# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_cmpnd01
_database_code_depnum_ccdc_archive 'CCDC 1908893'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2019-04-09 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;

# Start Validation Reply Form

#_vrf_PLAT971_mxm313ps
_vrf_PLAT971_cmpnd01             
;
PROBLEM: Check Calcd Resid. Dens.  0.72A   From Re1             4.75 eA-3
          
RESPONSE: This could not be modelled as it is too close to the atom
          and no twinnig was observed.
;

# End Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C26 H20 N7 O4 Re), C3 H6 O'
_chemical_formula_sum            'C55 H46 N14 O9 Re2'
_chemical_formula_weight         1419.46

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'
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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.0338(1)
_cell_length_b                   11.1396(1)
_cell_length_c                   28.5974(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.845(1)
_cell_angle_gamma                90
_cell_volume                     2874.29(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23788
_cell_measurement_theta_min      2.801
_cell_measurement_theta_max      31.603
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016586
_diffrn_orient_matrix_UB_12      -0.0211529
_diffrn_orient_matrix_UB_13      -0.0234153
_diffrn_orient_matrix_UB_21      0.0775532
_diffrn_orient_matrix_UB_22      0.0094276
_diffrn_orient_matrix_UB_23      -0.0006054
_diffrn_orient_matrix_UB_31      0.0128463
_diffrn_orient_matrix_UB_32      -0.0592989
_diffrn_orient_matrix_UB_33      0.0082535

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    4.274
_shelx_estimated_absorpt_T_min   0.449
_shelx_estimated_absorpt_T_max   0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91827
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_reflns_number            58556
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.853
_diffrn_reflns_theta_max         31.899
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9501
_reflns_number_gt                8290
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2015/1 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0450P)²+18.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9501
_refine_ls_number_parameters     379
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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
Re1 Re 0.78247(2) 0.34940(2) 0.07989(2) 0.02447(6) Uani 1 1 d . . . . .
C101 C 0.5870(5) 0.3867(4) 0.09955(18) 0.0320(9) Uani 1 1 d . . . . .
O101 O 0.4703(4) 0.4042(4) 0.11280(16) 0.0464(10) Uani 1 1 d . . . . .
C102 C 0.8184(5) 0.5176(4) 0.07357(17) 0.0296(9) Uani 1 1 d . . . . .
O102 O 0.8434(5) 0.6191(3) 0.07077(15) 0.0424(9) Uani 1 1 d . . . . .
C103 C 0.8525(5) 0.3611(4) 0.14396(18) 0.0300(9) Uani 1 1 d . . . . .
O103 O 0.8934(5) 0.3694(4) 0.18299(14) 0.0439(9) Uani 1 1 d . . . . .
N11 N 0.7599(4) 0.1568(3) 0.08159(13) 0.0240(7) Uani 1 1 d . . . . .
C12 C 0.8832(5) 0.0931(4) 0.07084(15) 0.0249(8) Uani 1 1 d . . . . .
C13 C 0.8882(5) -0.0325(4) 0.07059(16) 0.0283(8) Uani 1 1 d . . . . .
C14 C 0.7563(5) -0.0938(4) 0.07930(17) 0.0320(9) Uani 1 1 d . U . . .
H14 H 0.754440 -0.179050 0.079156 0.038 Uiso 1 1 calc R U . . .
C15 C 0.6305(6) -0.0308(4) 0.08797(18) 0.0340(10) Uani 1 1 d . . . . .
H15 H 0.540028 -0.071621 0.092538 0.041 Uiso 1 1 calc R U . . .
C16 C 0.6373(5) 0.0945(4) 0.09001(17) 0.0296(9) Uani 1 1 d . . . . .
H16 H 0.551007 0.137371 0.097738 0.035 Uiso 1 1 calc R U . . .
C17 C 1.0242(6) -0.0910(4) 0.06034(18) 0.0339(10) Uani 1 1 d . . . . .
H17 H 1.029776 -0.176143 0.061182 0.041 Uiso 1 1 calc R U . . .
N21 N 0.9927(4) 0.2837(3) 0.05669(13) 0.0244(7) Uani 1 1 d . . . . .
C22 C 1.0095(5) 0.1615(4) 0.05820(15) 0.0245(8) Uani 1 1 d . . . . .
C23 C 1.1408(5) 0.1023(4) 0.04717(16) 0.0276(8) Uani 1 1 d . . . . .
C24 C 1.2591(5) 0.1744(5) 0.03363(17) 0.0320(9) Uani 1 1 d . . . . .
H24 H 1.350470 0.138816 0.026133 0.038 Uiso 1 1 calc R U . . .
C25 C 1.2413(5) 0.2962(5) 0.03136(17) 0.0334(10) Uani 1 1 d . . . . .
H25 H 1.320253 0.345539 0.021880 0.040 Uiso 1 1 calc R U . . .
C26 C 1.1070(5) 0.3484(4) 0.04298(16) 0.0284(8) Uani 1 1 d . . . . .
H26 H 1.096906 0.433118 0.041014 0.034 Uiso 1 1 calc R U . . .
C27 C 1.1453(6) -0.0262(4) 0.04944(18) 0.0349(10) Uani 1 1 d . . . . .
H27 H 1.234661 -0.066855 0.043210 0.042 Uiso 1 1 calc R U . . .
N31 N 0.7661(4) 0.3639(3) -0.03135(14) 0.0281(7) Uani 1 1 d . . . . .
N32 N 0.7033(4) 0.3257(3) 0.00751(14) 0.0256(7) Uani 1 1 d . . . . .
N33 N 0.5790(4) 0.2662(4) -0.00284(15) 0.0327(8) Uani 1 1 d . . . . .
N34 N 0.5569(4) 0.2644(4) -0.04918(15) 0.0345(8) Uani 1 1 d . . . . .
C35 C 0.6721(5) 0.3240(4) -0.06595(17) 0.0271(8) Uani 1 1 d . . . . .
C41 C 0.6918(5) 0.3400(4) -0.11620(17) 0.0310(9) Uani 1 1 d . . . . .
C42 C 0.8120(6) 0.4006(6) -0.13251(19) 0.0417(12) Uani 1 1 d . . . . .
H42 H 0.883911 0.433099 -0.110678 0.050 Uiso 1 1 calc R U . . .
C43 C 0.8304(7) 0.4153(6) -0.1802(2) 0.0486(14) Uani 1 1 d . . . . .
H43 H 0.914774 0.456941 -0.190323 0.058 Uiso 1 1 calc R U . . .
C44 C 0.7270(6) 0.3700(5) -0.21313(19) 0.0395(11) Uani 1 1 d . . . . .
C45 C 0.6015(6) 0.3125(6) -0.1961(2) 0.0431(12) Uani 1 1 d . . . . .
H45 H 0.526820 0.282787 -0.217666 0.052 Uiso 1 1 calc R U . . .
C46 C 0.5855(6) 0.2988(5) -0.14907(19) 0.0399(11) Uani 1 1 d . . . . .
H46 H 0.499429 0.259990 -0.138645 0.048 Uiso 1 1 calc R U . . .
N61 N 0.7383(6) 0.3875(5) -0.26177(17) 0.0465(12) Uani 1 1 d . . . . .
C62 C 0.7270(8) 0.2779(6) -0.2898(2) 0.0501(14) Uani 1 1 d . . . . .
H62A H 0.637824 0.232368 -0.281641 0.060 Uiso 1 1 calc R U . . .
H62B H 0.814877 0.226821 -0.282696 0.060 Uiso 1 1 calc R U . . .
C63 C 0.7173(8) 0.3070(7) -0.3411(2) 0.0540(16) Uani 1 1 d . . . . .
H63A H 0.715367 0.231405 -0.359287 0.065 Uiso 1 1 calc R U . . .
H63B H 0.623605 0.350484 -0.348703 0.065 Uiso 1 1 calc R U . . .
O64 O 0.8377(5) 0.3779(5) -0.35420(16) 0.0594(12) Uani 1 1 d . . . . .
C65 C 0.8442(10) 0.4838(7) -0.3275(2) 0.065(2) Uani 1 1 d . . . . .
H65A H 0.753185 0.531300 -0.334474 0.078 Uiso 1 1 calc R U . . .
H65B H 0.929854 0.532314 -0.336623 0.078 Uiso 1 1 calc R U . . .
C66 C 0.8591(7) 0.4588(6) -0.2747(2) 0.0499(14) Uani 1 1 d . . . . .
H66A H 0.953402 0.416347 -0.266957 0.060 Uiso 1 1 calc R U . . .
H66B H 0.860004 0.535504 -0.257202 0.060 Uiso 1 1 calc R U . . .
O1 O 0.3168(10) 0.1210(9) -0.2016(3) 0.051(2) Uani 0.5 1 d . . P . .
C1 C 0.2098(12) 0.0698(14) -0.2159(4) 0.053(3) Uani 0.5 1 d . . P . .
C2 C 0.082(2) 0.1151(19) -0.2416(7) 0.086(5) Uani 0.5 1 d . U P . .
H2A H 0.011782 0.049282 -0.248409 0.129 Uiso 0.5 1 calc R U P . .
H2B H 0.033725 0.176454 -0.222970 0.129 Uiso 0.5 1 calc R U P . .
H2C H 0.111284 0.150661 -0.271068 0.129 Uiso 0.5 1 calc R U P . .
C3 C 0.1963(16) -0.0632(15) -0.2116(5) 0.065(4) Uani 0.5 1 d . . P . .
H3A H 0.100246 -0.089169 -0.225476 0.097 Uiso 0.5 1 calc R U P . .
H3B H 0.276100 -0.102008 -0.228033 0.097 Uiso 0.5 1 calc R U P . .
H3C H 0.203852 -0.085799 -0.178450 0.097 Uiso 0.5 1 calc R U 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
Re1 C102 1.912(4) . ?
Re1 C103 1.913(5) . ?
Re1 C101 1.925(5) . ?
Re1 N11 2.155(3) . ?
Re1 N21 2.170(4) . ?
Re1 N32 2.172(4) . ?
C101 O101 1.154(6) . ?
C102 O102 1.156(5) . ?
C103 O103 1.162(6) . ?
N11 C16 1.339(5) . ?
N11 C12 1.369(5) . ?
C12 C13 1.400(6) . ?
C12 C22 1.434(6) . ?
C13 C14 1.407(6) . ?
C13 C17 1.433(6) . ?
C14 C15 1.368(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C27 1.360(7) . ?
C17 H17 0.9500 . ?
N21 C26 1.334(5) . ?
N21 C22 1.370(5) . ?
C22 C23 1.407(6) . ?
C23 C24 1.406(6) . ?
C23 C27 1.433(7) . ?
C24 C25 1.368(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.400(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
N31 N32 1.342(5) . ?
N31 C35 1.347(6) . ?
N32 N33 1.324(5) . ?
N33 N34 1.330(6) . ?
N34 C35 1.343(6) . ?
C35 C41 1.468(7) . ?
C41 C42 1.380(7) . ?
C41 C46 1.388(7) . ?
C42 C43 1.391(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.388(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.410(7) . ?
C44 N61 1.413(7) . ?
C45 C46 1.369(8) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
N61 C66 1.414(7) . ?
N61 C62 1.462(8) . ?
C62 C63 1.499(8) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 O64 1.410(8) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
O64 C65 1.405(9) . ?
C65 C66 1.534(9) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
O1 C1 1.179(14) . ?
C1 C2 1.43(2) . ?
C1 C3 1.49(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?

