# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_Re4s10_F
_database_code_depnum_ccdc_archive 'CCDC 2024180'
loop_
_audit_author_name
_audit_author_address
'Gerard Parkin'
;Columbia University
United States of America
;
_audit_update_record             
;
2020-08-19 deposited with the CCDC.	2020-09-08 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            'C30 H16 Cl4 N8 O12 Re4 S4'
_chemical_formula_weight         1695.35

# start Validation Reply Form
_vrf_PLAT202_Re4s10_F            
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent ......... 1 Check
RESPONSE: These alerts refer to disordered CH2Cl2 molecules
(Atoms Cl5, Cl5A, Cl6, Cl6A, C37, C37A)
;
_vrf_PLAT260_Re4s10_F            
;
PROBLEM: Large Average Ueq of Residue Including Cl5A 0.140 Check
RESPONSE: These alerts refer to disordered CH2Cl2 molecules
(Atoms Cl5, Cl5A, Cl6, Cl6A, C37, C37A)
;
_vrf_PLAT336_Re4s10_F            
;
PROBLEM: Long Bond Distance for ..... C37A -Cl5A 1.870 Ang.
RESPONSE: These alerts refer to disordered CH2Cl2 molecules
(Atoms Cl5, Cl5A, Cl6, Cl6A, C37, C37A)
;
_vrf_PLAT342_Re4s10_F            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01337 Ang.
RESPONSE:
;
_vrf_PLAT971_Re4s10_F            
;
PROBLEM: Check Calcd Resid. Dens. 1.11A From Cl6A 2.22 eA-3
RESPONSE: These alerts refer to disordered CH2Cl2 molecules
(Atoms Cl5, Cl5A, Cl6, Cl6A, C37, C37A)
;
_vrf_PLAT977_Re4s10_F            
;
PROBLEM: Check Negative Difference Density on H21A -0.34 eA-3
RESPONSE: These alerts refer to disordered CH2Cl2 molecules
(Atoms Cl5, Cl5A, Cl6, Cl6A, C37, C37A)
;
# end Validation Reply Form

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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.1222(9)
_cell_length_b                   15.1915(7)
_cell_length_c                   13.8822(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.7910(10)
_cell_angle_gamma                90
_cell_volume                     4389.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.92

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.565
_exptl_crystal_F_000             3120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    11.495
_shelx_estimated_absorpt_T_min   0.460
_shelx_estimated_absorpt_T_max   0.597
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47546
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.660
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7752
_reflns_number_gt                5879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0242P)²+26.5713P] 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         7752
_refine_ls_number_parameters     558
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0673
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.016
_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
Re1 Re 0.64519(2) 0.23631(2) 0.54616(3) 0.01881(10) Uani 1 1 d . . . . .
Re2 Re 0.60598(2) 0.56706(2) 0.74779(3) 0.01810(9) Uani 1 1 d . . . . .
Re3 Re 0.82729(2) 0.72598(2) 0.60817(3) 0.02127(10) Uani 1 1 d . . . . .
Re4 Re 0.89698(2) 0.36998(2) 0.49649(3) 0.02445(10) Uani 1 1 d . . . . .
S1 S 0.58674(11) 0.37609(15) 0.57962(17) 0.0232(5) Uani 1 1 d . . . . .
S2 S 0.71416(11) 0.64322(15) 0.76123(16) 0.0225(5) Uani 1 1 d . . . . .
S3 S 0.85667(12) 0.60576(15) 0.49642(17) 0.0246(5) Uani 1 1 d . . . . .
S4 S 0.81702(11) 0.27679(15) 0.56675(19) 0.0263(6) Uani 1 1 d . . . . .
N1 N 0.6877(4) 0.3067(5) 0.6773(5) 0.0227(18) Uani 1 1 d . . . . .
N2 N 0.6636(3) 0.4458(5) 0.7412(5) 0.0195(17) Uani 1 1 d . . . . .
N3 N 0.6338(3) 0.6012(5) 0.6089(5) 0.0181(17) Uani 1 1 d . . . . .
N4 N 0.7297(4) 0.6673(5) 0.5716(5) 0.0193(17) Uani 1 1 d . . . . .
N5 N 0.8565(3) 0.6010(5) 0.6797(5) 0.0194(17) Uani 1 1 d . . . . .
N6 N 0.8852(3) 0.4635(5) 0.6162(5) 0.0209(17) Uani 1 1 d . . . . .
N7 N 0.7962(4) 0.3967(5) 0.4363(5) 0.0218(18) Uani 1 1 d . . . . .
N8 N 0.7002(3) 0.3290(5) 0.4672(6) 0.0210(17) Uani 1 1 d . . . . .
O1 O 0.7322(3) 0.0739(4) 0.5551(5) 0.0374(18) Uani 1 1 d . . . . .
O2 O 0.5750(3) 0.1742(4) 0.3461(5) 0.0305(16) Uani 1 1 d . . . . .
O3 O 0.5647(3) 0.1131(4) 0.6505(5) 0.0376(18) Uani 1 1 d . . . . .
O4 O 0.4709(3) 0.4944(5) 0.6789(5) 0.0363(18) Uani 1 1 d . . . . .
O5 O 0.5895(4) 0.5082(4) 0.9538(5) 0.042(2) Uani 1 1 d . . . . .
O6 O 0.5411(3) 0.7413(4) 0.7852(5) 0.0339(17) Uani 1 1 d . . . . .
O7 O 0.8000(4) 0.8433(5) 0.7764(5) 0.0415(19) Uani 1 1 d . . . . .
O8 O 0.7894(4) 0.8857(5) 0.4752(5) 0.050(2) Uani 1 1 d . . . . .
O9 O 0.9627(4) 0.8041(6) 0.6447(6) 0.056(2) Uani 1 1 d . . . . .
O10 O 0.9704(3) 0.4892(5) 0.3761(5) 0.0400(19) Uani 1 1 d . . . . .
O11 O 1.0248(4) 0.3001(5) 0.6098(6) 0.051(2) Uani 1 1 d . . . . .
O12 O 0.8986(4) 0.2342(6) 0.3350(7) 0.066(3) Uani 1 1 d . . . . .
C1 C 0.7015(4) 0.1375(6) 0.5499(7) 0.024(2) Uani 1 1 d . . . . .
C2 C 0.6006(5) 0.1969(6) 0.4222(7) 0.022(2) Uani 1 1 d . . . . .
C3 C 0.5931(5) 0.1622(6) 0.6109(7) 0.026(2) Uani 1 1 d . . . . .
C4 C 0.5223(5) 0.5182(6) 0.7040(7) 0.026(2) Uani 1 1 d . . . . .
C5 C 0.5961(4) 0.5323(6) 0.8768(7) 0.023(2) Uani 1 1 d . . . . .
