# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2047520'
loop_
_audit_author_name
_audit_author_address
'Fumiya Kobayashi'
;Tokyo University of Science
Japan
;
_audit_update_record             
;
2020-12-04 deposited with the CCDC.	2021-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C114 H102 Cl24 N36 O18 Re6'
_chemical_formula_sum            'C114 H102 Cl24 N36 O18 Re6'
_chemical_formula_weight         4232.31

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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   16.902(2)
_cell_length_b                   16.902(2)
_cell_length_c                   83.022(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     20539(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.405
_cell_measurement_theta_max      25.0482

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_F_000             12240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.829
_shelx_estimated_absorpt_T_min   0.593
_shelx_estimated_absorpt_T_max   0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1090
_exptl_absorpt_correction_T_max  0.1815
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29991
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_limit_l_max       98
_diffrn_reflns_theta_min         2.406
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4038
_reflns_number_gt                3528
_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.

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000        85        13 ' '
   2 -0.333  0.333  0.083       442       143 ' '
   3  0.000  0.000  0.250       443       143 ' '
   4  0.333  0.667  0.417       442       143 ' '
   5  0.000  0.000  0.500        85        13 ' '
   6 -0.333  0.333  0.583       443       143 ' '
   7  0.000  0.000  0.750       442       143 ' '
   8  0.333  0.667  0.917       443       143 ' '
   9  0.333  0.667  0.167        86        13 ' '
  10  0.333  0.667  0.667        86        13 ' '
  11  0.666  0.333  0.333        86        13 ' '
  12  0.667  0.333  0.833        86        13 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_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)+(0.0787P)²+1139.9890P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4038
_refine_ls_number_parameters     262
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1816
_refine_ls_wR_factor_gt          0.1782
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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
Re1 Re 0.42186(3) 0.48282(3) 0.31288(2) 0.0400(2) Uani 1 1 d . . . . .
C1 C 0.3266(8) 0.5420(8) 0.28384(18) 0.045(3) Uani 1 1 d . . . . .
H1 H 0.294762 0.563572 0.290260 0.054 Uiso 1 1 calc R U . . .
N1 N 0.3814(7) 0.5106(6) 0.28954(13) 0.039(2) Uani 1 1 d . . . . .
Cl1 Cl 0.6129(5) 0.7041(5) 0.27588(10) 0.127(2) Uani 1 1 d . . . . .
O1 O 0.4752(9) 0.4165(8) 0.34321(15) 0.083(4) Uani 1 1 d . . . . .
O2 O 0.3034(8) 0.5436(8) 0.33146(14) 0.075(3) Uani 1 1 d . . . . .
C2 C 0.3247(8) 0.5376(8) 0.26764(17) 0.044(3) Uani 1 1 d . . . . .
H2 H 0.291181 0.554178 0.260582 0.052 Uiso 1 1 calc R U . . .