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
C102 Re1 C103 88.5(2) . . ?
C102 Re1 C101 88.8(2) . . ?
C103 Re1 C101 88.3(2) . . ?
C102 Re1 N11 173.80(17) . . ?
C103 Re1 N11 94.20(16) . . ?
C101 Re1 N11 96.86(17) . . ?
C102 Re1 N21 98.39(17) . . ?
C103 Re1 N21 93.60(17) . . ?
C101 Re1 N21 172.63(16) . . ?
N11 Re1 N21 75.91(13) . . ?
C102 Re1 N32 94.51(17) . . ?
C103 Re1 N32 176.90(16) . . ?
C101 Re1 N32 92.36(18) . . ?
N11 Re1 N32 82.72(13) . . ?
N21 Re1 N32 85.37(13) . . ?
O101 C101 Re1 176.6(5) . . ?
O102 C102 Re1 178.0(5) . . ?
O103 C103 Re1 179.0(4) . . ?
C16 N11 C12 117.4(4) . . ?
C16 N11 Re1 126.9(3) . . ?
C12 N11 Re1 115.6(3) . . ?
N11 C12 C13 123.2(4) . . ?
N11 C12 C22 116.6(4) . . ?
C13 C12 C22 120.2(4) . . ?
C12 C13 C14 117.1(4) . . ?
C12 C13 C17 118.9(4) . . ?
C14 C13 C17 123.9(4) . . ?
C15 C14 C13 120.1(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 119.0(4) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
N11 C16 C15 123.0(4) . . ?
N11 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C27 C17 C13 120.8(4) . . ?
C27 C17 H17 119.6 . . ?
C13 C17 H17 119.6 . . ?
C26 N21 C22 117.4(4) . . ?
C26 N21 Re1 127.6(3) . . ?
C22 N21 Re1 115.0(3) . . ?
N21 C22 C23 123.5(4) . . ?
N21 C22 C12 116.6(4) . . ?
C23 C22 C12 119.8(4) . . ?
C24 C23 C22 117.0(4) . . ?
C24 C23 C27 124.2(4) . . ?
C22 C23 C27 118.7(4) . . ?
C25 C24 C23 119.4(4) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
N21 C26 C25 122.6(4) . . ?
N21 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C17 C27 C23 121.3(4) . . ?
C17 C27 H27 119.4 . . ?
C23 C27 H27 119.4 . . ?
N32 N31 C35 103.1(4) . . ?
N33 N32 N31 111.3(4) . . ?
N33 N32 Re1 120.6(3) . . ?
N31 N32 Re1 128.1(3) . . ?
N32 N33 N34 108.3(4) . . ?
N33 N34 C35 105.5(4) . . ?
N34 C35 N31 111.9(4) . . ?
N34 C35 C41 122.9(4) . . ?
N31 C35 C41 125.2(4) . . ?
C42 C41 C46 117.6(5) . . ?
C42 C41 C35 121.7(4) . . ?
C46 C41 C35 120.6(4) . . ?
C41 C42 C43 121.5(5) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C44 C43 C42 120.9(5) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 117.2(5) . . ?
C43 C44 N61 122.6(5) . . ?
C45 C44 N61 120.0(5) . . ?
C46 C45 C44 121.0(5) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C45 C46 C41 121.7(5) . . ?
C45 C46 H46 119.2 . . ?
C41 C46 H46 119.2 . . ?
C44 N61 C66 115.4(5) . . ?
C44 N61 C62 114.8(5) . . ?
C66 N61 C62 111.0(5) . . ?
N61 C62 C63 110.8(6) . . ?
N61 C62 H62A 109.5 . . ?
C63 C62 H62A 109.5 . . ?
N61 C62 H62B 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 108.1 . . ?
O64 C63 C62 111.9(5) . . ?
O64 C63 H63A 109.2 . . ?
C62 C63 H63A 109.2 . . ?
O64 C63 H63B 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C65 O64 C63 109.7(5) . . ?
O64 C65 C66 112.5(6) . . ?
O64 C65 H65A 109.1 . . ?
C66 C65 H65A 109.1 . . ?
O64 C65 H65B 109.1 . . ?
C66 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
N61 C66 C65 109.2(5) . . ?
N61 C66 H66A 109.8 . . ?
C65 C66 H66A 109.8 . . ?
N61 C66 H66B 109.8 . . ?
C65 C66 H66B 109.8 . . ?
H66A C66 H66B 108.3 . . ?
O1 C1 C2 129.6(15) . . ?
O1 C1 C3 121.3(12) . . ?
C2 C1 C3 109.0(13) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