C6 C 0.5642(4) 0.6772(6) 0.7673(6) 0.022(2) Uani 1 1 d . . . . .
C7 C 0.8082(5) 0.7974(7) 0.7138(7) 0.029(2) Uani 1 1 d . . . . .
C8 C 0.8035(5) 0.8242(7) 0.5252(7) 0.032(3) Uani 1 1 d . . . . .
C9 C 0.9128(5) 0.7720(7) 0.6323(8) 0.037(3) Uani 1 1 d . . . . .
C10 C 0.9433(5) 0.4472(7) 0.4239(7) 0.032(2) Uani 1 1 d . . . . .
C11 C 0.9777(5) 0.3273(7) 0.5668(8) 0.038(3) Uani 1 1 d . . . . .
C12 C 0.9002(5) 0.2846(7) 0.3968(9) 0.038(3) Uani 1 1 d . . . . .
C13 C 0.7367(4) 0.2946(6) 0.7508(6) 0.021(2) Uani 1 1 d . . . . .
H13A H 0.7621 0.2428 0.7531 0.026 Uiso 1 1 calc R U . . .
C14 C 0.7504(4) 0.3572(6) 0.8236(7) 0.024(2) Uani 1 1 d . . . . .
H14A H 0.7839 0.3488 0.8779 0.028 Uiso 1 1 calc R U . . .
C15 C 0.7138(4) 0.4319(6) 0.8142(6) 0.023(2) Uani 1 1 d . . . . .
H15A H 0.7242 0.4768 0.8619 0.027 Uiso 1 1 calc R U . . .
C16 C 0.6499(4) 0.3803(6) 0.6751(6) 0.0169(19) Uani 1 1 d . . . . .
C17 C 0.6096(5) 0.5952(6) 0.5152(6) 0.022(2) Uani 1 1 d . . . . .
H17A H 0.5689 0.5682 0.4959 0.027 Uiso 1 1 calc R U . . .
C18 C 0.6426(4) 0.6275(6) 0.4440(6) 0.023(2) Uani 1 1 d . . . . .
H18A H 0.6245 0.6257 0.3765 0.027 Uiso 1 1 calc R U . . .
C19 C 0.7024(5) 0.6620(6) 0.4760(6) 0.024(2) Uani 1 1 d . . . . .
H19A H 0.7261 0.6834 0.4285 0.029 Uiso 1 1 calc R U . . .
C20 C 0.6924(5) 0.6385(6) 0.6362(6) 0.022(2) Uani 1 1 d . . . . .
C21 C 0.8684(4) 0.5702(7) 0.7713(7) 0.028(2) Uani 1 1 d . . . . .
H21A H 0.8622 0.6070 0.8242 0.034 Uiso 1 1 calc R U . . .
C22 C 0.8895(5) 0.4851(6) 0.7889(7) 0.029(2) Uani 1 1 d . . . . .
H22A H 0.8988 0.4627 0.8536 0.035 Uiso 1 1 calc R U . . .
C23 C 0.8968(4) 0.4333(7) 0.7099(7) 0.027(2) Uani 1 1 d . . . . .
H23A H 0.9105 0.3741 0.7213 0.032 Uiso 1 1 calc R U . . .
C24 C 0.8673(4) 0.5487(6) 0.6043(6) 0.021(2) Uani 1 1 d . . . . .
C25 C 0.7627(5) 0.4456(6) 0.3659(7) 0.025(2) Uani 1 1 d . . . . .
H25A H 0.7844 0.4874 0.3324 0.030 Uiso 1 1 calc R U . . .
C26 C 0.6975(4) 0.4365(6) 0.3410(7) 0.024(2) Uani 1 1 d . . . . .
H26A H 0.6737 0.4684 0.2880 0.029 Uiso 1 1 calc R U . . .
C27 C 0.6679(5) 0.3794(6) 0.3958(6) 0.024(2) Uani 1 1 d . . . . .
H27A H 0.6224 0.3753 0.3826 0.029 Uiso 1 1 calc R U . . .
C28 C 0.7653(4) 0.3380(6) 0.4860(6) 0.021(2) Uani 1 1 d . . . . .
C37 C 0.9480(10) 0.1112(15) 0.6679(15) 0.042(3) Uani 0.490(13) 1 d D . P A 1
H29A H 0.9343 0.1719 0.6802 0.050 Uiso 0.490(13) 1 calc R U P A 1
H29B H 0.9748 0.0867 0.7273 0.050 Uiso 0.490(13) 1 calc R U P A 1
Cl5 Cl 0.9885(7) 0.1025(13) 0.5536(14) 0.140(2) Uani 0.490(13) 1 d D . P A 1
Cl6 Cl 0.8765(8) 0.0347(10) 0.6143(13) 0.140(2) Uani 0.490(13) 1 d D . P A 1
C37A C 0.9536(12) 0.019(2) 0.650(2) 0.109(13) Uiso 0.510(13) 1 d D . P A 2
H29C H 0.9859 0.0324 0.7090 0.130 Uiso 0.510(13) 1 calc R U P A 2
H29D H 0.9571 -0.0434 0.6318 0.130 Uiso 0.510(13) 1 calc R U P A 2
Cl5A Cl 0.9599(7) 0.0957(12) 0.5466(14) 0.140(2) Uani 0.510(13) 1 d D . P A 2
Cl6A Cl 0.8692(8) 0.0487(10) 0.6682(13) 0.140(2) Uani 0.510(13) 1 d D . P A 2
C38 C 0.5706(5) 0.6217(8) 1.1244(8) 0.042(3) Uani 1 1 d . . . . .
H30A H 0.5573 0.5633 1.0964 0.050 Uiso 1 1 calc R U . . .
H30B H 0.5464 0.6338 1.1780 0.050 Uiso 1 1 calc R U . . .
Cl7 Cl 0.65355(14) 0.6204(2) 1.1712(2) 0.0504(8) Uani 1 1 d . . . . .
Cl8 Cl 0.55268(14) 0.70238(17) 1.0339(2) 0.0394(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C3 1.903(10) . ?
Re1 C1 1.910(10) . ?
Re1 C2 1.912(10) . ?
Re1 N1 2.170(7) . ?
Re1 N8 2.229(7) . ?
Re1 S1 2.538(2) . ?
Re2 C5 1.912(9) . ?
Re2 C4 1.918(11) . ?
Re2 C6 1.932(10) . ?
Re2 N3 2.171(7) . ?
Re2 N2 2.219(7) . ?
Re2 S2 2.540(2) . ?
Re3 C8 1.899(11) . ?
Re3 C9 1.913(11) . ?
Re3 C7 1.921(11) . ?
Re3 N5 2.182(7) . ?
Re3 N4 2.224(7) . ?