N2 N 0.3812(7) 0.5043(7) 0.26339(13) 0.044(2) Uani 1 1 d . . . . .
H5 H 0.393929 0.495130 0.253524 0.053 Uiso 1 1 calc R U . . .
N3 N 0.4904(6) 0.4444(7) 0.29507(13) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.5499(9) 0.4100(10) 0.29469(19) 0.056(4) Uani 1 1 d . . . . .
H3 H 0.576704 0.396894 0.303613 0.068 Uiso 1 1 calc R U . . .
Cl2 Cl 0.7920(8) 0.6009(8) 0.27274(14) 0.191(4) Uani 1 1 d . . . . .
O3 O 0.5870(6) 0.6712(6) 0.31860(13) 0.060(3) Uani 1 1 d . . . . .
N4 N 0.5139(8) 0.4251(9) 0.26900(15) 0.056(3) Uani 1 1 d . . . . .
C4 C 0.5615(9) 0.3992(11) 0.2789(2) 0.063(4) Uani 1 1 d . . . . .
H4 H 0.598889 0.375922 0.275119 0.076 Uiso 1 1 calc R U . . .
N5 N 0.3037(6) 0.3474(6) 0.30808(12) 0.037(2) Uani 1 1 d . . . . .
C5 C 0.4131(7) 0.4886(8) 0.27691(14) 0.036(3) Uani 1 1 d . . . . .
N6 N 0.0853(6) 0.0103(6) 0.30096(12) 0.033(2) Uani 1 1 d . . . . .
C6 C 0.4728(8) 0.4514(8) 0.27974(15) 0.037(3) Uani 1 1 d . . . . .
C9 C 0.5249(9) 0.6017(11) 0.31668(18) 0.052(3) Uani 1 1 d . . . . .
C8 C 0.3485(10) 0.5184(9) 0.32496(17) 0.054(4) Uani 1 1 d . . . . .
C7 C 0.4554(10) 0.4418(9) 0.33201(19) 0.056(4) Uani 1 1 d . . . . .
C10 C 0.2201(9) 0.3340(8) 0.30665(19) 0.049(3) Uani 1 1 d . . . . .
H6 H 0.211955 0.385581 0.307336 0.059 Uiso 1 1 calc R U . . .
C11 C 0.1445(8) 0.2501(8) 0.30422(18) 0.047(3) Uani 1 1 d . . . . .
H7 H 0.085926 0.244627 0.303399 0.056 Uiso 1 1 calc R U . . .
C12 C 0.1530(7) 0.1742(7) 0.30299(15) 0.035(3) Uani 1 1 d . . . . .
C13 C 0.2390(8) 0.1851(7) 0.30426(15) 0.036(3) Uani 1 1 d . . . . .
H8 H 0.248010 0.134123 0.303447 0.043 Uiso 1 1 calc R U . . .
C14 C 0.3125(7) 0.2725(8) 0.30677(16) 0.039(3) Uani 1 1 d . . . . .
H9 H 0.371855 0.279888 0.307598 0.047 Uiso 1 1 calc R U . . .
C15 C 0.0714(8) 0.0826(8) 0.30128(15) 0.035(2) Uani 1 1 d . . . . .
C16 C 0.6907(19) 0.658(2) 0.2810(4) 0.144(11) Uani 1 1 d D . . . .
H10A H 0.746541 0.705717 0.286314 0.173 Uiso 1 1 calc R U . . .
H10B H 0.659391 0.605561 0.288457 0.173 Uiso 1 1 calc R U . . .
C17 C 0.716(4) 0.627(5) 0.2657(5) 0.40(6) Uani 1 1 d D . . . .
H11A H 0.743734 0.676896 0.257663 0.482 Uiso 1 1 calc R U . . .
H11B H 0.662868 0.573362 0.260904 0.482 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C8 1.911(16) . ?
Re1 C9 1.916(15) . ?
Re1 C7 1.928(16) . ?
Re1 N3 2.168(10) . ?
Re1 N1 2.183(11) . ?
Re1 N5 2.195(10) . ?
C1 C2 1.346(19) . ?
C1 N1 1.362(16) . ?
C1 H1 0.9500 . ?
N1 C5 1.313(15) . ?
Cl1 C16 1.88(3) . ?
O1 C7 1.141(18) . ?
O2 C8 1.174(18) . ?
C2 N2 1.375(16) . ?
C2 H2 0.9500 . ?
N2 C5 1.328(16) . ?
N2 H5 0.8800 . ?
N3 C6 1.326(16) . ?
N3 C3 1.393(17) . ?
C3 C4 1.35(2) . ?
C3 H3 0.9500 . ?
Cl2 C17 1.66(4) . ?
O3 C9 1.129(17) . ?
N4 C6 1.335(16) . ?
N4 C4 1.368(19) . ?
C4 H4 0.9500 . ?
N5 C10 1.319(15) . ?
N5 C14 1.350(14) . ?
C5 C6 1.451(16) . ?
N6 C15 1.322(13) 3 ?
N6 C15 1.355(13) . ?
C10 C11 1.369(17) . ?
C10 H6 0.9500 . ?
C11 C12 1.363(16) . ?
C11 H7 0.9500 . ?
C12 C13 1.374(16) . ?
C12 C15 1.478(15) . ?
C13 C14 1.390(15) . ?
C13 H8 0.9500 . ?
C14 H9 0.9500 . ?
C16 C17 1.51(2) . ?
C16 H10A 0.9900 . ?
C16 H10B 0.9900 . ?
C17 H11A 0.9900 . ?
C17 H11B 0.9900 . ?