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 N11 C12 C13 -3.2(7) . . . . ?
Re1 N11 C12 C13 179.5(4) . . . . ?
C16 N11 C12 C22 175.1(4) . . . . ?
Re1 N11 C12 C22 -2.2(5) . . . . ?
N11 C12 C13 C14 3.7(7) . . . . ?
C22 C12 C13 C14 -174.5(4) . . . . ?
N11 C12 C13 C17 -178.0(4) . . . . ?
C22 C12 C13 C17 3.8(7) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
C17 C13 C14 C15 -178.8(5) . . . . ?
C13 C14 C15 C16 -2.7(8) . . . . ?
C12 N11 C16 C15 -0.4(7) . . . . ?
Re1 N11 C16 C15 176.5(4) . . . . ?
C14 C15 C16 N11 3.4(8) . . . . ?
C12 C13 C17 C27 -2.2(7) . . . . ?
C14 C13 C17 C27 175.9(5) . . . . ?
C26 N21 C22 C23 1.5(7) . . . . ?
Re1 N21 C22 C23 -176.2(3) . . . . ?
C26 N21 C22 C12 -177.1(4) . . . . ?
Re1 N21 C22 C12 5.2(5) . . . . ?
N11 C12 C22 N21 -2.0(6) . . . . ?
C13 C12 C22 N21 176.3(4) . . . . ?
N11 C12 C22 C23 179.3(4) . . . . ?
C13 C12 C22 C23 -2.3(7) . . . . ?
N21 C22 C23 C24 -0.5(7) . . . . ?
C12 C22 C23 C24 178.0(4) . . . . ?
N21 C22 C23 C27 -179.3(4) . . . . ?
C12 C22 C23 C27 -0.8(7) . . . . ?
C22 C23 C24 C25 -0.6(7) . . . . ?
C27 C23 C24 C25 178.1(5) . . . . ?
C23 C24 C25 C26 0.8(8) . . . . ?
C22 N21 C26 C25 -1.4(7) . . . . ?
Re1 N21 C26 C25 176.0(3) . . . . ?
C24 C25 C26 N21 0.3(8) . . . . ?
C13 C17 C27 C23 -0.9(8) . . . . ?
C24 C23 C27 C17 -176.3(5) . . . . ?
C22 C23 C27 C17 2.4(7) . . . . ?
C35 N31 N32 N33 0.0(5) . . . . ?
C35 N31 N32 Re1 179.4(3) . . . . ?
N31 N32 N33 N34 -0.2(5) . . . . ?
Re1 N32 N33 N34 -179.7(3) . . . . ?
N32 N33 N34 C35 0.3(5) . . . . ?
N33 N34 C35 N31 -0.3(5) . . . . ?
N33 N34 C35 C41 178.5(4) . . . . ?
N32 N31 C35 N34 0.2(5) . . . . ?
N32 N31 C35 C41 -178.6(4) . . . . ?
N34 C35 C41 C42 -179.3(5) . . . . ?
N31 C35 C41 C42 -0.7(7) . . . . ?
N34 C35 C41 C46 3.5(7) . . . . ?
N31 C35 C41 C46 -177.8(5) . . . . ?
C46 C41 C42 C43 -3.0(9) . . . . ?
C35 C41 C42 C43 179.8(6) . . . . ?
C41 C42 C43 C44 0.5(10) . . . . ?
C42 C43 C44 C45 2.0(10) . . . . ?
C42 C43 C44 N61 177.2(6) . . . . ?
C43 C44 C45 C46 -2.1(10) . . . . ?
N61 C44 C45 C46 -177.4(6) . . . . ?
C44 C45 C46 C41 -0.3(10) . . . . ?
C42 C41 C46 C45 2.9(9) . . . . ?
C35 C41 C46 C45 -179.9(5) . . . . ?
C43 C44 N61 C66 -2.6(9) . . . . ?
C45 C44 N61 C66 172.5(6) . . . . ?
C43 C44 N61 C62 128.6(7) . . . . ?
C45 C44 N61 C62 -56.4(8) . . . . ?
C44 N61 C62 C63 171.5(5) . . . . ?
C66 N61 C62 C63 -55.3(7) . . . . ?
N61 C62 C63 O64 55.8(8) . . . . ?
C62 C63 O64 C65 -57.1(8) . . . . ?
C63 O64 C65 C66 58.0(8) . . . . ?
C44 N61 C66 C65 -172.3(6) . . . . ?
C62 N61 C66 C65 54.9(8) . . . . ?
O64 C65 C66 N61 -57.7(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15 N34 0.95 2.61 3.268(6) 126.8 3_655 yes
C16 H16 O64 0.95 2.43 3.225(6) 141.3 4_566 yes
C25 H25 N33 0.95 2.63 3.266(6) 124.9 1_655 yes
C26 H26 N31 0.95 2.60 3.425(6) 145.7 3_765 yes
C43 H43 O103 0.95 2.60 3.465(7) 151.7 3_765 yes
C62 H62A O103 0.99 2.64 3.485(8) 143.6 4_565 yes
C65 H65B O1 0.99 2.68 3.486(13) 139.3 2_654 yes

_refine_diff_density_max         4.842
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.164

####################################################################### 
# 
# 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_cmpnd03
_database_code_depnum_ccdc_archive 'CCDC 1908895'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2019-04-09 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;

# Start Validation Reply Form

#_vrf_PLAT973_mxm340ps
_vrf_PLAT973_cmpnd03             
;
PROBLEM: Check Calcd Positive Resid. Density on       Re1       2.02 eA-3 

RESPONSE: This could not be modelled as it is too close to the atom
          and no twinnig was observed.
;

# End Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H25 N8 O5 Re, C H2 Cl2 [+ solvent]'
_chemical_formula_sum            'C30 H27 Cl2 N8 O5 Re'
_chemical_formula_weight         836.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.0763(3)
_cell_length_b                   11.6224(3)
_cell_length_c                   13.4832(4)
_cell_angle_alpha                100.225(2)
_cell_angle_beta                 106.812(2)
_cell_angle_gamma                95.543(2)
_cell_volume                     1614.87(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14830
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      31.016
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0266163
_diffrn_orient_matrix_UB_12      0.0340119
_diffrn_orient_matrix_UB_13      -0.0295390
_diffrn_orient_matrix_UB_21      -0.0608839
_diffrn_orient_matrix_UB_22      0.0148421
_diffrn_orient_matrix_UB_23      -0.0234766
_diffrn_orient_matrix_UB_31      0.0131539
_diffrn_orient_matrix_UB_32      0.0506537
_diffrn_orient_matrix_UB_33      0.0417568

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.147
_exptl_absorpt_coefficient_mu    3.980
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81372
_exptl_absorpt_correction_T_max  1.0
__exptl_absorpt_process_details  
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            35882
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_av_R_equivalents  0.0441
_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       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         32.692
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11025
_reflns_number_gt                8441
_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.