Re3 S3 2.541(2) . ?
Re4 C12 1.906(11) . ?
Re4 C10 1.918(11) . ?
Re4 C11 1.928(12) . ?
Re4 N7 2.188(8) . ?
Re4 N6 2.232(7) . ?
Re4 S4 2.524(2) . ?
S1 C16 1.714(9) . ?
S2 C20 1.719(9) . ?
S3 C24 1.712(9) . ?
S4 C28 1.703(9) . ?
N1 C13 1.337(11) . ?
N1 C16 1.371(11) . ?
N2 C16 1.351(11) . ?
N2 C15 1.353(11) . ?
N3 C17 1.317(11) . ?
N3 C20 1.356(11) . ?
N4 C19 1.356(11) . ?
N4 C20 1.364(11) . ?
N5 C21 1.339(11) . ?
N5 C24 1.363(11) . ?
N6 C24 1.350(11) . ?
N6 C23 1.362(11) . ?
N7 C25 1.331(11) . ?
N7 C28 1.362(11) . ?
N8 C27 1.344(11) . ?
N8 C28 1.361(11) . ?
O1 C1 1.158(11) . ?
O2 C2 1.155(11) . ?
O3 C3 1.154(11) . ?
O4 C4 1.141(11) . ?
O5 C5 1.160(10) . ?
O6 C6 1.135(10) . ?
O7 C7 1.151(11) . ?
O8 C8 1.172(12) . ?
O9 C9 1.147(12) . ?
O10 C10 1.144(11) . ?
O11 C11 1.146(12) . ?
O12 C12 1.146(12) . ?
C13 C14 1.383(12) . ?
C13 H13A 0.9500 . ?
C14 C15 1.367(12) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
C17 C18 1.392(12) . ?
C17 H17A 0.9500 . ?
C18 C19 1.370(13) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C21 C22 1.375(13) . ?
C21 H21A 0.9500 . ?
C22 C23 1.380(13) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C25 C26 1.370(13) . ?
C25 H25A 0.9500 . ?
C26 C27 1.372(12) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C37 Cl5 1.931(18) . ?
C37 Cl6 1.951(17) . ?
C37 H29A 0.9900 . ?
C37 H29B 0.9900 . ?
C37A Cl5A 1.874(19) . ?
C37A Cl6A 1.895(19) . ?
C37A H29C 0.9900 . ?
C37A H29D 0.9900 . ?
C38 Cl8 1.749(10) . ?
C38 Cl7 1.762(11) . ?
C38 H30A 0.9900 . ?
C38 H30B 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
C3 Re1 C1 86.0(4) . . ?
C3 Re1 C2 90.2(4) . . ?
C1 Re1 C2 89.3(4) . . ?
C3 Re1 N1 94.9(3) . . ?
C1 Re1 N1 101.4(3) . . ?
C2 Re1 N1 168.4(3) . . ?
C3 Re1 N8 176.0(3) . . ?
C1 Re1 N8 97.7(3) . . ?
C2 Re1 N8 88.5(3) . . ?
N1 Re1 N8 85.7(3) . . ?
C3 Re1 S1 94.0(3) . . ?
C1 Re1 S1 166.5(3) . . ?
C2 Re1 S1 104.2(3) . . ?
N1 Re1 S1 65.1(2) . . ?
N8 Re1 S1 82.65(19) . . ?
C5 Re2 C4 87.1(4) . . ?
C5 Re2 C6 89.0(4) . . ?
C4 Re2 C6 87.8(4) . . ?
C5 Re2 N3 170.5(3) . . ?
C4 Re2 N3 100.7(3) . . ?
C6 Re2 N3 96.7(3) . . ?
C5 Re2 N2 87.6(3) . . ?
C4 Re2 N2 98.5(3) . . ?
C6 Re2 N2 172.6(3) . . ?
N3 Re2 N2 85.9(3) . . ?
C5 Re2 S2 107.3(3) . . ?
C4 Re2 S2 165.6(3) . . ?
C6 Re2 S2 91.2(3) . . ?
N3 Re2 S2 65.20(19) . . ?
N2 Re2 S2 83.58(19) . . ?
C8 Re3 C9 87.9(5) . . ?
C8 Re3 C7 87.2(4) . . ?
C9 Re3 C7 88.6(4) . . ?
C8 Re3 N5 169.8(3) . . ?
C9 Re3 N5 93.0(4) . . ?
C7 Re3 N5 102.9(3) . . ?
C8 Re3 N4 92.1(4) . . ?
C9 Re3 N4 176.1(4) . . ?
C7 Re3 N4 95.4(3) . . ?
N5 Re3 N4 86.3(3) . . ?
C8 Re3 S3 105.2(3) . . ?
C9 Re3 S3 92.8(3) . . ?
C7 Re3 S3 167.6(3) . . ?
N5 Re3 S3 64.71(19) . . ?
N4 Re3 S3 83.43(19) . . ?
C12 Re4 C10 87.2(4) . . ?
C12 Re4 C11 90.1(5) . . ?
C10 Re4 C11 89.2(4) . . ?
C12 Re4 N7 90.1(4) . . ?
C10 Re4 N7 103.6(4) . . ?
C11 Re4 N7 167.2(4) . . ?
C12 Re4 N6 174.7(4) . . ?
C10 Re4 N6 97.6(3) . . ?
C11 Re4 N6 92.2(4) . . ?
N7 Re4 N6 86.6(3) . . ?
C12 Re4 S4 90.5(3) . . ?
C10 Re4 S4 168.6(3) . . ?
C11 Re4 S4 102.0(3) . . ?
N7 Re4 S4 65.2(2) . . ?
N6 Re4 S4 84.41(19) . . ?
C16 S1 Re1 80.4(3) . . ?
C20 S2 Re2 79.9(3) . . ?
C24 S3 Re3 80.7(3) . . ?
C28 S4 Re4 80.6(3) . . ?
C13 N1 C16 120.2(8) . . ?
C13 N1 Re1 136.8(6) . . ?
C16 N1 Re1 103.1(5) . . ?
C16 N2 C15 116.4(8) . . ?
C16 N2 Re2 125.7(6) . . ?
C15 N2 Re2 117.7(6) . . ?
C17 N3 C20 119.2(8) . . ?
C17 N3 Re2 137.9(6) . . ?
C20 N3 Re2 102.9(5) . . ?
C19 N4 C20 115.3(8) . . ?
C19 N4 Re3 118.1(6) . . ?
C20 N4 Re3 126.5(6) . . ?
C21 N5 C24 119.8(8) . . ?
C21 N5 Re3 136.8(6) . . ?
C24 N5 Re3 103.2(5) . . ?
C24 N6 C23 116.2(8) . . ?
C24 N6 Re4 125.7(6) . . ?
