4 N3 C4 127.0(10) 10_556 27 ?
C4 N3 C4 180.0 3_556 27 ?
C4 N3 C4 53.0(10) . 36 ?
C4 N3 C4 78.2(17) 34 36 ?
C4 N3 C4 101.8(17) 10_556 36 ?
C4 N3 C4 127.0(10) 3_556 36 ?
C4 N3 C4 53.0(10) 27 36 ?
C4 N3 C4 180.0 . 25_556 ?
C4 N3 C4 127.0(10) 34 25_556 ?
C4 N3 C4 53.0(10) 10_556 25_556 ?
C4 N3 C4 78.2(17) 3_556 25_556 ?
C4 N3 C4 101.8(17) 27 25_556 ?
C4 N3 C4 127.0(10) 36 25_556 ?
C4 N3 C4 127.0(10) . 12_556 ?
C4 N3 C4 101.8(17) 34 12_556 ?
C4 N3 C4 78.2(17) 10_556 12_556 ?
C4 N3 C4 53.0(10) 3_556 12_556 ?
C4 N3 C4 127.0(10) 27 12_556 ?
C4 N3 C4 180.0 36 12_556 ?
C4 N3 C4 53.0(10) 25_556 12_556 ?
C4 C4 C4 90.0 34 36 ?
C4 C4 N3 63.5(5) 34 . ?
C4 C4 N3 63.5(5) 36 . ?
C4 C4 C5 119.2(5) 34 . ?
C4 C4 C5 119.2(5) 36 . ?
N3 C4 C5 82.8(16) . . ?
C4 C4 C4 45.000(1) 34 27 ?
C4 C4 C4 45.000(2) 36 27 ?
N3 C4 C4 50.9(8) . 27 ?
C5 C4 C4 133.7(8) . 27 ?
C4 C5 C4 92.7(17) . 3_556 ?

_refine_diff_density_max         1.960
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.211