 Residual electron density in the crystal which could not be interpreted
 as chemically reasonable moieties was effectively removed by use
 of the program SQUEEZE.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2015/1 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015)'
_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)+(0.0535P)²+2.6000P] 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         11025
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.80950(2) 0.22681(2) 0.97324(2) 0.03594(7) Uani 1 1 d . . . . .
O101 O 1.0920(3) 0.2897(4) 0.9932(3) 0.0557(10) Uani 1 1 d . . . . .
C101 C 0.9846(5) 0.2655(5) 0.9829(4) 0.0423(10) Uani 1 1 d . . . . .
O102 O 0.7946(4) -0.0150(4) 0.8299(4) 0.0672(12) Uani 1 1 d . . . . .
C102 C 0.7999(5) 0.0773(5) 0.8808(5) 0.0476(12) Uani 1 1 d . . . . .
O103 O 0.9010(4) 0.1134(4) 1.1647(4) 0.0688(12) Uani 1 1 d . . . . .
C103 C 0.8657(4) 0.1560(5) 1.0931(4) 0.0462(11) Uani 1 1 d . . . . .
N11 N 0.7943(4) 0.3915(4) 1.0696(3) 0.0371(8) Uani 1 1 d . . . . .
C12 C 0.6762(4) 0.3988(4) 1.0811(4) 0.0375(9) Uani 1 1 d . . . . .
C13 C 0.6491(5) 0.4989(5) 1.1424(4) 0.0440(11) Uani 1 1 d . . . . .
C14 C 0.7496(6) 0.5919(5) 1.1943(4) 0.0537(13) Uani 1 1 d . . . . .
H14 H 0.736465 0.660386 1.237658 0.064 Uiso 1 1 calc R U . . .
C15 C 0.8675(6) 0.5837(5) 1.1823(4) 0.0552(13) Uani 1 1 d . . . . .
H15 H 0.936269 0.646840 1.217178 0.066 Uiso 1 1 calc R U . . .
C16 C 0.8867(5) 0.4831(5) 1.1191(4) 0.0480(12) Uani 1 1 d . . . . .
H16 H 0.968830 0.479810 1.110983 0.058 Uiso 1 1 calc R U . . .
C17 C 0.5219(5) 0.4983(5) 1.1470(4) 0.0503(12) Uani 1 1 d . . . . .
H17 H 0.502544 0.564994 1.188148 0.060 Uiso 1 1 calc R U . . .
N21 N 0.6116(3) 0.2055(3) 0.9711(3) 0.0338(7) Uani 1 1 d . . . . .
C22 C 0.5789(4) 0.3004(4) 1.0286(4) 0.0385(10) Uani 1 1 d . . . . .
C23 C 0.4537(4) 0.3027(4) 1.0346(4) 0.0397(10) Uani 1 1 d . . . . .
C24 C 0.3622(4) 0.2014(5) 0.9801(4) 0.0448(11) Uani 1 1 d . . . . .
H24 H 0.277187 0.198637 0.982565 0.054 Uiso 1 1 calc R U . . .
C25 C 0.3957(4) 0.1077(5) 0.9240(4) 0.0446(11) Uani 1 1 d . . . . .
H25 H 0.334344 0.039066 0.887627 0.053 Uiso 1 1 calc R U . . .
C26 C 0.5214(4) 0.1125(4) 0.9199(4) 0.0385(10) Uani 1 1 d . . . . .
H26 H 0.542733 0.046893 0.879039 0.046 Uiso 1 1 calc R U . . .
C27 C 0.4292(5) 0.4065(5) 1.0951(4) 0.0486(12) Uani 1 1 d . . . . .
H27 H 0.345188 0.410556 1.098592 0.058 Uiso 1 1 calc R U . . .
N31 N 0.6150(4) 0.3249(4) 0.6892(3) 0.0404(8) Uani 1 1 d . . . . .
N32 N 0.6330(4) 0.2603(4) 0.7633(3) 0.0412(9) Uani 1 1 d . . . . .
N33 N 0.7374(3) 0.3106(3) 0.8410(3) 0.0365(8) Uani 1 1 d . . . . .
N34 N 0.7914(3) 0.4091(3) 0.8212(3) 0.0353(8) Uani 1 1 d . . . . .
C35 C 0.7130(4) 0.4151(4) 0.7266(3) 0.0340(8) Uani 1 1 d . . . . .
C41 C 0.7294(4) 0.5080(4) 0.6688(3) 0.0362(9) Uani 1 1 d . . . . .
C42 C 0.6642(5) 0.4858(4) 0.5594(4) 0.0449(11) Uani 1 1 d . . . . .
H42 H 0.613821 0.410711 0.524341 0.054 Uiso 1 1 calc R U . . .
C43 C 0.6728(5) 0.5719(4) 0.5028(4) 0.0439(11) Uani 1 1 d . . . . .
H43 H 0.625949 0.556777 0.429401 0.053 Uiso 1 1 calc R U . . .
C44 C 0.7491(5) 0.6805(4) 0.5518(4) 0.0387(9) Uani 1 1 d . . . . .
C45 C 0.8186(5) 0.7013(4) 0.6598(4) 0.0423(10) Uani 1 1 d . . . . .
H45 H 0.873688 0.774381 0.693512 0.051 Uiso 1 1 calc R U . . .
C46 C 0.8073(5) 0.6155(4) 0.7178(4) 0.0416(10) Uani 1 1 d . . . . .
H46 H 0.853312 0.630752 0.791321 0.050 Uiso 1 1 calc R U . . .
O47 O 0.8642(3) 0.8446(3) 0.5186(3) 0.0510(9) Uani 1 1 d . . . . .
C47 C 0.7629(5) 0.7774(4) 0.4939(4) 0.0401(10) Uani 1 1 d . . . . .
N48 N 0.6590(4) 0.7837(3) 0.4148(3) 0.0394(8) Uani 1 1 d . . . . .
H48 H 0.590122 0.730746 0.398959 0.047 Uiso 1 1 calc R U . . .
C49 C 0.6577(5) 0.8767(4) 0.3542(4) 0.0410(10) Uani 1 1 d . . . . .
H49A H 0.610920 0.842894 0.278384 0.049 Uiso 1 1 calc R U . . .
H49B H 0.746361 0.908166 0.360134 0.049 Uiso 1 1 calc R U . . .
C50 C 0.5941(5) 0.9768(4) 0.3951(4) 0.0435(11) Uani 1 1 d . . . . .
H50A H 0.507939 0.944001 0.394519 0.052 Uiso 1 1 calc R U . . .
H50B H 0.644674 1.014188 0.469407 0.052 Uiso 1 1 calc R U . . .
N51 N 0.5828(4) 1.0669(4) 0.3308(3) 0.0440(9) Uani 1 1 d . . . . .
C52 C 0.7086(6) 1.1329(5) 0.3429(5) 0.0527(13) Uani 1 1 d . . . . .
H52A H 0.763111 1.077536 0.320720 0.063 Uiso 1 1 calc R U . . .
H52B H 0.751119 1.172004 0.418365 0.063 Uiso 1 1 calc R U . . .
C53 C 0.6920(6) 1.2248(5) 0.2757(5) 0.0561(14) Uani 1 1 d . . . . .
H53A H 0.776527 1.270215 0.285620 0.067 Uiso 1 1 calc R U . . .
H53B H 0.655002 1.184863 0.199975 0.067 Uiso 1 1 calc R U . . .
O54 O 0.6098(5) 1.3050(3) 0.3036(3) 0.0598(10) Uani 1 1 d . . . . .
C55 C 0.4896(6) 1.2421(5) 0.2952(4) 0.0536(13) Uani 1 1 d . . . . .
H55A H 0.445353 1.202793 0.220123 0.064 Uiso 1 1 calc R U . . .
H55B H 0.436393 1.298860 0.317661 0.064 Uiso 1 1 calc R U . . .
C56 C 0.5022(6) 1.1502(4) 0.3623(4) 0.0480(12) Uani 1 1 d . . . . .
H56A H 0.540981 1.189267 0.438182 0.058 Uiso 1 1 calc R U . . .
H56B H 0.416742 1.106946 0.352734 0.058 Uiso 1 1 calc R U . . .
C1 C 0.9589(7) 1.1083(7) 0.6253(6) 0.081(2) Uani 1 1 d . . . . .
H1A H 0.924783 1.026109 0.584565 0.097 Uiso 1 1 calc R U . . .
H1B H 1.001314 1.149956 0.583448 0.097 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0690(2) 1.1063(2) 0.7458(2) 0.1035(8) Uani 1 1 d . . . . .
Cl2 Cl 0.83438(19) 1.1794(2) 0.64550(15) 0.0890(6) 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 C101 1.909(5) . ?
Re1 C103 1.915(5) . ?
Re1 C102 1.924(6) . ?
Re1 N11 2.164(4) . ?
Re1 N33 2.170(4) . ?
Re1 N21 2.174(4) . ?
O101 C101 1.157(6) . ?
O102 C102 1.152(7) . ?
O103 C103 1.148(6) . ?
N11 C16 1.331(6) . ?
N11 C12 1.370(6) . ?
C12 C13 1.414(7) . ?
C12 C22 1.416(6) . ?
C13 C14 1.395(8) . ?
C13 C17 1.427(7) . ?
C14 C15 1.373(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C27 1.338(8) . ?
C17 H17 0.9500 . ?
N21 C26 1.331(6) . ?
N21 C22 1.372(6) . ?
C22 C23 1.415(6) . ?
C23 C24 1.408(7) . ?
C23 C27 1.428(7) . ?
C24 C25 1.357(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
N31 N32 1.335(5) . ?
N31 C35 1.344(6) . ?
N32 N33 1.314(5) . ?
N33 N34 1.344(5) . ?
N34 C35 1.337(5) . ?
C35 C41 1.467(6) . ?
C41 C46 1.383(7) . ?
C41 C42 1.406(6) . ?
C42 C43 1.374(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.400(6) . ?
C44 C47 1.499(6) . ?
C45 C46 1.390(6) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
O47 C47 1.226(6) . ?
C47 N48 1.342(6) . ?
N48 C49 1.465(5) . ?
N48 H48 0.8800 . ?
C49 C50 1.519(7) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 N51 1.467(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
N51 C56 1.468(7) . ?
N51 C52 1.474(7) . ?
C52 C53 1.511(7) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 O54 1.441(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
O54 C55 1.420(8) . ?
C55 C56 1.509(7) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C1 Cl1 1.732(9) . ?