C23 N6 Re4 118.1(6) . . ?
C25 N7 C28 119.7(8) . . ?
C25 N7 Re4 138.2(6) . . ?
C28 N7 Re4 101.8(6) . . ?
C27 N8 C28 117.0(8) . . ?
C27 N8 Re1 118.7(6) . . ?
C28 N8 Re1 124.3(6) . . ?
O1 C1 Re1 174.7(8) . . ?
O2 C2 Re1 178.2(8) . . ?
O3 C3 Re1 175.5(8) . . ?
O4 C4 Re2 175.5(8) . . ?
O5 C5 Re2 177.5(8) . . ?
O6 C6 Re2 175.5(8) . . ?
O7 C7 Re3 175.7(9) . . ?
O8 C8 Re3 178.9(9) . . ?
O9 C9 Re3 176.1(11) . . ?
O10 C10 Re4 175.6(9) . . ?
O11 C11 Re4 178.0(10) . . ?
O12 C12 Re4 176.2(9) . . ?
N1 C13 C14 120.1(9) . . ?
N1 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C15 C14 C13 117.2(9) . . ?
C15 C14 H14A 121.4 . . ?
C13 C14 H14A 121.4 . . ?
N2 C15 C14 124.1(9) . . ?
N2 C15 H15A 118.0 . . ?
C14 C15 H15A 118.0 . . ?
N2 C16 N1 121.9(8) . . ?
N2 C16 S1 127.0(7) . . ?
N1 C16 S1 111.2(6) . . ?
N3 C17 C18 121.3(8) . . ?
N3 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C19 C18 C17 116.7(8) . . ?
C19 C18 H18A 121.6 . . ?
C17 C18 H18A 121.6 . . ?
N4 C19 C18 123.7(9) . . ?
N4 C19 H19A 118.1 . . ?
C18 C19 H19A 118.1 . . ?
N3 C20 N4 123.6(8) . . ?
N3 C20 S2 112.0(6) . . ?
N4 C20 S2 124.5(7) . . ?
N5 C21 C22 120.0(9) . . ?
N5 C21 H21A 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C21 C22 C23 118.1(9) . . ?
C21 C22 H22A 120.9 . . ?
C23 C22 H22A 120.9 . . ?
N6 C23 C22 122.7(9) . . ?
N6 C23 H23A 118.7 . . ?
C22 C23 H23A 118.7 . . ?
N6 C24 N5 123.0(8) . . ?
N6 C24 S3 125.7(7) . . ?
N5 C24 S3 111.3(7) . . ?
N7 C25 C26 121.1(9) . . ?
N7 C25 H25A 119.5 . . ?
C26 C25 H25A 119.5 . . ?
C25 C26 C27 117.2(9) . . ?
C25 C26 H26A 121.4 . . ?
C27 C26 H26A 121.4 . . ?
N8 C27 C26 123.2(9) . . ?
N8 C27 H27A 118.4 . . ?
C26 C27 H27A 118.4 . . ?
N8 C28 N7 121.7(8) . . ?
N8 C28 S4 125.8(7) . . ?
N7 C28 S4 112.4(7) . . ?
Cl5 C37 Cl6 94.0(11) . . ?
Cl5 C37 H29A 112.9 . . ?
Cl6 C37 H29A 112.9 . . ?
Cl5 C37 H29B 112.9 . . ?
Cl6 C37 H29B 112.9 . . ?
H29A C37 H29B 110.3 . . ?
Cl5A C37A Cl6A 98.3(13) . . ?
Cl5A C37A H29C 112.1 . . ?
Cl6A C37A H29C 112.1 . . ?
Cl5A C37A H29D 112.1 . . ?
Cl6A C37A H29D 112.1 . . ?
H29C C37A H29D 109.7 . . ?
Cl8 C38 Cl7 110.7(6) . . ?
Cl8 C38 H30A 109.5 . . ?
Cl7 C38 H30A 109.5 . . ?
Cl8 C38 H30B 109.5 . . ?
Cl7 C38 H30B 109.5 . . ?
H30A C38 H30B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N1 C13 C14 -1.7(13) . . . . ?
Re1 N1 C13 C14 178.8(7) . . . . ?
N1 C13 C14 C15 -2.6(13) . . . . ?
C16 N2 C15 C14 0.5(13) . . . . ?
Re2 N2 C15 C14 174.9(7) . . . . ?
C13 C14 C15 N2 3.2(14) . . . . ?
C15 N2 C16 N1 -5.0(12) . . . . ?
Re2 N2 C16 N1 -178.9(6) . . . . ?
C15 N2 C16 S1 175.7(7) . . . . ?
Re2 N2 C16 S1 1.8(11) . . . . ?
C13 N1 C16 N2 5.7(13) . . . . ?
Re1 N1 C16 N2 -174.6(7) . . . . ?
C13 N1 C16 S1 -175.0(6) . . . . ?
Re1 N1 C16 S1 4.7(7) . . . . ?
Re1 S1 C16 N2 175.3(8) . . . . ?
Re1 S1 C16 N1 -4.0(6) . . . . ?
C20 N3 C17 C18 -1.0(13) . . . . ?
Re2 N3 C17 C18 178.6(6) . . . . ?
N3 C17 C18 C19 2.9(13) . . . . ?
C20 N4 C19 C18 -2.3(13) . . . . ?
Re3 N4 C19 C18 -179.8(7) . . . . ?
C17 C18 C19 N4 -1.2(14) . . . . ?
C17 N3 C20 N4 -2.9(13) . . . . ?
Re2 N3 C20 N4 177.4(7) . . . . ?
C17 N3 C20 S2 178.1(7) . . . . ?
Re2 N3 C20 S2 -1.6(7) . . . . ?
C19 N4 C20 N3 4.5(12) . . . . ?
Re3 N4 C20 N3 -178.2(6) . . . . ?
C19 N4 C20 S2 -176.7(7) . . . . ?
Re3 N4 C20 S2 0.6(11) . . . . ?
Re2 S2 C20 N3 1.3(6) . . . . ?
Re2 S2 C20 N4 -177.6(8) . . . . ?
C24 N5 C21 C22 -1.9(13) . . . . ?
Re3 N5 C21 C22 -176.9(7) . . . . ?
N5 C21 C22 C23 -1.1(14) . . . . ?
C24 N6 C23 C22 1.5(13) . . . . ?
Re4 N6 C23 C22 -178.5(7) . . . . ?
C21 C22 C23 N6 1.3(14) . . . . ?
C23 N6 C24 N5 -4.7(13) . . . . ?
Re4 N6 C24 N5 175.3(6) . . . . ?
C23 N6 C24 S3 173.9(7) . . . . ?
Re4 N6 C24 S3 -6.1(11) . . . . ?
C21 N5 C24 N6 5.0(13) . . . . ?