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
C8 Re1 C9 88.6(6) . . ?
C8 Re1 C7 92.0(7) . . ?
C9 Re1 C7 88.0(6) . . ?
C8 Re1 N3 168.5(5) . . ?
C9 Re1 N3 94.9(5) . . ?
C7 Re1 N3 99.0(6) . . ?
C8 Re1 N1 94.3(5) . . ?
C9 Re1 N1 98.0(5) . . ?
C7 Re1 N1 171.4(5) . . ?
N3 Re1 N1 74.4(4) . . ?
C8 Re1 N5 91.6(5) . . ?
C9 Re1 N5 179.0(5) . . ?
C7 Re1 N5 93.0(5) . . ?
N3 Re1 N5 84.7(4) . . ?
N1 Re1 N5 81.0(4) . . ?
C2 C1 N1 109.1(11) . . ?
C2 C1 H1 125.4 . . ?
N1 C1 H1 125.4 . . ?
C5 N1 C1 106.6(11) . . ?
C5 N1 Re1 115.6(8) . . ?
C1 N1 Re1 137.7(9) . . ?
C1 C2 N2 106.1(11) . . ?
C1 C2 H2 126.9 . . ?
N2 C2 H2 126.9 . . ?
C5 N2 C2 107.4(11) . . ?
C5 N2 H5 126.3 . . ?
C2 N2 H5 126.3 . . ?
C6 N3 C3 104.8(11) . . ?
C6 N3 Re1 116.8(7) . . ?
C3 N3 Re1 138.3(10) . . ?
C4 C3 N3 105.2(13) . . ?
C4 C3 H3 127.4 . . ?
N3 C3 H3 127.4 . . ?
C6 N4 C4 101.0(12) . . ?
C3 C4 N4 113.1(12) . . ?
C3 C4 H4 123.4 . . ?
N4 C4 H4 123.4 . . ?
C10 N5 C14 116.2(10) . . ?
C10 N5 Re1 122.2(8) . . ?
C14 N5 Re1 121.5(7) . . ?
N1 C5 N2 110.8(11) . . ?
N1 C5 C6 117.6(11) . . ?
N2 C5 C6 131.5(11) . . ?
C15 N6 C15 116.2(11) 3 . ?
N3 C6 N4 115.7(11) . . ?
N3 C6 C5 115.4(10) . . ?
N4 C6 C5 128.8(12) . . ?
O3 C9 Re1 178.0(15) . . ?
O2 C8 Re1 175.4(14) . . ?
O1 C7 Re1 179.0(14) . . ?
N5 C10 C11 123.7(11) . . ?
N5 C10 H6 118.1 . . ?
C11 C10 H6 118.1 . . ?
C12 C11 C10 120.2(11) . . ?
C12 C11 H7 119.9 . . ?
C10 C11 H7 119.9 . . ?
C11 C12 C13 118.0(10) . . ?
C11 C12 C15 120.7(10) . . ?
C13 C12 C15 121.2(10) . . ?
C12 C13 C14 118.5(10) . . ?
C12 C13 H8 120.7 . . ?
C14 C13 H8 120.7 . . ?
N5 C14 C13 123.3(10) . . ?
N5 C14 H9 118.3 . . ?
C13 C14 H9 118.3 . . ?
N6 C15 N6 123.7(11) 2 . ?
N6 C15 C12 119.1(10) 2 . ?
N6 C15 C12 117.1(10) . . ?
C17 C16 Cl1 110(3) . . ?
C17 C16 H10A 109.8 . . ?
Cl1 C16 H10A 109.8 . . ?
C17 C16 H10B 109.8 . . ?
Cl1 C16 H10B 109.8 . . ?
H10A C16 H10B 108.2 . . ?
C16 C17 Cl2 101(3) . . ?
C16 C17 H11A 111.6 . . ?
Cl2 C17 H11A 111.6 . . ?
C16 C17 H11B 111.6 . . ?
Cl2 C17 H11B 111.6 . . ?
H11A C17 H11B 109.4 . . ?

_refine_diff_density_max         2.043
_refine_diff_density_min         -1.755
_refine_diff_density_rms         0.206



# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 85 13 ' '
2 -0.333 0.333 0.083 442 143 ' '
3 0.000 0.000 0.250 443 143 ' '
4 0.333 0.667 0.417 442 143 ' '
5 0.000 0.000 0.500 85 13 ' '
6 -0.333 0.333 0.583 443 143 ' '
7 0.000 0.000 0.750 442 143 ' '
8 0.333 0.667 0.917 443 143 ' '
9 0.333 0.667 0.167 86 13 ' '
10 0.333 0.667 0.667 86 13 ' '
11 0.666 0.333 0.333 86 13 ' '
12 0.667 0.333 0.833 86 13 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?




# Solvent Accessible Volume =      3176
# Electrons Found in S.A.V. =       931

# start Validation Reply Form
_vrf_PLAT043_1                   
;
PROBLEM: A Calculated and Reported Mol. Weight Differ by .. 296.82 Check 
RESPONSE: The alerts arise from the SQUEEZE of solvents in the crystal lattice.
;
_vrf_PLAT601_1                   
;
PROBLEM: A Unit Cell Contains Solvent Accessible VOIDS of . 440 Ang**3
RESPONSE: The alerts arise from the SQUEEZE of solvents in the crystal lattice.
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# end Validation Reply Form