C1 Cl2 1.737(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 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
C101 Re1 C103 87.91(19) . . ?
C101 Re1 C102 89.7(2) . . ?
C103 Re1 C102 89.4(2) . . ?
C101 Re1 N11 97.19(19) . . ?
C103 Re1 N11 93.1(2) . . ?
C102 Re1 N11 172.78(17) . . ?
C101 Re1 N33 94.72(17) . . ?
C103 Re1 N33 176.71(17) . . ?
C102 Re1 N33 92.58(19) . . ?
N11 Re1 N33 84.62(14) . . ?
C101 Re1 N21 172.94(18) . . ?
C103 Re1 N21 93.71(16) . . ?
C102 Re1 N21 97.23(18) . . ?
N11 Re1 N21 75.86(14) . . ?
N33 Re1 N21 83.45(13) . . ?
O101 C101 Re1 177.2(4) . . ?
O102 C102 Re1 176.5(5) . . ?
O103 C103 Re1 179.0(4) . . ?
C16 N11 C12 117.8(4) . . ?
C16 N11 Re1 127.1(3) . . ?
C12 N11 Re1 115.0(3) . . ?
N11 C12 C13 122.9(4) . . ?
N11 C12 C22 117.3(4) . . ?
C13 C12 C22 119.7(4) . . ?
C14 C13 C12 117.1(5) . . ?
C14 C13 C17 124.6(5) . . ?
C12 C13 C17 118.3(5) . . ?
C15 C14 C13 119.5(5) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.2(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
N11 C16 C15 122.4(5) . . ?
N11 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C27 C17 C13 121.9(5) . . ?
C27 C17 H17 119.0 . . ?
C13 C17 H17 119.0 . . ?
C26 N21 C22 118.1(4) . . ?
C26 N21 Re1 127.0(3) . . ?
C22 N21 Re1 114.8(3) . . ?
N21 C22 C23 122.5(4) . . ?
N21 C22 C12 117.0(4) . . ?
C23 C22 C12 120.6(5) . . ?
C24 C23 C22 117.1(4) . . ?
C24 C23 C27 124.8(4) . . ?
C22 C23 C27 118.0(5) . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 119.8(5) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
N21 C26 C25 122.5(5) . . ?
N21 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C17 C27 C23 121.4(5) . . ?
C17 C27 H27 119.3 . . ?
C23 C27 H27 119.3 . . ?
N32 N31 C35 105.1(4) . . ?
N33 N32 N31 108.4(4) . . ?
N32 N33 N34 111.4(3) . . ?
N32 N33 Re1 120.4(3) . . ?
N34 N33 Re1 128.1(3) . . ?
C35 N34 N33 103.1(4) . . ?
N34 C35 N31 112.0(4) . . ?
N34 C35 C41 125.1(4) . . ?
N31 C35 C41 122.9(4) . . ?
C46 C41 C42 119.2(4) . . ?
C46 C41 C35 122.3(4) . . ?
C42 C41 C35 118.5(4) . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 120.6(4) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C43 C44 C45 119.2(4) . . ?
C43 C44 C47 122.9(4) . . ?
C45 C44 C47 117.9(4) . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C41 C46 C45 120.2(4) . . ?
C41 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
O47 C47 N48 123.6(4) . . ?
O47 C47 C44 120.7(4) . . ?
N48 C47 C44 115.8(4) . . ?
C47 N48 C49 121.5(4) . . ?
C47 N48 H48 119.3 . . ?
C49 N48 H48 119.3 . . ?
N48 C49 C50 110.8(4) . . ?
N48 C49 H49A 109.5 . . ?
C50 C49 H49A 109.5 . . ?
N48 C49 H49B 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
N51 C50 C49 112.0(4) . . ?
N51 C50 H50A 109.2 . . ?
C49 C50 H50A 109.2 . . ?
N51 C50 H50B 109.2 . . ?
C49 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
C50 N51 C56 109.5(4) . . ?
C50 N51 C52 111.7(4) . . ?
C56 N51 C52 109.2(4) . . ?
N51 C52 C53 109.7(5) . . ?
N51 C52 H52A 109.7 . . ?
C53 C52 H52A 109.7 . . ?
N51 C52 H52B 109.7 . . ?
C53 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
O54 C53 C52 111.4(5) . . ?
O54 C53 H53A 109.4 . . ?
C52 C53 H53A 109.4 . . ?
O54 C53 H53B 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C55 O54 C53 110.8(4) . . ?
O54 C55 C56 112.3(5) . . ?
O54 C55 H55A 109.1 . . ?
C56 C55 H55A 109.1 . . ?
O54 C55 H55B 109.1 . . ?
C56 C55 H55B 109.1 . . ?
H55A C55 H55B 107.9 . . ?
N51 C56 C55 109.5(4) . . ?
N51 C56 H56A 109.8 . . ?
C55 C56 H56A 109.8 . . ?
N51 C56 H56B 109.8 . . ?
C55 C56 H56B 109.8 . . ?
H56A C56 H56B 108.2 . . ?
Cl1 C1 Cl2 110.3(4) . . ?
Cl1 C1 H1A 109.6 . . ?
Cl2 C1 H1A 109.6 . . ?
Cl1 C1 H1B 109.6 . . ?
Cl2 C1 H1B 109.6 . . ?
H1A C1 H1B 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 N11 C12 C13 0.2(6) . . . . ?
Re1 N11 C12 C13 179.0(3) . . . . ?
C16 N11 C12 C22 -179.6(4) . . . . ?
Re1 N11 C12 C22 -0.8(5) . . . . ?
N11 C12 C13 C14 -1.3(7) . . . . ?
C22 C12 C13 C14 178.5(4) . . . . ?
N11 C12 C13 C17 178.6(4) . . . . ?
C22 C12 C13 C17 -1.6(6) . . . . ?
C12 C13 C14 C15 1.3(8) . . . . ?
C17 C13 C14 C15 -178.6(5) . . . . ?
C13 C14 C15 C16 -0.2(9) . . . . ?
C12 N11 C16 C15 0.9(7) . . . . ?
Re1 N11 C16 C15 -177.7(4) . . . . ?
C14 C15 C16 N11 -0.9(8) . . . . ?
C14 C13 C17 C27 179.7(5) . . . . ?
C12 C13 C17 C27 -0.1(7) . . . . ?
C26 N21 C22 C23 -0.3(6) . . . . ?
Re1 N21 C22 C23 179.0(3) . . . . ?
C26 N21 C22 C12 -179.2(4) . . . . ?
Re1 N21 C22 C12 0.1(5) . . . . ?
N11 C12 C22 N21 0.5(6) . . . . ?
C13 C12 C22 N21 -179.4(4) . . . . ?
N11 C12 C22 C23 -178.4(4) . . . . ?
C13 C12 C22 C23 1.7(6) . . . . ?
N21 C22 C23 C24 1.1(6) . . . . ?
C12 C22 C23 C24 180.0(4) . . . . ?
N21 C22 C23 C27 -179.0(4) . . . . ?
C12 C22 C23 C27 -0.2(6) . . . . ?
C22 C23 C24 C25 -0.7(7) . . . . ?
C27 C23 C24 C25 179.4(4) . . . . ?
C23 C24 C25 C26 -0.5(7) . . . . ?
C22 N21 C26 C25 -1.0(6) . . . . ?
Re1 N21 C26 C25 179.9(3) . . . . ?
C24 C25 C26 N21 1.4(7) . . . . ?
C13 C17 C27 C23 1.8(8) . . . . ?
C24 C23 C27 C17 178.3(5) . . . . ?
C22 C23 C27 C17 -1.6(7) . . . . ?
C35 N31 N32 N33 0.0(5) . . . . ?
N31 N32 N33 N34 0.0(5) . . . . ?
N31 N32 N33 Re1 -175.6(3) . . . . ?
N32 N33 N34 C35 0.0(5) . . . . ?
Re1 N33 N34 C35 175.1(3) . . . . ?
N33 N34 C35 N31 0.0(5) . . . . ?
N33 N34 C35 C41 179.9(4) . . . . ?
N32 N31 C35 N34 0.0(5) . . . . ?
N32 N31 C35 C41 -179.9(4) . . . . ?
N34 C35 C41 C46 -18.0(7) . . . . ?
N31 C35 C41 C46 161.9(5) . . . . ?
N34 C35 C41 C42 161.4(5) . . . . ?
N31 C35 C41 C42 -18.7(7) . . . . ?
C46 C41 C42 C43 -3.2(8) . . . . ?
C35 C41 C42 C43 177.5(5) . . . . ?
C41 C42 C43 C44 2.2(8) . . . . ?
C42 C43 C44 C45 0.6(8) . . . . ?
C42 C43 C44 C47 179.5(5) . . . . ?
C43 C44 C45 C46 -2.3(8) . . . . ?
C47 C44 C45 C46 178.7(5) . . . . ?
C42 C41 C46 C45 1.4(7) . . . . ?
C35 C41 C46 C45 -179.3(5) . . . . ?
C44 C45 C46 C41 1.3(8) . . . . ?
C43 C44 C47 O47 -146.4(5) . . . . ?
C45 C44 C47 O47 32.5(7) . . . . ?
C43 C44 C47 N48 33.1(7) . . . . ?
C45 C44 C47 N48 -148.0(5) . . . . ?
O47 C47 N48 C49 -2.8(8) . . . . ?
C44 C47 N48 C49 177.7(4) . . . . ?
C47 N48 C49 C50 -98.6(5) . . . . ?
N48 C49 C50 N51 -175.7(4) . . . . ?
C49 C50 N51 C56 170.5(4) . . . . ?
C49 C50 N51 C52 -68.4(6) . . . . ?
C50 N51 C52 C53 -179.7(4) . . . . ?
C56 N51 C52 C53 -58.5(6) . . . . ?
N51 C52 C53 O54 57.6(6) . . . . ?
C52 C53 O54 C55 -56.2(6) . . . . ?
C53 O54 C55 C56 56.5(6) . . . . ?
C50 N51 C56 C55 -179.4(4) . . . . ?
C52 N51 C56 C55 58.1(6) . . . . ?
O54 C55 C56 N51 -57.9(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15 Cl1 0.95 2.83 3.507(6) 128.7 2_777 yes
C16 H16 N34 0.95 2.66 3.471(6) 143.7 2_767 yes
N48 H48 N31 0.88 2.21 2.990(6) 147.9 2_666 yes
C49 H49B Cl1 0.99 2.81 3.656(6) 143.2 2_776 yes
C50 H50B Cl2 0.99 2.91 3.846(6) 158.6 . yes
C52 H52B Cl2 0.99 2.91 3.829(6) 153.9 . yes
C1 H1B O47 0.99 2.31 3.205(9) 150.6 2_776 yes
C1 H1A O47 0.99 2.10 3.082(8) 171.8 . yes