Re3 N5 C24 N6 -178.5(7) . . . . ?
C21 N5 C24 S3 -173.7(7) . . . . ?
Re3 N5 C24 S3 2.7(7) . . . . ?
Re3 S3 C24 N6 179.0(8) . . . . ?
Re3 S3 C24 N5 -2.3(6) . . . . ?
C28 N7 C25 C26 -1.5(13) . . . . ?
Re4 N7 C25 C26 171.5(7) . . . . ?
N7 C25 C26 C27 4.2(13) . . . . ?
C28 N8 C27 C26 1.7(13) . . . . ?
Re1 N8 C27 C26 -178.0(7) . . . . ?
C25 C26 C27 N8 -4.4(14) . . . . ?
C27 N8 C28 N7 1.3(12) . . . . ?
Re1 N8 C28 N7 -179.1(6) . . . . ?
C27 N8 C28 S4 -175.4(7) . . . . ?
Re1 N8 C28 S4 4.3(11) . . . . ?
C25 N7 C28 N8 -1.4(13) . . . . ?
Re4 N7 C28 N8 -176.6(7) . . . . ?
C25 N7 C28 S4 175.7(7) . . . . ?
Re4 N7 C28 S4 0.5(7) . . . . ?
Re4 S4 C28 N8 176.5(8) . . . . ?
Re4 S4 C28 N7 -0.4(6) . . . . ?

_refine_diff_density_max         2.390
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.219

####################################################################### 
# 
# 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_Cd4s10_F
_database_code_depnum_ccdc_archive 'CCDC 2024181'
loop_
_audit_author_name
_audit_author_address
'Gerard Parkin'
;Columbia University
United States of America
;
_audit_update_record             
;
2020-08-19 deposited with the CCDC.	2020-09-08 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            'C38 H16 Cd4 Cl8 O12'
_chemical_formula_weight         1397.71

# start Validation Reply Form
_vrf_PLAT973_Cd4s10_F            
;
PROBLEM: Check Calcd Positive Resid. Density on Cd2 2.75 eA-3
RESPONSE: This refinement is intended to illustrate the impact of INCORRECTLY
refining rhenium as cadmium, which results in numerous alerts in this and
subsequent sections.
;
# end Validation Reply Form

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.1224(9)
_cell_length_b                   15.1913(7)
_cell_length_c                   13.8819(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.7881(7)
_cell_angle_gamma                90
_cell_volume                     4389.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.74

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_F_000             2672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.459
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.887
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47546
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.660
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7752
_reflns_number_gt                5879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1251P)²+97.5693P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7752
_refine_ls_number_parameters     559
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.2167
_refine_ls_wR_factor_gt          0.1947
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_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
Cd1 Cd 0.64519(4) 0.23627(5) 0.54613(6) 0.0128(2) Uani 1 1 d . . . . .
Cd2 Cd 0.60595(4) 0.56701(5) 0.74778(5) 0.0122(2) Uani 1 1 d . . . . .
Cd3 Cd 0.82729(4) 0.72600(5) 0.60819(6) 0.0154(2) Uani 1 1 d . . . . .
Cd4 Cd 0.89695(4) 0.37000(5) 0.49650(6) 0.0182(3) Uani 1 1 d . . . . .
Cl1 Cl 0.5867(2) 0.3761(3) 0.5794(4) 0.0638(12) Uani 1 1 d . . . . .
Cl2 Cl 0.7142(3) 0.6430(3) 0.7611(4) 0.0640(12) Uani 1 1 d . . . . .
Cl3 Cl 0.8570(3) 0.6059(3) 0.4964(4) 0.0662(13) Uani 1 1 d . . . . .
Cl4 Cl 0.8172(2) 0.2766(3) 0.5672(4) 0.0682(13) Uani 1 1 d . . . . .
O1 O 0.7346(8) 0.0716(10) 0.5555(14) 0.090(5) Uani 1 1 d . . . . .
O2 O 0.5755(8) 0.1759(11) 0.3463(11) 0.085(5) Uani 1 1 d . . . . .
O3 O 0.5650(9) 0.1120(10) 0.6511(13) 0.091(5) Uani 1 1 d . . . . .
O4 O 0.4723(8) 0.4936(10) 0.6802(12) 0.082(4) Uani 1 1 d . . . . .
O5 O 0.5891(9) 0.5082(10) 0.9551(10) 0.087(5) Uani 1 1 d . . . . .
O6 O 0.5397(8) 0.7431(9) 0.7836(12) 0.078(4) Uani 1 1 d . . . . .
O7 O 0.7995(9) 0.8452(11) 0.7766(12) 0.091(5) Uani 1 1 d . . . . .
O8 O 0.7921(10) 0.8850(11) 0.4745(13) 0.100(6) Uani 1 1 d . . . . .
O9 O 0.9637(9) 0.8016(14) 0.6455(15) 0.111(6) Uani 1 1 d . . . . .
O10 O 0.9695(8) 0.4900(11) 0.3754(13) 0.086(5) Uani 1 1 d . . . . .
O11 O 1.0253(8) 0.2994(13) 0.6087(17) 0.112(7) Uani 1 1 d . . . . .
O12 O 0.8977(10) 0.2317(13) 0.3349(16) 0.118(7) Uani 1 1 d . . . . .
C1 C 0.7018(10) 0.1390(13) 0.5503(16) 0.065(5) Uani 1 1 d . . . . .
C2 C 0.6030(12) 0.1986(13) 0.4251(15) 0.069(6) Uani 1 1 d . . . . .
C3 C 0.5941(11) 0.1630(14) 0.6106(16) 0.067(5) Uani 1 1 d . . . . .
C4 C 0.5235(10) 0.5173(14) 0.7040(16) 0.063(5) Uani 1 1 d . . . . .
C5 C 0.5944(10) 0.5314(14) 0.8764(16) 0.068(5) Uani 1 1 d . . . . .
C6 C 0.5645(10) 0.6766(15) 0.7660(15) 0.067(5) Uani 1 1 d . . . . .
C7 C 0.8069(10) 0.7958(15) 0.7125(16) 0.068(5) Uani 1 1 d . . . . .
C8 C 0.8034(11) 0.8228(14) 0.5249(16) 0.069(6) Uani 1 1 d . . . . .
C9 C 0.9137(10) 0.7708(18) 0.6315(19) 0.083(7) Uani 1 1 d . . . . .
C10 C 0.9416(11) 0.4470(15) 0.4253(15) 0.068(5) Uani 1 1 d . . . . .
C11 C 0.9757(12) 0.3255(15) 0.5635(19) 0.079(6) Uani 1 1 d . . . . .
C12 C 0.9014(11) 0.2838(14) 0.399(2) 0.077(7) Uani 1 1 d . . . . .