# SQUEEZE RESULTS (Version = 120716)
# 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 0.500 0.500 102 41 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_refine_diff_density_max         4.132
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.153

####################################################################### 
# 
# 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_cmpnd04
_database_code_depnum_ccdc_archive 'CCDC 1908896'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2019-04-09 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H22 N7 O4 Re [+solvent]'
_chemical_formula_sum            'C27 H22 N7 O4 Re [+solvent]'
_chemical_formula_weight         694.71

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'
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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.7738(4)
_cell_length_b                   9.4891(3)
_cell_length_c                   22.3890(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.512(3)
_cell_angle_gamma                90
_cell_volume                     2711.20(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5778
_cell_measurement_theta_min      2.346
_cell_measurement_theta_max      27.356
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0484083
_diffrn_orient_matrix_UB_12      -0.0012325
_diffrn_orient_matrix_UB_13      0.0143306
_diffrn_orient_matrix_UB_21      -0.0271107
_diffrn_orient_matrix_UB_22      -0.0079148
_diffrn_orient_matrix_UB_23      -0.0281568
_diffrn_orient_matrix_UB_31      0.0036439
_diffrn_orient_matrix_UB_32      -0.0742903
_diffrn_orient_matrix_UB_33      0.0027455

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    4.528
_shelx_estimated_absorpt_T_min   0.262
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31399
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_reflns_number            21273
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.331
_diffrn_reflns_theta_max         28.668
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6354
_reflns_number_gt                4568
_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.