C13 C 0.6876(8) 0.3047(11) 0.6756(12) 0.047(4) Uani 1 1 d . . . . .
C14 C 0.7373(10) 0.2948(13) 0.7500(14) 0.062(5) Uani 1 1 d . . . . .
H14A H 0.7635 0.2438 0.7518 0.074 Uiso 1 1 calc R U . . .
C15 C 0.7515(9) 0.3579(13) 0.8256(14) 0.059(5) Uani 1 1 d . . . . .
H15A H 0.7851 0.3501 0.8799 0.071 Uiso 1 1 calc R U . . .
C16 C 0.7130(10) 0.4317(13) 0.8143(14) 0.062(5) Uani 1 1 d . . . . .
H16A H 0.7225 0.4767 0.8621 0.075 Uiso 1 1 calc R U . . .
C17 C 0.6635(7) 0.4456(10) 0.7423(11) 0.039(3) Uani 1 1 d . . . . .
C18 C 0.6492(9) 0.3807(12) 0.6748(14) 0.054(4) Uani 1 1 d . . . . .
C19 C 0.6339(7) 0.6004(10) 0.6096(12) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.6106(9) 0.5941(15) 0.5146(13) 0.063(5) Uani 1 1 d . . . . .
H20A H 0.5701 0.5664 0.4951 0.076 Uiso 1 1 calc R U . . .
C21 C 0.6425(10) 0.6261(14) 0.4434(14) 0.063(5) Uani 1 1 d . . . . .
H21A H 0.6240 0.6230 0.3762 0.076 Uiso 1 1 calc R U . . .
C22 C 0.7034(11) 0.6636(12) 0.4738(15) 0.065(5) Uani 1 1 d . . . . .
H22A H 0.7264 0.6868 0.4265 0.078 Uiso 1 1 calc R U . . .
C23 C 0.7305(8) 0.6673(10) 0.5725(11) 0.041(4) Uani 1 1 d . . . . .
C24 C 0.6932(11) 0.6403(12) 0.6376(15) 0.066(5) Uani 1 1 d . . . . .
C25 C 0.8564(8) 0.6024(10) 0.6800(11) 0.042(4) Uani 1 1 d . . . . .
C26 C 0.8674(9) 0.5708(15) 0.7720(15) 0.066(5) Uani 1 1 d . . . . .
H26A H 0.8600 0.6073 0.8246 0.080 Uiso 1 1 calc R U . . .
C27 C 0.8899(11) 0.4839(14) 0.7909(16) 0.068(5) Uani 1 1 d . . . . .
H27A H 0.9001 0.4617 0.8557 0.082 Uiso 1 1 calc R U . . .
C28 C 0.8965(9) 0.4315(15) 0.7093(14) 0.063(5) Uani 1 1 d . . . . .
H28A H 0.9099 0.3721 0.7195 0.076 Uiso 1 1 calc R U . . .
C29 C 0.8843(8) 0.4636(10) 0.6166(12) 0.044(4) Uani 1 1 d . . . . .
C30 C 0.8667(9) 0.5482(14) 0.6027(14) 0.061(5) Uani 1 1 d . . . . .
C31 C 0.7963(8) 0.3970(10) 0.4357(12) 0.042(4) Uani 1 1 d . . . . .
C32 C 0.7640(9) 0.4457(12) 0.3678(14) 0.057(5) Uani 1 1 d . . . . .
H32A H 0.7859 0.4882 0.3355 0.069 Uiso 1 1 calc R U . . .
C33 C 0.6968(10) 0.4361(13) 0.3413(15) 0.064(5) Uani 1 1 d . . . . .
H33A H 0.6733 0.4675 0.2876 0.077 Uiso 1 1 calc R U . . .
C34 C 0.6671(10) 0.3801(13) 0.3960(14) 0.060(5) Uani 1 1 d . . . . .
H34A H 0.6215 0.3772 0.3841 0.072 Uiso 1 1 calc R U . . .
C35 C 0.6998(7) 0.3291(10) 0.4659(12) 0.043(4) Uani 1 1 d . . . . .
C36 C 0.7664(10) 0.3359(14) 0.4849(14) 0.062(5) Uani 1 1 d . . . . .
C37 C 0.962(5) 0.148(5) 0.681(7) 0.082(7) Uani 0.243(18) 1 d D . P A 1
H29A H 0.9929 0.1571 0.7423 0.099 Uiso 0.243(18) 1 calc R U P A 1
H29B H 0.9269 0.1911 0.6700 0.099 Uiso 0.243(18) 1 calc R U P A 1
Cl5 Cl 1.004(3) 0.111(5) 0.552(6) 0.263(9) Uani 0.243(18) 1 d D . P A 1
Cl6 Cl 0.937(3) 0.011(4) 0.641(6) 0.263(9) Uani 0.243(18) 1 d D . P A 1
C37A C 0.959(3) 0.109(6) 0.709(5) 0.28(5) Uiso 0.757(18) 1 d D . P A 2
H29C H 0.9897 0.0745 0.7554 0.332 Uiso 0.757(18) 1 calc R U P A 2
H29D H 0.9521 0.1697 0.7319 0.332 Uiso 0.757(18) 1 calc R U P A 2
Cl5A Cl 0.9646(12) 0.0947(16) 0.554(2) 0.263(9) Uani 0.757(18) 1 d D . P A 2
Cl6A Cl 0.8731(10) 0.0397(14) 0.637(2) 0.263(9) Uani 0.757(18) 1 d D . P A 2
C38 C 0.5705(12) 0.6193(16) 1.1273(18) 0.082(7) Uani 1 1 d . . . . .
H30A H 0.5465 0.6314 1.1813 0.099 Uiso 1 1 calc R U . . .
H30B H 0.5575 0.5607 1.0998 0.099 Uiso 1 1 calc R U . . .
Cl7 Cl 0.6539(3) 0.6208(5) 1.1719(5) 0.0928(19) Uani 1 1 d . . . . .
Cl8 Cl 0.5523(3) 0.7030(4) 1.0334(4) 0.0831(16) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 C2 1.85(2) . ?
Cd1 C3 1.88(2) . ?
Cd1 C1 1.89(2) . ?
Cd1 C13 2.137(17) . ?
Cd1 C35 2.235(16) . ?
Cd1 Cl1 2.539(5) . ?
Cd2 C4 1.90(2) . ?
Cd2 C6 1.92(2) . ?
Cd2 C5 1.92(2) . ?
Cd2 C19 2.162(16) . ?
Cd2 C17 2.218(16) . ?
Cd2 Cl2 2.539(5) . ?
Cd3 C8 1.89(2) . ?
Cd3 C7 1.90(2) . ?
Cd3 C9 1.92(2) . ?