 Residual electron density in the crystal which could not be interpreted
 as chemically reasonable moieties was effectively removed by use
 of the program SQUEEZE.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2015/1 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_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)+(0.0515P)²] 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         6354
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.72146(2) 0.69856(2) 0.07763(2) 0.03531(10) Uani 1 1 d . . . . .
O101 O 0.7841(4) 0.4594(5) -0.0062(2) 0.0531(12) Uani 1 1 d . . . . .
C101 C 0.7594(5) 0.5475(7) 0.0262(3) 0.0433(15) Uani 1 1 d . . . . .
O102 O 0.9216(3) 0.6480(5) 0.1558(2) 0.0495(11) Uani 1 1 d . . . . .
C102 C 0.8470(5) 0.6648(6) 0.1263(3) 0.0394(14) Uani 1 1 d . . . . .
O103 O 0.8525(3) 0.8882(5) -0.0012(2) 0.0497(11) Uani 1 1 d . . . . .
C103 C 0.8025(5) 0.8177(6) 0.0281(3) 0.0397(14) Uani 1 1 d . . . . .
N11 N 0.5706(4) 0.7492(5) 0.0334(2) 0.0361(11) Uani 1 1 d . . . . .
C12 C 0.5130(5) 0.8473(6) 0.0633(3) 0.0359(13) Uani 1 1 d . . . . .
C13 C 0.4099(4) 0.8836(6) 0.0446(3) 0.0392(14) Uani 1 1 d . . . . .
C14 C 0.3672(5) 0.8185(6) -0.0073(3) 0.0432(16) Uani 1 1 d . . . . .
H14 H 0.297788 0.839621 -0.021509 0.052 Uiso 1 1 calc R U . . .
C15 C 0.4275(5) 0.7232(6) -0.0372(3) 0.0427(15) Uani 1 1 d . . . . .
H15 H 0.400554 0.679996 -0.072969 0.051 Uiso 1 1 calc R U . . .
C16 C 0.5266(5) 0.6912(6) -0.0152(3) 0.0407(14) Uani 1 1 d . . . . .
H16 H 0.565806 0.623570 -0.036089 0.049 Uiso 1 1 calc R U . . .
C17 C 0.3553(5) 0.9842(6) 0.0790(3) 0.0455(15) Uani 1 1 d . . . . .
H17 H 0.284106 1.005287 0.068592 0.055 Uiso 1 1 calc R U . . .
N21 N 0.6617(4) 0.8701(5) 0.1309(2) 0.0357(11) Uani 1 1 d . . . . .
C22 C 0.5618(4) 0.9130(6) 0.1143(3) 0.0345(13) Uani 1 1 d . . . . .
C23 C 0.5095(5) 1.0165(6) 0.1451(3) 0.0379(14) Uani 1 1 d . . . . .
C24 C 0.5638(5) 1.0836(6) 0.1936(3) 0.0432(15) Uani 1 1 d . . . . .
H24 H 0.530962 1.156112 0.215292 0.052 Uiso 1 1 calc R U . . .
C25 C 0.6634(5) 1.0432(6) 0.2087(3) 0.0431(15) Uani 1 1 d . . . . .
H25 H 0.700957 1.087660 0.241003 0.052 Uiso 1 1 calc R U . . .
C26 C 0.7107(4) 0.9355(6) 0.1764(3) 0.0387(14) Uani 1 1 d . . . . .
H26 H 0.780496 0.908503 0.187539 0.046 Uiso 1 1 calc R U . . .
C27 C 0.4031(5) 1.0493(6) 0.1260(3) 0.0452(16) Uani 1 1 d . . . . .
H27 H 0.365873 1.118772 0.147061 0.054 Uiso 1 1 calc R U . . .
N31 N 0.5852(4) 0.4386(5) 0.2086(2) 0.0402(12) Uani 1 1 d . . . . .
N32 N 0.6647(4) 0.5005(5) 0.1817(2) 0.0383(11) Uani 1 1 d . . . . .
N33 N 0.6262(4) 0.5702(5) 0.1349(2) 0.0363(11) Uani 1 1 d . . . . .
N34 N 0.5210(4) 0.5573(5) 0.1301(2) 0.0385(12) Uani 1 1 d . . . . .
C35 C 0.4998(4) 0.4752(5) 0.1762(3) 0.0336(13) Uani 1 1 d . . . . .
C41 C 0.3916(4) 0.4288(5) 0.1887(3) 0.0353(13) Uani 1 1 d . . . . .
C42 C 0.3727(5) 0.3511(6) 0.2397(3) 0.0413(14) Uani 1 1 d . . . . .
H42 H 0.428480 0.328649 0.267545 0.050 Uiso 1 1 calc R U . . .
C43 C 0.2707(5) 0.3062(6) 0.2496(3) 0.0448(16) Uani 1 1 d . . . . .
H43 H 0.258738 0.251472 0.284218 0.054 Uiso 1 1 calc R U . . .
C44 C 0.1867(5) 0.3383(6) 0.2111(3) 0.0438(16) Uani 1 1 d . . . . .
C45 C 0.2068(5) 0.4201(6) 0.1594(3) 0.0449(15) Uani 1 1 d . . . . .
H45 H 0.151009 0.445257 0.132065 0.054 Uiso 1 1 calc R U . . .
C46 C 0.3084(5) 0.4629(6) 0.1494(3) 0.0411(14) Uani 1 1 d . . . . .
H46 H 0.321373 0.516843 0.114800 0.049 Uiso 1 1 calc R U . . .
C47 C 0.0756(6) 0.2975(7) 0.2238(3) 0.0526(17) Uani 1 1 d . . . . .
H47A H 0.077174 0.210886 0.248487 0.063 Uiso 1 1 calc R U . . .
H47B H 0.044114 0.373360 0.247488 0.063 Uiso 1 1 calc R U . . .
N51 N 0.0095(4) 0.2729(5) 0.1706(3) 0.0445(13) Uani 1 1 d . . . . .
C52 C -0.1010(5) 0.2708(7) 0.1850(3) 0.0484(16) Uani 1 1 d . . . . .
H52A H -0.119681 0.360522 0.204455 0.058 Uiso 1 1 calc R U . . .
H52B H -0.113771 0.192876 0.213239 0.058 Uiso 1 1 calc R U . . .
C53 C -0.1679(5) 0.2508(7) 0.1285(3) 0.0434(15) Uani 1 1 d . . . . .
H53A H -0.242711 0.251142 0.138350 0.052 Uiso 1 1 calc R U . . .
H53B H -0.156271 0.330533 0.101087 0.052 Uiso 1 1 calc R U . . .
O54 O -0.1451(3) 0.1253(6) 0.0999(2) 0.0661(14) Uani 1 1 d . . . . .
C55 C -0.0367(5) 0.1238(10) 0.0858(4) 0.076(3) Uani 1 1 d . . . . .
H55A H -0.023269 0.201561 0.057695 0.091 Uiso 1 1 calc R U . . .
H55B H -0.020773 0.033911 0.065650 0.091 Uiso 1 1 calc R U . . .
C56 C 0.0342(5) 0.1395(8) 0.1404(4) 0.060(2) Uani 1 1 d . . . . .
H56A H 0.024144 0.059304 0.167877 0.072 Uiso 1 1 calc R U . . .
H56B H 0.108185 0.139920 0.129041 0.072 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 C101 1.914(7) . ?
Re1 C103 1.918(6) . ?
Re1 C102 1.926(7) . ?
Re1 N21 2.176(5) . ?
Re1 N33 2.179(4) . ?
Re1 N11 2.181(5) . ?
O101 C101 1.160(7) . ?
O102 C102 1.147(7) . ?
O103 C103 1.151(7) . ?
N11 C16 1.323(8) . ?
N11 C12 1.378(8) . ?
C12 C13 1.408(8) . ?
C12 C22 1.421(8) . ?
C13 C14 1.404(8) . ?
C13 C17 1.428(8) . ?
C14 C15 1.381(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C27 1.343(8) . ?
C17 H17 0.9500 . ?
N21 C26 1.327(7) . ?
N21 C22 1.375(7) . ?
C22 C23 1.387(8) . ?
C23 C24 1.413(8) . ?
C23 C27 1.442(8) . ?
C24 C25 1.358(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.404(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
N31 C35 1.329(7) . ?
N31 N32 1.339(6) . ?
N32 N33 1.315(6) . ?
N33 N34 1.349(6) . ?
N34 C35 1.330(7) . ?
C35 C41 1.489(8) . ?
C41 C46 1.387(8) . ?
C41 C42 1.389(8) . ?
C42 C43 1.397(9) . ?
C42 H42 0.9500 . ?
C43 C44 1.381(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.426(9) . ?
C44 C47 1.510(9) . ?
C45 C46 1.387(8) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 N51 1.449(9) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
N51 C52 1.463(8) . ?
N51 C56 1.474(8) . ?
C52 C53 1.507(9) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 O54 1.389(8) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
O54 C55 1.433(8) . ?
C55 C56 1.497(10) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 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
C101 Re1 C103 86.4(3) . . ?
C101 Re1 C102 89.4(3) . . ?
C103 Re1 C102 88.2(2) . . ?
C101 Re1 N21 173.7(2) . . ?
C103 Re1 N21 95.0(2) . . ?
C102 Re1 N21 96.8(2) . . ?
C101 Re1 N33 95.6(2) . . ?
C103 Re1 N33 177.8(2) . . ?
C102 Re1 N33 92.7(2) . . ?
N21 Re1 N33 82.94(17) . . ?
C101 Re1 N11 97.7(2) . . ?
C103 Re1 N11 95.5(2) . . ?
C102 Re1 N11 172.2(2) . . ?
N21 Re1 N11 76.09(19) . . ?
N33 Re1 N11 83.40(17) . . ?
O101 C101 Re1 177.6(5) . . ?
O102 C102 Re1 178.4(6) . . ?
O103 C103 Re1 178.9(5) . . ?
C16 N11 C12 117.6(5) . . ?
C16 N11 Re1 128.1(4) . . ?
C12 N11 Re1 114.1(4) . . ?
N11 C12 C13 122.2(5) . . ?
N11 C12 C22 117.6(5) . . ?
C13 C12 C22 120.3(6) . . ?
C14 C13 C12 117.6(6) . . ?
C14 C13 C17 124.0(6) . . ?
C12 C13 C17 118.4(5) . . ?
C15 C14 C13 119.0(6) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C16 C15 C14 119.7(6) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
N11 C16 C15 123.8(6) . . ?
N11 C16 H16 118.1 . . ?
C15 C16 H16 118.1 . . ?
C27 C17 C13 121.0(6) . . ?
C27 C17 H17 119.5 . . ?
C13 C17 H17 119.5 . . ?
C26 N21 C22 118.0(5) . . ?
C26 N21 Re1 127.3(4) . . ?
C22 N21 Re1 114.7(4) . . ?
N21 C22 C23 122.5(5) . . ?
N21 C22 C12 117.1(5) . . ?
C23 C22 C12 120.4(5) . . ?
C22 C23 C24 118.1(5) . . ?
C22 C23 C27 118.2(5) . . ?
C24 C23 C27 123.7(6) . . ?
C25 C24 C23 119.1(6) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 119.9(6) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
N21 C26 C25 122.4(6) . . ?
N21 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C17 C27 C23 121.6(6) . . ?
C17 C27 H27 119.2 . . ?
C23 C27 H27 119.2 . . ?
C35 N31 N32 105.1(5) . . ?
N33 N32 N31 108.3(5) . . ?
N32 N33 N34 110.8(4) . . ?
N32 N33 Re1 123.4(4) . . ?
N34 N33 Re1 125.7(4) . . ?
C35 N34 N33 103.1(5) . . ?
N31 C35 N34 112.8(5) . . ?
N31 C35 C41 124.5(5) . . ?
N34 C35 C41 122.8(5) . . ?
C46 C41 C42 119.3(5) . . ?
C46 C41 C35 120.2(5) . . ?
C42 C41 C35 120.5(6) . . ?
C41 C42 C43 119.3(6) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C44 C43 C42 122.5(6) . . ?
C44 C43 H43 118.7 . . ?
C42 C43 H43 118.7 . . ?
C43 C44 C45 117.6(6) . . ?
C43 C44 C47 122.5(7) . . ?
C45 C44 C47 119.8(6) . . ?
C46 C45 C44 119.6(6) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C45 C46 C41 121.7(6) . . ?
C45 C46 H46 119.2 . . ?
C41 C46 H46 119.2 . . ?
N51 C47 C44 113.9(6) . . ?
N51 C47 H47A 108.8 . . ?
C44 C47 H47A 108.8 . . ?
N51 C47 H47B 108.8 . . ?
C44 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
C47 N51 C52 110.7(5) . . ?
C47 N51 C56 112.7(6) . . ?
C52 N51 C56 108.5(5) . . ?
N51 C52 C53 109.4(5) . . ?
N51 C52 H52A 109.8 . . ?
C53 C52 H52A 109.8 . . ?
N51 C52 H52B 109.8 . . ?
C53 C52 H52B 109.8 . . ?
H52A C52 H52B 108.2 . . ?
O54 C53 C52 111.8(5) . . ?
O54 C53 H53A 109.2 . . ?
C52 C53 H53A 109.2 . . ?
O54 C53 H53B 109.2 . . ?
C52 C53 H53B 109.2 . . ?
H53A C53 H53B 107.9 . . ?
C53 O54 C55 109.5(5) . . ?
O54 C55 C56 112.0(6) . . ?
O54 C55 H55A 109.2 . . ?
C56 C55 H55A 109.2 . . ?
O54 C55 H55B 109.2 . . ?
C56 C55 H55B 109.2 . . ?
H55A C55 H55B 107.9 . . ?
N51 C56 C55 109.0(6) . . ?
N51 C56 H56A 109.9 . . ?
C55 C56 H56A 109.9 . . ?
N51 C56 H56B 109.9 . . ?
C55 C56 H56B 109.9 . . ?
H56A C56 H56B 108.3 . . ?

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 N11 C12 C13 1.7(8) . . . . ?
Re1 N11 C12 C13 -174.0(4) . . . . ?
C16 N11 C12 C22 -177.9(5) . . . . ?
Re1 N11 C12 C22 6.4(6) . . . . ?
N11 C12 C13 C14 -1.6(8) . . . . ?
C22 C12 C13 C14 177.9(5) . . . . ?
N11 C12 C13 C17 178.7(5) . . . . ?
C22 C12 C13 C17 -1.8(8) . . . . ?
C12 C13 C14 C15 -0.1(8) . . . . ?
C17 C13 C14 C15 179.6(6) . . . . ?
C13 C14 C15 C16 1.6(9) . . . . ?
C12 N11 C16 C15 -0.1(9) . . . . ?
Re1 N11 C16 C15 175.0(4) . . . . ?
C14 C15 C16 N11 -1.6(9) . . . . ?
C14 C13 C17 C27 -175.6(6) . . . . ?
C12 C13 C17 C27 4.1(9) . . . . ?
C26 N21 C22 C23 -3.2(8) . . . . ?
Re1 N21 C22 C23 176.9(4) . . . . ?
C26 N21 C22 C12 176.4(5) . . . . ?
Re1 N21 C22 C12 -3.6(6) . . . . ?
N11 C12 C22 N21 -1.9(7) . . . . ?
C13 C12 C22 N21 178.5(5) . . . . ?
N11 C12 C22 C23 177.6(5) . . . . ?
C13 C12 C22 C23 -1.9(8) . . . . ?
N21 C22 C23 C24 2.9(8) . . . . ?
C12 C22 C23 C24 -176.6(5) . . . . ?
N21 C22 C23 C27 -177.1(5) . . . . ?
C12 C22 C23 C27 3.4(8) . . . . ?
C22 C23 C24 C25 -1.1(9) . . . . ?
C27 C23 C24 C25 178.9(6) . . . . ?
C23 C24 C25 C26 -0.3(9) . . . . ?
C22 N21 C26 C25 1.7(8) . . . . ?
Re1 N21 C26 C25 -178.4(4) . . . . ?
C24 C25 C26 N21 0.0(9) . . . . ?
C13 C17 C27 C23 -2.7(10) . . . . ?
C22 C23 C27 C17 -1.1(9) . . . . ?
C24 C23 C27 C17 178.9(6) . . . . ?
C35 N31 N32 N33 -0.4(6) . . . . ?
N31 N32 N33 N34 0.6(6) . . . . ?
N31 N32 N33 Re1 177.0(3) . . . . ?
N32 N33 N34 C35 -0.5(6) . . . . ?
Re1 N33 N34 C35 -176.9(4) . . . . ?
N32 N31 C35 N34 0.0(6) . . . . ?
N32 N31 C35 C41 179.1(5) . . . . ?
N33 N34 C35 N31 0.3(6) . . . . ?
N33 N34 C35 C41 -178.8(5) . . . . ?
N31 C35 C41 C46 -174.5(5) . . . . ?
N34 C35 C41 C46 4.5(8) . . . . ?
N31 C35 C41 C42 5.5(8) . . . . ?
N34 C35 C41 C42 -175.6(5) . . . . ?
C46 C41 C42 C43 1.4(8) . . . . ?
C35 C41 C42 C43 -178.5(5) . . . . ?
C41 C42 C43 C44 -1.2(9) . . . . ?
C42 C43 C44 C45 0.2(9) . . . . ?
C42 C43 C44 C47 -176.1(6) . . . . ?
C43 C44 C45 C46 0.6(9) . . . . ?
C47 C44 C45 C46 177.0(6) . . . . ?
C44 C45 C46 C41 -0.4(9) . . . . ?
C42 C41 C46 C45 -0.6(9) . . . . ?
C35 C41 C46 C45 179.3(5) . . . . ?
C43 C44 C47 N51 -150.2(6) . . . . ?
C45 C44 C47 N51 33.6(8) . . . . ?
C44 C47 N51 C52 -165.1(5) . . . . ?
C44 C47 N51 C56 73.2(7) . . . . ?
C47 N51 C52 C53 177.8(5) . . . . ?
C56 N51 C52 C53 -58.1(7) . . . . ?
N51 C52 C53 O54 60.0(7) . . . . ?
C52 C53 O54 C55 -58.7(8) . . . . ?
C53 O54 C55 C56 58.6(9) . . . . ?
C47 N51 C56 C55 -179.3(6) . . . . ?
C52 N51 C56 C55 57.7(8) . . . . ?
O54 C55 C56 N51 -58.4(9) . . . . ?

# SQUEEZE RESULTS (Version = 200818)
# 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 0.500 0.000 0.500 116 12 ' '
2 1.000 0.500 1.000 116 12 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_refine_diff_density_max         1.487
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.152