Cd3 C25 2.166(16) . ?
Cd3 C23 2.209(16) . ?
Cd3 Cl3 2.542(5) . ?
Cd4 C10 1.88(2) . ?
Cd4 C11 1.89(3) . ?
Cd4 C12 1.89(2) . ?
Cd4 C31 2.189(17) . ?
Cd4 C29 2.241(17) . ?
Cd4 Cl4 2.526(5) . ?
Cl1 C18 1.71(2) . ?
Cl2 C24 1.70(2) . ?
Cl3 C30 1.70(2) . ?
Cl4 C36 1.69(2) . ?
O1 C1 1.23(2) . ?
O2 C2 1.20(2) . ?
O3 C3 1.19(3) . ?
O4 C4 1.14(2) . ?
O5 C5 1.17(2) . ?
O6 C6 1.18(2) . ?
O7 C7 1.19(2) . ?
O8 C8 1.18(2) . ?
O9 C9 1.14(2) . ?
O10 C10 1.18(2) . ?
O11 C11 1.19(3) . ?
O12 C12 1.19(3) . ?
C13 C14 1.35(3) . ?
C13 C18 1.41(2) . ?
C14 C15 1.42(3) . ?
C15 C16 1.38(3) . ?
C16 C17 1.33(3) . ?
C17 C18 1.36(2) . ?
C19 C20 1.33(2) . ?
C19 C24 1.39(3) . ?
C20 C21 1.38(3) . ?
C21 C22 1.40(3) . ?
C22 C23 1.39(2) . ?
C23 C24 1.36(2) . ?
C25 C26 1.35(2) . ?
C25 C30 1.40(2) . ?
C26 C27 1.41(3) . ?
C27 C28 1.41(3) . ?
C28 C29 1.36(2) . ?
C29 C30 1.34(3) . ?
C31 C32 1.30(2) . ?
C31 C36 1.37(2) . ?
C32 C33 1.41(3) . ?
C33 C34 1.36(3) . ?
C34 C35 1.34(2) . ?
C35 C36 1.39(2) . ?
C37 Cl6 2.19(5) . ?
C37 Cl5 2.19(5) . ?
C37A Cl6A 2.19(5) . ?
C37A Cl5A 2.19(5) . ?
C38 Cl7 1.76(3) . ?
C38 Cl8 1.81(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Cd1 C3 91.2(9) . . ?
C2 Cd1 C1 89.4(9) . . ?
C3 Cd1 C1 86.2(9) . . ?
C2 Cd1 C13 168.8(8) . . ?
C3 Cd1 C13 94.6(8) . . ?
C1 Cd1 C13 100.4(8) . . ?
C2 Cd1 C35 87.3(8) . . ?
C3 Cd1 C35 176.0(7) . . ?
C1 Cd1 C35 97.5(7) . . ?
C13 Cd1 C35 86.2(6) . . ?
C2 Cd1 Cl1 104.4(6) . . ?
C3 Cd1 Cl1 94.2(6) . . ?
C1 Cd1 Cl1 166.1(6) . . ?
C13 Cd1 Cl1 65.7(5) . . ?
C35 Cd1 Cl1 82.6(4) . . ?
C4 Cd2 C6 88.5(9) . . ?
C4 Cd2 C5 86.0(9) . . ?
C6 Cd2 C5 89.4(9) . . ?
C4 Cd2 C19 100.6(8) . . ?
C6 Cd2 C19 96.5(7) . . ?
C5 Cd2 C19 171.3(8) . . ?
C4 Cd2 C17 97.9(7) . . ?
C6 Cd2 C17 172.7(8) . . ?
C5 Cd2 C17 87.4(7) . . ?
C19 Cd2 C17 86.0(6) . . ?
C4 Cd2 Cl2 165.6(7) . . ?
C6 Cd2 Cl2 91.2(6) . . ?
C5 Cd2 Cl2 108.4(7) . . ?
C19 Cd2 Cl2 65.1(4) . . ?
C17 Cd2 Cl2 83.6(4) . . ?
C8 Cd3 C7 87.7(10) . . ?
C8 Cd3 C9 88.5(11) . . ?
C7 Cd3 C9 90.3(10) . . ?
C8 Cd3 C25 169.8(8) . . ?
C7 Cd3 C25 102.5(8) . . ?
C9 Cd3 C25 92.4(9) . . ?
C8 Cd3 C23 92.1(8) . . ?
C7 Cd3 C23 94.3(7) . . ?
C9 Cd3 C23 175.3(9) . . ?
C25 Cd3 C23 86.1(6) . . ?
C8 Cd3 Cl3 104.7(7) . . ?
C7 Cd3 Cl3 167.4(7) . . ?
C9 Cd3 Cl3 91.8(8) . . ?
C25 Cd3 Cl3 65.1(4) . . ?
C23 Cd3 Cl3 83.6(4) . . ?
C10 Cd4 C11 90.2(10) . . ?
C10 Cd4 C12 88.0(10) . . ?
C11 Cd4 C12 87.5(10) . . ?
C10 Cd4 C31 102.8(8) . . ?
C11 Cd4 C31 166.9(8) . . ?
C12 Cd4 C31 91.0(8) . . ?
C10 Cd4 C29 97.5(8) . . ?
C11 Cd4 C29 93.8(8) . . ?
C12 Cd4 C29 174.4(8) . . ?
C31 Cd4 C29 86.4(6) . . ?
C10 Cd4 Cl4 168.2(7) . . ?
C11 Cd4 Cl4 101.4(7) . . ?
C12 Cd4 Cl4 90.4(7) . . ?
C31 Cd4 Cl4 65.6(4) . . ?
C29 Cd4 Cl4 84.0(4) . . ?
C18 Cl1 Cd1 80.7(6) . . ?
C24 Cl2 Cd2 80.7(8) . . ?
C30 Cl3 Cd3 81.1(7) . . ?
C36 Cl4 Cd4 80.0(7) . . ?
O1 C1 Cd1 174.6(17) . . ?
O2 C2 Cd1 178.7(19) . . ?
O3 C3 Cd1 175.3(18) . . ?
O4 C4 Cd2 174.5(18) . . ?
O5 C5 Cd2 178(2) . . ?
O6 C6 Cd2 175.6(19) . . ?
O7 C7 Cd3 173.1(19) . . ?
O8 C8 Cd3 176(2) . . ?
O9 C9 Cd3 176(2) . . ?
O10 C10 Cd4 174.7(19) . . ?
O11 C11 Cd4 178(2) . . ?
O12 C12 Cd4 173(2) . . ?
C14 C13 C18 117.9(17) . . ?
C14 C13 Cd1 138.6(15) . . ?
C18 C13 Cd1 103.4(12) . . ?
C13 C14 C15 122.1(19) . . ?
C16 C15 C14 114.8(18) . . ?
C17 C16 C15 125.9(18) . . ?
C16 C17 C18 117.2(17) . . ?
C16 C17 Cd2 118.0(13) . . ?
C18 C17 Cd2 124.6(12) . . ?
C17 C18 C13 121.8(17) . . ?
C17 C18 Cl1 128.2(14) . . ?
C13 C18 Cl1 110.0(13) . . ?
C20 C19 C24 118.4(16) . . ?
C20 C19 Cd2 138.7(13) . . ?
C24 C19 Cd2 102.9(12) . . ?
C19 C20 C21 122.8(18) . . ?
C20 C21 C22 117.6(18) . . ?
C23 C22 C21 120.9(19) . . ?
C24 C23 C22 117.0(18) . . ?
C24 C23 Cd3 126.3(14) . . ?
C22 C23 Cd3 116.5(13) . . ?
C23 C24 C19 122.9(18) . . ?
C23 C24 Cl2 125.6(17) . . ?
C19 C24 Cl2 111.3(14) . . ?
C26 C25 C30 119.6(17) . . ?
C26 C25 Cd3 137.3(14) . . ?
C30 C25 Cd3 103.0(12) . . ?
C25 C26 C27 121(2) . . ?
C28 C27 C26 117(2) . . ?
C29 C28 C27 122(2) . . ?
C30 C29 C28 118.8(18) . . ?
C30 C29 Cd4 124.4(13) . . ?
C28 C29 Cd4 116.8(13) . . ?
C29 C30 C25 121.9(18) . . ?
C29 C30 Cl3 127.4(16) . . ?
C25 C30 Cl3 110.6(14) . . ?
C32 C31 C36 121.4(17) . . ?
C32 C31 Cd4 138.0(13) . . ?
C36 C31 Cd4 100.4(13) . . ?
C31 C32 C33 120.7(18) . . ?
C34 C33 C32 117.2(19) . . ?
C35 C34 C33 122(2) . . ?
C34 C35 C36 118.4(17) . . ?
C34 C35 Cd1 118.7(13) . . ?
C36 C35 Cd1 122.9(13) . . ?
C31 C36 C35 119.5(18) . . ?
C31 C36 Cl4 114.0(15) . . ?
C35 C36 Cl4 126.5(15) . . ?
Cl6 C37 Cl5 71(2) . . ?
Cl6A C37A Cl5A 71(2) . . ?
Cl7 C38 Cl8 108.6(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C13 C14 C15 0(3) . . . . ?
Cd1 C13 C14 C15 179.0(15) . . . . ?
C13 C14 C15 C16 -3(3) . . . . ?
C14 C15 C16 C17 3(3) . . . . ?
C15 C16 C17 C18 1(3) . . . . ?
C15 C16 C17 Cd2 176.1(15) . . . . ?
C16 C17 C18 C13 -5(3) . . . . ?
Cd2 C17 C18 C13 -179.6(13) . . . . ?
C16 C17 C18 Cl1 175.8(15) . . . . ?
Cd2 C17 C18 Cl1 1(2) . . . . ?
C14 C13 C18 C17 5(3) . . . . ?
Cd1 C13 C18 C17 -175.0(15) . . . . ?
C14 C13 C18 Cl1 -176.0(14) . . . . ?
Cd1 C13 C18 Cl1 4.4(14) . . . . ?
Cd1 Cl1 C18 C17 175.7(18) . . . . ?
Cd1 Cl1 C18 C13 -3.7(12) . . . . ?
C24 C19 C20 C21 -1(3) . . . . ?
Cd2 C19 C20 C21 178.1(16) . . . . ?
C19 C20 C21 C22 3(3) . . . . ?
C20 C21 C22 C23 1(3) . . . . ?
C21 C22 C23 C24 -6(3) . . . . ?
C21 C22 C23 Cd3 178.9(15) . . . . ?
C22 C23 C24 C19 8(3) . . . . ?
Cd3 C23 C24 C19 -177.1(13) . . . . ?
C22 C23 C24 Cl2 -177.1(15) . . . . ?
Cd3 C23 C24 Cl2 -2(3) . . . . ?
C20 C19 C24 C23 -5(3) . . . . ?
Cd2 C19 C24 C23 175.9(16) . . . . ?
C20 C19 C24 Cl2 179.3(16) . . . . ?
Cd2 C19 C24 Cl2 0.3(15) . . . . ?
Cd2 Cl2 C24 C23 -175.7(18) . . . . ?
Cd2 Cl2 C24 C19 -0.2(13) . . . . ?
C30 C25 C26 C27 1(3) . . . . ?
Cd3 C25 C26 C27 -176.6(15) . . . . ?
C25 C26 C27 C28 -3(3) . . . . ?
C26 C27 C28 C29 2(3) . . . . ?
C27 C28 C29 C30 1(3) . . . . ?
C27 C28 C29 Cd4 -179.6(15) . . . . ?
C28 C29 C30 C25 -4(3) . . . . ?
Cd4 C29 C30 C25 176.7(13) . . . . ?
C28 C29 C30 Cl3 172.7(15) . . . . ?
Cd4 C29 C30 Cl3 -6(3) . . . . ?
C26 C25 C30 C29 3(3) . . . . ?
Cd3 C25 C30 C29 -178.6(16) . . . . ?
C26 C25 C30 Cl3 -174.1(15) . . . . ?
Cd3 C25 C30 Cl3 4.0(15) . . . . ?
Cd3 Cl3 C30 C29 179.4(19) . . . . ?
Cd3 Cl3 C30 C25 -3.4(13) . . . . ?
C36 C31 C32 C33 -1(3) . . . . ?
Cd4 C31 C32 C33 171.5(15) . . . . ?
C31 C32 C33 C34 6(3) . . . . ?
C32 C33 C34 C35 -7(3) . . . . ?
C33 C34 C35 C36 2(3) . . . . ?
C33 C34 C35 Cd1 -177.6(15) . . . . ?
C32 C31 C36 C35 -4(3) . . . . ?
Cd4 C31 C36 C35 -178.7(15) . . . . ?
C32 C31 C36 Cl4 177.7(15) . . . . ?
Cd4 C31 C36 Cl4 2.9(16) . . . . ?
C34 C35 C36 C31 3(3) . . . . ?
Cd1 C35 C36 C31 -177.1(13) . . . . ?
C34 C35 C36 Cl4 -178.4(16) . . . . ?
Cd1 C35 C36 Cl4 1(2) . . . . ?
Cd4 Cl4 C36 C31 -2.5(14) . . . . ?
Cd4 Cl4 C36 C35 179.2(19) . . . . ?

_refine_diff_density_max         2.296
_refine_diff_density_min         -2.400
_refine_diff_density_rms         0.311

